#------------------------------------------------------------------------------
#$Date: 2019-11-17 11:31:45 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229607 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/59/7045984.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_7045984
loop_
_publ_author_name
'Wendt, M.'
'Mahnke, L. K.'
'Näther, C'
'van Leusen, J.'
'Kögerler, P'
'Bensch, W.'
_publ_section_title
;
 Ordnung muss sein: heteroelement order and disorder in polyoxovanadates.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6672
_journal_page_last               6674
_journal_paper_doi               10.1039/c8dt00715b
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C18 H75 Ge3 N18 Ni3 O45 Sb3 V15'
_chemical_formula_weight         2787.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2018-03-16 deposited with the CCDC.
2018-04-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.600(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.1983(12)
_cell_length_b                   22.7116(15)
_cell_length_c                   14.4488(10)
_cell_measurement_reflns_used    29983
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.996
_cell_measurement_theta_min      2.510
_cell_volume                     4794.3(7)
_computing_cell_refinement       'X-Area (STOE, 2008'
_computing_data_collection       'X-Area (STOE, 2008'
_computing_data_reduction        'X-Area (STOE, 2008'
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008) and Diamond (Brandenburg, 1999)
;
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick,2015'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29983
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.996
_diffrn_reflns_theta_min         2.510
_exptl_absorpt_coefficient_mu    3.787
_exptl_absorpt_correction_T_max  0.6790
_exptl_absorpt_correction_T_min  0.4473
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-Red and X-Shape(STOE, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_description       block
_exptl_crystal_F_000             2694
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
;
 Flack x determined using 4336 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(8)
_refine_ls_extinction_coef       0.00207(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         11322
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0314
_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)+(0.0480P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0775
_reflns_Friedel_coverage         0.930
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.967
_reflns_number_gt                10007
_reflns_number_total             11322
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt00715b2.cif
_cod_data_source_block           Compound2
_cod_depositor_comments
'Adding full bibliography for 7045984--7045986.cif.'
_cod_original_cell_volume        4794.3(6)
_cod_database_code               7045984
_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'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.99802(10) 0.95569(6) 0.66416(10) 0.0209(2) Uani 0.7 1 d . . P A 1
Sb2 Sb 1.11966(15) 0.84279(8) 0.8889(2) 0.0187(4) Uani 0.35 1 d . . P A 1
Sb3 Sb 1.08941(14) 1.20266(7) 0.97718(17) 0.0240(3) Uani 0.45 1 d . . P B 1
Ge1 Ge 1.0095(3) 0.9493(2) 0.7010(4) 0.0167(8) Uani 0.3 1 d . . P A 2
Ge2 Ge 1.10226(13) 0.86112(7) 0.87480(17) 0.0181(3) Uani 0.65 1 d . . P A 2
Ge3 Ge 1.07834(16) 1.19040(9) 0.9959(2) 0.0247(4) Uani 0.55 1 d . . P B 2
V1 V 0.78111(6) 0.91537(4) 0.85372(8) 0.01547(18) Uani 1 1 d . . . . .
V2 V 0.82720(6) 1.00688(4) 0.67972(8) 0.01675(19) Uani 1 1 d . . . . .
V3 V 0.87483(6) 0.87946(4) 0.75824(8) 0.01606(18) Uani 1 1 d . . . . .
V4 V 1.19887(6) 0.99669(4) 0.96402(9) 0.01861(19) Uani 1 1 d . . . . .
V5 V 0.87342(7) 1.12391(4) 0.76703(9) 0.0213(2) Uani 1 1 d . . . . .
V6 V 1.05094(7) 1.08495(4) 0.81340(9) 0.0192(2) Uani 1 1 d . . . . .
V7 V 1.22436(7) 1.07871(4) 1.13352(9) 0.0191(2) Uani 1 1 d . . . . .
V8 V 1.0000 0.83025(5) 1.0000 0.0145(2) Uani 1 2 d S T P A .
O1 O 0.9805(11) 0.9685(6) 0.5678(14) 0.030(3) Uiso 0.3 1 d . . P A 2
O2 O 1.1610(5) 0.7962(3) 0.9066(7) 0.0350(17) Uani 0.65 1 d . . P A 2
O3 O 1.1508(7) 1.2337(4) 0.9900(9) 0.039(2) Uani 0.55 1 d . . P B 2
O4 O 1.1719(3) 0.91412(17) 0.9812(4) 0.0201(8) Uani 1 1 d . . . . .
