Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _audit_creation_method SHELXL _journal_coden_Cambridge 222 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Dalton Transactions' _publ_contact_author_name 'Prof Daniel Miguel ' _publ_contact_author_address ; Departamento de Química Inorgánica Universidad de Valladolid Facultad de Ciencias, Prado de la M Valladolid E-47005 SPAIN ; _publ_contact_author_phone +34-983-423232 _publ_contact_author_fax +34-983-423013 _publ_contact_author_email dmsj@qi.uva.es _publ_section_title ; Synthesis of asymmetric heterotrimetallic gold clusters containing Mo, W, and Mn. ; loop_ _publ_author_name _publ_author_address 'Mei Wang' ; Department of Chemistry Dalian University of Technology Zhongshan Road 158-46, Dalian 116012. CHINA ; 'Daniel Miguel' ; Departamento de Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; 'Eva M. Lopez' ; Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Química Universidad de Oviedo C/ Julian Claveria s/n 33006 Oviedo (ASTURIAS) SPAIN ; 'Julio Perez' ; Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Química Universidad de Oviedo C/ Julian Claveria s/n 33006 Oviedo (ASTURIAS) SPAIN ; 'Victor Riera' ; Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Química Universidad de Oviedo C/ Julian Claveria s/n 33006 Oviedo (ASTURIAS) SPAIN ; 'Claudette Bois' ; Laboratoire de Chimie des Metaux de Transition UA-CNRS 419 Universite Pierre et Marie Curie 4 Place Jussieu 75252 Paris Cedex 05 FRANCE ; 'Yves Jeannin' ; Laboratoire de Chimie des Metaux de Transition UA-CNRS 419 Universite Pierre et Marie Curie 4 Place Jussieu 75252 Paris Cedex 05 FRANCE ; data_Compound_3a_(e2) _database_code_CSD 195126 _chemical_name_systematic ; # IUPAC name, in full ? ; _cell_length_a 11.491(9) _cell_angle_alpha 69.10(4) _cell_length_b 14.175(8) _cell_angle_beta 73.66(6) _cell_length_c 16.125(7) _cell_angle_gamma 78.75(6) _cell_volume 2341(52) _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'Mo ' -1.8250 0.6880 3.7025 0.2772 17.2356 1.0958 12.8876 11.0040 3.7429 61.6584 4.3875 International_Tables_Vol_IV_Table_2.2B 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'Au ' -2.6880 8.7980 16.8819 0.4611 18.5913 8.6216 25.5582 1.4826 5.8600 36.3956 12.0658 International_Tables_Vol_IV_Table_2.2B 'Mn ' 0.2950 0.7290 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543 1.0896 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'S ' 0.1100 0.1240 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C43 H50 Au1 Mo1 Mn1 O7 S2 P2' _chemical_formula_moiety ' C43 H48 Au1 Mo1 Mn1 S2 P2 O1 H2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 1152.77 _cell_measurement_reflns_used 251 _cell_measurement_theta_min 15 _cell_measurement_theta_max 15.2 _cell_measurement_temperature 294 _cell_formula_units_Z 2 _exptl_crystal_description ' box ' _exptl_crystal_colour ' yellow' _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_meas ? _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 3.858 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _diffrn_standards_interval_time 'one hour' _diffrn_standards_interval_count 100 _diffrn_standards_number 2 _diffrn_standards_decay_% 0 _diffrn_ambient_temperature 293 _diffrn_reflns_number 9364 _reflns_number_total 8238 _diffrn_reflns_av_R_equivalents 0.03 _reflns_number_observed 5037 _diffrn_reflns_theta_min 1.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _reflns_observed_criterion >3.00\s(I) _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_diff_density_min -1.42 _refine_diff_density_max 0.67 _refine_ls_number_reflns 5037 _refine_ls_number_parameters 517 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0614 _refine_ls_wR_factor_obs 0.0699 _refine_ls_R_factor_all 0.0614 _refine_ls_wR_factor_all 0.0699 _refine_ls_goodness_of_fit_obs 1.1141 _refine_ls_goodness_of_fit_all 1.1141 _refine_ls_shift/esd_max 0.03961 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method 2\q/\w loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type Au(1) 0.24859(4) 0.78891(3) 0.14535(3) 0.0444 1.0000 Uani Mo(1) 0.16150(8) 0.81499(5) 0.31502(5) 0.0326 1.0000 Uani Mn(1) 0.3008(1) 0.6224(1) 0.2901(1) 0.0346 1.0000 Uani S(1) 0.3411(2) 0.7101(2) 0.3739(2) 0.0352 1.0000 Uani S(2) 0.1231(2) 0.6321(2) 0.3988(2) 0.0348 1.0000 Uani P(1) 0.2684(3) 0.8280(2) -0.0096(2) 0.0455 1.0000 Uani P(2) 0.1539(2) 0.6955(2) 0.5583(2) 0.0337 1.0000 Uani O(1) 0.0072(9) 0.9802(6) 0.3964(6) 0.0653 1.0000 Uani O(2) -0.0654(9) 0.8675(6) 0.2329(8) 0.0729 1.0000 Uani O(3) 0.2961(9) 1.0065(6) 0.1931(6) 0.0649 1.0000 Uani O(4) 0.404(1) 0.4191(6) 0.3845(8) 0.0783 1.0000 Uani O(5) 0.1948(9) 0.5396(7) 0.1874(6) 0.0614 1.0000 Uani O(6) 0.5323(8) 0.6512(7) 0.1486(6) 0.0617 1.0000 Uani O(100) 0.946(2) 0.463(1) 0.0944(8) 0.1269 1.0000 Uani C(1) 0.065(1) 0.9149(7) 0.3703(7) 0.0432 1.0000 Uani C(2) 0.023(1) 0.8469(8) 0.261(1) 0.0489 1.0000 Uani C(3) 0.248(1) 0.9344(7) 0.2349(7) 0.0402 1.0000 Uani C(4) 0.364(1) 0.4978(8) 0.3485(8) 0.0537 1.0000 Uani C(5) 0.235(1) 0.5743(8) 0.2259(8) 0.0476 1.0000 Uani C(6) 0.439(1) 0.6428(8) 0.2031(8) 0.0407 1.0000 Uani C(7) 0.1902(8) 0.7020(6) 0.4416(6) 0.0231 1.0000 Uani C(10) 0.122(1) 0.8345(8) -0.0342(7) 0.0505 1.0000 Uani C(11) 0.034(2) 0.786(2) 0.032(1) 0.0920 1.0000 Uani C(12) -0.081(2) 0.783(2) 0.020(1) 0.1000 1.0000 Uani C(13) -0.101(2) 0.831(2) -0.070(2) 0.1044 1.0000 Uani C(14) -0.013(2) 0.876(1) -0.136(1) 0.0754 1.0000 Uani C(15) 0.101(1) 0.877(1) -0.1197(9) 0.0738 1.0000 Uani C(20) 0.362(1) 0.7308(8) -0.0558(7) 0.0496 1.0000 Uani C(21) 0.316(2) 0.663(1) -0.073(1) 0.0796 1.0000 Uani C(22) 0.388(2) 0.585(1) -0.104(1) 0.0892 1.0000 Uani C(23) 0.511(2) 0.581(1) -0.116(1) 0.0929 1.0000 Uani C(24) 0.561(2) 0.647(1) -0.097(1) 0.0869 1.0000 Uani C(25) 0.484(1) 0.724(1) -0.069(1) 0.0751 1.0000 Uani C(30) 0.334(1) 0.9435(8) -0.0799(7) 0.0503 1.0000 Uani C(31) 0.375(2) 0.970(1) -0.1752(8) 0.0672 1.0000 Uani C(32) 0.421(2) 1.061(1) -0.2251(9) 0.0791 1.0000 Uani C(33) 0.430(1) 1.127(1) -0.187(1) 0.0693 1.0000 Uani C(34) 0.394(2) 1.106(1) -0.096(1) 0.0892 1.0000 Uani C(35) 0.347(2) 1.014(1) -0.042(1) 0.0800 1.0000 Uani C(40) 0.2679(9) 0.7624(7) 0.5685(7) 0.0365 1.0000 Uani C(41) 0.258(1) 0.8760(8) 0.5148(8) 0.0440 1.0000 Uani C(42) 0.364(1) 0.9246(9) 0.517(1) 0.0580 1.0000 Uani C(43) 0.370(1) 0.907(1) 0.614(1) 0.0535 1.0000 Uani C(44) 0.381(1) 0.794(1) 0.6660(9) 0.0605 