##############################################################################
###                                                                        ###
###        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 2.4.    #
#                                                                            #
# 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                                                              #
#                                                                            #
# This file may be used for bona fide research purposes within the           #
# scientific community so long as proper attribution is given to the journal # 
# article from which it was obtained.                                        #
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##############################################################################
                                             
data_global
_audit_creation_method     'form.cif (version 2.0)'
_journal_data_validation_number     ?
_journal_date_recd_electronic     2010-07-24
_journal_date_accepted     2010-08-10
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2010
_journal_volume     66
_journal_issue      9
_journal_page_first     m1119
_journal_page_last     m1119
_journal_paper_category     QM
_journal_coeditor_code     WM2381
_publ_contact_author_name     'Prof. Dr. Zhang, Xiutang'
_publ_contact_author_address
;
      Advanced Material Institute of Research,
      Department of Chemistry and Chemical Engineering,
      Qilu Normal University,
      Jinan, 250013,
      P. R.China
      College of Chemistry and Chemical Engineering
      Liaocheng University
      Liaocheng, 252059
      People's Republic of China
;
_publ_contact_author_email     'xiutangzhang@yahoo.com.cn'
_publ_contact_author_fax     '0086-531-66778061'
_publ_contact_author_phone     '0086-531-66778061'
_publ_section_title
;
Tris(2,2'-bipyridine)nickel(II) hexamolybdate
;
loop_
    _publ_author_name
    _publ_author_address
    'Fan, Liming'
;     Advanced Material Institute of Research,
      Department of Chemistry and Chemical Engineering,
      Qilu Normal University,
      Jinan 250013,
      People's Republic of China
      and
      and College of Chemistry and Chemical Engineering
      Liaocheng University
      Liaocheng 252059
      People's Republic of China
;
    'Wei, Peihai'
;     Advanced Material Institute of Research,
      Department of Chemistry and Chemical Engineering,
      Qilu Normal University,
      Jinan 250013,
      People's Republic of China
;
    'Pang, Shuming'
;     Advanced Material Institute of Research,
      Department of Chemistry and Chemical Engineering,
      Qilu Normal University,
      Jinan 250013,
      People's Republic of China
;
    'Zhang, Xiutang'
;     Advanced Material Institute of Research,
      Department of Chemistry and Chemical Engineering,
      Qilu Normal University,
      Jinan 250013,
      People's Republic of China
      and
      and College of Chemistry and Chemical Engineering
      Liaocheng University
      Liaocheng 252059
      People's Republic of China
;
data_I
_audit_creation_method     SHELXL-97
_chemical_name_systematic
;
Tris(2,2'-bipyridine)nickel(II) hexamolybdate
;
_chemical_name_common     ?
_chemical_formula_moiety     'C30 H24 N6 Ni 2+, Mo6 O19 2-'
_chemical_formula_sum     'C30 H24 Mo6 N6 Ni O19'
_chemical_formula_iupac     '[Ni (C10 H8 N2)3] [Mo6 O19]'
_chemical_formula_weight     1406.90
_chemical_melting_point     ?
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'P 21/n'
_symmetry_space_group_name_Hall     '-P 2yn'
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     12.3549(7)
_cell_length_b     18.9866(10)
_cell_length_c     17.1974(9)
_cell_angle_alpha     90.00
_cell_angle_beta     101.1140(10)
_cell_angle_gamma     90.00
_cell_volume     3958.5(4)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     9988
_cell_measurement_theta_min     2.25
_cell_measurement_theta_max     26.72
_cell_measurement_temperature     296(2)
_exptl_crystal_description     block
_exptl_crystal_colour     green
_exptl_crystal_size_max     0.12
_exptl_crystal_size_mid     0.10
_exptl_crystal_size_min     0.08
_exptl_crystal_density_diffrn     2.361
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     2712
_exptl_absorpt_coefficient_mu     2.391
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details     '(SADABS; Bruker, 2001)'
_exptl_absorpt_correction_T_min     0.7623
_exptl_absorpt_correction_T_max     0.8317
_exptl_special_details
;
;
_diffrn_ambient_temperature     296(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     'Bruker APEXII CCD'
_diffrn_measurement_method     'phi and omega scans'
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     27627
_diffrn_reflns_av_R_equivalents     0.0265
_diffrn_reflns_av_sigmaI/netI     0.0225
_diffrn_reflns_theta_min     2.16
_diffrn_reflns_theta_max     25.00
_diffrn_reflns_theta_full     25.00
_diffrn_measured_fraction_theta_max     0.998
_diffrn_measured_fraction_theta_full     0.998
_diffrn_reflns_limit_h_min     -14
_diffrn_reflns_limit_h_max     14
_diffrn_reflns_limit_k_min     -22
_diffrn_reflns_limit_k_max     22
_diffrn_reflns_limit_l_min     -20
_diffrn_reflns_limit_l_max     20
_diffrn_standards_number     0
_diffrn_standards_interval_count     .
_diffrn_standards_interval_time     .
_diffrn_standards_decay_%     ?