O5 O 0.7964(3) 0.94233(16) 0.7384(4) 0.0179(8) Uani 1 1 d . . . . .
O6 O 1.0030(3) 0.85282(17) 0.8691(3) 0.0197(8) Uani 1 1 d . . . . .
O7 O 1.0053(3) 1.14436(19) 0.8691(4) 0.0282(10) Uani 1 1 d . . . . .
O8 O 1.2383(3) 0.99547(17) 1.1196(4) 0.0201(8) Uani 1 1 d . . . . .
O9 O 0.7491(3) 1.01274(18) 0.5428(4) 0.0240(9) Uani 1 1 d . . . . .
O10 O 1.0827(3) 1.00191(19) 0.8075(4) 0.0239(8) Uani 1 1 d . . . . .
O11 O 1.1615(3) 1.07610(18) 0.9669(4) 0.0209(8) Uani 1 1 d . . . . .
O12 O 0.9132(3) 0.94322(16) 0.7024(4) 0.0203(8) Uani 1 1 d . . . . .
O13 O 1.3243(3) 1.10828(19) 1.1977(4) 0.0294(10) Uani 1 1 d . . . . .
O14 O 0.8181(3) 0.83089(18) 0.6571(4) 0.0258(9) Uani 1 1 d . . . . .
O15 O 0.6846(3) 0.88033(18) 0.7858(4) 0.0235(9) Uani 1 1 d . . . . .
O16 O 1.1402(3) 1.14395(18) 1.1103(4) 0.0275(10) Uani 1 1 d . . . . .
O17 O 1.0695(3) 1.1224(2) 0.7343(4) 0.0301(10) Uani 1 1 d . . . . .
O18 O 1.0699(3) 0.88349(19) 0.7415(4) 0.0234(8) Uani 1 1 d . . . . .
O19 O 1.2855(3) 0.9970(2) 0.9581(4) 0.0313(10) Uani 1 1 d . . . . .
O20 O 0.8194(4) 1.1719(2) 0.6652(5) 0.0366(11) Uani 1 1 d . . . . .
O21 O 1.0000 0.7594(2) 1.0000 0.0226(12) Uani 1 2 d S T P . .
O22 O 1.0000 1.2333(3) 1.0000 0.0358(17) Uani 1 2 d S T P . .
O23 O 0.8779(3) 0.85982(17) 0.8917(4) 0.0184(8) Uani 1 1 d . . . . .
O24 O 0.7959(3) 1.06179(16) 0.7532(4) 0.0204(8) Uani 1 1 d . . . . .
O25 O 0.9243(3) 1.06304(17) 0.7265(4) 0.0215(8) Uani 1 1 d . . . . .
Ni1 Ni 0.78285(6) 0.65837(4) 0.72091(7) 0.02516(18) Uani 1 1 d . . . . .
N1 N 0.7882(4) 0.5685(2) 0.6793(6) 0.0329(13) Uani 1 1 d . . . . .
H1C H 0.8024 0.5666 0.6288 0.039 Uiso 1 1 calc R U . . .
H1D H 0.8310 0.5480 0.7440 0.039 Uiso 1 1 calc R U . . .
C1 C 0.6956(6) 0.5440(3) 0.6266(8) 0.0429(19) Uani 1 1 d . . . . .
H1A H 0.6868 0.5365 0.6870 0.051 Uiso 1 1 calc R U . . .
H1B H 0.6883 0.5062 0.5877 0.051 Uiso 1 1 calc R U . . .
C2 C 0.6262(5) 0.5876(3) 0.5409(7) 0.0384(17) Uani 1 1 d . . . . .
H2A H 0.6326 0.5931 0.4780 0.046 Uiso 1 1 calc R U . . .
H2B H 0.5637 0.5729 0.5068 0.046 Uiso 1 1 calc R U . . .
N2 N 0.6406(4) 0.6438(2) 0.5990(5) 0.0290(12) Uani 1 1 d . . . . .
H2C H 0.6133 0.6430 0.6351 0.035 Uiso 1 1 calc R U . . .
H2D H 0.6151 0.6735 0.5464 0.035 Uiso 1 1 calc R U . . .
N3 N 0.7871(4) 0.6304(2) 0.8656(5) 0.0295(12) Uani 1 1 d . . . . .
H3C H 0.7350 0.6104 0.8410 0.035 Uiso 1 1 calc R U . . .
