Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'R. Hernandez-Molina' 'M. R. J. Elsegood' 'W. Clegg' 'A. G. Sykes' _publ_contact_author_name 'Prof A Sykes' _publ_contact_author_address ; Prof A Sykes Department of Chemistry City University of Hong Kong HONG KONG ; data_ags36 _database_code_CSD 158608 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H66 Mo3 O31 S4 Se4' _chemical_formula_weight 1630.71 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' '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8860(19) _cell_length_b 13.8899(19) _cell_length_c 17.180(2) _cell_angle_alpha 99.535(2) _cell_angle_beta 102.458(2) _cell_angle_gamma 117.597(2) _cell_volume 2729.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 4935 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 27.78 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.984 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 3.587 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.413 _exptl_absorpt_correction_T_max 0.841 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17886 _diffrn_reflns_av_R_equivalents 0.0759 _diffrn_reflns_av_sigmaI/netI 0.2116 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9356 _reflns_number_gt 4724 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0765P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9356 _refine_ls_number_parameters 747 _refine_ls_number_restraints 614 _refine_ls_R_factor_all 0.1438 _refine_ls_R_factor_gt 0.0707 _refine_ls_wR_factor_ref 0.1776 _refine_ls_wR_factor_gt 0.1599 _refine_ls_goodness_of_fit_ref 0.926 _refine_ls_restrained_S_all 0.898 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.58289(10) 0.31329(9) 0.54972(8) 0.0122(3) Uani 1 1 d U . . Mo2 Mo 0.35657(10) 0.12649(9) 0.49745(8) 0.0125(3) Uani 1 1 d U . . Mo3 Mo 0.48359(10) 0.15834(9) 0.38910(8) 0.0122(3) Uani 1 1 d U . . Se1 Se 0.66791(12) 0.22071(11) 0.48657(9) 0.0151(3) Uani 1 1 d U . . Se2 Se 0.50576(12) 0.18482(11) 0.62640(9) 0.0155(3) Uani 1 1 d U . . Se3 Se 0.39499(12) -0.01138(11) 0.42965(9) 0.0147(3) Uani 1 1 d U . . Se4 Se 0.41761(12) 0.28517(11) 0.43793(9) 0.0133(3) Uani 1 1 d U . . O1 O 0.7423(7) 0.3992(7) 0.6574(6) 0.0194(15) Uani 1 1 d U . . O2 O 0.6921(8) 0.4687(7) 0.5146(6) 0.0207(17) Uani 1 1 d U . . O3 O 0.5685(8) 0.4472(7) 0.6234(5) 0.0167(14) Uani 1 1 d U . . O4 O 0.2448(8) -0.0027(7) 0.5449(6) 0.0213(17) Uani 1 1 d U . . O5 O 0.1907(7) 0.0382(7) 0.3985(6) 0.0185(15) Uani 1 1 d U . . O6 O 0.2735(8) 0.2070(7) 0.5509(6) 0.0229(18) Uani 1 1 d U . . O7 O 0.5541(8) 0.2811(7) 0.3234(6) 0.0187(16) Uani 1 1 d U . . O8 O 0.5260(8) 0.0653(7) 0.3003(6) 0.0179(16) Uani 1 1 d U . . O9 O 0.3359(8) 0.0815(7) 0.2736(6) 0.0198(16) Uani 1 1 d U . . S1 S 0.2874(3) 0.2873(3) 0.2083(2) 0.0203(9) Uani 1 1 d . A . O10 O 0.2309(8) 0.1941(7) 0.2424(6) 0.023(2) Uani 1 1 d . . . O11 O 0.2702(9) 0.3825(8) 0.2395(6) 0.029(3) Uani 1 1 d . . . O12 O 0.4056(8) 0.3240(8) 0.2202(6) 0.026(2) Uani 1 1 d . . . C1 C 0.2134(12) 0.2338(11) 0.0999(9) 0.020(3) Uani 1 1 d U . . C2 C 0.263(3) 0.281(3) 0.0427(19) 0.019(4) Uani 0.493(16) 1 d PU A 1 H2 H 0.3406 0.3423 0.0607 0.023 Uiso 0.493(16) 1 calc PR A 1 C3 C 0.199(3) 0.239(3) -0.036(2) 0.029(6) Uani 0.493(16) 1 d PU A 1 H3 H 0.2319 0.2765 -0.0732 0.035 Uiso 0.493(16) 1 calc PR A 1 C4 C 0.0872(13) 0.1442(12) -0.0722(10) 0.026(3) Uani 1 1 d U . . C5 C 0.040(3) 0.092(3) -0.0169(19) 0.026(6) Uani 0.493(16) 1 d PU A 1 H5 H -0.0359 0.0264 -0.0377 0.031 Uiso 0.493(16) 1 calc PR A 1 C6 C 0.100(2) 0.134(3) 0.0686(19) 0.022(5) Uani 0.493(16) 1 d PU A 1 H6 H 0.0672 0.0976 0.1058 0.027 Uiso 0.493(16) 1 calc PR A 1 C7 C 0.0214(14) 0.0979(13) -0.1632(9) 0.036(4) Uani 1 1 d U A . H7A H 0.0695 0.1423 -0.1931 0.054 Uiso 1 1 calc R . . H7B H -0.0481 0.1030 -0.1731 0.054 Uiso 1 1 calc R . . H7C H -0.0008 0.0179 -0.1837 0.054 Uiso 1 1 calc R . . C2X C 0.261(3) 0.220(3) 0.0442(19) 0.026(5) Uani 0.507(16) 1 d PU A 2 H2X H 0.3397 0.2413 0.0624 0.031 Uiso 0.507(16) 1 calc PR A 2 C3X C 0.198(3) 0.176(3) -0.042(2) 0.027(5) Uani 0.507(16) 1 d PU A 2 H3X H 0.2364 0.1684 -0.0799 0.032 Uiso 0.507(16) 1 calc PR A 2 C5X C 0.041(2) 0.176(2) -0.0132(17) 0.021(5) Uani 0.507(16) 1 d PU A 2 H5X H -0.0312 0.1718 -0.0322 0.025 Uiso 0.507(16) 1 calc PR A 2 C6X C 0.100(2) 0.214(3) 0.0711(19) 0.027(5) Uani 0.507(16) 1 d PU A 2 H6X H 0.0653 0.2264 0.1103 0.032 Uiso 0.507(16) 1 calc PR A 2 S2 S 0.7460(3) 0.2127(3) 0.8100(2) 0.0217(9) Uani 1 1 d . B . O13 O 0.7658(9) 0.3101(8) 0.7800(6) 0.040(3) Uani 1 1 d . . . O14 O 0.7898(8) 0.1455(8) 0.7723(6) 0.029(3) Uani 1 1 d . . . O15 O 0.6272(8) 0.1396(8) 0.8014(6) 0.023(2) Uani 1 1 d . . . C8 C 0.8253(12) 0.2702(11) 0.9165(9) 0.020(3) Uani 1 1 d U . . C9 C 0.779(2) 0.222(2) 0.9748(18) 0.021(5) Uani 0.516(14) 1 d PU B 1 H9 H 0.7036 0.1568 0.9554 0.025 Uiso 0.516(14) 1 calc PR B 1 C10 C 0.841(2) 0.268(3) 1.0608(18) 0.024(5) Uani 0.516(14) 1 d PU B 1 H10 H 0.8059 0.2369 1.0996 0.029 Uiso 0.516(14) 1 calc PR B 1 C11 C 0.9510(12) 0.3563(12) 1.0875(9) 0.022(3) Uani 1 1 d U . . C12 C 0.991(2) 0.413(2) 1.0287(17) 0.026(5) Uani 0.516(14) 1 d PU B 1 H12 H 1.0620 0.4842 1.0488 0.031 Uiso 0.516(14) 1 calc PR B 1 C13 C 0.933(2) 0.371(2) 0.9482(18) 0.026(6) Uani 0.516(14) 1 d PU B 1 H13 H 0.9647 0.4094 0.9111 0.031 Uiso 0.516(14) 1 calc PR B 1 C14 C 1.0160(13) 0.4045(14) 1.1787(9) 0.038(4) Uani 1 1 d U B . H14A H 0.9742 0.3526 1.2076 0.056 Uiso 1 1 calc R . . H14B H 1.0244 0.4788 1.2001 0.056 Uiso 1 1 calc R . . H14C H 1.0926 0.4140 1.1886 0.056 Uiso 1 1 calc R . . C9X C 0.781(2) 0.290(2) 0.9710(18) 0.015(4) Uani 0.484(14) 1 d PU B 2 H9X H 0.7030 0.2723 0.9520 0.019 Uiso 0.484(14) 1 calc PR B 2 C10X C 0.843(2) 0.338(3) 1.0589(19) 0.022(5) Uani 0.484(14) 1 d PU B 2 H10X H 0.8099 0.3572 1.0969 0.027 Uiso 0.484(14) 1 calc PR B 2 C12X C 0.998(3) 0.327(3) 1.0296(19) 0.027(5) Uani 0.484(14) 1 d PU B 2 H12X H 1.0727 0.3385 1.0487 0.032 Uiso 0.484(14) 1 calc PR B 2 C13X C 0.936(2) 0.282(2) 0.9451(19) 0.020(5) Uani 0.484(14) 1 d PU B 2 H13X H 0.9663 0.2593 0.9064 0.024 Uiso 0.484(14) 1 calc PR B 2 S3 S 0.7796(4) 0.0612(3) 0.2580(3) 0.0307(10) Uani 1 1 d . C . O16 O 0.8492(10) 0.1861(9) 0.2750(7) 0.047(3) Uani 1 1 d . . . O17 O 0.6985(9) 0.0271(9) 0.3034(6) 0.035(3) Uani 1 1 d . . . O18 O 0.8512(8) 0.0121(8) 0.2740(6) 0.030(3) Uani 1 1 d . . . C15 C 0.7031(14) 0.0050(13) 0.1533(10) 0.032(3) Uani 1 1 d U . . C16 C 0.5886(15) -0.0690(15) 0.1218(11) 0.047(4) Uani 1 1 d U C . H16 H 0.5469 -0.0934 0.1588 0.057 Uiso 1 1 calc R . . C17 C 0.5315(17) -0.1096(17) 0.0377(12) 0.064(5) Uani 1 1 d U . . H17 H 0.4500 -0.1582 0.0186 0.077 Uiso 1 1 calc R C . C18 C 0.5820(16) -0.0860(14) -0.0189(10) 0.037(3) Uani 1 1 d U C . C19 C 0.680(4) 0.008(3) 0.012(2) 0.044(7) Uani 0.48(3) 1 d PU C 1 H19 H 0.7104 0.0472 -0.0248 0.053 Uiso 0.48(3) 1 calc PR C 1 C20 C 0.741(3) 0.055(3) 0.094(2) 0.037(6) Uani 0.48(3) 1 d PU C 1 H20 H 0.8122 0.1251 0.1119 0.045 Uiso 0.48(3) 1 calc PR C 1 C21 C 0.5217(18) -0.1332(16) -0.1118(10) 0.065(5) Uani 1 1 d U . . H21A H 0.5419 -0.0703 -0.1361 0.097 Uiso 1 1 calc R C . H21B H 0.4381 -0.1764 -0.1237 0.097 Uiso 1 1 calc R . . H21C H 0.5457 -0.1837 -0.1363 0.097 Uiso 1 1 calc R . . C19X C 0.708(3) -0.035(3) 0.012(2) 0.033(5) Uani 0.52(3) 1 d PU C 2 H19X H 0.7507 -0.0262 -0.0255 0.040 Uiso 0.52(3) 1 calc PR C 2 C20X C 0.760(3) -0.001(3) 0.0939(19) 0.028(5) Uani 0.52(3) 1 d PU C 2 H20X H 0.8388 0.0212 0.1143 0.034 Uiso 0.52(3) 1 calc PR C 2 S4 S 0.7782(3) 0.5513(3) 0.2278(3) 0.0244(9) Uani 1 1 d . D . O19 O 0.6904(9) 0.5129(8) 0.2654(7) 0.035(3) Uani 1 1 d . . . O20 O 0.8466(9) 0.6763(8) 0.2504(7) 0.035(3) Uani 1 1 d . . . O21 O 0.8499(8) 0.5020(8) 0.2431(6) 0.029(3) Uani 1 1 d . . . C22 C 0.7060(12) 0.5006(12) 0.1185(9) 0.024(3) Uani 1 1 d U . . C23 C 0.5926(15) 0.4367(15) 0.0846(11) 0.055(5) Uani 1 1 d U D . H23 H 0.5465 0.4150 0.1193 0.066 Uiso 1 1 calc R . . C24 C 0.5419(16) 0.4020(18) 0.0003(12) 0.069(6) Uani 1 1 d U . . H24 H 0.4600 0.3601 -0.0217 0.083 Uiso 1 1 calc R D . C25 C 0.5989(14) 0.4227(13) -0.0533(10) 0.034(3) Uani 1 1 d U D . C26 C 0.711(3) 0.511(3) -0.017(2) 0.027(6) Uani 0.51(3) 1 d PU D 1 H26 H 0.7520 0.5435 -0.0525 0.032 Uiso 0.51(3) 1 calc PR D 1 C27 C 0.765(3) 0.553(3) 0.0666(18) 0.022(5) Uani 0.51(3) 1 d PU D 1 H27 H 0.8416 0.6166 0.0900 0.026 Uiso 0.51(3) 1 calc PR D 1 C28 C 0.5426(16) 0.3809(16) -0.1469(10) 0.057(5) Uani 1 1 d U . . H28A H 0.4591 0.3465 -0.1608 0.086 Uiso 1 1 calc