#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:49:44 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179308 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/05/4320558.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_4320558
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 H108 Ge Mo6 O50 S8 Se8'
_chemical_formula_weight         3117.81
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   'geom except H2O-H coords freely refined'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.437(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.3558(5)
_cell_length_b                   34.0069(13)
_cell_length_c                   11.9249(5)
_cell_measurement_reflns_used    11925
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      2.48
_cell_volume                     5006.1(3)
_computing_cell_refinement       'Siemens SMART'
_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 0.997
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'Bruker SMART CCD difractometer'
_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  0.0530
_diffrn_reflns_av_sigmaI/netI    0.1097
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            32370
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.189
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.348
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3056
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.145
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       0.00025(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.873
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         11466
_refine_ls_number_restraints     403
_refine_ls_restrained_S_all      0.863
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0269P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0762
_reflns_number_gt                6992
_reflns_number_total             11466
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010256l_3.cif
_cod_data_source_block           ags35
_cod_database_code               4320558
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Mo1 Mo 0.27616(3) 0.486466(13) 0.61923(4) 0.01426(11) Uani 1 1 d . . .
Mo2 Mo 0.17689(3) 0.545942(13) 0.72961(4) 0.01384(11) Uani 1 1 d . . .
Mo3 Mo 0.12663(3) 0.469673(13) 0.77608(4) 0.01443(11) Uani 1 1 d . . .
Ge1 Ge 0.0000 0.5000 0.5000 0.01832(19) Uani 1 2 d S . .
Se1 Se 0.30535(4) 0.499159(16) 0.82114(4) 0.01620(13) Uani 1 1 d . . .
Se2 Se 0.17690(4) 0.540085(15) 0.52408(4) 0.01564(13) Uani 1 1 d . . .
Se3 Se 0.11754(4) 0.443913(15) 0.58331(4) 0.01659(13) Uani 1 1 d . . .
Se4 Se -0.00817(4) 0.519015(16) 0.71491(5) 0.01803(13) Uani 1 1 d . . .
O1 O 0.3195(3) 0.47072(11) 0.4478(3) 0.0224(9) Uani 1 1 d D . .
H1A H 0.292(4) 0.4844(11) 0.406(4) 0.034 Uiso 1 1 d D . .
H1B H 0.299(4) 0.4501(6) 0.437(5) 0.034 Uiso 1 1 d D . .
O2 O 0.4324(3) 0.51393(10) 0.6013(3) 0.0210(9) Uani 1 1 d D . .
H2A H 0.448(4) 0.5282(12) 0.647(3) 0.031 Uiso 1 1 d D . .
H2B H 0.425(4) 0.5247(13) 0.547(2) 0.031 Uiso 1 1 d D . .
O3 O 0.3792(3) 0.43632(11) 0.6454(4) 0.0245(9) Uani 1 1 d D . .
H3A H 0.360(4) 0.4162(8) 0.658(5) 0.037 Uiso 1 1 d D . .
H3B H 0.4370(19) 0.4367(14) 0.631(5) 0.037 Uiso 1 1 d D . .
O4 O 0.3139(3) 0.58602(11) 0.7363(3) 0.0220(9) Uani 1 1 d D . .
H4A H 0.326(4) 0.6028(11) 0.777(4) 0.033 Uiso 1 1 d D . .
H4B H 0.366(3) 0.5744(13) 0.735(5) 0.033 Uiso 1 1 d D . .
O5 O 0.1625(3) 0.56937(12) 0.8959(3) 0.0205(9) Uani 1 1 d D . .
H5A H 0.184(4) 0.5564(14) 0.943(3) 0.031 Uiso 1 1 d D . .
H5B H 0.108(2) 0.5773(15) 0.910(4) 0.031 Uiso 1 1 d D . .
O6 O 0.0974(3) 0.60328(12) 0.6995(3) 0.0224(9) Uani 1 1 d D . .
H6A H 0.044(3) 0.5926(15) 0.688(4) 0.034 Uiso 1 1 d D . .