H3D H 0.8357 0.6061 0.9114 0.035 Uiso 1 1 calc R U . . .
C3 C 0.7955(5) 0.6835(3) 0.9311(6) 0.0294(14) Uani 1 1 d . . . . .
H3A H 0.8598 0.6972 0.9804 0.035 Uiso 1 1 calc R U . . .
H3B H 0.7769 0.6741 0.9813 0.035 Uiso 1 1 calc R U . . .
C4 C 0.7343(5) 0.7308(3) 0.8457(6) 0.0284(14) Uani 1 1 d . . . . .
H4A H 0.6696 0.7180 0.8001 0.034 Uiso 1 1 calc R U . . .
H4B H 0.7408 0.7674 0.8871 0.034 Uiso 1 1 calc R U . . .
N4 N 0.7607(4) 0.7417(2) 0.7689(5) 0.0303(12) Uani 1 1 d . . . . .
H4C H 0.8127 0.7637 0.8058 0.036 Uiso 1 1 calc R U . . .
H4D H 0.7154 0.7616 0.7051 0.036 Uiso 1 1 calc R U . . .
N5 N 0.9265(4) 0.6670(3) 0.8225(6) 0.0395(15) Uani 1 1 d . . . . .
H5C H 0.9476 0.6859 0.8896 0.047 Uiso 1 1 calc R U . . .
H5D H 0.9533 0.6309 0.8397 0.047 Uiso 1 1 calc R U . . .
C5 C 0.9489(6) 0.7023(4) 0.7531(9) 0.048(2) Uani 1 1 d . . . . .
H5A H 0.9458 0.7449 0.7652 0.058 Uiso 1 1 calc R U . . .
H5B H 1.0120 0.6931 0.7801 0.058 Uiso 1 1 calc R U . . .
C6 C 0.8849(7) 0.6887(4) 0.6307(10) 0.057(3) Uani 1 1 d . . . . .
H6A H 0.8926 0.6473 0.6169 0.068 Uiso 1 1 calc R U . . .
H6B H 0.8973 0.7144 0.5860 0.068 Uiso 1 1 calc R U . . .
N6 N 0.7900(5) 0.6984(3) 0.5928(6) 0.0406(15) Uani 1 1 d . . . . .
H6C H 0.7490 0.6814 0.5228 0.049 Uiso 1 1 calc R U . . .
H6D H 0.7776 0.7375 0.5874 0.049 Uiso 1 1 calc R U . . .
Ni2 Ni 0.5000 0.98088(5) 0.5000 0.0256(2) Uani 1 2 d S T P . .
N11 N 0.5338(4) 0.9758(3) 0.6685(5) 0.0349(13) Uani 1 1 d . . . . .
H11C H 0.5862 0.9547 0.7157 0.042 Uiso 1 1 calc R U . . .
H11D H 0.5426 1.0125 0.6985 0.042 Uiso 1 1 calc R U . . .
C11 C 0.4569(6) 0.9464(4) 0.6594(8) 0.047(2) Uani 1 1 d . . . . .
H11A H 0.4774 0.9323 0.7362 0.056 Uiso 1 1 calc R U . . .
H11B H 0.4062 0.9747 0.6307 0.056 Uiso 1 1 calc R U . . .
C12 C 0.4253(6) 0.8967(4) 0.5798(8) 0.050(2) Uani 1 1 d . . . . .
H12A H 0.3697 0.8797 0.5667 0.060 Uiso 1 1 calc R U . . .
H12B H 0.4732 0.8659 0.6149 0.060 Uiso 1 1 calc R U . . .
N12 N 0.4044(4) 0.9145(3) 0.4684(6) 0.0349(13) Uani 1 1 d . . . . .
H12C H 0.3464 0.9289 0.4213 0.042 Uiso 1 1 calc R U . . .
H12D H 0.4089 0.8830 0.4333 0.042 Uiso 1 1 calc R U . . .
N13 N 0.5917(4) 1.0523(3) 0.5445(5) 0.0310(12) Uani 1 1 d . . . . .
H13C H 0.6316 1.0557 0.6226 0.037 Uiso 1 1 calc R U . . .
H13D H 0.6245 1.0456 0.5166 0.037 Uiso 1 1 calc R U . . .
C13 C 0.5368(6) 1.1078(3) 0.4935(8) 0.0413(18) Uani 1 1 d . . . . .
H13A H 0.5767 1.1424 0.5331 0.050 Uiso 1 1 calc R U . . .
