##############################################################################
###                                                                        ###
###        Electronic paper (Acta Crystallographica Section E)             ###
###                                                                        ###
##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section E. It conforms to the requirements of Notes      #
# for Authors for Section E, and 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 is obtainable 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_I
_audit_creation_method     SHELXL-97
_chemical_name_systematic
;
;
_chemical_name_common     ?
_chemical_formula_moiety     'C12 H16 N14 Ni'
_chemical_formula_sum     'C12 H16 N14 Ni'
_chemical_formula_iupac     '[Ni (N3)2 (C3 H4 N2)4]'
_chemical_formula_weight     415.10
_chemical_melting_point     ?
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'P 21/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     8.7870(10)
_cell_length_b     10.4640(10)
_cell_length_c     10.8660(10)
_cell_angle_alpha     90.00
_cell_angle_beta     110.670(10)
_cell_angle_gamma     90.00
_cell_volume     934.79(17)
_cell_formula_units_Z     2
_cell_measurement_reflns_used     2860
_cell_measurement_theta_min     1.95
_cell_measurement_theta_max     25.03
_cell_measurement_temperature     293(2)
_exptl_crystal_description     prism
_exptl_crystal_colour     blue
_exptl_crystal_size_max     0.32
_exptl_crystal_size_mid     0.23
_exptl_crystal_size_min     0.16
_exptl_crystal_density_diffrn     1.475
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     428
_exptl_absorpt_coefficient_mu     1.068
_exptl_absorpt_correction_type     empirical
_exptl_absorpt_process_details     '(SADABS; Sheldrick, 1996)'
_exptl_absorpt_correction_T_min     0.706
_exptl_absorpt_correction_T_max     0.843
_exptl_special_details
;
 ?
;
_diffrn_ambient_temperature     293(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Siemens SMART CCD'
_diffrn_measurement_method     'φ and ω'
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     2860
_diffrn_reflns_av_R_equivalents     0.0215
_diffrn_reflns_av_sigmaI/netI     0.0285
_diffrn_reflns_theta_min     2.58
_diffrn_reflns_theta_max     25.03
_diffrn_reflns_theta_full     25.03
_diffrn_measured_fraction_theta_max     0.985
_diffrn_measured_fraction_theta_full     0.985
_diffrn_reflns_limit_h_min     -10
_diffrn_reflns_limit_h_max     8
_diffrn_reflns_limit_k_min     -12
_diffrn_reflns_limit_k_max     8
_diffrn_reflns_limit_l_min     -6
_diffrn_reflns_limit_l_max     12
_diffrn_standards_number     none
_diffrn_standards_interval_count     none
_diffrn_standards_interval_time     none
_diffrn_standards_decay_%     none
_refine_special_details
;
All H atoms were generated geometrically and were constrained to ride
 on the parent atoms.  The highest residual peak
(0.25 eÅ⁻³) locates at the position (0.0223, 0.4787, 0.4044), which is
1.15 Å from Ni1; the deepest hole (-0.23 eÅ⁻³) locates at the position
(0.0692, 0.4738, 0.5642), which is 0.79 Å from Ni1.
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_reflns_number_total     1630
_reflns_number_gt     1340
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0430
_refine_ls_R_factor_gt     0.0321
_refine_ls_wR_factor_gt     0.0828
_refine_ls_wR_factor_ref     0.0917
_refine_ls_goodness_of_fit_ref     1.063
_refine_ls_restrained_S_all     1.063
_refine_ls_number_reflns     1630
_refine_ls_number_parameters     125
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
      'calc w = 1/[σ²(Fo²)+(0.0464P)²+0.368P] 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     <0.001
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.254
_refine_diff_density_min     -0.227
_refine_ls_extinction_method     SHELXL97
_refine_ls_extinction_coef     0.010(2)
_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' 0.0033 0.0016