H6B H 0.111(4) 0.6137(15) 0.646(3) 0.034 Uiso 1 1 d D . .
O7 O 0.0962(3) 0.47614(11) 0.9518(3) 0.0211(9) Uani 1 1 d D . .
H7A H 0.128(4) 0.4901(13) 0.988(4) 0.032 Uiso 1 1 d D . .
H7B H 0.068(4) 0.4613(12) 0.986(4) 0.032 Uiso 1 1 d D . .
O8 O 0.1961(3) 0.41446(11) 0.8423(3) 0.0204(9) Uani 1 1 d D . .
H8A H 0.216(4) 0.4102(15) 0.9026(17) 0.031 Uiso 1 1 d D . .
H8B H 0.229(4) 0.4015(14) 0.805(3) 0.031 Uiso 1 1 d D . .
O9 O -0.0166(3) 0.43409(12) 0.8042(3) 0.0223(9) Uani 1 1 d D . .
H9A H -0.032(4) 0.4169(11) 0.768(4) 0.033 Uiso 1 1 d D . .
H9B H -0.063(3) 0.4473(12) 0.815(5) 0.033 Uiso 1 1 d D . .
S1 S 0.30368(10) 0.52306(4) 0.15292(11) 0.0150(3) Uani 1 1 d . . .
O10 O 0.2901(3) 0.52291(10) 0.2734(3) 0.0207(9) Uani 1 1 d . . .
O11 O 0.1963(3) 0.52927(10) 0.0943(3) 0.0173(8) Uani 1 1 d . . .
O12 O 0.3586(3) 0.48917(10) 0.1105(3) 0.0236(9) Uani 1 1 d . . .
C1 C 0.3815(4) 0.56479(15) 0.1236(4) 0.0163(12) Uani 1 1 d . . .
C2 C 0.3593(4) 0.60002(16) 0.1760(5) 0.0232(13) Uani 1 1 d . . .
H2 H 0.3021 0.6017 0.2266 0.028 Uiso 1 1 calc R . .
C3 C 0.4211(4) 0.63268(16) 0.1540(5) 0.0268(14) Uani 1 1 d . . .
H3 H 0.4076 0.6567 0.1918 0.032 Uiso 1 1 calc R . .
C4 C 0.5029(4) 0.63103(17) 0.0775(5) 0.0242(14) Uani 1 1 d . . .
C5 C 0.5237(4) 0.59539(18) 0.0265(5) 0.0271(14) Uani 1 1 d . . .
H5 H 0.5804 0.5937 -0.0246 0.032 Uiso 1 1 calc R . .
C6 C 0.4635(4) 0.56239(17) 0.0487(4) 0.0220(13) Uani 1 1 d . . .
H6 H 0.4784 0.5382 0.0128 0.026 Uiso 1 1 calc R . .
C7 C 0.5680(5) 0.66735(17) 0.0516(5) 0.0395(17) Uani 1 1 d . . .
H7C H 0.6443 0.6629 0.0738 0.059 Uiso 1 1 calc R . .
H7D H 0.5404 0.6898 0.0932 0.059 Uiso 1 1 calc R . .
H7E H 0.5614 0.6728 -0.0291 0.059 Uiso 1 1 calc R . .
S2 S 0.11741(10) 0.38430(4) 0.10679(11) 0.0188(3) Uani 1 1 d . . .
O13 O 0.1112(3) 0.38154(10) 0.2287(3) 0.0216(9) Uani 1 1 d . . .
O14 O 0.2249(3) 0.39545(10) 0.0711(3) 0.0246(9) Uani 1 1 d . . .
O15 O 0.0342(3) 0.41126(10) 0.0586(3) 0.0210(9) Uani 1 1 d . . .
C8 C 0.0850(4) 0.33748(15) 0.0506(4) 0.0180(12) Uani 1 1 d . . .
C9 C 0.0321(4) 0.33405(18) -0.0530(5) 0.0284(14) Uani 1 1 d . . .
