#------------------------------------------------------------------------------
#$Date: 2016-03-24 13:58:10 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179647 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/00/4510026.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_4510026
loop_
_publ_author_name
'Zhang, Ying'
'Shen, Jian-Qiang'
'Zheng, Li-Hua'
'Zhang, Zhi-Ming'
'Li, Yu-Xin'
'Wang, En-Bo'
_publ_section_title
;
 Four Polyoxonibate-Based Inorganic--Organic Hybrids Assembly from
 Bicapped Heteropolyoxonibate with Effective Antitumor Activity
;
_journal_issue                   1
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              110
_journal_paper_doi               10.1021/cg401227g
_journal_volume                  14
_journal_year                    2014
_chemical_formula_sum            'C24 H138 Cu6 N24 Nb12 O63 Si V2'
_chemical_formula_weight         3397.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 129.11(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.746(4)
_cell_length_b                   20.789(4)
_cell_length_c                   14.940(3)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.05
_cell_volume                     5000(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.01
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_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  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24154
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.05
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.857
_exptl_absorpt_correction_T_max  0.7077
_exptl_absorpt_correction_T_min  0.5125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.264
_refine_diff_density_min         -1.371
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         5846
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1079P)²+68.2462P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1773
_refine_ls_wR_factor_ref         0.1887
_reflns_number_gt                4661
_reflns_number_total             5846
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg401227g_si_004.cif
_cod_data_source_block           1
_cod_original_cell_volume        4999.7(17)
_cod_original_sg_symbol_H-M      C2/M
_cod_database_code               4510026
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb -1.19090(4) -0.09076(3) -0.17462(6) 0.0311(2) Uani 1 1 d . . .
Nb2 Nb -1.0000 -0.17815(4) 0.0000 0.0341(2) Uani 1 2 d S . .
Nb3 Nb -0.85349(6) 0.0000 -0.06016(9) 0.0323(2) Uani 1 2 d S . .
Nb4 Nb -1.04259(4) -0.08973(4) -0.23687(6) 0.0360(2) Uani 1 1 d . . .
V1 V -1.19487(10) 0.0000 -0.34217(13) 0.0269(4) Uani 1 2 d S . .
Si1 Si -1.0000 0.0000 0.0000 0.0198(6) Uani 1 4 d SU . .
Cu1 Cu -0.7500 -0.2500 0.0000 0.0704(6) Uani 1 2 d S . .
Cu2 Cu -1.0000 -0.5000 -0.5000 0.0737(9) Uani 1 4 d S . .
Cu3 Cu -1.0000 0.0000 -0.5000 0.0709(8) Uani 1 4 d SU . .
Cu4 Cu -1.2500 -0.2500 -0.5000 0.0764(7) Uani 1 2 d S . .
C1 C -0.9117(13) -0.2354(9) -0.203(2) 0.138(7) Uani 1 1 d DU . .
H1A H -0.9674 -0.2208 -0.2373 0.166 Uiso 1 1 calc R . .
H1B H -0.9021 -0.2264 -0.2571 0.166 Uiso 1 1 calc R . .
C2 C -0.9085(11) -0.3039(10) -0.1871(18) 0.140(8) Uani 1 1 d D . .
H2A H -0.9355 -0.3255 -0.2605 0.168 Uiso 1 1 calc R . .
H2B H -0.9374 -0.3155 -0.1578 0.168 Uiso 1 1 calc R . .
C3 C -1.0877(16) -0.5000 -0.739(3) 0.143(12) Uani 1 2 d S . .
C4 C -1.1778(14) -0.3640(11) -0.3733(18) 0.138(7) Uani 1 1 d U . .
H4A H -1.2125 -0.3815 -0.3564 0.165 Uiso 1 1 calc R . .
H4B H -1.1429 -0.3987 -0.3644 0.165 Uiso 1 1 calc R . .
C5 C -1.1276(16) -0.3176(12) -0.293(2) 0.160(9) Uani 1 1 d U . .
H5A H -1.0761 -0.3155 -0.2813 0.192 Uiso 1 1 calc R . .
H5B H -1.1142 -0.3291 -0.2199 0.192 Uiso 1 1 calc R . .
C6 C -0.999(3) -0.5000 -0.698(5) 0.22(2) Uani 1 2 d SU . .