R D . H28B H 0.5591 0.3237 -0.1715 0.086 Uiso 1 1 calc R . . H28C H 0.5730 0.4452 -0.1693 0.086 Uiso 1 1 calc R . . C26X C 0.715(3) 0.459(3) -0.017(2) 0.031(5) Uani 0.49(3) 1 d PU D 2 H26X H 0.7580 0.4615 -0.0527 0.037 Uiso 0.49(3) 1 calc PR D 2 C27X C 0.766(3) 0.490(3) 0.061(2) 0.023(5) Uani 0.49(3) 1 d PU D 2 H27X H 0.8426 0.5049 0.0816 0.028 Uiso 0.49(3) 1 calc PR D 2 O1W O 0.3693(8) 0.4336(7) 0.5999(6) 0.020(2) Uani 1 1 d . . . O2W O 0.0153(9) -0.1231(9) 0.4904(7) 0.036(3) Uani 1 1 d . . . O3W O 0.0712(8) 0.1358(8) 0.3780(7) 0.032(3) Uani 1 1 d . . . O4W O 0.9145(9) 0.1895(8) 0.6642(6) 0.031(3) Uani 1 1 d . . . O5W O 0.1584(8) 0.1540(8) 0.6556(6) 0.030(3) Uani 1 1 d . . . O6W O 0.8532(10) 0.4599(8) 0.4632(8) 0.053(4) Uani 1 1 d . . . O7W O 0.7548(9) 0.3205(9) 0.2982(8) 0.048(3) Uani 1 1 d . . . O8W O 0.8393(10) 0.6507(8) 0.6428(7) 0.042(3) Uani 1 1 d . . . O9W O 0.9335(9) 0.4208(13) 0.6308(7) 0.071(5) Uani 1 1 d . . . O10W O 0.9761(11) 0.3078(11) 0.4869(12) 0.115(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0140(6) 0.0041(5) 0.0178(6) 0.0030(5) 0.0039(5) 0.0048(5) Mo2 0.0146(6) 0.0044(5) 0.0188(7) 0.0033(5) 0.0040(5) 0.0058(5) Mo3 0.0154(7) 0.0036(6) 0.0174(6) 0.0031(5) 0.0032(5) 0.0058(5) Se1 0.0151(8) 0.0061(7) 0.0226(9) 0.0045(7) 0.0045(7) 0.0051(6) Se2 0.0183(8) 0.0079(7) 0.0195(9) 0.0049(7) 0.0044(7) 0.0067(7) Se3 0.0185(8) 0.0037(7) 0.0230(9) 0.0051(6) 0.0068(7) 0.0064(6) Se4 0.0151(8) 0.0069(7) 0.0174(8) 0.0032(6) 0.0031(7) 0.0066(6) O1 0.0200(17) 0.005(3) 0.024(2) -0.0001(19) -0.0029(18) 0.0053(16) O2 0.029(3) 0.0027(17) 0.023(4) 0.0035(15) 0.008(3) 0.0026(18) O3 0.027(3) 0.0048(16) 0.018(3) 0.0021(17) 0.003(2) 0.0101(16) O4 0.022(3) 0.008(3) 0.031(5) 0.008(4) 0.012(3) 0.005(2) O5 0.0120(11) 0.009(3) 0.035(4) 0.006(3) 0.0005(11) 0.009(2) O6 0.020(2) 0.010(4) 0.042(5) 0.006(4) 0.016(3) 0.009(3) O7 0.026(4) 0.010(3) 0.0200(18) 0.007(3) 0.008(3) 0.008(3) O8 0.023(5) 0.011(4) 0.020(3) 0.003(2) 0.008(3) 0.010(4) O9 0.018(3) 0.019(4) 0.0173(10) 0.004(2) 0.0016(12) 0.008(3) S1 0.026(2) 0.0117(18) 0.022(2) 0.0028(17) 0.0022(19) 0.0117(18) O10 0.022(6) 0.012(5) 0.037(7) 0.015(5) 0.009(5) 0.009(5) O11 0.039(7) 0.019(6) 0.030(7) 0.001(5) 0.001(6) 0.023(5) O12 0.021(6) 0.022(6) 0.039(7) 0.015(5) 0.010(5) 0.013(5) C1 0.023(6) 0.017(6) 0.022(6) 0.006(5) 0.006(5) 0.013(5) C2 0.023(7) 0.015(8) 0.028(6) 0.007(6) 0.009(5) 0.015(5) C3 0.034(9) 0.024(11) 0.024(6) 0.007(9) 0.014(7) 0.009(7) C4 0.032(6) 0.019(6) 0.026(5) 0.005(5) 0.008(4) 0.013(5) C5 0.018(9) 0.025(11) 0.030(7) 0.009(8) 0.003(7) 0.009(7) C6 0.023(9) 0.020(11) 0.027(7) 0.008(9) 0.008(8) 0.013(7) C7 0.043(9) 0.031(9) 0.026(5) 0.000(6) 0.009(5) 0.017(8) C2X 0.028(8) 0.021(10) 0.029(7) 0.003(10) 0.011(5) 0.015(9) C3X 0.032(7) 0.024(11) 0.027(6) 0.006(10) 0.015(6) 0.016(9) C5X 0.018(9) 0.022(11) 0.022(7) 0.014(9) 0.009(6) 0.006(9) C6X 0.014(8) 0.028(12) 0.024(6) 0.000(10) 0.002(7) 0.003(9) S2 0.022(2) 0.0139(19) 0.021(2) 0.0039(18) 0.0005(19) 0.0067(18) O13 0.041(7) 0.020(6) 0.034(7) 0.014(6) -0.007(6) 0.003(6) O14 0.029(6) 0.016(5) 0.029(7) -0.006(5) 0.004(5) 0.009(5) O15 0.012(6) 0.024(6) 0.024(6) 0.003(5) -0.003(5) 0.007(5) C8 0.019(6) 0.015(6) 0.027(6) 0.004(5) 0.009(5) 0.010(5) C9 0.009(8) 0.019(10) 0.030(7) 0.010(8) 0.000(6) 0.005(7) C10 0.019(8) 0.024(11) 0.026(7) 0.004(9) 0.004(7) 0.011(7) C11 0.021(5) 0.022(6) 0.016(5) 0.003(5) -0.001(4) 0.010(5) C12 0.027(10) 0.022(10) 0.022(7) 0.004(7) 0.005(7) 0.010(7) C13 0.021(10) 0.028(10) 0.020(7) 0.011(9) 0.007(8) 0.005(7) C14 0.030(8) 0.048(10) 0.019(5) 0.003(6) -0.001(5) 0.015(8) C9X 0.016(6) 0.014(8) 0.023(6) 0.005(6) 0.004(4) 0.014(6) C10X 0.022(8) 0.021(10) 0.023(6) 0.004(9) 0.003(6) 0.013(9) C12X 0.024(9) 0.029(12) 0.026(7) 0.005(10) 0.006(6) 0.014(9) C13X 0.020(9) 0.020(11) 0.024(7) 0.003(9) 0.012(7) 0.013(9) S3 0.037(3) 0.029(2) 0.045(3) 0.021(2) 0.020(2) 0.026(2) O16 0.078(9) 0.036(7) 0.056(9) 0.024(7) 0.038(8) 0.041(7) O17 0.041(7) 0.051(7) 0.029(7) 0.016(6) 0.011(6) 0.034(6) O18 0.030(6) 0.025(6) 0.043(7) 0.009(5) 0.018(6) 0.020(5) C15 0.044(7) 0.038(8) 0.040(7) 0.025(6) 0.027(6) 0.032(6) C16 0.048(7) 0.053(10) 0.043(6) 0.009(8) 0.030(7) 0.023(7) C17 0.051(8) 0.075(11) 0.047(7) -0.012(9) 0.023(6) 0.024(8) C18 0.060(7) 0.038(7) 0.033(6) 0.020(6) 0.012(5) 0.039(6) C19 0.067(11) 0.040(11) 0.038(7) 0.026(9) 0.013(8) 0.035(8) C20 0.048(8) 0.036(8) 0.038(7) 0.026(7) 0.016(6) 0.024(5) C21 0.111(13) 0.055(11) 0.034(6) 0.011(8) 0.000(7) 0.057(10) C19X 0.058(7) 0.032(11) 0.037(7) 0.025(10) 0.028(7) 0.035(9) C20X 0.044(8) 0.034(11) 0.038(8) 0.028(9) 0.025(6) 0.034(9) S4 0.025(2) 0.0117(19) 0.032(3) 0.0035(18) 0.010(2) 0.0075(18) O19 0.028(7) 0.032(6) 0.040(7) 0.007(6) 0.015(6) 0.013(6) O20 0.030(7) 0.026(6) 0.041(7) 0.002(6) 0.006(6) 0.014(5) O21 0.025(6) 0.014(5) 0.040(7) 0.000(5) 0.000(5) 0.012(5) C22 0.026(6) 0.021(7) 0.034(6) 0.015(6) 0.012(5) 0.016(6) C23 0.028(6) 0.059(11) 0.038(6) -0.003(9) 0.015(6) -0.004(7) C24 0.029(7) 0.081(12) 0.040(6) 0.002(10) 0.007(5) -0.008(8) C25 0.039(6) 0.025(7) 0.035(6) 0.009(6) 0.010(5) 0.015(6) C26 0.035(8) 0.022(11) 0.033(6) 0.015(9) 0.014(7) 0.019(8) C27 0.026(7) 0.019(8) 0.031(6) 0.010(6) 0.015(5) 0.017(5) C28 0.065(11) 0.054(12) 0.035(6) -0.002(8) 0.003(6) 0.028(10) C26X 0.041(7) 0.020(11) 0.035(7) 0.008(11) 0.014(6) 0.016(10) C27X 0.035(8) 0.013(11) 0.034(8) 0.013(10) 0.016(6) 0.019(9) O1W 0.021(6) 0.008(5) 0.028(6) 0.004(5) 0.003(5) 0.008(5) O2W 0.033(7) 0.041(7) 0.045(8) 0.017(6) 0.023(6) 0.022(6) O3W 0.032(7) 0.016(5) 0.047(7) 0.009(5) 0.004(6) 0.015(5) O4W 0.033(7) 0.023(6) 0.036(7) 0.012(5) 0.013(6) 0.012(5) O5W 0.028(6) 0.020(6) 0.046(7) 0.018(6) 0.019(6) 0.011(5) O6W 0.067(9) 0.019(6) 0.098(11) 0.022(7) 0.058(9) 0.025(6) O7W 0.049(8) 0.026(6) 0.085(10) 0.022(7) 0.040(8) 0.024(6) O8W 0.056(8) 0.022(6) 0.046(8) 0.012(6) 0.029(7) 0.014(6) O9W 0.020(7) 0.135(13) 0.041(8) 0.025(9) 0.017(7) 0.027(8) O10W 0.035(9) 0.032(8) 0.25(2) 0.034(11) 0.035(12) 0.004(7) _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 O3 2.186(8) . ? Mo1 O1 2.191(9) . ? Mo1 O2 2.262(8) . ? Mo1 Se2 2.3840(18) . ? Mo1 Se1 2.3920(17) . ? Mo1 Se4 2.4754(18) . ? Mo1 Mo3 2.7910(17) . ? Mo1 Mo2 2.8055(17) . ? Mo2 O5 2.168(9) . ? Mo2 O6 2.177(8) . ? Mo2 O4 2.178(8) . ? Mo2 Se2 2.3929(19) . ? Mo2 Se3 2.4050(18) . ? Mo2 Se4 2.4518(17) . ? Mo2 Mo3 2.7816(16) . ? Mo3 O7 2.170(8) . ? Mo3 O8 2.188(8) . ? Mo3 O9 2.191(9) . ? Mo3 Se1 2.3919(19) . ? Mo3 Se3 2.4048(17) . ? Mo3 Se4 2.4462(17) . ? S1 O12 1.429(9) . ? S1 O10 1.464(9) . ? S1 O11 1.486(9) . ? S1 C1 1.757(14) . ? C1 C2X 1.31(3) . ? C1 C2 1.40(3) . ? C1 C6X 1.42(3) . ? C1 C6 1.43(3) . ? C2 C3 1.31(4) . ? C3 C4 1.39(4) . ? C4 C3X 1.34(3) . ? C4 C5 1.39(3) . ? C4 C5X 1.43(3) . ? C4 C7 1.48(2) . ? C5 C6 1.39(4) . ? C2X C3X 1.40(4) . ? C5X C6X 1.37(4) . ? S2 O15 1.438(9) . ? S2 O13 1.457(10) . ? S2 O14 1.468(10) . ? S2 C8 1.740(15) . ? C8 C9X 1.29(3) . ? C8 C13 1.40(3) . ? C8 C9 1.40(3) . ? C8 C13X 1.43(3) . ? C9 C10 1.40(4) . ? C10 C11 1.35(3) . ? C11 C10X 1.35(3) . ? C11 C12X 1.40(3) . ? C11 C12 1.43(3) . ? C11 C14 1.483(19) . ? C12 C13 1.31(4) . ? C9X C10X 1.43(4) . ? C12X C13X 1.38(4) . ? S3 O18 1.449(9) . ? S3 O17 1.453(10) . ? S3 O16 1.479(11) . ? S3 C15 1.708(17) . ? C15 C16 1.34(2) . ? C15 C20 1.39(3) . ? C15 C20X 1.43(3) . ? C16 C17 1.36(2) . ? C17 C18 1.32(2) . ? C18 C19 1.28(4) . ? C18 C19X 1.48(4) . ? C18 C21 1.50(2) . ? C19 C20 1.33(5) . ? C19X C20X 1.32(4) . ? S4 O19 1.428(10) . ? S4 O21 1.452(9) . ? S4 O20 1.469(10) . ? S4 C22 1.767(15) . ? C22 C23 1.32(2) . ? C22 C27 1.40(3) . ? C22 C27X 1.45(3) . ? C23 C24 1.36(2) . ? C24 C25 1.32(2) . ? C25 C26 1.36(4) . ? C25 C26X 1.39(4) . ? C25 C28 1.50(2) . ? C26 C27 1.35(4) . ? C26X C27X 1.26(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 O1 78.2(3) . . ? O3 Mo1 O2 76.7(3) . . ? O1 Mo1 O2 79.5(3) . . ? O3 Mo1 Se2 94.0(2) . . ? O1 Mo1 Se2 85.1(2) . . ? O2 Mo1 Se2 163.3(2) . . ? O3 Mo1 Se1 159.7(2) . . ? O1 Mo1 Se1 85.7(2) . . ? O2 Mo1 Se1 88.3(2) . . ? Se2 Mo1 Se1 96.92(6) . . ? O3 Mo1 Se4 85.1(2) . . ? O1 Mo1 Se4 160.0(2) . . ? O2 Mo1 Se4 86.1(2) . . ? Se2 Mo1 Se4 107.15(6) . . ? Se1 Mo1 Se4 107.74(7) . . ? O3 Mo1 Mo3 140.0(2) . . ? O1 Mo1 Mo3 140.0(2) . . ? O2 Mo1 Mo3 96.2(2) . . ? Se2 Mo1 Mo3 99.66(6) . . ? Se1 Mo1 Mo3 54.31(5) . . ? Se4 Mo1 Mo3 54.96(5) . . ? O3 Mo1 Mo2 101.5(2) . . ? O1 Mo1 Mo2 139.3(2) . . ? O2 Mo1 Mo2 140.7(2) . . ? Se2 Mo1 Mo2 54.18(5) . . ? Se1 Mo1 Mo2 98.71(6) . . ? Se4 