# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

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#                                CCDC 
# 
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#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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#  fide research purposes only. It may contain copyright material
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data_1

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H66 Ge2 K2 Mo16 N6 O71'
_chemical_formula_weight         3153.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
Mo Mo -1.6832 0.6857 '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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   24.552(5)
_cell_length_b                   17.135(3)
_cell_length_c                   19.302(4)
_cell_angle_alpha                90
_cell_angle_beta                 111.10(3)
_cell_angle_gamma                90
_cell_volume                     7576(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      3.050
_cell_measurement_theta_max      27.450

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.765
_exptl_crystal_F_000             6016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    3.560
_shelx_estimated_absorpt_T_min   0.458
_shelx_estimated_absorpt_T_max   0.508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.412
_exptl_absorpt_correction_T_max  0.457
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_diffrn_detector_area_resol_mean 0.01
_diffrn_reflns_number            35236
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.050
_diffrn_reflns_theta_max         27.450
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8633
_reflns_number_gt                6667
_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       auto
_computing_cell_refinement       auto
_computing_data_reduction        auto
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.1000P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8633
_refine_ls_number_parameters     478
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.1440
_refine_ls_wR_factor_gt          0.1322
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_restrained_S_all      0.990
_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
Mo1 Mo 0.09630(3) 0.06238(4) 0.06175(3) 0.02050(15) Uani 1 1 d . . . . .
Mo2 Mo 0.34641(3) 0.34254(4) 0.08553(3) 0.02160(15) Uani 1 1 d . . . . .
Mo3 Mo 0.39772(3) 0.13420(4) 0.17220(3) 0.02216(15) Uani 1 1 d . . . . .
Mo4 Mo 0.20310(3) 0.31141(3) 0.03267(3) 0.01535(14) Uani 1 1 d . . . . .
Mo5 Mo 0.16303(3) 0.22520(4) 0.19481(3) 0.02180(15) Uani 1 1 d . . . . .
Mo6 Mo 0.30414(3) 0.25560(4) 0.24683(3) 0.02367(16) Uani 1 1 d . . . . .
Mo7 Mo 0.17868(3) -0.04890(4) 0.00064(3) 0.02220(15) Uani 1 1 d . . . . .
Mo8 Mo 0.33977(3) -0.01263(4) 0.06260(3) 0.02140(15) Uani 1 1 d . . . . .
Ge1 Ge 0.24338(3) 0.12141(4) 0.10182(4) 0.01440(16) Uani 1 1 d . . . . .
O1 O 0.2793(2) 0.3111(3) 0.1139(2) 0.0170(10) Uani 1 1 d . . . . .
O2 O 0.1643(2) 0.2840(3) 0.0876(3) 0.0218(11) Uani 1 1 d . . . . .
O3 O 0.2405(2) 0.1741(3) 0.1781(3) 0.0193(10) Uani 1 1 d . . . . .
O4 O 0.3195(3) 0.2061(4) 0.3287(3) 0.0408(16) Uani 1 1 d . . . . .
O5 O 0.2277(3) 0.2974(3) 0.2342(3) 0.0279(12) Uani 1 1 d . . . . .
O6 O 0.4024(2) 0.0606(3) 0.0972(3) 0.0273(12) Uani 1 1 d . . . . .
O7 O 0.2299(2) 0.1845(3) 0.0243(2) 0.0155(9) Uani 1 1 d . . . . .
O8 O 0.1909(2) 0.0468(3) 0.0820(3) 0.0190(10) Uani 1 1 d . . . . .
O9 O 0.3561(2) 0.2040(3) 0.2098(3) 0.0222(11) Uani 1 1 d . . . . .
O10 O 0.1921(2) 0.4110(3) 0.0229(3) 0.0217(11) Uani 1 1 d . . . . .
O11 O 0.3123(2) 0.0783(3) 0.1250(3) 0.0176(10) Uani 1 1 d . . . . .
O12 O 0.1008(2) -0.0111(3) -0.0130(3) 0.0257(12) Uani 1 1 d . . . . .
O13 O 0.3381(3) 0.3432(4) 0.2730(3) 0.0362(14) Uani 1 1 d . . . . .
O14 O 0.1210(2) 0.1518(3) 0.1229(3) 0.0271(12) Uani 1 1 d . . . . .
O15 O 0.1850(3) -0.1171(4) 0.0686(3) 0.0343(13) Uani 1 1 d . . . . .
O16 O 0.0989(3) -0.0038(4) 0.1298(3) 0.0308(13) Uani 1 1 d . . . . .
O17 O 0.3572(3) -0.0763(4) 0.1364(3) 0.0381(15) Uani 1 1 d . . . . .
O18 O 0.2588(2) -0.0330(3) 0.0195(3) 0.0271(12) Uani 1 1 d . . . . .
O19 O 0.3272(3) 0.4417(3) 0.0723(3) 0.0259(12) Uani 1 1 d . . . . .
O20 O 0.1084(2) 0.1489(3) -0.0227(3) 0.0225(11) Uani 1 1 d . . . . .
O21 O 0.3617(3) -0.0591(4) -0.0018(3) 0.0341(14) Uani 1 1 d . . . . .
O22 O 0.1738(3) 0.1721(4) 0.2741(3) 0.0372(15) Uani 1 1 d . . . . .
O23 O 0.4552(2) 0.1902(4) 0.1727(3) 0.0312(13) Uani 1 1 d . . . . .
O24 O 0.3469(2) 0.2205(3) 0.0612(2) 0.0179(10) Uani 1 1 d . . . . .
O25 O 0.4256(3) 0.0759(4) 0.2483(3) 0.0362(14) Uani 1 1 d . . . . .
O26 O 0.1598(3) -0.1014(4) -0.0799(3) 0.0365(14) Uani 1 1 d . . . . .
O27 O 0.4006(2) 0.3415(3) 0.1699(3) 0.0284(12) Uani 1 1 d . . . . .
O28 O 0.0231(3) 0.0821(4) 0.0221(3) 0.0335(13) Uani 1 1 d . . . . .
O29 O 0.1088(3) 0.2889(4) 0.1923(3) 0.0368(14) Uani 1 1 d . . . . .
O1W O 0.0281(3) -0.1802(5) 0.1795(4) 0.054(2) Uani 1 1 d . U . . .