C7 C -0.858(2) -0.0801(19) -0.345(3) 0.110(11) Uani 0.50 1 d PU . .
C8 C -0.8289(18) -0.0237(14) -0.379(3) 0.092(9) Uani 0.50 1 d P . .
N1 N -0.8537(6) -0.1982(6) -0.1000(9) 0.085(4) Uani 1 1 d . . .
H1C H -0.8745 -0.1903 -0.0633 0.102 Uiso 1 1 calc R . .
H1D H -0.8434 -0.1604 -0.1180 0.102 Uiso 1 1 calc R . .
N2 N -0.8194(6) -0.3244(6) -0.1034(10) 0.091(4) Uani 1 1 d . . .
H2C H -0.8016 -0.3374 -0.1420 0.109 Uiso 1 1 calc R . .
H2D H -0.8144 -0.3576 -0.0608 0.109 Uiso 1 1 calc R . .
N3 N -1.0993(10) -0.5000 -0.6632(19) 0.127(9) Uani 1 2 d S . .
N4 N -0.9478(11) -0.5355(10) -0.5686(19) 0.076(6) Uani 0.50 1 d P . .
N5 N -1.2305(9) -0.3438(7) -0.4909(12) 0.114(5) Uani 1 1 d U . .
H5C H -1.2793 -0.3648 -0.5305 0.137 Uiso 1 1 calc R . .
H5D H -1.2066 -0.3533 -0.5228 0.137 Uiso 1 1 calc R . .
N6 N -1.1687(11) -0.2526(7) -0.3300(12) 0.147(8) Uani 1 1 d . . .
H6A H -1.1303 -0.2217 -0.3041 0.177 Uiso 1 1 calc R . .
H6B H -1.1946 -0.2456 -0.3002 0.177 Uiso 1 1 calc R . .
N7 N -0.8997(10) 0.0000 -0.4862(14) 0.090(5) Uani 1 2 d S . .
N8 N -0.9308(11) -0.0772(13) -0.3635(18) 0.081(6) Uani 0.50 1 d PU . .
O1 O -1.0453(5) -0.0653(4) -0.0802(8) 0.078(2) Uani 1 1 d U . .
O2 O -1.1965(7) -0.0659(3) -0.0580(7) 0.085(3) Uani 1 1 d . . .
O3 O -1.0718(4) -0.1273(4) -0.3626(5) 0.0548(18) Uani 1 1 d . . .
O4 O -0.9024(8) 0.0000 0.0556(11) 0.080(3) Uani 1 2 d S . .
O5 O -1.1193(5) -0.1611(5) -0.0900(8) 0.082(3) Uani 1 1 d U . .
O6 O -1.1583(4) -0.0861(3) -0.2787(6) 0.0523(18) Uani 1 1 d . . .
O7 O -1.2734(5) 0.0000 -0.4792(6) 0.044(2) Uani 1 2 d S . .
O8 O -1.0000 -0.2614(4) 0.0000 0.069(3) Uani 1 2 d S . .
O9 O -1.2869(4) -0.1303(3) -0.2707(5) 0.0520(16) Uani 1 1 d . . .
O10 O -1.0878(5) 0.0000 -0.3083(10) 0.056(3) Uani 1 2 d S . .
O11 O -0.7858(9) 0.0000 -0.0917(13) 0.084(4) Uani 1 2 d S . .
O12 O -1.2282(7) 0.0000 -0.2470(8) 0.050(2) Uani 1 2 d S . .
O13 O -0.9339(4) -0.0652(4) -0.1698(8) 0.089(3) Uani 1 1 d U . .
O14 O -1.0103(8) 0.0000 0.1015(10) 0.082(4) Uani 1 2 d SU . .
O15 O -1.0118(5) -0.1594(5) -0.1379(8) 0.083(3) Uani 1 1 d U . .
O1W O -0.7113(10) -0.2217(8) -0.1317(14) 0.156(6) Uani 1 1 d U . .
O2W O -1.0769(10) -0.3286(9) -0.5260(14) 0.092(5) Uani 0.60 1 d PU A 1
O2WA O -1.0646(18) -0.3852(15) -0.509(2) 0.101(8) Uiso 0.40 1 d P B 2
O3W O -1.0287(15) -0.3883(12) 0.015(2) 0.118(8) Uani 0.51 1 d PU . .
