#------------------------------------------------------------------------------
#$Date: 2016-03-04 13:35:45 +0200 (Fri, 04 Mar 2016) $
#$Revision: 177468 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/04/2020405.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2020405
loop_
_publ_author_name
'Dou, Ming-Yu'
'Lu, Jing'
_publ_section_title
;
 A novel octanuclear nickel(II)--molybdenum(VI) heterometallic cluster
 based on the salicylhydroxamate ligand
;
_journal_coeditor_code           QS3051
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              161
_journal_page_last               165
_journal_paper_doi               10.1107/S2053229616000243
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac
'[Mo2 Ni6 (C7 H4 N O3)2 (C2 H3 O2)4 O6 (O H)2 (C5 H5 N)8], H2 O'
_chemical_formula_moiety         'C31 H32 Mo1 N5  Ni3 O11.5'
_chemical_formula_sum            'C62 H64 Mo2 N10 Ni6 O23'
_chemical_formula_weight         1861.38
_chemical_name_systematic
'Di-μ₃-acetato-di-μ₂-acetato-di-μ₃-hydroxido-di-μ₃-oxido-tetraoxidooctakis(pyridine-κN)bis(μ₅-salicylhydroxamato)hexanickel(II)dimolybdenum(VI) dihydrate'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                111.551(7)
_cell_angle_beta                 95.979(7)
_cell_angle_gamma                98.854(6)
_cell_formula_units_Z            1
_cell_length_a                   10.5079(8)
_cell_length_b                   12.7461(9)
_cell_length_c                   14.5850(13)
_cell_measurement_reflns_used    6238
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.74
_cell_volume                     1767.6(3)
_computing_cell_refinement
;
SMART (Bruker, 2002)
;
_computing_data_collection
;
SMART (Bruker, 2002)
;
_computing_data_reduction
;
SAINT (Bruker, 2002)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0894
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11408
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    1.987
_exptl_absorpt_correction_T_max  0.5871
_exptl_absorpt_correction_T_min  0.4366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2002)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             942
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.887
_refine_diff_density_min         -0.508
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         6238
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0298P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.1044
_reflns_number_gt                4334