H13B H 0.5106 1.1101 0.4107 0.050 Uiso 1 1 calc R U . . .
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'
Ge Ge 0.1547 1.8001 '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'
Ni Ni 0.3393 1.1124 '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
O12 Sb1 O18 95.07(17) . .
O12 Sb1 O10 91.98(18) . .
O18 Sb1 O10 90.48(19) . .
O4 Sb2 O18 94.12(19) . .
O4 Sb2 O6 92.65(19) . .
O18 Sb2 O6 91.58(18) . .
O7 Sb3 O22 92.42(19) . .
O7 Sb3 O16 90.5(2) . .
O22 Sb3 O16 91.60(17) . .
O1 Ge1 O18 107.8(6) . .
O1 Ge1 O10 111.8(6) . .
O18 Ge1 O10 106.9(3) . .
O1 Ge1 O12 112.8(6) . .
O18 Ge1 O12 111.2(3) . .
O10 Ge1 O12 106.3(3) . .
O1 Ge1 Ge2 142.2(6) . .
O18 Ge1 Ge2 34.36(16) . .
O10 Ge1 Ge2 88.0(2) . .
O12 Ge1 Ge2 90.3(2) . .
O2 Ge2 O18 107.2(3) . .
O2 Ge2 O4 110.2(3) . .
O18 Ge2 O4 111.3(2) . .
O2 Ge2 O6 112.1(3) . .
O18 Ge2 O6 108.7(2) . .
O4 Ge2 O6 107.3(2) . .
O2 Ge2 Ge1 142.0(3) . .
O18 Ge2 Ge1 34.73(17) . .
O4 Ge2 Ge1 91.66(18) . .
O6 Ge2 Ge1 88.96(17) . .
O3 Ge3 O16 109.1(4) . .
O3 Ge3 O22 110.6(4) . .
O16 Ge3 O22 113.0(2) . .
O3 Ge3 O7 114.1(4) . .
O16 Ge3 O7 106.6(2) . .
O22 Ge3 O7 103.4(2) . .
O3 Ge3 Ge3 144.3(3) . 2_757
O16 Ge3 Ge3 93.21(18) . 2_757
O22 Ge3 Ge3 33.70(18) . 2_757
O7 Ge3 Ge3 84.02(17) . 2_757
O15 V1 O8 108.77(19) . 2_757
O15 V1 O5 107.0(2) . .
O8 V1 O5 90.63(16) 2_757 .
O15 V1 O23 108.77(19) . .
O8 V1 O23 142.16(18) 2_757 .
O5 V1 O23 83.02(16) . .
O15 V1 O4 104.8(2) . 2_757
O8 V1 O4 76.98(17) 2_757 2_757
O5 V1 O4 148.15(18) . 2_757
O23 V1 O4 89.03(17) . 2_757
O15 V1 V3 107.94(16) . .
O8 V1 V3 126.34(12) 2_757 .
O5 V1 V3 41.41(11) . .
O23 V1 V3 42.38(12) . .
O4 V1 V3 127.89(12) 2_757 .
O15 V1 V4 110.40(16) . 2_757
O8 V1 V4 37.09(12) 2_757 2_757
O5 V1 V4 122.94(12) . 2_757
O23 V1 V4 121.50(13) . 2_757
O4 V1 V4 39.93(11) 2_757 2_757
V3 V1 V4 141.65(4) . 2_757
O9 V2 O24 106.8(2) . .
O9 V2 O5 109.1(2) . .
O24 V2 O5 89.50(16) . .
O9 V2 O25 109.0(2) . .
O24 V2 O25 83.67(17) . .
O5 V2 O25 141.67(19) . .
O9 V2 O12 106.9(2) . .
O24 V2 O12 146.29(19) . .
O5 V2 O12 77.55(15) . .
O25 V2 O12 87.55(16) . .
O9 V2 V5 106.15(16) . .
O24 V2 V5 42.17(12) . .
O5 V2 V5 126.82(12) . .
O25 V2 V5 42.79(12) . .
O12 V2 V5 127.18(13) . .
O9 V2 V3 112.54(16) . .
O24 V2 V3 121.46(12) . .
O5 V2 V3 37.66(11) . .
O25 V2 V3 119.78(13) . .
O12 V2 V3 39.91(11) . .
V5 V2 V3 141.31(4) . .
O14 V3 O5 110.8(2) . .
O14 V3 O23 111.4(2) . .
O5 V3 O23 84.13(17) . .
