#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:49:44 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179308 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/05/4320557.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4320557
loop_
_publ_author_name
'Mi-Sook Seo'
'Vladimir P. Fedin'
'Maxim N. Sokolov'
'Rita Hernandez-Molina'
'Achim Sokolowski'
'Mark R. J. Elsegood'
'William Clegg'
'A. Geoffrey Sykes'
_publ_section_title
;
 Preparation, Structure, and Reactivity of Ge-Containing Heterometallic
 Cube Derivatives of [M3E4(H2O)9]4+ (M = Mo, W; E = S, Se)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6115
_journal_page_last               6122
_journal_paper_doi               10.1021/ic010256l
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C56 H82 Ge O65 S16 W6'
_chemical_formula_weight         3483.87
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.715(2)
_cell_angle_beta                 104.859(2)
_cell_angle_gamma                117.882(2)
_cell_formula_units_Z            1
_cell_length_a                   13.6001(13)
_cell_length_b                   13.9790(14)
_cell_length_c                   18.4290(18)
_cell_measurement_reflns_used    14150
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.69
_cell_volume                     2935.4(5)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_sigmaI/netI    0.1181
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19142
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.483
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_correction_T_min  0.081
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'brown/purple dichroic'
_exptl_crystal_density_diffrn    1.971
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1670
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.619
_refine_diff_density_min         -3.982
_refine_diff_density_rms         0.340
_refine_ls_extinction_coef       0.00183(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         10174
_refine_ls_number_restraints     413
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1078
_refine_ls_R_factor_gt           0.0816
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0962P)²+65.6362P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2025
_refine_ls_wR_factor_ref         0.2097
_reflns_number_gt                7264
_reflns_number_total             10174
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010256l_2.cif
_cod_data_source_block           ags31
_cod_database_code               4320557
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.29718(8) 0.05106(8) 0.53873(8) 0.0135(3) Uani 0.935(3) 1 d PU A 1
W2 W 0.27674(7) 0.15555(7) 0.65367(8) 0.0137(3) Uani 0.935(3) 1 d PU A 1
W3 W 0.27823(7) 0.23164(6) 0.52324(9) 0.0152(3) Uani 0.935(3) 1 d PU A 1
W1X W 0.2840(14) 0.0546(14) 0.5083(13) 0.0202(14) Uani 0.065(3) 1 d PU A 2
W2X W 0.2713(11) 0.1710(11) 0.6210(12) 0.0145(13) Uani 0.065(3) 1 d PU A 2
W3X W 0.2602(12) 0.2376(10) 0.4838(12) 0.0192(15) Uani 0.065(3) 1 d PU A 2
Ge1 Ge 0.0000 0.0000 0.5000 0.0193(6) Uani 1 2 d SU . .
S1 S 0.1491(4) -0.0299(3) 0.5955(3) 0.0176(8) Uani 1 1 d U . .
S2 S 0.1306(4) 0.1874(3) 0.5796(3) 0.0182(8) Uani 1 1 d U . .
S3 S 0.1548(4) 0.0607(3) 0.4397(3) 0.0184(7) Uani 1 1 d U . .
S4 S 0.4393(4) 0.2305(3) 0.6075(3) 0.0211(9) Uani 1 1 d U . .
O1 O 0.2255(12) -0.1168(10) 0.4799(8) 0.031(3) Uani 1 1 d . . .
O2 O 0.4057(11) 0.0700(10) 0.4657(9) 0.033(4) Uani 1 1 d . . .
O3 O 0.4111(10) -0.0009(9) 0.6038(8) 0.022(3) Uani 1 1 d . . .
O4 O 0.3669(10) 0.3127(10) 0.7286(8) 0.027(3) Uani 1 1 d . . .
O5 O 0.3834(10) 0.1222(10) 0.7444(7) 0.026(3) Uani 1 1 d . . .
O6 O 0.1825(12) 0.1226(11) 0.7374(7) 0.028(3) Uani 1 1 d . . .
O7 O 0.3654(11) 0.4054(10) 0.5712(8) 0.032(3) Uani 1 1 d . . .
O8 O 0.3849(12) 0.2972(12) 0.4503(10) 0.048(4) Uani 1 1 d . . .
O9 O 0.1797(12) 0.2878(11) 0.4417(9) 0.039(4) Uani 1 1 d . . .
S5 S 0.6782(4) 0.3781(4) 0.8117(3) 0.0326(12) Uani 1 1 d U B .
O10 O 0.7699(14) 0.4219(13) 0.7729(9) 0.043(3) Uani 1 1 d U . .
