#------------------------------------------------------------------------------
#$Date: 2017-02-04 16:03:33 +0200 (Sat, 04 Feb 2017) $
#$Revision: 191671 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/16/7041662.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7041662
loop_
_publ_author_name
'Wendt, M.'
'Polzin, P.'
'van Leusen, J.'
'Näther, C'
'Kögerler, P'
'Bensch, W.'
_publ_section_title
;
 In situ ligand exchange-mediated 0D/1D transformation of a
 polyoxovanadate.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1618
_journal_page_last               1623
_journal_paper_doi               10.1039/c6dt04412c
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety
'V15Sb6O42, NiC4H16N4, NiC36H24N6, C12H8N2, C2H8N2, H2O'
_chemical_formula_sum            'C76 H104 N16 Ni3 O62 Sb6 V15'
_chemical_formula_weight         3904.48
_chemical_name_common            '[Ni(phen)3]2{[Ni(en)2]V15Sb6O42(H2O)}x19H2O'
_chemical_name_systematic
;
 '[Ni(C12H8N2)3]2{[Ni(C2N2H8)2]V15Sb6O42(H2O)} x 19H2O'
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2016-09-13 deposited with the CCDC.
2017-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.117(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.2523(12)
_cell_length_b                   31.159(2)
_cell_length_c                   18.7101(11)
_cell_measurement_reflns_used    65692
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.004
_cell_measurement_theta_min      2.321
_cell_volume                     12381.4(13)
_computing_cell_refinement       'STOE-IPDS Program Package'
_computing_data_collection       'STOE-IPDS Program Package'
_computing_data_reduction        'STOE-IPDS Program Package'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            65694
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.004
_diffrn_reflns_theta_min         2.321
_exptl_absorpt_coefficient_mu    2.898
_exptl_absorpt_correction_T_max  0.7241
_exptl_absorpt_correction_T_min  0.5232
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape (STOE & CIE, 2014)'
_exptl_crystal_colour            brown-green
_exptl_crystal_density_diffrn    2.095
_exptl_crystal_description       block
_exptl_crystal_F_000             7612
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.344
_refine_diff_density_min         -1.330
_refine_diff_density_rms         0.158
_refine_ls_extinction_coef       0.000276(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         13452
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0612P)²+35.0216P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11790
_reflns_number_total             13452
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt04412c2.cif
_cod_data_source_block           neu
_cod_depositor_comments          'Adding full bibliography for 7041662.cif.'
_cod_original_cell_volume        12381.2(14)
_cod_database_code               7041662
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_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'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Sb1 Sb 0.28473(2) 0.21538(2) 0.32176(2) 0.01276(7) Uani 1 1 d . . .
Sb2 Sb 0.39459(2) 0.13647(2) 0.37878(2) 0.01178(7) Uani 1 1 d . . .
Sb3 Sb 0.46528(2) 0.39567(2) 0.33388(2) 0.01351(7) Uani 1 1 d . . .
V1 V 0.36096(3) 0.31219(2) 0.33627(3) 0.00785(11) Uani 1 1 d . . .
V2 V 0.5000 0.12381(2) 0.2500 0.00825(15) Uani 1 2 d S T P
V3 V 0.34130(3) 0.25410(2) 0.16033(3) 0.00634(11) Uani 1 1 d . . .
V4 V 0.42187(3) 0.24861(2) 0.43731(3) 0.00728(11) Uani 1 1 d . . .
V5 V 0.53381(3) 0.18861(2) 0.41912(3) 0.00650(11) Uani 1 1 d . . .
V6 V 0.52341(3) 0.30744(2) 0.42294(3) 0.00618(11) Uani 1 1 d . . .
V7 V 0.37889(3) 0.16117(2) 0.18588(3) 0.00757(11) Uani 1 1 d . . .
V8 V 0.38196(3) 0.33959(2) 0.18504(3) 0.00828(11) Uani 1 1 d . . .
O1 O 0.35096(11) 0.25161(7) 0.36653(12) 0.0112(5) Uani 1 1 d . . .
O2 O 0.33128(12) 0.20797(7) 0.23293(12) 0.0121(5) Uani 1 1 d . . .
O3 O 0.31236(12) 0.16224(8) 0.36626(13) 0.0152(5) Uani 1 1 d . . .
O4 O 0.41504(12) 0.14141(8) 0.27870(12) 0.0137(5) Uani 1 1 d . . .
O5 O 0.43916(11) 0.18825(7) 0.41001(12) 0.0108(5) Uani 1 1 d . . .
O6 O 0.40860(12) 0.35674(8) 0.28344(12) 0.0123(5) Uani 1 1 d . . .
O7 O 0.5000 0.42226(11) 0.2500 0.0150(7) Uani 1 2 d S T P
O8 O 0.53280(11) 0.35491(8) 0.35042(12) 0.0116(5) Uani 1 1 d . . .
O9 O 0.34066(11) 0.29527(7) 0.23864(12) 0.0102(4) Uani 1 1 d . . .
O10 O 0.43300(11) 0.30666(7) 0.40133(12) 0.0095(4) Uani 1 1 d . . .
O11 O 0.30406(12) 0.33809(9) 0.37149(13) 0.0180(5) Uani 1 1 d . . .
O12 O 0.53483(11) 0.14778(7) 0.34004(12) 0.0096(4) Uani 1 1 d . . .