Mo1 Mo2 54.90(5) . . ? Mo3 Mo1 Mo2 59.61(4) . . ? O5 Mo2 O6 80.3(3) . . ? O5 Mo2 O4 76.7(3) . . ? O6 Mo2 O4 77.7(3) . . ? O5 Mo2 Se2 162.6(2) . . ? O6 Mo2 Se2 95.3(3) . . ? O4 Mo2 Se2 86.0(3) . . ? O5 Mo2 Se3 87.8(2) . . ? O6 Mo2 Se3 163.3(2) . . ? O4 Mo2 Se3 88.3(2) . . ? Se2 Mo2 Se3 92.63(6) . . ? O5 Mo2 Se4 88.6(2) . . ? O6 Mo2 Se4 82.3(2) . . ? O4 Mo2 Se4 156.8(2) . . ? Se2 Mo2 Se4 107.63(6) . . ? Se3 Mo2 Se4 109.20(7) . . ? O5 Mo2 Mo3 94.7(2) . . ? O6 Mo2 Mo3 137.5(2) . . ? O4 Mo2 Mo3 142.6(2) . . ? Se2 Mo2 Mo3 99.70(6) . . ? Se3 Mo2 Mo3 54.66(5) . . ? Se4 Mo2 Mo3 55.30(4) . . ? O5 Mo2 Mo1 143.4(2) . . ? O6 Mo2 Mo1 100.4(2) . . ? O4 Mo2 Mo1 139.7(3) . . ? Se2 Mo2 Mo1 53.89(5) . . ? Se3 Mo2 Mo1 96.13(6) . . ? Se4 Mo2 Mo1 55.69(5) . . ? Mo3 Mo2 Mo1 59.94(4) . . ? O7 Mo3 O8 79.5(3) . . ? O7 Mo3 O9 80.3(3) . . ? O8 Mo3 O9 76.2(3) . . ? O7 Mo3 Se1 94.0(2) . . ? O8 Mo3 Se1 86.3(2) . . ? O9 Mo3 Se1 162.3(2) . . ? O7 Mo3 Se3 165.6(2) . . ? O8 Mo3 Se3 87.5(2) . . ? O9 Mo3 Se3 90.7(2) . . ? Se1 Mo3 Se3 91.22(6) . . ? O7 Mo3 Se4 81.6(2) . . ? O8 Mo3 Se4 156.6(2) . . ? O9 Mo3 Se4 87.2(2) . . ? Se1 Mo3 Se4 108.70(7) . . ? Se3 Mo3 Se4 109.39(6) . . ? O7 Mo3 Mo2 137.1(2) . . ? O8 Mo3 Mo2 141.7(2) . . ? O9 Mo3 Mo2 96.1(2) . . ? Se1 Mo3 Mo2 99.37(6) . . ? Se3 Mo3 Mo2 54.67(5) . . ? Se4 Mo3 Mo2 55.49(5) . . ? O7 Mo3 Mo1 97.4(2) . . ? O8 Mo3 Mo1 140.4(2) . . ? O9 Mo3 Mo1 142.8(2) . . ? Se1 Mo3 Mo1 54.31(5) . . ? Se3 Mo3 Mo1 96.51(6) . . ? Se4 Mo3 Mo1 55.95(5) . . ? Mo2 Mo3 Mo1 60.46(4) . . ? Mo3 Se1 Mo1 71.38(6) . . ? Mo1 Se2 Mo2 71.93(6) . . ? Mo3 Se3 Mo2 70.67(5) . . ? Mo3 Se4 Mo2 69.21(5) . . ? Mo3 Se4 Mo1 69.09(5) . . ? Mo2 Se4 Mo1 69.41(5) . . ? O12 S1 O10 113.6(5) . . ? O12 S1 O11 113.0(6) . . ? O10 S1 O11 110.6(6) . . ? O12 S1 C1 107.4(6) . . ? O10 S1 C1 106.3(6) . . ? O11 S1 C1 105.4(6) . . ? C2X C1 C2 35.8(14) . . ? C2X C1 C6X 118(2) . . ? C2 C1 C6X 103.3(19) . . ? C2X C1 C6 104(2) . . ? C2 C1 C6 119(2) . . ? C6X C1 C6 45.4(15) . . ? C2X C1 S1 123.2(17) . . ? C2 C1 S1 122.7(16) . . ? C6X C1 S1 118.4(15) . . ? C6 C1 S1 118.6(15) . . ? C3 C2 C1 118(3) . . ? C2 C3 C4 127(3) . . ? C3X C4 C5 104(2) . . ? C3X C4 C3 36.4(15) . . ? C5 C4 C3 116(2) . . ? C3X C4 C5X 116(2) . . ? C5 C4 C5X 48.4(15) . . ? C3 C4 C5X 97(2) . . ? C3X C4 C7 122.8(19) . . ? C5 C4 C7 120.4(18) . . ? C3 C4 C7 124.1(19) . . ? C5X C4 C7 120.6(17) . . ? C4 C5 C6 121(3) . . ? C5 C6 C1 120(3) . . ? C1 C2X C3X 121(3) . . ? C4 C3X C2X 123(3) . . ? C6X C5X C4 120(3) . . ? C5X C6X C1 121(3) . . ? O15 S2 O13 112.9(6) . . ? O15 S2 O14 110.3(6) . . ? O13 S2 O14 113.5(6) . . ? O15 S2 C8 107.6(6) . . ? O13 S2 C8 105.5(6) . . ? O14 S2 C8 106.6(6) . . ? C9X C8 C13 99(2) . . ? C9X C8 C9 41.0(14) . . ? C13 C8 C9 117(2) . . ? C9X C8 C13X 119(2) . . ? C13 C8 C13X 52.3(16) . . ? C9 C8 C13X 99.0(18) . . ? C9X C8 S2 121.0(16) . . ? C13 C8 S2 121.8(15) . . ? C9 C8 S2 121.0(15) . . ? C13X C8 S2 119.7(15) . . ? C10 C9 C8 122(2) . . ? C11 C10 C9 119(3) . . ? C10X C11 C10 42.0(15) . . ? C10X C11 C12X 119(2) . . ? C10 C11 C12X 104(2) . . ? C10X C11 C12 94.8(19) . . ? C10 C11 C12 118(2) . . ? C12X C11 C12 52.1(16) . . ? C10X C11 C14 119.9(18) . . ? C10 C11 C14 118.6(18) . . ? C12X C11 C14 121.5(17) . . ? C12 C11 C14 122.4(17) . . ? C13 C12 C11 122(3) . . ? C12 C13 C8 121(2) . . ? C8 C9X C10X 122(3) . . ? C11 C10X C9X 120(3) . . ? C13X C12X C11 121(3) . . ? C12X C13X C8 119(2) . . ? O18 S3 O17 109.8(6) . . ? O18 S3 O16 112.0(6) . . ? O17 S3 O16 113.5(6) . . ? O18 S3 C15 106.8(7) . . ? O17 S3 C15 108.2(7) . . ? O16 S3 C15 106.2(7) . . ? C16 C15 C20 110(2) . . ? C16 C15 C20X 112.8(19) . . ? C20 C15 C20X 38.5(15) . . ? C16 C15 S3 123.4(13) . . ? C20 C15 S3 124(2) . . ? C20X C15 S3 119.9(17) . . ? C15 C16 C17 121.0(17) . . ? C18 C17 C16 124.2(19) . . ? C19 C18 C17 111(2) . . ? C19 C18 C19X 35.2(17) . . ? C17 C18 C19X 115.0(19) . . ? C19 C18 C21 120(2) . . ? C17 C18 C21 125.2(18) . . ? C19X C18 C21 117.8(19) . . ? C18 C19 C20 124(3) . . ? C19 C20 C15 122(3) . . ? C20X C19X C18 118(3) . . ? C19X C20X C15 123(3) . . ? O19 S4 O21 112.5(6) . . ? O19 S4 O20 112.4(6) . . ? O21 S4 O20 112.3(6) . . ? O19 S4 C22 106.3(7) . . ? O21 S4 C22 106.4(6) . . ? O20 S4 C22 106.4(6) . . ? C23 C22 C27 115.9(18) . . ? C23 C22 C27X 113.4(19) . . ? C27 C22 C27X 35.6(13) . . ? C23 C22 S4 122.8(13) . . ? C27 C22 S4 119.1(16) . . ? C27X C22 S4 120.1(16) . . ? C22 C23 C24 120.1(17) . . ? C25 C24 C23 124.2(18) . . ? C24 C25 C26 113(2) . . ? C24 C25 C26X 112(2) . . ? C26 C25 C26X 31.2(14) . . ? C24 C25 C28 124.2(17) . . ? C26 C25 C28 120(2) . . ? C26X C25 C28 121(2) . . ? C27 C26 C25 123(3) . . ? C26 C27 C22 119(3) . . ? C27X C26X C25 125(3) . . ? C26X C27X C22 119(3) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 3.137 _refine_diff_density_min -1.438 _refine_diff_density_rms 0.268 #===END data_ags37 _database_code_CSD 158609 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H69 O32.50 S4 Se4 W3' _chemical_formula_weight 1921.46 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' 'Se' 'Se' -0.0929 2.2259 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9215(7) _cell_length_b 15.4869(7) _cell_length_c 16.9541(8) _cell_angle_alpha 101.655(2) _cell_angle_beta 96.056(2) _cell_angle_gamma 109.195(2) _cell_volume 2844.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 16832 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 28.68 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1838 _exptl_absorpt_coefficient_mu 8.844 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.191 _exptl_absorpt_correction_T_max 0.503 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 25158 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0761 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 28.71 _reflns_number_total 13149 _reflns_number_gt 9071 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00059(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 13149 _refine_ls_number_parameters 895 _refine_ls_number_restraints 1596 _refine_ls_R_factor_all 0.0741 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1108 _refine_ls_wR_factor_gt 0.1041 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.939 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.12176(3) 0.21473(2) 0.61443(2) 0.02407(9) Uani 1 1 d . . . W2 W -0.07563(3) 0.18276(2) 0.495958(19) 0.02427(9) Uani 1 1 d . . . W3 W 0.15385(3) 0.24577(2) 0.46165(2) 0.03612(11) Uani 1 1 d . . . Se1 Se 0.07681(8) 0.34037(5) 0.56356(6) 0.0368(2) Uani 1 1 d . . . Se2 Se -0.05353(7) 0.07051(5) 0.57191(5) 0.02438(17) Uani 1 1 d . . . Se3 Se -0.01434(8) 0.11311(6) 0.37596(5) 0.0347(2) Uani 1 1 d . . . Se4 Se 0.24578(7) 0.15666(5) 0.53081(5) 0.03084(19) Uani 1 1 d . . . O1 O 0.1876(5) 0.1514(4) 0.7056(3) 0.0285(12) Uani 1 1 d . . . O2 O 0.0525(5) 0.2620(4) 0.7221(4) 0.0464(17) Uani 1 1 d . . . O3 O 0.2803(5) 0.3312(4) 0.6854(4) 0.0418(15) Uani 1 1 d . . . O4 O -0.1573(5) 0.2605(4) 0.4317(3) 0.0374(14) Uani 1 1 d . . . O5 O -0.1919(5) 0.2213(4) 0.5784(3) 0.0373(14) Uani 1 1 d . . . O6 O -0.2560(5) 0.0797(4) 0.4384(4) 0.0364(14) Uani 1 1 d . . . O7 O 0.3220(6) 0.3648(5) 0.4968(5) 0.075(3) Uani 1 1 d . . . O8 O 0.2518(6) 0.2074(5) 0.3580(4) 0.059(2) Uani 1 1 d . . . O9 O 0.1299(7) 0.3350(5) 0.3839(5) 0.067(2) Uani 1 1 d . . . S1 S 0.43492(19) 0.05599(15) 0.76085(14) 0.0368(5) Uani 1 1 d D A . O10 O 0.4730(6) -0.0247(5) 0.7468(4) 0.0569(19) Uani 1 1 d D . . O11 O 0.5219(5) 0.1392(4) 0.7462(4) 0.0475(16) Uani 1 1 d D . . O12 O 0.3135(5) 0.0340(4) 0.7147(4) 0.0391(14) Uani 1 1 d D . . C1 C 0.4266(7) 0.0838(5) 0.8661(4) 0.0372(18) Uani 1 1 d DU . . C2 C 0.3157(11) 0.0570(11) 0.8920(8) 0.050(4) Uani 0.547(14) 1 d PDU A 1 H2 H 0.2426 0.0227 0.8536 0.060 Uiso 0.547(14) 1 calc PR A 1 C3 C 0.3152(13) 0.0820(12) 0.9756(8) 0.064(5) Uani 0.547(14) 1 d PDU A 1 H3 H 0.2402 0.0648 0.9939 0.077 Uiso 0.547(14) 1 calc PR A 1 C4 C 0.4209(10) 0.1313(8) 1.0329(6) 0.067(3) Uani 1 1 d DU . . C5 C 0.5243(14) 0.1548(15) 1.0045(8) 0.067(5) Uani 0.547(14) 1 d PDU A 1 H5 H 0.5984 0.1850 1.0427 0.080 Uiso 0.547(14) 1 calc PR A 1 C6 C 0.5273(13) 0.1371(15) 0.9221(8) 0.062(5) Uani 0.547(14) 1 d PDU A 1 H6 H 0.6014 0.1627 0.9044 0.074 Uiso 0.547(14) 1 calc PR A 1 C7 C 0.4231(15) 0.1600(10) 1.1228(6) 0.118(6) Uani 1 1 d DU A . H7A H 0.5066 0.1951 1.1515 0.177 Uiso 1 1 calc R . . H7B H 0.3891 0.1036 1.1428 0.177 Uiso 1 1 calc R . . H7C H 0.3749 0.2002 1.1329 0.177 Uiso 1 1 calc R . . C2X C 0.3533(15) 0.1275(12) 