O11 O 0.5998(12) 0.4232(12) 0.7944(9) 0.041(3) Uani 1 1 d U . .
O12 O 0.6124(12) 0.2565(12) 0.7931(9) 0.042(3) Uani 1 1 d U . .
C1 C 0.7466(16) 0.4149(15) 0.9105(12) 0.025(3) Uani 1 1 d U . .
C2 C 0.700(4) 0.447(3) 0.961(3) 0.024(5) Uani 0.44(3) 1 d PU B 1
H2 H 0.6319 0.4540 0.9422 0.029 Uiso 0.44(3) 1 calc PR B 1
C3 C 0.756(4) 0.466(4) 1.037(3) 0.027(4) Uani 0.44(3) 1 d PU B 1
H3 H 0.7205 0.4819 1.0713 0.033 Uiso 0.44(3) 1 calc PR B 1
C4 C 0.8559(18) 0.4658(16) 1.0690(13) 0.033(4) Uani 1 1 d U . .
C5 C 0.905(4) 0.437(4) 1.018(3) 0.030(5) Uani 0.44(3) 1 d PU B 1
H5 H 0.9753 0.4336 1.0382 0.036 Uiso 0.44(3) 1 calc PR B 1
C6 C 0.853(4) 0.414(4) 0.942(3) 0.028(5) Uani 0.44(3) 1 d PU B 1
H6 H 0.8878 0.3970 0.9092 0.033 Uiso 0.44(3) 1 calc PR B 1
C7 C 0.913(2) 0.493(2) 1.1536(13) 0.044(5) Uani 1 1 d U B .
H7A H 0.9330 0.5686 1.1734 0.066 Uiso 1 1 calc R . .
H7B H 0.9852 0.4885 1.1652 0.066 Uiso 1 1 calc R . .
H7C H 0.8597 0.4414 1.1777 0.066 Uiso 1 1 calc R . .
C2X C 0.762(4) 0.506(3) 0.954(2) 0.039(11) Uani 0.56(3) 1 d P B 2
H2X H 0.7372 0.5530 0.9304 0.047 Uiso 0.56(3) 1 calc PR B 2
C3X C 0.813(3) 0.530(3) 1.031(3) 0.043(12) Uani 0.56(3) 1 d P B 2
H3X H 0.8206 0.5923 1.0601 0.051 Uiso 0.56(3) 1 calc PR B 2
C5X C 0.839(4) 0.374(4) 1.024(3) 0.051(14) Uani 0.56(3) 1 d P B 2
H5X H 0.8678 0.3288 1.0480 0.062 Uiso 0.56(3) 1 calc PR B 2
C6X C 0.783(4) 0.345(5) 0.948(4) 0.070(19) Uani 0.56(3) 1 d P B 2
H6X H 0.7674 0.2788 0.9198 0.083 Uiso 0.56(3) 1 calc PR B 2
S6 S 0.5853(5) 0.3736(5) 0.2637(3) 0.0381(14) Uani 1 1 d . C .
O13 O 0.7120(14) 0.4310(15) 0.2843(10) 0.059(5) Uani 1 1 d . . .
O14 O 0.5382(15) 0.4392(13) 0.2908(9) 0.048(4) Uani 1 1 d . . .
O15 O 0.5416(14) 0.2646(14) 0.2873(9) 0.044(4) Uani 1 1 d . . .
C8 C 0.5271(19) 0.3441(17) 0.1625(12) 0.033(4) Uani 1 1 d U . .
C9 C 0.464(2) 0.384(2) 0.1253(14) 0.045(4) Uani 1 1 d U C .
H9 H 0.4476 0.4310 0.1535 0.054 Uiso 1 1 calc R . .
C10 C 0.420(2) 0.361(2) 0.0469(14) 0.048(4) Uani 1 1 d U . .
H10 H 0.3664 0.3841 0.0225 0.057 Uiso 1 1 calc R C .
C11 C 0.451(2) 0.305(2) 0.0025(13) 0.041(4) Uani 1 1 d U C .
C12 C 0.494(4) 0.235(4) 0.043(3) 0.038(5) Uani 0.50(4) 1 d PU C 1
H12 H 0.4947 0.1765 0.0150 0.045 Uiso 0.50(4) 1 calc PR C 1
C13 C 0.534(4) 0.260(4) 0.124(3) 0.035(5) Uani 0.50(4) 1 d PU C 1
H13 H 0.5652 0.2194 0.1519 0.042 Uiso 0.50(4) 1 calc PR C 1
C14 C 0.406(2) 0.284(3) -0.0796(14) 0.060(6) Uani 1 1 d U . .