H9 H 0.0097 0.3570 -0.0928 0.034 Uiso 1 1 calc R . .
C10 C 0.0117(4) 0.29801(18) -0.0986(5) 0.0286(15) Uani 1 1 d . . .
H10 H -0.0235 0.2963 -0.1709 0.034 Uiso 1 1 calc R . .
C11 C 0.0410(4) 0.26401(18) -0.0423(5) 0.0264(14) Uani 1 1 d . . .
C12 C 0.0932(5) 0.26786(18) 0.0622(5) 0.0377(17) Uani 1 1 d . . .
H12 H 0.1140 0.2449 0.1029 0.045 Uiso 1 1 calc R . .
C13 C 0.1156(4) 0.30421(17) 0.1087(5) 0.0294(15) Uani 1 1 d . . .
H13 H 0.1519 0.3062 0.1803 0.035 Uiso 1 1 calc R . .
C14 C 0.0203(5) 0.22381(18) -0.0900(5) 0.0403(17) Uani 1 1 d . . .
H14A H -0.0484 0.2137 -0.0636 0.060 Uiso 1 1 calc R . .
H14B H 0.0793 0.2061 -0.0654 0.060 Uiso 1 1 calc R . .
H14C H 0.0165 0.2253 -0.1722 0.060 Uiso 1 1 calc R . .
S3 S 0.26512(11) 0.84582(4) 1.00952(13) 0.0228(3) Uani 1 1 d . . .
O16 O 0.3246(4) 0.86427(12) 0.9247(4) 0.0534(14) Uani 1 1 d . . .
O17 O 0.3157(3) 0.84942(11) 1.1209(4) 0.0456(12) Uani 1 1 d . . .
O18 O 0.1527(3) 0.85943(11) 1.0112(3) 0.0309(10) Uani 1 1 d . . .
C15 C 0.2603(4) 0.79502(16) 0.9785(5) 0.0201(13) Uani 1 1 d . . .
C16 C 0.2163(5) 0.78304(18) 0.8758(5) 0.0334(15) Uani 1 1 d . . .
H16 H 0.1925 0.8018 0.8212 0.040 Uiso 1 1 calc R . .
C17 C 0.2074(5) 0.74326(18) 0.8539(5) 0.0341(16) Uani 1 1 d . . .
H17 H 0.1768 0.7350 0.7833 0.041 Uiso 1 1 calc R . .
C18 C 0.2415(4) 0.71519(17) 0.9307(5) 0.0296(15) Uani 1 1 d . . .
C19 C 0.2858(5) 0.72859(17) 1.0304(5) 0.0330(15) Uani 1 1 d . . .
H19 H 0.3115 0.7100 1.0848 0.040 Uiso 1 1 calc R . .
C20 C 0.2947(5) 0.76741(16) 1.0546(5) 0.0304(15) Uani 1 1 d . . .
H20 H 0.3252 0.7754 1.1254 0.036 Uiso 1 1 calc R . .
C21 C 0.2309(5) 0.67172(17) 0.9056(6) 0.049(2) Uani 1 1 d . . .
H21A H 0.3031 0.6604 0.8978 0.074 Uiso 1 1 calc R . .
H21B H 0.1876 0.6680 0.8357 0.074 Uiso 1 1 calc R . .
H21C H 0.1952 0.6586 0.9673 0.074 Uiso 1 1 calc R . .
S4 S 0.26071(12) 0.33740(4) 0.63368(13) 0.0265(4) Uani 1 1 d . . .
O19 O 0.2943(4) 0.34327(12) 0.5218(3) 0.0457(12) Uani 1 1 d . . .
O20 O 0.1460(3) 0.33184(12) 0.6447(4) 0.0452(13) Uani 1 1 d . . .
O21 O 0.3014(3) 0.36865(10) 0.7083(3) 0.0256(9) Uani 1 1 d . . .
C22 C 0.3241(4) 0.29366(15) 0.6808(4) 0.0187(12) Uani 1 1 d . . .
