# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_1
_database_code_depnum_ccdc_archive 'CCDC 1419955'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;

# start Validation Reply Form

_vrf_PLAT306_shelx_1             
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... Ow2 Check

RESPONSE: The hydrogens of the water molecule were not added.
;

_vrf_PLAT342_shelx_1             
;
PROBLEM: Low Bond Precision on C-C Bonds .........0.0328 Ang

RESPONSE: The quality of this crystal was poor.
;

# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H34 Cu3 Ge N7 O45.50 W12'
_chemical_formula_weight         3762.11

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'
Cu Cu 0.3201 1.2651 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   23.410(3)
_cell_length_b                   12.9698(16)
_cell_length_c                   22.779(3)
_cell_angle_alpha                90
_cell_angle_beta                 109.576(2)
_cell_angle_gamma                90
_cell_volume                     6516.3(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2030
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      22.29

_exptl_crystal_description       block
_exptl_crystal_colour            Lyons_blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.835
_exptl_crystal_F_000             6680
_exptl_transmission_factor_min   0.031
_exptl_transmission_factor_max   0.052
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    22.600
_shelx_estimated_absorpt_T_min   0.088
_shelx_estimated_absorpt_T_max   0.123
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            33282
_diffrn_reflns_av_unetI/netI     0.1212
_diffrn_reflns_av_R_equivalents  0.1032
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.821
_diffrn_reflns_theta_max         25.043
_diffrn_reflns_theta_full        25.043
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             11518
_reflns_number_gt                6957
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0205P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11518
_refine_ls_number_parameters     946
_refine_ls_number_restraints     210
_refine_ls_R_factor_all          0.1084
_refine_ls_R_factor_gt           0.0526
_refine_ls_wR_factor_ref         0.0992
_refine_ls_wR_factor_gt          0.0848
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      0.999
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
W1 W 0.36290(4) 0.09247(6) 0.14501(4) 0.0181(2) Uani 1 1 d . . . . .
W2 W 0.40760(4) -0.00427(6) 0.28930(4) 0.0194(2) Uani 1 1 d . . . . .
W3 W 0.19944(4) 0.13477(6) 0.05890(4) 0.0217(2) Uani 1 1 d . . . . .
W4 W 0.27866(4) 0.30183(6) 0.19494(4) 0.0217(2) Uani 1 1 d . . . . .
W5 W 0.17162(4) -0.11115(6) 0.08135(4) 0.0221(2) Uani 1 1 d . . . . .
W6 W 0.22079(4) -0.22312(6) 0.24164(5) 0.0261(2) Uani 1 1 d . . . . .
W7 W 0.09560(4) 0.07561(6) 0.12478(4) 0.0224(2) Uani 1 1 d . . . . .
W8 W 0.29342(4) -0.07306(7) 0.36293(4) 0.0259(2) Uani 1 1 d . . . . .
W9 W 0.17604(4) 0.23930(6) 0.26111(4) 0.0227(2) Uani 1 1 d . . . . .
W10 W 0.32373(4) 0.20339(7) 0.33945(4) 0.0262(2) Uani 1 1 d . . . . .
W11 W 0.14518(4) -0.03524(6) 0.28563(4) 0.0233(2) Uani 1 1 d . . . . .
W12 W 0.33487(4) -0.15531(6) 0.16735(4) 0.0194(2) Uani 1 1 d . . . . .
Ge1 Ge 0.25117(9) 0.03718(15) 0.21276(10) 0.0146(5) Uani 1 1 d . . . . .
Cu3 Cu 0.15127(11) -0.27899(18) -0.06972(12) 0.0228(6) Uani 1 1 d . . . . .
Cu2 Cu 0.07709(11) -0.49604(17) -0.07470(12) 0.0222(6) Uani 1 1 d . . . . .
Cu1 Cu 0.46100(11) -0.68339(19) 0.12480(12) 0.0249(6) Uani 1 1 d . . . . .
O40 O 0.4034(5) -0.1274(9) 0.2403(6) 0.017(3) Uani 1 1 d . U . . .
O39 O 0.1186(6) 0.1493(9) 0.0625(6) 0.024(3) Uani 1 1 d . U . . .
O41 O 0.2115(5) -0.3704(9) -0.0142(6) 0.016(3) Uani 1 1 d . . . . .
O38 O 0.2567(5) -0.1321(9) 0.1064(6) 0.019(3) Uani 1 1 d . U . . .
O37 O 0.2570(6) 0.1598(9) 0.2437(6) 0.020(3) Uani 1 1 d . . . . .
O36 O 0.4058(5) 0.1451(9) 0.1047(6) 0.018(3) Uani 1 1 d . U . . .
O35 O 0.3693(5) -0.0485(9) 0.1275(6) 0.018(3) Uani 1 1 d . . . . .
O34 O 0.2824(5) 0.0995(9) 0.0876(6) 0.017(3) Uani 1 1 d . U . . .
O33 O 0.3197(5) 0.0036(9) 0.2067(6) 0.022(3) Uani 1 1 d . . . . .
O32 O 0.3603(6) -0.0714(9) 0.3320(6) 0.025(3) Uani 1 1 d . . . . .
O31 O 0.2956(6) 0.4191(9) 0.1712(7) 0.029(4) Uani 1 1 d . . . . .
O30 O 0.4248(5) 0.0695(9) 0.2241(6) 0.023(3) Uani 1 1 d . . . . .
O43 O 0.0852(5) -0.3505(9) -0.0596(6) 0.023(3) Uani 1 1 d . . . . .
O29 O 0.1785(6) -0.0022(9) 0.0275(6) 0.021(3) Uani 1 1 d . . . . .
O42 O 0.1656(5) -0.5255(9) -0.0385(6) 0.017(3) Uani 1 1 d . . . . .
O28 O 0.2116(5) -0.0572(9) 0.3612(6) 0.019(3) Uani 1 1 d . U . . .
O27 O 0.1295(6) 0.1856(9) 0.1821(6) 0.022(3) Uani 1 1 d . U . . .
O26 O 0.3297(6) 0.3043(9) 0.2817(6) 0.028(4) Uani 1 1 d . . . . .
O25 O 0.2101(6) 0.3370(9) 0.2182(6) 0.022(3) Uani 1 1 d . U . . .
O24 O 0.4795(6) -0.0203(9) 0.3411(6) 0.025(3) Uani 1 1 d . . . . .
O23 O 0.3404(5) 0.2145(9) 0.1818(6) 0.023(3) Uani 1 1 d . . . . .
O22 O 0.2336(6) -0.0494(9) 0.2608(6) 0.023(3) Uani 1 1 d . . . . .
O21 O 0.0868(6) -0.0413(10) 0.3150(6) 0.027(3) Uani 1 1 d . U . . .
O20 O 0.2699(6) -0.2086(10) 0.3266(7) 0.036(4) Uani 1 1 d . . . . .
O19 O 0.0218(6) 0.1024(10) 0.1005(6) 0.030(4) Uani 1 1 d . . . . .
O18 O 0.2906(6) -0.2093(9) 0.2166(6) 0.024(3) Uani 1 1 d . . . . .
O17 O 0.0958(6) -0.0513(9) 0.0805(6) 0.023(3) Uani 1 1 d . U . . .
O16 O 0.1959(5) 0.0329(9) 0.1413(6) 0.019(3) Uani 1 1 d . U . . .
O1W O 0.4431(6) -0.6607(10) 0.2017(7) 0.034(4) Uani 1 1 d . . . . .
HW1A H 0.4596 -0.6537 0.2409 0.052 Uiso 1 1 d R U . . .
HW2A H 0.4077 -0.6847 0.1948 0.052 Uiso 1 1 d R U . . .
O15 O 0.3827(6) 0.1216(10) 0.3159(6) 0.028(4) Uani 1 1 d . . . . .
O14 O 0.3684(6) 0.2575(10) 0.4090(6) 0.033(4) Uani 1 1 d . U . . .
O13 O 0.1935(6) 0.1961(10) -0.0089(6) 0.033(4) Uani 1 1 d . . . . .
O12 O 0.3291(7) -0.1063(11) 0.4395(7) 0.045(5) Uani 1 1 d . . . . .
O11 O 0.3598(6) -0.2606(10) 0.1397(7) 0.036(4) Uani 1 1 d . . . . .
O10 O 0.3008(6) 0.0737(9) 0.3654(6) 0.022(3) Uani 1 1 d . . . . .
O9 O 0.2086(6) -0.3520(10) 0.2388(7) 0.036(4) Uani 1 1 d . . . . .
O8 O 0.1525(6) -0.1760(9) 0.2643(6) 0.025(4) Uani 1 1 d . . . . .
O7 O 0.2465(6) 0.2582(11) 0.3336(7) 0.032(4) Uani 1 1 d . . . . .
O6 O 0.1767(6) -0.1808(9) 0.1565(7) 0.029(4) Uani 1 1 d . . . . .
O5 O 0.1050(6) -0.0041(10) 0.1989(6) 0.028(4) Uani 1 1 d . . . . .
O4 O 0.1243(6) 0.3162(10) 0.2763(7) 0.032(4) Uani 1 1 d . . . . .
O3 O 0.2256(6) 0.2431(9) 0.1200(6) 0.029(4) Uani 1 1 d . . . . .
O2 O 0.1629(6) 0.1100(10) 0.2940(6) 0.025(3) Uani 1 1 d . . . . .
N6 N 0.3818(7) -0.6165(12) 0.0774(7) 0.020(4) Uani 1 1 d . . . . .
N5 N 0.2121(7) -0.1730(12) -0.0708(8) 0.027(4) Uani 1 1 d . U . . .
C2 C 0.2106(9) -0.4683(14) -0.0145(9) 0.017(5) Uani 1 1 d . U . . .
N4 N -0.0129(7) -0.4913(12) -0.0888(8) 0.030(5) Uani 1 1 d . . . . .
N3 N 0.5309(7) -0.7821(11) 0.1624(8) 0.020(4) Uani 1 1 d . . . . .
O1 O 0.1446(7) -0.2074(11) 0.0277(7) 0.044(4) Uani 1 1 d . . . . .
C1 C 0.1297(9) -0.1174(15) -0.1580(10) 0.023(5) Uani 1 1 d . U . . .
N2 N 0.1001(8) -0.1999(12) -0.1433(8) 0.026(4) Uani 1 1 d . . . . .
N1 N 0.0579(7) -0.6428(12) -0.0961(9) 0.029(5) Uani 1 1 d . . . . .
C33 C 0.3694(9) -0.5160(14) 0.0896(9) 0.019(5) Uani 1 1 d . U . . .
H33A H 0.3997 -0.4794 0.1192 0.023 Uiso 1 1 calc R U . . .
N10 N 0.4936(8) -0.6868(12) 0.0563(8) 0.031(5) Uani 1 1 d . . . . .
C31 C 0.5430(9) -0.8290(14) 0.2175(9) 0.020(5) Uani 1 1 d . U . . .
H31A H 0.5204 -0.8145 0.2432 0.024 Uiso 1 1 calc R U . . .
C30 C 0.2703(8) -0.5184(13) 0.0174(9) 0.015(4) Uani 1 1 d . U . . .
C29 C 0.0957(8) -0.7130(13) -0.1015(9) 0.017(5) Uani 1 1 d . . . . .
H29A H 0.1352 -0.6929 -0.0961 0.021 Uiso 1 1 calc R U . . .
C34 C 0.1902(9) -0.0986(14) -0.1161(9) 0.020(5) Uani 1 1 d . U . . .
C28 C 0.3164(9) -0.4678(15) 0.0614(9) 0.025(5) Uani 1 1 d . U . . .
H28A H 0.3111 -0.4000 0.0719 0.031 Uiso 1 1 calc R U . . .
C27 C -0.0410(9) -0.5831(14) -0.1015(9) 0.020(5) Uani 1 1 d . U . . .
C26 C -0.1075(10) -0.4149(18) -0.0927(11) 0.045(7) Uani 1 1 d . . . . .
H26A H -0.1294 -0.3564 -0.0898 0.054 Uiso 1 1 calc R U . . .
C25 C 0.0805(9) -0.8166(15) -0.1147(10) 0.029(5) Uani 1 1 d . U . . .
H25A H 0.1088 -0.8666 -0.1153 0.035 Uiso 1 1 calc R U . . .
C24 C -0.0008(9) -0.6708(14) -0.1061(10) 0.023(5) Uani 1 1 d . . . . .
C23 C 0.5652(8) -0.8008(16) 0.1268(10) 0.026(5) Uani 1 1 d . . . . .
C22 C 0.3366(10) -0.6595(15) 0.0332(10) 0.028(5) Uani 1 1 d . . . . .
H22A H 0.3440 -0.7247 0.0203 0.033 Uiso 1 1 calc R U . . .
C21 C 0.2806(9) -0.6203(14) 0.0040(9) 0.024(5) Uani 1 1 d . U . . .
H21A H 0.2502 -0.6597 -0.0237 0.028 Uiso 1 1 calc R U . . .
C20 C 0.0431(9) -0.2208(15) -0.1771(10) 0.027(5) Uani 1 1 d . . . . .
H20A H 0.0233 -0.2760 -0.1663 0.032 Uiso 1 1 calc R U . . .
C38 C 0.2795(11) 0.0041(18) -0.0721(11) 0.041(6) Uani 1 1 d . U . . .
H38A H 0.3013 0.0645 -0.0708 0.049 Uiso 1 1 calc R U . . .
C19 C 0.5900(11) -0.8996(18) 0.2354(12) 0.050(7) Uani 1 1 d . U . . .
H19A H 0.5971 -0.9350 0.2727 0.060 Uiso 1 1 calc R U . . .
C18 C -0.0452(10) -0.4074(17) -0.0839(11) 0.042(7) Uani 1 1 d . . . . .
H18A H -0.0259 -0.3438 -0.0746 0.050 Uiso 1 1 calc R U . . .
C17 C 0.4717(10) -0.6308(15) 0.0011(10) 0.032(6) Uani 1 1 d . U . . .
H17A H 0.4384 -0.5878 -0.0053 0.038 Uiso 1 1 calc R U . . .
C16 C -0.1033(10) -0.5934(17) -0.1097(10) 0.037(6) Uani 1 1 d . U . . .
H16A H -0.1223 -0.6573 -0.1179 0.044 Uiso 1 1 calc R U . . .
C15 C 0.0126(10) -0.1603(16) -0.2290(10) 0.033(6) Uani 1 1 d . U . . .
H15A H -0.0270 -0.1759 -0.2535 0.039 Uiso 1 1 calc R U . . .
C14 C 0.5417(10) -0.7470(16) 0.0640(12) 0.037(6) Uani 1 1 d . . . . .
C13 C 0.0970(11) -0.0581(17) -0.2109(10) 0.040(6) Uani 1 1 d . . . . .
H13A H 0.1152 -0.0024 -0.2233 0.048 Uiso 1 1 calc R U . . .
C12 C 0.6140(10) -0.8669(16) 0.1446(11) 0.035(6) Uani 1 1 d . U . . .
H12A H 0.6380 -0.8758 0.1196 0.042 Uiso 1 1 calc R U . . .
C11 C -0.1349(10) -0.5067(16) -0.1053(10) 0.035(6) Uani 1 1 d . . . . .
H11A H -0.1760 -0.5117 -0.1112 0.042 Uiso 1 1 calc R U . . .
C10 C -0.0203(10) -0.7681(16) -0.1204(12) 0.049(8) Uani 1 1 d . . . . .
H10A H -0.0602 -0.7864 -0.1257 0.059 Uiso 1 1 calc R U . . .
C9 C 0.0403(11) -0.0829(18) -0.2425(12) 0.045(6) Uani 1 1 d . U . . .
H9A H 0.0192 -0.0420 -0.2763 0.054 Uiso 1 1 calc R U . . .
C8 C 0.6267(12) -0.920(2) 0.2003(13) 0.062(8) Uani 1 1 d . U . . .
H8A H 0.6585 -0.9669 0.2135 0.074 Uiso 1 1 calc R U . . .
C37 C 0.2656(9) -0.1577(15) -0.0303(10) 0.026(5) Uani 1 1 d . U . . .
H37A H 0.2815 -0.2097 -0.0012 0.031 Uiso 1 1 calc R U . . .
C36 C 0.3004(9) -0.0732(15) -0.0265(10) 0.026(5) Uani 1 1 d . . . . .
H36A H 0.3373 -0.0662 0.0055 0.031 Uiso 1 1 calc R U . . .
C7 C 0.5480(14) -0.701(2) -0.0334(15) 0.069(9) Uani 1 1 d . . . . .
H7A H 0.5659 -0.7059 -0.0641 0.083 Uiso 1 1 calc R U . . .
C6 C 0.0198(11) -0.8385(19) -0.1270(11) 0.050(7) Uani 1 1 d . U . . .
H6A H 0.0060 -0.9045 -0.1403 0.059 Uiso 1 1 calc R U . . .
C35 C 0.2238(11) -0.0150(17) -0.1198(11) 0.047(7) Uani 1 1 d . . . . .
H35A H 0.2101 0.0296 -0.1536 0.056 Uiso 1 1 calc R U . . .
C5 C 0.4985(11) -0.6376(18) -0.0441(12) 0.048(7) Uani 1 1 d . U . . .
H5A H 0.4834 -0.6003 -0.0810 0.058 Uiso 1 1 calc R U . . .
C4 C 0.5726(11) -0.758(2) 0.0211(13) 0.053(8) Uani 1 1 d . . . . .
H4A H 0.6067 -0.7992 0.0285 0.064 Uiso 1 1 calc R U . . .
O2W O 0.4978(10) -0.642(2) 0.3248(10) 0.135(10) Uani 1 1 d . . . . .
O3W O 0.4387(18) 0.442(3) 0.4911(19) 0.086(13) Uani 0.5 1 d . U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O36 1.713(11) . ?
W1 O35 1.888(12) . ?
W1 O34 1.902(12) . ?
W1 O30 1.920(13) . ?
W1 O23 1.944(12) . ?
W1 O33 2.297(12) . ?
W2 O24 1.714(13) . ?
W2 O15 1.899(12) . ?
W2 O32 1.911(12) . ?
W2 O30 1.919(13) . ?
W2 O40 1.932(12) . ?
W2 O33 2.279(13) . ?
W3 O13 1.700(13) . ?
W3 O34 1.886(12) . ?
W3 O29 1.916(12) . ?
W3 O3 1.927(13) . ?
W3 O39 1.931(12) . ?
W3 O16 2.319(12) . ?
W4 O31 1.705(12) . ?
W4 O3 1.902(14) . ?
W4 O25 1.907(12) . ?
W4 O23 1.937(12) . ?
W4 O26 1.937(13) . ?
W4 O37 2.293(12) . ?
W5 O1 1.712(13) . ?
W5 O38 1.898(12) . ?
W5 O6 1.904(14) . ?
W5 O29 1.913(12) . ?
W5 O17 1.931(12) . ?
W5 O16 2.271(12) . ?
W6 O9 1.694(13) . ?
W6 O20 1.900(15) . ?
W6 O18 1.912(12) . ?
W6 O8 1.936(12) . ?
W6 O6 1.946(15) . ?
W6 O22 2.295(12) . ?
W7 O19 1.664(13) . ?
W7 O27 1.917(12) . ?
W7 O5 1.928(13) . ?
W7 O39 1.932(12) . ?
W7 O17 1.931(12) . ?
W7 O16 2.317(12) . ?
W8 O12 1.718(14) . ?
W8 O10 1.911(12) . ?
W8 O28 1.914(12) . ?
W8 O32 1.920(12) . ?
W8 O20 1.942(14) . ?
W8 O22 2.299(13) . ?
W9 O4 1.692(12) . ?
W9 O27 1.896(13) . ?
W9 O2 1.904(13) . ?
W9 O7 1.919(13) . ?
W9 O25 1.928(12) . ?
W9 O37 2.307(12) . ?
W10 O14 1.727(14) . ?
W10 O26 1.893(12) . ?
W10 O7 1.905(12) . ?
W10 O10 1.918(12) . ?
W10 O15 1.954(13) . ?
W10 O37 2.289(13) . ?
W11 O21 1.711(12) . ?
W11 O8 1.912(12) . ?
W11 O28 1.915(13) . ?
W11 O2 1.924(13) . ?
W11 O5 1.926(14) . ?
W11 O22 2.329(12) . ?
W12 O11 1.688(13) . ?
W12 O18 1.897(12) . ?
W12 O38 1.915(12) . ?
W12 O40 1.918(12) . ?
W12 O35 1.971(12) . ?
W12 O33 2.322(12) . ?
Ge1 O16 1.708(13) . ?
Ge1 O22 1.711(11) . ?
Ge1 O33 1.712(12) . ?
Ge1 O37 1.726(12) . ?
Cu3 O43 1.883(12) . ?
Cu3 O41 1.949(12) . ?
Cu3 N5 1.985(16) . ?
Cu3 N2 1.989(17) . ?
Cu2 O43 1.916(12) . ?
Cu2 N1 1.979(16) . ?
Cu2 O42 1.993(12) . ?
Cu2 N4 2.024(16) . ?
Cu1 O1W 1.955(13) . ?
Cu1 N10 1.954(18) . ?
Cu1 N6 2.004(16) . ?
Cu1 N3 2.028(15) . ?
O41 C2 1.27(2) . ?
O42 C2 1.26(2) . ?
N6 C22 1.32(2) . ?
N6 C33 1.38(2) . ?
N5 C37 1.30(2) . ?
N5 C34 1.38(2) . ?
C2 C30 1.49(2) . ?
N4 C27 1.34(2) . ?
N4 C18 1.35(2) . ?
N3 C31 1.34(2) . ?
N3 C23 1.34(2) . ?
C1 N2 1.38(2) . ?
C1 C13 1.42(3) . ?
C1 C34 1.44(3) . ?
N2 C20 1.33(2) . ?
N1 C29 1.30(2) . ?
N1 C24 1.37(2) . ?
C33 C28 1.34(2) . ?
N10 C14 1.33(2) . ?
N10 C17 1.39(2) . ?
C31 C19 1.38(3) . ?
C30 C28 1.37(3) . ?
C30 C21 1.40(2) . ?
C29 C25 1.40(2) . ?
C34 C35 1.36(3) . ?
C27 C16 1.41(3) . ?
C27 C24 1.50(2) . ?
C26 C11 1.34(3) . ?
C26 C18 1.41(3) . ?
C25 C6 1.38(3) . ?
C24 C10 1.34(3) . ?
C23 C12 1.38(3) . ?
C23 C14 1.52(3) . ?
C22 C21 1.35(3) . ?
C20 C15 1.40(3) . ?
C38 C36 1.41(3) . ?
C38 C35 1.41(3) . ?
C19 C8 1.38(3) . ?
C17 C5 1.38(3) . ?
C16 C11 1.37(3) . ?
C15 C9 1.29(3) . ?
C14 C4 1.40(3) . ?
C13 C9 1.32(3) . ?
C12 C8 1.39(3) . ?
C10 C6 1.35(3) . ?
C37 C36 1.35(2) . ?
C7 C5 1.37(3) . ?
C7 C4 1.39(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
_geom_angle_publ_flag
O36 W1 O35 99.8(5) . . ?
O36 W1 O34 103.6(5) . . ?
O35 W1 O34 91.8(5) . . ?
O36 W1 O30 99.9(5) . . ?
O35 W1 O30 87.7(5) . . ?
O34 W1 O30 156.2(5) . . ?
O36 W1 O23 101.4(5) . . ?
O35 W1 O23 158.7(5) . . ?
O34 W1 O23 84.8(5) . . ?
O30 W1 O23 87.1(5) . . ?
O36 W1 O33 170.0(5) . . ?
O35 W1 O33 74.1(5) . . ?
O34 W1 O33 84.7(5) . . ?
O30 W1 O33 72.3(5) . . ?
O23 W1 O33 84.6(5) . . ?
O24 W2 O15 102.7(6) . . ?
O24 W2 O32 101.4(6) . . ?
O15 W2 O32 86.4(5) . . ?
O24 W2 O30 100.4(6) . . ?
O15 W2 O30 89.1(5) . . ?
O32 W2 O30 158.2(5) . . ?
O24 W2 O40 98.4(5) . . ?
O15 W2 O40 158.9(5) . . ?
O32 W2 O40 89.4(5) . . ?
O30 W2 O40 87.1(5) . . ?
O24 W2 O33 168.7(5) . . ?
O15 W2 O33 86.3(5) . . ?
O32 W2 O33 85.6(5) . . ?
O30 W2 O33 72.8(5) . . ?
O40 W2 O33 72.7(5) . . ?
O13 W3 O34 100.9(6) . . ?
O13 W3 O29 99.3(6) . . ?
O34 W3 O29 90.5(5) . . ?
O13 W3 O3 103.0(6) . . ?
O34 W3 O3 83.4(5) . . ?
O29 W3 O3 157.6(5) . . ?
O13 W3 O39 102.0(6) . . ?
O34 W3 O39 156.8(5) . . ?
O29 W3 O39 88.5(5) . . ?
O3 W3 O39 88.7(5) . . ?
O13 W3 O16 170.7(6) . . ?
O34 W3 O16 83.9(5) . . ?
O29 W3 O16 72.5(5) . . ?
O3 W3 O16 85.4(5) . . ?
O39 W3 O16 73.7(5) . . ?
O31 W4 O3 103.0(6) . . ?
O31 W4 O25 100.5(5) . . ?
O3 W4 O25 89.3(5) . . ?
O31 W4 O23 102.0(5) . . ?
O3 W4 O23 85.6(5) . . ?
O25 W4 O23 157.5(5) . . ?
O31 W4 O26 100.3(6) . . ?
O3 W4 O26 156.4(5) . . ?
O25 W4 O26 90.1(6) . . ?
O23 W4 O26 86.0(6) . . ?
O31 W4 O37 169.3(6) . . ?
O3 W4 O37 85.9(5) . . ?
O25 W4 O37 73.4(5) . . ?
O23 W4 O37 84.4(4) . . ?
O26 W4 O37 71.3(5) . . ?
O1 W5 O38 102.1(6) . . ?
O1 W5 O6 101.1(6) . . ?
O38 W5 O6 85.4(5) . . ?
O1 W5 O29 99.9(6) . . ?
O38 W5 O29 89.6(5) . . ?
O6 W5 O29 159.0(5) . . ?
O1 W5 O17 99.7(6) . . ?
O38 W5 O17 158.2(5) . . ?
O6 W5 O17 88.8(5) . . ?
O29 W5 O17 88.3(5) . . ?
O1 W5 O16 170.6(6) . . ?
O38 W5 O16 84.9(5) . . ?
O6 W5 O16 85.5(5) . . ?
O29 W5 O16 73.7(5) . . ?
O17 W5 O16 73.7(5) . . ?
O9 W6 O20 100.0(6) . . ?
O9 W6 O18 103.4(6) . . ?
O20 W6 O18 90.5(6) . . ?
O9 W6 O8 100.3(6) . . ?
O20 W6 O8 88.2(6) . . ?
O18 W6 O8 156.2(5) . . ?
O9 W6 O6 102.3(6) . . ?
O20 W6 O6 157.6(5) . . ?
O18 W6 O6 84.1(5) . . ?
O8 W6 O6 88.1(5) . . ?
O9 W6 O22 170.4(6) . . ?
O20 W6 O22 73.3(5) . . ?
O18 W6 O22 83.9(5) . . ?
O8 W6 O22 72.9(5) . . ?
O6 W6 O22 84.5(5) . . ?
O19 W7 O27 102.6(6) . . ?
O19 W7 O5 101.8(6) . . ?
O27 W7 O5 84.4(5) . . ?
O19 W7 O39 99.6(6) . . ?
O27 W7 O39 88.8(5) . . ?
O5 W7 O39 158.5(5) . . ?
O19 W7 O17 100.9(6) . . ?
O27 W7 O17 156.5(5) . . ?
O5 W7 O17 88.8(5) . . ?
O39 W7 O17 89.3(5) . . ?
O19 W7 O16 170.5(5) . . ?
O27 W7 O16 84.3(5) . . ?
O5 W7 O16 85.2(5) . . ?
O39 W7 O16 73.8(5) . . ?
O17 W7 O16 72.6(5) . . ?
O12 W8 O10 102.2(6) . . ?
O12 W8 O28 101.0(6) . . ?
O10 W8 O28 88.5(5) . . ?
O12 W8 O32 101.3(6) . . ?
O10 W8 O32 85.6(5) . . ?
O28 W8 O32 157.6(6) . . ?
O12 W8 O20 100.2(7) . . ?
O10 W8 O20 157.5(6) . . ?
O28 W8 O20 87.1(5) . . ?
O32 W8 O20 90.1(5) . . ?
O12 W8 O22 170.2(6) . . ?
O10 W8 O22 85.2(5) . . ?
O28 W8 O22 72.5(5) . . ?
O32 W8 O22 85.5(5) . . ?
O20 W8 O22 72.5(5) . . ?
O4 W9 O27 100.8(6) . . ?
O4 W9 O2 102.6(6) . . ?
O27 W9 O2 86.1(5) . . ?
O4 W9 O7 102.5(6) . . ?
O27 W9 O7 156.7(5) . . ?
O2 W9 O7 88.8(6) . . ?
O4 W9 O25 99.3(6) . . ?
O27 W9 O25 87.9(5) . . ?
O2 W9 O25 158.0(5) . . ?
O7 W9 O25 88.3(6) . . ?
O4 W9 O37 170.0(5) . . ?
O27 W9 O37 85.2(5) . . ?
O2 W9 O37 85.7(5) . . ?
O7 W9 O37 71.7(5) . . ?
O25 W9 O37 72.7(5) . . ?
O14 W10 O26 101.2(6) . . ?
O14 W10 O7 100.5(6) . . ?
O26 W10 O7 89.0(6) . . ?
O14 W10 O10 102.7(6) . . ?
O26 W10 O10 156.0(5) . . ?
O7 W10 O10 89.5(6) . . ?
O14 W10 O15 101.9(6) . . ?
O26 W10 O15 87.8(6) . . ?
O7 W10 O15 157.6(6) . . ?
O10 W10 O15 84.5(5) . . ?
O14 W10 O37 170.0(5) . . ?
O26 W10 O37 72.2(5) . . ?
O7 W10 O37 72.4(5) . . ?
O10 W10 O37 84.6(5) . . ?
O15 W10 O37 85.6(5) . . ?
O21 W11 O8 102.0(6) . . ?
O21 W11 O28 99.0(6) . . ?
O8 W11 O28 88.3(5) . . ?
O21 W11 O2 100.3(6) . . ?
O8 W11 O2 157.7(5) . . ?
O28 W11 O2 88.5(5) . . ?
O21 W11 O5 103.4(6) . . ?
O8 W11 O5 89.7(5) . . ?
O28 W11 O5 157.5(5) . . ?
O2 W11 O5 84.9(5) . . ?
O21 W11 O22 169.0(5) . . ?
O8 W11 O22 72.5(5) . . ?
O28 W11 O22 71.7(5) . . ?
O2 W11 O22 85.5(5) . . ?
O5 W11 O22 86.3(5) . . ?
O11 W12 O18 104.3(6) . . ?
O11 W12 O38 102.9(6) . . ?
O18 W12 O38 84.7(5) . . ?
O11 W12 O40 100.5(6) . . ?
O18 W12 O40 91.2(5) . . ?
O38 W12 O40 156.5(5) . . ?
O11 W12 O35 98.7(6) . . ?
O18 W12 O35 157.0(5) . . ?
O38 W12 O35 89.7(5) . . ?
O40 W12 O35 85.1(5) . . ?
O11 W12 O33 168.3(5) . . ?
O18 W12 O33 85.1(5) . . ?
O38 W12 O33 84.7(5) . . ?
O40 W12 O33 71.9(5) . . ?
O35 W12 O33 72.1(4) . . ?
O16 Ge1 O22 108.7(6) . . ?
O16 Ge1 O33 110.2(6) . . ?
O22 Ge1 O33 108.5(6) . . ?
O16 Ge1 O37 110.5(6) . . ?
O22 Ge1 O37 110.3(6) . . ?
O33 Ge1 O37 108.6(6) . . ?
O43 Cu3 O41 93.8(5) . . ?
O43 Cu3 N5 164.7(6) . . ?
O41 Cu3 N5 93.6(6) . . ?
O43 Cu3 N2 94.0(6) . . ?
O41 Cu3 N2 164.1(6) . . ?
N5 Cu3 N2 82.2(7) . . ?
O43 Cu2 N1 172.8(6) . . ?
O43 Cu2 O42 95.1(5) . . ?
N1 Cu2 O42 92.0(6) . . ?
O43 Cu2 N4 91.9(6) . . ?
N1 Cu2 N4 81.5(6) . . ?
O42 Cu2 N4 162.6(6) . . ?
O1W Cu1 N10 167.7(6) . . ?
O1W Cu1 N6 88.9(6) . . ?
N10 Cu1 N6 96.8(7) . . ?
O1W Cu1 N3 95.8(6) . . ?
N10 Cu1 N3 81.2(7) . . ?
N6 Cu1 N3 166.2(6) . . ?
W12 O40 W2 121.5(6) . . ?
W3 O39 W7 120.1(7) . . ?
C2 O41 Cu3 126.7(12) . . ?
W5 O38 W12 153.1(7) . . ?
Ge1 O37 W10 123.5(6) . . ?
Ge1 O37 W4 122.9(6) . . ?
W10 O37 W4 94.1(4) . . ?
Ge1 O37 W9 121.7(6) . . ?
W10 O37 W9 93.6(4) . . ?
W4 O37 W9 93.0(4) . . ?
W1 O35 W12 120.6(6) . . ?
W3 O34 W1 156.5(7) . . ?
Ge1 O33 W2 123.8(7) . . ?
Ge1 O33 W1 122.6(6) . . ?
W2 O33 W1 93.8(4) . . ?
Ge1 O33 W12 121.7(6) . . ?
W2 O33 W12 93.8(4) . . ?
W1 O33 W12 93.1(4) . . ?
W2 O32 W8 151.0(7) . . ?
W2 O30 W1 121.1(6) . . ?
Cu3 O43 Cu2 120.0(6) . . ?
W5 O29 W3 120.8(7) . . ?
C2 O42 Cu2 132.2(12) . . ?
W8 O28 W11 122.7(6) . . ?
W9 O27 W7 153.5(7) . . ?
W10 O26 W4 122.3(6) . . ?
W4 O25 W9 120.9(6) . . ?
W4 O23 W1 150.1(7) . . ?
Ge1 O22 W6 124.6(7) . . ?
Ge1 O22 W8 122.6(7) . . ?
W6 O22 W8 93.3(4) . . ?
Ge1 O22 W11 121.8(6) . . ?
W6 O22 W11 93.1(4) . . ?
W8 O22 W11 93.1(4) . . ?
W6 O20 W8 120.8(7) . . ?
W12 O18 W6 154.4(7) . . ?
W5 O17 W7 120.0(6) . . ?
Ge1 O16 W5 123.8(6) . . ?
Ge1 O16 W7 123.4(6) . . ?
W5 O16 W7 93.6(4) . . ?
Ge1 O16 W3 122.1(6) . . ?
W5 O16 W3 93.0(4) . . ?
W7 O16 W3 92.4(4) . . ?
W2 O15 W10 151.1(7) . . ?
W8 O10 W10 153.7(7) . . ?
W11 O8 W6 121.4(6) . . ?
W10 O7 W9 122.3(7) . . ?
W5 O6 W6 151.9(7) . . ?
W11 O5 W7 152.2(7) . . ?
W4 O3 W3 153.4(7) . . ?
W9 O2 W11 151.8(7) . . ?
C22 N6 C33 112.6(17) . . ?
C22 N6 Cu1 126.2(14) . . ?
C33 N6 Cu1 121.2(13) . . ?
C37 N5 C34 116.9(17) . . ?
C37 N5 Cu3 128.5(15) . . ?
C34 N5 Cu3 113.9(13) . . ?
O42 C2 O41 127.2(18) . . ?
O42 C2 C30 117.9(16) . . ?
O41 C2 C30 115.0(16) . . ?
C27 N4 C18 119.1(18) . . ?
C27 N4 Cu2 114.5(13) . . ?
C18 N4 Cu2 126.4(15) . . ?
C31 N3 C23 120.3(18) . . ?
C31 N3 Cu1 124.9(13) . . ?
C23 N3 Cu1 114.9(14) . . ?
N2 C1 C13 117.0(19) . . ?
N2 C1 C34 115.8(18) . . ?
C13 C1 C34 127.2(19) . . ?
C20 N2 C1 120.6(18) . . ?
C20 N2 Cu3 126.1(14) . . ?
C1 N2 Cu3 113.3(14) . . ?
C29 N1 C24 118.4(17) . . ?
C29 N1 Cu2 126.2(13) . . ?
C24 N1 Cu2 115.4(12) . . ?
C28 C33 N6 124.4(19) . . ?
C14 N10 C17 117.7(19) . . ?
C14 N10 Cu1 116.5(15) . . ?
C17 N10 Cu1 125.8(15) . . ?
N3 C31 C19 118.3(19) . . ?
C28 C30 C21 117.6(18) . . ?
C28 C30 C2 121.9(17) . . ?
C21 C30 C2 120.6(17) . . ?
N1 C29 C25 124.1(18) . . ?
C35 C34 N5 122(2) . . ?
C35 C34 C1 124(2) . . ?
N5 C34 C1 114.5(17) . . ?
C33 C28 C30 120.1(19) . . ?
N4 C27 C16 121.3(18) . . ?
N4 C27 C24 114.5(17) . . ?
C16 C27 C24 124.2(18) . . ?
C11 C26 C18 119(2) . . ?
C6 C25 C29 114(2) . . ?
C10 C24 N1 122.1(18) . . ?
C10 C24 C27 123.9(19) . . ?
N1 C24 C27 114.0(16) . . ?
N3 C23 C12 123(2) . . ?
N3 C23 C14 112.7(18) . . ?
C12 C23 C14 124(2) . . ?
N6 C22 C21 128(2) . . ?
C22 C21 C30 117.2(19) . . ?
N2 C20 C15 120.3(19) . . ?
C36 C38 C35 116(2) . . ?
C8 C19 C31 123(3) . . ?
N4 C18 C26 121(2) . . ?
C5 C17 N10 121(2) . . ?
C11 C16 C27 118(2) . . ?
C9 C15 C20 119(2) . . ?
N10 C14 C4 125(2) . . ?
N10 C14 C23 114.6(19) . . ?
C4 C14 C23 120(2) . . ?
C9 C13 C1 119(2) . . ?
C23 C12 C8 119(2) . . ?
C26 C11 C16 121(2) . . ?
C24 C10 C6 118(2) . . ?
C15 C9 C13 124(3) . . ?
C19 C8 C12 117(3) . . ?
N5 C37 C36 126(2) . . ?
C37 C36 C38 119(2) . . ?
C5 C7 C4 123(3) . . ?
C10 C6 C25 123(2) . . ?
C34 C35 C38 120(2) . . ?
C7 C5 C17 118(3) . . ?
C7 C4 C14 114(3) . . ?