O4W O -1.1328(18) -0.2343(14) -0.485(3) 0.120(9) Uani 0.46 1 d PU . .
O5W O -1.0750(18) -0.2010(14) -0.514(2) 0.124(8) Uani 0.51 1 d PU . .
O6W O -1.095(3) -0.5000 -0.155(4) 0.166(17) Uani 0.50 2 d SPU . .
O7W O -0.6766(15) 0.0866(12) -0.062(2) 0.117(7) Uani 0.52 1 d PU . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Nb Nb -2.0727 0.6215 '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'
Si Si 0.0817 0.0704 '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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
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
O9 Nb1 O2 100.6(4) . .
O9 Nb1 O5 101.0(4) . .
O2 Nb1 O5 94.2(4) . .
O9 Nb1 O6 98.5(3) . .
O2 Nb1 O6 158.0(3) . .
O5 Nb1 O6 92.7(3) . .
O9 Nb1 O12 98.2(4) . .
O2 Nb1 O12 90.7(3) . .
O5 Nb1 O12 158.9(4) . .
O6 Nb1 O12 75.8(3) . .
O9 Nb1 O1 156.8(3) . .
O2 Nb1 O1 100.4(4) . .
O5 Nb1 O1 67.7(4) . .
O6 Nb1 O1 63.3(3) . .
O12 Nb1 O1 91.3(4) . .
O9 Nb1 O4 155.8(3) . 5_355
O2 Nb1 O4 66.7(4) . 5_355
O5 Nb1 O4 100.4(4) . 5_355
O6 Nb1 O4 91.5(4) . 5_355
O12 Nb1 O4 62.9(4) . 5_355
O1 Nb1 O4 45.7(3) . 5_355
O9 Nb1 V1 100.7(2) . .
O2 Nb1 V1 126.4(2) . .
O5 Nb1 V1 128.4(2) . .
O6 Nb1 V1 37.97(16) . .
O12 Nb1 V1 37.8(2) . .
O1 Nb1 V1 74.2(2) . .
O4 Nb1 V1 74.1(3) 5_355 .
O8 Nb2 O15 101.5(3) . 2_355
O8 Nb2 O15 101.5(3) . .
O15 Nb2 O15 157.0(6) 2_355 .
O8 Nb2 O5 100.4(3) . .
O15 Nb2 O5 87.2(4) 2_355 .
O15 Nb2 O5 88.7(3) . .
O8 Nb2 O5 100.4(3) . 2_355
O15 Nb2 O5 88.7(3) 2_355 2_355
O15 Nb2 O5 87.2(4) . 2_355
O5 Nb2 O5 159.3(6) . 2_355
O8 Nb2 O1 158.00(18) . 2_355
O15 Nb2 O1 63.5(4) 2_355 2_355
O15 Nb2 O1 94.4(4) . 2_355
O5 Nb2 O1 95.1(4) . 2_355
O5 Nb2 O1 65.0(3) 2_355 2_355
O8 Nb2 O1 158.00(18) . .
O15 Nb2 O1 94.4(4) 2_355 .
O15 Nb2 O1 63.5(4) . .
O5 Nb2 O1 65.0(3) . .
O5 Nb2 O1 95.1(4) 2_355 .
O1 Nb2 O1 44.0(4) 2_355 .
O11 Nb3 O2 100.8(5) . 5_355
O11 Nb3 O2 100.8(5) . 2_355
O2 Nb3 O2 90.0(4) 5_355 2_355
O11 Nb3 O13 100.4(5) . .
O2 Nb3 O13 158.8(5) 5_355 .
O2 Nb3 O13 87.5(4) 2_355 .
O11 Nb3 O13 100.4(5) . 6
O2 Nb3 O13 87.5(4) 5_355 6
O2 Nb3 O13 158.8(5) 2_355 6
O13 Nb3 O13 87.3(5) . 6
O11 Nb3 O14 156.7(6) . 5_355
O2 Nb3 O14 95.6(4) 5_355 5_355
O2 Nb3 O14 95.6(4) 2_355 5_355
O13 Nb3 O14 63.8(3) . 5_355
O13 Nb3 O14 63.8(3) 6 5_355
O11 Nb3 O4 159.6(6) . .
O2 Nb3 O4 65.6(3) 5_355 .
