# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global data_s5gao13 #TrackingRef '15961_web_deposit_cif_file_0_GeorginaRosair_1354882535.7a.cif' _audit_creation_date 2012-12-04 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C47 H59 Au2 O P2 S, F6 Sb' _chemical_formula_sum 'C47 H59 Au2 F6 O P2 S Sb' _chemical_formula_weight 1363.63 _chemical_melting_point ? 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' F F 0.0171 0.0103 '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' Sb Sb -0.5866 1.5461 '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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 13.4006(7) _cell_length_b 13.5192(7) _cell_length_c 15.7860(8) _cell_angle_alpha 68.403(2) _cell_angle_beta 80.115(2) _cell_angle_gamma 65.851(2) _cell_volume 2425.6(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9866 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.246 _cell_measurement_theta_min 2.700 _exptl_absorpt_coefficient_mu 6.752 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.3951 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. R(int) was 0.1311 before and 0.0479 after correction. The Ratio of minimum to maximum transmission is 0.5300. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.867 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1316 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_unetI/netI 0.0349 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 35962 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 1.39 _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'MO K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 9001 _reflns_number_total 9865 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'SAINT v7.68A (Bruker, 2009)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.988 _refine_diff_density_min -1.476 _refine_diff_density_rms 0.164 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 553 _refine_ls_number_reflns 9865 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0259 _refine_ls_R_factor_gt 0.0216 _refine_ls_restrained_S_all 1.139 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+1.8558P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.0707 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Au1 Au 0.359854(12) 0.592644(13) 0.264425(10) 0.01281(5) Uani 1 1 d . . . Sb1 Sb 0.19274(2) -0.04974(2) 0.756066(18) 0.01725(7) Uani 1 1 d . . . S1 S 0.40887(8) 0.39466(8) 0.32252(6) 0.0127(2) Uani 1 1 d . . . P1 P 0.31040(8) 0.78663(9) 0.20815(7) 0.0125(2) Uani 1 1 d . . . F1 F 0.2762(3) -0.0132(2) 0.81421(19) 0.0386(7) Uani 1 1 d . . . O1 O 0.3379(3) 0.4468(3) 0.4760(2) 0.0304(8) Uani 1 1 d . . . C1 C 0.2416(3) 0.8397(3) 0.0965(3) 0.0162(8) Uani 1 1 d . . . Au2 Au 0.239005(12) 0.403594(12) 0.297064(9) 0.01226(5) Uani 1 1 d . . . P2 P 0.07433(8) 0.39731(9) 0.28785(7) 0.0125(2) Uani 1 1 d . . . F2 F 0.0759(2) -0.0094(3) 0.8361(2) 0.0518(9) Uani 1 1 d . . . C2 C 0.3342(3) 0.7999(4) 0.0306(3) 0.0192(9) Uani 1 1 d . . . H2A H 0.3033 0.8094 -0.0251 0.029 Uiso 1 1 calc R . . H2B H 0.3794 0.7187 0.0593 0.029 Uiso 1 1 calc R . . H2C H 0.3794 0.8459 0.0154 0.029 Uiso 1 1 calc R . . F3 F 0.1099(3) -0.0888(3) 0.7002(2) 0.0594(10) Uani 1 1 d . . . C3 C 0.1621(4) 0.7784(4) 0.1077(3) 0.0199(9) Uani 1 1 d . . . H3A H 0.1008 0.8044 0.1484 0.030 Uiso 1 1 calc R . . H3B H 0.2010 0.6951 0.1337 0.030 Uiso 1 1 calc R . . H3C H 0.1342 0.7969 0.0480 0.030 Uiso 1 1 calc R . . F4 F 0.3116(3) -0.0936(3) 0.6801(2) 0.0545(9) Uani 1 1 d . . . C4 C 0.1772(4) 0.9696(4) 0.0573(3) 0.0222(9) Uani 1 1 d . . . H4A H 0.2255 1.0105 0.0501 0.033 Uiso 1 1 calc R . . H4B H 0.1160 0.9932 0.0989 0.033 Uiso 1 1 calc R . . H4C H 0.1490 0.9879 -0.0022 0.033 Uiso 1 1 calc R . . F5 F 0.2419(2) -0.1996(2) 0.84053(19) 0.0362(7) Uani 1 1 d . . . C5 C 0.2271(3) 0.8463(4) 0.2989(3) 0.0174(9) Uani 1 1 d . . . F6 F 0.1446(3) 0.0993(3) 0.6742(2) 0.0472(8) Uani 1 1 d . . . C6 C 0.3009(4) 0.7873(4) 0.3818(3) 0.0270(11) Uani 1 1 d . . . H6A H 0.2599 0.8117 0.4330 0.041 Uiso 1 1 calc R . . H6B H 0.3649 0.8088 0.3665 0.041 Uiso 1 1 calc R . . H6C H 0.3249 0.7038 0.3987 0.041 Uiso 1 1 calc R . . C7 C 0.1290(4) 0.8103(4) 0.3228(3) 0.0234(10) Uani 1 1 d . . . H7A H 0.0891 0.8317 0.3756 0.035 Uiso 1 1 calc R . . H7B H 0.1544 0.7269 0.3376 0.035 Uiso 1 1 calc R . . H7C H 0.0805 0.8492 0.2708 0.035 Uiso 1 1 calc R . . C8 C 0.1868(4) 0.9768(4) 0.2762(3) 0.0291(11) Uani 1 1 d . . . H8A H 0.1470 1.0158 0.2191 0.044 Uiso 1 1 calc R . . H8B H 0.2496 0.9988 0.2696 0.044 Uiso 1 1 calc R . . H8C H 0.1380 0.9990 0.3255 0.044 Uiso 1 1 calc R . . C9 C 0.4270(3) 0.8320(3) 0.1791(3) 0.0140(8) Uani 1 1 d . . . C10 C 0.4075(4) 0.9495(4) 0.1417(3) 0.0186(9) Uani 1 1 d . . . H10 H 0.3344 1.0037 0.1387 0.022 Uiso 1 1 calc R . . C11 C 0.4919(4) 0.9891(4) 0.1090(3) 0.0193(9) Uani 1 1 d . . . H11 H 0.4764 1.0692 0.0841 0.023 Uiso 1 1 calc R . . C12 C 0.5994(4) 0.9106(4) 0.1128(3) 0.0207(9) Uani 1 1 d . . . H12 H 0.6579 0.9366 0.0903 0.025 Uiso 1 1 calc R . . C13 C 0.6201(3) 0.7944(4) 0.1498(3) 0.0193(9) Uani 1 1 d . . . H13 H 0.6935 0.7410 0.1516 0.023 Uiso 1 1 calc R . . C14 C 0.5363(3) 0.7529(4) 0.1848(3) 0.0157(9) Uani 1 1 d . . . C15 C 0.5740(3) 0.6243(3) 0.2269(3) 0.0150(8) Uani 1 1 d . . . C16 C 0.5803(3) 0.5730(4) 0.3213(3) 0.0179(9) Uani 1 1 d . . . H16 H 0.5514 0.6193 0.3595 0.021 Uiso 1 1 calc R . . C17 C 0.6289(4) 0.4540(4) 0.3598(3) 0.0251(10) Uani 1 1 d . . . H17 H 0.6345 0.4196 0.4241 0.030 Uiso 1 1 calc R . . C18 C 0.6692(4) 0.3851(4) 0.3047(4) 0.0288(11) Uani 1 1 d . . . H18 H 0.7005 0.3039 0.3313 0.035 Uiso 1 1 calc R . . C19 C 0.6636(4) 0.4354(4) 0.2111(3) 0.0281(11) Uani 1 1 d . . . H19 H 0.6917 0.3887 0.1733 0.034 Uiso 1 1 calc R . . C20 C 0.6168(3) 0.5546(4) 0.1720(3) 0.0216(9) Uani 1 1 d . . . H20 H 0.6140 0.5887 0.1075 0.026 Uiso 1 1 calc R . . C21 C 0.3877(3) 0.3695(4) 0.4462(3) 0.0176(9) Uani 1 1 d . . . C22 C 0.4386(3) 0.2470(4) 0.5032(3) 0.0178(9) Uani 1 1 d . . . C23 C 0.3950(4) 0.2108(4) 0.5915(3) 0.0228(10) Uani 1 1 d . . . H23 H 0.3341 0.2639 0.6131 0.027 Uiso 1 1 calc R . . C24 C 0.4407(4) 0.0980(4) 0.6467(3) 0.0295(11) Uani 1 1 d . . . H24 H 0.4110 0.0733 0.7062 0.035 Uiso 1 1 calc R . . C25 C 0.5302(4) 0.0204(4) 0.6153(3) 0.0321(12) Uani 1 1 d . . . H25 H 0.5613 -0.0574 0.6534 0.039 Uiso 1 1 calc R . . C26 C 0.5738(4) 0.0558(4) 0.5292(3) 0.0289(11) Uani 1 1 d . . . H26 H 0.6357 0.0028 0.5085 0.035 Uiso 1 1 calc R . . C27 C 0.5275(3) 0.1688(4) 0.4727(3) 0.0194(9) Uani 1 1 d . . . H27 H 0.5568 0.1924 0.4128 0.023 Uiso 1 1 calc R . . C28 C 0.0591(3) 0.2821(4) 0.3956(3) 0.0176(9) Uani 1 1 d . . . C29 C 0.1663(4) 0.1769(4) 0.4027(3) 0.0225(10) Uani 1 1 d . . . H29A H 0.1620 0.1125 0.4564 0.034 Uiso 1 1 calc R . . H29B H 0.2276 0.1957 0.4085 0.034 Uiso 1 1 calc R . . H29C H 0.1775 0.1556 0.3478 0.034 Uiso 1 1 calc R . . C30 C 0.0503(4) 0.3224(4) 0.4764(3) 0.0210(9) Uani 1 1 d . . . H30A H -0.0217 0.3831 0.4773 0.032 Uiso 1 1 calc R . . H30B H 0.1075 0.3523 0.4704 0.032 Uiso 1 1 calc R . . H30C H 0.0594 0.2575 0.5333 0.032 Uiso 1 1 calc R . . C31 C -0.0364(4) 0.2450(4) 0.4001(3) 0.0225(10) Uani 1 1 d . . . H31A H -0.0395 0.1890 0.4603 0.034 Uiso 1 1 calc R . . H31B H -0.0254 0.2100 0.3531 0.034 Uiso 1 1 calc R . . H31C H -0.1052 0.3123 0.3899 0.034 Uiso 1 1 calc R . . C32 C -0.0363(3) 0.5425(3) 0.2729(3) 0.0168(9) Uani 1 1 d . . . C33 C -0.0358(4) 0.6132(4) 0.1708(3) 0.0206(9) Uani 1 1 d . . . H33A H -0.0849 0.6934 0.1614 0.031 Uiso 1 1 calc R . . H33B H -0.0607 0.5816 0.1356 0.031 Uiso 1 1 calc R . . H33C H 0.0386 0.6097 0.1507 0.031 Uiso 1 1 calc R . . C34 C -0.0065(4) 0.6015(4) 0.3260(3) 0.0219(9) Uani 1 1 d . . . H34A H -0.0615 0.6795 0.3157 0.033 Uiso 1 1 calc R . . H34B H 0.0654 0.6052 0.3049 0.033 Uiso 1 1 calc R . . H34C H -0.0045 0.5574 0.3912 0.033 Uiso 1 1 calc R . . C35 C -0.1510(3) 0.5428(4) 0.3035(3) 0.0205(9) Uani 1 1 d . . . H35A H -0.1516 0.4998 0.3689 0.031 Uiso 1 1 calc R . . H35B H -0.1715 0.5066 0.2694 0.031 Uiso 1 1 calc R . . H35C H -0.2034 0.6221 0.2920 0.031 Uiso 1 1 calc R . . C36 C 0.0661(3) 0.3522(3) 0.1936(3) 0.0151(8) Uani 1 1 d . . . C37 C -0.0295(3) 0.3397(4) 0.1842(3) 0.0176(9) Uani 1 1 d . . . H37 H -0.0905 0.3616 0.2235 0.021 Uiso 1 1 calc R . . C38 C -0.0386(3) 0.2970(4) 0.1203(3) 0.0192(9) Uani 1 1 d . . . H38 H -0.1046 0.2892 0.1157 0.023 Uiso 1 1 calc R . . C39 C 0.0496(4) 0.2658(4) 0.0631(3) 0.0212(10) Uani 1 1 d . . . H39 H 0.0453 0.2340 0.0199 0.025 Uiso 1 1 calc R . . C40 C 0.1440(3) 0.2805(4) 0.0682(3) 0.0190(9) Uani 1 1 d . . . H40 H 0.2034 0.2600 0.0273 0.023 Uiso 1 1 calc R . . C41 C 0.1544(3) 0.3249(3) 0.1321(3) 0.0137(8) Uani 1 1 d . . . C42 C 0.2592(3) 0.3415(3) 0.1271(3) 0.0147(8) Uani 1 1 d . . . C43 C 0.2652(4) 0.4483(4) 0.0820(3) 0.0216(9) Uani 1 1 d . . . H43 H 0.2009 0.5127 0.0576 0.026 Uiso 1 1 calc R . . C44 C 0.3645(4) 0.4624(4) 0.0721(3) 0.0291(11) Uani 1 1 d . . . H44 H 0.3676 0.5361 0.0414 0.035 Uiso 1 1 calc R . . C45 C 0.4587(4) 0.3681(5) 0.1073(3) 0.0321(12) Uani 1 1 d . . . H45 H 0.5265 0.3773 0.1012 0.039 Uiso 1 1 calc R . . C46 C 0.4536(4) 0.2621(5) 0.1508(3) 0.0297(11) Uani 1 1 d . . . H46 H 0.5182 0.1975 0.1742 0.036 Uiso 1 1 calc R . . C47 C 0.3549(3) 0.2482(4) 0.1610(3) 0.0212(9) Uani 1 1 d . . . H47 H 0.3525 0.1740 0.1914 0.025 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 Au1 0.01046(9) 0.01260(9) 0.01580(8) -0.00411(6) -0.00062(6) -0.00519(6) Sb1 0.01272(14) 0.02088(15) 0.01822(14) -0.00736(12) 0.00026(11) -0.00590(12) S1 0.0098(5) 0.0144(5) 0.0150(5) -0.0048(4) -0.0011(4) -0.0052(4) P1 0.0111(5) 0.0136(5) 0.0141(5) -0.0052(4) 0.0015(4) -0.0060(4) F1 0.055(2) 0.0423(18) 0.0335(15) -0.0037(13) -0.0116(14) -0.0372(16) O1 0.042(2) 0.0222(17) 0.0223(16) -0.0129(14) -0.0030(14) -0.0021(15) C1 0.017(2) 0.016(2) 0.0144(19) -0.0047(16) 0.0005(16) -0.0048(17) Au2 0.00924(9) 0.01609(9) 0.01369(8) -0.00683(6) 0.00007(6) -0.00541(7) P2 0.0102(5) 0.0172(5) 0.0131(5) -0.0077(4) 0.0013(4) -0.0062(4) F2 0.0274(17) 0.059(2) 0.0456(18) -0.0147(16) 0.0207(14) -0.0049(15) C2 0.021(2) 0.022(2) 0.0143(19) -0.0054(17) 0.0019(17) -0.0092(19) F3 0.071(3) 0.085(3) 0.0466(19) -0.0106(18) -0.0241(18) -0.054(2) C3 0.019(2) 0.025(2) 0.018(2) -0.0044(18) -0.0056(17) -0.0120(19) F4 0.045(2) 0.062(2) 0.053(2) -0.0340(18) 0.0299(16) -0.0155(17) C4 0.021(2) 0.019(2) 