C23 C 0.4179(5) 0.28077(16) 0.6348(5) 0.0277(14) Uani 1 1 d . . .
H23 H 0.4504 0.2959 0.5784 0.033 Uiso 1 1 calc R . .
C24 C 0.4646(5) 0.24610(17) 0.6700(5) 0.0292(15) Uani 1 1 d . . .
H24 H 0.5306 0.2377 0.6397 0.035 Uiso 1 1 calc R . .
C25 C 0.4157(4) 0.22316(16) 0.7499(5) 0.0255(14) Uani 1 1 d . . .
C26 C 0.3246(4) 0.23719(16) 0.7989(5) 0.0247(14) Uani 1 1 d . . .
H26 H 0.2935 0.2227 0.8574 0.030 Uiso 1 1 calc R . .
C27 C 0.2790(4) 0.27170(16) 0.7643(5) 0.0225(13) Uani 1 1 d . . .
H27 H 0.2153 0.2808 0.7979 0.027 Uiso 1 1 calc R . .
C28 C 0.4612(5) 0.18337(17) 0.7807(6) 0.0425(18) Uani 1 1 d . . .
H28A H 0.4598 0.1797 0.8622 0.064 Uiso 1 1 calc R . .
H28B H 0.5361 0.1816 0.7571 0.064 Uiso 1 1 calc R . .
H28C H 0.4174 0.1629 0.7429 0.064 Uiso 1 1 calc R . .
O1W O 0.9567(3) 0.13077(13) 0.1953(3) 0.0308(10) Uani 1 1 d D . .
H1WA H 0.923(3) 0.1294(18) 0.142(3) 0.046 Uiso 1 1 d D . .
H1WB H 1.013(2) 0.1377(18) 0.180(4) 0.046 Uiso 1 1 d D . .
O2W O 0.2992(3) 0.09972(11) 0.8616(3) 0.0239(9) Uani 1 1 d D . .
H2WB H 0.251(3) 0.1023(16) 0.822(4) 0.036 Uiso 1 1 d D . .
H2WA H 0.298(4) 0.1150(13) 0.906(3) 0.036 Uiso 1 1 d D . .
O3W O 0.5286(3) 0.93632(12) 0.2511(3) 0.0220(9) Uani 1 1 d D . .
H3WA H 0.548(4) 0.9495(14) 0.296(4) 0.033 Uiso 1 1 d D . .
H3WB H 0.571(3) 0.9251(14) 0.225(4) 0.033 Uiso 1 1 d D . .
O4W O 0.4231(3) 0.93573(11) 0.9270(3) 0.0221(9) Uani 1 1 d D . .
H4WB H 0.409(4) 0.9144(5) 0.923(5) 0.033 Uiso 1 1 d D . .
H4WA H 0.390(4) 0.9480(12) 0.889(4) 0.033 Uiso 1 1 d D . .
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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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 Mo1 O2 80.28(14) . . ?
O3 Mo1 O1 77.01(15) . . ?
O2 Mo1 O1 76.11(14) . . ?
O3 Mo1 Se2 160.50(11) . . ?
O2 Mo1 Se2 93.67(10) . . ?
O1 Mo1 Se2 83.55(10) . . ?
O3 Mo1 Se1 86.31(12) . . ?
O2 Mo1 Se1 85.80(10) . . ?
O1 Mo1 Se1 157.11(10) . . ?
Se2 Mo1 Se1 111.89(2) . . ?
O3 Mo1 Se3 91.20(11) . . ?
O2 Mo1 Se3 160.87(10) . . ?
O1 Mo1 Se3 85.32(10) . . ?
Se2 Mo1 Se3 88.72(2) . . ?
Se1 Mo1 Se3 110.90(2) . . ?
O3 Mo1 Mo2 142.66(12) . . ?
O2 Mo1 Mo2 98.56(10) . . ?
O1 Mo1 Mo2 139.41(10) . . ?
Se2 Mo1 Mo2 56.346(18) . . ?
Se1 Mo1 Mo2 56.509(18) . . ?