0.8952(9) 0.051(5) Uani 0.453(14) 1 d PDU A 2 H2X H 0.2990 0.1397 0.8576 0.061 Uiso 0.453(14) 1 calc PR A 2 C3X C 0.3549(16) 0.1548(14) 0.9776(8) 0.056(5) Uani 0.453(14) 1 d PDU A 2 H3X H 0.3081 0.1913 0.9960 0.067 Uiso 0.453(14) 1 calc PR A 2 C5X C 0.5115(16) 0.1024(16) 1.0055(9) 0.053(5) Uani 0.453(14) 1 d PDU A 2 H5X H 0.5740 0.1017 1.0448 0.064 Uiso 0.453(14) 1 calc PR A 2 C6X C 0.5141(16) 0.0744(16) 0.9225(9) 0.052(5) Uani 0.453(14) 1 d PDU A 2 H6X H 0.5730 0.0499 0.9047 0.062 Uiso 0.453(14) 1 calc PR A 2 S2 S -0.0516(9) 0.0904(9) 0.8260(6) 0.050(2) Uani 0.518(13) 1 d PD B 1 O13 O -0.1363(18) -0.0074(13) 0.7907(13) 0.096(8) Uani 0.518(13) 1 d PD B 1 O14 O 0.0718(13) 0.0986(17) 0.8194(11) 0.058(6) Uani 0.518(13) 1 d PD B 1 O15 O -0.0895(13) 0.1570(13) 0.7898(9) 0.044(4) Uani 0.518(13) 1 d PD B 1 C8 C -0.0566(17) 0.1165(16) 0.9306(8) 0.067(6) Uani 0.518(13) 1 d PDU B 1 C9 C 0.0190(18) 0.0982(16) 0.9864(12) 0.073(6) Uani 0.518(13) 1 d PDU B 1 H9 H 0.0716 0.0667 0.9687 0.088 Uiso 0.518(13) 1 calc PR B 1 C10 C 0.017(2) 0.1264(17) 1.0684(11) 0.074(6) Uani 0.518(13) 1 d PDU B 1 H10 H 0.0724 0.1168 1.1074 0.089 Uiso 0.518(13) 1 calc PR B 1 C11 C -0.061(2) 0.1678(19) 1.0954(10) 0.072(6) Uani 0.518(13) 1 d PDU B 1 C12 C -0.1290(18) 0.1909(18) 1.0390(9) 0.073(6) Uani 0.518(13) 1 d PDU B 1 H12 H -0.1757 0.2275 1.0574 0.087 Uiso 0.518(13) 1 calc PR B 1 C13 C -0.1320(17) 0.1628(18) 0.9564(9) 0.069(5) Uani 0.518(13) 1 d PDU B 1 H13 H -0.1849 0.1751 0.9179 0.083 Uiso 0.518(13) 1 calc PR B 1 C14 C -0.055(3) 0.2024(19) 1.1856(10) 0.084(9) Uani 0.518(13) 1 d PDU B 1 H14A H -0.1242 0.2219 1.1944 0.127 Uiso 0.518(13) 1 calc PR B 1 H14B H 0.0201 0.2565 1.2089 0.127 Uiso 0.518(13) 1 calc PR B 1 H14C H -0.0576 0.1516 1.2125 0.127 Uiso 0.518(13) 1 calc PR B 1 S2X S -0.0700(9) 0.0511(6) 0.8114(6) 0.0329(19) Uani 0.482(13) 1 d PD B 2 O13X O -0.1565(18) -0.0441(11) 0.7792(13) 0.049(5) Uiso 0.482(13) 1 d PD B 2 O14X O 0.0537(13) 0.0620(14) 0.8067(14) 0.043(6) Uiso 0.482(13) 1 d PD B 2 O15X O -0.1064(16) 0.1196(10) 0.7765(10) 0.036(5) Uiso 0.482(13) 1 d PD B 2 C8X C -0.0733(17) 0.0870(16) 0.9174(9) 0.059(6) Uani 0.482(13) 1 d PDU B 2 C9X C 0.0282(18) 0.1373(16) 0.9780(12) 0.074(7) Uani 0.482(13) 1 d PDU B 2 H9X H 0.1058 0.1562 0.9633 0.088 Uiso 0.482(13) 1 calc PR B 2 C10X C 0.0186(19) 0.1604(18) 1.0591(12) 0.081(7) Uani 0.482(13) 1 d PDU B 2 H10X H 0.0898 0.1947 1.0992 0.097 Uiso 0.482(13) 1 calc PR B 2 C11X C -0.0907(19) 0.135(2) 1.0832(11) 0.078(7) Uani 0.482(13) 1 d PDU B 2 C12X C -0.1912(17) 0.0881(19) 1.0235(10) 0.077(7) Uani 0.482(13) 1 d PDU B 2 H12X H -0.2683 0.0694 1.0389 0.093 Uiso 0.482(13) 1 calc PR B 2 C13X C -0.1846(16) 0.0667(19) 0.9418(10) 0.067(6) Uani 0.482(13) 1 d PDU B 2 H13X H -0.2568 0.0378 0.9018 0.081 Uiso 0.482(13) 1 calc PR B 2 C14X C -0.103(3) 0.154(2) 1.1715(12) 0.115(13) Uani 0.482(13) 1 d PDU B 2 H14D H -0.0226 0.1872 1.2060 0.173 Uiso 0.482(13) 1 calc PR B 2 H14E H -0.1416 0.0941 1.1853 0.173 Uiso 0.482(13) 1 calc PR B 2 H14F H -0.1524 0.1934 1.1808 0.173 Uiso 0.482(13) 1 calc PR B 2 S3 S 0.1672(3) 0.5220(2) 0.7852(2) 0.0740(10) Uani 1 1 d . C . O16 O 0.1552(9) 0.5902(6) 0.7435(6) 0.095(3) Uani 1 1 d . . . O17 O 0.0568(6) 0.4362(5) 0.7640(5) 0.078(3) Uani 1 1 d . . . O18 O 0.2733(6) 0.4979(5) 0.7751(5) 0.070(2) Uani 1 1 d . . . C15 C 0.1807(8) 0.5722(7) 0.8892(6) 0.073(3) Uani 1 1 d DU . . C16 C 0.2637(13) 0.5646(12) 0.9458(9) 0.063(5) Uani 0.523(13) 1 d PDU C 1 H16 H 0.3172 0.5339 0.9285 0.075 Uiso 0.523(13) 1 calc PR C 1 C17 C 0.2715(14) 0.6006(12) 1.0273(9) 0.063(5) Uani 0.523(13) 1 d PDU C 1 H17 H 0.3327 0.5965 1.0654 0.076 Uiso 0.523(13) 1 calc PR C 1 C18 C 0.1946(8) 0.6423(8) 1.0559(6) 0.092(4) Uani 1 1 d DU . . C19 C 0.1258(18) 0.6660(15) 0.9982(9) 0.103(7) Uani 0.523(13) 1 d PDU C 1 H19 H 0.0844 0.7072 1.0162 0.124 Uiso 0.523(13) 1 calc PR C 1 C20 C 0.1168(19) 0.6305(16) 0.9147(10) 0.097(7) Uani 0.523(13) 1 d PDU C 1 H20 H 0.0680 0.6457 0.8757 0.116 Uiso 0.523(13) 1 calc PR C 1 C21 C 0.2040(11) 0.6772(10) 1.1466(7) 0.114(5) Uani 1 1 d DU C . H21A H 0.2894 0.7064 1.1731 0.170 Uiso 1 1 calc R . . H21B H 0.1639 0.6240 1.1692 0.170 Uiso 1 1 calc R . . H21C H 0.1649 0.7240 1.1568 0.170 Uiso 1 1 calc R . . C16X C 0.2881(13) 0.6219(12) 0.9411(9) 0.062(6) Uani 0.477(13) 1 d PDU C 2 H16X H 0.3604 0.6350 0.9193 0.075 Uiso 0.477(13) 1 calc PR C 2 C17X C 0.2957(13) 0.6537(14) 1.0239(10) 0.066(6) Uani 0.477(13) 1 d PDU C 2 H17X H 0.3727 0.6840 1.0588 0.080 Uiso 0.477(13) 1 calc PR C 2 C19X C 0.0860(13) 0.5797(16) 1.0090(10) 0.094(8) Uani 0.477(13) 1 d PDU C 2 H19X H 0.0171 0.5601 1.0337 0.112 Uiso 0.477(13) 1 calc PR C 2 C20X C 0.0775(13) 0.5454(14) 0.9254(10) 0.078(7) Uani 0.477(13) 1 d PDU C 2 H20X H 0.0020 0.5038 0.8925 0.093 Uiso 0.477(13) 1 calc PR C 2 S4 S 0.6888(5) 0.5533(3) 0.7493(3) 0.1133(16) Uani 1 1 d DU . . O19 O 0.8234(18) 0.584(2) 0.759(2) 0.181(12) Uani 0.467(19) 1 d PDU D 1 O20 O 0.645(3) 0.6128(13) 0.7044(11) 0.132(8) Uani 0.467(19) 1 d PDU D 1 O21 O 0.641(3) 0.4546(10) 0.7149(17) 0.094(8) Uani 0.467(19) 1 d PDU D 1 O19X O 0.792(2) 0.6187(16) 0.7337(17) 0.152(9) Uani 0.533(19) 1 d PDU D 2 O20X O 0.5604(19) 0.5304(15) 0.7098(9) 0.124(7) Uani 0.533(19) 1 d PDU D 2 O21X O 0.6831(17) 0.4555(8) 0.7353(16) 0.094(8) Uani 0.533(19) 1 d PDU D 2 C22 C 0.6840(8) 0.5841(6) 0.8523(6) 0.059(2) Uani 1 1 d DU D . C23 C 0.7897(13) 0.6307(16) 0.9086(10) 0.089(7) Uani 0.54(2) 1 d PDU D 1 H23 H 0.8649 0.6453 0.8905 0.107 Uiso 0.54(2) 1 calc PR D 1 C24 C 0.7877(14) 0.6564(17) 0.9906(10) 0.102(7) Uani 0.54(2) 1 d PDU D 1 H24 H 0.8619 0.6887 1.0283 0.123 Uiso 0.54(2) 1 calc PR D 1 C25 C 0.6819(10) 0.6366(8) 1.0190(6) 0.082(3) Uani 1 1 d DU . . C26 C 0.5775(13) 0.5874(17) 0.9633(8) 0.063(5) Uani 0.54(2) 1 d PDU D 1 H26 H 0.5028 0.5715 0.9821 0.076 Uiso 0.54(2) 1 calc PR D 1 C27 C 0.5768(12) 0.5600(15) 0.8811(8) 0.044(4) Uani 0.54(2) 1 d PDU D 1 H27 H 0.5026 0.5245 0.8440 0.053 Uiso 0.54(2) 1 calc PR D 1 C28 C 0.6849(15) 0.6703(10) 1.1088(7) 0.138(6) Uani 1 1 d DU D . H28A H 0.7375 0.6470 1.1400 0.208 Uiso 1 1 calc R . . H28B H 0.6029 0.6463 1.1203 0.208 Uiso 1 1 calc R . . H28C H 0.7161 0.7395 1.1248 0.208 Uiso 1 1 calc R . . C23X C 0.7751(17) 0.5843(18) 0.9102(10) 0.091(7) Uani 0.46(2) 1 d PDU D 2 H23X H 0.8386 0.5651 0.8933 0.109 Uiso 0.46(2) 1 calc PR D 2 C24X C 0.7735(18) 0.6124(18) 0.9921(11) 0.086(6) Uani 0.46(2) 1 d PDU D 2 H24X H 0.8385 0.6150 1.0312 0.103 Uiso 0.46(2) 1 calc PR D 2 C26X C 0.5981(18) 0.6431(19) 0.9614(9) 0.053(5) Uani 0.46(2) 1 d PDU D 2 H26X H 0.5416 0.6706 0.9789 0.064 Uiso 0.46(2) 1 calc PR D 2 C27X C 0.5931(19) 0.611(2) 0.8792(10) 0.053(5) Uani 0.46(2) 1 d PDU D 2 H27X H 0.5268 0.6078 0.8408 0.063 Uiso 0.46(2) 1 calc PR D 2 O1W O -0.3991(5) -0.0138(4) 0.5285(4) 0.0483(17) Uani 1 1 d . . . O2W O -0.2924(5) 0.1152(5) 0.6739(4) 0.0533(18) Uani 1 1 d . . . O3W O -0.1533(6) 0.3953(5) 0.6578(5) 0.067(2) Uani 1 1 d . . . O4W O -0.3582(10) 0.2074(6) 0.3304(6) 0.138(5) Uani 1 1 d . . . O5W O 0.5312(6) 0.3599(6) 0.5563(5) 0.069(2) Uani 1 1 d . . . O6W O 0.4809(7) 0.3050(6) 0.7373(7) 0.097(3) Uani 1 1 d . . . O7W O 0.4195(12) 0.6307(8) 0.6905(8) 0.163(6) Uani 1 1 d . . . O8W O 0.092(2) 0.4996(18) 0.4474(15) 0.126(7) Uani 0.50 1 d PU E 1 O8WX O -0.1253(19) 0.4345(9) 0.4784(14) 0.125(9) Uani 0.50 1 d P F 2 O8WY O -0.0219(10) 0.4163(8) 0.3859(9) 0.047(3) Uani 0.50 1 d PU G 3 O9W O 0.312(2) 0.0972(13) 0.3267(12) 0.118(8) Uani 0.50 1 d P H 1 O9WX O 0.4639(15) 0.1913(14) 0.396(2) 0.225(19) Uani 0.50 1 d P I 2 O10W O 0.5532(9) 0.2001(7) 0.4973(7) 0.111(4) Uani 1 1 d . . . O11W O 0.3267(8) 0.5383(5) 0.5309(6) 0.096(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.02359(17) 0.01689(15) 0.03069(19) 0.00066(12) 0.00346(13) 0.00958(13) W2 0.02897(18) 0.01792(16) 0.02611(18) 0.00219(12) 0.00273(13) 0.01141(13) W3 0.0373(2) 0.02938(19) 0.0532(2) 0.02429(17) 0.01804(17) 0.01565(16) Se1 0.0351(5) 0.0155(4) 0.0546(6) 0.0004(4) -0.0066(4) 0.0121(3) Se2 0.0258(4) 0.0205(4) 0.0262(4) 0.0061(3) 0.0048(3) 0.0075(3) Se3 0.0569(6) 0.0312(4) 0.0262(4) 0.0098(4) 0.0117(4) 0.0262(4) Se4 0.0313(4) 0.0269(4) 0.0431(5) 0.0131(4) 0.0164(4) 0.0164(4) O1 0.028(3) 0.029(3) 0.029(3) 0.005(2) 0.002(2) 0.013(2) O2 0.044(4) 0.054(4) 0.039(4) -0.015(3) -0.002(3) 0.034(3) O3 0.040(3) 0.019(3) 0.056(4) -0.004(3) -0.009(3) 0.010(3) O4 0.049(4) 0.025(3) 0.034(3) 0.004(3) -0.007(3) 0.015(3) O5 0.033(3) 0.041(3) 0.039(4) 0.002(3) 0.002(3) 