0.022(2) -0.0043(18) -0.0010(18) -0.0050(19) F5 0.0381(17) 0.0212(14) 0.0476(17) -0.0027(13) -0.0120(14) -0.0132(13) C5 0.016(2) 0.021(2) 0.016(2) -0.0103(17) 0.0058(16) -0.0076(18) F6 0.0424(19) 0.0330(17) 0.0410(17) 0.0119(14) -0.0084(14) -0.0086(15) C6 0.027(3) 0.037(3) 0.019(2) -0.013(2) -0.0008(19) -0.010(2) C7 0.020(2) 0.032(3) 0.026(2) -0.017(2) 0.0113(18) -0.016(2) C8 0.039(3) 0.022(2) 0.027(2) -0.014(2) 0.012(2) -0.012(2) C9 0.013(2) 0.019(2) 0.0130(18) -0.0077(16) 0.0016(15) -0.0078(17) C10 0.018(2) 0.022(2) 0.018(2) -0.0080(17) 0.0028(17) -0.0095(18) C11 0.026(2) 0.023(2) 0.015(2) -0.0056(17) 0.0007(17) -0.015(2) C12 0.025(2) 0.033(3) 0.0141(19) -0.0099(18) 0.0037(17) -0.020(2) C13 0.014(2) 0.029(2) 0.019(2) -0.0095(18) 0.0012(16) -0.0117(19) C14 0.016(2) 0.023(2) 0.0125(18) -0.0085(17) 0.0010(16) -0.0103(18) C15 0.0064(19) 0.017(2) 0.023(2) -0.0083(17) -0.0015(16) -0.0042(16) C16 0.010(2) 0.023(2) 0.026(2) -0.0099(18) -0.0001(17) -0.0094(18) C17 0.016(2) 0.024(2) 0.034(2) -0.002(2) -0.0082(19) -0.010(2) C18 0.011(2) 0.020(2) 0.055(3) -0.011(2) -0.007(2) -0.0048(19) C19 0.013(2) 0.031(3) 0.050(3) -0.025(2) 0.002(2) -0.008(2) C20 0.013(2) 0.033(3) 0.028(2) -0.018(2) 0.0014(18) -0.0115(19) C21 0.016(2) 0.023(2) 0.018(2) -0.0072(18) -0.0040(16) -0.0086(18) C22 0.018(2) 0.022(2) 0.017(2) -0.0060(17) -0.0020(16) -0.0111(19) C23 0.026(3) 0.030(3) 0.020(2) -0.0105(19) 0.0024(18) -0.017(2) C24 0.044(3) 0.040(3) 0.014(2) -0.004(2) -0.001(2) -0.029(3) C25 0.049(3) 0.021(2) 0.025(2) 0.001(2) -0.009(2) -0.015(2) C26 0.031(3) 0.022(2) 0.028(2) -0.006(2) -0.008(2) -0.003(2) C27 0.018(2) 0.019(2) 0.020(2) -0.0048(17) -0.0018(17) -0.0062(18) C28 0.019(2) 0.019(2) 0.0154(19) -0.0050(17) 0.0031(16) -0.0091(18) C29 0.020(2) 0.018(2) 0.027(2) -0.0047(18) -0.0025(18) -0.0067(19) C30 0.022(2) 0.027(2) 0.017(2) -0.0066(18) -0.0003(17) -0.012(2) C31 0.021(2) 0.030(3) 0.020(2) -0.0065(19) 0.0031(18) -0.016(2) C32 0.016(2) 0.018(2) 0.017(2) -0.0081(17) 0.0008(16) -0.0059(18) C33 0.022(2) 0.018(2) 0.018(2) -0.0050(17) -0.0005(17) -0.0053(19) C34 0.019(2) 0.018(2) 0.031(2) -0.0149(19) -0.0018(18) -0.0022(18) C35 0.012(2) 0.024(2) 0.023(2) -0.0077(18) -0.0005(17) -0.0055(18) C36 0.015(2) 0.017(2) 0.0143(19) -0.0053(16) -0.0011(16) -0.0063(17) C37 0.014(2) 0.025(2) 0.017(2) -0.0100(17) 0.0017(16) -0.0079(18) C38 0.017(2) 0.024(2) 0.021(2) -0.0075(18) -0.0037(17) -0.0108(19) C39 0.029(3) 0.024(2) 0.015(2) -0.0048(18) -0.0054(18) -0.012(2) C40 0.019(2) 0.023(2) 0.017(2) -0.0082(17) 0.0022(17) -0.0082(19) C41 0.013(2) 0.014(2) 0.0141(19) -0.0036(16) -0.0017(15) -0.0054(17) C42 0.016(2) 0.020(2) 0.0137(19) -0.0107(16) 0.0060(16) -0.0095(17) C43 0.024(2) 0.025(2) 0.018(2) -0.0096(18) 0.0057(18) -0.011(2) C44 0.040(3) 0.039(3) 0.026(2) -0.019(2) 0.016(2) -0.031(3) C45 0.024(3) 0.061(4) 0.032(3) -0.032(3) 0.015(2) -0.027(3) C46 0.018(2) 0.046(3) 0.030(2) -0.024(2) 0.0039(19) -0.008(2) C47 0.017(2) 0.030(3) 0.020(2) -0.0124(19) 0.0017(17) -0.0093(19) _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 Au1 S1 2.3233(10) . ? Au1 P1 2.2740(10) . ? Sb1 F1 1.865(3) . ? Sb1 F2 1.865(3) . ? Sb1 F3 1.857(3) . ? Sb1 F4 1.850(3) . ? Sb1 F5 1.881(3) . ? Sb1 F6 1.858(3) . ? S1 Au2 2.3262(10) . ? S1 C21 1.846(4) . ? P1 C1 1.885(4) . ? P1 C5 1.874(4) . ? P1 C9 1.832(4) . ? O1 C21 1.200(5) . ? C1 C2 1.528(6) . ? C1 C3 1.551(6) . ? C1 C4 1.534(6) . ? Au2 P2 2.2739(10) . ? P2 C28 1.884(4) . ? P2 C32 1.873(4) . ? P2 C36 1.838(4) . ? C5 C6 1.535(6) . ? C5 C7 1.524(6) . ? C5 C8 1.534(6) . ? C9 C10 1.402(6) . ? C9 C14 1.410(6) . ? C10 C11 1.386(6) . ? C11 C12 1.392(6) . ? C12 C13 1.382(6) . ? C13 C14 1.398(6) . ? C14 C15 1.505(6) . ? C15 C16 1.394(6) . ? C15 C20 1.399(6) . ? C16 C17 1.393(6) . ? C17 C18 1.393(7) . ? C18 C19 1.380(7) . ? C19 C20 1.394(6) . ? C21 C22 1.486(6) . ? C22 C23 1.406(6) . ? C22 C27 1.384(6) . ? C23 C24 1.379(7) . ? C24 C25 1.390(7) . ? C25 C26 1.377(7) . ? C26 C27 1.388(6) . ? C28 C29 1.538(6) . ? C28 C30 1.531(6) . ? C28 C31 1.537(6) . ? C32 C33 1.542(5) . ? C32 C34 1.537(6) . ? C32 C35 1.528(6) . ? C36 C37 1.397(6) . ? C36 C41 1.411(5) . ? C37 C38 1.377(6) . ? C38 C39 1.377(6) . ? C39 C40 1.378(6) . ? C40 C41 1.399(6) . ? C41 C42 1.495(5) . ? C42 C43 1.383(6) . ? C42 C47 1.392(6) . ? C43 C44 1.395(6) . ? C44 C45 1.390(7) . ? C45 C46 1.368(7) . ? C46 C47 1.385(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 P1 Au1 S1 179.50(4) . . ? F1 Sb1 F2 89.67(15) . . ? F1 Sb1 F5 88.61(12) . . ? F2 Sb1 F5 88.31(14) . . ? F3 Sb1 F1 178.83(14) . . ? F3 Sb1 F2 90.01(17) . . ? F3 Sb1 F5 90.25(14) . . ? F3 Sb1 F6 90.71(15) . . ? F4 Sb1 F1 89.35(15) . . ? F4 Sb1 F2 178.01(15) . . ? F4 Sb1 F3 90.93(17) . . ? F4 Sb1 F5 89.94(14) . . ? F4 Sb1 F6 90.52(15) . . ? F6 Sb1 F1 90.42(14) . . ? F6 Sb1 F2 91.22(14) . . ? F6 Sb1 F5 178.93(14) . . ? Au1 S1 Au2 93.94(3) . . ? C21 S1 Au1 101.70(14) . . ? C21 S1 Au2 96.46(13) . . ? C1 P1 Au1 107.36(13) . . ? C5 P1 Au1 107.64(13) . . ? C5 P1 C1 116.58(19) . . ? C9 P1 Au1 113.48(14) . . ? C9 P1 C1 104.82(18) . . ? C9 P1 C5 107.16(18) . . ? C2 C1 P1 104.8(3) . . ? C2 C1 C3 108.1(3) . . ? C2 C1 C4 110.4(3) . . ? C3 C1 P1 109.1(3) . . ? C4 C1 P1 116.4(3) . . ? C4 C1 C3 107.8(3) . . ? P2 Au2 S1 173.61(3) . . ? C28 P2 Au2 105.42(14) . . ? C32 P2 Au2 109.88(13) . . ? C32 P2 C28 114.00(18) . . ? C36 P2 Au2 114.17(13) . . ? C36 P2 C28 105.86(18) . . ? C36 P2 C32 107.62(18) . . ? C6 C5 P1 105.7(3) . . ? C7 C5 P1 107.7(3) . . ? C7 C5 C6 109.0(3) . . ? C7 C5 C8 109.2(4) . . ? C8 C5 P1 116.6(3) . . ? C8 C5 C6 108.4(4) . . ? C10 C9 P1 119.1(3) . . ? C10 C9 C14 118.2(4) . . ? C14 C9 P1 122.4(3) . . ? C11 C10 C9 121.9(4) . . ? C10 C11 C12 119.6(4) . . ? C13 C12 C11 119.2(4) . . ? C12 C13 C14 122.0(4) . . ? C9 C14 C15 126.1(4) . . ? C13 C14 C9 119.0(4) . . ? C13 C14 C15 114.9(4) . . ? C16 C15 C14 120.1(4) . . ? C16 C15 C20 119.1(4) . . ? C20 C15 C14 120.3(4) . . ? C17 C16 C15 120.1(4) . . ? C18 C17 C16 120.5(4) . . ? C19 C18 C17 119.7(4) . . ? C18 C19 C20 120.2(4) . . ? C19 C20 C15 120.4(4) . . ? O1 C21 S1 121.9(3) . . ? O1 C21 C22 124.3(4) . . ? C22 C21 S1 113.8(3) . . ? C23 C22 C21 118.2(4) . . ? C27 C22 C21 122.4(4) . . ? C27 C22 C23 119.5(4) . . ? C24 C23 C22 119.8(4) . . ? C23 C24 C25 120.1(4) . . ? C26 C25 C24 120.2(4) . . ? C25 C26 C27 120.2(5) . . ? C22 C27 C26 120.2(4) . . ? C29 C28 P2 105.6(3) . . ? C30 C28 P2 108.3(3) . . ? C30 C28 C29 108.4(3) . . ? C30 C28 C31 109.7(3) . . ? C31 C28 P2 116.5(3) . . ? C31 C28 C29 108.0(4) . . ? C33 C32 P2 106.8(3) . . ? C34 C32 P2 108.6(3) . . ? C34 C32 C33 107.5(3) . . ? C35 C32 P2 115.3(3) . . ? C35 C32 C33 109.7(3) . . ? C35 C32 C34 108.7(3) . . ? C37 C36 P2 119.0(3) . . ? C37 C36 C41 118.3(4) . . ? C41 C36 P2 122.6(3) . . ? C38 C37 C36 122.5(4) . . ? C37 C38 C39 118.8(4) . . ? C38 C39 C40 120.3(4) . . ? C39 C40 C41 121.7(4) . . ? C36 C41 C42 125.7(3) . . ? C40 C41 C36 118.3(4) . . ? C40 C41 C42 116.0(3) . . ? C43 C42 C41 120.7(4) . . ? C43 C42 C47 118.5(4) . . ? C47 C42 C41 120.6(4) . . ? C42 C43 C44 120.8(4) . . ? C45 C44 C43 119.7(4) . . ? C46 C45 C44 119.7(4) . . ? C45 C46 C47 120.5(5) . . ? C46 C47 C42 120.7(4) . . ? _database_code_depnum_ccdc_archive 'CCDC 914704' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global data_4457 #TrackingRef '19836_web_deposit_cif_file_0_GeorginaRosair_1366889069.914705.cif' _audit_creation_date 2013-04-24 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C44 H63 Au2 P2 S, F6 Sb, C0.5 H0.5 Cl1.5' _chemical_formula_sum 'C44.50 H63.50 Au2 Cl1.50 F6 P2 S Sb' _chemical_formula_weight 1375.31 _chemical_melting_point ? 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.0540(8) _cell_length_b 30.084(2) _cell_length_c 13.5903(8) _cell_angle_alpha 90.00 _cell_angle_beta 96.316(3) _cell_angle_gamma 90.00 _cell_volume 4898.4(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9935 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 32.748 _cell_measurement_theta_min 2.487 _exptl_absorpt_coefficient_mu 6.765 _exptl_absorpt_correction_T_max 0.7465 _exptl_absorpt_correction_T_min 0.6012 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. R(int) was 0.0930 before and 0.0533 after correction. The Ratio of minimum to maximum transmission is 0.8054. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.865 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description BLOCK _exptl_crystal_F_000 2660 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_unetI/netI 0.0360 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 136621 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 33.32 _diffrn_reflns_theta_min 1.35 _diffrn_ambient_temperature 100.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _reflns_number_gt 15296 _reflns_number_total 18696 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'SAINT v7.68A (Bruker, 2009)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 4.071 _refine_diff_density_min -4.718 _refine_diff_density_rms 0.184 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 645 _refine_ls_number_reflns 18696 _refine_ls_number_restraints 130 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0328 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+17.2895P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0713 _refine_ls_wR_factor_ref 0.0765 _refine_special_details ; The highest residual peak of 4.07 e\%A^-3^ is 0.54 \%A from SB1. All SB-F distances restrained using the SADI (same distance) restraint SADI 0.02 and equivalent F-F distances restrained to be the same using SADI 0.04. The two F6 components had relative occupancies of 0.555(15) and 0.445(15). Solvent C-Cl restrained with SADI Cl1 C1S C1S Cl2 C1S Cl2_$1 . The CHCl3 is disordered over a centre of inversion. One Cl position is split into two components Cl2 and Cl2a whose combined occupancy is 0.75. t-butyl C-C distances were restrained with SADI C4A C3A C3A C2A C2B C1 C2A C1 C4B C3B. 