# Electronic Supplementary Material (ESI) for Catalysis Science & Technology # 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_chbo489 #TrackingRef 'web_deposit_cif_file_0_AntonioM.Echavarren_1365746154.CHBO489.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H61 Au Cl4 O3 P' _chemical_formula_weight 1163.79 _chemical_absolute_configuration ad 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' Cl Cl 0.1484 0.1585 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.0107(6) _cell_length_b 22.8169(16) _cell_length_c 25.9541(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5336.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6620 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 23.10 _exptl_crystal_description Plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.00 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2356 _exptl_absorpt_coefficient_mu 3.029 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7515 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_support 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47713 _diffrn_reflns_av_R_equivalents 0.1095 _diffrn_reflns_av_sigmaI/netI 0.1080 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 27.12 _reflns_number_total 11307 _reflns_number_gt 8939 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius Apex v1.0-22 2002' _computing_cell_refinement 'Bruker-Nonius Apex v1.0-22 2002' _computing_data_reduction 'SAINT+ Version 7.06A Bruker-Nonius, 2004' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+5.5987P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.005(7) _refine_ls_number_reflns 11307 _refine_ls_number_parameters 595 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0834 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1164 _refine_ls_wR_factor_gt 0.1045 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au -0.16026(4) 1.058508(10) 0.243726(8) 0.02300(7) Uani 1 1 d . . . P1 P -0.0015(3) 0.99884(6) 0.20682(6) 0.0203(4) Uani 1 1 d . . . O1 O 0.0007(6) 0.92881(15) 0.21225(16) 0.0215(12) Uani 1 1 d . . . C1 C -0.1187(8) 0.8970(2) 0.1918(2) 0.0184(17) Uani 1 1 d . . . Cl1 Cl -0.3147(3) 1.12996(8) 0.27313(7) 0.0394(6) Uani 1 1 d . . . O2 O -0.0205(6) 1.00895(17) 0.14711(16) 0.0218(12) Uani 1 1 d . . . C2 C -0.2107(8) 0.8668(3) 0.2283(2) 0.0192(17) Uani 1 1 d . . . C3 C -0.3285(11) 0.8365(2) 0.2088(2) 0.0247(17) Uani 1 1 d . . . H3A H -0.3885 0.8141 0.2316 0.030 Uiso 1 1 calc R . . O3 O 0.1655(8) 1.01066(17) 0.22019(16) 0.0282(12) Uani 1 1 d . . . C4 C -0.3643(10) 0.8373(2) 0.1553(2) 0.0233(18) Uani 1 1 d . . . C5 C -0.4951(10) 0.8113(3) 0.1374(3) 0.0293(19) Uani 1 1 d . . . H5A H -0.5570 0.7905 0.1607 0.035 Uiso 1 1 calc R . . C6 C -0.5350(10) 0.8153(3) 0.0865(3) 0.0274(19) Uani 1 1 d . . . H6A H -0.6249 0.7981 0.0748 0.033 Uiso 1 1 calc R . . C7 C -0.4430(10) 0.8450(3) 0.0519(3) 0.0239(18) Uani 1 1 d . . . H7A H -0.4725 0.8486 0.0169 0.029 Uiso 1 1 calc R . . C8 C -0.3110(10) 0.8689(3) 0.0675(2) 0.0232(19) Uani 1 1 d . . . H8A H -0.2481 0.8876 0.0432 0.028 Uiso 1 1 calc R . . C9 C -0.2682(9) 0.8655(2) 0.1205(2) 0.0203(16) Uani 1 1 d . . . C10 C -0.1342(9) 0.8932(2) 0.1392(2) 0.0185(17) Uani 1 1 d . . . C11 C -0.0160(9) 0.9161(2) 0.1041(2) 0.0171(15) Uani 1 1 d . . . C12 C 0.0467(9) 0.8795(3) 0.0645(2) 0.0206(17) Uani 1 1 d . . . C13 C 0.0155(9) 0.8197(3) 0.0598(2) 0.0243(17) Uani 1 1 d . . . H13A H -0.0495 0.8017 0.0839 0.029 Uiso 1 1 calc R . . C14 C 0.0765(10) 0.7863(3) 0.0211(2) 0.0250(18) Uani 1 1 d . . . H14A H 0.0527 0.7458 0.0186 0.030 Uiso 1 1 calc R . . C15 C 0.1751(10) 0.8121(3) -0.0150(2) 0.0262(17) Uani 1 1 d . . . H15A H 0.2142 0.7892 -0.0423 0.031 Uiso 1 1 calc R . . C16 C 0.2142(9) 0.8697(3) -0.0105(3) 0.0258(18) Uani 1 1 d . . . H16A H 0.2828 0.8864 -0.0341 0.031 Uiso 1 1 calc R . . C17 C 0.1515(11) 0.9049(3) 0.0297(2) 0.0256(17) Uani 1 1 d . . . C18 C 0.1979(9) 0.9636(3) 0.0363(2) 0.0215(19) Uani 1 1 d . . . H18A H 0.2650 0.9801 0.0121 0.026 Uiso 1 1 calc R . . C19 C 0.1491(10) 0.9976(2) 0.0766(2) 0.0190(15) Uani 1 1 d . . . C20 C 0.0408(9) 0.9721(3) 0.1086(2) 0.0201(17) Uani 1 1 d . . . C21 C -0.1646(11) 0.8655(2) 0.2833(2) 0.0228(15) Uani 1 1 d . . . C22 C -0.0446(11) 0.8291(3) 0.2978(3) 0.033(2) Uani 1 1 d . . . C23 C 0.0027(13) 0.8310(4) 0.3492(3) 0.050(3) Uani 1 1 d . . . H23A H 0.0840 0.8072 0.3594 0.060 Uiso 1 1 calc R . . C24 C -0.0655(12) 0.8668(4) 0.3861(3) 0.045(3) Uani 1 1 d . . . C25 C -0.1873(12) 0.8993(3) 0.3702(3) 0.0389(18) Uani 1 1 d U . . H25A H -0.2387 0.9221 0.3951 0.047 Uiso 1 1 calc R . . C26 C -0.2370(11) 0.9002(3) 0.3200(3) 0.033(2) Uani 1 1 d . . . C27 C 0.0267(11) 0.7873(3) 0.2600(4) 0.045(2) Uani 1 1 d . . . H27A H -0.0185 0.7955 0.2255 0.054 Uiso 1 1 calc R . . C28 C 0.1928(17) 0.7961(5) 0.2542(5) 0.088(3) Uani 1 1 d U . . H28A H 0.2319 0.7680 0.2291 0.132 Uiso 1 1 calc R . . H28B H 0.2412 0.7899 0.2876 0.132 Uiso 1 1 calc R . . H28C H 0.2125 0.8361 0.2422 0.132 Uiso 1 1 calc R . . C29 C -0.0076(16) 0.7240(4) 0.2725(4) 0.067(3) Uani 1 1 d U . . H29A H 0.0411 0.6984 0.2473 0.100 Uiso 1 1 calc R . . H29B H -0.1152 0.7177 0.2712 0.100 Uiso 1 1 calc R . . H29C H 0.0290 0.7148 0.3071 0.100 Uiso 1 1 calc R . . C30 C -0.0082(16) 0.8735(4) 0.4415(4) 0.062(2) Uani 1 1 d U . . C31 C 0.1227(14) 0.9132(4) 0.4433(4) 0.064(4) Uani 1 1 d . . . H31A H 0.1609 0.9151 0.4786 0.096 Uiso 1 1 calc R . . H31B H 0.0931 0.9526 0.4320 0.096 Uiso 1 1 calc R . . H31C H 0.2002 0.8982 0.4203 0.096 Uiso 1 1 calc R . . C32 C 0.004(2) 0.8216(6) 0.4688(6) 0.103(4) Uani 1 1 d U . . H32A H 0.0461 0.8296 0.5029 0.155 Uiso 1 1 calc R . . H32B H 0.0691 0.7945 0.4501 0.155 Uiso 1 1 calc R . . H32C H -0.0944 0.8039 0.4728 0.155 Uiso 1 1 calc R . . C33 C -0.3712(11) 0.9375(3) 0.3071(3) 0.039(2) Uani 1 1 d . . . H33A H -0.3605 0.9503 0.2704 0.047 Uiso 1 1 calc R . . C34 C -0.3820(12) 0.9932(4) 0.3402(3) 0.046(2) Uani 1 1 d U . . H34A H -0.2890 1.0153 0.3376 0.069 Uiso 1 1 calc R . . H34B H -0.3995 0.9822 0.3762 0.069 Uiso 1 1 calc R . . H34C H -0.4643 1.0175 0.3279 0.069 Uiso 1 1 calc R . . C35 C -0.5150(14) 0.9039(3) 0.3112(4) 0.052(3) Uani 1 1 d . . . H35A H -0.5086 0.8682 0.2904 0.079 Uiso 1 1 calc R . . H35B H -0.5968 0.9283 0.2986 0.079 Uiso 1 1 calc R . . H35C H -0.5330 0.8935 0.3473 0.079 Uiso 1 1 calc R . . C36 C 0.2114(8) 1.0572(3) 0.0876(2) 0.0220(16) Uani 1 1 d . . . C37 C 0.3577(9) 1.0624(3) 0.1061(2) 0.0213(15) Uani 1 1 d . . . C38 C 0.4099(10) 1.1188(3) 0.1194(3) 0.0244(17) Uani 1 1 d . . . H38A H 0.5087 1.1230 0.1316 0.029 Uiso 1 1 calc R . . C39 C 0.3206(11) 1.1684(3) 0.1150(3) 0.030(2) Uani 1 1 d . . . C40 C 0.1805(11) 1.1621(3) 0.0958(3) 0.031(2) Uani 1 1 d . . . H40A H 0.1213 1.1962 0.0913 0.037 Uiso 1 1 calc R . . C41 C 0.1200(9) 1.1075(3) 0.0824(3) 0.025(2) Uani 1 1 d . . . C42 C 0.4628(10) 1.0109(3) 0.1112(3) 0.0255(19) Uani 1 1 d . . . H42A H 0.4065 0.9745 0.1024 0.031 Uiso 1 1 calc R . . C43 C 0.5241(11) 1.0038(3) 0.1656(3) 0.039(2) Uani 1 1 d . . . H43A H 0.5915 0.9701 0.1667 0.059 Uiso 1 1 calc R . . H43B H 0.4420 0.9975 0.1897 0.059 Uiso 1 1 calc R . . H43C H 0.5783 1.0394 0.1754 0.059 Uiso 1 1 calc R . . C44 C 0.5873(12) 1.0173(3) 0.0728(4) 0.051(3) Uani 1 1 d . . . H44A H 0.5459 1.0217 0.0381 0.076 Uiso 1 1 calc R . . H44B H 0.6505 0.9823 0.0740 0.076 Uiso 1 1 calc R . . H44C H 0.6466 1.0519 0.0813 0.076 Uiso 1 1 calc R . . C45 C 0.3808(11) 1.2286(3) 0.1313(3) 0.037(2) Uani 1 1 d . . . H45A H 0.2905 1.2527 0.1387 0.045 Uiso 1 1 calc R . . C46 C 0.4632(13) 1.2277(4) 0.1798(4) 0.052(2) Uani 1 1 d U . . H46A H 0.4975 1.2674 0.1879 0.078 Uiso 1 1 calc R . . H46B H 0.5490 1.2015 0.1765 0.078 Uiso 1 1 calc R . . H46C H 0.3985 1.2136 0.2075 0.078 Uiso 1 1 calc R . . C47 C 0.4534(17) 1.2581(5) 0.0893(5) 0.074(3) Uani 1 1 d U . . H47A H 0.4893 1.2964 0.1010 0.110 Uiso 1 1 calc R . . H47B H 0.3830 1.2635 0.0610 0.110 Uiso 1 1 calc R . . H47C H 0.5376 1.2345 0.0774 0.110 Uiso 1 1 calc R . . C48 C -0.0354(11) 1.1041(3) 0.0583(3) 0.033(2) Uani 1 1 d . . . H48A H -0.0746 1.0638 0.0650 0.040 Uiso 1 1 calc R . . C49 C -0.1433(17) 1.1468(4) 0.0816(4) 0.066(3) Uani 1 1 d U . . H49A H -0.1470 1.1411 0.1190 0.099 Uiso 1 1 calc R . . H49B H -0.2421 1.1404 0.0669 0.099 Uiso 1 1 calc R . . H49C H -0.1109 1.1870 0.0740 0.099 Uiso 1 1 calc R . . C50 C -0.0263(18) 1.1116(5) 0.0001(5) 0.077(3) Uani 1 1 d U . . H50A H -0.1263 1.1094 -0.0147 0.116 Uiso 1 1 calc R . . H50B H 0.0355 1.0804 -0.0145 0.116 Uiso 1 1 calc R . . H50C H 0.0176 1.1498 -0.0080 0.116 Uiso 1 1 calc R . . C51 C 0.2079(9) 1.0438(2) 0.2635(3) 0.0250(18) Uani 1 1 d . . . C52 C 0.2712(9) 1.0978(3) 0.2567(3) 0.0310(18) Uani 1 1 d . . . H52A H 0.2819 1.1135 0.2230 0.037 Uiso 1 1 calc R . . C53 C 0.3198(12) 1.1296(3) 0.2990(3) 0.041(2) Uani 1 1 d . . . H53A H 0.3672 1.1664 0.2945 0.049 Uiso 1 1 calc R . . C54 C 0.2987(12) 1.1071(3) 0.3474(3) 0.044(3) Uani 1 1 d . . . H54A H 0.3312 1.1289 0.3765 0.053 Uiso 1 1 calc R . . C55 C 0.2310(12) 1.0534(4) 0.3549(3) 0.044(2) Uani 1 1 d . . . H55A H 0.2160 1.0389 0.3888 0.053 Uiso 1 1 calc R . . C56 C 0.1848(11) 1.0207(3) 0.3124(3) 0.032(2) Uani 1 1 d . . . H56A H 0.1388 0.9836 0.3168 0.039 Uiso 1 1 calc R . . Cl1S Cl -0.3346(4) 1.15730(9) 0.43190(8) 0.0494(6) Uani 1 1 d . . . Cl2S Cl -0.1226(3) 1.06231(10) 0.43522(9) 0.0572(7) Uani 1 1 d . . . Cl3S Cl -0.0441(4) 1.17090(10) 0.38499(10) 0.0579(7) Uani 1 1 d . . . C1S C -0.1918(12) 1.1216(3) 0.3984(3) 0.040(3) Uani 1 1 d . . . H1SA H -0.2321 1.1062 0.3652 0.049 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 0.02793(16) 0.02314(10) 0.01792(10) -0.00238(9) 0.00116(11) -0.00068(12) P1 0.0260(14) 0.0179(7) 0.0171(8) -0.0029(6) 0.0012(8) -0.0047(7) O1 0.030(4) 0.016(2) 0.018(2) 0.0002(15) -0.004(2) -0.0060(19) C1 0.018(5) 0.014(3) 0.023(3) -0.005(2) 0.002(3) 0.000(2) Cl1 0.0473(18) 0.0362(9) 0.0348(9) -0.0050(7) 0.0035(9) 0.0139(9) O2 0.031(4) 0.019(2) 0.016(2) -0.0026(16) 0.006(2) 0.001(2) C2 0.022(5) 0.019(3) 0.016(3) 0.001(2) 0.009(3) 0.001(2) C3 0.033(5) 0.021(3) 0.020(3) 0.001(2) 0.006(3) -0.011(3) O3 0.039(4) 0.023(2) 0.022(2) -0.0080(16) 0.000(3) -0.004(2) C4 0.028(6) 0.018(3) 0.024(3) -0.002(2) -0.002(3) -0.005(3) C5 0.036(6) 0.026(3) 0.026(4) -0.002(3) 0.002(3) -0.005(3) C6 0.027(6) 0.031(3) 0.025(4) -0.003(3) -0.003(3) -0.007(3) C7 0.039(6) 0.015(3) 0.018(3) -0.005(2) 0.000(3) 0.000(3) C8 0.031(6) 0.022(3) 0.016(3) -0.005(2) 0.001(3) 0.001(3) C9 0.024(5) 0.016(3) 0.021(3) 0.000(2) 0.002(3) -0.006(3) C10 0.022(6) 0.015(3) 0.018(3) -0.001(2) -0.002(3) 0.002(3) C11 0.018(5) 0.015(3) 0.019(3) -0.004(2) 0.001(3) 0.000(3) C12 0.028(6) 0.023(3) 0.011(3) 0.000(2) 0.001(3) -0.001(3) C13 0.031(6) 0.026(3) 0.015(3) -0.005(2) -0.001(3) -0.007(3) C14 0.032(6) 0.026(3) 0.017(3) -0.003(2) -0.011(3) -0.001(3) C15 0.031(6) 0.030(3) 0.018(3) -0.007(2) -0.003(3) 0.007(3) C16 0.023(6) 0.032(3) 0.022(3) -0.006(3) 0.003(3) -0.004(3) C17 0.035(6) 0.024(3) 0.017(3) -0.001(2) -0.005(4) -0.005(3) C18 0.020(6) 0.026(3) 0.018(3) 0.004(2) 0.004(3) -0.009(3) C19 0.025(5) 0.018(3) 0.013(3) 0.002(2) -0.005(3) -0.001(3) C20 0.024(5) 0.019(3) 0.017(3) -0.001(2) 0.004(3) 0.001(3) C21 0.025(5) 0.019(3) 0.024(3) 0.006(2) -0.004(4) -0.011(3) C22 0.036(7) 0.040(4) 0.024(4) 0.013(3) -0.003(3) -0.012(4) C23 0.051(8) 0.055(5) 0.043(5) 0.028(4) -0.014(5) -0.020(5) C24 0.064(8) 0.050(5) 0.019(4) 0.005(3) -0.001(4) -0.034(5) C25 0.041(3) 0.038(2) 0.037(2) 0.0001(17) 0.0007(18) -0.0030(18) C26 0.060(7) 0.023(3) 0.016(3) 0.001(3) 0.006(3) -0.014(3) C27 0.032(6) 0.055(4) 0.048(5) 0.033(4) 0.003(4) 0.010(4) C28 0.087(4) 0.086(3) 0.090(4) -0.0004(19) 0.0020(19) -0.0003(19) C29 0.067(3) 0.066(3) 0.068(3) -0.0007(18) 0.0025(19) -0.0020(19) C30 0.062(3) 0.063(3) 0.060(3) 0.0016(18) -0.0025(19) -0.0024(19) C31 0.080(12) 0.074(6) 0.038(5) -0.010(4) -0.027(5) -0.022(6) C32 0.105(4) 0.103(4) 0.102(4) 0.0018(19) -0.0025(19) -0.0019(19) C33 0.059(8) 0.023(3) 0.035(4) -0.004(3) 0.017(4) -0.005(4) C34 0.048(3) 0.043(2) 0.046(3) -0.0017(17) 0.0047(18) -0.0023(18) C35 0.061(9) 0.024(4) 0.073(7) -0.003(4) 0.007(6) 0.007(4) C36 0.037(5) 0.014(2) 0.015(3) 0.003(3) 0.003(2) -0.001(3) C37 0.028(5) 0.023(3) 0.013(3) 0.003(2) 0.001(3) -0.005(3) C38 0.027(5) 0.023(3) 0.024(4) 0.000(3) -0.005(3) -0.006(3) C39 0.045(7) 0.017(3) 0.029(3) 0.000(2) 0.000(4) -0.007(3) C40 0.042(7) 0.021(3) 0.031(4) 0.005(2) -0.004(4) 0.004(3) C41 0.026(6) 0.028(3) 0.021(3) 0.007(3) -0.002(3) -0.008(3) C42 0.033(6) 0.017(3) 0.027(4) -0.008(2) 0.007(3) -0.004(3) C43 0.042(7) 0.046(4) 0.030(4) -0.007(3) -0.012(4) 0.017(4) C44 0.058(8) 0.021(4) 0.073(6) 0.010(4) 0.033(5) 0.013(4) C45 0.061(8) 0.011(3) 0.040(4) -0.001(3) 0.002(4) -0.001(3) C46 0.054(3) 0.049(3) 0.053(3) -0.0015(18) -0.0038(18) -0.0018(18) C47 0.076(3) 0.072(3) 0.073(3) -0.0009(19) 0.0024(19) -0.0044(19) C48 0.038(7) 0.026(3) 0.035(4) 0.009(3) -0.005(4) 0.003(3) C49 0.066(3) 0.063(3) 0.069(3) -0.0020(18) -0.0012(19) -0.0016(19) C50 0.077(3) 0.080(3) 0.075(3) 0.0047(19) -0.0022(19) -0.0021(19) C51 0.027(6) 0.019(3) 0.029(4) -0.003(2) -0.004(3) 0.004(2) C52 0.032(5) 0.028(3) 0.033(4) -0.002(3) 0.003(4) -0.002(3) C53 0.046(7) 0.035(4) 0.041(4) -0.014(3) 0.001(5) -0.012(4) C54 0.058(9) 0.041(4) 0.033(4) -0.015(3) -0.007(4) -0.005(4) C55 0.058(7) 0.046(4) 0.027(4) 0.001(4) 0.003(4) 0.006(5) C56 0.034(7) 0.034(3) 0.029(4) 0.001(3) -0.001(4) 0.001(3) Cl1S 0.0497(18) 0.0569(11) 0.0416(11) -0.0033(8) 0.0031(13) 0.0108(12) Cl2S 0.072(2) 0.0467(11) 0.0529(12) -0.0005(10) -0.0122(11) 0.0108(12) Cl3S 0.059(2) 0.0521(12) 0.0627(15) -0.0106(11) 0.0102(13) -0.0115(12) C1S 0.049(8) 0.043(4) 0.029(4) -0.013(3) -0.013(4) 0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.1948(19) . ? Au1 Cl1 2.275(2) . ? P1 O3 1.568(7) . ? P1 O2 1.576(5) . ? P1 O1 1.604(4) . ? O1 C1 1.403(8) . ? C1 C10 1.374(9) . ? C1 C2 1.436(9) . ? O2 C20 1.418(7) . ? C2 C3 1.364(11) . ? C2 C21 1.487(9) . ? C3 C4 1.427(9) . ? O3 C51 1.407(8) . ? C4 C5 1.400(11) . ? C4 C9 1.406(10) . ? C5 C6 1.372(10) . ? C6 C7 1.397(10) . ? C7 C8 1.370(11) . ? C8 C9 1.431(9) . ? C9 C10 1.447(10) . ? C10 C11 1.497(10) . ? C11 C20 1.381(8) . ? C11 C12 1.439(9) . ? C12 C13 1.398(9) . ? C12 C17 1.430(11) . ? C13 C14 1.376(10) . ? C14 C15 1.420(11) . ? C15 C16 1.365(9) . ? C16 C17 1.433(10) . ? C17 C18 1.415(9) . ? C18 C19 1.374(9) . ? C19 C20 1.407(10) . ? C19 C36 1.499(9) . ? C21 C26 1.400(10) . ? C21 C22 1.414(12) . ? C22 C23 1.402(11) . ? C22 C27 1.512(12) . ? C23 C24 1.400(14) . ? C24 C25 1.389(14) . ? C24 C30 1.536(14) . ? C25 C26 1.377(11) . ? C26 C33 1.516(13) . ? C27 C29 1.513(12) . ? C27 C28 1.518(18) . ? C30 C32 1.386(16) . ? C30 C31 1.488(16) . ? C33 C35 1.509(14) . ? C33 C34 1.537(10) . ? C36 C37 1.407(10) . ? C36 C41 1.420(10) . ? C37 C38 1.414(9) . ? C37 C42 1.515(10) . ? C38 C39 1.393(11) . ? C39 C40 1.365(13) . ? C39 C45 1.536(9) . ? C40 C41 1.403(10) . ? C41 C48 1.536(12) . ? C42 C44 1.508(12) . ? C42 C43 1.526(10) . ? C45 C47 1.439(14) . ? C45 C46 1.461(13) . ? C48 C49 1.504(15) . ? C48 C50 1.521(14) . ? C51 C52 1.370(9) . ? C51 C56 1.391(10) . ? C52 C53 1.388(10) . ? C53 C54 1.371(11) . ? C54 C55 1.382(12) . ? C55 C56 1.394(11) . ? Cl1S C1S 1.754(10) . ? Cl2S C1S 1.769(8) . ? Cl3S C1S 1.777(10) . ? 