Se3 Mo1 Mo2 98.55(2) . . ?
O3 Mo1 Mo3 98.51(10) . . ?
O2 Mo1 Mo3 141.88(10) . . ?
O1 Mo1 Mo3 141.22(10) . . ?
Se2 Mo1 Mo3 97.60(2) . . ?
Se1 Mo1 Mo3 56.211(18) . . ?
Se3 Mo1 Mo3 56.055(18) . . ?
Mo2 Mo1 Mo3 59.782(16) . . ?
O5 Mo2 O4 80.15(15) . . ?
O5 Mo2 O6 76.65(14) . . ?
O4 Mo2 O6 78.00(14) . . ?
O5 Mo2 Se2 162.21(10) . . ?
O4 Mo2 Se2 93.11(11) . . ?
O6 Mo2 Se2 85.89(10) . . ?
O5 Mo2 Se4 95.18(10) . . ?
O4 Mo2 Se4 162.91(10) . . ?
O6 Mo2 Se4 84.93(10) . . ?
Se2 Mo2 Se4 86.46(2) . . ?
O5 Mo2 Se1 84.71(10) . . ?
O4 Mo2 Se1 84.42(10) . . ?
O6 Mo2 Se1 156.21(10) . . ?
Se2 Mo2 Se1 111.18(2) . . ?
Se4 Mo2 Se1 111.68(2) . . ?
O5 Mo2 Mo3 97.83(10) . . ?
O4 Mo2 Mo3 140.58(10) . . ?
O6 Mo2 Mo3 140.32(10) . . ?
Se2 Mo2 Mo3 97.76(2) . . ?
Se4 Mo2 Mo3 56.112(18) . . ?
Se1 Mo2 Mo3 56.316(18) . . ?
O5 Mo2 Mo1 140.76(10) . . ?
O4 Mo2 Mo1 96.72(10) . . ?
O6 Mo2 Mo1 141.43(10) . . ?
Se2 Mo2 Mo1 56.001(18) . . ?
Se4 Mo2 Mo1 97.18(2) . . ?
Se1 Mo2 Mo1 56.123(18) . . ?
Mo3 Mo2 Mo1 60.332(16) . . ?
O7 Mo3 O9 74.41(14) . . ?
O7 Mo3 O8 79.61(14) . . ?
O9 Mo3 O8 77.18(15) . . ?
O7 Mo3 Se4 94.30(11) . . ?
O9 Mo3 Se4 83.11(10) . . ?
O8 Mo3 Se4 160.27(10) . . ?
O7 Mo3 Se3 160.46(10) . . ?
O9 Mo3 Se3 86.61(11) . . ?
O8 Mo3 Se3 91.90(10) . . ?
Se4 Mo3 Se3 87.84(2) . . ?
O7 Mo3 Se1 86.46(10) . . ?
O9 Mo3 Se1 156.60(11) . . ?
O8 Mo3 Se1 86.35(11) . . ?
Se4 Mo3 Se1 112.17(2) . . ?
Se3 Mo3 Se1 110.73(2) . . ?
O7 Mo3 Mo2 98.68(10) . . ?
O9 Mo3 Mo2 138.71(10) . . ?
O8 Mo3 Mo2 142.76(11) . . ?
Se4 Mo3 Mo2 56.436(18) . . ?
Se3 Mo3 Mo2 98.66(2) . . ?
Se1 Mo3 Mo2 56.490(18) . . ?
O7 Mo3 Mo1 142.32(10) . . ?
O9 Mo3 Mo1 142.57(11) . . ?
O8 Mo3 Mo1 99.12(10) . . ?
Se4 Mo3 Mo1 97.08(2) . . ?
Se3 Mo3 Mo1 56.092(18) . . ?
Se1 Mo3 Mo1 56.001(18) . . ?
Mo2 Mo3 Mo1 59.886(16) . . ?
Se3 Ge1 Se3 180.0 . 3_566 ?
Se3 Ge1 Se2 96.483(16) . 3_566 ?