1.0000 Uani C(45) 0.271(1) 0.746(1) 0.6685(8) 0.0547 1.0000 Uani C(50) 0.176(1) 0.5632(7) 0.6310(7) 0.0416 1.0000 Uani C(51) 0.305(1) 0.5163(9) 0.597(1) 0.0529 1.0000 Uani C(52) 0.325(1) 0.407(1) 0.664(1) 0.0730 1.0000 Uani C(53) 0.226(2) 0.3414(9) 0.675(1) 0.0732 1.0000 Uani C(54) 0.103(1) 0.3905(8) 0.7068(9) 0.0534 1.0000 Uani C(55) 0.079(1) 0.4968(8) 0.6422(8) 0.0439 1.0000 Uani C(60) -0.0015(9) 0.7537(7) 0.5908(7) 0.0373 1.0000 Uani C(61) -0.095(1) 0.7305(9) 0.5495(8) 0.0488 1.0000 Uani C(62) -0.215(1) 0.793(1) 0.570(1) 0.0620 1.0000 Uani C(63) -0.263(1) 0.775(1) 0.671(1) 0.0712 1.0000 Uani C(64) -0.169(1) 0.796(1) 0.712(1) 0.0677 1.0000 Uani C(65) -0.049(1) 0.7314(9) 0.6938(8) 0.0532 1.0000 Uani H11 0.0502 0.7522 0.0940 0.094(9) 1.0000 Uiso H12 -0.1467 0.7493 0.0719 0.094(9) 1.0000 Uiso H13 -0.1807 0.8298 -0.0815 0.094(9) 1.0000 Uiso H14 -0.0269 0.9091 -0.1986 0.094(9) 1.0000 Uiso H15 0.1674 0.9106 -0.1716 0.094(9) 1.0000 Uiso H21 0.2255 0.6677 -0.0650 0.094(9) 1.0000 Uiso H22 0.3507 0.5354 -0.1185 0.094(9) 1.0000 Uiso H23 0.5629 0.5253 -0.1370 0.094(9) 1.0000 Uiso H24 0.6525 0.6410 -0.1048 0.094(9) 1.0000 Uiso H25 0.5196 0.7765 -0.0580 0.094(9) 1.0000 Uiso H31 0.3712 0.9220 -0.2068 0.094(9) 1.0000 Uiso H32 0.4501 1.0779 -0.2937 0.094(9) 1.0000 Uiso H33 0.4612 1.1934 -0.2253 0.094(9) 1.0000 Uiso H34 0.4023 1.1551 -0.0661 0.094(9) 1.0000 Uiso H35 0.3205 0.9992 0.0248 0.094(9) 1.0000 Uiso H40 0.3544 0.7401 0.5405 0.094(9) 1.0000 Uiso H50 0.1690 0.5512 0.6973 0.094(9) 1.0000 Uiso H60 -0.0114 0.8304 0.5663 0.094(9) 1.0000 Uiso H411 0.1795 0.9093 0.5437 0.094(9) 1.0000 Uiso H412 0.2584 0.8861 0.4503 0.094(9) 1.0000 Uiso H421 0.3525 0.9993 0.4844 0.094(9) 1.0000 Uiso H422 0.4415 0.8942 0.4847 0.094(9) 1.0000 Uiso H431 0.4424 0.9368 0.6129 0.094(9) 1.0000 Uiso H432 0.2940 0.9404 0.6451 0.094(9) 1.0000 Uiso H441 0.3857 0.7836 0.7299 0.094(9) 1.0000 Uiso H442 0.4574 0.7603 0.6352 0.094(9) 1.0000 Uiso H451 0.1944 0.7801 0.6990 0.094(9) 1.0000 Uiso H452 0.2786 0.6720 0.7039 0.094(9) 1.0000 Uiso H511 0.3668 0.5587 0.5950 0.094(9) 1.0000 Uiso H512 0.3138 0.5136 0.5344 0.094(9) 1.0000 Uiso H521 0.3242 0.4112 0.7245 0.094(9) 1.0000 Uiso H522 0.4071 0.3743 0.6390 0.094(9) 1.0000 Uiso H531 0.2402 0.2731 0.7219 0.094(9) 1.0000 Uiso H532 0.2320 0.3318 0.6159 0.094(9) 1.0000 Uiso H541 0.0962 0.3945 0.7688 0.094(9) 1.0000 Uiso H542 0.0405 0.3475 0.7110 0.094(9) 1.0000 Uiso H551 -0.0032 0.5279 0.6669 0.094(9) 1.0000 Uiso H552 0.0815 0.4924 0.5809 0.094(9) 1.0000 Uiso H611 -0.1065 0.6566 0.5779 0.094(9) 1.0000 Uiso H612 -0.0635 0.7467 0.4822 0.094(9) 1.0000 Uiso H621 -0.2039 0.8667 0.5381 0.094(9) 1.0000 Uiso H622 -0.2760 0.7742 0.5460 0.094(9) 1.0000 Uiso H631 -0.3398 0.8214 0.6814 0.094(9) 1.0000 Uiso H632 -0.2812 0.7030 0.7023 0.094(9) 1.0000 Uiso H641 -0.2027 0.7807 0.7794 0.094(9) 1.0000 Uiso H642 -0.1558 0.8696 0.6837 0.094(9) 1.0000 Uiso H651 0.0115 0.7478 0.7200 0.094(9) 1.0000 Uiso H652 -0.0615 0.6576 0.7242 0.094(9) 1.0000 Uiso 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 Au(1) 0.0437(3) 0.0489(2) 0.0414(2) -0.0141(2) -0.0091(2) -0.0074(2) Mo(1) 0.0285(5) 0.0293(4) 0.0412(4) -0.0117(3) -0.0074(4) -0.0020(3) Mn(1) 0.0316(9) 0.0297(7) 0.0490(7) -0.0175(6) -0.0094(7) 0.0002(6) S(1) 0.025(1) 0.039(1) 0.047(1) -0.016(1) -0.008(1) -0.003(1) S(2) 0.032(1) 0.034(1) 0.047(1) -0.014(1) -0.011(1) -0.010(1) P(1) 0.055(2) 0.039(1) 0.043(1) -0.013(1) -0.010(1) 0.000(1) P(2) 0.031(2) 0.035(1) 0.041(1) -0.0132(9) -0.006(1) -0.011(1) O(1) 0.076(7) 0.047(4) 0.084(6) -0.028(4) -0.002(5) 0.012(4) O(2) 0.068(7) 0.046(5) 0.135(9) -0.000(5) -0.048(7) -0.003(4) O(3) 0.058(6) 0.055(5) 0.079(6) -0.011(4) -0.008(5) -0.014(4) O(4) 0.110(9) 0.042(5) 0.121(8) -0.016(5) -0.051(7) 0.023(5) O(5) 0.071(7) 0.073(6) 0.095(6) -0.051(5) -0.032(5) -0.009(5) O(6) 0.038(5) 0.088(6) 0.078(6) -0.043(5) -0.001(5) -0.004(4) O(100) 0.23(2) 0.15(1) 0.080(7) -0.016(8) -0.05(1) -0.08(1) C(1) 0.043(7) 0.042(5) 0.043(5) -0.010(4) 0.001(5) -0.015(5) C(2) 0.035(7) 0.032(5) 0.100(9) -0.013(5) -0.019(7) 0.003(5) C(3) 0.026(6) 0.040(5) 0.061(6) -0.008(5) -0.002(5) -0.010(4) C(4) 0.065(9) 0.040(6) 0.067(7) -0.018(5) -0.026(7) 0.000(5) C(5) 0.056(8) 0.041(5) 0.062(6) -0.029(5) -0.014(6) 0.001(5) C(6) 0.032(6) 0.042(5) 0.073(7) -0.034(5) -0.007(6) -0.003(4) C(7) 0.016(5) 0.026(4) 0.049(5) -0.014(3) -0.015(4) -0.001(3) C(10) 0.051(8) 0.046(6) 0.049(6) -0.006(5) -0.013(6) 0.003(5) C(11) 0.08(1) 0.18(2) 0.067(9) 0.00(1) -0.026(9) -0.05(1) C(12) 0.07(1) 0.25(3) 0.08(1) -0.01(1) -0.03(1) -0.06(2) C(13) 0.11(2) 0.15(2) 0.12(2) -0.03(1) -0.08(1) 0.02(1) C(14) 0.07(1) 0.09(1) 0.074(9) -0.012(8) -0.033(9) -0.016(8) C(15) 0.07(1) 0.09(1) 0.064(8) -0.005(7) -0.028(8) -0.003(8) C(20) 0.041(7) 0.053(6) 0.056(6) -0.024(5) -0.002(6) 0.006(5) C(21) 0.09(1) 0.066(8) 0.10(1) -0.039(8) -0.03(1) 0.020(8) C(22) 0.10(1) 0.066(9) 0.12(1) -0.044(9) -0.01(1) -0.010(9) C(23) 0.10(1) 0.07(1) 0.11(1) -0.036(9) -0.01(1) 0.01(1) C(24) 0.06(1) 0.10(1) 0.11(1) -0.04(1) 0.01(1) -0.005(9) C(25) 0.07(1) 0.069(9) 0.087(9) -0.031(8) -0.001(8) -0.015(8) C(30) 0.054(8) 0.045(6) 0.051(6) -0.016(5) -0.006(5) -0.007(5) C(31) 0.11(1) 0.073(9) 0.045(6) -0.011(6) -0.019(7) -0.038(9) C(32) 0.11(1) 0.08(1) 0.059(8) -0.006(7) -0.011(8) -0.040(9) C(33) 0.07(1) 0.052(7) 0.08(1) -0.001(6) 0.007(8) -0.014(6) C(34) 0.14(2) 0.061(9) 0.10(1) -0.030(8) 0.01(1) -0.04(1) C(35) 0.15(2) 0.066(8) 0.068(8) -0.024(7) 0.012(9) -0.05(1) C(40) 0.025(6) 0.045(5) 0.053(5) -0.017(4) -0.004(5) -0.014(4) C(41) 0.041(7) 0.039(5) 0.075(7) -0.013(5) -0.022(6) -0.015(5) C(42) 0.054(9) 0.054(7) 0.093(9) -0.023(6) -0.017(8) -0.023(6) C(43) 0.06(1) 0.086(9) 0.089(9) -0.050(8) 0.004(8) -0.050(8) C(44) 0.07(1) 0.088(9) 0.068(7) -0.023(7) -0.019(7) -0.042(8) C(45) 0.067(9) 0.075(8) 0.052(6) -0.015(5) -0.011(6) -0.041(7) C(50) 0.031(6) 0.045(5) 0.054(6) -0.011(4) -0.014(5) -0.005(4) C(51) 0.030(7) 0.049(6) 0.097(9) -0.003(6) -0.022(7) 0.001(5) C(52) 0.051(9) 0.066(9) 0.11(1) 0.017(8) -0.028(9) -0.000(7) C(53) 0.08(1) 0.036(6) 0.15(2) -0.002(8) -0.06(1) -0.000(6) C(54) 0.059(9) 0.039(6) 0.087(8) -0.005(5) -0.039(7) -0.012(5) C(55) 0.037(7) 0.045(5) 0.064(6) -0.011(5) -0.021(6) -0.011(5) C(60) 0.024(6) 0.047(5) 0.057(5) -0.020(5) -0.009(5) -0.008(4) C(61) 0.031(7) 0.063(7) 0.058(6) -0.019(5) -0.008(5) -0.006(5) C(62) 0.043(8) 0.059(7) 0.083(9) -0.018(7) -0.002(7) -0.006(6) C(63) 