_reflns_number_total             6238
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            qs3051sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2020405.cif.'
_cod_original_cell_volume        1767.6(2)
_cod_database_code               2020405
_cod_database_fobs_code          2020405
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_symmetry_multiplicity
Ni Ni1 0.94587(6) 0.44119(5) 0.07153(5) 0.02408(18) Uani d . 1 1
Ni Ni2 0.92605(7) 0.64918(6) 0.31885(5) 0.0319(2) Uani d . 1 1
Ni Ni3 1.02780(7) 0.73525(6) 0.16868(5) 0.02695(19) Uani d . 1 1
Mo Mo1 1.21127(5) 0.38549(4) 0.05418(4) 0.02680(15) Uani d . 1 1
O O1 1.3068(3) 0.5309(3) 0.1757(3) 0.0318(9) Uani d . 1 1
O O2 1.1240(3) 0.5341(3) 0.0556(3) 0.0236(8) Uani d . 1 1
O O3 1.0886(4) 0.7702(3) 0.3156(3) 0.0341(10) Uani d . 1 1
O O4 1.0424(4) 0.5366(3) 0.3334(3) 0.0367(10) Uani d . 1 1
O O5 1.0618(3) 0.4169(3) 0.1809(3) 0.0296(9) Uani d . 1 1
O O6 0.8786(4) 0.8259(3) 0.2012(3) 0.0381(10) Uani d . 1 1
O O7 0.7991(4) 0.7537(3) 0.3071(3) 0.0423(11) Uani d . 1 1
O O8 0.9046(3) 0.5865(3) 0.1661(3) 0.0264(9) Uani d . 1 1
H H5A 0.8271 0.5882 0.1442 0.032 Uiso d R 1 1
O O9 0.9536(3) 0.6842(3) 0.0160(3) 0.0260(9) Uani d . 1 1
O O10 1.2661(4) 0.2909(3) 0.0996(3) 0.0367(10) Uani d . 1 1
O O11 1.3063(3) 0.3906(3) -0.0337(3) 0.0340(10) Uani d . 1 1
O O12 0.7689(9) 0.9221(7) 0.0782(8) 0.075(4) Uani d P 0.489(10) 1
H H12C 0.8036 0.9014 0.1223 0.090 Uiso d PR 0.489(10) 1
H H12D 0.7544 0.8653 0.0220 0.090 Uiso d PR 0.489(10) 1
N N1 1.1651(4) 0.6359(3) 0.1432(3) 0.0252(11) Uani d . 1 1
N N2 0.7823(4) 0.3257(4) 0.0615(3) 0.0317(12) Uani d . 1 1
N N3 0.7641(5) 0.5313(4) 0.3251(4) 0.0369(12) Uani d . 1 1
N N4 0.9642(5) 0.7399(4) 0.4773(4) 0.0413(13) Uani d . 1 1
N N5 1.1476(5) 0.8830(4) 0.1649(4) 0.0344(12) Uani d . 1 1
C C1 1.2557(5) 0.6227(4) 0.2037(4) 0.0256(13) Uani d . 1 1
C C2 1.2977(5) 0.7109(4) 0.3059(4) 0.0298(14) Uani d . 1 1
C C3 1.4221(6) 0.7250(5) 0.3566(5) 0.0397(16) Uani d . 1 1
H H3 1.4770 0.6786 0.3240 0.048 Uiso calc R 1 1
C C4 1.4681(6) 0.8031(5) 0.4516(5) 0.0539(19) Uani d . 1 1
H H4 1.5526 0.8106 0.4831 0.065 Uiso calc R 1 1
C C5 1.3866(6) 0.8704(6) 0.4998(5) 0.055(2) Uani d . 1 1
H H5 1.4164 0.9243 0.5650 0.066 Uiso calc R 1 1
C C6 1.2617(6) 0.8601(5) 0.4540(5) 0.0456(17) Uani d . 1 1
H H6 1.2091 0.9079 0.4884 0.055 Uiso calc R 1 1
C C7 1.2119(5) 0.7792(4) 0.3568(4) 0.0307(14) Uani d . 1 1
C C8 0.7915(6) 0.2359(5) 0.0860(5) 0.0463(17) Uani d . 1 1