Se3 Ge1 Se2 83.517(16) 3_566 3_566 ?
Se3 Ge1 Se2 83.517(16) . . ?
Se3 Ge1 Se2 96.483(16) 3_566 . ?
Se2 Ge1 Se2 180.00(2) 3_566 . ?
Se3 Ge1 Se4 81.457(16) . . ?
Se3 Ge1 Se4 98.544(16) 3_566 . ?
Se2 Ge1 Se4 99.763(16) 3_566 . ?
Se2 Ge1 Se4 80.237(16) . . ?
Se3 Ge1 Se4 98.543(16) . 3_566 ?
Se3 Ge1 Se4 81.457(16) 3_566 3_566 ?
Se2 Ge1 Se4 80.237(16) 3_566 3_566 ?
Se2 Ge1 Se4 99.763(16) . 3_566 ?
Se4 Ge1 Se4 180.0 . 3_566 ?
Mo1 Se1 Mo3 67.79(2) . . ?
Mo1 Se1 Mo2 67.37(2) . . ?
Mo3 Se1 Mo2 67.193(19) . . ?
Mo1 Se2 Mo2 67.65(2) . . ?
Mo1 Se2 Ge1 93.63(2) . . ?
Mo2 Se2 Ge1 96.76(2) . . ?
Mo3 Se3 Mo1 67.85(2) . . ?
Mo3 Se3 Ge1 95.71(2) . . ?
Mo1 Se3 Ge1 93.65(2) . . ?
Mo3 Se4 Mo2 67.452(19) . . ?
Mo3 Se4 Ge1 93.86(2) . . ?
Mo2 Se4 Ge1 94.94(2) . . ?
O12 S1 O10 114.8(2) . . ?
O12 S1 O11 111.9(2) . . ?
O10 S1 O11 109.1(2) . . ?
O12 S1 C1 107.8(2) . . ?
O10 S1 C1 106.7(2) . . ?
O11 S1 C1 106.0(2) . . ?
C6 C1 C2 120.5(5) . . ?
C6 C1 S1 120.2(4) . . ?
C2 C1 S1 119.2(4) . . ?
C3 C2 C1 119.3(5) . . ?
C2 C3 C4 121.1(5) . . ?
C5 C4 C3 118.4(5) . . ?
C5 C4 C7 121.0(5) . . ?
C3 C4 C7 120.6(5) . . ?
C6 C5 C4 121.1(5) . . ?
C5 C6 C1 119.5(5) . . ?
O14 S2 O13 113.1(2) . . ?
O14 S2 O15 110.6(2) . . ?
O13 S2 O15 111.3(2) . . ?
O14 S2 C8 108.5(2) . . ?
O13 S2 C8 107.4(2) . . ?
O15 S2 C8 105.6(2) . . ?
C13 C8 C9 119.6(5) . . ?
C13 C8 S2 119.9(4) . . ?
C9 C8 S2 120.5(4) . . ?
C10 C9 C8 120.5(5) . . ?
C9 C10 C11 121.4(6) . . ?
C10 C11 C12 117.5(6) . . ?
C10 C11 C14 122.9(6) . . ?
C12 C11 C14 119.5(6) . . ?
C13 C12 C11 121.6(6) . . ?
C8 C13 C12 119.4(6) . . ?
O16 S3 O17 113.6(3) . . ?
O16 S3 O18 112.9(3) . . ?
O17 S3 O18 109.4(2) . . ?
O16 S3 C15 107.2(3) . . ?
O17 S3 C15 106.5(2) . . ?
O18 S3 C15 106.8(2) . . ?
C20 C15 C16 119.2(5) . . ?
C20 C15 S3 121.9(4) . . ?
C16 C15 S3 118.9(5) . . ?
C15 C16 C17 118.8(6) . . ?
C18 C17 C16 122.2(6) . . ?
C19 C18 C17 116.6(6) . . ?
C19 C18 C21 121.7(6) . . ?
C17 C18 C21 121.7(6) . . ?
C20 C19 C18 122.4(6) . . ?