0.047(9) 0.077(9) 0.10(1) -0.036(8) 0.012(8) -0.008(7) C(64) 0.06(1) 0.10(1) 0.083(9) -0.057(8) 0.026(8) -0.021(8) C(65) 0.047(8) 0.069(7) 0.063(6) -0.035(6) 0.007(6) -0.022(6) _refine_ls_extinction_coef 109.9(136) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Au(1) Mo(1) 2.768(1) yes Au(1) Mn(1) 2.772(2) yes Au(1) P(1) 2.313(3) yes Mo(1) Mn(1) 2.982(2) yes Mo(1) S(1) 2.501(3) yes Mo(1) S(2) 2.520(2) yes Mo(1) C(1) 1.94(1) yes Mo(1) C(2) 1.92(1) yes Mo(1) C(3) 1.97(1) yes Mo(1) C(7) 2.167(9) yes Mn(1) S(1) 2.316(3) yes Mn(1) S(2) 2.304(3) yes Mn(1) C(4) 1.79(1) yes Mn(1) C(5) 1.80(1) yes Mn(1) C(6) 1.79(1) yes S(1) C(7) 1.771(9) yes S(2) C(7) 1.765(9) yes P(1) C(10) 1.81(1) yes P(1) C(20) 1.82(1) yes P(1) C(30) 1.79(1) yes P(2) C(40) 1.83(1) yes P(2) C(50) 1.83(1) yes P(2) C(60) 1.83(1) yes P(2) C(7) 1.784(9) yes O(1) C(1) 1.17(1) yes O(2) C(2) 1.18(1) yes O(3) C(3) 1.15(1) yes O(4) C(4) 1.14(1) yes O(5) C(5) 1.14(1) yes O(6) C(6) 1.18(1) yes C(10) C(11) 1.33(2) yes C(10) C(15) 1.36(2) yes C(11) C(12) 1.40(2) yes C(12) C(13) 1.42(3) yes C(13) C(14) 1.32(3) yes C(14) C(15) 1.41(2) yes C(20) C(21) 1.33(2) yes C(20) C(25) 1.34(2) yes C(21) C(22) 1.40(2) yes C(22) C(23) 1.35(3) yes C(23) C(24) 1.36(3) yes C(24) C(25) 1.41(2) yes C(30) C(31) 1.40(2) yes C(30) C(35) 1.39(2) yes C(31) C(32) 1.37(2) yes C(32) C(33) 1.33(2) yes C(33) C(34) 1.34(2) yes C(34) C(35) 1.38(2) yes C(40) C(41) 1.53(2) yes C(40) C(45) 1.56(2) yes C(41) C(42) 1.51(2) yes C(42) C(43) 1.52(2) yes C(43) C(44) 1.52(2) yes C(44) C(45) 1.53(2) yes C(50) C(51) 1.54(2) yes C(50) C(55) 1.53(1) yes C(51) C(52) 1.56(2) yes C(52) C(53) 1.54(2) yes C(53) C(54) 1.49(2) yes C(54) C(55) 1.53(1) yes C(60) C(61) 1.54(2) yes C(60) C(65) 1.53(1) yes C(61) C(62) 1.51(2) yes C(62) C(63) 1.52(2) yes C(63) C(64) 1.53(2) yes C(64) C(65) 1.52(2) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Mo(1) Au(1) Mo(1) 65.13(3) yes P(1) Au(1) Mo(1) 156.32(8) yes P(1) Au(1) Mn(1) 137.87(7) yes Mn(1) Mo(1) Au(1) 57.50(7) yes S(1) Mo(1) Au(1) 93.47(6) yes S(1) Mo(1) Mn(1) 49.01(6) yes S(2) Mo(1) Au(1) 94.78(6) yes S(2) Mo(1) Mn(1) 48.62(7) yes S(2) Mo(1) S(1) 67.85(9) yes C(1) Mo(1) Au(1) 140.0(3) yes C(1) Mo(1) Mn(1) 162.3(3) yes C(1) Mo(1) S(1) 119.9(4) yes C(1) Mo(1) S(2) 116.9(3) yes C(2) Mo(1) Au(1) 73.9(4) yes C(2) Mo(1) Mn(1) 109.1(4) yes C(2) Mo(1) S(1) 157.6(3) yes C(2) Mo(1) S(2) 94.3(3) yes C(2) Mo(1) C(1) 79.7(5) yes C(3) Mo(1) Au(1) 73.5(3) yes C(3) Mo(1) Mn(1) 111.9(3) yes C(3) Mo(1) S(1) 96.1(3) yes C(3) Mo(1) S(2) 159.9(3) yes C(3) Mo(1) C(1) 81.1(4) yes C(3) Mo(1) C(2) 97.8(5) yes C(7) Mo(1) Au(1) 124.2(2) yes C(7) Mo(1) Mn(1) 66.7(2) yes C(7) Mo(1) S(1) 43.8(3) yes C(7) Mo(1) S(2) 43.4(2) yes C(7) Mo(1) C(1) 95.7(4) yes C(7) Mo(1) C(2) 129.8(5) yes C(7) Mo(1) C(3) 131.1(4) yes Mo(1) Mn(1) Au(1) 57.36(7) yes S(1) Mn(1) Au(1) 97.62(8) yes S(1) Mn(1) Mo(1) 54.60(7) yes S(2) Mn(1) Au(1) 99.82(8) yes S(2) Mn(1) Mo(1) 55.17(7) yes S(2) Mn(1) S(1) 74.70(10) yes C(4) Mn(1) Au(1) 158.5(4) yes C(4) Mn(1) Mo(1) 144.1(4) yes C(4) Mn(1) S(1) 98.5(4) yes C(4) Mn(1) S(2) 98.1(5) yes C(5) Mn(1) Au(1) 74.4(4) yes C(5) Mn(1) Mo(1) 111.5(4) yes C(5) Mn(1) S(1) 165.7(4) yes C(5) Mn(1) S(2) 94.7(4) yes C(5) Mn(1) C(4) 92.4(5) yes C(6) Mn(1) Au(1) 72.8(4) yes C(6) Mn(1) Mo(1) 112.9(3) yes C(6) Mn(1) S(1) 96.3(3) yes C(6) Mn(1) S(2) 167.7(3) yes C(6) Mn(1) C(4) 91.3(6) yes C(6) Mn(1) C(5) 92.6(5) yes Mn(1) S(1) Mo(1) 76.39(8) yes C(7) S(1) Mo(1) 58.0(3) yes C(7) S(1) Mn(1) 89.9(3) yes Mn(1) S(2) Mo(1) 76.21(8) yes C(7) S(2) Mo(1) 57.6(3) yes C(7) S(2) Mn(1) 90.4(3) yes C(10) P(1) Au(1) 110.7(4) yes C(20) P(1) Au(1) 113.3(4) yes C(20) P(1) C(10) 103.9(6) yes C(30) P(1) Au(1) 115.5(4) yes C(30) P(1) C(10) 107.9(6) yes C(30) P(1) C(20) 104.7(6) yes C(40) P(2) C(7) 105.8(5) yes C(50) P(2) C(7) 109.8(5) yes C(50) P(2) C(40) 106.4(5) yes C(60) P(2) C(7) 110.6(4) yes C(60) P(2) C(40) 112.0(5) yes C(60) P(2) C(50) 111.9(5) yes O(1) C(1) Mo(1) 174.6(10) yes O(2) C(2) Mo(1) 175.8(13) yes O(3) C(3) Mo(1) 175.2(10) yes O(4) C(4) Mn(1) 178.9(13) yes O(5) C(5) Mn(1) 177.1(11) yes O(6) C(6) Mn(1) 176.5(10) yes S(1) C(7) Mo(1) 78.2(4) yes S(2) C(7) Mo(1) 79.0(3) yes P(2) C(7) Mo(1) 135.5(5) yes S(1) C(7) S(2) 104.7(4) yes S(1) C(7) P(2) 121.9(5) yes S(2) C(7) P(2) 124.0(5) yes C(11) C(10) P(1) 118.6(10) C(15) C(10) P(1) 123.2(11) C(11) C(10) C(15) 117.8(14) no C(10) C(11) C(12) 123.6(15) no C(11) C(12) C(13) 116.8(18) no C(12) C(13) C(14) 119.7(18) no C(13) C(14) C(15) 121.2(14) no C(10) C(15) C(14) 120.8(14) no C(21) C(20) C(25) 117.9(12) no C(20) C(21) C(22) 123.3(17) no C(21) C(22) C(23) 116.3(16) no C(22) C(23) C(24) 122.5(15) no C(23) C(24) C(25) 117.6(17) no C(20) C(25) C(24) 122.3(14) no P(1) C(30) C(31) 124.0(9) no P(1) C(30) C(35) 121.3(9) no C(31) C(30) C(35) 114.7(11) no C(30) C(31) C(32) 121.2(12) no C(31) C(32) C(33) 122.0(13) no C(32) C(33) C(34) 120.3(13) no C(33) C(34) C(35) 119.2(14) no C(30) C(35) C(34) 122.5(13) no C(41) C(40) C(45) 110.2(9) no C(40) C(41) C(42) 110.7(10) no C(41) C(42) C(43) 111.4(11) no C(43) C(44) C(45) 110.5(12) no C(40) C(45) C(44) 107.9(9) no C(51) C(50) C(55) 111.6(9) no C(50) C(51) C(52) 108.7(11) no C(51) C(52) C(53) 111.7(12) no C(52) C(53) C(54) 110.9(12) no C(53) C(54) C(55) 112.0(11) no C(50) C(55) C(54) 110.6(9) no C(61) C(60) C(65) 110.7(9) no C(60) C(61) C(62) 109.6(10) no C(61) C(62) C(63) 111.8(12) no C(62) C(63) C(64) 110.9(12) no C(63) C(64) C(65) 110.9(10) no C(60) C(65) C(64) 108.9(11) no '' '' data_Compound_6a_wm183am _database_code_CSD 195127 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H53 Au Mo2 O5 P2 S2' _chemical_formula_weight 1188.78 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' P P 0.1023 0.0942 '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' Au Au -2.0133 8.8022 '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 12.2628(9) _cell_length_b 12.8670(10) _cell_length_c 15.5143(11) _cell_angle_alpha 92.635(2) _cell_angle_beta 111.3350(10) _cell_angle_gamma 91.071(2) _cell_volume 2276.