H14A H 0.3345 0.2116 -0.0979 0.089 Uiso 1 1 calc R C .
H14B H 0.4652 0.2834 -0.1011 0.089 Uiso 1 1 calc R . .
H14C H 0.3891 0.3413 -0.0959 0.089 Uiso 1 1 calc R . .
C12X C 0.549(4) 0.304(3) 0.044(2) 0.029(11) Uani 0.50(4) 1 d PU C 2
H12X H 0.5893 0.2842 0.0165 0.035 Uiso 0.50(4) 1 calc PR C 2
C13X C 0.589(4) 0.328(4) 0.117(3) 0.041(13) Uani 0.50(4) 1 d PU C 2
H13X H 0.6631 0.3348 0.1414 0.049 Uiso 0.50(4) 1 calc PR C 2
S7 S 1.0753(4) 0.8853(4) 0.2232(3) 0.0298(12) Uani 1 1 d . . .
O16 O 1.1242(13) 1.0010(12) 0.2449(9) 0.044(4) Uani 1 1 d . . .
O17 O 1.1591(12) 0.8468(13) 0.2425(9) 0.043(4) Uani 1 1 d . . .
O18 O 0.9763(11) 0.8232(12) 0.2545(8) 0.032(3) Uani 1 1 d . . .
C15 C 1.010(2) 0.848(2) 0.1233(13) 0.050(4) Uani 1 1 d U . .
C16 C 0.948(3) 0.892(3) 0.0862(14) 0.060(5) Uani 1 1 d U . .
H16 H 0.9405 0.9462 0.1134 0.072 Uiso 1 1 calc R . .
C17 C 0.896(3) 0.858(3) 0.0069(15) 0.067(5) Uani 1 1 d U . .
H17 H 0.8432 0.8823 -0.0173 0.081 Uiso 1 1 calc R . .
C18 C 0.914(3) 0.797(3) -0.0347(15) 0.064(5) Uani 1 1 d U . .
C19 C 0.970(3) 0.754(3) 0.0003(16) 0.076(5) Uani 1 1 d U . .
H19 H 0.9758 0.6994 -0.0285 0.092 Uiso 1 1 calc R . .
C20 C 1.026(3) 0.783(3) 0.0805(15) 0.071(5) Uani 1 1 d U . .
H20 H 1.0748 0.7547 0.1033 0.085 Uiso 1 1 calc R . .
C21 C 0.864(3) 0.772(2) -0.1244(14) 0.067(7) Uani 1 1 d U . .
H21A H 0.7783 0.7390 -0.1401 0.100 Uiso 1 1 calc R . .
H21B H 0.8839 0.7205 -0.1455 0.100 Uiso 1 1 calc R . .
H21C H 0.8976 0.8407 -0.1435 0.100 Uiso 1 1 calc R . .
S8 S 0.7971(5) 0.1136(5) 0.1815(4) 0.0414(15) Uani 1 1 d . D .
O19 O 0.8666(16) 0.0582(16) 0.2026(10) 0.055(5) Uani 1 1 d . . .
O20 O 0.6973(15) 0.0702(14) 0.2109(12) 0.061(6) Uani 1 1 d . . .
O21 O 0.8690(16) 0.2333(13) 0.2015(10) 0.060(5) Uani 1 1 d . . .
C22 C 0.7395(18) 0.0827(17) 0.0804(14) 0.037(4) Uani 1 1 d U . .
C23 C 0.727(4) -0.015(3) 0.038(3) 0.037(5) Uani 0.50(2) 1 d PU D 1
H23 H 0.7558 -0.0593 0.0630 0.044 Uiso 0.50(2) 1 calc PR D 1
C24 C 0.676(4) -0.038(4) -0.034(3) 0.038(5) Uani 0.50(2) 1 d PU D 1
H24 H 0.6561 -0.1077 -0.0608 0.045 Uiso 0.50(2) 1 calc PR D 1
C25 C 0.6476(18) 0.0322(18) -0.0769(15) 0.041(4) Uani 1 1 d U . .
C26 C 0.667(4) 0.124(4) -0.040(3) 0.044(6) Uani 0.50(2) 1 d PU D 1
H26 H 0.6481 0.1717 -0.0682 0.053 Uiso 0.50(2) 1 calc PR D 1
C27 C 0.714(4) 0.155(4) 0.037(3) 0.038(5) Uani 0.50(2) 1 d PU D 1
H27 H 0.7301 0.2243 0.0623 0.046 Uiso 0.50(2) 1 calc PR D 1
C28 C 0.607(2) 0.010(2) -0.1626(15) 0.051(5) Uani 1 1 d U D .
