##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section B. It has been peer reviewed under the auspices  #
# of the IUCr Commission on Journals.                                        #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary may be obtained from        #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
# cif/home.html                                                              #
#                                                                            #
#           Copyright International Union of Crystallography                 #
#                                                                            #
##############################################################################

data_global
_audit_creation_method     'from SHELXL-97 with Word-Perfect Macro PRPKAPPA'
_journal_date_recd_electronic     2001-10-16
_journal_date_accepted     2001-10-31
_journal_name_full     'Acta Crystallographica, Section B'
_journal_year     2002
_journal_volume     58
_journal_issue      1
_journal_page_first     78
_journal_page_last     93
_publ_contact_author_name
;
Dr Christopher Glidewell
;
_publ_contact_author_address
;
School of Chemistry,
University of St Andrews,
St Andrews, Fife KY16 9ST, UK
;
_publ_contact_author_email     'cg@st-andrews.ac.uk'
_publ_contact_author_fax     '01334-483808'
_publ_contact_author_phone     '01334-463839'
_publ_section_title
;
[Ni(cyclam)(OCOR)2]: a finite molecular complex; hydrogen-bonded
supramolecular aggregation in one, two and three dimensions; and
coordination polymers in one and two dimensions
;
loop_
    _publ_author_name
    _publ_author_footnote
    _publ_author_address
    'Zakaria, Choudhury M'
;   CMZ is on leave from Department of Chemistry,
    University of Rajshahi, Rajshahi, Bangladesh.
;
;    School of Chemistry,
     University of St Andrews,
     St Andrews, Fife KY16 9ST, UK
;
    'Ferguson, George' .
;    School of Chemistry,
     University of St Andrews,
     St Andrews, Fife KY16 9ST, UK
;
    'Lough, Alan J.' .
;    Lash Miller Chemical Laboratories,
     University of Toronto,
     Toronto, Ontario, Canada M5S 3H6
;
    'Glidewell, Christopher' .
;    School of Chemistry,
     University of St Andrews,
     St Andrews, Fife KY16 9ST, UK
;
data_I
_chemical_name_systematic
;
Bis-(2-naphthoato)-1,4,8,11-tetraazacyclotetradecanenickel(II)
;
_chemical_name_common     ?
_chemical_formula_moiety     'C32 H38 N4 Ni O4'
_chemical_formula_sum     'C32 H38 N4 Ni O4'
_chemical_formula_weight     601.37
_chemical_melting_point     ?
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'P21/c'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, y+1/2, -z+1/2'
    '-x, -y, -z'
    'x, -y-1/2, z-1/2'
_cell_length_a     11.4970(4)
_cell_length_b     10.6563(4)
_cell_length_c     11.9407(4)
_cell_angle_alpha     90.00
_cell_angle_beta     92.2080(17)
_cell_angle_gamma     90.00
_cell_volume     1461.83(9)
_cell_formula_units_Z     2
_cell_measurement_reflns_used     3144
_cell_measurement_theta_min     2.61
_cell_measurement_theta_max     27.51
_cell_measurement_temperature     150(2)
_exptl_crystal_description     block
_exptl_crystal_colour     purple
_exptl_crystal_size_max      .36
_exptl_crystal_size_mid      .26
_exptl_crystal_size_min      .18
_exptl_crystal_density_diffrn     1.366
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     636
_exptl_absorpt_coefficient_mu      .707
_exptl_absorpt_correction_type     Multi-scan
_exptl_absorpt_process_details     'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min      .7848
_exptl_absorpt_correction_T_max      .8832
_exptl_special_details
;
 The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling
 algorithm [Fox, G.C. & Holmes, K.C. (1966).  Acta Cryst. 20,
 886-891] which effectively corrects for
 absorption effects. High redundancy data were used in the scaling
 program hence the 'multi-scan' code word was used. No transmission
 coefficients are available from the program (only scale factors for each
 frame). The scale factors in the experimental table are calculated
 from the 'size' command in the SHELXL-97 input file.
;
_diffrn_ambient_temperature     150(2)
_diffrn_radiation_type     'Mo K\a'
_diffrn_radiation_wavelength      .71073
_diffrn_radiation_source     'fine-focus sealed X-ray tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Kappa-CCD'
_diffrn_measurement_method     'φ scans, and ω scans with κ offsets'
_diffrn_reflns_number     9394
_diffrn_reflns_av_R_equivalents      .022
_diffrn_reflns_av_sigmaI/netI      .0421
_diffrn_reflns_theta_min     2.61
_diffrn_reflns_theta_max     27.51
_diffrn_reflns_theta_full     27.51
_diffrn_measured_fraction_theta_max      .992
_diffrn_measured_fraction_theta_full      .992
_diffrn_reflns_limit_h_min     0
_diffrn_reflns_limit_h_max     14
_diffrn_reflns_limit_k_min     0
_diffrn_reflns_limit_k_max     13
_diffrn_reflns_limit_l_min     -15
_diffrn_reflns_limit_l_max     15
_diffrn_standards_decay_%     negligible
_reflns_number_total     3328
_reflns_number_gt     2895
_reflns_threshold_expression     >2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all      .0363
_refine_ls_R_factor_gt      .0297
_refine_ls_wR_factor_gt      .0725
_refine_ls_wR_factor_ref      .0765
_refine_ls_goodness_of_fit_ref     1.029
_refine_ls_restrained_S_all     1.029
_refine_ls_number_reflns     3328
_refine_ls_number_parameters     187
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
              'w=1/[σ²(Fo²)+(0.0155P)²+0.7435P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max      .001
_refine_ls_shift/su_mean      .000
_refine_diff_density_max      .287
_refine_diff_density_min      -.367
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'C' 'C'  .0033  .0016
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'H' 'H'  .0000  .0000
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'N' 'N'  .0061  .0033
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Ni' 'Ni'  .3393 1.1124
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'O' 'O'  .0106  .0060
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'Kappa-CCD server software (Nonius, 1997)'
_computing_cell_refinement     'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction     'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)'
_computing_structure_refinement     'SHELXL-97 (Sheldrick, 1997b)'
_computing_molecular_graphics     'PLATON (Spek, 20001)'
_computing_publication_material
                    'SHELXL-97 (Sheldrick, 1997b) and PRPKAPPA (Ferguson, 1999)'
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Ni1  .5000  .5000  .5000  .01919(9) Uani d S 1 . . Ni
    O1  .39898(9)  .34617(10)  .54652(8)  .0268(2) Uani d . 1 . . O
    O2  .39786(11)  .22396(11)  .39435(10)  .0384(3) Uani d . 1 . . O
    C11  .24257(12)  .19082(13)  .64991(12)  .0217(3) Uani d . 1 . . C
    C12  .27874(12)  .16666(13)  .54398(12)  .0210(3) Uani d . 1 . . C
    C13  .23432(13)  .06007(14)  .48509(13)  .0270(3) Uani d . 1 . . C
    C14  .15576(14)  -.01766(15)  .53301(14)  .0308(3) Uani d . 1 . . C
    C15  .11721(13)  .00529(14)  .64248(14)  .0275(3) Uani d . 1 . . C
    C16  .03531(15)  -.07267(17)  .69482(16)  .0396(4) Uani d . 1 . . C
    C17  -.00158(16)  -.0457(2)  .79955(17)  .0442(5) Uani d . 1 . . C
    C18  .04227(15)  .05950(18)  .85834(15)  .0383(4) Uani d . 1 . . C
    C19  .12280(13)  .13622(15)  .81110(13)  .0290(3) Uani d . 1 . . C
    C110  .16119(12)  .11186(14)  .70172(12)  .0232(3) Uani d . 1 . . C
    C111  .36627(12)  .25133(13)  .48961(12)  .0220(3) Uani d . 1 . . C
    N1  .60752(11)  .39074(12)  .40417(10)  .0245(3) Uani d . 1 . . N
    C2  .71607(14)  .37508(17)  .47247(14)  .0325(4) Uani d . 1 . . C
    C3  .68618(14)  .35421(17)  .59425(14)  .0334(4) Uani d . 1 . . C
    N4  .61582(11)  .46044(13)  .63234(10)  .0263(3) Uani d . 1 . . N
    C5  .56383(14)  .43833(16)  .74220(12)  .0302(3) Uani d . 1 . . C
    C6  .48728(14)  .54690(16)  .77773(12)  .0312(3) Uani d . 1 . . C
    C7  .37303(14)  .56273(15)  .71011(12)  .0286(3) Uani d . 1 . . C
    H11  .2726  .2619  .6894  .026 Uiso calc R 1 . . H
    H13  .2594  .0427  .4118  .032 Uiso calc R 1 . . H
    H14  .1265  -.0882  .4923  .037 Uiso calc R 1 . . H
    H16  .0057  -.1447  .6565  .048 Uiso calc R 1 . . H
    H17  -.0572  -.0984  .8329  .053 Uiso calc R 1 . . H
    H18  .0161  .0776  .9311  .046 Uiso calc R 1 . . H
    H19  .1531  .2062  .8520  .035 Uiso calc R 1 . . H
    H1  .5731  .3120  .3970  .029 Uiso calc R 1 . . H
    H2A  .7652  .4509  .4664  .039 Uiso calc R 1 . . H
    H2B  .7603  .3023  .4450  .039 Uiso calc R 1 . . H
    H3A  .6420  .2750  .6011  .040 Uiso calc R 1 . . H
    H3B  .7586  .3474  .6415  .040 Uiso calc R 1 . . H
    H4  .6654  .5290  .6408  .032 Uiso calc R 1 . . H
    H5A  .6270  .4255  .7998  .036 Uiso calc R 1 . . H
    H5B  .5166  .3607  .7380  .036 Uiso calc R 1 . . H
    H6A  .5324  .6256  .7724  .037 Uiso calc R 1 . . H
    H6B  .4693  .5350  .8574  .037 Uiso calc R 1 . . H
    H7A  .3322  .4810  .7053  .034 Uiso calc R 1 . . H
    H7B  .3226  .6226  .7491  .034 Uiso calc R 1 . . H
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Ni1 N4 3_666 2.070(2) no
    Ni1 N4 . 2.070(2) no
    Ni1 N1 3_666 2.074(2) no
    Ni1 N1 . 2.074(2) no
    Ni1 O1 3_666 2.096(2) no
    Ni1 O1 . 2.096(2) no
    O1 C111 . 1.267(2) no
    O2 C111 . 1.242(2) no
    C11 C12 . 1.371(2) no
    C11 C110 . 1.418(2) no
    C11 H11 .  .95 no
    C12 C13 . 1.420(2) no
    C12 C111 . 1.516(2) no
    C13 C14 . 1.367(2) no
    C13 H13 .  .95 no
    C14 C15 . 1.418(2) no
    C14 H14 .  .95 no
    C15 C16 . 1.419(2) no
    C15 C110 . 1.421(2) no
    C16 C17 . 1.367(3) no
    C16 H16 .  .95 no
    C17 C18 . 1.406(3) no
    C17 H17 .  .95 no
    C18 C19 . 1.373(2) no
    C18 H18 .  .95 no
    C19 C110 . 1.419(2) no
    C19 H19 .  .95 no
    N1 C2 . 1.474(2) no
    N1 C7 3_666 1.477(2) no
    N1 H1 .  .93 no
    C2 C3 . 1.523(2) no
    C2 H2A .  .99 no
    C2 H2B .  .99 no
    C3 N4 . 1.473(2) no
    C3 H3A .  .99 no
    C3 H3B .  .99 no
    N4 C5 . 1.481(2) no
    N4 H4 .  .93 no
    C5 C6 . 1.524(2) no
    C5 H5A .  .99 no
    C5 H5B .  .99 no
    C6 C7 . 1.524(2) no
    C6 H6A .  .99 no
    C6 H6B .  .99 no
    C7 N1 3_666 1.477(2) no
    C7 H7A .  .99 no
    C7 H7B .  .99 no
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    N4 Ni1 N4 3_666 . 180.0 no
    N4 Ni1 N1 3_666 3_666 85.83(5) no
    N4 Ni1 N1 . 3_666 94.17(5) no
    N4 Ni1 N1 3_666 . 94.17(5) no
    N4 Ni1 N1 . . 85.83(5) no
    N1 Ni1 N1 3_666 . 180.0 no
    N4 Ni1 O1 3_666 3_666 89.15(5) no
    N4 Ni1 O1 . 3_666 90.85(5) no
    N1 Ni1 O1 3_666 3_666 93.17(4) no
    N1 Ni1 O1 . 3_666 86.83(4) no
    N4 Ni1 O1 3_666 . 90.85(5) no
    N4 Ni1 O1 . . 89.15(5) no
    N1 Ni1 O1 3_666 . 86.83(4) no
    N1 Ni1 O1 . . 93.17(4) no
    O1 Ni1 O1 3_666 . 180.0 no
    C111 O1 Ni1 . . 129.63(9) no
    C12 C11 C110 . . 121.3(2) no
    C12 C11 H11 . . 119.3 no
    C110 C11 H11 . . 119.3 no
    C11 C12 C13 . . 119.4(2) no
    C11 C12 C111 . . 120.9(2) no
    C13 C12 C111 . . 119.7(2) no
    C14 C13 C12 . . 120.5(2) no
    C14 C13 H13 . . 119.7 no
    C12 C13 H13 . . 119.7 no
    C13 C14 C15 . . 121.1(2) no
    C13 C14 H14 . . 119.5 no
    C15 C14 H14 . . 119.5 no
    C14 C15 C16 . . 122.8(2) no
    C14 C15 C110 . . 118.6(2) no
    C16 C15 C110 . . 118.6(2) no
    C17 C16 C15 . . 121.0(2) no
    C17 C16 H16 . . 119.5 no
    C15 C16 H16 . . 119.5 no
    C16 C17 C18 . . 120.5(2) no
    C16 C17 H17 . . 119.8 no
    C18 C17 H17 . . 119.8 no
    C19 C18 C17 . . 120.3(2) no
    C19 C18 H18 . . 119.9 no
    C17 C18 H18 . . 119.9 no
    C18 C19 C110 . . 120.5(2) no
    C18 C19 H19 . . 119.7 no
    C110 C19 H19 . . 119.7 no
    C11 C110 C19 . . 121.8(2) no
    C11 C110 C15 . . 119.0(2) no
    C19 C110 C15 . . 119.2(2) no
    O2 C111 O1 . . 126.0(12) no
    O2 C111 C12 . . 118.3(2) no
    O1 C111 C12 . . 115.7(2) no
    C2 N1 C7 . 3_666 113.2(2) no
    C2 N1 Ni1 . . 105.56(9) no
    C7 N1 Ni1 3_666 . 115.8(2) no
    C2 N1 H1 . . 107.3 no
    C7 N1 H1 3_666 . 107.3 no
    Ni1 N1 H1 . . 107.3 no
    N1 C2 C3 . . 109.1(2) no
    N1 C2 H2A . . 109.9 no
    C3 C2 H2A . . 109.9 no
    N1 C2 H2B . . 109.9 no
    C3 C2 H2B . . 109.9 no
    H2A C2 H2B . . 108.3 no
    N4 C3 C2 . . 109.2(2) no
    N4 C3 H3A . . 109.8 no
    C2 C3 H3A . . 109.8 no
    N4 C3 H3B . . 109.8 no
    C2 C3 H3B . . 109.8 no
    H3A C3 H3B . . 108.3 no
    C3 N4 C5 . . 113.4(2) no
    C3 N4 Ni1 . . 105.41(9) no
    C5 N4 Ni1 . . 116.02(9) no
    C3 N4 H4 . . 107.2 no
    C5 N4 H4 . . 107.2 no
    Ni1 N4 H4 . . 107.2 no
    N4 C5 C6 . . 112.5(2) no
    N4 C5 H5A . . 109.1 no
    C6 C5 H5A . . 109.1 no
    N4 C5 H5B . . 109.1 no
    C6 C5 H5B . . 109.1 no
    H5A C5 H5B . . 107.8 no
    C5 C6 C7 . . 115.6(2) no
    C5 C6 H6A . . 108.4 no
    C7 C6 H6A . . 108.4 no
    C5 C6 H6B . . 108.4 no
    C7 C6 H6B . . 108.4 no
    H6A C6 H6B . . 107.4 no
    N1 C7 C6 3_666 . 111.6(2) no
    N1 C7 H7A 3_666 . 109.3 no
    C6 C7 H7A . . 109.3 no
    N1 C7 H7B 3_666 . 109.3 no
    C6 C7 H7B . . 109.3 no
    H7A C7 H7B . . 108.0 no
loop_
    _geom_torsion_atom_site_label_1
    _geom_torsion_atom_site_label_2
    _geom_torsion_atom_site_label_3
    _geom_torsion_atom_site_label_4
    _geom_torsion_site_symmetry_1
    _geom_torsion_site_symmetry_2
    _geom_torsion_site_symmetry_3
    _geom_torsion_site_symmetry_4
    _geom_torsion
    _geom_torsion_publ_flag
    N4 Ni1 O1 C111 3_666 . . . 56.5(2) no
    N4 Ni1 O1 C111 . . . . -123.5(2) no
    N1 Ni1 O1 C111 3_666 . . . 142.3(3) no
    N1 Ni1 O1 C111 . . . . -37.7(2) no
    C110 C11 C12 C13 . . . .  -.3(2) no
    C110 C11 C12 C111 . . . . -179.7(2) no
    C11 C12 C13 C14 . . . .  .3(2) no
    C111 C12 C13 C14 . . . . 179.7(2) no
    C12 C13 C14 C15 . . . .  -.4(2) no
    C13 C14 C15 C16 . . . . 179.6(2) no
    C13 C14 C15 C110 . . . .  .5(2) no
    C14 C15 C16 C17 . . . . -178.5(2) no
    C110 C15 C16 C17 . . . .  .6(3) no
    C15 C16 C17 C18 . . . .  -.8(3) no
    C16 C17 C18 C19 . . . .  -.1(3) no
    C17 C18 C19 C110 . . . . 1.2(2) no
    C12 C11 C110 C19 . . . . -179.7(2) no
    C12 C11 C110 C15 . . . .  .4(2) no
    C18 C19 C110 C11 . . . . 178.8(2) no
    C18 C19 C110 C15 . . . . -1.4(2) no
    C14 C15 C110 C11 . . . .  -.5(2) no
    C16 C15 C110 C11 . . . . -179.6(2) no
    C14 C15 C110 C19 . . . . 179.7(2) no
    C16 C15 C110 C19 . . . .  .5(2) no
    Ni1 O1 C111 O2 . . . . 7.4(2) no
    Ni1 O1 C111 C12 . . . . -171.29(9) no
    C11 C12 C111 O2 . . . . 178.6(2) no
    C13 C12 C111 O2 . . . .  -.7(2) no
    C11 C12 C111 O1 . . . . -2.5(2) no
    C13 C12 C111 O1 . . . . 178.1(2) no
    N4 Ni1 N1 C2 3_666 . . . 165.9(2) no
    N4 Ni1 N1 C2 . . . . -14.1(2) no
    O1 Ni1 N1 C2 3_666 . . . 77.03(9) no
    O1 Ni1 N1 C2 . . . . -103.0(2) no
    N4 Ni1 N1 C7 3_666 . . 3_666 39.8(2) no
    N4 Ni1 N1 C7 . . . 3_666 -140.2(2) no
    O1 Ni1 N1 C7 3_666 . . 3_666 -49.1(2) no
    O1 Ni1 N1 C7 . . . 3_666 130.9(2) no
    C7 N1 C2 C3 3_666 . . . 168.1(2) no
    Ni1 N1 C2 C3 . . . . 40.4(2) no
    N1 C2 C3 N4 . . . . -56.9(2) no
    C2 C3 N4 C5 . . . . 169.2(2) no
    C2 C3 N4 Ni1 . . . . 41.3(2) no
    N1 Ni1 N4 C3 3_666 . . . 164.86(9) no
    N1 Ni1 N4 C3 . . . . -15.14(9) no
    O1 Ni1 N4 C3 3_666 . . . -101.90(9) no
    O1 Ni1 N4 C3 . . . . 78.10(9) no
    N1 Ni1 N4 C5 3_666 . . . 38.9(2) no
    N1 Ni1 N4 C5 . . . . -141.4(2) no
    O1 Ni1 N4 C5 3_666 . . . 131.8(2) no
    O1 Ni1 N4 C5 . . . . -48.2(2) no
    C3 N4 C5 C6 . . . . -177.6(2) no
    Ni1 N4 C5 C6 . . . . -55.4(2) no
    N4 C5 C6 C7 . . . . 70.1(2) no
    C5 C6 C7 N1 . . . 3_666 -71.1(2) no
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    _geom_hbond_publ_flag
    N1 H1 O2 .  .93 2.22 2.994(2) 140 y
data_II
_chemical_name_systematic
;
Bis-(3,5-dinitrobenzoato)-1,4,8,11-tetraazacyclotetradecanenickel(II)
;
_chemical_name_common     ?
_chemical_formula_moiety     'C24 H30 N8 Ni O12'
_chemical_formula_sum     'C24 H30 N8 Ni O12'
_chemical_formula_weight     681.27
_chemical_melting_point     ?