O2W O 0.3755(6) 0.2432(6) 0.6344(6) 0.098(4) Uani 1 1 d . U . . .
O3W O 0.2478(7) -0.2619(10) 0.0662(8) 0.134(5) Uani 1 1 d . U . . .
O4W O -0.0314(6) -0.2755(9) 0.0152(8) 0.125(5) Uani 1 1 d . U . . .
O5W O 0.5000 -0.058(2) 0.2500 0.124(11) Uiso 0.62 2 d S . P . .
O6W O -0.0051(13) 0.1822(18) 0.1392(15) 0.129(9) Uiso 0.55 1 d . . P . .
O7W O 0.4476(12) 0.1430(16) 0.3918(13) 0.118(8) Uiso 0.55 1 d . . P . .
O8W O 0.5079(14) 0.029(2) 0.0867(16) 0.141(10) Uiso 0.52 1 d . . P . .
O9W O 0.0976(11) -0.2841(16) -0.0073(13) 0.122(8) Uiso 0.57 1 d . . P . .
C1 C 0.2123(5) 0.5010(5) 0.2235(5) 0.038(2) Uani 1 1 d . . . . .
H1A H 0.2094 0.5532 0.2426 0.046 Uiso 1 1 calc R U . . .
C2 C 0.2596(6) 0.5020(9) 0.1913(7) 0.063(3) Uani 1 1 d . . . . .
H2A H 0.2973 0.5092 0.2304 0.076 Uiso 1 1 calc R U . . .
H2B H 0.2601 0.4530 0.1664 0.076 Uiso 1 1 calc R U . . .
C3 C 0.4740(6) 0.5063(9) 0.2133(6) 0.064(3) Uani 1 1 d . . . . .
C4 C 0.1524(5) 0.4772(8) 0.1705(6) 0.051(3) Uani 1 1 d . . . . .
H4A H 0.1251 0.4793 0.1956 0.076 Uiso 1 1 calc R U . . .
H4B H 0.1541 0.4250 0.1532 0.076 Uiso 1 1 calc R U . . .
H4C H 0.1402 0.5123 0.1289 0.076 Uiso 1 1 calc R U . . .
C5 C 0.421(2) 0.541(3) 0.215(2) 0.145(19) Uani 0.5 1 d . U P . .
H5A H 0.3914 0.5382 0.1663 0.217 Uiso 0.5 1 calc R U P . .
H5B H 0.4285 0.5952 0.2291 0.217 Uiso 0.5 1 calc R U P . .
H5C H 0.4086 0.5144 0.2498 0.217 Uiso 0.5 1 calc R U P . .
N1 N 0.2297(4) 0.4449(4) 0.2872(4) 0.0393(19) Uani 1 1 d . . . . .
H1B H 0.2649 0.4577 0.3193 0.059 Uiso 1 1 calc R U . . .
H1C H 0.2308 0.3968 0.2704 0.059 Uiso 1 1 calc R U . . .
H1D H 0.2039 0.4469 0.3098 0.059 Uiso 1 1 calc R U . . .
N2 N 0.4856(6) 0.4874(10) 0.1511(6) 0.092(4) Uani 1 1 d . U . . .
H2C H 0.5217 0.4684 0.1644 0.138 Uiso 1 1 calc R U . . .
H2D H 0.4826 0.5299 0.1234 0.138 Uiso 1 1 calc R U . . .
H2E H 0.4602 0.4517 0.1250 0.138 Uiso 1 1 calc R U . . .
N3 N 0.2476(6) 0.5664(9) 0.1384(7) 0.096(5) Uani 1 1 d . . . . .
H3A H 0.2752 0.5680 0.1185 0.144 Uiso 1 1 calc R U . . .
H3B H 0.2475 0.6111 0.1617 0.144 Uiso 1 1 calc R U . . .
H3C H 0.2130 0.5593 0.1027 0.144 Uiso 1 1 calc R U . . .
K1 K 0.07520(19) -0.1673(3) 0.0699(3) 0.0455(10) Uani 0.5 1 d . . 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
Mo1 O28 1.715(6) . ?
Mo1 O16 1.719(5) . ?
Mo1 O14 1.896(6) . ?
Mo1 O12 1.947(5) . ?
Mo1 O8 2.228(5) . ?
Mo1 O20 2.300(5) . ?
Mo1 K1 3.980(5) . ?
Mo2 O27 1.692(5) . ?
Mo2 O19 1.758(6) . ?
Mo2 O20 1.921(5) 7 ?
Mo2 O1 1.988(5) . ?
Mo2 O24 2.145(5) . ?
Mo2 O7 2.314(4) 7 ?
Mo3 O25 1.703(6) . ?
Mo3 O23 1.705(6) . ?
Mo3 O9 1.880(5) . ?
Mo3 O6 1.954(5) . ?
Mo3 O11 2.184(5) . ?
Mo4 O2 1.726(5) . ?
Mo4 O10 1.727(5) . ?
Mo4 O24 1.868(5) 7 ?
Mo4 O1 1.962(5) . ?
Mo4 O7 2.286(5) 7 ?
Mo4 O7 2.295(5) . ?
Mo5 O29 1.710(6) . ?
Mo5 O22 1.718(6) . ?
Mo5 O14 1.881(5) . ?
Mo5 O5 1.939(6) . ?
Mo5 O3 2.221(5) . ?
Mo5 O2 2.311(5) . ?
Mo6 O13 1.703(6) . ?
Mo6 O4 1.713(6) . ?
Mo6 O9 1.891(5) . ?
Mo6 O5 1.941(6) . ?
Mo6 O3 2.158(5) . ?
Mo6 K1 3.936(5) 4 ?
Mo7 O26 1.711(6) . ?
Mo7 O15 1.722(6) . ?
Mo7 O18 1.887(6) . ?
Mo7 O12 1.945(6) . ?
Mo7 O8 2.215(5) . ?
Mo7 O19 2.287(5) 7 ?
Mo7 K1 3.847(5) . ?
Mo8 O21 1.717(6) . ?
Mo8 O17 1.722(6) . ?
Mo8 O18 1.890(6) . ?
Mo8 O6 1.910(6) . ?
Mo8 O11 2.217(5) . ?
Mo8 O10 2.332(5) 7 ?
Ge1 O11 1.750(5) . ?
Ge1 O3 1.750(5) . ?
Ge1 O8 1.757(5) . ?
