#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:45:22 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180052 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/46/7034663.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_7034663
loop_
_publ_author_name
'Zhao, De-Chuan'
'Hu, Yang-Yang'
'Ding, Hong'
'Guo, Hai-Yang'
'Cui, Xiao-Bing'
'Zhang, Xiao'
'Huo, Qi-Sheng'
'Xu, Ji-Qing'
_publ_section_title
;
 Polyoxometalate-based organic-inorganic hybrid compounds containing
 transition metal mixed-organic-ligand complexes of N-containing and
 pyridinecarboxylate ligands.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8971
_journal_page_last               8983
_journal_paper_doi               10.1039/c5dt00201j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C84 H68 Cl6 Cu6 N14 O50 Si W12'
_chemical_formula_weight         4901.69
_chemical_name_systematic
; 
 ? 
;
_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
_audit_update_record
;
2015-03-09 deposited with the CCDC.
2015-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                71.19(3)
_cell_angle_beta                 88.84(3)
_cell_angle_gamma                80.19(3)
_cell_formula_units_Z            1
_cell_length_a                   11.702(2)
_cell_length_b                   14.419(3)
_cell_length_c                   18.071(4)
_cell_measurement_reflns_used    24255
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      3.02
_cell_volume                     2842.1(12)
_computing_data_collection       'Bruker XSCANS'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker P4'
_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  0.0370
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27840
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    13.425
_exptl_absorpt_correction_T_max  0.1961
_exptl_absorpt_correction_T_min  0.1032
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.864
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2247
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.261
_refine_diff_density_min         -1.761
_refine_diff_density_rms         0.279
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     799
_refine_ls_number_reflns         12791
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0284P)²+101.7622P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1295
_reflns_number_gt                10914
_reflns_number_total             12791
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00201j2.cif
_cod_data_source_block           k2
_cod_depositor_comments
'Adding full bibliography for 7034662--7034666.cif.'
_cod_original_cell_volume        2842.1(10)
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               7034663
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
O23 O 0.7154(10) 0.3359(7) 0.1553(6) 0.048(3) Uani 1 1 d .
O24 O 0.6626(9) 0.3031(6) 0.0481(6) 0.042(2) Uani 1 1 d .
N13 N 0.6640(11) 0.6667(8) -0.0450(7) 0.043(3) Uani 1 1 d .
W1 W 0.07448(4) 0.70996(4) 0.53503(3) 0.03017(12) Uani 1 1 d .
W2 W -0.01184(4) 0.72536(3) 0.34480(3) 0.03018(12) Uani 1 1 d .
W3 W 0.18864(5) 0.37087(4) 0.39635(3) 0.03376(13) Uani 1 1 d .
W4 W 0.25899(4) 0.58447(4) 0.42779(3) 0.03500(13) Uani 1 1 d .
W5 W 0.27050(4) 0.36286(4) 0.58505(3) 0.03472(13) Uani 1 1 d .
W6 W 0.08039(4) 0.48597(4) 0.69063(3) 0.02985(12) Uani 1 1 d .
Si1 Si 0.0000 0.5000 0.5000 0.0241(9) Uani 1 2 d S
O1 O 0.0008(12) 0.4414(11) 0.4377(8) 0.019(3) Uani 0.50 1 d P
O2 O 0.0650(13) 0.4320(11) 0.5826(9) 0.026(3) Uani 0.50 1 d P
O3 O 0.1394(12) 0.4609(11) 0.4831(8) 0.020(3) Uani 0.50 1 d P
O4 O 0.0550(12) 0.5994(10) 0.4647(8) 0.019(3) Uani 0.50 1 d P
O5 O 0.2124(12) 0.6622(10) 0.4938(8) 0.078(4) Uani 1 1 d U
O6 O 0.3795(8) 0.6245(8) 0.3933(6) 0.044(2) Uani 1 1 d .
O7 O 0.2783(9) 0.3113(8) 0.3469(6) 0.053(3) Uani 1 1 d .
O8 O 0.3969(8) 0.2941(7) 0.6280(6) 0.047(2) Uani 1 1 d .
O9 O -0.1704(9) 0.7287(9) 0.3684(8) 0.068(4) Uani 1 1 d .
O10 O -0.0830(8) 0.7158(8) 0.5665(7) 0.065(4) Uani 1 1 d .
O11 O 0.1187(10) 0.4793(10) 0.7820(6) 0.062(3) Uani 1 1 d .
O12 O 0.1092(9) 0.8109(8) 0.5511(8) 0.060(3) Uani 1 1 d .
O13 O 0.1502(12) 0.6767(10) 0.3504(8) 0.074(4) Uani 1 1 d U
O14 O -0.0197(11) 0.8332(7) 0.2719(6) 0.055(3) Uani 1 1 d .
O15 O 0.3177(13) 0.4791(11) 0.5210(8) 0.078(4) Uani 1 1 d U
O16 O -0.0287(10) 0.6357(9) 0.2893(9) 0.075(4) Uani 1 1 d .
O17 O 0.1169(12) 0.6099(10) 0.6322(8) 0.071(3) Uani 1 1 d U
O18 O 0.2223(11) 0.4299(10) 0.6573(8) 0.069(3) Uani 1 1 d U
O19 O 0.0752(9) 0.4529(8) 0.3151(7) 0.065(4) Uani 1 1 d .