0.020(3) O6 0.026(3) 0.031(3) 0.044(4) 0.005(3) -0.012(3) 0.007(2) O7 0.043(4) 0.051(4) 0.126(7) 0.051(5) 0.002(4) -0.005(3) O8 0.061(5) 0.088(5) 0.055(5) 0.050(4) 0.036(4) 0.035(4) O9 0.086(5) 0.038(4) 0.074(5) 0.035(4) -0.001(4) 0.013(4) S1 0.0341(12) 0.0343(12) 0.0411(13) 0.0051(10) -0.0027(10) 0.0169(10) O10 0.062(5) 0.056(4) 0.061(5) 0.005(4) -0.004(4) 0.043(4) O11 0.042(4) 0.051(4) 0.048(4) 0.013(3) 0.013(3) 0.014(3) O12 0.029(3) 0.039(3) 0.043(4) 0.004(3) -0.006(3) 0.012(3) C1 0.041(5) 0.033(5) 0.038(4) 0.014(4) 0.001(3) 0.013(4) C2 0.044(7) 0.077(12) 0.046(7) 0.024(8) 0.006(6) 0.038(8) C3 0.074(8) 0.097(13) 0.056(7) 0.037(9) 0.032(6) 0.060(9) C4 0.108(8) 0.064(7) 0.042(5) 0.019(5) 0.014(5) 0.041(6) C5 0.083(9) 0.048(11) 0.044(7) 0.009(9) -0.013(7) 0.001(10) C6 0.050(8) 0.064(12) 0.051(8) 0.008(10) 0.005(6) -0.001(9) C7 0.222(18) 0.133(13) 0.046(6) 0.029(7) 0.032(8) 0.119(13) C2X 0.055(11) 0.064(12) 0.051(8) 0.033(10) 0.010(9) 0.032(9) C3X 0.075(13) 0.056(13) 0.050(8) 0.021(10) 0.022(9) 0.034(10) C5X 0.054(11) 0.054(13) 0.040(7) 0.025(10) -0.007(7) 0.003(9) C6X 0.051(11) 0.052(12) 0.045(8) 0.006(10) -0.010(8) 0.018(9) S2 0.044(4) 0.079(7) 0.037(4) 0.019(5) 0.017(3) 0.028(5) O13 0.088(17) 0.083(19) 0.11(2) 0.044(17) 0.034(14) 0.009(16) O14 0.044(9) 0.12(2) 0.042(11) 0.048(13) 0.032(8) 0.042(11) O15 0.033(8) 0.068(13) 0.036(8) 0.014(9) 0.005(6) 0.022(9) C8 0.044(11) 0.141(15) 0.041(9) 0.046(10) 0.019(8) 0.049(10) C9 0.050(10) 0.146(16) 0.045(9) 0.045(11) 0.009(8) 0.051(10) C10 0.072(12) 0.123(16) 0.043(8) 0.042(10) 0.002(9) 0.046(10) C11 0.066(13) 0.115(16) 0.036(8) 0.030(10) 0.010(8) 0.029(10) C12 0.052(11) 0.139(16) 0.046(8) 0.035(10) 0.021(8) 0.049(10) C13 0.040(10) 0.149(16) 0.043(8) 0.044(11) 0.022(8) 0.049(10) C14 0.12(2) 0.09(2) 0.037(9) 0.023(12) 0.023(12) 0.013(17) S2X 0.036(4) 0.038(5) 0.029(4) 0.009(4) 0.012(3) 0.018(4) C8X 0.045(9) 0.111(14) 0.045(9) 0.032(10) 0.027(7) 0.045(10) C9X 0.053(9) 0.134(17) 0.049(9) 0.049(12) 0.019(8) 0.037(11) C10X 0.068(9) 0.137(17) 0.047(9) 0.039(12) 0.011(8) 0.041(12) C11X 0.082(11) 0.121(16) 0.041(9) 0.031(11) 0.026(7) 0.038(13) C12X 0.062(10) 0.132(18) 0.048(9) 0.019(12) 0.038(8) 0.043(12) C13X 0.045(8) 0.132(16) 0.043(8) 0.030(11) 0.029(7) 0.046(10) C14X 0.14(3) 0.13(3) 0.045(10) 0.027(16) 0.045(13) 0.00(2) S3 0.0615(19) 0.0562(18) 0.088(2) -0.0315(16) -0.0179(16) 0.0398(16) O16 0.124(8) 0.054(5) 0.107(7) -0.005(5) 0.006(6) 0.050(5) O17 0.054(5) 0.070(5) 0.086(6) -0.041(4) -0.019(4) 0.038(4) O18 0.054(4) 0.060(5) 0.082(6) -0.026(4) -0.001(4) 0.033(4) C15 0.048(6) 0.059(6) 0.087(7) -0.045(6) -0.012(5) 0.033(5) C16 0.043(10) 0.048(11) 0.081(9) -0.021(10) 0.005(8) 0.020(9) C17 0.039(10) 0.050(12) 0.082(8) -0.016(10) 0.007(8) 0.012(8) C18 0.042(6) 0.087(8) 0.096(7) -0.068(6) -0.011(5) 0.022(6) C19 0.045(11) 0.105(15) 0.119(10) -0.078(11) -0.017(10) 0.047(11) C20 0.069(13) 0.092(15) 0.111(9) -0.050(12) -0.014(11) 0.059(11) C21 0.065(8) 0.118(12) 0.106(8) -0.063(8) 0.004(7) 0.025(8) C16X 0.036(8) 0.051(12) 0.085(10) -0.021(11) -0.002(7) 0.023(9) C17X 0.040(8) 0.053(13) 0.081(9) -0.019(11) -0.011(7) 0.012(10) C19X 0.042(8) 0.078(15) 0.111(11) -0.065(12) 0.002(8) 0.014(10) C20X 0.035(8) 0.061(13) 0.099(11) -0.060(11) -0.018(8) 0.025(9) S4 0.174(4) 0.072(2) 0.098(3) -0.008(2) 0.079(3) 0.050(3) O19 0.166(10) 0.17(3) 0.15(3) 0.000(19) 0.111(15) -0.011(14) O20 0.30(2) 0.044(11) 0.079(10) 0.032(9) 0.132(14) 0.052(14) O21 0.16(2) 0.067(7) 0.048(10) 0.004(8) -0.015(14) 0.040(11) O19X 0.269(17) 0.073(12) 0.084(15) 0.056(11) 0.055(15) -0.007(15) O20X 0.227(12) 0.116(18) 0.031(8) -0.001(9) 0.037(9) 0.071(14) O21X 0.064(11) 0.044(6) 0.14(2) -0.028(8) 0.078(12) -0.009(7) C22 0.054(5) 0.038(5) 0.081(5) 0.000(4) 0.019(4) 0.018(5) C23 0.034(7) 0.049(14) 0.158(11) -0.006(13) 0.012(8) 0.000(9) C24 0.070(9) 0.053(15) 0.131(10) -0.024(14) -0.045(8) 0.002(12) C25 0.106(8) 0.062(7) 0.060(6) -0.010(6) -0.027(5) 0.037(7) C26 0.071(8) 0.069(13) 0.050(7) -0.007(9) 0.001(6) 0.041(10) C27 0.037(7) 0.045(11) 0.043(7) 0.004(8) -0.002(6) 0.013(8) C28 0.238(19) 0.107(12) 0.053(6) -0.011(8) -0.034(8) 0.077(13) C23X 0.046(12) 0.060(16) 0.138(11) -0.025(14) -0.013(9) 0.022(11) C24X 0.065(11) 0.038(14) 0.119(9) -0.017(13) -0.053(10) 0.015(11) C26X 0.061(11) 0.053(13) 0.053(7) 0.014(10) 0.013(8) 0.029(10) C27X 0.066(11) 0.053(13) 0.051(7) 0.008(11) 0.005(9) 0.042(10) O1W 0.031(3) 0.042(4) 0.069(5) 0.000(3) 0.008(3) 0.017(3) O2W 0.037(4) 0.083(5) 0.043(4) 0.013(4) 0.009(3) 0.026(4) O3W 0.051(4) 0.066(5) 0.084(6) -0.004(4) 0.020(4) 0.031(4) O4W 0.192(11) 0.052(5) 0.129(9) -0.010(5) -0.106(8) 0.052(6) O5W 0.047(4) 0.081(5) 0.068(5) 0.009(4) 0.005(4) 0.015(4) O6W 0.044(5) 0.060(5) 0.182(10) 0.051(6) -0.019(5) 0.010(4) O7W 0.205(13) 0.101(8) 0.143(11) 0.076(8) -0.030(9) -0.004(9) O8W 0.153(18) 0.133(17) 0.137(18) 0.048(15) 0.059(15) 0.092(15) O8WX 0.156(18) 0.016(7) 0.16(2) -0.021(10) -0.088(16) 0.039(10) O8WY 0.028(6) 0.027(6) 0.079(10) 0.018(6) -0.014(6) 0.004(5) O9W 0.15(2) 0.071(13) 0.094(15) 0.000(11) -0.025(14) 0.020(13) O9WX 0.037(11) 0.066(13) 0.50(5) -0.06(2) -0.050(19) 0.032(10) O10W 0.094(7) 0.084(7) 0.159(10) 0.006(7) 0.032(7) 0.049(6) O11W 0.092(7) 0.046(5) 0.134(9) 0.030(5) 0.011(6) 0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O3 2.163(5) . ? W1 O2 2.174(6) . ? W1 O1 2.198(5) . ? W1 Se4 2.4095(8) . ? W1 Se2 2.4161(8) . ? W1 Se1 2.4664(8) . ? W1 W2 2.7661(5) . ? W1 W3 2.7708(5) . ? W2 O4 2.159(5) . ? W2 O6 2.190(5) . ? W2 O5 2.201(5) . ? W2 Se3 2.4045(9) . ? W2 Se2 2.4255(8) . ? W2 Se1 2.4673(9) . ? W2 W3 2.7540(5) . ? W3 O9 2.155(6) . ? W3 O7 2.155(7) . ? W3 O8 2.295(6) . ? W3 Se3 2.4130(10) . ? W3 Se4 2.4201(8) . ? W3 Se1 2.4843(10) . ? S1 O10 1.449(6) . ? S1 O11 1.450(6) . ? S1 O12 1.467(5) . ? S1 C1 1.771(8) . ? C1 C2X 1.345(12) . ? C1 C6 1.347(12) . ? C1 C2 1.395(12) . ? C1 C6X 1.403(12) . ? C2 C3 1.393(13) . ? C3 C4 1.387(12) . ? C4 C5 1.335(12) . ? C4 C3X 1.343(12) . ? C4 C5X 1.385(13) . ? C4 C7 1.494(11) . ? C5 C6 1.376(13) . ? C2X C3X 1.372(13) . ? C5X C6X 1.393(14) . ? S2 O14 1.453(10) . ? S2 O15 1.465(11) . ? S2 O13 1.474(14) . ? S2 C8 1.750(12) . ? C8 C9 1.373(13) . ? C8 C13 1.375(13) . ? C9 C10 1.375(13) . ? C10 C11 1.364(13) . ? C11 C12 1.365(13) . ? C11 C14 1.501(14) . ? C12 C13 1.372(13) . ? S2X O14X 1.441(12) . ? S2X O13X 1.446(13) . ? S2X O15X 1.472(12) . ? S2X C8X 1.779(13) . ? C8X C9X 1.387(13) . ? C8X C13X 1.388(13) . ? C9X C10X 1.375(14) . ? C10X C11X 1.363(13) . ? C11X C12X 1.365(13) . ? C11X C14X 1.498(15) . ? C12X C13X 1.374(13) . ? S3 O16 1.419(9) . ? S3 O18 1.449(7) . ? S3 O17 1.478(8) . ? S3 C15 1.744(10) . ? C15 C16 1.355(12) . ? C15 C16X 1.359(12) . ? C15 C20 1.396(12) . ? C15 C20X 1.410(13) . ? C16 C17 1.362(13) . ? C17 C18 1.359(12) . ? C18 C17X 1.347(13) . ? C18 C19X 1.376(12) . ? C18 C19 1.392(13) . ? C18 C21 1.502(12) . ? C19 C20 1.390(14) . ? C16X C17X 1.374(14) . ? C19X C20X 1.391(14) . ? S4 O19X 1.403(18) . ? S4 O21 1.414(15) . ? S4 O21X 1.463(13) . ? S4 O20 1.486(18) . ? S4 O19 1.496(19) . ? S4 O20X 1.500(19) . ? S4 C22 1.728(10) . ? C22 C27X 1.373(12) . ? C22 C23 1.374(13) . ? C22 C27 1.380(12) . ? C22 C23X 1.383(13) . ? C23 C24 1.371(14) . ? C24 C25 1.361(13) . ? C25 C24X 1.359(13) . ? C25 C26 1.364(12) . ? C25 C26X 1.364(12) . ? C25 C28 1.499(12) . ? C26 C27 1.370(13) . ? C23X C24X 1.373(14) . ? C26X C27X 1.369(13) . ? 