#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:48:43 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178964 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/93/4119307.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_4119307
loop_
_publ_author_name
'Luke A. Wilkinson'
'Laura McNeill'
'Anthony J. H. M. Meijer'
'Nathan J. Patmore'
_publ_section_title
;
 Mixed Valency in Hydrogen Bonded 'Dimers of Dimers'
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1723
_journal_page_last               1726
_journal_paper_doi               10.1021/ja312176x
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C56 H84 Mo2 N2 O10 S2, 2(C2 H6 O S)'
_chemical_formula_sum            'C60 H96 Mo2 N2 O12 S4'
_chemical_formula_weight         1357.51
_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                96.497(2)
_cell_angle_beta                 107.341(2)
_cell_angle_gamma                103.535(2)
_cell_formula_units_Z            2
_cell_length_a                   13.5032(4)
_cell_length_b                   14.9415(5)
_cell_length_c                   17.9245(6)
_cell_measurement_reflns_used    6797
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      2.352
_cell_volume                     3290.33(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0628
_diffrn_reflns_av_sigmaI/netI    0.0789
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34287
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.12
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.566
_exptl_absorpt_correction_T_max  0.9508
_exptl_absorpt_correction_T_min  0.8266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       block
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.209
_refine_diff_density_min         -1.930
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         11518
_refine_ls_number_restraints     145
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1279
_refine_ls_R_factor_gt           0.0674
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0781P)²+21.0551P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1625
_refine_ls_wR_factor_ref         0.2072
_reflns_number_gt                7049
_reflns_number_total             11518
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja312176x_si_002_1.cif
_cod_data_source_block           2(DMSO)2.2DMSO
_cod_original_cell_volume        3290.33(18)
_cod_database_code               4119307
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
C1 C 0.2790(6) 0.3287(5) 0.1129(4) 0.0291(16) Uani 1 1 d . . .
C2 C 0.1847(6) 0.3400(5) 0.0480(4) 0.0304(16) Uani 1 1 d . A .
C3 C 0.1997(7) 0.3853(5) -0.0131(5) 0.0387(19) Uani 1 1 d . A .
C4 C 0.1078(8) 0.3890(6) -0.0733(5) 0.050(2) Uani 1 1 d . A .
H4 H 0.1172 0.4195 -0.1155 0.060 Uiso 1 1 calc R . .
C5 C 0.0043(8) 0.3503(7) -0.0742(5) 0.055(3) Uani 1 1 d . . .
C6 C -0.0087(7) 0.3044(6) -0.0137(5) 0.049(2) Uani 1 1 d . B .
H6 H -0.0798 0.2756 -0.0147 0.059 Uiso 1 1 calc R . .
C7 C 0.0788(6) 0.2990(5) 0.0485(5) 0.0396(19) Uani 1 1 d . . .
C8 C 0.3124(9) 0.4327(7) -0.0144(7) 0.067(2) Uani 1 1 d U . .
H8 H 0.3621 0.4414 0.0415 0.081 Uiso 0.549(10) 1 calc PR A 5
H8A H 0.3584 0.3920 0.0034 0.081 Uiso 0.451(10) 1 d PR A 6
C9 C 0.3497(16) 0.3706(14) -0.0635(12) 0.070(3) Uiso 0.549(10) 1 d PU A 5
H9A H 0.4226 0.4029 -0.0619 0.105 Uiso 0.549(10) 1 calc PR A 5
H9B H 0.3002 0.3548 -0.1187 0.105 Uiso 0.549(10) 1 calc PR A 5
H9C H 0.3509 0.3129 -0.0425 0.105 Uiso 0.549(10) 1 calc PR A 5
C10 C 0.3274(16) 0.5315(13) -0.0331(12) 0.071(3) Uiso 0.549(10) 1 d PU A 5