O20 O 0.2553(13) 0.4867(11) 0.3789(9) 0.081(4) Uani 1 1 d U
O21 O 0.0119(12) 0.7689(10) 0.4305(8) 0.076(4) Uani 1 1 d U
O22 O 0.2632(13) 0.3206(11) 0.4956(9) 0.083(4) Uani 1 1 d U
N1 N 0.6549(10) 0.2856(7) 0.3109(7) 0.038(3) Uani 1 1 d .
N2 N 0.7418(10) 0.0961(7) 0.3403(6) 0.034(2) Uani 1 1 d .
N3 N 0.7024(10) 0.0087(7) 0.1189(6) 0.034(2) Uani 1 1 d .
N4 N 0.7648(10) 0.1424(8) -0.0043(6) 0.038(3) Uani 1 1 d .
N5 N 0.2284(11) 0.1993(10) 0.1731(8) 0.047(3) Uani 1 1 d .
N6 N 0.3515(10) 0.0386(8) 0.1509(7) 0.040(3) Uani 1 1 d .
C1 C 0.6202(14) 0.3836(11) 0.2960(10) 0.051(4) Uani 1 1 d .
H1A H 0.6341 0.4272 0.2474 0.062 Uiso 1 1 calc R
C2 C 0.5639(14) 0.4222(13) 0.3513(11) 0.056(4) Uani 1 1 d .
H2A H 0.5423 0.4906 0.3398 0.068 Uiso 1 1 calc R
C3 C 0.5403(13) 0.3590(12) 0.4227(11) 0.054(4) Uani 1 1 d .
H3A H 0.5014 0.3844 0.4593 0.064 Uiso 1 1 calc R
C4 C 0.5748(12) 0.2565(10) 0.4403(9) 0.042(3) Uani 1 1 d .
C5 C 0.5560(14) 0.1845(11) 0.5118(9) 0.049(4) Uani 1 1 d .
H5A H 0.5142 0.2048 0.5499 0.059 Uiso 1 1 calc R
C6 C 0.5972(15) 0.0875(13) 0.5260(9) 0.058(4) Uani 1 1 d .
H6A H 0.5839 0.0417 0.5737 0.070 Uiso 1 1 calc R
C7 C 0.6620(12) 0.0532(11) 0.4680(8) 0.041(3) Uani 1 1 d .
C8 C 0.7098(16) -0.0485(13) 0.4820(10) 0.059(4) Uani 1 1 d .
H8A H 0.6983 -0.0972 0.5285 0.071 Uiso 1 1 calc R
C9 C 0.7737(15) -0.0718(13) 0.4240(11) 0.059(4) Uani 1 1 d .
H9A H 0.8077 -0.1376 0.4317 0.071 Uiso 1 1 calc R
C10 C 0.7886(14) 0.0014(10) 0.3535(8) 0.046(4) Uani 1 1 d .
H10A H 0.8322 -0.0165 0.3151 0.056 Uiso 1 1 calc R
C11 C 0.6785(12) 0.1206(9) 0.3974(8) 0.036(3) Uani 1 1 d .
C12 C 0.6340(11) 0.2242(9) 0.3826(8) 0.034(3) Uani 1 1 d .
C13 C 0.6738(13) -0.0574(11) 0.1836(8) 0.042(3) Uani 1 1 d .
H13A H 0.6307 -0.0353 0.2204 0.051 Uiso 1 1 calc R
C14 C 0.7066(16) -0.1590(12) 0.1975(9) 0.059(5) Uani 1 1 d .
H14A H 0.6817 -0.2035 0.2420 0.071 Uiso 1 1 calc R
C15 C 0.7740(14) -0.1942(10) 0.1478(9) 0.047(4) Uani 1 1 d .
H15A H 0.7979 -0.2623 0.1584 0.056 Uiso 1 1 calc R
C16 C 0.8071(13) -0.1265(11) 0.0800(10) 0.046(3) Uani 1 1 d .
C17 C 0.8780(13) -0.1549(12) 0.0216(11) 0.054(4) Uani 1 1 d .
H17A H 0.9045 -0.2218 0.0285 0.065 Uiso 1 1 calc R
C18 C 0.9058(13) -0.0854(11) -0.0424(10) 0.049(4) Uani 1 1 d .
H18A H 0.9489 -0.1048 -0.0804 0.058 Uiso 1 1 calc R
C19 C 0.8702(11) 0.0173(10) -0.0530(8) 0.037(3) Uani 1 1 d .
C20 C 0.8989(15) 0.0935(14) -0.1188(9) 0.054(4) Uani 1 1 d .
H20A H 0.9435 0.0777 -0.1577 0.065 Uiso 1 1 calc R
C21 C 0.8605(16) 0.1897(17) -0.1245(9) 0.069(5) Uani 1 1 d .
H21A H 0.8780 0.2407 -0.1675 0.083 Uiso 1 1 calc R
C22 C 0.7945(15) 0.2118(12) -0.0652(9) 0.052(4) Uani 1 1 d .