O2 Nb3 O4 65.6(3) 2_355 .
O13 Nb3 O4 94.3(4) . .
O13 Nb3 O4 94.3(4) 6 .
O14 Nb3 O4 43.6(4) 5_355 .
O3 Nb4 O15 102.5(4) . .
O3 Nb4 O13 100.4(4) . .
O15 Nb4 O13 95.3(4) . .
O3 Nb4 O10 96.4(4) . .
O15 Nb4 O10 158.2(4) . .
O13 Nb4 O10 91.8(3) . .
O3 Nb4 O6 98.1(3) . .
O15 Nb4 O6 91.1(3) . .
O13 Nb4 O6 158.5(4) . .
O10 Nb4 O6 75.4(3) . .
O3 Nb4 O1 157.4(3) . .
O15 Nb4 O1 66.7(4) . .
O13 Nb4 O1 100.3(4) . .
O10 Nb4 O1 91.7(4) . .
O6 Nb4 O1 63.6(3) . .
O3 Nb4 O14 154.0(4) . 5_355
O15 Nb4 O14 100.7(4) . 5_355
O13 Nb4 O14 65.7(4) . 5_355
O10 Nb4 O14 63.7(4) . 5_355
O6 Nb4 O14 93.0(4) . 5_355
O1 Nb4 O14 46.7(4) . 5_355
O3 Nb4 V1 99.8(2) . .
O15 Nb4 V1 126.6(2) . .
O13 Nb4 V1 127.2(2) . .
O10 Nb4 V1 37.7(2) . .
O6 Nb4 V1 37.73(16) . .
O1 Nb4 V1 74.2(2) . .
O14 Nb4 V1 75.1(3) 5_355 .
O7 V1 O12 112.8(5) . .
O7 V1 O10 113.7(5) . .
O12 V1 O10 133.5(5) . .
O7 V1 O6 112.8(2) . 6
O12 V1 O6 81.5(2) . 6
O10 V1 O6 80.9(2) . 6
O7 V1 O6 112.8(2) . .
O12 V1 O6 81.5(2) . .
O10 V1 O6 80.9(2) . .
O6 V1 O6 134.4(5) 6 .
O7 V1 Nb1 120.9(2) . 6
O12 V1 Nb1 40.94(12) . 6
O10 V1 Nb1 110.3(3) . 6
O6 V1 Nb1 40.54(18) 6 6
O6 V1 Nb1 111.4(2) . 6
O7 V1 Nb1 120.9(2) . .
O12 V1 Nb1 40.94(12) . .
O10 V1 Nb1 110.3(3) . .
O6 V1 Nb1 111.4(2) 6 .
O6 V1 Nb1 40.54(18) . .
Nb1 V1 Nb1 75.16(5) 6 .
O7 V1 Nb4 121.9(2) . 6
O12 V1 Nb4 110.4(3) . 6
O10 V1 Nb4 40.36(13) . 6
O6 V1 Nb4 40.59(18) 6 6
O6 V1 Nb4 110.3(2) . 6
Nb1 V1 Nb4 74.02(4) 6 6
Nb1 V1 Nb4 117.17(6) . 6
O7 V1 Nb4 121.9(2) . .
O12 V1 Nb4 110.4(3) . .
O10 V1 Nb4 40.36(13) . .
O6 V1 Nb4 110.3(2) 6 .
O6 V1 Nb4 40.59(18) . .
Nb1 V1 Nb4 117.17(6) 6 .
Nb1 V1 Nb4 74.02(4) . .
Nb4 V1 Nb4 73.74(5) 6 .
O4 Si1 O4 180.0(9) 5_355 .
O4 Si1 O1 71.1(4) 5_355 .
O4 Si1 O1 108.9(4) . .
O4 Si1 O1 108.9(4) 5_355 5_355
O4 Si1 O1 71.1(4) . 5_355
O1 Si1 O1 180.0(8) . 5_355
O4 Si1 O1 71.1(4) 5_355 6
O4 Si1 O1 108.9(4) . 6
O1 Si1 O1 110.2(7) . 6
O1 Si1 O1 69.8(7) 5_355 6
O4 Si1 O1 108.9(4) 5_355 2_355
O4 Si1 O1 71.1(4) . 2_355
O1 Si1 O1 69.8(7) . 2_355
O1 Si1 O1 110.2(7) 5_355 2_355
O1 Si1 O1 180.0(4) 6 2_355
O4 Si1 O14 68.4(6) 5_355 .