O13 O 0.5000 0.07255(11) 0.2500 0.0214(8) Uani 1 2 d S T P
O14 O 0.39662(11) 0.29469(7) 0.11796(12) 0.0101(4) Uani 1 1 d . . .
O15 O 0.38836(11) 0.20840(7) 0.12055(12) 0.0096(4) Uani 1 1 d . . .
O16 O 0.27540(11) 0.25781(8) 0.11199(12) 0.0115(5) Uani 1 1 d . . .
O17 O 0.39555(13) 0.25077(8) 0.51827(13) 0.0150(5) Uani 1 1 d . . .
O18 O 0.51156(11) 0.24735(7) 0.43978(12) 0.0104(5) Uani 1 1 d . . .
O19 O 0.55293(12) 0.16399(8) 0.49297(12) 0.0149(5) Uani 1 1 d . . .
O20 O 0.53593(12) 0.33072(8) 0.49951(12) 0.0134(5) Uani 1 1 d . . .
O21 O 0.32957(12) 0.12705(8) 0.15162(13) 0.0160(5) Uani 1 1 d . . .
O22 O 0.32986(12) 0.37296(8) 0.15289(13) 0.0166(5) Uani 1 1 d . . .
Ni1 Ni 0.2500 0.2500 0.0000 0.00998(12) Uani 1 2 d S . P
N1 N 0.28438(15) 0.18702(10) 0.00459(16) 0.0163(6) Uani 1 1 d . . .
H1N1 H 0.3021 0.1801 -0.0374 0.020 Uiso 1 1 calc R U .
H2N1 H 0.3143 0.1846 0.0404 0.020 Uiso 1 1 calc R U .
C1 C 0.2310(2) 0.15767(12) 0.0180(2) 0.0229(8) Uani 1 1 d . . .
H1A H 0.2468 0.1308 0.0406 0.027 Uiso 1 1 calc R U .
H1B H 0.2087 0.1502 -0.0277 0.027 Uiso 1 1 calc R U .
C2 C 0.18618(19) 0.17996(13) 0.0670(2) 0.0231(8) Uani 1 1 d . . .
H2A H 0.1485 0.1619 0.0735 0.028 Uiso 1 1 calc R U .
H2B H 0.2070 0.1849 0.1145 0.028 Uiso 1 1 calc R U .
N2 N 0.16783(15) 0.22124(10) 0.03408(16) 0.0173(6) Uani 1 1 d . . .
H1N2 H 0.1490 0.2383 0.0665 0.021 Uiso 1 1 calc R U .
H2N2 H 0.1404 0.2169 -0.0037 0.021 Uiso 1 1 calc R U .
Ni2 Ni 0.24406(2) 0.46939(2) 0.48926(2) 0.01539(10) Uani 1 1 d . . .
N11 N 0.22156(16) 0.47292(10) 0.59865(17) 0.0193(6) Uani 1 1 d . . .
N12 N 0.31107(15) 0.42752(11) 0.53535(17) 0.0190(6) Uani 1 1 d . . .
C11 C 0.1762(2) 0.49522(14) 0.6299(2) 0.0280(9) Uani 1 1 d . . .
H11 H 0.1541 0.5164 0.6025 0.034 Uiso 1 1 calc R U .
C12 C 0.1596(2) 0.48905(15) 0.7003(2) 0.0323(10) Uani 1 1 d . . .
H12 H 0.1265 0.5053 0.7199 0.039 Uiso 1 1 calc R U .
C13 C 0.1920(2) 0.45883(14) 0.7413(2) 0.0278(9) Uani 1 1 d . . .
H13 H 0.1807 0.4537 0.7892 0.033 Uiso 1 1 calc R U .
C14 C 0.24126(19) 0.43577(12) 0.7124(2) 0.0205(8) Uani 1 1 d . . .
C15 C 0.2787(2) 0.40522(14) 0.7517(2) 0.0253(8) Uani 1 1 d . . .
H15 H 0.2708 0.4001 0.8006 0.030 Uiso 1 1 calc R U .
C16 C 0.3251(2) 0.38348(15) 0.7203(2) 0.0284(9) Uani 1 1 d . . .
H16 H 0.3496 0.3635 0.7477 0.034 Uiso 1 1 calc R U .
C17 C 0.33828(19) 0.38994(14) 0.6462(2) 0.0246(8) Uani 1 1 d . . .
C18 C 0.3845(2) 0.36681(16) 0.6100(3) 0.0335(10) Uani 1 1 d . . .
H18 H 0.4100 0.3463 0.6349 0.040 Uiso 1 1 calc R U .
C19 C 0.3924(2) 0.37418(16) 0.5381(3) 0.0337(10) Uani 1 1 d . . .
H19 H 0.4231 0.3587 0.5130 0.040 Uiso 1 1 calc R U .
C20 C 0.3547(2) 0.40470(14) 0.5028(2) 0.0248(8) Uani 1 1 d . . .
H20 H 0.3603 0.4095 0.4533 0.030 Uiso 1 1 calc R U .
C21 C 0.30275(18) 0.41994(12) 0.6057(2) 0.0173(7) Uani 1 1 d . . .
C22 C 0.25355(17) 0.44365(11) 0.63943(19) 0.0154(7) Uani 1 1 d . . .
N31 N 0.18170(15) 0.41899(10) 0.46914(16) 0.0170(6) Uani 1 1 d . . .