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'H' 'H' 0.0000 0.0000
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'N' 'N' 0.0061 0.0033
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Ni' 'Ni' 0.3393 1.1124
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'SMART (Siemens, 1996)'
_computing_cell_refinement     'SMART and SAINT (Siemens, 1994)'
_computing_data_reduction     'SMART and SAINT'
_computing_structure_solution     'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics     'SHELXTL (Siemens, 1994)'
_computing_publication_material     'SHELXL97'
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 0.0000 0.5000 0.5000 0.03846(19) Uani d S 1 . . Ni
    N7 0.0973(2) 0.31533(18) 0.51691(19) 0.0448(5) Uani d . 1 . . N
    N6 0.2147(3) 0.1367(2) 0.6062(2) 0.0591(6) Uani d . 1 . . N
    H6B 0.2621 0.0805 0.6651 0.071 Uiso calc R 1 . . H
    N5 0.2344(2) 0.5822(2) 0.5441(2) 0.0488(5) Uani d . 1 . . N
    N4 0.4970(3) 0.6155(3) 0.6224(3) 0.0731(8) Uani d . 1 . . N
    H4B 0.5988 0.6037 0.6657 0.088 Uiso calc R 1 . . H
    N3 0.0360(3) 0.49130(19) 0.70434(19) 0.0465(5) Uani d . 1 . . N
    C6 0.1673(3) 0.2523(3) 0.6276(3) 0.0540(6) Uani d . 1 . . C
    H6A 0.1816 0.2848 0.7106 0.065 Uiso calc R 1 . . H
    C5 0.1021(4) 0.2337(3) 0.4205(3) 0.0572(7) Uani d . 1 . . C
    H5A 0.0612 0.2514 0.3309 0.069 Uiso calc R 1 . . H
    N2 -0.0726(3) 0.5088(2) 0.7427(2) 0.0524(6) Uani d . 1 . . N
    C4 0.3752(3) 0.5362(3) 0.6187(3) 0.0589(7) Uani d . 1 . . C
    H4A 0.3891 0.4588 0.6634 0.071 Uiso calc R 1 . . H
    C3 0.2697(4) 0.6958(3) 0.4980(3) 0.0689(8) Uani d . 1 . . C
    H3A 0.1933 0.7506 0.4416 0.083 Uiso calc R 1 . . H
    C2 0.1747(4) 0.1233(3) 0.4743(3) 0.0641(8) Uani d . 1 . . C
    H2A 0.1936 0.0525 0.4300 0.077 Uiso calc R 1 . . H
    C1 0.4309(4) 0.7167(4) 0.5461(4) 0.0789(10) Uani d . 1 . . C
    H1A 0.4858 0.7870 0.5299 0.095 Uiso calc R 1 . . H
    N1 -0.1763(4) 0.5287(3) 0.7830(3) 0.0893(10) Uani d . 1 . . N
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    Ni1 0.0337(3) 0.0406(3) 0.0378(3) -0.00024(17) 0.00861(18) 0.00100(17)
    N7 0.0412(11) 0.0439(11) 0.0455(11) 0.0035(9) 0.0106(9) 0.0021(9)
    N6 0.0580(14) 0.0527(13) 0.0646(15) 0.0143(11) 0.0194(11) 0.0144(11)
    N5 0.0396(11) 0.0540(13) 0.0505(11) -0.0062(10) 0.0131(9) -0.0019(10)
    N4 0.0373(12) 0.104(2) 0.0753(17) -0.0122(14) 0.0171(11) -0.0165(16)
    N3 0.0432(12) 0.0543(13) 0.0399(11) -0.0003(9) 0.0121(9) -0.0003(9)
    C6 0.0570(16) 0.0510(15) 0.0502(15) 0.0072(13) 0.0141(12) 0.0019(12)
    C5 0.0648(17) 0.0554(16) 0.0507(14) 0.0056(14) 0.0196(13) 0.0004(13)
    N2 0.0493(13) 0.0621(14) 0.0424(11) -0.0024(11) 0.0119(10) 0.0095(10)
    C4 0.0435(15) 0.0750(18) 0.0558(16) -0.0006(14) 0.0146(13) -0.0024(14)
    C3 0.0563(18) 0.0672(19) 0.081(2) -0.0123(15) 0.0209(15) 0.0103(16)
    C2 0.075(2) 0.0515(16) 0.0716(19) 0.0115(15) 0.0336(16) -0.0034(14)
    C1 0.062(2) 0.085(2) 0.093(2) -0.0260(18) 0.0323(18) -0.0063(19)
    N1 0.0642(17) 0.143(3) 0.0732(18) 0.0100(17) 0.0396(15) 0.0230(17)
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 N7 3_566 2.095(2) no
    Ni1 N7 . 2.095(2) yes
    Ni1 N5 3_566 2.124(2) no
    Ni1 N5 . 2.124(2) yes
    Ni1 N3 3_566 2.131(2) no
    Ni1 N3 . 2.131(2) yes
    N7 C6 . 1.318(3) no
    N7 C5 . 1.364(3) no
    N6 C6 . 1.326(3) no
    N6 C2 . 1.357(3) no
    N6 H6B . 0.8600 no
    N5 C4 . 1.308(3) no
    N5 C3 . 1.368(3) no
    N4 C1 . 1.343(4) no
    N4 C4 . 1.344(4) no
    N4 H4B . 0.8600 no
    N3 N2 . 1.183(3) yes
    C6 H6A . 0.9300 no
    C5 C2 . 1.349(4) no
    C5 H5A . 0.9300 no
    N2 N1 . 1.160(3) yes
    C4 H4A . 0.9300 no
    C3 C1 . 1.343(4) no
    C3 H3A . 0.9300 no
    C2 H2A . 0.9300 no
    C1 H1A . 0.9300 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
    N7 Ni1 N7 3_566 . 180.0 no
    N7 Ni1 N5 3_566 3_566 91.20(10)
                                  no
    N7 Ni1 N5 . 3_566 88.80(10)
                              yes
    N7 Ni1 N5 3_566 . 88.80(10)