H28A H 0.6065 0.0748 -0.1804 0.077 Uiso 1 1 calc R . .
H28B H 0.5278 -0.0539 -0.1819 0.077 Uiso 1 1 calc R . .
H28C H 0.6605 -0.0051 -0.1814 0.077 Uiso 1 1 calc R . .
C23X C 0.794(3) 0.058(2) 0.0382(18) 0.004(7) Uani 0.50(2) 1 d PU D 2
H23X H 0.8638 0.0562 0.0624 0.005 Uiso 0.50(2) 1 calc PR D 2
C24X C 0.751(4) 0.035(3) -0.036(3) 0.047(14) Uani 0.50(2) 1 d P D 2
H24X H 0.7933 0.0201 -0.0644 0.056 Uiso 0.50(2) 1 calc PR D 2
C26X C 0.593(4) 0.058(3) -0.040(3) 0.036(12) Uani 0.50(2) 1 d P D 2
H26X H 0.5256 0.0625 -0.0670 0.043 Uiso 0.50(2) 1 calc PR D 2
C27X C 0.630(4) 0.081(3) 0.042(2) 0.029(11) Uani 0.50(2) 1 d P D 2
H27X H 0.5870 0.0951 0.0705 0.035 Uiso 0.50(2) 1 calc PR D 2
O1W O 0.6370(11) 0.1459(11) 0.6780(8) 0.033(3) Uani 1 1 d . . .
O2W O 1.0391(12) 0.7229(11) 0.3757(9) 0.038(4) Uani 1 1 d . . .
O3W O 0.7594(12) 0.6258(11) 0.2160(9) 0.039(4) Uani 1 1 d . . .
O4W O 0.6361(11) 0.1979(11) 0.5386(9) 0.035(4) Uani 1 1 d . . .
O5W O 0.3204(12) 0.8272(12) 0.6633(10) 0.045(4) Uani 1 1 d . . .
O6W O 0.8988(17) 0.8039(18) 0.7024(11) 0.068(6) Uani 1 1 d . . .
O7W O 0.8851(14) 0.4202(16) 0.6725(9) 0.065(6) Uani 1 1 d . . .
O8W O 1.005(2) 0.683(2) 0.5409(18) 0.033(7) Uani 0.50 1 d P . .
O9W O 0.616(2) 0.4560(17) 0.5215(13) 0.113(10) Uani 1 1 d . . .
O10W O 1.0873(19) 0.6173(17) 0.6760(16) 0.096(8) Uani 1 1 d . . .
O11W O 0.3532(17) 0.1287(19) 0.3302(12) 0.110(10) Uani 1 1 d . . .
O12W O 0.676(5) 0.546(5) 0.670(3) 0.113(17) Uani 0.50 1 d PU . .
O13W O 0.734(4) 0.409(4) 0.541(3) 0.14(2) Uani 0.50 1 d PU . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
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
O3 W1 O1 76.4(5) . . ?
O3 W1 O2 80.0(5) . . ?
O1 W1 O2 76.8(5) . . ?
O3 W1 S1 97.0(4) . . ?
O1 W1 S1 84.2(4) . . ?
O2 W1 S1 161.0(4) . . ?
O3 W1 S4 86.2(3) . . ?
O1 W1 S4 158.5(4) . . ?
O2 W1 S4 88.1(4) . . ?
S1 W1 S4 110.61(16) . . ?
O3 W1 S3 162.4(4) . . ?
O1 W1 S3 86.7(4) . . ?
O2 W1 S3 91.8(4) . . ?
S1 W1 S3 85.70(16) . . ?
S4 W1 S3 109.23(16) . . ?
O3 W1 W2 98.8(4) . . ?
O1 W1 W2 138.5(4) . . ?
O2 W1 W2 143.8(4) . . ?
S1 W1 W2 55.18(11) . . ?
S4 W1 W2 55.88(12) . . ?
S3 W1 W2 96.93(12) . . ?
O3 W1 W3 141.3(3) . . ?
O1 W1 W3 141.4(4) . . ?
O2 W1 W3 98.4(3) . . ?
S1 W1 W3 95.60(11) . . ?
S4 W1 W3 55.15(12) . . ?
S3 W1 W3 54.97(11) . . ?
W2 W1 W3 60.16(4) . . ?
O4 W2 O5 81.7(5) . . ?
O4 W2 O6 78.1(5) . . ?
O5 W2 O6 77.5(5) . . ?
O4 W2 S1 164.2(4) . . ?