O14 V3 O12 108.7(2) . .
O5 V3 O12 78.81(16) . .
O23 V3 O12 139.79(18) . .
O14 V3 O6 109.4(2) . .
O5 V3 O6 139.66(18) . .
O23 V3 O6 78.72(16) . .
O12 V3 O6 91.25(17) . .
O14 V3 V1 112.61(16) . .
O5 V3 V1 42.17(12) . .
O23 V3 V1 42.74(11) . .
O12 V3 V1 116.27(12) . .
O6 V3 V1 116.61(12) . .
O14 V3 V8 115.26(17) . .
O5 V3 V8 115.39(13) . .
O23 V3 V8 38.25(11) . .
O12 V3 V8 122.42(14) . .
O6 V3 V8 40.52(11) . .
V1 V3 V8 78.73(3) . .
O14 V3 V2 115.17(17) . .
O5 V3 V2 38.13(11) . .
O23 V3 V2 114.90(12) . .
O12 V3 V2 40.69(11) . .
O6 V3 V2 121.96(12) . .
V1 V3 V2 77.91(3) . .
V8 V3 V2 129.31(4) . .
O19 V4 O8 111.4(2) . .
O19 V4 O11 111.1(2) . .
O8 V4 O11 83.03(18) . .
O19 V4 O10 110.4(2) . .
O8 V4 O10 138.06(17) . .
O11 V4 O10 79.56(18) . .
O19 V4 O4 109.2(2) . .
O8 V4 O4 77.70(17) . .
O11 V4 O4 139.33(16) . .
O10 V4 O4 91.38(18) . .
O19 V4 V7 111.77(19) . .
O8 V4 V7 41.65(12) . .
O11 V4 V7 42.40(13) . .
O10 V4 V7 116.99(12) . .
O4 V4 V7 115.39(13) . .
O19 V4 V6 115.91(19) . .
O8 V4 V6 114.10(13) . .
O11 V4 V6 38.68(13) . .
O10 V4 V6 40.93(12) . .
O4 V4 V6 122.54(13) . .
V7 V4 V6 78.77(4) . .
O19 V4 V1 115.19(19) . 2_757
O8 V4 V1 37.67(12) . 2_757
O11 V4 V1 114.05(13) . 2_757
O10 V4 V1 121.31(13) . 2_757
O4 V4 V1 40.07(13) . 2_757
V7 V4 V1 77.44(3) . 2_757
V6 V4 V1 128.53(4) . 2_757
O20 V5 O24 113.1(2) . .
O20 V5 O25 110.4(2) . .
O24 V5 O25 84.15(16) . .
O20 V5 O7 109.3(2) . .
O24 V5 O7 137.58(19) . .
O25 V5 O7 78.90(18) . .
O20 V5 O16 109.1(2) . 2_757
O24 V5 O16 77.68(18) . 2_757
O25 V5 O16 140.37(19) . 2_757
O7 V5 O16 91.2(2) . 2_757
O20 V5 V2 111.7(2) . .
O24 V5 V2 42.48(12) . .
O25 V5 V2 42.97(11) . .
O7 V5 V2 117.10(13) . .
O16 V5 V2 116.70(13) 2_757 .
O20 V5 V6 113.03(19) . .
O24 V5 V6 115.53(12) . .
O25 V5 V6 38.38(12) . .
O7 V5 V6 40.71(13) . .
O16 V5 V6 123.84(15) 2_757 .
V2 V5 V6 79.56(4) . .
O20 V5 V7 116.59(19) . 2_757
O24 V5 V7 37.26(13) . 2_757
O25 V5 V7 114.80(12) . 2_757
O7 V5 V7 120.99(15) . 2_757
O16 V5 V7 40.43(12) 2_757 2_757
V2 V5 V7 78.08(3) . 2_757
V6 V5 V7 130.12(4) . 2_757
O17 V6 O25 110.5(2) . .
O17 V6 O11 110.8(2) . .
O25 V6 O11 138.68(18) . .
O17 V6 O10 106.3(2) . .
O25 V6 O10 89.56(17) . .
O11 V6 O10 79.57(18) . .
O17 V6 O7 104.1(2) . .
O25 V6 O7 79.17(19) . .
O11 V6 O7 90.38(19) . .
O10 V6 O7 149.60(19) . .
O17 V6 V4 112.90(17) . .
O25 V6 V4 120.59(12) . .
O11 V6 V4 39.07(12) . .