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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Au1 Au 0.654937(10) 0.085889(4) 0.404904(9) 0.01220(3) Uani 1 1 d . . . Au2 Au 0.664210(11) 0.159019(5) 0.599869(9) 0.01554(3) Uani 1 1 d . . . S1 S 0.68896(9) 0.08316(3) 0.57614(6) 0.02021(18) Uani 1 1 d . A . P1 P 0.64160(8) 0.08663(3) 0.23619(6) 0.01329(15) Uani 1 1 d . . . P2 P 0.65923(8) 0.23450(3) 0.61817(7) 0.01796(18) Uani 1 1 d . . . C1 C 0.8435(4) 0.07857(15) 0.5976(4) 0.0382(13) Uani 1 1 d D . . H1AA H 0.8763 0.1013 0.5567 0.046 Uiso 0.514(8) 1 calc PR A 1 H1AB H 0.8674 0.0858 0.6679 0.046 Uiso 0.514(8) 1 calc PR A 1 C2A C 0.8940(6) 0.0315(2) 0.5737(5) 0.0191(15) Uani 0.514(8) 1 d PD A 1 H2AA H 0.8534 0.0191 0.5126 0.029 Uiso 0.514(8) 1 calc PR A 1 H2AB H 0.9737 0.0346 0.5636 0.029 Uiso 0.514(8) 1 calc PR A 1 C3A C 0.8818(7) 0.0005(2) 0.6613(5) 0.0227(17) Uani 0.514(8) 1 d PD A 1 H3AA H 0.8045 0.0025 0.6791 0.027 Uiso 0.514(8) 1 calc PR A 1 H3AB H 0.9327 0.0106 0.7191 0.027 Uiso 0.514(8) 1 calc PR A 1 C4A C 0.9081(7) -0.0485(3) 0.6391(7) 0.0272(19) Uani 0.514(8) 1 d PD A 1 H4AA H 0.8561 -0.0591 0.5837 0.041 Uiso 0.514(8) 1 calc PR A 1 H4AB H 0.9004 -0.0667 0.6978 0.041 Uiso 0.514(8) 1 calc PR A 1 H4AC H 0.9847 -0.0507 0.6218 0.041 Uiso 0.514(8) 1 calc PR A 1 C5 C 0.7113(4) 0.13912(13) 0.1998(3) 0.0225(8) Uani 1 1 d . . . C6 C 0.7344(9) 0.1428(2) 0.0920(4) 0.086(3) Uani 1 1 d . . . H6A H 0.7841 0.1186 0.0765 0.129 Uiso 1 1 calc R . . H6B H 0.7701 0.1714 0.0815 0.129 Uiso 1 1 calc R . . H6C H 0.6640 0.1407 0.0488 0.129 Uiso 1 1 calc R . . C7 C 0.8225(4) 0.14500(15) 0.2656(4) 0.0318(10) Uani 1 1 d . . . H7A H 0.8101 0.1414 0.3353 0.048 Uiso 1 1 calc R . . H7B H 0.8523 0.1748 0.2556 0.048 Uiso 1 1 calc R . . H7C H 0.8760 0.1226 0.2481 0.048 Uiso 1 1 calc R . . C8 C 0.6341(4) 0.17683(15) 0.2247(5) 0.0490(16) Uani 1 1 d . . . H8A H 0.5614 0.1735 0.1855 0.073 Uiso 1 1 calc R . . H8B H 0.6671 0.2054 0.2094 0.073 Uiso 1 1 calc R . . H8C H 0.6244 0.1757 0.2954 0.073 Uiso 1 1 calc R . . C9 C 0.7053(3) 0.03371(12) 0.1950(3) 0.0172(6) Uani 1 1 d . . . C10 C 0.8274(4) 0.03087(15) 0.2414(3) 0.0256(8) Uani 1 1 d . . . H10A H 0.8723 0.0529 0.2102 0.038 Uiso 1 1 calc R . . H10B H 0.8565 0.0010 0.2311 0.038 Uiso 1 1 calc R . . H10C H 0.8313 0.0369 0.3126 0.038 Uiso 1 1 calc R . . C11 C 0.7006(4) 0.02641(14) 0.0837(3) 0.0255(8) Uani 1 1 d . . . H11A H 0.6225 0.0251 0.0548 0.038 Uiso 1 1 calc R . . H11B H 0.7379 -0.0016 0.0709 0.038 Uiso 1 1 calc R . . H11C H 0.7382 0.0510 0.0539 0.038 Uiso 1 1 calc R . . C12 C 0.6393(4) -0.00392(14) 0.2388(4) 0.0349(11) Uani 1 1 d . . . H12A H 0.6476 -0.0015 0.3111 0.052 Uiso 1 1 calc R . . H12B H 0.6681 -0.0327 0.2195 0.052 Uiso 1 1 calc R . . H12C H 0.5602 -0.0014 0.2136 0.052 Uiso 1 1 calc R . . C13 C 0.4996(3) 0.08632(11) 0.1726(2) 0.0155(6) Uani 1 1 d . . . C14 C 0.4843(4) 0.08937(13) 0.0685(3) 0.0226(8) Uani 1 1 d . . . H14 H 0.5479 0.0927 0.0336 0.027 Uiso 1 1 calc R . . C15 C 0.3796(4) 0.08762(14) 0.0154(3) 0.0290(9) Uani 1 1 d . . . H15 H 0.3717 0.0901 -0.0547 0.035 Uiso 1 1 calc R . . C16 C 0.2863(4) 0.08220(14) 0.0655(3) 0.0302(10) Uani 1 1 d . . . H16 H 0.2140 0.0807 0.0299 0.036 Uiso 1 1 calc R . . C17 C 0.2993(3) 0.07898(13) 0.1680(3) 0.0241(8) Uani 1 1 d . . . H17 H 0.2351 0.0750 0.2018 0.029 Uiso 1 1 calc R . . C18 C 0.4041(3) 0.08145(11) 0.2229(3) 0.0162(6) Uani 1 1 d . . . C19 C 0.4047(3) 0.08057(12) 0.3327(3) 0.0149(6) Uani 1 1 d . . . C20 C 0.4078(3) 0.04039(12) 0.3847(3) 0.0199(7) Uani 1 1 d . . . H20 H 0.4166 0.0132 0.3511 0.024 Uiso 1 1 calc R . . C21 C 0.3979(4) 0.04031(14) 0.4853(3) 0.0303(10) Uani 1 1 d . . . H21 H 0.4007 0.0129 0.5203 0.036 Uiso 1 1 calc R . . C22 C 0.3841(4) 0.07978(14) 0.5359(3) 0.0280(9) Uani 1 1 d . . . H22 H 0.3776 0.0793 0.6049 0.034 Uiso 1 1 calc R . . C23 C 0.3797(3) 0.11963(13) 0.4850(3) 0.0217(7) Uani 1 1 d . . . H23 H 0.3692 0.1467 0.5188 0.026 Uiso 1 1 calc R . . C24 C 0.3906(3) 0.12013(13) 0.3842(3) 0.0199(7) Uani 1 1 d . . . H24 H 0.3885 0.1477 0.3498 0.024 Uiso 1 1 calc R . . C25 C 0.7939(3) 0.25490(13) 0.5775(3) 0.0202(7) Uani 1 1 d . . . C26 C 0.7971(4) 0.24159(15) 0.4685(3) 0.0275(9) Uani 1 1 d . . . H26A H 0.7738 0.2105 0.4593 0.041 Uiso 1 1 calc R . . H26B H 0.8733 0.2450 0.4507 0.041 Uiso 1 1 calc R . . H26C H 0.7464 0.2607 0.4260 0.041 Uiso 1 1 calc R . . C27 C 0.8862(3) 0.22978(15) 0.6418(3) 0.0267(8) Uani 1 1 d . . . H27A H 0.8824 0.2370 0.7116 0.040 Uiso 1 1 calc R . . H27B H 0.9592 0.2386 0.6229 0.040 Uiso 1 1 calc R . . H27C H 0.8760 0.1977 0.6318 0.040 Uiso 1 1 calc R . . C28 C 0.8171(4) 0.30466(14) 0.5885(4) 0.0316(10) Uani 1 1 d . . . H28A H 0.7536 0.3214 0.5560 0.047 Uiso 1 1 calc R . . H28B H 0.8845 0.3121 0.5577 0.047 Uiso 1 1 calc R . . H28C H 0.8281 0.3124 0.6590 0.047 Uiso 1 1 calc R . . C29 C 0.5278(3) 0.25659(15) 0.5475(3) 0.0271(9) Uani 1 1 d . . . C30 C 0.5106(4) 0.23448(16) 0.4449(3) 0.0312(10) Uani 1 1 d . . . H30A H 0.5638 0.2469 0.4028 0.047 Uiso 1 1 calc R . . H30B H 0.4343 0.2401 0.4146 0.047 Uiso 1 1 calc R . . H30C H 0.5226 0.2024 0.4520 0.047 Uiso 1 1 calc R . . C31 C 0.5201(4) 0.30688(16) 0.5333(4) 0.0415(13) Uani 1 1 d . . . H31A H 0.5224 0.3214 0.5980 0.062 Uiso 1 1 calc R . . H31B H 0.4499 0.3143 0.4933 0.062 Uiso 1 1 calc R . . H31C H 0.5830 0.3172 0.4994 0.062 Uiso 1 1 calc R . . C32 C 0.4330(4) 0.24068(18) 0.6070(4) 0.0388(12) Uani 1 1 d . . . H32A H 0.4417 0.2088 0.6208 0.058 Uiso 1 1 calc R . . H32B H 0.3607 0.2460 0.5684 0.058 Uiso 1 1 calc R . . H32C H 0.4366 0.2571 0.6696 0.058 Uiso 1 1 calc R . . C33 C 0.6547(3) 0.25456(17) 0.7455(3) 0.0285(9) Uani 1 1 d . . . C34 C 0.6520(4) 0.30079(19) 0.7623(4) 0.0393(12) Uani 1 1 d . . . H34 H 0.6594 0.3206 0.7090 0.047 Uiso 1 1 calc R . . C35 C 0.6385(4) 0.3180(2) 0.8553(5) 0.057(2) Uani 1 1 d . . . H35 H 0.6371 0.3493 0.8651 0.068 Uiso 1 1 calc R . . C36 C 0.6271(5) 0.2895(3) 0.9336(5) 0.065(2) Uani 1 1 d . . . H36 H 0.6166 0.3010 0.9970 0.077 Uiso 1 1 calc R . . C37 C 0.6310(4) 0.2438(3) 0.9185(4) 0.0522(18) Uani 1 1 d . . . H37 H 0.6239 0.2245 0.9727 0.063 Uiso 1 1 calc R . . C38 C 0.6452(3) 0.22541(19) 0.8257(3) 0.0338(11) Uani 1 1 d . . . C39 C 0.6504(4) 0.1760(2) 0.8211(3) 0.0367(12) Uani 1 1 d . . . C40 C 0.7530(5) 0.15479(18) 0.8315(3) 0.0364(12) Uani 1 1 d . . . H40 H 0.8193 0.1721 0.8353 0.044 Uiso 1 1 calc R . . C41 C 0.7612(6) 0.1082(2) 0.8364(3) 0.0504(16) Uani 1 1 d . . . H41 H 0.8322 0.0941 0.8439 0.060 Uiso 1 1 calc R . . C42 C 0.6650(8) 0.0832(2) 0.8303(4) 0.067(2) Uani 1 1 d . . . H42 H 0.6697 0.0517 0.8342 0.080 Uiso 1 1 calc R . . C43 C 0.5616(8) 0.1036(3) 0.8185(4) 0.080(3) Uani 1 1 d . . . H43 H 0.4958 0.0860 0.8124 0.096 Uiso 1 1 calc R . . C44 C 0.5529(5) 0.1501(3) 0.8153(3) 0.057(2) Uani 1 1 d . . . H44 H 0.4817 0.1640 0.8093 0.068 Uiso 1 1 calc R . . Sb1 Sb 0.15147(2) 0.141109(11) 0.74834(3) 0.03293(7) Uani 1 1 d D . . F1A F 0.2965(4) 0.1250(3) 0.7356(6) 0.0396(19) Uani 0.555(15) 1 d PD B 1 F6A F 0.2028(13) 0.1584(6) 0.8787(9) 0.063(4) Uani 0.555(15) 1 d PD B 1 F3A F 0.0067(8) 0.1507(5) 0.7799(11) 0.043(3) Uani 0.555(15) 1 d PD B 1 F5A F 0.0957(13) 0.1206(7) 0.6264(9) 0.114(7) Uani 0.555(15) 1 d PD B 1 F2A F 0.1625(13) 0.1985(4) 0.7082(12) 0.094(5) Uani 0.555(15) 1 d PD B 1 F4A F 0.1334(7) 0.0817(2) 0.8060(9) 0.069(3) Uani 0.555(15) 1 d PD B 1 F1B F 0.2924(7) 0.1488(6) 0.6894(9) 0.068(5) Uani 0.445(15) 1 d PD B 2 F4B F 0.1685(12) 0.0824(3) 0.7412(14) 0.094(6) Uani 0.445(15) 1 d PD B 2 F5B F 0.0861(16) 0.1399(5) 0.6136(9) 0.052(3) Uani 0.445(15) 1 d PD B 2 F6B F 0.2247(17) 0.1480(7) 0.8713(10) 0.068(5) Uani 0.445(15) 1 d PD B 2 F2B F 0.1457(14) 0.2033(3) 0.7347(11) 0.060(5) Uani 0.445(15) 1 d PD B 2 F3B F 0.0112(11) 0.1406(7) 0.7897(15) 0.066(6) Uani 0.445(15) 1 d PD B 2 Cl1 Cl -0.01535(18) 0.08157(8) 1.02322(18) 0.0568(5) Uani 0.75 1 d PD C 1 Cl2 Cl -0.0650(5) 0.00657(11) 0.9315(6) 0.0321(12) Uani 0.400(11) 1 d PD . 1 C1S C 0.0234(7) 0.0315(2) 0.9752(6) 0.033(2) Uani 0.50 1 d PD . . H1S H 0.0822 0.0356 0.9295 0.040 Uiso 0.50 1 calc PR C 1 Cl2A Cl -0.0943(3) 0.00975(13) 0.8911(4) 0.0133(11) Uani 0.350(11) 1 d P C -2 C2B C 0.8634(7) 0.0299(2) 0.6293(6) 0.0198(17) Uani 0.486(8) 1 d PD A 2 H2BA H 0.9379 0.0268 0.6673 0.030 Uiso 0.486(8) 1 calc PR A 2 H2BB H 0.8064 0.0205 0.6721 0.030 Uiso 0.486(8) 1 calc PR A 2 C3B C 0.8563(6) 0.0011(2) 0.5372(6) 0.0176(15) Uani 0.486(8) 1 d PD A 2 H3BA H 0.9098 0.0122 0.4927 0.021 Uiso 0.486(8) 1 calc PR A 2 H3BB H 0.7803 0.0033 0.5016 0.021 Uiso 0.486(8) 1 calc PR A 2 C4B C 0.8822(7) -0.0477(3) 0.5620(8) 0.027(2) Uani 0.486(8) 1 d PD A 2 H4BA H 0.9555 -0.0498 0.6009 0.041 Uiso 0.486(8) 1 calc PR A 2 H4BB H 0.8829 -0.0646 0.5005 0.041 Uiso 0.486(8) 1 calc PR A 2 H4BC H 0.8250 -0.0597 0.6004 0.041 Uiso 0.486(8) 1 calc PR A 2 H1BC H 0.868(9) 0.093(4) 0.542(9) 0.033 Uiso 0.486(8) 1 d P A 2 H1BD H 0.852(9) 0.101(4) 0.666(8) 0.033 Uiso 0.486(8) 1 d P A 2 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 Au1 0.01190(5) 0.01503(6) 0.00956(5) 0.00096(4) 0.00076(4) -0.00044(4) Au2 0.01798(6) 0.01762(6) 0.01104(5) -0.00152(4) 0.00164(4) -0.00330(5) S1 0.0322(5) 0.0162(4) 0.0110(3) 0.0018(3) -0.0032(3) -0.0084(4) P1 0.0173(4) 0.0123(4) 0.0108(3) 0.0006(3) 0.0035(3) 0.0004(3) P2 0.0163(4) 0.0194(4) 0.0176(4) -0.0074(3) -0.0005(3) 0.0023(3) C1 0.036(2) 0.019(2) 0.051(3) -0.0003(19) -0.033(2) 0.0002(18) C2A 0.015(3) 0.026(4) 0.016(3) 0.001(3) 0.000(2) 0.005(3) C3A 0.022(3) 0.027(4) 0.020(3) 0.005(3) 0.003(3) 0.004(3) C4A 0.023(4) 0.024(4) 0.035(5) 0.007(3) 0.006(3) 0.005(3) C5 0.038(2) 0.0140(16) 0.0160(16) 0.0015(12) 0.0037(15) -0.0063(15) C6 0.185(9) 0.059(4) 0.019(2) -0.009(2) 0.028(4) -0.086(5) C7 0.0217(19) 0.025(2) 0.049(3) 0.0066(19) 0.0086(19) -0.0077(16) C8 0.033(3) 0.0100(18) 0.098(5) -0.007(2) -0.019(3) 0.0011(17) C9 0.0198(16) 0.0153(16) 0.0178(15) -0.0013(12) 0.0079(13) 0.0003(13) C10 0.026(2) 0.028(2) 0.0227(18) -0.0029(15) 0.0015(15) 0.0087(16) C11 0.029(2) 0.025(2) 0.0230(18) -0.0094(15) 0.0028(15) 0.0039(16) C12 0.042(3) 0.0133(17) 0.054(3) 0.0011(18) 0.030(2) 0.0021(17) C13 0.0222(16) 0.0119(14) 0.0116(13) -0.0017(11) -0.0019(12) 0.0021(13) C14 0.032(2) 0.0197(18) 0.0149(15) -0.0024(13) -0.0028(14) 0.0055(15) C15 0.044(3) 0.0229(19) 0.0170(17) -0.0064(14) -0.0099(16) 0.0125(18) C16 0.033(2) 0.024(2) 0.028(2) -0.0076(16) -0.0198(17) 0.0070(17) C17 0.0217(18) 0.0208(18) 0.0277(19) -0.0023(15) -0.0062(15) -0.0004(14) C18 0.0191(16) 0.0107(14) 0.0178(15) 0.0004(12) -0.0025(12) 0.0007(12) C19 0.0115(14) 0.0155(15) 0.0178(15) -0.0016(12) 0.0017(11) -0.0024(12) C20 0.0227(18) 0.0140(15) 0.0249(18) 0.0006(13) 0.0116(14) -0.0010(13) C21 0.048(3) 0.0206(19) 0.026(2) 0.0043(15) 0.0221(19) -0.0015(18) C22 0.038(2) 0.026(2) 0.0238(19) 0.0000(15) 