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 O2 79.1(2) . . ? O3 W1 O1 78.0(2) . . ? O2 W1 O1 76.5(2) . . ? O3 W1 Se4 90.23(16) . . ? O2 W1 Se4 160.40(15) . . ? O1 W1 Se4 85.27(13) . . ? O3 W1 Se2 163.31(17) . . ? O2 W1 Se2 90.64(17) . . ? O1 W1 Se2 86.82(14) . . ? Se4 W1 Se2 95.54(3) . . ? O3 W1 Se1 83.01(15) . . ? O2 W1 Se1 85.83(17) . . ? O1 W1 Se1 156.14(14) . . ? Se4 W1 Se1 109.35(3) . . ? Se2 W1 Se1 109.59(3) . . ? O3 W1 W2 138.84(15) . . ? O2 W1 W2 98.55(15) . . ? O1 W1 W2 141.99(14) . . ? Se4 W1 W2 100.26(2) . . ? Se2 W1 W2 55.32(2) . . ? Se1 W1 W2 55.91(2) . . ? O3 W1 W3 97.26(17) . . ? O2 W1 W3 141.99(17) . . ? O1 W1 W3 140.31(13) . . ? Se4 W1 W3 55.17(2) . . ? Se2 W1 W3 98.90(2) . . ? Se1 W1 W3 56.27(2) . . ? W2 W1 W3 59.654(12) . . ? O4 W2 O6 76.4(2) . . ? O4 W2 O5 77.1(2) . . ? O6 W2 O5 76.8(2) . . ? O4 W2 Se3 93.28(16) . . ? O6 W2 Se3 84.53(16) . . ? O5 W2 Se3 160.51(15) . . ? O4 W2 Se2 160.83(16) . . ? O6 W2 Se2 87.29(14) . . ? O5 W2 Se2 89.59(15) . . ? Se3 W2 Se2 95.09(3) . . ? O4 W2 Se1 83.87(15) . . ? O6 W2 Se1 156.24(14) . . ? O5 W2 Se1 86.13(15) . . ? Se3 W2 Se1 109.95(3) . . ? Se2 W2 Se1 109.24(3) . . ? O4 W2 W3 99.83(16) . . ? O6 W2 W3 139.60(16) . . ? O5 W2 W3 142.48(15) . . ? Se3 W2 W3 55.28(2) . . ? Se2 W2 W3 99.12(2) . . ? Se1 W2 W3 56.50(2) . . ? O4 W2 W1 139.75(14) . . ? O6 W2 W1 142.16(14) . . ? O5 W2 W1 97.84(14) . . ? Se3 W2 W1 100.34(2) . . ? Se2 W2 W1 55.00(2) . . ? Se1 W2 W1 55.88(2) . . ? W3 W2 W1 60.258(13) . . ? O9 W3 O7 76.7(3) . . ? O9 W3 O8 78.1(3) . . ? O7 W3 O8 79.5(3) . . ? O9 W3 Se3 91.08(19) . . ? O7 W3 Se3 159.8(2) . . ? O8 W3 Se3 82.40(19) . . ? O9 W3 Se4 160.0(2) . . ? O7 W3 Se4 89.89(19) . . ? O8 W3 Se4 84.91(16) . . ? Se3 W3 Se4 97.26(3) . . ? O9 W3 Se1 85.7(2) . . ? O7 W3 Se1 86.2(2) . . ? O8 W3 Se1 160.49(17) . . ? Se3 W3 Se1 109.10(3) . . ? Se4 W3 Se1 108.41(3) . . ? O9 W3 W2 99.4(2) . . ? O7 W3 W2 142.1(2) . . ? O8 W3 W2 137.37(19) . . ? Se3 W3 W2 54.99(2) . . ? Se4 W3 W2 100.33(2) . . ? Se1 W3 W2 55.91(2) . . ? O9 W3 W1 141.4(2) . . ? O7 W3 W1 99.5(2) . . ? O8 W3 W1 139.70(16) . . ? Se3 W3 W1 99.99(2) . . ? Se4 W3 W1 54.81(2) . . ? Se1 W3 W1 55.66(2) . . ? W2 W3 W1 60.088(12) . . ? W1 Se1 W2 68.20(2) . . ? W1 Se1 W3 68.07(2) . . ? W2 Se1 W3 67.58(2) . . ? W1 Se2 W2 69.68(2) . . ? W2 Se3 W3 69.73(3) . . ? W1 Se4 W3 70.02(2) . . ? O10 S1 O11 112.6(4) . . ? O10 S1 O12 112.1(4) . . ? O11 S1 O12 111.6(4) . . ? O10 S1 C1 106.6(4) . . ? O11 S1 C1 106.7(4) . . ? O12 S1 C1 106.8(4) . . ? C2X C1 C6 97.6(12) . . ? C2X C1 C2 43.7(8) . . ? C6 C1 C2 118.9(10) . . ? C2X C1 C6X 118.3(11) . . ? C6 C1 C6X 39.6(10) . . ? C2 C1 C6X 109.1(11) . . ? C2X C1 S1 122.7(8) . . ? C6 C1 S1 119.9(8) . . ? C2 C1 S1 121.0(7) . . ? C6X C1 S1 118.1(8) . . ? C3 C2 C1 118.2(12) . . ? C4 C3 C2 122.0(12) . . ? C5 C4 C3X 98.1(12) . . ? C5 C4 C5X 33.2(10) . . ? C3X C4 C5X 115.6(11) . . ? C5 C4 C3 117.1(11) . . ? C3X C4 C3 45.7(9) . . ? C5X C4 C3 108.0(12) . . ? C5 C4 C7 119.7(11) . . ? C3X C4 C7 122.4(10) . . ? C5X C4 C7 119.7(10) . . ? C3 C4 C7 123.2(11) . . ? C4 C5 C6 122.3(13) . . ? C1 C6 C5 120.9(13) . . ? C1 C2X C3X 121.7(13) . . ? C4 C3X C2X 121.7(13) . . ? C4 C5X C6X 122.3(13) . . ? C5X C6X C1 117.6(13) . . ? O14 S2 O15 112.5(10) . . ? O14 S2 O13 111.2(12) . . ? O15 S2 O13 111.2(12) . . ? O14 S2 C8 106.9(10) . . ? O15 S2 C8 108.2(9) . . ? O13 S2 C8 106.5(11) . . ? C9 C8 C13 120.5(13) . . ? C9 C8 S2 121.2(13) . . ? C13 C8 S2 118.0(12) . . ? C8 C9 C10 118.8(14) . . ? C11 C10 C9 121.9(14) . . ? C10 C11 C12 117.6(13) . . ? C10 C11 C14 120.1(15) . . ? C12 C11 C14 121.3(15) . . ? C11 C12 C13 122.1(14) . . ? C12 C13 C8 118.6(13) . . ? O14X S2X O13X 115.1(12) . . ? O14X S2X O15X 111.5(12) . . ? O13X S2X O15X 111.8(11) . . ? O14X S2X C8X 106.0(11) . . ? O13X S2X C8X 108.2(11) . . ? O15X S2X C8X 103.3(10) . . ? C9X C8X C13X 116.8(13) . . ? C9X C8X S2X 124.5(13) . . ? C13X C8X S2X 118.6(12) . . ? C10X C9X C8X 121.1(15) . . ? C11X C10X C9X 121.6(15) . . ? C10X C11X C12X 117.5(14) . . ? C10X C11X C14X 122.6(16) . . ? C12X C11X C14X 119.9(16) . . ? C11X C12X C13X 122.2(14) . . ? C12X C13X C8X 120.5(14) . . ? O16 S3 O18 114.0(6) . . ? O16 S3 O17 111.9(5) . . ? O18 S3 O17 110.9(4) . . ? O16 S3 C15 106.3(5) . . ? O18 S3 C15 107.6(4) . . ? O17 S3 C15 105.5(5) . . ? C16 C15 C16X 37.0(8) . . ? C16 C15 C20 118.4(11) . . ? C16X C15 C20 99.1(11) . . ? C16 C15 C20X 100.2(12) . . ? C16X C15 C20X 116.6(11) . . ? C20 C15 C20X 55.3(13) . . ? C16 C15 S3 120.7(8) . . ? C16X C15 S3 123.9(9) . . ? C20 C15 S3 120.4(9) . . ? C20X C15 S3 118.3(8) . . ? C15 C16 C17 120.8(13) . . ? C18 C17 C16 122.3(13) . . ? C17X C18 C17 34.1(9) . . ? C17X C18 C19X 118.8(11) . . ? C17 C18 C19X 100.6(12) . . ? C17X C18 C19 100.4(14) . . ? C17 C18 C19 116.2(11) . . ? C19X C18 C19 57.0(14) . . ? C17X C18 C21 119.9(10) . . ? C17 C18 C21 120.0(11) . . ? C19X C18 C21 119.5(11) . . ? C19 C18 C21 122.6(10) . . ? C20 C19 C18 121.0(12) . . ? C19 C20 C15 118.9(13) . . ? C15 C16X C17X 122.3(14) . . ? C18 C17X C16X 120.3(14) . . ? C18 C19X C20X 119.8(13) . . ? C19X C20X C15 120.1(13) . . ? O19X S4 O21 127(2) . . ? O19X S4 O21X 116.7(14) . . ? O21 S4 O21X 23.0(14) . . ? O19X S4 O20 73.8(13) . . ? O21 S4 O20 117.1(14) . . ? O21X S4 O20 138.3(14) . . ? O19X S4 O19 36.1(14) . . ? O21 S4 O19 107.3(16) . . ? O21X S4 O19 88.4(17) . . ? O20 S4 O19 109.9(15) . . ? O19X S4 O20X 126.6(14) . . ? O21 S4 O20X 73.8(13) . . ? O21X S4 O20X 96.2(11) . . ? O20 S4 O20X 54.6(11) . . ? O19 S4 O20X 159.2(16) . . ? O19X S4 C22 108.9(12) . . ? O21 S4 C22 113.0(13) . . ? O21X S4 C22 103.3(11) . . ? O20 S4 C22 111.0(7) . . ? O19 S4 C22 96.3(14) . . ? O20X S4 C22 102.2(7) . . ? C27X C22 C23 109.9(12) . . ? C27X C22 C27 32.0(10) . . ? C23 C22 C27 118.0(11) . . ? C27X C22 C23X 118.3(12) . . ? C23 C22 C23X 28.9(10) . . ? C27 C22 C23X 109.2(12) . . ? C27X C22 S4 121.7(9) . . ? C23 C22 S4 119.9(10) . . ? C27 C22 S4 122.0(9) . . ? C23X C22 S4 119.9(10) . . ? C24 C23 C22 120.7(14) . . ? C25 C24 C23 121.5(14) . . ? C24X C25 C24 27.8(11) . . ? C24X C25 C26 109.4(12) . . ? C24 C25 C26 117.6(12) . . ? C24X C25 C26X 117.0(12) . . ? C24 C25 C26X 107.2(14) . . ? C26 C25 C26X 35.2(11) . . ? C24X C25 C28 120.9(11) . . ? C24 C25 C28 119.2(11) . . ? C26 C25 C28 123.2(11) . . ? C26X C25 C28 121.3(11) . . ? C25 C26 C27 122.2(13) . . ? C26 C27 C22 119.8(12) . . ? C24X C23X C22 119.8(15) . . ? C25 C24X C23X 122.2(15) . . ? C25 C26X C27X 121.9(14) . . ? C26X C27X C22 120.0(14) . . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 5.288 _refine_diff_density_min -2.441 _refine_diff_density_rms 0.208 #===END data_ags34 _database_code_CSD 158610 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H108 As Mo6 O50 S8 Se8' _chemical_formula_weight 3120.14 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' 'As' 'As' 0.0499 2.0058 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c 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' _cell_length_a 12.3516(11) _cell_length_b 34.072(3) _cell_length_c 11.9253(11) _cell_angle_alpha 90.00 _cell_angle_beta 92.645(4) _cell_angle_gamma 90.00 _cell_volume 5013.4(8) _cell_formula_units_Z 2 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 19942 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 28.53 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.067 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3058 _exptl_absorpt_coefficient_mu 4.216 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.297 _exptl_absorpt_correction_T_max 0.920 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 43190 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0710 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 28.50 _reflns_number_total 11896 _reflns_number_gt 8351 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom for CH, free with restraints for OH' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00035(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 11896 _refine_ls_number_parameters 666 _refine_ls_number_restraints 403 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0764 _refine_ls_wR_factor_gt 0.0712 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 0.914 _refine_ls_shift/su_max 0.018 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.27745(3) 0.486553(11) 0.61793(3) 0.01173(8) Uani 1 1 d . . . Mo2 Mo 0.17738(3) 0.546002(10) 0.72764(3) 0.01188(8) Uani 1 1 d . . . Mo3 Mo 0.12594(3) 0.469031(11) 0.77719(3) 0.01191(8) Uani 1 1 d . . . As1 As 0.0000 0.5000 0.5000 0.01734(14) Uani 1 2 d S . . Se1 Se 0.30473(3) 0.498974(13) 0.82064(3) 0.01455(10) Uani 1 1 d . . . Se2 Se 0.17736(3) 0.540061(12) 0.52214(3) 0.01300(9) Uani 1 1 d . . . Se3 Se 0.11881(3) 0.443947(12) 0.58350(3) 0.01318(9) Uani 1 1 d . . . Se4 Se -0.00751(3) 0.518730(12) 0.71339(3) 0.01401(10) Uani 1 1 d . . . O1 O 0.3209(2) 0.47083(9) 0.4477(2) 0.0177(7) Uani 1 1 d D . . H1A H 0.307(4) 0.4853(9) 0.400(3) 0.027 Uiso 1 1 d D . . H1B H 0.303(4) 0.4505(6) 0.426(3) 0.027 Uiso 1 1 d D . . O2 O 0.4336(2) 0.51418(9) 0.6012(2) 0.0172(6) Uani 1 1 d D . . H2A H 0.458(4) 0.5270(10) 0.649(2) 0.026 Uiso 1 1 d D . . H2B H 0.428(4) 0.5266(11) 0.549(2) 0.026 Uiso 1 1 d D . . O3 O 0.3792(2) 0.43603(9) 0.6452(3) 0.0218(7) Uani 1 1 d D . . H3A H 0.361(3) 0.4152(7) 0.659(4) 0.033 Uiso 1 1 d D . . H3B H 0.4376(17) 0.4361(12) 0.631(4) 0.033 Uiso 1 1 d D . . O4 O 0.3141(2) 0.58577(9) 0.7364(3) 0.0195(7) Uani 1 1 d D . . H4A H 0.312(3) 0.6051(8) 0.705(4) 0.029 Uiso 1 1 d D . . H4B H 0.3723(17) 0.5802(12) 0.748(4) 0.029 Uiso 1 1 d D . . O5 