N32 N 0.16366(17) 0.50391(10) 0.45864(17) 0.0211(7) Uani 1 1 d . . .
C31 C 0.1932(2) 0.37679(12) 0.4710(2) 0.0215(8) Uani 1 1 d . . .
H31 H 0.2336 0.3672 0.4876 0.026 Uiso 1 1 calc R U .
C32 C 0.1484(2) 0.34631(13) 0.4499(2) 0.0280(9) Uani 1 1 d . . .
H32 H 0.1585 0.3166 0.4509 0.034 Uiso 1 1 calc R U .
C33 C 0.0897(2) 0.35983(15) 0.4275(2) 0.0336(11) Uani 1 1 d . . .
H33 H 0.0583 0.3394 0.4141 0.040 Uiso 1 1 calc R U .
C34 C 0.0758(2) 0.40336(16) 0.4244(2) 0.0289(9) Uani 1 1 d . . .
C35 C 0.0159(2) 0.4204(2) 0.4014(3) 0.0473(14) Uani 1 1 d . . .
H35 H -0.0176 0.4012 0.3889 0.057 Uiso 1 1 calc R U .
C36 C 0.0060(3) 0.4631(2) 0.3972(3) 0.0515(15) Uani 1 1 d . . .
H36 H -0.0339 0.4735 0.3805 0.062 Uiso 1 1 calc R U .
C37 C 0.0547(2) 0.49333(18) 0.4177(3) 0.0373(11) Uani 1 1 d . . .
C38 C 0.0464(3) 0.53823(19) 0.4163(3) 0.0480(15) Uani 1 1 d . . .
H38 H 0.0072 0.5503 0.4007 0.058 Uiso 1 1 calc R U .
C39 C 0.0949(3) 0.56410(16) 0.4373(3) 0.0487(16) Uani 1 1 d . . .
H39 H 0.0893 0.5943 0.4386 0.058 Uiso 1 1 calc R U .
C40 C 0.1544(3) 0.54587(14) 0.4576(3) 0.0360(11) Uani 1 1 d . . .
H40 H 0.1884 0.5644 0.4707 0.043 Uiso 1 1 calc R U .
C41 C 0.11441(19) 0.47792(13) 0.4406(2) 0.0217(8) Uani 1 1 d . . .
C42 C 0.12414(18) 0.43223(13) 0.44503(19) 0.0194(7) Uani 1 1 d . . .
N51 N 0.27532(16) 0.46493(10) 0.38357(17) 0.0193(6) Uani 1 1 d . . .
N52 N 0.31188(16) 0.51889(11) 0.48829(18) 0.0217(7) Uani 1 1 d . . .
C51 C 0.2551(2) 0.43901(14) 0.3311(2) 0.0264(9) Uani 1 1 d . . .
H51 H 0.2198 0.4212 0.3389 0.032 Uiso 1 1 calc R U .
C52 C 0.2838(2) 0.43681(16) 0.2646(2) 0.0353(11) Uani 1 1 d . . .
H52 H 0.2678 0.4179 0.2285 0.042 Uiso 1 1 calc R U .
C53 C 0.3347(2) 0.46202(17) 0.2525(2) 0.0347(11) Uani 1 1 d . . .
H53 H 0.3549 0.4605 0.2081 0.042 Uiso 1 1 calc R U .
C54 C 0.3570(2) 0.49027(14) 0.3059(2) 0.0258(9) Uani 1 1 d . . .
C55 C 0.4104(3) 0.51763(17) 0.2980(3) 0.0396(12) Uani 1 1 d . . .
H55 H 0.4323 0.5173 0.2547 0.048 Uiso 1 1 calc R U .
C56 C 0.4298(3) 0.54397(17) 0.3518(3) 0.0446(13) Uani 1 1 d . . .
H56 H 0.4652 0.5620 0.3453 0.054 Uiso 1 1 calc R U .
C57 C 0.3985(2) 0.54538(13) 0.4184(3) 0.0323(10) Uani 1 1 d . . .
C58 C 0.4167(2) 0.57219(15) 0.4759(4) 0.0461(14) Uani 1 1 d . . .
H58 H 0.4526 0.5902 0.4727 0.055 Uiso 1 1 calc R U .
C59 C 0.3828(3) 0.57229(17) 0.5360(4) 0.0488(15) Uani 1 1 d . . .
H59 H 0.3949 0.5904 0.5750 0.059 Uiso 1 1 calc R U .
C60 C 0.3298(2) 0.54547(16) 0.5405(3) 0.0351(11) Uani 1 1 d . . .
H60 H 0.3060 0.5464 0.5825 0.042 Uiso 1 1 calc R U .
C61 C 0.34555(19) 0.51910(12) 0.4276(2) 0.0225(8) Uani 1 1 d . . .
C62 C 0.32531(19) 0.49067(12) 0.3706(2) 0.0206(8) Uani 1 1 d . . .
O31 O 0.53444(18) 0.32236(13) 0.64605(17) 0.0434(9) Uani 1 1 d . . .
H1O H 0.5201 0.2972 0.6449 0.065 Uiso 1 1 d R U .
H2O H 0.5420 0.3266 0.6029 0.065 Uiso 1 1 d R U .
O32 O 0.3833(2) 0.28370(13) 0.7541(2) 0.0493(10) Uani 1 1 d . . .