H22A H 0.7707 0.2781 -0.0690 0.063 Uiso 1 1 calc R
C23 C 0.8026(11) 0.0457(10) 0.0022(8) 0.036(3) Uani 1 1 d .
C24 C 0.7683(12) -0.0254(10) 0.0682(8) 0.038(3) Uani 1 1 d .
C25 C 0.4099(14) -0.0389(10) 0.1341(11) 0.052(4) Uani 1 1 d .
H25A H 0.4523 -0.0274 0.0889 0.063 Uiso 1 1 calc R
C26 C 0.4103(17) -0.1359(11) 0.1808(12) 0.064(5) Uani 1 1 d .
H26A H 0.4500 -0.1891 0.1669 0.076 Uiso 1 1 calc R
C27 C 0.3524(17) -0.1507(14) 0.2458(13) 0.072(5) Uani 1 1 d U
H27A H 0.3572 -0.2154 0.2799 0.087 Uiso 1 1 calc R
C28 C 0.2827(17) -0.0718(15) 0.2661(10) 0.064(5) Uani 1 1 d U
C29 C 0.210(2) -0.084(2) 0.3317(11) 0.095(9) Uani 1 1 d .
H29A H 0.2084 -0.1470 0.3667 0.114 Uiso 1 1 calc R
C30 C 0.144(2) -0.003(2) 0.3430(12) 0.102(10) Uani 1 1 d .
H30A H 0.0983 -0.0116 0.3864 0.122 Uiso 1 1 calc R
C31 C 0.1441(15) 0.0944(18) 0.2886(10) 0.070(6) Uani 1 1 d .
C32 C 0.074(2) 0.178(3) 0.2966(18) 0.111(11) Uani 1 1 d .
H32A H 0.0242 0.1731 0.3381 0.134 Uiso 1 1 calc R
C33 C 0.079(2) 0.267(2) 0.2411(19) 0.105(10) Uani 1 1 d .
H33A H 0.0288 0.3234 0.2439 0.126 Uiso 1 1 calc R
C34 C 0.1584(17) 0.2789(16) 0.1789(14) 0.079(6) Uani 1 1 d .
H34A H 0.1608 0.3414 0.1430 0.095 Uiso 1 1 calc R
C35 C 0.2160(13) 0.1088(15) 0.2258(9) 0.056(5) Uani 1 1 d .
C36 C 0.2868(13) 0.0259(11) 0.2138(8) 0.045(3) Uani 1 1 d .
C37 C 0.7090(19) 0.6302(12) 0.0263(11) 0.070(6) Uani 1 1 d .
H37A H 0.7333 0.6727 0.0496 0.084 Uiso 1 1 calc R
C38 C 0.7216(17) 0.5276(10) 0.0685(9) 0.060(5) Uani 1 1 d .
H38A H 0.7572 0.5025 0.1182 0.073 Uiso 1 1 calc R
C39 C 0.6820(11) 0.4665(10) 0.0367(8) 0.037(3) Uani 1 1 d .
C40 C 0.6341(12) 0.5061(10) -0.0388(8) 0.037(3) Uani 1 1 d .
H40A H 0.6064 0.4657 -0.0628 0.044 Uiso 1 1 calc R
C41 C 0.6280(13) 0.6085(10) -0.0788(9) 0.044(3) Uani 1 1 d .
H41A H 0.5980 0.6351 -0.1300 0.052 Uiso 1 1 calc R
C42 C 0.6873(12) 0.3570(9) 0.0853(8) 0.036(3) Uani 1 1 d .
Cu1 Cu 0.73565(15) 0.21231(12) 0.24259(9) 0.0387(4) Uani 1 1 d .
Cu2 Cu 0.67191(15) 0.15697(12) 0.08847(9) 0.0374(4) Uani 1 1 d .
Cu3 Cu 0.35207(15) 0.18470(11) 0.09657(9) 0.0365(4) Uani 1 1 d .
Cl1 Cl 0.8676(3) 0.1354(3) 0.1791(2) 0.0488(8) Uani 1 1 d .
Cl2 Cl 0.5459(3) 0.1653(3) 0.18728(19) 0.0393(7) Uani 1 1 d .
Cl3 Cl 0.4637(3) 0.1602(3) -0.0011(2) 0.0499(9) Uani 1 1 d .
OW2 O 0.967(3) 0.347(2) 0.0392(18) 0.203(11) Uani 1 1 d U
OW1 O 1.105(4) 0.542(3) 0.125(3) 0.297(17) Uani 1 1 d U
OW3 O 1.299(3) 0.552(3) 0.205(2) 0.261(15) Uani 1 1 d 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'
Cl Cl 0.1484 0.1585 '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'
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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
C42 O23 Cu1 132.9(8) . .
C42 O24 Cu2 126.6(9) . .
C37 N13 C41 120.4(12) . .
C37 N13 Cu3 116.7(10) . 2_665
C41 N13 Cu3 122.9(10) . 2_665
O12 W1 O5 101.3(6) . .
O12 W1 O17 101.9(6) . .
O5 W1 O17 89.4(6) . .
O12 W1 O21 100.0(6) . .
O5 W1 O21 88.0(6) . .
O17 W1 O21 158.0(6) . .
O12 W1 O10 101.5(6) . .