_symmetry_cell_setting     triclinic
_symmetry_space_group_name_H-M     'P-1'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, -y, -z'
_cell_length_a     7.7663(3)
_cell_length_b     9.7845(6)
_cell_length_c     10.4026(7)
_cell_angle_alpha     99.826(2)
_cell_angle_beta     97.966(2)
_cell_angle_gamma     108.388(2)
_cell_volume     723.30(7)
_cell_formula_units_Z     1
_cell_measurement_reflns_used     5718
_cell_measurement_theta_min     2.82
_cell_measurement_theta_max     27.19
_cell_measurement_temperature     293(2)
_exptl_crystal_description     plate
_exptl_crystal_colour     colourless
_exptl_crystal_size_max      .30
_exptl_crystal_size_mid      .24
_exptl_crystal_size_min      .02
_exptl_crystal_density_diffrn     1.564
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     354
_exptl_absorpt_coefficient_mu      .748
_exptl_absorpt_correction_type     Multi-scan
_exptl_absorpt_process_details     'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min      .8067
_exptl_absorpt_correction_T_max      .9852
_exptl_special_details
;
 The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling
 algorithm [Fox, G.C. & Holmes, K.C. (1966).  Acta Cryst. 20,
 886-891]which effectively corrects for
 absorption effects. High redundancy data were used in the scaling
 program hence the 'multi-scan' code word was used. No transmission
 coefficients are available from the program (only scale factors for each
 frame). The scale factors in the experimental table are calculated
 from the 'size' command in the SHELXL-97 input file.
;
_diffrn_ambient_temperature     293(2)
_diffrn_radiation_type     'Mo K\a'
_diffrn_radiation_wavelength      .71073
_diffrn_radiation_source     'fine-focus sealed X-ray tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Kappa-CCD'
_diffrn_measurement_method     'φ scans, and ω scans with κ offsets'
_diffrn_reflns_number     17662
_diffrn_reflns_av_R_equivalents      .075
_diffrn_reflns_av_sigmaI/netI      .0638
_diffrn_reflns_theta_min     2.82
_diffrn_reflns_theta_max     27.19
_diffrn_reflns_theta_full     25.50
_diffrn_measured_fraction_theta_max      .972
_diffrn_measured_fraction_theta_full      .986
_diffrn_reflns_limit_h_min     0
_diffrn_reflns_limit_h_max     9
_diffrn_reflns_limit_k_min     -12
_diffrn_reflns_limit_k_max     11
_diffrn_reflns_limit_l_min     -13
_diffrn_reflns_limit_l_max     13
_diffrn_standards_decay_%     negligible
_reflns_number_total     3135
_reflns_number_gt     2560
_reflns_threshold_expression     >2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all      .0578
_refine_ls_R_factor_gt      .0421
_refine_ls_wR_factor_gt      .0887
_refine_ls_wR_factor_ref      .0968
_refine_ls_goodness_of_fit_ref     1.055
_refine_ls_restrained_S_all     1.055
_refine_ls_number_reflns     3135
_refine_ls_number_parameters     206
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
                      'w=1/[σ²(Fo²)P)²+0.3293P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max      .000
_refine_ls_shift/su_mean      .000
_refine_diff_density_max      .285
_refine_diff_density_min      -.431
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef      .013(3)
_refine_ls_extinction_expression
                                  'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'C' 'C'  .0033  .0016
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'H' 'H'  .0000  .0000
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'N' 'N'  .0061  .0033
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Ni' 'Ni'  .3393 1.1124
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'O' 'O'  .0106  .0060
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'Kappa-CCD server software (Nonius, 1997)'
_computing_cell_refinement     'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction     'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)'
_computing_structure_refinement     'SHELXL-97 (Sheldrick, 1997b)'
_computing_molecular_graphics     ' PLATON (Spek, 2001)'
_computing_publication_material
                    'SHELXL-97 (Sheldrick, 1997b) and PRPKAPPA (Ferguson, 1999)'
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Ni1  .5000  .5000  .5000  .03420(15) Uani d S 1 . . Ni
    N1  .2732(3)  .5215(2)  .57420(19)  .0407(5) Uani d . 1 . . N
    C2  .2156(4)  .4009(3)  .6446(3)  .0529(7) Uani d . 1 . . C
    C3  .2281(4)  .2618(3)  .5626(3)  .0538(7) Uani d . 1 . . C
    N4  .4181(3)  .2920(2)  .5391(2)  .0415(5) Uani d . 1 . . N
    C5  .4378(4)  .1739(3)  .4400(3)  .0469(6) Uani d . 1 . . C
    C6  .6350(4)  .2085(3)  .4189(3)  .0494(6) Uani d . 1 . . C
    C7  .7033(4)  .3306(3)  .3461(3)  .0484(6) Uani d . 1 . . C
    O11  .3435(2)  .40263(19)  .30221(16)  .0456(4) Uani d . 1 . . O
    O12  .1530(2)  .5311(2)  .28440(18)  .0547(5) Uani d . 1 . . O
    O32  .0894(3)  -.0360(3)  -.2587(2)  .0800(7) Uani d . 1 . . O
    O31  .2989(3)  .0153(2)  -.0804(2)  .0681(6) Uani d . 1 . . O
    O51  -.3909(3)  .3286(3)  -.0794(2)  .0696(6) Uani d . 1 . . O
    O52  -.4066(3)  .1585(2)  -.2464(2)  .0704(6) Uani d . 1 . . O
    N3  .1675(4)  .0330(2)  -.1442(2)  .0537(6) Uani d . 1 . . N
    N5  -.3274(3)  .2430(3)  -.1391(2)  .0520(6) Uani d . 1 . . N
    C11  .1133(3)  .3314(2)  .1059(2)  .0362(5) Uani d . 1 . . C
    C12  .1873(3)  .2326(3)  .0429(2)  .0402(5) Uani d . 1 . . C
    C13  .0918(3)  .1419(3)  -.0800(2)  .0422(6) Uani d . 1 . . C
    C14  -.0744(4)  .1447(3)  -.1438(2)  .0454(6) Uani d . 1 . . C
    C15  -.1450(3)  .2432(3)  -.0773(2)  .0406(5) Uani d . 1 . . C
    C16  -.0543(3)  .3368(3)  .0452(2)  .0387(5) Uani d . 1 . . C
    C17  .2114(3)  .4321(3)  .2431(2)  .0373(5) Uani d . 1 . . C
    H1  .1802  .5011  .5024  .049 Uiso calc R 1 . . H
    H2A  .0894  .3839  .6563  .063 Uiso calc R 1 . . H
    H2B  .2958  .4277  .7319  .063 Uiso calc R 1 . . H
    H3A  .1973  .1828  .6097  .065 Uiso calc R 1 . . H
    H3B  .1406  .2307  .4781  .065 Uiso calc R 1 . . H
    H4  .4912  .2983  .6178  .050 Uiso calc R 1 . . H
    H5A  .3560  .1601  .3558  .056 Uiso calc R 1 . . H
    H5B  .3999  .0820  .4694  .056 Uiso calc R 1 . . H
    H6A  .6451  .1189  .3693  .059 Uiso calc R 1 . . H
    H6B  .7172  .2355  .5054  .059 Uiso calc R 1 . . H
    H7A  .8211  .3316  .3244  .058 Uiso calc R 1 . . H
    H7B  .6156  .3098  .2631  .058 Uiso calc R 1 . . H
    H12  .2993  .2276  .0829  .048 Uiso calc R 1 . . H
    H14  -.1359  .0836  -.2272  .055 Uiso calc R 1 . . H
    H16  -.1049  .4026  .0865  .046 Uiso calc R 1 . . H
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Ni1 N1 . 2.073(2) no
    Ni1 N1 2_666 2.073(2) no
    Ni1 N4 . 2.062(2) no
    Ni1 N4 2_666 2.062(2) no
    Ni1 O11 2_666 2.127(2) no
    Ni1 O11 . 2.127(2) no
    N1 C2 . 1.477(3) no
    N1 C7 2_666 1.482(3) no
    N1 H1 .  .91 no
    C2 C3 . 1.516(4) no
    C2 H2A .  .97 no
    C2 H2B .  .97 no
    C3 N4 . 1.474(3) no
    C3 H3A .  .97 no
    C3 H3B .  .97 no
    N4 C5 . 1.473(3) no
    N4 H4 .  .91 no
    C5 C6 . 1.516(4) no
    C5 H5A .  .97 no
    C5 H5B .  .97 no
    C6 C7 . 1.517(4) no
    C6 H6A .  .97 no
    C6 H6B .  .97 no
    C7 N1 2_666 1.482(3) no
    C7 H7A .  .97 no
    C7 H7B .  .97 no
    O11 C17 . 1.259(3) no
    O12 C17 . 1.233(3) no
    O31 N3 . 1.214(3) no
    O32 N3 . 1.229(3) no
    O51 N5 . 1.224(3) no
    O52 N5 . 1.218(3) no
    N3 C13 . 1.479(3) no
    N5 C15 . 1.472(3) no
    C11 C12 . 1.391(3) no
    C11 C16 . 1.386(3) no
    C11 C17 . 1.527(3) no
    C12 C13 . 1.381(3) no
    C12 H12 .  .93 no
    C13 C14 . 1.377(4) no
    C14 C15 . 1.386(4) no
    C14 H14 .  .93 no
    C15 C16 . 1.380(3) no
    C16 H16 .  .93 no
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    N4 Ni1 N4 . 2_666 180.0 no
    N4 Ni1 N1 . . 85.46(8) no
    N4 Ni1 N1 2_666 . 94.54(8) no
    N4 Ni1 N1 . 2_666 94.54(8) no
    N4 Ni1 N1 2_666 2_666 85.46(8) no
    N1 Ni1 N1 . 2_666 180.0 no
    N4 Ni1 O11 . 2_666 91.86(7) no
    N4 Ni1 O11 2_666 2_666 88.14(7) no
    N1 Ni1 O11 . 2_666 86.49(7) no
    N1 Ni1 O11 2_666 2_666 93.51(7) no
    N4 Ni1 O11 . . 88.14(7) no
    N4 Ni1 O11 2_666 . 91.86(7) no
    N1 Ni1 O11 . . 93.51(7) no
    N1 Ni1 O11 2_666 . 86.49(7) no
    O11 Ni1 O11 2_666 . 180 no
    C2 N1 C7 . 2_666 114.0(2) no
    C2 N1 Ni1 . . 105.8(2) no
    C7 N1 Ni1 2_666 . 116.7(2) no
    C2 N1 H1 . . 106.6 no
    C7 N1 H1 2_666 . 106.6 no
    Ni1 N1 H1 . . 106.6 no
    N1 C2 C3 . . 108.7(2) no
    N1 C2 H2A . . 109.9 no
    C3 C2 H2A . . 109.9 no
    N1 C2 H2B . . 109.9 no
    C3 C2 H2B . . 109.9 no
    H2A C2 H2B . . 108.3 no
    N4 C3 C2 . . 109.3(2) no
    N4 C3 H3A . . 109.8 no
    C2 C3 H3A . . 109.8 no
    N4 C3 H3B . . 109.8 no
    C2 C3 H3B . . 109.8 no
    H3A C3 H3B . . 108.3 no
    C5 N4 C3 . . 113.9(2) no
    C5 N4 Ni1 . . 115.8(2) no
    C3 N4 Ni1 . . 106.1(2) no
    C5 N4 H4 . . 106.8 no
    C3 N4 H4 . . 106.8 no
    Ni1 N4 H4 . . 106.8 no
    N4 C5 C6 . . 112.4(2) no
    N4 C5 H5A . . 109.1 no
    C6 C5 H5A . . 109.1 no
    N4 C5 H5B . . 109.1 no
    C6 C5 H5B . . 109.1 no
    H5A C5 H5B . . 107.9 no
    C5 C6 C7 . . 116.2(2) no
    C5 C6 H6A . . 108.2 no
    C7 C6 H6A . . 108.2 no
    C5 C6 H6B . . 108.2 no
    C7 C6 H6B . . 108.2 no
    H6A C6 H6B . . 107.4 no
    N1 C7 C6 2_666 . 112.6(2) no
    N1 C7 H7A 2_666 . 109.1 no
    C6 C7 H7A . . 109.1 no
    N1 C7 H7B 2_666 . 109.1 no
    C6 C7 H7B . . 109.1 no
    H7A C7 H7B . . 107.8 no
    C17 O11 Ni1 . . 127.9(2) no
    O31 N3 O32 . . 124.4(3) no
    O31 N3 C13 . . 118.5(2) no
    O32 N3 C13 . . 117.0(3) no
    O52 N5 O51 . . 123.7(2) no
    O52 N5 C15 . . 118.5(2) no
    O51 N5 C15 . . 117.9(2) no
    C16 C11 C12 . . 119.8(2) no
    C16 C11 C17 . . 119.2(2) no
    C12 C11 C17 . . 121.0(2) no
    C13 C12 C11 . . 118.9(2) no
    C13 C12 H12 . . 120.6 no
    C11 C12 H12 . . 120.6 no
    C14 C13 C12 . . 123.0(2) no
    C14 C13 N3 . . 118.3(2) no
    C12 C13 N3 . . 118.6(2) no
    C13 C14 C15 . . 116.5(2) no
    C13 C14 H14 . . 121.8 no
    C15 C14 H14 . . 121.8 no
    C16 C15 C14 . . 122.8(2) no
    C16 C15 N5 . . 119.3(2) no
    C14 C15 N5 . . 117.9(2) no
    C15 C16 C11 . . 119.1(2) no
    C15 C16 H16 . . 120.5 no
    C11 C16 H16 . . 120.5 no
    O12 C17 O11 . . 127.2(2) no
    O12 C17 C11 . . 117.4(2) no
    O11 C17 C11 . . 115.4(2) no
loop_
    _geom_torsion_atom_site_label_1
    _geom_torsion_atom_site_label_2
    _geom_torsion_atom_site_label_3
    _geom_torsion_atom_site_label_4
    _geom_torsion_site_symmetry_1
    _geom_torsion_site_symmetry_2
    _geom_torsion_site_symmetry_3
    _geom_torsion_site_symmetry_4
    _geom_torsion
    _geom_torsion_publ_flag
    N4 Ni1 N1 C2 . . . . 15.0(2) no
    N4 Ni1 N1 C2 2_666 . . . -165.0(2) no
    O11 Ni1 N1 C2 2_666 . . . -77.1(2) no
    O11 Ni1 N1 C2 . . . . 102.9(2) no
    N4 Ni1 N1 C7 . . . 2_666 143.0(2) no
    N4 Ni1 N1 C7 2_666 . . 2_666 -37.0(2) no
    O11 Ni1 N1 C7 2_666 . . 2_666 50.9(2) no
    O11 Ni1 N1 C7 . . . 2_666 -129.2(2) no
    C7 N1 C2 C3 2_666 . . . -170.5(2) no
    Ni1 N1 C2 C3 . . . . -41.0(2) no
    N1 C2 C3 N4 . . . . 56.4(3) no
    C2 C3 N4 C5 . . . . -169.1(2) no
    C2 C3 N4 Ni1 . . . . -40.5(2) no
    N1 Ni1 N4 C5 . . . . 141.5(12) no
    N1 Ni1 N4 C5 2_666 . . . -38.5(2) no
    O11 Ni1 N4 C5 2_666 . . . -132.1(2) no
    O11 Ni1 N4 C5 . . . . 47.9(2) no
    N1 Ni1 N4 C3 . . . . 14.1(2) no
    N1 Ni1 N4 C3 2_666 . . . -165.9(2) no
    O11 Ni1 N4 C3 2_666 . . . 100.4(2) no
    O11 Ni1 N4 C3 . . . . -79.6(2) no
    C3 N4 C5 C6 . . . . -179.8(2) no
    Ni1 N4 C5 C6 . . . . 56.8(3) no
    N4 C5 C6 C7 . . . . -71.0(3) no
    C5 C6 C7 N1 . . . 2_666 68.7(3) no
    N4 Ni1 O11 C17 . . . . 121.4(2) no
    N4 Ni1 O11 C17 2_666 . . . -58.6(2) no
    N1 Ni1 O11 C17 . . . . 36.0(2) no
    N1 Ni1 O11 C17 2_666 . . . -144.0(2) no
    C16 C11 C12 C13 . . . .  .4(3) no
    C17 C11 C12 C13 . . . . 178.8(2) no
    C11 C12 C13 C14 . . . .  .0(4) no
    C11 C12 C13 N3 . . . . -177.7(2) no
    O31 N3 C13 C14 . . . . -169.6(2) no
    O32 N3 C13 C14 . . . . 9.0(3) no
    O31 N3 C13 C12 . . . . 8.2(3) no
    O32 N3 C13 C12 . . . . -173.2(2) no
    C12 C13 C14 C15 . . . .  -.9(4) no
    N3 C13 C14 C15 . . . . 176.9(2) no
    C13 C14 C15 C16 . . . . 1.3(4) no
    C13 C14 C15 N5 . . . . -176.6(2) no
    O52 N5 C15 C16 . . . . -179.1(2) no
    O51 N5 C15 C16 . . . . 1.0(3) no
    O52 N5 C15 C14 . . . . -1.1(3) no
    O51 N5 C15 C14 . . . . 179.0(2) no
    C14 C15 C16 C11 . . . .  -.9(4) no
    N5 C15 C16 C11 . . . . 177.0(2) no
    C12 C11 C16 C15 . . . .  .0(3) no
    C17 C11 C16 C15 . . . . -178.4(2) no
    Ni1 O11 C17 O12 . . . . 5.5(4) no
    Ni1 O11 C17 C11 . . . . -173.8(2) no
    C16 C11 C17 O12 . . . . -11.8(3) no
    C12 C11 C17 O12 . . . . 169.8(2) no
    C16 C11 C17 O11 . . . . 167.5(2) no
    C12 C11 C17 O11 . . . . -10.9(3) no
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    _geom_hbond_publ_flag
    N1 H1 O12 .  .91 2.33 3.056(3) 137 y
    N4 H4 O52 1_656  .91 2.35 3.132(3) 144 y
    C2 H2A O12 2_566  .97 2.40 3.287(4) 152 y
data_III
_chemical_name_systematic
;
Bis-(4-nitrobenzoato)-1,4,8,11-tetraazacyclotetradecanenickel(II)
;
_chemical_name_common     ?
_chemical_formula_moiety     'C24 H32 N6 Ni O8'
_chemical_formula_sum     'C24 H32 N6 Ni O8'
_chemical_formula_weight     591.27
_chemical_melting_point     ?
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'P21/n'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    'x+1/2, -y+1/2, z+1/2'
    '-x, -y, -z'
    '-x-1/2, y-1/2, -z-1/2'
_cell_length_a     12.8106(3)
_cell_length_b     8.4187(2)
_cell_length_c     12.8397(4)
_cell_angle_alpha     90.00
_cell_angle_beta     114.2543(10)
_cell_angle_gamma     90.00
_cell_volume     1262.51(6)
_cell_formula_units_Z     2
_cell_measurement_reflns_used     2781
_cell_measurement_theta_min     2.93
_cell_measurement_theta_max     27.79
_cell_measurement_temperature     150(2)
_exptl_crystal_description     block
_exptl_crystal_colour     colourless
_exptl_crystal_size_max      .26
_exptl_crystal_size_mid      .24
_exptl_crystal_size_min      .22
_exptl_crystal_density_diffrn     1.555
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     620
_exptl_absorpt_coefficient_mu      .831
_exptl_absorpt_correction_type     Multi-scan
_exptl_absorpt_process_details     'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min      .8130
_exptl_absorpt_correction_T_max      .8384
_exptl_special_details
;
 The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling
 algorithm [Fox, G.C. & Holmes, K.C. (1966).  Acta Cryst. 20,
 886-891] which effectively corrects for
 absorption effects. High redundancy data were used in the scaling
 program hence the 'multi-scan' code word was used. No transmission
 coefficients are available from the program (only scale factors for each
 frame). The scale factors in the experimental table are calculated
 from the 'size' command in the SHELXL-97 input file.