O5 W2 S1 94.6(4) . . ?
O6 W2 S1 86.2(4) . . ?
O4 W2 S2 93.6(4) . . ?
O5 W2 S2 163.5(4) . . ?
O6 W2 S2 86.1(4) . . ?
S1 W2 S2 85.66(16) . . ?
O4 W2 S4 84.7(4) . . ?
O5 W2 S4 86.2(4) . . ?
O6 W2 S4 157.7(4) . . ?
S1 W2 S4 110.47(16) . . ?
S2 W2 S4 109.22(17) . . ?
O4 W2 W1 140.0(3) . . ?
O5 W2 W1 96.8(4) . . ?
O6 W2 W1 141.0(4) . . ?
S1 W2 W1 55.47(11) . . ?
S2 W2 W1 96.96(12) . . ?
S4 W2 W1 55.45(11) . . ?
O4 W2 W3 96.6(4) . . ?
O5 W2 W3 141.1(4) . . ?
O6 W2 W3 140.6(4) . . ?
S1 W2 W3 95.81(12) . . ?
S2 W2 W3 54.99(11) . . ?
S4 W2 W3 55.05(12) . . ?
W1 W2 W3 60.17(3) . . ?
O8 W3 O7 80.1(6) . . ?
O8 W3 O9 77.0(6) . . ?
O7 W3 O9 78.0(5) . . ?
O8 W3 S2 161.2(4) . . ?
O7 W3 S2 93.3(4) . . ?
O9 W3 S2 84.4(4) . . ?
O8 W3 S3 93.5(5) . . ?
O7 W3 S3 162.0(4) . . ?
O9 W3 S3 84.2(4) . . ?
S2 W3 S3 87.40(15) . . ?
O8 W3 S4 87.1(5) . . ?
O7 W3 S4 86.6(4) . . ?
O9 W3 S4 159.4(4) . . ?
S2 W3 S4 110.26(17) . . ?
S3 W3 S4 110.07(16) . . ?
O8 W3 W2 142.7(4) . . ?
O7 W3 W2 98.2(4) . . ?
O9 W3 W2 139.5(4) . . ?
S2 W3 W2 55.34(12) . . ?
S3 W3 W2 96.97(12) . . ?
S4 W3 W2 55.76(12) . . ?
O8 W3 W1 99.1(4) . . ?
O7 W3 W1 141.9(4) . . ?
O9 W3 W1 139.5(4) . . ?
S2 W3 W1 96.84(11) . . ?
S3 W3 W1 55.54(12) . . ?
S4 W3 W1 55.44(11) . . ?
W2 W3 W1 59.67(3) . . ?
S3 W1X O2 115.2(12) . . ?
S3 W1X O1 100.1(9) . . ?
O2 W1X O1 83.2(8) . . ?
S3 W1X S4 116.8(8) . . ?
O2 W1X S4 87.7(7) . . ?
O1 W1X S4 142.3(11) . . ?
S3 W1X S1 87.2(6) . . ?
O2 W1X S1 153.0(11) . . ?
O1 W1X S1 77.8(7) . . ?
S4 W1X S1 95.6(7) . . ?
S3 W1X W2X 88.6(7) . . ?
O2 W1X W2X 135.5(9) . . ?
O1 W1X W2X 131.5(9) . . ?
S4 W1X W2X 47.8(4) . . ?
S1 W1X W2X 54.8(4) . . ?
S3 W1X W3X 51.5(5) . . ?
O2 W1X W3X 104.6(8) . . ?
O1 W1X W3X 151.3(9) . . ?
S4 W1X W3X 66.3(6) . . ?
S1 W1X W3X 101.3(6) . . ?
W2X W1X W3X 60.2(5) . . ?
S2 W2X S4 137.8(11) . . ?
S2 W2X O4 97.9(6) . . ?
S4 W2X O4 85.7(6) . . ?
S2 W2X S1 91.0(5) . . ?
S4 W2X S1 115.2(6) . . ?
O4 W2X S1 135.9(10) . . ?
S2 W2X W1X 107.6(7) . . ?
S4 W2X W1X 63.6(5) . . ?
O4 W2X W1X 149.0(7) . . ?
S1 W2X W1X 62.2(5) . . ?
S2 W2X W3X 67.6(6) . . ?
S4 W2X W3X 72.9(7) . . ?
O4 W2X W3X 115.3(8) . . ?
S1 W2X W3X 108.0(7) . . ?
W1X W2X W3X 61.7(6) . . ?
O9 W3X O8 104.1(13) . . ?
O9 W3X S3 105.0(9) . . ?