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 Cl1 171.68(7) . . ? O3 P1 O2 107.3(3) . . ? O3 P1 O1 98.0(3) . . ? O2 P1 O1 103.5(2) . . ? O3 P1 Au1 114.99(17) . . ? O2 P1 Au1 105.5(2) . . ? O1 P1 Au1 126.0(2) . . ? C1 O1 P1 118.2(4) . . ? C10 C1 O1 119.1(6) . . ? C10 C1 C2 124.6(6) . . ? O1 C1 C2 116.2(5) . . ? C20 O2 P1 124.3(4) . . ? C3 C2 C1 116.6(6) . . ? C3 C2 C21 124.3(6) . . ? C1 C2 C21 118.9(7) . . ? C2 C3 C4 122.0(6) . . ? C51 O3 P1 122.0(5) . . ? C5 C4 C9 120.0(6) . . ? C5 C4 C3 120.5(7) . . ? C9 C4 C3 119.5(7) . . ? C6 C5 C4 120.8(7) . . ? C5 C6 C7 119.7(8) . . ? C8 C7 C6 121.2(7) . . ? C7 C8 C9 119.8(7) . . ? C4 C9 C8 118.4(7) . . ? C4 C9 C10 119.9(6) . . ? C8 C9 C10 121.5(6) . . ? C1 C10 C9 116.4(6) . . ? C1 C10 C11 120.7(7) . . ? C9 C10 C11 122.9(5) . . ? C20 C11 C12 116.9(6) . . ? C20 C11 C10 122.3(6) . . ? C12 C11 C10 120.7(5) . . ? C13 C12 C17 118.2(6) . . ? C13 C12 C11 123.4(6) . . ? C17 C12 C11 118.3(5) . . ? C14 C13 C12 121.7(7) . . ? C13 C14 C15 120.0(6) . . ? C16 C15 C14 120.4(6) . . ? C15 C16 C17 119.9(7) . . ? C18 C17 C12 120.2(6) . . ? C18 C17 C16 120.1(7) . . ? C12 C17 C16 119.6(6) . . ? C19 C18 C17 122.1(7) . . ? C18 C19 C20 116.0(6) . . ? C18 C19 C36 122.5(7) . . ? C20 C19 C36 121.4(5) . . ? C11 C20 C19 126.1(6) . . ? C11 C20 O2 117.7(6) . . ? C19 C20 O2 116.2(5) . . ? C26 C21 C22 120.6(6) . . ? C26 C21 C2 120.8(7) . . ? C22 C21 C2 118.6(6) . . ? C23 C22 C21 117.8(8) . . ? C23 C22 C27 120.6(9) . . ? C21 C22 C27 121.6(7) . . ? C24 C23 C22 122.4(10) . . ? C25 C24 C23 117.1(8) . . ? C25 C24 C30 119.3(9) . . ? C23 C24 C30 123.5(10) . . ? C26 C25 C24 123.1(8) . . ? C25 C26 C21 118.9(8) . . ? C25 C26 C33 118.6(7) . . ? C21 C26 C33 122.5(7) . . ? C22 C27 C29 112.1(8) . . ? C22 C27 C28 113.5(9) . . ? C29 C27 C28 110.4(9) . . ? C32 C30 C31 116.3(12) . . ? C32 C30 C24 114.9(10) . . ? C31 C30 C24 110.8(9) . . ? C35 C33 C26 112.6(6) . . ? C35 C33 C34 109.0(7) . . ? C26 C33 C34 112.9(7) . . ? C37 C36 C41 120.5(6) . . ? C37 C36 C19 119.5(6) . . ? C41 C36 C19 119.9(7) . . ? C36 C37 C38 118.1(6) . . ? C36 C37 C42 123.4(6) . . ? C38 C37 C42 118.5(7) . . ? C39 C38 C37 121.8(8) . . ? C40 C39 C38 118.6(6) . . ? C40 C39 C45 121.4(7) . . ? C38 C39 C45 120.0(8) . . ? C39 C40 C41 122.9(7) . . ? C40 C41 C36 118.0(8) . . ? C40 C41 C48 120.0(7) . . ? C36 C41 C48 121.8(6) . . ? C44 C42 C37 109.4(6) . . ? C44 C42 C43 110.6(8) . . ? C37 C42 C43 112.9(5) . . ? C47 C45 C46 115.3(10) . . ? C47 C45 C39 111.8(7) . . ? C46 C45 C39 113.9(6) . . ? C49 C48 C50 111.2(8) . . ? C49 C48 C41 113.1(8) . . ? C50 C48 C41 110.5(8) . . ? C52 C51 C56 121.4(7) . . ? C52 C51 O3 119.6(6) . . ? C56 C51 O3 119.0(6) . . ? C51 C52 C53 119.9(7) . . ? C54 C53 C52 119.2(7) . . ? C53 C54 C55 121.4(7) . . ? C54 C55 C56 119.7(7) . . ? C51 C56 C55 118.3(7) . . ? Cl1S C1S Cl2S 110.3(5) . . ? Cl1S C1S Cl3S 110.6(4) . . ? Cl2S C1S Cl3S 109.0(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Au1 P1 O3 77.5(6) . . . . ? Cl1 Au1 P1 O2 -40.4(7) . . . . ? Cl1 Au1 P1 O1 -160.5(6) . . . . ? O3 P1 O1 C1 -165.1(5) . . . . ? O2 P1 O1 C1 -55.1(5) . . . . ? Au1 P1 O1 C1 65.9(5) . . . . ? P1 O1 C1 C10 70.6(7) . . . . ? P1 O1 C1 C2 -113.9(5) . . . . ? O3 P1 O2 C20 68.9(6) . . . . ? O1 P1 O2 C20 -34.1(6) . . . . ? Au1 P1 O2 C20 -168.0(5) . . . . ? C10 C1 C2 C3 -5.7(10) . . . . ? O1 C1 C2 C3 179.0(6) . . . . ? C10 C1 C2 C21 168.4(6) . . . . ? O1 C1 C2 C21 -6.8(9) . . . . ? C1 C2 C3 C4 -3.6(10) . . . . ? C21 C2 C3 C4 -177.4(7) . . . . ? O2 P1 O3 C51 135.6(4) . . . . ? O1 P1 O3 C51 -117.5(4) . . . . ? Au1 P1 O3 C51 18.6(5) . . . . ? C2 C3 C4 C5 -172.7(7) . . . . ? C2 C3 C4 C9 6.2(11) . . . . ? C9 C4 C5 C6 -3.4(11) . . . . ? C3 C4 C5 C6 175.6(7) . . . . ? C4 C5 C6 C7 1.1(11) . . . . ? C5 C6 C7 C8 1.8(11) . . . . ? C6 C7 C8 C9 -2.3(10) . . . . ? C5 C4 C9 C8 2.8(10) . . . . ? C3 C4 C9 C8 -176.2(6) . . . . ? C5 C4 C9 C10 179.0(6) . . . . ? C3 C4 C9 C10 0.0(10) . . . . ? C7 C8 C9 C4 0.0(9) . . . . ? C7 C8 C9 C10 -176.2(6) . . . . ? O1 C1 C10 C9 -173.3(5) . . . . ? C2 C1 C10 C9 11.6(10) . . . . ? O1 C1 C10 C11 7.6(9) . . . . ? C2 C1 C10 C11 -167.5(6) . . . . ? C4 C9 C10 C1 -8.4(9) . . . . ? C8 C9 C10 C1 167.7(6) . . . . ? C4 C9 C10 C11 170.7(6) . . . . ? C8 C9 C10 C11 -13.2(10) . . . . ? C1 C10 C11 C20 -51.4(10) . . . . ? C9 C10 C11 C20 129.6(7) . . . . ? C1 C10 C11 C12 126.9(7) . . . . ? C9 C10 C11 C12 -52.1(10) . . . . ? C20 C11 C12 C13 170.9(7) . . . . ? C10 C11 C12 C13 -7.4(11) . . . . ? C20 C11 C12 C17 -6.1(10) . . . . ? C10 C11 C12 C17 175.6(7) . . . . ? C17 C12 C13 C14 -3.6(11) . . . . ? C11 C12 C13 C14 179.4(7) . . . . ? C12 C13 C14 C15 0.7(12) . . . . ? C13 C14 C15 C16 2.3(12) . . . . ? C14 C15 C16 C17 -2.1(12) . . . . ? C13 C12 C17 C18 -173.6(7) . . . . ? C11 C12 C17 C18 3.6(11) . . . . ? C13 C12 C17 C16 3.7(11) . . . . ? C11 C12 C17 C16 -179.1(7) . . . . ? C15 C16 C17 C18 176.4(7) . . . . ? C15 C16 C17 C12 -0.9(12) . . . . ? C12 C17 C18 C19 2.2(12) . . . . ? C16 C17 C18 C19 -175.1(7) . . . . ? C17 C18 C19 C20 -5.0(11) . . . . ? C17 C18 C19 C36 172.3(7) . . . . ? C12 C11 C20 C19 3.3(11) . . . . ? C10 C11 C20 C19 -178.3(7) . . . . ? C12 C11 C20 O2 179.5(6) . . . . ? C10 C11 C20 O2 -2.2(10) . . . . ? C18 C19 C20 C11 2.2(12) . . . . ? C36 C19 C20 C11 -175.1(7) . . . . ? C18 C19 C20 O2 -174.0(6) . . . . ? C36 C19 C20 O2 8.7(11) . . . . ? P1 O2 C20 C11 68.1(8) . . . . ? P1 O2 C20 C19 -115.3(6) . . . . ? C3 C2 C21 C26 -80.9(9) . . . . ? C1 C2 C21 C26 105.4(9) . . . . ? C3 C2 C21 C22 100.0(10) . . . . ? C1 C2 C21 C22 -73.7(8) . . . . ? C26 C21 C22 C23 -2.7(11) . . . . ? C2 C21 C22 C23 176.4(7) . . . . ? C26 C21 C22 C27 174.6(7) . . . . ? C2 C21 C22 C27 -6.3(11) . . . . ? C21 C22 C23 C24 0.8(12) . . . . ? C27 C22 C23 C24 -176.5(8) . . . . ? C22 C23 C24 C25 2.3(13) . . . . ? C22 C23 C24 C30 -174.9(8) . . . . ? C23 C24 C25 C26 -3.7(13) . . . . ? C30 C24 C25 C26 173.6(8) . . . . ? C24 C25 C26 C21 1.9(12) . . . . ? C24 C25 C26 C33 -179.9(8) . . . . ? C22 C21 C26 C25 1.4(11) . . . . ? C2 C21 C26 C25 -177.7(7) . . . . ? C22 C21 C26 C33 -176.7(7) . . . . ? C2 C21 C26 C33 4.2(11) . . . . ? C23 C22 C27 C29 67.6(12) . . . . ? C21 C22 C27 C29 -109.6(9) . . . . ? C23 C22 C27 C28 -58.4(11) . . . . ? C21 C22 C27 C28 124.4(10) . . . . ? C25 C24 C30 C32 126.2(12) . . . . ? C23 C24 C30 C32 -56.7(16) . . . . ? C25 C24 C30 C31 -99.6(12) . . . . ? C23 C24 C30 C31 77.5(11) . . . . ? C25 C26 C33 C35 -91.5(9) . . . . ? C21 C26 C33 C35 86.6(9) . . . . ? C25 C26 C33 C34 32.5(10) . . . . ? C21 C26 C33 C34 -149.4(7) . . . . ? C18 C19 C36 C37 -69.4(8) . . . . ? C20 C19 C36 C37 107.8(8) . . . . ? C18 C19 C36 C41 114.3(8) . . . . ? C20 C19 C36 C41 -68.5(8) . . . . ? C41 C36 C37 C38 0.4(9) . . . . ? C19 C36 C37 C38 -175.9(5) . . . . ? C41 C36 C37 C42 -178.2(6) . . . . ? C19 C36 C37 C42 5.5(9) . . . . ? C36 C37 C38 C39 0.4(9) . . . . ? C42 C37 C38 C39 179.1(6) . . . . ? C37 C38 C39 C40 -2.1(11) . . . . ? C37 C38 C39 C45 178.3(6) . . . . ? C38 C39 C40 C41 2.9(11) . . . . ? C45 C39 C40 C41 -177.5(7) . . . . ? C39 C40 C41 C36 -2.1(11) . . . . ? C39 C40 C41 C48 -176.6(7) . . . . ? C37 C36 C41 C40 0.4(9) . . . . ? C19 C36 C41 C40 176.6(6) . . . . ? C37 C36 C41 C48 174.8(6) . . . . ? C19 C36 C41 C48 -8.9(9) . . . . ? C36 C37 C42 C44 112.3(8) . . . . ? C38 C37 C42 C44 -66.3(8) . . . . ? C36 C37 C42 C43 -124.0(7) . . . . ? C38 C37 C42 C43 57.4(9) . . . . ? C40 C39 C45 C47 -90.0(11) . . . . ? C38 C39 C45 C47 89.5(10) . . . . ? C40 C39 C45 C46 137.2(9) . . . . ? C38 C39 C45 C46 -43.3(11) . . . . ? C40 C41 C48 C49 -38.8(10) . . . . ? C36 C41 C48 C49 146.8(7) . . . . ? C40 C41 C48 C50 86.5(9) . . . . ? C36 C41 C48 C50 -87.8(8) . . . . ? P1 O3 C51 C52 -111.0(7) . . . . ? P1 O3 C51 C56 69.2(8) . . . . ? C56 C51 C52 C53 2.8(13) . . . . ? O3 C51 C52 C53 -176.9(8) . . . . ? C51 C52 C53 C54 -2.3(14) . . . . ? C52 C53 C54 C55 0.5(16) . . . . ? C53 C54 C55 C56 0.9(16) . . . . ? C52 C51 C56 C55 -1.4(13) . . . . ? O3 C51 C56 C55 178.4(8) . . . . ? C54 C55 C56 C51 -0.5(14) . . . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 27.12 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.940 _refine_diff_density_min -1.640 _refine_diff_density_rms 0.151 _database_code_depnum_ccdc_archive 'CCDC 933751' ####################################################################### # # 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_cbo416_0m #TrackingRef 'web_deposit_cif_file_1_AntonioM.Echavarren_1365746154.CBO416_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H45 Au Cl O3 P Si2' _chemical_formula_weight 1157.55 _chemical_absolute_configuration ad 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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.7873(3) _cell_length_b 12.8393(4) _cell_length_c 39.6173(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4978.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9184 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 39.36 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2320 _exptl_absorpt_coefficient_mu 3.137 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4529 _exptl_absorpt_correction_T_max 0.7444 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 70648 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -70 _diffrn_reflns_limit_l_max 62 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 39.97 _reflns_number_total 27809 _reflns_number_gt 26365 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+5.2187P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.020(2) _refine_ls_number_reflns 27809 _refine_ls_number_parameters 631 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0850 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.118 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.463552(9) 0.631765(6) 0.141009(2) 0.01424(2) Uani 1 1 d . . . C1 C 0.8066(2) 0.40488(16) 0.08786(5) 0.0120(3) Uani 1 1 d . . . P1 P 0.67684(7) 0.59101(4) 0.132792(14) 0.01142(9) Uani 1 1 d . . . O1 O 0.73209(17) 0.47604(11) 0.14049(4) 0.0128(2) Uani 1 1 d . . . Cl1 Cl 0.24938(7) 0.69565(5) 0.147072(17) 0.02185(11) Uani 1 1 d . . . Si1 Si 0.86879(7) 0.82597(5) 0.075723(17) 0.01331(10) Uani 1 1 d . . . C2 C 0.7241(2) 0.39756(15) 0.11587(5) 0.0111(3) Uani 1 1 d . . . O2 O 0.72015(18) 0.61357(12) 0.09479(4) 0.0128(3) Uani 1 1 d . . . Si2 Si 0.56160(7) 0.29205(5) 0.167146(16) 0.01183(10) Uani 1 1 d . . . C3 C 0.6386(2) 0.31152(16) 0.12400(5) 0.0122(3) Uani 1 1 d . . . O3 O 0.78537(19) 0.65733(13) 0.15386(4) 0.0146(3) Uani 1 1 d . . . C4 C 0.6324(3) 0.23392(17) 0.09974(6) 0.0142(3) Uani 1 1 d . . . H4 H 0.5769 0.1746 0.1040 0.017 Uiso 1 1 calc R . . C5 C 0.7052(3) 0.23921(16) 0.06895(5) 0.0143(3) Uani 1 1 d . . . C6 C 0.6910(3) 0.15888(18) 0.04462(6) 0.0193(4) Uani 1 1 d . . . H6 H 0.6311 0.1022 0.0489 0.023 Uiso 1 1 calc R . . C7 C 0.7630(3) 0.1624(2) 0.01488(6) 0.0224(5) Uani 1 1 d . . . H7 H 0.7527 0.1084 -0.0013 0.027 Uiso 1 1 calc R . . C8 C 0.8523(3) 0.2465(2) 0.00846(6) 0.0210(5) Uani 1 1 d . . . H8 H 0.9025 0.2484 -0.0121 0.025 Uiso 1 1 calc R . . C9 C 0.8676(3) 0.32575(18) 0.03156(6) 0.0167(4) Uani 1 1 d . . . H9 H 0.9271 0.3822 0.0266 0.020 Uiso 1 1 calc R . . C10 C 0.7952(2) 0.32430(16) 0.06288(5) 0.0129(3) Uani 1 1 d . . . C11 C 0.9029(2) 0.49478(15) 0.08359(5) 0.0114(3) Uani 1 1 d . . . C12 C 0.8570(2) 0.59649(16) 0.08521(5) 0.0116(3) Uani 1 1 d . . . C13 C 0.9345(2) 0.68619(16) 0.07728(6) 0.0136(3) Uani 1 1 d . . . C14 C 1.0710(2) 0.66817(17) 0.07024(6) 0.0146(3) Uani 1 1 d . . . H14 H 1.1274 0.7256 0.0644 0.018 Uiso 1 1 calc R . . C15 C 1.1301(2) 0.56730(17) 0.07147(6) 0.0139(3) Uani 1 1 d . . . C16 C 1.2733(3) 0.5535(2) 0.06657(6) 0.0178(4) Uani 1 1 d . . . H16 H 1.3291 0.6121 0.0616 0.021 Uiso 1 1 calc R . . C17 C 1.3309(3) 0.4567(2) 0.06892(7) 0.0206(4) Uani 1 1 d . . . H17 H 1.4263 0.4481 0.0655 0.025 Uiso 1 1 calc R . . C18 C 1.2483(3) 0.3692(2) 0.07649(6) 0.0201(4) Uani 