_refine_special_details
;
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 >
σ(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     6968
_reflns_number_gt     5819
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0333
_refine_ls_R_factor_gt     0.0234
_refine_ls_wR_factor_gt     0.0652
_refine_ls_wR_factor_ref     0.0721
_refine_ls_goodness_of_fit_ref     1.001
_refine_ls_restrained_S_all     1.001
_refine_ls_number_reflns     6968
_refine_ls_number_parameters     559
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
         'calc w=1/[σ²(Fo²)+(0.0470P)²+0.0562P] 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     0.009
_refine_ls_shift/su_mean     0.002
_refine_diff_density_max     0.474
_refine_diff_density_min     -0.536
_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' 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'
    'O' 'O' 0.0106 0.0060
                         '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'
    'Mo' 'Mo' -1.6832 0.6857
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'APEX2 (Bruker, 2004)'
_computing_cell_refinement     'SAINT-Plus (Bruker, 2001)'
_computing_data_reduction     'SAINT-Plus (Bruker, 2001)'
_computing_structure_solution     'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics     'SHELXTL (Sheldrick, 2008)'
_computing_publication_material     'SHELXTL (Sheldrick, 2008)'
loop_
    _atom_site_type_symbol
    _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
    C C1 0.2047(3) 0.7484(2) 0.7553(2) 0.0372(8) Uani d . 1 . .
    H H1 0.1832 0.7861 0.7834 0.045 Uiso calc R 1 . .
    C C2 0.1962(3) 0.6817(2) 0.7838(2) 0.0427(9) Uani d . 1 . .
    H H2 0.1696 0.6743 0.8302 0.051 Uiso calc R 1 . .
    C C3 0.2280(3) 0.6259(2) 0.7419(2) 0.0477(10) Uani d . 1 . .
    H H3 0.2229 0.5799 0.7596 0.057 Uiso calc R 1 . .
    C C4 0.2672(3) 0.63901(19) 0.6741(2) 0.0437(9) Uani d . 1 . .
    H H4 0.2883 0.6019 0.6450 0.052 Uiso calc R 1 . .
    C C5 0.2752(3) 0.70811(17) 0.6490(2) 0.0313(8) Uani d . 1 . .
    C C6 0.3212(3) 0.72633(18) 0.5787(2) 0.0342(8) Uani d . 1 . .
    C C7 0.3484(3) 0.6771(2) 0.5263(2) 0.0471(10) Uani d . 1 . .
    H H7 0.3358 0.6295 0.5334 0.057 Uiso calc R 1 . .
    C C8 0.3943(4) 0.6991(2) 0.4636(2) 0.0530(11) Uani d . 1 . .
    H H8 0.4127 0.6666 0.4279 0.064 Uiso calc R 1 . .
    C C9 0.4126(3) 0.7691(2) 0.4546(2) 0.0469(10) Uani d . 1 . .
    H H9 0.4441 0.7850 0.4129 0.056 Uiso calc R 1 . .
    C C10 0.3838(3) 0.8157(2) 0.5080(2) 0.0405(9) Uani d . 1 . .
    H H10 0.3962 0.8635 0.5013 0.049 Uiso calc R 1 . .
    C C11 0.5056(3) 0.85816(19) 0.7315(2) 0.0409(9) Uani d . 1 . .
    H H11 0.5233 0.8418 0.6845 0.049 Uiso calc R 1 . .
    C C12 0.5877(3) 0.8614(2) 0.7979(3) 0.0469(10) Uani d . 1 . .
    H H12 0.6594 0.8479 0.7956 0.056 Uiso calc R 1 . .
    C C13 0.5618(3) 0.8847(2) 0.8674(3) 0.0478(10) Uani d . 1 . .
    H H13 0.6158 0.8873 0.9132 0.057 Uiso calc R 1 . .
    C C14 0.4549(3) 0.90433(19) 0.8687(2) 0.0427(9) Uani d . 1 . .
    H H14 0.4356 0.9193 0.9157 0.051 Uiso calc R 1 . .
    C C15 0.3769(3) 0.90155(17) 0.7999(2) 0.0310(7) Uani d . 1 . .
    C C16 0.2599(3) 0.92287(16) 0.7947(2) 0.0301(7) Uani d . 1 . .
    C C17 0.2196(3) 0.94944(19) 0.8589(2) 0.0411(9) Uani d . 1 . .
    H H17 0.2662 0.9555 0.9078 0.049 Uiso calc R 1 . .
    C C18 0.1088(3) 0.9667(2) 0.8489(2) 0.0447(9) Uani d . 1 . .
    H H18 0.0802 0.9844 0.8912 0.054 Uiso calc R 1 . .
    C C19 0.0415(3) 0.9576(2) 0.7760(2) 0.0459(10) Uani d . 1 . .
    H H19 -0.0329 0.9693 0.7678 0.055 Uiso calc R 1 . .
    C C20 0.0872(3) 0.93069(19) 0.7155(2) 0.0407(9) Uani d . 1 . .
    H H20 0.0418 0.9243 0.6662 0.049 Uiso calc R 1 . .
    C C21 0.3602(3) 1.00319(19) 0.5998(2) 0.0455(9) Uani d . 1 . .
    H H21 0.4128 0.9962 0.6457 0.055 Uiso calc R 1 . .
    C C22 0.3655(4) 1.0633(2) 0.5560(3) 0.0539(11) Uani d . 1 . .
    H H22 0.4210 1.0962 0.5719 0.065 Uiso calc R 1 . .
    C C23 0.2880(4) 1.0738(2) 0.4886(3) 0.0653(13) Uani d . 1 . .
    H H23 0.2898 1.1140 0.4581 0.078 Uiso calc R 1 . .
    C C24 0.2077(4) 1.0237(2) 0.4670(3) 0.0570(11) Uani d . 1 . .