H10A H 0.3019 0.5695 0.0013 0.106 Uiso 0.549(10) 1 calc PR A 5
H10B H 0.2857 0.5274 -0.0891 0.106 Uiso 0.549(10) 1 calc PR A 5
H10C H 0.4042 0.5607 -0.0236 0.106 Uiso 0.549(10) 1 calc PR A 5
C9A C 0.3134(19) 0.4468(17) -0.0980(14) 0.069(3) Uiso 0.451(10) 1 d PU A 6
H9A1 H 0.2847 0.3858 -0.1347 0.103 Uiso 0.451(10) 1 calc PR A 6
H9A2 H 0.3877 0.4756 -0.0954 0.103 Uiso 0.451(10) 1 calc PR A 6
H9A3 H 0.2684 0.4878 -0.1171 0.103 Uiso 0.451(10) 1 calc PR A 6
C10A C 0.3553(19) 0.5155(16) 0.0390(15) 0.070(3) Uiso 0.451(10) 1 d PU A 6
H10D H 0.4281 0.5452 0.0389 0.105 Uiso 0.451(10) 1 calc PR A 6
H10E H 0.3593 0.5039 0.0924 0.105 Uiso 0.451(10) 1 calc PR A 6
H10F H 0.3094 0.5571 0.0242 0.105 Uiso 0.451(10) 1 calc PR A 6
C11 C -0.1050(14) 0.3515(12) -0.1333(8) 0.054(3) Uiso 0.625(14) 1 d PDU B 7
H11 H -0.1663 0.3163 -0.1181 0.065 Uiso 0.625(14) 1 calc PR B 7
C12 C -0.1169(13) 0.3109(11) -0.2175(8) 0.058(3) Uiso 0.625(14) 1 d PDU B 7
H12A H -0.1099 0.2469 -0.2204 0.087 Uiso 0.625(14) 1 calc PR B 7
H12B H -0.0604 0.3498 -0.2334 0.087 Uiso 0.625(14) 1 calc PR B 7
H12C H -0.1882 0.3095 -0.2535 0.087 Uiso 0.625(14) 1 calc PR B 7
C13 C -0.1048(14) 0.4538(11) -0.1310(10) 0.057(3) Uiso 0.625(14) 1 d PU B 7
H13A H -0.0973 0.4830 -0.0770 0.086 Uiso 0.625(14) 1 calc PR B 7
H13B H -0.1729 0.4569 -0.1687 0.086 Uiso 0.625(14) 1 calc PR B 7
H13C H -0.0441 0.4874 -0.1458 0.086 Uiso 0.625(14) 1 calc PR B 7
C11A C -0.0754(17) 0.3763(14) -0.1503(15) 0.043(6) Uiso 0.375(14) 1 d PD B 8
H11A H -0.0409 0.4046 -0.1876 0.052 Uiso 0.375(14) 1 calc PR B 8
C12A C -0.1661(18) 0.2867(15) -0.1862(16) 0.056(3) Uiso 0.375(14) 1 d PDU B 8
H12D H -0.1378 0.2373 -0.2055 0.084 Uiso 0.375(14) 1 calc PR B 8
H12E H -0.2221 0.2972 -0.2308 0.084 Uiso 0.375(14) 1 calc PR B 8
H12F H -0.1971 0.2672 -0.1457 0.084 Uiso 0.375(14) 1 calc PR B 8
C13A C -0.133(2) 0.4401(16) -0.1086(15) 0.043(6) Uiso 0.375(14) 1 d P B 8
H13D H -0.0811 0.5017 -0.0825 0.064 Uiso 0.375(14) 1 calc PR B 8
H13E H -0.1562 0.4093 -0.0689 0.064 Uiso 0.375(14) 1 calc PR B 8
H13F H -0.1955 0.4479 -0.1492 0.064 Uiso 0.375(14) 1 calc PR B 8
C14 C 0.0567(9) 0.2472(7) 0.1130(7) 0.071(2) Uani 1 1 d U B .
H14 H 0.1283 0.2450 0.1490 0.085 Uiso 1 1 calc R . .
C15 C -0.0110(9) 0.1502(7) 0.0836(7) 0.078(2) Uani 1 1 d U . .
H15A H 0.0219 0.1153 0.0529 0.117 Uiso 1 1 calc R B .
H15B H -0.0830 0.1494 0.0492 0.117 Uiso 1 1 calc R . .
H15C H -0.0174 0.1209 0.1288 0.117 Uiso 1 1 calc R . .
C16 C 0.0106(10) 0.3013(8) 0.1627(7) 0.085(3) Uani 1 1 d U . .
H16A H 0.0572 0.3660 0.1820 0.128 Uiso 1 1 calc R B .
H16B H 0.0064 0.2719 0.2082 0.128 Uiso 1 1 calc R . .
H16C H -0.0620 0.3015 0.1304 0.128 Uiso 1 1 calc R . .
C17 C 0.5800(6) 0.4358(5) 0.2620(4) 0.0301(16) Uani 1 1 d . . .
C18 C 0.6610(7) 0.5296(5) 0.2807(5) 0.0399(19) Uani 1 1 d . . .
C19 C 0.7724(7) 0.5366(6) 0.3073(5) 0.044(2) Uani 1 1 d . . .
C20 C 0.8442(8) 0.6248(7) 0.3234(6) 0.065(3) Uani 1 1 d . . .
H20 H 0.9196 0.6308 0.3413 0.078 Uiso 1 1 calc R . .
C21 C 0.8106(11) 0.7050(7) 0.3146(7) 0.074(3) Uani 1 1 d . . .
C22 C 0.7016(10) 0.6958(7) 0.2901(6) 0.069(3) Uani 1 1 d . . .
H22 H 0.6776 0.7504 0.2850 0.083 Uiso 1 1 calc R . .
C23 C 0.6264(8) 0.6102(6) 0.2726(5) 0.051(2) Uani 1 1 d . . .
C24 C 0.8147(8) 0.4512(7) 0.3191(6) 0.0598(19) Uani 1 1 d U . .
H24 H 0.7510 0.3977 0.3140 0.072 Uiso 1 1 calc R . .
C25 C 0.8590(9) 0.4232(8) 0.2559(6) 0.070(2) Uani 1 1 d U . .
H25A H 0.8841 0.3677 0.2656 0.106 Uiso 1 1 calc R . .
H25B H 0.9198 0.4749 0.2571 0.106 Uiso 1 1 calc R . .