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PRISM _exptl_crystal_colour brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.735 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 3.963 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.715011 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10393 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0685 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 23.28 _reflns_number_total 6502 _reflns_number_gt 4657 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0130P)^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 6502 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0597 _refine_ls_wR_factor_gt 0.0568 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.002 _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 Mo2 Mo 0.28991(4) 0.45918(4) 0.29609(4) 0.03086(15) Uani 1 1 d . . . Mo1 Mo 0.17666(5) 0.27104(4) 0.34671(4) 0.03394(15) Uani 1 1 d . . . Au1 Au 0.33188(3) 0.27778(2) 0.21792(2) 0.05092(11) Uani 1 1 d . . . S1 S 0.08122(13) 0.39396(12) 0.22896(10) 0.0325(4) Uani 1 1 d . . . S2 S 0.19889(13) 0.45454(12) 0.41950(10) 0.0342(4) Uani 1 1 d . . . P2 P 0.03347(14) 0.61302(12) 0.28796(11) 0.0299(4) Uani 1 1 d . . . P1 P 0.39470(15) 0.16067(14) 0.13200(12) 0.0385(4) Uani 1 1 d . . . C1 C 0.0259(7) 0.2141(6) 0.3335(5) 0.054(2) Uani 1 1 d . . . O1 O -0.0658(5) 0.1755(5) 0.3230(4) 0.0816(18) Uani 1 1 d . . . C2 C 0.1659(6) 0.1447(6) 0.2697(5) 0.0445(18) Uani 1 1 d . . . O2 O 0.1543(4) 0.0644(4) 0.2296(4) 0.0694(16) Uani 1 1 d . . . C4 C 0.3128(5) 0.4846(5) 0.1802(5) 0.0445(18) Uani 1 1 d . . . O4 O 0.3260(5) 0.5094(4) 0.1131(4) 0.0767(17) Uani 1 1 d . . . C5 C 0.3799(6) 0.5930(6) 0.3315(5) 0.054(2) Uani 1 1 d . . . O5 O 0.4348(4) 0.6684(4) 0.3492(4) 0.0884(19) Uani 1 1 d . . . C6 C 0.4437(6) 0.4017(5) 0.3703(5) 0.0475(19) Uani 1 1 d . . . O6 O 0.5296(4) 0.3731(4) 0.4210(4) 0.0743(17) Uani 1 1 d . . . C7 C 0.1247(5) 0.5027(4) 0.3100(4) 0.0289(15) Uani 1 1 d . . . C8 C 0.3460(6) 0.1770(6) 0.4323(5) 0.058(2) Uani 1 1 d . . . H8A H 0.3026 0.1208 0.3949 0.070 Uiso 1 1 calc R . . H8B H 0.4199 0.1945 0.4322 0.070 Uiso 1 1 calc R . . C9 C 0.3002(6) 0.2351(5) 0.4883(4) 0.0507(19) Uani 1 1 d . . . H9 H 0.3436 0.2913 0.5256 0.061 Uiso 1 1 calc R . . C10 C 0.1890(6) 0.2089(5) 0.4885(4) 0.054(2) Uani 1 1 d . . . H10A H 0.1456 0.1527 0.4511 0.065 Uiso 1 1 calc R . . H10B H 0.1586 0.2477 0.5259 0.065 Uiso 1 1 calc R . . C20 C 0.5118(6) 0.2197(5) 0.1042(4) 0.0369(16) Uani 1 1 d . . . C21 C 0.4942(6) 0.3137(5) 0.0614(5) 0.0497(19) Uani 1 1 d . . . H21 H 0.4244 0.3470 0.0512 0.060 Uiso 1 1 calc R . . C22 C 0.5776(7) 0.3582(6) 0.0337(5) 0.060(2) Uani 1 1 d . . . H22 H 0.5619 0.4192 0.0021 0.071 Uiso 1 1 calc R . . C23 C 0.6822(7) 0.3145(6) 0.0521(6) 0.068(2) Uani 1 1 d . . . H23 H 0.7391 0.3462 0.0345 0.081 Uiso 1 1 calc R . . C24 C 0.7042(7) 0.2243(6) 0.0961(6) 0.073(2) Uani 1 1 d . . . H24 H 0.7766 0.1945 0.1095 0.087 Uiso 1 1 calc R . . C25 C 0.6185(6) 0.1762(6) 0.1214(5) 0.055(2) Uani 1 1 d . . . H25 H 0.6339 0.1135 0.1504 0.066 Uiso 1 1 calc R . . C30 C 0.4518(5) 0.0432(5) 0.1900(4) 0.0378(16) Uani 1 1 d . . . C31 C 0.4464(6) -0.0510(6) 0.1437(5) 0.056(2) Uani 1 1 d . . . H31 H 0.4141 -0.0551 0.0793 0.067 Uiso 1 1 calc R . . C32 C 0.4870(7) -0.1401(6) 0.1892(6) 0.071(2) Uani 1 1 d . . . H32 H 0.4795 -0.2037 0.1562 0.086 Uiso 1 1 calc R . . C33 C 0.5383(7) -0.1334(7) 0.2832(7) 0.079(3) Uani 1 1 d . . . H33 H 0.5691 -0.1922 0.3148 0.095 Uiso 1 1 calc R . . C34 C 0.5447(8) -0.0408(7) 0.3310(6) 0.085(3) Uani 1 1 d . . . H34 H 0.5787 -0.0371 0.3954 0.102 Uiso 1 1 calc R . . C35 C 0.5011(7) 0.0483(6) 0.2849(5) 0.067(2) Uani 1 1 d . . . H35 H 0.5052 0.1111 0.3183 0.081 Uiso 1 1 calc R . . C40 C 0.2916(5) 0.1108(5) 0.0205(4) 0.0376(16) Uani 1 1 d . . . C41 C 0.1905(6) 0.0560(5) 0.0171(5) 0.0479(18) Uani 1 1 d . . . H41 H 0.1767 0.0479 0.0716 0.057 Uiso 1 1 calc R . . C42 C 0.1114(6) 0.0143(5) -0.0649(5) 0.0509(19) Uani 1 1 d . . . H42 H 0.0448 -0.0221 -0.0657 0.061 Uiso 1 1 calc R . . C43 C 0.1296(7) 0.0256(6) -0.1449(5) 0.058(2) Uani 1 1 d . . . H43 H 0.0753 -0.0032 -0.2003 0.070 Uiso 1 1 calc R . . C44 C 0.2266(7) 0.0785(6) -0.1453(5) 0.059(2) Uani 1 1 d . . . H44 H 0.2383 0.0863 -0.2007 0.071 Uiso 1 1 calc R . . C45 C 0.3075(6) 0.1205(5) -0.0625(5) 0.0469(18) Uani 1 1 d . . . H45 H 0.3742 0.1560 -0.0627 0.056 Uiso 1 1 calc R . . C50 C 0.0186(5) 0.6731(5) 0.1806(4) 0.0349(16) Uani 1 1 d . . . H50 H -0.0307 0.7329 0.1781 0.042 Uiso 1 1 calc R . . C51 C -0.0446(5) 0.6074(5) 0.0930(4) 0.0441(18) Uani 1 1 d . . . H51A H -0.1181 0.5802 0.0945 0.053 Uiso 1 1 calc R . . H51B H 0.0026 0.5488 0.0895 0.053 Uiso 1 1 calc R . . C52 C -0.0688(6) 0.6696(5) 0.0075(4) 0.0494(19) Uani 1 1 d . . . H52A H -0.1070 0.6244 -0.0476 0.059 Uiso 1 1 calc R . . H52B H -0.1214 0.7246 0.0082 0.059 Uiso 1 1 calc R . . C53 C 0.0422(6) 0.7163(6) 0.0037(5) 0.060(2) Uani 1 1 d . . . H53A H 0.0231 0.7608 -0.0482 0.072 Uiso 1 1 calc R . . H53B H 0.0896 0.6611 -0.0066 0.072 Uiso 1 1 calc R . . C54 C 0.1117(6) 0.7791(5) 0.0916(4) 0.053(2) Uani 1 1 d . . . H54A H 0.1863 0.8014 0.0888 0.063 Uiso 1 1 calc R . . H54B H 0.0697 0.8410 0.0962 0.063 Uiso 1 1 calc R . . C55 C 0.1338(5) 0.7190(5) 0.1770(4) 0.0421(17) Uani 1 1 d . . . H55A H 0.1721 0.7648 0.2317 0.051 Uiso 1 1 calc R . . H55B H 0.1858 0.6631 0.1773 0.051 Uiso 1 1 calc R . . C60 C -0.1131(5) 0.5651(5) 0.2737(4) 0.0345(16) Uani 1 1 d . . . H60 H -0.1340 0.5135 0.2213 0.041 Uiso 1 1 calc R . . C61 C -0.1194(5) 0.5036(5) 0.3541(4) 0.0474(18) Uani 1 1 d . . . H61A H -0.0583 0.4531 0.3704 0.057 Uiso 1 1 calc R . . H61B H -0.1062 0.5507 0.4079 0.057 Uiso 1 1 calc R . . C62 C -0.2382(6) 0.4475(6) 0.3276(5) 0.062(2) Uani 1 1 d . . . H62A H -0.2477 0.3953 0.2780 0.074 Uiso 1 1 calc R . . H62B H -0.2418 0.4123 0.3804 0.074 Uiso 1 1 calc R . . C63 C -0.3366(6) 0.5224(7) 0.2962(5) 0.072(2) Uani 1 1 d . . . H63A H -0.4111 0.4836 0.2757 0.086 Uiso 1 1 calc R . . H63B H -0.3328 0.5691 0.3482 0.086 Uiso 1 1 calc R . . C64 C -0.3306(6) 0.5851(6) 0.2190(5) 0.063(2) Uani 1 1 d . . . H64A H -0.3918 0.6353 0.2040 0.076 Uiso 1 1 calc R . . H64B H -0.3444 0.5392 0.1644 0.076 Uiso 1 1 calc R . . C65 C -0.2117(5) 0.6424(5) 0.2448(5) 0.0467(18) Uani 1 1 d . . . H65A H -0.2009 0.6935 0.2954 0.056 Uiso 1 1 calc R . . H65B H -0.2093 0.6788 0.1921 0.056 Uiso 1 1 calc R . . C70 C 0.0859(5) 0.7109(4) 0.3843(4) 0.0391(17) Uani 1 1 d . . . H70 H 0.0566 0.6862 0.4310 0.047 Uiso 1 1 calc R . . C71 C 0.0295(6) 0.8163(5) 0.3579(5) 0.053(2) Uani 1 1 d . . . H71A H 0.0551 0.8452 0.3114 0.064 Uiso 1 1 calc R . . H71B H -0.0551 0.8060 0.3312 0.064 Uiso 1 1 calc R . . C72 C 0.0626(7) 0.8935(5) 0.4426(5) 0.075(3) Uani 1 1 d . . . H72A H 0.0314 0.9607 0.4228 0.090 Uiso 1 1 calc R . . H72B H 0.0271 0.8692 0.4850 0.090 Uiso 1 1 calc R . . C73 C 0.1881(7) 0.9054(5) 0.4908(6) 0.075(3) Uani 1 1 d . . . H73A H 0.2045 0.9519 0.5454 0.090 Uiso 1 1 calc R . . H73B H 0.2226 0.9370 0.4507 0.090 Uiso 1 1 calc R . . C74 C 0.2440(7) 0.8024(5) 0.5196(5) 0.075(3) Uani 1 1 d . . . H74A H 0.2149 0.7729 0.5640 0.090 Uiso 1 1 calc R . . H74B H 0.3283 0.8131 0.5491 0.090 Uiso 1 1 calc R . . C75 C 0.2144(6) 0.7265(5) 0.4331(5) 0.063(2) Uani 1 1 d . . . H75A H 0.2485 0.7542 0.3911 0.076 Uiso 1 1 calc R . . H75B H 0.2486 0.6600 0.4519 0.076 Uiso 1 1 calc R . . 