;
_diffrn_ambient_temperature     150(2)
_diffrn_radiation_type     'Mo K\a'
_diffrn_radiation_wavelength      .71073
_diffrn_radiation_source     'fine-focus sealed X-ray tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Kappa-CCD'
_diffrn_measurement_method     'φ scans, and ω scans with κ offsets'
_diffrn_reflns_number     8828
_diffrn_reflns_av_R_equivalents      .040
_diffrn_reflns_av_sigmaI/netI      .042
_diffrn_reflns_theta_min     2.93
_diffrn_reflns_theta_max     27.79
_diffrn_reflns_theta_full     27.79
_diffrn_measured_fraction_theta_max      .971
_diffrn_measured_fraction_theta_full      .971
_diffrn_reflns_limit_h_min     0
_diffrn_reflns_limit_h_max     16
_diffrn_reflns_limit_k_min     0
_diffrn_reflns_limit_k_max     10
_diffrn_reflns_limit_l_min     -16
_diffrn_reflns_limit_l_max     15
_diffrn_standards_decay_%     negligible
_reflns_number_total     2894
_reflns_number_gt     2456
_reflns_threshold_expression     >2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all      .0394
_refine_ls_R_factor_gt      .0303
_refine_ls_wR_factor_gt      .0750
_refine_ls_wR_factor_ref      .0797
_refine_ls_goodness_of_fit_ref     1.038
_refine_ls_restrained_S_all     1.038
_refine_ls_number_reflns     2894
_refine_ls_number_parameters     178
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
              'w=1/[σ²(Fo²)+(0.0314P)²+0.5307P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max      .001
_refine_ls_shift/su_mean      .000
_refine_diff_density_max      .367
_refine_diff_density_min      -.390
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'C' 'C'  .0033  .0016
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'H' 'H'  .0000  .0000
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'N' 'N'  .0061  .0033
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Ni' 'Ni'  .3393 1.1124
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'O' 'O'  .0106  .0060
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'Kappa-CCD server softare (Nonius, 1997)'
_computing_cell_refinement     'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction     'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)'
_computing_structure_refinement     'SHELXL-97 (Sheldrick, 1997b)'
_computing_molecular_graphics     'PLATON (Spek, 2001)'
_computing_publication_material
                   'SHELXL-97  (Sheldrick, 1997b) and PRPKAPPA (Ferguson, 1999)'
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Ni1  .5000  .5000  .5000  .01595(11) Uani d S 1 . . Ni
    N1  .57282(10)  .33040(15)  .62464(11)  .0193(3) Uani d . 1 . . N
    C2  .62427(13)  .21138(19)  .57574(14)  .0228(3) Uani d . 1 . . C
    C3  .54312(13)  .18189(19)  .45225(14)  .0226(3) Uani d . 1 . . C
    N4  .52317(10)  .33495(16)  .39076(11)  .0195(3) Uani d . 1 . . N
    C5  .43331(14)  .3272(2)  .27367(14)  .0238(3) Uani d . 1 . . C
    C6  .40728(14)  .48956(19)  .21559(14)  .0236(3) Uani d . 1 . . C
    C7  .34781(13)  .6063(2)  .26408(13)  .0217(3) Uani d . 1 . . C
    O11  .33036(9)  .42120(13)  .46359(10)  .0218(3) Uani d . 1 . . O
    O12  .34942(10)  .22940(17)  .59137(12)  .0410(4) Uani d . 1 . . O
    O41  -.23591(12)  .2008(2)  .40490(17)  .0595(5) Uani d . 1 . . O
    O42  -.25454(10)  .41423(19)  .30553(12)  .0423(4) Uani d . 1 . . O
    N14  -.19596(12)  .3093(2)  .36853(14)  .0343(4) Uani d . 1 . . N
    C11  .16301(13)  .32350(19)  .47697(13)  .0195(3) Uani d . 1 . . C
    C12  .09284(14)  .4217(2)  .38919(14)  .0239(3) Uani d . 1 . . C
    C13  -.02574(14)  .4187(2)  .35172(15)  .0262(4) Uani d . 1 . . C
    C14  -.07089(13)  .3137(2)  .40536(14)  .0250(4) Uani d . 1 . . C
    C15  -.00398(14)  .2141(2)  .49259(15)  .0271(4) Uani d . 1 . . C
    C16  .11389(14)  .2198(2)  .52871(14)  .0245(4) Uani d . 1 . . C
    C17  .29251(13)  .32381(19)  .51547(14)  .0210(3) Uani d . 1 . . C
    H1  .5135  .2805  .6359  .023 Uiso calc R 1 . . H
    H2A  .6378  .1112  .6197  .027 Uiso calc R 1 . . H
    H2B  .6987  .2506  .5798  .027 Uiso calc R 1 . . H
    H3A  .5771  .1043  .4171  .027 Uiso calc R 1 . . H
    H3B  .4698  .1382  .4482  .027 Uiso calc R 1 . . H
    H4  .5910  .3615  .3848  .023 Uiso calc R 1 . . H
    H5A  .3625  .2836  .2760  .029 Uiso calc R 1 . . H
    H5B  .4580  .2538  .2279  .029 Uiso calc R 1 . . H
    H6A  .4801  .5376  .2217  .028 Uiso calc R 1 . . H
    H6B  .3584  .4740  .1334  .028 Uiso calc R 1 . . H
    H7A  .3159  .6952  .2098  .026 Uiso calc R 1 . . H
    H7B  .2834  .5521  .2730  .026 Uiso calc R 1 . . H
    H12  .1264  .4923  .3540  .029 Uiso calc R 1 . . H
    H13  -.0737  .4861  .2918  .031 Uiso calc R 1 . . H
    H15  -.0380  .1431  .5272  .032 Uiso calc R 1 . . H
    H16  .1614  .1527  .5890  .029 Uiso calc R 1 . . H
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Ni1 N1 3_666 2.060(2) no
    Ni1 N1 . 2.060(2) no
    Ni1 N4 3_666 2.080(2) no
    Ni1 N4 . 2.080(2) no
    Ni1 O11 3_666 2.132(2) no
    Ni1 O11 . 2.132(2) no
    N1 C7 3_666 1.472(2) no
    N1 C2 . 1.474(2) no
    N1 H1 .  .93 no
    C2 C3 . 1.517(2) no
    C2 H2A .  .99 no
    C2 H2B .  .99 no
    C3 N4 . 1.478(2) no
    C3 H3A .  .99 no
    C3 H3B .  .99 no
    N4 C5 . 1.472(2) no
    N4 H4 .  .93 no
    C5 C6 . 1.527(2) no
    C5 H5A .  .99 no
    C5 H5B .  .99 no
    C6 C7 . 1.524(2) no
    C6 H6A .  .99 no
    C6 H6B .  .99 no
    C7 N1 3_666 1.472(2) no
    C7 H7A .  .99 no
    C7 H7B .  .99 no
    O11 C17 . 1.271(2) no
    O12 C17 . 1.237(2) no
    O41 N14 . 1.229(2) no
    O42 N14 . 1.224(2) no
    N14 C14 . 1.473(2) no
    C11 C12 . 1.389(2) no
    C11 C16 . 1.394(2) no
    C11 C17 . 1.524(2) no
    C12 C13 . 1.393(2) no
    C12 H12 .  .95 no
    C13 C14 . 1.385(2) no
    C13 H13 .  .95 no
    C14 C15 . 1.380(3) no
    C15 C16 . 1.386(2) no
    C15 H15 .  .95 no
    C16 H16 .  .95 no
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    N1 Ni1 N1 3_666 . 180.0 no
    N1 Ni1 N4 3_666 3_666 85.20(5) no
    N1 Ni1 N4 . 3_666 94.80(5) no
    N1 Ni1 N4 3_666 . 94.80(5) no
    N1 Ni1 N4 . . 85.20(5) no
    N4 Ni1 N4 3_666 . 180.0 no
    N1 Ni1 O11 3_666 3_666 92.88(5) no
    N1 Ni1 O11 . 3_666 87.12(5) no
    N4 Ni1 O11 3_666 3_666 93.39(5) no
    N4 Ni1 O11 . 3_666 86.61(5) no
    N1 Ni1 O11 3_666 . 87.12(5) no
    N1 Ni1 O11 . . 92.88(5) no
    N4 Ni1 O11 3_666 . 86.61(5) no
    N4 Ni1 O11 . . 93.39(5) no
    O11 Ni1 O11 3_666 . 180.0 no
    C7 N1 C2 3_666 . 114.1(2) no
    C7 N1 Ni1 3_666 . 114.5(2) no
    C2 N1 Ni1 . . 106.2(2) no
    C7 N1 H1 3_666 . 107.2 no
    C2 N1 H1 . . 107.2 no
    Ni1 N1 H1 . . 107.2 no
    N1 C2 C3 . . 108.8(2) no
    N1 C2 H2A . . 109.9 no
    C3 C2 H2A . . 109.9 no
    N1 C2 H2B . . 109.9 no
    C3 C2 H2B . . 109.9 no
    H2A C2 H2B . . 108.3 no
    N4 C3 C2 . . 108.0(2) no
    N4 C3 H3A . . 110.1 no
    C2 C3 H3A . . 110.1 no
    N4 C3 H3B . . 110.1 no
    C2 C3 H3B . . 110.1 no
    H3A C3 H3B . . 108.4 no
    C5 N4 C3 . . 113.5(2) no
    C5 N4 Ni1 . . 116.7(2) no
    C3 N4 Ni1 . . 105.28(9) no
    C5 N4 H4 . . 106.9 no
    C3 N4 H4 . . 106.9 no
    Ni1 N4 H4 . . 106.9 no
    N4 C5 C6 . . 112.4(2) no
    N4 C5 H5A . . 109.1 no
    C6 C5 H5A . . 109.1 no
    N4 C5 H5B . . 109.1 no
    C6 C5 H5B . . 109.1 no
    H5A C5 H5B . . 107.9 no
    C7 C6 C5 . . 115.04(13) no
    C7 C6 H6A . . 108.5 no
    C5 C6 H6A . . 108.5 no
    C7 C6 H6B . . 108.5 no
    C5 C6 H6B . . 108.5 no
    H6A C6 H6B . . 107.5 no
    N1 C7 C6 3_666 . 111.6(2) no
    N1 C7 H7A 3_666 . 109.3 no
    C6 C7 H7A . . 109.3 no
    N1 C7 H7B 3_666 . 109.3 no
    C6 C7 H7B . . 109.3 no
    H7A C7 H7B . . 108.0 no
    C17 O11 Ni1 . . 131.3(2) no
    O42 N14 O41 . . 123.3(2) no
    O42 N14 C14 . . 119.0(2) no
    O41 N14 C14 . . 117.7(2) no
    C12 C11 C16 . . 119.4(2) no
    C12 C11 C17 . . 121.2(2) no
    C16 C11 C17 . . 119.4(2) no
    C11 C12 C13 . . 121.3(2) no
    C11 C12 H12 . . 119.3 no
    C13 C12 H12 . . 119.3 no
    C14 C13 C12 . . 117.3(2) no
    C14 C13 H13 . . 121.3 no
    C12 C13 H13 . . 121.3 no
    C15 C14 C13 . . 123.0(2) no
    C15 C14 N14 . . 118.5(2) no
    C13 C14 N14 . . 118.5(2) no
    C14 C15 C16 . . 118.6(2) no
    C14 C15 H15 . . 120.7 no
    C16 C15 H15 . . 120.7 no
    C15 C16 C11 . . 120.4(2) no
    C15 C16 H16 . . 119.8 no
    C11 C16 H16 . . 119.8 no
    O12 C17 O11 . . 126.8(2) no
    O12 C17 C11 . . 117.7(2) no
    O11 C17 C11 . . 115.5(2) no
loop_
    _geom_torsion_atom_site_label_1
    _geom_torsion_atom_site_label_2
    _geom_torsion_atom_site_label_3
    _geom_torsion_atom_site_label_4
    _geom_torsion_site_symmetry_1
    _geom_torsion_site_symmetry_2
    _geom_torsion_site_symmetry_3
    _geom_torsion_site_symmetry_4
    _geom_torsion
    _geom_torsion_publ_flag
    N4 Ni1 N1 C7 3_666 . . 3_666 -39.6(12) no
    N4 Ni1 N1 C7 . . . 3_666 140.4(2) no
    O11 Ni1 N1 C7 3_666 . . 3_666 53.5(2) no
    O11 Ni1 N1 C7 . . . 3_666 -126.5(2) no
    N4 Ni1 N1 C2 3_666 . . . -166.51(9) no
    N4 Ni1 N1 C2 . . . . 13.49(9) no
    O11 Ni1 N1 C2 3_666 . . . -73.34(9) no
    O11 Ni1 N1 C2 . . . . 106.66(9) no
    C7 N1 C2 C3 3_666 . . . -168.2(2) no
    Ni1 N1 C2 C3 . . . . -41.1(2) no
    N1 C2 C3 N4 . . . . 58.2(11) no
    C2 C3 N4 C5 . . . . -172.0(2) no
    C2 C3 N4 Ni1 . . . . -43.2(2) no
    N1 Ni1 N4 C5 3_666 . . . -36.6(2) no
    N1 Ni1 N4 C5 . . . . 143.4(2) no
    O11 Ni1 N4 C5 3_666 . . . -129.2(2) no
    O11 Ni1 N4 C5 . . . . 50.8(2) no
    N1 Ni1 N4 C3 3_666 . . . -163.41(9) no
    N1 Ni1 N4 C3 . . . . 16.59(9) no
    O11 Ni1 N4 C3 3_666 . . . 103.98(9) no
    O11 Ni1 N4 C3 . . . . -76.02(9) no
    C3 N4 C5 C6 . . . . 175.1(2) no
    Ni1 N4 C5 C6 . . . . 52.5(2) no
    N4 C5 C6 C7 . . . . -69.4(2) no
    C5 C6 C7 N1 . . . 3_666 74.1(2) no
    N1 Ni1 O11 C17 3_666 . . . -169.7(2) no
    N1 Ni1 O11 C17 . . . . 10.3(12) no
    N4 Ni1 O11 C17 3_666 . . . -84.3(2) no
    N4 Ni1 O11 C17 . . . . 95.7(2) no
    C16 C11 C12 C13 . . . .  .0(2) no
    C17 C11 C12 C13 . . . . 178.3(2) no
    C11 C12 C13 C14 . . . .  -.1(2) no
    C12 C13 C14 C15 . . . .  .0(3) no
    C12 C13 C14 N14 . . . . 179.2(2) no
    O42 N14 C14 C15 . . . . 167.8(2) no
    O41 N14 C14 C15 . . . . -10.9(2) no
    O42 N14 C14 C13 . . . . -11.5(2) no
    O41 N14 C14 C13 . . . . 169.8(2) no
    C13 C14 C15 C16 . . . .  .3(3) no
    N14 C14 C15 C16 . . . . -178.9(2) no
    C14 C15 C16 C11 . . . .  -.5(3) no
    C12 C11 C16 C15 . . . .  .3(2) no
    C17 C11 C16 C15 . . . . -178.0(2) no
    Ni1 O11 C17 O12 . . . . -13.3(3) no
    Ni1 O11 C17 C11 . . . . 167.9(2) no
    C12 C11 C17 O12 . . . . -177.5(2) no
    C16 C11 C17 O12 . . . .  .8(2) no
    C12 C11 C17 O11 . . . . 1.4(2) no
    C16 C11 C17 O11 . . . . 179.6(2) no
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    _geom_hbond_publ_flag
    N1 H1 O12 .  .93 1.99 2.845(2) 153 y
    N4 H4 O41 1_655  .93 2.52 3.221(2) 132 y
    C16 H16 O42 2_555  .95 2.60 3.439(2) 148 y
data_IV
_chemical_name_systematic
;
Bis-(3-hydroxybenzoato)-1,4,8,11-tetraazacyclotetradecanenickel(II)
;
_chemical_name_common     ?
_chemical_formula_moiety     'C24 H34 N4 Ni O6'
_chemical_formula_sum     'C24 H34 N4 Ni O6'
_chemical_formula_weight     533.26
_chemical_melting_point     ?
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'P21/c'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, y+1/2, -z+1/2'
    '-x, -y, -z'
    'x, -y-1/2, z-1/2'
_cell_length_a     8.5180(3)
_cell_length_b     13.2496(5)
_cell_length_c     10.7720(4)
_cell_angle_alpha     90.00
_cell_angle_beta     101.161(2)
_cell_angle_gamma     90.00
_cell_volume     1192.74(8)
_cell_formula_units_Z     2
_cell_measurement_reflns_used     2748
_cell_measurement_theta_min     2.88
_cell_measurement_theta_max     27.53
_cell_measurement_temperature     150(2)
_exptl_crystal_description     needle
_exptl_crystal_colour     colourless
_exptl_crystal_size_max      .40
_exptl_crystal_size_mid      .28
_exptl_crystal_size_min      .22
_exptl_crystal_density_diffrn     1.485
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     564
_exptl_absorpt_coefficient_mu      .862
_exptl_absorpt_correction_type     Multi-scan
_exptl_absorpt_process_details     'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min      .7243
_exptl_absorpt_correction_T_max      .8330
_exptl_special_details
;
 The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling
 algorithm [Fox, G.C. & Holmes, K.C. (1966).  Acta Cryst. 20,
 886-891] which effectively corrects for
 absorption effects. High redundancy data were used in the scaling
 program hence the 'multi-scan' code word was used. No transmission
 coefficients are available from the program (only scale factors for each
 frame). The scale factors in the experimental table are calculated
 from the 'size' command in the SHELXL-97 input file.