O5 W1 O10 157.2(6) . .
O17 W1 O10 87.7(5) . .
O21 W1 O10 86.3(6) . .
O12 W1 O4 157.6(6) . .
O5 W1 O4 65.0(5) . .
O17 W1 O4 95.8(5) . .
O21 W1 O4 63.4(5) . .
O10 W1 O4 92.8(6) . .
O12 W1 O1 157.7(6) . 2_566
O5 W1 O1 94.3(5) . 2_566
O17 W1 O1 62.1(5) . 2_566
O21 W1 O1 96.4(5) . 2_566
O10 W1 O1 64.4(5) . 2_566
O4 W1 O1 44.7(5) . 2_566
O14 W2 O21 99.6(6) . .
O14 W2 O9 100.3(6) . .
O21 W2 O9 89.5(6) . .
O14 W2 O13 100.7(6) . .
O21 W2 O13 87.7(6) . .
O9 W2 O13 159.0(6) . .
O14 W2 O16 101.7(6) . .
O21 W2 O16 158.7(6) . .
O9 W2 O16 88.0(4) . .
O13 W2 O16 87.1(5) . .
O14 W2 O4 157.8(5) . .
O21 W2 O4 63.6(5) . .
O9 W2 O4 94.1(6) . .
O13 W2 O4 66.1(5) . .
O16 W2 O4 95.5(6) . .
O14 W2 O2 156.6(6) . 2_566
O21 W2 O2 97.9(6) . 2_566
O9 W2 O2 64.3(5) . 2_566
O13 W2 O2 95.5(6) . 2_566
O16 W2 O2 62.1(6) . 2_566
O4 W2 O2 45.5(5) . 2_566
O7 W3 O10 102.2(6) . 2_566
O7 W3 O22 100.8(6) . .
O10 W3 O22 88.6(6) 2_566 .
O7 W3 O20 100.3(6) . .
O10 W3 O20 157.6(6) 2_566 .
O22 W3 O20 88.1(6) . .
O7 W3 O19 101.3(6) . .
O10 W3 O19 88.8(4) 2_566 .
O22 W3 O19 157.8(6) . .
O20 W3 O19 86.0(6) . .
O7 W3 O3 155.8(5) . .
O10 W3 O3 95.3(6) 2_566 .
O22 W3 O3 62.6(6) . .
O20 W3 O3 63.6(5) . .
O19 W3 O3 95.7(6) . .
O7 W3 O1 156.9(5) . .
O10 W3 O1 63.3(5) 2_566 .
O22 W3 O1 96.8(6) . .
O20 W3 O1 95.1(6) . .
O19 W3 O1 62.6(5) . .
O3 W3 O1 47.3(5) . .
O6 W4 O20 100.5(6) . .
O6 W4 O5 101.3(6) . .
O20 W4 O5 158.1(6) . .
O6 W4 O13 99.4(6) . .
O20 W4 O13 90.1(6) . .
O5 W4 O13 87.8(6) . .
O6 W4 O15 100.9(6) . .
O20 W4 O15 88.1(6) . .
O5 W4 O15 86.4(6) . .
O13 W4 O15 159.6(6) . .
O6 W4 O3 155.3(5) . .
O20 W4 O3 62.3(6) . .
O5 W4 O3 96.5(6) . .
O13 W4 O3 98.4(5) . .
O15 W4 O3 63.0(5) . .
O6 W4 O4 156.3(5) . .
O20 W4 O4 96.6(6) . .
O5 W4 O4 63.0(5) . .
O13 W4 O4 64.2(5) . .
O15 W4 O4 95.9(5) . .
O3 W4 O4 48.5(5) . .
O8 W5 O15 102.0(6) . .
O8 W5 O18 100.6(5) . .
O15 W5 O18 88.4(6) . .
O8 W5 O9 99.0(6) . 2_566
O15 W5 O9 159.0(6) . 2_566
O18 W5 O9 88.7(5) . 2_566
O8 W5 O22 100.8(6) . .
O15 W5 O22 89.0(6) . .
O18 W5 O22 158.5(6) . .
O9 W5 O22 86.1(6) 2_566 .
O8 W5 O3 157.5(5) . .
O15 W5 O3 65.0(6) . .
O18 W5 O3 97.3(5) . .
O9 W5 O3 94.8(6) 2_566 .
O22 W5 O3 62.4(6) . .
O8 W5 O2 154.5(5) . .
O15 W5 O2 96.8(6) . .
O18 W5 O2 62.6(5) . .
O9 W5 O2 63.6(5) 2_566 .
O22 W5 O2 96.5(6) . .
O3 W5 O2 47.8(5) . .
O11 W6 O19 100.3(6) . 2_566
O11 W6 O17 101.0(6) . .
O19 W6 O17 88.5(5) 2_566 .
O11 W6 O16 100.7(6) . 2_566
O19 W6 O16 88.0(5) 2_566 2_566
O17 W6 O16 158.2(6) . 2_566
O11 W6 O18 101.2(6) . .
O19 W6 O18 158.5(6) 2_566 .
O17 W6 O18 86.2(6) . .
O16 W6 O18 89.2(5) 2_566 .
O11 W6 O2 157.8(6) . .