O4 Si1 O14 111.6(6) . .
O1 Si1 O14 108.7(4) . .
O1 Si1 O14 71.3(4) 5_355 .
O1 Si1 O14 108.7(4) 6 .
O1 Si1 O14 71.3(4) 2_355 .
O4 Si1 O14 111.6(6) 5_355 5_355
O4 Si1 O14 68.4(6) . 5_355
O1 Si1 O14 71.3(4) . 5_355
O1 Si1 O14 108.7(4) 5_355 5_355
O1 Si1 O14 71.3(4) 6 5_355
O1 Si1 O14 108.7(4) 2_355 5_355
O14 Si1 O14 180.0(8) . 5_355
N1 Cu1 N1 180.0(7) 7_345 .
N1 Cu1 N2 94.1(5) 7_345 .
N1 Cu1 N2 85.9(5) . .
N1 Cu1 N2 85.9(5) 7_345 7_345
N1 Cu1 N2 94.1(5) . 7_345
N2 Cu1 N2 180.0(5) . 7_345
N3 Cu2 N3 180.000(2) . 5_344
N3 Cu2 N4 98.6(8) . 2_354
N3 Cu2 N4 81.4(8) 5_344 2_354
N3 Cu2 N4 98.6(8) . 5_344
N3 Cu2 N4 81.4(8) 5_344 5_344
N4 Cu2 N4 42.3(13) 2_354 5_344
N3 Cu2 N4 81.4(8) . .
N3 Cu2 N4 98.6(8) 5_344 .
N4 Cu2 N4 137.7(13) 2_354 .
N4 Cu2 N4 180.000(4) 5_344 .
N3 Cu2 N4 81.4(8) . 6_545
N3 Cu2 N4 98.6(8) 5_344 6_545
N4 Cu2 N4 180.0(7) 2_354 6_545
N4 Cu2 N4 137.7(13) 5_344 6_545
N4 Cu2 N4 42.3(13) . 6_545
N7 Cu3 N7 180.000(1) 5_354 .
N7 Cu3 N8 83.0(6) 5_354 2_354
N7 Cu3 N8 97.0(6) . 2_354
N7 Cu3 N8 97.0(6) 5_354 6
N7 Cu3 N8 83.0(6) . 6
N8 Cu3 N8 180.0(16) 2_354 6
N7 Cu3 N8 83.0(6) 5_354 5_354
N7 Cu3 N8 97.0(6) . 5_354
N8 Cu3 N8 90.6(12) 2_354 5_354
N8 Cu3 N8 89.4(12) 6 5_354
N7 Cu3 N8 97.0(6) 5_354 .
N7 Cu3 N8 83.0(6) . .
N8 Cu3 N8 89.4(12) 2_354 .
N8 Cu3 N8 90.6(12) 6 .
N8 Cu3 N8 180.000(2) 5_354 .
N5 Cu4 N5 180.0(10) 7_244 .
N5 Cu4 N6 85.0(6) 7_244 7_244
N5 Cu4 N6 95.0(6) . 7_244
N5 Cu4 N6 95.0(6) 7_244 .
N5 Cu4 N6 85.0(6) . .
N6 Cu4 N6 180.000(2) 7_244 .
N5 Cu4 O4W 88.6(8) 7_244 7_244
N5 Cu4 O4W 91.4(8) . 7_244
N6 Cu4 O4W 83.4(10) 7_244 7_244
N6 Cu4 O4W 96.6(10) . 7_244
N5 Cu4 O4W 91.4(8) 7_244 .
N5 Cu4 O4W 88.6(8) . .
N6 Cu4 O4W 96.6(10) 7_244 .
N6 Cu4 O4W 83.4(10) . .
O4W Cu4 O4W 180.000(2) 7_244 .
C2 C1 N1 115.9(19) . .
C2 C1 H1A 108.3 . .
N1 C1 H1A 108.3 . .
C2 C1 H1B 108.3 . .
N1 C1 H1B 108.3 . .
H1A C1 H1B 107.4 . .
C1 C2 N2 108.9(16) . .
C1 C2 H2A 109.9 . .