H H8 0.8738 0.2282 0.1096 0.056 Uiso calc R 1 1
C C9 0.6841(7) 0.1540(6) 0.0778(6) 0.064(2) Uani d . 1 1
H H9 0.6934 0.0931 0.0968 0.077 Uiso calc R 1 1
C C10 0.5615(7) 0.1642(6) 0.0406(6) 0.069(2) Uani d . 1 1
H H10 0.4877 0.1089 0.0327 0.082 Uiso calc R 1 1
C C11 0.5498(6) 0.2562(6) 0.0154(5) 0.054(2) Uani d . 1 1
H H11 0.4686 0.2656 -0.0086 0.065 Uiso calc R 1 1
C C12 0.6624(6) 0.3342(5) 0.0269(5) 0.0420(16) Uani d . 1 1
H H12 0.6551 0.3967 0.0097 0.050 Uiso calc R 1 1
C C13 0.7714(7) 0.4784(6) 0.3882(5) 0.0567(19) Uani d . 1 1
H H13 0.8520 0.4920 0.4282 0.068 Uiso calc R 1 1
C C14 0.6689(7) 0.4052(6) 0.3988(6) 0.067(2) Uani d . 1 1
H H14 0.6794 0.3718 0.4453 0.080 Uiso calc R 1 1
C C15 0.5552(7) 0.3837(6) 0.3410(6) 0.067(2) Uani d . 1 1
H H15 0.4839 0.3347 0.3466 0.081 Uiso calc R 1 1
C C16 0.5416(7) 0.4328(6) 0.2729(6) 0.064(2) Uani d . 1 1
H H16 0.4622 0.4161 0.2304 0.077 Uiso calc R 1 1
C C17 0.6487(6) 0.5084(6) 0.2682(5) 0.0497(18) Uani d . 1 1
H H17 0.6389 0.5442 0.2235 0.060 Uiso calc R 1 1
C C18 0.9185(8) 0.8347(6) 0.5184(6) 0.078(3) Uani d . 1 1
H H18 0.8592 0.8536 0.4781 0.094 Uiso calc R 1 1
C C19 0.9545(9) 0.9056(7) 0.6168(7) 0.095(3) Uani d . 1 1
H H19 0.9211 0.9720 0.6424 0.114 Uiso calc R 1 1
C C20 1.0398(8) 0.8788(7) 0.6780(6) 0.079(3) Uani d . 1 1
H H20 1.0644 0.9254 0.7458 0.095 Uiso calc R 1 1
C C21 1.0869(8) 0.7835(7) 0.6374(5) 0.070(2) Uani d . 1 1
H H21 1.1460 0.7630 0.6765 0.084 Uiso calc R 1 1
C C22 1.0468(7) 0.7161(6) 0.5369(5) 0.0522(19) Uani d . 1 1
H H22 1.0803 0.6500 0.5099 0.063 Uiso calc R 1 1
C C23 1.0936(6) 0.9447(5) 0.1219(5) 0.0421(16) Uani d . 1 1
H H23 1.0072 0.9175 0.0889 0.051 Uiso calc R 1 1
C C24 1.1617(7) 1.0485(5) 0.1243(5) 0.056(2) Uani d . 1 1
H H24 1.1204 1.0902 0.0942 0.067 Uiso calc R 1 1
C C25 1.2874(7) 1.0887(6) 0.1704(6) 0.069(2) Uani d . 1 1
H H25 1.3341 1.1587 0.1740 0.083 Uiso calc R 1 1
C C26 1.3439(7) 1.0227(6) 0.2117(6) 0.074(2) Uani d . 1 1
H H26 1.4311 1.0470 0.2429 0.089 Uiso calc R 1 1
C C27 1.2727(6) 0.9216(6) 0.2071(5) 0.0541(19) Uani d . 1 1
H H27 1.3136 0.8777 0.2348 0.065 Uiso calc R 1 1
C C28 1.0902(5) 0.4596(5) 0.2759(5) 0.0321(14) Uani d . 1 1
C C29 1.1857(6) 0.4101(6) 0.3223(5) 0.0488(18) Uani d . 1 1
H H29A 1.2675 0.4648 0.3490 0.073 Uiso calc R 1 1
H H29B 1.1990 0.3404 0.2725 0.073 Uiso calc R 1 1
H H29C 1.1521 0.3933 0.3753 0.073 Uiso calc R 1 1
C C30 0.7968(6) 0.8139(5) 0.2548(5) 0.0387(16) Uani d . 1 1
C C31 0.6862(6) 0.8750(6) 0.2571(6) 0.071(2) Uani d . 1 1