H3O H 0.4091 0.2921 0.7863 0.074 Uiso 1 1 d R U .
H4O H 0.3635 0.2664 0.7794 0.074 Uiso 1 1 d R U .
O33 O 0.4587(2) 0.25099(13) 0.64785(19) 0.0479(10) Uani 1 1 d . . .
H5O H 0.4333 0.2454 0.6136 0.072 Uiso 1 1 d R U .
H6O H 0.4426 0.2676 0.6774 0.072 Uiso 1 1 d R U .
O34 O 0.33057(17) 0.21661(12) 0.8179(2) 0.0422(9) Uani 1 1 d . . .
H7O H 0.3576 0.2041 0.8444 0.063 Uiso 1 1 d R U .
H8O H 0.3009 0.2262 0.8417 0.063 Uiso 1 1 d R U .
O35 O 0.55200(18) 0.18906(13) 0.63537(19) 0.0445(9) Uani 1 1 d . . .
H9O H 0.5484 0.1727 0.5998 0.067 Uiso 1 1 d R U .
H10O H 0.5314 0.2115 0.6263 0.067 Uiso 1 1 d R U .
O36 O 0.3054(2) 0.15162(17) 0.7202(3) 0.0741(17) Uani 1 1 d . . .
H11O H 0.3062 0.1761 0.7388 0.111 Uiso 1 1 d R U .
H12O H 0.2720 0.1571 0.6966 0.111 Uiso 1 1 d R U .
O37 O 0.3872(2) 0.08871(15) 0.7677(3) 0.0626(12) Uani 1 1 d . . .
H13O H 0.4209 0.1021 0.7615 0.094 Uiso 1 1 d R U .
H14O H 0.3663 0.1082 0.7468 0.094 Uiso 1 1 d R U .
O38 O 0.5000 0.1404(2) 0.7500 0.0493(14) Uani 1 2 d S T P
H15O H 0.4828 0.1592 0.7748 0.074 Uiso 1 1 d R U .
O39 O 0.5000 0.38480(19) 0.7500 0.0531(15) Uani 1 2 d S T P
H16O H 0.4868 0.3685 0.7834 0.080 Uiso 1 1 d R U .
O40 O 0.1962(3) 0.3914(2) 0.1063(3) 0.0490(15) Uani 0.7 1 d . . P
O40' O 0.1451(12) 0.3954(7) 0.0867(11) 0.093(6) Uani 0.3 1 d . . P
O41 O 0.2251(3) 0.2136(2) 0.4666(3) 0.077(2) Uani 0.8 1 d . . P
O42 O 0.5000 0.2471(4) 0.2500 0.084(8) Uani 0.4 2 d S T P
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'
V V 0.3005 0.5294 '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'
Sb Sb -0.5866 1.5461 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O3 Sb1 O1 96.14(10) . .
O3 Sb1 O2 96.22(10) . .
O1 Sb1 O2 93.01(10) . .
O3 Sb2 O4 94.81(10) . .
O3 Sb2 O5 96.90(10) . .
O4 Sb2 O5 95.72(10) . .
O6 Sb3 O8 96.41(10) . .
O6 Sb3 O7 96.99(9) . .
O8 Sb3 O7 96.17(9) . .
O11 V1 O10 112.10(12) . .
O11 V1 O9 112.17(12) . .
O10 V1 O9 135.72(10) . .
O11 V1 O1 105.61(13) . .
O10 V1 O1 79.96(9) . .
O9 V1 O1 89.29(10) . .
O11 V1 O6 104.79(13) . .
O10 V1 O6 88.25(10) . .
O9 V1 O6 79.74(9) . .
O1 V1 O6 149.60(11) . .
O11 V1 V4 112.65(10) . .
O10 V1 V4 39.54(7) . .
O9 V1 V4 119.41(7) . .
O1 V1 V4 40.53(7) . .
O6 V1 V4 123.73(7) . .
O11 V1 V8 112.46(10) . .
O10 V1 V8 118.55(7) . .
O9 V1 V8 39.10(7) . .
O1 V1 V8 124.07(7) . .
O6 V1 V8 40.72(6) . .
V4 V1 V8 134.89(2) . .
O13 V2 O12 112.37(7) . 2_655
O13 V2 O12 112.36(7) . .
O12 V2 O12 135.27(14) 2_655 .
O13 V2 O4 106.08(8) . 2_655
O12 V2 O4 88.89(10) 2_655 2_655
O12 V2 O4 78.97(10) . 2_655
O13 V2 O4 106.08(8) . .
O12 V2 O4 78.97(10) 2_655 .
O12 V2 O4 88.89(10) . .
O4 V2 O4 147.84(15) 2_655 .
O13 V2 V7 112.581(16) . 2_655
O12 V2 V7 118.77(7) 2_655 2_655
O12 V2 V7 39.32(7) . 2_655
O4 V2 V7 39.79(7) 2_655 2_655
O4 V2 V7 123.76(7) . 2_655
O13 V2 V7 112.581(17) . .
O12 V2 V7 39.32(7) 2_655 .
O12 V2 V7 118.78(7) . .
O4 V2 V7 123.76(7) 2_655 .
O4 V2 V7 39.79(7) . .
V7 V2 V7 134.84(3) 2_655 .
O16 V3 O15 106.63(11) . .
O16 V3 O14 104.43(11) . .
O15 V3 O14 89.58(10) . .