N2 C2 H2A 109.9 . .
C1 C2 H2B 109.9 . .
N2 C2 H2B 109.9 . .
H2A C2 H2B 108.3 . .
N3 C3 C6 119(3) . .
C5 C4 N5 116(2) . .
C5 C4 H4A 108.3 . .
N5 C4 H4A 108.3 . .
C5 C4 H4B 108.3 . .
N5 C4 H4B 108.3 . .
H4A C4 H4B 107.4 . .
C4 C5 N6 112(2) . .
C4 C5 H5A 109.3 . .
N6 C5 H5A 109.3 . .
C4 C5 H5B 109.3 . .
N6 C5 H5B 109.3 . .
H5A C5 H5B 108.0 . .
C3 C6 N4 101(3) . 6_545
C3 C6 N4 101(3) . .
N4 C6 N4 52(2) 6_545 .
N8 C7 C8 121(3) . .
C8 C8 N7 69.7(13) 6 .
C8 C8 C7 139.9(18) 6 .
N7 C8 C7 107(2) . .
C1 N1 Cu1 106.9(9) . .
C1 N1 H1C 110.3 . .
Cu1 N1 H1C 110.3 . .
C1 N1 H1D 110.3 . .
Cu1 N1 H1D 110.3 . .
H1C N1 H1D 108.6 . .
C2 N2 Cu1 109.3(10) . .
C2 N2 H2C 109.8 . .
Cu1 N2 H2C 109.8 . .
C2 N2 H2D 109.8 . .
Cu1 N2 H2D 109.8 . .
H2C N2 H2D 108.3 . .
C3 N3 Cu2 117.2(16) . .
N4 N4 C6 63.9(11) 6_545 .
N4 N4 Cu2 68.8(7) 6_545 .
C6 N4 Cu2 105.4(19) . .
C4 N5 Cu4 109.9(11) . .
C4 N5 H5C 109.7 . .
Cu4 N5 H5C 109.7 . .
C4 N5 H5D 109.7 . .
Cu4 N5 H5D 109.7 . .
H5C N5 H5D 108.2 . .
C5 N6 Cu4 109.0(12) . .
C5 N6 H6A 109.9 . .
Cu4 N6 H6A 109.9 . .
C5 N6 H6B 109.9 . .
Cu4 N6 H6B 109.9 . .
H6A N6 H6B 108.3 . .
C8 N7 C8 41(3) 6 .
C8 N7 Cu3 113.1(15) 6 .
C8 N7 Cu3 113.1(15) . .
C7 N8 Cu3 102(2) . .
Si1 O1 Nb4 121.4(5) . .
Si1 O1 Nb1 121.6(5) . .
Nb4 O1 Nb1 99.8(3) . .
Si1 O1 Nb2 123.1(5) . .
Nb4 O1 Nb2 92.0(3) . .
Nb1 O1 Nb2 91.5(3) . .
Nb1 O2 Nb3 136.3(5) . 5_355
Si1 O4 Nb1 121.5(4) . 5_355
Si1 O4 Nb1 121.5(4) . 2_355
Nb1 O4 Nb1 99.3(4) 5_355 2_355
Si1 O4 Nb3 124.2(7) . .
Nb1 O4 Nb3 91.3(4) 5_355 .
Nb1 O4 Nb3 91.3(4) 2_355 .
Nb1 O5 Nb2 135.7(5) . .
V1 O6 Nb1 101.5(3) . .
V1 O6 Nb4 101.7(3) . .
Nb1 O6 Nb4 130.1(4) . .
V1 O10 Nb4 102.0(3) . 6
V1 O10 Nb4 102.0(3) . .
Nb4 O10 Nb4 130.0(5) 6 .
V1 O12 Nb1 101.2(3) . 6
V1 O12 Nb1 101.2(3) . .
Nb1 O12 Nb1 131.8(5) 6 .
Nb4 O13 Nb3 137.5(6) . .
Si1 O14 Nb4 120.5(4) . 5_355
Si1 O14 Nb4 120.5(4) . 2_355
Nb4 O14 Nb4 99.5(4) 5_355 2_355
Si1 O14 Nb3 123.7(6) . 5_355
Nb4 O14 Nb3 93.0(4) 5_355 5_355
Nb4 O14 Nb3 93.0(4) 2_355 5_355
Nb4 O15 Nb2 137.8(5) . .