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 Mo2 0.0299(3) 0.0292(3) 0.0353(3) 0.0039(3) 0.0138(3) 0.0020(3) Mo1 0.0378(4) 0.0284(4) 0.0334(3) 0.0034(3) 0.0101(3) 0.0001(3) Au1 0.0499(2) 0.0501(2) 0.04779(19) -0.00892(15) 0.01254(15) 0.01681(15) S1 0.0337(10) 0.0317(10) 0.0295(9) -0.0004(7) 0.0088(7) 0.0042(8) S2 0.0400(10) 0.0334(10) 0.0278(9) 0.0022(7) 0.0106(8) 0.0025(8) P2 0.0337(10) 0.0281(10) 0.0286(9) 0.0020(8) 0.0121(8) 0.0036(8) P1 0.0401(11) 0.0366(11) 0.0389(11) 0.0015(8) 0.0142(9) 0.0078(9) C1 0.057(5) 0.057(6) 0.046(5) -0.016(4) 0.018(4) 0.005(4) O1 0.053(4) 0.091(5) 0.101(5) -0.005(4) 0.031(3) -0.021(3) C2 0.045(5) 0.045(5) 0.043(4) -0.001(4) 0.016(4) -0.006(4) O2 0.082(4) 0.056(4) 0.081(4) -0.015(3) 0.044(3) -0.004(3) C4 0.043(4) 0.038(5) 0.057(5) 0.004(4) 0.023(4) 0.013(3) O4 0.102(4) 0.080(4) 0.079(4) 0.037(3) 0.065(4) 0.019(3) C5 0.038(5) 0.055(6) 0.074(6) 0.002(4) 0.029(4) -0.006(4) O5 0.067(4) 0.058(4) 0.139(5) -0.004(4) 0.039(4) -0.031(3) C6 0.049(5) 0.043(5) 0.049(5) 0.001(4) 0.017(4) -0.005(4) O6 0.040(3) 0.086(4) 0.079(4) 0.020(3) -0.002(3) 0.016(3) C7 0.029(4) 0.031(4) 0.027(3) 0.000(3) 0.010(3) 0.000(3) C8 0.052(5) 0.071(6) 0.044(5) 0.028(4) 0.004(4) 0.007(4) C9 0.060(6) 0.046(5) 0.038(4) 0.010(4) 0.007(4) 0.005(4) C10 0.072(6) 0.047(5) 0.047(5) -0.003(4) 0.026(4) -0.001(4) C20 0.039(4) 0.035(4) 0.040(4) 0.002(3) 0.017(3) 0.008(3) C21 0.041(5) 0.043(5) 0.066(5) 0.000(4) 0.020(4) 0.010(4) C22 0.078(6) 0.040(5) 0.072(6) 0.009(4) 0.039(5) -0.001(5) C23 0.060(6) 0.054(6) 0.108(7) 0.005(5) 0.054(5) 0.001(5) C24 0.050(5) 0.059(6) 0.121(8) 0.010(5) 0.044(5) 0.015(5) C25 0.061(5) 0.043(5) 0.065(5) 0.018(4) 0.028(4) 0.003(4) C30 0.041(4) 0.038(4) 0.035(4) 0.005(3) 0.014(3) 0.006(3) C31 0.064(5) 0.057(6) 0.046(5) 0.013(4) 0.016(4) 0.021(4) C32 0.089(7) 0.053(6) 0.066(6) 0.013(5) 0.020(5) 0.007(5) C33 0.079(6) 0.062(7) 0.094(8) 0.044(6) 0.023(6) 0.008(5) C34 0.106(8) 0.083(7) 0.050(6) 0.023(5) 0.005(5) 0.013(6) C35 0.080(6) 0.056(6) 0.056(6) 0.001(4) 0.012(5) 0.009(5) C40 0.031(4) 0.037(4) 0.046(4) 0.003(3) 0.016(3) 0.015(3) C41 0.052(5) 0.047(5) 0.049(5) 0.004(4) 0.021(4) 0.013(4) C42 0.043(5) 0.042(5) 0.064(5) 0.001(4) 0.015(4) 0.004(4) C43 0.057(6) 0.047(5) 0.054(5) -0.002(4) 0.001(4) 0.011(4) C44 0.078(6) 0.059(6) 0.035(5) 0.007(4) 0.015(4) 0.011(5) C45 0.049(5) 0.041(5) 0.051(5) 0.003(4) 0.019(4) 0.001(4) C50 0.037(4) 0.038(4) 0.031(4) 0.002(3) 0.014(3) 0.005(3) C51 0.049(4) 0.047(5) 0.036(4) 0.003(3) 0.015(3) 0.002(4) C52 0.057(5) 0.055(5) 0.035(4) 0.006(4) 0.015(4) 0.006(4) C53 0.075(6) 0.071(6) 0.045(5) 0.019(4) 0.033(4) 0.006(5) C54 0.050(5) 0.062(5) 0.054(5) 0.019(4) 0.026(4) 0.001(4) C55 0.044(4) 0.043(4) 0.045(4) 0.016(3) 0.021(3) 0.002(3) C60 0.032(4) 0.035(4) 0.036(4) 0.002(3) 0.013(3) 0.005(3) C61 0.043(5) 0.047(5) 0.055(5) 0.012(4) 0.019(4) 0.009(4) C62 0.053(5) 0.072(6) 0.070(5) 0.019(4) 0.032(4) -0.002(5) C63 0.042(5) 0.099(7) 0.078(6) 0.001(5) 0.027(4) -0.009(5) C64 0.034(5) 0.069(6) 0.083(6) 0.011(5) 0.016(4) 0.013(4) C65 0.044(5) 0.044(5) 0.054(5) 0.009(4) 0.019(4) 0.014(4) C70 0.042(4) 0.024(4) 0.045(4) -0.003(3) 0.009(3) 0.003(3) C71 0.057(5) 0.031(4) 0.061(5) -0.004(4) 0.010(4) 0.014(4) C72 0.092(7) 0.033(5) 0.096(7) -0.007(5) 0.032(6) 0.011(5) C73 0.070(6) 0.031(5) 0.104(7) -0.028(5) 0.012(5) -0.002(4) C74 0.075(6) 0.045(5) 0.074(6) -0.017(4) -0.008(5) 0.013(4) C75 0.067(6) 0.046(5) 0.066(5) 0.001(4) 0.011(4) 0.011(4) _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 Mo2 C4 1.958(7) . ? Mo2 C5 1.972(8) . ? Mo2 C6 1.994(8) . ? Mo2 C7 2.194(6) . ? Mo2 S1 2.4976(16) . ? Mo2 S2 2.5453(16) . ? Mo2 Au1 2.7244(6) . ? Mo2 Mo1 3.0411(8) . ? Mo1 C1 1.912(8) . ? Mo1 C2 1.946(7) . ? Mo1 C9 2.243(6) . ? Mo1 C10 2.328(6) . ? Mo1 C8 2.402(6) . ? Mo1 S1 2.4470(16) . ? Mo1 S2 2.5360(16) . ? Mo1 Au1 3.2250(6) . ? Au1 P1 2.2906(17) . ? Au1 C6 2.687(7) . ? S1 C7 1.774(6) . ? S2 C7 1.759(6) . ? P2 C7 1.791(6) . ? P2 C50 1.819(6) . ? P2 C60 1.821(6) . ? P2 C70 1.825(6) . ? P1 C20 1.807(6) . ? P1 C40 1.810(6) . ? P1 C30 1.814(6) . ? C1 O1 1.173(8) . ? C2 O2 1.160(7) . ? C4 O4 1.168(7) . ? C5 O5 1.133(7) . ? C6 O6 1.142(7) . ? C8 C9 1.392(9) . ? C9 C10 1.399(9) . ? C20 C25 1.373(8) . ? C20 C21 1.389(8) . ? C21 C22 1.370(9) . ? C22 C23 1.349(9) . ? C23 C24 1.355(10) . ? C24 C25 1.392(9) . ? C30 C31 1.368(8) . ? C30 C35 1.372(8) . ? C31 C32 1.379(9) . ? C32 C33 1.360(10) . ? C33 C34 1.360(10) . ? C34 C35 1.390(10) . ? C40 C45 1.383(8) . ? C40 C41 1.398(8) . ? C41 C42 1.367(8) . ? C42 C43 1.352(9) . ? C43 C44 1.361(9) . ? C44 C45 1.385(8) . ? C50 C51 1.505(7) . ? C50 C55 1.542(8) . ? C51 C52 1.519(8) . ? C52 C53 1.499(8) . ? C53 C54 1.506(8) . ? C54 C55 1.505(8) . ? C60 C65 1.531(8) . ? C60 C61 1.532(8) . ? C61 C62 1.519(8) . ? C62 C63 1.511(9) . ? C63 C64 1.497(9) . ? C64 C65 1.529(8) . ? C70 C75 1.485(8) . ? C70 C71 1.539(8) . ? C71 C72 1.535(9) . ? C72 C73 1.447(9) . ? C73 C74 1.515(9) . ? C74 C75 1.548(9) . ? 