0.0183(17) -0.0029(17) C23 0.0230(18) 0.0207(18) 0.0225(17) -0.0077(14) 0.0075(14) -0.0036(14) C24 0.0224(18) 0.0158(16) 0.0212(17) -0.0009(13) 0.0012(14) 0.0001(13) C25 0.0201(17) 0.0166(16) 0.0231(17) 0.0003(13) -0.0018(14) 0.0007(13) C26 0.029(2) 0.029(2) 0.0256(19) -0.0020(16) 0.0071(16) -0.0083(17) C27 0.0172(17) 0.026(2) 0.037(2) 0.0047(17) 0.0004(16) 0.0017(15) C28 0.035(2) 0.0157(18) 0.041(3) -0.0016(17) -0.0093(19) -0.0033(16) C29 0.0211(18) 0.026(2) 0.031(2) -0.0136(16) -0.0073(15) 0.0091(16) C30 0.028(2) 0.032(2) 0.031(2) -0.0110(18) -0.0106(17) 0.0096(18) C31 0.032(2) 0.028(2) 0.060(3) -0.017(2) -0.017(2) 0.015(2) C32 0.0178(19) 0.049(3) 0.048(3) -0.028(2) -0.0039(18) 0.0049(19) C33 0.0161(17) 0.044(3) 0.0257(19) -0.0196(18) 0.0012(14) -0.0014(17) C34 0.026(2) 0.046(3) 0.045(3) -0.030(2) -0.002(2) 0.006(2) C35 0.023(2) 0.080(5) 0.065(4) -0.056(4) -0.005(2) 0.006(3) C36 0.029(3) 0.126(7) 0.039(3) -0.057(4) 0.004(2) -0.003(3) C37 0.027(2) 0.107(5) 0.023(2) -0.029(3) 0.0082(18) -0.011(3) C38 0.0157(17) 0.066(3) 0.0202(18) -0.018(2) 0.0040(14) -0.0100(19) C39 0.032(2) 0.069(4) 0.0093(15) -0.0055(18) 0.0032(15) -0.026(2) C40 0.047(3) 0.047(3) 0.0136(17) 0.0046(17) -0.0045(17) -0.024(2) C41 0.089(5) 0.048(3) 0.0128(18) 0.0060(19) -0.004(2) -0.028(3) C42 0.115(7) 0.072(4) 0.014(2) 0.006(2) 0.003(3) -0.061(5) C43 0.110(6) 0.115(6) 0.017(2) -0.008(3) 0.017(3) -0.097(6) C44 0.049(3) 0.107(5) 0.017(2) -0.016(3) 0.014(2) -0.051(3) Sb1 0.01959(13) 0.03360(16) 0.04340(17) -0.01772(13) -0.00640(12) 0.00769(11) F1A 0.023(3) 0.050(4) 0.048(4) -0.010(3) 0.012(2) 0.004(2) F6A 0.052(6) 0.078(8) 0.052(5) -0.030(5) -0.023(4) 0.018(6) F3A 0.024(4) 0.064(6) 0.042(5) 0.018(4) 0.012(3) 0.016(4) F5A 0.055(7) 0.22(2) 0.065(7) -0.096(10) 0.010(6) -0.049(11) F2A 0.063(6) 0.111(10) 0.111(10) 0.078(8) 0.018(7) -0.001(6) F4A 0.074(5) 0.021(3) 0.123(8) 0.007(4) 0.059(5) 0.006(3) F1B 0.033(4) 0.116(12) 0.058(7) -0.044(7) 0.015(4) -0.013(5) F4B 0.100(10) 0.029(5) 0.150(15) 0.003(6) -0.002(10) 0.026(5) F5B 0.050(6) 0.068(7) 0.038(5) -0.023(4) 0.003(4) -0.021(5) F6B 0.061(9) 0.088(11) 0.045(7) 0.012(7) -0.034(6) 0.030(7) F2B 0.083(10) 0.016(4) 0.074(8) -0.004(4) -0.025(7) -0.021(4) F3B 0.043(7) 0.105(14) 0.048(7) 0.015(8) -0.001(6) -0.035(8) Cl1 0.0441(10) 0.0571(12) 0.0700(14) -0.0200(10) 0.0098(10) -0.0031(9) Cl2 0.037(2) 0.0327(15) 0.028(3) 0.0196(13) 0.010(2) 0.0217(13) C1S 0.043(5) 0.026(4) 0.035(4) 0.016(4) 0.030(4) 0.023(4) Cl2A 0.0142(12) 0.0112(13) 0.0129(19) -0.0031(11) -0.0058(12) 0.0011(8) C2B 0.023(4) 0.019(4) 0.016(3) 0.001(3) -0.002(3) 0.003(3) C3B 0.014(3) 0.018(3) 0.020(3) 0.001(3) 0.002(3) 0.001(3) C4B 0.018(4) 0.022(4) 0.042(5) 0.001(4) 0.005(3) 0.004(3) _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 Au1 S1 2.3196(9) . ? Au1 P1 2.2810(9) . ? Au2 S1 2.3285(10) . ? Au2 P2 2.2858(10) . ? S1 C1 1.859(5) . ? P1 C5 1.880(4) . ? P1 C9 1.880(4) . ? P1 C13 1.830(4) . ? P2 C25 1.874(4) . ? P2 C29 1.882(4) . ? P2 C33 1.839(4) . ? C1 H1AA 0.9900 . ? C1 H1AB 0.9900 . ? C1 C2A 1.590(8) . ? C1 C2B 1.537(8) . ? C1 H1BC 0.95(12) . ? C1 H1BD 1.14(11) . ? C2A H2AA 0.9900 . ? C2A H2AB 0.9900 . ? C2A C3A 1.531(9) . ? C3A H3AA 0.9900 . ? C3A H3AB 0.9900 . ? C3A C4A 1.544(10) . ? C4A H4AA 0.9800 . ? C4A H4AB 0.9800 . ? C4A H4AC 0.9800 . ? C5 C6 1.524(6) . ? C5 C7 1.538(6) . ? C5 C8 1.528(7) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.539(6) . ? C9 C11 1.523(5) . ? C9 C12 1.540(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.410(5) . ? C13 C18 1.410(5) . ? C14 H14 0.9500 . ? C14 C15 1.384(6) . ? C15 H15 0.9500 . ? C15 C16 1.386(7) . ? C16 H16 0.9500 . ? C16 C17 1.389(6) . ? C17 H17 0.9500 . ? C17 C18 1.396(5) . ? C18 C19 1.492(5) . ? C19 C20 1.399(5) . ? C19 C24 1.400(5) . ? C20 H20 0.9500 . ? C20 C21 1.385(5) . ? C21 H21 0.9500 . ? C21 C22 1.391(6) . ? C22 H22 0.9500 . ? C22 C23 1.382(6) . ? C23 H23 0.9500 . ? C23 C24 1.390(5) . ? C24 H24 0.9500 . ? C25 C26 1.540(6) . ? C25 C27 1.536(6) . ? C25 C28 1.527(6) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.538(6) . ? C29 C31 1.527(7) . ? C29 C32 1.547(7) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.410(7) . ? C33 C38 1.413(7) . ? C34 H34 0.9500 . ? C34 C35 1.392(7) . ? C35 H35 0.9500 . ? C35 C36 1.385(11) . ? C36 H36 0.9500 . ? C36 C37 1.390(11) . ? C37 H37 0.9500 . ? C37 C38 1.406(6) . ? C38 C39 1.488(8) . ? C39 C40 1.386(8) . ? C39 C44 1.406(7) . ? C40 H40 0.9500 . ? C40 C41 1.407(8) . ? C41 H41 0.9500 . ? C41 C42 1.377(9) . ? C42 H42 0.9500 . ? C42 C43 1.384(12) . ? C43 H43 0.9500 . ? C43 C44 1.404(11) . ? C44 H44 0.9500 . ? Sb1 F1A 1.840(5) . ? Sb1 F6A 1.885(9) . ? Sb1 F3A 1.865(8) . ? Sb1 F5A 1.826(9) . ? Sb1 F2A 1.819(10) . ? Sb1 F4A 1.973(6) . ? Sb1 F1B 1.970(8) . ? Sb1 F4B 1.781(8) . ? Sb1 F5B 1.913(11) . ? Sb1 F6B 1.814(11) . ? Sb1 F2B 1.881(9) . ? Sb1 F3B 1.840(11) . ? Cl1 C1S 1.726(7) . ? Cl2 Cl2 2.333(17) 3_557 ? Cl2 C1S 1.742(9) 3_557 ? Cl2 C1S 1.383(11) . ? C1S Cl2 1.742(9) 3_557 ? C1S H1S 1.0000 . ? C1S Cl2A 1.841(10) . ? C2B H2BA 0.9900 . ? C2B H2BB 0.9900 . ? C2B C3B 1.517(11) . ? C3B H3BA 0.9900 . ? C3B H3BB 0.9900 . ? C3B C4B 1.529(10) . ? C4B H4BA 0.9800 . ? C4B H4BB 0.9800 . ? C4B H4BC 0.9800 . ? 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 P1 Au1 S1 173.72(4) . . ? P2 Au2 S1 173.69(4) . . ? Au1 S1 Au2 95.34(3) . . ? C1 S1 Au1 102.94(19) . . ? C1 S1 Au2 101.10(14) . . ? C5 P1 Au1 106.78(12) . . ? C9 P1 Au1 107.76(12) . . ? C9 P1 C5 115.09(18) . . ? C13 P1 Au1 115.68(12) . . ? C13 P1 C5 107.56(18) . . ? C13 P1 C9 104.28(16) . . ? C25 P2 Au2 105.03(12) . . ? C25 P2 C29 116.2(2) . . ? C29 P2 Au2 109.03(14) . . ? C33 P2 Au2 115.61(17) . . ? C33 P2 C25 106.63(18) . . ? C33 P2 C29 104.71(19) . . ? S1 C1 H1AA 108.4 . . ? S1 C1 H1AB 108.4 . . ? S1 C1 H1BC 104(7) . . ? S1 C1 H1BD 95(6) . . ? H1AA C1 H1AB 107.4 . . ? H1AA C1 H1BC 18.4 . . ? H1AA C1 H1BD 92.6 . . ? H1AB C1 H1BC 125.2 . . ? H1AB C1 H1BD 25.2 . . ? C2A C1 S1 115.7(4) . . ? C2A C1 H1AA 108.4 . . ? C2A C1 H1AB 108.4 . . ? C2A C1 H1BC 96(7) . . ? C2A C1 H1BD 133(6) . . ? C2B C1 S1 103.7(4) . . ? C2B C1 H1AA 139.0 . . ? C2B C1 H1AB 85.3 . . ? C2B C1 C2A 32.5(4) . . ? C2B C1 H1BC 128(7) . . ? C2B C1 H1BD 110(6) . . ? H1BC C1 H1BD 111(9) . . ? C1 C2A H2AA 110.1 . . ? C1 C2A H2AB 110.1 . . ? H2AA C2A H2AB 108.4 . . ? C3A C2A C1 108.2(6) . . ? C3A C2A H2AA 110.1 . . ? C3A C2A H2AB 110.1 . . ? C2A C3A H3AA 109.0 . . ? C2A C3A H3AB 109.0 . . ? C2A C3A C4A 112.9(6) . . ? H3AA C3A H3AB 107.8 . . ? C4A C3A H3AA 109.0 . . ? C4A C3A H3AB 109.0 . . ? C6 C5 P1 116.6(3) . . ? C6 C5 C7 108.1(5) . . ? C6 C5 C8 109.9(5) . . ? C7 C5 P1 109.2(3) . . ? C8 C5 P1 105.3(3) . . ? C8 C5 C7 107.3(4) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 P1 109.2(3) . . ? C10 C9 C12 108.2(4) . . ? C11 C9 P1 116.5(3) . . ? C11 C9 C10 109.2(3) . . ? C11 C9 C12 108.2(3) . . ? C12 C9 P1 105.2(2) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 P1 119.1(3) . . ? C18 C13 P1 122.9(3) . . ? C18 C13 C14 118.0(3) . . ? C13 C14 H14 118.9 . . ? C15 C14 C13 122.1(4) . . ? C15 C14 H14 118.9 . . ? C14 C15 H15 120.3 . . ? C14 C15 C16 119.4(4) . . ? C16 C15 H15 120.3 . . ? C15 C16 H16 120.2 . . ? C15 C16 C17 119.5(4) . . ? C17 C16 H16 120.2 . . ? C16 C17 H17 119.1 . . ? C16 C17 C18 121.8(4) . . ? C18 C17 H17 119.1 . . ? C13 C18 C19 124.9(3) . . ? C17 C18 C13 119.1(3) . . ? C17 C18 C19 115.9(3) . . ? C20 C19 C18 121.2(3) . . ? C20 C19 C24 118.7(3) . . ? C24 C19 C18 119.8(3) . . ? C19 C20 H20 120.0 . . ? C21 C20 C19 120.0(4) . . ? C21 C20 H20 120.0 . . ? C20 C21 H21 119.5 . . ? C20 C21 C22 120.9(4) . . ? C22 C21 H21 119.5 . . ? C21 C22 H22 120.2 . . ? C23 C22 C21 119.5(4) . . ? C23 C22 H22 120.2 . . ? C22 C23 H23 120.0 . . ? C22 C23 C24 120.0(4) . . ? C24 C23 H23 120.0 . . ? C19 C24 H24 119.6 . . ? C23 C24 C19 120.8(4) . . ? C23 C24 H24 119.6 . . ? C26 C25 P2 108.2(3) . . ? C27 C25 P2 105.6(3) . . ? C27 C25 C26 109.0(3) . . ? C28 C25 P2 116.6(3) . . ? C28 C25 C26 109.0(3) . . ? C28 C25 C27 108.2(3) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 P2 109.4(3) . . ? C30 C29 C32 107.8(4) . . ? C31 C29 P2 116.8(3) . . ? C31 C29 C30 108.3(4) . . ? C31 C29 C32 109.6(4) . . ? C32 C29 P2 104.6(3) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 P2 118.6(4) . . ? C34 C33 C38 118.8(4) . . ? C38 C33 P2 122.3(4) . . ? C33 C34 H34 119.3 . . ? C35 C34 C33 121.4(6) . . ? C35 C34 H34 119.3 . . ? C34 C35 H35 120.0 . . ? C36 C35 C34 119.9(6) . . ? C36 C35 H35 120.0 . . ? C35 C36 H36 120.3 . . ? C35 C36 C37 119.4(5) . . ? C37 C36 H36 120.3 . . ? C36 C37 H37 119.0 . . ? C36 C37 C38 122.1(6) . . ? C38 C37 H37 119.0 . . ? C33 C38 C39 125.5(4) . . ? C37 C38 C33 118.4(5) . . ? C37 C38 C39 116.1(5) . . ? C40 C39 C38 119.8(4) . . ? C40 C39 C44 118.8(6) . . ? C44 C39 C38 121.2(6) . . ? C39 C40 H40 119.3 . . ? C39 C40 C41 121.4(5) . . ? C41 C40 H40 119.3 . . ? C40 C41 H41 120.4 . . ? C42 C41 C40 119.2(7) . . ? C42 C41 H41 120.4 . . ? C41 C42 H42 119.8 . . ? C41 C42 C43 120.4(7) . . ? C43 C42 H42 119.8 . . ? C42 C43 H43 119.7 . . ? C42 C43 C44 120.7(6) . . ? C44 C43 H43 119.7 . . ? C39 C44 H44 120.2 . . ? C43 C44 C39 119.5(7) . . ? C43 C44 H44 120.2 . . ? F1A Sb1 F6A 86.8(5) . . ? F1A Sb1 F3A 170.1(5) . . ? F1A Sb1 F4A 87.0(3) . . ? F1A Sb1 F1B 28.6(4) . . ? F1A Sb1 F5B 101.6(6) . . ? F1A Sb1 F2B 106.1(6) . . ? F1A Sb1 F3B 160.2(6) . . ? F6A Sb1 F4A 85.2(6) . . ? F6A Sb1 F1B 98.1(6) . . ? F6A Sb1 F5B 164.5(6) . . ? F3A Sb1 F6A 87.7(6) . . ? F3A Sb1 F4A 84.3(5) . . ? F3A Sb1 F1B 161.1(7) . . ? F3A Sb1 F5B 85.7(8) . . ? F3A Sb1 F2B 81.0(8) . . ? F5A Sb1 F1A 94.8(5) . . ? F5A Sb1 F6A 175.3(8) . . ? F5A Sb1 F3A 90.0(7) . . ? F5A Sb1 F4A 90.5(6) . . ? F5A Sb1 F1B 85.3(6) . . ? F5A Sb1 F5B 18.7(8) . . ? F5A Sb1 F2B 104.0(8) . . ? F5A Sb1 F3B 90.9(9) . . ? F2A Sb1 F1A 96.9(5) . . ? F2A Sb1 F6A 89.6(7) . . ? F2A Sb1 F3A 91.3(6) . . ? F2A Sb1 F5A 94.6(7) . . ? F2A Sb1 F4A 173.3(5) . . ? F2A Sb1 F1B 70.8(7) . . ? F2A Sb1 F5B 76.5(7) . . ? F2A Sb1 F2B 14.0(8) . . ? F2A Sb1 F3B 101.5(9) . . ? F1B Sb1 F4A 114.0(5) . . ? F4B Sb1 F1A 67.5(5) . . ? F4B Sb1 F6A 107.3(7) . . ? F4B Sb1 F3A 106.4(7) . . ? F4B Sb1 F5A 69.4(7) . . ? F4B Sb1 F2A 155.7(7) . . ? F4B Sb1 F4A 31.0(5) . . ? F4B Sb1 F1B 89.1(5) . . ? F4B Sb1 F5B 88.1(6) . . ? F4B Sb1 F6B 96.7(8) . . ? F4B Sb1 F2B 169.7(7) . . ? F4B Sb1 F3B 97.1(7) . . ? F5B Sb1 F4A 108.1(5) . . ? F5B Sb1 F1B 84.0(7) . . ? F6B Sb1 F1A 75.3(7) . . ? F6B Sb1 F6A 13.1(8) . . ? F6B Sb1 F3A 98.2(9) . . ? F6B Sb1 F5A 165.5(8) . . ? F6B Sb1 F2A 97.1(9) . . ? F6B Sb1 F4A 78.6(8) . . ? F6B Sb1 F1B 90.4(8) . . ? F6B Sb1 F5B 172.6(10) . . ? F6B Sb1 F2B 89.1(7) . . ? F6B Sb1 F3B 95.2(8) . . ? F2B Sb1 F6A 79.8(7) . . ? F2B Sb1 F4A 159.3(5) . . ? F2B Sb1 F1B 82.4(6) . . ? F2B Sb1 F5B 85.3(6) . . ? F3B Sb1 F6A 86.1(9) . . ? F3B Sb1 F3A 10.3(10) . . ? F3B Sb1 F4A 74.0(7) . . ? F3B Sb1 F1B 171.1(7) . . ? F3B Sb1 F5B 89.8(8) . . ? F3B Sb1 F2B 90.8(7) . . ? C1S Cl2 Cl2 36.1(3) 3_557 3_557 ? C1S Cl2 Cl2 48.0(4) . 