H25C H 0.8024 0.4084 0.2036 0.106 Uiso 1 1 calc R . .
C26 C 0.8954(8) 0.4634(8) 0.4017(6) 0.067(2) Uani 1 1 d U . .
H26A H 0.9195 0.4066 0.4063 0.101 Uiso 1 1 calc R . .
H26B H 0.8611 0.4739 0.4417 0.101 Uiso 1 1 calc R . .
H26C H 0.9577 0.5174 0.4105 0.101 Uiso 1 1 calc R . .
C27 C 0.8927(16) 0.7996(11) 0.3303(11) 0.145(4) Uani 1 1 d U . .
H27 H 0.8459 0.8420 0.3152 0.174 Uiso 1 1 calc R . .
C28 C 0.9555(14) 0.8130(10) 0.2822(11) 0.148(5) Uani 1 1 d U . .
H28A H 0.9098 0.7884 0.2264 0.221 Uiso 1 1 calc R . .
H28B H 1.0111 0.7800 0.2967 0.221 Uiso 1 1 calc R . .
H28C H 0.9902 0.8803 0.2894 0.221 Uiso 1 1 calc R . .
C29 C 0.9490(15) 0.8366(11) 0.4171(11) 0.150(5) Uani 1 1 d U . .
H29A H 0.8963 0.8257 0.4451 0.226 Uiso 1 1 calc R . .
H29B H 0.9836 0.9042 0.4262 0.226 Uiso 1 1 calc R . .
H29C H 1.0040 0.8044 0.4373 0.226 Uiso 1 1 calc R . .
C30 C 0.5061(9) 0.6045(8) 0.2443(6) 0.069(2) Uani 1 1 d U . .
H30 H 0.4654 0.5385 0.2156 0.083 Uiso 1 1 calc R . .
C31 C 0.4674(9) 0.6253(7) 0.3142(6) 0.070(2) Uani 1 1 d U . .
H31A H 0.3901 0.6208 0.2941 0.105 Uiso 1 1 calc R . .
H31B H 0.5079 0.6888 0.3447 0.105 Uiso 1 1 calc R . .
H31C H 0.4792 0.5797 0.3487 0.105 Uiso 1 1 calc R . .
C32 C 0.4765(10) 0.6705(8) 0.1850(7) 0.078(2) Uani 1 1 d U . .
H32A H 0.3985 0.6630 0.1684 0.117 Uiso 1 1 calc R . .
H32B H 0.4966 0.6542 0.1381 0.117 Uiso 1 1 calc R . .
H32C H 0.5158 0.7359 0.2112 0.117 Uiso 1 1 calc R . .
C33 C 0.5417(6) 0.1891(5) 0.3336(5) 0.0352(18) Uani 1 1 d . . .
C34 C 0.5921(7) 0.1308(6) 0.3874(5) 0.0381(18) Uani 1 1 d . . .
C35 C 0.5614(7) 0.0321(6) 0.3622(5) 0.043(2) Uani 1 1 d . . .
C36 C 0.6096(7) -0.0205(6) 0.4128(5) 0.047(2) Uani 1 1 d . . .
H36 H 0.5890 -0.0868 0.3961 0.056 Uiso 1 1 calc R . .
C37 C 0.6862(7) 0.0198(6) 0.4864(6) 0.049(2) Uani 1 1 d . C .
C38 C 0.7146(7) 0.1160(6) 0.5104(5) 0.045(2) Uani 1 1 d . . .
H38 H 0.7668 0.1443 0.5615 0.054 Uiso 1 1 calc R . .
C39 C 0.6696(7) 0.1728(6) 0.4628(5) 0.0394(19) Uani 1 1 d . . .
C40 C 0.4772(7) -0.0195(6) 0.2811(5) 0.049(2) Uani 1 1 d . . .
H40 H 0.4326 0.0233 0.2613 0.059 Uiso 1 1 calc R . .
C41 C 0.5340(8) -0.0380(7) 0.2216(6) 0.060(3) Uani 1 1 d . . .
H41A H 0.5823 0.0212 0.2197 0.089 Uiso 1 1 calc R . .
H41B H 0.4799 -0.0653 0.1686 0.089 Uiso 1 1 calc R . .
H41C H 0.5762 -0.0818 0.2383 0.089 Uiso 1 1 calc R . .
C42 C 0.4006(8) -0.1100(7) 0.2844(6) 0.064(3) Uani 1 1 d . . .
H42A H 0.3638 -0.0967 0.3222 0.097 Uiso 1 1 calc R . .
H42B H 0.4417 -0.1544 0.3019 0.097 Uiso 1 1 calc R . .
H42C H 0.3469 -0.1375 0.2314 0.097 Uiso 1 1 calc R . .
C43 C 0.7393(8) -0.0408(7) 0.5413(6) 0.058(3) Uani 1 1 d . . .