O10 V6 V4 40.55(13) . .
O7 V6 V4 124.74(15) . .
O17 V6 V5 109.71(17) . .
O25 V6 V5 38.84(12) . .
O11 V6 V5 122.25(13) . .
O10 V6 V5 124.68(12) . .
O7 V6 V5 40.53(14) . .
V4 V6 V5 137.39(4) . .
O13 V7 O24 108.5(2) . 2_757
O13 V7 O8 107.0(2) . .
O24 V7 O8 89.83(16) 2_757 .
O13 V7 O11 110.5(2) . .
O24 V7 O11 140.83(18) 2_757 .
O8 V7 O11 81.91(18) . .
O13 V7 O16 106.0(2) . .
O24 V7 O16 76.97(17) 2_757 .
O8 V7 O16 146.87(18) . .
O11 V7 O16 89.37(19) . .
O13 V7 V4 108.15(17) . .
O24 V7 V4 125.40(12) 2_757 .
O8 V7 V4 41.02(13) . .
O11 V7 V4 41.89(12) . .
O16 V7 V4 127.83(15) . .
O13 V7 V5 111.28(17) . 2_757
O24 V7 V5 37.25(12) 2_757 2_757
O8 V7 V5 121.79(12) . 2_757
O11 V7 V5 120.81(13) . 2_757
O16 V7 V5 39.74(13) . 2_757
V4 V7 V5 140.54(4) . 2_757
O21 V8 O23 110.46(12) . 2_757
O21 V8 O23 110.46(12) . .
O23 V8 O23 139.1(2) 2_757 .
O21 V8 O6 104.91(12) . 2_757
O23 V8 O6 79.02(16) 2_757 2_757
O23 V8 O6 90.60(17) . 2_757
O21 V8 O6 104.92(12) . .
O23 V8 O6 90.60(17) 2_757 .
O23 V8 O6 79.02(16) . .
O6 V8 O6 150.2(2) 2_757 .
O21 V8 V3 111.68(3) . 2_757
O23 V8 V3 38.85(12) 2_757 2_757
O23 V8 V3 121.36(13) . 2_757
O6 V8 V3 40.22(12) 2_757 2_757
O6 V8 V3 124.99(12) . 2_757
O21 V8 V3 111.68(3) . .
O23 V8 V3 121.37(13) 2_757 .
O23 V8 V3 38.85(12) . .
O6 V8 V3 124.99(12) 2_757 .
O6 V8 V3 40.22(11) . .
V3 V8 V3 136.64(5) 2_757 .
Ge2 O4 V4 129.6(2) . .
Sb2 O4 V4 138.9(2) . .
Ge2 O4 V1 128.7(2) . 2_757
Sb2 O4 V1 121.1(2) . 2_757
V4 O4 V1 100.01(18) . 2_757
V3 O5 V2 104.21(17) . .
V3 O5 V1 96.42(17) . .
V2 O5 V1 147.2(2) . .
Ge2 O6 V3 133.1(2) . .
V3 O6 Sb2 142.9(2) . .
Ge2 O6 V8 126.1(2) . .
V3 O6 V8 99.26(17) . .
Sb2 O6 V8 117.9(2) . .
Ge3 O7 V5 135.9(3) . .
Sb3 O7 V5 142.3(2) . .
Ge3 O7 V6 124.5(2) . .
Sb3 O7 V6 118.3(2) . .
V5 O7 V6 98.8(2) . .
V4 O8 V7 97.33(19) . .
V4 O8 V1 105.24(19) . 2_757
V7 O8 V1 147.9(2) . 2_757
Ge1 O10 V4 133.9(3) . .
Ge1 O10 V6 126.2(3) . .
V4 O10 V6 98.52(19) . .
V4 O10 Sb1 142.8(2) . .
V6 O10 Sb1 118.7(2) . .
V6 O11 V4 102.2(2) . .
V6 O11 V7 149.3(2) . .
V4 O11 V7 95.71(19) . .
Ge1 O12 V3 130.9(3) . .
Sb1 O12 V3 139.1(2) . .
Ge1 O12 V2 128.5(2) . .
Sb1 O12 V2 121.46(19) . .
V3 O12 V2 99.41(17) . .
Ge3 O16 V5 130.4(3) . 2_757
Ge3 O16 V7 128.0(3) . .
V5 O16 V7 99.8(2) 2_757 .
V5 O16 Sb3 139.5(2) 2_757 .