_refine_diff_density_max         2.668
_refine_diff_density_min         -2.197
_refine_diff_density_rms         0.410



####################################################################### 
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# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_2
_database_code_depnum_ccdc_archive 'CCDC 1419956'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;

# start Validation Reply Form

_vrf_PLAT306_shelx_2             
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1w Check

RESPONSE: The hydrogens of the water molecule were not added.
;

_vrf_PLAT342_shelx_2             
;
PROBLEM: Low Bond Precision on C-C Bonds .........0.0230 Ang

RESPONSE: The quality of this crystal was poor.
;

_vrf_PLAT430_shelx_2             
;
PROBLEM: Short Inter D...A Contact O1w .. N7 .. 2.78 Ang.

RESPONSE: There should be a strong hydrogen bond between the
two atoms.
;

# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H46 Cl4 Cu4 Ge N10 O46 W12'
_chemical_formula_weight         4317.82

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'
Cu Cu 0.3201 1.2651 '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'
W W -0.8490 6.8722 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   20.681(4)
_cell_length_b                   13.187(3)
_cell_length_c                   32.788(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8942(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    61214
_cell_measurement_theta_min      3.02
_cell_measurement_theta_max      27.45

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.207
_exptl_crystal_F_000             7792
_exptl_transmission_factor_min   0.201
_exptl_transmission_factor_max   1.000
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    16.839
_shelx_estimated_absorpt_T_min   0.088
_shelx_estimated_absorpt_T_max   0.187
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            79213
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_av_R_equivalents  0.0905
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         3.087
_diffrn_reflns_theta_max         27.491
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10201
_reflns_number_gt                8736
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0195P)²+481.1118P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10201
_refine_ls_number_parameters     637
_refine_ls_number_restraints     474
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0626
_refine_ls_wR_factor_ref         0.1300
_refine_ls_wR_factor_gt          0.1250
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