H43 H 0.8185 -0.0215 0.5495 0.070 Uiso 0.477(15) 1 calc PR C 9
H43A H 0.7915 0.0038 0.5907 0.070 Uiso 0.523(15) 1 d PR C 10
C44 C 0.7278(16) -0.0274(14) 0.6151(12) 0.054(6) Uiso 0.477(15) 1 d P C 9
H44A H 0.7586 -0.0701 0.6463 0.081 Uiso 0.477(15) 1 calc PR C 9
H44B H 0.6508 -0.0401 0.6088 0.081 Uiso 0.477(15) 1 calc PR C 9
H44C H 0.7657 0.0377 0.6429 0.081 Uiso 0.477(15) 1 calc PR C 9
C45 C 0.6942(17) -0.1496(14) 0.5030(12) 0.059(6) Uiso 0.477(15) 1 d P C 9
H45A H 0.7400 -0.1836 0.5344 0.089 Uiso 0.477(15) 1 calc PR C 9
H45B H 0.6948 -0.1593 0.4482 0.089 Uiso 0.477(15) 1 calc PR C 9
H45C H 0.6201 -0.1732 0.5028 0.089 Uiso 0.477(15) 1 calc PR C 9
C44A C 0.6579(17) -0.0998(14) 0.5646(13) 0.070(6) Uiso 0.523(15) 1 d P C 10
H44D H 0.6913 -0.1361 0.6019 0.105 Uiso 0.523(15) 1 calc PR C 10
H44E H 0.6030 -0.1429 0.5173 0.105 Uiso 0.523(15) 1 calc PR C 10
H44F H 0.6237 -0.0608 0.5905 0.105 Uiso 0.523(15) 1 calc PR C 10
C45A C 0.800(2) -0.0893(18) 0.5043(16) 0.098(9) Uiso 0.523(15) 1 d P C 10
H45D H 0.8465 -0.1149 0.5443 0.147 Uiso 0.523(15) 1 calc PR C 10
H45E H 0.8447 -0.0450 0.4829 0.147 Uiso 0.523(15) 1 calc PR C 10
H45F H 0.7495 -0.1406 0.4610 0.147 Uiso 0.523(15) 1 calc PR C 10
C46 C 0.7026(6) 0.2783(6) 0.4939(5) 0.0398(19) Uani 1 1 d . . .
H46 H 0.6845 0.3088 0.4466 0.048 Uiso 1 1 calc R . .
C47 C 0.8239(7) 0.3205(6) 0.5397(5) 0.053(2) Uani 1 1 d . . .
H47A H 0.8652 0.3055 0.5058 0.079 Uiso 1 1 calc R . .
H47B H 0.8438 0.2942 0.5879 0.079 Uiso 1 1 calc R . .
H47C H 0.8401 0.3888 0.5547 0.079 Uiso 1 1 calc R . .
C48 C 0.6373(7) 0.3019(6) 0.5447(5) 0.050(2) Uani 1 1 d . . .
H48A H 0.6585 0.3700 0.5636 0.075 Uiso 1 1 calc R . .
H48B H 0.6508 0.2708 0.5905 0.075 Uiso 1 1 calc R . .
H48C H 0.5602 0.2802 0.5129 0.075 Uiso 1 1 calc R . .
C49 C 0.2546(6) 0.1044(5) 0.1954(5) 0.0360(18) Uani 1 1 d . . .
C50 C 0.1723(7) 0.0165(6) 0.1814(5) 0.045(2) Uani 1 1 d . . .
H50 H 0.1191 0.0129 0.2065 0.054 Uiso 1 1 calc R . .
C51 C 0.1706(7) -0.0589(6) 0.1338(6) 0.052(2) Uani 1 1 d . . .
H51 H 0.1159 -0.1160 0.1246 0.062 Uiso 1 1 calc R . .
C52 C 0.2516(6) -0.0546(6) 0.0956(5) 0.046(2) Uani 1 1 d . . .
C53 C 0.6915(9) 0.1516(13) 0.1220(8) 0.089(5) Uani 0.753(17) 1 d PDU D 3
H53A H 0.6853 0.0969 0.1476 0.134 Uiso 0.753(17) 1 calc PR D 3
H53B H 0.6989 0.2074 0.1599 0.134 Uiso 0.753(17) 1 calc PR D 3
H53C H 0.7553 0.1611 0.1051 0.134 Uiso 0.753(17) 1 calc PR D 3
C54 C 0.6177(16) 0.2419(8) 0.0141(11) 0.080(5) Uani 0.753(17) 1 d PDU D 3
H54A H 0.5629 0.2471 -0.0341 0.120 Uiso 0.753(17) 1 calc PR D 3
H54B H 0.6864 0.2479 0.0045 0.120 Uiso 0.753(17) 1 calc PR D 3
H54C H 0.6273 0.2919 0.0582 0.120 Uiso 0.753(17) 1 calc PR D 3
C53A C 0.687(3) 0.221(3) 0.105(2) 0.090(6) Uani 0.247(17) 1 d PDU D 4
H53D H 0.7203 0.1970 0.1517 0.134 Uiso 0.247(17) 1 calc PR D 4
H53E H 0.6626 0.2746 0.1214 0.134 Uiso 0.247(17) 1 calc PR D 4
H53F H 0.7396 0.2413 0.0783 0.134 Uiso 0.247(17) 1 calc PR D 4
C54A C 0.555(5) 0.209(3) -0.028(3) 0.080(6) Uani 0.247(17) 1 d PDU D 4
H54D H 0.4916 0.1771 -0.0752 0.120 Uiso 0.247(17) 1 calc PR D 4
H54E H 0.6188 0.2282 -0.0437 0.120 Uiso 0.247(17) 1 calc PR D 4
H54F H 0.5422 0.2646 -0.0018 0.120 Uiso 0.247(17) 1 calc PR D 4
N1 N 0.3259(5) 0.1132(4) 0.1574(3) 0.0313(14) Uani 1 1 d . . .