    H H24 0.1540 1.0303 0.4216 0.068 Uiso calc R 1 . .
    C C25 0.2060(3) 0.96389(18) 0.5121(2) 0.0360(8) Uani d . 1 . .
    C C26 0.1217(3) 0.90776(18) 0.4935(2) 0.0349(8) Uani d . 1 . .
    C C27 0.0483(3) 0.9037(2) 0.4220(2) 0.0529(11) Uani d . 1 . .
    H H27 0.0494 0.9374 0.3828 0.064 Uiso calc R 1 . .
    C C28 -0.0262(4) 0.8494(3) 0.4097(2) 0.0641(13) Uani d . 1 . .
    H H28 -0.0764 0.8461 0.3620 0.077 Uiso calc R 1 . .
    C C29 -0.0265(3) 0.8002(2) 0.4676(2) 0.0554(11) Uani d . 1 . .
    H H29 -0.0772 0.7634 0.4602 0.066 Uiso calc R 1 . .
    C C30 0.0501(3) 0.8061(2) 0.5371(2) 0.0439(9) Uani d . 1 . .
    H H30 0.0504 0.7725 0.5765 0.053 Uiso calc R 1 . .
    Mo Mo1 0.78107(3) 0.201308(17) 0.957341(19) 0.03791(9) Uani d . 1 . .
    Mo Mo2 0.66433(3) 0.063859(18) 0.733433(19) 0.03975(10) Uani d . 1 . .
    Mo Mo3 0.82030(2) 0.038531(16) 0.907938(19) 0.03494(9) Uani d . 1 . .
    Mo Mo4 0.56817(2) 0.097421(17) 0.894435(19) 0.03583(9) Uani d . 1 . .
    Mo Mo5 0.62406(3) 0.227585(18) 0.78320(2) 0.04239(10) Uani d . 1 . .
    Mo Mo6 0.87528(2) 0.167533(17) 0.795574(19) 0.03537(9) Uani d . 1 . .
    N N1 0.2427(2) 0.76195(14) 0.68892(16) 0.0305(6) Uani d . 1 . .
    N N2 0.3387(2) 0.79591(15) 0.56930(16) 0.0328(7) Uani d . 1 . .
    N N3 0.4013(2) 0.87750(14) 0.73126(16) 0.0320(6) Uani d . 1 . .
    N N4 0.1938(2) 0.91327(14) 0.72410(17) 0.0329(6) Uani d . 1 . .
    N N5 0.1243(2) 0.85861(15) 0.55014(16) 0.0336(6) Uani d . 1 . .
    N N6 0.2817(2) 0.95434(14) 0.57853(17) 0.0336(7) Uani d . 1 . .
    Ni Ni1 0.26519(3) 0.86154(2) 0.64110(2) 0.02895(11) Uani d . 1 . .
    O O1 0.8233(2) 0.25281(15) 1.03673(16) 0.0553(7) Uani d . 1 . .
    O O2 0.8935(2) -0.02945(14) 0.95332(18) 0.0530(7) Uani d . 1 . .
    O O3 0.6193(2) 0.01285(17) 0.65399(17) 0.0612(8) Uani d . 1 . .
    O O4 0.5487(2) 0.29421(16) 0.73646(19) 0.0661(9) Uani d . 1 . .
    O O5 0.4599(2) 0.07256(15) 0.93400(16) 0.0505(7) Uani d . 1 . .
    O O6 0.9841(2) 0.19293(15) 0.75756(17) 0.0508(7) Uani d . 1 . .
    O O7 0.7549(2) 0.00033(12) 0.80675(15) 0.0426(6) Uani d . 1 . .
    O O8 0.92547(19) 0.08525(12) 0.85333(15) 0.0382(6) Uani d . 1 . .
    O O9 0.85473(18) 0.11392(13) 0.98427(14) 0.0385(6) Uani d . 1 . .
    O O10 0.68230(19) 0.02940(12) 0.93946(14) 0.0380(6) Uani d . 1 . .
    O O11 0.6499(2) 0.16021(13) 0.97714(14) 0.0406(6) Uani d . 1 . .
    O O12 0.89135(19) 0.21893(12) 0.89103(15) 0.0388(6) Uani d . 1 . .
    O O13 0.55100(19) 0.04720(13) 0.79866(15) 0.0400(6) Uani d . 1 . .
    O O14 0.7956(2) 0.10435(14) 0.71345(14) 0.0444(6) Uani d . 1 . .
    O O15 0.5892(2) 0.15067(14) 0.70706(14) 0.0457(6) Uani d . 1 . .
    O O16 0.7612(2) 0.23554(13) 0.75091(15) 0.0452(6) Uani d . 1 . .
    O O17 0.51973(19) 0.18101(13) 0.83857(15) 0.0428(6) Uani d . 1 . .
    O O18 0.6892(2) 0.26559(12) 0.88422(16) 0.0466(6) Uani d . 1 . .
    O O19 0.72228(16) 0.13273(10) 0.84515(12) 0.0287(5) Uani d . 1 . .