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 C4 Mo2 C5 80.0(3) . . ? C4 Mo2 C6 101.1(3) . . ? C5 Mo2 C6 83.0(3) . . ? C4 Mo2 C7 118.7(2) . . ? C5 Mo2 C7 100.8(2) . . ? C6 Mo2 C7 140.1(2) . . ? C4 Mo2 S1 98.47(19) . . ? C5 Mo2 S1 138.9(2) . . ? C6 Mo2 S1 136.51(19) . . ? C7 Mo2 S1 43.83(15) . . ? C4 Mo2 S2 161.49(18) . . ? C5 Mo2 S2 100.8(2) . . ? C6 Mo2 S2 97.34(19) . . ? C7 Mo2 S2 42.77(15) . . ? S1 Mo2 S2 68.57(5) . . ? C4 Mo2 Au1 69.64(19) . . ? C5 Mo2 Au1 131.32(19) . . ? C6 Mo2 Au1 67.39(19) . . ? C7 Mo2 Au1 126.86(15) . . ? S1 Mo2 Au1 84.02(4) . . ? S2 Mo2 Au1 119.88(4) . . ? C4 Mo2 Mo1 129.30(19) . . ? C5 Mo2 Mo1 150.4(2) . . ? C6 Mo2 Mo1 86.79(19) . . ? C7 Mo2 Mo1 70.39(15) . . ? S1 Mo2 Mo1 51.30(4) . . ? S2 Mo2 Mo1 53.10(4) . . ? Au1 Mo2 Mo1 67.766(18) . . ? C1 Mo1 C2 78.3(3) . . ? C1 Mo1 C9 106.9(3) . . ? C2 Mo1 C9 104.9(3) . . ? C1 Mo1 C10 71.9(3) . . ? C2 Mo1 C10 103.5(3) . . ? C9 Mo1 C10 35.6(2) . . ? C1 Mo1 C8 118.0(3) . . ? C2 Mo1 C8 75.6(3) . . ? C9 Mo1 C8 34.7(2) . . ? C10 Mo1 C8 61.5(2) . . ? C1 Mo1 S1 89.3(2) . . ? C2 Mo1 S1 101.0(2) . . ? C9 Mo1 S1 151.61(19) . . ? C10 Mo1 S1 145.08(18) . . ? C8 Mo1 S1 150.34(17) . . ? C1 Mo1 S2 108.5(2) . . ? C2 Mo1 S2 167.7(2) . . ? C9 Mo1 S2 83.12(19) . . ? C10 Mo1 S2 88.48(17) . . ? C8 Mo1 S2 108.59(18) . . ? S1 Mo1 S2 69.49(5) . . ? C1 Mo1 Mo2 140.8(2) . . ? C2 Mo1 Mo2 114.88(19) . . ? C9 Mo1 Mo2 104.74(19) . . ? C10 Mo1 Mo2 132.45(17) . . ? C8 Mo1 Mo2 101.19(17) . . ? S1 Mo1 Mo2 52.80(4) . . ? S2 Mo1 Mo2 53.38(4) . . ? C1 Mo1 Au1 135.68(19) . . ? C2 Mo1 Au1 65.09(19) . . ? C9 Mo1 Au1 106.1(2) . . ? C10 Mo1 Au1 138.69(18) . . ? C8 Mo1 Au1 77.26(17) . . ? S1 Mo1 Au1 74.77(4) . . ? S2 Mo1 Au1 104.07(4) . . ? Mo2 Mo1 Au1 51.440(14) . . ? P1 Au1 C6 133.25(16) . . ? P1 Au1 Mo2 162.17(5) . . ? C6 Au1 Mo2 43.25(16) . . ? P1 Au1 Mo1 136.99(5) . . ? C6 Au1 Mo1 72.98(14) . . ? Mo2 Au1 Mo1 60.794(16) . . ? C7 S1 Mo1 92.96(19) . . ? C7 S1 Mo2 58.93(18) . . ? Mo1 S1 Mo2 75.90(5) . . ? C7 S2 Mo1 90.37(19) . . ? C7 S2 Mo2 57.88(18) . . ? Mo1 S2 Mo2 73.52(4) . . ? C7 P2 C50 113.7(3) . . ? C7 P2 C60 106.7(3) . . ? C50 P2 C60 105.8(3) . . ? C7 P2 C70 111.1(3) . . ? C50 P2 C70 109.5(3) . . ? C60 P2 C70 109.8(3) . . ? C20 P1 C40 103.6(3) . . ? C20 P1 C30 106.3(3) . . ? C40 P1 C30 103.0(3) . . ? C20 P1 Au1 109.8(2) . . ? C40 P1 Au1 118.6(2) . . ? C30 P1 Au1 114.4(2) . . ? O1 C1 Mo1 177.0(6) . . ? O2 C2 Mo1 172.8(6) . . ? O4 C4 Mo2 173.7(6) . . ? O5 C5 Mo2 176.6(6) . . ? O6 C6 Mo2 172.5(6) . . ? O6 C6 Au1 116.8(5) . . ? Mo2 C6 Au1 69.4(2) . . ? S2 C7 S1 107.1(3) . . ? S2 C7 P2 125.5(3) . . ? S1 C7 P2 118.0(3) . . ? S2 C7 Mo2 79.3(2) . . ? S1 C7 Mo2 77.2(2) . . ? P2 C7 Mo2 137.3(3) . . ? C9 C8 Mo1 66.4(4) . . ? C8 C9 C10 120.1(7) . . ? C8 C9 Mo1 78.9(4) . . ? C10 C9 Mo1 75.5(4) . . ? C9 C10 Mo1 68.9(4) . . ? C25 C20 C21 116.9(6) . . ? C25 C20 P1 123.8(5) . . ? C21 C20 P1 119.3(5) . . ? C22 C21 C20 121.4(7) . . ? C23 C22 C21 120.6(7) . . ? C22 C23 C24 119.8(7) . . ? C23 C24 C25 120.2(7) . . ? C20 C25 C24 121.0(7) . . ? C31 C30 C35 118.2(6) . . ? C31 C30 P1 123.2(5) . . ? C35 C30 P1 118.6(5) . . ? C30 C31 C32 122.3(7) . . ? C33 C32 C31 118.9(8) . . ? C32 C33 C34 120.0(8) . . ? C33 C34 C35 120.8(8) . . ? C30 C35 C34 119.7(7) . . ? C45 C40 C41 117.0(6) . . ? C45 C40 P1 124.2(5) . . ? C41 C40 P1 118.8(5) . . ? C42 C41 C40 121.1(7) . . ? C43 C42 C41 120.4(7) . . ? C42 C43 C44 120.8(7) . . ? C43 C44 C45 119.3(7) . . ? C40 C45 C44 121.5(6) . . ? C51 C50 C55 109.3(5) . . ? C51 C50 P2 115.6(4) . . ? C55 C50 P2 114.7(4) . . ? C50 C51 C52 111.6(5) . . ? C53 C52 C51 111.3(6) . . ? C52 C53 C54 111.9(5) . . ? C55 C54 C53 112.7(6) . . ? C54 C55 C50 111.4(5) . . ? C65 C60 C61 110.2(5) . . ? C65 C60 P2 117.5(4) . . ? C61 C60 P2 114.6(4) . . ? C62 C61 C60 110.7(5) . . ? C63 C62 C61 111.4(6) . . ? C64 C63 C62 111.9(6) . . ? C63 C64 C65 111.9(6) . . ? C64 C65 C60 110.2(6) . . ? C75 C70 C71 110.0(6) . . ? C75 C70 P2 117.9(5) . . ? C71 C70 P2 112.0(4) . . ? C72 C71 C70 111.3(6) . . ? C73 C72 C71 112.2(6) . . ? C72 C73 C74 112.2(7) . . ? C73 C74 C75 109.4(6) . . ? C70 C75 C74 111.4(6) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.859 _refine_diff_density_min -0.862 _refine_diff_density_rms 0.095 #===END data_Compound_6c_(wm182) _database_code_CSD 195128 _chemical_melting_point ? _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' Enraf-nonius CAD4 ' _refine_ls_matrix_type full _refine_ls_weighting_scheme ; Chebychev polynomial (Carruthers & Watkin, 1979) ; _atom_sites_solution_primary Direct_Methods _atom_sites_solution_hydrogens Geometric _refine_ls_hydrogen_treatment ; H atoms placed geometrically after each cycle ; #**************************************************************************** _chemical_name_systematic ; # IUPAC name, in full ? ; _cell_length_a 12.213(2) _cell_angle_alpha 92.61(9) _cell_length_b 12.867(3) _cell_angle_beta 111.38(9) _cell_length_c 15.503(4) _cell_angle_gamma 91.13(8) _cell_volume 2264.37 _symmetry_cell_setting 'triclinic ' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'Au ' -2.6880 8.7980 16.8819 0.4611 18.5913 8.6216 25.5582 1.4826 5.8600 36.3956 12.0658 International_Tables_Vol_IV_Table_2.2B 'Mo ' -1.8250 0.6880 3.7025 0.2772 17.2356 1.0958 12.8876 11.0040 3.7429 61.6584 4.3875 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'S ' 0.1100 0.1240 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B 'W ' -1.4210 6.8720 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560 9.8875 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C45 H53 Au1 W1 Mo1 P2 S2 O5 ' _chemical_formula_moiety ' C45 H53 Au1 W1 Mo1 P2 S2 O5 ' _chemical_compound_source ; ? ; _chemical_formula_weight 1267.72 _cell_measurement_reflns_used 2 _cell_measurement_theta_min 12 _cell_measurement_theta_max 13 _cell_measurement_temperature 293 _cell_formula_units_Z 2.00 _exptl_crystal_description ' parallelepiped ' _exptl_crystal_colour ' brown ' _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.87 _exptl_crystal_density_meas ? _exptl_crystal_F_000 1224.83 _exptl_absorpt_coefficient_mu 6.28 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.6667 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _diffrn_standards_interval_time 3600 _diffrn_standards_interval_count 100 _diffrn_standards_number 2 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 293 _diffrn_reflns_number 5832 _reflns_number_total 5311 _diffrn_reflns_av_R_equivalents 0.048 _reflns_number_observed 2911 _diffrn_reflns_theta_min 1.00 _diffrn_reflns_theta_max 22.00 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -12 _reflns_limit_h_max 11 _reflns_limit_k_min -13 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _refine_ls_structure_factor_coef F _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -1.57 _refine_diff_density_max 2.45 _refine_ls_number_reflns 2911 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0522 _refine_ls_R_factor_all 0.0522 _refine_ls_wR_factor_obs 0.0595 _refine_ls_wR_factor_all 0.0595 _refine_ls_goodness_of_fit_obs 1.4752 _refine_ls_goodness_of_fit_all 1.4752 _refine_ls_shift/esd_max 0.008036 _refine_ls_abs_structure_details ' from Flack enantiopole 0.000' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method 