Ge1 O7 1.777(4) . ?
O4 K1 3.403(8) 4 ?
O7 Mo4 2.286(5) 7 ?
O7 Mo2 2.314(5) 7 ?
O10 Mo8 2.332(5) 7 ?
O12 K1 3.293(7) . ?
O13 K1 3.018(8) 4 ?
O15 K1 2.837(8) . ?
O16 K1 3.006(8) . ?
O19 Mo7 2.287(5) 7 ?
O20 Mo2 1.921(5) 7 ?
O24 Mo4 1.868(5) 7 ?
O28 K1 2.832(8) 5 ?
O1W K1 2.760(9) . ?
O4W K1 3.068(15) . ?
O9W K1 2.67(3) . ?
C1 N1 1.495(11) . ?
C1 C4 1.513(14) . ?
C1 C2 1.502(15) . ?
C2 N3 1.459(19) . ?
C3 N2 1.370(16) . ?
C3 C5 1.44(5) . ?
C3 C3 1.53(2) 2_655 ?
K1 O28 2.832(8) 5 ?
K1 O13 3.018(7) 4_545 ?
K1 O4 3.403(8) 4_545 ?
K1 Mo6 3.936(5) 4_545 ?

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
O28 Mo1 O16 102.4(3) . . ?
O28 Mo1 O14 99.6(3) . . ?
O16 Mo1 O14 98.2(3) . . ?
O28 Mo1 O12 97.3(3) . . ?
O16 Mo1 O12 98.2(3) . . ?
O14 Mo1 O12 153.2(2) . . ?
O28 Mo1 O8 163.9(2) . . ?
O16 Mo1 O8 92.2(2) . . ?
O14 Mo1 O8 84.7(2) . . ?
O12 Mo1 O8 73.7(2) . . ?
O28 Mo1 O20 86.5(2) . . ?
O16 Mo1 O20 171.1(2) . . ?
O14 Mo1 O20 80.0(2) . . ?
O12 Mo1 O20 80.5(2) . . ?
O8 Mo1 O20 79.00(18) . . ?
O28 Mo1 K1 94.7(2) . . ?
O16 Mo1 K1 44.5(2) . . ?
O14 Mo1 K1 142.35(18) . . ?
O12 Mo1 K1 55.46(18) . . ?
O8 Mo1 K1 90.96(15) . . ?
O20 Mo1 K1 135.82(15) . . ?
O27 Mo2 O19 103.1(3) . . ?
O27 Mo2 O20 100.1(3) . 7 ?
O19 Mo2 O20 91.2(2) . 7 ?
O27 Mo2 O1 100.0(2) . . ?
O19 Mo2 O1 95.5(2) . . ?
O20 Mo2 O1 156.7(2) 7 . ?
O27 Mo2 O24 97.8(2) . . ?
O19 Mo2 O24 159.0(2) . . ?
O20 Mo2 O24 83.5(2) 7 . ?
O1 Mo2 O24 82.3(2) . . ?
O27 Mo2 O7 167.5(2) . 7 ?
O19 Mo2 O7 88.5(2) . 7 ?
O20 Mo2 O7 84.13(19) 7 7 ?
O1 Mo2 O7 73.80(17) . 7 ?
O24 Mo2 O7 70.81(17) . 7 ?
O25 Mo3 O23 104.5(3) . . ?
O25 Mo3 O9 98.4(3) . . ?
O23 Mo3 O9 101.7(3) . . ?
O25 Mo3 O6 98.5(3) . . ?
O23 Mo3 O6 95.6(3) . . ?
O9 Mo3 O6 151.9(2) . . ?
O25 Mo3 O11 97.5(3) . . ?
O23 Mo3 O11 156.7(2) . . ?
O9 Mo3 O11 82.4(2) . . ?
O6 Mo3 O11 73.2(2) . . ?
O2 Mo4 O10 103.7(3) . . ?
O2 Mo4 O24 101.6(2) . 7 ?
O10 Mo4 O24 99.2(2) . 7 ?
O2 Mo4 O1 94.9(2) . . ?
O10 Mo4 O1 99.0(2) . . ?
O24 Mo4 O1 151.6(2) 7 . ?
O2 Mo4 O7 162.9(2) . 7 ?
O10 Mo4 O7 91.6(2) . 7 ?
O24 Mo4 O7 83.00(19) 7 7 ?
O1 Mo4 O7 74.92(18) . 7 ?
O2 Mo4 O7 91.2(2) . . ?
O10 Mo4 O7 165.0(2) . . ?
O24 Mo4 O7 76.07(19) 7 . ?
O1 Mo4 O7 80.72(19) . . ?
O7 Mo4 O7 73.84(19) 7 . ?
O29 Mo5 O22 103.4(3) . . ?
O29 Mo5 O14 101.0(3) . . ?
O22 Mo5 O14 99.9(3) . . ?
O29 Mo5 O5 97.1(3) . . ?
O22 Mo5 O5 98.4(3) . . ?
O14 Mo5 O5 150.4(2) . . ?
O29 Mo5 O3 161.3(3) . . ?
O22 Mo5 O3 93.2(3) . . ?
O14 Mo5 O3 84.3(2) . . ?
O5 Mo5 O3 71.7(2) . . ?
O29 Mo5 O2 87.6(3) . . ?
O22 Mo5 O2 168.9(3) . . ?
O14 Mo5 O2 79.1(2) . . ?
O5 Mo5 O2 78.5(2) . . ?
O3 Mo5 O2 75.74(18) . . ?
O13 Mo6 O4 104.0(3) . . ?
O13 Mo6 O9 101.5(3) . . ?
O4 Mo6 O9 99.4(3) . . ?
O13 Mo6 O5 93.4(3) . . ?
O4 Mo6 O5 100.4(3) . . ?
O9 Mo6 O5 151.5(2) . . ?
O13 Mo6 O3 157.1(3) . . ?
O4 Mo6 O3 96.7(3) . . ?
O9 Mo6 O3 84.4(2) . . ?
O5 Mo6 O3 73.1(2) . . ?
O13 Mo6 K1 46.2(2) . 4 ?
O4 Mo6 K1 59.5(2) . 4 ?
O9 Mo6 K1 95.99(16) . 4 ?
O5 Mo6 K1 111.70(17) . 4 ?
O3 Mo6 K1 156.01(15) . 4 ?