;
_diffrn_ambient_temperature     150(2)
_diffrn_radiation_type     'Mo K\a'
_diffrn_radiation_wavelength      .71073
_diffrn_radiation_source     'fine-focus sealed X-ray tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Kappa-CCD'
_diffrn_measurement_method     'φ scans, and ω scans with κ offsets'
_diffrn_reflns_number     9996
_diffrn_reflns_av_R_equivalents      .040
_diffrn_reflns_av_sigmaI/netI      .0439
_diffrn_reflns_theta_min     2.88
_diffrn_reflns_theta_max     27.53
_diffrn_reflns_theta_full     27.53
_diffrn_measured_fraction_theta_max      .992
_diffrn_measured_fraction_theta_full      .992
_diffrn_reflns_limit_h_min     0
_diffrn_reflns_limit_h_max     11
_diffrn_reflns_limit_k_min     0
_diffrn_reflns_limit_k_max     17
_diffrn_reflns_limit_l_min     -13
_diffrn_reflns_limit_l_max     13
_diffrn_standards_decay_%     negligible
_reflns_number_total     2721
_reflns_number_gt     2194
_reflns_threshold_expression     >2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all      .0467
_refine_ls_R_factor_gt      .0319
_refine_ls_wR_factor_gt      .0702
_refine_ls_wR_factor_ref      .0759
_refine_ls_goodness_of_fit_ref     1.041
_refine_ls_restrained_S_all     1.041
_refine_ls_number_reflns     2721
_refine_ls_number_parameters     162
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
              'w=1/[σ²(Fo²)+(0.0232P)²+0.6219P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max      .001
_refine_ls_shift/su_mean      .000
_refine_diff_density_max      .333
_refine_diff_density_min      -.362
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef      .0036(10)
_refine_ls_extinction_expression
                                  'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'C' 'C'  .0033  .0016
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'H' 'H'  .0000  .0000
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'N' 'N'  .0061  .0033
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Ni' 'Ni'  .3393 1.1124
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'O' 'O'  .0106  .0060
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'Kappa-CCD server software (Nonius, 1997)'
_computing_cell_refinement     'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction     'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)'
_computing_structure_refinement     'SHELXL-97 (Sheldrick, 1997b)'
_computing_molecular_graphics     'PLATON (Spek, 2001)'
_computing_publication_material
                   'SHELXL-97  (Sheldrick, 1997b) and PRPKAPPA (Ferguson, 1999)'
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Ni1  .5000  .5000  .5000  .01498(11) Uani d S 1 . . Ni
    N1  .43833(18)  .62473(11)  .38455(13)  .0188(3) Uani d . 1 . . N
    C2  .3062(2)  .59176(15)  .28307(18)  .0254(4) Uani d . 1 . . C
    C3  .3435(2)  .48667(14)  .24034(17)  .0255(4) Uani d . 1 . . C
    N4  .36826(19)  .41851(11)  .35181(14)  .0205(3) Uani d . 1 . . N
    C5  .4336(2)  .31855(14)  .32804(18)  .0249(4) Uani d . 1 . . C
    C6  .4585(2)  .25182(14)  .44562(18)  .0267(4) Uani d . 1 . . C
    C7  .5968(2)  .28196(13)  .55099(18)  .0236(4) Uani d . 1 . . C
    O11  .71243(15)  .47431(9)  .43020(12)  .0211(3) Uani d . 1 . . O
    O12  .74555(16)  .60133(9)  .30107(13)  .0256(3) Uani d . 1 . . O
    O13 1.07609(17)  .20467(10)  .32970(12)  .0275(3) Uani d . 1 . . O
    C11  .8565(2)  .44052(13)  .26869(16)  .0184(4) Uani d . 1 . . C
    C12  .9286(2)  .35489(14)  .32983(17)  .0200(4) Uani d . 1 . . C
    C13 1.0080(2)  .28633(14)  .26516(17)  .0197(4) Uani d . 1 . . C
    C14 1.0144(2)  .30365(14)  .13851(17)  .0219(4) Uani d . 1 . . C
    C15  .9400(2)  .38830(14)  .07732(17)  .0226(4) Uani d . 1 . . C
    C16  .8619(2)  .45748(14)  .14164(17)  .0213(4) Uani d . 1 . . C
    C17  .7665(2)  .51106(13)  .33895(16)  .0180(4) Uani d . 1 . . C
    H1  .5252  .6387  .3466  .023 Uiso calc R 1 . . H
    H2A  .2942  .6393  .2109  .030 Uiso calc R 1 . . H
    H2B  .2046  .5908  .3148  .030 Uiso calc R 1 . . H
    H3A  .2537  .4618  .1750  .031 Uiso calc R 1 . . H
    H3B  .4411  .4884  .2033  .031 Uiso calc R 1 . . H
    H4  .2682  .4073  .3717  .025 Uiso calc R 1 . . H
    H5A  .5371  .3276  .3006  .030 Uiso calc R 1 . . H
    H5B  .3591  .2846  .2586  .030 Uiso calc R 1 . . H
    H6A  .3588  .2523  .4800  .032 Uiso calc R 1 . . H
    H6B  .4764  .1817  .4199  .032 Uiso calc R 1 . . H
    H7A  .6187  .2265  .6136  .028 Uiso calc R 1 . . H
    H7B  .6941  .2923  .5150  .028 Uiso calc R 1 . . H
    H3 1.1246  .1706  .2831  .041 Uiso calc R 1 . . H
    H12  .9237  .3431  .4160  .024 Uiso calc R 1 . . H
    H14 1.0695  .2578  .0942  .026 Uiso calc R 1 . . H
    H15  .9423  .3991  -.0095  .027 Uiso calc R 1 . . H
    H16  .8127  .5157  .0994  .026 Uiso calc R 1 . . H
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Ni1 N4 . 2.069(2) no
    Ni1 N4 3_666 2.069(2) no
    Ni1 N1 . 2.074(2) no
    Ni1 N1 3_666 2.074(2) no
    Ni1 O11 3_666 2.117(2) no
    Ni1 O11 . 2.117(2) no
    N1 C2 . 1.475(2) no
    N1 C7 3_666 1.477(2) no
    N1 H1 .  .93 no
    C2 C3 . 1.519(3) no
    C2 H2A .  .99 no
    C2 H2B .  .99 no
    C3 N4 . 1.485(2) no
    C3 H3A .  .99 no
    C3 H3B .  .99 no
    N4 C5 . 1.478(2) no
    N4 H4 .  .93 no
    C5 C6 . 1.525(3) no
    C5 H5A .  .99 no
    C5 H5B .  .99 no
    C6 C7 . 1.523(3) no
    C6 H6A .  .99 no
    C6 H6B .  .99 no
    C7 N1 3_666 1.477(2) no
    C7 H7A .  .99 no
    C7 H7B .  .99 no
    O11 C17 . 1.261(2) no
    O12 C17 . 1.265(2) no
    O13 C13 . 1.354(2) no
    O13 H3 .  .84 no
    C11 C12 . 1.393(3) no
    C11 C16 . 1.396(2) no
    C11 C17 . 1.503(2) no
    C12 C13 . 1.397(2) no
    C12 H12 .  .95 no
    C13 C14 . 1.395(2) no
    C14 C15 . 1.390(3) no
    C14 H14 .  .95 no
    C15 C16 . 1.393(3) no
    C15 H15 .  .95 no
    C16 H16 .  .95 no
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    N4 Ni1 N4 . 3_666 180.0 no
    N4 Ni1 N1 . . 85.22(6) no
    N4 Ni1 N1 3_666 . 94.78(6) no
    N4 Ni1 N1 . 3_666 94.78(6) no
    N4 Ni1 N1 3_666 3_666 85.22(6) no
    N1 Ni1 N1 . 3_666 180.0 no
    N4 Ni1 O11 . 3_666 89.12(6) no
    N4 Ni1 O11 3_666 3_666 90.88(6) no
    N1 Ni1 O11 . 3_666 87.14(5) no
    N1 Ni1 O11 3_666 3_666 92.86(5) no
    N4 Ni1 O11 . . 90.88(6) no
    N4 Ni1 O11 3_666 . 89.12(6) no
    N1 Ni1 O11 . . 92.86(5) no
    N1 Ni1 O11 3_666 . 87.14(5) no
    O11 Ni1 O11 3_666 . 180.0 no
    C2 N1 C7 . 3_666 113.7(2) no
    C2 N1 Ni1 . . 106.1(2) no
    C7 N1 Ni1 3_666 . 115.9(2) no
    C2 N1 H1 . . 106.9 no
    C7 N1 H1 3_666 . 106.9 no
    Ni1 N1 H1 . . 106.9 no
    N1 C2 C3 . . 108.8(2) no
    N1 C2 H2A . . 109.9 no
    C3 C2 H2A . . 109.9 no
    N1 C2 H2B . . 109.9 no
    C3 C2 H2B . . 109.9 no
    H2A C2 H2B . . 108.3 no
    N4 C3 C2 . . 108.5(2) no
    N4 C3 H3A . . 110.0 no
    C2 C3 H3A . . 110.0 no
    N4 C3 H3B . . 110.0 no
    C2 C3 H3B . . 110.0 no
    H3A C3 H3B . . 108.4 no
    C5 N4 C3 . . 113.9(2) no
    C5 N4 Ni1 . . 115.8(2) no
    C3 N4 Ni1 . . 106.1(2) no
    C5 N4 H4 . . 106.9 no
    C3 N4 H4 . . 106.9 no
    Ni1 N4 H4 . . 106.9 no
    N4 C5 C6 . . 111.8(2) no
    N4 C5 H5A . . 109.2 no
    C6 C5 H5A . . 109.2 no
    N4 C5 H5B . . 109.2 no
    C6 C5 H5B . . 109.2 no
    H5A C5 H5B . . 107.9 no
    C7 C6 C5 . . 115.5(2) no
    C7 C6 H6A . . 108.4 no
    C5 C6 H6A . . 108.4 no
    C7 C6 H6B . . 108.4 no
    C5 C6 H6B . . 108.4 no
    H6A C6 H6B . . 107.5 no
    N1 C7 C6 3_666 . 111.8(2) no
    N1 C7 H7A 3_666 . 109.2 no
    C6 C7 H7A . . 109.2 no
    N1 C7 H7B 3_666 . 109.2 no
    C6 C7 H7B . . 109.2 no
    H7A C7 H7B . . 107.9 no
    C17 O11 Ni1 . . 132.9(2) no
    C13 O13 H3 . . 109.5 no
    C12 C11 C16 . . 120.0(2) no
    C12 C11 C17 . . 119.3(2) no
    C16 C11 C17 . . 120.7(12) no
    C11 C12 C13 . . 120.4(2) no
    C11 C12 H12 . . 119.8 no
    C13 C12 H12 . . 119.8 no
    O13 C13 C14 . . 122.7(2) no
    O13 C13 C12 . . 117.7(2) no
    C14 C13 C12 . . 119.7(2) no
    C15 C14 C13 . . 119.7(2) no
    C15 C14 H14 . . 120.1 no
    C13 C14 H14 . . 120.1 no
    C14 C15 C16 . . 120.9(2) no
    C14 C15 H15 . . 119.6 no
    C16 C15 H15 . . 119.6 no
    C15 C16 C11 . . 119.4(2) no
    C15 C16 H16 . . 120.3 no
    C11 C16 H16 . . 120.3 no
    O11 C17 O12 . . 124.5(2) no
    O11 C17 C11 . . 116.8(2) no
    O12 C17 C11 . . 118.6(2) no
loop_
    _geom_torsion_atom_site_label_1
    _geom_torsion_atom_site_label_2
    _geom_torsion_atom_site_label_3
    _geom_torsion_atom_site_label_4
    _geom_torsion_site_symmetry_1
    _geom_torsion_site_symmetry_2
    _geom_torsion_site_symmetry_3
    _geom_torsion_site_symmetry_4
    _geom_torsion
    _geom_torsion_publ_flag
    N4 Ni1 N1 C2 . . . . 14.9(2) no
    N4 Ni1 N1 C2 3_666 . . . -165.1(2) no
    O11 Ni1 N1 C2 3_666 . . . -74.4(2) no
    O11 Ni1 N1 C2 . . . . 105.6(2) no
    N4 Ni1 N1 C7 . . . 3_666 142.1(2) no
    N4 Ni1 N1 C7 3_666 . . 3_666 -38.0(2) no
    O11 Ni1 N1 C7 3_666 . . 3_666 52.7(2) no
    O11 Ni1 N1 C7 . . . 3_666 -127.3(2) no
    C7 N1 C2 C3 3_666 . . . -167.0(2) no
    Ni1 N1 C2 C3 . . . . -41.5(2) no
    N1 C2 C3 N4 . . . . 56.9(2) no
    C2 C3 N4 C5 . . . . -169.7(2) no
    C2 C3 N4 Ni1 . . . . -41.1(2) no
    N1 Ni1 N4 C5 . . . . 142.0(2) no
    N1 Ni1 N4 C5 3_666 . . . -38.0(2) no
    O11 Ni1 N4 C5 3_666 . . . -130.8320 no
    O11 Ni1 N4 C5 . . . . 49.2(2) no
    N1 Ni1 N4 C3 . . . . 14.6(2) no
    N1 Ni1 N4 C3 3_666 . . . -165.4(2) no
    O11 Ni1 N4 C3 3_666 . . . 101.8(2) no
    O11 Ni1 N4 C3 . . . . -78.2(2) no
    C3 N4 C5 C6 . . . . 179.4(2) no
    Ni1 N4 C5 C6 . . . . 56.0(2) no
    N4 C5 C6 C7 . . . . -71.9(2) no
    C5 C6 C7 N1 . . . 3_666 71.7(2) no
    N4 Ni1 O11 C17 . . . . 75.4(2) no
    N4 Ni1 O11 C17 3_666 . . . -104.6(2) no
    N1 Ni1 O11 C17 . . . . -9.9(2) no
    N1 Ni1 O11 C17 3_666 . . . 170.1(2) no
    C16 C11 C12 C13 . . . .  .8(3) no
    C17 C11 C12 C13 . . . . 177.7(2) no
    C11 C12 C13 O13 . . . . 179.8(2) no
    C11 C12 C13 C14 . . . .  -.3(3) no
    O13 C13 C14 C15 . . . . 179.1(2) no
    C12 C13 C14 C15 . . . .  -.8(3) no
    C13 C14 C15 C16 . . . . 1.5(3) no
    C14 C15 C16 C11 . . . . -1.0(3) no
    C12 C11 C16 C15 . . . .  -.1(3) no
    C17 C11 C16 C15 . . . . -177.0(2) no
    Ni1 O11 C17 O12 . . . . 34.1(3) no
    Ni1 O11 C17 C11 . . . . -143.6(2) no
    C12 C11 C17 O11 . . . . -24.2(2) no
    C16 C11 C17 O11 . . . . 152.7(2) no
    C12 C11 C17 O12 . . . . 157.9(2) no
    C16 C11 C17 O12 . . . . -25.1(3) no
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    _geom_hbond_publ_flag
    N1 H1 O12 .  .93 2.09 2.943(2) 152 y
    O13 H3 O12 2_745  .84 1.81 2.645(2) 172 y
data_V
_chemical_name_systematic
;
Bis-(4-aminobenzoato)-1,4,8,11-tetraazacyclotetradecanenickel(II)
;
_chemical_name_common     ?
_chemical_formula_moiety     'C24 H36 N6 Ni O4'
_chemical_formula_sum     'C24 H36 N6 Ni O4'
_chemical_formula_weight     531.30
_chemical_melting_point     ?
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'C2/c'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, y, -z+1/2'
    'x+1/2, y+1/2, z'
    '-x+1/2, y+1/2, -z+1/2'
    '-x, -y, -z'
    'x, -y, z-1/2'
    '-x+1/2, -y+1/2, -z'
    'x+1/2, -y+1/2, z-1/2'
_cell_length_a     18.4430(4)
_cell_length_b     8.4149(2)
_cell_length_c     16.8262(4)
_cell_angle_alpha     90.00
_cell_angle_beta     107.8774(14)
_cell_angle_gamma     90.00
_cell_volume     2485.27(10)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     2913
_cell_measurement_theta_min     2.81
_cell_measurement_theta_max     27.50
_cell_measurement_temperature     150(2)
_exptl_crystal_description     block
_exptl_crystal_colour     colourless
_exptl_crystal_size_max      .42
_exptl_crystal_size_mid      .40
_exptl_crystal_size_min      .38
_exptl_crystal_density_diffrn     1.420
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     1128
_exptl_absorpt_coefficient_mu      .823
_exptl_absorpt_correction_type     Multi-scan
_exptl_absorpt_process_details     'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min      .7236
_exptl_absorpt_correction_T_max      .7449
_exptl_special_details
;
 The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling
 algorithm [Fox, G.C. & Holmes, K.C. (1966).  Acta Cryst. 20,
 886-891] which effectively corrects for
 absorption effects. High redundancy data were used in the scaling
 program hence the 'multi-scan' code word was used. No transmission
 coefficients are available from the program (only scale factors for each
 frame). The scale factors in the experimental table are calculated
 from the 'size' command in the SHELXL-97 input file.
;
_diffrn_ambient_temperature     150(2)
_diffrn_radiation_type     'Mo K\a'
_diffrn_radiation_wavelength      .71073
_diffrn_radiation_source     'fine-focus sealed X-ray tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Kappa-CCD'
_diffrn_measurement_method     'φ scans, and ω scans with κ offsets'
_diffrn_reflns_number     12342
_diffrn_reflns_av_R_equivalents      .032
_diffrn_reflns_av_sigmaI/netI      .0338
_diffrn_reflns_theta_min     2.81
_diffrn_reflns_theta_max     27.50
_diffrn_reflns_theta_full     27.50
_diffrn_measured_fraction_theta_max      .992
_diffrn_measured_fraction_theta_full      .992
_diffrn_reflns_limit_h_min     0
_diffrn_reflns_limit_h_max     23
_diffrn_reflns_limit_k_min     0
_diffrn_reflns_limit_k_max     10
_diffrn_reflns_limit_l_min     -21
_diffrn_reflns_limit_l_max     20
_diffrn_standards_decay_%     negligible
_reflns_number_total     2823
_reflns_number_gt     2395
_reflns_threshold_expression     >2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all      .0366
_refine_ls_R_factor_gt      .0283
_refine_ls_wR_factor_gt      .0696
_refine_ls_wR_factor_ref      .0738
_refine_ls_goodness_of_fit_ref     1.050
_refine_ls_restrained_S_all     1.050
_refine_ls_number_reflns     2823
_refine_ls_number_parameters     161
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
              'w=1/[σ²(Fo²)+(0.0282P)²+2.6861P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max      .000
_refine_ls_shift/su_mean      .000
_refine_diff_density_max      .320
_refine_diff_density_min      -.344
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef      .0023(3)
_refine_ls_extinction_expression
                                  'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'C' 'C'  .0033  .0016
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'H' 'H'  .0000  .0000
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'N' 'N'  .0061  .0033
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Ni' 'Ni'  .3393 1.1124
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'O' 'O'  .0106  .0060
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'Kappa-CCD server software (Nonius, 1997)'
_computing_cell_refinement     'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction     'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)'