2\q/\w loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type AU1 0.33305(9) 0.27949(8) 0.21713(8) 0.0441(4) 1.0000 Uiso W1 0.28911(8) 0.45932(7) 0.29579(7) 0.0265(3) 1.0000 Uiso MO1 0.1768(2) 0.2706(2) 0.3468(1) 0.0302(5) 1.0000 Uiso P1 0.3965(5) 0.1602(5) 0.1317(4) 0.034(2) 1.0000 Uiso P2 0.0321(5) 0.6127(4) 0.2876(4) 0.026(1) 1.0000 Uiso S2 0.0801(5) 0.3925(4) 0.2289(4) 0.030(1) 1.0000 Uiso S1 0.1984(5) 0.4545(4) 0.4191(4) 0.031(1) 1.0000 Uiso O1 -0.063(2) 0.177(2) 0.325(2) 0.081(7) 1.0000 Uiso O2 0.158(2) 0.064(2) 0.229(1) 0.065(5) 1.0000 Uiso O4 0.324(2) 0.509(1) 0.112(1) 0.062(5) 1.0000 Uiso O5 0.433(2) 0.670(2) 0.346(1) 0.070(6) 1.0000 Uiso O6 0.528(2) 0.375(1) 0.424(1) 0.063(5) 1.0000 Uiso C1 0.027(3) 0.212(2) 0.334(2) 0.064(8) 1.0000 Uiso C2 0.163(2) 0.144(2) 0.270(2) 0.033(6) 1.0000 Uiso C4 0.313(2) 0.485(2) 0.180(2) 0.037(6) 1.0000 Uiso C5 0.378(2) 0.589(2) 0.331(2) 0.051(7) 1.0000 Uiso C6 0.436(2) 0.405(2) 0.370(2) 0.036(6) 1.0000 Uiso C7 0.123(2) 0.504(2) 0.307(2) 0.026(5) 1.0000 Uiso C8 0.345(2) 0.179(2) 0.430(2) 0.054(7) 1.0000 Uiso C9 0.301(2) 0.233(2) 0.489(2) 0.037(6) 1.0000 Uiso C10 0.190(2) 0.209(2) 0.491(2) 0.053(8) 1.0000 Uiso C20 0.513(2) 0.221(2) 0.106(2) 0.042(6) 1.0000 Uiso C21 0.494(2) 0.315(2) 0.060(2) 0.043(7) 1.0000 Uiso C22 0.576(2) 0.361(2) 0.033(2) 0.047(7) 1.0000 Uiso C23 0.682(3) 0.318(2) 0.053(2) 0.060(8) 1.0000 Uiso C24 0.703(3) 0.226(2) 0.093(2) 0.063(8) 1.0000 Uiso C25 0.619(3) 0.175(2) 0.119(2) 0.061(8) 1.0000 Uiso C30 0.453(2) 0.045(2) 0.192(2) 0.037(6) 1.0000 Uiso C31 0.444(2) -0.050(2) 0.141(2) 0.045(7) 1.0000 Uiso C32 0.490(2) -0.141(2) 0.191(2) 0.058(8) 1.0000 Uiso C33 0.539(3) -0.133(2) 0.285(2) 0.063(8) 1.0000 Uiso C34 0.542(3) -0.045(3) 0.331(2) 0.08(1) 1.0000 Uiso C35 0.501(2) 0.052(2) 0.288(2) 0.051(7) 1.0000 Uiso C40 0.291(2) 0.110(2) 0.020(2) 0.028(5) 1.0000 Uiso C41 0.189(2) 0.055(2) 0.018(2) 0.046(7) 1.0000 Uiso C42 0.109(2) 0.016(2) -0.066(2) 0.043(7) 1.0000 Uiso C43 0.132(2) 0.025(2) -0.149(2) 0.056(8) 1.0000 Uiso C44 0.227(2) 0.081(2) -0.144(2) 0.050(7) 1.0000 Uiso C45 0.304(2) 0.124(2) -0.061(2) 0.047(7) 1.0000 Uiso C50 0.017(2) 0.671(2) 0.180(2) 0.033(6) 1.0000 Uiso C51 0.131(2) 0.718(2) 0.176(2) 0.050(7) 1.0000 Uiso C52 0.114(2) 0.781(2) 0.092(2) 0.039(6) 1.0000 Uiso C53 0.041(3) 0.714(2) 0.005(2) 0.069(9) 1.0000 Uiso C54 -0.076(2) 0.667(2) 0.006(2) 0.041(6) 1.0000 Uiso C55 -0.046(2) 0.607(2) 0.093(2) 0.034(6) 1.0000 Uiso C60 -0.114(2) 0.564(2) 0.274(2) 0.030(5) 1.0000 Uiso C61 -0.215(2) 0.641(2) 0.245(2) 0.041(6) 1.0000 Uiso C62 -0.331(2) 0.584(2) 0.221(2) 0.057(8) 1.0000 Uiso C63 -0.333(2) 0.517(2) 0.300(2) 0.055(8) 1.0000 Uiso C64 -0.243(2) 0.447(2) 0.323(2) 0.055(8) 1.0000 Uiso C65 -0.120(2) 0.502(2) 0.355(2) 0.053(7) 1.0000 Uiso C70 0.082(2) 0.710(2) 0.383(2) 0.033(6) 1.0000 Uiso C71 0.030(2) 0.816(2) 0.359(2) 0.049(7) 1.0000 Uiso C72 0.061(3) 0.893(2) 0.444(2) 0.063(8) 1.0000 Uiso C73 0.189(3) 0.904(2) 0.488(2) 0.069(9) 1.0000 Uiso C74 0.247(2) 0.804(2) 0.517(2) 0.055(7) 1.0000 Uiso C75 0.215(2) 0.726(2) 0.434(2) 0.048(7) 1.0000 Uiso H81 0.4260 0.1970 0.4292 0.08(1) 1.0000 Uiso H82 0.2977 0.1200 0.3864 0.08(1) 1.0000 Uiso H91 0.3502 0.2922 0.5323 0.08(1) 1.0000 Uiso H101 0.1583 0.2488 0.5339 0.08(1) 1.0000 Uiso H102 0.1390 0.1509 0.4486 0.08(1) 1.0000 Uiso H211 0.4161 0.3503 0.0474 0.08(1) 1.0000 Uiso H221 0.5583 0.4270 -0.0027 0.08(1) 1.0000 Uiso H231 0.7463 0.3571 0.0385 0.08(1) 1.0000 Uiso H241 0.7816 0.1913 0.1024 0.08(1) 1.0000 Uiso H251 0.6368 0.1053 0.1496 0.08(1) 1.0000 Uiso H311 0.4042 -0.0541 0.0703 0.08(1) 1.0000 Uiso H321 0.4856 -0.2116 0.1568 0.08(1) 1.0000 Uiso H331 0.5738 -0.1979 0.3192 0.08(1) 1.0000 Uiso H341 0.5774 -0.0438 0.4028 0.08(1) 1.0000 Uiso H351 0.5044 0.1205 0.3251 0.08(1) 1.0000 Uiso H411 0.1743 0.0441 0.0783 0.08(1) 1.0000 Uiso H421 0.0333 -0.0207 -0.0694 0.08(1) 1.0000 Uiso H431 0.0771 -0.0105 -0.2112 0.08(1) 1.0000 Uiso H441 0.2429 0.0936 -0.2033 0.08(1) 1.0000 Uiso H451 0.3761 0.1669 -0.0591 0.08(1) 1.0000 Uiso H501 -0.0386 0.7306 0.1646 0.08(1) 1.0000 Uiso H511 0.1719 0.7643 0.2348 0.08(1) 1.0000 Uiso H512 0.1861 0.6599 0.1765 0.08(1) 1.0000 Uiso H521 0.0703 0.8459 0.0961 0.08(1) 1.0000 Uiso H522 0.1923 0.8036 0.0894 0.08(1) 1.0000 Uiso H531 0.0248 0.7572 -0.0510 0.08(1) 1.0000 Uiso H532 0.0920 0.6547 -0.0020 0.08(1) 1.0000 Uiso H541 -0.1310 0.7238 0.0065 0.08(1) 1.0000 Uiso H542 -0.1165 0.6195 -0.0518 0.08(1) 1.0000 Uiso H551 -0.1200 0.5745 0.0955 0.08(1) 1.0000 Uiso H552 0.0066 0.5481 0.0882 0.08(1) 1.0000 Uiso H601 -0.1513 0.5108 0.2205 0.08(1) 1.0000 Uiso H611 -0.2029 0.6946 0.2972 0.08(1) 1.0000 Uiso H612 -0.2116 0.6795 0.1897 0.08(1) 1.0000 Uiso H621 -0.3957 0.6370 0.2060 0.08(1) 1.0000 Uiso H622 -0.3470 0.5388 0.1619 0.08(1) 1.0000 Uiso H631 -0.3928 0.5240 0.3317 0.08(1) 1.0000 Uiso H641 -0.2554 0.3673 0.3204 0.08(1) 1.0000 Uiso H651 -0.1068 0.5502 0.4108 0.08(1) 1.0000 Uiso H652 -0.0554 0.4496 0.3721 0.08(1) 1.0000 Uiso H701 0.0552 0.6923 0.4366 0.08(1) 1.0000 Uiso H711 0.0625 0.8457 0.3134 0.08(1) 1.0000 Uiso H712 -0.0586 0.8070 0.3261 0.08(1) 1.0000 Uiso H721 0.0231 0.9618 0.4264 0.08(1) 1.0000 Uiso H722 0.0272 0.8635 0.4904 0.08(1) 1.0000 Uiso H731 0.2116 0.9562 0.5424 0.08(1) 1.0000 Uiso H732 0.2193 0.9337 0.4403 0.08(1) 1.0000 Uiso H741 0.3354 0.8154 0.5459 0.08(1) 1.0000 Uiso H742 0.2197 0.7748 0.5657 0.08(1) 1.0000 Uiso H751 0.2507 0.7515 0.3897 0.08(1) 1.0000 Uiso H752 0.2503 0.6566 0.4561 0.08(1) 1.0000 Uiso _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag AU1 . W1 . 2.720(1) yes AU1 . MO1 . 3.242(2) yes AU1 . P1 . 2.307(6) yes W1 . MO1 . 3.040(2) yes W1 . S2 . 2.497(6) yes W1 . S1 . 2.538(6) yes W1 . C4 . 1.96(2) yes W1 . C5 . 1.92(3) yes W1 . C6 . 1.91(2) yes W1 . C7 . 2.18(2) yes MO1 . S2 . 2.441(6) yes MO1 . S1 . 2.539(6) yes MO1 . C1 . 1.90(3) yes MO1 . C2 . 1.94(2) yes MO1 . C8 . 2.36(3) yes MO1 . C9 . 2.25(2) yes MO1 . C10 . 2.35(3) yes P1 . C20 . 1.79(2) yes P1 . C30 . 1.80(2) yes P1 . C40 . 1.82(2) yes P2 . C7 . 1.77(2) yes P2 . C50 . 1.81(2) yes P2 . C60 . 1.82(2) yes P2 . C70 . 1.81(2) yes S2 . C7 . 1.77(2) yes S1 . C7 . 1.80(2) yes O1 . C1 . 1.14(3) yes O2 . C2 . 1.17(3) yes O4 . C4 . 1.17(3) yes O5 . C5 . 1.20(3) yes O6 . C6 . 1.21(3) yes C8 . C9 . 1.40(3) yes C8 . H81 . 1.01(3) no C8 . H82 . 1.01(3) no C9 . C10 . 1.38(3) yes C9 . H91 . 1.02(2) no C10 . H101 . 