V7 O16 Sb3 120.5(2) . .
Ge2 O18 Ge1 110.9(3) . .
Sb1 O18 Sb2 136.1(2) . .
Ge3 O22 Ge3 112.6(4) . 2_757
Sb3 O22 Sb3 138.6(3) . 2_757
V8 O23 V3 102.90(17) . .
V8 O23 V1 149.6(2) . .
V3 O23 V1 94.88(17) . .
V5 O24 V7 105.5(2) . 2_757
V5 O24 V2 95.34(18) . .
V7 O24 V2 150.2(2) 2_757 .
V6 O25 V5 102.8(2) . .
V6 O25 V2 152.3(2) . .
V5 O25 V2 94.23(17) . .
N5 Ni1 N2 170.8(2) . .
N5 Ni1 N6 82.7(3) . .
N2 Ni1 N6 91.2(3) . .
N5 Ni1 N4 95.0(2) . .
N2 Ni1 N4 92.0(2) . .
N6 Ni1 N4 91.5(2) . .
N5 Ni1 N3 92.3(3) . .
N2 Ni1 N3 94.6(2) . .
N6 Ni1 N3 170.9(2) . .
N4 Ni1 N3 81.3(2) . .
N5 Ni1 N1 92.2(2) . .
N2 Ni1 N1 81.7(2) . .
N6 Ni1 N1 97.2(2) . .
N4 Ni1 N1 169.3(2) . .
N3 Ni1 N1 90.6(2) . .
C1 N1 Ni1 105.9(4) . .
N1 C1 C2 108.4(6) . .
N2 C2 C1 109.2(6) . .
C2 N2 Ni1 109.0(4) . .
C3 N3 Ni1 108.2(4) . .
N3 C3 C4 108.2(6) . .
N4 C4 C3 108.9(5) . .
C4 N4 Ni1 107.8(4) . .
C5 N5 Ni1 107.4(5) . .
C6 C5 N5 110.8(7) . .
C5 C6 N6 109.1(7) . .
C6 N6 Ni1 106.1(5) . .
N11 Ni2 N11 173.7(3) 2_656 .
N11 Ni2 N13 91.5(2) 2_656 .
N11 Ni2 N13 93.2(3) . .
N11 Ni2 N13 93.2(2) 2_656 2_656
N11 Ni2 N13 91.5(2) . 2_656
N13 Ni2 N13 81.0(3) . 2_656
N11 Ni2 N12 81.3(3) 2_656 2_656
N11 Ni2 N12 94.2(2) . 2_656
N13 Ni2 N12 94.6(2) . 2_656
N13 Ni2 N12 173.0(2) 2_656 2_656
N11 Ni2 N12 94.2(2) 2_656 .
N11 Ni2 N12 81.3(3) . .
N13 Ni2 N12 173.0(2) . .
N13 Ni2 N12 94.6(2) 2_656 .
N12 Ni2 N12 90.2(3) 2_656 .
C11 N11 Ni2 108.0(5) . .
C12 C11 N11 108.9(6) . .
C11 C12 N12 111.8(7) . .
C12 N12 Ni2 108.3(5) . .
C13 N13 Ni2 108.5(4) . .
C13 C13 N13 109.3(5) 2_656 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb1 O12 1.946(4) .
Sb1 O18 1.976(4) .
Sb1 O10 1.990(5) .
Sb2 O4 1.948(5) .
Sb2 O18 1.977(5) .
Sb2 O6 1.979(4) .
Sb3 O7 1.920(5) .
Sb3 O22 1.970(3) .
Sb3 O16 2.053(5) .
Ge1 O1 1.721(16) .
Ge1 O18 1.737(6) .
Ge1 O10 1.769(7) .
Ge1 O12 1.770(6) .
Ge1 Ge2 2.848(4) .
Ge2 O2 1.716(7) .
Ge2 O18 1.721(5) .
Ge2 O4 1.759(5) .
Ge2 O6 1.769(4) .
Ge3 O3 1.686(8) .
Ge3 O16 1.702(5) .
Ge3 O22 1.758(4) .
Ge3 O7 1.820(5) .
Ge3 Ge3 2.924(4) 2_757
V1 O15 1.620(4) .
V1 O8 1.935(4) 2_757
V1 O5 1.944(4) .
V1 O23 1.960(4) .
V1 O4 1.997(4) 2_757
V1 V3 2.8780(13) .
V1 V4 3.0552(13) 2_757
V2 O9 1.612(5) .