3_557 ? C1S Cl2 C1S 84.1(6) . 3_557 ? Cl1 C1S Cl2 111.5(5) . 3_557 ? Cl1 C1S H1S 111.5 . . ? Cl1 C1S Cl2A 108.8(4) . . ? Cl2 C1S Cl1 114.1(5) . . ? Cl2 C1S Cl2 95.9(6) . 3_557 ? Cl2 C1S H1S 111.5 3_557 . ? Cl2 C1S H1S 111.5 . . ? Cl2 C1S Cl2A 111.0(6) 3_557 . ? Cl2 C1S Cl2A 15.37(17) . . ? Cl2A C1S H1S 102.1 . . ? C1 C2B H2BA 109.9 . . ? C1 C2B H2BB 109.9 . . ? H2BA C2B H2BB 108.3 . . ? C3B C2B C1 108.7(6) . . ? C3B C2B H2BA 109.9 . . ? C3B C2B H2BB 109.9 . . ? C2B C3B H3BA 109.2 . . ? C2B C3B H3BB 109.2 . . ? C2B C3B C4B 112.0(7) . . ? H3BA C3B H3BB 107.9 . . ? C4B C3B H3BA 109.2 . . ? C4B C3B H3BB 109.2 . . ? C3B C4B H4BA 109.5 . . ? C3B C4B H4BB 109.5 . . ? C3B C4B H4BC 109.5 . . ? H4BA C4B H4BB 109.5 . . ? H4BA C4B H4BC 109.5 . . ? H4BB C4B H4BC 109.5 . . ? _database_code_depnum_ccdc_archive 'CCDC 914705' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global # Attachment '15964_web_deposit_cif_file_6_GeorginaRosair_1354882535.8a.cif' data_4458 #TrackingRef '15964_web_deposit_cif_file_6_GeorginaRosair_1354882535.8a.cif' _audit_creation_date 2012-11-15 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C26 H34 Au N P, F6 Sb' _chemical_formula_sum 'C26 H34 Au F6 N P Sb' _chemical_formula_weight 824.23 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Sb Sb -0.5866 1.5461 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 7.5686(4) _cell_length_b 17.4546(9) _cell_length_c 20.8291(11) _cell_angle_alpha 90.00 _cell_angle_beta 95.628(3) _cell_angle_gamma 90.00 _cell_volume 2738.4(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9761 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 35.910 _cell_measurement_theta_min 2.946 _exptl_absorpt_coefficient_mu 6.453 _exptl_absorpt_correction_T_max 0.7471 _exptl_absorpt_correction_T_min 0.5019 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. R(int) was 0.1212 before and 0.0469 after correction. The Ratio of minimum to maximum transmission is 0.6718. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.999 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_description BLOCK _exptl_crystal_F_000 1584 _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.26 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_unetI/netI 0.0286 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 69144 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 36.02 _diffrn_reflns_theta_min 2.29 _diffrn_ambient_temperature 100.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'MO K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number 0 _reflns_number_gt 10873 _reflns_number_total 12891 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction 'SAINT v7.68A (Bruker, 2009)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; XS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 3.291 _refine_diff_density_min -2.036 _refine_diff_density_rms 0.120 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 337 _refine_ls_number_reflns 12891 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0235 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0120P)^2^+3.0619P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.0480 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Au1 Au 0.097411(10) 0.247608(4) 0.332417(3) 0.01537(2) Uani 1 1 d . . . Sb1 Sb 0.350070(17) 0.602140(7) 0.324628(6) 0.01631(3) Uani 1 1 d . . . P1 P -0.02089(6) 0.29158(2) 0.42059(2) 0.01179(7) Uani 1 1 d . . . F1 F 0.3446(2) 0.63744(11) 0.23952(7) 0.0445(4) Uani 1 1 d . . . F2 F 0.3267(2) 0.70305(8) 0.35290(9) 0.0469(4) Uani 1 1 d . . . F3 F 0.3632(2) 0.57034(10) 0.41046(6) 0.0363(3) Uani 1 1 d . . . F4 F 0.3670(3) 0.50147(8) 0.29687(9) 0.0497(5) Uani 1 1 d . . . F5 F 0.59712(18) 0.61226(9) 0.33017(7) 0.0352(3) Uani 1 1 d . . . F6 F 0.10090(19) 0.59469(11) 0.31700(8) 0.0416(4) Uani 1 1 d . . . N1 N 0.1757(3) 0.21042(10) 0.24255(9) 0.0236(4) Uani 1 1 d . . . H1A H 0.268(4) 0.1803(16) 0.2486(13) 0.028 Uiso 1 1 d . . . H1B H 0.086(4) 0.1804(16) 0.2232(13) 0.028 Uiso 1 1 d . . . C2 C 0.2182(3) 0.27495(10) 0.20283(8) 0.0164(3) Uani 1 1 d . . . C3 C 0.0841(3) 0.31088(11) 0.16355(10) 0.0204(4) Uani 1 1 d . . . H3 H -0.0344 0.2924 0.1611 0.025 Uiso 1 1 calc R . . C4 C 0.1265(3) 0.37438(12) 0.12788(10) 0.0231(4) Uani 1 1 d . . . H4 H 0.0364 0.3990 0.1003 0.028 Uiso 1 1 calc R . . C5 C 0.2986(3) 0.40219(11) 0.13212(10) 0.0234(4) Uani 1 1 d . . . H5 H 0.3261 0.4462 0.1082 0.028 Uiso 1 1 calc R . . C6 C 0.4301(3) 0.36556(11) 0.17134(10) 0.0205(4) Uani 1 1 d . . . H6 H 0.5483 0.3845 0.1743 0.025 Uiso 1 1 calc R . . C7 C 0.3905(3) 0.30122(11) 0.20645(9) 0.0186(3) Uani 1 1 d . . . H7 H 0.4816 0.2755 0.2327 0.022 Uiso 1 1 calc R . . C8 C -0.1094(2) 0.21108(9) 0.46406(8) 0.0117(3) Uani 1 1 d . . . C9 C -0.2321(2) 0.22789(10) 0.50842(9) 0.0142(3) Uani 1 1 d . . . H9 H -0.2540 0.2800 0.5183 0.017 Uiso 1 1 calc R . . C10 C -0.3224(2) 0.17095(11) 0.53835(9) 0.0170(3) Uani 1 1 d . . . H10 H -0.4044 0.1840 0.5683 0.020 Uiso 1 1 calc R . . C11 C -0.2915(2) 0.09473(11) 0.52408(9) 0.0179(3) Uani 1 1 d . . . H11 H -0.3547 0.0552 0.5433 0.021 Uiso 1 1 calc R . . C12 C -0.1679(2) 0.07658(10) 0.48155(9) 0.0154(3) Uani 1 1 d . . . H12 H -0.1468 0.0242 0.4726 0.018 Uiso 1 1 calc R . . C13 C -0.0728(2) 0.13304(9) 0.45121(8) 0.0121(3) Uani 1 1 d . . . C14 C 0.0599(2) 0.10485(9) 0.40844(8) 0.0131(3) Uani 1 1 d . . . C15 C 0.0021(3) 0.06635(11) 0.35125(9) 0.0187(3) Uani 1 1 d . . . H15 H -0.1214 0.0601 0.3393 0.022 Uiso 1 1 calc R . . C16 C 0.1248(3) 0.03706(11) 0.31164(10) 0.0239(4) Uani 1 1 d . . . H16 H 0.0845 0.0104 0.2732 0.029 Uiso 1 1 calc R . . C17 C 0.3052(3) 0.04693(11) 0.32831(10) 0.0231(4) Uani 1 1 d . . . H17 H 0.3884 0.0283 0.3008 0.028 Uiso 1 1 calc R . . C18 C 0.3639(3) 0.08413(11) 0.38543(10) 0.0214(4) Uani 1 1 d . . . H18 H 0.4876 0.0908 0.3970 0.026 Uiso 1 1 calc R . . C19 C 0.2422(2) 0.11174(10) 0.42588(9) 0.0164(3) Uani 1 1 d . . . H19 H 0.2835 0.1354 0.4656 0.020 Uiso 1 1 calc R . . C20 C -0.2168(3) 0.35231(10) 0.38754(9) 0.0169(3) Uani 1 1 d . . . C21 C -0.3646(3) 0.29661(13) 0.36280(10) 0.0234(4) Uani 1 1 d . . . H21A H -0.3176 0.2591 0.3339 0.035 Uiso 1 1 calc R . . H21B H -0.4620 0.3252 0.3393 0.035 Uiso 1 1 calc R . . H21C H -0.4088 0.2699 0.3994 0.035 Uiso 1 1 calc R . . C22 C -0.1625(3) 0.39804(13) 0.32905(10) 0.0273(4) Uani 1 1 d . . . H22A H -0.0596 0.4303 0.3427 0.041 Uiso 1 1 calc R . . H22B H -0.2617 0.4305 0.3118 0.041 Uiso 1 1 calc R . . H22C H -0.1317 0.3624 0.2956 0.041 Uiso 1 1 calc R . . C23 C -0.2870(3) 0.41013(11) 0.43442(9) 0.0192(3) Uani 1 1 d . . . H23A H -0.3201 0.3831 0.4727 0.029 Uiso 1 1 calc R . . H23B H -0.3913 0.4364 0.4132 0.029 Uiso 1 1 calc R . . H23C H -0.1943 0.4478 0.4473 0.029 Uiso 1 1 calc R . . C24 C 0.1363(2) 0.34426(10) 0.48036(9) 0.0161(3) Uani 1 1 d . . . C25 C 0.2047(3) 0.41514(11) 0.44653(11) 0.0234(4) Uani 1 1 d . . . H25A H 0.2465 0.3998 0.4053 0.035 Uiso 1 1 calc R . . H25B H 0.3029 0.4383 0.4741 0.035 Uiso 1 1 calc R . . H25C H 0.1083 0.4525 0.4386 0.035 Uiso 1 1 calc R . . C26 C 0.0581(3) 0.36743(11) 0.54268(9) 0.0187(3) Uani 1 1 d . . . H26A H -0.0446 0.4010 0.5322 0.028 Uiso 1 1 calc R . . H26B H 0.1482 0.3947 0.5710 0.028 Uiso 1 1 calc R . . H26C H 0.0205 0.3214 0.5647 0.028 Uiso 1 1 calc R . . C27 C 0.2936(3) 0.29022(11) 0.49926(10) 0.0206(4) Uani 1 1 d . . . H27A H 0.2522 0.2459 0.5225 0.031 Uiso 1 1 calc R . . H27B H 0.3846 0.3176 0.5271 0.031 Uiso 1 1 calc R . . H27C H 0.3442 0.2728 0.4602 0.031 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 Au1 0.02098(3) 0.01265(3) 0.01418(3) 0.00271(2) 0.01031(2) 0.00366(2) Sb1 0.01939(5) 0.01563(5) 0.01484(5) -0.00048(4) 0.00635(4) -0.00231(4) P1 0.01332(19) 0.01065(17) 0.01224(18) 0.00162(14) 0.00554(15) 0.00126(14) F1 0.0515(10) 0.0625(11) 0.0203(7) 0.0156(7) 0.0072(7) 0.0003(8) F2 0.0612(11) 0.0199(7) 0.0658(11) -0.0107(7) 0.0383(9) -0.0050(7) F3 0.0389(8) 0.0509(9) 0.0201(6) 0.0107(6) 0.0080(6) -0.0082(7) F4 0.0707(12) 0.0216(7) 0.0627(11) -0.0186(7) 0.0358(9) -0.0128(7) F5 0.0211(7) 0.0481(9) 0.0376(8) 0.0045(7) 0.0095(6) -0.0049(6) F6 0.0212(7) 0.0671(11) 0.0364(8) 0.0007(8) 0.0023(6) -0.0059(7) N1 0.0386(11) 0.0141(7) 0.0211(8) 0.0032(6) 0.0180(7) 0.0038(7) C2 0.0264(9) 0.0130(7) 0.0113(7) 0.0001(6) 0.0094(6) 0.0033(6) C3 0.0195(9) 0.0221(9) 0.0200(8) -0.0014(7) 0.0030(7) -0.0017(7) C4 0.0263(10) 0.0243(9) 0.0183(9) 0.0039(7) 0.0000(7) 0.0040(7) C5 0.0323(11) 0.0177(8) 0.0213(9) 0.0046(7) 0.0085(8) 0.0002(7) C6 0.0213(9) 0.0202(8) 0.0208(9) -0.0033(7) 0.0065(7) -0.0025(7) C7 0.0224(9) 0.0205(8) 0.0130(7) -0.0013(6) 0.0026(6) 0.0062(7) C8 0.0114(7) 0.0130(7) 0.0111(7) 0.0014(5) 0.0025(5) -0.0009(5) C9 0.0146(7) 0.0144(7) 0.0143(7) 0.0009(6) 0.0049(6) 0.0010(6) C10 0.0154(8) 0.0201(8) 0.0165(8) 0.0032(6) 0.0062(6) -0.0004(6) C11 0.0147(8) 0.0193(8) 0.0200(8) 0.0048(6) 0.0038(6) -0.0034(6) C12 0.0167(8) 0.0132(7) 0.0162(7) 0.0010(6) 0.0016(6) -0.0013(6) C13 0.0121(7) 0.0135(7) 0.0106(6) 0.0003(5) 0.0004(5) 0.0001(5) C14 0.0173(7) 0.0099(6) 0.0126(7) 0.0005(5) 0.0033(6) 0.0022(5) C15 0.0230(9) 0.0175(8) 0.0156(8) -0.0023(6) 0.0022(7) 0.0008(6) C16 0.0391(12) 0.0176(8) 0.0160(8) -0.0008(7) 0.0073(8) 0.0050(8) C17 0.0328(11) 0.0167(8) 0.0219(9) 0.0045(7) 0.0131(8) 0.0094(7) C18 0.0198(9) 0.0186(8) 0.0273(10) 0.0050(7) 0.0092(7) 0.0055(7) C19 0.0167(8) 0.0133(7) 0.0196(8) -0.0001(6) 0.0031(6) 0.0025(6) C20 0.0195(8) 0.0179(8) 0.0139(7) 0.0026(6) 0.0048(6) 0.0065(6) C21 0.0215(9) 0.0290(10) 0.0186(9) -0.0021(7) -0.0036(7) 0.0062(7) C22 0.0368(12) 0.0269(10) 0.0199(9) 0.0103(8) 0.0116(8) 0.0147(9) C23 0.0206(9) 0.0188(8) 0.0189(8) 0.0006(6) 0.0052(7) 0.0075(6) C24 0.0133(7) 0.0139(7) 0.0218(8) -0.0021(6) 0.0059(6) -0.0013(6) C25 0.0235(10) 0.0147(8) 0.0336(11) -0.0013(7) 0.0109(8) -0.0040(7) C26 0.0174(8) 0.0186(8) 0.0204(8) -0.0050(6) 0.0034(7) -0.0005(6) C27 0.0139(8) 0.0193(8) 0.0286(10) -0.0037(7) 0.0012(7) 0.0020(6) _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 Au1 P1 2.2553(4) . ? Au1 N1 2.1197(17) . ? Sb1 F1 1.8734(14) . ? Sb1 F2 1.8710(14) . ? Sb1 F3 1.8653(13) . ? Sb1 F4 1.8582(14) . ? Sb1 F5 1.8704(14) . ? Sb1 F6 1.8815(15) . ? P1 C8 1.8335(17) . ? P1 C20 1.8964(18) . ? P1 C24 1.8765(19) . ? N1 H1A 0.87(3) . ? N1 H1B 0.92(3) . ? N1 C2 1.452(2) . ? C2 C3 1.389(3) . ? C2 C7 1.378(3) . ? C3 H3 0.9500 . ? C3 C4 1.389(3) . ? C4 H4 0.9500 . ? C4 C5 1.385(3) . ? C5 H5 0.9500 . ? C5 C6 1.381(3) . ? C6 H6 0.9500 . ? C6 C7 1.389(3) . ? C7 H7 0.9500 . ? C8 C9 1.404(2) . ? C8 C13 1.421(2) . ? C9 H9 0.9500 . ? C9 C10 1.388(2) . ? C10 H10 0.9500 . ? C10 C11 1.388(3) . ? C11 H11 0.9500 . ? C11 C12 1.386(3) . ? C12 H12 0.9500 . ? C12 C13 1.406(2) . ? C13 C14 1.490(2) . ? C14 C15 1.400(2) . ? C14 C19 1.397(3) . ? C15 H15 0.9500 . ? C15 C16 1.398(3) . ? C16 H16 0.9500 . ? C16 C17 1.386(3) . ? C17 H17 0.9500 . ? C17 C18 1.390(3) . ? C18 H18 0.9500 . ? C18 C19 1.394(3) . ? C19 H19 0.9500 . ? C20 C21 1.533(3) . ? C20 C22 1.545(3) . ? C20 C23 1.535(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.538(3) . ? C24 C26 1.533(3) . ? C24 C27 1.540(3) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? 