O16 V3 O9 109.78(11) . .
O15 V3 O9 143.48(10) . .
O14 V3 O9 84.15(10) . .
O16 V3 O2 108.37(11) . .
O15 V3 O2 78.37(10) . .
O14 V3 O2 147.06(10) . .
O9 V3 O2 87.62(10) . .
O16 V3 V8 105.81(9) . .
O15 V3 V8 127.19(8) . .
O14 V3 V8 42.23(7) . .
O9 V3 V8 43.00(7) . .
O2 V3 V8 127.31(7) . .
O16 V3 V7 111.57(9) . .
O15 V3 V7 37.89(7) . .
O14 V3 V7 122.14(7) . .
O9 V3 V7 121.24(7) . .
O2 V3 V7 40.51(7) . .
V8 V3 V7 142.55(2) . .
O17 V4 O18 110.76(12) . .
O17 V4 O10 109.39(11) . .
O18 V4 O10 83.87(10) . .
O17 V4 O1 109.95(12) . .
O18 V4 O1 139.16(11) . .
O10 V4 O1 79.82(9) . .
O17 V4 O5 110.49(11) . .
O18 V4 O5 78.01(10) . .
O10 V4 O5 139.85(10) . .
O1 V4 O5 90.94(9) . .
O17 V4 V6 110.29(9) . .
O18 V4 V6 41.90(7) . .
O10 V4 V6 42.97(7) . .
O1 V4 V6 117.93(7) . .
O5 V4 V6 115.87(7) . .
O17 V4 V1 113.72(9) . .
O18 V4 V1 115.91(7) . .
O10 V4 V1 39.07(7) . .
O1 V4 V1 40.86(7) . .
O5 V4 V1 122.88(7) . .
V6 V4 V1 80.00(2) . .
O17 V4 V5 115.02(9) . .
O18 V4 V5 37.59(7) . .
O10 V4 V5 115.14(7) . .
O1 V4 V5 122.24(7) . .
O5 V4 V5 40.51(7) . .
V6 V4 V5 77.74(2) . .
V1 V4 V5 130.83(2) . .
O19 V5 O18 109.47(11) . .
O19 V5 O15 106.66(12) . 2_655
O18 V5 O15 89.64(10) . 2_655
O19 V5 O12 109.20(11) . .
O18 V5 O12 141.11(10) . .
O15 V5 O12 83.32(10) 2_655 .
O19 V5 O5 106.75(12) . .
O18 V5 O5 76.76(10) . .
O15 V5 O5 146.47(10) 2_655 .
O12 V5 O5 88.35(10) . .
O19 V5 V7 107.09(10) . 2_655
O18 V5 V7 125.85(8) . 2_655
O15 V5 V7 41.70(7) 2_655 2_655
O12 V5 V7 42.64(7) . 2_655
O5 V5 V7 127.40(7) . 2_655
O19 V5 V4 111.51(10) . .
O18 V5 V4 36.96(7) . .
O15 V5 V4 121.80(7) 2_655 .
O12 V5 V4 120.92(7) . .
O5 V5 V4 39.89(7) . .
V7 V5 V4 141.38(2) 2_655 .
O20 V6 O18 108.08(11) . .
O20 V6 O14 108.94(12) . 2_655
O18 V6 O14 89.26(10) . 2_655
O20 V6 O10 108.52(12) . .
O18 V6 O10 83.53(10) . .
O14 V6 O10 142.25(10) 2_655 .
O20 V6 O8 104.42(11) . .
O18 V6 O8 147.32(10) . .
O14 V6 O8 76.97(10) 2_655 .
O10 V6 O8 89.48(10) . .
O20 V6 V4 107.74(9) . .
O18 V6 V4 41.59(7) . .
O14 V6 V4 125.82(7) 2_655 .
O10 V6 V4 42.93(7) . .
O8 V6 V4 128.85(7) . .
O20 V6 V8 110.23(9) . 2_655
O18 V6 V8 121.34(8) . 2_655
O14 V6 V8 36.77(7) 2_655 2_655
O10 V6 V8 122.15(7) . 2_655
O8 V6 V8 40.24(7) . 2_655
V4 V6 V8 142.00(2) . 2_655
O21 V7 O15 109.47(11) . .
O21 V7 O12 111.25(12) . 2_655
O15 V7 O12 83.40(10) . 2_655
O21 V7 O4 111.80(12) . .
O15 V7 O4 138.62(10) . .
O12 V7 O4 79.26(10) 2_655 .
O21 V7 O2 108.94(12) . .
O15 V7 O2 77.80(10) . .
O12 V7 O2 139.34(10) 2_655 .
O4 V7 O2 91.55(10) . .
O21 V7 V5 110.53(10) . 2_655
O15 V7 V5 41.97(7) . 2_655
O12 V7 V5 42.46(7) 2_655 2_655
O4 V7 V5 116.97(8) . 2_655
O2 V7 V5 115.68(7) . 2_655
O21 V7 V2 115.78(10) . .
O15 V7 V2 115.91(7) . .
O12 V7 V2 39.41(6) 2_655 .
O4 V7 V2 40.00(7) . .
O2 V7 V2 122.85(7) . .
V5 V7 V2 79.927(18) 2_655 .
O21 V7 V3 113.80(10) . .
O15 V7 V3 37.40(7) . .
O12 V7 V3 114.04(7) 2_655 .