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
W1 W 0.54866(3) 0.65717(4) 0.08179(2) 0.02507(13) Uani 1 1 d . . . . .
W2 W 0.35769(3) 0.55775(5) -0.05543(2) 0.02567(13) Uani 1 1 d . . . . .
W3 W 0.40712(3) 0.71567(4) 0.02618(2) 0.02982(14) Uani 1 1 d . . . . .
W4 W 0.63780(3) 0.65626(5) -0.01061(2) 0.03810(17) Uani 1 1 d . . . . .
W5 W 0.59026(3) 0.49787(6) -0.09230(2) 0.03980(18) Uani 1 1 d . . . . .
W6 W 0.49650(4) 0.71274(5) -0.06602(2) 0.04430(19) Uani 1 1 d . . . . .
Ge1 Ge 0.5000 0.5000 0.0000 0.0204(4) Uani 1 2 d S . P . .
O1 O 0.5483(11) 0.5749(18) -0.0339(7) 0.044(3) Uani 0.5 1 d . U P . .
O2 O 0.5628(10) 0.5452(17) 0.0260(6) 0.038(3) Uani 0.5 1 d . U P . .
O3 O 0.5524(9) 0.4077(14) 0.0174(6) 0.027(3) Uani 0.5 1 d . U P . .
O4 O 0.4785(11) 0.5798(19) 0.0369(7) 0.044(3) Uani 0.5 1 d . U P . .
Cu2 Cu 0.62307(8) 0.31903(14) -0.27657(5) 0.0289(4) Uani 1 1 d . . . . .
Cu1 Cu 0.51167(7) 0.48550(14) -0.29012(5) 0.0254(4) Uani 1 1 d . . . . .
Cl2 Cl 0.60487(16) 0.5106(3) -0.25558(12) 0.0354(8) Uani 1 1 d . . . . .
Cl1 Cl 0.51512(17) 0.2882(3) -0.27840(13) 0.0388(9) Uani 1 1 d . . . . .
O19 O 0.6275(5) 0.3537(9) -0.3343(3) 0.036(2) Uani 1 1 d . U . . .
N5 N 0.4539(5) 0.5186(9) -0.2432(3) 0.025(2) Uani 1 1 d . . . . .
N4 N 0.7194(5) 0.2957(10) -0.2779(4) 0.029(3) Uani 1 1 d . . . . .
O17 O 0.7028(6) 0.7317(9) -0.0147(4) 0.047(3) Uani 1 1 d . U . . .
O16 O 0.6322(5) 0.4969(11) -0.1354(3) 0.046(3) Uani 1 1 d . U . . .
O18 O 0.5571(5) 0.4828(8) -0.3422(3) 0.032(2) Uani 1 1 d . U . . .
N2 N 0.4271(5) 0.4869(10) -0.3210(4) 0.030(3) Uani 1 1 d . . . . .
N7 N 0.6747(7) 0.4787(11) -0.4719(4) 0.040(3) Uani 1 1 d . . . . .
O15 O 0.3631(6) 0.8189(10) 0.0380(5) 0.059(3) Uani 1 1 d . U . . .
O14 O 0.3777(6) 0.6179(11) 0.0646(4) 0.059(3) Uani 1 1 d . U . . .
O13 O 0.6725(6) 0.5456(9) 0.0196(4) 0.052(3) Uani 1 1 d . U . . .
C21 C 0.6004(7) 0.4247(11) -0.3540(4) 0.029(3) Uani 1 1 d . . . . .
C20 C 0.6269(7) 0.4443(11) -0.3964(4) 0.030(3) Uani 1 1 d . . . . .
N1 N 0.6366(6) 0.2766(10) -0.2185(4) 0.035(3) Uani 1 1 d . . . . .
O12 O 0.4928(5) 0.8126(9) -0.0967(3) 0.041(3) Uani 1 1 d . U . . .
O11 O 0.4566(7) 0.7643(12) -0.0189(4) 0.066(3) Uani 1 1 d . U . . .
O10 O 0.5714(8) 0.7330(10) 0.1202(4) 0.067(4) Uani 1 1 d . U . . .
O9 O 0.5744(8) 0.7305(12) -0.0367(5) 0.076(3) Uani 1 1 d . U . . .
C19 C 0.3118(7) 0.4990(12) -0.3101(5) 0.034(3) Uani 1 1 d . . . . .
O8 O 0.4178(8) 0.6459(12) -0.0797(4) 0.069(3) Uani 1 1 d . U . . .
C18 C 0.6651(6) 0.3727(12) -0.4153(4) 0.029(3) Uani 1 1 d . . . . .
H18A H 0.6753 0.3125 -0.4019 0.034 Uiso 1 1 calc R U . . .
C17 C 0.2616(7) 0.5146(12) -0.2813(6) 0.040(4) Uani 1 1 d . . . . .
H17A H 0.2189 0.5119 -0.2900 0.047 Uiso 1 1 calc R U . . .
O7 O 0.2916(6) 0.5857(13) -0.0826(4) 0.067(4) Uani 1 1 d . U . . .
C16 C 0.3021(8) 0.4793(13) -0.3515(5) 0.041(4) Uani 1 1 d . . . . .
H16A H 0.2605 0.4744 -0.3621 0.049 Uiso 1 1 calc R U . . .
C15 C 0.7221(9) 0.2396(11) -0.1695(5) 0.042(4) Uani 1 1 d . . . . .
C14 C 0.7456(7) 0.2742(11) -0.2410(5) 0.034(3) Uani 1 1 d . . . . .
O5 O 0.6029(7) 0.7072(10) 0.0389(4) 0.058(3) Uani 1 1 d . U . . .
C13 C 0.3543(8) 0.4673(14) -0.3758(5) 0.047(4) Uani 1 1 d . . . . .
H13A H 0.3483 0.4568 -0.4036 0.056 Uiso 1 1 calc R U . . .
O35 O 0.6467(8) 0.5747(12) -0.0574(5) 0.078(3) Uani 1 1 d . U . . .
C12 C 0.6881(7) 0.3911(12) -0.4543(4) 0.034(3) Uani 1 1 d . . . . .
H12A H 0.7126 0.3425 -0.4678 0.041 Uiso 1 1 calc R U . . .
C11 C 0.4204(9) 0.5564(13) -0.1754(5) 0.045(4) Uani 1 1 d . . . . .
H11A H 0.4323 0.5671 -0.1483 0.054 Uiso 1 1 calc R U . . .
O32 O 0.5372(8) 0.6118(13) -0.0965(5) 0.082(3) Uani 1 1 d . U . . .
C10 C 0.8325(9) 0.2334(13) -0.1945(6) 0.049(4) Uani 1 1 d . . . . .
H10A H 0.8763 0.2227 -0.1898 0.059 Uiso 1 1 calc R U . . .
C9 C 0.3395(7) 0.5383(12) -0.2267(5) 0.032(3) Uani 1 1 d . . . . .
C8 C 0.3763(7) 0.5016(10) -0.2965(4) 0.025(3) Uani 1 1 d . . . . .
C7 C 0.3895(7) 0.5200(10) -0.2545(4) 0.025(3) Uani 1 1 d . . . . .
C6 C 0.6994(8) 0.2638(11) -0.2084(5) 0.034(3) Uani 1 1 d . . . . .
C5 C 0.6736(11) 0.2285(13) -0.1393(5) 0.055(6) Uani 1 1 d . . . . .
H5A H 0.6852 0.2138 -0.1125 0.066 Uiso 1 1 calc R U . . .
C4 C 0.7598(7) 0.3019(14) -0.3099(5) 0.040(4) Uani 1 1 d . . . . .
H4A H 0.7432 0.3176 -0.3355 0.048 Uiso 1 1 calc R U . . .
C3 C 0.3585(8) 0.5584(13) -0.1860(5) 0.038(4) Uani 1 1 d . . . . .
H3A H 0.3273 0.5733 -0.1665 0.045 Uiso 1 1 calc R U . . .
C2 C 0.4680(7) 0.5379(12) -0.2050(4) 0.032(3) Uani 1 1 d . . . . .
H2A H 0.5113 0.5395 -0.1972 0.038 Uiso 1 1 calc R U . . .
C1 C 0.7902(10) 0.2253(14) -0.1630(6) 0.053(5) Uani 1 1 d . . . . .
H1A H 0.8054 0.2104 -0.1370 0.063 Uiso 1 1 calc R U . . .
C30 C 0.8514(8) 0.2628(13) -0.2687(6) 0.047(5) Uani 1 1 d . . . . .
H30A H 0.8954 0.2505 -0.2659 0.057 Uiso 1 1 calc R U . . .
C29 C 0.5934(9) 0.2657(14) -0.1893(6) 0.049(5) Uani 1 1 d . . . . .
H29A H 0.5500 0.2759 -0.1955 0.059 Uiso 1 1 calc R U . . .
C28 C 0.6139(10) 0.5330(16) -0.4158(5) 0.057(6) Uani 1 1 d . . . . .
H28A H 0.5880 0.5814 -0.4032 0.069 Uiso 1 1 calc R U . . .
C27 C 0.4173(8) 0.4705(13) -0.3601(5) 0.041(4) Uani 1 1 d . . . . .
H27A H 0.4524 0.4608 -0.3774 0.049 Uiso 1 1 calc R U . . .
C26 C 0.8111(8) 0.2580(12) -0.2346(5) 0.039(4) Uani 1 1 d . . . . .
C25 C 0.6102(10) 0.2392(15) -0.1495(5) 0.050(5) Uani 1 1 d . . . . .
H25A H 0.5782 0.2289 -0.1300 0.060 Uiso 1 1 calc R U . . .
C24 C 0.8272(8) 0.2850(16) -0.3056(6) 0.052(5) Uani 1 1 d . . . . .
H24A H 0.8543 0.2892 -0.3281 0.063 Uiso 1 1 calc R U . . .
C23 C 0.6389(13) 0.5521(16) -0.4544(7) 0.078(8) Uani 1 1 d . . . . .
H23A H 0.6313 0.6133 -0.4676 0.094 Uiso 1 1 calc R U . . .
O1W O 0.7328(5) 0.5643(9) -0.5400(3) 0.039(3) Uani 1 1 d . . . . .
O36 O 0.6060(6) 0.5479(9) 0.0880(4) 0.055(3) Uani 1 1 d . U . . .
C50 C 0.2744(7) 0.5330(12) -0.2418(5) 0.037(4) Uani 1 1 d . . . . .
H50A H 0.2403 0.5426 -0.2237 0.045 Uiso 1 1 calc R U . . .
O34 O 0.5152(6) 0.4227(11) -0.1067(5) 0.066(3) Uani 1 1 d . U . . .
O33 O 0.3506(8) 0.6503(12) -0.0118(4) 0.069(3) Uani 1 1 d . U . . .
O30 O 0.4815(6) 0.7372(12) 0.0589(4) 0.065(3) Uani 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O10 1.677(12) . ?
W1 O34 1.877(13) 5_665 ?
W1 O36 1.877(12) . ?
W1 O30 1.898(13) . ?
W1 O5 1.915(12) . ?
W1 O4 2.31(2) . ?
W1 O2 2.37(2) . ?
W2 O7 1.674(11) . ?
W2 O8 1.879(13) . ?
W2 O33 1.886(13) . ?
W2 O13 1.904(11) 5_665 ?
W2 O36 1.909(12) 5_665 ?
W2 O3 2.29(2) 5_665 ?
W2 O2 2.34(2) 5_665 ?
W3 O15 1.683(12) . ?
W3 O30 1.897(14) . ?
W3 O14 1.903(11) . ?
W3 O11 1.909(13) . ?
W3 O33 1.914(13) . ?
W3 O3 2.322(18) 5_665 ?
W3 O4 2.35(2) . ?
W4 O17 1.677(11) . ?
W4 O9 1.847(14) . ?
W4 O35 1.882(15) . ?
W4 O5 1.900(13) . ?
W4 O13 1.904(12) . ?
W4 O1 2.27(2) . ?
W4 O2 2.45(2) . ?
W5 O16 1.660(10) . ?
W5 O32 1.865(16) . ?
W5 O14 1.896(13) 5_665 ?
W5 O34 1.901(14) . ?
W5 O35 1.924(15) . ?
W5 O1 2.33(2) . ?
W5 O4 2.52(2) 5_665 ?
W6 O12 1.659(11) . ?
W6 O32 1.864(15) . ?
W6 O11 1.878(14) . ?
W6 O9 1.891(14) . ?
W6 O8 1.904(14) . ?
W6 O1 2.36(2) . ?
W6 O3 2.467(18) 5_665 ?
Ge1 O4 1.66(2) . ?
Ge1 O4 1.66(2) 5_665 ?
Ge1 O2 1.66(2) 5_665 ?
Ge1 O2 1.66(2) . ?
Ge1 O3 1.726(18) 5_665 ?
Ge1 O3 1.726(18) . ?
Ge1 O1 1.79(2) 5_665 ?
Ge1 O1 1.79(2) . ?
O2 W2 2.34(2) 5_665 ?
O3 W2 2.29(2) 5_665 ?
O3 W3 2.322(18) 5_665 ?
O3 W6 2.467(18) 5_665 ?
O4 W5 2.52(2) 5_665 ?
Cu2 O19 1.950(11) . ?
Cu2 N1 2.003(12) . ?
Cu2 N4 2.016(11) . ?
Cu2 Cl1 2.270(4) . ?
Cu2 Cl2 2.645(4) . ?
Cu1 O18 1.949(9) . ?
Cu1 N5 1.997(11) . ?
Cu1 N2 2.022(11) . ?
Cu1 Cl2 2.260(4) . ?
Cu1 Cl1 2.630(4) . ?
O19 C21 1.267(18) . ?
N5 C2 1.311(17) . ?
N5 C7 1.381(17) . ?
N4 C4 1.343(18) . ?
N4 C14 1.357(19) . ?
O18 C21 1.240(16) . ?
N2 C27 1.314(18) . ?
N2 C8 1.337(17) . ?
N7 C12 1.32(2) . ?
N7 C23 1.35(2) . ?
O14 W5 1.896(13) 5_665 ?
O13 W2 1.904(11) 5_665 ?
C21 C20 1.519(19) . ?
C20 C28 1.36(2) . ?
C20 C18 1.38(2) . ?
N1 C29 1.32(2) . ?
N1 C6 1.350(19) . ?
C19 C16 1.40(2) . ?
C19 C8 1.41(2) . ?
C19 C17 1.42(2) . ?
C18 C12 1.386(19) . ?
C17 C50 1.35(2) . ?
C16 C13 1.35(2) . ?
C15 C6 1.40(2) . ?
C15 C5 1.42(3) . ?
C15 C1 1.44(3) . ?
C14 C26 1.39(2) . ?
C14 C6 1.44(2) . ?
C13 C27 1.40(2) . ?
C11 C3 1.33(2) . ?
C11 C2 1.40(2) . ?
C10 C1 1.36(3) . ?
C10 C26 1.43(2) . ?
C9 C7 1.401(19) . ?
C9 C3 1.41(2) . ?
C9 C50 1.44(2) . ?
C8 C7 1.426(18) . ?
C5 C25 1.36(3) . ?
C4 C24 1.42(2) . ?
C30 C24 1.34(3) . ?
C30 C26 1.40(2) . ?
C29 C25 1.40(2) . ?
C28 C23 1.39(2) . ?
O36 W2 1.909(12) 5_665 ?
O34 W1 1.877(13) 5_665 ?

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
_geom_angle_publ_flag
O10 W1 O34 101.9(8) . 5_665 ?
O10 W1 O36 101.5(7) . . ?
O34 W1 O36 88.0(5) 5_665 . ?
O10 W1 O30 99.9(7) . . ?
O34 W1 O30 88.3(6) 5_665 . ?
O36 W1 O30 158.6(7) . . ?
O10 W1 O5 100.4(7) . . ?
O34 W1 O5 157.7(7) 5_665 . ?
O36 W1 O5 88.5(5) . . ?
O30 W1 O5 87.0(6) . . ?
O10 W1 O4 157.1(8) . . ?
O34 W1 O4 65.6(7) 5_665 . ?
O36 W1 O4 97.3(8) . . ?
O30 W1 O4 62.1(8) . . ?
O5 W1 O4 93.0(7) . . ?
O10 W1 O2 156.6(8) . . ?
O34 W1 O2 94.2(8) 5_665 . ?
O36 W1 O2 61.8(6) . . ?
O30 W1 O2 97.5(7) . . ?
O5 W1 O2 64.9(7) . . ?
O4 W1 O2 46.3(8) . . ?
O7 W2 O8 100.3(8) . . ?
O7 W2 O33 101.4(7) . . ?
O8 W2 O33 88.4(6) . . ?
O7 W2 O13 102.6(7) . 5_665 ?
O8 W2 O13 157.1(7) . 5_665 ?
O33 W2 O13 88.3(6) . 5_665 ?
O7 W2 O36 100.7(7) . 5_665 ?
O8 W2 O36 87.3(6) . 5_665 ?
O33 W2 O36 158.0(7) . 5_665 ?
O13 W2 O36 87.2(5) 5_665 5_665 ?
O7 W2 O3 155.8(8) . 5_665 ?
O8 W2 O3 64.5(7) . 5_665 ?
O33 W2 O3 61.4(7) . 5_665 ?
O13 W2 O3 94.2(6) 5_665 5_665 ?
O36 W2 O3 97.5(6) 5_665 5_665 ?
O7 W2 O2 157.2(8) . 5_665 ?
O8 W2 O2 94.0(8) . 5_665 ?
O33 W2 O2 96.8(8) . 5_665 ?
O13 W2 O2 63.9(7) 5_665 5_665 ?
O36 W2 O2 62.0(7) 5_665 5_665 ?
O3 W2 O2 47.1(7) 5_665 5_665 ?
O15 W3 O30 100.8(7) . . ?
O15 W3 O14 102.9(7) . . ?
O30 W3 O14 89.2(5) . . ?
O15 W3 O11 101.4(7) . . ?
O30 W3 O11 87.3(6) . . ?
O14 W3 O11 155.8(7) . . ?
O15 W3 O33 100.6(7) . . ?
O30 W3 O33 158.6(7) . . ?
O14 W3 O33 86.0(6) . . ?
O11 W3 O33 88.5(6) . . ?
O15 W3 O3 154.7(7) . 5_665 ?
O30 W3 O3 99.2(7) . 5_665 ?
O14 W3 O3 92.8(7) . 5_665 ?
O11 W3 O3 64.2(6) . 5_665 ?
O33 W3 O3 60.3(7) . 5_665 ?
O15 W3 O4 157.4(7) . . ?
O30 W3 O4 61.3(8) . . ?
O14 W3 O4 65.5(7) . . ?
O11 W3 O4 92.0(8) . . ?
O33 W3 O4 97.9(8) . . ?
O3 W3 O4 48.0(7) 5_665 . ?
O17 W4 O9 102.6(7) . . ?
O17 W4 O35 101.2(7) . . ?
O9 W4 O35 89.8(6) . . ?
O17 W4 O5 99.4(6) . . ?
O9 W4 O5 86.5(6) . . ?
O35 W4 O5 159.3(7) . . ?
O17 W4 O13 101.2(6) . . ?
O9 W4 O13 156.2(7) . . ?
O35 W4 O13 87.1(6) . . ?
O5 W4 O13 88.2(5) . . ?
O17 W4 O1 155.0(7) . . ?
O9 W4 O1 61.1(8) . . ?
O35 W4 O1 62.4(8) . . ?
O5 W4 O1 98.3(7) . . ?
O13 W4 O1 96.9(7) . . ?
O17 W4 O2 154.4(7) . . ?
O9 W4 O2 95.4(7) . . ?
O35 W4 O2 96.8(8) . . ?
O5 W4 O2 63.4(7) . . ?
O13 W4 O2 61.6(6) . . ?
O1 W4 O2 50.6(8) . . ?
O16 W5 O32 104.6(7) . . ?
O16 W5 O14 102.6(6) . 5_665 ?
O32 W5 O14 152.8(7) . 5_665 ?
O16 W5 O34 102.2(6) . . ?
O32 W5 O34 85.5(7) . . ?
O14 W5 O34 89.1(5) 5_665 . ?
O16 W5 O35 101.2(7) . . ?
O32 W5 O35 88.7(6) . . ?
O14 W5 O35 85.8(6) 5_665 . ?
O34 W5 O35 156.6(7) . . ?
O16 W5 O1 153.7(8) . . ?
O32 W5 O1 59.4(7) . . ?
O14 W5 O1 95.0(7) 5_665 . ?
O34 W5 O1 97.3(8) . . ?
O35 W5 O1 60.6(8) . . ?
O16 W5 O4 154.8(7) . 5_665 ?
O32 W5 O4 92.8(8) . 5_665 ?
O14 W5 O4 61.7(6) 5_665 5_665 ?
O34 W5 O4 60.5(7) . 5_665 ?
O35 W5 O4 97.3(8) . 5_665 ?
O1 W5 O4 51.5(8) . 5_665 ?
O12 W6 O32 105.3(7) . . ?
O12 W6 O11 101.0(6) . . ?
O32 W6 O11 153.7(8) . . ?
O12 W6 O9 104.4(7) . . ?
O32 W6 O9 88.6(6) . . ?
O11 W6 O9 84.9(7) . . ?
O12 W6 O8 100.7(6) . . ?
O32 W6 O8 85.9(7) . . ?
O11 W6 O8 89.2(6) . . ?
O9 W6 O8 154.9(7) . . ?
O12 W6 O1 154.7(7) . . ?
O32 W6 O1 58.9(8) . . ?
O11 W6 O1 96.4(7) . . ?
O9 W6 O1 58.8(8) . . ?
O8 W6 O1 97.8(8) . . ?
O12 W6 O3 152.1(6) . 5_665 ?
O32 W6 O3 94.1(7) . 5_665 ?
O11 W6 O3 61.4(6) . 5_665 ?
O9 W6 O3 95.8(7) . 5_665 ?
O8 W6 O3 60.3(6) . 5_665 ?
O1 W6 O3 53.2(7) . 5_665 ?
O4 Ge1 O4 180.0(11) . 5_665 ?
O4 Ge1 O2 113.0(11) . 5_665 ?
O4 Ge1 O2 67.0(11) 5_665 5_665 ?
O4 Ge1 O2 67.1(11) . . ?
O4 Ge1 O2 113.0(11) 5_665 . ?
O2 Ge1 O2 180.0 5_665 . ?
O4 Ge1 O3 68.1(10) . 5_665 ?
O4 Ge1 O3 111.9(10) 5_665 5_665 ?
O2 Ge1 O3 66.0(10) 5_665 5_665 ?
O2 Ge1 O3 114.0(10) . 5_665 ?
O4 Ge1 O3 111.9(10) . . ?
O4 Ge1 O3 68.1(10) 5_665 . ?
O2 Ge1 O3 114.0(10) 5_665 . ?
O2 Ge1 O3 66.0(10) . . ?
O3 Ge1 O3 180.0 5_665 . ?
O4 Ge1 O1 75.5(11) . 5_665 ?
O4 Ge1 O1 104.5(11) 5_665 5_665 ?
O2 Ge1 O1 71.6(10) 5_665 5_665 ?
O2 Ge1 O1 108.4(10) . 5_665 ?
O3 Ge1 O1 104.1(10) 5_665 5_665 ?
O3 Ge1 O1 75.9(10) . 5_665 ?
O4 Ge1 O1 104.6(11) . . ?
O4 Ge1 O1 75.5(11) 5_665 . ?
O2 Ge1 O1 108.4(10) 5_665 . ?
O2 Ge1 O1 71.6(10) . . ?
O3 Ge1 O1 75.9(10) 5_665 . ?
O3 Ge1 O1 104.1(10) . . ?
O1 Ge1 O1 180.0(12) 5_665 . ?
Ge1 O1 W4 120.4(11) . . ?
Ge1 O1 W5 118.5(12) . . ?
W4 O1 W5 100.3(9) . . ?
Ge1 O1 W6 116.7(11) . . ?
W4 O1 W6 99.0(9) . . ?
W5 O1 W6 97.9(8) . . ?
Ge1 O2 W2 123.5(12) . 5_665 ?
Ge1 O2 W1 121.5(11) . . ?
W2 O2 W1 97.4(8) 5_665 . ?
Ge1 O2 W4 117.3(10) . . ?
W2 O2 W4 96.0(8) 5_665 . ?
W1 O2 W4 94.8(8) . . ?
Ge1 O3 W2 123.4(10) . 5_665 ?
Ge1 O3 W3 121.1(9) . 5_665 ?
W2 O3 W3 100.5(7) 5_665 5_665 ?
Ge1 O3 W6 114.2(9) . 5_665 ?
W2 O3 W6 96.3(6) 5_665 5_665 ?
W3 O3 W6 95.4(7) 5_665 5_665 ?
Ge1 O4 W1 125.2(12) . . ?
Ge1 O4 W3 122.8(12) . . ?
W1 O4 W3 98.8(9) . . ?
Ge1 O4 W5 114.6(12) . 5_665 ?
W1 O4 W5 94.3(8) . 5_665 ?
W3 O4 W5 93.6(8) . 5_665 ?
O19 Cu2 N1 168.9(5) . . ?
O19 Cu2 N4 88.2(5) . . ?
N1 Cu2 N4 80.8(5) . . ?
O19 Cu2 Cl1 93.6(3) . . ?
N1 Cu2 Cl1 96.5(4) . . ?
N4 Cu2 Cl1 160.7(4) . . ?
O19 Cu2 Cl2 92.0(3) . . ?
N1 Cu2 Cl2 92.3(4) . . ?
N4 Cu2 Cl2 107.0(4) . . ?
Cl1 Cu2 Cl2 92.16(14) . . ?
O18 Cu1 N5 165.4(5) . . ?
O18 Cu1 N2 88.7(4) . . ?
N5 Cu1 N2 82.3(4) . . ?
O18 Cu1 Cl2 91.8(3) . . ?
N5 Cu1 Cl2 95.3(3) . . ?
N2 Cu1 Cl2 171.0(4) . . ?
O18 Cu1 Cl1 95.5(3) . . ?
N5 Cu1 Cl1 96.9(4) . . ?
N2 Cu1 Cl1 96.1(4) . . ?
Cl2 Cu1 Cl1 92.77(15) . . ?
Cu1 Cl2 Cu2 81.45(13) . . ?
Cu2 Cl1 Cu1 81.59(13) . . ?
C21 O19 Cu2 130.3(9) . . ?
C2 N5 C7 118.0(12) . . ?
C2 N5 Cu1 130.2(10) . . ?
C7 N5 Cu1 111.9(8) . . ?
C4 N4 C14 117.5(13) . . ?
C4 N4 Cu2 128.5(10) . . ?
C14 N4 Cu2 114.0(10) . . ?
C21 O18 Cu1 129.2(10) . . ?
C27 N2 C8 119.2(12) . . ?
C27 N2 Cu1 128.4(10) . . ?
C8 N2 Cu1 112.3(9) . . ?
C12 N7 C23 123.9(14) . . ?
W5 O14 W3 138.7(7) 5_665 . ?
W4 O13 W2 138.3(7) . 5_665 ?
O18 C21 O19 128.2(13) . . ?
O18 C21 C20 116.1(13) . . ?
O19 C21 C20 115.6(12) . . ?
C28 C20 C18 119.7(14) . . ?
C28 C20 C21 120.3(14) . . ?
C18 C20 C21 120.1(14) . . ?
C29 N1 C6 117.3(15) . . ?
C29 N1 Cu2 128.8(12) . . ?
C6 N1 Cu2 113.8(10) . . ?
W6 O11 W3 138.7(8) . . ?
W4 O9 W6 140.8(10) . . ?
C16 C19 C8 116.6(14) . . ?
C16 C19 C17 124.6(15) . . ?
C8 C19 C17 118.8(14) . . ?
W2 O8 W6 138.7(8) . . ?
C20 C18 C12 119.3(15) . . ?
C50 C17 C19 121.6(14) . . ?
C13 C16 C19 118.7(14) . . ?
C6 C15 C5 115.0(17) . . ?
C6 C15 C1 119.8(17) . . ?
C5 C15 C1 125.2(18) . . ?
N4 C14 C26 123.7(15) . . ?
N4 C14 C6 114.7(13) . . ?
C26 C14 C6 121.5(15) . . ?
W4 O5 W1 136.7(8) . . ?
C16 C13 C27 121.4(15) . . ?
W4 O35 W5 136.6(10) . . ?
N7 C12 C18 119.0(14) . . ?
C3 C11 C2 119.9(15) . . ?
W6 O32 W5 143.3(9) . . ?
C1 C10 C26 121.4(17) . . ?
C7 C9 C3 116.1(13) . . ?
C7 C9 C50 117.4(14) . . ?
C3 C9 C50 126.5(14) . . ?
N2 C8 C19 123.5(13) . . ?
N2 C8 C7 117.0(12) . . ?
C19 C8 C7 119.5(13) . . ?
N5 C7 C9 122.6(12) . . ?
N5 C7 C8 116.3(12) . . ?
C9 C7 C8 121.1(13) . . ?
N1 C6 C15 125.3(15) . . ?
N1 C6 C14 116.3(14) . . ?
C15 C6 C14 118.4(15) . . ?
C25 C5 C15 120.0(16) . . ?
N4 C4 C24 121.6(16) . . ?
C11 C3 C9 120.8(14) . . ?
N5 C2 C11 122.5(15) . . ?
C10 C1 C15 120.5(17) . . ?
C24 C30 C26 120.6(15) . . ?
N1 C29 C25 122.6(17) . . ?
C20 C28 C23 120.5(16) . . ?
N2 C27 C13 120.5(15) . . ?
C14 C26 C30 117.1(16) . . ?
C14 C26 C10 118.4(17) . . ?
C30 C26 C10 124.4(16) . . ?
C5 C25 C29 119.7(16) . . ?
C30 C24 C4 119.4(16) . . ?
N7 C23 C28 117.5(17) . . ?
W1 O36 W2 138.5(8) . 5_665 ?
C17 C50 C9 121.7(14) . . ?
W1 O34 W5 139.4(8) 5_665 . ?
W2 O33 W3 137.5(10) . . ?
W3 O30 W1 137.2(9) . . ?