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 N1 Au1 P1 172.28(6) . . ? F1 Sb1 F6 90.79(7) . . ? F2 Sb1 F1 89.67(8) . . ? F2 Sb1 F6 88.10(8) . . ? F3 Sb1 F1 177.42(8) . . ? F3 Sb1 F2 88.64(8) . . ? F3 Sb1 F5 90.56(7) . . ? F3 Sb1 F6 91.10(7) . . ? F4 Sb1 F1 90.71(8) . . ? F4 Sb1 F2 178.49(8) . . ? F4 Sb1 F3 91.03(8) . . ? F4 Sb1 F5 90.54(8) . . ? F4 Sb1 F6 90.43(8) . . ? F5 Sb1 F1 87.51(7) . . ? F5 Sb1 F2 90.94(8) . . ? F5 Sb1 F6 178.06(7) . . ? C8 P1 Au1 109.57(6) . . ? C8 P1 C20 107.28(8) . . ? C8 P1 C24 106.66(8) . . ? C20 P1 Au1 104.67(6) . . ? C24 P1 Au1 115.50(6) . . ? C24 P1 C20 112.92(8) . . ? Au1 N1 H1A 110.2(18) . . ? Au1 N1 H1B 107.7(18) . . ? H1A N1 H1B 105(2) . . ? C2 N1 Au1 111.24(12) . . ? C2 N1 H1A 109.3(18) . . ? C2 N1 H1B 112.8(17) . . ? C3 C2 N1 119.71(19) . . ? C7 C2 N1 119.24(18) . . ? C7 C2 C3 121.02(17) . . ? C2 C3 H3 120.6 . . ? C4 C3 C2 118.76(19) . . ? C4 C3 H3 120.6 . . ? C3 C4 H4 119.6 . . ? C5 C4 C3 120.71(19) . . ? C5 C4 H4 119.6 . . ? C4 C5 H5 120.2 . . ? C6 C5 C4 119.61(18) . . ? C6 C5 H5 120.2 . . ? C5 C6 H6 119.8 . . ? C5 C6 C7 120.40(19) . . ? C7 C6 H6 119.8 . . ? C2 C7 C6 119.48(18) . . ? C2 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C9 C8 P1 117.54(13) . . ? C9 C8 C13 118.56(15) . . ? C13 C8 P1 123.66(13) . . ? C8 C9 H9 118.9 . . ? C10 C9 C8 122.18(16) . . ? C10 C9 H9 118.9 . . ? C9 C10 H10 120.3 . . ? C11 C10 C9 119.30(17) . . ? C11 C10 H10 120.3 . . ? C10 C11 H11 120.2 . . ? C12 C11 C10 119.62(16) . . ? C12 C11 H11 120.2 . . ? C11 C12 H12 118.9 . . ? C11 C12 C13 122.28(16) . . ? C13 C12 H12 118.9 . . ? C8 C13 C14 125.77(15) . . ? C12 C13 C8 117.99(15) . . ? C12 C13 C14 116.23(15) . . ? C15 C14 C13 119.67(16) . . ? C19 C14 C13 121.50(15) . . ? C19 C14 C15 118.71(16) . . ? C14 C15 H15 119.7 . . ? C16 C15 C14 120.52(19) . . ? C16 C15 H15 119.7 . . ? C15 C16 H16 119.9 . . ? C17 C16 C15 120.11(19) . . ? C17 C16 H16 119.9 . . ? C16 C17 H17 120.1 . . ? C16 C17 C18 119.82(18) . . ? C18 C17 H17 120.1 . . ? C17 C18 H18 119.9 . . ? C17 C18 C19 120.3(2) . . ? C19 C18 H18 119.9 . . ? C14 C19 H19 119.7 . . ? C18 C19 C14 120.51(18) . . ? C18 C19 H19 119.7 . . ? C21 C20 P1 106.64(13) . . ? C21 C20 C22 107.73(17) . . ? C21 C20 C23 110.14(16) . . ? C22 C20 P1 108.42(13) . . ? C23 C20 P1 116.33(13) . . ? C23 C20 C22 107.30(15) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 P1 108.07(14) . . ? C25 C24 C27 108.87(16) . . ? C26 C24 P1 114.73(13) . . ? C26 C24 C25 110.55(15) . . ? C26 C24 C27 107.37(16) . . ? C27 C24 P1 107.07(12) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1B F6 0.92(3) 2.17(3) 3.081(3) 171(2) 2_545 _database_code_depnum_ccdc_archive 'CCDC 914706' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global # Attachment '15965_web_deposit_cif_file_8_GeorginaRosair_1354882535.8b.cif' data_4340 #TrackingRef '15965_web_deposit_cif_file_8_GeorginaRosair_1354882535.8b.cif' _audit_creation_date 2012-08-01 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C27 H35 Au N O P, F6 Sb' _chemical_formula_sum 'C27 H35 Au F6 N O P Sb' _chemical_formula_weight 853.25 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Sb Sb -0.5866 1.5461 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 13.1268(4) _cell_length_b 11.7372(4) _cell_length_c 19.9682(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.108(2) _cell_angle_gamma 90.00 _cell_volume 2955.75(17) _cell_formula_units_Z 4 _cell_measurement_reflns_used 4328 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 26.14 _cell_measurement_theta_min 2.74 _exptl_absorpt_coefficient_mu 5.985 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Twinabs (Bruker, 2008)' _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.917 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description PLATE _exptl_crystal_F_000 1644 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0691 _diffrn_reflns_av_unetI/netI 0.0441 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 102285 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 30.16 _diffrn_reflns_theta_min 2.41 _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed tube' _diffrn_source_current 35.0 _diffrn_source_power 1.75 _diffrn_source_voltage 50.0 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _reflns_number_gt 7299 _reflns_number_total 8722 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation, 2011) ; _refine_diff_density_max 0.681 _refine_diff_density_min -1.098 _refine_diff_density_rms 0.168 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 351 _refine_ls_number_reflns 8722 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_gt 0.0298 _refine_ls_restrained_S_all 0.965 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+0.8583P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.0692 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Au1 Au 0.207895(12) 0.735926(12) 0.236951(8) 0.01486(4) Uani 1 1 d . . . P1 P 0.35190(8) 0.80319(8) 0.31739(5) 0.01395(19) Uani 1 1 d . . . O7 O 0.0483(3) 0.1952(3) 0.19181(18) 0.0294(8) Uani 1 1 d . . . N1 N 0.0685(3) 0.6690(3) 0.1677(2) 0.0240(8) Uani 1 1 d . . . H1 H 0.0195 0.7116 0.1398 0.029 Uiso 1 1 calc R . . C1 C 0.0615(3) 0.5455(3) 0.1707(2) 0.0162(8) Uani 1 1 d . . . C2 C 0.0520(3) 0.4785(4) 0.1125(2) 0.0191(8) Uani 1 1 d . . . H2 H 0.0481 0.5130 0.0688 0.023 Uiso 1 1 calc R . . C3 C 0.0480(3) 0.3598(4) 0.1176(2) 0.0185(8) Uani 1 1 d . . . H3 H 0.0422 0.3136 0.0777 0.022 Uiso 1 1 calc R . . C4 C 0.0526(3) 0.3102(4) 0.1812(2) 0.0194(8) Uani 1 1 d . . . C5 C 0.0607(4) 0.3781(4) 0.2398(2) 0.0246(10) Uani 1 1 d . . . H5 H 0.0623 0.3440 0.2832 0.029 Uiso 1 1 calc R . . C6 C 0.0663(3) 0.4949(4) 0.2344(2) 0.0223(9) Uani 1 1 d . . . H6 H 0.0736 0.5411 0.2746 0.027 Uiso 1 1 calc R . . C7 C 0.0494(4) 0.1224(4) 0.1347(3) 0.0354(12) Uani 1 1 d . . . H7A H -0.0121 0.1394 0.0952 0.053 Uiso 1 1 calc R . . H7B H 0.0463 0.0427 0.1487 0.053 Uiso 1 1 calc R . . H7C H 0.1147 0.1352 0.1211 0.053 Uiso 1 1 calc R . . C8 C 0.3176(3) 0.9481(3) 0.3451(2) 0.0185(8) Uani 1 1 d . . . C9 C 0.4091(4) 1.0120(4) 0.3959(2) 0.0262(10) Uani 1 1 d . . . H9A H 0.4345 0.9677 0.4389 0.039 Uiso 1 1 calc R . . H9B H 0.3840 1.0866 0.4067 0.039 Uiso 1 1 calc R . . H9C H 0.4671 1.0225 0.3744 0.039 Uiso 1 1 calc R . . C10 C 0.2248(3) 0.9344(4) 0.3770(2) 0.0227(9) Uani 1 1 d . . . H10A H 0.1683 0.8901 0.3453 0.034 Uiso 1 1 calc R . . H10B H 0.1975 1.0097 0.3843 0.034 Uiso 1 1 calc R . . H10C H 0.2492 0.8947 0.4217 0.034 Uiso 1 1 calc R . . C11 C 0.2815(4) 1.0185(4) 0.2778(2) 0.0267(10) Uani 1 1 d . . . H11A H 0.3408 1.0271 0.2573 0.040 Uiso 1 1 calc R . . H11B H 0.2581 1.0939 0.2886 0.040 Uiso 1 1 calc R . . H11C H 0.2227 0.9795 0.2447 0.040 Uiso 1 1 calc R . . C12 C 0.3890(4) 0.6966(3) 0.3906(2) 0.0197(8) Uani 1 1 d . . . C13 C 0.4468(4) 0.7449(4) 0.4629(2) 0.0260(10) Uani 1 1 d . . . H13A H 0.5106 0.7858 0.4601 0.039 Uiso 1 1 calc R . . H13B H 0.4670 0.6823 0.4964 0.039 Uiso 1 1 calc R . . H13C H 0.3996 0.7974 0.4782 0.039 Uiso 1 1 calc R . . C14 C 0.4602(4) 0.6054(4) 0.3699(2) 0.0273(10) Uani 1 1 d . . . H14A H 0.4278 0.5810 0.3218 0.041 Uiso 1 1 calc R . . H14B H 0.4674 0.5396 0.4012 0.041 Uiso 1 1 calc R . . H14C H 0.5304 0.6379 0.3738 0.041 Uiso 1 1 calc R . . C15 C 0.2882(4) 0.6368(4) 0.3965(2) 0.0263(10) Uani 1 1 d . . . H15A H 0.2367 0.6938 0.4021 0.039 Uiso 1 1 calc R . . H15B H 0.3057 0.5857 0.4369 0.039 Uiso 1 1 calc R . . H15C H 0.2577 0.5924 0.3541 0.039 Uiso 1 1 calc R . . C16 C 0.4675(3) 0.8215(3) 0.2840(2) 0.0169(8) Uani 1 1 d . . . C17 C 0.5657(3) 0.8462(3) 0.3315(2) 0.0198(8) Uani 1 1 d . . . H17 H 0.5691 0.8572 0.3792 0.024 Uiso 1 1 calc R . . C18 C 0.6581(3) 0.8551(4) 0.3108(3) 0.0249(10) Uani 1 1 d . . . H18 H 0.7239 0.8708 0.3441 0.030 Uiso 1 1 calc R . . C19 C 0.6530(3) 0.8408(4) 0.2407(3) 0.0260(10) Uani 1 1 d . . . H19 H 0.7154 0.8477 0.2256 0.031 Uiso 1 1 calc R . . C20 C 0.5563(4) 0.8164(4) 0.1929(2) 0.0232(9) Uani 1 1 d . . . H20 H 0.5534 0.8064 0.1452 0.028 Uiso 1 1 calc R . . C21 C 0.4629(3) 0.8063(3) 0.2135(2) 0.0155(8) Uani 1 1 d . . . C22 C 0.3663(3) 0.7766(3) 0.1558(2) 0.0165(8) Uani 1 1 d . . . C23 C 0.3452(3) 0.6627(4) 0.1363(2) 0.0193(8) Uani 1 1 d . . . H23 H 0.3885 0.6041 0.1623 0.023 Uiso 1 1 calc R . . C24 C 0.2608(4) 0.6347(4) 0.0788(2) 0.0238(9) Uani 1 1 d . . . H24 H 0.2481 0.5572 0.0654 0.029 Uiso 1 1 calc R . . C25 C 0.1955(4) 0.7182(4) 0.0412(2) 0.0272(10) Uani 1 1 d . . . H25 H 0.1375 0.6986 0.0026 0.033 Uiso 1 1 calc R . . C26 C 0.2162(4) 0.8329(4) 0.0610(2) 0.0246(9) Uani 1 1 d . . . H26 H 0.1715 0.8912 0.0357 0.030 Uiso 1 1 calc R . . C27 C 0.3015(3) 0.8611(4) 0.1171(2) 0.0211(9) Uani 1 1 d . . . H27 H 0.3159 0.9389 0.1293 0.025 Uiso 1 1 calc R . . Sb1 Sb 0.79845(2) 0.70182(2) 0.539578(14) 0.01739(6) Uani 1 1 d . . . F1 F 0.9283(2) 0.7522(3) 0.52634(15) 0.0348(7) Uani 1 1 d . . . F2 F 0.7653(2) 0.6233(3) 0.45489(14) 0.0387(7) Uani 1 1 d . . . F3 F 0.7322(2) 0.8324(2) 