1.02(3) no C10 . H102 . 1.01(3) no C20 . C21 . 1.42(3) yes C20 . C25 . 1.38(3) yes C21 . C22 . 1.35(3) yes C21 . H211 . 1.02(2) no C22 . C23 . 1.34(3) yes C22 . H221 . 1.02(3) no C23 . C24 . 1.35(4) yes C23 . H231 . 1.02(3) no C24 . C25 . 1.40(4) yes C24 . H241 . 1.03(3) no C25 . H251 . 1.02(3) no C30 . C31 . 1.40(3) yes C30 . C35 . 1.38(3) yes C31 . C32 . 1.44(4) yes C31 . H311 . 1.03(3) no C32 . C33 . 1.35(4) yes C32 . H321 . 1.03(3) no C33 . C34 . 1.30(4) yes C33 . H331 . 1.03(3) no C34 . C35 . 1.45(4) yes C34 . H341 . 1.03(3) no C35 . H351 . 1.03(3) no C40 . C41 . 1.40(3) yes C40 . C45 . 1.34(3) yes C41 . C42 . 1.38(3) yes C41 . H411 . 1.03(3) no C42 . C43 . 1.42(4) yes C42 . H421 . 1.02(2) no C43 . C44 . 1.33(3) yes C43 . H431 . 1.03(3) no C44 . C45 . 1.37(3) yes C44 . H441 . 1.02(3) no C45 . H451 . 1.02(3) no C50 . C51 . 1.53(3) yes C50 . C55 . 1.49(3) yes C50 . H501 . 1.02(2) no C51 . C52 . 1.52(3) yes C51 . H511 . 1.01(3) no C51 . H512 . 1.02(3) no C52 . C53 . 1.53(4) yes C52 . H521 . 1.02(2) no C52 . H522 . 1.01(2) no C53 . C54 . 1.54(4) yes C53 . H531 . 1.01(3) no C53 . H532 . 1.02(3) no C54 . C55 . 1.51(3) yes C54 . H541 . 1.01(2) no C54 . H542 . 1.01(2) no C55 . H551 . 1.01(2) no C55 . H552 . 1.02(2) no C60 . C61 . 1.54(3) yes C60 . C65 . 1.53(3) yes C60 . H601 . 1.02(2) no C61 . C62 . 1.49(3) yes C61 . H611 . 1.01(2) no C61 . H612 . 1.02(2) no C62 . C63 . 1.54(4) yes C62 . H621 . 1.02(3) no C62 . H622 . 1.02(3) no C63 . C64 . 1.39(4) yes C63 . H631 . 1.02(3) no C64 . C65 . 1.54(4) yes C64 . H641 . 1.03(3) no C65 . H651 . 1.01(3) no C65 . H652 . 1.02(3) no C70 . C71 . 1.51(3) yes C70 . C75 . 1.53(3) yes C70 . H701 . 1.03(2) no C71 . C72 . 1.54(4) yes C71 . H711 . 1.02(3) no C71 . H712 . 1.02(3) no C72 . C73 . 1.46(4) yes C72 . H721 . 1.01(3) no C72 . H722 . 1.03(3) no C73 . C74 . 1.48(4) yes C73 . H731 . 1.01(3) no C73 . H732 . 1.03(3) no C74 . C75 . 1.52(4) yes C74 . H741 . 1.01(3) no C74 . H742 . 1.02(3) no C75 . H751 . 1.01(3) no C75 . H752 . 1.01(3) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag W1 . AU1 . MO1 . 60.57(5) no W1 . AU1 . P1 . 163.4(2) no MO1 . AU1 . P1 . 136.0(2) no AU1 . W1 . MO1 . 68.23(5) no AU1 . W1 . S2 . 84.2(1) no MO1 . W1 . S2 . 51.2(1) no AU1 . W1 . S1 . 120.5(1) no MO1 . W1 . S1 . 53.2(1) no S2 . W1 . S1 . 68.6(2) no AU1 . W1 . C4 . 69.0(7) no MO1 . W1 . C4 . 129.4(7) no S2 . W1 . C4 . 98.9(7) no S1 . W1 . C4 . 161.9(7) no AU1 . W1 . C5 . 130.6(8) no MO1 . W1 . C5 . 150.1(8) no S2 . W1 . C5 . 139.6(8) no S1 . W1 . C5 . 100.7(8) no C4 . W1 . C5 . 80.1(11) no AU1 . W1 . C6 . 68.2(7) no MO1 . W1 . C6 . 85.9(7) no S2 . W1 . C6 . 135.8(7) no S1 . W1 . C6 . 95.9(7) no C4 . W1 . C6 . 102.1(10) no AU1 . W1 . C7 . 127.5(6) no MO1 . W1 . C7 . 71.6(6) no S2 . W1 . C7 . 44.0(6) no S1 . W1 . C7 . 44.1(6) no C4 . W1 . C7 . 117.9(9) no C5 . W1 . C6 . 82.4(10) no C5 . W1 . C7 . 100.7(10) no C6 . W1 . C7 . 139.9(9) no AU1 . MO1 . W1 . 51.19(4) no AU1 . MO1 . S2 . 74.5(1) no W1 . MO1 . S2 . 52.8(1) no AU1 . MO1 . S1 . 103.7(1) no W1 . MO1 . S1 . 53.2(1) no S2 . MO1 . S1 . 69.5(2) no AU1 . MO1 . C1 . 135.6(9) no W1 . MO1 . C1 . 141.1(9) no S2 . MO1 . C1 . 89.6(9) no S1 . MO1 . C1 . 109.1(9) no AU1 . MO1 . C2 . 66.4(7) no W1 . MO1 . C2 . 115.7(7) no S2 . MO1 . C2 . 100.7(7) no S1 . MO1 . C2 . 168.1(7) no C1 . MO1 . C2 . 76.7(11) no AU1 . MO1 . C8 . 76.8(7) no W1 . MO1 . C8 . 100.8(7) no S2 . MO1 . C8 . 149.7(7) no S1 . MO1 . C8 . 108.8(7) no C1 . MO1 . C8 . 118.1(11) no AU1 . MO1 . C9 . 106.4(6) no W1 . MO1 . C9 . 105.4(6) no S2 . MO1 . C9 . 152.3(6) no S1 . MO1 . C9 . 83.7(6) no C1 . MO1 . C9 . 106.2(11) no AU1 . MO1 . C10 . 138.9(7) no W1 . MO1 . C10 . 132.0(7) no S2 . MO1 . C10 . 144.9(7) no S1 . MO1 . C10 . 88.2(7) no C1 . MO1 . C10 . 72.1(11) no C2 . MO1 . C8 . 76.1(9) no C2 . MO1 . C9 . 104.9(9) no C8 . MO1 . C9 . 35.1(9) no C2 . MO1 . C10 . 103.6(9) no C8 . MO1 . C10 . 62.2(9) no C9 . MO1 . C10 . 35.0(8) no AU1 . P1 . C20 . 108.3(8) no AU1 . P1 . C30 . 113.6(8) no C20 . P1 . C30 . 107.3(11) no AU1 . P1 . C40 . 117.8(7) no C20 . P1 . C40 . 105.1(11) no C30 . P1 . C40 . 103.9(10) no C7 . P2 . C50 . 111.5(10) no C7 . P2 . C60 . 107.0(10) no C50 . P2 . C60 . 106.2(10) no C7 . P2 . C70 . 112.7(10) no C50 . P2 . C70 . 110.4(11) no C60 . P2 . C70 . 108.7(10) no W1 . S2 . MO1 . 76.0(2) no W1 . S2 . C7 . 58.4(7) no MO1 . S2 . C7 . 94.6(7) no W1 . S1 . MO1 . 73.6(2) no W1 . S1 . C7 . 57.3(7) no MO1 . S1 . C7 . 90.7(7) no MO1 . C1 . O1 . 179.7(28) no MO1 . C2 . O2 . 175.0(21) no W1 . C4 . O4 . 173.6(21) no W1 . C5 . O5 . 175.0(24) no W1 . C6 . O6 . 173.4(21) no W1 . C7 . P2 . 139.4(12) no W1 . C7 . S2 . 77.6(8) no P2 . C7 . S2 . 119.9(12) no W1 . C7 . S1 . 78.6(8) no P2 . C7 . S1 . 123.9(13) no S2 . C7 . S1 . 105.1(11) no MO1 . C8 . C9 . 68.2(14) no MO1 . C9 . C8 . 76.6(15) no MO1 . C9 . C10 . 76.2(15) no C8 . C9 . C10 . 122.1(24) no MO1 . C10 . C9 . 68.8(15) no P1 . C20 . C21 . 119.9(18) no P1 . C20 . C25 . 123.6(21) no C21 . C20 . C25 . 116.2(23) no C20 . C21 . C22 . 122.5(23) no C21 . C22 . C23 . 119.7(26) no C22 . C23 . C24 . 120.8(28) no C23 . C24 . C25 . 120.9(28) no C20 . C25 . C24 . 119.7(27) no P1 . C30 . C31 . 119.8(19) no P1 . C30 . C35 . 119.0(19) no C31 . C30 . C35 . 121.2(23) no C30 . C31 . C32 . 118.5(24) no C31 . C32 . C33 . 119.5(26) no C32 . C33 . C34 . 121.6(31) no C33 . C34 . C35 . 123.5(32) no C30 . C35 . C34 . 115.6(25) no P1 . C40 . C41 . 118.7(18) no P1 . C40 . C45 . 123.2(18) no C41 . C40 . C45 . 118.1(22) no C40 . C41 . C42 . 118.8(23) no C41 . C42 . C43 . 120.9(24) no C42 . C43 . C44 . 117.6(26) no C43 . C44 . C45 . 121.4(26) no C40 . C45 . C44 . 122.9(24) no P2 . C50 . C51 . 114.9(17) no P2 . C50 . C55 . 117.0(16) no C51 . C50 . C55 . 109.6(19) no C50 . C51 . C52 . 114.0(21) noo C51 . C52 . C53 . 108.9(21) no C52 . C53 . C54 . 115.4(24) no C53 . C54 . C55 . 107.0(21) no C50 . C55 . C54 . 114.0(19) no P2 . C60 . C61 . 117.4(16) no P2 . C60 . C65 . 114.9(16) no C61 . C60 . C65 . 110.6(19) no C60 . C61 . C62 . 110.2(20) no C61 . C62 . C63 . 112.0(23) no C62 . C63 . C64 . 111.4(24) no C63 . C64 . C65 . 112.5(24) no C60 . C65 . C64 . 108.1(21) no P2 . C70 . C71 . 114.1(17) no P2 . C70 . C75 . 116.9(17) no C71 . C70 . C75 . 108.3(20) no C70 . C71 . C72 . 113.0(22) no C71 . C72 . C73 . 108.3(24) no C72 . C73 . C74 . 113.9(26) no C73 . C74 . C75 . 110.5(24) no C70 . C75 . C74 . 112.8(21) no #===END