H H31A 0.7101 0.9383 0.2373 0.107 Uiso calc R 1 1
H H31B 0.6669 0.9036 0.3237 0.107 Uiso calc R 1 1
H H31C 0.6103 0.8224 0.2118 0.107 Uiso calc R 1 1
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'
O O 0.0106 0.0060 '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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O8 Ni1 N2 . . 99.94(15) y
O8 Ni1 O5 . . 94.19(14) y
N2 Ni1 O5 . . 97.24(17) y
O8 Ni1 O2 . 2_765 94.19(13) y
N2 Ni1 O2 . 2_765 94.66(17) y
O5 Ni1 O2 . 2_765 164.04(14) y
O8 Ni1 O2 . . 91.54(13) y
N2 Ni1 O2 . . 168.18(14) y
O5 Ni1 O2 . . 84.64(14) y
O2 Ni1 O2 2_765 . 81.58(14) y
O8 Ni1 O9 . 2_765 163.33(14) y
N2 Ni1 O9 . 2_765 95.88(15) y
O5 Ni1 O9 . 2_765 78.55(13) y
O2 Ni1 O9 2_765 2_765 89.71(13) y
O2 Ni1 O9 . 2_765 72.99(12) y
O8 Ni2 O7 . . 86.92(15) y
O8 Ni2 O4 . . 94.40(14) y
O7 Ni2 O4 . . 175.63(17) y
O8 Ni2 N3 . . 96.28(17) y
O7 Ni2 N3 . . 88.23(18) y
O4 Ni2 N3 . . 87.49(17) y
O8 Ni2 N4 . . 170.72(18) y
O7 Ni2 N4 . . 89.55(18) y
O4 Ni2 N4 . . 89.76(18) y
N3 Ni2 N4 . . 92.18(19) y
O8 Ni2 O3 . . 84.81(14) y
O7 Ni2 O3 . . 91.35(15) y
O4 Ni2 O3 . . 92.91(14) y
N3 Ni2 O3 . . 178.81(16) y
N4 Ni2 O3 . . 86.71(17) y
O3 Ni3 N1 . . 85.18(16) y
O3 Ni3 O6 . . 91.96(15) y
N1 Ni3 O6 . . 174.19(17) y
O3 Ni3 O9 . . 174.44(15) y
N1 Ni3 O9 . . 94.05(15) y
O6 Ni3 O9 . . 88.31(14) y
O3 Ni3 O8 . . 85.80(15) y
N1 Ni3 O8 . . 84.72(15) y
O6 Ni3 O8 . . 90.03(14) y
O9 Ni3 O8 . . 88.64(13) y
O3 Ni3 N5 . . 96.61(17) y
N1 Ni3 N5 . . 95.75(17) y
O6 Ni3 N5 . . 89.60(16) y
O9 Ni3 N5 . . 88.95(17) y
O8 Ni3 N5 . . 177.58(17) y
O10 Mo1 O11 . . 104.67(17) y
O10 Mo1 O9 . 2_765 106.80(17) y
O11 Mo1 O9 . 2_765 105.57(16) y
O10 Mo1 O1 . . 94.89(16) y
O11 Mo1 O1 . . 100.82(16) y
O9 Mo1 O1 2_765 . 139.85(13) y
O10 Mo1 O2 . . 157.59(15) y
O11 Mo1 O2 . . 95.03(14) y
O9 Mo1 O2 2_765 . 77.34(13) y
O1 Mo1 O2 . . 70.62(12) y
O10 Mo1 O5 . . 86.98(15) y
O11 Mo1 O5 . . 167.82(14) y
O9 Mo1 O5 2_765 . 73.71(13) y
O1 Mo1 O5 . . 74.18(13) y
O2 Mo1 O5 . . 72.87(12) y
C1 O1 Mo1 . . 119.9(3) ?
N1 O2 Ni1 . 2_765 114.9(3) ?
N1 O2 Ni1 . . 107.6(2) ?
Ni1 O2 Ni1 2_765 . 98.42(14) ?
N1 O2 Mo1 . . 115.8(3) ?
Ni1 O2 Mo1 2_765 . 124.39(15) ?
Ni1 O2 Mo1 . . 86.75(12) ?
C7 O3 Ni3 . . 124.7(3) ?
C7 O3 Ni2 . . 123.7(3) ?
Ni3 O3 Ni2 . . 92.33(15) ?
C28 O4 Ni2 . . 136.3(4) ?
C28 O5 Ni1 . . 137.8(3) ?
C28 O5 Mo1 . . 129.3(3) ?
Ni1 O5 Mo1 . . 81.45(13) ?
C30 O6 Ni3 . . 125.9(4) ?
C30 O7 Ni2 . . 129.6(4) ?
Ni1 O8 Ni2 . . 129.22(17) ?
Ni1 O8 Ni3 . . 112.05(15) ?