1 1 d . . . H18 H 1.2893 0.3024 0.0784 0.024 Uiso 1 1 calc R . . C19 C 1.1097(3) 0.37960(18) 0.08111(6) 0.0165(4) Uani 1 1 d . . . H19 H 1.0559 0.3200 0.0861 0.020 Uiso 1 1 calc R . . C20 C 1.0463(3) 0.47937(15) 0.07844(5) 0.0134(3) Uani 1 1 d . . . C21 C 0.8877(3) 0.89240(17) 0.11728(6) 0.0163(4) Uani 1 1 d . . . C22 C 0.8244(4) 0.9890(2) 0.12227(8) 0.0273(6) Uani 1 1 d . . . H22 H 0.7655 1.0159 0.1053 0.033 Uiso 1 1 calc R . . C23 C 0.8463(4) 1.0461(3) 0.15161(9) 0.0334(7) Uani 1 1 d . . . H23 H 0.8039 1.1121 0.1543 0.040 Uiso 1 1 calc R . . C24 C 0.9291(3) 1.0076(3) 0.17684(8) 0.0269(6) Uani 1 1 d . . . H24 H 0.9430 1.0465 0.1970 0.032 Uiso 1 1 calc R . . C25 C 0.9918(3) 0.9121(2) 0.17263(8) 0.0250(5) Uani 1 1 d . . . H25 H 1.0488 0.8851 0.1899 0.030 Uiso 1 1 calc R . . C26 C 0.9716(3) 0.85499(17) 0.14299(7) 0.0191(4) Uani 1 1 d . . . H26 H 1.0158 0.7896 0.1403 0.023 Uiso 1 1 calc R . . C27 C 0.6859(3) 0.84491(17) 0.06224(6) 0.0164(4) Uani 1 1 d . . . C28 C 0.6512(3) 0.87786(19) 0.02960(6) 0.0188(4) Uani 1 1 d . . . H28 H 0.7206 0.8838 0.0129 0.023 Uiso 1 1 calc R . . C29 C 0.5164(3) 0.9021(2) 0.02119(7) 0.0233(5) Uani 1 1 d . . . H29 H 0.4952 0.9253 -0.0010 0.028 Uiso 1 1 calc R . . C30 C 0.4135(3) 0.8923(2) 0.04500(9) 0.0266(5) Uani 1 1 d . . . H30 H 0.3217 0.9077 0.0391 0.032 Uiso 1 1 calc R . . C31 C 0.4449(3) 0.8598(2) 0.07772(8) 0.0266(5) Uani 1 1 d . . . H31 H 0.3748 0.8529 0.0942 0.032 Uiso 1 1 calc R . . C32 C 0.5796(3) 0.8379(2) 0.08596(7) 0.0205(4) Uani 1 1 d . . . H32 H 0.6007 0.8173 0.1084 0.025 Uiso 1 1 calc R . . C33 C 0.9772(3) 0.89364(17) 0.04345(6) 0.0175(4) Uani 1 1 d . . . C34 C 1.0301(3) 0.99405(19) 0.04841(8) 0.0240(5) Uani 1 1 d . . . H34 H 1.0174 1.0279 0.0695 0.029 Uiso 1 1 calc R . . C35 C 0.7043(2) 0.28978(17) 0.19870(6) 0.0140(3) Uani 1 1 d . . . C36 C 0.8422(3) 0.29164(19) 0.18950(6) 0.0172(4) Uani 1 1 d . . . H36 H 0.8661 0.2995 0.1664 0.021 Uiso 1 1 calc R . . C37 C 0.9450(3) 0.2822(2) 0.21347(7) 0.0210(4) Uani 1 1 d . . . H37 H 1.0380 0.2824 0.2066 0.025 Uiso 1 1 calc R . . C38 C 0.6737(3) 0.28067(19) 0.23326(6) 0.0175(4) Uani 1 1 d . . . H38 H 0.5809 0.2803 0.2402 0.021 Uiso 1 1 calc R . . C39 C 0.4782(3) 0.16018(16) 0.16647(6) 0.0154(4) Uani 1 1 d . . . C40 C 0.3661(3) 0.1369(2) 0.14554(7) 0.0220(4) Uani 1 1 d . . . H40 H 0.3329 0.1884 0.1304 0.026 Uiso 1 1 calc R . . C41 C 0.5243(3) 0.08084(17) 0.18787(7) 0.0197(4) Uani 1 1 d . . . H41 H 0.6004 0.0934 0.2022 0.024 Uiso 1 1 calc R . . C42 C 0.4603(4) -0.01646(19) 0.18854(8) 0.0273(5) Uani 1 1 d . . . H42 H 0.4932 -0.0689 0.2034 0.033 Uiso 1 1 calc R . . C43 C 0.3513(4) -0.0371(2) 0.16812(10) 0.0307(7) Uani 1 1 d . . . H43 H 0.3087 -0.1036 0.1686 0.037 Uiso 1 1 calc R . . C44 C 0.4318(2) 0.39079(17) 0.18100(6) 0.0151(4) Uani 1 1 d . . . C45 C 0.4621(3) 0.46270(17) 0.20660(6) 0.0202(4) Uani 1 1 d . . . H45 H 0.5531 0.4684 0.2147 0.024 Uiso 1 1 calc R . . C46 C 0.3608(4) 0.5258(2) 0.22032(8) 0.0282(6) Uani 1 1 d . . . H46 H 0.3830 0.5735 0.2378 0.034 Uiso 1 1 calc R . . C47 C 0.2280(4) 0.5195(2) 0.20864(10) 0.0309(7) Uani 1 1 d . . . H47 H 0.1583 0.5606 0.2187 0.037 Uiso 1 1 calc R . . C48 C 0.1969(3) 0.4532(2) 0.18220(11) 0.0301(6) Uani 1 1 d . . . H48 H 0.1069 0.4517 0.1732 0.036 Uiso 1 1 calc R . . C49 C 0.3032(4) 0.0401(2) 0.14655(9) 0.0304(7) Uani 1 1 d . . . H49 H 0.2268 0.0265 0.1324 0.037 Uiso 1 1 calc R . . C50 C 0.7759(3) 0.2722(2) 0.25744(7) 0.0213(5) Uani 1 1 d . . . H50 H 0.7526 0.2664 0.2806 0.026 Uiso 1 1 calc R . . C51 C 0.9124(3) 0.2723(2) 0.24761(7) 0.0218(5) Uani 1 1 d . . . H51 H 0.9827 0.2658 0.2640 0.026 Uiso 1 1 calc R . . C52 C 0.2970(3) 0.3890(2) 0.16888(9) 0.0239(5) Uani 1 1 d . . . H52 H 0.2739 0.3425 0.1511 0.029 Uiso 1 1 calc R . . C53 C 1.1010(4) 1.0444(2) 0.02272(11) 0.0316(7) Uani 1 1 d . . . H53 H 1.1364 1.1123 0.0264 0.038 Uiso 1 1 calc R . . C54 C 1.1200(4) 0.9968(3) -0.00795(10) 0.0331(7) Uani 1 1 d . . . H54 H 1.1675 1.0324 -0.0254 0.040 Uiso 1 1 calc R . . C55 C 1.0703(3) 0.8967(3) -0.01367(8) 0.0279(6) Uani 1 1 d . . . H55 H 1.0844 0.8632 -0.0348 0.033 Uiso 1 1 calc R . . C56 C 0.9991(3) 0.8466(2) 0.01223(7) 0.0218(5) Uani 1 1 d . . . H56 H 0.9647 0.7784 0.0084 0.026 Uiso 1 1 calc R . . C57 C 0.7732(3) 0.66210(18) 0.18932(6) 0.0156(4) Uani 1 1 d . . . C58 C 0.7236(3) 0.7522(2) 0.20334(8) 0.0241(5) Uani 1 1 d . . . H58 H 0.6979 0.8096 0.1896 0.029 Uiso 1 1 calc R . . C59 C 0.8141(3) 0.5777(2) 0.20861(7) 0.0233(5) Uani 1 1 d . . . H59 H 0.8511 0.5171 0.1983 0.028 Uiso 1 1 calc R . . C60 C 0.7994(4) 0.5840(3) 0.24354(8) 0.0339(8) Uani 1 1 d . . . H60 H 0.8249 0.5264 0.2572 0.041 Uiso 1 1 calc R . . C61 C 0.7486(4) 0.6723(4) 0.25844(8) 0.0369(9) Uani 1 1 d . . . H61 H 0.7384 0.6754 0.2823 0.044 Uiso 1 1 calc R . . C62 C 0.7120(4) 0.7571(3) 0.23864(9) 0.0333(7) Uani 1 1 d . . . H62 H 0.6790 0.8188 0.2490 0.040 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 0.01284(3) 0.01457(3) 0.01532(3) -0.00052(3) 0.00193(3) 0.00185(3) C1 0.0142(9) 0.0103(7) 0.0116(7) 0.0015(6) 0.0027(6) 0.0027(6) P1 0.0132(2) 0.01005(19) 0.01102(19) -0.00066(15) 0.00270(16) 0.00011(16) O1 0.0181(7) 0.0100(5) 0.0103(5) -0.0006(5) 0.0009(6) 0.0010(4) Cl1 0.0154(3) 0.0261(3) 0.0241(3) -0.0034(2) -0.00107(19) 0.00577(19) Si1 0.0172(3) 0.0101(2) 0.0127(2) 0.00066(18) 0.0031(2) 0.00187(19) C2 0.0129(9) 0.0105(6) 0.0099(6) 0.0001(5) 0.0005(6) 0.0014(6) O2 0.0127(7) 0.0119(6) 0.0138(6) 0.0021(5) 0.0032(5) 0.0031(5) Si2 0.0123(3) 0.0119(2) 0.0113(2) 0.00079(17) 0.00071(18) -0.00120(17) C3 0.0146(9) 0.0109(7) 0.0111(7) -0.0003(6) 0.0012(6) -0.0003(6) O3 0.0161(8) 0.0139(6) 0.0138(6) -0.0023(5) 0.0021(5) -0.0026(5) C4 0.0170(10) 0.0122(7) 0.0134(8) -0.0002(6) 0.0001(7) -0.0007(6) C5 0.0207(10) 0.0112(7) 0.0110(7) -0.0006(6) -0.0004(7) 0.0015(7) C6 0.0290(13) 0.0142(8) 0.0148(8) -0.0035(7) -0.0003(8) 0.0003(8) C7 0.0350(15) 0.0190(9) 0.0133(8) -0.0058(7) 0.0004(9) 0.0024(9) C8 0.0297(14) 0.0206(10) 0.0126(8) -0.0036(7) 0.0021(8) 0.0045(9) C9 0.0225(11) 0.0157(8) 0.0119(7) 0.0000(6) 0.0027(7) 0.0029(7) C10 0.0177(10) 0.0108(7) 0.0102(7) 0.0008(6) 0.0001(6) 0.0034(6) C11 0.0139(9) 0.0105(7) 0.0098(7) 0.0002(5) 0.0019(6) 0.0011(6) C12 0.0129(9) 0.0107(7) 0.0113(7) 0.0013(6) 0.0026(6) 0.0021(6) C13 0.0173(10) 0.0099(6) 0.0136(7) 0.0017(6) 0.0035(6) 0.0016(6) C14 0.0148(9) 0.0130(7) 0.0160(8) 0.0004(6) 0.0031(7) 0.0004(6) C15 0.0140(9) 0.0150(8) 0.0127(7) 0.0002(6) 0.0013(6) 0.0011(6) C16 0.0145(10) 0.0210(9) 0.0179(9) -0.0012(7) 0.0033(7) 0.0019(7) C17 0.0136(10) 0.0273(11) 0.0208(10) 0.0004(8) 0.0017(8) 0.0057(8) C18 0.0209(10) 0.0223(9) 0.0171(8) 0.0003(9) 0.0006(8) 0.0108(9) C19 0.0167(9) 0.0164(9) 0.0163(8) 0.0026(7) -0.0004(7) 0.0055(7) C20 0.0147(9) 0.0124(7) 0.0131(7) 0.0006(6) 0.0017(7) 0.0032(7) C21 0.0187(10) 0.0146(8) 0.0158(8) -0.0006(6) 0.0008(7) 0.0046(7) C22 0.0358(16) 0.0238(11) 0.0224(11) -0.0099(9) -0.0094(11) 0.0164(11) C23 0.0345(17) 0.0324(14) 0.0332(15) -0.0179(12) -0.0116(13) 0.0142(12) C24 0.0274(14) 0.0331(13) 0.0201(11) -0.0087(10) -0.0013(9) -0.0007(10) C25 0.0251(13) 0.0278(12) 0.0223(11) 0.0023(9) -0.0077(9) -0.0033(9) C26 0.0166(10) 0.0175(8) 0.0232(9) 0.0026(7) -0.0019(9) 0.0007(7) C27 0.0198(11) 0.0126(7) 0.0168(8) 0.0004(6) 0.0009(7) 0.0018(6) C28 0.0235(11) 0.0163(9) 0.0167(8) 0.0006(7) -0.0009(7) 0.0011(8) C29 0.0295(15) 0.0209(9) 0.0195(9) 0.0002(8) -0.0067(9) 0.0042(9) C30 0.0216(13) 0.0264(12) 0.0318(14) 0.0008(10) -0.0032(10) 0.0065(9) C31 0.0215(13) 0.0308(12) 0.0276(11) 0.0036(11) 0.0032(9) 0.0076(10) C32 0.0203(11) 0.0213(9) 0.0199(10) 0.0055(8) 0.0036(8) 0.0067(8) C33 0.0189(11) 0.0134(7) 0.0202(9) 0.0044(7) 0.0034(8) 0.0005(7) C34 0.0209(12) 0.0159(8) 0.0353(13) 0.0039(8) 0.0024(11) -0.0013(9) C35 0.0146(9) 0.0130(7) 0.0143(8) 0.0007(6) -0.0007(7) -0.0011(6) C36 0.0152(10) 0.0193(9) 0.0170(9) 0.0020(7) 0.0002(7) 0.0007(7) C37 0.0148(11) 0.0246(10) 0.0237(10) 0.0024(8) -0.0026(8) 0.0008(8) C38 0.0197(11) 0.0186(9) 0.0141(8) 0.0009(7) 0.0003(7) 0.0002(7) C39 0.0166(11) 0.0139(7) 0.0157(8) -0.0007(6) 0.0021(7) -0.0024(7) C40 0.0224(11) 0.0213(9) 0.0224(10) -0.0012(9) 0.0001(8) -0.0102(9) C41 0.0223(12) 0.0141(8) 0.0226(10) 0.0031(7) 0.0035(9) 0.0005(8) C42 0.0354(15) 0.0137(8) 0.0329(13) 0.0052(8) 0.0069(13) -0.0002(10) C43 0.0358(17) 0.0168(10) 0.0394(17) -0.0012(10) 0.0067(13) -0.0093(10) C44 0.0156(9) 0.0136(7) 0.0162(8) -0.0006(6) 0.0030(7) -0.0014(6) C45 0.0261(12) 0.0160(8) 0.0185(9) -0.0032(7) -0.0008(10) 0.0020(9) C46 0.0431(19) 0.0204(10) 0.0210(11) -0.0035(9) 0.0054(11) 0.0084(11) C47 0.0329(17) 0.0213(11) 0.0385(16) -0.0001(11) 0.0163(13) 0.0061(10) C48 0.0148(12) 0.0243(12) 0.051(2) -0.0020(12) 0.0053(12) 0.0016(9) C49 0.0290(15) 0.0253(11) 0.0370(17) -0.0027(11) -0.0012(12) -0.0148(11) C50 0.0275(13) 0.0218(10) 0.0146(9) 0.0012(8) -0.0035(9) 0.0027(9) C51 0.0238(13) 0.0211(10) 0.0203(10) -0.0004(8) -0.0081(9) 0.0019(9) C52 0.0146(11) 0.0205(10) 0.0366(14) -0.0055(9) -0.0030(9) 0.0010(8) C53 0.0221(14) 0.0227(11) 0.050(2) 0.0148(12) 0.0017(13) -0.0053(10) C54 0.0197(13) 0.0394(16) 0.0401(17) 0.0242(14) 0.0049(12) -0.0006(11) C55 0.0222(13) 0.0406(15) 0.0208(10) 0.0120(11) 0.0070(9) 0.0035(10) C56 0.0254(12) 0.0208(10) 0.0193(9) 0.0034(8) 0.0071(8) 0.0003(8) C57 0.0153(10) 0.0164(8) 0.0150(8) -0.0053(7) 0.0020(7) -0.0023(7) C58 0.0186(12) 0.0268(11) 0.0269(12) -0.0137(10) 0.0018(9) 0.0037(9) C59 0.0317(14) 0.0191(10) 0.0192(10) 0.0003(8) -0.0040(10) -0.0063(9) C60 0.0437(19) 0.0395(16) 0.0185(11) 0.0041(11) -0.0050(12) -0.0214(14) C61 0.0288(16) 0.063(2) 0.0184(11) -0.0122(13) 0.0072(11) -0.0235(16) C62 0.0211(14) 0.0470(18) 0.0319(15) -0.0240(14) 0.0066(11) -0.0025(12) _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 2.1766(6) . ? Au1 Cl1 2.2637(7) . ? C1 C2 1.376(3) . ? C1 C10 1.436(3) . ? C1 C11 1.500(3) . ? P1 O2 1.5908(17) . ? P1 O3 1.5968(19) . ? P1 O1 1.6014(15) . ? O1 C2 1.404(3) . ? Si1 C21 1.863(2) . ? Si1 C33 1.875(2) . ? Si1 C27 1.884(3) . ? Si1 C13 1.907(2) . ? C2 C3 1.423(3) . ? O2 C12 1.409(3) . ? Si2 C35 1.874(2) . ? Si2 C44 1.877(2) . ? Si2 C39 1.880(2) . ? Si2 C3 1.885(2) . ? C3 C4 1.386(3) . ? O3 C57 1.411(3) . ? C4 C5 1.414(3) . ? C5 C6 1.419(3) . ? C5 C10 1.424(3) . ? C6 C7 1.373(4) . ? C7 C8 1.412(4) . ? C8 C9 1.377(3) . ? C9 C10 1.429(3) . ? C11 C12 1.382(3) . ? C11 C20 1.432(3) . ? C12 C13 1.415(3) . ? C13 C14 1.384(3) . ? C14 C15 1.419(3) . ? C15 C20 1.423(3) . ? C15 C16 1.426(3) . ? C16 C17 1.369(4) . ? C17 C18 1.416(4) . ? C18 C19 1.375(4) . ? C19 C20 1.428(3) . ? C21 C26 1.394(3) . ? C21 C22 1.400(3) . ? C22 C23 1.391(4) . ? C23 C24 1.378(5) . ? C24 C25 1.381(5) . ? C25 C26 1.398(4) . ? C27 C28 1.402(3) . ? C27 C32 1.405(4) . ? C28 C29 1.395(4) . ? C29 C30 1.386(5) . ? C30 C31 1.396(4) . ? C31 C32 1.388(4) . ? C33 C56 1.393(4) . ? C33 C34 1.403(3) . ? C34 C53 1.391(4) . ? C35 C36 1.398(4) . ? C35 C38 1.406(3) . ? C36 C37 1.389(4) . ? C37 C51 1.395(4) . ? C38 C50 1.389(4) . ? C39 C41 1.400(3) . ? C39 C40 1.407(4) . ? C40 C49 1.387(4) . ? C41 C42 1.397(4) . ? C42 C43 1.365(5) . ? C43 C49 1.391(5) . ? C44 C45 1.403(3) . ? C44 C52 1.404(4) . ? C45 C46 1.391(4) . ? C46 C47 1.382(6) . ? C47 C48 1.384(5) . ? C48 C52 1.385(4) . ? C50 C51 1.392(5) . ? C53 C54 1.373(6) . ? C54 C55 1.393(5) . ? C55 C56 1.397(4) . ? C57 C58 1.372(3) . ? C57 C59 1.385(4) . ? C58 C62 1.404(5) . ? C59 C60 1.393(4) . ? C60 C61 1.371(6) . ? C61 C62 1.389(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 Cl1 172.34(2) . . ? C2 C1 C10 117.5(2) . . ? C2 C1 C11 120.82(19) . . ? C10 C1 C11 121.69(19) . . ? O2 P1 O3 102.73(10) . . ? O2 P1 O1 104.96(9) . . ? O3 P1 O1 99.64(10) . . ? O2 P1 Au1 110.69(7) . . ? O3 P1 Au1 115.57(7) . . ? O1 P1 Au1 121.13(7) . . ? C2 O1 P1 120.68(14) . . ? C21 Si1 C33 109.51(12) . . ? C21 Si1 C27 106.62(11) . . ? C33 Si1 C27 106.54(11) . . ? C21 Si1 C13 111.62(10) . . ? C33 Si1 C13 105.50(10) . . ? C27 Si1 C13 116.81(10) . . ? C1 C2 O1 118.57(19) . . ? C1 C2 C3 125.51(19) . . ? O1 C2 C3 115.65(18) . . ? C12 O2 P1 118.66(14) . . ? C35 Si2 C44 108.66(11) . . ? C35 Si2 C39 108.61(10) . . ? C44 Si2 C39 108.57(11) . . ? C35 Si2 C3 108.00(11) . . ? C44 Si2 C3 116.50(10) . . ? C39 Si2 C3 106.27(10) . . ? C4 C3 C2 115.28(19) . . ? C4 C3 Si2 121.08(16) . . ? C2 C3 Si2 122.91(15) . . ? C57 O3 P1 119.15(15) . . ? C3 C4 C5 122.8(2) . . ? C4 C5 C6 120.1(2) . . ? C4 C5 C10 119.63(19) . . ? C6 C5 C10 120.2(2) . . ? C7 C6 C5 120.6(2) . . ? C6 C7 C8 119.8(2) . . ? C9 C8 C7 120.8(2) . . ? C8 C9 C10 120.9(2) . . ? C5 C10 C9 117.6(2) . . ? C5 C10 C1 118.9(2) . . ? C9 C10 C1 123.4(2) . . ? C12 C11 C20 117.11(19) . . ? C12 C11 C1 121.2(2) . . ? C20 C11 C1 121.71(18) . . ? C11 C12 O2 117.93(19) . . ? C11 C12 C13 125.8(2) . . ? O2 C12 C13 116.29(17) . . ? C14 C13 C12 115.24(19) . . ? C14 C13 Si1 118.43(16) . . ? C12 C13 Si1 126.33(17) . . ? C13 C14 C15 122.6(2) . . ? C14 C15 C20 119.7(2) . . ? C14 C15 C16 120.6(2) . . ? C20 C15 C16 119.7(2) . . ? C17 C16 C15 120.6(2) . . ? C16 C17 C18 120.0(2) . . ? C19 C18 C17 120.9(2) . . ? C18 C19 C20 120.4(2) . . ? C15 C20 C19 118.4(2) . . ? C15 C20 C11 118.89(18) . . ? C19 C20 C11 122.7(2) . . ? C26 C21 C22 117.6(2) . . ? C26 C21 Si1 123.14(17) . . ? C22 C21 Si1 119.08(19) . . ? C23 C22 C21 121.1(3) . . ? C24 C23 C22 120.5(3) . . ? C23 C24 C25 119.4(3) . . ? C24 C25 C26 120.3(3) . . ? C21 C26 C25 121.1(2) . . ? C28 C27 C32 117.2(2) . . ? C28 C27 Si1 122.1(2) . . ? C32 C27 Si1 120.37(19) . . ? C29 C28 C27 121.1(3) . . ? C30 C29 C28 120.3(3) . . ? C29 C30 C31 120.0(3) . . ? C32 C31 C30 119.2(3) . . ? C31 