O4 V7 V3 121.88(8) . .
O2 V7 V3 40.43(7) . .
V5 V7 V3 77.41(2) 2_655 .
V2 V7 V3 130.01(2) . .
O22 V8 O14 110.60(11) . .
O22 V8 O9 109.50(12) . .
O14 V8 O9 84.61(10) . .
O22 V8 O6 109.90(12) . .
O14 V8 O6 139.46(10) . .
O9 V8 O6 80.24(10) . .
O22 V8 O8 109.71(12) . 2_655
O14 V8 O8 77.67(10) . 2_655
O9 V8 O8 140.53(10) . 2_655
O6 V8 O8 90.72(10) . 2_655
O22 V8 V3 110.06(10) . .
O14 V8 V3 42.38(7) . .
O9 V8 V3 43.32(7) . .
O6 V8 V3 118.73(7) . .
O8 V8 V3 116.28(7) 2_655 .
O22 V8 V1 114.15(10) . .
O14 V8 V1 116.34(7) . .
O9 V8 V1 39.07(7) . .
O6 V8 V1 41.25(7) . .
O8 V8 V1 123.06(7) 2_655 .
V3 V8 V1 80.30(2) . .
O22 V8 V6 114.88(9) . 2_655
O14 V8 V6 37.18(7) . 2_655
O9 V8 V6 115.38(7) . 2_655
O6 V8 V6 121.89(8) . 2_655
O8 V8 V6 40.54(7) 2_655 2_655
V3 V8 V6 77.83(2) . 2_655
V1 V8 V6 130.59(2) . 2_655
Sb1 O1 V4 140.89(12) . .
Sb1 O1 V1 120.46(11) . .
V4 O1 V1 98.60(10) . .
Sb1 O2 V3 123.86(12) . .
Sb1 O2 V7 137.08(12) . .
V3 O2 V7 99.06(10) . .
Sb2 O3 Sb1 131.86(13) . .
Sb2 O4 V7 141.22(14) . .
Sb2 O4 V2 118.55(11) . .
V7 O4 V2 100.20(11) . .
Sb2 O5 V4 140.17(13) . .
Sb2 O5 V5 120.21(12) . .
V4 O5 V5 99.61(10) . .
Sb3 O6 V8 140.89(14) . .
Sb3 O6 V1 120.81(11) . .
V8 O6 V1 98.02(10) . .
Sb3 O7 Sb3 129.54(18) 2_655 .
Sb3 O8 V8 140.93(13) . 2_655
Sb3 O8 V6 119.80(12) . .
V8 O8 V6 99.22(10) 2_655 .
V1 O9 V8 101.83(11) . .
V1 O9 V3 151.92(13) . .
V8 O9 V3 93.68(10) . .
V1 O10 V4 101.39(10) . .
V1 O10 V6 152.07(13) . .
V4 O10 V6 94.10(10) . .
V5 O12 V7 94.90(10) . 2_655
V5 O12 V2 152.16(13) . .
V7 O12 V2 101.27(10) 2_655 .
V8 O14 V3 95.39(11) . .
V8 O14 V6 106.06(11) . 2_655
V3 O14 V6 149.48(13) . 2_655
V3 O15 V7 104.71(11) . .
V3 O15 V5 148.68(13) . 2_655
V7 O15 V5 96.34(10) . 2_655
V3 O16 Ni1 134.76(14) . .
V4 O18 V6 96.51(10) . .
V4 O18 V5 105.46(11) . .
V6 O18 V5 149.02(14) . .
N2 Ni1 N2 180.0 . 7
N2 Ni1 N1 96.92(13) . 7
N2 Ni1 N1 83.08(13) 7 7
N2 Ni1 N1 83.08(13) . .
N2 Ni1 N1 96.92(13) 7 .
N1 Ni1 N1 180.0 7 .
N2 Ni1 O16 86.21(10) . .
N2 Ni1 O16 93.80(10) 7 .
N1 Ni1 O16 90.49(10) 7 .
N1 Ni1 O16 89.51(10) . .
N2 Ni1 O16 93.79(10) . 7
N2 Ni1 O16 86.20(10) 7 7
N1 Ni1 O16 89.51(10) 7 7
N1 Ni1 O16 90.49(10) . 7
O16 Ni1 O16 180.00(13) . 7
C1 N1 Ni1 108.4(2) . .
N1 C1 C2 108.7(3) . .
N2 C2 C1 108.0(3) . .
C2 N2 Ni1 107.0(2) . .
N31 Ni2 N32 80.17(13) . .
N31 Ni2 N12 91.33(13) . .
N32 Ni2 N12 167.00(13) . .
N31 Ni2 N52 168.64(13) . .
N32 Ni2 N52 100.01(13) . .
N12 Ni2 N52 90.26(13) . .
N31 Ni2 N51 90.07(12) . .
N32 Ni2 N51 93.42(13) . .
N12 Ni2 N51 96.43(13) . .
N52 Ni2 N51 78.57(13) . .
N31 Ni2 N11 92.81(13) . .
N32 Ni2 N11 91.53(13) . .
N12 Ni2 N11 78.99(13) . .
N52 Ni2 N11 98.54(13) . .
N51 Ni2 N11 174.64(13) . .
C11 N11 C22 117.2(3) . .
C11 N11 Ni2 129.8(3) . .
C22 N11 Ni2 112.4(2) . .