Ni2 O8 Ni3 . . 92.65(13) ?
Ni1 O8 H5A . . 106.9 ?
Ni2 O8 H5A . . 106.9 ?
Ni3 O8 H5A . . 107.0 ?
Mo1 O9 Ni3 2_765 . 130.21(18) ?
Mo1 O9 Ni1 2_765 2_765 97.63(14) ?
Ni3 O9 Ni1 . 2_765 109.47(14) ?
H12C O12 H12D . . 108.1 ?
C1 N1 O2 . . 110.1(4) ?
C1 N1 Ni3 . . 131.9(4) ?
O2 N1 Ni3 . . 112.5(3) ?
C8 N2 C12 . . 117.5(5) ?
C8 N2 Ni1 . . 120.6(4) ?
C12 N2 Ni1 . . 121.9(4) ?
C17 N3 C13 . . 115.9(6) ?
C17 N3 Ni2 . . 122.0(5) ?
C13 N3 Ni2 . . 122.1(5) ?
C22 N4 C18 . . 116.5(6) ?
C22 N4 Ni2 . . 122.8(4) ?
C18 N4 Ni2 . . 120.0(5) ?
C27 N5 C23 . . 117.2(6) ?
C27 N5 Ni3 . . 124.3(4) ?
C23 N5 Ni3 . . 118.5(4) ?
N1 C1 O1 . . 121.0(5) ?
N1 C1 C2 . . 119.2(4) ?
O1 C1 C2 . . 119.8(5) ?
C3 C2 C7 . . 118.5(5) ?
C3 C2 C1 . . 119.5(5) ?
C7 C2 C1 . . 121.9(5) ?
C4 C3 C2 . . 123.4(5) ?
C4 C3 H3 . . 118.3 ?
C2 C3 H3 . . 118.3 ?
C3 C4 C5 . . 118.1(6) ?
C3 C4 H4 . . 120.9 ?
C5 C4 H4 . . 120.9 ?
C4 C5 C6 . . 121.4(6) ?
C4 C5 H5 . . 119.3 ?
C6 C5 H5 . . 119.3 ?
C5 C6 C7 . . 121.4(6) ?
C5 C6 H6 . . 119.3 ?
C7 C6 H6 . . 119.3 ?
O3 C7 C6 . . 119.5(5) ?
O3 C7 C2 . . 123.3(5) ?
C6 C7 C2 . . 117.2(5) ?
N2 C8 C9 . . 122.7(6) ?
N2 C8 H8 . . 118.7 ?
C9 C8 H8 . . 118.7 ?
C8 C9 C10 . . 118.6(7) ?
C8 C9 H9 . . 120.7 ?
C10 C9 H9 . . 120.7 ?
C11 C10 C9 . . 119.6(7) ?
C11 C10 H10 . . 120.2 ?
C9 C10 H10 . . 120.2 ?
C10 C11 C12 . . 117.6(6) ?
C10 C11 H11 . . 121.2 ?
C12 C11 H11 . . 121.2 ?
N2 C12 C11 . . 124.0(6) ?
N2 C12 H12 . . 118.0 ?
C11 C12 H12 . . 118.0 ?
N3 C13 C14 . . 124.9(7) ?
N3 C13 H13 . . 117.6 ?
C14 C13 H13 . . 117.6 ?
C15 C14 C13 . . 117.9(7) ?
C15 C14 H14 . . 121.0 ?
C13 C14 H14 . . 121.0 ?
C14 C15 C16 . . 120.3(8) ?
C14 C15 H15 . . 119.9 ?
C16 C15 H15 . . 119.9 ?
C15 C16 C17 . . 118.6(7) ?
C15 C16 H16 . . 120.7 ?
C17 C16 H16 . . 120.7 ?
N3 C17 C16 . . 122.4(7) ?
N3 C17 H17 . . 118.8 ?
C16 C17 H17 . . 118.8 ?
N4 C18 C19 . . 123.0(8) ?