O8 W3X S3 110.8(9) . . ?
O9 W3X O7 85.0(8) . . ?
O8 W3X O7 83.2(8) . . ?
S3 W3X O7 159.5(11) . . ?
O9 W3X S2 85.4(8) . . ?
O8 W3X S2 160.5(11) . . ?
S3 W3X S2 82.3(5) . . ?
O7 W3X S2 80.7(6) . . ?
O9 W3X W2X 127.4(10) . . ?
O8 W3X W2X 122.2(11) . . ?
S3 W3X W2X 82.2(7) . . ?
O7 W3X W2X 77.6(7) . . ?
S2 W3X W2X 43.1(4) . . ?
O9 W3X W1X 148.7(9) . . ?
O8 W3X W1X 92.3(8) . . ?
S3 W3X W1X 43.8(5) . . ?
O7 W3X W1X 123.9(8) . . ?
S2 W3X W1X 87.6(6) . . ?
W2X W3X W1X 58.1(5) . . ?
S3 Ge1 S3 179.999(1) 2_556 . ?
S3 Ge1 S2 82.02(14) 2_556 2_556 ?
S3 Ge1 S2 97.98(14) . 2_556 ?
S3 Ge1 S2 97.98(14) 2_556 . ?
S3 Ge1 S2 82.02(14) . . ?
S2 Ge1 S2 180.0 2_556 . ?
S3 Ge1 S1 100.23(14) 2_556 . ?
S3 Ge1 S1 79.77(14) . . ?
S2 Ge1 S1 101.02(14) 2_556 . ?
S2 Ge1 S1 78.98(14) . . ?
S3 Ge1 S1 79.77(14) 2_556 2_556 ?
S3 Ge1 S1 100.23(14) . 2_556 ?
S2 Ge1 S1 78.98(14) 2_556 2_556 ?
S2 Ge1 S1 101.02(14) . 2_556 ?
S1 Ge1 S1 179.999(1) . 2_556 ?
W2 S1 W1 69.35(11) . . ?
W2 S1 W2X 15.3(5) . . ?
W1 S1 W2X 60.5(4) . . ?
W2 S1 Ge1 96.51(16) . . ?
W1 S1 Ge1 95.91(16) . . ?
W2X S1 Ge1 85.1(4) . . ?
W2 S1 W1X 74.2(4) . . ?
W1 S1 W1X 10.7(4) . . ?
W2X S1 W1X 63.0(5) . . ?
Ge1 S1 W1X 85.9(5) . . ?
W2X S2 W3 55.3(6) . . ?
W2X S2 W2 14.4(5) . . ?
W3 S2 W2 69.67(12) . . ?
W2X S2 Ge1 97.2(4) . . ?
W3 S2 Ge1 94.91(16) . . ?
W2 S2 Ge1 97.86(16) . . ?
W2X S2 W3X 69.3(5) . . ?
W3 S2 W3X 14.5(4) . . ?
W2 S2 W3X 83.7(4) . . ?
Ge1 S2 W3X 89.6(3) . . ?
W1X S3 W3X 84.7(7) . . ?
W1X S3 W3 71.6(5) . . ?
W3X S3 W3 18.1(6) . . ?
W1X S3 W1 9.4(6) . . ?
W3X S3 W1 84.5(6) . . ?
W3 S3 W1 69.49(13) . . ?
W1X S3 Ge1 106.9(6) . . ?
W3X S3 Ge1 103.9(4) . . ?
W3 S3 Ge1 95.44(16) . . ?
W1 S3 Ge1 97.83(17) . . ?
W2X S4 W3 53.8(6) . . ?
W2X S4 W1 65.0(4) . . ?
W3 S4 W1 69.41(13) . . ?
W2X S4 W2 15.4(5) . . ?
W3 S4 W2 69.19(12) . . ?
W1 S4 W2 68.68(11) . . ?
W2X S4 W1X 68.6(5) . . ?
W3 S4 W1X 61.5(5) . . ?
W1 S4 W1X 12.0(5) . . ?
W2 S4 W1X 75.2(4) . . ?
W1X O1 W1 14.8(6) . . ?
W1X O2 W1 14.0(6) . . ?
W2 O4 W2X 15.9(5) . . ?
W3 O7 W3X 18.1(5) . . ?
W3X O8 W3 18.6(7) . . ?
W3X O9 W3 14.4(7) . . ?
O11 S5 O12 111.2(9) . . ?
O11 S5 O10 112.8(10) . . ?
O12 S5 O10 110.4(9) . . ?
O11 S5 C1 107.0(9) . . ?