O 0.1621(2) 0.56913(10) 0.8946(2) 0.0196(7) Uani 1 1 d D . . H5A H 0.172(3) 0.5547(11) 0.943(3) 0.029 Uiso 1 1 d D . . H5B H 0.109(2) 0.5794(12) 0.905(4) 0.029 Uiso 1 1 d D . . O6 O 0.0981(2) 0.60344(9) 0.6974(2) 0.0180(7) Uani 1 1 d D . . H6A H 0.0363(13) 0.6035(13) 0.699(3) 0.027 Uiso 1 1 d D . . H6B H 0.112(3) 0.6140(13) 0.644(2) 0.027 Uiso 1 1 d D . . O7 O 0.0954(2) 0.47618(9) 0.9529(2) 0.0179(7) Uani 1 1 d D . . H7A H 0.126(3) 0.4896(11) 0.993(3) 0.027 Uiso 1 1 d D . . H7B H 0.069(3) 0.4601(10) 0.986(3) 0.027 Uiso 1 1 d D . . O8 O 0.1952(2) 0.41431(9) 0.8430(2) 0.0194(7) Uani 1 1 d D . . H8A H 0.217(4) 0.4108(13) 0.9037(16) 0.029 Uiso 1 1 d D . . H8B H 0.217(4) 0.3978(10) 0.808(3) 0.029 Uiso 1 1 d D . . O9 O -0.0171(2) 0.43349(9) 0.8042(3) 0.0179(7) Uani 1 1 d D . . H9A H -0.024(3) 0.4138(8) 0.775(4) 0.027 Uiso 1 1 d D . . H9B H -0.072(2) 0.4412(11) 0.820(4) 0.027 Uiso 1 1 d D . . S1 S 0.30345(8) 0.52306(3) 0.15185(8) 0.0156(2) Uani 1 1 d . . . O10 O 0.2917(2) 0.52274(9) 0.2736(2) 0.0215(7) Uani 1 1 d . . . O11 O 0.1956(2) 0.52953(9) 0.0941(2) 0.0186(7) Uani 1 1 d . . . O12 O 0.3571(2) 0.48889(9) 0.1095(2) 0.0228(7) Uani 1 1 d . . . C1 C 0.3820(3) 0.56457(13) 0.1233(3) 0.0175(9) Uani 1 1 d . . . C2 C 0.3594(4) 0.60004(13) 0.1744(4) 0.0225(10) Uani 1 1 d . . . H2 H 0.3017 0.6018 0.2242 0.027 Uiso 1 1 calc R . . C3 C 0.4206(4) 0.63261(14) 0.1527(4) 0.0290(11) Uani 1 1 d . . . H3 H 0.4066 0.6567 0.1897 0.035 Uiso 1 1 calc R . . C4 C 0.5033(4) 0.63070(14) 0.0768(4) 0.0254(11) Uani 1 1 d . . . C5 C 0.5250(4) 0.59512(15) 0.0259(4) 0.0274(11) Uani 1 1 d . . . H5 H 0.5813 0.5934 -0.0254 0.033 Uiso 1 1 calc R . . C6 C 0.4645(3) 0.56185(14) 0.0498(4) 0.0218(10) Uani 1 1 d . . . H6 H 0.4802 0.5374 0.0156 0.026 Uiso 1 1 calc R . . C7 C 0.5689(4) 0.66698(15) 0.0507(4) 0.0407(14) Uani 1 1 d . . . H7C H 0.6463 0.6607 0.0571 0.061 Uiso 1 1 calc R . . H7D H 0.5530 0.6879 0.1040 0.061 Uiso 1 1 calc R . . H7E H 0.5497 0.6758 -0.0258 0.061 Uiso 1 1 calc R . . S2 S 0.11742(8) 0.38446(3) 0.10866(9) 0.0186(2) Uani 1 1 d . . . O13 O 0.1113(2) 0.38185(9) 0.2306(2) 0.0219(7) Uani 1 1 d . . . O14 O 0.2245(2) 0.39516(9) 0.0732(2) 0.0252(7) Uani 1 1 d . . . O15 O 0.0344(2) 0.41135(9) 0.0602(2) 0.0223(7) Uani 1 1 d . . . C8 C 0.0846(3) 0.33786(13) 0.0524(4) 0.0191(10) Uani 1 1 d . . . C9 C 0.0326(4) 0.33477(15) -0.0520(4) 0.0280(11) Uani 1 1 d . . . H9 H 0.0110 0.3577 -0.0925 0.034 Uiso 1 1 calc R . . C10 C 0.0124(4) 0.29814(15) -0.0971(4) 0.0303(12) Uani 1 1 d . . . H10 H -0.0225 0.2962 -0.1695 0.036 Uiso 1 1 calc R . . C11 C 0.0415(4) 0.26424(15) -0.0399(4) 0.0288(11) Uani 1 1 d . . . C12 C 0.0917(4) 0.26815(15) 0.0654(4) 0.0374(13) Uani 1 1 d . . . H12 H 0.1110 0.2453 0.1074 0.045 Uiso 1 1 calc R . . C13 C 0.1143(4) 0.30460(15) 0.1106(4) 0.0329(12) Uani 1 1 d . . . H13 H 0.1505 0.3067 0.1823 0.039 Uiso 1 1 calc R . . C14 C 0.0189(4) 0.22414(15) -0.0890(5) 0.0405(14) Uani 1 1 d . . . H14A H -0.0515 0.2148 -0.0654 0.061 Uiso 1 1 calc R . . H14B H 0.0758 0.2059 -0.0625 0.061 Uiso 1 1 calc R . . H14C H 0.0178 0.2257 -0.1711 0.061 Uiso 1 1 calc R . . S3 S 0.26597(9) 0.84561(3) 1.00936(10) 0.0226(3) Uani 1 1 d . . . O16 O 0.3241(3) 0.86441(11) 0.9226(3) 0.0509(11) Uani 1 1 d . . . O17 O 0.3178(3) 0.84941(10) 1.1201(3) 0.0404(10) Uani 1 1 d . . . O18 O 0.1532(3) 0.85900(9) 1.0101(3) 0.0269(8) Uani 1 1 d . . . C15 C 0.2610(3) 0.79510(13) 0.9782(4) 0.0202(10) Uani 1 1 d . . . C16 C 0.2172(4) 0.78307(15) 0.8751(4) 0.0332(12) Uani 1 1 d . . . H16 H 0.1932 0.8018 0.8205 0.040 Uiso 1 1 calc R . . C17 C 0.2089(4) 0.74330(16) 0.8523(4) 0.0374(13) Uani 1 1 d . . . H17 H 0.1789 0.7352 0.7813 0.045 Uiso 1 1 calc R . . C18 C 0.2423(4) 0.71527(14) 0.9283(4) 0.0291(12) Uani 1 1 d . . . C19 C 0.2867(4) 0.72815(15) 1.0292(4) 0.0363(13) Uani 1 1 d . . . H19 H 0.3116 0.7093 1.0831 0.044 Uiso 1 1 calc R . . C20 C 0.2965(4) 0.76731(14) 1.0553(4) 0.0298(12) Uani 1 1 d . . . H20 H 0.3276 0.7752 1.1261 0.036 Uiso 1 1 calc R . . C21 C 0.2311(5) 0.67196(15) 0.9025(5) 0.0491(16) Uani 1 1 d . . . H21A H 0.3028 0.6597 0.9066 0.074 Uiso 1 1 calc R . . H21B H 0.1979 0.6686 0.8269 0.074 Uiso 1 1 calc R . . H21C H 0.1852 0.6596 0.9574 0.074 Uiso 1 1 calc R . . S4 S 0.26013(10) 0.33735(4) 0.63417(10) 0.0268(3) Uani 1 1 d . . . O19 O 0.2931(3) 0.34351(10) 0.5217(3) 0.0472(11) Uani 1 1 d . . . O20 O 0.1448(3) 0.33171(10) 0.6448(3) 0.0444(10) Uani 1 1 d . . . O21 O 0.3018(2) 0.36875(9) 0.7098(2) 0.0257(7) Uani 1 1 d . . . C22 C 0.3228(3) 0.29370(12) 0.6813(4) 0.0190(10) Uani 1 1 d . . . C23 C 0.4170(4) 0.28106(14) 0.6353(4) 0.0281(11) Uani 1 1 d . . . H23 H 0.4506 0.2964 0.5803 0.034 Uiso 1 1 calc R . . C24 C 0.4620(4) 0.24574(15) 0.6703(4) 0.0325(12) Uani 1 1 d . . . H24 H 0.5269 0.2369 0.6387 0.039 Uiso 1 1 calc R . . C25 C 0.4141(4) 0.22288(14) 0.7506(4) 0.0275(11) Uani 1 1 d . . . C26 C 0.3232(4) 0.23716(14) 0.7998(4) 0.0260(11) Uani 1 1 d . . . H26 H 0.2919 0.2226 0.8580 0.031 Uiso 1 1 calc R . . C27 C 0.2774(4) 0.27207(13) 0.7657(4) 0.0241(10) Uani 1 1 d . . . H27 H 0.2145 0.2815 0.7999 0.029 Uiso 1 1 calc R . . C28 C 0.4582(5) 0.18266(15) 0.7808(5) 0.0451(15) Uani 1 1 d . . . H28A H 0.4598 0.1793 0.8625 0.068 Uiso 1 1 calc R . . H28B H 0.5318 0.1801 0.7544 0.068 Uiso 1 1 calc R . . H28C H 0.4116 0.1625 0.7452 0.068 Uiso 1 1 calc R . . O1W O 0.9565(3) 0.13097(11) 0.1959(3) 0.0298(8) Uani 1 1 d D . . H1WA H 0.930(3) 0.1278(16) 0.139(2) 0.045 Uiso 1 1 d D . . H1WB H 1.014(2) 0.1385(16) 0.189(4) 0.045 Uiso 1 1 d D . . O2W O 0.2994(3) 0.09970(9) 0.8630(3) 0.0240(7) Uani 1 1 d D . . H2WB H 0.252(3) 0.1025(14) 0.822(3) 0.036 Uiso 1 1 d D . . H2WA H 0.297(4) 0.1152(11) 0.909(3) 0.036 Uiso 1 1 d D . . O3W O 0.5290(2) 0.93666(10) 0.2530(3) 0.0214(7) Uani 1 1 d D . . H3WA H 0.556(3) 0.9501(12) 0.295(3) 0.032 Uiso 1 1 d D . . H3WB H 0.570(3) 0.9259(12) 0.220(3) 0.032 Uiso 1 1 d D . . O4W O 0.4232(3) 0.93559(9) 0.9267(2) 0.0209(7) Uani 1 1 d D . . H4WB H 0.413(4) 0.9143(6) 0.936(4) 0.031 Uiso 1 1 d D . . H4WA H 0.396(4) 0.9427(11) 0.873(2) 0.031 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01071(16) 0.01437(19) 0.01026(17) 0.00013(14) 0.00200(13) 0.00078(14) Mo2 0.01113(17) 0.0138(2) 0.01079(17) 0.00019(14) 0.00117(13) 0.00033(14) Mo3 0.01130(17) 0.0142(2) 0.01032(17) 0.00012(14) 0.00153(13) 0.00005(14) As1 0.0166(3) 0.0181(3) 0.0176(3) 0.0021(3) 0.0046(2) 0.0015(3) Se1 0.0133(2) 0.0182(2) 0.0122(2) 0.00046(17) 0.00036(16) 0.00023(17) Se2 0.0120(2) 0.0149(2) 0.0122(2) 0.00133(17) 0.00186(16) 0.00036(16) Se3 0.0122(2) 0.0154(2) 0.0121(2) -0.00085(17) 0.00203(16) -0.00006(16) Se4 0.01144(19) 0.0159(2) 0.0148(2) 0.00141(17) 0.00265(16) 0.00040(17) O1 0.0248(17) 0.0171(17) 0.0116(15) -0.0013(13) 0.0038(13) -0.0002(14) O2 0.0132(15) 0.0229(18) 0.0154(15) 0.0014(13) 0.0017(13) -0.0035(13) O3 0.0167(16) 0.0143(17) 0.0351(19) 0.0089(15) 0.0091(15) 0.0039(13) O4 0.0156(15) 0.0164(18) 0.0263(18) 0.0076(14) -0.0015(14) 0.0001(13) O5 0.0210(17) 0.025(2) 0.0131(16) 0.0012(13) 0.0011(13) 0.0058(14) O6 0.0162(15) 0.0200(18) 0.0182(16) 0.0053(13) 0.0042(13) 0.0031(14) O7 0.0200(17) 0.0189(19) 0.0149(16) -0.0009(13) 0.0038(13) -0.0021(13) O8 0.0255(17) 0.0190(18) 0.0140(15) 0.0027(13) 0.0038(14) 0.0101(14) O9 0.0160(15) 0.0127(17) 0.0253(18) 0.0002(13) 0.0044(13) -0.0014(13) S1 0.0163(5) 0.0193(6) 0.0112(5) 0.0016(4) 0.0006(4) 0.0004(4) O10 0.0267(17) 0.0274(19) 0.0107(15) 0.0029(13) 0.0022(13) -0.0047(14) O11 0.0146(15) 0.0258(18) 0.0153(15) 0.0010(13) -0.0010(12) -0.0009(13) O12 0.0278(17) 0.0176(17) 0.0235(17) -0.0027(13) 0.0057(14) 0.0004(13) C1 0.016(2) 0.025(3) 0.011(2) 0.0005(18) -0.0005(17) -0.0025(18) C2 0.023(2) 0.026(3) 0.019(2) 0.003(2) 0.0061(19) 0.005(2) C3 0.036(3) 0.023(3) 0.027(3) 0.000(2) -0.003(2) 0.001(2) C4 0.028(3) 0.030(3) 0.017(2) 0.006(2) -0.007(2) -0.009(2) C5 0.024(2) 0.040(3) 0.019(2) -0.004(2) 0.004(2) -0.011(2) C6 0.026(2) 0.021(3) 0.019(2) -0.0030(19) 0.0021(19) 0.000(2) C7 0.050(3) 0.036(3) 0.035(3) 0.005(3) -0.003(3) -0.018(3) S2 0.0162(5) 0.0237(6) 0.0164(5) 0.0047(5) 0.0045(4) 0.0039(4) O13 0.0216(16) 0.0312(19) 0.0131(15) 0.0050(13) 0.0039(13) 0.0027(14) O14 0.0178(16) 0.034(2) 0.0248(17) 0.0080(15) 0.0076(14) 0.0011(14) O15 0.0225(16) 0.0230(18) 0.0220(17) 0.0083(14) 0.0069(13) 0.0084(13) C8 0.017(2) 0.021(3) 0.020(2) 0.0037(19) 0.0062(18) 0.0043(18) C9 0.033(3) 0.028(3) 0.024(3) 0.005(2) 0.002(2) 0.002(2) C10 0.030(3) 0.038(3) 0.022(3) 0.000(2) -0.004(2) -0.002(2) C11 