C32 C27 122.2(3) . . ? C56 C33 C34 117.8(2) . . ? C56 C33 Si1 119.44(18) . . ? C34 C33 Si1 122.6(2) . . ? C53 C34 C33 120.6(3) . . ? C36 C35 C38 117.4(2) . . ? C36 C35 Si2 123.04(18) . . ? C38 C35 Si2 119.48(19) . . ? C37 C36 C35 121.3(2) . . ? C36 C37 C51 120.3(3) . . ? C50 C38 C35 121.7(3) . . ? C41 C39 C40 117.0(2) . . ? C41 C39 Si2 120.44(19) . . ? C40 C39 Si2 122.58(18) . . ? C49 C40 C39 121.3(3) . . ? C42 C41 C39 121.2(3) . . ? C43 C42 C41 120.8(3) . . ? C42 C43 C49 119.3(3) . . ? C45 C44 C52 117.2(2) . . ? C45 C44 Si2 120.8(2) . . ? C52 C44 Si2 121.65(18) . . ? C46 C45 C44 121.0(3) . . ? C47 C46 C45 120.4(3) . . ? C46 C47 C48 119.7(3) . . ? C47 C48 C52 119.9(3) . . ? C40 C49 C43 120.4(3) . . ? C38 C50 C51 119.9(2) . . ? C50 C51 C37 119.4(2) . . ? C48 C52 C44 121.6(3) . . ? C54 C53 C34 120.6(3) . . ? C53 C54 C55 120.5(3) . . ? C54 C55 C56 118.7(3) . . ? C33 C56 C55 121.9(3) . . ? C58 C57 C59 122.6(3) . . ? C58 C57 O3 118.0(2) . . ? C59 C57 O3 119.4(2) . . ? C57 C58 C62 118.0(3) . . ? C57 C59 C60 118.2(3) . . ? C61 C60 C59 120.9(3) . . ? C60 C61 C62 119.9(3) . . ? C61 C62 C58 120.4(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Au1 P1 O2 -56.4(2) . . . . ? Cl1 Au1 P1 O3 59.8(2) . . . . ? Cl1 Au1 P1 O1 -180(33) . . . . ? O2 P1 O1 C2 -39.26(18) . . . . ? O3 P1 O1 C2 -145.32(16) . . . . ? Au1 P1 O1 C2 86.79(17) . . . . ? C10 C1 C2 O1 -179.27(19) . . . . ? C11 C1 C2 O1 -0.2(3) . . . . ? C10 C1 C2 C3 7.0(3) . . . . ? C11 C1 C2 C3 -173.9(2) . . . . ? P1 O1 C2 C1 69.7(2) . . . . ? P1 O1 C2 C3 -115.96(19) . . . . ? O3 P1 O2 C12 53.07(16) . . . . ? O1 P1 O2 C12 -50.70(17) . . . . ? Au1 P1 O2 C12 177.01(13) . . . . ? C1 C2 C3 C4 -5.4(3) . . . . ? O1 C2 C3 C4 -179.31(19) . . . . ? C1 C2 C3 Si2 164.89(18) . . . . ? O1 C2 C3 Si2 -9.0(3) . . . . ? C35 Si2 C3 C4 113.5(2) . . . . ? C44 Si2 C3 C4 -124.0(2) . . . . ? C39 Si2 C3 C4 -2.9(2) . . . . ? C35 Si2 C3 C2 -56.3(2) . . . . ? C44 Si2 C3 C2 66.3(2) . . . . ? C39 Si2 C3 C2 -172.68(18) . . . . ? O2 P1 O3 C57 175.75(17) . . . . ? O1 P1 O3 C57 -76.39(18) . . . . ? Au1 P1 O3 C57 55.11(18) . . . . ? C2 C3 C4 C5 -0.2(3) . . . . ? Si2 C3 C4 C5 -170.66(18) . . . . ? C3 C4 C5 C6 -177.8(2) . . . . ? C3 C4 C5 C10 3.7(4) . . . . ? C4 C5 C6 C7 -178.9(3) . . . . ? C10 C5 C6 C7 -0.4(4) . . . . ? C5 C6 C7 C8 0.2(4) . . . . ? C6 C7 C8 C9 -0.5(4) . . . . ? C7 C8 C9 C10 1.0(4) . . . . ? C4 C5 C10 C9 179.4(2) . . . . ? C6 C5 C10 C9 0.8(3) . . . . ? C4 C5 C10 C1 -2.0(3) . . . . ? C6 C5 C10 C1 179.5(2) . . . . ? C8 C9 C10 C5 -1.2(4) . . . . ? C8 C9 C10 C1 -179.7(2) . . . . ? C2 C1 C10 C5 -3.0(3) . . . . ? C11 C1 C10 C5 177.9(2) . . . . ? C2 C1 C10 C9 175.6(2) . . . . ? C11 C1 C10 C9 -3.6(3) . . . . ? C2 C1 C11 C12 -54.3(3) . . . . ? C10 C1 C11 C12 124.8(2) . . . . ? C2 C1 C11 C20 124.3(2) . . . . ? C10 C1 C11 C20 -56.6(3) . . . . ? C20 C11 C12 O2 -171.56(19) . . . . ? C1 C11 C12 O2 7.1(3) . . . . ? C20 C11 C12 C13 10.1(3) . . . . ? C1 C11 C12 C13 -171.3(2) . . . . ? P1 O2 C12 C11 69.9(2) . . . . ? P1 O2 C12 C13 -111.55(19) . . . . ? C11 C12 C13 C14 -5.9(3) . . . . ? O2 C12 C13 C14 175.7(2) . . . . ? C11 C12 C13 Si1 174.38(18) . . . . ? O2 C12 C13 Si1 -4.0(3) . . . . ? C21 Si1 C13 C14 -88.8(2) . . . . ? C33 Si1 C13 C14 30.1(2) . . . . ? C27 Si1 C13 C14 148.16(19) . . . . ? C21 Si1 C13 C12 90.9(2) . . . . ? C33 Si1 C13 C12 -150.2(2) . . . . ? C27 Si1 C13 C12 -32.1(2) . . . . ? C12 C13 C14 C15 -1.1(3) . . . . ? Si1 C13 C14 C15 178.61(18) . . . . ? C13 C14 C15 C20 3.4(4) . . . . ? C13 C14 C15 C16 -175.1(2) . . . . ? C14 C15 C16 C17 177.7(2) . . . . ? C20 C15 C16 C17 -0.8(4) . . . . ? C15 C16 C17 C18 -0.4(4) . . . . ? C16 C17 C18 C19 0.9(4) . . . . ? C17 C18 C19 C20 -0.2(4) . . . . ? C14 C15 C20 C19 -177.0(2) . . . . ? C16 C15 C20 C19 1.5(3) . . . . ? C14 C15 C20 C11 0.9(3) . . . . ? C16 C15 C20 C11 179.4(2) . . . . ? C18 C19 C20 C15 -1.0(3) . . . . ? C18 C19 C20 C11 -178.9(2) . . . . ? C12 C11 C20 C15 -7.1(3) . . . . ? C1 C11 C20 C15 174.25(19) . . . . ? C12 C11 C20 C19 170.8(2) . . . . ? C1 C11 C20 C19 -7.9(3) . . . . ? C33 Si1 C21 C26 -100.4(2) . . . . ? C27 Si1 C21 C26 144.7(2) . . . . ? C13 Si1 C21 C26 16.1(3) . . . . ? C33 Si1 C21 C22 74.1(3) . . . . ? C27 Si1 C21 C22 -40.8(3) . . . . ? C13 Si1 C21 C22 -169.5(2) . . . . ? C26 C21 C22 C23 1.0(5) . . . . ? Si1 C21 C22 C23 -173.8(3) . . . . ? C21 C22 C23 C24 -1.3(6) . . . . ? C22 C23 C24 C25 0.7(6) . . . . ? C23 C24 C25 C26 0.2(5) . . . . ? C22 C21 C26 C25 -0.1(4) . . . . ? Si1 C21 C26 C25 174.4(2) . . . . ? C24 C25 C26 C21 -0.5(4) . . . . ? C21 Si1 C27 C28 132.5(2) . . . . ? C33 Si1 C27 C28 15.6(2) . . . . ? C13 Si1 C27 C28 -101.9(2) . . . . ? C21 Si1 C27 C32 -40.1(2) . . . . ? C33 Si1 C27 C32 -157.0(2) . . . . ? C13 Si1 C27 C32 85.5(2) . . . . ? C32 C27 C28 C29 -0.3(4) . . . . ? Si1 C27 C28 C29 -173.1(2) . . . . ? C27 C28 C29 C30 -1.0(4) . . . . ? C28 C29 C30 C31 1.1(4) . . . . ? C29 C30 C31 C32 0.1(5) . . . . ? C30 C31 C32 C27 -1.4(5) . . . . ? C28 C27 C32 C31 1.5(4) . . . . ? Si1 C27 C32 C31 174.5(2) . . . . ? C21 Si1 C33 C56 168.2(2) . . . . ? C27 Si1 C33 C56 -76.9(2) . . . . ? C13 Si1 C33 C56 47.9(2) . . . . ? C21 Si1 C33 C34 -16.5(3) . . . . ? C27 Si1 C33 C34 98.4(2) . . . . ? C13 Si1 C33 C34 -136.8(2) . . . . ? C56 C33 C34 C53 0.5(4) . . . . ? Si1 C33 C34 C53 -174.9(3) . . . . ? C44 Si2 C35 C36 -133.2(2) . . . . ? C39 Si2 C35 C36 108.9(2) . . . . ? C3 Si2 C35 C36 -6.0(2) . . . . ? C44 Si2 C35 C38 50.0(2) . . . . ? C39 Si2 C35 C38 -67.9(2) . . . . ? C3 Si2 C35 C38 177.25(18) . . . . ? C38 C35 C36 C37 1.6(4) . . . . ? Si2 C35 C36 C37 -175.23(19) . . . . ? C35 C36 C37 C51 -1.1(4) . . . . ? C36 C35 C38 C50 -0.9(4) . . . . ? Si2 C35 C38 C50 176.00(19) . . . . ? C35 Si2 C39 C41 1.0(2) . . . . ? C44 Si2 C39 C41 -117.0(2) . . . . ? C3 Si2 C39 C41 116.9(2) . . . . ? C35 Si2 C39 C40 179.3(2) . . . . ? C44 Si2 C39 C40 61.3(2) . . . . ? C3 Si2 C39 C40 -64.7(2) . . . . ? C41 C39 C40 C49 1.0(4) . . . . ? Si2 C39 C40 C49 -177.4(2) . . . . ? C40 C39 C41 C42 -0.7(4) . . . . ? Si2 C39 C41 C42 177.7(2) . . . . ? C39 C41 C42 C43 0.4(5) . . . . ? C41 C42 C43 C49 -0.4(5) . . . . ? C35 Si2 C44 C45 12.8(2) . . . . ? C39 Si2 C44 C45 130.8(2) . . . . ? C3 Si2 C44 C45 -109.4(2) . . . . ? C35 Si2 C44 C52 -160.4(2) . . . . ? C39 Si2 C44 C52 -42.5(2) . . . . ? C3 Si2 C44 C52 77.4(2) . . . . ? C52 C44 C45 C46 2.9(4) . . . . ? Si2 C44 C45 C46 -170.6(2) . . . . ? C44 C45 C46 C47 -0.7(4) . . . . ? C45 C46 C47 C48 -2.7(5) . . . . ? C46 C47 C48 C52 3.8(5) . . . . ? C39 C40 C49 C43 -1.0(5) . . . . ? C42 C43 C49 C40 0.7(5) . . . . ? C35 C38 C50 C51 -0.2(4) . . . . ? C38 C50 C51 C37 0.7(4) . . . . ? C36 C37 C51 C50 -0.1(4) . . . . ? C47 C48 C52 C44 -1.5(5) . . . . ? C45 C44 C52 C48 -1.8(4) . . . . ? Si2 C44 C52 C48 171.7(2) . . . . ? C33 C34 C53 C54 0.2(5) . . . . ? C34 C53 C54 C55 -0.9(5) . . . . ? C53 C54 C55 C56 0.9(5) . . . . ? C34 C33 C56 C55 -0.4(4) . . . . ? Si1 C33 C56 C55 175.1(2) . . . . ? C54 C55 C56 C33 -0.2(5) . . . . ? P1 O3 C57 C58 -104.8(2) . . . . ? P1 O3 C57 C59 76.6(3) . . . . ? C59 C57 C58 C62 -1.2(4) . . . . ? O3 C57 C58 C62 -179.7(3) . . . . ? C58 C57 C59 C60 2.3(4) . . . . ? O3 C57 C59 C60 -179.2(3) . . . . ? C57 C59 C60 C61 -1.4(5) . . . . ? C59 C60 C61 C62 -0.5(5) . . . . ? C60 C61 C62 C58 1.6(5) . . . . ? C57 C58 C62 C61 -0.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 37.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 3.589 _refine_diff_density_min -3.318 _refine_diff_density_rms 0.137 _database_code_depnum_ccdc_archive 'CCDC 933752' ####################################################################### # # 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_mo_rs271p41 #TrackingRef 'web_deposit_cif_file_2_AntonioM.Echavarren_1365746154.mo_RS271P41X.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H25 Au Cl Fe P' _chemical_formula_weight 728.76 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' P P 0.1023 0.0942 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+1/4' 'y, -x, z+3/4' _cell_length_a 13.2861(14) _cell_length_b 13.2861(14) _cell_length_c 14.7974(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2612.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9853 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 29.81 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.853 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 6.349 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2517 _exptl_absorpt_correction_T_max 0.5693 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 33908 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0253 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 30.01 _reflns_number_total 6715 _reflns_number_gt 6497 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0746P)^2^+2.6694P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _chemical_absolute_configuration ad _refine_ls_abs_structure_Flack -0.011(5) _refine_ls_number_reflns 6715 _refine_ls_number_parameters 325 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0302 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0805 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 0.864 _refine_ls_restrained_S_all 0.864 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C8 C 0.6321(4) 0.8614(4) 1.1383(3) 0.0300(10) Uani 1 1 d . . . H8 H 0.6575 0.9215 1.1643 0.036 Uiso 1 1 calc R . . C10 C 0.6580(3) 0.6903(3) 1.0884(3) 0.0236(8) Uani 1 1 d . . . C9 C 0.6929(3) 0.7793(4) 1.1303(3) 0.0291(9) Uani 1 1 d . . . H9 H 0.7597 0.7819 1.1532 0.035 Uiso 1 1 calc R . . C6 C 0.4924(3) 0.7720(3) 1.0671(3) 0.0200(7) Uani 1 1 d . . . C12 C 0.5236(3) 0.5978(3) 1.0108(3) 0.0214(8) Uani 1 1 d . . . H12 H 0.4570 0.5940 0.9879 0.026 Uiso 1 1 calc R . . C3 C 0.3114(3) 0.7015(3) 1.0767(3) 0.0234(8) Uani 1 1 d . . . H3 H 0.3197 0.6618 1.1336 0.028 Uiso 1 1 calc R . . C5 C 0.2393(3) 0.7735(3) 0.9498(3) 0.0243(8) Uani 1 1 d . . . H5 H 0.1896 0.7916 0.9018 0.029 Uiso 1 1 calc R . . C1 C 0.3411(3) 0.8101(3) 0.9567(3) 0.0187(7) Uani 1 1 d . . . C2 C 0.3865(3) 0.7645(3) 1.0366(3) 0.0206(7) Uani 1 1 d . . . C19 C 0.1850(4) 0.9821(4) 1.0624(4) 0.0350(11) Uani 1 1 d . . . H19 H 0.1616 1.0164 1.0060 0.042 Uiso 1 1 calc R . . C11 C 0.5566(3) 0.6866(3) 1.0550(3) 0.0196(7) Uani 1 1 d . . . C7 C 0.5310(4) 0.8575(3) 1.1080(3) 0.0262(9) Uani 1 1 d . . . H7 H 0.4889 0.9146 1.1159 0.031 Uiso 1 1 calc R . . C16 C 0.2815(4) 0.9334(4) 1.1842(3) 0.0369(11) Uani 1 1 d . . . H16 H 0.3386 0.9270 1.2279 0.044 Uiso 1 1 calc R . . C17 C 0.1896(5) 0.8812(4) 1.1885(4) 0.0394(13) Uani 1 1 d . . . H17 H 0.1704 0.8312 1.2359 0.047 Uiso 1 1 calc R . . C13 C 0.5876(4) 0.5171(3) 1.0009(3) 0.0265(9) Uani 1 1 d . . . H13 H 0.5650 0.4589 0.9695 0.032 Uiso 1 1 calc R . . C14 C 0.6848(4) 0.5192(4) 1.0360(4) 0.0326(10) Uani 1 1 d . . . H14 H 0.7271 0.4620 1.0297 0.039 Uiso 1 1 calc R . . C15 C 0.7202(3) 0.6039(4) 1.0799(4) 0.0296(9) Uani 1 1 d . . . H15 H 0.7863 0.6044 1.1044 0.036 Uiso 1 1 calc R . . C20 C 0.2792(4) 0.9969(4) 1.1059(4) 0.0348(11) Uani 1 1 d . . . H20 H 0.3342 1.0428 1.0853 0.042 Uiso 1 1 calc R . . C18 C 0.1286(4) 0.9113(4) 1.1149(4) 0.0402(13) Uani 1 1 d . . . H18 H 0.0590 0.8868 1.1015 0.048 Uiso 1 1 calc R . . C4 C 0.2219(3) 0.7072(3) 1.0243(4) 0.0277(9) Uani 1 1 d . . . H4 H 0.1573 0.6715 1.0378 0.033 Uiso 1 1 calc R . . C21 C 0.4141(3) 0.8223(3) 0.7743(3) 0.0196(7) Uani 1 1 d . . . C22 C 0.4023(4) 0.7192(3) 0.7680(3) 0.0296(10) Uani 1 1 d . . . H22 H 0.3822 0.6817 0.8196 0.036 Uiso 1 1 calc R . . C26 C 0.4438(4) 0.8755(4) 0.6969(3) 0.0317(10) Uani 1 1 d . . . H26 H 0.4537 0.9462 0.7005 0.038 Uiso 1 1 calc R . . C27 C 0.3077(3) 0.9889(3) 0.8522(3) 0.0234(8) Uani 1 1 d . . . C29 C 0.2468(5) 1.1579(4) 0.8760(4) 0.0449(14) Uani 1 1 d . . . H29 H 0.2561 1.2234 0.9002 0.054 Uiso 1 1 calc R . . C28 C 0.3207(4) 1.0856(3) 0.8872(4) 0.0330(10) Uani 1 1 d . . . H28 H 0.3806 1.1019 0.9189 0.040 Uiso 1 1 calc R . . C32 C 0.2202(3) 0.9662(3) 0.8027(3) 0.0261(9) Uani 1 1 d . . . H32 H 0.2112 0.9014 0.7769 0.031 Uiso 1 1 calc R . . Au1 Au 0.548210(11) 0.958483(11) 0.916393(15) 0.02319(6) Uani 1 1 d . . . Fe1 Fe 0.26088(5) 0.84826(5) 1.06901(4) 0.02243(12) Uani 1 1 d . . . P1 P 0.39981(8) 0.89302(7) 0.87821(7) 0.01913(19) Uani 1 1 d . . . Cl1 Cl 0.70234(9) 1.02987(10) 0.94039(9) 0.0359(3) Uani 1 1 d . . . C23 C 0.4197(5) 0.6702(4) 0.6864(4) 0.0373(12) Uani 1 1 d . . . H23 H 0.4133 0.5991 0.6829 0.045 Uiso 1 1 calc R . . C24 C 0.4462(4) 0.7245(4) 0.6106(4) 0.0358(11) Uani 1 1 d . . . H24 H 0.4559 0.6908 0.5546 0.043 Uiso 1 1 calc R . . C25 C 0.4588(4) 0.8272(4) 0.6155(4) 0.0374(11) Uani 1 1 d . . . H25 H 0.4776 0.8645 0.5634 0.045 Uiso 1 1 calc R . . C31 C 0.1463(4) 1.0408(4) 0.7921(4) 0.0387(12) Uani 1 1 d . . . H31 H 0.0868 1.0262 0.7590 0.046 Uiso 1 1 calc R . . C30 C 0.1593(5) 1.1349(4) 0.8294(4) 0.0478(16) Uani 1 1 d . . . H30 H 0.1080 1.1843 0.8231 0.057 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 C8 0.032(2) 0.032(2) 0.025(2) -0.0099(17) -0.0055(17) -0.0092(17) C10 0.0207(18) 0.032(2) 0.018(2) 0.0066(15) 0.0017(15) -0.0006(15) C9 0.0240(19) 0.040(2) 0.023(2) -0.0013(18) -0.0008(16) -0.0063(17) C6 0.0240(17) 0.0187(16) 0.0173(19) -0.0001(14) -0.0014(15) -0.0028(13) C12 0.0250(18) 0.0242(18) 0.0149(19) 0.0012(15) 0.0001(14) -0.0022(14) C3 0.0230(18) 0.0218(18) 0.025(2) 0.0024(15) -0.0003(16) 0.0002(14) C5 0.0237(18) 0.0268(19) 0.022(2) 0.0016(16) -0.0028(15) -0.0019(14) C1 0.0206(17) 0.0189(16) 0.0165(19) 0.0000(14) -0.0017(14) -0.0023(13) C2 0.0265(18) 0.0196(17) 0.0155(19) 0.0028(14) -0.0012(14) -0.0003(14) C19 