0.49411(14) 0.0339(7) Uani 1 1 d . . . F4 F 0.6726(2) 0.6536(2) 0.55692(16) 0.0353(7) Uani 1 1 d . . . F5 F 0.8346(2) 0.7817(2) 0.62494(13) 0.0267(6) Uani 1 1 d . . . F6 F 0.8698(2) 0.5734(2) 0.58610(15) 0.0333(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 Au1 0.01083(7) 0.01744(7) 0.01515(7) -0.00246(5) 0.00166(6) -0.00110(6) P1 0.0113(5) 0.0157(5) 0.0144(5) -0.0014(4) 0.0027(4) -0.0007(4) O7 0.0266(18) 0.0209(15) 0.038(2) 0.0040(14) 0.0051(15) -0.0048(13) N1 0.0175(19) 0.0202(18) 0.026(2) 0.0028(15) -0.0070(16) 0.0018(14) C1 0.0079(18) 0.0208(19) 0.019(2) -0.0035(15) 0.0030(16) -0.0007(14) C2 0.015(2) 0.027(2) 0.0138(19) 0.0015(16) 0.0020(16) -0.0028(16) C3 0.0132(19) 0.025(2) 0.017(2) -0.0052(16) 0.0037(16) -0.0029(15) C4 0.012(2) 0.023(2) 0.022(2) 0.0007(17) 0.0029(16) -0.0007(16) C5 0.021(2) 0.037(3) 0.014(2) 0.0045(18) 0.0018(17) -0.0078(19) C6 0.018(2) 0.029(2) 0.020(2) -0.0058(17) 0.0050(17) -0.0058(17) C7 0.033(3) 0.022(2) 0.052(3) -0.003(2) 0.013(3) -0.001(2) C8 0.017(2) 0.0166(18) 0.021(2) -0.0017(15) 0.0039(16) 0.0017(15) C9 0.018(2) 0.026(2) 0.034(3) -0.0114(19) 0.0068(19) -0.0049(17) C10 0.016(2) 0.024(2) 0.030(2) -0.0059(17) 0.0087(19) -0.0005(16) C11 0.034(3) 0.021(2) 0.023(2) 0.0019(17) 0.005(2) 0.0044(18) C12 0.019(2) 0.0189(18) 0.017(2) 0.0022(15) -0.0016(17) 0.0000(16) C13 0.023(2) 0.038(3) 0.015(2) -0.0007(18) 0.0003(18) -0.0029(19) C14 0.032(3) 0.021(2) 0.029(2) 0.0026(18) 0.008(2) 0.0049(18) C15 0.029(3) 0.025(2) 0.023(2) 0.0046(18) 0.004(2) -0.0062(19) C16 0.0114(18) 0.0164(18) 0.023(2) 0.0002(16) 0.0043(16) 0.0006(14) C17 0.015(2) 0.0183(19) 0.025(2) -0.0028(16) 0.0038(17) -0.0018(15) C18 0.0115(19) 0.026(2) 0.035(3) -0.0083(19) 0.0029(19) -0.0026(16) C19 0.016(2) 0.024(2) 0.042(3) -0.004(2) 0.015(2) -0.0046(16) C20 0.023(2) 0.024(2) 0.025(2) -0.0002(17) 0.0090(18) 0.0001(17) C21 0.0136(18) 0.0119(16) 0.022(2) 0.0008(14) 0.0061(16) 0.0013(14) C22 0.0155(19) 0.0179(18) 0.0169(19) 0.0004(15) 0.0057(16) 0.0006(15) C23 0.0136(19) 0.023(2) 0.022(2) -0.0008(16) 0.0072(17) 0.0007(16) C24 0.023(2) 0.025(2) 0.025(2) -0.0072(17) 0.0100(19) -0.0037(17) C25 0.021(2) 0.043(3) 0.015(2) -0.0003(18) 0.0010(18) -0.002(2) C26 0.026(2) 0.032(2) 0.015(2) 0.0020(17) 0.0039(19) 0.0020(19) C27 0.022(2) 0.022(2) 0.020(2) 0.0030(16) 0.0081(18) 0.0010(17) Sb1 0.01427(13) 0.01916(13) 0.01710(13) -0.00044(9) 0.00163(11) 0.00001(10) F1 0.0203(14) 0.062(2) 0.0222(15) 0.0024(13) 0.0066(11) -0.0117(14) F2 0.0355(18) 0.0510(18) 0.0251(15) -0.0180(13) 0.0010(13) 0.0003(14) F3 0.0368(17) 0.0275(14) 0.0281(15) 0.0056(12) -0.0065(13) 0.0049(12) F4 0.0174(13) 0.0433(17) 0.0454(18) 0.0064(14) 0.0092(13) -0.0040(12) F5 0.0319(15) 0.0277(13) 0.0170(13) -0.0036(10) 0.0010(11) 0.0036(11) F6 0.0320(16) 0.0238(13) 0.0417(17) 0.0039(12) 0.0061(14) 0.0089(11) _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 Au1 P1 2.2565(10) . ? Au1 N1 2.116(4) . ? P1 C8 1.881(4) . ? P1 C12 1.883(4) . ? P1 C16 1.832(4) . ? O7 C4 1.370(5) . ? O7 C7 1.428(6) . ? N1 C1 1.454(5) . ? C1 C2 1.380(5) . ? C1 C6 1.391(6) . ? C2 C3 1.398(6) . ? C3 C4 1.382(6) . ? C4 C5 1.395(6) . ? C5 C6 1.379(6) . ? C8 C9 1.536(6) . ? C8 C10 1.531(6) . ? C8 C11 1.535(6) . ? C12 C13 1.541(6) . ? C12 C14 1.552(6) . ? C12 C15 1.530(6) . ? C16 C17 1.402(6) . ? C16 C21 1.403(6) . ? C17 C18 1.389(6) . ? C18 C19 1.394(7) . ? C19 C20 1.390(6) . ? C20 C21 1.403(6) . ? C21 C22 1.500(6) . ? C22 C23 1.398(6) . ? C22 C27 1.393(6) . ? C23 C24 1.396(6) . ? C24 C25 1.378(6) . ? C25 C26 1.407(6) . ? C26 C27 1.387(6) . ? Sb1 F1 1.891(3) . ? Sb1 F2 1.868(3) . ? Sb1 F3 1.868(3) . ? Sb1 F4 1.867(3) . ? Sb1 F5 1.887(3) . ? Sb1 F6 1.878(3) . ? 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 N1 Au1 P1 175.76(11) . . ? C8 P1 Au1 107.68(14) . . ? C8 P1 C12 113.81(19) . . ? C12 P1 Au1 107.78(14) . . ? C16 P1 Au1 113.40(14) . . ? C16 P1 C8 106.92(19) . . ? C16 P1 C12 107.39(19) . . ? C4 O7 C7 117.1(4) . . ? C1 N1 Au1 113.3(3) . . ? C2 C1 N1 121.7(4) . . ? C2 C1 C6 119.9(4) . . ? C6 C1 N1 118.4(4) . . ? C1 C2 C3 120.2(4) . . ? C4 C3 C2 119.6(4) . . ? O7 C4 C3 124.4(4) . . ? O7 C4 C5 115.4(4) . . ? C3 C4 C5 120.2(4) . . ? C6 C5 C4 119.8(4) . . ? C5 C6 C1 120.4(4) . . ? C9 C8 P1 115.4(3) . . ? C10 C8 P1 108.1(3) . . ? C10 C8 C9 110.0(3) . . ? C10 C8 C11 109.4(4) . . ? C11 C8 P1 105.7(3) . . ? C11 C8 C9 108.0(4) . . ? C13 C12 P1 115.9(3) . . ? C13 C12 C14 109.1(4) . . ? C14 C12 P1 107.2(3) . . ? C15 C12 P1 108.8(3) . . ? C15 C12 C13 108.0(4) . . ? C15 C12 C14 107.5(4) . . ? C17 C16 P1 118.5(3) . . ? C17 C16 C21 118.7(4) . . ? C21 C16 P1 122.7(3) . . ? C18 C17 C16 122.0(4) . . ? C17 C18 C19 119.1(4) . . ? C20 C19 C18 119.6(4) . . ? C19 C20 C21 121.5(4) . . ? C16 C21 C22 126.3(4) . . ? C20 C21 C16 119.1(4) . . ? C20 C21 C22 114.6(4) . . ? C23 C22 C21 119.8(4) . . ? C27 C22 C21 121.1(4) . . ? C27 C22 C23 118.9(4) . . ? C24 C23 C22 120.4(4) . . ? C25 C24 C23 120.8(4) . . ? C24 C25 C26 119.0(4) . . ? C27 C26 C25 120.3(4) . . ? C26 C27 C22 120.7(4) . . ? F2 Sb1 F1 91.16(13) . . ? F2 Sb1 F5 178.90(13) . . ? F2 Sb1 F6 90.62(13) . . ? F3 Sb1 F1 89.53(13) . . ? F3 Sb1 F2 90.27(13) . . ? F3 Sb1 F5 89.88(12) . . ? F3 Sb1 F6 177.90(13) . . ? F4 Sb1 F1 177.42(13) . . ? F4 Sb1 F2 91.28(14) . . ? F4 Sb1 F3 91.28(13) . . ? F4 Sb1 F5 89.81(13) . . ? F4 Sb1 F6 90.59(13) . . ? F5 Sb1 F1 87.75(13) . . ? F6 Sb1 F1 88.56(13) . . ? F6 Sb1 F5 89.19(12) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 F1 0.88 2.29 3.054(5) 145.1 4_475 N1 H1 F5 0.88 2.36 3.006(5) 130.0 4_475 _audit_update_record ; 2012-08-01 # Formatted by publCIF ; _database_code_depnum_ccdc_archive 'CCDC 914707' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global # Attachment '19837_web_deposit_cif_file_2_GeorginaRosair_1366889069.914708.cif' data_4371 #TrackingRef '19837_web_deposit_cif_file_2_GeorginaRosair_1366889069.914708.cif' _audit_creation_date 2012-08-22 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C24 H38 Au N P, F6 Sb' _chemical_formula_sum 'C24 H38 Au F6 N P Sb' _chemical_formula_weight 804.24 _chemical_melting_point ? 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 7.6009(4) _cell_length_b 17.7750(9) _cell_length_c 20.5702(10) _cell_angle_alpha 90.00 _cell_angle_beta 98.499(2) _cell_angle_gamma 90.00 _cell_volume 2748.6(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9251 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 34.79 _cell_measurement_theta_min 2.50 _exptl_absorpt_coefficient_mu 6.426 _exptl_absorpt_correction_T_max 0.7469 _exptl_absorpt_correction_T_min 0.5540 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. R(int) was 0.0904 before and 0.0472 after correction. The Ratio of minimum to maximum transmission is 0.7417. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.943 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description PLATE _exptl_crystal_F_000 1552 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.04 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_unetI/netI 0.0312 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_number 82430 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 35.19 _diffrn_reflns_theta_min 1.52 _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.965 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number 0 _reflns_number_gt 9108 _reflns_number_total 11854 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'Bruker SAINT (Bruker 2011)' _computing_data_collection 'Bruker APEX2 (Bruker 2011)' _computing_data_reduction 'Bruker SAINT (Bruker 2011)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 1.763 _refine_diff_density_min -1.797 _refine_diff_density_rms 0.153 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 349 _refine_ls_number_reflns 11854 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0285 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+4.2216P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.0691 _refine_special_details ; Disordered butyl chain equivalent C-C distances restrained to be the same with SADI 0.02 C3B C4B C4B C5 C3A C4A C4A C5. The relative occupancies are 0.515(7) and 0.485(7) for the two components 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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Au1 Au 0.560595(13) 0.748404(6) 0.825021(5) 0.01709(3) Uani 1 1 d . A . P1 P 0.43657(8) 0.79353(4) 0.91016(3) 0.01466(11) Uani 1 1 d . . . N1 N 0.6545(4) 0.70628(15) 0.74135(12) 0.0233(5) Uani 1 1 d . . . H1A H 0.755(6) 0.688(2) 0.754(2) 0.040(11) Uiso 1 1 d . . . H1B H 0.586(6) 0.673(3) 0.724(2) 0.055(14) Uiso 1 1 d . . . C2A C 0.6283(8) 0.7505(3) 0.6815(2) 0.0148(10) Uani 0.485(7) 1 d P A 1 H2AA H 0.5020 0.7655 0.6706 0.018 Uiso 0.485(7) 1 calc PR A 1 H2AB H 0.6617 0.7209 0.6445 0.018 Uiso 0.485(7) 1 calc PR A 1 C2B C 0.7212(13) 0.7664(4) 0.6945(3) 0.0317(16) Uani 0.515(7) 1 d P A 2 H2BA H 0.8385 0.7854 0.7153 0.038 Uiso 0.515(7) 1 calc PR A 2 H2BB H 0.7388 0.7411 0.6530 0.038 Uiso 0.515(7) 1 calc PR A 2 C3A C 0.7476(6) 0.8208(3) 0.6939(2) 0.0144(10) Uani 0.515(7) 1 d PD A 1 H3AA H 0.7060 0.8526 0.7281 0.017 Uiso 0.515(7) 1 calc PR A 1 H3AB H 0.8716 0.8053 0.7098 0.017 Uiso 0.515(7) 1 calc PR A 1 C3B C 0.6020(9) 0.8313(4) 0.6782(3) 0.0303(15) Uani 0.485(7) 1 d PD A 2 H3BA H 0.5940 0.8608 0.7184 0.036 Uiso 0.485(7) 1 calc PR A 2 H3BB H 0.4812 0.8133 0.6604 0.036 Uiso 0.485(7) 1 calc PR A 2 C4A C 0.7411(10) 0.8650(4) 0.6312(4) 0.0261(15) Uani 0.515(7) 1 d PD A 1 H4AA H 0.7707 0.8318 0.5958 0.031 Uiso 0.515(7) 1 calc PR A 1 H4AB H 0.6197 0.8850 0.6178 0.031 Uiso 0.515(7) 1 calc PR A 1 C4B C 0.6736(13) 0.8823(4) 0.6264(4) 0.034(2) Uani 0.485(7) 1 d PD A 2 H4BA H 0.5828 0.9217 0.6139 0.041 Uiso 0.485(7) 1 calc PR A 2 H4BB H 0.6768 0.8509 0.5868 0.041 Uiso 0.485(7) 1 calc PR A 2 C5 C 0.8638(6) 0.9248(2) 0.64112(19) 0.0443(9) Uani 1 1 d D . . H5A H 0.8451 0.9531 0.6804 0.066 Uiso 1 1 calc R A 1 H5B H 0.8464 0.9582 0.6028 0.066 Uiso 1 1 calc R A 1 H5C H 0.9851 0.9047 0.6470 0.066 Uiso 1 1 calc R A 1 C6 C 0.2275(4) 0.84471(17) 0.87371(13) 0.0228(5) Uani 1 1 d . . . C7 C 0.2647(5) 0.8865(2) 0.81124(17) 0.0405(9) Uani 1 1 d . . . H7A H 0.3600 0.9233 0.8231 0.061 Uiso 1 1 calc R . . H7B H 0.1566 0.9124 0.7910 0.061 Uiso 1 1 calc R . . H7C H 0.3012 0.8501 0.7800 0.061 Uiso 1 1 calc R . . C8 C 0.0864(4) 0.7842(2) 0.85239(15) 0.0302(7) Uani 1 