N2 N 0.3196(5) 0.0333(5) 0.1082(4) 0.0414(16) Uani 1 1 d . . .
H2 H 0.3649 0.0395 0.0813 0.050 Uiso 1 1 calc R . .
O1 O 0.2879(4) 0.3523(3) 0.1854(3) 0.0281(11) Uani 1 1 d . . .
O2 O 0.3438(4) 0.2901(3) 0.0928(3) 0.0290(11) Uani 1 1 d . . .
O3 O 0.5162(4) 0.4239(3) 0.3029(3) 0.0299(11) Uani 1 1 d . . .
O4 O 0.5737(4) 0.3716(3) 0.2073(3) 0.0305(11) Uani 1 1 d . . .
O5 O 0.4845(4) 0.2359(4) 0.3565(3) 0.0378(13) Uani 1 1 d . . .
O6 O 0.5525(4) 0.1857(3) 0.2658(3) 0.0314(11) Uani 1 1 d . . .
O7 O 0.2618(4) 0.1763(4) 0.2467(3) 0.0391(13) Uani 1 1 d . . .
O8 O 0.2602(5) -0.1217(4) 0.0524(4) 0.0594(18) Uani 1 1 d . . .
O9 O 0.4881(5) 0.1371(4) 0.0735(4) 0.0585(17) Uani 1 1 d . D .
S1 S 0.5754(2) 0.13243(17) 0.03865(15) 0.0548(6) Uani 1 1 d D . .
S2 S 0.2360(4) 0.3393(3) 0.3904(3) 0.0553(13) Uani 0.50 1 d PDU E 1
O10 O 0.3447(7) 0.3768(8) 0.3815(6) 0.041(3) Uiso 0.50 1 d PD E 1
C55 C 0.1615(15) 0.420(2) 0.3515(17) 0.112(9) Uiso 0.50 1 d PD E 1
H55A H 0.1432 0.4094 0.2934 0.168 Uiso 0.50 1 calc PR E 1
H55B H 0.2060 0.4844 0.3751 0.168 Uiso 0.50 1 calc PR E 1
H55C H 0.0950 0.4085 0.3649 0.168 Uiso 0.50 1 calc PR E 1
C56 C 0.2789(19) 0.3558(17) 0.5034(10) 0.079(5) Uiso 0.50 1 d PDU E 1
H56A H 0.3121 0.3066 0.5209 0.119 Uiso 0.50 1 calc PR E 1
H56B H 0.2154 0.3517 0.5200 0.119 Uiso 0.50 1 calc PR E 1
H56C H 0.3314 0.4175 0.5276 0.119 Uiso 0.50 1 calc PR E 1
S2A S 0.3101(5) 0.4264(4) 0.4227(4) 0.047(2) Uani 0.347(7) 1 d PDU E 2
O10A O 0.3020(10) 0.3397(7) 0.3668(7) 0.065(4) Uiso 0.50 1 d PD E 2
C55A C 0.4439(12) 0.4707(11) 0.4843(10) 0.082(7) Uiso 0.50 1 d PD . 2
H55D H 0.4682 0.4187 0.5017 0.124 Uiso 0.50 1 d PR . 2
H55E H 0.4520 0.5158 0.5298 0.124 Uiso 0.50 1 d PR . 2
H55F H 0.4862 0.4996 0.4543 0.124 Uiso 0.50 1 d PR . 2
C56A C 0.2438(16) 0.3908(12) 0.4881(10) 0.067(5) Uiso 0.50 1 d PDU E 2
H56D H 0.1659 0.3664 0.4591 0.101 Uiso 0.50 1 calc PR E 2
H56E H 0.2573 0.4445 0.5303 0.101 Uiso 0.50 1 calc PR E 2
H56F H 0.2707 0.3415 0.5118 0.101 Uiso 0.50 1 calc PR E 2
S3 S -0.0643(3) 0.1848(3) 0.3313(2) 0.0979(11) Uiso 1 1 d D . .
O11 O -0.0075(9) 0.2577(8) 0.4033(7) 0.139(4) Uiso 1 1 d . F .