_refine_diff_density_max         3.671
_refine_diff_density_min         -4.627
_refine_diff_density_rms         0.325



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_3
_database_code_depnum_ccdc_archive 'CCDC 1419957'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;

# start Validation Reply Form

_vrf_PLAT342_shelx_3             
;
PROBLEM: Low Bond Precision on C-C Bonds .........0.0328 Ang

RESPONSE: The quality of this crystal was poor.
;

# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H42 Cl4 Cu4 Ge N10 O44 W12'
_chemical_formula_weight         4281.78

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'
Cu Cu 0.3201 1.2651 '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'
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'
W W -0.8490 6.8722 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.475(2)
_cell_length_b                   12.627(3)
_cell_length_c                   15.450(3)
_cell_angle_alpha                88.57(3)
_cell_angle_beta                 68.68(3)
_cell_angle_gamma                87.78(3)
_cell_volume                     2083.7(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    17907
_cell_measurement_theta_min      3.17
_cell_measurement_theta_max      27.49

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.412
_exptl_crystal_F_000             1928
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    18.062
_shelx_estimated_absorpt_T_min   0.173
_shelx_estimated_absorpt_T_max   0.241
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.4138
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20607
_diffrn_reflns_av_unetI/netI     0.0936
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.168
_diffrn_reflns_theta_max         27.475
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9418
_reflns_number_gt                8141
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker XSCANS'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+155.2573P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9418
_refine_ls_number_parameters     628
_refine_ls_number_restraints     528
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0753
_refine_ls_wR_factor_ref         0.1776
_refine_ls_wR_factor_gt          0.1713
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
W1 W 2.11872(8) 0.73430(6) -0.12834(6) 0.0411(2) Uani 1 1 d . . . . .
W2 W 1.80037(7) 0.67585(6) -0.06736(6) 0.0335(2) Uani 1 1 d . . . . .
W3 W 2.23839(6) 0.35121(5) -0.16980(4) 0.02090(16) Uani 1 1 d . . . . .
W4 W 2.03194(7) 0.52284(7) -0.23643(5) 0.0341(2) Uani 1 1 d . . . . .
W6 W 1.92021(7) 0.28713(6) -0.10968(5) 0.02720(18) Uani 1 1 d . . . . .
W7 W 1.68134(6) 0.43833(6) 0.05744(5) 0.02523(17) Uani 1 1 d . . . . .
Ge1 Ge 2.0000 0.5000 0.0000 0.0176(5) Uani 1 2 d S . P . .
O1 O 2.108(3) 0.597(2) -0.011(2) 0.046(4) Uani 0.5 1 d . U P . .
O2 O 1.854(3) 0.547(2) 0.037(2) 0.041(4) Uani 0.5 1 d . U P . .
O3 O 1.986(3) 0.591(3) -0.089(2) 0.044(4) Uani 0.5 1 d . U P . .
O4 O 2.040(3) 0.429(2) -0.099(2) 0.044(4) Uani 0.5 1 d . U P . .
O29 O 2.1806(15) 0.4425(14) -0.2489(13) 0.056(3) Uani 1 1 d . U . . .
O28 O 1.8804(17) 0.5985(15) -0.1722(14) 0.068(3) Uani 1 1 d . U . . .
O25 O 1.7625(18) 0.3545(15) -0.0491(13) 0.067(4) Uani 1 1 d . U . . .
O24 O 1.7032(16) 0.7566(12) -0.0962(11) 0.047(4) Uani 1 1 d . U . . .
O23 O 2.2563(18) 0.6589(15) -0.1322(12) 0.065(4) Uani 1 1 d . U . . .
O22 O 1.5337(15) 0.4102(17) 0.0802(12) 0.064(5) Uani 1 1 d . U . . .
O21 O 2.0961(15) 0.2668(14) -0.1523(13) 0.056(3) Uani 1 1 d . U . . .
O20 O 1.7630(18) 0.7117(14) 0.0570(12) 0.059(3) Uani 1 1 d . U . . .
O19 O 1.8836(15) 0.1866(13) -0.1642(13) 0.053(4) Uani 1 1 d . U . . .
O18 O 2.3360(17) 0.4609(14) -0.1547(12) 0.056(3) Uani 1 1 d . U . . .
O17 O 2.1749(15) 0.8442(12) -0.1878(11) 0.045(3) Uani 1 1 d . U . . .
O16 O 2.0892(18) 0.7794(15) -0.0038(13) 0.068(4) Uani 1 1 d . U . . .
O15 O 1.9424(16) 0.3970(15) -0.2005(14) 0.063(3) Uani 1 1 d . U . . .
Cu1 Cu 2.7261(2) -0.02797(17) -0.35089(15) 0.0281(5) Uani 1 1 d . . . . .
Cu2 Cu 2.5510(2) 0.19173(17) -0.31274(15) 0.0264(5) Uani 1 1 d . . . . .
Cl2 Cl 2.4931(5) 0.0343(4) -0.3408(4) 0.0353(10) Uani 1 1 d . . . . .
Cl1 Cl 2.6581(6) -0.1911(4) -0.2994(4) 0.0452(12) Uani 1 1 d . . . . .
O13 O 2.5603(13) 0.1473(11) -0.1922(8) 0.033(3) Uani 1 1 d . U . . .
N2 N 2.5860(14) 0.2484(13) -0.4430(11) 0.031(3) Uani 1 1 d . . . . .
N4 N 2.8357(15) 0.0983(13) -0.4071(12) 0.034(4) Uani 1 1 d . . . . .
O12 O 2.0442(14) 0.5342(14) -0.3449(11) 0.049(4) Uani 1 1 d . U . . .
O11 O 2.7072(13) 0.0130(11) -0.2260(9) 0.038(3) Uani 1 1 d . U . . .
N3 N 2.7704(15) -0.0594(13) -0.4849(12) 0.033(4) Uani 1 1 d . . . . .
O10 O 2.3509(14) 0.2791(12) -0.2504(11) 0.047(3) Uani 1 1 d . U . . .
C32 C 2.6294(16) 0.0796(13) -0.0746(12) 0.024(4) Uani 1 1 d . . . . .
N1 N 2.6163(15) 0.3297(12) -0.2982(11) 0.030(3) Uani 1 1 d . . . . .
N5 N 2.5368(17) 0.1467(15) 0.0795(13) 0.047(5) Uani 1 1 d . . . . .
C30 C 2.8665(17) 0.1805(16) -0.3644(13) 0.031(4) Uani 1 1 d . . . . .
H30A H 2.8350 0.1826 -0.2999 0.037 Uiso 1 1 calc R U . . .
C29 C 2.5742(18) 0.2021(17) -0.5168(12) 0.034(4) Uani 1 1 d . . . . .
H29A H 2.5521 0.1316 -0.5125 0.041 Uiso 1 1 calc R U . . .
C28 C 2.6106(18) 0.0807(16) 0.1091(15) 0.037(4) Uani 1 1 d . U . . .
H28A H 2.6038 0.0820 0.1709 0.044 Uiso 1 1 calc R U . . .
C27 C 2.6315(18) 0.0804(14) -0.1719(12) 0.030(4) Uani 1 1 d . . . . .
C26 C 2.8818(16) 0.1005(16) -0.4997(15) 0.033(4) Uani 1 1 d . . . . .
C25 C 2.8479(17) 0.0100(18) -0.5434(13) 0.034(4) Uani 1 1 d . . . . .
C24 C 2.6196(18) 0.3521(16) -0.4527(14) 0.036(4) Uani 1 1 d . . . . .
C23 C 2.702(2) 0.5328(17) -0.2992(18) 0.050(6) Uani 1 1 d . . . . .
H23A H 2.7323 0.6000 -0.2994 0.060 Uiso 1 1 calc R U . . .
C22 C 2.6398(18) 0.3955(14) -0.3743(15) 0.032(4) Uani 1 1 d . . . . .
C21 C 2.6798(19) 0.4992(17) -0.3778(18) 0.045(5) Uani 1 1 d . . . . .
C20 C 2.7018(19) 0.0120(15) -0.0419(14) 0.033(4) Uani 1 1 d . . . . .
H20A H 2.7577 -0.0358 -0.0825 0.040 Uiso 1 1 calc R U . . .
C19 C 2.638(2) 0.3700(16) -0.2276(14) 0.039(5) Uani 1 1 d . . . . .
H19A H 2.6246 0.3258 -0.1761 0.047 Uiso 1 1 calc R U . . .
O8 O 1.7018(18) 0.5550(14) -0.0243(12) 0.059(3) Uani 1 1 d . U . . .
O7 O 2.1169(16) 0.6446(15) -0.2254(13) 0.065(3) Uani 1 1 d . U . . .
C39 C 2.941(2) 0.2593(19) -0.413(2) 0.051(6) Uani 1 1 d . . . . .
H39A H 2.9605 0.3137 -0.3811 0.062 Uiso 1 1 calc R U . . .
C18 C 2.6400(19) 0.4131(19) -0.5325(16) 0.044(5) Uani 1 1 d . . . . .
C17 C 2.693(2) 0.014(2) 0.0506(16) 0.046(5) Uani 1 1 d . . . . .
H17A H 2.7442 -0.0314 0.0712 0.055 Uiso 1 1 calc R U . . .
C16 C 2.739(3) -0.139(2) -0.5257(19) 0.057(7) Uani 1 1 d . . . . .
H16A H 2.6892 -0.1905 -0.4870 0.069 Uiso 1 1 calc R U . . .
C15 C 2.5457(19) 0.1470(17) -0.0104(14) 0.038(5) Uani 1 1 d . . . . .
H15A H 2.4946 0.1935 -0.0294 0.046 Uiso 1 1 calc R U . . .
C12 C 2.6784(19) 0.4681(16) -0.2212(14) 0.036(4) Uani 1 1 d . . . . .
H12A H 2.6897 0.4905 -0.1680 0.043 Uiso 1 1 calc R U . . .
C11 C 2.680(2) 0.520(2) -0.5357(17) 0.057(7) Uani 1 1 d . . . . .
H11A H 2.6971 0.5609 -0.5893 0.068 Uiso 1 1 calc R U . . .
C10 C 2.978(2) 0.0815(19) -0.6937(18) 0.047(5) Uani 1 1 d . U . . .
H10A H 3.0126 0.0752 -0.7579 0.057 Uiso 1 1 calc R U . . .
C9 C 2.854(2) -0.082(2) -0.6780(18) 0.058(7) Uani 1 1 d . . . . .
H9A H 2.8810 -0.0914 -0.7419 0.069 Uiso 1 1 calc R U . . .
C8 C 2.629(2) 0.3657(19) -0.6094(15) 0.043(5) Uani 1 1 d . . . . .
H8A H 2.6427 0.4033 -0.6646 0.052 Uiso 1 1 calc R U . . .
C7 C 2.694(2) 0.5602(19) -0.458(2) 0.056(7) Uani 1 1 d . . . . .
H7A H 2.7133 0.6311 -0.4589 0.067 Uiso 1 1 calc R U . . .
C6 C 2.988(2) 0.258(2) -0.507(2) 0.055(7) Uani 1 1 d . . . . .
H6A H 3.0384 0.3128 -0.5395 0.067 Uiso 1 1 calc R U . . .
C5 C 2.772(3) -0.152(2) -0.616(2) 0.070(10) Uani 1 1 d . . . . .
H5A H 2.7410 -0.2082 -0.6385 0.084 Uiso 1 1 calc R U . . .
C4 C 2.8940(19) 0.003(2) -0.6405(16) 0.047(6) Uani 1 1 d . . . . .
C3 C 2.595(2) 0.259(2) -0.6007(14) 0.054(7) Uani 1 1 d . . . . .
H3A H 2.5862 0.2257 -0.6509 0.065 Uiso 1 1 calc R U . . .
C2 C 3.009(2) 0.165(2) -0.6536(15) 0.057(7) Uani 1 1 d . . . . .
H2A H 3.0627 0.2150 -0.6908 0.069 Uiso 1 1 calc R U . . .
O14 O 1.9416(18) 0.7577(15) -0.0934(14) 0.071(4) Uani 1 1 d . U . . .
C1 C 2.9601(18) 0.177(2) -0.5548(15) 0.046(6) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O17 1.661(15) . ?
W1 O23 1.794(18) . ?
W1 O7 1.908(17) . ?
W1 O14 1.92(2) . ?
W1 O16 1.926(19) . ?
W1 O3 2.34(3) . ?
W1 O1 2.45(3) . ?
W2 O24 1.653(15) . ?
W2 O28 1.830(16) . ?
W2 O14 1.868(18) . ?
W2 O20 1.873(16) . ?
W2 O8 1.894(18) . ?
W2 O3 2.26(3) . ?
W2 O2 2.48(3) . ?
W3 O10 1.686(14) . ?
W3 O18 1.885(16) . ?
W3 O20 1.892(19) 2_965 ?
W3 O21 1.917(16) . ?
W3 O29 1.929(17) . ?
W3 O4 2.32(3) . ?
W3 O2 2.33(3) 2_965 ?
W4 O12 1.633(16) . ?
W4 O15 1.886(18) . ?
W4 O28 1.894(18) . ?
W4 O7 1.896(17) . ?
W4 O29 1.901(17) . ?
W4 O3 2.32(3) . ?
W4 O4 2.43(3) . ?
W6 O19 1.688(14) . ?
W6 O25 1.888(17) . ?
W6 O21 1.891(16) . ?
W6 O16 1.89(2) 2_965 ?
W6 O15 1.905(18) . ?
W6 O1 2.32(3) 2_965 ?
W6 O4 2.35(3) . ?
W7 O22 1.652(15) . ?
W7 O8 1.881(19) . ?
W7 O25 1.895(18) . ?
W7 O18 1.943(16) 2_965 ?
W7 O23 1.953(18) 2_965 ?
W7 O1 2.28(3) 2_965 ?
W7 O2 2.38(3) . ?
Ge1 O2 1.65(3) . ?
Ge1 O2 1.65(3) 2_965 ?
Ge1 O4 1.70(3) 2_965 ?
Ge1 O4 1.70(3) . ?
Ge1 O1 1.74(3) 2_965 ?
Ge1 O1 1.74(3) . ?
Ge1 O3 1.82(3) 2_965 ?
Ge1 O3 1.82(3) . ?
O1 W7 2.28(3) 2_965 ?
O1 W6 2.32(3) 2_965 ?
O2 W3 2.33(3) 2_965 ?
O23 W7 1.953(18) 2_965 ?
O20 W3 1.892(19) 2_965 ?
O18 W7 1.943(16) 2_965 ?
O16 W6 1.89(2) 2_965 ?
Cu1 O11 1.943(13) . ?
Cu1 N3 1.991(16) . ?
Cu1 N4 2.042(16) . ?
Cu1 Cl1 2.252(6) . ?
Cu1 Cl2 2.707(5) . ?
Cu2 O13 1.969(13) . ?
Cu2 N1 1.972(15) . ?
Cu2 N2 2.021(17) . ?
Cu2 Cl2 2.222(5) . ?
Cu2 O10 2.381(15) . ?
O13 C27 1.26(2) . ?
N2 C29 1.35(2) . ?
N2 C24 1.37(3) . ?
N4 C26 1.33(3) . ?
N4 C30 1.37(2) . ?
O11 C27 1.28(2) . ?
N3 C16 1.33(3) . ?
N3 C25 1.35(3) . ?
C32 C20 1.38(3) . ?
C32 C15 1.38(2) . ?
C32 C27 1.49(2) . ?
N1 C19 1.32(2) . ?
N1 C22 1.37(2) . ?
N5 C28 1.35(3) . ?
N5 C15 1.36(3) . ?
C30 C39 1.36(3) . ?
C30 H30A 0.9300 . ?
C29 C3 1.41(3) . ?
C29 H29A 0.9300 . ?
C28 C17 1.34(3) . ?
C28 H28A 0.9300 . ?
C26 C1 1.39(3) . ?
C26 C25 1.48(3) . ?
C25 C4 1.40(3) . ?
C24 C18 1.39(3) . ?
C24 C22 1.44(3) . ?
C23 C12 1.39(3) . ?
C23 C21 1.41(3) . ?
C23 H23A 0.9300 . ?
C22 C21 1.40(3) . ?
C21 C7 1.41(3) . ?
C20 C17 1.40(3) . ?
C20 H20A 0.9300 . ?
C19 C12 1.36(3) . ?
C19 H19A 0.9300 . ?
C39 C6 1.35(4) . ?
C39 H39A 0.9300 . ?
C18 C8 1.39(3) . ?
C18 C11 1.44(4) . ?
C17 H17A 0.9300 . ?
C16 C5 1.32(4) . ?
C16 H16A 0.9300 . ?
C15 H15A 0.9300 . ?
C12 H12A 0.9300 . ?
C11 C7 1.38(4) . ?
C11 H11A 0.9300 . ?
C10 C2 1.36(4) . ?
C10 C4 1.43(3) . ?
C10 H10A 0.9300 . ?
C9 C5 1.40(4) . ?
C9 C4 1.40(4) . ?
C9 H9A 0.9300 . ?
C8 C3 1.40(4) . ?
C8 H8A 0.9300 . ?
C7 H7A 0.9300 . ?
C6 C1 1.40(3) . ?
C6 H6A 0.9300 . ?
C5 H5A 0.9300 . ?
C3 H3A 0.9300 . ?
C2 C1 1.43(3) . ?
C2 H2A 0.9300 . ?