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
    C1 0.0354(19) 0.045(2) 0.031(2) -0.0048(16) 0.0068(16) -0.0007(16)
    C2 0.043(2) 0.049(2) 0.035(2) -0.0051(18) 0.0053(17) 0.0113(18)
    C3 0.052(2) 0.038(2) 0.052(3) -0.0061(18) 0.007(2) 0.0122(19)
    C4 0.052(2) 0.031(2) 0.047(2) -0.0004(17) 0.0077(19) -0.0009(17)
    C5 0.0310(18) 0.0308(18) 0.0292(18) 0.0004(14) -0.0018(14) -0.0009(15)
    C6 0.0374(19) 0.034(2) 0.0293(19) 0.0038(15) 0.0024(15) 0.0001(15)
    C7 0.070(3) 0.033(2) 0.041(2) 0.0031(19) 0.017(2) -0.0066(17)
    C8 0.072(3) 0.049(3) 0.042(2) 0.010(2) 0.019(2) -0.0105(19)
    C9 0.053(2) 0.059(3) 0.031(2) 0.012(2) 0.0124(18) 0.0000(18)
    C10 0.049(2) 0.041(2) 0.035(2) 0.0021(17) 0.0152(18) 0.0047(16)
    C11 0.037(2) 0.039(2) 0.049(2) 0.0037(16) 0.0136(18) -0.0044(17)
    C12 0.0312(19) 0.042(2) 0.065(3) 0.0029(17) 0.0023(19) -0.005(2)
    C13 0.039(2) 0.043(2) 0.054(3) 0.0010(18) -0.0102(19) -0.0046(19)
    C14 0.048(2) 0.043(2) 0.035(2) -0.0041(18) 0.0024(17) -0.0071(17)
    C15 0.0348(18) 0.0252(17) 0.0335(19) -0.0018(14) 0.0080(15) 0.0007(14)
    C16 0.0398(19) 0.0212(16) 0.0306(19) -0.0001(14) 0.0101(15) 0.0036(14)
    C17 0.049(2) 0.040(2) 0.035(2) 0.0059(17) 0.0096(17) -0.0043(16)
    C18 0.048(2) 0.047(2) 0.043(2) 0.0073(18) 0.0213(19) -0.0042(18)
    C19 0.036(2) 0.048(2) 0.056(3) 0.0133(18) 0.0144(19) 0.0000(19)
    C20 0.039(2) 0.045(2) 0.036(2) 0.0075(17) 0.0029(17) -0.0038(17)
    C21 0.045(2) 0.041(2) 0.051(2) -0.0072(18) 0.0105(19) -0.0045(19)
    C22 0.065(3) 0.034(2) 0.067(3) -0.014(2) 0.022(2) -0.005(2)
    C23 0.094(4) 0.037(2) 0.070(3) -0.006(2) 0.027(3) 0.014(2)
    C24 0.070(3) 0.045(2) 0.052(3) 0.002(2) 0.002(2) 0.016(2)
    C25 0.043(2) 0.0325(19) 0.034(2) 0.0056(16) 0.0113(16) 0.0015(15)
    C26 0.0335(19) 0.040(2) 0.0321(19) 0.0030(15) 0.0080(15) 0.0051(16)
    C27 0.048(2) 0.072(3) 0.037(2) -0.009(2) 0.0019(19) 0.012(2)
    C28 0.048(3) 0.105(4) 0.035(2) -0.019(3) -0.0030(19) 0.001(2)
    C29 0.042(2) 0.075(3) 0.048(3) -0.023(2) 0.007(2) -0.006(2)
    C30 0.038(2) 0.051(2) 0.044(2) -0.0113(18) 0.0117(18) 0.0042(18)
    Mo1 0.03947(19) 0.03603(18) 0.03897(19) -0.00078(14) 0.00938(15)
                                                                    -0.00888(14)
    Mo2 0.03436(18) 0.0506(2) 0.03378(19) -0.00618(14) 0.00537(14) -0.00796(15)
    Mo3 0.03277(17) 0.03014(17) 0.04154(19) 0.00591(13) 0.00619(14) 0.00551(13)
    Mo4 0.02880(17) 0.04349(19) 0.03698(19) 0.00007(13) 0.01082(13) 0.00503(14)
    Mo5 0.03764(19) 0.0421(2) 0.0484(2) 0.01227(14) 0.01073(15) 0.01602(15)
    Mo6 0.03013(17) 0.03729(18) 0.04096(19) -0.00224(13) 0.01251(14) 0.00231(14)
    N1 0.0344(15) 0.0301(15) 0.0261(15) -0.0028(12) 0.0033(12) 0.0019(12)
    N2 0.0369(16) 0.0336(16) 0.0287(16) 0.0019(13) 0.0080(13) -0.0001(12)
    N3 0.0312(15) 0.0300(15) 0.0344(16) 0.0018(12) 0.0054(13) -0.0015(12)
    N4 0.0319(15) 0.0318(15) 0.0350(17) 0.0048(12) 0.0064(13) 0.0019(12)
    N5 0.0311(15) 0.0364(16) 0.0335(16) -0.0016(13) 0.0069(13) 0.0005(13)
    N6 0.0352(16) 0.0285(15) 0.0378(17) -0.0021(12) 0.0089(13) -0.0007(13)
    Ni1 0.0297(2) 0.0287(2) 0.0287(2) 0.00063(18) 0.00644(18) -0.00019(18)
    O1 0.0588(18) 0.0545(17) 0.0537(18) -0.0036(14) 0.0139(15) -0.0208(14)