0.018(2) 0.034(3) 0.035(3) -0.003(2) 0.007(2) -0.001(2) C12 0.046(3) 0.025(3) 0.040(3) 0.012(2) -0.008(3) 0.006(2) C13 0.043(3) 0.029(3) 0.026(3) 0.005(2) -0.008(2) 0.009(2) C14 0.033(3) 0.036(3) 0.053(4) -0.006(3) 0.004(3) -0.004(2) S3 0.0227(6) 0.0173(6) 0.0279(6) -0.0052(5) 0.0025(5) -0.0006(5) O16 0.068(3) 0.029(2) 0.058(3) -0.0049(19) 0.038(2) -0.014(2) O17 0.042(2) 0.030(2) 0.047(2) -0.0198(17) -0.0228(18) 0.0124(17) O18 0.0282(18) 0.0276(19) 0.0250(17) -0.0051(15) 0.0012(14) 0.0080(15) C15 0.017(2) 0.019(3) 0.025(2) -0.003(2) 0.0067(19) -0.0013(18) C16 0.041(3) 0.033(3) 0.025(3) -0.003(2) -0.006(2) 0.005(2) C17 0.036(3) 0.039(3) 0.037(3) -0.018(3) -0.001(2) -0.003(3) C18 0.025(3) 0.022(3) 0.042(3) -0.013(2) 0.012(2) -0.003(2) C19 0.050(3) 0.024(3) 0.035(3) 0.007(2) 0.002(3) 0.002(2) C20 0.038(3) 0.024(3) 0.026(3) -0.005(2) 0.000(2) 0.002(2) C21 0.053(4) 0.029(3) 0.067(4) -0.015(3) 0.016(3) -0.010(3) S4 0.0360(7) 0.0190(7) 0.0253(6) 0.0009(5) 0.0000(5) 0.0071(5) O19 0.088(3) 0.030(2) 0.025(2) 0.0083(16) 0.009(2) 0.020(2) O20 0.0262(19) 0.030(2) 0.075(3) -0.003(2) -0.0124(19) 0.0062(16) O21 0.0316(18) 0.0180(18) 0.0281(18) 0.0012(14) 0.0073(15) 0.0012(14) C22 0.024(2) 0.014(2) 0.020(2) -0.0022(18) 0.0001(19) -0.0004(18) C23 0.033(3) 0.025(3) 0.027(3) 0.002(2) 0.011(2) 0.004(2) C24 0.027(3) 0.033(3) 0.038(3) 0.000(2) 0.005(2) 0.007(2) C25 0.030(3) 0.023(3) 0.029(3) 0.000(2) -0.008(2) 0.001(2) C26 0.027(3) 0.028(3) 0.022(2) 0.003(2) 0.000(2) -0.005(2) C27 0.020(2) 0.024(3) 0.029(3) -0.001(2) 0.004(2) 0.000(2) C28 0.046(3) 0.030(3) 0.058(4) 0.010(3) -0.009(3) 0.008(3) O1W 0.0302(19) 0.032(2) 0.0271(19) 0.0026(16) -0.0059(16) 0.0019(17) O2W 0.0293(19) 0.022(2) 0.0203(18) 0.0015(14) -0.0021(14) 0.0020(15) O3W 0.0137(15) 0.032(2) 0.0190(18) -0.0027(14) 0.0022(13) -0.0010(14) O4W 0.0219(17) 0.0228(19) 0.0183(17) 0.0000(14) 0.0035(13) -0.0023(15) _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 O3 2.147(3) . ? Mo1 O2 2.164(3) . ? Mo1 O1 2.190(3) . ? Mo1 Se2 2.4549(5) . ? Mo1 Se3 2.4579(6) . ? Mo1 Se1 2.4619(6) . ? Mo1 Mo2 2.7370(5) . ? Mo1 Mo3 2.7917(5) . ? Mo2 O5 2.158(3) . ? Mo2 O4 2.164(3) . ? Mo2 O6 2.211(3) . ? Mo2 Se2 2.4590(6) . ? Mo2 Se4 2.4641(5) . ? Mo2 Se1 2.4719(6) . ? Mo2 Mo3 2.7686(5) . ? Mo3 O7 2.160(3) . ? Mo3 O9 2.178(3) . ? Mo3 O8 2.182(3) . ? Mo3 Se4 2.4591(6) . ? Mo3 Se3 2.4607(6) . ? Mo3 Se1 2.4659(6) . ? As1 Se3 2.5803(4) . ? As1 Se3 2.5803(4) 3_566 ? As1 Se2 2.5843(4) 3_566 ? As1 Se2 2.5843(4) . ? As1 Se4 2.6293(5) 3_566 ? As1 Se4 2.6293(5) . ? S1 O12 1.442(3) . ? S1 O10 1.466(3) . ? S1 O11 1.488(3) . ? S1 C1 1.757(4) . ? C1 C6 1.378(6) . ? C1 C2 1.388(6) . ? C2 C3 1.374(6) . ? C3 C4 1.397(6) . ? C4 C5 1.387(7) . ? C4 C7 1.518(6) . ? C5 C6 1.394(6) . ? S2 O14 1.454(3) . ? S2 O13 1.462(3) . ? S2 O15 1.473(3) . ? S2 C8 1.764(5) . ? C8 C13 1.370(6) . ? C8 C9 1.378(6) . ? C9 C10 1.377(7) . ? C10 C11 1.380(7) . ? C11 C12 1.381(7) . ? C11 C14 1.508(7) . ? C12 C13 1.377(7) . ? S3 O16 1.437(4) . ? S3 O17 1.447(3) . ? S3 O18 1.466(3) . ? S3 C15 1.761(5) . ? C15 C20 1.378(6) . ? C15 C16 1.382(6) . ? C16 C17 1.385(7) . ? C17 C18 1.367(7) . ? C18 C19 1.371(7) . ? C18 C21 1.512(7) . ? C19 C20 1.374(6) . ? S4 O19 1.435(3) . ? S4 O20 1.449(4) . ? S4 O21 1.476(3) . ? S4 C22 1.757(4) . ? C22 C23 1.378(6) . ? C22 C27 1.387(6) . ? C23 C24 1.382(6) . ? C24 C25 1.388(7) . ? C25 C26 1.379(6) . ? C25 C28 1.512(6) . ? C26 C27 1.371(6) . ? 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 81.07(11) . . ? O3 Mo1 O1 77.13(12) . . ? O2 Mo1 O1 76.28(11) . . ? O3 Mo1 Se2 160.81(9) . . ? O2 Mo1 Se2 93.78(8) . . ? O1 Mo1 Se2 83.70(8) . . ? O3 Mo1 Se3 90.47(9) . . ? O2 Mo1 Se3 161.56(8) . . ? O1 Mo1 Se3 85.90(8) . . ? Se2 Mo1 Se3 88.879(18) . . ? O3 Mo1 Se1 86.37(9) . . ? O2 Mo1 Se1 86.20(8) . . ? O1 Mo1 Se1 157.48(8) . . ? Se2 Mo1 Se1 111.86(2) . . ? Se3 Mo1 Se1 109.727(18) . . ? O3 Mo1 Mo2 142.66(9) . . ? O2 Mo1 Mo2 98.42(8) . . ? O1 Mo1 Mo2 139.42(8) . . ? Se2 Mo1 Mo2 56.223(15) . . ? Se3 Mo1 Mo2 98.214(17) . . ? Se1 Mo1 Mo2 56.482(14) . . ? O3 Mo1 Mo3 97.56(8) . . ? O2 Mo1 Mo3 141.66(8) . . ? O1 Mo1 Mo3 141.17(8) . . ? Se2 Mo1 Mo3 97.840(17) . . ? Se3 Mo1 Mo3 55.465(14) . . ? Se1 Mo1 Mo3 55.560(14) . . ? Mo2 Mo1 Mo3 60.093(13) . . ? O5 Mo2 O4 80.09(12) . . ? O5 Mo2 O6 76.73(11) . . ? O4 Mo2 O6 78.01(11) . . ? O5 Mo2 Se2 162.50(8) . . ? O4 Mo2 Se2 93.66(9) . . ? O6 Mo2 Se2 86.01(8) . . ? O5 Mo2 Se4 94.66(8) . . ? O4 Mo2 Se4 163.37(8) . . ? O6 Mo2 Se4 85.44(8) . . ? Se2 Mo2 Se4 86.717(17) . . ? O5 Mo2 Se1 84.47(8) . . ? O4 Mo2 Se1 84.56(8) . . ? O6 Mo2 Se1 156.21(8) . . ? Se2 Mo2 Se1 111.381(19) . . ? Se4 Mo2 Se1 110.80(2) . . ? O5 Mo2 Mo1 140.53(8) . . ? O4 Mo2 Mo1 96.77(9) . . ? O6 Mo2 Mo1 141.58(8) . . ? Se2 Mo2 Mo1 56.081(14) . . ? Se4 Mo2 Mo1 97.208(18) . . ? Se1 Mo2 Mo1 56.132(15) . . ? O5 Mo2 Mo3 96.80(9) . . ? O4 Mo2 Mo3 140.28(8) . . ? O6 Mo2 Mo3 140.28(8) . . ? Se2 Mo2 Mo3 98.351(17) . . ? Se4 Mo2 Mo3 55.696(14) . . ? Se1 Mo2 Mo3 55.792(15) . . ? Mo1 Mo2 Mo3 60.932(14) . . ? O7 Mo3 O9 74.93(11) . . ? O7 Mo3 O8 80.24(11) . . ? O9 Mo3 O8 77.23(12) . . ? O7 Mo3 Se4 94.46(9) . . ? O9 Mo3 Se4 83.79(8) . . ? O8 Mo3 Se4 161.02(9) . . ? O7 Mo3 Se3 161.71(8) . . ? O9 Mo3 Se3 87.22(8) . . ? O8 Mo3 Se3 92.15(8) . . ? Se4 Mo3 Se3 87.382(18) . . ? O7 Mo3 Se1 86.82(8) . . ? O9 Mo3 Se1 157.47(8) . . ? O8 Mo3 Se1 86.88(9) . . ? Se4 Mo3 Se1 111.17(2) . . ? Se3 Mo3 Se1 109.502(18) . . ? O7 Mo3 Mo2 98.76(8) . . ? O9 Mo3 Mo2 138.93(8) . . ? O8 Mo3 Mo2 142.76(9) . . ? Se4 Mo3 Mo2 55.865(15) . . ? Se3 Mo3 Mo2 97.314(17) . . ? Se1 Mo3 Mo2 55.999(14) . . ? O7 Mo3 Mo1 142.05(8) . . ? O9 Mo3 Mo1 142.49(8) . . ? O8 Mo3 Mo1 99.42(8) . . ? Se4 Mo3 Mo1 95.914(17) . . ? Se3 Mo3 Mo1 55.371(14) . . ? Se1 Mo3 Mo1 55.425(14) . . ? Mo2 Mo3 Mo1 58.975(12) . . ? Se3 As1 Se3 180.0 . 3_566 ? Se3 As1 Se2 96.478(14) . 3_566 ? Se3 As1 Se2 83.522(14) 3_566 3_566 ? Se3 As1 Se2 83.522(14) . . ? Se3 As1 Se2 96.478(14) 3_566 . ? Se2 As1 Se2 180.000(16) 3_566 . ? Se3 As1 Se4 98.569(13) . 3_566 ? Se3 As1 Se4 81.431(13) 3_566 3_566 ? Se2 As1 Se4 80.822(13) 3_566 3_566 ? Se2 As1 Se4 99.178(13) . 3_566 ? Se3 As1 Se4 81.431(13) . . ? Se3 As1 Se4 98.569(13) 3_566 . ? Se2 As1 Se4 99.178(13) 3_566 . ? Se2 As1 Se4 80.822(13) . . ? Se4 As1 Se4 180.0 3_566 . ? Mo1 Se1 Mo3 69.015(15) . . ? Mo1 Se1 Mo2 67.386(16) . . ? Mo3 Se1 Mo2 68.208(16) . . ? Mo1 Se2 Mo2 67.697(16) . . ? Mo1 Se2 As1 93.531(17) . . ? Mo2 Se2 As1 96.109(16) . . ? Mo1 Se3 Mo3 69.164(16) . . ? Mo1 Se3 As1 93.562(17) . . ? Mo3 Se3 As1 95.752(17) . . ? Mo3 Se4 Mo2 68.439(16) . . ? Mo3 Se4 As1 94.544(16) . . ? Mo2 Se4 As1 94.838(15) . . ? O12 S1 O10 114.14(18) . . ? O12 S1 O11 111.92(18) . . ? O10 S1 O11 109.39(17) . . ? O12 S1 C1 108.39(19) . . ? O10 S1 C1 106.19(19) . . ? O11 S1 C1 106.37(18) . . ? C6 C1 C2 120.5(4) . . ? C6 C1 S1 120.0(3) . . ? C2 C1 S1 119.4(3) . . ? C3 C2 C1 119.8(4) . . ? C2 C3 C4 120.6(5) . . ? C5 C4 C3 119.1(4) . . ? C5 C4 C7 120.4(4) . . ? C3 C4 C7 120.5(5) . . ? C4 C5 C6 120.3(4) . . ? C1 C6 C5 119.6(4) . . ? O14 S2 O13 113.20(18) . . ? O14 S2 O15 110.86(18) . . ? O13 S2 O15 111.18(17) . . ? O14 S2 C8 108.15(19) . . ? O13 S2 C8 107.58(19) . . ? O15 S2 C8 105.47(19) . . ? C13 C8 C9 119.8(4) . . ? C13 C8 S2 120.0(4) . . ? C9 C8 S2 120.1(3) . . ? C10 C9 C8 119.4(4) . . ? C9 C10 C11 121.8(5) . . ? C10 C11 C12 117.7(5) . . ? C10 C11 C14 121.8(5) . . ? C12 C11 C14 120.5(5) . . ? C13 C12 C11 121.1(5) . . ? C8 C13 C12 120.2(5) . . ? O16 S3 O17 113.8(2) . . ? O16 S3 O18 111.8(2) . . ? O17 S3 O18 110.3(2) . . ? O16 S3 C15 107.3(2) . . ? O17 S3 C15 106.9(2) . . ? O18 S3 C15 106.3(2) . . ? C20 C15 C16 119.3(4) . . ? C20 C15 S3 121.6(4) . . ? C16 C15 S3 119.1(4) . . ? C15 C16 C17 119.2(5) . . ? C18 C17 C16 122.4(5) . . ? C17 C18 C19 117.0(5) . . ? C17 C18 C21 121.6(5) . . ? C19 C18 C21 121.3(5) . . ? C18 C19 C20 122.5(5) . . ? C19 C20 C15 119.6(5) . . ? O19 S4 O20 115.1(2) . . ? O19 S4 O21 111.0(2) . . ? O20 S4 O21 111.1(2) . . ? O19 S4 C22 106.4(2) . . ? O20 S4 C22 106.3(2) . . ? O21 S4 C22 106.4(2) . . ? C23 C22 C27 120.0(4) . . ? C23 C22 S4 120.3(3) . . ? C27 C22 S4 119.7(3) . . ? C22 C23 C24 119.2(4) . . ? C23 C24 C25 121.2(5) . . ? C26 C25 C24 118.5(4) . . ? C26 C25 C28 120.7(5) . . ? C24 C25 C28 120.8(5) . . ? C27 C26 C25 120.9(4) . . ? C26 C27 C22 120.1(4) . . ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.202 _refine_diff_density_min -0.873 _refine_diff_density_rms 0.144 #===END