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
_geom_angle_publ_flag
O17 W1 O23 103.8(8) . . ?
O17 W1 O7 101.0(8) . . ?
O23 W1 O7 85.9(9) . . ?
O17 W1 O14 102.4(9) . . ?
O23 W1 O14 153.9(9) . . ?
O7 W1 O14 89.0(7) . . ?
O17 W1 O16 100.5(8) . . ?
O23 W1 O16 91.3(8) . . ?
O7 W1 O16 158.4(9) . . ?
O14 W1 O16 84.1(8) . . ?
O17 W1 O3 153.2(9) . . ?
O23 W1 O3 95.6(10) . . ?
O7 W1 O3 61.6(9) . . ?
O14 W1 O3 59.8(9) . . ?
O16 W1 O3 97.4(10) . . ?
O17 W1 O1 153.1(9) . . ?
O23 W1 O1 59.1(9) . . ?
O7 W1 O1 98.3(9) . . ?
O14 W1 O1 96.5(10) . . ?
O16 W1 O1 62.3(9) . . ?
O3 W1 O1 53.7(10) . . ?
O24 W2 O28 104.2(9) . . ?
O24 W2 O14 102.6(9) . . ?
O28 W2 O14 90.2(8) . . ?
O24 W2 O20 101.5(8) . . ?
O28 W2 O20 154.2(9) . . ?
O14 W2 O20 85.9(8) . . ?
O24 W2 O8 101.5(8) . . ?
O28 W2 O8 85.1(8) . . ?
O14 W2 O8 155.9(9) . . ?
O20 W2 O8 88.1(7) . . ?
O24 W2 O3 155.1(10) . . ?
O28 W2 O3 59.3(10) . . ?
O14 W2 O3 62.0(10) . . ?
O20 W2 O3 96.9(10) . . ?
O8 W2 O3 95.7(10) . . ?
O24 W2 O2 153.4(9) . . ?
O28 W2 O2 94.4(10) . . ?
O14 W2 O2 96.1(10) . . ?
O20 W2 O2 60.8(8) . . ?
O8 W2 O2 60.8(8) . . ?
O3 W2 O2 51.5(11) . . ?
O10 W3 O18 99.5(8) . . ?
O10 W3 O20 102.6(8) . 2_965 ?
O18 W3 O20 89.7(7) . 2_965 ?
O10 W3 O21 100.3(8) . . ?
O18 W3 O21 160.3(8) . . ?
O20 W3 O21 85.1(7) 2_965 . ?
O10 W3 O29 100.4(8) . . ?
O18 W3 O29 90.1(8) . . ?
O20 W3 O29 156.7(8) 2_965 . ?
O21 W3 O29 87.3(7) . . ?
O10 W3 O4 155.7(9) . . ?
O18 W3 O4 99.4(9) . . ?
O20 W3 O4 92.7(10) 2_965 . ?
O21 W3 O4 61.9(9) . . ?
O29 W3 O4 64.4(9) . . ?
O10 W3 O2 157.7(9) . 2_965 ?
O18 W3 O2 64.5(9) . 2_965 ?
O20 W3 O2 64.0(9) 2_965 2_965 ?
O21 W3 O2 96.3(9) . 2_965 ?
O29 W3 O2 95.2(10) . 2_965 ?
O4 W3 O2 46.6(10) . 2_965 ?
O12 W4 O15 101.1(9) . . ?
O12 W4 O28 103.1(9) . . ?
O15 W4 O28 87.7(8) . . ?
O12 W4 O7 100.5(9) . . ?
O15 W4 O7 158.4(9) . . ?
O28 W4 O7 87.4(7) . . ?
O12 W4 O29 100.9(8) . . ?
O15 W4 O29 88.5(7) . . ?
O28 W4 O29 156.0(9) . . ?
O7 W4 O29 87.5(8) . . ?
O12 W4 O3 152.1(10) . . ?
O15 W4 O3 97.8(10) . . ?
O28 W4 O3 57.3(9) . . ?
O7 W4 O3 62.1(10) . . ?
O29 W4 O3 99.8(9) . . ?
O12 W4 O4 155.2(9) . . ?
O15 W4 O4 62.4(9) . . ?
O28 W4 O4 94.9(10) . . ?
O7 W4 O4 97.1(9) . . ?
O29 W4 O4 62.5(9) . . ?
O3 W4 O4 52.6(11) . . ?
O19 W6 O25 102.1(9) . . ?
O19 W6 O21 100.0(8) . . ?
O25 W6 O21 157.7(9) . . ?
O19 W6 O16 101.1(9) . 2_965 ?
O25 W6 O16 89.9(8) . 2_965 ?
O21 W6 O16 88.5(8) . 2_965 ?
O19 W6 O15 100.2(9) . . ?
O25 W6 O15 84.8(8) . . ?
O21 W6 O15 88.7(7) . . ?
O16 W6 O15 158.7(9) 2_965 . ?
O19 W6 O1 155.9(10) . 2_965 ?
O25 W6 O1 59.8(10) . 2_965 ?
O21 W6 O1 99.6(10) . 2_965 ?
O16 W6 O1 65.6(10) 2_965 2_965 ?
O15 W6 O1 94.1(11) . 2_965 ?
O19 W6 O4 154.5(10) . . ?
O25 W6 O4 96.4(10) . . ?
O21 W6 O4 61.8(9) . . ?
O16 W6 O4 96.3(10) 2_965 . ?
O15 W6 O4 64.0(10) . . ?
O1 W6 O4 49.5(11) 2_965 . ?
O22 W7 O8 101.7(9) . . ?
O22 W7 O25 100.8(9) . . ?
O8 W7 O25 87.0(8) . . ?
O22 W7 O18 101.1(8) . 2_965 ?
O8 W7 O18 87.4(7) . 2_965 ?
O25 W7 O18 158.1(8) . 2_965 ?
O22 W7 O23 107.0(9) . 2_965 ?
O8 W7 O23 151.2(8) . 2_965 ?
O25 W7 O23 90.4(8) . 2_965 ?
O18 W7 O23 84.4(8) 2_965 2_965 ?
O22 W7 O1 155.7(10) . 2_965 ?
O8 W7 O1 93.0(11) . 2_965 ?
O25 W7 O1 60.5(9) . 2_965 ?
O18 W7 O1 98.6(9) 2_965 2_965 ?
O23 W7 O1 61.1(10) 2_965 2_965 ?
O22 W7 O2 156.9(10) . . ?
O8 W7 O2 63.2(9) . . ?
O25 W7 O2 96.0(9) . . ?
O18 W7 O2 62.7(8) 2_965 . ?
O23 W7 O2 88.6(10) 2_965 . ?
O1 W7 O2 47.3(10) 2_965 . ?
O2 Ge1 O2 180.0 . 2_965 ?
O2 Ge1 O4 66.4(13) . 2_965 ?
O2 Ge1 O4 113.6(13) 2_965 2_965 ?
O2 Ge1 O4 113.6(13) . . ?
O2 Ge1 O4 66.4(13) 2_965 . ?
O4 Ge1 O4 180.0 2_965 . ?
O2 Ge1 O1 66.9(14) . 2_965 ?
O2 Ge1 O1 113.1(14) 2_965 2_965 ?
O4 Ge1 O1 110.7(14) 2_965 2_965 ?
O4 Ge1 O1 69.3(14) . 2_965 ?
O2 Ge1 O1 113.1(14) . . ?
O2 Ge1 O1 66.9(14) 2_965 . ?
O4 Ge1 O1 69.3(14) 2_965 . ?
O4 Ge1 O1 110.7(14) . . ?
O1 Ge1 O1 180.0 2_965 . ?
O2 Ge1 O3 107.2(15) . 2_965 ?
O2 Ge1 O3 72.8(15) 2_965 2_965 ?
O4 Ge1 O3 73.4(14) 2_965 2_965 ?
O4 Ge1 O3 106.6(14) . 2_965 ?
O1 Ge1 O3 75.0(14) 2_965 2_965 ?
O1 Ge1 O3 105.0(14) . 2_965 ?
O2 Ge1 O3 72.8(15) . . ?
O2 Ge1 O3 107.2(15) 2_965 . ?
O4 Ge1 O3 106.6(14) 2_965 . ?
O4 Ge1 O3 73.4(14) . . ?
O1 Ge1 O3 105.0(14) 2_965 . ?
O1 Ge1 O3 75.0(14) . . ?
O3 Ge1 O3 180.0(13) 2_965 . ?
Ge1 O1 W7 123.4(15) . 2_965 ?
Ge1 O1 W6 120.3(16) . 2_965 ?
W7 O1 W6 100.4(11) 2_965 2_965 ?
Ge1 O1 W1 114.7(15) . . ?
W7 O1 W1 96.7(12) 2_965 . ?
W6 O1 W1 95.8(11) 2_965 . ?
Ge1 O2 W3 124.7(13) . 2_965 ?
Ge1 O2 W7 122.3(14) . . ?
W3 O2 W7 97.5(11) 2_965 . ?
Ge1 O2 W2 116.1(16) . . ?
W3 O2 W2 94.8(10) 2_965 . ?
W7 O2 W2 94.4(9) . . ?
Ge1 O3 W2 119.6(16) . . ?
Ge1 O3 W4 117.0(15) . . ?
W2 O3 W4 100.7(11) . . ?
Ge1 O3 W1 116.6(13) . . ?
W2 O3 W1 100.3(12) . . ?
W4 O3 W1 99.0(12) . . ?
Ge1 O4 W3 122.3(15) . . ?
Ge1 O4 W6 120.8(16) . . ?
W3 O4 W6 98.8(11) . . ?
Ge1 O4 W4 117.0(16) . . ?
W3 O4 W4 96.7(11) . . ?
W6 O4 W4 95.6(10) . . ?
W4 O29 W3 136.3(10) . . ?
W2 O28 W4 142.4(12) . . ?
W6 O25 W7 138.5(12) . . ?
W1 O23 W7 141.7(10) . 2_965 ?
W6 O21 W3 137.2(11) . . ?
W2 O20 W3 139.8(10) . 2_965 ?
W3 O18 W7 135.0(10) . 2_965 ?
W6 O16 W1 136.2(10) 2_965 . ?
W4 O15 W6 137.9(11) . . ?
O11 Cu1 N3 171.3(7) . . ?
O11 Cu1 N4 91.4(6) . . ?
N3 Cu1 N4 81.0(7) . . ?
O11 Cu1 Cl1 90.8(5) . . ?
N3 Cu1 Cl1 95.4(5) . . ?
N4 Cu1 Cl1 163.8(5) . . ?
O11 Cu1 Cl2 96.8(5) . . ?
N3 Cu1 Cl2 89.3(5) . . ?
N4 Cu1 Cl2 105.4(5) . . ?
Cl1 Cu1 Cl2 90.3(2) . . ?
O13 Cu2 N1 88.5(6) . . ?
O13 Cu2 N2 165.6(6) . . ?
N1 Cu2 N2 82.2(6) . . ?
O13 Cu2 Cl2 94.0(4) . . ?
N1 Cu2 Cl2 174.7(5) . . ?
N2 Cu2 Cl2 94.5(5) . . ?
O13 Cu2 O10 96.1(6) . . ?
N1 Cu2 O10 84.9(6) . . ?
N2 Cu2 O10 94.0(6) . . ?
Cl2 Cu2 O10 99.4(4) . . ?
Cu2 Cl2 Cu1 83.33(17) . . ?
C27 O13 Cu2 131.4(12) . . ?
C29 N2 C24 117.5(18) . . ?
C29 N2 Cu2 130.1(14) . . ?
C24 N2 Cu2 112.4(13) . . ?
C26 N4 C30 116.0(17) . . ?
C26 N4 Cu1 114.0(13) . . ?
C30 N4 Cu1 129.9(14) . . ?
C27 O11 Cu1 130.0(14) . . ?
C16 N3 C25 115(2) . . ?
C16 N3 Cu1 130.5(18) . . ?
C25 N3 Cu1 114.4(12) . . ?
W3 O10 Cu2 153.6(10) . . ?
C20 C32 C15 116.5(17) . . ?
C20 C32 C27 124.5(16) . . ?
C15 C32 C27 119.0(18) . . ?
C19 N1 C22 115.1(17) . . ?
C19 N1 Cu2 131.3(14) . . ?
C22 N1 Cu2 113.6(12) . . ?
C28 N5 C15 120.7(18) . . ?
C39 C30 N4 123(2) . . ?
C39 C30 H30A 118.7 . . ?
N4 C30 H30A 118.7 . . ?
N2 C29 C3 121(2) . . ?
N2 C29 H29A 119.5 . . ?
C3 C29 H29A 119.5 . . ?
C17 C28 N5 121(2) . . ?
C17 C28 H28A 119.6 . . ?
N5 C28 H28A 119.6 . . ?
O13 C27 O11 127.1(17) . . ?
O13 C27 C32 117.6(15) . . ?
O11 C27 C32 115.4(18) . . ?
N4 C26 C1 125(2) . . ?
N4 C26 C25 114.5(17) . . ?
C1 C26 C25 120(2) . . ?
N3 C25 C4 125(2) . . ?
N3 C25 C26 116.0(16) . . ?
C4 C25 C26 119(2) . . ?
N2 C24 C18 125(2) . . ?
N2 C24 C22 115.3(17) . . ?
C18 C24 C22 120.1(19) . . ?
C12 C23 C21 121.4(19) . . ?
C12 C23 H23A 119.3 . . ?
C21 C23 H23A 119.3 . . ?
N1 C22 C21 124(2) . . ?
N1 C22 C24 116.0(16) . . ?
C21 C22 C24 120(2) . . ?
C22 C21 C23 116(2) . . ?
C22 C21 C7 118(2) . . ?
C23 C21 C7 126(2) . . ?
C32 C20 C17 121.6(19) . . ?
C32 C20 H20A 119.2 . . ?
C17 C20 H20A 119.2 . . ?
N1 C19 C12 128(2) . . ?
N1 C19 H19A 116.0 . . ?
C12 C19 H19A 116.0 . . ?
W7 O8 W2 141.3(10) . . ?
W4 O7 W1 137.2(11) . . ?
C6 C39 C30 120(2) . . ?
C6 C39 H39A 120.1 . . ?
C30 C39 H39A 120.1 . . ?
C24 C18 C8 118(2) . . ?
C24 C18 C11 119(2) . . ?
C8 C18 C11 122(2) . . ?
C28 C17 C20 119(2) . . ?
C28 C17 H17A 120.5 . . ?
C20 C17 H17A 120.5 . . ?
C5 C16 N3 126(3) . . ?
C5 C16 H16A 117.0 . . ?
N3 C16 H16A 117.0 . . ?
N5 C15 C32 121(2) . . ?
N5 C15 H15A 119.3 . . ?
C32 C15 H15A 119.3 . . ?
C19 C12 C23 115.8(18) . . ?
C19 C12 H12A 122.1 . . ?
C23 C12 H12A 122.1 . . ?
C7 C11 C18 119(2) . . ?
C7 C11 H11A 120.5 . . ?
C18 C11 H11A 120.5 . . ?
C2 C10 C4 122(2) . . ?
C2 C10 H10A 118.9 . . ?
C4 C10 H10A 118.9 . . ?
C5 C9 C4 118(2) . . ?
C5 C9 H9A 121.1 . . ?
C4 C9 H9A 121.1 . . ?
C18 C8 C3 118(2) . . ?
C18 C8 H8A 121.1 . . ?
C3 C8 H8A 121.1 . . ?
C11 C7 C21 123(2) . . ?
C11 C7 H7A 118.5 . . ?
C21 C7 H7A 118.5 . . ?
C39 C6 C1 121(2) . . ?
C39 C6 H6A 119.7 . . ?
C1 C6 H6A 119.7 . . ?
C16 C5 C9 120(3) . . ?
C16 C5 H5A 120.1 . . ?
C9 C5 H5A 120.1 . . ?
C25 C4 C9 117(2) . . ?
C25 C4 C10 118(2) . . ?
C9 C4 C10 125(2) . . ?
C8 C3 C29 121(2) . . ?
C8 C3 H3A 119.6 . . ?
C29 C3 H3A 119.6 . . ?
C10 C2 C1 121(2) . . ?
C10 C2 H2A 119.6 . . ?
C1 C2 H2A 119.6 . . ?
W2 O14 W1 137.6(11) . . ?
C26 C1 C6 115(2) . . ?
C26 C1 C2 119(2) . . ?
C6 C1 C2 125(2) . . ?

_refine_diff_density_max         3.367
_refine_diff_density_min         -5.138
_refine_diff_density_rms         0.406



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_4
_database_code_depnum_ccdc_archive 'CCDC 1419958'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT342_shelx_4             
;
PROBLEM: Low Bond Precision on C-C Bonds .........0.07 Ang
RESPONSE: The quality of this crystal was poor.
;

_vrf_PLAT780_shelx_4             
;
PROBLEM: Coordinates do not Form a Properly Connected Set     Please Do 
RESPONSE: the atoms here can not fit to asymmetric
to make a traditional connected set.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H40 Cl2 Cu4 Ge N10 O46 W12'
_chemical_formula_weight         4144.79

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'
Ge Ge 0.1547 1.8001 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.1378(9)
_cell_length_b                   13.5053(8)
_cell_length_c                   23.9776(11)
_cell_angle_alpha                90
_cell_angle_beta                 128.069(3)
_cell_angle_gamma                90
_cell_volume                     3859.2(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8933
_cell_measurement_theta_min      3.2330
_cell_measurement_theta_max      28.2080

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.567
_exptl_crystal_F_000             3720
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    19.433
_shelx_estimated_absorpt_T_min   0.058
_shelx_estimated_absorpt_T_max   0.112
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.043
_exptl_absorpt_correction_T_max  0.098
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   
;
 R(int) was 0.0478 before and 0.0456 after correction.
;
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19015
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.939
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7059
_reflns_number_gt                6455
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+1294.9978P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7059
_refine_ls_number_parameters     592
_refine_ls_number_restraints     702
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.1040
_refine_ls_wR_factor_ref         0.2306
_refine_ls_wR_factor_gt          0.2274
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
W1 W 0.71360(12) -0.16093(11) 0.03740(7) 0.0281(3) Uani 1 1 d . . . . .
W2 W 0.46148(14) -0.13983(11) -0.13766(8) 0.0346(4) Uani 1 1 d . . . . .
W4 W 0.49505(15) 0.12069(12) -0.13311(8) 0.0382(4) Uani 1 1 d . . . . .
W5 W 0.75545(12) -0.01768(10) 0.17519(7) 0.0291(3) Uani 1 1 d . . . . .
W7 W 0.46246(14) -0.26084(10) -0.00645(8) 0.0366(4) Uani 1 1 d . . . . .
W8 W 0.74896(12) 0.09949(11) 0.04060(8) 0.0314(4) Uani 1 1 d . . . . .
Ge1 Ge 0.5000 0.0000 0.0000 0.0245(10) Uani 1 2 d S . P . .
Cu1 Cu 0.8724(4) 0.2977(4) -0.0226(2) 0.0390(11) Uani 1 1 d . . . . .
Cu2 Cu 0.9309(4) -0.3878(3) 0.1233(2) 0.0351(10) Uani 1 1 d . . . . .
Cl1 Cl 0.9521(11) 0.3976(7) -0.0959(6) 0.050(3) Uani 1 1 d . . . . .
O1 O 0.528(5) -0.113(5) -0.022(3) 0.057(5) Uani 0.5 1 d . U P . .
O2 O 0.559(5) 0.096(5) -0.018(3) 0.056(5) Uani 0.5 1 d . U P . .
O3 O 0.641(5) -0.020(5) 0.050(3) 0.055(6) Uani 0.5 1 d . U P . .
O4 O 0.437(5) 0.001(5) -0.089(3) 0.058(5) Uani 0.5 1 d . U P . .
O8 O 0.494(3) 0.229(3) -0.0846(18) 0.069(6) Uani 1 1 d . U . . .
O10 O 0.768(3) -0.126(2) 0.1295(17) 0.057(5) Uani 1 1 d . U . . .
O11 O 0.322(3) -0.205(3) -0.0480(18) 0.061(5) Uani 1 1 d . U . . .
O14 O 0.498(3) -0.013(3) -0.1575(19) 0.066(5) Uani 1 1 d . U . . .
O17 O 0.613(3) -0.169(3) -0.0655(18) 0.064(4) Uani 1 1 d . U . . .
O18 O 0.432(3) -0.243(3) -0.0962(17) 0.061(5) Uani 1 1 d . U . . .
O19 O 0.648(3) 0.107(3) -0.0593(18) 0.066(5) Uani 1 1 d . U . . .
O20 O 0.320(3) -0.092(3) -0.1779(19) 0.064(5) Uani 1 1 d . U . . .
O21 O 0.862(2) 0.149(2) 0.0569(15) 0.048(6) Uani 1 1 d . U . . .
O23 O 0.333(3) 0.105(3) -0.1885(19) 0.067(6) Uani 1 1 d . U . . .
O24 O 0.495(2) 0.177(2) -0.1942(15) 0.044(6) Uani 1 1 d . U . . .
O25 O 0.877(3) -0.027(2) 0.2564(17) 0.056(7) Uani 1 1 d . U . . .
O26 O 0.765(3) -0.033(2) 0.0269(16) 0.053(5) Uani 1 1 d . U . . .
O27 O 0.618(3) -0.253(3) 0.0360(17) 0.062(5) Uani 1 1 d . U . . .
O29 O 0.438(2) -0.3829(19) -0.0096(15) 0.042(6) Uani 1 1 d . U . . .
O30 O 0.807(3) 0.545(2) 0.0386(16) 0.060(8) Uani 1 1 d . U . . .
O31 O 0.867(2) 0.404(2) 0.0274(14) 0.045(6) Uani 1 1 d . U . . .
O32 O 0.716(2) 0.320(2) -0.1048(16) 0.049(6) Uani 1 1 d . U . . .
O33 O 0.444(2) -0.207(2) -0.2043(15) 0.048(6) Uani 1 1 d . U . . .
O34 O 0.818(3) -0.233(2) 0.0558(15) 0.045(6) Uani 1 1 d . U . . .
O50 O 0.793(3) 0.069(2) 0.1326(17) 0.056(5) Uani 1 1 d . U . . .
N1 N 1.036(2) 0.282(2) 0.0492(16) 0.030(7) Uani 1 1 d . . . . .
N2 N 0.884(2) 0.178(2) -0.0647(14) 0.028(6) Uani 1 1 d . . . . .
N3 N 1.026(2) -0.300(2) 0.2067(15) 0.032(7) Uani 1 1 d . . . . .
N4 N 0.840(2) -0.391(2) 0.1578(16) 0.032(7) Uani 1 1 d . . . . .
C1 C 1.109(3) 0.338(4) 0.1032(19) 0.049(12) Uani 1 1 d . . . . .
H1 H 1.0828 0.3912 0.1136 0.059 Uiso 1 1 calc R U . . .
C2 C 1.216(4) 0.323(3) 0.143(2) 0.047(10) Uani 1 1 d . . . . .
H2 H 1.2639 0.3695 0.1772 0.056 Uiso 1 1 calc R U . . .
C3 C 1.259(3) 0.242(4) 0.136(2) 0.048(11) Uani 1 1 d . . . . .
H3 H 1.3355 0.2280 0.1682 0.058 Uiso 1 1 calc R U . . .
C4 C 1.187(3) 0.181(3) 0.078(2) 0.045(10) Uani 1 1 d . U . . .
H4 H 1.2165 0.1268 0.0701 0.055 Uiso 1 1 calc R U . . .
C5 C 1.073(3) 0.197(3) 0.031(2) 0.034(8) Uani 1 1 d . U . . .
C6 C 0.988(3) 0.149(2) -0.0295(17) 0.026(7) Uani 1 1 d . U . . .
C7 C 1.007(4) 0.061(3) -0.056(2) 0.049(10) Uani 1 1 d . U . . .
H7 H 1.0781 0.0334 -0.0284 0.059 Uiso 1 1 calc R U . . .
C8 C 0.928(3) 0.021(3) -0.115(2) 0.045(10) Uani 1 1 d . U . . .
H8 H 0.9446 -0.0299 -0.1333 0.054 Uiso 1 1 calc R U . . .
C9 C 0.820(4) 0.054(3) -0.151(2) 0.047(10) Uani 1 1 d . . . . .
H9 H 0.7602 0.0220 -0.1914 0.056 Uiso 1 1 calc R U . . .
C10 C 0.802(3) 0.137(3) -0.124(2) 0.037(9) Uani 1 1 d . U . . .
H10 H 0.7302 0.1631 -0.1493 0.045 Uiso 1 1 calc R U . . .
C11 C 1.121(4) -0.257(4) 0.231(2) 0.055(12) Uani 1 1 d . . . . .
H11 H 1.1515 -0.2719 0.2084 0.066 Uiso 1 1 calc R U . . .
C12 C 1.178(3) -0.194(3) 0.285(2) 0.042(9) Uani 1 1 d . U . . .
H12 H 1.2421 -0.1630 0.2962 0.050 Uiso 1 1 calc R U . . .
C13 C 1.141(4) -0.175(3) 0.321(2) 0.051(11) Uani 1 1 d . U . . .
H13 H 1.1841 -0.1358 0.3613 0.061 Uiso 1 1 calc R U . . .
C14 C 1.044(4) -0.213(3) 0.302(2) 0.046(10) Uani 1 1 d . U . . .
H14 H 1.0168 -0.1943 0.3257 0.055 Uiso 1 1 calc R U . . .
C15 C 0.980(3) -0.283(3) 0.2414(19) 0.033(8) Uani 1 1 d . U . . .
C16 C 0.881(3) -0.330(3) 0.217(2) 0.038(9) Uani 1 1 d . U . . .
C17 C 0.818(5) -0.316(4) 0.241(3) 0.069(16) Uani 1 1 d . . . . .
H17 H 0.8429 -0.2750 0.2790 0.083 Uiso 1 1 calc R U . . .
C18 C 0.718(4) -0.366(4) 0.206(3) 0.063(14) Uani 1 1 d . . . . .
H18 H 0.6746 -0.3572 0.2207 0.076 Uiso 1 1 calc R U . . .
C19 C 0.680(4) -0.425(3) 0.153(2) 0.047(10) Uani 1 1 d . U . . .
H19 H 0.6133 -0.4598 0.1313 0.057 Uiso 1 1 calc R U . . .
C20 C 0.745(3) -0.436(3) 0.128(2) 0.038(9) Uani 1 1 d . . . . .
H20 H 0.7172 -0.4760 0.0890 0.046 Uiso 1 1 calc R U . . .
C22 C 0.622(3) 0.553(3) -0.099(2) 0.041(9) Uani 1 1 d . U . . .
H22 H 0.6397 0.6074 -0.0696 0.049 Uiso 1 1 calc R U . . .
C23 C 0.526(4) 0.559(3) -0.167(3) 0.057(13) Uani 1 1 d . . . . .
H23 H 0.4791 0.6132 -0.1821 0.069 Uiso 1 1 calc R U . . .
C24 C 0.500(3) 0.482(3) -0.214(2) 0.043(9) Uani 1 1 d . U . . .
N5 N 0.569(3) 0.400(2) -0.1871(17) 0.038(7) Uani 1 1 d . U . . .
C26 C 0.668(3) 0.393(3) -0.1175(19) 0.031(8) Uani 1 1 d . U . . .
C27 C 0.692(3) 0.474(3) -0.0700(19) 0.030(8) Uani 1 1 d . . . . .
C28 C 0.794(3) 0.476(3) 0.003(2) 0.031(8) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O34 1.67(3) . ?
W1 O10 1.88(3) . ?
W1 O27 1.90(3) . ?
W1 O17 1.94(3) . ?
W1 O26 1.97(3) . ?
W1 O3 2.31(6) . ?
W1 O1 2.32(6) . ?
W2 O33 1.71(3) . ?
W2 O20 1.84(3) . ?
W2 O17 1.88(3) . ?
W2 O18 1.92(3) . ?
W2 O14 1.95(4) . ?
W2 O1 2.31(6) . ?
W2 O4 2.37(7) . ?
W4 O24 1.65(3) . ?
W4 O19 1.86(3) . ?
W4 O8 1.88(3) . ?
W4 O14 1.91(4) . ?
W4 O23 1.95(3) . ?
W4 O2 2.31(6) . ?
W4 O4 2.37(7) . ?
W5 O25 1.66(3) . ?
W5 O50 1.86(3) . ?
W5 O20 1.90(3) 3_655 ?
W5 O10 1.91(3) . ?
W5 O23 1.96(4) 3_655 ?
W5 O4 2.32(6) 3_655 ?
W5 O3 2.36(6) . ?
W7 O29 1.68(3) . ?
W7 O11 1.86(3) . ?
W7 O8 1.90(3) 3_655 ?
W7 O27 1.90(3) . ?
W7 O18 1.92(3) . ?
W7 O1 2.37(7) . ?
W7 O2 2.37(6) 3_655 ?
W8 O21 1.65(3) . ?
W8 O26 1.86(3) . ?
W8 O11 1.86(3) 3_655 ?
W8 O19 1.89(3) . ?
W8 O50 1.91(3) . ?
W8 O2 2.29(6) . ?
W8 O3 2.41(6) . ?
Ge1 O3 1.71(6) 3_655 ?
Ge1 O3 1.71(6) . ?
Ge1 O4 1.73(6) 3_655 ?
Ge1 O4 1.73(6) . ?
Ge1 O1 1.75(7) . ?
Ge1 O1 1.75(7) 3_655 ?
Ge1 O2 1.78(7) . ?
Ge1 O2 1.78(7) 3_655 ?
Cu1 O31 1.90(3) . ?
Cu1 O32 1.96(3) . ?
Cu1 N2 1.97(3) . ?
Cu1 N1 1.98(3) . ?
Cu2 O30 1.94(3) 1_545 ?
Cu2 N3 1.98(3) . ?
Cu2 N4 1.99(3) . ?
Cu2 Cl1 2.240(12) 3_755 ?
Cl1 Cu2 2.240(12) 3_755 ?
O2 W7 2.37(6) 3_655 ?
O4 W5 2.32(6) 3_655 ?
O8 W7 1.90(3) 3_655 ?
O11 W8 1.86(3) 3_655 ?
O20 W5 1.90(3) 3_655 ?
O23 W5 1.96(4) 3_655 ?
O30 C28 1.20(4) . ?
O30 Cu2 1.94(3) 1_565 ?
O31 C28 1.31(4) . ?
O32 C26 1.15(4) . ?
N1 C1 1.30(5) . ?
N1 C5 1.46(5) . ?
N2 C10 1.30(5) . ?
N2 C6 1.31(4) . ?
N3 C11 1.31(6) . ?
N3 C15 1.39(5) . ?
N4 C20 1.31(5) . ?
N4 C16 1.41(5) . ?
C1 C2 1.29(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.33(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.40(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.37(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.37(5) . ?
C6 C7 1.45(5) . ?
C7 C8 1.28(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.38(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.39(5) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.33(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.31(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.34(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.48(6) . ?
C14 H14 0.9300 . ?
C15 C16 1.38(5) . ?
C16 C17 1.39(6) . ?
C17 C18 1.37(7) . ?
C17 H17 0.9300 . ?
C18 C19 1.30(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.42(6) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C22 C27 1.36(5) . ?
C22 C23 1.36(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.39(7) . ?
C23 H23 0.9300 . ?
C24 N5 1.38(5) . ?
N5 C26 1.40(5) . ?
C26 C27 1.46(5) . ?
C27 C28 1.45(5) . ?