0.045(3) 0.028(2) 0.032(3) 0.0061(19) 0.012(2) 0.0126(19) C11 0.0226(18) 0.0203(17) 0.016(2) 0.0033(14) 0.0022(14) -0.0037(13) C7 0.032(2) 0.0224(19) 0.024(2) -0.0037(16) -0.0047(17) -0.0011(16) C16 0.052(3) 0.039(2) 0.019(3) -0.0052(18) 0.0015(19) 0.011(2) C17 0.054(3) 0.041(3) 0.024(3) 0.0052(19) 0.016(2) 0.018(2) C13 0.035(2) 0.0203(18) 0.025(2) 0.0020(16) 0.0084(18) -0.0012(15) C14 0.032(2) 0.031(2) 0.035(3) 0.0087(19) 0.012(2) 0.0036(18) C15 0.0204(18) 0.040(2) 0.028(3) 0.0106(19) 0.0041(16) 0.0015(16) C20 0.050(3) 0.026(2) 0.028(3) -0.0028(18) 0.007(2) 0.0062(19) C18 0.038(3) 0.043(3) 0.040(3) 0.009(2) 0.014(2) 0.016(2) C4 0.027(2) 0.027(2) 0.029(3) 0.0055(17) -0.0010(17) -0.0053(15) C21 0.0238(18) 0.0155(16) 0.019(2) -0.0034(14) -0.0030(14) -0.0005(13) C22 0.052(3) 0.0168(18) 0.020(2) 0.0000(15) -0.007(2) -0.0007(17) C26 0.044(3) 0.026(2) 0.025(2) 0.0005(17) 0.0045(19) -0.0040(18) C27 0.032(2) 0.0188(17) 0.019(2) 0.0046(14) 0.0056(16) 0.0024(15) C29 0.073(4) 0.024(2) 0.037(3) 0.007(2) 0.017(3) 0.015(2) C28 0.054(3) 0.0188(19) 0.027(2) 0.0013(16) 0.010(2) 0.0039(19) C32 0.026(2) 0.028(2) 0.024(2) 0.0118(17) 0.0009(16) 0.0019(15) Au1 0.02743(8) 0.02210(8) 0.02003(9) -0.00439(6) -0.00017(6) -0.00707(5) Fe1 0.0266(3) 0.0219(3) 0.0187(3) 0.0034(2) 0.0018(2) 0.0035(2) P1 0.0252(5) 0.0157(4) 0.0165(5) -0.0021(3) -0.0003(4) -0.0014(3) Cl1 0.0342(5) 0.0378(6) 0.0359(7) -0.0047(5) -0.0044(4) -0.0160(4) C23 0.057(3) 0.024(2) 0.031(3) -0.0077(18) -0.009(2) 0.0033(19) C24 0.047(3) 0.039(3) 0.021(2) -0.0128(19) -0.007(2) 0.014(2) C25 0.050(3) 0.039(3) 0.023(3) -0.002(2) 0.009(2) -0.001(2) C31 0.035(2) 0.044(3) 0.038(3) 0.017(2) 0.003(2) 0.009(2) C30 0.066(4) 0.040(3) 0.037(3) 0.019(2) 0.018(3) 0.028(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 C8 C9 1.363(7) . ? C8 C7 1.416(6) . ? C10 C9 1.413(7) . ? C10 C15 1.421(7) . ? C10 C11 1.436(6) . ? C6 C7 1.385(6) . ? C6 C11 1.430(6) . ? C6 C2 1.482(6) . ? C12 C13 1.376(6) . ? C12 C11 1.419(6) . ? C3 C4 1.421(6) . ? C3 C2 1.431(6) . ? C3 Fe1 2.066(4) . ? C5 C4 1.430(6) . ? C5 C1 1.441(5) . ? C5 Fe1 2.044(5) . ? C1 C2 1.459(6) . ? C1 P1 1.780(4) . ? C1 Fe1 2.039(4) . ? C2 Fe1 2.062(4) . ? C19 C20 1.421(8) . ? C19 C18 1.432(8) . ? C19 Fe1 2.047(5) . ? C16 C17 1.405(9) . ? C16 C20 1.434(7) . ? C16 Fe1 2.064(5) . ? C17 C18 1.416(8) . ? C17 Fe1 2.052(5) . ? C13 C14 1.392(7) . ? C14 C15 1.383(8) . ? C20 Fe1 2.063(5) . ? C18 Fe1 2.062(5) . ? C4 Fe1 2.054(5) . ? C21 C22 1.382(5) . ? C21 C26 1.402(6) . ? C21 P1 1.812(4) . ? C22 C23 1.391(7) . ? C26 C25 1.378(7) . ? C27 C28 1.395(6) . ? C27 C32 1.407(7) . ? C27 P1 1.808(4) . ? C29 C30 1.386(11) . ? C29 C28 1.383(7) . ? C32 C31 1.404(6) . ? Au1 P1 2.2278(11) . ? Au1 Cl1 2.2845(11) . ? C23 C24 1.380(8) . ? C24 C25 1.377(8) . ? C31 C30 1.377(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 C8 C7 120.4(4) . . ? C9 C10 C15 121.5(4) . . ? C9 C10 C11 119.2(4) . . ? C15 C10 C11 119.2(4) . . ? C8 C9 C10 120.8(4) . . ? C7 C6 C11 119.0(4) . . ? C7 C6 C2 122.7(4) . . ? C11 C6 C2 118.3(3) . . ? C13 C12 C11 120.5(4) . . ? C4 C3 C2 109.1(4) . . ? C4 C3 Fe1 69.4(3) . . ? C2 C3 Fe1 69.6(2) . . ? C4 C5 C1 107.8(4) . . ? C4 C5 Fe1 70.0(3) . . ? C1 C5 Fe1 69.1(3) . . ? C5 C1 C2 107.7(4) . . ? C5 C1 P1 125.0(3) . . ? C2 C1 P1 127.2(3) . . ? C5 C1 Fe1 69.5(3) . . ? C2 C1 Fe1 70.0(2) . . ? P1 C1 Fe1 127.4(2) . . ? C3 C2 C1 106.9(4) . . ? C3 C2 C6 125.2(4) . . ? C1 C2 C6 127.6(4) . . ? C3 C2 Fe1 69.9(2) . . ? C1 C2 Fe1 68.3(2) . . ? C6 C2 Fe1 131.5(3) . . ? C20 C19 C18 107.8(5) . . ? C20 C19 Fe1 70.4(3) . . ? C18 C19 Fe1 70.2(3) . . ? C12 C11 C6 122.3(4) . . ? C12 C11 C10 118.5(4) . . ? C6 C11 C10 119.3(4) . . ? C6 C7 C8 121.3(4) . . ? C17 C16 C20 108.0(5) . . ? C17 C16 Fe1 69.6(3) . . ? C20 C16 Fe1 69.6(3) . . ? C16 C17 C18 108.9(5) . . ? C16 C17 Fe1 70.5(3) . . ? C18 C17 Fe1 70.2(3) . . ? C12 C13 C14 121.2(4) . . ? C15 C14 C13 120.5(4) . . ? C14 C15 C10 120.1(4) . . ? C19 C20 C16 107.6(5) . . ? C19 C20 Fe1 69.2(3) . . ? C16 C20 Fe1 69.7(3) . . ? C17 C18 C19 107.6(5) . . ? C17 C18 Fe1 69.5(3) . . ? C19 C18 Fe1 69.0(3) . . ? C3 C4 C5 108.5(4) . . ? C3 C4 Fe1 70.3(3) . . ? C5 C4 Fe1 69.2(3) . . ? C22 C21 C26 118.4(4) . . ? C22 C21 P1 124.0(4) . . ? C26 C21 P1 117.5(3) . . ? C21 C22 C23 120.2(5) . . ? C25 C26 C21 121.3(4) . . ? C28 C27 C32 119.5(4) . . ? C28 C27 P1 119.1(4) . . ? C32 C27 P1 121.3(3) . . ? C30 C29 C28 120.1(5) . . ? C29 C28 C27 120.5(6) . . ? C31 C32 C27 119.0(5) . . ? P1 Au1 Cl1 174.16(5) . . ? C1 Fe1 C5 41.33(16) . . ? C1 Fe1 C19 115.8(2) . . ? C5 Fe1 C19 108.2(2) . . ? C1 Fe1 C17 175.1(2) . . ? C5 Fe1 C17 141.4(2) . . ? C19 Fe1 C17 68.2(2) . . ? C1 Fe1 C4 69.06(18) . . ? C5 Fe1 C4 40.85(18) . . ? C19 Fe1 C4 130.8(2) . . ? C17 Fe1 C4 110.8(2) . . ? C1 Fe1 C2 41.69(16) . . ? C5 Fe1 C2 69.56(17) . . ? C19 Fe1 C2 148.93(19) . . ? C17 Fe1 C2 133.5(2) . . ? C4 Fe1 C2 68.70(17) . . ? C1 Fe1 C20 113.07(19) . . ? C5 Fe1 C20 135.2(2) . . ? C19 Fe1 C20 40.5(2) . . ? C17 Fe1 C20 67.8(2) . . ? C4 Fe1 C20 171.3(2) . . ? C2 Fe1 C20 118.8(2) . . ? C1 Fe1 C18 144.6(2) . . ? C5 Fe1 C18 111.2(2) . . ? C19 Fe1 C18 40.8(2) . . ? C17 Fe1 C18 40.2(2) . . ? C4 Fe1 C18 105.2(2) . . ? C2 Fe1 C18 170.2(2) . . ? C20 Fe1 C18 68.0(2) . . ? C1 Fe1 C3 68.90(17) . . ? C5 Fe1 C3 68.54(18) . . ? C19 Fe1 C3 169.4(2) . . ? C17 Fe1 C3 107.7(2) . . ? C4 Fe1 C3 40.36(17) . . ? C2 Fe1 C3 40.56(16) . . ? C20 Fe1 C3 148.3(2) . . ? C18 Fe1 C3 130.0(2) . . ? C1 Fe1 C16 137.8(2) . . ? C5 Fe1 C16 175.8(2) . . ? C19 Fe1 C16 68.2(2) . . ? C17 Fe1 C16 39.9(3) . . ? C4 Fe1 C16 143.1(2) . . ? C2 Fe1 C16 112.3(2) . . ? C20 Fe1 C16 40.7(2) . . ? C18 Fe1 C16 67.6(3) . . ? C3 Fe1 C16 115.4(2) . . ? C1 P1 C27 106.16(19) . . ? C1 P1 C21 106.19(19) . . ? C27 P1 C21 104.8(2) . . ? C1 P1 Au1 117.63(14) . . ? C27 P1 Au1 112.19(15) . . ? C21 P1 Au1 108.95(14) . . ? C24 C23 C22 120.2(4) . . ? C25 C24 C23 120.4(5) . . ? C24 C25 C26 119.4(5) . . ? C30 C31 C32 120.5(6) . . ? C31 C30 C29 120.3(5) . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.432 _refine_diff_density_min -0.648 _refine_diff_density_rms 0.106 _database_code_depnum_ccdc_archive 'CCDC 933753' ####################################################################### # # 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_mo_rs311_0m #TrackingRef 'web_deposit_cif_file_3_AntonioM.Echavarren_1365746154.mo_RS311_0mX.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H33 Au Cl Fe P' _chemical_formula_weight 688.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P3(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' _cell_length_a 9.7478(14) _cell_length_b 9.7478(14) _cell_length_c 23.296(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1917.0(5) _cell_formula_units_Z 3 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9975 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 36.38 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.790 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1014 _exptl_absorpt_coefficient_mu 6.482 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3572 _exptl_absorpt_correction_T_max 0.3572 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 21902 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0500 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 36.43 _reflns_number_total 10116 _reflns_number_gt 9859 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0795P)^2^+6.7436P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _chemical_absolute_configuration ad _refine_ls_abs_structure_Flack 0.010(6) _refine_ls_number_reflns 10116 _refine_ls_number_parameters 295 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1231 _refine_ls_wR_factor_gt 0.1219 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au -0.080178(18) 0.73927(2) 0.184280(9) 0.01045(5) Uani 1 1 d . . . C1 C 0.3243(5) 0.9804(5) 0.1940(2) 0.0087(7) Uani 1 1 d . . . C2 C 0.4898(6) 1.0310(6) 0.2014(3) 0.0133(8) Uani 1 1 d . . . H2 H 0.5310 0.9669 0.2149 0.016 Uiso 1 1 calc R . . C3 C 0.5805(6) 1.1917(6) 0.1850(3) 0.0142(9) Uani 1 1 d . . . H3 H 0.6929 1.2538 0.1854 0.017 Uiso 1 1 calc R . . C4 C 0.4741(7) 1.2447(6) 0.1678(3) 0.0137(9) Uani 1 1 d . . . H4 H 0.5040 1.3486 0.1552 0.016 Uiso 1 1 calc R . . C5 C 0.3169(6) 1.1173(5) 0.1727(2) 0.0097(7) Uani 1 1 d . . . C6 C 0.1750(6) 1.1248(6) 0.1544(2) 0.0113(8) Uani 1 1 d . . . C7 C 0.1626(6) 1.1653(6) 0.0961(2) 0.0120(8) Uani 1 1 d . . . C8 C 0.2814(7) 1.2020(7) 0.0543(3) 0.0155(9) Uani 1 1 d . . . H8 H 0.3752 1.2012 0.0647 0.019 Uiso 1 1 calc R . . C9 C 0.2633(8) 1.2386(8) -0.0011(3) 0.0206(11) Uani 1 1 d . . . H9 H 0.3441 1.2617 -0.0285 0.025 Uiso 1 1 calc R . . C10 C 0.1270(9) 1.2423(8) -0.0175(3) 0.0219(11) Uani 1 1 d . . . H10 H 0.1166 1.2694 -0.0558 0.026 Uiso 1 1 calc R . . C11 C 0.0087(8) 1.2069(7) 0.0214(3) 0.0200(11) Uani 1 1 d . . . H11 H -0.0839 1.2085 0.0098 0.024 Uiso 1 1 calc R . . C12 C 0.0229(6) 1.1678(6) 0.0789(3) 0.0145(9) Uani 1 1 d . . . C13 C -0.0984(6) 1.1328(7) 0.1195(3) 0.0159(9) Uani 1 1 d . . . H13 H -0.1915 1.1335 0.1080 0.019 Uiso 1 1 calc R . . C14 C -0.0828(7) 1.0979(6) 0.1751(3) 0.0177(10) Uani 1 1 d . . . H14 H -0.1643 1.0760 0.2021 0.021 Uiso 1 1 calc R . . C15 C 0.0543(6) 1.0941(6) 0.1927(3) 0.0136(8) Uani 1 1 d . . . H15 H 0.0637 1.0700 0.2316 0.016 Uiso 1 1 calc R . . C16 C 0.2976(9) 1.1446(8) 0.3240(3) 0.0236(12) Uani 1 1 d . . . H16 H 0.1856 1.0605 0.3315 0.028 Uiso 1 1 calc R . . C17 C 0.4384(9) 1.1386(8) 0.3390(3) 0.0234(12) Uani 1 1 d . . . H17 H 0.4414 1.0489 0.3586 0.028 Uiso 1 1 calc R . . C18 C 0.5716(9) 1.2822(9) 0.3202(3) 0.0254(13) Uani 1 1 d . . . H18 H 0.6850 1.3112 0.3246 0.031 Uiso 1 1 calc R . . C19 C 0.5167(10) 1.3768(8) 0.2938(3) 0.0254(13) Uani 1 1 d . . . H19 H 0.5846 1.4847 0.2771 0.030 Uiso 1 1 calc R . . C20 C 0.3482(9) 1.2931(9) 0.2964(3) 0.0241(12) Uani 1 1 d . . . H20 H 0.2774 1.3317 0.2814 0.029 Uiso 1 1 calc R . . C21 C 0.2025(6) 0.7025(6) 0.1209(3) 0.0131(8) Uani 1 1 d . . . C22 C 0.0519(8) 0.5506(6) 0.1011(3) 0.0178(10) Uani 1 1 d . . . H22A H 0.0725 0.5155 0.0643 0.027 Uiso 1 1 calc R . . H22B H -0.0351 0.5728 0.0965 0.027 Uiso 1 1 calc R . . H22C H 0.0227 0.4672 0.1299 0.027 Uiso 1 1 calc R . . C23 C 0.2366(7) 0.8331(7) 0.0770(3) 0.0152(9) Uani 1 1 d . . . H23A H 0.3413 0.9250 0.0845 0.023 Uiso 1 1 calc R . . H23B H 0.1558 0.8645 0.0802 0.023 Uiso 1 1 calc R . . H23C H 0.2344 0.7933 0.0382 0.023 Uiso 1 1 calc R . . C24 C 0.3424(8) 0.6724(8) 0.1225(3) 0.0205(11) Uani 1 1 d . . . H24A H 0.3650 0.6514 0.0835 0.031 Uiso 1 1 calc R . . H24B H 0.3157 0.5806 0.1469 0.031 Uiso 1 1 calc R . . H24C H 0.4358 0.7659 0.1380 0.031 Uiso 1 1 calc R . . C25 C 0.1780(6) 0.6655(6) 0.2546(2) 0.0117(8) Uani 1 1 d . . . C26 C 0.0721(7) 0.4861(7) 0.2436(3) 0.0195(11) Uani 1 1 d . . . H26A H 0.1169 0.4539 0.2123 0.029 Uiso 1 1 calc R . . H26B H -0.0347 0.4631 0.2331 0.029 Uiso 1 1 calc R . . H26C H 0.0667 0.4275 0.2785 0.029 Uiso 1 1 calc R . . C27 C 0.3448(7) 0.7022(7) 0.2713(3) 0.0162(9) Uani 1 1 d . . . H27A H 0.3379 0.6285 0.3013 0.024 Uiso 1 1 calc R . . H27B H 0.4053 0.8111 0.2857 0.024 Uiso 1 1 calc R . . H27C H 0.3982 0.6905 0.2375 0.024 Uiso 1 1 calc R . . C28 C 0.1064(8) 0.7092(8) 0.3055(3) 0.0196(10) Uani 1 1 d . . . H28A H 0.1191 0.6618 0.3408 0.029 Uiso 1 1 calc R . . H28B H -0.0065 0.6690 0.2984 0.029 Uiso 1 1 calc R . . H28C H 0.1611 0.8247 0.3097 0.029 Uiso 1 1 calc R . . Cl1 Cl -0.33826(15) 0.67831(17) 0.17336(8) 0.0184(2) Uani 1 1 d . . . Fe1 Fe 0.42875(10) 1.16715(9) 0.25063(4) 0.01185(13) Uani 1 1 d . . . P1 P 0.16538(14) 0.77559(15) 0.19084(6) 0.00809(19) 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 0.00725(7) 0.01070(7) 0.01458(8) -0.00020(6) -0.00145(6) 0.00536(6) C1 0.0057(14) 0.0093(16) 0.011(2) 0.0018(13) 0.0015(13) 0.0037(13) C2 0.0115(18) 0.0139(19) 0.015(2) -0.0027(16) -0.0027(16) 0.0066(16) C3 0.0100(17) 0.0120(19) 0.018(3) -0.0011(16) -0.0023(16) 0.0033(15) C4 0.016(2) 0.0094(17) 0.013(2) -0.0013(15) -0.0026(16) 0.0042(15) C5 0.0125(17) 0.0092(16) 0.008(2) -0.0004(13) -0.0022(14) 0.0059(14) C6 0.0120(17) 0.0112(17) 0.014(2) 0.0002(15) -0.0007(15) 0.0083(14) C7 0.0135(18) 0.0108(17) 0.012(2) -0.0003(15) -0.0030(15) 0.0061(15) C8 0.0134(19) 0.019(2) 0.013(3) 0.0030(18) 0.0005(17) 0.0066(17) C9 0.026(3) 0.025(3) 0.011(3) 0.003(2) -0.0003(19) 0.012(2) C10 0.030(3) 0.022(2) 0.013(3) 0.0017(19) -0.007(2) 0.012(2) C11 0.025(3) 0.018(2) 0.020(3) 0.0005(19) -0.009(2) 0.013(2) C12 0.0154(19) 0.0110(17) 0.017(2) 0.0000(16) -0.0047(17) 0.0064(16) C13 0.0120(18) 0.015(2) 0.024(3) 0.0008(18) -0.0028(17) 0.0093(16) C14 0.014(2) 0.014(2) 0.028(3) 0.0031(19) 0.0041(19) 0.0093(17) C15 0.0146(19) 0.0118(18) 0.015(2) 0.0009(16) 0.0002(16) 0.0073(16) C16 0.035(3) 0.025(3) 0.014(3) -0.002(2) 0.006(2) 0.018(3) C17 0.037(3) 0.023(3) 0.012(3) -0.001(2) -0.005(2) 0.016(3) C18 0.032(3) 0.028(3) 0.018(3) -0.011(2) -0.014(3) 0.016(3) C19 0.040(4) 0.016(2) 0.016(3) -0.008(2) -0.006(2) 0.011(2) C20 0.039(3) 0.026(3) 0.018(3) -0.009(2) -0.006(2) 0.024(3) C21 0.017(2) 0.0146(19) 0.012(2) -0.0023(16) -0.0033(16) 0.0109(16) C22 0.025(2) 0.0124(19) 0.015(3) -0.0070(17) -0.008(2) 0.0086(18) C23 0.020(2) 0.017(2) 0.011(2) -0.0011(16) 0.0010(17) 0.0108(18) C24 0.021(2) 0.027(3) 0.023(3) -0.004(2) -0.002(2) 0.019(2) C25 0.0131(18) 0.0159(19) 0.009(2) 0.0016(15) -0.0014(15) 0.0097(16) C26 0.020(2) 0.013(2) 0.023(3) 0.0006(19) -0.006(2) 0.0066(18) C27 0.015(2) 0.021(2) 0.016(3) 0.0039(18) -0.0022(17) 0.0114(18) C28 0.024(3) 0.027(3) 0.016(3) 0.005(2) 0.003(2) 0.018(2) Cl1 0.0084(4) 0.0182(5) 0.0296(8) -0.0033(5) -0.0038(4) 0.0075(4) Fe1 0.0152(3) 0.0112(3) 0.0097(3) -0.0027(2) -0.0033(2) 0.0069(2) P1 0.0075(4) 0.0085(4) 0.0097(5) -0.0011(4) -0.0015(4) 0.0051(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.2429(12) . ? Au1 Cl1 2.2917(13) . ? C1 C2 1.442(7) . ? C1 C5 1.459(6) . ? C1 P1 1.816(5) . ? C1 Fe1 2.058(5) . ? C2 C3 1.412(8) . ? C2 Fe1 2.055(6) . ? C3 C4 1.428(8) . ? C3 Fe1 2.056(6) . ? C4 C5 1.414(7) . ? C4 Fe1 2.038(6) . ? C5 C6 1.483(7) . ? C5 Fe1 2.048(5) . ? C6 C15 1.385(8) . ? C6 C7 1.436(8) . ? C7 C8 1.416(8) . ? C7 C12 1.431(7) . ? C8 C9 1.373(9) . ? C9 C10 1.400(10) . ? C10 C11 1.368(11) . ? C11 C12 1.418(9) . ? C12 C13 1.417(9) . ? C13 C14 1.367(9) . ? C14 C15 1.416(8) . ? C16 C20 1.427(10) . ? C16 C17 1.446(11) . ? C16 Fe1 2.078(7) . ? C17 C18 1.421(11) . ? C17 Fe1 2.087(7) . ? C18 C19 1.417(11) . ? C18 Fe1 2.064(7) . ? C19 C20 1.424(11) . ? C19 Fe1 2.042(6) . ? C20 Fe1 2.056(6) . ? C21 C24 1.532(8) . ? C21 C23 1.536(8) . ? C21 C22 1.545(8) . ? C21 P1 1.884(6) . ? C25 C27 1.530(7) . ? C25 C28 1.540(8) . ? C25 C26 1.544(8) . ? C25 P1 1.873(5) . ? 