    O2 0.0491(16) 0.0368(14) 0.071(2) 0.0091(12) 0.0052(14) 0.0127(14)
    O3 0.0499(17) 0.083(2) 0.0496(18) -0.0156(16) 0.0074(14) -0.0250(16)
    O4 0.0562(18) 0.0578(19) 0.083(2) 0.0200(15) 0.0104(17) 0.0318(17)
    O5 0.0364(15) 0.0683(19) 0.0500(17) -0.0068(13) 0.0166(13) 0.0075(14)
    O6 0.0387(15) 0.0616(18) 0.0562(18) -0.0080(13) 0.0190(13) 0.0004(14)
    O7 0.0456(15) 0.0323(13) 0.0498(16) -0.0011(11) 0.0088(12) -0.0086(12)
    O8 0.0291(12) 0.0359(13) 0.0509(16) 0.0035(10) 0.0107(11) -0.0012(12)
    O9 0.0338(13) 0.0443(14) 0.0343(14) 0.0037(11) -0.0011(11) 0.0012(11)
    O10 0.0367(13) 0.0373(14) 0.0397(14) -0.0002(11) 0.0069(11) 0.0099(11)
    O11 0.0406(14) 0.0464(15) 0.0374(14) 0.0032(11) 0.0138(12) -0.0033(12)
    O12 0.0347(13) 0.0365(13) 0.0460(15) -0.0058(11) 0.0095(11) -0.0041(11)
    O13 0.0340(13) 0.0445(15) 0.0409(15) -0.0064(11) 0.0055(11) -0.0028(12)
    O14 0.0385(14) 0.0629(17) 0.0352(14) -0.0063(13) 0.0155(12) -0.0075(13)
    O15 0.0370(14) 0.0622(17) 0.0351(14) 0.0028(12) 0.0001(11) 0.0132(13)
    O16 0.0437(15) 0.0428(15) 0.0516(16) -0.0004(12) 0.0153(13) 0.0189(12)
    O17 0.0329(13) 0.0500(15) 0.0471(15) 0.0098(12) 0.0117(12) 0.0082(12)
    O18 0.0501(16) 0.0320(13) 0.0602(18) 0.0073(12) 0.0165(13) -0.0011(12)
    O19 0.0266(12) 0.0287(12) 0.0313(12) 0.0019(9) 0.0069(10) 0.0021(10)
_geom_special_details
;
All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s 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
    C1 N1 . 1.341(4) ?
    C1 C2 . 1.369(5) ?
    C1 H1 . 0.9300 ?
    C2 C3 . 1.381(5) ?
    C2 H2 . 0.9300 ?
    C3 C4 . 1.369(5) ?
    C3 H3 . 0.9300 ?
    C4 C5 . 1.391(5) ?
    C4 H4 . 0.9300 ?
    C5 N1 . 1.336(4) ?
    C5 C6 . 1.472(5) ?
    C6 N2 . 1.353(4) ?
    C6 C7 . 1.383(5) ?
    C7 C8 . 1.377(6) ?
    C7 H7 . 0.9300 ?
    C8 C9 . 1.361(6) ?
    C8 H8 . 0.9300 ?
    C9 C10 . 1.371(5) ?
    C9 H9 . 0.9300 ?
    C10 N2 . 1.338(4) ?
    C10 H10 . 0.9300 ?
    C11 N3 . 1.339(4) ?
    C11 C12 . 1.374(5) ?
    C11 H11 . 0.9300 ?
    C12 C13 . 1.370(6) ?
    C12 H12 . 0.9300 ?
    C13 C14 . 1.377(5) ?
    C13 H13 . 0.9300 ?
    C14 C15 . 1.375(5) ?
    C14 H14 . 0.9300 ?
    C15 N3 . 1.353(4) ?
    C15 C16 . 1.487(5) ?
    C16 N4 . 1.339(4) ?
    C16 C17 . 1.390(5) ?
    C17 C18 . 1.385(5) ?
    C17 H17 . 0.9300 ?
    C18 C19 . 1.376(5) ?
    C18 H18 . 0.9300 ?
    C19 C20 . 1.372(5) ?
    C19 H19 . 0.9300 ?
    C20 N4 . 1.338(4) ?
    C20 H20 . 0.9300 ?
    C21 N6 . 1.341(4) ?
    C21 C22 . 1.376(5) ?
    C21 H21 . 0.9300 ?
    C22 C23 . 1.368(6) ?
    C22 H22 . 0.9300 ?
    C23 C24 . 1.372(6) ?
    C23 H23 . 0.9300 ?
    C24 C25 . 1.378(5) ?
    C24 H24 . 0.9300 ?
    C25 N6 . 1.342(4) ?
    C25 C26 . 1.481(5) ?
    C26 N5 . 1.344(4) ?
    C26 C27 . 1.382(5) ?
    C27 C28 . 1.371(6) ?
    C27 H27 . 0.9300 ?
    C28 C29 . 1.367(6) ?
    C28 H28 . 0.9300 ?
    C29 C30 . 1.379(5) ?
    C29 H29 . 0.9300 ?
    C30 N5 . 1.343(4) ?
    C30 H30 . 0.9300 ?
    Mo1 O1 . 1.679(3) ?
    Mo1 O11 . 1.888(2) ?
    Mo1 O9 . 1.906(2) ?
    Mo1 O18 . 1.952(3) ?
    Mo1 O12 . 1.967(2) ?
    Mo1 O19 . 2.325(2) ?
    Mo2 O3 . 1.680(3) ?
    Mo2 O14 . 1.885(2) ?
    Mo2 O15 . 1.903(3) ?