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
_geom_angle_publ_flag
O34 W1 O10 100.1(14) . . ?
O34 W1 O27 102.2(15) . . ?
O10 W1 O27 87.8(14) . . ?
O34 W1 O17 100.1(14) . . ?
O10 W1 O17 159.7(15) . . ?
O27 W1 O17 87.1(14) . . ?
O34 W1 O26 99.3(14) . . ?
O10 W1 O26 90.6(13) . . ?
O27 W1 O26 158.3(14) . . ?
O17 W1 O26 87.0(13) . . ?
O34 W1 O3 153.6(19) . . ?
O10 W1 O3 62.5(19) . . ?
O27 W1 O3 97.0(19) . . ?
O17 W1 O3 98.8(19) . . ?
O26 W1 O3 63.4(18) . . ?
O34 W1 O1 156.2(19) . . ?
O10 W1 O1 98.2(19) . . ?
O27 W1 O1 63.5(19) . . ?
O17 W1 O1 62.1(19) . . ?
O26 W1 O1 95.5(19) . . ?
O3 W1 O1 50(2) . . ?
O33 W2 O20 103.8(15) . . ?
O33 W2 O17 98.4(15) . . ?
O20 W2 O17 157.5(16) . . ?
O33 W2 O18 98.6(15) . . ?
O20 W2 O18 87.8(15) . . ?
O17 W2 O18 85.1(14) . . ?
O33 W2 O14 98.0(15) . . ?
O20 W2 O14 88.6(15) . . ?
O17 W2 O14 92.2(14) . . ?
O18 W2 O14 163.4(15) . . ?
O33 W2 O1 154.6(19) . . ?
O20 W2 O1 94.6(19) . . ?
O17 W2 O1 63.1(19) . . ?
O18 W2 O1 64.2(19) . . ?
O14 W2 O1 99.9(19) . . ?
O33 W2 O4 154.3(19) . . ?
O20 W2 O4 59.4(19) . . ?
O17 W2 O4 100.8(19) . . ?
O18 W2 O4 99.9(19) . . ?
O14 W2 O4 64.5(19) . . ?
O1 W2 O4 51(2) . . ?
O24 W4 O19 102.3(15) . . ?
O24 W4 O8 101.1(16) . . ?
O19 W4 O8 88.1(14) . . ?
O24 W4 O14 98.8(15) . . ?
O19 W4 O14 87.1(14) . . ?
O8 W4 O14 160.1(16) . . ?
O24 W4 O23 97.3(15) . . ?
O19 W4 O23 160.2(16) . . ?
O8 W4 O23 90.9(15) . . ?
O14 W4 O23 87.1(15) . . ?
O24 W4 O2 153.4(19) . . ?
O19 W4 O2 59.3(19) . . ?
O8 W4 O2 62(2) . . ?
O14 W4 O2 99(2) . . ?
O23 W4 O2 103.0(19) . . ?
O24 W4 O4 155.4(19) . . ?
O19 W4 O4 95(2) . . ?
O8 W4 O4 96(2) . . ?
O14 W4 O4 64.9(19) . . ?
O23 W4 O4 65.0(19) . . ?
O2 W4 O4 51(2) . . ?
O25 W5 O50 101.6(15) . . ?
O25 W5 O20 106.0(15) . 3_655 ?
O50 W5 O20 85.7(15) . 3_655 ?
O25 W5 O10 100.5(15) . . ?
O50 W5 O10 89.8(13) . . ?
O20 W5 O10 153.5(15) 3_655 . ?
O25 W5 O23 97.7(15) . 3_655 ?
O50 W5 O23 160.7(15) . 3_655 ?
O20 W5 O23 88.6(14) 3_655 3_655 ?
O10 W5 O23 87.2(14) . 3_655 ?
O25 W5 O4 157(2) . 3_655 ?
O50 W5 O4 95.3(19) . 3_655 ?
O20 W5 O4 59.8(19) 3_655 3_655 ?
O10 W5 O4 94.8(19) . 3_655 ?
O23 W5 O4 65.9(19) 3_655 3_655 ?
O25 W5 O3 154.2(19) . . ?
O50 W5 O3 63.0(18) . . ?
O20 W5 O3 93.9(19) 3_655 . ?
O10 W5 O3 61.1(18) . . ?
O23 W5 O3 99.1(19) 3_655 . ?
O4 W5 O3 49(2) 3_655 . ?
O29 W7 O11 102.9(14) . . ?
O29 W7 O8 100.6(15) . 3_655 ?
O11 W7 O8 89.9(14) . 3_655 ?
O29 W7 O27 104.1(14) . . ?
O11 W7 O27 153.0(15) . . ?
O8 W7 O27 86.2(15) 3_655 . ?
O29 W7 O18 100.3(14) . . ?
O11 W7 O18 86.7(14) . . ?
O8 W7 O18 159.0(16) 3_655 . ?
O27 W7 O18 87.5(14) . . ?
O29 W7 O1 157.6(19) . . ?
O11 W7 O1 91.5(19) . . ?
O8 W7 O1 96(2) 3_655 . ?
O27 W7 O1 62.4(18) . . ?
O18 W7 O1 63.1(19) . . ?
O29 W7 O2 150.2(18) . 3_655 ?
O11 W7 O2 57.9(18) . 3_655 ?
O8 W7 O2 60.3(19) 3_655 3_655 ?
O27 W7 O2 97.5(19) . 3_655 ?
O18 W7 O2 100.9(19) . 3_655 ?
O1 W7 O2 52(2) . 3_655 ?
O21 W8 O26 101.8(14) . . ?
O21 W8 O11 104.2(15) . 3_655 ?
O26 W8 O11 154.0(14) . 3_655 ?
O21 W8 O19 101.0(15) . . ?
O26 W8 O19 85.6(14) . . ?
O11 W8 O19 90.7(14) 3_655 . ?
O21 W8 O50 103.9(14) . . ?
O26 W8 O50 90.3(13) . . ?
O11 W8 O50 82.3(14) 3_655 . ?
O19 W8 O50 155.1(15) . . ?
O21 W8 O2 152(2) . . ?
O26 W8 O2 96.9(19) . . ?
O11 W8 O2 59.6(19) 3_655 . ?
O19 W8 O2 59.3(19) . . ?
O50 W8 O2 97.0(19) . . ?
O21 W8 O3 156.6(19) . . ?
O26 W8 O3 62.6(17) . . ?
O11 W8 O3 92.2(18) 3_655 . ?
O19 W8 O3 95.3(19) . . ?
O50 W8 O3 61.3(18) . . ?
O2 W8 O3 52(2) . . ?
O3 Ge1 O3 180.0 3_655 . ?
O3 Ge1 O4 112(3) 3_655 3_655 ?
O3 Ge1 O4 68(3) . 3_655 ?
O3 Ge1 O4 68(3) 3_655 . ?
O3 Ge1 O4 112(3) . . ?
O4 Ge1 O4 180.0 3_655 . ?
O3 Ge1 O1 111(3) 3_655 . ?
O3 Ge1 O1 69(3) . . ?
O4 Ge1 O1 109(3) 3_655 . ?
O4 Ge1 O1 71(3) . . ?
O3 Ge1 O1 69(3) 3_655 3_655 ?
O3 Ge1 O1 111(3) . 3_655 ?
O4 Ge1 O1 71(3) 3_655 3_655 ?
O4 Ge1 O1 109(3) . 3_655 ?
O1 Ge1 O1 180.0 . 3_655 ?
O3 Ge1 O2 108(3) 3_655 . ?
O3 Ge1 O2 72(3) . . ?
O4 Ge1 O2 110(3) 3_655 . ?
O4 Ge1 O2 70(3) . . ?
O1 Ge1 O2 108(3) . . ?
O1 Ge1 O2 72(3) 3_655 . ?
O3 Ge1 O2 72(3) 3_655 3_655 ?
O3 Ge1 O2 108(3) . 3_655 ?
O4 Ge1 O2 70(3) 3_655 3_655 ?
O4 Ge1 O2 110(3) . 3_655 ?
O1 Ge1 O2 72(3) . 3_655 ?
O1 Ge1 O2 108(3) 3_655 3_655 ?
O2 Ge1 O2 180.0 . 3_655 ?
O31 Cu1 O32 91.2(12) . . ?
O31 Cu1 N2 173.1(12) . . ?
O32 Cu1 N2 92.6(12) . . ?
O31 Cu1 N1 93.0(12) . . ?
O32 Cu1 N1 170.1(13) . . ?
N2 Cu1 N1 84.2(12) . . ?
O30 Cu2 N3 165.4(13) 1_545 . ?
O30 Cu2 N4 87.6(14) 1_545 . ?
N3 Cu2 N4 81.2(13) . . ?
O30 Cu2 Cl1 95.4(11) 1_545 3_755 ?
N3 Cu2 Cl1 96.9(10) . 3_755 ?
N4 Cu2 Cl1 172.7(9) . 3_755 ?
Ge1 O1 W2 120(3) . . ?
Ge1 O1 W1 119(3) . . ?
W2 O1 W1 99(2) . . ?
Ge1 O1 W7 119(3) . . ?
W2 O1 W7 98(2) . . ?
W1 O1 W7 98(2) . . ?
Ge1 O2 W8 119(3) . . ?
Ge1 O2 W4 120(3) . . ?
W8 O2 W4 100(2) . . ?
Ge1 O2 W7 117(3) . 3_655 ?
W8 O2 W7 98(2) . 3_655 ?
W4 O2 W7 98(2) . 3_655 ?
Ge1 O3 W1 122(3) . . ?
Ge1 O3 W5 121(3) . . ?
W1 O3 W5 98(2) . . ?
Ge1 O3 W8 117(3) . . ?
W1 O3 W8 98(2) . . ?
W5 O3 W8 96(2) . . ?
Ge1 O4 W5 122(3) . 3_655 ?
Ge1 O4 W2 118(3) . . ?
W5 O4 W2 98(2) 3_655 . ?
Ge1 O4 W4 119(3) . . ?
W5 O4 W4 98(2) 3_655 . ?
W2 O4 W4 97(2) . . ?
W4 O8 W7 139(2) . 3_655 ?
W1 O10 W5 137.6(18) . . ?
W7 O11 W8 143(2) . 3_655 ?
W4 O14 W2 134(2) . . ?
W2 O17 W1 135(2) . . ?
W7 O18 W2 134.5(19) . . ?
W4 O19 W8 141(2) . . ?
W2 O20 W5 142(2) . 3_655 ?
W4 O23 W5 130.7(19) . 3_655 ?
W8 O26 W1 135.9(16) . . ?
W1 O27 W7 136.4(19) . . ?
C28 O30 Cu2 138(3) . 1_565 ?
C28 O31 Cu1 129(2) . . ?
C26 O32 Cu1 125(3) . . ?
W5 O50 W8 139.5(18) . . ?
C1 N1 C5 121(3) . . ?
C1 N1 Cu1 130(3) . . ?
C5 N1 Cu1 109(2) . . ?
C10 N2 C6 122(3) . . ?
C10 N2 Cu1 126(3) . . ?
C6 N2 Cu1 112(2) . . ?
C11 N3 C15 118(3) . . ?
C11 N3 Cu2 129(3) . . ?
C15 N3 Cu2 113(2) . . ?
C20 N4 C16 118(3) . . ?
C20 N4 Cu2 127(3) . . ?
C16 N4 Cu2 115(2) . . ?
C2 C1 N1 123(4) . . ?
C2 C1 H1 118.4 . . ?
N1 C1 H1 118.4 . . ?
C1 C2 C3 122(5) . . ?
C1 C2 H2 119.1 . . ?
C3 C2 H2 119.1 . . ?
C2 C3 C4 118(4) . . ?
C2 C3 H3 121.2 . . ?
C4 C3 H3 121.2 . . ?
C5 C4 C3 123(4) . . ?
C5 C4 H4 118.7 . . ?
C3 C4 H4 118.7 . . ?
C6 C5 C4 133(4) . . ?
C6 C5 N1 114(3) . . ?
C4 C5 N1 113(3) . . ?
N2 C6 C5 121(3) . . ?
N2 C6 C7 117(3) . . ?
C5 C6 C7 122(3) . . ?
C8 C7 C6 122(4) . . ?
C8 C7 H7 119.0 . . ?
C6 C7 H7 119.0 . . ?
C7 C8 C9 119(4) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?
C8 C9 C10 118(4) . . ?
C8 C9 H9 121.2 . . ?
C10 C9 H9 121.2 . . ?
N2 C10 C9 122(4) . . ?
N2 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
N3 C11 C12 127(4) . . ?
N3 C11 H11 116.6 . . ?
C12 C11 H11 116.6 . . ?
C13 C12 C11 119(4) . . ?
C13 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
C12 C13 C14 121(5) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C13 C14 C15 120(4) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C16 C15 N3 119(3) . . ?
C16 C15 C14 127(4) . . ?
N3 C15 C14 115(3) . . ?
C15 C16 C17 127(4) . . ?
C15 C16 N4 112(3) . . ?
C17 C16 N4 121(4) . . ?
C18 C17 C16 117(5) . . ?
C18 C17 H17 121.4 . . ?
C16 C17 H17 121.4 . . ?
C19 C18 C17 124(5) . . ?
C19 C18 H18 118.1 . . ?
C17 C18 H18 118.1 . . ?
C18 C19 C20 118(4) . . ?
C18 C19 H19 121.1 . . ?
C20 C19 H19 121.1 . . ?
N4 C20 C19 123(4) . . ?
N4 C20 H20 118.6 . . ?
C19 C20 H20 118.6 . . ?
C27 C22 C23 125(4) . . ?
C27 C22 H22 117.5 . . ?
C23 C22 H22 117.5 . . ?
C22 C23 C24 119(4) . . ?
C22 C23 H23 120.3 . . ?
C24 C23 H23 120.3 . . ?
N5 C24 C23 118(4) . . ?
C24 N5 C26 124(3) . . ?
O32 C26 N5 114(3) . . ?
O32 C26 C27 129(4) . . ?
N5 C26 C27 117(3) . . ?
C22 C27 C28 121(3) . . ?
C22 C27 C26 117(3) . . ?
C28 C27 C26 121(3) . . ?
O30 C28 O31 122(3) . . ?
O30 C28 C27 117(3) . . ?
O31 C28 C27 121(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 Ge1 O1 W2 58(4) 3_655 . . . ?
O3 Ge1 O1 W2 -122(4) . . . . ?
O4 Ge1 O1 W2 -179(3) 3_655 . . . ?
O4 Ge1 O1 W2 1(3) . . . . ?
O2 Ge1 O1 W2 -60(4) . . . . ?
O2 Ge1 O1 W2 120(4) 3_655 . . . ?
O3 Ge1 O1 W1 180(3) 3_655 . . . ?
O3 Ge1 O1 W1 0(3) . . . . ?
O4 Ge1 O1 W1 -57(4) 3_655 . . . ?
O4 Ge1 O1 W1 123(4) . . . . ?
O2 Ge1 O1 W1 62(4) . . . . ?
O2 Ge1 O1 W1 -118(4) 3_655 . . . ?
O3 Ge1 O1 W7 -62(4) 3_655 . . . ?
O3 Ge1 O1 W7 118(4) . . . . ?
O4 Ge1 O1 W7 62(4) 3_655 . . . ?
O4 Ge1 O1 W7 -118(4) . . . . ?
O2 Ge1 O1 W7 -180(3) . . . . ?
O2 Ge1 O1 W7 0(3) 3_655 . . . ?
O3 Ge1 O2 W8 179(3) 3_655 . . . ?
O3 Ge1 O2 W8 -1(3) . . . . ?
O4 Ge1 O2 W8 57(4) 3_655 . . . ?
O4 Ge1 O2 W8 -123(4) . . . . ?
O1 Ge1 O2 W8 -62(4) . . . . ?
O1 Ge1 O2 W8 118(4) 3_655 . . . ?
O3 Ge1 O2 W4 -58(4) 3_655 . . . ?
O3 Ge1 O2 W4 122(4) . . . . ?
O4 Ge1 O2 W4 -180(3) 3_655 . . . ?
O4 Ge1 O2 W4 0(3) . . . . ?
O1 Ge1 O2 W4 62(4) . . . . ?
O1 Ge1 O2 W4 -118(4) 3_655 . . . ?
O3 Ge1 O2 W7 61(4) 3_655 . . 3_655 ?
O3 Ge1 O2 W7 -119(4) . . . 3_655 ?
O4 Ge1 O2 W7 -61(4) 3_655 . . 3_655 ?
O4 Ge1 O2 W7 119(4) . . . 3_655 ?
O1 Ge1 O2 W7 -180(3) . . . 3_655 ?
O1 Ge1 O2 W7 0(3) 3_655 . . 3_655 ?
O4 Ge1 O3 W1 122(4) 3_655 . . . ?
O4 Ge1 O3 W1 -58(4) . . . . ?
O1 Ge1 O3 W1 0(3) . . . . ?
O1 Ge1 O3 W1 -180(3) 3_655 . . . ?
O2 Ge1 O3 W1 -118(4) . . . . ?
O2 Ge1 O3 W1 62(4) 3_655 . . . ?
O4 Ge1 O3 W5 -3(3) 3_655 . . . ?
O4 Ge1 O3 W5 177(3) . . . . ?
O1 Ge1 O3 W5 -125(4) . . . . ?
O1 Ge1 O3 W5 55(4) 3_655 . . . ?
O2 Ge1 O3 W5 117(4) . . . . ?
O2 Ge1 O3 W5 -63(4) 3_655 . . . ?
O4 Ge1 O3 W8 -119(4) 3_655 . . . ?
O4 Ge1 O3 W8 61(4) . . . . ?
O1 Ge1 O3 W8 119(4) . . . . ?
O1 Ge1 O3 W8 -61(4) 3_655 . . . ?
O2 Ge1 O3 W8 1(3) . . . . ?
O2 Ge1 O3 W8 -179(3) 3_655 . . . ?
O3 Ge1 O4 W5 -3(3) 3_655 . . 3_655 ?
O3 Ge1 O4 W5 177(3) . . . 3_655 ?
O1 Ge1 O4 W5 120(4) . . . 3_655 ?
O1 Ge1 O4 W5 -60(4) 3_655 . . 3_655 ?
O2 Ge1 O4 W5 -123(4) . . . 3_655 ?
O2 Ge1 O4 W5 57(4) 3_655 . . 3_655 ?
O3 Ge1 O4 W2 -124(4) 3_655 . . . ?
O3 Ge1 O4 W2 56(4) . . . . ?
O1 Ge1 O4 W2 -1(3) . . . . ?
O1 Ge1 O4 W2 179(3) 3_655 . . . ?
O2 Ge1 O4 W2 116(4) . . . . ?
O2 Ge1 O4 W2 -64(4) 3_655 . . . ?
O3 Ge1 O4 W4 119(4) 3_655 . . . ?
O3 Ge1 O4 W4 -61(4) . . . . ?
O1 Ge1 O4 W4 -118(4) . . . . ?
O1 Ge1 O4 W4 62(4) 3_655 . . . ?
O2 Ge1 O4 W4 0(3) . . . . ?
O2 Ge1 O4 W4 180(3) 3_655 . . . ?
O24 W4 O8 W7 -155(3) . . . 3_655 ?
O19 W4 O8 W7 -53(3) . . . 3_655 ?
O14 W4 O8 W7 23(7) . . . 3_655 ?
O23 W4 O8 W7 108(3) . . . 3_655 ?
O2 W4 O8 W7 3(3) . . . 3_655 ?
O4 W4 O8 W7 43(4) . . . 3_655 ?
O34 W1 O10 W5 151(3) . . . . ?
O27 W1 O10 W5 -107(3) . . . . ?
O17 W1 O10 W5 -31(6) . . . . ?
O26 W1 O10 W5 51(3) . . . . ?
O3 W1 O10 W5 -8(3) . . . . ?
O1 W1 O10 W5 -44(3) . . . . ?
O29 W7 O11 W8 140(3) . . . 3_655 ?
O8 W7 O11 W8 39(3) 3_655 . . 3_655 ?
O27 W7 O11 W8 -42(5) . . . 3_655 ?
O18 W7 O11 W8 -120(3) . . . 3_655 ?
O1 W7 O11 W8 -57(4) . . . 3_655 ?
O2 W7 O11 W8 -15(3) 3_655 . . 3_655 ?
O33 W2 O17 W1 -162(3) . . . . ?
O20 W2 O17 W1 8(6) . . . . ?
O18 W2 O17 W1 -64(3) . . . . ?
O14 W2 O17 W1 100(3) . . . . ?
O1 W2 O17 W1 0(3) . . . . ?
O4 W2 O17 W1 35(3) . . . . ?
O24 W4 O19 W8 151(3) . . . . ?
O8 W4 O19 W8 50(3) . . . . ?
O14 W4 O19 W8 -110(3) . . . . ?
O23 W4 O19 W8 -37(6) . . . . ?
O2 W4 O19 W8 -8(3) . . . . ?
O4 W4 O19 W8 -46(3) . . . . ?
O21 W8 O19 W4 -150(3) . . . . ?
O26 W8 O19 W4 109(3) . . . . ?
O11 W8 O19 W4 -46(3) 3_655 . . . ?
O50 W8 O19 W4 27(6) . . . . ?
O2 W8 O19 W4 8(3) . . . . ?
O3 W8 O19 W4 47(3) . . . . ?
O33 W2 O20 W5 -149(3) . . . 3_655 ?
O17 W2 O20 W5 41(6) . . . 3_655 ?
O18 W2 O20 W5 113(3) . . . 3_655 ?
O14 W2 O20 W5 -51(3) . . . 3_655 ?
O1 W2 O20 W5 49(4) . . . 3_655 ?
O4 W2 O20 W5 10(3) . . . 3_655 ?
O21 W8 O26 W1 154(2) . . . . ?
O11 W8 O26 W1 -24(5) 3_655 . . . ?
O19 W8 O26 W1 -106(3) . . . . ?
O50 W8 O26 W1 49(3) . . . . ?
O2 W8 O26 W1 -48(3) . . . . ?
O3 W8 O26 W1 -8(3) . . . . ?
O34 W1 O27 W7 -156(3) . . . . ?
O10 W1 O27 W7 104(3) . . . . ?
O17 W1 O27 W7 -56(3) . . . . ?
O26 W1 O27 W7 19(6) . . . . ?
O3 W1 O27 W7 43(3) . . . . ?
O1 W1 O27 W7 4(3) . . . . ?
O25 W5 O50 W8 152(3) . . . . ?
O20 W5 O50 W8 -103(3) 3_655 . . . ?
O10 W5 O50 W8 51(3) . . . . ?
O23 W5 O50 W8 -30(6) 3_655 . . . ?
O4 W5 O50 W8 -44(3) 3_655 . . . ?
O3 W5 O50 W8 -6(3) . . . . ?
C5 N1 C1 C2 1(6) . . . . ?
Cu1 N1 C1 C2 -174(3) . . . . ?
N1 C1 C2 C3 -7(7) . . . . ?
C1 C2 C3 C4 8(7) . . . . ?
C2 C3 C4 C5 -4(7) . . . . ?
C3 C4 C5 C6 178(4) . . . . ?
C3 C4 C5 N1 -1(6) . . . . ?
C1 N1 C5 C6 -176(4) . . . . ?
Cu1 N1 C5 C6 0(4) . . . . ?
C1 N1 C5 C4 3(5) . . . . ?
Cu1 N1 C5 C4 179(3) . . . . ?
C10 N2 C6 C5 177(3) . . . . ?
Cu1 N2 C6 C5 3(4) . . . . ?
C10 N2 C6 C7 -7(5) . . . . ?
Cu1 N2 C6 C7 -180(3) . . . . ?
C4 C5 C6 N2 179(4) . . . . ?
N1 C5 C6 N2 -2(5) . . . . ?
C4 C5 C6 C7 2(7) . . . . ?
N1 C5 C6 C7 -179(3) . . . . ?
N2 C6 C7 C8 8(6) . . . . ?
C5 C6 C7 C8 -175(4) . . . . ?
C6 C7 C8 C9 -8(7) . . . . ?
C7 C8 C9 C10 6(7) . . . . ?
C6 N2 C10 C9 5(6) . . . . ?
Cu1 N2 C10 C9 177(3) . . . . ?
C8 C9 C10 N2 -5(6) . . . . ?
C15 N3 C11 C12 -3(6) . . . . ?
Cu2 N3 C11 C12 175(3) . . . . ?
N3 C11 C12 C13 4(7) . . . . ?
C11 C12 C13 C14 -6(7) . . . . ?
C12 C13 C14 C15 5(7) . . . . ?
C11 N3 C15 C16 -179(4) . . . . ?
Cu2 N3 C15 C16 3(4) . . . . ?
C11 N3 C15 C14 2(5) . . . . ?
Cu2 N3 C15 C14 -176(3) . . . . ?
C13 C14 C15 C16 178(4) . . . . ?
C13 C14 C15 N3 -4(6) . . . . ?
N3 C15 C16 C17 -175(4) . . . . ?
C14 C15 C16 C17 4(7) . . . . ?
N3 C15 C16 N4 0(5) . . . . ?
C14 C15 C16 N4 179(4) . . . . ?
C20 N4 C16 C15 -177(3) . . . . ?
Cu2 N4 C16 C15 -3(4) . . . . ?
C20 N4 C16 C17 -2(5) . . . . ?
Cu2 N4 C16 C17 172(3) . . . . ?
C15 C16 C17 C18 176(4) . . . . ?
N4 C16 C17 C18 2(6) . . . . ?
C16 C17 C18 C19 1(7) . . . . ?
C17 C18 C19 C20 -3(7) . . . . ?
C16 N4 C20 C19 0(6) . . . . ?
Cu2 N4 C20 C19 -173(3) . . . . ?
C18 C19 C20 N4 2(7) . . . . ?
C27 C22 C23 C24 -5(7) . . . . ?
C22 C23 C24 N5 4(6) . . . . ?
C23 C24 N5 C26 -4(6) . . . . ?
Cu1 O32 C26 N5 163(2) . . . . ?
Cu1 O32 C26 C27 -21(6) . . . . ?
C24 N5 C26 O32 -179(4) . . . . ?
C24 N5 C26 C27 4(5) . . . . ?
C23 C22 C27 C28 178(4) . . . . ?
C23 C22 C27 C26 4(6) . . . . ?
O32 C26 C27 C22 180(4) . . . . ?
N5 C26 C27 C22 -4(5) . . . . ?
O32 C26 C27 C28 6(6) . . . . ?
N5 C26 C27 C28 -178(3) . . . . ?
Cu2 O30 C28 O31 24(7) 1_565 . . . ?
Cu2 O30 C28 C27 -157(3) 1_565 . . . ?
Cu1 O31 C28 O30 -171(3) . . . . ?
Cu1 O31 C28 C27 10(5) . . . . ?
C22 C27 C28 O30 8(6) . . . . ?
C26 C27 C28 O30 -179(4) . . . . ?
C22 C27 C28 O31 -173(4) . . . . ?
C26 C27 C28 O31 1(5) . . . . ?