O19 W6 O2 95.2(6) 2_566 .
O17 W6 O2 95.1(6) . .
O16 W6 O2 63.9(6) 2_566 .
O18 W6 O2 64.6(5) . .
O11 W6 O1 157.7(6) . 2_566
O19 W6 O1 65.7(5) 2_566 2_566
O17 W6 O1 63.0(5) . 2_566
O16 W6 O1 96.1(6) 2_566 2_566
O18 W6 O1 93.4(5) . 2_566
O2 W6 O1 44.4(5) . 2_566
O4 Si1 O4 180.0(10) . 2_566
O4 Si1 O1 68.7(7) . 2_566
O4 Si1 O1 111.3(7) 2_566 2_566
O4 Si1 O1 111.3(7) . .
O4 Si1 O1 68.7(7) 2_566 .
O1 Si1 O1 180.000(2) 2_566 .
O4 Si1 O2 70.0(7) . 2_566
O4 Si1 O2 110.0(7) 2_566 2_566
O1 Si1 O2 113.2(7) 2_566 2_566
O1 Si1 O2 66.8(7) . 2_566
O4 Si1 O2 110.0(7) . .
O4 Si1 O2 70.0(7) 2_566 .
O1 Si1 O2 66.8(7) 2_566 .
O1 Si1 O2 113.2(7) . .
O2 Si1 O2 180.0(8) 2_566 .
O4 Si1 O3 105.5(7) . 2_566
O4 Si1 O3 74.5(7) 2_566 2_566
O1 Si1 O3 71.8(7) 2_566 2_566
O1 Si1 O3 108.2(7) . 2_566
O2 Si1 O3 71.6(7) 2_566 2_566
O2 Si1 O3 108.4(7) . 2_566
O4 Si1 O3 74.5(7) . .
O4 Si1 O3 105.5(7) 2_566 .
O1 Si1 O3 108.2(7) 2_566 .
O1 Si1 O3 71.8(7) . .
O2 Si1 O3 108.4(7) 2_566 .
O2 Si1 O3 71.6(7) . .
O3 Si1 O3 180.0(9) 2_566 .
Si1 O1 O2 56.8(7) . 2_566
Si1 O1 O4 55.6(6) . 2_566
O2 O1 O4 94.6(9) 2_566 2_566
Si1 O1 W6 124.1(8) . 2_566
O2 O1 W6 67.3(7) 2_566 2_566
O4 O1 W6 135.9(8) 2_566 2_566
Si1 O1 W1 122.7(7) . 2_566
O2 O1 W1 133.5(9) 2_566 2_566
O4 O1 W1 67.2(6) 2_566 2_566
W6 O1 W1 95.7(5) 2_566 2_566
Si1 O1 W3 119.0(7) . .
O2 O1 W3 129.4(8) 2_566 .
O4 O1 W3 125.6(8) 2_566 .
W6 O1 W3 94.4(5) 2_566 .
W1 O1 W3 93.4(5) 2_566 .
Si1 O2 O1 56.4(7) . 2_566
Si1 O2 O4 54.7(6) . 2_566
O1 O2 O4 94.1(9) 2_566 2_566
Si1 O2 W6 124.6(8) . .
O1 O2 W6 68.3(7) 2_566 .
O4 O2 W6 134.4(9) 2_566 .
Si1 O2 W2 121.2(8) . 2_566
O1 O2 W2 134.9(9) 2_566 2_566
O4 O2 W2 66.4(6) 2_566 2_566
W6 O2 W2 96.0(6) . 2_566
Si1 O2 W5 119.2(8) . .
O1 O2 W5 128.3(9) 2_566 .
O4 O2 W5 126.5(9) 2_566 .
W6 O2 W5 94.9(5) . .
W2 O2 W5 93.8(5) 2_566 .
Si1 O3 W5 121.4(7) . .
Si1 O3 W3 121.9(7) . .
W5 O3 W3 97.7(5) . .
Si1 O3 W4 118.1(7) . .
W5 O3 W4 95.6(5) . .
W3 O3 W4 96.3(5) . .
Si1 O4 O1 55.7(6) . 2_566
Si1 O4 O2 55.3(6) . 2_566
O1 O4 O2 94.6(9) 2_566 2_566
Si1 O4 W1 123.8(7) . .
O1 O4 W1 68.1(6) 2_566 .
O2 O4 W1 136.6(9) 2_566 .
Si1 O4 W2 123.3(7) . .
O1 O4 W2 135.1(9) 2_566 .
O2 O4 W2 68.0(6) 2_566 .
W1 O4 W2 95.9(5) . .
Si1 O4 W4 118.9(7) . .
O1 O4 W4 127.6(8) 2_566 .
O2 O4 W4 126.1(8) 2_566 .
W1 O4 W4 93.7(5) . .
W2 O4 W4 93.7(5) . .
W1 O5 W4 138.0(8) . .
W2 O9 W5 138.0(7) . 2_566
W3 O10 W1 138.5(7) 2_566 .
W2 O13 W4 135.9(8) . .
W5 O15 W4 136.3(8) . .
W6 O16 W2 137.5(8) 2_566 .
W6 O17 W1 138.9(8) . .
W5 O18 W6 137.4(7) . .