V2 O24 1.930(4) .
V2 O5 1.936(4) .
V2 O25 1.945(4) .
V2 O12 2.009(4) .
V2 V5 2.8458(14) .
V2 V3 3.0397(12) .
V3 O14 1.619(4) .
V3 O5 1.916(4) .
V3 O23 1.947(4) .
V3 O12 1.977(4) .
V3 O6 1.979(4) .
V3 V8 3.0251(11) .
V4 O19 1.629(4) .
V4 O8 1.910(4) .
V4 O11 1.937(4) .
V4 O10 1.974(4) .
V4 O4 1.991(4) .
V4 V7 2.8860(14) .
V4 V6 3.0026(14) .
V4 V1 3.0553(13) 2_757
V5 O20 1.611(5) .
V5 O24 1.919(4) .
V5 O25 1.939(4) .
V5 O7 1.982(5) .
V5 O16 1.982(5) 2_757
V5 V6 3.0145(13) .
V5 V7 3.0552(13) 2_757
V6 O17 1.614(4) .
V6 O25 1.919(4) .
V6 O11 1.920(5) .
V6 O10 1.989(4) .
V6 O7 1.989(4) .
V7 O13 1.616(4) .
V7 O24 1.920(4) 2_757
V7 O8 1.934(4) .
V7 O11 1.956(4) .
V7 O16 2.011(4) .
V7 V5 3.0551(13) 2_757
V8 O21 1.609(6) .
V8 O23 1.921(4) 2_757
V8 O23 1.921(4) .
V8 O6 1.991(4) 2_757
V8 O6 1.991(4) .
V8 V3 3.0251(11) 2_757
O4 V1 1.997(4) 2_757
O8 V1 1.935(4) 2_757
O16 V5 1.982(4) 2_757
O22 Ge3 1.758(4) 2_757
O22 Sb3 1.970(3) 2_757
O24 V7 1.920(4) 2_757
Ni1 N5 2.110(6) .
Ni1 N2 2.116(6) .
Ni1 N6 2.134(6) .
Ni1 N4 2.135(5) .
Ni1 N3 2.142(6) .
Ni1 N1 2.147(5) .
N1 C1 1.483(9) .
C1 C2 1.499(13) .
C2 N2 1.462(9) .
N3 C3 1.483(8) .
C3 C4 1.509(10) .
C4 N4 1.468(8) .
N5 C5 1.517(11) .
C5 C6 1.457(15) .
C6 N6 1.485(11) .
Ni2 N11 2.129(6) 2_656
Ni2 N11 2.129(6) .
Ni2 N13 2.133(6) .
Ni2 N13 2.133(6) 2_656
Ni2 N12 2.134(6) 2_656
Ni2 N12 2.134(6) .
N11 C11 1.483(11) .
C11 C12 1.462(14) .
C12 N12 1.473(10) .
N13 C13 1.501(10) .
C13 C13 1.458(15) 2_656
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 H1C O9 0.91 2.40 3.125(7) 136.9 4_646
C1 H1B O1 0.99 2.64 3.218(18) 117.2 4_646
C2 H2A O25 0.99 2.57 3.442(9) 146.5 4_646
C2 H2B O1 0.99 2.53 3.149(17) 120.5 4_646
N2 H2C O17 0.91 2.07 2.958(7) 166.0 3_445
N3 H3C O17 0.91 2.45 3.217(7) 142.6 3_445
C4 H4A O17 0.99 2.62 3.449(8) 141.1 3_445
C4 H4B O2 0.99 2.48 3.242(10) 133.5 2_757
N4 H4C O23 0.91 2.44 3.222(6) 144.0 .
N5 H5C O21 0.91 2.10 2.947(7) 153.5 .
N6 H6C O20 0.91 2.22 3.062(9) 152.9 4_646
N6 H6D O14 0.91 2.27 3.101(7) 151.1 .
N11 H11C O15 0.91 2.22 3.092(7) 160.4 .
C11 H11B O9 0.99 2.56 3.435(9) 146.8 2_656
N12 H12C O5 0.91 2.24 3.109(7) 159.3 2_656
N12 H12D O15 0.91 2.55 3.101(8) 119.7 2_656
N13 H13C O13 0.91 2.52 3.323(8) 148.0 2_757
N13 H13C O24 0.91 2.41 3.096(7) 132.5 .
N13 H13D O9 0.91 2.20 3.017(7) 149.6 .