    Mo2 O7 . 1.937(2) ?
    Mo2 O13 . 1.981(2) ?
    Mo2 O19 . 2.320(2) ?
    Mo3 O2 . 1.680(2) ?
    Mo3 O10 . 1.894(2) ?
    Mo3 O7 . 1.914(2) ?
    Mo3 O9 . 1.933(2) ?
    Mo3 O8 . 1.956(2) ?
    Mo3 O19 . 2.308(2) ?
    Mo4 O5 . 1.681(2) ?
    Mo4 O13 . 1.879(2) ?
    Mo4 O17 . 1.892(2) ?
    Mo4 O10 . 1.958(2) ?
    Mo4 O11 . 1.977(2) ?
    Mo4 O19 . 2.327(2) ?
    Mo5 O4 . 1.680(3) ?
    Mo5 O16 . 1.888(2) ?
    Mo5 O18 . 1.910(3) ?
    Mo5 O15 . 1.953(3) ?
    Mo5 O17 . 1.955(3) ?
    Mo5 O19 . 2.314(2) ?
    Mo6 O6 . 1.675(3) ?
    Mo6 O12 . 1.887(2) ?
    Mo6 O8 . 1.891(2) ?
    Mo6 O16 . 1.956(2) ?
    Mo6 O14 . 1.966(2) ?
    Mo6 O19 . 2.315(2) ?
    N4 Ni1 . 2.066(3) y
    N3 Ni1 . 2.078(3) y
    N2 Ni1 . 2.082(3) y
    N6 Ni1 . 2.095(3) y
    N1 Ni1 . 2.101(3) y
    N5 Ni1 . 2.105(3) y
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 C1 C2 . . 123.1(4) ?
    N1 C1 H1 . . 118.5 ?
    C2 C1 H1 . . 118.5 ?
    C1 C2 C3 . . 118.3(4) ?
    C1 C2 H2 . . 120.8 ?
    C3 C2 H2 . . 120.8 ?
    C4 C3 C2 . . 119.2(4) ?
    C4 C3 H3 . . 120.4 ?
    C2 C3 H3 . . 120.4 ?
    C3 C4 C5 . . 119.6(4) ?
    C3 C4 H4 . . 120.2 ?
    C5 C4 H4 . . 120.2 ?
    N1 C5 C4 . . 121.0(3) ?
    N1 C5 C6 . . 116.4(3) ?
    C4 C5 C6 . . 122.6(3) ?
    N2 C6 C7 . . 121.1(3) ?
    N2 C6 C5 . . 115.0(3) ?
    C7 C6 C5 . . 123.8(3) ?
    C8 C7 C6 . . 119.6(4) ?
    C8 C7 H7 . . 120.2 ?
    C6 C7 H7 . . 120.2 ?
    C9 C8 C7 . . 119.2(4) ?
    C9 C8 H8 . . 120.4 ?
    C7 C8 H8 . . 120.4 ?
    C10 C9 C8 . . 118.9(4) ?
    C10 C9 H9 . . 120.5 ?
    C8 C9 H9 . . 120.5 ?
    N2 C10 C9 . . 123.2(4) ?
    N2 C10 H10 . . 118.4 ?
    C9 C10 H10 . . 118.4 ?
    N3 C11 C12 . . 123.1(4) ?
    N3 C11 H11 . . 118.4 ?
    C12 C11 H11 . . 118.4 ?
    C13 C12 C11 . . 118.7(4) ?
    C13 C12 H12 . . 120.7 ?
    C11 C12 H12 . . 120.7 ?
    C12 C13 C14 . . 119.2(4) ?
    C12 C13 H13 . . 120.4 ?
    C14 C13 H13 . . 120.4 ?
    C15 C14 C13 . . 119.4(4) ?
    C15 C14 H14 . . 120.3 ?
    C13 C14 H14 . . 120.3 ?
    N3 C15 C14 . . 121.8(3) ?
    N3 C15 C16 . . 114.7(3) ?
    C14 C15 C16 . . 123.5(3) ?
    N4 C16 C17 . . 121.3(3) ?
    N4 C16 C15 . . 115.7(3) ?
    C17 C16 C15 . . 123.0(3) ?
    C18 C17 C16 . . 118.9(4) ?
    C18 C17 H17 . . 120.5 ?
    C16 C17 H17 . . 120.5 ?
    C19 C18 C17 . . 119.4(3) ?
    C19 C18 H18 . . 120.3 ?
    C17 C18 H18 . . 120.3 ?
    C18 C19 C20 . . 118.3(3) ?
    C18 C19 H19 . . 120.9 ?
    C20 C19 H19 . . 120.9 ?
    N4 C20 C19 . . 123.2(3) ?
    N4 C20 H20 . . 118.4 ?
    C19 C20 H20 . . 118.4 ?
    N6 C21 C22 . . 122.2(4) ?
    N6 C21 H21 . . 118.9 ?
    C22 C21 H21 . . 118.9 ?
    C23 C22 C21 . . 119.0(4) ?
    C23 C22 H22 . . 120.5 ?
    C21 C22 H22 . . 120.5 ?
    C22 C23 C24 . . 118.7(4) ?
    C22 C23 H23 . . 120.7 ?
    C24 C23 H23 . . 120.7 ?
    C23 C24 C25 . . 120.5(4) ?
    C23 C24 H24 . . 119.8 ?
    C25 C24 H24 . . 119.8 ?