W6 O19 W3 136.9(7) 2_566 .
W3 O20 W4 137.6(8) . .
W2 O21 W1 136.7(8) . .
W3 O22 W5 137.0(8) . .
C1 N1 C12 117.5(13) . .
C1 N1 Cu1 129.6(11) . .
C12 N1 Cu1 112.8(8) . .
C10 N2 C11 118.3(11) . .
C10 N2 Cu1 129.6(9) . .
C11 N2 Cu1 111.8(8) . .
C13 N3 C24 117.9(12) . .
C13 N3 Cu2 128.7(10) . .
C24 N3 Cu2 113.2(8) . .
C22 N4 C23 118.6(12) . .
C22 N4 Cu2 129.2(10) . .
C23 N4 Cu2 112.2(8) . .
C34 N5 C35 117.2(15) . .
C34 N5 Cu3 131.1(14) . .
C35 N5 Cu3 111.6(10) . .
C25 N6 C36 120.9(13) . .
C25 N6 Cu3 128.7(10) . .
C36 N6 Cu3 110.3(10) . .
N1 C1 C2 121.9(16) . .
N1 C1 H1A 119.1 . .
C2 C1 H1A 119.1 . .
C3 C2 C1 119.9(15) . .
C3 C2 H2A 120.0 . .
C1 C2 H2A 120.0 . .
C2 C3 C4 119.8(14) . .
C2 C3 H3A 120.1 . .
C4 C3 H3A 120.1 . .
C3 C4 C12 116.7(14) . .
C3 C4 C5 124.8(14) . .
C12 C4 C5 118.5(12) . .
C6 C5 C4 121.4(13) . .
C6 C5 H5A 119.3 . .
C4 C5 H5A 119.3 . .
C5 C6 C7 120.8(15) . .
C5 C6 H6A 119.6 . .
C7 C6 H6A 119.6 . .
C11 C7 C8 118.6(13) . .
C11 C7 C6 119.2(13) . .
C8 C7 C6 122.2(14) . .
C9 C8 C7 117.1(16) . .
C9 C8 H8A 121.4 . .
C7 C8 H8A 121.4 . .
C8 C9 C10 121.2(16) . .
C8 C9 H9A 119.4 . .
C10 C9 H9A 119.4 . .
N2 C10 C9 121.3(14) . .
N2 C10 H10A 119.4 . .
C9 C10 H10A 119.4 . .
N2 C11 C7 123.4(11) . .
N2 C11 C12 116.7(12) . .
C7 C11 C12 119.8(12) . .
N1 C12 C4 124.1(12) . .
N1 C12 C11 115.5(12) . .
C4 C12 C11 120.3(12) . .
N3 C13 C14 121.4(14) . .
N3 C13 H13A 119.3 . .
C14 C13 H13A 119.3 . .
C15 C14 C13 121.2(14) . .
C15 C14 H14A 119.4 . .
C13 C14 H14A 119.4 . .
C14 C15 C16 118.6(14) . .
C14 C15 H15A 120.7 . .
C16 C15 H15A 120.7 . .
C15 C16 C24 117.4(14) . .
C15 C16 C17 124.0(14) . .
C24 C16 C17 118.6(15) . .
C18 C17 C16 120.5(14) . .
C18 C17 H17A 119.7 . .
C16 C17 H17A 119.7 . .
C17 C18 C19 120.9(13) . .
C17 C18 H18A 119.6 . .
C19 C18 H18A 119.6 . .
C23 C19 C20 117.5(13) . .
C23 C19 C18 119.4(13) . .
C20 C19 C18 123.1(13) . .
C21 C20 C19 119.1(14) . .
C21 C20 H20A 120.4 . .
C19 C20 H20A 120.4 . .
C20 C21 C22 119.5(15) . .
C20 C21 H21A 120.2 . .
C22 C21 H21A 120.2 . .
N4 C22 C21 122.5(16) . .
N4 C22 H22A 118.7 . .
C21 C22 H22A 118.7 . .
N4 C23 C19 122.7(12) . .
N4 C23 C24 116.3(12) . .
C19 C23 C24 121.0(13) . .
N3 C24 C16 123.3(13) . .
N3 C24 C23 117.1(12) . .
C16 C24 C23 119.5(13) . .
N6 C25 C26 122.7(17) . .
N6 C25 H25A 118.6 . .
C26 C25 H25A 118.6 . .
C27 C26 C25 117.8(18) . .
C27 C26 H26A 121.1 . .
C25 C26 H26A 121.1 . .
C26 C27 C28 122.8(17) . .
C26 C27 H27A 118.6 . .
C28 C27 H27A 118.6 . .
C29 C28 C27 125(2) . .
C29 C28 C36 119(2) . .
C27 C28 C36 115.2(16) . .
C30 C29 C28 120(2) . .
C30 C29 H29A 120.0 . .
C28 C29 H29A 120.0 . .
C29 C30 C31 120.8(19) . .
C29 C30 H30A 119.6 . .
C31 C30 H30A 119.6 . .
C35 C31 C32 117(2) . .
C35 C31 C30 121(2) . .
C32 C31 C30 122(2) . .
C33 C32 C31 118(2) . .
C33 C32 H32A 121.2 . .