O26 Mo7 O15 104.9(3) . . ?
O26 Mo7 O18 100.0(3) . . ?
O15 Mo7 O18 98.6(3) . . ?
O26 Mo7 O12 97.0(3) . . ?
O15 Mo7 O12 98.2(3) . . ?
O18 Mo7 O12 152.1(2) . . ?
O26 Mo7 O8 163.3(3) . . ?
O15 Mo7 O8 90.5(2) . . ?
O18 Mo7 O8 83.7(2) . . ?
O12 Mo7 O8 74.0(2) . . ?
O26 Mo7 O19 85.8(3) . 7 ?
O15 Mo7 O19 169.3(2) . 7 ?
O18 Mo7 O19 80.4(2) . 7 ?
O12 Mo7 O19 79.0(2) . 7 ?
O8 Mo7 O19 78.74(18) . 7 ?
O26 Mo7 K1 92.4(2) . . ?
O15 Mo7 K1 42.8(2) . . ?
O18 Mo7 K1 141.43(18) . . ?
O12 Mo7 K1 58.84(18) . . ?
O8 Mo7 K1 94.67(15) . . ?
O19 Mo7 K1 137.26(17) 7 . ?
O21 Mo8 O17 104.8(3) . . ?
O21 Mo8 O18 98.6(3) . . ?
O17 Mo8 O18 99.0(3) . . ?
O21 Mo8 O6 97.7(3) . . ?
O17 Mo8 O6 101.4(3) . . ?
O18 Mo8 O6 149.5(2) . . ?
O21 Mo8 O11 162.6(2) . . ?
O17 Mo8 O11 91.7(3) . . ?
O18 Mo8 O11 83.7(2) . . ?
O6 Mo8 O11 73.3(2) . . ?
O21 Mo8 O10 86.9(2) . 7 ?
O17 Mo8 O10 168.2(3) . 7 ?
O18 Mo8 O10 78.1(2) . 7 ?
O6 Mo8 O10 77.3(2) . 7 ?
O11 Mo8 O10 76.65(18) . 7 ?
O11 Ge1 O3 109.3(2) . . ?
O11 Ge1 O8 108.3(2) . . ?
O3 Ge1 O8 108.0(2) . . ?
O11 Ge1 O7 110.0(2) . . ?
O3 Ge1 O7 110.1(2) . . ?
O8 Ge1 O7 111.0(2) . . ?
Mo4 O1 Mo2 115.2(2) . . ?
Mo4 O2 Mo5 149.0(3) . . ?
Ge1 O3 Mo6 127.7(3) . . ?
Ge1 O3 Mo5 128.4(3) . . ?
Mo6 O3 Mo5 97.1(2) . . ?
Mo6 O4 K1 94.8(3) . 4 ?
Mo6 O5 Mo5 115.6(3) . . ?
Mo8 O6 Mo3 115.4(3) . . ?
Ge1 O7 Mo4 118.4(2) . 7 ?
Ge1 O7 Mo4 119.2(2) . . ?
Mo4 O7 Mo4 106.16(19) 7 . ?
Ge1 O7 Mo2 119.6(2) . 7 ?
Mo4 O7 Mo2 92.91(16) 7 7 ?
Mo4 O7 Mo2 95.53(17) . 7 ?
Ge1 O8 Mo7 126.5(3) . . ?
Ge1 O8 Mo1 126.0(3) . . ?
Mo7 O8 Mo1 95.62(19) . . ?
Mo3 O9 Mo6 167.8(3) . . ?
Mo4 O10 Mo8 144.6(3) . 7 ?
Ge1 O11 Mo3 128.0(3) . . ?
Ge1 O11 Mo8 127.8(2) . . ?
Mo3 O11 Mo8 95.78(19) . . ?
Mo7 O12 Mo1 115.5(3) . . ?
Mo7 O12 K1 90.8(2) . . ?
Mo1 O12 K1 95.4(2) . . ?
Mo6 O13 K1 109.8(3) . 4 ?
Mo5 O14 Mo1 165.2(3) . . ?
Mo7 O15 K1 112.8(3) . . ?
Mo1 O16 K1 111.9(3) . . ?
Mo8 O18 Mo7 165.8(3) . . ?
Mo2 O19 Mo7 145.1(3) . 7 ?
Mo2 O20 Mo1 138.4(3) 7 . ?
Mo4 O24 Mo2 116.3(2) 7 . ?
Mo1 O28 K1 154.3(3) . 5 ?
N1 C1 C4 107.8(9) . . ?
N1 C1 C2 108.2(9) . . ?
C4 C1 C2 115.5(9) . . ?
N3 C2 C1 108.0(11) . . ?
N2 C3 C5 126(2) . . ?
N2 C3 C3 116.4(15) . 2_655 ?
C5 C3 C3 116(2) . 2_655 ?
O9W K1 O1W 126.5(6) . . ?
O9W K1 O15 80.5(6) . . ?
O1W K1 O15 133.8(3) . . ?
O9W K1 O28 109.7(6) . 5 ?
O1W K1 O28 91.4(2) . 5 ?
O15 K1 O28 115.8(2) . 5 ?
O9W K1 O16 149.7(6) . . ?
O1W K1 O16 81.8(2) . . ?
O15 K1 O16 70.6(2) . . ?
O28 K1 O16 76.4(2) 5 . ?
O9W K1 O13 113.1(6) . 4_545 ?
O1W K1 O13 64.7(2) . 4_545 ?
O15 K1 O13 70.3(2) . 4_545 ?
O28 K1 O13 137.1(3) 5 4_545 ?
O16 K1 O13 65.77(19) . 4_545 ?
O9W K1 O4W 71.1(6) . . ?
O1W K1 O4W 71.0(4) . . ?
O15 K1 O4W 151.1(4) . . ?
O28 K1 O4W 70.5(3) 5 . ?
O16 K1 O4W 135.9(4) . . ?
O13 K1 O4W 126.0(3) 4_545 . ?
O9W K1 O12 103.0(6) . . ?
O1W K1 O12 130.0(3) . . ?
O15 K1 O12 53.21(18) . . ?
O28 K1 O12 62.95(19) 5 . ?
O16 K1 O12 52.04(16) . . ?
O13 K1 O12 104.5(2) 4_545 . ?
O4W K1 O12 127.8(3) . . ?