                              no
    N7 Ni1 N5 . . 91.20(10)
                          yes
    N5 Ni1 N5 3_566 . 180.0 no
    N7 Ni1 N3 3_566 3_566 87.90(10)
                                  no
    N7 Ni1 N3 . 3_566 92.10(10)
                              yes
    N5 Ni1 N3 3_566 3_566 90.40(10)
                                  no
    N5 Ni1 N3 . 3_566 89.60(10)
                              yes
    N7 Ni1 N3 3_566 . 92.10(10)
                              no
    N7 Ni1 N3 . . 87.90(10)
                          yes
    N5 Ni1 N3 3_566 . 89.60(10)
                              no
    N5 Ni1 N3 . . 90.40(10)
                          yes
    N3 Ni1 N3 3_566 . 180.0 no
    C6 N7 C5 . . 104.8(2) no
    C6 N7 Ni1 . . 125.89(17) no
    C5 N7 Ni1 . . 129.26(17) no
    C6 N6 C2 . . 107.4(2) no
    C6 N6 H6B . . 126.3 no
    C2 N6 H6B . . 126.3 no
    C4 N5 C3 . . 105.0(2) no
    C4 N5 Ni1 . . 128.35(19) no
    C3 N5 Ni1 . . 126.65(18) no
    C1 N4 C4 . . 107.6(3) no
    C1 N4 H4B . . 126.2 no
    C4 N4 H4B . . 126.2 no
    N2 N3 Ni1 . . 121.28(17) yes
    N7 C6 N6 . . 111.7(2) no
    N7 C6 H6A . . 124.1 no
    N6 C6 H6A . . 124.1 no
    C2 C5 N7 . . 110.0(2) no
    C2 C5 H5A . . 125.0 no
    N7 C5 H5A . . 125.0 no
    N1 N2 N3 . . 177.9(3) yes
    N5 C4 N4 . . 111.2(3) no
    N5 C4 H4A . . 124.4 no
    N4 C4 H4A . . 124.4 no
    C1 C3 N5 . . 110.1(3) no
    C1 C3 H3A . . 124.9 no
    N5 C3 H3A . . 124.9 no
    C5 C2 N6 . . 106.0(2) no
    C5 C2 H2A . . 127.0 no
    N6 C2 H2A . . 127.0 no
    N4 C1 C3 . . 106.2(3) no
    N4 C1 H1A . . 126.9 no
    C3 C1 H1A . . 126.9 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
    N6 H6B N3 2_546 0.86 2.06 2.858(3) 153
    N4 H4B N1 1_655 0.86 2.09 2.929(4) 165
data_global
_journal_date_recd_electronic     2002-09-10
_journal_date_accepted     2002-09-17
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2002
_journal_volume     58
_journal_issue     10
_journal_page_first     m566
_journal_page_last     m568
_journal_paper_category     EM
_publ_contact_author_name     'Can-Zhong Lu'
_publ_contact_author_address
;
The State Key Laboratory of Structural Chemistry
Fujian Institute of Research on the Structure of Matter
Chinese Academy of Sciences
Fuzhou
Fujian 350002
People's Republic of China
;
_publ_contact_author_email     czlu@ms.fjirsm.ac.cn
_publ_contact_author_fax     '86-591-3714946'
_publ_contact_author_phone     '86-591-3705794'
_publ_section_title
;
Diazidotetraimidazolenickel(II)
;
loop_
    _publ_author_name
    _publ_author_address
    'Quan-Zheng Zhang'
;
The State Key Laboratory of Structural Chemistry
Fujian Institute of Research on the Structure of Matter
Chinese Academy of Sciences
Fuzhou
Fujian 350002
People's Republic of China
;
    'Chuan-De Wu'
;
The State Key Laboratory of Structural Chemistry
Fujian Institute of Research on the Structure of Matter
Chinese Academy of Sciences
Fuzhou
Fujian 350002
People's Republic of China
;
    'Wen-Bin Yang'
;
The State Key Laboratory of Structural Chemistry
Fujian Institute of Research on the Structure of Matter
Chinese Academy of Sciences
Fuzhou
Fujian 350002
People's Republic of China
;
    'Ya-Qin Yu'
;
The State Key Laboratory of Structural Chemistry
Fujian Institute of Research on the Structure of Matter
Chinese Academy of Sciences
Fuzhou
Fujian 350002
People's Republic of China
;
    'Shu-Mei Chen'
;
The State Key Laboratory of Structural Chemistry
Fujian Institute of Research on the Structure of Matter
Chinese Academy of Sciences
Fuzhou
Fujian 350002
People's Republic of China
;
    'Xiao-Ping Zhan'
;
The State Key Laboratory of Structural Chemistry
Fujian Institute of Research on the Structure of Matter
Chinese Academy of Sciences
Fuzhou
Fujian 350002
People's Republic of China
;
    'Can-Zhong Lu'
;
The State Key Laboratory of Structural Chemistry
Fujian Institute of Research on the Structure of Matter
Chinese Academy of Sciences
Fuzhou
Fujian 350002
People's Republic of China
;