C31 C32 H32A 121.2 . .
C32 C33 C34 123(2) . .
C32 C33 H33A 118.5 . .
C34 C33 H33A 118.5 . .
N5 C34 C33 119(2) . .
N5 C34 H34A 120.5 . .
C33 C34 H34A 120.5 . .
N5 C35 C31 125.6(19) . .
N5 C35 C36 115.0(12) . .
C31 C35 C36 119.4(18) . .
N6 C36 C35 119.7(13) . .
N6 C36 C28 120.3(16) . .
C35 C36 C28 119.8(15) . .
N13 C37 C38 121.4(14) . .
N13 C37 H37A 119.3 . .
C38 C37 H37A 119.3 . .
C39 C38 C37 119.7(14) . .
C39 C38 H38A 120.2 . .
C37 C38 H38A 120.2 . .
C38 C39 C40 118.3(13) . .
C38 C39 C42 119.3(12) . .
C40 C39 C42 122.4(12) . .
C39 C40 C41 119.2(12) . .
C39 C40 H40A 120.4 . .
C41 C40 H40A 120.4 . .
N13 C41 C40 121.0(13) . .
N13 C41 H41A 119.5 . .
C40 C41 H41A 119.5 . .
O23 C42 O24 130.2(11) . .
O23 C42 C39 115.0(11) . .
O24 C42 C39 114.8(11) . .
O23 Cu1 N1 89.6(4) . .
O23 Cu1 N2 172.0(5) . .
N1 Cu1 N2 82.4(4) . .
O23 Cu1 Cl1 92.0(4) . .
N1 Cu1 Cl1 165.5(4) . .
N2 Cu1 Cl1 96.0(3) . .
O23 Cu1 Cl2 89.0(3) . .
N1 Cu1 Cl2 98.3(3) . .
N2 Cu1 Cl2 90.9(3) . .
Cl1 Cu1 Cl2 96.13(13) . .
O23 Cu1 Cu2 73.5(3) . .
N1 Cu1 Cu2 137.6(3) . .
N2 Cu1 Cu2 111.7(3) . .
Cl1 Cu1 Cu2 56.37(11) . .
Cl2 Cu1 Cu2 44.27(8) . .
O24 Cu2 N3 171.2(4) . .
O24 Cu2 N4 90.6(4) . .
N3 Cu2 N4 81.2(4) . .
O24 Cu2 Cl2 92.7(3) . .
N3 Cu2 Cl2 95.8(3) . .
N4 Cu2 Cl2 171.9(3) . .
O24 Cu2 Cl1 91.3(3) . .
N3 Cu2 Cl1 86.0(3) . .
N4 Cu2 Cl1 93.2(3) . .
Cl2 Cu2 Cl1 94.02(12) . .
O24 Cu2 Cl3 94.0(3) . .
N3 Cu2 Cl3 88.9(3) . .
N4 Cu2 Cl3 87.3(3) . .
Cl2 Cu2 Cl3 85.17(12) . .
Cl1 Cu2 Cl3 174.70(13) . .
O24 Cu2 Cu1 76.5(3) . .
N3 Cu2 Cu1 106.7(3) . .
N4 Cu2 Cu1 132.6(3) . .
Cl2 Cu2 Cu1 55.35(9) . .
Cl1 Cu2 Cu1 43.00(8) . .
Cl3 Cu2 Cu1 138.15(10) . .
N5 Cu3 N6 82.3(5) . .
N5 Cu3 N13 92.6(5) . 2_665
N6 Cu3 N13 174.3(5) . 2_665
N5 Cu3 Cl3 168.9(4) . .
N6 Cu3 Cl3 94.5(4) . .
N13 Cu3 Cl3 90.0(4) 2_665 .
N5 Cu3 Cl2 99.6(4) . .
N6 Cu3 Cl2 87.8(3) . .
N13 Cu3 Cl2 95.7(4) 2_665 .
Cl3 Cu3 Cl2 90.87(14) . .
Cu1 Cl1 Cu2 80.63(12) . .
Cu2 Cl2 Cu1 80.38(11) . .
Cu2 Cl2 Cu3 93.60(12) . .
Cu1 Cl2 Cu3 159.82(15) . .
Cu3 Cl3 Cu2 89.87(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O23 C42 1.238(16) .
O23 Cu1 1.944(9) .
O24 C42 1.251(16) .
O24 Cu2 1.979(9) .
N13 C37 1.307(19) .
N13 C41 1.311(17) .
N13 Cu3 2.019(10) 2_665
W1 O12 1.688(10) .
W1 O5 1.881(14) .
W1 O17 1.889(13) .
W1 O21 1.907(14) .
W1 O10 1.913(10) .
W1 O4 2.377(14) .
W1 O1 2.393(14) 2_566
W2 O14 1.672(9) .
W2 O21 1.890(14) .
W2 O9 1.892(10) .
W2 O13 1.900(14) .
W2 O16 1.909(11) .
W2 O4 2.377(13) .
W2 O2 2.405(15) 2_566
W3 O7 1.670(9) .
W3 O10 1.869(10) 2_566
W3 O22 1.875(15) .
W3 O20 1.894(15) .
W3 O19 1.935(11) .