C57 C 0.064(3) 0.178(6) 0.326(4) 0.12(3) Uiso 0.28(4) 1 d PD F 15
H57A H 0.1145 0.2414 0.3408 0.183 Uiso 0.28(4) 1 calc PR F 15
H57B H 0.0559 0.1492 0.2722 0.183 Uiso 0.28(4) 1 calc PR F 15
H57C H 0.0934 0.1398 0.3637 0.183 Uiso 0.28(4) 1 calc PR F 15
C58 C -0.125(4) 0.089(2) 0.370(3) 0.056(13) Uiso 0.28(4) 1 d PD F 15
H58A H -0.0686 0.0738 0.4111 0.084 Uiso 0.28(4) 1 calc PR F 15
H58B H -0.1635 0.0343 0.3269 0.084 Uiso 0.28(4) 1 calc PR F 15
H58C H -0.1762 0.1073 0.3935 0.084 Uiso 0.28(4) 1 calc PR F 15
C57A C 0.019(2) 0.1127(19) 0.3152(14) 0.113(10) Uiso 0.72(4) 1 d PD F 16
H57D H 0.0799 0.1501 0.3024 0.169 Uiso 0.72(4) 1 calc PR F 16
H57E H -0.0234 0.0599 0.2708 0.169 Uiso 0.72(4) 1 calc PR F 16
H57F H 0.0473 0.0888 0.3636 0.169 Uiso 0.72(4) 1 calc PR F 16
C58A C -0.165(2) 0.0956(14) 0.3482(18) 0.115(9) Uiso 0.72(4) 1 d PD F 16
H58D H -0.1303 0.0656 0.3905 0.172 Uiso 0.72(4) 1 calc PR F 16
H58E H -0.2045 0.0484 0.2991 0.172 Uiso 0.72(4) 1 calc PR F 16
H58F H -0.2159 0.1240 0.3644 0.172 Uiso 0.72(4) 1 calc PR F 16
S4 S 0.2380(4) 0.0630(3) 0.9050(3) 0.088(2) Uani 0.710(10) 1 d PDU G 11
S4A S 0.1874(14) 0.1025(10) 0.8535(9) 0.121(6) Uani 0.290(10) 1 d PDU G 12
O12 O 0.1666(12) 0.0136(11) 0.8201(9) 0.179(5) Uiso 1 1 d D . .
C59 C 0.3157(17) 0.1763(15) 0.8991(13) 0.182(9) Uiso 1 1 d . . .
H59A H 0.3728 0.1685 0.8778 0.273 Uiso 0.710(10) 1 calc PR G 11
H59B H 0.3484 0.2162 0.9524 0.273 Uiso 0.710(10) 1 calc PR G 11
H59C H 0.2681 0.2058 0.8638 0.273 Uiso 0.710(10) 1 calc PR G 11
H59D H 0.3504 0.1795 0.8582 0.273 Uiso 0.290(10) 1 d PR G 12
H59E H 0.3527 0.1461 0.9403 0.273 Uiso 0.290(10) 1 d PR G 12
H59F H 0.3200 0.2399 0.9232 0.273 Uiso 0.290(10) 1 d PR G 12
C60 C 0.1493(11) 0.1104(9) 0.9452(8) 0.097(4) Uiso 1 1 d . . .
H60A H 0.0966 0.0591 0.9542 0.146 Uiso 0.710(10) 1 calc PR G 11
H60B H 0.1111 0.1437 0.9074 0.146 Uiso 0.710(10) 1 calc PR G 11
H60C H 0.1919 0.1542 0.9958 0.146 Uiso 0.710(10) 1 calc PR G 11
H60D H 0.0757 0.0692 0.9315 0.146 Uiso 0.290(10) 1 d PR G 12
H60E H 0.1525 0.1739 0.9687 0.146 Uiso 0.290(10) 1 d PR G 12
H60F H 0.1999 0.0865 0.9837 0.146 Uiso 0.290(10) 1 d PR G 12
Mo1 Mo 0.39141(5) 0.29693(5) 0.27042(4) 0.03065(19) Uani 1 1 d . . .
Mo2 Mo 0.45023(5) 0.24410(4) 0.18312(4) 0.02958(19) Uani 1 1 d . E .
S2B S 0.3449(9) 0.3640(9) 0.4566(6) 0.063(6) Uiso 0.153(7) 1 d PDU E 13
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'
S S 0.1246 0.1234 '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
O2 C1 O1 121.9(6) .
O2 C1 C2 118.2(6) .
O1 C1 C2 119.7(6) .
C3 C2 C7 120.4(7) .
C3 C2 C1 121.3(7) .
C7 C2 C1 118.2(7) .
C2 C3 C4 118.0(8) .
C2 C3 C8 122.0(7) .
C4 C3 C8 120.0(8) .
C5 C4 C3 122.8(9) .
C4 C5 C6 118.2(8) .
C4 C5 C11 129.6(11) .
C6 C5 C11 112.1(10) .
C4 C5 C11A 106.2(12) .
C6 C5 C11A 135.6(12) .
C5 C6 C7 122.1(9) .
C6 C7 C2 118.4(8) .
C6 C7 C14 118.5(8) .
C2 C7 C14 123.1(8) .
C10A C8 C9 137.7(16) .
C10A C8 C3 109.6(13) .
C9 C8 C3 112.0(11) .
C10A C8 C10 53.1(12) .
C9 C8 C10 113.0(13) .
C3 C8 C10 114.9(11) .
C10A C8 C9A 111.2(15) .
C9 C8 C9A 58.2(12) .
C3 C8 C9A 113.2(12) .
C10 C8 C9A 60.8(12) .
C12 C11 C13 106.8(14) .
C12 C11 C5 110.9(12) .