    N6 C25 C24 . . 120.5(4) ?
    N6 C25 C26 . . 115.6(3) ?
    C24 C25 C26 . . 123.9(3) ?
    N5 C26 C27 . . 121.7(3) ?
    N5 C26 C25 . . 115.2(3) ?
    C27 C26 C25 . . 123.0(3) ?
    C28 C27 C26 . . 119.0(4) ?
    C28 C27 H27 . . 120.5 ?
    C26 C27 H27 . . 120.5 ?
    C29 C28 C27 . . 119.9(4) ?
    C29 C28 H28 . . 120.0 ?
    C27 C28 H28 . . 120.1 ?
    C28 C29 C30 . . 118.5(4) ?
    C28 C29 H29 . . 120.7 ?
    C30 C29 H29 . . 120.7 ?
    N5 C30 C29 . . 122.5(4) ?
    N5 C30 H30 . . 118.7 ?
    C29 C30 H30 . . 118.7 ?
    O1 Mo1 O11 . . 103.71(12) ?
    O1 Mo1 O9 . . 104.51(12) ?
    O11 Mo1 O9 . . 89.01(10) ?
    O1 Mo1 O18 . . 102.16(13) ?
    O11 Mo1 O18 . . 87.81(11) ?
    O9 Mo1 O18 . . 153.14(10) ?
    O1 Mo1 O12 . . 103.36(12) ?
    O11 Mo1 O12 . . 152.83(10) ?
    O9 Mo1 O12 . . 86.40(10) ?
    O18 Mo1 O12 . . 84.37(11) ?
    O1 Mo1 O19 . . 178.41(12) ?
    O11 Mo1 O19 . . 77.08(9) ?
    O9 Mo1 O19 . . 76.84(9) ?
    O18 Mo1 O19 . . 76.45(9) ?
    O12 Mo1 O19 . . 75.79(8) ?
    O3 Mo2 O14 . . 104.40(13) ?
    O3 Mo2 O15 . . 103.63(13) ?
    O14 Mo2 O15 . . 90.04(12) ?
    O3 Mo2 O7 . . 103.27(13) ?
    O14 Mo2 O7 . . 87.90(11) ?
    O15 Mo2 O7 . . 152.67(10) ?
    O3 Mo2 O13 . . 102.07(12) ?
    O14 Mo2 O13 . . 153.52(10) ?
    O15 Mo2 O13 . . 84.70(11) ?
    O7 Mo2 O13 . . 85.10(11) ?
    O3 Mo2 O19 . . 178.16(11) ?
    O14 Mo2 O19 . . 77.42(9) ?
    O15 Mo2 O19 . . 76.57(9) ?
    O7 Mo2 O19 . . 76.39(8) ?
    O13 Mo2 O19 . . 76.12(9) ?
    O2 Mo3 O10 . . 103.34(12) ?
    O2 Mo3 O7 . . 103.09(13) ?
    O10 Mo3 O7 . . 88.85(11) ?
    O2 Mo3 O9 . . 103.01(12) ?
    O10 Mo3 O9 . . 88.04(10) ?
    O7 Mo3 O9 . . 153.73(10) ?
    O2 Mo3 O8 . . 102.91(12) ?
    O10 Mo3 O8 . . 153.73(10) ?
    O7 Mo3 O8 . . 86.47(11) ?
    O9 Mo3 O8 . . 84.87(10) ?
    O2 Mo3 O19 . . 179.07(11) ?
    O10 Mo3 O19 . . 77.57(8) ?
    O7 Mo3 O19 . . 77.10(9) ?
    O9 Mo3 O19 . . 76.76(9) ?
    O8 Mo3 O19 . . 76.19(8) ?
    O5 Mo4 O13 . . 104.36(12) ?
    O5 Mo4 O17 . . 104.04(12) ?
    O13 Mo4 O17 . . 90.54(11) ?
    O5 Mo4 O10 . . 102.90(12) ?
    O13 Mo4 O10 . . 87.88(11) ?
    O17 Mo4 O10 . . 152.54(10) ?
    O5 Mo4 O11 . . 102.35(12) ?
    O13 Mo4 O11 . . 153.12(10) ?
    O17 Mo4 O11 . . 85.82(11) ?
    O10 Mo4 O11 . . 83.35(10) ?
    O5 Mo4 O19 . . 177.53(11) ?
    O13 Mo4 O19 . . 77.82(9) ?
    O17 Mo4 O19 . . 76.96(9) ?
    O10 Mo4 O19 . . 75.92(8) ?
    O11 Mo4 O19 . . 75.41(9) ?
    O4 Mo5 O16 . . 104.16(13) ?
    O4 Mo5 O18 . . 104.37(14) ?
    O16 Mo5 O18 . . 89.58(11) ?
    O4 Mo5 O15 . . 102.23(14) ?
    O16 Mo5 O15 . . 87.55(11) ?
    O18 Mo5 O15 . . 153.14(10) ?
    O4 Mo5 O17 . . 102.54(13) ?
    O16 Mo5 O17 . . 153.20(10) ?
    O18 Mo5 O17 . . 85.97(11) ?
    O15 Mo5 O17 . . 84.68(11) ?
    O4 Mo5 O19 . . 177.68(13) ?
    O16 Mo5 O19 . . 77.11(9) ?
    O18 Mo5 O19 . . 77.50(9) ?
    O15 Mo5 O19 . . 75.82(9) ?