O12 S5 C1 106.3(9) . . ?
O10 S5 C1 108.8(9) . . ?
C2X C1 C2 38(2) . . ?
C2X C1 C6X 118(4) . . ?
C2 C1 C6X 104(3) . . ?
C2X C1 C6 103(3) . . ?
C2 C1 C6 118(3) . . ?
C6X C1 C6 42(2) . . ?
C2X C1 S5 123(2) . . ?
C2 C1 S5 122(2) . . ?
C6X C1 S5 119(3) . . ?
C6 C1 S5 120(2) . . ?
C3 C2 C1 117(4) . . ?
C4 C3 C2 126(4) . . ?
C3 C4 C5X 102(3) . . ?
C3 C4 C3X 39(2) . . ?
C5X C4 C3X 117(3) . . ?
C3 C4 C5 117(3) . . ?
C5X C4 C5 40(2) . . ?
C3X C4 C5 104(3) . . ?
C3 C4 C7 122(3) . . ?
C5X C4 C7 122(3) . . ?
C3X C4 C7 122(3) . . ?
C5 C4 C7 121(3) . . ?
C6 C5 C4 120(4) . . ?
C5 C6 C1 122(4) . . ?
C3X C2X C1 121(4) . . ?
C2X C3X C4 122(4) . . ?
C6X C5X C4 122(4) . . ?
C5X C6X C1 120(5) . . ?
O13 S6 O14 114.1(11) . . ?
O13 S6 O15 110.4(10) . . ?
O14 S6 O15 112.4(9) . . ?
O13 S6 C8 108.0(10) . . ?
O14 S6 C8 105.7(10) . . ?
O15 S6 C8 105.7(10) . . ?
C9 C8 C13 120(3) . . ?
C9 C8 C13X 109(3) . . ?
C13 C8 C13X 39(2) . . ?
C9 C8 S6 122.6(18) . . ?
C13 C8 S6 116(2) . . ?
C13X C8 S6 121(3) . . ?
C8 C9 C10 122(2) . . ?
C9 C10 C11 122(2) . . ?
C12X C11 C10 111(3) . . ?
C12X C11 C14 125(3) . . ?
C10 C11 C14 121(2) . . ?
C12X C11 C12 36(2) . . ?
C10 C11 C12 114(3) . . ?
C14 C11 C12 121(3) . . ?
C13 C12 C11 117(4) . . ?
C8 C13 C12 119(4) . . ?
C13X C12X C11 124(4) . . ?
C12X C13X C8 122(4) . . ?
O16 S7 O17 114.7(10) . . ?
O16 S7 O18 111.2(9) . . ?
O17 S7 O18 110.3(9) . . ?
O16 S7 C15 108.5(11) . . ?
O17 S7 C15 107.0(10) . . ?
O18 S7 C15 104.6(11) . . ?
C20 C15 C16 116(2) . . ?
C20 C15 S7 123(2) . . ?
C16 C15 S7 121.0(19) . . ?
C15 C16 C17 119(2) . . ?
C18 C17 C16 124(3) . . ?
C19 C18 C17 116(3) . . ?
C19 C18 C21 122(3) . . ?
C17 C18 C21 122(3) . . ?
C18 C19 C20 123(3) . . ?
C15 C20 C19 121(3) . . ?
O21 S8 O20 113.3(11) . . ?
O21 S8 O19 112.5(12) . . ?
O20 S8 O19 111.6(10) . . ?
O21 S8 C22 104.9(10) . . ?
O20 S8 C22 107.1(11) . . ?
O19 S8 C22 106.8(10) . . ?
C23X C22 C27 99(3) . . ?
C23X C22 C23 41.5(19) . . ?
C27 C22 C23 118(3) . . ?
C23X C22 C27X 120(3) . . ?
C27 C22 C27X 47(2) . . ?
C23 C22 C27X 104(3) . . ?
C23X C22 S8 120(2) . . ?
C27 C22 S8 123(2) . . ?
C23 C22 S8 119(2) . . ?
C27X C22 S8 120(2) . . ?
C24 C23 C22 117(4) . . ?
C23 C24 C25 125(4) . . ?
C26X C25 C26 46(3) . . ?
C26X C25 C24X 119(4) . . ?
C26 C25 C24X 98(3) . . ?
C26X C25 C24 103(3) . . ?
C26 C25 C24 118(4) . . ?
C24X C25 C24 44(2) . . ?
C26X C25 C28 120(3) . . ?
C26 C25 C28 119(3) . . ?
C24X C25 C28 121(3) . . ?