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 Cl1 174.28(5) . . ? C2 C1 C5 106.6(4) . . ? C2 C1 P1 125.1(4) . . ? C5 C1 P1 125.9(3) . . ? C2 C1 Fe1 69.4(3) . . ? C5 C1 Fe1 68.8(3) . . ? P1 C1 Fe1 140.5(3) . . ? C3 C2 C1 108.7(5) . . ? C3 C2 Fe1 70.0(3) . . ? C1 C2 Fe1 69.6(3) . . ? C2 C3 C4 108.1(4) . . ? C2 C3 Fe1 69.8(3) . . ? C4 C3 Fe1 68.9(3) . . ? C5 C4 C3 108.9(4) . . ? C5 C4 Fe1 70.1(3) . . ? C3 C4 Fe1 70.3(3) . . ? C4 C5 C1 107.6(4) . . ? C4 C5 C6 124.1(4) . . ? C1 C5 C6 128.1(4) . . ? C4 C5 Fe1 69.4(3) . . ? C1 C5 Fe1 69.5(3) . . ? C6 C5 Fe1 129.9(4) . . ? C15 C6 C7 119.3(5) . . ? C15 C6 C5 121.1(5) . . ? C7 C6 C5 119.6(5) . . ? C8 C7 C12 117.9(5) . . ? C8 C7 C6 123.4(5) . . ? C12 C7 C6 118.8(5) . . ? C9 C8 C7 121.2(5) . . ? C8 C9 C10 120.6(6) . . ? C11 C10 C9 120.3(6) . . ? C10 C11 C12 120.6(6) . . ? C13 C12 C11 120.9(5) . . ? C13 C12 C7 119.7(5) . . ? C11 C12 C7 119.4(6) . . ? C14 C13 C12 120.6(5) . . ? C13 C14 C15 120.3(5) . . ? C6 C15 C14 121.2(6) . . ? C20 C16 C17 107.3(6) . . ? C20 C16 Fe1 69.0(4) . . ? C17 C16 Fe1 70.0(4) . . ? C18 C17 C16 107.7(6) . . ? C18 C17 Fe1 69.1(4) . . ? C16 C17 Fe1 69.4(4) . . ? C19 C18 C17 108.6(7) . . ? C19 C18 Fe1 69.0(4) . . ? C17 C18 Fe1 70.8(4) . . ? C18 C19 C20 108.1(6) . . ? C18 C19 Fe1 70.7(4) . . ? C20 C19 Fe1 70.2(4) . . ? C19 C20 C16 108.4(6) . . ? C19 C20 Fe1 69.1(4) . . ? C16 C20 Fe1 70.7(4) . . ? C24 C21 C23 109.3(5) . . ? C24 C21 C22 109.5(5) . . ? C23 C21 C22 107.7(5) . . ? C24 C21 P1 114.2(4) . . ? C23 C21 P1 105.4(3) . . ? C22 C21 P1 110.5(4) . . ? C27 C25 C28 108.4(5) . . ? C27 C25 C26 109.7(4) . . ? C28 C25 C26 107.6(5) . . ? C27 C25 P1 115.7(4) . . ? C28 C25 P1 106.5(3) . . ? C26 C25 P1 108.6(4) . . ? C4 Fe1 C19 101.0(3) . . ? C4 Fe1 C5 40.5(2) . . ? C19 Fe1 C5 125.6(3) . . ? C4 Fe1 C2 68.4(2) . . ? C19 Fe1 C2 144.0(3) . . ? C5 Fe1 C2 69.1(2) . . ? C4 Fe1 C1 69.0(2) . . ? C19 Fe1 C1 167.2(3) . . ? C5 Fe1 C1 41.64(19) . . ? C2 Fe1 C1 41.04(19) . . ? C4 Fe1 C20 110.3(3) . . ? C19 Fe1 C20 40.7(3) . . ? C5 Fe1 C20 106.5(2) . . ? C2 Fe1 C20 174.9(3) . . ? C1 Fe1 C20 133.9(3) . . ? C4 Fe1 C3 40.8(2) . . ? C19 Fe1 C3 109.4(3) . . ? C5 Fe1 C3 68.6(2) . . ? C2 Fe1 C3 40.2(2) . . ? C1 Fe1 C3 68.64(19) . . ? C20 Fe1 C3 141.6(3) . . ? C4 Fe1 C18 125.4(3) . . ? C19 Fe1 C18 40.4(3) . . ? C5 Fe1 C18 163.7(3) . . ? C2 Fe1 C18 117.1(3) . . ? C1 Fe1 C18 152.2(2) . . ? C20 Fe1 C18 67.9(3) . . ? C3 Fe1 C18 105.6(3) . . ? C4 Fe1 C16 145.6(3) . . ? C19 Fe1 C16 68.2(3) . . ? C5 Fe1 C16 118.5(3) . . ? C2 Fe1 C16 138.8(3) . . ? C1 Fe1 C16 115.3(3) . . ? C20 Fe1 C16 40.4(3) . . ? C3 Fe1 C16 172.7(3) . . ? C18 Fe1 C16 67.9(3) . . ? C4 Fe1 C17 165.4(3) . . ? C19 Fe1 C17 67.9(3) . . ? C5 Fe1 C17 153.9(3) . . ? C2 Fe1 C17 114.7(3) . . ? C1 Fe1 C17 123.3(2) . . ? C20 Fe1 C17 67.9(3) . . ? C3 Fe1 C17 132.2(3) . . ? C18 Fe1 C17 40.0(3) . . ? C16 Fe1 C17 40.6(3) . . ? C1 P1 C25 109.4(2) . . ? C1 P1 C21 103.4(2) . . ? C25 P1 C21 112.9(2) . . ? C1 P1 Au1 115.64(15) . . ? C25 P1 Au1 109.54(17) . . ? C21 P1 Au1 105.83(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 C2 C3 -0.2(6) . . . . ? P1 C1 C2 C3 162.8(4) . . . . ? Fe1 C1 C2 C3 -59.2(4) . . . . ? C5 C1 C2 Fe1 59.0(4) . . . . ? P1 C1 C2 Fe1 -138.0(4) . . . . ? C1 C2 C3 C4 0.6(7) . . . . ? Fe1 C2 C3 C4 -58.4(4) . . . . ? C1 C2 C3 Fe1 59.0(4) . . . . ? C2 C3 C4 C5 -0.7(7) . . . . ? Fe1 C3 C4 C5 -59.7(4) . . . . ? C2 C3 C4 Fe1 59.0(4) . . . . ? C3 C4 C5 C1 0.5(6) . . . . ? Fe1 C4 C5 C1 -59.2(4) . . . . ? C3 C4 C5 C6 -175.3(5) . . . . ? Fe1 C4 C5 C6 124.9(5) . . . . ? C3 C4 C5 Fe1 59.8(4) . . . . ? C2 C1 C5 C4 -0.2(6) . . . . ? P1 C1 C5 C4 -163.1(4) . . . . ? Fe1 C1 C5 C4 59.1(4) . . . . ? C2 C1 C5 C6 175.4(5) . . . . ? P1 C1 C5 C6 12.5(8) . . . . ? Fe1 C1 C5 C6 -125.3(6) . . . . ? C2 C1 C5 Fe1 -59.3(4) . . . . ? P1 C1 C5 Fe1 137.8(4) . . . . ? C4 C5 C6 C15 -122.6(6) . . . . ? C1 C5 C6 C15 62.5(7) . . . . ? Fe1 C5 C6 C15 -31.9(7) . . . . ? C4 C5 C6 C7 57.2(7) . . . . ? C1 C5 C6 C7 -117.8(6) . . . . ? Fe1 C5 C6 C7 147.8(4) . . . . ? C15 C6 C7 C8 178.6(5) . . . . ? C5 C6 C7 C8 -1.2(8) . . . . ? C15 C6 C7 C12 -1.9(7) . . . . ? C5 C6 C7 C12 178.3(4) . . . . ? C12 C7 C8 C9 -0.1(8) . . . . ? C6 C7 C8 C9 179.4(6) . . . . ? C7 C8 C9 C10 0.7(10) . . . . ? C8 C9 C10 C11 -1.0(10) . . . . ? C9 C10 C11 C12 0.7(10) . . . . ? C10 C11 C12 C13 179.3(6) . . . . ? C10 C11 C12 C7 -0.1(8) . . . . ? C8 C7 C12 C13 -179.6(5) . . . . ? C6 C7 C12 C13 0.9(7) . . . . ? C8 C7 C12 C11 -0.2(7) . . . . ? C6 C7 C12 C11 -179.7(5) . . . . ? C11 C12 C13 C14 -178.9(5) . . . . ? C7 C12 C13 C14 0.5(8) . . . . ? C12 C13 C14 C15 -0.9(8) . . . . ? C7 C6 C15 C14 1.6(8) . . . . ? C5 C6 C15 C14 -178.6(5) . . . . ? C13 C14 C15 C6 -0.2(8) . . . . ? C20 C16 C17 C18 -0.4(8) . . . . ? Fe1 C16 C17 C18 58.7(5) . . . . ? C20 C16 C17 Fe1 -59.1(5) . . . . ? C16 C17 C18 C19 0.0(8) . . . . ? Fe1 C17 C18 C19 58.8(5) . . . . ? C16 C17 C18 Fe1 -58.9(5) . . . . ? C17 C18 C19 C20 0.5(8) . . . . ? Fe1 C18 C19 C20 60.5(5) . . . . ? C17 C18 C19 Fe1 -60.0(5) . . . . ? C18 C19 C20 C16 -0.8(8) . . . . ? Fe1 C19 C20 C16 60.0(5) . . . . ? C18 C19 C20 Fe1 -60.8(5) . . . . ? C17 C16 C20 C19 0.7(8) . . . . ? Fe1 C16 C20 C19 -59.1(5) . . . . ? C17 C16 C20 Fe1 59.8(5) . . . . ? C5 C4 Fe1 C19 -133.3(4) . . . . ? C3 C4 Fe1 C19 107.0(4) . . . . ? C3 C4 Fe1 C5 -119.7(4) . . . . ? C5 C4 Fe1 C2 82.7(3) . . . . ? C3 C4 Fe1 C2 -37.0(3) . . . . ? C5 C4 Fe1 C1 38.5(3) . . . . ? C3 C4 Fe1 C1 -81.2(3) . . . . ? C5 C4 Fe1 C20 -92.0(4) . . . . ? C3 C4 Fe1 C20 148.3(3) . . . . ? C5 C4 Fe1 C3 119.7(4) . . . . ? C5 C4 Fe1 C18 -168.7(3) . . . . ? C3 C4 Fe1 C18 71.5(4) . . . . ? C5 C4 Fe1 C16 -65.9(5) . . . . ? C3 C4 Fe1 C16 174.4(4) . . . . ? C5 C4 Fe1 C17 -171.9(9) . . . . ? C3 C4 Fe1 C17 68.3(11) . . . . ? C18 C19 Fe1 C4 -133.1(5) . . . . ? C20 C19 Fe1 C4 108.4(4) . . . . ? C18 C19 Fe1 C5 -168.6(4) . . . . ? C20 C19 Fe1 C5 72.9(5) . . . . ? C18 C19 Fe1 C2 -64.9(7) . . . . ? C20 C19 Fe1 C2 176.6(4) . . . . ? C18 C19 Fe1 C1 -170.4(11) . . . . ? C20 C19 Fe1 C1 71.1(13) . . . . ? C18 C19 Fe1 C20 118.5(7) . . . . ? C18 C19 Fe1 C3 -91.6(5) . . . . ? C20 C19 Fe1 C3 149.9(4) . . . . ? C20 C19 Fe1 C18 -118.5(7) . . . . ? C18 C19 Fe1 C16 81.1(5) . . . . ? C20 C19 Fe1 C16 -37.4(4) . . . . ? C18 C19 Fe1 C17 37.1(5) . . . . ? C20 C19 Fe1 C17 -81.4(5) . . . . ? C1 C5 Fe1 C4 119.1(4) . . . . ? C6 C5 Fe1 C4 -117.8(6) . . . . ? C4 C5 Fe1 C19 61.5(4) . . . . ? C1 C5 Fe1 C19 -179.4(4) . . . . ? C6 C5 Fe1 C19 -56.3(6) . . . . ? C4 C5 Fe1 C2 -80.8(3) . . . . ? C1 C5 Fe1 C2 38.2(3) . . . . ? C6 C5 Fe1 C2 161.4(5) . . . . ? C4 C5 Fe1 C1 -119.1(4) . . . . ? C6 C5 Fe1 C1 123.1(6) . . . . ? C4 C5 Fe1 C20 102.0(4) . . . . ? C1 C5 Fe1 C20 -138.9(3) . . . . ? C6 C5 Fe1 C20 -15.8(5) . . . . ? C4 C5 Fe1 C3 -37.6(3) . . . . ? C1 C5 Fe1 C3 81.5(3) . . . . ? C6 C5 Fe1 C3 -155.4(5) . . . . ? C4 C5 Fe1 C18 34.5(11) . . . . ? C1 C5 Fe1 C18 153.6(9) . . . . ? C6 C5 Fe1 C18 -83.3(11) . . . . ? C4 C5 Fe1 C16 144.0(3) . . . . ? C1 C5 Fe1 C16 -96.9(3) . . . . ? C6 C5 Fe1 C16 26.2(5) . . . . ? C4 C5 Fe1 C17 175.4(5) . . . . ? C1 C5 Fe1 C17 -65.5(6) . . . . ? C6 C5 Fe1 C17 57.6(7) . . . . ? C3 C2 Fe1 C4 37.6(3) . . . . ? C1 C2 Fe1 C4 -82.4(3) . . . . ? C3 C2 Fe1 C19 -41.0(6) . . . . ? C1 C2 Fe1 C19 -161.0(4) . . . . ? C3 C2 Fe1 C5 81.2(3) . . . . ? C1 C2 Fe1 C5 -38.8(3) . . . . ? C3 C2 Fe1 C1 120.0(5) . . . . ? C3 C2 Fe1 C20 113(3) . . . . ? C1 C2 Fe1 C20 -7(3) . . . . ? C1 C2 Fe1 C3 -120.0(5) . . . . ? C3 C2 Fe1 C18 -82.2(4) . . . . ? C1 C2 Fe1 C18 157.8(4) . . . . ? C3 C2 Fe1 C16 -169.0(4) . . . . ? C1 C2 Fe1 C16 71.0(5) . . . . ? C3 C2 Fe1 C17 -126.9(4) . . . . ? C1 C2 Fe1 C17 113.1(4) . . . . ? C2 C1 Fe1 C4 80.8(3) . . . . ? C5 C1 Fe1 C4 -37.5(3) . . . . ? P1 C1 Fe1 C4 -158.6(4) . . . . ? C2 C1 Fe1 C19 120.4(12) . . . . ? C5 C1 Fe1 C19 2.1(13) . . . . ? P1 C1 Fe1 C19 -119.1(12) . . . . ? C2 C1 Fe1 C5 118.3(4) . . . . ? P1 C1 Fe1 C5 -121.2(5) . . . . ? C5 C1 Fe1 C2 -118.3(4) . . . . ? P1 C1 Fe1 C2 120.6(5) . . . . ? C2 C1 Fe1 C20 179.2(4) . . . . ? C5 C1 Fe1 C20 60.9(4) . . . . ? P1 C1 Fe1 C20 -60.3(6) . . . . ? C2 C1 Fe1 C3 36.9(3) . . . . ? C5 C1 Fe1 C3 -81.4(3) . . . . ? P1 C1 Fe1 C3 157.4(5) . . . . ? C2 C1 Fe1 C18 -46.2(7) . . . . ? C5 C1 Fe1 C18 -164.5(6) . . . . ? P1 C1 Fe1 C18 74.4(7) . . . . ? C2 C1 Fe1 C16 -136.5(4) . . . . ? C5 C1 Fe1 C16 105.3(4) . . . . ? P1 C1 Fe1 C16 -15.9(5) . . . . ? C2 C1 Fe1 C17 -90.4(4) . . . . ? C5 C1 Fe1 C17 151.3(4) . . . . ? P1 C1 Fe1 C17 30.1(5) . . . . ? C19 C20 Fe1 C4 -83.2(4) . . . . ? C16 C20 Fe1 C4 157.4(4) . . . . ? C16 C20 Fe1 C19 -119.4(6) . . . . ? C19 C20 Fe1 C5 -125.8(4) . . . . ? C16 C20 Fe1 C5 114.8(4) . . . . ? C19 C20 Fe1 C2 -157(3) . . . . ? C16 C20 Fe1 C2 84(3) . . . . ? C19 C20 Fe1 C1 -163.1(4) . . . . ? C16 C20 Fe1 C1 77.5(5) . . . . ? C19 C20 Fe1 C3 -49.6(6) . . . . ? C16 C20 Fe1 C3 -169.0(4) . . . . ? C19 C20 Fe1 C18 37.9(5) . . . . ? C16 C20 Fe1 C18 -81.5(5) . . . . ? C19 C20 Fe1 C16 119.4(6) . . . . ? C19 C20 Fe1 C17 81.3(5) . . . . ? C16 C20 Fe1 C17 -38.1(5) . . . . ? C2 C3 Fe1 C4 -119.8(4) . . . . ? C2 C3 Fe1 C19 155.9(4) . . . . ? C4 C3 Fe1 C19 -84.3(4) . . . . ? C2 C3 Fe1 C5 -82.5(3) . . . . ? C4 C3 Fe1 C5 37.3(3) . . . . ? C4 C3 Fe1 C2 119.8(4) . . . . ? C2 C3 Fe1 C1 -37.6(3) . . . . ? C4 C3 Fe1 C1 82.2(3) . . . . ? C2 C3 Fe1 C20 -172.4(4) . . . . ? C4 C3 Fe1 C20 -52.6(5) . . . . ? C2 C3 Fe1 C18 113.6(4) . . . . ? C4 C3 Fe1 C18 -126.6(3) . . . . ? C2 C3 Fe1 C16 86(2) . . . . ? C4 C3 Fe1 C16 -154.0(19) . . . . ? C2 C3 Fe1 C17 78.6(4) . . . . ? C4 C3 Fe1 C17 -161.6(3) . . . . ? C19 C18 Fe1 C4 61.6(6) . . . . ? C17 C18 Fe1 C4 -178.7(4) . . . . ? C17 C18 Fe1 C19 119.7(7) . . . . ? C19 C18 Fe1 C5 34.8(12) . . . . ? C17 C18 Fe1 C5 154.4(8) . . . . ? C19 C18 Fe1 C2 143.3(5) . . . . ? C17 C18 Fe1 C2 -97.1(5) . . . . ? C19 C18 Fe1 C1 175.4(5) . . . . ? C17 C18 Fe1 C1 -64.9(8) . . . . ? C19 C18 Fe1 C20 -38.2(5) . . . . ? C17 C18 Fe1 C20 81.5(5) . . . . ? C19 C18 Fe1 C3 101.7(5) . . . . ? C17 C18 Fe1 C3 -138.7(4) . . . . ? C19 C18 Fe1 C16 -81.9(5) . . . . ? C17 C18 Fe1 C16 37.7(4) . . . . ? C19 C18 Fe1 C17 -119.7(7) . . . . ? C20 C16 Fe1 C4 -39.6(7) . . . . ? C17 C16 Fe1 C4 -158.2(4) . . . . ? C20 C16 Fe1 C19 37.7(4) . . . . ? C17 C16 Fe1 C19 -80.9(4) . . . . ? C20 C16 Fe1 C5 -82.1(5) . . . . ? C17 C16 Fe1 C5 159.4(4) . . . . ? C20 C16 Fe1 C2 -172.3(4) . . . . ? C17 C16 Fe1 C2 69.2(6) . . . . ? C20 C16 Fe1 C1 -128.9(4) . . . . ? C17 C16 Fe1 C1 112.5(4) . . . . ? C17 C16 Fe1 C20 -118.6(6) . . . . ? C20 C16 Fe1 C3 109.9(19) . . . . ? C17 C16 Fe1 C3 -9(2) . . . . ? C20 C16 Fe1 C18 81.4(5) . . . . ? C17 C16 Fe1 C18 -37.2(4) . . . . ? C20 C16 Fe1 C17 118.6(6) . . . . ? C18 C17 Fe1 C4 4.1(13) . . . . ? C16 C17 Fe1 C4 123.4(10) . . . . ? C18 C17 Fe1 C19 -37.4(5) . . . . ? C16 C17 Fe1 C19 81.9(5) . . . . ? C18 C17 Fe1 C5 -164.0(5) . . . . ? C16 C17 Fe1 C5 -44.6(7) . . . . ? C18 C17 Fe1 C2 103.3(4) . . . . ? C16 C17 Fe1 C2 -137.3(4) . . . . ? C18 C17 Fe1 C1 149.6(4) . . . . ? C16 C17 Fe1 C1 -91.0(4) . . . . ? C18 C17 Fe1 C20 -81.5(5) . . . . ? C16 C17 Fe1 C20 37.9(4) . . . . ? C18 C17 Fe1 C3 59.2(5) . . . . ? C16 C17 Fe1 C3 178.5(4) . . . . ? C16 C17 Fe1 C18 119.4(6) . . . . ? C18 C17 Fe1 C16 -119.4(6) . . . . ? C2 C1 P1 C25 52.3(5) . . . . ? C5 C1 P1 C25 -147.9(4) . . . . ? Fe1 C1 P1 C25 -47.7(4) . . . . ? C2 C1 P1 C21 -68.2(5) . . . . ? C5 C1 P1 C21 91.6(5) . . . . ? Fe1 C1 P1 C21 -168.3(4) . . . . ? C2 C1 P1 Au1 176.6(4) . . . . ? C5 C1 P1 Au1 -23.6(5) . . . . ? Fe1 C1 P1 Au1 76.5(4) . . . . ? C27 C25 P1 C1 -41.7(5) . . . . ? C28 C25 P1 C1 78.9(4) . . . . ? C26 C25 P1 C1 -165.6(4) . . . . ? C27 C25 P1 C21 72.9(5) . . . . ? C28 C25 P1 C21 -166.5(4) . . . . ? C26 C25 P1 C21 -51.0(4) . . . . ? C27 C25 P1 Au1 -169.4(4) . . . . ? C28 C25 P1 Au1 -48.9(4) . . . . ? C26 C25 P1 Au1 66.7(4) . . . . ? C24 C21 P1 C1 74.5(5) . . . . ? C23 C21 P1 C1 -45.5(4) . . . . ? C22 C21 P1 C1 -161.5(4) . . . . ? C24 C21 P1 C25 -43.7(5) . . . . ? C23 C21 P1 C25 -163.6(3) . . . . ? C22 C21 P1 C25 80.3(4) . . . . ? C24 C21 P1 Au1 -163.5(4) . . . . ? C23 C21 P1 Au1 76.6(4) . . . . ? C22 C21 P1 Au1 -39.5(4) . . . . ? Cl1 Au1 P1 C1 155.0(6) . . . . ? Cl1 Au1 P1 C25 -80.8(6) . . . . ? Cl1 Au1 P1 C21 41.2(7) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 36.43 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 3.247 _refine_diff_density_min -5.503 _refine_diff_density_rms 0.212 _database_code_depnum_ccdc_archive 'CCDC 933754' ####################################################################### # # 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_rs374a_0m #TrackingRef 'web_deposit_cif_file_4_AntonioM.Echavarren_1365746154.RS374a_0mX.