C19 C20 C15 120.7(6) . . ?
O19 S4 O20 115.4(3) . . ?
O19 S4 O21 111.2(3) . . ?
O20 S4 O21 110.7(2) . . ?
O19 S4 C22 105.9(2) . . ?
O20 S4 C22 106.6(2) . . ?
O21 S4 C22 106.4(2) . . ?
C23 C22 C27 119.2(5) . . ?
C23 C22 S4 120.8(4) . . ?
C27 C22 S4 120.0(4) . . ?
C24 C23 C22 120.2(5) . . ?
C23 C24 C25 120.2(5) . . ?
C26 C25 C24 119.0(5) . . ?
C26 C25 C28 120.8(5) . . ?
C24 C25 C28 120.2(5) . . ?
C27 C26 C25 120.4(5) . . ?
C26 C27 C22 120.8(5) . . ?
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
Mo1 O3 2.143(3) . ?
Mo1 O2 2.163(4) . ?
Mo1 O1 2.201(4) . ?
Mo1 Se2 2.4491(7) . ?
Mo1 Se1 2.4577(7) . ?
Mo1 Se3 2.4592(7) . ?
Mo1 Mo2 2.7322(6) . ?
Mo1 Mo3 2.7445(6) . ?
Mo2 O5 2.152(4) . ?
Mo2 O4 2.172(4) . ?
Mo2 O6 2.206(4) . ?
Mo2 Se2 2.4590(7) . ?
Mo2 Se4 2.4625(7) . ?
Mo2 Se1 2.4687(7) . ?
Mo2 Mo3 2.7293(6) . ?
Mo3 O7 2.155(4) . ?
Mo3 O9 2.182(4) . ?
Mo3 O8 2.197(3) . ?
Mo3 Se4 2.4532(7) . ?
Mo3 Se3 2.4581(7) . ?
Mo3 Se1 2.4637(7) . ?
Ge1 Se3 2.5712(5) . ?
Ge1 Se3 2.5712(5) 3_566 ?
Ge1 Se2 2.5816(5) 3_566 ?
Ge1 Se2 2.5816(5) . ?
Ge1 Se4 2.6492(6) . ?
Ge1 Se4 2.6492(6) 3_566 ?
S1 O12 1.440(4) . ?
S1 O10 1.453(3) . ?
S1 O11 1.488(3) . ?
S1 C1 1.757(5) . ?
C1 C6 1.381(7) . ?
C1 C2 1.385(7) . ?
C2 C3 1.379(7) . ?
C3 C4 1.391(7) . ?
C4 C5 1.385(8) . ?
C4 C7 1.513(7) . ?
C5 C6 1.378(7) . ?
S2 O14 1.461(3) . ?
S2 O13 1.462(4) . ?
S2 O15 1.476(3) . ?
S2 C8 1.767(5) . ?
C8 C13 1.371(7) . ?
C8 C9 1.378(7) . ?
C9 C10 1.360(8) . ?
C10 C11 1.378(8) . ?
C11 C12 1.385(8) . ?
C11 C14 1.498(8) . ?
C12 C13 1.378(8) . ?
S3 O16 1.421(4) . ?
S3 O17 1.449(4) . ?
S3 O18 1.465(4) . ?
S3 C15 1.767(5) . ?
C15 C20 1.361(7) . ?
C15 C16 1.380(7) . ?
C16 C17 1.381(8) . ?
C17 C18 1.377(8) . ?
C18 C19 1.366(8) . ?
C18 C21 1.512(7) . ?
C19 C20 1.355(7) . ?
S4 O19 1.428(4) . ?
S4 O20 1.441(4) . ?
S4 O21 1.461(4) . ?
S4 C22 1.762(5) . ?
C22 C23 1.376(7) . ?
C22 C27 1.380(7) . ?
C23 C24 1.370(7) . ?
C24 C25 1.389(7) . ?
C25 C26 1.375(7) . ?
C25 C28 1.505(7) . ?
C26 C27 1.359(7) . ?