O5W O4W Cu4 157(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Nb1 O9 1.759(5) .
Nb1 O2 1.890(8) .
Nb1 O5 1.891(7) .
Nb1 O6 2.052(6) .
Nb1 O12 2.067(4) .
Nb1 O1 2.454(9) .
Nb1 O4 2.475(8) 5_355
Nb1 V1 3.0940(15) .
Nb2 O8 1.731(9) .
Nb2 O15 1.955(8) 2_355
Nb2 O15 1.955(8) .
Nb2 O5 1.965(7) .
Nb2 O5 1.965(7) 2_355
Nb2 O1 2.530(9) 2_355
Nb2 O1 2.530(9) .
Nb3 O11 1.740(9) .
Nb3 O2 1.939(7) 5_355
Nb3 O2 1.939(7) 2_355
Nb3 O13 1.963(7) .
Nb3 O13 1.963(7) 6
Nb3 O14 2.483(13) 5_355
Nb3 O4 2.498(13) .
Nb4 O3 1.751(6) .
Nb4 O15 1.871(8) .
Nb4 O13 1.871(8) .
Nb4 O10 2.058(4) .
Nb4 O6 2.066(6) .
Nb4 O1 2.430(9) .
Nb4 O14 2.444(8) 5_355
Nb4 V1 3.1088(16) .
V1 O7 1.624(7) .
V1 O12 1.934(8) .
V1 O10 1.943(8) .
V1 O6 1.943(6) 6
V1 O6 1.943(6) .
V1 Nb1 3.0940(15) 6
V1 Nb4 3.1088(16) 6
Si1 O4 1.633(12) 5_355
Si1 O4 1.633(12) .
Si1 O1 1.656(8) .
Si1 O1 1.656(8) 5_355
Si1 O1 1.656(8) 6
Si1 O1 1.656(8) 2_355
Si1 O14 1.659(13) .
Si1 O14 1.659(13) 5_355
Cu1 N1 1.991(9) 7_345
Cu1 N1 1.991(9) .
Cu1 N2 2.012(12) .
Cu1 N2 2.012(12) 7_345
Cu2 N3 1.96(2) .
Cu2 N3 1.96(2) 5_344
Cu2 N4 2.04(2) 2_354
Cu2 N4 2.04(2) 5_344
Cu2 N4 2.04(2) .
Cu2 N4 2.04(2) 6_545
Cu3 N7 1.957(15) 5_354
Cu3 N7 1.957(15) .
Cu3 N8 2.26(3) 2_354
Cu3 N8 2.26(3) 6
Cu3 N8 2.26(3) 5_354
Cu3 N8 2.26(3) .
Cu4 N5 1.979(14) 7_244
Cu4 N5 1.979(14) .
Cu4 N6 1.973(14) 7_244
Cu4 N6 1.973(14) .
Cu4 O4W 2.32(3) 7_244
Cu4 O4W 2.32(3) .
C1 C2 1.437(10) .
C1 N1 1.44(2) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 N2 1.499(19) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 N3 1.30(4) .
C3 C6 1.52(6) .
C4 C5 1.37(3) .
C4 N5 1.43(2) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 N6 1.50(3) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 N4 1.68(5) 6_545
C6 N4 1.68(5) .
C7 N8 1.37(4) .
C7 C8 1.53(5) .
C8 C8 0.98(6) 6
C8 N7 1.42(3) .
N1 H1C 0.9000 .
N1 H1D 0.9000 .
N2 H2C 0.9000 .
N2 H2D 0.9000 .
N4 N4 1.47(4) 6_545
N5 H5C 0.9000 .
N5 H5D 0.9000 .
N6 H6A 0.9000 .
N6 H6B 0.9000 .
N7 C8 1.42(3) 6
O2 Nb3 1.939(7) 5_355
O4 Nb1 2.475(8) 5_355
O4 Nb1 2.475(8) 2_355
O10 Nb4 2.058(4) 6
O12 Nb1 2.067(4) 6
O14 Nb4 2.444(8) 5_355
O14 Nb4 2.444(8) 2_355
O14 Nb3 2.483(13) 5_355
O3W O3W 1.52(5) 2_355
O4W O5W 1.67(4) .