_computing_structure_refinement     'SHELXL-97 (Sheldrick, 1997b)'
_computing_molecular_graphics     'PLATON (Spek, 2001)'
_computing_publication_material
                    'SHELXL-97 (Sheldrick, 1997b) and PRPKAPPA (Ferguson, 1999)'
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Ni1  .5000  .5000  .5000  .01544(10) Uani d S 1 . . Ni
    N1  .55981(7)  .42978(16)  .42106(8)  .0203(3) Uani d . 1 . . N
    C2  .50599(10)  .3387(2)  .35408(10)  .0266(4) Uani d . 1 . . C
    C3  .45702(11)  .2348(2)  .39085(11)  .0294(4) Uani d . 1 . . C
    N4  .41827(8)  .33600(16)  .43749(8)  .0238(3) Uani d . 1 . . N
    C5  .38198(10)  .2450(2)  .49033(12)  .0316(4) Uani d . 1 . . C
    C6  .34463(10)  .3531(2)  .53936(12)  .0323(4) Uani d . 1 . . C
    C7  .39919(10)  .4466(2)  .60996(11)  .0270(4) Uani d . 1 . . C
    O11  .55427(6)  .32521(13)  .58986(7)  .0219(2) Uani d . 1 . . O
    O12  .64821(6)  .21858(14)  .54774(7)  .0231(3) Uani d . 1 . . O
    N14  .69692(8)  -.14447(18)  .89459(9)  .0283(3) Uani d . 1 . . N
    C11  .63534(8)  .13716(17)  .67784(9)  .0165(3) Uani d . 1 . . C
    C12  .59138(9)  .13522(18)  .73217(9)  .0186(3) Uani d . 1 . . C
    C13  .61119(9)  .04265(19)  .80356(10)  .0206(3) Uani d . 1 . . C
    C14  .67787(9)  -.04965(19)  .82489(10)  .0201(3) Uani d . 1 . . C
    C15  .72308(9)  -.0451(2)  .77074(10)  .0224(3) Uani d . 1 . . C
    C16  .70153(9)  .04533(19)  .69872(10)  .0201(3) Uani d . 1 . . C
    C17  .61086(8)  .23363(18)  .59906(9)  .0170(3) Uani d . 1 . . C
    H1  .5964  .3580  .4509  .024 Uiso calc R 1 . . H
    H2A  .5343  .2714  .3255  .032 Uiso calc R 1 . . H
    H2B  .4732  .4123  .3125  .032 Uiso calc R 1 . . H
    H3A  .4187  .1778  .3456  .035 Uiso calc R 1 . . H
    H3B  .4893  .1550  .4289  .035 Uiso calc R 1 . . H
    H4  .3800  .3916  .3984  .029 Uiso calc R 1 . . H
    H5A  .4210  .1784  .5299  .038 Uiso calc R 1 . . H
    H5B  .3429  .1732  .4545  .038 Uiso calc R 1 . . H
    H6A  .3112  .4293  .4999  .039 Uiso calc R 1 . . H
    H6B  .3118  .2871  .5630  .039 Uiso calc R 1 . . H
    H7A  .3702  .4970  .6439  .032 Uiso calc R 1 . . H
    H7B  .4366  .3727  .6465  .032 Uiso calc R 1 . . H
    H14A  .6672  -.1481  .9267  .034 Uiso calc R 1 . . H
    H14B  .7389  -.2017  .9072  .034 Uiso calc R 1 . . H
    H12  .5468  .1990  .7198  .022 Uiso calc R 1 . . H
    H13  .5794  .0415  .8385  .025 Uiso calc R 1 . . H
    H15  .7689  -.1050  .7840  .027 Uiso calc R 1 . . H
    H16  .7324  .0450  .6627  .024 Uiso calc R 1 . . H
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Ni1 N1 5_666 2.057(2) no
    Ni1 N1 . 2.057(2) no
    Ni1 N4 5_666 2.076(2) no
    Ni1 N4 . 2.076(2) no
    Ni1 O11 5_666 2.127(2) no
    Ni1 O11 . 2.127(2) no
    N1 C2 . 1.468(2) no
    N1 C7 5_666 1.473(2) no
    N1 H1 .  .93 no
    C2 C3 . 1.518(2) no
    C2 H2A .  .99 no
    C2 H2B .  .99 no
    C3 N4 . 1.482(2) no
    C3 H3A .  .99 no
    C3 H3B .  .99 no
    N4 C5 . 1.480(2) no
    N4 H4 .  .93 no
    C5 C6 . 1.527(3) no
    C5 H5A .  .99 no
    C5 H5B .  .99 no
    C6 C7 . 1.519(3) no
    C6 H6A .  .99 no
    C6 H6B .  .99 no
    C7 N1 5_666 1.473(2) no
    C7 H7A .  .99 no
    C7 H7B .  .99 no
    O11 C17 . 1.268(2) no
    O12 C17 . 1.266(2) no
    N14 C14 . 1.372(2) no
    N14 H14A .  .88 no
    N14 H14B .  .88 no
    C11 C16 . 1.395(2) no
    C11 C12 . 1.396(2) no
    C11 C17 . 1.501(2) no
    C12 C13 . 1.383(2) no
    C12 H12 .  .95 no
    C13 C14 . 1.405(2) no
    C13 H13 .  .95 no
    C14 C15 . 1.412(2) no
    C15 C16 . 1.382(2) no
    C15 H15 .  .95 no
    C16 H16 .  .95 no
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    N1 Ni1 N1 5_666 . 180.0 no
    N1 Ni1 N4 5_666 5_666 86.08(5) no
    N1 Ni1 N4 . 5_666 93.92(5) no
    N1 Ni1 N4 5_666 . 93.92(5) no
    N1 Ni1 N4 . . 86.08(5) no
    N4 Ni1 N4 5_666 . 180.0 no
    N1 Ni1 O11 5_666 5_666 91.83(5) no
    N1 Ni1 O11 . 5_666 88.18(5) no
    N4 Ni1 O11 5_666 5_666 90.60(5) no
    N4 Ni1 O11 . 5_666 89.40(5) no
    N1 Ni1 O11 5_666 . 88.18(5) no
    N1 Ni1 O11 . . 91.82(5) no
    N4 Ni1 O11 5_666 . 89.40(5) no
    N4 Ni1 O11 . . 90.60(5) no
    O11 Ni1 O11 5_666 . 180.0 no
    C2 N1 C7 . 5_666 113.4(2) no
    C2 N1 Ni1 . . 106.0(2) no
    C7 N1 Ni1 5_666 . 117.5(2) no
    C2 N1 H1 . . 106.4 no
    C7 N1 H1 5_666 . 106.4 no
    Ni1 N1 H1 . . 106.4 no
    N1 C2 C3 . . 109.5(2) no
    N1 C2 H2A . . 109.8 no
    C3 C2 H2A . . 109.8 no
    N1 C2 H2B . . 109.8 no
    C3 C2 H2B . . 109.8 no
    H2A C2 H2B . . 108.2 no
    N4 C3 C2 . . 109.2(2) no
    N4 C3 H3A . . 109.8 no
    C2 C3 H3A . . 109.8 no
    N4 C3 H3B . . 109.8 no
    C2 C3 H3B . . 109.8 no
    H3A C3 H3B . . 108.3 no
    C5 N4 C3 . . 113.7(2) no
    C5 N4 Ni1 . . 115.6(2) no
    C3 N4 Ni1 . . 104.9(2) no
    C5 N4 H4 . . 107.4 no
    C3 N4 H4 . . 107.4 no
    Ni1 N4 H4 . . 107.4 no
    N4 C5 C6 . . 112.2(2) no
    N4 C5 H5A . . 109.2 no
    C6 C5 H5A . . 109.2 no
    N4 C5 H5B . . 109.2 no
    C6 C5 H5B . . 109.2 no
    H5A C5 H5B . . 107.9 no
    C7 C6 C5 . . 115.5(2) no
    C7 C6 H6A . . 108.4 no
    C5 C6 H6A . . 108.4 no
    C7 C6 H6B . . 108.4 no
    C5 C6 H6B . . 108.4 no
    H6A C6 H6B . . 107.5 no
    N1 C7 C6 5_666 . 112.2(2) no
    N1 C7 H7A 5_666 . 109.2 no
    C6 C7 H7A . . 109.2 no
    N1 C7 H7B 5_666 . 109.2 no
    C6 C7 H7B . . 109.2 no
    H7A C7 H7B . . 107.9 no
    C17 O11 Ni1 . . 134.2(2) no
    C14 N14 H14A . . 120.0 no
    C14 N14 H14B . . 120.0 no
    H14A N14 H14B . . 120.0 no
    C16 C11 C12 . . 117.9(12) no
    C16 C11 C17 . . 121.7(2) no
    C12 C11 C17 . . 120.45(2) no
    C13 C12 C11 . . 121.6(2) no
    C13 C12 H12 . . 119.2 no
    C11 C12 H12 . . 119.2 no
    C12 C13 C14 . . 120.7(2) no
    C12 C13 H13 . . 119.7 no
    C14 C13 H13 . . 119.7 no
    N14 C14 C13 . . 120.9(2) no
    N14 C14 C15 . . 121.4(2) no
    C13 C14 C15 . . 117.7(2) no
    C16 C15 C14 . . 120.9(2) no
    C16 C15 H15 . . 119.6 no
    C14 C15 H15 . . 119.6 no
    C15 C16 C11 . . 121.3(2) no
    C15 C16 H16 . . 119.3 no
    C11 C16 H16 . . 119.3 no
    O12 C17 O11 . . 125.3(2) no
    O12 C17 C11 . . 118.0(2) no
    O11 C17 C11 . . 116.7(2) no
loop_
    _geom_torsion_atom_site_label_1
    _geom_torsion_atom_site_label_2
    _geom_torsion_atom_site_label_3
    _geom_torsion_atom_site_label_4
    _geom_torsion_site_symmetry_1
    _geom_torsion_site_symmetry_2
    _geom_torsion_site_symmetry_3
    _geom_torsion_site_symmetry_4
    _geom_torsion
    _geom_torsion_publ_flag
    N4 Ni1 N1 C2 5_666 . . . -166.3(2) no
    N4 Ni1 N1 C2 . . . . 13.7(2) no
    O11 Ni1 N1 C2 5_666 . . . -75.8(2) no
    O11 Ni1 N1 C2 . . . . 104.2(2) no
    N4 Ni1 N1 C7 5_666 . . 5_666 -38.4(2) no
    N4 Ni1 N1 C7 . . . 5_666 141.6(2) no
    O11 Ni1 N1 C7 5_666 . . 5_666 52.1(2) no
    O11 Ni1 N1 C7 . . . 5_666 -127.9(2) no
    C7 N1 C2 C3 5_666 . . . -170.3(2) no
    Ni1 N1 C2 C3 . . . . -40.0(2) no
    N1 C2 C3 N4 . . . . 56.3(2) no
    C2 C3 N4 C5 . . . . -168.0(2) no
    C2 C3 N4 Ni1 . . . . -40.8(2) no
    N1 Ni1 N4 C5 5_666 . . . -39.0(2) no
    N1 Ni1 N4 C5 . . . . 141.10(10)
                                  no
    O11 Ni1 N4 C5 5_666 . . . -130.7(2) no
    O11 Ni1 N4 C5 . . . . 49.3(2) no
    N1 Ni1 N4 C3 5_666 . . . -164.9(2) no
    N1 Ni1 N4 C3 . . . . 15.1(2) no
    O11 Ni1 N4 C3 5_666 . . . 103.3(2) no
    O11 Ni1 N4 C3 . . . . -76.7(2) no
    C3 N4 C5 C6 . . . . 178.3(2) no
    Ni1 N4 C5 C6 . . . . 57.0(2) no
    N4 C5 C6 C7 . . . . -70.8(2) no
    C5 C6 C7 N1 . . . 5_666 69.0(2) no
    N1 Ni1 O11 C17 5_666 . . . -168.7(2) no
    N1 Ni1 O11 C17 . . . . 11.4(2) no
    N4 Ni1 O11 C17 5_666 . . . -82.6(2) no
    N4 Ni1 O11 C17 . . . . 97.5(2) no
    C16 C11 C12 C13 . . . . -1.6(2) no
    C17 C11 C12 C13 . . . . 177.5(2) no
    C11 C12 C13 C14 . . . . 1.8(2) no
    C12 C13 C14 N14 . . . . -178.5(2) no
    C12 C13 C14 C15 . . . .  -.5(2) no
    N14 C14 C15 C16 . . . . 177.1(2) no
    C13 C14 C15 C16 . . . . -1.0(2) no
    C14 C15 C16 C11 . . . . 1.1(3) no
    C12 C11 C16 C15 . . . .  .1(2) no
    C17 C11 C16 C15 . . . . -179.0(2) no
    Ni1 O11 C17 O12 . . . . -5.3(2) no
    Ni1 O11 C17 C11 . . . . 174.1(2) no
    C16 C11 C17 O12 . . . . 6.3(2) no
    C12 C11 C17 O12 . . . . -172.8(2) no
    C16 C11 C17 O11 . . . . -173.1(2) no
    C12 C11 C17 O11 . . . . 7.8(2) no
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    _geom_hbond_publ_flag
    N1 H1 O12 .  .93 2.00 2.868(2) 155 y
    N14 H14A O12 6_556  .88 2.25 3.043(2) 150 y
    N14 H14B O12 4_646  .88 2.10 2.954(2) 165 y
data_VI
_chemical_name_systematic
;
[Aqua-(5-hydroxyisophthalato)-1,4,8,11-
tetraazacyclotetradecanenickel(II)] tetrahydrate
;
_chemical_name_common     ?
_chemical_formula_moiety     'C18 H30 N4 Ni O6, 4(H2 O)'
_chemical_formula_sum     'C18 H38 N4 Ni O10'
_chemical_formula_weight     529.23
_chemical_melting_point     ?
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'Cc'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    'x, -y, z+1/2'
    'x+1/2, y+1/2, z'
    'x+1/2, -y+1/2, z+1/2'
_cell_length_a     18.4057(8)
_cell_length_b     9.6927(4)
_cell_length_c     13.4648(5)
_cell_angle_alpha     90.00
_cell_angle_beta     96.724(2)
_cell_angle_gamma     90.00
_cell_volume     2385.61(17)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     2739
_cell_measurement_theta_min     2.75
_cell_measurement_theta_max     27.48
_cell_measurement_temperature     150(2)
_exptl_crystal_description     plate
_exptl_crystal_colour     purple
_exptl_crystal_size_max      .36
_exptl_crystal_size_mid      .34
_exptl_crystal_size_min      .04
_exptl_crystal_density_diffrn     1.474
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     1128
_exptl_absorpt_coefficient_mu      .873
_exptl_absorpt_correction_type     Multi-scan
_exptl_absorpt_process_details     'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min      .7441
_exptl_absorpt_correction_T_max      .9659
_exptl_special_details
;
 The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling
 algorithm [Fox, G.C. & Holmes, K.C. (1966).  Acta Cryst. 20,
 886-891] which effectively corrects for
 absorption effects. High redundancy data were used in the scaling
 program hence the 'multi-scan' code word was used. No transmission
 coefficients are available from the program (only scale factors for each
 frame). The scale factors in the experimental table are calculated
 from the 'size' command in the SHELXL-97 input file.
;
_diffrn_ambient_temperature     150(2)
_diffrn_radiation_type     'Mo K\a'
_diffrn_radiation_wavelength      .71073
_diffrn_radiation_source     'fine-focus sealed X-ray tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Kappa-CCD'
_diffrn_measurement_method     'φ scans, and ω scans with κ offsets'
_diffrn_reflns_number     9912
_diffrn_reflns_av_R_equivalents      .051
_diffrn_reflns_av_sigmaI/netI      .0633
_diffrn_reflns_theta_min     2.75
_diffrn_reflns_theta_max     27.48
_diffrn_reflns_theta_full     27.48
_diffrn_measured_fraction_theta_max      .993
_diffrn_measured_fraction_theta_full      .993
_diffrn_reflns_limit_h_min     -23
_diffrn_reflns_limit_h_max     23
_diffrn_reflns_limit_k_min     -12
_diffrn_reflns_limit_k_max     12
_diffrn_reflns_limit_l_min     -17
_diffrn_reflns_limit_l_max     17
_diffrn_standards_decay_%     negligible
_reflns_number_total     5106
_reflns_number_gt     4757
_reflns_threshold_expression     >2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all      .0397
_refine_ls_R_factor_gt      .0344
_refine_ls_wR_factor_gt      .0782
_refine_ls_wR_factor_ref      .0817
_refine_ls_goodness_of_fit_ref     1.031
_refine_ls_restrained_S_all     1.030
_refine_ls_number_reflns     5106
_refine_ls_number_parameters     342
_refine_ls_number_restraints     12
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
                      'w=1/[σ²(Fo²)P)²+2.7841P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max      .009
_refine_ls_shift/su_mean      .001
_refine_diff_density_max      .348
_refine_diff_density_min      -.362
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef      .0014(3)
_refine_ls_extinction_expression
                                  'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details     'Flack (1983),  2357 Friedel pairs'
_refine_ls_abs_structure_Flack      .434(11)
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'C' 'C'  .0033  .0016
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'H' 'H'  .0000  .0000
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'N' 'N'  .0061  .0033
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Ni' 'Ni'  .3393 1.1124
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'O' 'O'  .0106  .0060
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'Kappa-CCD server software (Nonius, 1997)'
_computing_cell_refinement     'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction     'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)'
_computing_structure_refinement     'SHELXL-97 (Sheldrick, 1997b)'
_computing_molecular_graphics     'PLATON (Spek, 2001)'
_computing_publication_material
                    'SHELXL-97 (Sheldrick, 1997b) and PRPKAPPA (Ferguson, 1999)'
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Ni1  .500367(18)  .19694(3)  .50001(2)  .01553(9) Uani d . 1 . . Ni
    N1  .51041(13)  .0522(2)  .38875(16)  .0181(5) Uani d . 1 . . N
    C2  .57352(16)  .0933(4)  .3380(2)  .0239(6) Uani d . 1 . . C
    C3  .57334(16)  .2497(4)  .3287(2)  .0221(6) Uani d . 1 . . C
    N4  .57657(13)  .3102(2)  .43020(16)  .0204(5) Uani d . 1 . . N
    C5  .56531(18)  .4616(3)  .4298(2)  .0267(6) Uani d . 1 . . C
    C6  .56375(18)  .5197(3)  .5343(2)  .0279(6) Uani d . 1 . . C
    C7  .49540(17)  .4861(3)  .5834(2)  .0240(6) Uani d . 1 . . C
    N8  .49288(13)  .3398(2)  .61357(16)  .0192(5) Uani d . 1 . . N
    C9  .42410(18)  .3013(3)  .6536(2)  .0243(7) Uani d . 1 . . C
    C10  .42015(17)  .1450(4)  .6640(2)  .0248(7) Uani d . 1 . . C
    N11  .42452(13)  .0827(2)  .56478(16)  .0187(5) Uani d . 1 . . N
    C12  .43508(17)  -.0686(3)  .5693(2)  .0249(6) Uani d . 1 . . C
    C13  .44081(17)  -.1301(3)  .4667(2)  .0240(6) Uani d . 1 . . C
    C14  .51042(16)  -.0937(3)  .4208(2)  .0226(6) Uani d . 1 . . C
    O1  .41696(11)  .3069(2)  .41743(13)  .0200(4) Uani d . 1 . . O
    O2  .37648(11)  .1701(2)  .28844(14)  .0227(4) Uani d . 1 . . O
    O3  .25257(12)  .7176(2)  .47024(14)  .0234(4) Uani d . 1 . . O
    O4  .24784(12)  .8581(2)  .34041(14)  .0239(4) Uani d . 1 . . O
    O5  .22645(11)  .5052(2)  .05556(13)  .0194(4) Uani d . 1 . . O
    C21  .33005(14)  .3993(3)  .29374(19)  .0173(5) Uani d . 1 . . C
    C22  .31571(15)  .5105(3)  .35362(18)  .0169(5) Uani d . 1 . . C
    C23  .27343(14)  .6215(3)  .31330(18)  .0156(5) Uani d . 1 . . C