C13 C11 C5 107.6(13) .
C12A C11A C13A 101.2(19) .
C12A C11A C5 103.4(17) .
C13A C11A C5 101.9(17) .
C15 C14 C16 110.7(9) .
C15 C14 C7 114.6(9) .
C16 C14 C7 110.5(9) .
O4 C17 O3 121.5(7) .
O4 C17 C18 121.1(6) .
O3 C17 C18 117.4(6) .
C23 C18 C19 120.2(8) .
C23 C18 C17 120.0(8) .
C19 C18 C17 119.8(7) .
C20 C19 C18 117.7(8) .
C20 C19 C24 120.0(9) .
C18 C19 C24 122.3(8) .
C19 C20 C21 122.5(10) .
C22 C21 C20 118.2(9) .
C22 C21 C27 121.4(13) .
C20 C21 C27 120.3(14) .
C23 C22 C21 122.0(10) .
C22 C23 C18 119.4(10) .
C22 C23 C30 119.4(9) .
C18 C23 C30 121.1(8) .
C25 C24 C26 111.3(8) .
C25 C24 C19 112.5(8) .
C26 C24 C19 112.8(8) .
C28 C27 C29 116.5(17) .
C28 C27 C21 118.5(15) .
C29 C27 C21 111.4(13) .
C31 C30 C23 111.4(9) .
C31 C30 C32 109.3(7) .
C23 C30 C32 113.3(9) .
O6 C33 O5 123.1(7) .
O6 C33 C34 118.5(6) .
O5 C33 C34 118.3(7) .
C39 C34 C35 119.7(7) .
C39 C34 C33 120.7(7) .
C35 C34 C33 119.6(7) .
C36 C35 C34 118.6(8) .
C36 C35 C40 118.3(7) .
C34 C35 C40 123.1(7) .
C37 C36 C35 122.3(8) .
C36 C37 C38 118.4(8) .
C36 C37 C43 121.0(8) .
C38 C37 C43 120.6(8) .
C37 C38 C39 122.3(8) .
C38 C39 C34 118.7(8) .
C38 C39 C46 119.6(7) .
C34 C39 C46 121.7(7) .
C42 C40 C41 110.5(8) .
C42 C40 C35 113.8(8) .
C41 C40 C35 109.7(7) .
C44 C43 C44A 54.7(11) .
C44 C43 C45A 136.0(15) .
C44A C43 C45A 115.6(15) .
C44 C43 C37 112.6(11) .
C44A C43 C37 108.7(11) .
C45A C43 C37 110.9(13) .
C44 C43 C45 108.7(13) .
C44A C43 C45 60.3(11) .
C45A C43 C45 58.4(12) .
C37 C43 C45 112.6(10) .
C48 C46 C39 110.4(7) .
C48 C46 C47 110.4(7) .
C39 C46 C47 113.8(7) .
O7 C49 N1 118.1(7) .
O7 C49 C50 120.8(7) .
N1 C49 C50 121.1(7) .
C51 C50 C49 120.5(8) .
C50 C51 C52 120.4(8) .
O8 C52 N2 120.4(7) .
O8 C52 C51 125.7(8) .
N2 C52 C51 113.8(7) .
C49 N1 N2 115.7(6) .
C49 N1 Mo2 119.8(5) .
N2 N1 Mo2 124.3(5) .
C52 N2 N1 128.1(7) .
C1 O1 Mo1 117.1(4) .
C1 O2 Mo2 116.9(4) .
C17 O3 Mo1 118.1(4) .
C17 O4 Mo2 117.3(5) .
C33 O5 Mo1 116.9(5) .
C33 O6 Mo2 116.2(4) .
C49 O7 Mo1 118.2(5) .
O9 S1 C53 104.1(6) .
O9 S1 C54 106.9(6) .
C53 S1 C54 94.6(9) .
O9 S1 C54A 99.9(18) .
C53 S1 C54A 125(2) .
O9 S1 C53A 102.4(16) .
C54 S1 C53A 58.7(17) .
C54A S1 C53A 90(2) .
O10 S2 C55 103.8(9) .
O10 S2 C56 99.6(8) .
C55 S2 C56 112.8(12) .
S2 O10 Mo1 120.2(6) .
O10A S2A C56A 107.6(5) .
O10A S2A C55A 107.5(5) .
C56A S2A C55A 102.9(10) .
S2A O10A Mo1 137.2(7) .
C55A C55A S2A 160(2) 2_666
O11 S3 C58A 110.2(10) .
O11 S3 C57 89(2) .
C58A S3 C57 127(2) .
O11 S3 C58 101.9(15) .
C57 S3 C58 111(3) .
O11 S3 C57A 111.2(10) .
C58A S3 C57A 97.3(11) .
C58 S3 C57A 84.4(16) .
O12 S4 C60 104.0(8) .
O12 S4 C59 107.1(9) .
C60 S4 C59 94.0(8) .
O12 S4A C59 123.6(15) .
O12 S4A C60 110.1(13) .
C59 S4A C60 94.9(10) .
S4A O12 S4 52.2(8) .
O7 Mo1 O3 174.31(18) .