_refine_diff_density_max         3.271
_refine_diff_density_min         -2.801
_refine_diff_density_rms         0.463



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_5
_database_code_depnum_ccdc_archive 'CCDC 1419959'
_audit_update_record             
;
2015-12-07 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT306_shelx_5             
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O3w Check
RESPONSE: The hydrogens of the water molecule were not added.
;

_vrf_PLAT342_shelx_5             
;
PROBLEM: Low Bond Precision on C-C Bonds .........0.0219 Ang
RESPONSE: The quality of this crystal was poor.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H49 As2 Cu3 N9 O73 W18'
_chemical_formula_weight         5641.78

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'
As As 0.0499 2.0058 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   16.729(3)
_cell_length_b                   18.897(4)
_cell_length_c                   17.003(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.82(3)
_cell_angle_gamma                90
_cell_volume                     5219.5(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    34562
_cell_measurement_theta_min      3.03
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            dark_green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.590
_exptl_crystal_F_000             5010
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    21.074
_shelx_estimated_absorpt_T_min   0.133
_shelx_estimated_absorpt_T_max   0.186
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.1854
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            47689
_diffrn_reflns_av_unetI/netI     0.0812
_diffrn_reflns_av_R_equivalents  0.0825
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.023
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             12254
_reflns_number_gt                8788
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker XSCANS'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0491P)²+18.7487P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12254
_refine_ls_number_parameters     874
_refine_ls_number_restraints     935
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0463
_refine_ls_wR_factor_ref         0.1143
_refine_ls_wR_factor_gt          0.1053
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      0.984
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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
W2 W 0.16441(3) -3.06289(2) 2.85405(3) 0.02649(11) Uani 1 1 d . . . . .
W4 W 0.37556(3) -3.06236(2) 2.81404(3) 0.02763(12) Uani 1 1 d . . . . .
W10 W 0.23672(3) -3.15178(2) 3.02789(3) 0.02550(11) Uani 1 1 d . . . . .
W9 W 0.08448(3) -3.16021(2) 2.66218(3) 0.02850(12) Uani 1 1 d . . . . .
W8 W 0.29550(3) -3.16047(2) 2.62230(3) 0.02992(12) Uani 1 1 d . . . . .
W7 W 0.44788(3) -3.15209(2) 2.98765(3) 0.02622(11) Uani 1 1 d . . . . .
W6 W 0.52003(3) -3.16075(3) 2.71800(3) 0.03348(13) Uani 1 1 d . . . . .
W5 W 0.03894(4) -3.2500 2.99457(4) 0.03074(16) Uani 1 2 d S T P . .
As2 As 0.15949(8) -3.2500 2.84815(9) 0.0191(3) Uani 1 2 d S T P . .
W3 W -0.03410(3) -3.16057(2) 2.82109(3) 0.03049(12) Uani 1 1 d . . . . .
As1 As 0.37534(8) -3.2500 2.80719(9) 0.0202(3) Uani 1 2 d S T P . .
W1 W 0.59298(4) -3.2500 2.89170(4) 0.03059(16) Uani 1 2 d S T P . .
O36 O -0.0314(4) -3.1789(4) 2.9327(5) 0.0312(16) Uani 1 1 d . U . . .
O35 O 0.2552(4) -3.1208(4) 3.1247(5) 0.0330(18) Uani 1 1 d . U . . .
O34 O 0.3085(6) -3.2500 2.7168(6) 0.024(2) Uani 1 2 d S TU P . .
O33 O -0.1161(4) -3.1040(4) 2.7962(5) 0.041(2) Uani 1 1 d . U . . .
O32 O 0.4134(5) -3.1676(4) 2.6467(5) 0.0343(17) Uani 1 1 d . U . . .
O31 O 0.4374(4) -3.0671(4) 2.9248(5) 0.0312(17) Uani 1 1 d . U . . .
O30 O 0.0018(4) -3.1679(4) 2.7229(5) 0.0325(17) Uani 1 1 d . U . . .
O28 O 0.4716(6) -3.2500 2.7895(6) 0.029(2) Uani 1 2 d S TU P . .
O29 O 0.6050(4) -3.1793(4) 2.8137(5) 0.0346(17) Uani 1 1 d . U . . .
O27 O 0.6894(6) -3.2500 2.9540(7) 0.039(3) Uani 1 2 d S TU P . .
O26 O 0.1480(6) -3.2500 2.7481(6) 0.026(2) Uani 1 2 d S TU P . .
O25 O 0.0496(6) -3.2500 2.6118(6) 0.030(2) Uani 1 2 d S TU P . .
O24 O 0.1843(4) -3.1658(4) 2.6248(4) 0.0300(16) Uani 1 1 d . U . . .
O23 O 0.1397(4) -2.9758(4) 2.8408(5) 0.038(2) Uani 1 1 d . U . . .
O22 O 0.4345(6) -3.2500 3.0085(6) 0.028(2) Uani 1 2 d S TU P . .
O21 O 0.3134(4) -3.0994(4) 2.7131(4) 0.0286(15) Uani 1 1 d . U . . .
O20 O 0.3682(4) -3.1771(4) 2.8605(4) 0.0251(15) Uani 1 1 d . U . . .
O19 O 0.1239(4) -3.1824(4) 3.0178(4) 0.0268(15) Uani 1 1 d . U . . .
O18 O 0.0630(5) -3.2500 2.8673(6) 0.025(2) Uani 1 2 d S TU P . .
O17 O 0.1975(4) -3.0665(4) 2.9693(5) 0.0299(16) Uani 1 1 d . U . . .
O16 O -0.0877(6) -3.2500 2.7951(7) 0.036(3) Uani 1 2 d S TU P . .
O15 O 0.2892(6) -3.2500 2.5671(6) 0.032(2) Uani 1 2 d S TU P . .
O14 O 0.5360(4) -3.1821(4) 2.9403(5) 0.0296(16) Uani 1 1 d . U . . .
O13 O 0.1398(4) -3.0991(4) 2.7468(4) 0.0280(15) Uani 1 1 d . U . . .
O12 O 0.2627(6) -3.2500 3.0424(6) 0.029(2) Uani 1 2 d S TU P . .
O11 O 0.4703(4) -3.1000(4) 2.7806(4) 0.0291(16) Uani 1 1 d . U . . .
O10 O 0.2770(4) -3.0524(4) 2.8480(4) 0.0280(16) Uani 1 1 d . U . . .
O9 O 0.2067(4) -3.1764(4) 2.8903(4) 0.0226(14) Uani 1 1 d . U . . .
O8 O 0.0563(4) -3.0988(4) 2.8567(4) 0.0284(16) Uani 1 1 d . U . . .
O7 O 0.3434(4) -3.1358(4) 3.0097(4) 0.0279(16) Uani 1 1 d . U . . .
Cu1 Cu -0.08586(11) -3.2500 3.15450(11) 0.0310(5) Uani 1 2 d S T P . .
Cu2 Cu 0.3441(2) -3.0578(2) 2.4369(2) 0.0611(10) Uani 0.5 1 d . . P . .
Cu4 Cu -0.25163(13) -3.2500 3.20774(13) 0.0400(5) Uani 1 2 d S T P . .
O52 O -0.2646(5) -3.3252(5) 3.1274(5) 0.042(2) Uani 1 1 d . U . . .
O6 O 0.5074(5) -3.1236(4) 3.0774(5) 0.041(2) Uani 1 1 d . U . . .
O5 O 0.0333(5) -3.1041(4) 2.5896(5) 0.041(2) Uani 1 1 d . U . . .
O4 O 0.3900(5) -2.9757(4) 2.7929(5) 0.0376(19) Uani 1 1 d . U . . .
O3 O 0.0056(6) -3.2500 3.0829(7) 0.040(3) Uani 1 2 d S TU P B .
O2 O 0.2860(5) -3.1036(4) 2.5426(5) 0.043(2) Uani 1 1 d . U . . .
O1 O 0.5704(5) -3.1038(4) 2.6673(5) 0.047(2) Uani 1 1 d . U . . .
O51 O 0.5470(6) -3.2500 2.6754(7) 0.038(2) Uani 1 2 d S TU P . .
O50 O -0.1487(5) -3.3216(5) 3.0854(6) 0.052(2) Uani 1 1 d . U . . .
C13 C -0.2198(7) -3.3421(6) 3.0831(8) 0.032(3) Uani 1 1 d . . . . .
N3 N -0.2190(7) -3.3211(6) 3.2988(6) 0.049(3) Uani 1 1 d . . . . .
C7 C -0.2184(7) -3.4051(6) 2.9513(8) 0.042(3) Uani 1 1 d . . . . .
H7A H -0.1679 -3.3843 2.9518 0.050 Uiso 1 1 calc R U . . .
C8 C -0.2536(8) -3.4480(7) 2.8897(10) 0.053(4) Uani 1 1 d . . . . .
H8A H -0.2270 -3.4571 2.8486 0.064 Uiso 1 1 calc R U . . .
N1 N -0.3257(7) -3.4770(6) 2.8872(7) 0.044(3) Uani 1 1 d . . . . .
C10 C -0.3632(7) -3.4680(6) 2.9465(9) 0.046(3) Uani 1 1 d . . . . .
H10A H -0.4131 -3.4908 2.9439 0.055 Uiso 1 1 calc R U . . .
C11 C -0.3304(6) -3.4258(6) 3.0119(8) 0.034(3) Uani 1 1 d . . . . .
H11A H -0.3572 -3.4202 3.0536 0.041 Uiso 1 1 calc R U . . .
C12 C -0.2560(7) -3.3914(6) 3.0144(7) 0.030(3) Uani 1 1 d . . . . .
C40 C 0.285(2) -2.832(2) 2.367(2) 0.062(9) Uani 0.5 1 d . U P A -1
H40A H 0.2710 -2.8726 2.3348 0.074 Uiso 0.5 1 calc R U P A -1
N15 N 0.2868(12) -2.6962(12) 2.3787(14) 0.032(5) Uani 0.5 1 d . U P A -1
C42 C 0.325(3) -2.707(3) 2.449(3) 0.101(14) Uani 0.5 1 d . U P A -1
H42A H 0.3430 -2.6680 2.4814 0.121 Uiso 0.5 1 calc R U P A -1
C43 C 0.3452(18) -2.7785(14) 2.488(2) 0.054(8) Uani 0.5 1 d . U P A -1
H43A H 0.3742 -2.7831 2.5414 0.065 Uiso 0.5 1 calc R U P A -1
C39 C 0.321(2) -2.8326(17) 2.443(2) 0.065(9) Uani 0.5 1 d D U P A -1
C5 C -0.1894(7) -3.2856(7) 3.3720(8) 0.042(3) Uani 1 1 d . . . . .
O1W O -0.3913(9) -3.2500 3.1917(12) 0.113(7) Uani 1 2 d S TU P . .
C6 C -0.1310(8) -3.2860(8) 3.5171(8) 0.064(5) Uani 1 1 d . . . . .
H6A H -0.1109 -3.3104 3.5652 0.076 Uiso 1 1 calc R U . . .
C4 C -0.1622(9) -3.3249(9) 3.4421(9) 0.059(4) Uani 1 1 d . . . . .
C1 C -0.2203(16) -3.3878(10) 3.2941(12) 0.118(9) Uani 1 1 d . U . . .
H1A H -0.2341 -3.4095 3.2436 0.142 Uiso 1 1 calc R U . . .
C3 C -0.1600(15) -3.3983(13) 3.4373(12) 0.129(10) Uani 1 1 d . U . . .
H3A H -0.1322 -3.4255 3.4808 0.155 Uiso 1 1 calc R U . . .
C2 C -0.2010(14) -3.4293(13) 3.3644(15) 0.116(7) Uani 1 1 d . U . . .
H2A H -0.2154 -3.4769 3.3625 0.139 Uiso 1 1 calc R U . . .
C14 C -0.0489(10) -3.1341(8) 3.2790(10) 0.068(10) Uani 0.5 1 d G . P B -1
H14A H -0.0827 -3.1043 3.2418 0.082 Uiso 0.5 1 calc R U P B -1
C15 C -0.0082(12) -3.1083(7) 3.3545(11) 0.069(10) Uani 0.5 1 d G . P B -1
H15A H -0.0148 -3.0613 3.3679 0.083 Uiso 0.5 1 calc R U P B -1
C16 C 0.0423(11) -3.1528(9) 3.4101(8) 0.054(8) Uani 0.5 1 d G U P B -1
H16A H 0.0695 -3.1356 3.4606 0.065 Uiso 0.5 1 calc R U P B -1
C17 C 0.0521(8) -3.2231(8) 3.3901(7) 0.037(6) Uani 0.5 1 d G . P B -1
C18 C 0.0114(8) -3.2488(7) 3.3146(8) 0.038(4) Uani 0.5 1 d G U P B -1
N8 N -0.0391(8) -3.2044(8) 3.2590(7) 0.038(5) Uani 0.5 1 d G . P B -1
C19 C 0.1034(17) -3.271(3) 3.4406(16) 0.07(2) Uani 0.5 1 d . . P B -1
H19A H 0.1352 -3.2548 3.4900 0.089 Uiso 0.5 1 calc R U P B -1
C20 C 0.108(3) -3.340(2) 3.420(2) 0.089(14) Uani 0.5 1 d . . P B -1
H20A H 0.1375 -3.3712 3.4588 0.107 Uiso 0.5 1 calc R U P B -1
C24 C 0.0204(9) -3.3170(7) 3.2921(9) 0.038(6) Uani 0.5 1 d G . P B -1
C21 C 0.0701(10) -3.3673(10) 3.3400(9) 0.061(9) Uani 0.5 1 d G . P B -1
C25 C 0.0840(11) -3.4321(9) 3.3070(14) 0.094(15) Uani 0.5 1 d G . P B -1
H25A H 0.1172 -3.4657 3.3390 0.113 Uiso 0.5 1 calc R U P B -1
C26 C 0.0483(12) -3.4466(7) 3.2260(15) 0.070(10) Uani 0.5 1 d G . P B -1
H26A H 0.0576 -3.4900 3.2039 0.084 Uiso 0.5 1 calc R U P B -1
C27 C -0.0014(11) -3.3963(9) 3.1782(10) 0.065(10) Uani 0.5 1 d G . P B -1
H27A H -0.0253 -3.4061 3.1240 0.078 Uiso 0.5 1 calc R U P B -1
N9 N -0.0153(8) -3.3315(7) 3.2112(9) 0.048(6) Uani 0.5 1 d G . P B -1
O45 O 0.3052(14) -2.9546(10) 2.4294(14) 0.074(5) Uani 0.5 1 d . U P A -1
O2W O 0.4383(14) -3.0403(13) 2.5258(14) 0.093(7) Uani 0.5 1 d . U P A .
HW2A H 0.4689 -3.0544 2.5704 0.139 Uiso 0.5 1 d R U P . .
HW2B H 0.4501 -2.9972 2.5197 0.139 Uiso 0.5 1 d R U P . .
C31 C 0.1949(15) -3.243(4) 2.2463(17) 0.053(7) Uani 0.5 1 d . U P A -1
H31A H 0.1575 -3.2602 2.2009 0.064 Uiso 0.5 1 calc R U P A -1
O46 O 0.3969(18) -2.9151(16) 2.5431(18) 0.119(9) Uani 0.5 1 d D U P A -1
C38 C 0.345(2) -2.9072(18) 2.4692(19) 0.097(11) Uani 0.5 1 d D U P A -1
N12 N 0.2501(9) -3.0814(10) 2.3489(8) 0.047(6) Uani 0.5 1 d G . P A -1
C35 C 0.1908(11) -3.0358(7) 2.3050(10) 0.053(7) Uani 0.5 1 d G U P A -1
H35A H 0.1911 -2.9883 2.3194 0.064 Uiso 0.5 1 calc R U P A -1
C36 C 0.1311(10) -3.0611(9) 2.2397(10) 0.057(8) Uani 0.5 1 d G . P A -1
H36A H 0.0914 -3.0305 2.2103 0.069 Uiso 0.5 1 calc R U P A -1
C37 C 0.1306(10) -3.1321(10) 2.2182(9) 0.070(10) Uani 0.5 1 d G . P A -1
H37A H 0.0907 -3.1490 2.1744 0.084 Uiso 0.5 1 calc R U P A -1
C33 C 0.1899(12) -3.1777(7) 2.2621(12) 0.055(7) Uani 0.5 1 d G U P A -1
C34 C 0.2497(10) -3.1524(9) 2.3274(11) 0.073(11) Uani 0.5 1 d G . P A -1
N13 N 0.3677(12) -3.1604(8) 2.4284(12) 0.064(8) Uani 0.5 1 d G . P A -1
C29 C 0.3070(9) -3.1922(10) 2.3686(10) 0.065(9) Uani 0.5 1 d G . P A -1
C30 C 0.3086(11) -3.2648(10) 2.3563(11) 0.060(8) Uani 0.5 1 d G U P A -1
C51 C 0.3709(15) -3.3057(8) 2.4037(15) 0.118(16) Uani 0.5 1 d G U P A -1
H51A H 0.3720 -3.3543 2.3954 0.141 Uiso 0.5 1 calc R U P A -1
C52 C 0.4316(11) -3.2740(12) 2.4635(12) 0.082(11) Uani 0.5 1 d G U P A -1
H52A H 0.4733 -3.3013 2.4952 0.099 Uiso 0.5 1 calc R U P A -1
C28 C 0.4300(9) -3.2013(12) 2.4758(9) 0.076(10) Uani 0.5 1 d G U P A -1
H28A H 0.4707 -3.1801 2.5158 0.091 Uiso 0.5 1 calc R U P A -1
O3W O 0.5822(16) -2.7500 1.7994(17) 0.207(15) Uani 1 2 d S T P . .
O4W O -0.4290(17) -3.5696(15) 2.7712(18) 0.286(13) Uani 1 1 d . U . . .
HW4A H -0.3947 -3.5463 2.8068 0.428 Uiso 1 1 d R U . . .
HW4B H -0.4215 -3.6133 2.7826 0.428 Uiso 1 1 d R U . . .
C41 C 0.2665(15) -2.740(3) 2.3303(17) 0.081(9) Uani 0.5 1 d . U P A -1
H41A H 0.2423 -2.7294 2.2764 0.097 Uiso 0.5 1 calc R U P A -1
C32 C 0.2491(17) -3.2889(15) 2.2890(18) 0.049(7) Uani 0.5 1 d . . P A -1
H32A H 0.2472 -3.3363 2.2741 0.059 Uiso 0.5 1 calc R U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W2 O23 1.698(8) . ?
W2 O13 1.899(7) . ?
W2 O17 1.906(8) . ?
W2 O10 1.920(7) . ?
W2 O8 1.941(7) . ?
W2 O9 2.296(7) . ?
W4 O4 1.706(8) . ?
W4 O10 1.883(7) . ?
W4 O21 1.914(7) . ?
W4 O31 1.922(7) . ?
W4 O11 1.942(7) . ?
W4 O20 2.322(7) . ?
W10 O35 1.704(8) . ?
W10 O7 1.907(7) . ?
W10 O12 1.909(2) . ?
W10 O17 1.926(7) . ?
W10 O19 1.941(7) . ?
W10 O9 2.319(7) . ?
W9 O5 1.696(7) . ?
W9 O13 1.903(7) . ?
W9 O30 1.919(8) . ?
W9 O24 1.927(8) . ?
W9 O25 1.927(5) . ?
W9 O26 2.324(7) . ?
W8 O2 1.707(8) . ?
W8 O24 1.873(7) . ?
W8 O21 1.894(7) . ?
W8 O32 1.921(8) . ?
W8 O15 1.925(5) . ?
W8 O34 2.307(7) . ?
W7 O6 1.699(8) . ?
W7 O7 1.898(7) . ?
W7 O22 1.907(3) . ?
W7 O31 1.913(7) . ?
W7 O14 1.926(7) . ?
W7 O20 2.302(7) . ?
W6 O1 1.720(8) . ?
W6 O11 1.889(7) . ?
W6 O32 1.907(8) . ?
W6 O29 1.921(8) . ?
W6 O51 1.931(5) . ?
W6 O28 2.335(7) . ?
W5 O3 1.722(11) . ?
W5 O19 1.882(7) . ?
W5 O19 1.882(7) 4_5/5 ?
W5 O36 1.925(7) 4_5/5 ?
W5 O36 1.925(7) . ?
W5 O18 2.294(10) . ?
As2 O26 1.666(10) . ?
As2 O9 1.674(7) . ?
As2 O9 1.674(7) 4_5/5 ?
As2 O18 1.721(9) . ?
W3 O33 1.710(7) . ?
W3 O8 1.893(7) . ?
W3 O30 1.909(8) . ?
W3 O16 1.915(5) . ?
W3 O36 1.919(8) . ?
W3 O18 2.346(6) . ?
As1 O20 1.668(7) 4_5/5 ?
As1 O20 1.668(7) . ?
As1 O34 1.672(9) . ?
As1 O28 1.706(10) . ?
W1 O27 1.706(10) . ?
W1 O14 1.901(8) . ?
W1 O14 1.901(7) 4_5/5 ?
W1 O29 1.926(8) 4_5/5 ?
W1 O29 1.926(8) . ?
W1 O28 2.336(10) . ?
O34 W8 2.307(7) 4_5/5 ?
O28 W6 2.335(7) 4_5/5 ?
O26 W9 2.324(6) 4_5/5 ?
O25 W9 1.928(4) 4_5/5 ?
O22 W7 1.907(3) 4_5/5 ?
O18 W3 2.346(6) 4_5/5 ?
O16 W3 1.915(4) 4_5/5 ?
O15 W8 1.925(5) 4_5/5 ?
O12 W10 1.909(2) 4_5/5 ?
Cu1 O50 1.930(9) . ?
Cu1 O50 1.930(9) 4_5/5 ?
Cu1 N8 1.962(11) . ?
Cu1 N9 2.038(12) . ?
Cu1 O3 2.171(11) . ?
Cu2 O2W 1.93(2) . ?
Cu2 N12 1.946(13) . ?
Cu2 N13 1.992(16) . ?
Cu2 O45 2.05(2) . ?
Cu2 O2 2.399(9) . ?
Cu4 O52 1.946(9) . ?
Cu4 O52 1.946(9) 4_5/5 ?
Cu4 N3 2.024(11) 4_5/5 ?
Cu4 N3 2.024(11) . ?
Cu4 O1W 2.286(15) . ?
O52 C13 1.226(14) . ?
O51 W6 1.931(5) 4_5/5 ?
O50 C13 1.243(13) . ?
C13 C12 1.503(16) . ?
N3 C1 1.26(2) . ?
N3 C5 1.397(15) . ?
C7 C8 1.344(17) . ?
C7 C12 1.393(16) . ?
C8 N1 1.315(16) . ?
N1 C10 1.322(17) . ?
C10 C11 1.372(17) . ?
C11 C12 1.396(15) . ?
C40 C39 1.30(5) . ?
C40 C41 1.85(7) . ?
N15 C41 1.16(5) . ?
N15 C42 1.24(5) . ?
C42 C43 1.50(5) . ?
C43 C39 1.28(4) . ?
C39 C38 1.503(10) . ?
C5 C5 1.35(3) 4_5/5 ?
C5 C4 1.385(18) . ?
C6 C6 1.36(3) 4_5/5 ?
C6 C4 1.46(2) . ?
C4 C3 1.39(3) . ?
C1 C2 1.40(3) . ?
C3 C2 1.39(3) . ?
C14 C15 1.3900 . ?
C14 N8 1.3900 . ?
C15 C16 1.3900 . ?
C16 C17 1.3900 . ?
C17 C19 1.39(4) . ?
C17 C18 1.3900 . ?
C18 C24 1.362(18) . ?
C18 N8 1.3900 . ?
C19 C20 1.36(7) . ?
C20 C21 1.45(4) . ?
C24 C21 1.3900 . ?
C24 N9 1.3900 . ?
C21 C25 1.3900 . ?
C25 C26 1.3900 . ?
C26 C27 1.3900 . ?
C27 N9 1.3900 . ?
O45 C38 1.22(4) . ?
C31 C33 1.26(7) . ?
C31 C32 1.34(5) . ?
O46 C38 1.354(10) . ?
N12 C35 1.3900 . ?
N12 C34 1.3900 . ?
C35 C36 1.3900 . ?
C36 C37 1.3900 . ?
C37 C33 1.3900 . ?
C33 C34 1.3900 . ?
C34 C29 1.286(18) . ?
N13 C29 1.3900 . ?
N13 C28 1.3900 . ?
C29 C30 1.3900 . ?
C30 C51 1.3900 . ?
C30 C32 1.40(3) . ?
C51 C52 1.3900 . ?
C52 C28 1.3900 . ?