W3 O3 2.344(14) .
W3 O1 2.468(14) .
W4 O6 1.649(9) .
W4 O20 1.897(14) .
W4 O5 1.899(14) .
W4 O13 1.907(14) .
W4 O15 1.912(14) .
W4 O3 2.403(14) .
W4 O4 2.458(14) .
W5 O8 1.680(9) .
W5 O15 1.869(14) .
W5 O18 1.886(13) .
W5 O9 1.896(10) 2_566
W5 O22 1.910(14) .
W5 O3 2.333(14) .
W5 O2 2.437(16) .
W6 O11 1.688(10) .
W6 O19 1.872(10) 2_566
W6 O17 1.875(13) .
W6 O16 1.876(11) 2_566
W6 O18 1.895(13) .
W6 O2 2.343(15) .
W6 O1 2.358(14) 2_566
Si1 O4 1.607(13) .
Si1 O4 1.607(13) 2_566
Si1 O1 1.609(13) 2_566
Si1 O1 1.609(13) .
Si1 O2 1.618(16) 2_566
Si1 O2 1.618(16) .
Si1 O3 1.688(14) 2_566
Si1 O3 1.688(14) .
O1 O2 1.78(2) 2_566
O1 O4 1.815(19) 2_566
O1 W6 2.358(14) 2_566
O1 W1 2.393(14) 2_566
O2 O1 1.78(2) 2_566
O2 O4 1.85(2) 2_566
O2 W2 2.405(15) 2_566
O4 O1 1.815(19) 2_566
O4 O2 1.85(2) 2_566
O9 W5 1.896(10) 2_566
O10 W3 1.869(10) 2_566
O16 W6 1.876(11) 2_566
O19 W6 1.872(10) 2_566
N1 C1 1.342(17) .
N1 C12 1.357(17) .
N1 Cu1 1.997(11) .
N2 C10 1.326(17) .
N2 C11 1.363(16) .
N2 Cu1 1.997(10) .
N3 C13 1.327(16) .
N3 C24 1.347(17) .
N3 Cu2 1.997(10) .
N4 C22 1.314(17) .
N4 C23 1.357(17) .
N4 Cu2 2.027(11) .
N5 C34 1.32(2) .
N5 C35 1.37(2) .
N5 Cu3 2.013(12) .
N6 C25 1.326(19) .
N6 C36 1.332(18) .
N6 Cu3 2.019(11) .
C1 C2 1.40(2) .
C1 H1A 0.9300 .
C2 C3 1.37(2) .
C2 H2A 0.9300 .
C3 C4 1.40(2) .
C3 H3A 0.9300 .
C4 C12 1.400(18) .
C4 C5 1.41(2) .
C5 C6 1.34(2) .
C5 H5A 0.9300 .
C6 C7 1.45(2) .
C6 H6A 0.9300 .
C7 C11 1.365(19) .
C7 C8 1.42(2) .
C8 C9 1.37(2) .
C8 H8A 0.9300 .
C9 C10 1.40(2) .
C9 H9A 0.9300 .
C10 H10A 0.9300 .
C11 C12 1.434(17) .
C13 C14 1.39(2) .
C13 H13A 0.9300 .
C14 C15 1.35(2) .
C14 H14A 0.9300 .
C15 C16 1.39(2) .
C15 H15A 0.9300 .
C16 C24 1.398(19) .
C16 C17 1.45(2) .
C17 C18 1.34(2) .
C17 H17A 0.9300 .
C18 C19 1.419(19) .
C18 H18A 0.9300 .
C19 C23 1.381(18) .
C19 C20 1.41(2) .
C20 C21 1.35(3) .
C20 H20A 0.9300 .
C21 C22 1.39(2) .
C21 H21A 0.9300 .
C22 H22A 0.9300 .
C23 C24 1.402(19) .
C25 C26 1.38(2) .
C25 H25A 0.9300 .
C26 C27 1.32(3) .
C26 H26A 0.9300 .
C27 C28 1.43(3) .
C27 H27A 0.9300 .
C28 C29 1.43(3) .
C28 C36 1.43(2) .
C29 C30 1.35(4) .
C29 H29A 0.9300 .
C30 C31 1.44(3) .
C30 H30A 0.9300 .
C31 C35 1.38(2) .
C31 C32 1.38(3) .
C32 C33 1.37(4) .
C32 H32A 0.9300 .
C33 C34 1.43(3) .
C33 H33A 0.9300 .
C34 H34A 0.9300 .
C35 C36 1.41(2) .
C37 C38 1.413(19) .
C37 H37A 0.9300 .
C38 C39 1.342(19) .
C38 H38A 0.9300 .
C39 C40 1.386(18) .
C39 C42 1.530(17) .
C40 C41 1.408(18) .
C40 H40A 0.9300 .
C41 H41A 0.9300 .
Cu1 Cl1 2.258(4) .
Cu1 Cl2 2.726(4) .
Cu1 Cu2 3.266(2) .
Cu2 Cl2 2.313(4) .
Cu2 Cl1 2.757(4) .
Cu2 Cl3 2.938(5) .
Cu3 N13 2.019(10) 2_665
Cu3 Cl3 2.257(4) .
Cu3 Cl2 2.748(4) .