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H38 Fe O S' _chemical_formula_weight 526.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.6442(11) _cell_length_b 15.8547(15) _cell_length_c 17.740(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2712.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9909 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 35.03 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.656 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8800 _exptl_absorpt_correction_T_max 0.9081 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 22848 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 36.32 _reflns_number_total 11023 _reflns_number_gt 9728 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+0.4550P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _chemical_absolute_configuration ad _refine_ls_abs_structure_Flack -0.002(10) _refine_ls_number_reflns 11023 _refine_ls_number_parameters 323 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0532 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1108 _refine_ls_wR_factor_gt 0.1062 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5572(2) 0.75270(14) 0.81096(13) 0.0347(4) Uani 1 1 d . . . H1 H 0.4605 0.7709 0.8232 0.042 Uiso 1 1 calc R . . Fe1 Fe 0.73340(2) 0.783767(14) 0.871064(13) 0.01937(5) Uani 1 1 d . . . O1 O 0.93150(13) 0.97158(9) 0.80075(7) 0.0256(2) Uani 1 1 d . . . S1 S 0.81725(4) 0.98660(2) 0.85628(2) 0.01906(7) Uani 1 1 d . . . C2 C 0.6242(2) 0.67866(13) 0.83825(14) 0.0345(4) Uani 1 1 d . . . H2 H 0.5825 0.6356 0.8727 0.041 Uiso 1 1 calc R . . C3 C 0.7599(2) 0.67650(13) 0.80824(13) 0.0369(5) Uani 1 1 d . . . H3 H 0.8306 0.6316 0.8175 0.044 Uiso 1 1 calc R . . C4 C 0.7783(3) 0.74903(17) 0.76271(12) 0.0418(5) Uani 1 1 d . . . H4 H 0.8641 0.7641 0.7341 0.050 Uiso 1 1 calc R . . C5 C 0.6520(3) 0.79680(15) 0.76444(12) 0.0387(5) Uani 1 1 d . . . H5 H 0.6341 0.8511 0.7375 0.046 Uiso 1 1 calc R . . C6 C 0.81070(15) 0.89452(9) 0.91336(8) 0.0164(2) Uani 1 1 d . . . C7 C 0.69829(14) 0.86646(9) 0.96135(8) 0.0160(2) Uani 1 1 d . . . C8 C 0.73709(15) 0.78366(10) 0.98629(9) 0.0209(3) Uani 1 1 d . . . H8 H 0.6796 0.7464 1.0193 0.025 Uiso 1 1 calc R . . C9 C 0.87035(16) 0.76255(11) 0.95648(10) 0.0225(3) Uani 1 1 d . . . H9 H 0.9221 0.7089 0.9658 0.027 Uiso 1 1 calc R . . C10 C 0.91598(15) 0.83076(10) 0.91079(9) 0.0195(3) Uani 1 1 d . . . H10 H 1.0056 0.8340 0.8825 0.023 Uiso 1 1 calc R . . C11 C 0.88346(16) 1.06272(10) 0.92203(10) 0.0203(3) Uani 1 1 d . . . C12 C 0.79791(18) 1.09244(11) 0.97954(11) 0.0261(3) Uani 1 1 d . . . H12 H 0.7075 1.0698 0.9862 0.031 Uiso 1 1 calc R . . C13 C 0.8467(2) 1.15582(11) 1.02721(11) 0.0279(3) Uani 1 1 d . . . H13 H 0.7894 1.1752 1.0672 0.034 Uiso 1 1 calc R . . C14 C 0.9778(2) 1.19129(11) 1.01750(12) 0.0268(3) Uani 1 1 d . . . C15 C 1.06056(19) 1.16141(11) 0.95850(12) 0.0278(3) Uani 1 1 d . . . H15 H 1.1498 1.1852 0.9507 0.033 Uiso 1 1 calc R . . C16 C 1.01425(17) 1.09705(11) 0.91074(11) 0.0242(3) Uani 1 1 d . . . H16 H 1.0717 1.0771 0.8711 0.029 Uiso 1 1 calc R . . C17 C 1.0257(2) 1.26186(12) 1.06843(13) 0.0345(4) Uani 1 1 d . . . H17A H 0.9710 1.2614 1.1150 0.052 Uiso 1 1 calc R . . H17B H 1.0134 1.3160 1.0427 0.052 Uiso 1 1 calc R . . H17C H 1.1240 1.2539 1.0807 0.052 Uiso 1 1 calc R . . C18 C 0.59138(14) 0.92128(10) 0.99855(9) 0.0173(2) Uani 1 1 d . . . C19 C 0.61176(15) 0.93861(11) 1.07641(9) 0.0204(3) Uani 1 1 d . . . C20 C 0.52304(16) 0.99622(11) 1.11252(9) 0.0245(3) Uani 1 1 d . . . H20 H 0.5360 1.0073 1.1647 0.029 Uiso 1 1 calc R . . C21 C 0.41625(16) 1.03774(12) 1.07409(10) 0.0244(3) Uani 1 1 d . . . C22 C 0.39593(16) 1.01780(11) 0.99891(10) 0.0237(3) Uani 1 1 d . . . H22 H 0.3211 1.0435 0.9727 0.028 Uiso 1 1 calc R . . C23 C 0.48097(15) 0.96149(10) 0.96012(9) 0.0184(3) Uani 1 1 d . . . C24 C 0.72998(16) 0.90253(11) 1.12373(9) 0.0231(3) Uani 1 1 d . . . H24 H 0.7907 0.8681 1.0899 0.028 Uiso 1 1 calc R . . C25 C 0.6731(2) 0.84445(13) 1.18569(11) 0.0305(4) Uani 1 1 d . . . H25A H 0.6186 0.7991 1.1627 0.046 Uiso 1 1 calc R . . H25B H 0.6140 0.8771 1.2198 0.046 Uiso 1 1 calc R . . H25C H 0.7505 0.8200 1.2141 0.046 Uiso 1 1 calc R . . C26 C 0.81876(18) 0.97239(13) 1.15889(10) 0.0284(3) Uani 1 1 d . . . H26A H 0.8932 0.9470 1.1889 0.043 Uiso 1 1 calc R . . H26B H 0.7607 1.0077 1.1914 0.043 Uiso 1 1 calc R . . H26C H 0.8592 1.0071 1.1188 0.043 Uiso 1 1 calc R . . C27 C 0.32302(19) 1.10361(12) 1.11017(10) 0.0284(3) Uani 1 1 d . . . H27 H 0.2885 1.1405 1.0685 0.034 Uiso 1 1 calc R . . C28 C 0.1952(2) 1.06101(14) 1.14491(14) 0.0399(5) Uani 1 1 d . . . H28A H 0.1322 1.1042 1.1646 0.060 Uiso 1 1 calc R . . H28B H 0.2244 1.0238 1.1861 0.060 Uiso 1 1 calc R . . H28C H 0.1474 1.0278 1.1062 0.060 Uiso 1 1 calc R . . C29 C 0.3971(2) 1.16077(14) 1.16554(14) 0.0378(4) Uani 1 1 d . . . H29A H 0.4779 1.1862 1.1410 0.057 Uiso 1 1 calc R . . H29B H 0.4275 1.1277 1.2092 0.057 Uiso 1 1 calc R . . H29C H 0.3337 1.2053 1.1822 0.057 Uiso 1 1 calc R . . C30 C 0.44701(14) 0.94741(10) 0.87763(9) 0.0200(3) Uani 1 1 d . . . H30 H 0.5219 0.9118 0.8552 0.024 Uiso 1 1 calc R . . C31 C 0.30861(17) 0.89914(11) 0.87043(11) 0.0261(3) Uani 1 1 d . . . H31A H 0.2325 0.9351 0.8879 0.039 Uiso 1 1 calc R . . H31B H 0.3123 0.8479 0.9012 0.039 Uiso 1 1 calc R . . H31C H 0.2932 0.8838 0.8176 0.039 Uiso 1 1 calc R . . C32 C 0.43947(18) 1.03051(11) 0.83290(11) 0.0259(3) Uani 1 1 d . . . H32A H 0.5243 1.0632 0.8415 0.039 Uiso 1 1 calc R . . H32B H 0.3590 1.0632 0.8498 0.039 Uiso 1 1 calc R . . H32C H 0.4303 1.0180 0.7790 0.039 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 C1 0.0283(8) 0.0321(9) 0.0436(11) -0.0158(8) -0.0106(8) 0.0001(7) Fe1 0.01725(9) 0.01727(10) 0.02358(10) -0.00342(8) 0.00115(7) -0.00115(7) O1 0.0249(5) 0.0302(6) 0.0216(5) 0.0009(5) 0.0051(4) -0.0024(5) S1 0.01702(14) 0.01985(16) 0.02030(16) 0.00164(12) -0.00073(11) -0.00096(12) C2 0.0298(9) 0.0244(8) 0.0491(12) -0.0083(8) -0.0017(8) -0.0079(7) C3 0.0286(9) 0.0303(9) 0.0517(12) -0.0214(8) -0.0021(8) 0.0016(7) C4 0.0421(11) 0.0532(13) 0.0303(9) -0.0202(9) 0.0085(8) -0.0125(10) C5 0.0548(13) 0.0350(11) 0.0265(8) -0.0045(7) -0.0117(8) -0.0082(9) C6 0.0144(5) 0.0168(6) 0.0179(6) -0.0003(4) -0.0004(4) -0.0003(4) C7 0.0133(5) 0.0177(6) 0.0171(6) -0.0002(5) 0.0005(4) 0.0008(4) C8 0.0183(6) 0.0203(6) 0.0242(6) 0.0041(5) 0.0021(5) 0.0019(6) C9 0.0174(6) 0.0210(7) 0.0291(8) 0.0023(6) 0.0008(5) 0.0029(5) C10 0.0142(5) 0.0202(7) 0.0242(7) -0.0009(5) 0.0020(5) 0.0013(5) C11 0.0185(6) 0.0145(6) 0.0279(7) 0.0020(5) -0.0014(5) -0.0003(5) C12 0.0228(7) 0.0220(8) 0.0337(8) -0.0033(6) 0.0043(6) -0.0022(5) C13 0.0302(8) 0.0181(7) 0.0355(9) -0.0032(6) 0.0036(7) -0.0001(6) C14 0.0287(8) 0.0167(7) 0.0350(9) -0.0001(6) -0.0048(6) -0.0001(6) C15 0.0230(7) 0.0207(8) 0.0396(9) -0.0023(7) -0.0022(6) -0.0032(6) C16 0.0185(6) 0.0216(7) 0.0324(8) 0.0002(6) 0.0003(6) -0.0014(5) C17 0.0376(9) 0.0224(8) 0.0435(11) -0.0083(8) -0.0030(8) -0.0027(7) C18 0.0136(5) 0.0190(6) 0.0192(6) -0.0020(5) 0.0003(5) -0.0003(4) C19 0.0140(5) 0.0261(8) 0.0210(6) -0.0038(6) 0.0009(5) -0.0008(5) C20 0.0177(6) 0.0335(9) 0.0223(7) -0.0082(6) 0.0012(5) 0.0011(6) C21 0.0162(6) 0.0290(8) 0.0282(8) -0.0092(6) 0.0012(5) 0.0018(5) C22 0.0157(6) 0.0249(7) 0.0305(8) -0.0045(6) -0.0022(5) 0.0028(5) C23 0.0131(5) 0.0182(6) 0.0237(7) -0.0021(5) -0.0017(5) -0.0008(4) C24 0.0192(6) 0.0311(8) 0.0191(6) -0.0025(6) -0.0021(5) 0.0020(5) C25 0.0320(8) 0.0323(9) 0.0272(8) 0.0022(7) -0.0041(7) -0.0030(7) C26 0.0196(6) 0.0388(10) 0.0268(7) 0.0000(7) -0.0047(6) -0.0036(6) C27 0.0239(7) 0.0331(9) 0.0282(8) -0.0040(7) 0.0020(6) 0.0050(7) C28 0.0381(10) 0.0300(9) 0.0517(12) -0.0009(8) 0.0273(9) 0.0011(7) C29 0.0407(11) 0.0332(10) 0.0396(11) -0.0090(9) -0.0019(9) 0.0057(8) C30 0.0154(5) 0.0213(7) 0.0233(7) 0.0009(5) -0.0034(5) -0.0004(5) C31 0.0194(6) 0.0296(8) 0.0294(7) 0.0005(7) -0.0050(6) -0.0051(5) C32 0.0230(7) 0.0252(8) 0.0295(8) 0.0050(6) -0.0020(6) 0.0001(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 C1 C5 1.417(3) . ? C1 C2 1.425(3) . ? C1 Fe1 2.0658(19) . ? Fe1 C10 2.0377(16) . ? Fe1 C9 2.0380(17) . ? Fe1 C8 2.0444(16) . ? Fe1 C4 2.046(2) . ? Fe1 C3 2.0494(19) . ? Fe1 C6 2.0500(15) . ? Fe1 C2 2.0553(19) . ? Fe1 C5 2.058(2) . ? Fe1 C7 2.0973(15) . ? O1 S1 1.4971(13) . ? S1 C6 1.7779(15) . ? S1 C11 1.7958(17) . ? C2 C3 1.413(3) . ? C3 C4 1.416(4) . ? C4 C5 1.434(4) . ? C6 C10 1.433(2) . ? C6 C7 1.448(2) . ? C7 C8 1.435(2) . ? C7 C18 1.501(2) . ? C8 C9 1.429(2) . ? C9 C10 1.421(2) . ? C11 C16 1.388(2) . ? C11 C12 1.394(2) . ? C12 C13 1.395(3) . ? C13 C14 1.394(3) . ? C14 C15 1.399(3) . ? C14 C17 1.511(3) . ? C15 C16 1.399(3) . ? C18 C23 1.416(2) . ? C18 C19 1.422(2) . ? C19 C20 1.406(2) . ? C19 C24 1.527(2) . ? C20 C21 1.400(2) . ? C21 C22 1.385(2) . ? C21 C27 1.519(2) . ? C22 C23 1.394(2) . ? C23 C30 1.516(2) . ? C24 C26 1.533(2) . ? C24 C25 1.535(3) . ? C27 C29 1.515(3) . ? C27 C28 1.535(3) . ? C30 C32 1.540(2) . ? C30 C31 1.544(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 C5 C1 C2 108.1(2) . . ? C5 C1 Fe1 69.63(12) . . ? C2 C1 Fe1 69.37(11) . . ? C10 Fe1 C9 40.82(7) . . ? C10 Fe1 C8 68.87(6) . . ? C9 Fe1 C8 40.99(6) . . ? C10 Fe1 C4 103.91(8) . . ? C9 Fe1 C4 121.13(9) . . ? C8 Fe1 C4 159.31(9) . . ? C10 Fe1 C3 112.56(7) . . ? C9 Fe1 C3 100.75(8) . . ? C8 Fe1 C3 122.74(9) . . ? C4 Fe1 C3 40.47(11) . . ? C10 Fe1 C6 41.06(6) . . ? C9 Fe1 C6 68.50(6) . . ? C8 Fe1 C6 68.18(6) . . ? C4 Fe1 C6 119.84(8) . . ? C3 Fe1 C6 149.83(8) . . ? C10 Fe1 C2 146.83(8) . . ? C9 Fe1 C2 114.13(8) . . ? C8 Fe1 C2 106.94(8) . . ? C4 Fe1 C2 67.92(10) . . ? C3 Fe1 C2 40.27(9) . . ? C6 Fe1 C2 169.89(7) . . ? C10 Fe1 C5 127.63(9) . . ? C9 Fe1 C5 161.25(9) . . ? C8 Fe1 C5 157.76(9) . . ? C4 Fe1 C5 40.91(11) . . ? C3 Fe1 C5 68.35(10) . . ? C6 Fe1 C5 112.90(8) . . ? C2 Fe1 C5 68.03(10) . . ? C10 Fe1 C1 167.57(9) . . ? C9 Fe1 C1 151.35(9) . . ? C8 Fe1 C1 122.02(8) . . ? C4 Fe1 C1 67.98(9) . . ? C3 Fe1 C1 67.92(8) . . ? C6 Fe1 C1 133.82(7) . . ? C2 Fe1 C1 40.46(9) . . ? C5 Fe1 C1 40.18(10) . . ? C10 Fe1 C7 69.32(6) . . ? C9 Fe1 C7 68.90(6) . . ? C8 Fe1 C7 40.52(6) . . ? C4 Fe1 C7 156.92(9) . . ? C3 Fe1 C7 162.59(8) . . ? C6 Fe1 C7 40.86(6) . . ? C2 Fe1 C7 129.82(8) . . ? C5 Fe1 C7 125.28(8) . . ? C1 Fe1 C7 114.23(7) . . ? O1 S1 C6 105.69(7) . . ? O1 S1 C11 105.82(8) . . ? C6 S1 C11 101.22(7) . . ? C3 C2 C1 108.2(2) . . ? C3 C2 Fe1 69.64(11) . . ? C1 C2 Fe1 70.17(11) . . ? C2 C3 C4 108.1(2) . . ? C2 C3 Fe1 70.09(11) . . ? C4 C3 Fe1 69.63(11) . . ? C3 C4 C5 108.07(19) . . ? C3 C4 Fe1 69.90(12) . . ? C5 C4 Fe1 70.01(11) . . ? C1 C5 C4 107.5(2) . . ? C1 C5 Fe1 70.20(12) . . ? C4 C5 Fe1 69.08(12) . . ? C10 C6 C7 109.41(13) . . ? C10 C6 S1 122.39(11) . . ? C7 C6 S1 127.85(11) . . ? C10 C6 Fe1 69.01(9) . . ? C7 C6 Fe1 71.32(8) . . ? S1 C6 Fe1 120.52(8) . . ? C8 C7 C6 105.49(12) . . ? C8 C7 C18 124.97(13) . . ? C6 C7 C18 126.48(13) . . ? C8 C7 Fe1 67.76(9) . . ? C6 C7 Fe1 67.81(8) . . ? C18 C7 Fe1 143.95(10) . . ? C9 C8 C7 109.54(13) . . ? C9 C8 Fe1 69.26(9) . . ? C7 C8 Fe1 71.72(9) . . ? C10 C9 C8 108.14(14) . . ? C10 C9 Fe1 69.58(10) . . ? C8 C9 Fe1 69.75(9) . . ? C9 C10 C6 107.40(13) . . ? C9 C10 Fe1 69.60(9) . . ? C6 C10 Fe1 69.93(8) . . ? C16 C11 C12 120.72(16) . . ? C16 C11 S1 119.53(13) . . ? C12 C11 S1 119.47(12) . . ? C11 C12 C13 119.15(16) . . ? C14 C13 C12 121.45(17) . . ? C13 C14 C15 118.24(17) . . ? C13 C14 C17 120.17(19) . . ? C15 C14 C17 121.57(18) . . ? C14 C15 C16 121.18(17) . . ? C11 C16 C15 119.24(17) . . ? C23 C18 C19 118.99(14) . . ? C23 C18 C7 124.43(14) . . ? C19 C18 C7 116.35(13) . . ? C20 C19 C18 118.94(14) . . ? C20 C19 C24 116.57(14) . . ? C18 C19 C24 124.39(13) . . ? C21 C20 C19 122.10(15) . . ? C22 C21 C20 117.77(15) . . ? C22 C21 C27 118.61(16) . . ? C20 C21 C27 123.61(16) . . ? C21 C22 C23 122.58(15) . . ? C22 C23 C18 119.54(15) . . ? C22 C23 C30 116.34(14) . . ? C18 C23 C30 124.12(13) . . ? C19 C24 C26 111.72(14) . . ? C19 C24 C25 110.58(14) . . ? C26 C24 C25 109.99(14) . . ? C29 C27 C21 113.91(16) . . ? C29 C27 C28 112.42(18) . . ? C21 C27 C28 109.99(16) . . ? C23 C30 C32 112.43(13) . . ? C23 C30 C31 109.86(13) . . ? C32 C30 C31 109.91(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 Fe1 C10 12.6(4) . . . . ? C2 C1 Fe1 C10 132.3(3) . . . . ? C5 C1 Fe1 C9 -153.33(16) . . . . ? C2 C1 Fe1 C9 -33.7(2) . . . . ? C5 C1 Fe1 C8 162.09(12) . . . . ? C2 C1 Fe1 C8 -78.26(15) . . . . ? C5 C1 Fe1 C4 -38.32(14) . . . . ? C2 C1 Fe1 C4 81.34(15) . . . . ? C5 C1 Fe1 C3 -82.15(15) . . . . ? C2 C1 Fe1 C3 37.51(14) . . . . ? C5 C1 Fe1 C6 72.51(16) . . . . ? C2 C1 Fe1 C6 -167.83(12) . . . . ? C5 C1 Fe1 C2 -119.66(19) . . . . ? C2 C1 Fe1 C5 119.66(19) . . . . ? C5 C1 Fe1 C7 116.66(13) . . . . ? C2 C1 Fe1 C7 -123.68(13) . . . . ? C5 C1 C2 C3 -0.5(2) . . . . ? Fe1 C1 C2 C3 -59.48(14) . . . . ? C5 C1 C2 Fe1 59.01(14) . . . . ? C10 Fe1 C2 C3 -43.9(2) . . . . ? C9 Fe1 C2 C3 -77.74(16) . . . . ? C8 Fe1 C2 C3 -121.01(14) . . . . ? C4 Fe1 C2 C3 37.71(15) . . . . ? C6 Fe1 C2 C3 179.3(4) . . . . ? C5 Fe1 C2 C3 82.00(16) . . . . ? C1 Fe1 C2 C3 119.2(2) . . . . ? C7 Fe1 C2 C3 -159.68(13) . . . . ? C10 Fe1 C2 C1 -163.08(14) . . . . ? C9 Fe1 C2 C1 163.06(13) . . . . ? C8 Fe1 C2 C1 119.79(13) . . . . ? C4 Fe1 C2 C1 -81.49(16) . . . . ? C3 Fe1 C2 