O9W K1 O4 64.9(5) . 4_545 ?
O1W K1 O4 87.1(2) . 4_545 ?
O15 K1 O4 70.8(2) . 4_545 ?
O28 K1 O4 171.3(3) 5 4_545 ?
O16 K1 O4 111.8(2) . 4_545 ?
O13 K1 O4 49.11(18) 4_545 4_545 ?
O4W K1 O4 100.9(3) . 4_545 ?
O12 K1 O4 124.0(2) . 4_545 ?
O9W K1 Mo7 84.7(6) . . ?
O1W K1 Mo7 145.1(2) . . ?
O15 K1 Mo7 24.36(13) . . ?
O28 K1 Mo7 91.75(17) 5 . ?
O16 K1 Mo7 65.29(14) . . ?
O13 K1 Mo7 90.16(16) 4_545 . ?
O4W K1 Mo7 141.9(3) . . ?
O12 K1 Mo7 30.36(11) . . ?
O4 K1 Mo7 94.34(16) 4_545 . ?
O9W K1 Mo6 90.6(5) . 4_545 ?
O1W K1 Mo6 70.83(18) . 4_545 ?
O15 K1 Mo6 72.53(16) . 4_545 ?
O28 K1 Mo6 158.8(2) 5 4_545 ?
O16 K1 Mo6 89.36(16) . 4_545 ?
O13 K1 Mo6 24.03(13) 4_545 4_545 ?
O4W K1 Mo6 112.3(3) . 4_545 ?
O12 K1 Mo6 119.73(16) . 4_545 ?
O4 K1 Mo6 25.70(11) 4_545 4_545 ?
Mo7 K1 Mo6 96.42(10) . 4_545 ?
O9W K1 Mo1 131.6(6) . . ?
O1W K1 Mo1 101.9(2) . . ?
O15 K1 Mo1 64.04(16) . . ?
O28 K1 Mo1 63.86(16) 5 . ?
O16 K1 Mo1 23.63(11) . . ?
O13 K1 Mo1 85.77(17) 4_545 . ?
O4W K1 Mo1 133.7(3) . . ?
O12 K1 Mo1 29.15(10) . . ?
O4 K1 Mo1 124.79(18) 4_545 . ?
Mo7 K1 Mo1 49.71(6) . . ?
Mo6 K1 Mo1 107.52(11) 4_545 . ?

_refine_diff_density_max         2.291
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.220

_shelxl_version_number           2013-2

_database_code_depnum_ccdc_archive 'CCDC 989934'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ge2 H60 Mo16 Na12 O88'
_chemical_formula_weight         3424.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
Mo Mo -1.6832 0.6857 '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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_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'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   21.051(4)
_cell_length_b                   15.483(3)
_cell_length_c                   13.472(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.62(3)
_cell_angle_gamma                90
_cell_volume                     4267.8(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      3.057
_cell_measurement_theta_max      27.482

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.665
_exptl_crystal_F_000             3264
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    3.142
_shelx_estimated_absorpt_T_min   0.587
_shelx_estimated_absorpt_T_max   0.667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.556
_exptl_absorpt_correction_T_max  0.644
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_diffrn_detector_area_resol_mean 0.01
_diffrn_reflns_number            20526
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.057
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             5014
_reflns_number_gt                4582
_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       auto
_computing_cell_refinement       auto
_computing_data_reduction        auto
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0606P)²+66.5414P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5014
_refine_ls_number_parameters     300
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0399
_refine_ls_wR_factor_ref         0.1237
_refine_ls_wR_factor_gt          0.1212
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.095
_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
Mo1 Mo 0.5000 0.38345(4) 0.0000 0.01669(15) Uani 1 2 d S T P . .
Mo2 Mo 0.36244(3) 0.5000 -0.02650(5) 0.02409(17) Uani 1 2 d S T P . .
Mo3 Mo 0.37628(2) 0.37832(3) -0.26904(4) 0.02241(13) Uani 1 1 d . . . . .
Mo4 Mo 0.32988(3) 0.39430(3) 0.22146(4) 0.02313(14) Uani 1 1 d . . . . .
Mo5 Mo 0.48661(3) 0.27173(3) 0.25071(4) 0.02235(13) Uani 1 1 d . . . . .
Ge1 Ge 0.47831(4) 0.5000 0.21278(6) 0.01562(17) Uani 1 2 d S T P . .
O1 O 0.4675(3) 0.5000 0.0762(4) 0.0161(10) Uani 1 2 d S T P . .
O2 O 0.41683(19) 0.4120(3) -0.0870(3) 0.0201(8) Uani 1 1 d . . . . .
O3 O 0.4024(3) 0.5000 0.2432(4) 0.0203(11) Uani 1 2 d S T P . .
O4 O 0.2811(3) 0.5000 0.1835(5) 0.0257(12) Uani 1 2 d S T P . .
O5 O 0.3677(3) 0.5000 -0.2685(5) 0.0246(12) Uani 1 2 d S T P . .
O6 O 0.4745(2) 0.3153(3) 0.0839(3) 0.0220(8) Uani 1 1 d . . . . .
O7 O 0.3439(2) 0.4143(3) 0.0576(3) 0.0271(9) Uani 1 1 d . . . . .
O8 O 0.3294(3) 0.3938(3) 0.3491(4) 0.0366(11) Uani 1 1 d . . . . .
O9 O 0.3556(2) 0.3625(3) -0.3980(3) 0.0342(10) Uani 1 1 d . . . . .
O10 O 0.4243(2) 0.2714(3) -0.2322(3) 0.0251(9) Uani 1 1 d . . . . .
O11 O 0.52181(19) 0.5926(3) 0.2629(3) 0.0210(8) Uani 1 1 d . . . . .
O12 O 0.5029(3) 0.2608(3) 0.3804(4) 0.0378(11) Uani 1 1 d . . . . .
O13 O 0.2942(3) 0.5000 -0.1210(5) 0.0283(13) Uani 1 2 d S T P . .
O14 O 0.4036(2) 0.3216(3) 0.2267(3) 0.0278(9) Uani 1 1 d . . . . .
O15 O 0.4671(3) 0.1689(3) 0.2061(4) 0.0355(11) Uani 1 1 d . . . . .
O16 O 0.2682(2) 0.3248(3) 0.1688(4) 0.0382(11) Uani 1 1 d . . . . .