O7 Mo1 Mo2 94.69(14) .
O3 Mo1 Mo2 91.00(12) .
O7 Mo1 O5 87.7(2) .
O3 Mo1 O5 92.26(19) .
Mo2 Mo1 O5 91.24(13) .
O7 Mo1 O1 88.60(19) .
O3 Mo1 O1 91.24(18) .
Mo2 Mo1 O1 90.90(12) .
O5 Mo1 O1 175.87(19) .
O7 Mo1 O10A 77.7(3) .
O3 Mo1 O10A 96.6(3) .
Mo2 Mo1 O10A 172.4(2) .
O5 Mo1 O10A 89.0(3) .
O1 Mo1 O10A 88.4(3) .
O7 Mo1 O10 92.7(3) .
O3 Mo1 O10 81.6(3) .
Mo2 Mo1 O10 172.4(2) .
O5 Mo1 O10 87.3(3) .
O1 Mo1 O10 91.0(3) .
Mo1 Mo2 O2 91.89(12) .
Mo1 Mo2 O4 91.90(12) .
O2 Mo2 O4 91.42(18) .
Mo1 Mo2 O6 91.98(12) .
O2 Mo2 O6 174.51(18) .
O4 Mo2 O6 92.35(19) .
Mo1 Mo2 N1 89.03(16) .
O2 Mo2 N1 88.8(2) .
O4 Mo2 N1 179.0(2) .
O6 Mo2 N1 87.4(2) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O2 1.268(8) .
C1 O1 1.269(8) .
C1 C2 1.505(10) .
C2 C3 1.391(10) .
C2 C7 1.420(11) .
C3 C4 1.398(11) .
C3 C8 1.529(13) .
C4 C5 1.377(13) .
C5 C6 1.377(13) .
C5 C11 1.545(18) .
C5 C11A 1.62(3) .
C6 C7 1.387(11) .
C7 C14 1.525(13) .
C8 C10A 1.36(2) .
C8 C9 1.48(2) .
C8 C10 1.53(2) .
C8 C9A 1.54(2) .
C11 C12 1.509(14) .
C11 C13 1.52(2) .
C11A C12A 1.509(14) .
C11A C13A 1.61(3) .
C14 C15 1.461(14) .
C14 C16 1.496(14) .
C17 O4 1.262(8) .
C17 O3 1.283(8) .
C17 C18 1.493(11) .
C18 C23 1.398(11) .
C18 C19 1.410(11) .
C19 C20 1.382(12) .
C19 C24 1.525(12) .
C20 C21 1.387(15) .
C21 C22 1.372(16) .
C21 C27 1.516(16) .
C22 C23 1.370(13) .
C23 C30 1.529(14) .
C24 C25 1.495(13) .
C24 C26 1.515(13) .
C27 C28 1.38(2) .
C27 C29 1.49(2) .
C30 C31 1.523(12) .
C30 C32 1.559(13) .
C33 O6 1.263(8) .
C33 O5 1.277(8) .
C33 C34 1.494(10) .
C34 C39 1.404(11) .
C34 C35 1.415(11) .
C35 C36 1.383(11) .
C35 C40 1.533(12) .
C36 C37 1.375(12) .
C37 C38 1.379(12) .
C37 C43 1.545(11) .
C38 C39 1.384(11) .
C39 C46 1.523(11) .
C40 C42 1.518(12) .
C40 C41 1.524(12) .
C43 C44 1.38(2) .
C43 C44A 1.44(2) .
C43 C45A 1.46(3) .
C43 C45 1.59(2) .
C46 C48 1.511(11) .
C46 C47 1.533(11) .
C49 O7 1.297(9) .
C49 N1 1.327(9) .
C49 C50 1.448(11) .
C50 C51 1.326(11) .
C51 C52 1.446(11) .
C52 O8 1.245(9) .
C52 N2 1.366(10) .
C53 S1 1.752(10) .
C54 S1 1.752(9) .
C53A S1 1.752(10) .
C54A S1 1.752(10) .
N1 N2 1.371(8) .
N1 Mo2 2.157(6) .
O1 Mo1 2.126(5) .
O2 Mo2 2.117(5) .
O3 Mo1 2.109(5) .
O4 Mo2 2.120(5) .
O5 Mo1 2.119(5) .
O6 Mo2 2.122(5) .
O7 Mo1 2.098(5) .
O9 S1 1.501(6) .
S2 O10 1.506(8) .
S2 C55 1.81(2) .
S2 C56 1.903(17) .
O10 Mo1 2.520(10) .
S2A O10A 1.505(8) .
S2A C56A 1.733(11) .
S2A C55A 1.734(11) .
O10A Mo1 2.492(10) .
C55A C55A 1.46(3) 2_666
S3 O11 1.463(12) .
S3 C58A 1.792(11) .
S3 C57 1.792(11) .
S3 C58 1.792(11) .
S3 C57A 1.793(11) .
S4 O12 1.526(15) .
S4 C60 1.804(13) .
S4 C59 1.80(2) .
S4A O12 1.322(16) .
S4A C59 1.72(2) .
S4A C60 1.86(2) .
Mo1 Mo2 2.1114(8) .