N4 C18 H18 . . 118.5 ?
C19 C18 H18 . . 118.5 ?
C18 C19 C20 . . 119.7(7) ?
C18 C19 H19 . . 120.2 ?
C20 C19 H19 . . 120.2 ?
C21 C20 C19 . . 117.9(7) ?
C21 C20 H20 . . 121.0 ?
C19 C20 H20 . . 121.0 ?
C20 C21 C22 . . 119.2(7) ?
C20 C21 H21 . . 120.4 ?
C22 C21 H21 . . 120.4 ?
N4 C22 C21 . . 123.7(6) ?
N4 C22 H22 . . 118.1 ?
C21 C22 H22 . . 118.1 ?
N5 C23 C24 . . 122.3(6) ?
N5 C23 H23 . . 118.9 ?
C24 C23 H23 . . 118.9 ?
C25 C24 C23 . . 119.9(7) ?
C25 C24 H24 . . 120.1 ?
C23 C24 H24 . . 120.1 ?
C24 C25 C26 . . 117.6(7) ?
C24 C25 H25 . . 121.2 ?
C26 C25 H25 . . 121.2 ?
C27 C26 C25 . . 120.1(7) ?
C27 C26 H26 . . 119.9 ?
C25 C26 H26 . . 119.9 ?
N5 C27 C26 . . 122.9(6) ?
N5 C27 H27 . . 118.6 ?
C26 C27 H27 . . 118.6 ?
O4 C28 O5 . . 125.7(5) ?
O4 C28 C29 . . 117.4(5) ?
O5 C28 C29 . . 116.9(5) ?
C28 C29 H29A . . 109.5 ?
C28 C29 H29B . . 109.5 ?
H29A C29 H29B . . 109.5 ?
C28 C29 H29C . . 109.5 ?
H29A C29 H29C . . 109.5 ?
H29B C29 H29C . . 109.5 ?
O6 C30 O7 . . 125.6(5) ?
O6 C30 C31 . . 117.4(6) ?
O7 C30 C31 . . 117.0(6) ?
C30 C31 H31A . . 109.5 ?
C30 C31 H31B . . 109.5 ?
H31A C31 H31B . . 109.5 ?
C30 C31 H31C . . 109.5 ?
H31A C31 H31C . . 109.5 ?
H31B C31 H31C . . 109.5 ?
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 O8 . 2.004(3) y
Ni1 N2 . 2.038(5) y
Ni1 O5 . 2.049(4) y
Ni1 O2 2_765 2.072(4) y
Ni1 O2 . 2.138(3) y
Ni1 O9 2_765 2.146(3) y
Ni2 O8 . 2.045(3) y
Ni2 O7 . 2.062(4) y
Ni2 O4 . 2.076(4) y
Ni2 N3 . 2.123(5) y
Ni2 N4 . 2.131(5) y
Ni2 O3 . 2.135(4) y
Ni3 O3 . 2.031(4) y
Ni3 N1 . 2.038(4) y
Ni3 O6 . 2.080(3) y
Ni3 O9 . 2.099(4) y
Ni3 O8 . 2.111(3) y
Ni3 N5 . 2.120(5) y
Mo1 O10 . 1.716(4) y
Mo1 O11 . 1.718(4) y
Mo1 O9 2_765 1.824(3) y
Mo1 O1 . 2.056(4) y
Mo1 O2 . 2.222(3) y
Mo1 O5 . 2.510(4) y
O1 C1 . 1.308(5) ?
O2 N1 . 1.413(5) ?
O2 Ni1 2_765 2.072(4) ?
O3 C7 . 1.339(6) ?
O4 C28 . 1.246(6) ?
O5 C28 . 1.271(6) ?
O6 C30 . 1.249(7) ?
O7 C30 . 1.266(7) ?
O8 H5A . 0.8500 ?
O9 Mo1 2_765 1.824(3) ?
O9 Ni1 2_765 2.146(3) ?
O12 H12C . 0.8500 ?