    O17 Mo5 O19 . . 76.12(9) ?
    O6 Mo6 O12 . . 103.46(12) ?
    O6 Mo6 O8 . . 103.67(12) ?
    O12 Mo6 O8 . . 90.08(10) ?
    O6 Mo6 O16 . . 103.22(12) ?
    O12 Mo6 O16 . . 86.98(11) ?
    O8 Mo6 O16 . . 152.90(10) ?
    O6 Mo6 O14 . . 102.92(12) ?
    O12 Mo6 O14 . . 153.44(10) ?
    O8 Mo6 O14 . . 86.64(11) ?
    O16 Mo6 O14 . . 84.12(11) ?
    O6 Mo6 O19 . . 178.63(11) ?
    O12 Mo6 O19 . . 77.51(9) ?
    O8 Mo6 O19 . . 77.24(9) ?
    O16 Mo6 O19 . . 75.83(9) ?
    O14 Mo6 O19 . . 76.06(9) ?
    C1 N1 C5 . . 118.7(3) ?
    C1 N1 Ni1 . . 126.9(2) ?
    C5 N1 Ni1 . . 114.3(2) ?
    C10 N2 C6 . . 118.0(3) ?
    C10 N2 Ni1 . . 126.5(2) ?
    C6 N2 Ni1 . . 114.5(2) ?
    C11 N3 C15 . . 117.8(3) ?
    C11 N3 Ni1 . . 127.0(2) ?
    C15 N3 Ni1 . . 114.6(2) ?
    C20 N4 C16 . . 118.8(3) ?
    C20 N4 Ni1 . . 125.7(2) ?
    C16 N4 Ni1 . . 115.1(2) ?
    C30 N5 C26 . . 118.3(3) ?
    C30 N5 Ni1 . . 125.7(2) ?
    C26 N5 Ni1 . . 114.9(2) ?
    C21 N6 C25 . . 119.2(3) ?
    C21 N6 Ni1 . . 125.4(3) ?
    C25 N6 Ni1 . . 115.5(2) ?
    N4 Ni1 N3 . . 78.88(11) ?
    N4 Ni1 N2 . . 171.03(11) ?
    N3 Ni1 N2 . . 98.46(11) ?
    N4 Ni1 N6 . . 92.97(11) ?
    N3 Ni1 N6 . . 96.64(11) ?
    N2 Ni1 N6 . . 95.86(11) ?
    N4 Ni1 N1 . . 92.93(11) ?
    N3 Ni1 N1 . . 89.33(10) ?
    N2 Ni1 N1 . . 78.42(11) ?
    N6 Ni1 N1 . . 172.31(11) ?
    N4 Ni1 N5 . . 97.11(11) ?
    N3 Ni1 N5 . . 173.07(11) ?
    N2 Ni1 N5 . . 86.35(11) ?
    N6 Ni1 N5 . . 77.82(11) ?
    N1 Ni1 N5 . . 96.56(11) ?
    Mo3 O7 Mo2 . . 116.45(12) ?
    Mo6 O8 Mo3 . . 116.48(11) ?
    Mo1 O9 Mo3 . . 116.57(11) ?
    Mo3 O10 Mo4 . . 116.47(12) ?
    Mo1 O11 Mo4 . . 117.16(12) ?
    Mo6 O12 Mo1 . . 116.61(11) ?
    Mo4 O13 Mo2 . . 116.26(12) ?
    Mo2 O14 Mo6 . . 116.55(12) ?
    Mo2 O15 Mo5 . . 116.95(12) ?
    Mo5 O16 Mo6 . . 116.83(12) ?
    Mo4 O17 Mo5 . . 116.94(12) ?
    Mo5 O18 Mo1 . . 116.14(12) ?
    Mo3 O19 Mo5 . . 179.53(11) ?
    Mo3 O19 Mo6 . . 90.08(7) ?
    Mo5 O19 Mo6 . . 90.07(7) ?
    Mo3 O19 Mo2 . . 90.06(7) ?
    Mo5 O19 Mo2 . . 90.38(7) ?
    Mo6 O19 Mo2 . . 89.97(7) ?
    Mo3 O19 Mo1 . . 89.65(7) ?
    Mo5 O19 Mo1 . . 89.91(7) ?
    Mo6 O19 Mo1 . . 89.95(7) ?
    Mo2 O19 Mo1 . . 179.69(11) ?
    Mo3 O19 Mo4 . . 89.93(7) ?
    Mo5 O19 Mo4 . . 89.92(7) ?
    Mo6 O19 Mo4 . . 179.72(12) ?
    Mo2 O19 Mo4 . . 89.75(7) ?
    Mo1 O19 Mo4 . . 90.33(7) ?
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
    C29 H29 O11 2_556 0.93 2.48 3.293(5) 145.5
    C2 H2 O1 3_667 0.93 2.66 3.381(5) 134.4
    C14 H14 O5 3_667 0.93 2.67 3.386(4) 134.7
    C14 H14 O11 3_667 0.93 2.75 3.396(4) 127.3
    C8 H8 O2 4_565 0.93 2.66 3.228(5) 120.1
    C7 H7 O2 4_565 0.93 2.53 3.169(4) 126.0
    C12 H12 O16 2_656 0.93 2.54 3.241(4) 132.2
    C9 H9 O15 3_666 0.93 2.36 3.165(4) 144.3
    C21 H21 O3 1_565 0.93 2.54 3.163(5) 124.2