    C24  .24506(15)  .6192(3)  .2125(2)  .0171(5) Uani d . 1 . . C
    C25  .25802(14)  .5062(3)  .15356(18)  .0151(5) Uani d . 1 . . C
    C26  .30025(14)  .3959(3)  .19354(18)  .0164(5) Uani d . 1 . . C
    C27  .37760(15)  .2817(3)  .33636(18)  .0168(5) Uani d . 1 . . C
    C28  .25685(14)  .7408(3)  .37872(18)  .0164(5) Uani d . 1 . . C
    O6  .58776(11)  .0983(2)  .59862(14)  .0214(4) Uani d D 1 . . O
    O7  .63580(12)  .2779(2)  .74172(16)  .0275(5) Uani d D 1 . . O
    O8  .67775(13)  .2377(2)  .93999(15)  .0287(5) Uani d D 1 . . O
    O9  .76311(12)  .4569(2) 1.00127(16)  .0254(4) Uani d D 1 . . O
    O10  .75061(12)  .5538(2) 1.19632(14)  .0247(4) Uani d D 1 . . O
    H1  .4694  .0630  .3421  .022 Uiso calc R 1 . . H
    H2A  .5701  .0506  .2708  .029 Uiso calc R 1 . . H
    H2B  .6195  .0620  .3770  .029 Uiso calc R 1 . . H
    H3A  .6161  .2804  .2962  .027 Uiso calc R 1 . . H
    H3B  .5283  .2806  .2872  .027 Uiso calc R 1 . . H
    H4  .6227  .2922  .4636  .025 Uiso calc R 1 . . H
    H5A  .5185  .4836  .3888  .032 Uiso calc R 1 . . H
    H5B  .6052  .5066  .3984  .032 Uiso calc R 1 . . H
    H6C  .5687  .6212  .5311  .034 Uiso calc R 1 . . H
    H6D  .6069  .4841  .5776  .034 Uiso calc R 1 . . H
    H7C  .4941  .5453  .6431  .029 Uiso calc R 1 . . H
    H7D  .4516  .5074  .5360  .029 Uiso calc R 1 . . H
    H8  .5315  .3241  .6633  .023 Uiso calc R 1 . . H
    H9C  .3817  .3346  .6079  .029 Uiso calc R 1 . . H
    H9D  .4224  .3452  .7197  .029 Uiso calc R 1 . . H
    H10C  .4612  .1118  .7122  .030 Uiso calc R 1 . . H
    H10D  .3736  .1185  .6890  .030 Uiso calc R 1 . . H
    H11  .3796  .0983  .5272  .022 Uiso calc R 1 . . H
    H12A  .3934  -.1116  .5980  .030 Uiso calc R 1 . . H
    H12B  .4802  -.0899  .6141  .030 Uiso calc R 1 . . H
    H13A  .3982  -.0989  .4205  .029 Uiso calc R 1 . . H
    H13B  .4377  -.2318  .4718  .029 Uiso calc R 1 . . H
    H14A  .5535  -.1108  .4706  .027 Uiso calc R 1 . . H
    H14B  .5146  -.1541  .3625  .027 Uiso calc R 1 . . H
    H5  .2404  .4350  .0265  .029 Uiso calc R 1 . . H
    H22  .3347  .5113  .4223  .020 Uiso calc R 1 . . H
    H24  .2169  .6948  .1843  .020 Uiso calc R 1 . . H
    H26  .3087  .3189  .1529  .020 Uiso calc R 1 . . H
    H6A  .609(2)  .143(4)  .653(3)  .052(13) Uiso d D 1 . . H
    H6B  .6248(18)  .050(4)  .577(3)  .040(11) Uiso d D 1 . . H
    H7A  .641(2)  .259(4)  .804(2)  .038(11) Uiso d D 1 . . H
    H7B  .670(2)  .334(4)  .722(3)  .040(11) Uiso d D 1 . . H
    H8A  .710(2)  .301(4)  .960(3)  .050(13) Uiso d D 1 . . H
    H8B  .697(3)  .163(4)  .968(4)  .068(15) Uiso d D 1 . . H
    H9A  .758(2)  .489(4) 1.059(2)  .035(10) Uiso d D 1 . . H
    H9B  .758(2)  .520(3)  .954(2)  .030(10) Uiso d D 1 . . H
    H10A  .7918(17)  .602(3) 1.222(2)  .026(8) Uiso d D 1 . . H
    H10B  .752(4)  .489(5) 1.240(4)  .11(2) Uiso d D 1 . . H
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Ni1 N11 . 2.054(2) no
    Ni1 N1 . 2.077(2) no
    Ni1 N8 . 2.079(2) no
    Ni1 O1 . 2.081(2) no
    Ni1 N4 . 2.089(2) no
    Ni1 O6 . 2.183(2) no
    N1 C2 . 1.470(4) no
    N1 C14 . 1.479(4) no
    N1 H1 .  .9300 no
    C2 C3 . 1.521(5) no
    C2 H2A .  .9900 no
    C2 H2B .  .9900 no
    C3 N4 . 1.481(4) no
    C3 H3A .  .9900 no
    C3 H3B .  .9900 no
    N4 C5 . 1.482(4) no
    N4 H4 .  .9300 no
    C5 C6 . 1.520(4) no
    C5 H5A .  .9900 no
    C5 H5B .  .9900 no
    C6 C7 . 1.523(5) no
    C6 H6C .  .9900 no
    C6 H6D .  .9900 no
    C7 N8 . 1.477(4) no
    C7 H7C .  .9900 no
    C7 H7D .  .9900 no
    N8 C9 . 1.481(4) no
    N8 H8 .  .9300 no
    C9 C10 . 1.524(4) no
    C9 H9C .  .9900 no
    C9 H9D .  .9900 no
    C10 N11 . 1.477(4) no
    C10 H10C .  .9900 no
    C10 H10D .  .9900 no
    N11 C12 . 1.480(4) no
    N11 H11 .  .9300 no
    C12 C13 . 1.519(4) no
    C12 H12A .  .9900 no
    C12 H12B .  .9900 no
    C13 C14 . 1.527(4) no
    C13 H13A .  .9900 no
    C13 H13B .  .9900 no
    C14 H14A .  .9900 no
    C14 H14B .  .9900 no
    O1 C27 . 1.261(3) no
    O2 C27 . 1.258(3) no
    O3 C28 . 1.264(3) no
    O4 C28 . 1.252(3) no
    O5 C25 . 1.378(3) no
    O5 H5 .  .8400 no
    C21 C22 . 1.390(4) no
    C21 C26 . 1.396(3) no
    C21 C27 . 1.509(4) no
    C22 C23 . 1.399(4) no
    C22 H22 .  .9500 no
    C23 C24 . 1.396(3) no
    C23 C28 . 1.507(4) no
    C24 C25 . 1.390(4) no
    C24 H24 .  .9500 no
    C25 C26 . 1.392(4) no
    C26 H26 .  .9500 no
    O6 H6A .  .90(3) no
    O6 H6B .  .90(3) no
    O7 H7A .  .86(3) no
    O7 H7B .  .89(3) no
    O8 H8A .  .88(3) no
    O8 H8B .  .87(3) no
    O9 H9A .  .85(3) no
    O9 H9B .  .88(3) no
    O10 H10A .  .92(3) no
    O10 H10B .  .87(3) no
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    N11 Ni1 N1 . . 93.70(9) no
    N11 Ni1 N8 . . 86.6(2) no
    N1 Ni1 N8 . . 178.5(2) no
    N11 Ni1 O1 . . 90.42(9) no
    N1 Ni1 O1 . . 94.76(8) no
    N8 Ni1 O1 . . 86.77(8) no
    N11 Ni1 N4 . . 178.34(9) no
    N1 Ni1 N4 . . 84.80(9) no
    N8 Ni1 N4 . . 94.97(9) no
    O1 Ni1 N4 . . 89.01(9) no
    N11 Ni1 O6 . . 89.69(8) no
    N1 Ni1 O6 . . 91.22(8) no
    N8 Ni1 O6 . . 87.25(8) no
    O1 Ni1 O6 . . 174.00(8) no
    N4 Ni1 O6 . . 91.04(8) no
    C2 N1 C14 . . 115.0(2) no
    C2 N1 Ni1 . . 107.1(2) no
    C14 N1 Ni1 . . 115.6(2) no
    C2 N1 H1 . . 106.1 no
    C14 N1 H1 . . 106.1 no
    Ni1 N1 H1 . . 106.1 no
    N1 C2 C3 . . 108.3(2) no
    N1 C2 H2A . . 110.0 no
    C3 C2 H2A . . 110.0 no
    N1 C2 H2B . . 110.0 no
    C3 C2 H2B . . 110.0 no
    H2A C2 H2B . . 108.4 no
    N4 C3 C2 . . 108.6(2) no
    N4 C3 H3A . . 110.0 no
    C2 C3 H3A . . 110.0 no
    N4 C3 H3B . . 110.0 no
    C2 C3 H3B . . 110.0 no
    H3A C3 H3B . . 108.3 no
    C3 N4 C5 . . 113.4(2) no
    C3 N4 Ni1 . . 104.5(2) no
    C5 N4 Ni1 . . 114.9(2) no
    C3 N4 H4 . . 107.9 no
    C5 N4 H4 . . 107.9 no
    Ni1 N4 H4 . . 107.9 no
    N4 C5 C6 . . 112.4(2) no
    N4 C5 H5A . . 109.1 no
    C6 C5 H5A . . 109.1 no
    N4 C5 H5B . . 109.1 no
    C6 C5 H5B . . 109.1 no
    H5A C5 H5B . . 107.9 no
    C5 C6 C7 . . 115.4(3) no
    C5 C6 H6C . . 108.4 no
    C7 C6 H6C . . 108.4 no
    C5 C6 H6D . . 108.4 no
    C7 C6 H6D . . 108.4 no
    H6C C6 H6D . . 107.5 no
    N8 C7 C6 . . 112.2(2) no
    N8 C7 H7C . . 109.2 no
    C6 C7 H7C . . 109.2 no
    N8 C7 H7D . . 109.2 no
    C6 C7 H7D . . 109.2 no
    H7C C7 H7D . . 107.9 no
    C7 N8 C9 . . 113.4(2) no
    C7 N8 Ni1 . . 115.5(2) no
    C9 N8 Ni1 . . 103.5(2) no
    C7 N8 H8 . . 108.0 no
    C9 N8 H8 . . 108.0 no
    Ni1 N8 H8 . . 108.0 no
    N8 C9 C10 . . 109.6(2) no
    N8 C9 H9C . . 109.7 no
    C10 C9 H9C . . 109.7 no
    N8 C9 H9D . . 109.7 no
    C10 C9 H9D . . 109.7 no
    H9C C9 H9D . . 108.2 no
    N11 C10 C9 . . 108.4(2) no
    N11 C10 H10C . . 110.0 no
    C9 C10 H10C . . 110.0 no
    N11 C10 H10D . . 110.0 no
    C9 C10 H10D . . 110.0 no
    H10C C10 H10D . . 108.4 no
    C10 N11 C12 . . 112.9(2) no
    C10 N11 Ni1 . . 106.0(2) no
    C12 N11 Ni1 . . 117.3(2) no
    C10 N11 H11 . . 106.7 no
    C12 N11 H11 . . 106.7 no
    Ni1 N11 H11 . . 106.7 no
    N11 C12 C13 . . 112.0(2) no
    N11 C12 H12A . . 109.2 no
    C13 C12 H12A . . 109.2 no
    N11 C12 H12B . . 109.2 no
    C13 C12 H12B . . 109.2 no
    H12A C12 H12B . . 107.9 no
    C12 C13 C14 . . 115.3(2) no
    C12 C13 H13A . . 108.4 no
    C14 C13 H13A . . 108.4 no
    C12 C13 H13B . . 108.4 no
    C14 C13 H13B . . 108.4 no
    H13A C13 H13B . . 107.5 no
    N1 C14 C13 . . 111.6(2) no
    N1 C14 H14A . . 109.3 no
    C13 C14 H14A . . 109.3 no
    N1 C14 H14B . . 109.3 no
    C13 C14 H14B . . 109.3 no
    H14A C14 H14B . . 108.0 no
    C27 O1 Ni1 . . 132.6(2) no
    C25 O5 H5 . . 109.5 no
    C22 C21 C26 . . 119.9(2) no
    C22 C21 C27 . . 120.4(2) no
    C26 C21 C27 . . 119.6(2) no
    C21 C22 C23 . . 120.4(2) no
    C21 C22 H22 . . 119.8 no
    C23 C22 H22 . . 119.8 no
    C24 C23 C22 . . 119.6(2) no
    C24 C23 C28 . . 120.1(2) no
    C22 C23 C28 . . 120.3(2) no
    C25 C24 C23 . . 119.9(2) no
    C25 C24 H24 . . 120.1 no
    C23 C24 H24 . . 120.1 no
    O5 C25 C24 . . 118.1(2) no
    O5 C25 C26 . . 121.2(2) no
    C24 C25 C26 . . 120.6(2) no
    C25 C26 C21 . . 119.6(2) no
    C25 C26 H26 . . 120.2 no
    C21 C26 H26 . . 120.2 no
    O2 C27 O1 . . 125.7(2) no
    O2 C27 C21 . . 118.7(2) no
    O1 C27 C21 . . 115.6(2) no
    O4 C28 O3 . . 122.9(2) no
    O4 C28 C23 . . 118.9(2) no
    O3 C28 C23 . . 118.2(2) no
    Ni1 O6 H6A . . 120(3) no
    Ni1 O6 H6B . . 124(2) no
    H6A O6 H6B . . 103(4) no
    H7A O7 H7B . . 115(4) no
    H8A O8 H8B . . 103(4) no
    H9A O9 H9B . . 113(4) no
    H10A O10 H10B . . 99(5) no
loop_
    _geom_torsion_atom_site_label_1
    _geom_torsion_atom_site_label_2
    _geom_torsion_atom_site_label_3
    _geom_torsion_atom_site_label_4
    _geom_torsion_site_symmetry_1
    _geom_torsion_site_symmetry_2
    _geom_torsion_site_symmetry_3
    _geom_torsion_site_symmetry_4
    _geom_torsion
    _geom_torsion_publ_flag
    N11 Ni1 N1 C2 . . . . -169.5(2) no
    O1 Ni1 N1 C2 . . . . 99.8(2) no
    N4 Ni1 N1 C2 . . . . 11.2(2) no
    O6 Ni1 N1 C2 . . . . -79.7(12) no
    N11 Ni1 N1 C14 . . . . -39.9(2) no
    O1 Ni1 N1 C14 . . . . -130.6(2) no
    N4 Ni1 N1 C14 . . . . 140.8(2) no
    O6 Ni1 N1 C14 . . . . 49.9(2) no
    C14 N1 C2 C3 . . . . -168.8(2) no
    Ni1 N1 C2 C3 . . . . -38.9(2) no
    N1 C2 C3 N4 . . . . 58.3(3) no
    C2 C3 N4 C5 . . . . -171.2(2) no
    C2 C3 N4 Ni1 . . . . -45.3(2) no
    N1 Ni1 N4 C3 . . . . 18.8(2) no
    N8 Ni1 N4 C3 . . . . -162.7(2) no
    O1 Ni1 N4 C3 . . . . -76.1(2) no
    O6 Ni1 N4 C3 . . . . 110.0(2) no
    N1 Ni1 N4 C5 . . . . 143.8(2) no
    N8 Ni1 N4 C5 . . . . -37.8(2) no
    O1 Ni1 N4 C5 . . . . 48.9(2) no
    O6 Ni1 N4 C5 . . . . -125.1(2) no
    C3 N4 C5 C6 . . . . 176.1(2) no
    Ni1 N4 C5 C6 . . . . 56.0(3) no
    N4 C5 C6 C7 . . . . -72.3(3) no
    C5 C6 C7 N8 . . . . 72.0(3) no
    C6 C7 N8 C9 . . . . -175.1(2) no
    C6 C7 N8 Ni1 . . . . -55.9(3) no
    N11 Ni1 N8 C7 . . . . -141.4(2) no
    O1 Ni1 N8 C7 . . . . -50.8(2) no
    N4 Ni1 N8 C7 . . . . 37.9(2) no
    O6 Ni1 N8 C7 . . . . 128.7(2) no
    N11 Ni1 N8 C9 . . . . -16.9(2) no
    O1 Ni1 N8 C9 . . . . 73.7(2) no
    N4 Ni1 N8 C9 . . . . 162.5(2) no
    O6 Ni1 N8 C9 . . . . -106.8(2) no
    C7 N8 C9 C10 . . . . 169.3(2) no
    Ni1 N8 C9 C10 . . . . 43.5(2) no
    N8 C9 C10 N11 . . . . -58.1(3) no
    C9 C10 N11 C12 . . . . 169.3(2) no
    C9 C10 N11 Ni1 . . . . 39.5(3) no
    N1 Ni1 N11 C10 . . . . 165.8(2) no
    N8 Ni1 N11 C10 . . . . -12.7(2) no
    O1 Ni1 N11 C10 . . . . -99.4(2) no
    O6 Ni1 N11 C10 . . . . 74.6(2) no
    N1 Ni1 N11 C12 . . . . 38.7(2) no
    N8 Ni1 N11 C12 . . . . -139.8(2) no
    O1 Ni1 N11 C12 . . . . 133.5(2) no
    O6 Ni1 N11 C12 . . . . -52.5(2) no
    C10 N11 C12 C13 . . . . -179.0(2) no
    Ni1 N11 C12 C13 . . . . -55.3(3) no
    N11 C12 C13 C14 . . . . 69.5(3) no
    C2 N1 C14 C13 . . . . -176.3(2) no
    Ni1 N1 C14 C13 . . . . 58.0(3) no
    C12 C13 C14 N1 . . . . -71.6(3) no
    N11 Ni1 O1 C27 . . . . -82.8(3) no
    N1 Ni1 O1 C27 . . . . 10.9(3) no
    N8 Ni1 O1 C27 . . . . -169.4(3) no
    N4 Ni1 O1 C27 . . . . 95.6(3) no
    C26 C21 C22 C23 . . . . -2.0(4) no
    C27 C21 C22 C23 . . . . 178.1(2) no
    C21 C22 C23 C24 . . . .  .6(4) no
    C21 C22 C23 C28 . . . . 178.9(2) no
    C22 C23 C24 C25 . . . . 1.0(4) no
    C28 C23 C24 C25 . . . . -177.3(3) no
    C23 C24 C25 O5 . . . . 177.2(2) no
    C23 C24 C25 C26 . . . . -1.2(4) no
    O5 C25 C26 C21 . . . . -178.6(2) no
    C24 C25 C26 C21 . . . .  -.2(4) no
    C22 C21 C26 C25 . . . . 1.8(4) no
    C27 C21 C26 C25 . . . . -178.3(2) no
    Ni1 O1 C27 O2 . . . . 6.7(4) no
    Ni1 O1 C27 C21 . . . . -171.4(2) no
    C22 C21 C27 O2 . . . . 164.3(3) no
    C26 C21 C27 O2 . . . . -15.6(4) no
    C22 C21 C27 O1 . . . . -17.5(4) no
    C26 C21 C27 O1 . . . . 162.7(2) no
    C24 C23 C28 O4 . . . . -31.6(4) no
    C22 C23 C28 O4 . . . . 150.1(3) no
    C24 C23 C28 O3 . . . . 148.3(3) no
    C22 C23 C28 O3 . . . . -30.0(4) no
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    _geom_hbond_publ_flag
    N1 H1 O2 .  .93 2.06 2.903(3) 150 y
    N4 H4 O3 3_545  .93 2.49 3.344(3) 153 y
    N8 H8 O7 .  .93 2.13 3.032(3) 164 y
    N11 H11 O9 4_454  .93 2.20 3.018(3) 147 y
    O5 H5 O3 2_564  .84 1.69 2.519(3) 169 y
    O6 H6A O7 .  .90(3) 1.80(3) 2.670(3) 161(4) y
    O6 H6B O5 4  .90(3) 2.00(3) 2.864(3) 160(4) y
    O7 H7A O8 .  .86(3) 1.88(3) 2.719(3) 164(4) y
    O7 H7B O10 2_564  .89(3) 1.91(3) 2.793(3) 172(4) y
    O8 H8A O9 .  .88(3) 1.84(3) 2.712(3) 169(4) y
    O8 H8B O5 3_546  .87(3) 1.97(3) 2.824(3) 167(5) y
    O9 H9A O10 .  .85(3) 1.97(3) 2.824(3) 176(4) y
    O9 H9B O4 4_565  .88(3) 1.93(3) 2.801(3) 174(4) y
    O10 H10A O2 3_556  .92(3) 1.83(3) 2.739(3) 169(3) y
    O10 H10B O4 3_546  .87(3) 1.85(3) 2.718(3) 174(8) y
data_VII
_chemical_name_systematic
;
catena-poly[terephthalato-1,4,8,11-
-tetraazacyclotetradecanenickel(II)] monohydrate
;
_chemical_name_common     ?
_chemical_formula_moiety     'C18 H28 N4 Ni O4, H2 O'
_chemical_formula_sum     'C18 H30 N4 Ni O5'
_chemical_formula_weight     441.17
_chemical_melting_point     ?
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'C2/c'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, y, -z+1/2'
    'x+1/2, y+1/2, z'
    '-x+1/2, y+1/2, -z+1/2'
    '-x, -y, -z'
    'x, -y, z-1/2'
    '-x+1/2, -y+1/2, -z'
    'x+1/2, -y+1/2, z-1/2'
_cell_length_a     16.2155(4)
_cell_length_b     16.0404(6)
_cell_length_c     8.8937(3)
_cell_angle_alpha     90.00
_cell_angle_beta     118.4900(16)
_cell_angle_gamma     90.00
_cell_volume     2033.14(11)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     2402
_cell_measurement_theta_min     2.63
_cell_measurement_theta_max     27.49
_cell_measurement_temperature     150(2)
_exptl_crystal_description     block
_exptl_crystal_colour     purple
_exptl_crystal_size_max      .18
_exptl_crystal_size_mid      .16
_exptl_crystal_size_min      .16
_exptl_crystal_density_diffrn     1.441
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     936
_exptl_absorpt_coefficient_mu      .991
_exptl_absorpt_correction_type     Multi-scan
_exptl_absorpt_process_details     'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min      .8418
_exptl_absorpt_correction_T_max      .8576
_exptl_special_details
;
 The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling
 algorithm [Fox, G.C. & Holmes, K.C. (1966).  Acta Cryst. 20,
 886-891] which effectively corrects for
 absorption effects. High redundancy data were used in the scaling
 program hence the 'multi-scan' code word was used. No transmission
 coefficients are available from the program (only scale factors for each
 frame). The scale factors in the experimental table are calculated
 from the 'size' command in the SHELXL-97 input file.