C24 C25 C28 123(3) . . ?
C25 C26 C27 123(4) . . ?
C26 C27 C22 119(4) . . ?
C24X C23X C22 120(3) . . ?
C23X C24X C25 124(4) . . ?
C25 C26X C27X 121(4) . . ?
C26X C27X C22 116(3) . . ?
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 O3 2.133(12) . ?
W1 O1 2.170(12) . ?
W1 O2 2.179(13) . ?
W1 S1 2.344(4) . ?
W1 S4 2.354(4) . ?
W1 S3 2.356(5) . ?
W1 W2 2.6622(12) . ?
W1 W3 2.6757(12) . ?
W2 O4 2.135(12) . ?
W2 O5 2.140(12) . ?
W2 O6 2.183(12) . ?
W2 S1 2.336(4) . ?
W2 S2 2.347(5) . ?
W2 S4 2.366(4) . ?
W2 W3 2.6753(13) . ?
W3 O8 2.150(15) . ?
W3 O7 2.157(12) . ?
W3 O9 2.176(13) . ?
W3 S2 2.337(4) . ?
W3 S3 2.339(5) . ?
W3 S4 2.346(5) . ?
W1X S3 1.92(2) . ?
W1X O2 1.94(2) . ?
W1X O1 2.13(2) . ?
W1X S4 2.566(18) . ?
W1X S1 2.647(19) . ?
W1X W2X 2.67(2) . ?
W1X W3X 2.77(2) . ?
W2X S2 1.994(16) . ?
W2X S4 2.124(14) . ?
W2X O4 2.333(19) . ?
W2X S1 2.445(14) . ?
W2X W3X 2.73(2) . ?
W3X O9 1.62(2) . ?
W3X O8 1.792(19) . ?
W3X S3 2.174(13) . ?
W3X O7 2.338(18) . ?
W3X S2 2.697(17) . ?
Ge1 S3 2.451(4) 2_556 ?
Ge1 S3 2.451(4) . ?
Ge1 S2 2.473(4) 2_556 ?
Ge1 S2 2.473(4) . ?
Ge1 S1 2.532(5) . ?
Ge1 S1 2.532(5) 2_556 ?
S5 O11 1.452(15) . ?
S5 O12 1.474(15) . ?
S5 O10 1.492(16) . ?
S5 C1 1.74(2) . ?
C1 C2X 1.37(5) . ?
C1 C2 1.41(5) . ?
C1 C6X 1.41(5) . ?
C1 C6 1.42(5) . ?
C2 C3 1.36(6) . ?
C3 C4 1.34(5) . ?
C4 C5X 1.38(5) . ?
C4 C3X 1.40(5) . ?
C4 C5 1.42(5) . ?
C4 C7 1.49(3) . ?
C5 C6 1.34(7) . ?
C2X C3X 1.35(6) . ?
C5X C6X 1.35(7) . ?
S6 O13 1.449(17) . ?
S6 O14 1.473(17) . ?
S6 O15 1.488(16) . ?
S6 C8 1.77(2) . ?
C8 C9 1.31(3) . ?
C8 C13 1.40(5) . ?
C8 C13X 1.41(5) . ?
C9 C10 1.37(3) . ?
C10 C11 1.37(3) . ?
C11 C12X 1.36(5) . ?
C11 C14 1.44(3) . ?
C11 C12 1.49(5) . ?
C12 C13 1.42(6) . ?
C12X C13X 1.28(6) . ?
S7 O16 1.418(16) . ?
S7 O17 1.449(15) . ?
S7 O18 1.499(13) . ?
S7 C15 1.76(2) . ?
C15 C20 1.29(3) . ?
C15 C16 1.34(3) . ?
C16 C17 1.40(3) . ?
C17 C18 1.26(4) . ?
C18 C19 1.26(4) . ?
C18 C21 1.57(3) . ?
C19 C20 1.42(4) . ?
S8 O21 1.456(17) . ?
S8 O20 1.464(16) . ?
S8 O19 1.471(17) . ?
S8 C22 1.77(3) . ?
C22 C23X 1.34(4) . ?
C22 C27 1.43(5) . ?
C22 C23 1.46(5) . ?
C22 C27X 1.46(4) . ?
C23 C24 1.27(6) . ?
C24 C25 1.42(5) . ?
C25 C26X 1.29(5) . ?
C25 C26 1.30(5) . ?
C25 C24X 1.40(5) . ?
C25 C28 1.50(3) . ?
C26 C27 1.35(7) . ?
C23X C24X 1.30(6) . ?
C26X C27X 1.43(6) . ?