O17 O 0.3079(2) 0.3461(3) -0.2304(4) 0.0334(10) Uani 1 1 d . . . . .
Na1 Na 0.2606(2) 0.3542(3) 0.4577(3) 0.0663(10) Uani 1 1 d . . . . .
Na2 Na 0.1666(3) 0.2571(4) 0.0072(5) 0.1066(19) Uani 1 1 d . . . . .
Na3 Na 0.08312(18) 0.5000 0.0610(3) 0.0338(8) Uani 1 2 d S T P . .
Na4 Na 0.5505(3) 0.3868(4) 0.5089(5) 0.0388(14) Uani 0.5 1 d . . P A 1
O11W O 0.5656(9) 0.4485(14) 0.5069(12) 0.099(6) Uani 0.5 1 d . U P B 2
O1W O 0.1853(3) 0.3648(4) -0.1570(6) 0.0619(18) Uani 1 1 d . . . . .
O2W O -0.0197(4) 0.5000 0.1148(6) 0.0385(16) Uani 1 2 d S T P . .
O3W O 0.0665(3) 0.3473(3) 0.0613(4) 0.0413(12) Uani 1 1 d . . . . .
O4W O 0.1574(4) 0.5000 0.2257(6) 0.0482(19) Uani 1 2 d S T P . .
O5W O 0.1800(4) 0.5000 -0.0059(7) 0.054(2) Uani 1 2 d S T P . .
O6W O 0.2036(10) 0.5000 0.6804(13) 0.140(7) Uani 1 2 d S T P . .
O7W O 0.2836(4) 0.2140(5) 0.4132(6) 0.075(2) Uani 1 1 d . . . . .
O8W O 0.1532(5) 0.3590(5) 0.3484(7) 0.094(3) Uani 1 1 d . U . . .
O9W O 0.2474(8) 0.5000 0.4980(13) 0.113(5) Uani 1 2 d S TU P . .
O10W O 0.4107(7) 0.1500(11) 0.4694(15) 0.085(5) 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
Mo1 O6 1.721(4) 2_655 ?
Mo1 O6 1.721(4) . ?
Mo1 O2 1.916(4) . ?
Mo1 O2 1.916(4) 2_655 ?
Mo1 O1 2.260(3) 5_665 ?
Mo1 O1 2.260(3) . ?
Mo2 O13 1.680(6) . ?
Mo2 O7 1.845(4) . ?
Mo2 O7 1.845(4) 6_565 ?
Mo2 O2 2.066(4) 6_565 ?
Mo2 O2 2.066(4) . ?
Mo2 O1 2.316(5) . ?
Mo3 O9 1.706(5) . ?
Mo3 O17 1.716(5) . ?
Mo3 O5 1.8930(9) . ?
Mo3 O10 1.943(4) . ?
Mo3 O11 2.174(4) 5_665 ?
Mo3 O2 2.456(4) . ?
Mo4 O16 1.706(5) . ?
Mo4 O8 1.721(5) . ?
Mo4 O14 1.904(4) . ?
Mo4 O4 1.936(3) . ?
Mo4 O3 2.210(4) . ?
Mo4 O7 2.316(4) . ?
Mo5 O12 1.708(5) . ?
Mo5 O15 1.718(5) . ?
Mo5 O14 1.868(4) . ?
Mo5 O10 1.948(4) 2_655 ?
Mo5 O11 2.220(4) 6_565 ?
Mo5 O6 2.303(4) . ?
Ge1 O3 1.741(5) . ?
Ge1 O11 1.749(4) . ?
Ge1 O11 1.749(4) 6_565 ?
Ge1 O1 1.801(5) . ?
O1 Mo1 2.260(3) 5_665 ?
O3 Mo4 2.210(4) 6_565 ?
O4 Mo4 1.936(3) 6_565 ?
O5 Mo3 1.8929(9) 6_565 ?
O7 Na2 2.787(7) 7 ?
O8 Na1 2.369(6) . ?
O8 Na4 2.791(8) 2_656 ?
O9 Na1 2.442(6) 1_554 ?
O9 Na4 2.771(8) 2_655 ?
O10 Mo5 1.948(4) 2_655 ?
O11 Mo3 2.174(4) 5_665 ?
O11 Mo5 2.220(4) 6_565 ?
O12 Na4 2.644(8) . ?
O12 Na4 2.842(8) 2_656 ?
O16 Na2 2.867(8) . ?
Na1 O7W 2.334(10) . ?
Na1 O9W 2.353(7) . ?
Na1 O8W 2.392(9) . ?
Na1 O7W 2.403(8) 7_556 ?
Na1 O9 2.442(6) 1_556 ?
Na1 Na1 3.487(9) 7_556 ?
Na1 Na4 3.928(8) 2_656 ?
Na2 O3W 2.766(8) . ?
Na2 O7 2.787(7) 7 ?
Na2 O1W 2.870(10) . ?
Na2 Na2 3.568(12) 7 ?
Na3 O3W 2.390(5) 6_565 ?
Na3 O3W 2.390(5) . ?
Na3 O4W 2.395(9) . ?
Na3 O5W 2.415(9) . ?
Na3 O2W 2.430(9) 5_565 ?
Na3 O2W 2.439(8) . ?
Na3 Na3 3.498(8) 5_565 ?
Na4 Na4 2.081(12) 2_656 ?
Na4 O9 2.771(8) 2_655 ?
Na4 O8 2.791(8) 2_656 ?
Na4 O12 2.842(8) 2_656 ?
Na4 Na4 3.506(14) 6_565 ?
Na4 Na1 3.928(8) 2_656 ?
Na4 Na4 4.077(14) 5_666 ?
O11W O11W 1.59(4) 6_565 ?
O2W Na3 2.430(9) 5_565 ?
O7W Na1 2.403(8) 7_556 ?
O9W Na1 2.353(7) 6_565 ?

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
O6 Mo1 O6 104.4(3) 2_655 . ?
O6 Mo1 O2 96.95(18) 2_655 . ?
O6 Mo1 O2 99.34(18) . . ?
O6 Mo1 O2 99.35(18) 2_655 2_655 ?
O6 Mo1 O2 96.95(18) . 2_655 ?
O2 Mo1 O2 153.3(2) . 2_655 ?
O6 Mo1 O1 90.97(17) 2_655 5_665 ?