C20 N12 C21 117.9(3) . .
C20 N12 Ni2 128.2(3) . .
C21 N12 Ni2 113.4(2) . .
N11 C11 C12 123.7(4) . .
C13 C12 C11 118.8(4) . .
C12 C13 C14 120.1(4) . .
C13 C14 C22 116.8(4) . .
C13 C14 C15 123.8(4) . .
C22 C14 C15 119.4(4) . .
C16 C15 C14 120.9(4) . .
C15 C16 C17 121.4(4) . .
C21 C17 C18 116.7(4) . .
C21 C17 C16 119.5(4) . .
C18 C17 C16 123.7(4) . .
C19 C18 C17 119.7(4) . .
C18 C19 C20 119.1(4) . .
N12 C20 C19 123.0(4) . .
N12 C21 C17 123.5(4) . .
N12 C21 C22 117.2(3) . .
C17 C21 C22 119.2(3) . .
N11 C22 C14 123.4(3) . .
N11 C22 C21 117.0(3) . .
C14 C22 C21 119.5(3) . .
C31 N31 C42 118.1(3) . .
C31 N31 Ni2 128.5(3) . .
C42 N31 Ni2 113.1(2) . .
C40 N32 C41 118.3(4) . .
C40 N32 Ni2 129.5(3) . .
C41 N32 Ni2 112.2(2) . .
N31 C31 C32 122.8(4) . .
C33 C32 C31 118.9(4) . .
C32 C33 C34 120.2(4) . .
C33 C34 C42 117.5(4) . .
C33 C34 C35 124.0(5) . .
C42 C34 C35 118.5(5) . .
C36 C35 C34 121.1(5) . .
C35 C36 C37 121.4(5) . .
C41 C37 C38 117.0(5) . .
C41 C37 C36 119.2(5) . .
C38 C37 C36 123.8(5) . .
C39 C38 C37 119.4(5) . .
C38 C39 C40 119.9(5) . .
N32 C40 C39 121.9(5) . .
N32 C41 C37 123.4(4) . .
N32 C41 C42 117.9(3) . .
C37 C41 C42 118.7(4) . .
N31 C42 C34 122.5(4) . .
N31 C42 C41 116.5(3) . .
C34 C42 C41 120.9(4) . .
C51 N51 C62 117.3(4) . .
C51 N51 Ni2 128.8(3) . .
C62 N51 Ni2 113.8(2) . .
C60 N52 C61 117.7(4) . .
C60 N52 Ni2 128.9(3) . .
C61 N52 Ni2 112.9(2) . .
N51 C51 C52 123.0(4) . .
C53 C52 C51 119.4(4) . .
C52 C53 C54 119.5(4) . .
C53 C54 C62 117.4(4) . .
C53 C54 C55 123.3(4) . .
C62 C54 C55 119.3(4) . .
C56 C55 C54 120.5(4) . .
C55 C56 C57 121.7(4) . .
C58 C57 C61 116.8(4) . .
C58 C57 C56 124.0(4) . .
C61 C57 C56 119.2(4) . .
C59 C58 C57 119.7(4) . .
C58 C59 C60 119.9(5) . .
N52 C60 C59 122.4(5) . .
N52 C61 C57 123.4(4) . .
N52 C61 C62 117.5(3) . .
C57 C61 C62 119.0(4) . .
N51 C62 C54 123.4(4) . .
N51 C62 C61 116.3(3) . .
C54 C62 C61 120.3(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb1 O3 1.935(3) .
Sb1 O1 1.967(2) .
Sb1 O2 1.979(2) .
Sb2 O3 1.930(3) .
Sb2 O4 1.944(2) .
Sb2 O5 1.949(2) .
Sb3 O6 1.931(2) .
Sb3 O8 1.933(2) .
Sb3 O7 1.9442(15) .
V1 O11 1.614(3) .
V1 O10 1.928(2) .
V1 O9 1.935(2) .
V1 O1 1.984(2) .
V1 O6 2.001(3) .
V1 V4 2.9990(7) .
V1 V8 3.0044(8) .
V2 O13 1.597(4) .
V2 O12 1.962(2) 2_655
V2 O12 1.962(2) .
V2 O4 1.980(3) 2_655
V2 O4 1.980(3) .
V2 V7 3.0316(6) 2_655
V2 V7 3.0316(6) .
V3 O16 1.643(2) .
V3 O15 1.907(2) .
V3 O14 1.918(2) .
V3 O9 1.948(2) .
V3 O2 1.994(2) .
V3 V8 2.8330(8) .
V3 V7 3.0369(8) .
V4 O17 1.635(2) .
V4 O18 1.905(2) .
V4 O10 1.948(2) .
V4 O1 1.971(2) .
V4 O5 1.987(2) .
V4 V6 2.8519(8) .
V4 V5 3.0547(8) .
V5 O19 1.619(2) .
V5 O18 1.933(2) .
V5 O15 1.938(2) 2_655
V5 O12 1.952(2) .
V5 O5 2.012(2) .
V5 V7 2.8812(8) 2_655
V6 O20 1.619(2) .
V6 O18 1.917(2) .
V6 O14 1.931(2) 2_655
V6 O10 1.949(2) .
V6 O8 2.022(2) .
V6 V8 3.0707(8) 2_655
V7 O21 1.610(2) .
V7 O15 1.928(2) .
V7 O12 1.959(2) 2_655
V7 O4 1.971(2) .