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
_geom_angle_publ_flag
O23 W2 O13 103.4(3) . . ?
O23 W2 O17 100.0(4) . . ?
O13 W2 O17 156.6(3) . . ?
O23 W2 O10 95.9(3) . . ?
O13 W2 O10 88.7(3) . . ?
O17 W2 O10 90.6(3) . . ?
O23 W2 O8 98.2(3) . . ?
O13 W2 O8 84.7(3) . . ?
O17 W2 O8 90.4(3) . . ?
O10 W2 O8 165.4(3) . . ?
O23 W2 O9 172.0(3) . . ?
O13 W2 O9 84.4(3) . . ?
O17 W2 O9 72.3(3) . . ?
O10 W2 O9 82.4(3) . . ?
O8 W2 O9 84.1(3) . . ?
O4 W4 O10 98.5(4) . . ?
O4 W4 O21 103.7(3) . . ?
O10 W4 O21 89.0(3) . . ?
O4 W4 O31 100.4(3) . . ?
O10 W4 O31 90.6(3) . . ?
O21 W4 O31 155.7(3) . . ?
O4 W4 O11 97.1(3) . . ?
O10 W4 O11 164.3(3) . . ?
O21 W4 O11 84.9(3) . . ?
O31 W4 O11 89.1(3) . . ?
O4 W4 O20 171.9(3) . . ?
O10 W4 O20 82.4(3) . . ?
O21 W4 O20 84.4(3) . . ?
O31 W4 O20 71.5(3) . . ?
O11 W4 O20 82.6(3) . . ?
O35 W10 O7 98.1(3) . . ?
O35 W10 O12 103.0(4) . . ?
O7 W10 O12 89.0(4) . . ?
O35 W10 O17 100.0(3) . . ?
O7 W10 O17 90.0(3) . . ?
O12 W10 O17 156.9(4) . . ?
O35 W10 O19 97.8(3) . . ?
O7 W10 O19 163.8(3) . . ?
O12 W10 O19 84.7(3) . . ?
O17 W10 O19 90.0(3) . . ?
O35 W10 O9 171.4(3) . . ?
O7 W10 O9 81.6(3) . . ?
O12 W10 O9 85.6(4) . . ?
O17 W10 O9 71.4(3) . . ?
O19 W10 O9 83.1(3) . . ?
O5 W9 O13 103.9(3) . . ?
O5 W9 O30 97.8(4) . . ?
O13 W9 O30 85.5(3) . . ?
O5 W9 O24 96.9(4) . . ?
O13 W9 O24 88.8(3) . . ?
O30 W9 O24 165.1(3) . . ?
O5 W9 O25 100.4(4) . . ?
O13 W9 O25 155.6(3) . . ?
O30 W9 O25 89.5(4) . . ?
O24 W9 O25 89.9(4) . . ?
O5 W9 O26 171.7(3) . . ?
O13 W9 O26 84.3(3) . . ?
O30 W9 O26 83.5(3) . . ?
O24 W9 O26 82.3(3) . . ?
O25 W9 O26 71.4(3) . . ?
O2 W8 O24 98.5(4) . . ?
O2 W8 O21 103.3(4) . . ?
O24 W8 O21 88.8(3) . . ?
O2 W8 O32 96.4(4) . . ?
O24 W8 O32 164.9(3) . . ?
O21 W8 O32 85.0(3) . . ?
O2 W8 O15 100.5(4) . . ?
O24 W8 O15 91.4(4) . . ?
O21 W8 O15 155.9(4) . . ?
O32 W8 O15 88.7(4) . . ?
O2 W8 O34 171.8(3) . . ?
O24 W8 O34 82.7(3) . . ?
O21 W8 O34 84.8(3) . . ?
O32 W8 O34 83.0(3) . . ?
O15 W8 O34 71.3(3) . . ?
O6 W7 O7 98.1(4) . . ?
O6 W7 O22 102.2(4) . . ?
O7 W7 O22 88.1(4) . . ?
O6 W7 O31 101.0(4) . . ?
O7 W7 O31 90.5(3) . . ?
O22 W7 O31 156.7(4) . . ?
O6 W7 O14 97.3(4) . . ?
O7 W7 O14 164.4(3) . . ?
O22 W7 O14 85.8(4) . . ?
O31 W7 O14 89.5(3) . . ?
O6 W7 O20 173.1(3) . . ?
O7 W7 O20 82.2(3) . . ?
O22 W7 O20 84.7(3) . . ?
O31 W7 O20 72.1(3) . . ?
O14 W7 O20 82.9(3) . . ?
O1 W6 O11 103.7(4) . . ?
O1 W6 O32 102.7(4) . . ?
O11 W6 O32 85.9(3) . . ?
O1 W6 O29 100.8(4) . . ?
O11 W6 O29 88.3(3) . . ?
O32 W6 O29 156.5(3) . . ?
O1 W6 O51 100.0(4) . . ?
O11 W6 O51 156.4(3) . . ?
O32 W6 O51 88.3(4) . . ?
O29 W6 O51 88.1(4) . . ?
O1 W6 O28 170.3(3) . . ?
O11 W6 O28 83.7(3) . . ?
O32 W6 O28 83.9(3) . . ?
O29 W6 O28 72.9(3) . . ?
O51 W6 O28 72.9(3) . . ?
O3 W5 O19 101.7(4) . . ?
O3 W5 O19 101.7(3) . 4_5/5 ?
O19 W5 O19 85.5(4) . 4_5/5 ?
O3 W5 O36 101.2(3) . 4_5/5 ?
O19 W5 O36 157.1(3) . 4_5/5 ?
O19 W5 O36 88.5(3) 4_5/5 4_5/5 ?
O3 W5 O36 101.2(3) . . ?
O19 W5 O36 88.5(3) . . ?
O19 W5 O36 157.1(3) 4_5/5 . ?
O36 W5 O36 88.6(4) 4_5/5 . ?
O3 W5 O18 171.5(4) . . ?
O19 W5 O18 84.5(3) . . ?
O19 W5 O18 84.5(3) 4_5/5 . ?
O36 W5 O18 72.9(3) 4_5/5 . ?
O36 W5 O18 72.9(3) . . ?
O26 As2 O9 111.4(3) . . ?
O26 As2 O9 111.4(3) . 4_5/5 ?
O9 As2 O9 112.4(4) . 4_5/5 ?
O26 As2 O18 108.0(5) . . ?
O9 As2 O18 106.7(3) . . ?
O9 As2 O18 106.7(3) 4_5/5 . ?
O33 W3 O8 103.1(4) . . ?
O33 W3 O30 103.3(4) . . ?
O8 W3 O30 86.0(3) . . ?
O33 W3 O16 101.0(4) . . ?
O8 W3 O16 155.9(3) . . ?
O30 W3 O16 87.8(4) . . ?
O33 W3 O36 100.7(4) . . ?
O8 W3 O36 88.1(3) . . ?
O30 W3 O36 156.0(3) . . ?
O16 W3 O36 88.2(4) . . ?
O33 W3 O18 169.5(3) . . ?
O8 W3 O18 84.3(3) . . ?
O30 W3 O18 84.5(3) . . ?
O16 W3 O18 72.0(3) . . ?
O36 W3 O18 71.8(3) . . ?
O20 As1 O20 111.2(5) 4_5/5 . ?
O20 As1 O34 112.4(3) 4_5/5 . ?
O20 As1 O34 112.4(3) . . ?
O20 As1 O28 106.8(3) 4_5/5 . ?
O20 As1 O28 106.8(3) . . ?
O34 As1 O28 106.9(5) . . ?
O27 W1 O14 103.2(4) . . ?
O27 W1 O14 103.2(4) . 4_5/5 ?
O14 W1 O14 84.9(4) . 4_5/5 ?
O27 W1 O29 100.9(4) . 4_5/5 ?
O14 W1 O29 155.9(3) . 4_5/5 ?
O14 W1 O29 88.7(3) 4_5/5 4_5/5 ?
O27 W1 O29 100.9(4) . . ?
O14 W1 O29 88.7(3) . . ?
O14 W1 O29 155.9(3) 4_5/5 . ?
O29 W1 O29 87.8(5) 4_5/5 . ?
O27 W1 O28 170.9(5) . . ?
O14 W1 O28 83.4(3) . . ?
O14 W1 O28 83.4(3) 4_5/5 . ?
O29 W1 O28 72.8(3) 4_5/5 . ?
O29 W1 O28 72.8(3) . . ?
W3 O36 W5 122.2(4) . . ?
As1 O34 W8 124.8(3) . . ?
As1 O34 W8 124.8(3) . 4_5/5 ?
W8 O34 W8 94.3(3) . 4_5/5 ?
W6 O32 W8 152.8(5) . . ?
W7 O31 W4 122.9(4) . . ?
W3 O30 W9 151.9(4) . . ?
As1 O28 W6 123.4(3) . . ?
As1 O28 W6 123.4(3) . 4_5/5 ?
W6 O28 W6 92.5(4) . 4_5/5 ?
As1 O28 W1 123.9(5) . . ?
W6 O28 W1 92.2(3) . . ?
W6 O28 W1 92.2(3) 4_5/5 . ?
W6 O29 W1 122.1(4) . . ?
As2 O26 W9 124.5(3) . . ?
As2 O26 W9 124.5(3) . 4_5/5 ?
W9 O26 W9 93.8(3) . 4_5/5 ?
W9 O25 W9 123.4(5) . 4_5/5 ?
W8 O24 W9 161.5(4) . . ?
W7 O22 W7 152.0(6) . 4_5/5 ?
W8 O21 W4 154.2(4) . . ?
As1 O20 W7 125.4(4) . . ?
As1 O20 W4 124.7(4) . . ?
W7 O20 W4 93.5(2) . . ?
W5 O19 W10 152.9(4) . . ?
As2 O18 W5 124.2(5) . . ?
As2 O18 W3 122.8(3) . . ?
W5 O18 W3 93.0(3) . . ?
As2 O18 W3 122.8(3) . 4_5/5 ?
W5 O18 W3 93.0(3) . 4_5/5 ?
W3 O18 W3 92.2(3) . 4_5/5 ?
W2 O17 W10 122.8(4) . . ?
W3 O16 W3 123.9(5) 4_5/5 . ?
W8 O15 W8 123.0(6) 4_5/5 . ?
W1 O14 W7 153.4(4) . . ?
W2 O13 W9 154.1(4) . . ?
W10 O12 W10 153.0(6) 4_5/5 . ?
W6 O11 W4 152.6(4) . . ?
W4 O10 W2 161.5(4) . . ?
As2 O9 W2 125.3(3) . . ?
As2 O9 W10 124.4(4) . . ?
W2 O9 W10 93.6(2) . . ?
W3 O8 W2 152.3(4) . . ?
W7 O7 W10 161.4(4) . . ?
O50 Cu1 O50 89.0(6) . 4_5/5 ?
O50 Cu1 N8 154.3(6) . . ?
O50 Cu1 N8 106.5(5) 4_5/5 . ?
O50 Cu1 N9 85.9(5) . . ?
O50 Cu1 N9 171.0(6) 4_5/5 . ?
N8 Cu1 N9 81.0(6) . . ?
O50 Cu1 O3 90.7(4) . . ?
O50 Cu1 O3 90.7(4) 4_5/5 . ?
N8 Cu1 O3 109.0(5) . . ?
N9 Cu1 O3 81.9(5) . . ?
O2W Cu2 N12 176.6(9) . . ?
O2W Cu2 N13 94.9(9) . . ?
N12 Cu2 N13 81.9(8) . . ?
O2W Cu2 O45 94.2(10) . . ?
N12 Cu2 O45 89.1(8) . . ?
N13 Cu2 O45 170.9(8) . . ?
O2W Cu2 O2 82.9(8) . . ?
N12 Cu2 O2 95.5(6) . . ?
N13 Cu2 O2 80.0(7) . . ?
O45 Cu2 O2 102.2(7) . . ?
O52 Cu4 O52 93.8(5) . 4_5/5 ?
O52 Cu4 N3 170.3(4) . 4_5/5 ?
O52 Cu4 N3 91.0(4) 4_5/5 4_5/5 ?
O52 Cu4 N3 91.0(4) . . ?
O52 Cu4 N3 170.3(4) 4_5/5 . ?
N3 Cu4 N3 83.2(6) 4_5/5 . ?
O52 Cu4 O1W 88.7(4) . . ?
O52 Cu4 O1W 88.7(4) 4_5/5 . ?
N3 Cu4 O1W 99.9(5) 4_5/5 . ?
N3 Cu4 O1W 99.9(5) . . ?
C13 O52 Cu4 129.8(8) . . ?
W5 O3 Cu1 155.2(6) . . ?
W8 O2 Cu2 147.6(5) . . ?
W6 O51 W6 121.7(5) . 4_5/5 ?
C13 O50 Cu1 128.0(9) . . ?
O52 C13 O50 128.3(12) . . ?
O52 C13 C12 116.6(10) . . ?
O50 C13 C12 115.1(11) . . ?
C1 N3 C5 122.2(13) . . ?
C1 N3 Cu4 128.1(12) . . ?
C5 N3 Cu4 109.7(8) . . ?
C8 C7 C12 121.2(12) . . ?
N1 C8 C7 120.3(13) . . ?
C8 N1 C10 121.4(12) . . ?
N1 C10 C11 121.5(12) . . ?
C10 C11 C12 118.5(12) . . ?
C7 C12 C11 117.0(11) . . ?
C7 C12 C13 122.7(10) . . ?
C11 C12 C13 120.2(11) . . ?
C39 C40 C41 110(3) . . ?
C41 N15 C42 124(4) . . ?
N15 C42 C43 126(4) . . ?
C39 C43 C42 117(3) . . ?
C43 C39 C40 127(4) . . ?
C43 C39 C38 124(3) . . ?
C40 C39 C38 109(3) . . ?
C5 C5 C4 122.4(9) 4_5/5 . ?
C5 C5 N3 118.7(7) 4_5/5 . ?
C4 C5 N3 118.9(12) . . ?
C6 C6 C4 120.3(8) 4_5/5 . ?
C5 C4 C3 119.4(15) . . ?
C5 C4 C6 117.3(14) . . ?
C3 C4 C6 123.1(14) . . ?
N3 C1 C2 120.5(19) . . ?
C4 C3 C2 117.2(19) . . ?
C3 C2 C1 119(2) . . ?
C15 C14 N8 120.0 . . ?
C16 C15 C14 120.0 . . ?
C15 C16 C17 120.0 . . ?
C19 C17 C16 124(2) . . ?
C19 C17 C18 116(2) . . ?
C16 C17 C18 120.0 . . ?
C24 C18 N8 118.1(11) . . ?
C24 C18 C17 121.9(11) . . ?
N8 C18 C17 120.0 . . ?
C18 N8 C14 120.0 . . ?
C18 N8 Cu1 113.3(8) . . ?
C14 N8 Cu1 126.6(8) . . ?
C20 C19 C17 122(3) . . ?
C19 C20 C21 123(3) . . ?
C18 C24 C21 124.9(12) . . ?
C18 C24 N9 114.5(12) . . ?
C21 C24 N9 120.0 . . ?
C24 C21 C25 120.0 . . ?
C24 C21 C20 112.0(18) . . ?
C25 C21 C20 127.7(18) . . ?
C26 C25 C21 120.0 . . ?
C25 C26 C27 120.0 . . ?
N9 C27 C26 120.0 . . ?
C27 N9 C24 120.0 . . ?
C27 N9 Cu1 127.5(9) . . ?
C24 N9 Cu1 112.5(9) . . ?
C38 O45 Cu2 123(2) . . ?
C33 C31 C32 126(4) . . ?
O45 C38 O46 125(3) . . ?
O45 C38 C39 117(3) . . ?
O46 C38 C39 116(3) . . ?
C35 N12 C34 120.0 . . ?
C35 N12 Cu2 127.7(10) . . ?
C34 N12 Cu2 112.1(10) . . ?
C36 C35 N12 120.0 . . ?
C35 C36 C37 120.0 . . ?
C33 C37 C36 120.0 . . ?
C31 C33 C37 124.4(19) . . ?
C31 C33 C34 115.6(19) . . ?
C37 C33 C34 120.0 . . ?
C29 C34 C33 122.3(16) . . ?
C29 C34 N12 117.7(16) . . ?
C33 C34 N12 120.0 . . ?
C29 N13 C28 120.0 . . ?
C29 N13 Cu2 110.5(11) . . ?
C28 N13 Cu2 129.3(11) . . ?
C34 C29 C30 122.2(16) . . ?
C34 C29 N13 117.7(16) . . ?
C30 C29 N13 120.0 . . ?
C29 C30 C51 120.0 . . ?
C29 C30 C32 114.1(18) . . ?
C51 C30 C32 125.6(19) . . ?
C52 C51 C30 120.0 . . ?
C51 C52 C28 120.0 . . ?
C52 C28 N13 120.0 . . ?
N15 C41 C40 116(3) . . ?
C31 C32 C30 119(4) . . ?

_refine_diff_density_max         2.081
_refine_diff_density_min         -2.358
_refine_diff_density_rms         0.316