O6 Mo1 O1 164.12(17) . 5_665 ?
O2 Mo1 O1 82.44(18) . 5_665 ?
O2 Mo1 O1 76.26(17) 2_655 5_665 ?
O6 Mo1 O1 164.12(17) 2_655 . ?
O6 Mo1 O1 90.97(17) . . ?
O2 Mo1 O1 76.26(17) . . ?
O2 Mo1 O1 82.43(18) 2_655 . ?
O1 Mo1 O1 74.0(2) 5_665 . ?
O13 Mo2 O7 101.4(2) . . ?
O13 Mo2 O7 101.4(2) . 6_565 ?
O7 Mo2 O7 91.9(3) . 6_565 ?
O13 Mo2 O2 98.91(19) . 6_565 ?
O7 Mo2 O2 158.96(18) . 6_565 ?
O7 Mo2 O2 89.18(18) 6_565 6_565 ?
O13 Mo2 O2 98.91(19) . . ?
O7 Mo2 O2 89.18(18) . . ?
O7 Mo2 O2 158.96(18) 6_565 . ?
O2 Mo2 O2 82.5(2) 6_565 . ?
O13 Mo2 O1 168.0(2) . . ?
O7 Mo2 O1 86.80(17) . . ?
O7 Mo2 O1 86.80(17) 6_565 . ?
O2 Mo2 O1 72.28(14) 6_565 . ?
O2 Mo2 O1 72.28(14) . . ?
O9 Mo3 O17 103.6(2) . . ?
O9 Mo3 O5 98.3(2) . . ?
O17 Mo3 O5 101.6(2) . . ?
O9 Mo3 O10 97.5(2) . . ?
O17 Mo3 O10 95.6(2) . . ?
O5 Mo3 O10 153.1(2) . . ?
O9 Mo3 O11 94.7(2) . 5_665 ?
O17 Mo3 O11 159.91(19) . 5_665 ?
O5 Mo3 O11 83.6(2) . 5_665 ?
O10 Mo3 O11 73.54(16) . 5_665 ?
O9 Mo3 O2 173.08(19) . . ?
O17 Mo3 O2 83.01(19) . . ?
O5 Mo3 O2 78.2(2) . . ?
O10 Mo3 O2 83.60(16) . . ?
O11 Mo3 O2 79.05(14) 5_665 . ?
O16 Mo4 O8 103.3(2) . . ?
O16 Mo4 O14 100.1(2) . . ?
O8 Mo4 O14 99.0(2) . . ?
O16 Mo4 O4 96.8(2) . . ?
O8 Mo4 O4 98.1(2) . . ?
O14 Mo4 O4 152.4(2) . . ?
O16 Mo4 O3 162.9(2) . . ?
O8 Mo4 O3 92.1(2) . . ?
O14 Mo4 O3 84.35(17) . . ?
O4 Mo4 O3 73.49(18) . . ?
O16 Mo4 O7 86.7(2) . . ?
O8 Mo4 O7 169.9(2) . . ?
O14 Mo4 O7 80.17(18) . . ?
O4 Mo4 O7 79.2(2) . . ?
O3 Mo4 O7 77.79(18) . . ?
O12 Mo5 O15 103.9(2) . . ?
O12 Mo5 O14 99.9(2) . . ?
O15 Mo5 O14 100.7(2) . . ?
O12 Mo5 O10 99.4(2) . 2_655 ?
O15 Mo5 O10 96.3(2) . 2_655 ?
O14 Mo5 O10 150.24(18) . 2_655 ?
O12 Mo5 O11 92.0(2) . 6_565 ?
O15 Mo5 O11 161.97(19) . 6_565 ?
O14 Mo5 O11 84.51(17) . 6_565 ?
O10 Mo5 O11 72.40(16) 2_655 6_565 ?
O12 Mo5 O6 167.7(2) . . ?
O15 Mo5 O6 88.1(2) . . ?
O14 Mo5 O6 79.98(17) . . ?
O10 Mo5 O6 76.38(16) 2_655 . ?
O11 Mo5 O6 75.71(14) 6_565 . ?
O3 Ge1 O11 109.59(16) . . ?
O3 Ge1 O11 109.59(16) . 6_565 ?
O11 Ge1 O11 110.1(3) . 6_565 ?
O3 Ge1 O1 109.8(3) . . ?
O11 Ge1 O1 108.85(16) . . ?
O11 Ge1 O1 108.85(16) 6_565 . ?
Ge1 O1 Mo1 119.02(15) . . ?
Ge1 O1 Mo1 119.02(15) . 5_665 ?
Mo1 O1 Mo1 106.0(2) . 5_665 ?
Ge1 O1 Mo2 118.9(3) . . ?
Mo1 O1 Mo2 94.44(15) . . ?
Mo1 O1 Mo2 94.44(15) 5_665 . ?
Mo1 O2 Mo2 114.99(18) . . ?
Mo1 O2 Mo3 127.94(19) . . ?
Mo2 O2 Mo3 116.07(17) . . ?
Ge1 O3 Mo4 127.77(14) . . ?
Ge1 O3 Mo4 127.77(14) . 6_565 ?
Mo4 O3 Mo4 95.5(2) . 6_565 ?
Mo4 O4 Mo4 115.4(3) . 6_565 ?
Mo3 O5 Mo3 168.9(4) 6_565 . ?
Mo1 O6 Mo5 147.2(2) . . ?
Mo2 O7 Mo4 140.7(2) . . ?
Mo2 O7 Na2 120.4(2) . 7 ?
Mo4 O7 Na2 98.8(2) . 7 ?
Mo4 O8 Na1 140.0(3) . . ?
Mo4 O8 Na4 117.9(3) . 2_656 ?
Na1 O8 Na4 98.8(2) . 2_656 ?
Mo3 O9 Na1 141.5(3) . 1_554 ?
Mo3 O9 Na4 119.1(3) . 2_655 ?
Na1 O9 Na4 97.6(2) 1_554 2_655 ?
Mo3 O10 Mo5 115.1(2) . 2_655 ?
Ge1 O11 Mo3 127.3(2) . 5_665 ?
Ge1 O11 Mo5 127.7(2) . 6_565 ?
Mo3 O11 Mo5 96.68(16) 5_665 6_565 ?
Mo5 O12 Na4 123.4(3) . . ?
Mo5 O12 Na4 117.4(3) . 2_656 ?