;
_diffrn_ambient_temperature     150(2)
_diffrn_radiation_type     'Mo K\a'
_diffrn_radiation_wavelength      .71073
_diffrn_radiation_source     'fine-focus sealed X-ray tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Kappa-CCD'
_diffrn_measurement_method     'φ scans, and ω scans with κ offsets'
_diffrn_reflns_number     12978
_diffrn_reflns_av_R_equivalents      .088
_diffrn_reflns_av_sigmaI/netI      .0786
_diffrn_reflns_theta_min     2.63
_diffrn_reflns_theta_max     27.49
_diffrn_reflns_theta_full     27.49
_diffrn_measured_fraction_theta_max      .997
_diffrn_measured_fraction_theta_full      .997
_diffrn_reflns_limit_h_min     0
_diffrn_reflns_limit_h_max     20
_diffrn_reflns_limit_k_min     0
_diffrn_reflns_limit_k_max     20
_diffrn_reflns_limit_l_min     -11
_diffrn_reflns_limit_l_max     10
_diffrn_standards_decay_%     negligible
_reflns_number_total     2333
_reflns_number_gt     1622
_reflns_threshold_expression     >2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all      .0888
_refine_ls_R_factor_gt      .0515
_refine_ls_wR_factor_gt      .1155
_refine_ls_wR_factor_ref      .1471
_refine_ls_goodness_of_fit_ref     1.067
_refine_ls_restrained_S_all     1.066
_refine_ls_number_reflns     2333
_refine_ls_number_parameters     134
_refine_ls_number_restraints     1
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
                      'w=1/[σ²(Fo²)+(0.0754P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max      .000
_refine_ls_shift/su_mean      .000
_refine_diff_density_max      .831
_refine_diff_density_min      -.853
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef      .0193(17)
_refine_ls_extinction_expression
                                  'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'C' 'C'  .0033  .0016
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'H' 'H'  .0000  .0000
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'N' 'N'  .0061  .0033
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Ni' 'Ni'  .3393 1.1124
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'O' 'O'  .0106  .0060
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'Kappa-CCD server software (Nonius, 1997)'
_computing_cell_refinement     'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction     'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)'
_computing_structure_refinement     'SHELXL-97 (Sheldrick, 1997b)'
_computing_molecular_graphics     'PLATON (Spek, 2001)'
_computing_publication_material
                    'SHELXL-97 (Sheldrick, 1997b) and PRPKAPPA (Ferguson, 1999)'
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Ni1  .2500  .2500  .0000  .0247(2) Uani d S 1 . . Ni
    N1  .17290(19)  .34829(15)  .0202(3)  .0269(6) Uani d . 1 . . N
    C2  .2208(2)  .3725(2)  .2020(4)  .0333(8) Uani d . 1 . . C
    C3  .2515(2)  .2942(2)  .3125(4)  .0326(8) Uani d . 1 . . C
    N4  .31102(19)  .24304(15)  .2643(3)  .0267(6) Uani d . 1 . . N
    C5  .3266(2)  .1572(2)  .3344(4)  .0334(8) Uani d . 1 . . C
    C6  .3900(2)  .1077(2)  .2841(4)  .0350(8) Uani d . 1 . . C
    C7  .3461(2)  .08048(19)  .0968(4)  .0333(8) Uani d . 1 . . C
    O1  .14783(15)  .16226(13)  -.0325(3)  .0301(5) Uani d . 1 . . O
    O2  .03070(16)  .22725(14)  -.0099(3)  .0338(6) Uani d . 1 . . O
    C11  .0346(2)  .07824(19)  -.0107(4)  .0270(7) Uani d . 1 . . C
    C12  .0720(2)  .0063(2)  -.0410(4)  .0304(7) Uani d . 1 . . C
    C13  -.0374(2)  .07130(19)  .0316(4)  .0288(7) Uani d . 1 . . C
    C14  .0733(2)  .16271(19)  -.0194(4)  .0268(7) Uani d . 1 . . C
    O3  .0000  .3041(3)  .2500  .0708(14) Uani d SD 1 . . O
    H1  .1149  .3266  -.0026  .032 Uiso calc R 1 . . H
    H2A  .1778  .4056  .2284  .040 Uiso calc R 1 . . H
    H2B  .2763  .4073  .2266  .040 Uiso calc R 1 . . H
    H3A  .2871  .3098  .4348  .039 Uiso calc R 1 . . H
    H3B  .1957  .2618  .2953  .039 Uiso calc R 1 . . H
    H4  .3693  .2689  .3091  .032 Uiso calc R 1 . . H
    H5A  .2655  .1284  .2910  .040 Uiso calc R 1 . . H
    H5B  .3557  .1598  .4607  .040 Uiso calc R 1 . . H
    H6A  .4117  .0573  .3568  .042 Uiso calc R 1 . . H
    H6B  .4461  .1419  .3104  .042 Uiso calc R 1 . . H
    H7A  .3891  .0412  .0830  .040 Uiso calc R 1 . . H
    H7B  .2866  .0507  .0656  .040 Uiso calc R 1 . . H
    H12  .1218  .0104  -.0684  .037 Uiso calc R 1 . . H
    H13  -.0629  .1201  .0541  .035 Uiso calc R 1 . . H
    H3  .008(6)  .266(3)  .190(8)  .11(2) Uiso d D 1 . . H
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Ni1 N1 7 2.072(3) no
    Ni1 N1 . 2.072(3) no
    Ni1 N4 . 2.073(3) no
    Ni1 N4 7 2.073(3) no
    Ni1 O1 . 2.086(2) no
    Ni1 O1 7 2.086(2) no
    N1 C2 . 1.473(4) no
    N1 C7 7 1.476(4) no
    N1 H1 .  .93 no
    C2 C3 . 1.524(4) no
    C2 H2A .  .99 no
    C2 H2B .  .99 no
    C3 N4 . 1.477(4) no
    C3 H3A .  .99 no
    C3 H3B .  .99 no
    N4 C5 . 1.482(4) no
    N4 H4 .  .93 no
    C5 C6 . 1.525(5) no
    C5 H5A .  .99 no
    C5 H5B .  .99 no
    C6 C7 . 1.530(4) no
    C6 H6A .  .99 no
    C6 H6B .  .99 no
    C7 N1 7 1.476(4) no
    C7 H7A .  .99 no
    C7 H7B .  .99 no
    O1 C14 . 1.269(3) no
    O2 C14 . 1.269(4) no
    C11 C12 . 1.388(4) no
    C11 C13 . 1.392(4) no
    C11 C14 . 1.510(4) no
    C12 C13 5 1.385(4) no
    C12 H12 .  .95 no
    C13 C12 5 1.385(4) no
    C13 H13 .  .95 no
    O3 H3 .  .86(7) no
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    N1 Ni1 N1 7 . 180 no
    N1 Ni1 N4 7 . 94.4(2) no
    N1 Ni1 N4 . . 85.7(2) no
    N1 Ni1 N4 7 7 85.7(2) no
    N1 Ni1 N4 . 7 94.4(2) no
    N4 Ni1 N4 . 7 180 no
    N1 Ni1 O1 7 . 87.0(2) no
    N1 Ni1 O1 . . 93.1(2) no
    N4 Ni1 O1 . . 92.22(9) no
    N4 Ni1 O1 7 . 87.78(9) no
    N1 Ni1 O1 7 7 93.1(2) no
    N1 Ni1 O1 . 7 87.0(2) no
    N4 Ni1 O1 . 7 87.78(9) no
    N4 Ni1 O1 7 7 92.22(9) no
    O1 Ni1 O1 . 7 180 no
    C2 N1 C7 . 7 113.2(2) no
    C2 N1 Ni1 . . 105.7(2) no
    C7 N1 Ni1 7 . 117.4(2) no
    C2 N1 H1 . . 106.6 no
    C7 N1 H1 7 . 106.6 no
    Ni1 N1 H1 . . 106.6 no
    N1 C2 C3 . . 109.3(3) no
    N1 C2 H2A . . 109.8 no
    C3 C2 H2A . . 109.8 no
    N1 C2 H2B . . 109.8 no
    C3 C2 H2B . . 109.8 no
    H2A C2 H2B . . 108.3 no
    N4 C3 C2 . . 109.1(2) no
    N4 C3 H3A . . 109.9 no
    C2 C3 H3A . . 109.9 no
    N4 C3 H3B . . 109.9 no
    C2 C3 H3B . . 109.9 no
    H3A C3 H3B . . 108.3 no
    C3 N4 C5 . . 113.4(2) no
    C3 N4 Ni1 . . 105.9(2) no
    C5 N4 Ni1 . . 114.9(2) no
    C3 N4 H4 . . 107.4 no
    C5 N4 H4 . . 107.4 no
    Ni1 N4 H4 . . 107.4 no
    N4 C5 C6 . . 111.4(3) no
    N4 C5 H5A . . 109.4 no
    C6 C5 H5A . . 109.4 no
    N4 C5 H5B . . 109.4 no
    C6 C5 H5B . . 109.4 no
    H5A C5 H5B . . 108.0 no
    C5 C6 C7 . . 116.1(3) no
    C5 C6 H6A . . 108.3 no
    C7 C6 H6A . . 108.3 no
    C5 C6 H6B . . 108.3 no
    C7 C6 H6B . . 108.3 no
    H6A C6 H6B . . 107.4 no
    N1 C7 C6 7 . 112.3(3) no
    N1 C7 H7A 7 . 109.2 no
    C6 C7 H7A . . 109.2 no
    N1 C7 H7B 7 . 109.2 no
    C6 C7 H7B . . 109.2 no
    H7A C7 H7B . . 107.9 no
    C14 O1 Ni1 . . 135.4(2) no
    C12 C11 C13 . . 119.1(3) no
    C12 C11 C14 . . 120.4(3) no
    C13 C11 C14 . . 120.5(3) no
    C13 C12 C11 5 . 120.5(3) no
    C13 C12 H12 5 . 119.7 no
    C11 C12 H12 . . 119.7 no
    C12 C13 C11 5 . 120.3(3) no
    C12 C13 H13 5 . 119.8 no
    C11 C13 H13 . . 119.8 no
    O1 C14 O2 . . 125.7(3) no
    O1 C14 C11 . . 115.9(3) no
    O2 C14 C11 . . 118.4(3) no
loop_
    _geom_torsion_atom_site_label_1
    _geom_torsion_atom_site_label_2
    _geom_torsion_atom_site_label_3
    _geom_torsion_atom_site_label_4
    _geom_torsion_site_symmetry_1
    _geom_torsion_site_symmetry_2
    _geom_torsion_site_symmetry_3
    _geom_torsion_site_symmetry_4
    _geom_torsion
    _geom_torsion_publ_flag
    N4 Ni1 N1 C2 . . . . 15.2(2) no
    N4 Ni1 N1 C2 7 . . . -164.8(2) no
    O1 Ni1 N1 C2 . . . . 107.2(2) no
    O1 Ni1 N1 C2 7 . . . -72.8(2) no
    N4 Ni1 N1 C7 . . . 7 142.5(2) no
    N4 Ni1 N1 C7 7 . . 7 -37.5(2) no
    O1 Ni1 N1 C7 . . . 7 -125.5(2) no
    O1 Ni1 N1 C7 7 . . 7 54.5(2) no
    C7 N1 C2 C3 7 . . . -170.9(3) no
    Ni1 N1 C2 C3 . . . . -41.1(3) no
    N1 C2 C3 N4 . . . . 56.1(3) no
    C2 C3 N4 C5 . . . . -166.7(3) no
    C2 C3 N4 Ni1 . . . . -39.8(3) no
    N1 Ni1 N4 C3 7 . . . -166.2(2) no
    N1 Ni1 N4 C3 . . . . 13.8(2) no
    O1 Ni1 N4 C3 . . . . -79.1(2) no
    O1 Ni1 N4 C3 7 . . . 100.9(2) no
    N1 Ni1 N4 C5 7 . . . -40.2(2) no
    N1 Ni1 N4 C5 . . . . 139.8(2) no
    O1 Ni1 N4 C5 . . . . 46.9(2) no
    O1 Ni1 N4 C5 7 . . . -133.1(2) no
    C3 N4 C5 C6 . . . . -178.8(2) no
    Ni1 N4 C5 C6 . . . . 59.1(3) no
    N4 C5 C6 C7 . . . . -72.6(4) no
    C5 C6 C7 N1 . . . 7 68.4(4) no
    N1 Ni1 O1 C14 7 . . . 170.1(3) no
    N1 Ni1 O1 C14 . . . . -9.9(3) no
    N4 Ni1 O1 C14 . . . . 75.9(3) no
    N4 Ni1 O1 C14 7 . . . -104.1(3) no
    C13 C11 C12 C13 . . . 5  .9(5) no
    C14 C11 C12 C13 . . . 5 179.4(3) no
    C12 C11 C13 C12 . . . 5  -.9(5) no
    C14 C11 C13 C12 . . . 5 -179.4(3) no
    Ni1 O1 C14 O2 . . . . 14.0(5) no
    Ni1 O1 C14 C11 . . . . -164.5(2) no
    C12 C11 C14 O1 . . . . -9.0(4) no
    C13 C11 C14 O1 . . . . 169.5(3) no
    C12 C11 C14 O2 . . . . 172.3(3) no
    C13 C11 C14 O2 . . . . -9.2(4) no
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    _geom_hbond_publ_flag
    N1 H1 O2 .  .93 2.08 2.927(4) 151 y
    N4 H4 O2 8_556  .93 2.33 3.182(3) 152 y
    O3 H3 O2 .  .86(7) 2.09(4) 2.865(3) 152(5) y
data_VIII
_chemical_name_systematic
;
 ?
;
_chemical_name_common     ?
_chemical_formula_moiety
                   '2(C15 H25 N4 Ni O4), C10 H28 N4 Ni O2, 2(Cl O4), 0.86(H2 O)'
_chemical_formula_sum     'C40 H79.72 Cl2 N12 Ni3 O18.86'
_chemical_formula_weight     1277.62
_chemical_melting_point     ?
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'P21/c'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, y+1/2, -z+1/2'
    '-x, -y, -z'
    'x, -y-1/2, z-1/2'
_cell_length_a     10.8295(3)
_cell_length_b     16.9416(5)
_cell_length_c     14.9596(5)
_cell_angle_alpha     90.00
_cell_angle_beta     93.6260(13)
_cell_angle_gamma     90.00
_cell_volume     2739.13(14)
_cell_formula_units_Z     2
_cell_measurement_reflns_used     6029
_cell_measurement_theta_min     2.56
_cell_measurement_theta_max     27.53
_cell_measurement_temperature     150(2)
_exptl_crystal_description     plate
_exptl_crystal_colour     purple
_exptl_crystal_size_max      .40
_exptl_crystal_size_mid      .36
_exptl_crystal_size_min      .12
_exptl_crystal_density_diffrn     1.550
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     1345
_exptl_absorpt_coefficient_mu     1.199
_exptl_absorpt_correction_type     Multi-scan
_exptl_absorpt_process_details     'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min      .6455
_exptl_absorpt_correction_T_max      .8694
_exptl_special_details
;
 The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling
 algorithm [Fox, G.C. & Holmes, K.C. (1966).  Acta Cryst. 20,
 886-891] which effectively corrects for
 absorption effects. High redundancy data were used in the scaling
 program hence the 'multi-scan' code word was used. No transmission
 coefficients are available from the program (only scale factors for each
 frame). The scale factors in the experimental table are calculated
 from the 'size' command in the SHELXL-97 input file.
;
_diffrn_ambient_temperature     150(2)
_diffrn_radiation_type     'Mo K\a'
_diffrn_radiation_wavelength      .71073
_diffrn_radiation_source     'fine-focus sealed X-ray tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Kappa-CCD'
_diffrn_measurement_method     'φ scans, and ω scans with κ offsets'
_diffrn_reflns_number     20675
_diffrn_reflns_av_R_equivalents      .039
_diffrn_reflns_av_sigmaI/netI      .0464
_diffrn_reflns_theta_min     2.56
_diffrn_reflns_theta_max     27.53
_diffrn_reflns_theta_full     27.53
_diffrn_measured_fraction_theta_max      .994
_diffrn_measured_fraction_theta_full      .994
_diffrn_reflns_limit_h_min     0
_diffrn_reflns_limit_h_max     14
_diffrn_reflns_limit_k_min     0
_diffrn_reflns_limit_k_max     21
_diffrn_reflns_limit_l_min     -19
_diffrn_reflns_limit_l_max     19
_diffrn_standards_decay_%     negligible
_reflns_number_total     6277
_reflns_number_gt     5362
_reflns_threshold_expression     >2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all      .0437
_refine_ls_R_factor_gt      .0342
_refine_ls_wR_factor_gt      .0841
_refine_ls_wR_factor_ref      .0904
_refine_ls_goodness_of_fit_ref     1.032
_refine_ls_restrained_S_all     1.033
_refine_ls_number_reflns     6277
_refine_ls_number_parameters     377
_refine_ls_number_restraints     12
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
              'w=1/[σ²(Fo²)+(0.0347P)²+1.8839P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max      .002
_refine_ls_shift/su_mean      .000
_refine_diff_density_max      .448
_refine_diff_density_min      -.616
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef      .0031(6)
_refine_ls_extinction_expression
                                  'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'C' 'C'  .0033  .0016
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'H' 'H'  .0000  .0000
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Cl' 'Cl'  .1484  .1585
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'N' 'N'  .0061  .0033
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Ni' 'Ni'  .3393 1.1124
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'O' 'O'  .0106  .0060
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'Kappa-CCD server software (Nonius, 1997)'
_computing_cell_refinement     'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction     'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)'
_computing_structure_refinement     'SHELXL-97 (Sheldrick, 1997b)'
_computing_molecular_graphics     'PLATON (Spek, 2001)'
_computing_publication_material
                    'SHELXL-97 (Sheldrick, 1997b) and PRPKAPPA (Ferguson, 1999)'
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Ni1  .5000  .5000  .5000  .02030(10) Uani d S 1 . . Ni
    O1  .38485(14)  .60422(9)  .51792(10)  .0259(3) Uani d D 1 . . O
    N1  .39309(15)  .43568(10)  .58281(11)  .0236(3) Uani d . 1 . . N
    N4  .37720(15)  .46280(10)  .39646(11)  .0237(3) Uani d . 1 . . N
    C2  .27679(19)  .41805(12)  .52933(14)  .0272(4) Uani d . 1 . . C
    C3  .30689(19)  .39725(12)  .43400(14)  .0274(4) Uani d . 1 . . C
    C5  .4313(2)  .44231(13)  .31113(14)  .0302(5) Uani d . 1 . . C
    C6  .5073(2)  .50998(14)  .27584(14)  .0330(5) Uani d . 1 . . C
    C7  .6280(2)  .52759(14)  .32990(14)  .0302(5) Uani d . 1 . . C
    Ni2  .05830(2)  .726187(13)  .219586(15)  .01786(9) Uani d . 1 . . Ni
    N21  .24350(16)  .74376(10)  .25471(11)  .0243(3) Uani d . 1 . . N
    N24  .11892(16)  .65442(9)  .11953(10)  .0229(3) Uani d . 1 . . N
    N28  -.12864(16)  .70977(10)  .18166(11)  .0232(3) Uani d . 1 . . N
    N211  -.00371(16)  .79631(9)  .32214(10)  .0229(3) Uani d . 1 . . N
    C22  .3101(2)  .71693(13)  .17691(15)  .0309(5) Uani d . 1 . . C
    C23  .2520(2)  .64054(13)  .14163(14)  .0293(4) Uani d . 1 . . C
    C25  .0468(2)  .58163(12)  .10260(14)  .0290(4) Uani d . 1 . . C
    C26  -.0892(2)  .59926(13)  .07795(14)  .0312(5) Uani d . 1 . . C
    C27  -.1634(2)  .62875(13)  .15456(14)  .0286(4) Uani d . 1 . . C
    C29  -.1968(2)  .73968(14)  .25759(14)  .0302(4) Uani d . 1 . . C
    C210  -.1339(2)  .81369(12)  .29573(14)  .0286(4) Uani d . 1 . . C
    C212  .0701(2)  .86785(12)  .34468(13)  .0295(5) Uani d . 1 . . C
    C213  .2064(2)  .84962(13)  .36452(14)  .0332(5) Uani d . 1 . . C
    C214  .2767(2)  .82481(13)  .28417(14)  .0307(5) Uani d . 1 . . C
    O31  .22188(12)  .61039(8)  .37722(9)  .0241(3) Uani d . 1 . . O
    O32  .03561(12)  .63084(8)  .30767(8)  .0203(3) Uani d . 1 . . O
    O33  .05499(14)  .67231(8)  .64061(8)  .0238(3) Uani d . 1 . . O
    O34  .06560(15)  .71343(8)  .49881(9)  .0294(3) Uani d . 1 . . O
    C31  .04684(16)  .55333(10)  .43868(11)  .0159(3) Uani d . 1 . . C
    C32  .03135(16)  .57742(10)  .52690(11)  .0163(3) Uani d . 1 . . C
    C33  .01418(16)  .47667(10)  .41329(11)  .0170(3) Uani d . 1 . . C
    C37  .10573(17)  .60403(10)  .37045(11)  .0175(3) Uani d . 1 . . C