V7 O2 1.998(2) .
V7 V5 2.8811(8) 2_655
V8 O22 1.619(2) .
V8 O14 1.913(2) .
V8 O9 1.936(2) .
V8 O6 1.980(2) .
V8 O8 2.010(3) 2_655
V8 V6 3.0706(8) 2_655
O7 Sb3 1.9441(15) 2_655
O8 V8 2.009(3) 2_655
O12 V7 1.959(2) 2_655
O14 V6 1.931(2) 2_655
O15 V5 1.938(2) 2_655
O16 Ni1 2.158(2) .
Ni1 N2 2.084(3) .
Ni1 N2 2.084(3) 7
Ni1 N1 2.095(3) 7
Ni1 N1 2.095(3) .
Ni1 O16 2.158(2) 7
N1 C1 1.486(5) .
C1 C2 1.514(6) .
C2 N2 1.473(5) .
Ni2 N31 2.080(3) .
Ni2 N32 2.081(3) .
Ni2 N12 2.094(3) .
Ni2 N52 2.112(3) .
Ni2 N51 2.114(3) .
Ni2 N11 2.122(3) .
N11 C11 1.341(5) .
N11 C22 1.356(5) .
N12 C20 1.333(5) .
N12 C21 1.355(5) .
C11 C12 1.389(6) .
C12 C13 1.382(6) .
C13 C14 1.396(6) .
C14 C22 1.421(5) .
C14 C15 1.427(6) .
C15 C16 1.349(7) .
C16 C17 1.438(6) .
C17 C21 1.406(5) .
C17 C18 1.412(6) .
C18 C19 1.381(7) .
C19 C20 1.394(6) .
C21 C22 1.444(5) .
N31 C31 1.337(5) .
N31 C42 1.352(5) .
N32 C40 1.322(5) .
N32 C41 1.356(5) .
C31 C32 1.391(6) .
C32 C33 1.369(7) .
C33 C34 1.389(7) .
C34 C42 1.408(6) .
C34 C35 1.432(7) .
C35 C36 1.349(9) .
C36 C37 1.440(8) .
C37 C41 1.409(6) .
C37 C38 1.410(8) .
C38 C39 1.356(9) .
C39 C40 1.424(8) .
C41 C42 1.441(6) .
N51 C51 1.330(5) .
N51 C62 1.360(5) .
N52 C60 1.326(5) .
N52 C61 1.365(5) .
C51 C52 1.407(6) .
C52 C53 1.362(8) .
C53 C54 1.402(7) .
C54 C62 1.406(5) .
C54 C55 1.432(7) .
C55 C56 1.351(8) .
C56 C57 1.435(7) .
C57 C58 1.405(7) .
C57 C61 1.407(6) .
C58 C59 1.358(9) .
C59 C60 1.408(7) .
C61 C62 1.440(6) .
O40 O40' 1.14(2) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1N1 O40 0.91 2.57 3.241(7) 130.7 7
N1 H2N1 O15 0.91 2.26 3.111(4) 155.8 .
C1 H1B O22 0.99 2.56 3.536(4) 170.1 7
N2 H1N2 O34 0.91 2.60 3.379(5) 143.6 7_556
N2 H2N2 O14 0.91 2.28 3.151(4) 160.2 7
C12 H12 O37 0.95 2.63 3.322(6) 130.4 4_556
C19 H19 O10 0.95 2.66 3.446(5) 140.7 .
C19 H19 O20 0.95 2.57 3.438(5) 151.7 .
C31 H31 N12 0.95 2.63 3.163(5) 115.7 .
C32 H32 O17 0.95 2.47 3.228(5) 136.5 7_556
C39 H39 O19 0.95 2.53 3.412(6) 154.3 3_455
C51 H51 N31 0.95 2.60 3.129(5) 115.8 .
C51 H51 O36 0.95 2.57 3.234(7) 127.1 7_556
C52 H52 O22 0.95 2.42 3.072(5) 126.0 .
C59 H59 O8 0.95 2.66 3.549(5) 156.8 5_666
C59 H59 O22 0.95 2.34 3.023(6) 128.3 6_566
O31 H1O O33 0.84 1.95 2.746(6) 158.7 .
O31 H2O O20 0.84 1.94 2.756(4) 164.2 .
O32 H3O O31 0.84 1.95 2.784(5) 169.2 2_656
O32 H4O O34 0.84 1.86 2.673(6) 163.2 .
O33 H5O O17 0.84 1.94 2.728(4) 156.4 .
O33 H6O O32 0.84 2.01 2.792(6) 154.9 .
O34 H7O O35 0.84 2.00 2.751(5) 148.3 2_656
O34 H8O O16 0.84 1.93 2.766(4) 171.2 7_556
O35 H9O O19 0.84 2.02 2.777(4) 149.0 .
O35 H10O O33 0.84 2.03 2.783(6) 149.5 .
O36 H11O O34 0.84 2.00 2.767(6) 152.0 .
O36 H12O O11 0.84 2.03 2.857(5) 170.0 7_556
O37 H13O O38 0.84 2.08 2.917(6) 174.5 .
O37 H14O O36 0.84 1.92 2.746(7) 165.4 .
O38 H15O O35 0.84 2.08 2.880(5) 158.9 2_656
O39 H16O O31 0.86 2.01 2.865(5) 169.8 2_656