Na4 O12 Na4 44.4(3) . 2_656 ?
Mo5 O14 Mo4 166.3(3) . . ?
Mo4 O16 Na2 154.8(3) . . ?
O7W Na1 O9W 174.1(5) . . ?
O7W Na1 O8 83.6(3) . . ?
O9W Na1 O8 91.0(5) . . ?
O7W Na1 O8W 95.4(3) . . ?
O9W Na1 O8W 88.1(5) . . ?
O8 Na1 O8W 103.8(3) . . ?
O7W Na1 O7W 85.2(3) . 7_556 ?
O9W Na1 O7W 99.6(5) . 7_556 ?
O8 Na1 O7W 163.5(3) . 7_556 ?
O8W Na1 O7W 89.3(3) . 7_556 ?
O7W Na1 O9 94.2(3) . 1_556 ?
O9W Na1 O9 83.4(4) . 1_556 ?
O8 Na1 O9 88.5(2) . 1_556 ?
O8W Na1 O9 165.2(3) . 1_556 ?
O7W Na1 O9 80.3(2) 7_556 1_556 ?
O7W Na1 Na1 43.4(2) . 7_556 ?
O9W Na1 Na1 141.4(5) . 7_556 ?
O8 Na1 Na1 125.9(3) . 7_556 ?
O8W Na1 Na1 93.1(3) . 7_556 ?
O7W Na1 Na1 41.8(2) 7_556 7_556 ?
O9 Na1 Na1 86.1(2) 1_556 7_556 ?
O7W Na1 Na4 83.3(2) . 2_656 ?
O9W Na1 Na4 91.2(4) . 2_656 ?
O8 Na1 Na4 44.60(18) . 2_656 ?
O8W Na1 Na4 148.4(3) . 2_656 ?
O7W Na1 Na4 121.9(3) 7_556 2_656 ?
O9 Na1 Na4 44.36(16) 1_556 2_656 ?
Na1 Na1 Na4 106.6(2) 7_556 2_656 ?
O3W Na2 O7 123.7(3) . 7 ?
O3W Na2 O16 95.4(2) . . ?
O7 Na2 O16 125.2(3) 7 . ?
O3W Na2 O1W 99.3(3) . . ?
O7 Na2 O1W 109.1(3) 7 . ?
O16 Na2 O1W 99.2(3) . . ?
O3W Na2 Na2 150.0(3) . 7 ?
O7 Na2 Na2 86.0(2) 7 7 ?
O16 Na2 Na2 59.75(19) . 7 ?
O1W Na2 Na2 71.3(3) . 7 ?
O3W Na3 O3W 163.1(3) 6_565 . ?
O3W Na3 O4W 93.58(17) 6_565 . ?
O3W Na3 O4W 93.58(17) . . ?
O3W Na3 O5W 97.92(16) 6_565 . ?
O3W Na3 O5W 97.92(16) . . ?
O4W Na3 O5W 85.5(3) . . ?
O3W Na3 O2W 87.39(17) 6_565 5_565 ?
O3W Na3 O2W 87.39(17) . 5_565 ?
O4W Na3 O2W 172.9(3) . 5_565 ?
O5W Na3 O2W 87.4(3) . 5_565 ?
O3W Na3 O2W 81.87(16) 6_565 . ?
O3W Na3 O2W 81.87(16) . . ?
O4W Na3 O2W 99.0(3) . . ?
O5W Na3 O2W 175.5(3) . . ?
O2W Na3 O2W 88.1(3) 5_565 . ?
O3W Na3 Na3 82.52(16) 6_565 5_565 ?
O3W Na3 Na3 82.52(16) . 5_565 ?
O4W Na3 Na3 142.9(3) . 5_565 ?
O5W Na3 Na3 131.6(3) . 5_565 ?
O2W Na3 Na3 44.2(2) 5_565 5_565 ?
O2W Na3 Na3 44.0(2) . 5_565 ?
Na4 Na4 O12 72.9(3) 2_656 . ?
Na4 Na4 O9 140.9(5) 2_656 2_655 ?
O12 Na4 O9 75.8(2) . 2_655 ?
Na4 Na4 O8 144.6(5) 2_656 2_656 ?
O12 Na4 O8 128.3(3) . 2_656 ?
O9 Na4 O8 74.2(2) 2_655 2_656 ?
Na4 Na4 O12 62.8(3) 2_656 2_656 ?
O12 Na4 O12 72.6(2) . 2_656 ?
O9 Na4 O12 127.6(3) 2_655 2_656 ?
O8 Na4 O12 94.2(2) 2_656 2_656 ?
Na4 Na4 Na4 90.000(1) 2_656 6_565 ?
O12 Na4 Na4 137.55(18) . 6_565 ?
O9 Na4 Na4 97.81(17) 2_655 6_565 ?
O8 Na4 Na4 87.76(18) 2_656 6_565 ?
O12 Na4 Na4 133.36(17) 2_656 6_565 ?
Na4 Na4 Na1 172.62(12) 2_656 2_656 ?
O12 Na4 Na1 101.4(2) . 2_656 ?
O9 Na4 Na1 38.04(14) 2_655 2_656 ?
O8 Na4 Na1 36.58(14) 2_656 2_656 ?
O12 Na4 Na1 111.5(2) 2_656 2_656 ?
Na4 Na4 Na1 97.38(12) 6_565 2_656 ?
Na4 Na4 Na4 59.31(17) 2_656 5_666 ?
O12 Na4 Na4 119.0(3) . 5_666 ?
O9 Na4 Na4 120.9(3) 2_655 5_666 ?
O8 Na4 Na4 112.5(3) 2_656 5_666 ?
O12 Na4 Na4 110.9(3) 2_656 5_666 ?
Na4 Na4 Na4 30.69(17) 6_565 5_666 ?
Na1 Na4 Na4 128.1(2) 2_656 5_666 ?
Na3 O2W Na3 91.9(3) 5_565 . ?
Na3 O3W Na2 112.2(2) . . ?
Na1 O7W Na1 94.8(3) . 7_556 ?
Na1 O9W Na1 147.1(9) 6_565 . ?

_refine_diff_density_max         2.144
_refine_diff_density_min         -1.337
_refine_diff_density_rms         0.193

_shelxl_version_number           2013-2

_database_code_depnum_ccdc_archive 'CCDC 989935'