    C38  .05380(17)  .66177(10)  .55700(11)  .0180(4) Uani d . 1 . . C
    O2  .6171(6) 1.0018(3)  .5361(5)  .080(3) Uani d P  .430(9) . . O
    Cl1  .56740(10)  .78843(7)  .45060(7)  .0347(2) Uani d P  .914(4) A 1 Cl
    O3  .4901(2)  .76585(13)  .52103(15)  .0531(7) Uani d P  .914(4) A 1 O
    O4  .5410(2)  .73697(12)  .37519(14)  .0498(6) Uani d P  .914(4) A 1 O
    O5  .5434(3)  .86856(12)  .42446(17)  .0570(7) Uani d P  .914(4) A 1 O
    O6  .6948(3)  .7793(2)  .4816(3)  .0500(7) Uani d P  .914(4) A 1 O
    Cl21  .5838(12)  .8020(8)  .4670(9)  .0347(2) Uani d PD  .086(4) A 2 Cl
    O23  .540(2)  .8302(13)  .5482(13)  .052(5) Uiso d PD  .086(4) A 2 O
    O24  .502(2)  .7348(12)  .4352(15)  .052(5) Uiso d PD  .086(4) A 2 O
    O25  .569(3)  .8595(15)  .3952(15)  .052(5) Uiso d PD  .086(4) A 2 O
    O26  .708(3)  .773(2)  .477(3)  .052(5) Uiso d PD  .086(4) A 2 O
    H1A  .415(3)  .6503(16)  .5209(19)  .050(6) Uiso d D 1 . . H
    H1B  .328(3)  .6076(18)  .4750(18)  .050(6) Uiso d D 1 . . H
    H11  .4333  .3879  .5944  .028 Uiso calc R 1 . . H
    H4  .3217  .5039  .3844  .028 Uiso calc R 1 . . H
    H2A  .2214  .4646  .5286  .033 Uiso calc R 1 . . H
    H2B  .2338  .3733  .5564  .033 Uiso calc R 1 . . H
    H3A  .3565  .3482  .4342  .033 Uiso calc R 1 . . H
    H3B  .2294  .3883  .3967  .033 Uiso calc R 1 . . H
    H5A  .3640  .4287  .2659  .036 Uiso calc R 1 . . H
    H5B  .4849  .3953  .3204  .036 Uiso calc R 1 . . H
    H6A  .5265  .4976  .2136  .040 Uiso calc R 1 . . H
    H6B  .4558  .5583  .2739  .040 Uiso calc R 1 . . H
    H7A  .6748  .4778  .3401  .036 Uiso calc R 1 . . H
    H7B  .6789  .5635  .2951  .036 Uiso calc R 1 . . H
    H21  .2651  .7100  .3021  .029 Uiso calc R 1 . . H
    H24  .1127  .6837  .0668  .027 Uiso calc R 1 . . H
    H28  -.1479  .7425  .1329  .028 Uiso calc R 1 . . H
    H211  -.0026  .7652  .3734  .027 Uiso calc R 1 . . H
    H22A  .3985  .7082  .1951  .037 Uiso calc R 1 . . H
    H22B  .3046  .7577  .1294  .037 Uiso calc R 1 . . H
    H23A  .2926  .6232  .0875  .035 Uiso calc R 1 . . H
    H23B  .2629  .5986  .1875  .035 Uiso calc R 1 . . H
    H25A  .0534  .5480  .1569  .035 Uiso calc R 1 . . H
    H25B  .0819  .5519  .0532  .035 Uiso calc R 1 . . H
    H26A  -.0940  .6394  .0298  .037 Uiso calc R 1 . . H
    H26B  -.1289  .5506  .0533  .037 Uiso calc R 1 . . H
    H27A  -.2527  .6273  .1357  .034 Uiso calc R 1 . . H
    H27B  -.1494  .5930  .2066  .034 Uiso calc R 1 . . H
    H29A  -.1983  .6987  .3047  .036 Uiso calc R 1 . . H
    H29B  -.2833  .7519  .2368  .036 Uiso calc R 1 . . H
    H10A  -.1386  .8561  .2502  .034 Uiso calc R 1 . . H
    H10B  -.1766  .8321  .3484  .034 Uiso calc R 1 . . H
    H12A  .0372  .8936  .3976  .035 Uiso calc R 1 . . H
    H12B  .0611  .9054  .2940  .035 Uiso calc R 1 . . H
    H13A  .2136  .8069  .4097  .040 Uiso calc R 1 . . H
    H13B  .2469  .8970  .3916  .040 Uiso calc R 1 . . H
    H14A  .2578  .8620  .2341  .037 Uiso calc R 1 . . H
    H14B  .3668  .8274  .3002  .037 Uiso calc R 1 . . H
    H33  .0233  .4607  .3532  .020 Uiso calc R 1 . . H
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Ni1 N1 3_666 2.060(2) no
    Ni1 N1 . 2.060(2) no
    Ni1 N4 . 2.075(2) no
    Ni1 N4 3_666 2.075(2) no
    Ni1 O1 3_666 2.188(2) no
    Ni1 O1 . 2.188(2) no
    O1 H1A .  .85(3) no
    O1 H1B .  .86(3) no
    N1 C7 3_666 1.477(3) no
    N1 C2 . 1.479(3) no
    N1 H11 .  .93 no
    N4 C3 . 1.477(3) no
    N4 C5 . 1.479(3) no
    N4 H4 .  .93 no
    C2 C3 . 1.524(3) no
    C2 H2A .  .99 no
    C2 H2B .  .99 no
    C3 H3A .  .99 no
    C3 H3B .  .99 no
    C5 C6 . 1.525(3) no
    C5 H5A .  .99 no
    C5 H5B .  .99 no
    C6 C7 . 1.523(3) no
    C6 H6A .  .99 no
    C6 H6B .  .99 no
    C7 N1 3_666 1.477(3) no
    C7 H7A .  .99 no
    C7 H7B .  .99 no
    Ni2 N21 . 2.063(2) no
    Ni2 N24 . 2.067(2) no
    Ni2 N211 . 2.085(2) no
    Ni2 O33 4_575 2.085(2) no
    Ni2 N28 . 2.086(2) no
    Ni2 O32 . 2.109(2) no
    N21 C22 . 1.479(3) no
    N21 C214 . 1.480(3) no
    N21 H21 .  .93 no
    N24 C25 . 1.473(3) no
    N24 C23 . 1.477(3) no
    N24 H24 .  .93 no
    N28 C27 . 1.474(3) no
    N28 C29 . 1.482(3) no
    N28 H28 .  .93 no
    N211 C210 . 1.469(3) no
    N211 C212 . 1.479(3) no
    N211 H211 .  .93 no
    C22 C23 . 1.519(3) no
    C22 H22A .  .99 no
    C22 H22B .  .99 no
    C23 H23A .  .99 no
    C23 H23B .  .99 no
    C25 C26 . 1.525(3) no
    C25 H25A .  .99 no
    C25 H25B .  .99 no
    C26 C27 . 1.525(3) no
    C26 H26A .  .99 no
    C26 H26B .  .99 no
    C27 H27A .  .99 no
    C27 H27B .  .99 no
    C29 C210 . 1.521(3) no
    C29 H29A .  .99 no
    C29 H29B .  .99 no
    C210 H10A .  .99 no
    C210 H10B .  .99 no
    C212 C213 . 1.519(3) no
    C212 H12A .  .99 no
    C212 H12B .  .99 no
    C213 C214 . 1.523(3) no
    C213 H13A .  .99 no
    C213 H13B .  .99 no
    C214 H14A .  .99 no
    C214 H14B .  .99 no
    O31 C37 . 1.260(2) no
    O32 C37 . 1.255(2) no
    O33 C38 . 1.263(2) no
    O33 Ni2 4_576 2.086(2) no
    O34 C38 . 1.247(2) no
    C31 C33 . 1.393(2) no
    C31 C32 . 1.401(2) no
    C31 C37 . 1.506(2) no
    C32 C33 3_566 1.393(2) no
    C32 C38 . 1.513(2) no
    C33 C32 3_566 1.393(2) no
    C33 H33 .  .95 no
    Cl1 O5 . 1.432(2) no
    Cl1 O6 . 1.436(3) no
    Cl1 O3 . 1.438(2) no
    Cl1 O4 . 1.440(2) no
    Cl21 O23 . 1.42(2) no
    Cl21 O26 . 1.43(2) no
    Cl21 O25 . 1.45(2) no
    Cl21 O24 . 1.50(2) no
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    N1 Ni1 N1 3_666 . 180 no
    N1 Ni1 N4 3_666 . 94.00(6) no
    N1 Ni1 N4 . . 86.00(6) no
    N1 Ni1 N4 3_666 3_666 85.99(6) no
    N1 Ni1 N4 . 3_666 94.01(6) no
    N4 Ni1 N4 . 3_666 180 no
    N1 Ni1 O1 3_666 3_666 90.39(6) no
    N1 Ni1 O1 . 3_666 89.60(6) no
    N4 Ni1 O1 . 3_666 90.39(6) no
    N4 Ni1 O1 3_666 3_666 89.61(6) no
    N1 Ni1 O1 3_666 . 89.61(6) no
    N1 Ni1 O1 . . 90.40(6) no
    N4 Ni1 O1 . . 89.61(6) no
    N4 Ni1 O1 3_666 . 90.39(6) no
    O1 Ni1 O1 3_666 . 180 no
    Ni1 O1 H1A . . 122(2) no
    Ni1 O1 H1B . . 110(2) no
    H1A O1 H1B . . 103(3) no
    C7 N1 C2 3_666 . 112.9(2) no
    C7 N1 Ni1 3_666 . 115.7(2) no
    C2 N1 Ni1 . . 105.9(2) no
    C7 N1 H11 3_666 . 107.3 no
    C2 N1 H11 . . 107.3 no
    Ni1 N1 H11 . . 107.3 no
    C3 N4 C5 . . 113.2(2) no
    C3 N4 Ni1 . . 105.4(2) no
    C5 N4 Ni1 . . 116.4(2) no
    C3 N4 H4 . . 107.1 no
    C5 N4 H4 . . 107.1 no
    Ni1 N4 H4 . . 107.1 no
    N1 C2 C3 . . 109.12(16) no
    N1 C2 H2A . . 109.9 no
    C3 C2 H2A . . 109.9 no
    N1 C2 H2B . . 109.9 no
    C3 C2 H2B . . 109.9 no
    H2A C2 H2B . . 108.3 no
    N4 C3 C2 . . 109.1(2) no
    N4 C3 H3A . . 109.9 no
    C2 C3 H3A . . 109.9 no
    N4 C3 H3B . . 109.9 no
    C2 C3 H3B . . 109.9 no
    H3A C3 H3B . . 108.3 no
    N4 C5 C6 . . 112.0(2) no
    N4 C5 H5A . . 109.2 no
    C6 C5 H5A . . 109.2 no
    N4 C5 H5B . . 109.2 no
    C6 C5 H5B . . 109.2 no
    H5A C5 H5B . . 107.9 no
    C7 C6 C5 . . 115.3(2) no
    C7 C6 H6A . . 108.4 no
    C5 C6 H6A . . 108.4 no
    C7 C6 H6B . . 108.4 no
    C5 C6 H6B . . 108.4 no
    H6A C6 H6B . . 107.5 no
    N1 C7 C6 3_666 . 112.1(2) no
    N1 C7 H7A 3_666 . 109.2 no
    C6 C7 H7A . . 109.2 no
    N1 C7 H7B 3_666 . 109.2 no
    C6 C7 H7B . . 109.2 no
    H7A C7 H7B . . 107.9 no
    N21 Ni2 N24 . . 85.48(7) no
    N21 Ni2 N211 . . 94.80(7) no
    N24 Ni2 N211 . . 178.71(6) no
    N21 Ni2 O33 . 4_575 90.39(6) no
    N24 Ni2 O33 . 4_575 93.99(6) no
    N211 Ni2 O33 . 4_575 87.26(6) no
    N21 Ni2 N28 . . 178.82(6) no
    N24 Ni2 N28 . . 94.12(7) no
    N211 Ni2 N28 . . 85.63(7) no
    O33 Ni2 N28 4_575 . 88.53(6) no
    N21 Ni2 O32 . . 95.81(6) no
    N24 Ni2 O32 . . 93.26(6) no
    N211 Ni2 O32 . . 85.47(6) no
    O33 Ni2 O32 4_575 . 170.81(5) no
    N28 Ni2 O32 . . 85.32(6) no
    C22 N21 C214 . . 113.5(2) no
    C22 N21 Ni2 . . 105.7(2) no
    C214 N21 Ni2 . . 115.1(2) no
    C22 N21 H21 . . 107.4 no
    C214 N21 H21 . . 107.4 no
    Ni2 N21 H21 . . 107.4 no
    C25 N24 C23 . . 113.9(2) no
    C25 N24 Ni2 . . 115.3(2) no
    C23 N24 Ni2 . . 106.4(2) no
    C25 N24 H24 . . 106.9 no
    C23 N24 H24 . . 106.9 no
    Ni2 N24 H24 . . 106.9 no
    C27 N28 C29 . . 113.5(2) no
    C27 N28 Ni2 . . 115.2(2) no
    C29 N28 Ni2 . . 105.5(2) no
    C27 N28 H28 . . 107.4 no
    C29 N28 H28 . . 107.4 no
    Ni2 N28 H28 . . 107.4 no
    C210 N211 C212 . . 113.1(2) no
    C210 N211 Ni2 . . 105.3(2) no
    C212 N211 Ni2 . . 116.1(2) no
    C210 N211 H211 . . 107.3 no
    C212 N211 H211 . . 107.3 no
    Ni2 N211 H211 . . 107.3 no
    N21 C22 C23 . . 108.9(2) no
    N21 C22 H22A . . 109.9 no
    C23 C22 H22A . . 109.9 no
    N21 C22 H22B . . 109.9 no
    C23 C22 H22B . . 109.9 no
    H22A C22 H22B . . 108.3 no
    N24 C23 C22 . . 108.6(2) no
    N24 C23 H23A . . 110.0 no
    C22 C23 H23A . . 110.0 no
    N24 C23 H23B . . 110.0 no
    C22 C23 H23B . . 110.0 no
    H23A C23 H23B . . 108.4 no
    N24 C25 C26 . . 111.8(2) no
    N24 C25 H25A . . 109.3 no
    C26 C25 H25A . . 109.3 no
    N24 C25 H25B . . 109.3 no
    C26 C25 H25B . . 109.3 no
    H25A C25 H25B . . 107.9 no
    C27 C26 C25 . . 115.4(2) no
    C27 C26 H26A . . 108.4 no
    C25 C26 H26A . . 108.4 no
    C27 C26 H26B . . 108.4 no
    C25 C26 H26B . . 108.4 no
    H26A C26 H26B . . 107.5 no
    N28 C27 C26 . . 112.0(2) no
    N28 C27 H27A . . 109.2 no
    C26 C27 H27A . . 109.2 no
    N28 C27 H27B . . 109.2 no
    C26 C27 H27B . . 109.2 no
    H27A C27 H27B . . 107.9 no
    N28 C29 C210 . . 109.7(2) no
    N28 C29 H29A . . 109.7 no
    C210 C29 H29A . . 109.7 no
    N28 C29 H29B . . 109.7 no
    C210 C29 H29B . . 109.7 no
    H29A C29 H29B . . 108.2 no
    N211 C210 C29 . . 109.6(2) no
    N211 C210 H10A . . 109.8 no
    C29 C210 H10A . . 109.8 no
    N211 C210 H10B . . 109.8 no
    C29 C210 H10B . . 109.8 no
    H10A C210 H10B . . 108.2 no
    N211 C212 C213 . . 112.5(2) no
    N211 C212 H12A . . 109.1 no
    C213 C212 H12A . . 109.1 no
    N211 C212 H12B . . 109.1 no
    C213 C212 H12B . . 109.1 no
    H12A C212 H12B . . 107.8 no
    C212 C213 C214 . . 115.5(2) no
    C212 C213 H13A . . 108.4 no
    C214 C213 H13A . . 108.4 no
    C212 C213 H13B . . 108.4 no
    C214 C213 H13B . . 108.4 no
    H13A C213 H13B . . 107.5 no
    N21 C214 C213 . . 111.5(2) no
    N21 C214 H14A . . 109.3 no
    C213 C214 H14A . . 109.3 no
    N21 C214 H14B . . 109.3 no
    C213 C214 H14B . . 109.3 no
    H14A C214 H14B . . 108.0 no
    C37 O32 Ni2 . . 131.0(2) no
    C38 O33 Ni2 . 4_576 132.6(2) no
    C33 C31 C32 . . 119.0(2) no
    C33 C31 C37 . . 117.3(2) no
    C32 C31 C37 . . 123.6(2) no
    C33 C32 C31 3_566 . 118.8(2) no
    C33 C32 C38 3_566 . 119.1(2) no
    C31 C32 C38 . . 121.9(2) no
    C31 C33 C32 . 3_566 122.2(2) no
    C31 C33 H33 . . 118.9 no
    C32 C33 H33 3_566 . 118.9 no
    O32 C37 O31 . . 125.7(2) no
    O32 C37 C31 . . 116.8(2) no
    O31 C37 C31 . . 117.2(2) no
    O34 C38 O33 . . 126.7(2) no
    O34 C38 C32 . . 118.5(2) no
    O33 C38 C32 . . 114.8(2) no
    O5 Cl1 O6 . . 110.1(2) no
    O5 Cl1 O3 . . 110.4(2) no
    O6 Cl1 O3 . . 109.1(2) no
    O5 Cl1 O4 . . 109.7(2) no
    O6 Cl1 O4 . . 109.1(2) no
    O3 Cl1 O4 . . 108.5(2) no
    O23 Cl21 O26 . . 113(2) no
    O23 Cl21 O25 . . 113(2) no
    O26 Cl21 O25 . . 111(2) no
    O23 Cl21 O24 . . 108(2) no
    O26 Cl21 O24 . . 108(2) no
    O25 Cl21 O24 . . 104(2) no
loop_
    _geom_torsion_atom_site_label_1
    _geom_torsion_atom_site_label_2
    _geom_torsion_atom_site_label_3
    _geom_torsion_atom_site_label_4
    _geom_torsion_site_symmetry_1
    _geom_torsion_site_symmetry_2
    _geom_torsion_site_symmetry_3
    _geom_torsion_site_symmetry_4
    _geom_torsion
    _geom_torsion_publ_flag
    N4 Ni1 N1 C7 . . . 3_666 -140.2(2) no
    N4 Ni1 N1 C7 3_666 . . 3_666 39.9(2) no
    O1 Ni1 N1 C7 3_666 . . 3_666 129.4(2) no
    O1 Ni1 N1 C7 . . . 3_666 -50.6(2) no
    N4 Ni1 N1 C2 . . . . -14.3(2) no
    N4 Ni1 N1 C2 3_666 . . . 165.7(2) no
    O1 Ni1 N1 C2 3_666 . . . -104.8(2) no
    O1 Ni1 N1 C2 . . . . 75.2(2) no
    N1 Ni1 N4 C3 3_666 . . . 165.4(2) no
    N1 Ni1 N4 C3 . . . . -14.6(2) no
    O1 Ni1 N4 C3 3_666 . . . 74.9(2) no
    O1 Ni1 N4 C3 . . . . -105.1(2) no
    N1 Ni1 N4 C5 3_666 . . . 39.0(2) no
    N1 Ni1 N4 C5 . . . . -141.0(2) no
    O1 Ni1 N4 C5 3_666 . . . -51.4(2) no
    O1 Ni1 N4 C5 . . . . 128.6(2) no
    C7 N1 C2 C3 3_666 . . . 1678.0(2) no
    Ni1 N1 C2 C3 . . . . 40.5(2) no
    C5 N4 C3 C2 . . . . 169.0(2) no
    Ni1 N4 C3 C2 . . . . 40.6420 no
    N1 C2 C3 N4 . . . . -56.3(2) no
    C3 N4 C5 C6 . . . . -177.89(2) no
    Ni1 N4 C5 C6 . . . . -55.4(2) no
    N4 C5 C6 C7 . . . . 69.7(2) no
    C5 C6 C7 N1 . . . 3_666 -71.4(2) no
    N24 Ni2 N21 C22 . . . . 16.1(2) no
    N211 Ni2 N21 C22 . . . . -165.1(2) no
    O33 Ni2 N21 C22 4_575 . . . -77.9(2) no
    O32 Ni2 N21 C22 . . . . 108.9(2) no
    N24 Ni2 N21 C214 . . . . 142.1(2) no
    N211 Ni2 N21 C214 . . . . -39.2(2) no
    O33 Ni2 N21 C214 4_575 . . . 48.1(2) no
    O32 Ni2 N21 C214 . . . . -125.1(2) no
    N21 Ni2 N24 C25 . . . . 140.5(2) no
    O33 Ni2 N24 C25 4_575 . . . -129.5(2) no
    N28 Ni2 N24 C25 . . . . -40.7(2) no
    O32 Ni2 N24 C25 . . . . 44.9(2) no
    N21 Ni2 N24 C23 . . . . 13.2(2) no
    O33 Ni2 N24 C23 4_575 . . . 103.3(2) no
    N28 Ni2 N24 C23 . . . . -167.9(2) no
    O32 Ni2 N24 C23 . . . . -82.4(2) no
    N24 Ni2 N28 C27 . . . . 40.1(2) no
    N211 Ni2 N28 C27 . . . . -138.6(2) no
    O33 Ni2 N28 C27 4_575 . . . 134.0(2) no
    O32 Ni2 N28 C27 . . . . -52.8(2) no
    N24 Ni2 N28 C29 . . . . 166.1(2) no
    N211 Ni2 N28 C29 . . . . -12.7(2) no
    O33 Ni2 N28 C29 4_575 . . . -100.0(2) no
    O32 Ni2 N28 C29 . . . . 73.2(2) no
    N21 Ni2 N211 C210 . . . . 162.9(2) no
    O33 Ni2 N211 C210 4_575 . . . 72.7(2) no
    N28 Ni2 N211 C210 . . . . -16.1(2) no
    O32 Ni2 N211 C210 . . . . -101.7(2) no
    N21 Ni2 N211 C212 . . . . 36.9(2) no
    O33 Ni2 N211 C212 4_575 . . . -53.3(2) no
    N28 Ni2 N211 C212 . . . . -142.0(2) no
    O32 Ni2 N211 C212 . . . . 132.3(2) no
    C214 N21 C22 C23 . . . . -169.4(2) no
    Ni2 N21 C22 C23 . . . . -42.4(2) no
    C25 N24 C23 C22 . . . . -167.9(2) no
    Ni2 N24 C23 C22 . . . . -39.8(2) no
    N21 C22 C23 N24 . . . . 56.6(2) no
    C23 N24 C25 C26 . . . . -178.6(2) no
    Ni2 N24 C25 C26 . . . . 58.0(2) no
    N24 C25 C26 C27 . . . . -71.7(2) no
    C29 N28 C27 C26 . . . . -178.6(2) no
    Ni2 N28 C27 C26 . . . . -56.8(2) no
    C25 C26 C27 N28 . . . . 71.1(2) no
    C27 N28 C29 C210 . . . . 166.0(2) no
    Ni2 N28 C29 C210 . . . . 38.9(2) no
    C212 N211 C210 C29 . . . . 169.7(2) no
    Ni2 N211 C210 C29 . . . . 41.8(2) no
    N28 C29 C210 N211 . . . . -56.4(2) no
    C210 N211 C212 C213 . . . . -175.4(2) no
    Ni2 N211 C212 C213 . . . . -53.4(2) no
    N211 C212 C213 C214 . . . . 70.3(2) no
    C22 N21 C214 C213 . . . . -179.8(2) no
    Ni2 N21 C214 C213 . . . . 58.4(2) no
    C212 C213 C214 N21 . . . . -73.2(2) no
    N21 Ni2 O32 C37 . . . . 10.84(16) no
    N24 Ni2 O32 C37 . . . . 96.62(16) no
    N211 Ni2 O32 C37 . . . . -83.5(2) no
    N28 Ni2 O32 C37 . . . . -169.5(2) no
    C33 C31 C32 C33 . . . 3_566 1.1(3) no
    C37 C31 C32 C33 . . . 3_566 -174.3(2) no
    C33 C31 C32 C38 . . . . -174.4(2) no
    C37 C31 C32 C38 . . . . 10.2(3) no
    C32 C31 C33 C32 . . . 3_566 -1.2(3) no
    C37 C31 C33 C32 . . . 3_566 174.6(2) no
    Ni2 O32 C37 O31 . . . . -25.6(3) no
    Ni2 O32 C37 C31 . . . . 160.6(2) no
    C33 C31 C37 O32 . . . . 75.1(2) no
    C32 C31 C37 O32 . . . . -109.4(2) no
    C33 C31 C37 O31 . . . . -99.3(2) no
    C32 C31 C37 O31 . . . . 76.3(2) no
    Ni2 O33 C38 O34 4_576 . . . 7.0(3) no
    Ni2 O33 C38 C32 4_576 . . . -170.9(2) no
    C33 C32 C38 O34 3_566 . . . -163.1(2) no
    C31 C32 C38 O34 . . . . 12.4(3) no
    C33 C32 C38 O33 3_566 . . . 15.0(2) no
    C31 C32 C38 O33 . . . . -169.6(2) no
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    _geom_hbond_publ_flag
    O1 H1A O3 .  .85(3) 2.12(3) 2.965(3) 177(3) y
    O1 H1A O24 .  .85(3) 2.17(4) 2.87(2) 139(3) y
    O1 H1B O31 .  .86(3) 1.80(3) 2.662(2) 173(3) y
    N1 H11 O4 3_666  .93 2.18 3.066(3) 159 y
    N1 H11 O24 3_666  .93 2.25 3.12(2) 156 y
    N4 H4 O31 .  .93 2.10 3.017(2) 167 y
    N21 H21 O31 .  .93 2.10 2.928(2) 148 y
    N24 H24 O34 4_575  .93 2.07 2.911(2) 150 y
    N211 H211 O34 .  .93 2.16 3.045(2) 159 y