O12 H12D . 0.8500 ?
N1 C1 . 1.303(6) ?
N2 C8 . 1.331(7) ?
N2 C12 . 1.343(7) ?
N3 C17 . 1.322(7) ?
N3 C13 . 1.328(8) ?
N4 C22 . 1.311(8) ?
N4 C18 . 1.325(7) ?
N5 C27 . 1.326(7) ?
N5 C23 . 1.328(7) ?
C1 C2 . 1.469(7) ?
C2 C3 . 1.385(7) ?
C2 C7 . 1.425(7) ?
C3 C4 . 1.357(8) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.368(8) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.374(8) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.397(7) ?
C6 H6 . 0.9300 ?
C8 C9 . 1.377(8) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.389(9) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.369(9) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.375(8) ?
C11 H11 . 0.9300 ?
C12 H12 . 0.9300 ?
C13 C14 . 1.374(9) ?
C13 H13 . 0.9300 ?
C14 C15 . 1.316(9) ?
C14 H14 . 0.9300 ?
C15 C16 . 1.362(10) ?
C15 H15 . 0.9300 ?
C16 C17 . 1.389(9) ?
C16 H16 . 0.9300 ?
C17 H17 . 0.9300 ?
C18 C19 . 1.359(10) ?
C18 H18 . 0.9300 ?
C19 C20 . 1.368(10) ?
C19 H19 . 0.9300 ?
C20 C21 . 1.337(9) ?
C20 H20 . 0.9300 ?
C21 C22 . 1.378(9) ?
C21 H21 . 0.9300 ?
C22 H22 . 0.9300 ?
C23 C24 . 1.390(8) ?
C23 H23 . 0.9300 ?
C24 C25 . 1.347(9) ?
C24 H24 . 0.9300 ?
C25 C26 . 1.369(9) ?
C25 H25 . 0.9300 ?
C26 C27 . 1.363(9) ?
C26 H26 . 0.9300 ?
C27 H27 . 0.9300 ?
C28 C29 . 1.494(7) ?
C29 H29A . 0.9600 ?
C29 H29B . 0.9600 ?
C29 H29C . 0.9600 ?
C30 C31 . 1.493(7) ?
C31 H31A . 0.9600 ?
C31 H31B . 0.9600 ?
C31 H31C . 0.9600 ?
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
C31 H31A O12 . 0.96 2.41 3.064(13) 125.3
C29 H29B O10 . 0.96 2.57 3.304(7) 133.6
C23 H23 O12 . 0.93 2.50 3.353(11) 151.8
C22 H22 O4 . 0.93 2.40 2.999(7) 122.3
C18 H18 O7 . 0.93 2.31 2.932(9) 123.9
C16 H16 O10 1_455 0.93 2.52 3.397(8) 156.8
C16 H16 O1 1_455 0.93 2.60 3.343(8) 137.2
C12 H12 O11 2_765 0.93 2.56 3.436(7) 156.3
C11 H11 O11 1_455 0.93 2.59 3.444(7) 152.6
C9 H9 O12 1_545 0.93 2.37 3.218(11) 152.2
C8 H8 O5 . 0.93 2.65 3.182(7) 116.7
O12 H12D O10 2_765 0.85 2.09 2.924(10) 168.7
O12 H12C O6 . 0.85 1.93 2.770(11) 168.9
O8 H5A O11 2_765 0.85 2.15 2.907(5) 149.0
C9 H9 O12 1_545 0.93 2.37 3.218(11) 152.2
C25 H25 O10 1_565 0.93 2.47 3.138(9) 129.2
C16 H16 O10 1_455 0.93 2.52 3.397(8) 156.8
C11 H11 O11 1_455 0.93 2.59 3.444(7) 152.6
O8 H5A O11 2_765 0.85 2.15 2.907(5) 149.0
O12 H12D O10 2_765 0.85 2.09 2.924(10) 168.7
O12 H12C O6 . 0.85 1.93 2.770(11) 168.9