1 d . . . H8A H 0.1323 0.7485 0.8227 0.045 Uiso 1 1 calc R . . H8B H -0.0217 0.8081 0.8297 0.045 Uiso 1 1 calc R . . H8C H 0.0587 0.7574 0.8912 0.045 Uiso 1 1 calc R . . C9 C 0.1557(4) 0.90259(17) 0.91888(16) 0.0269(6) Uani 1 1 d . . . H9A H 0.1363 0.8780 0.9599 0.040 Uiso 1 1 calc R . . H9B H 0.0430 0.9232 0.8968 0.040 Uiso 1 1 calc R . . H9C H 0.2423 0.9434 0.9288 0.040 Uiso 1 1 calc R . . C10 C 0.5951(4) 0.85364(16) 0.96549(15) 0.0242(6) Uani 1 1 d . . . C11 C 0.7609(4) 0.80468(19) 0.98651(16) 0.0282(6) Uani 1 1 d . . . H11A H 0.7286 0.7615 1.0119 0.042 Uiso 1 1 calc R . . H11B H 0.8520 0.8346 1.0137 0.042 Uiso 1 1 calc R . . H11C H 0.8076 0.7868 0.9473 0.042 Uiso 1 1 calc R . . C12 C 0.5263(4) 0.8801(2) 1.02841(18) 0.0379(8) Uani 1 1 d . . . H12A H 0.4210 0.9118 1.0166 0.057 Uiso 1 1 calc R . . H12B H 0.6194 0.9090 1.0556 0.057 Uiso 1 1 calc R . . H12C H 0.4948 0.8362 1.0531 0.057 Uiso 1 1 calc R . . C13 C 0.6456(5) 0.92141(18) 0.9259(2) 0.0410(9) Uani 1 1 d . . . H13A H 0.6842 0.9038 0.8851 0.061 Uiso 1 1 calc R . . H13B H 0.7427 0.9493 0.9519 0.061 Uiso 1 1 calc R . . H13C H 0.5422 0.9545 0.9153 0.061 Uiso 1 1 calc R . . C14 C 0.3684(3) 0.71691(14) 0.96080(12) 0.0155(4) Uani 1 1 d . . . C15 C 0.2566(4) 0.73469(15) 1.00738(13) 0.0195(5) Uani 1 1 d . . . H15 H 0.2291 0.7859 1.0144 0.023 Uiso 1 1 calc R . . C16 C 0.1857(4) 0.67923(17) 1.04331(14) 0.0256(6) Uani 1 1 d . . . H16 H 0.1112 0.6927 1.0747 0.031 Uiso 1 1 calc R . . C17 C 0.2236(4) 0.60452(18) 1.03351(16) 0.0309(7) Uani 1 1 d . . . H17 H 0.1741 0.5663 1.0575 0.037 Uiso 1 1 calc R . . C18 C 0.3351(4) 0.58587(17) 0.98800(16) 0.0266(6) Uani 1 1 d . . . H18 H 0.3605 0.5344 0.9811 0.032 Uiso 1 1 calc R . . C19 C 0.4109(3) 0.64103(15) 0.95215(13) 0.0182(5) Uani 1 1 d . . . C20 C 0.5334(4) 0.61172(15) 0.90738(13) 0.0208(5) Uani 1 1 d . . . C21 C 0.4623(4) 0.57341(18) 0.85042(17) 0.0313(7) Uani 1 1 d . . . H21 H 0.3370 0.5692 0.8389 0.038 Uiso 1 1 calc R . . C22 C 0.5753(5) 0.5411(2) 0.81018(18) 0.0386(8) Uani 1 1 d . . . H22 H 0.5262 0.5146 0.7716 0.046 Uiso 1 1 calc R . . C23 C 0.7569(5) 0.54747(18) 0.82614(17) 0.0336(7) Uani 1 1 d . . . H23 H 0.8326 0.5263 0.7981 0.040 Uiso 1 1 calc R . . C24 C 0.8292(4) 0.58445(17) 0.88263(16) 0.0279(6) Uani 1 1 d . . . H24 H 0.9546 0.5887 0.8936 0.033 Uiso 1 1 calc R . . C25 C 0.7176(4) 0.61583(16) 0.92399(15) 0.0232(5) Uani 1 1 d . . . H25 H 0.7680 0.6400 0.9636 0.028 Uiso 1 1 calc R . . Sb2 Sb 0.09681(3) 0.603574(11) 0.669522(9) 0.02472(5) Uani 1 1 d . . . F1 F 0.0414(5) 0.70200(13) 0.64097(16) 0.0858(11) Uani 1 1 d . . . F2 F 0.0872(4) 0.63324(16) 0.75623(11) 0.0661(8) Uani 1 1 d . . . F3 F 0.3381(4) 0.6253(2) 0.67820(13) 0.0827(11) Uani 1 1 d . . . F4 F 0.0990(3) 0.57581(13) 0.58228(8) 0.0356(4) Uani 1 1 d . . . F5 F -0.1463(3) 0.58283(14) 0.66177(11) 0.0428(5) Uani 1 1 d . . . F6 F 0.1485(3) 0.50576(12) 0.69821(10) 0.0403(5) 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 Au1 0.01882(4) 0.01851(5) 0.01567(4) 0.00143(3) 0.00824(3) 0.00224(4) P1 0.0161(3) 0.0130(3) 0.0163(3) 0.0009(2) 0.0073(2) 0.0004(2) N1 0.0251(12) 0.0278(13) 0.0188(10) -0.0016(9) 0.0092(9) 0.0005(10) C2A 0.011(2) 0.021(3) 0.011(2) -0.0002(18) -0.0004(16) -0.005(2) C2B 0.046(5) 0.035(4) 0.017(3) 0.003(2) 0.014(3) 0.011(3) C3A 0.020(2) 0.012(2) 0.0117(19) -0.0009(15) 0.0027(16) -0.0009(16) C3B 0.030(3) 0.034(4) 0.028(3) 0.003(3) 0.007(2) 0.003(3) C4A 0.035(4) 0.020(4) 0.026(3) 0.006(2) 0.011(3) 0.011(3) C4B 0.079(7) 0.011(3) 0.017(3) 0.000(2) 0.018(4) 0.004(4) C5 0.055(2) 0.043(2) 0.0348(18) -0.0044(16) 0.0066(16) 0.0168(18) C6 0.0240(13) 0.0264(14) 0.0198(12) 0.0066(10) 0.0088(10) 0.0095(11) C7 0.0436(19) 0.050(2) 0.0320(16) 0.0231(15) 0.0199(14) 0.0256(17) C8 0.0204(13) 0.046(2) 0.0227(13) -0.0058(13) -0.0012(10) 0.0070(13) C9 0.0277(14) 0.0217(14) 0.0342(15) 0.0043(11) 0.0143(12) 0.0082(11) C10 0.0187(12) 0.0219(13) 0.0341(15) -0.0113(11) 0.0103(11) -0.0050(10) C11 0.0194(12) 0.0330(16) 0.0325(15) -0.0115(12) 0.0052(11) -0.0037(11) C12 0.0245(14) 0.047(2) 0.0441(19) -0.0303(16) 0.0109(13) -0.0080(13) C13 0.0347(17) 0.0172(14) 0.077(3) -0.0071(16) 0.0273(18) -0.0073(13) C14 0.0150(10) 0.0163(12) 0.0160(10) 0.0024(8) 0.0048(8) -0.0002(9) C15 0.0196(11) 0.0200(13) 0.0198(11) 0.0030(9) 0.0059(9) 0.0022(9) C16 0.0265(13) 0.0296(15) 0.0245(13) 0.0075(11) 0.0161(11) 0.0039(11) C17 0.0334(15) 0.0257(15) 0.0382(16) 0.0154(13) 0.0203(13) 0.0038(12) C18 0.0284(14) 0.0190(13) 0.0351(15) 0.0048(11) 0.0136(12) 0.0027(11) C19 0.0182(11) 0.0158(12) 0.0220(11) 0.0026(9) 0.0075(9) 0.0015(9) C20 0.0257(13) 0.0149(12) 0.0240(12) 0.0012(9) 0.0108(10) 0.0014(10) C21 0.0322(15) 0.0261(15) 0.0383(17) -0.0107(13) 0.0144(13) -0.0055(12) C22 0.052(2) 0.0283(17) 0.0395(18) -0.0142(14) 0.0216(16) -0.0041(15) C23 0.0459(19) 0.0201(14) 0.0409(17) 0.0010(12) 0.0268(15) 0.0079(13) C24 0.0282(14) 0.0219(14) 0.0368(16) 0.0057(12) 0.0159(12) 0.0081(11) C25 0.0254(13) 0.0180(13) 0.0279(13) 0.0036(10) 0.0097(10) 0.0054(10) Sb2 0.03402(10) 0.02245(9) 0.02035(8) -0.00493(7) 0.01287(7) -0.00813(8) F1 0.162(3) 0.0210(12) 0.094(2) 0.0073(13) 0.083(2) 0.0050(15) F2 0.097(2) 0.0743(18) 0.0340(12) -0.0340(12) 0.0340(13) -0.0411(16) F3 0.0509(15) 0.152(3) 0.0457(15) -0.0081(17) 0.0105(12) -0.0645(18) F4 0.0430(11) 0.0489(12) 0.0161(8) 0.0000(7) 0.0088(7) 0.0120(9) F5 0.0288(10) 0.0599(15) 0.0421(12) 0.0128(10) 0.0129(8) 0.0098(10) F6 0.0454(12) 0.0421(12) 0.0342(10) 0.0131(9) 0.0089(9) 0.0154(10) _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 Au1 P1 2.2555(6) . ? Au1 N1 2.097(2) . ? P1 C6 1.888(3) . ? P1 C10 1.866(3) . ? P1 C14 1.835(3) . ? N1 H1A 0.84(4) . ? N1 H1B 0.83(5) . ? N1 C2A 1.449(6) . ? N1 C2B 1.573(8) . ? C2A H2AA 0.9900 . ? C2A H2AB 0.9900 . ? C2A C3A 1.542(7) . ? C2B H2BA 0.9900 . ? C2B H2BB 0.9900 . ? C2B C3B 1.475(9) . ? C3A H3AA 0.9900 . ? C3A H3AB 0.9900 . ? C3A C4A 1.504(8) . ? C3B H3BA 0.9900 . ? C3B H3BB 0.9900 . ? C3B C4B 1.556(8) . ? C4A H4AA 0.9900 . ? C4A H4AB 0.9900 . ? C4A C5 1.409(8) . ? C4B H4BA 0.9900 . ? C4B H4BB 0.9900 . ? C4B C5 1.619(9) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.546(4) . ? C6 C8 1.536(5) . ? C6 C9 1.539(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.540(4) . ? C10 C12 1.539(4) . ? C10 C13 1.535(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.407(4) . ? C14 C19 1.404(4) . ? C15 H15 0.9500 . ? C15 C16 1.388(4) . ? C16 H16 0.9500 . ? C16 C17 1.380(4) . ? C17 H17 0.9500 . ? C17 C18 1.393(4) . ? C18 H18 0.9500 . ? C18 C19 1.401(4) . ? C19 C20 1.497(4) . ? C20 C21 1.393(4) . ? C20 C25 1.393(4) . ? C21 H21 0.9500 . ? C21 C22 1.401(4) . ? C22 H22 0.9500 . ? C22 C23 1.375(5) . ? C23 H23 0.9500 . ? C23 C24 1.377(5) . ? C24 H24 0.9500 . ? C24 C25 1.402(4) . ? C25 H25 0.9500 . ? Sb2 F1 1.873(3) . ? Sb2 F2 1.872(2) . ? Sb2 F3 1.857(2) . ? Sb2 F4 1.8636(17) . ? Sb2 F5 1.868(2) . ? Sb2 F6 1.859(2) . ? 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 N1 Au1 P1 175.22(8) . . ? C6 P1 Au1 106.67(9) . . ? C10 P1 Au1 111.77(9) . . ? C10 P1 C6 113.32(14) . . ? C14 P1 Au1 111.24(8) . . ? C14 P1 C6 106.94(12) . . ? C14 P1 C10 106.84(13) . . ? Au1 N1 H1A 107(3) . . ? Au1 N1 H1B 110(3) . . ? H1A N1 H1B 110(4) . . ? C2A N1 Au1 118.8(3) . . ? C2A N1 H1A 119(3) . . ? C2A N1 H1B 92(3) . . ? C2A N1 C2B 29.2(3) . . ? C2B N1 Au1 116.1(3) . . ? C2B N1 H1A 95(3) . . ? C2B N1 H1B 117(3) . . ? N1 C2A H2AA 110.3 . . ? N1 C2A H2AB 110.3 . . ? N1 C2A C3A 107.2(4) . . ? H2AA C2A H2AB 108.5 . . ? C3A C2A H2AA 110.3 . . ? C3A C2A H2AB 110.3 . . ? N1 C2B H2BA 108.4 . . ? N1 C2B H2BB 108.4 . . ? H2BA C2B H2BB 107.5 . . ? C3B C2B N1 115.4(6) . . ? C3B C2B H2BA 108.4 . . ? C3B C2B H2BB 108.4 . . ? C2A C3A H3AA 109.7 . . ? C2A C3A H3AB 109.7 . . ? H3AA C3A H3AB 108.2 . . ? C4A C3A C2A 109.7(4) . . ? C4A C3A H3AA 109.7 . . ? C4A C3A H3AB 109.7 . . ? C2B C3B H3BA 109.6 . . ? C2B C3B H3BB 109.6 . . ? C2B C3B C4B 110.2(6) . . ? H3BA C3B H3BB 108.1 . . ? C4B C3B H3BA 109.6 . . ? C4B C3B H3BB 109.6 . . ? C3A C4A H4AA 109.8 . . ? C3A C4A H4AB 109.8 . . ? H4AA C4A H4AB 108.2 . . ? C5 C4A C3A 109.5(6) . . ? C5 C4A H4AA 109.8 . . ? C5 C4A H4AB 109.8 . . ? C3B C4B H4BA 106.7 . . ? C3B C4B H4BB 106.7 . . ? C3B C4B C5 122.4(6) . . ? H4BA C4B H4BB 106.6 . . ? C5 C4B H4BA 106.7 . . ? C5 C4B H4BB 106.7 . . ? C4A C5 C4B 21.2(3) . . ? C4A C5 H5A 109.5 . . ? C4A C5 H5B 109.5 . . ? C4A C5 H5C 109.5 . . ? C4B C5 H5A 99.2 . . ? C4B C5 H5B 97.0 . . ? C4B C5 H5C 130.6 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 P1 108.35(19) . . ? C8 C6 P1 106.7(2) . . ? C8 C6 C7 107.7(3) . . ? C8 C6 C9 110.2(2) . . ? C9 C6 P1 115.8(2) . . ? C9 C6 C7 107.8(3) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 P1 105.99(19) . . ? C12 C10 P1 114.8(2) . . ? C12 C10 C11 107.6(3) . . ? C13 C10 P1 108.4(2) . . ? C13 C10 C11 109.5(2) . . ? C13 C10 C12 110.5(3) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 P1 118.0(2) . . ? C19 C14 P1 123.45(18) . . ? C19 C14 C15 118.4(2) . . ? C14 C15 H15 119.2 . . ? C16 C15 C14 121.6(3) . . ? C16 C15 H15 119.2 . . ? C15 C16 H16 120.0 . . ? C17 C16 C15 120.0(2) . . ? C17 C16 H16 120.0 . . ? C16 C17 H17 120.4 . . ? C16 C17 C18 119.2(3) . . ? C18 C17 H17 120.4 . . ? C17 C18 H18 119.1 . . ? C17 C18 C19 121.7(3) . . ? C19 C18 H18 119.1 . . ? C14 C19 C20 126.0(2) . . ? C18 C19 C14 119.0(2) . . ? C18 C19 C20 115.0(2) . . ? C21 C20 C19 119.2(3) . . ? C25 C20 C19 121.7(3) . . ? C25 C20 C21 118.9(3) . . ? C20 C21 H21 119.9 . . ? C20 C21 C22 120.1(3) . . ? C22 C21 H21 119.9 . . ? C21 C22 H22 119.8 . . ? C23 C22 C21 120.4(3) . . ? C23 C22 H22 119.8 . . ? C22 C23 H23 119.9 . . ? C22 C23 C24 120.1(3) . . ? C24 C23 H23 119.9 . . ? C23 C24 H24 120.0 . . ? C23 C24 C25 120.0(3) . . ? C25 C24 H24 120.0 . . ? C20 C25 C24 120.4(3) . . ? C20 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? F2 Sb2 F1 89.83(14) . . ? F3 Sb2 F1 90.49(17) . . ? F3 Sb2 F2 91.53(12) . . ? F3 Sb2 F4 89.91(11) . . ? F3 Sb2 F5 179.10(14) . . ? F3 Sb2 F6 90.28(14) . . ? F4 Sb2 F1 88.79(11) . . ? F4 Sb2 F2 178.01(12) . . ? F4 Sb2 F5 90.86(10) . . ? F5 Sb2 F1 89.07(14) . . ? F5 Sb2 F2 87.68(11) . . ? F6 Sb2 F1 179.17(12) . . ? F6 Sb2 F2 89.84(12) . . ? F6 Sb2 F4 91.51(9) . . ? F6 Sb2 F5 90.15(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1B F3 0.83(5) 2.15(5) 2.936(4) 157(4) . _database_code_depnum_ccdc_archive 'CCDC 914708'