C1 -119.2(2) . . . . ? C6 Fe1 C2 C1 60.1(5) . . . . ? C5 Fe1 C2 C1 -37.20(15) . . . . ? C7 Fe1 C2 C1 81.12(16) . . . . ? C1 C2 C3 C4 0.4(2) . . . . ? Fe1 C2 C3 C4 -59.46(14) . . . . ? C1 C2 C3 Fe1 59.81(14) . . . . ? C10 Fe1 C3 C2 155.75(13) . . . . ? C9 Fe1 C3 C2 114.80(14) . . . . ? C8 Fe1 C3 C2 77.11(15) . . . . ? C4 Fe1 C3 C2 -119.2(2) . . . . ? C6 Fe1 C3 C2 -179.76(14) . . . . ? C5 Fe1 C3 C2 -81.12(15) . . . . ? C1 Fe1 C3 C2 -37.68(14) . . . . ? C7 Fe1 C3 C2 63.1(3) . . . . ? C10 Fe1 C3 C4 -85.08(15) . . . . ? C9 Fe1 C3 C4 -126.03(14) . . . . ? C8 Fe1 C3 C4 -163.72(13) . . . . ? C6 Fe1 C3 C4 -60.6(2) . . . . ? C2 Fe1 C3 C4 119.2(2) . . . . ? C5 Fe1 C3 C4 38.05(15) . . . . ? C1 Fe1 C3 C4 81.49(15) . . . . ? C7 Fe1 C3 C4 -177.8(2) . . . . ? C2 C3 C4 C5 -0.1(2) . . . . ? Fe1 C3 C4 C5 -59.85(13) . . . . ? C2 C3 C4 Fe1 59.75(14) . . . . ? C10 Fe1 C4 C3 108.58(13) . . . . ? C9 Fe1 C4 C3 68.16(15) . . . . ? C8 Fe1 C4 C3 41.9(3) . . . . ? C6 Fe1 C4 C3 149.69(11) . . . . ? C2 Fe1 C4 C3 -37.52(13) . . . . ? C5 Fe1 C4 C3 -118.99(19) . . . . ? C1 Fe1 C4 C3 -81.33(14) . . . . ? C7 Fe1 C4 C3 178.30(16) . . . . ? C10 Fe1 C4 C5 -132.43(13) . . . . ? C9 Fe1 C4 C5 -172.86(12) . . . . ? C8 Fe1 C4 C5 160.86(19) . . . . ? C3 Fe1 C4 C5 118.99(19) . . . . ? C6 Fe1 C4 C5 -91.32(14) . . . . ? C2 Fe1 C4 C5 81.46(14) . . . . ? C1 Fe1 C4 C5 37.65(13) . . . . ? C7 Fe1 C4 C5 -62.7(2) . . . . ? C2 C1 C5 C4 0.4(2) . . . . ? Fe1 C1 C5 C4 59.26(13) . . . . ? C2 C1 C5 Fe1 -58.86(14) . . . . ? C3 C4 C5 C1 -0.2(2) . . . . ? Fe1 C4 C5 C1 -59.97(14) . . . . ? C3 C4 C5 Fe1 59.78(14) . . . . ? C10 Fe1 C5 C1 -176.59(11) . . . . ? C9 Fe1 C5 C1 138.0(2) . . . . ? C8 Fe1 C5 C1 -43.6(3) . . . . ? C4 Fe1 C5 C1 118.63(18) . . . . ? C3 Fe1 C5 C1 80.98(14) . . . . ? C6 Fe1 C5 C1 -131.66(12) . . . . ? C2 Fe1 C5 C1 37.45(12) . . . . ? C7 Fe1 C5 C1 -86.64(14) . . . . ? C10 Fe1 C5 C4 64.78(16) . . . . ? C9 Fe1 C5 C4 19.3(3) . . . . ? C8 Fe1 C5 C4 -162.18(19) . . . . ? C3 Fe1 C5 C4 -37.65(13) . . . . ? C6 Fe1 C5 C4 109.71(13) . . . . ? C2 Fe1 C5 C4 -81.18(14) . . . . ? C1 Fe1 C5 C4 -118.63(19) . . . . ? C7 Fe1 C5 C4 154.74(12) . . . . ? O1 S1 C6 C10 10.51(14) . . . . ? C11 S1 C6 C10 -99.64(13) . . . . ? O1 S1 C6 C7 -161.96(13) . . . . ? C11 S1 C6 C7 87.89(14) . . . . ? O1 S1 C6 Fe1 -72.69(10) . . . . ? C11 S1 C6 Fe1 177.16(8) . . . . ? C9 Fe1 C6 C10 38.17(9) . . . . ? C8 Fe1 C6 C10 82.43(9) . . . . ? C4 Fe1 C6 C10 -76.32(13) . . . . ? C3 Fe1 C6 C10 -35.64(19) . . . . ? C2 Fe1 C6 C10 145.2(4) . . . . ? C5 Fe1 C6 C10 -121.62(11) . . . . ? C1 Fe1 C6 C10 -163.53(12) . . . . ? C7 Fe1 C6 C10 120.35(12) . . . . ? C10 Fe1 C6 C7 -120.35(12) . . . . ? C9 Fe1 C6 C7 -82.18(9) . . . . ? C8 Fe1 C6 C7 -37.92(8) . . . . ? C4 Fe1 C6 C7 163.32(11) . . . . ? C3 Fe1 C6 C7 -156.00(16) . . . . ? C2 Fe1 C6 C7 24.9(5) . . . . ? C5 Fe1 C6 C7 118.03(11) . . . . ? C1 Fe1 C6 C7 76.12(13) . . . . ? C10 Fe1 C6 S1 116.10(13) . . . . ? C9 Fe1 C6 S1 154.27(11) . . . . ? C8 Fe1 C6 S1 -161.46(10) . . . . ? C4 Fe1 C6 S1 39.78(13) . . . . ? C3 Fe1 C6 S1 80.46(18) . . . . ? C2 Fe1 C6 S1 -98.7(5) . . . . ? C5 Fe1 C6 S1 -5.51(13) . . . . ? C1 Fe1 C6 S1 -47.43(15) . . . . ? C7 Fe1 C6 S1 -123.54(13) . . . . ? C10 C6 C7 C8 -1.16(16) . . . . ? S1 C6 C7 C8 172.10(12) . . . . ? Fe1 C6 C7 C8 57.51(10) . . . . ? C10 C6 C7 C18 159.67(14) . . . . ? S1 C6 C7 C18 -27.1(2) . . . . ? Fe1 C6 C7 C18 -141.66(15) . . . . ? C10 C6 C7 Fe1 -58.67(10) . . . . ? S1 C6 C7 Fe1 114.59(12) . . . . ? C10 Fe1 C7 C8 -81.29(9) . . . . ? C9 Fe1 C7 C8 -37.46(9) . . . . ? C4 Fe1 C7 C8 -158.0(2) . . . . ? C3 Fe1 C7 C8 18.3(3) . . . . ? C6 Fe1 C7 C8 -118.57(12) . . . . ? C2 Fe1 C7 C8 66.94(13) . . . . ? C5 Fe1 C7 C8 156.54(11) . . . . ? C1 Fe1 C7 C8 111.61(11) . . . . ? C10 Fe1 C7 C6 37.29(9) . . . . ? C9 Fe1 C7 C6 81.12(9) . . . . ? C8 Fe1 C7 C6 118.57(12) . . . . ? C4 Fe1 C7 C6 -39.4(2) . . . . ? C3 Fe1 C7 C6 136.9(2) . . . . ? C2 Fe1 C7 C6 -174.48(11) . . . . ? C5 Fe1 C7 C6 -84.88(12) . . . . ? C1 Fe1 C7 C6 -129.81(11) . . . . ? C10 Fe1 C7 C18 159.3(2) . . . . ? C9 Fe1 C7 C18 -156.8(2) . . . . ? C8 Fe1 C7 C18 -119.4(2) . . . . ? C4 Fe1 C7 C18 82.6(3) . . . . ? C3 Fe1 C7 C18 -101.0(3) . . . . ? C6 Fe1 C7 C18 122.1(2) . . . . ? C2 Fe1 C7 C18 -52.4(2) . . . . ? C5 Fe1 C7 C18 37.2(2) . . . . ? C1 Fe1 C7 C18 -7.8(2) . . . . ? C6 C7 C8 C9 1.59(17) . . . . ? C18 C7 C8 C9 -159.61(14) . . . . ? Fe1 C7 C8 C9 59.14(11) . . . . ? C6 C7 C8 Fe1 -57.55(10) . . . . ? C18 C7 C8 Fe1 141.25(14) . . . . ? C10 Fe1 C8 C9 -37.61(9) . . . . ? C4 Fe1 C8 C9 35.3(3) . . . . ? C3 Fe1 C8 C9 66.31(12) . . . . ? C6 Fe1 C8 C9 -81.88(10) . . . . ? C2 Fe1 C8 C9 107.51(11) . . . . ? C5 Fe1 C8 C9 -179.26(19) . . . . ? C1 Fe1 C8 C9 149.12(11) . . . . ? C7 Fe1 C8 C9 -120.12(13) . . . . ? C10 Fe1 C8 C7 82.50(9) . . . . ? C9 Fe1 C8 C7 120.12(13) . . . . ? C4 Fe1 C8 C7 155.4(2) . . . . ? C3 Fe1 C8 C7 -173.58(10) . . . . ? C6 Fe1 C8 C7 38.24(8) . . . . ? C2 Fe1 C8 C7 -132.37(10) . . . . ? C5 Fe1 C8 C7 -59.1(2) . . . . ? C1 Fe1 C8 C7 -90.76(11) . . . . ? C7 C8 C9 C10 -1.45(19) . . . . ? Fe1 C8 C9 C10 59.19(12) . . . . ? C7 C8 C9 Fe1 -60.64(11) . . . . ? C8 Fe1 C9 C10 -119.43(13) . . . . ? C4 Fe1 C9 C10 74.37(13) . . . . ? C3 Fe1 C9 C10 112.19(11) . . . . ? C6 Fe1 C9 C10 -38.39(9) . . . . ? C2 Fe1 C9 C10 152.20(10) . . . . ? C5 Fe1 C9 C10 59.7(3) . . . . ? C1 Fe1 C9 C10 175.42(15) . . . . ? C7 Fe1 C9 C10 -82.40(10) . . . . ? C10 Fe1 C9 C8 119.43(13) . . . . ? C4 Fe1 C9 C8 -166.20(11) . . . . ? C3 Fe1 C9 C8 -128.38(11) . . . . ? C6 Fe1 C9 C8 81.04(10) . . . . ? C2 Fe1 C9 C8 -88.36(12) . . . . ? C5 Fe1 C9 C8 179.1(2) . . . . ? C1 Fe1 C9 C8 -65.15(19) . . . . ? C7 Fe1 C9 C8 37.04(9) . . . . ? C8 C9 C10 C6 0.70(18) . . . . ? Fe1 C9 C10 C6 59.99(11) . . . . ? C8 C9 C10 Fe1 -59.29(11) . . . . ? C7 C6 C10 C9 0.30(17) . . . . ? S1 C6 C10 C9 -173.40(12) . . . . ? Fe1 C6 C10 C9 -59.78(11) . . . . ? C7 C6 C10 Fe1 60.08(10) . . . . ? S1 C6 C10 Fe1 -113.62(11) . . . . ? C8 Fe1 C10 C9 37.77(9) . . . . ? C4 Fe1 C10 C9 -121.87(12) . . . . ? C3 Fe1 C10 C9 -80.09(12) . . . . ? C6 Fe1 C10 C9 118.39(13) . . . . ? C2 Fe1 C10 C9 -51.07(18) . . . . ? C5 Fe1 C10 C9 -159.49(11) . . . . ? C1 Fe1 C10 C9 -169.7(3) . . . . ? C7 Fe1 C10 C9 81.28(10) . . . . ? C9 Fe1 C10 C6 -118.39(13) . . . . ? C8 Fe1 C10 C6 -80.63(9) . . . . ? C4 Fe1 C10 C6 119.74(11) . . . . ? C3 Fe1 C10 C6 161.51(11) . . . . ? C2 Fe1 C10 C6 -169.46(14) . . . . ? C5 Fe1 C10 C6 82.12(12) . . . . ? C1 Fe1 C10 C6 71.9(4) . . . . ? C7 Fe1 C10 C6 -37.12(8) . . . . ? O1 S1 C11 C16 3.47(15) . . . . ? C6 S1 C11 C16 113.51(14) . . . . ? O1 S1 C11 C12 177.41(14) . . . . ? C6 S1 C11 C12 -72.55(15) . . . . ? C16 C11 C12 C13 -1.7(3) . . . . ? S1 C11 C12 C13 -175.59(14) . . . . ? C11 C12 C13 C14 1.5(3) . . . . ? C12 C13 C14 C15 -0.3(3) . . . . ? C12 C13 C14 C17 177.93(19) . . . . ? C13 C14 C15 C16 -0.6(3) . . . . ? C17 C14 C15 C16 -178.83(18) . . . . ? C12 C11 C16 C15 0.8(3) . . . . ? S1 C11 C16 C15 174.69(14) . . . . ? C14 C15 C16 C11 0.4(3) . . . . ? C8 C7 C18 C23 -129.77(17) . . . . ? C6 C7 C18 C23 72.9(2) . . . . ? Fe1 C7 C18 C23 -29.6(3) . . . . ? C8 C7 C18 C19 55.7(2) . . . . ? C6 C7 C18 C19 -101.54(18) . . . . ? Fe1 C7 C18 C19 155.89(15) . . . . ? C23 C18 C19 C20 -1.0(2) . . . . ? C7 C18 C19 C20 173.75(14) . . . . ? C23 C18 C19 C24 -177.36(15) . . . . ? C7 C18 C19 C24 -2.6(2) . . . . ? C18 C19 C20 C21 -0.7(3) . . . . ? C24 C19 C20 C21 175.90(16) . . . . ? C19 C20 C21 C22 2.6(3) . . . . ? C19 C20 C21 C27 -176.80(17) . . . . ? C20 C21 C22 C23 -2.9(3) . . . . ? C27 C21 C22 C23 176.56(16) . . . . ? C21 C22 C23 C18 1.2(3) . . . . ? C21 C22 C23 C30 -178.91(16) . . . . ? C19 C18 C23 C22 0.8(2) . . . . ? C7 C18 C23 C22 -173.54(15) . . . . ? C19 C18 C23 C30 -179.05(14) . . . . ? C7 C18 C23 C30 6.6(2) . . . . ? C20 C19 C24 C26 -54.7(2) . . . . ? C18 C19 C24 C26 121.72(17) . . . . ? C20 C19 C24 C25 68.19(19) . . . . ? C18 C19 C24 C25 -115.42(18) . . . . ? C22 C21 C27 C29 -142.13(19) . . . . ? C20 C21 C27 C29 37.3(3) . . . . ? C22 C21 C27 C28 90.6(2) . . . . ? C20 C21 C27 C28 -89.9(2) . . . . ? C22 C23 C30 C32 53.67(18) . . . . ? C18 C23 C30 C32 -126.47(16) . . . . ? C22 C23 C30 C31 -69.07(18) . . . . ? C18 C23 C30 C31 110.78(17) . . . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.051 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.085 _database_code_depnum_ccdc_archive 'CCDC 933755' ####################################################################### # # 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_chbo550_0m #TrackingRef 'web_deposit_cif_file_5_AntonioM.Echavarren_1365746154.CHBO550_0mXe.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H57 Au Cl O3 P' _chemical_formula_weight 729.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 19.461(2) _cell_length_b 9.2739(11) _cell_length_c 20.008(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.325(2) _cell_angle_gamma 90.00 _cell_volume 3340.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5596 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 30.87 _exptl_crystal_description Plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 4.558 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3417 _exptl_absorpt_correction_T_max 0.9558 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith MicroMount' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 23505 _diffrn_reflns_av_R_equivalents 0.0644 _diffrn_reflns_av_sigmaI/netI 0.0721 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 31.07 _reflns_number_total 8558 _reflns_number_gt 7397 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2011.4-0' _computing_cell_refinement 'Bruker APEX2 v2011.4-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution Sir2011 _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0999P)^2^+52.9838P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.024(13) _refine_ls_number_reflns 8558 _refine_ls_number_parameters 334 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0805 _refine_ls_R_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.1771 _refine_ls_wR_factor_gt 0.1694 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.166852(17) 0.97423(8) 0.291909(14) 0.02083(10) Uani 1 1 d . . . Cl1 Cl 0.21351(18) 1.1939(4) 0.33441(13) 0.0317(6) Uani 1 1 d . . . P1 P 0.11930(12) 0.7660(3) 0.24392(11) 0.0152(5) Uani 1 1 d . . . O1 O 0.1271(3) 0.6368(8) 0.2975(3) 0.0145(13) Uani 1 1 d . . . O2 O 0.1544(4) 0.7182(9) 0.1885(3) 0.0165(14) Uani 1 1 d . . . O3 O 0.0327(3) 0.7638(11) 0.1956(3) 0.0235(17) Uani 1 1 d . . . C1 C 0.1817(5) 0.6383(12) 0.3720(4) 0.0160(18) Uani 1 1 d . . . H1 H 0.1824 0.7331 0.3939 0.019 Uiso 1 1 calc R . . C2 C 0.1571(5) 0.5220(12) 0.4129(5) 0.0166(19) Uani 1 1 d . . . H2 H 0.1590 0.4289 0.3906 0.020 Uiso 1 1 calc R . . C3 C 0.2149(6) 0.5179(13) 0.4912(5) 0.024(3) Uani 1 1 d . . . H3A H 0.2166 0.6111 0.5137 0.029 Uiso 1 1 calc R . . H3B H 0.2002 0.4466 0.5186 0.029 Uiso 1 1 calc R . . C4 C 0.2921(5) 0.480(3) 0.4926(4) 0.029(2) Uani 1 1 d . . . H4A H 0.2909 0.3859 0.4715 0.035 Uiso 1 1 calc R . . H4B H 0.3275 0.4777 0.5422 0.035 Uiso 1 1 calc R . . C5 C 0.3170(5) 0.5952(15) 0.4494(5) 0.025(2) Uani 1 1 d . . . H5 H 0.3201 0.6894 0.4725 0.030 Uiso 1 1 calc R . . C6 C 0.2584(5) 0.6034(13) 0.3709(5) 0.022(2) Uani 1 1 d . . . H6A H 0.2725 0.6776 0.3443 0.027 Uiso 1 1 calc R . . H6B H 0.2565 0.5120 0.3466 0.027 Uiso 1 1 calc R . . C7 C 0.0771(6) 0.5434(16) 0.4088(5) 0.027(2) Uani 1 1 d . . . H7 H 0.0456 0.5493 0.3573 0.032 Uiso 1 1 calc R . . C8 C 0.0511(8) 0.409(2) 0.4380(8) 0.046(4) Uani 1 1 d . . . H8A H 0.0652 0.3240 0.4192 0.068 Uiso 1 1 calc R . . H8B H -0.0019 0.4120 0.4233 0.068 Uiso 1 1 calc R . . H8C H 0.0739 0.4085 0.4898 0.068 Uiso 1 1 calc R . . C9 C 0.0644(7) 0.684(2) 0.4430(6) 0.038(3) Uani 1 1 d . . . H9A H 0.0897 0.6790 0.4945 0.057 Uiso 1 1 calc R . . H9B H 0.0122 0.6971 0.4312 0.057 Uiso 1 1 calc R . . H9C H 0.0834 0.7637 0.4246 0.057 Uiso 1 1 calc R . . C10 C 0.3930(6) 0.5579(19) 0.4483(7) 0.036(3) Uani 1 1 d . . . H10A H 0.4288 0.5512 0.4969 0.054 Uiso 1 1 calc R . . H10B H 0.4079 0.6319 0.4230 0.054 Uiso 1 1 calc R . . H10C H 0.3901 0.4672 0.4242 0.054 Uiso 1 1 calc R . . C11 C 0.1205(5) 0.6168(13) 0.1290(5) 0.019(2) Uani 1 1 d . . . H11 H 0.0688 0.6452 0.1023 0.023 Uiso 1 1 calc R . . C12 C 0.1220(4) 0.464(2) 0.1566(4) 0.023(2) Uani 1 1 d . . . H12A H 0.0945 0.4599 0.1880 0.027 Uiso 1 1 calc R . . H12B H 0.1730 0.4361 0.1846 0.027 Uiso 1 1 calc R . . C13 C 0.0881(6) 0.3591(15) 0.0940(6) 0.025(2) Uani 1 1 d . . . H13 H 0.0359 0.3863 0.0687 0.030 Uiso 1 1 calc R . . C14 C 0.1261(6) 0.3730(15) 0.0403(6) 0.026(2) Uani 1 1 d . . . H14A H 0.1767 0.3379 0.0627 0.031 Uiso 1 1 calc R . . H14B H 0.1003 0.3127 -0.0013 0.031 Uiso 1 1 calc R . . C15 C 0.1274(6) 0.5254(14) 0.0155(5) 0.023(2) Uani 1 1 d . . . H15A H 0.0769 0.5563 -0.0123 0.028 Uiso 1 1 calc R . . H15B H 0.1548 0.5285 -0.0161 0.028 Uiso 1 1 calc R . . C16 C 0.1635(5) 0.6317(14) 0.0792(5) 0.020(2) Uani 1 1 d . . . H16 H 0.2139 0.5962 0.1064 0.024 Uiso 1 1 calc R . . C17 C 0.1712(6) 0.7855(16) 0.0575(5) 0.029(3) Uani 1 1 d . . . H17 H 0.1946 0.8397 0.1025 0.035 Uiso 1 1 calc R . . C18 C 0.2224(6) 0.801(2) 0.0157(6) 0.039(4) Uani 1 1 d . . . H18A H 0.1989 0.7591 -0.0314 0.059 Uiso 1 1 calc R . . H18B H 0.2685 0.7523 0.0413 0.059 Uiso 1 1 calc R . . H18C H 0.2319 0.9013 0.0110 0.059 Uiso 1 1 calc R . . C19 C 0.0968(7) 0.8593(17) 0.0160(6) 0.031(3) Uani 1 1 d . . . H19A H 0.1054 0.9576 0.0064 0.046 Uiso 1 1 calc R . . H19B H 0.0667 0.8569 0.0445 0.046 Uiso 1 1 calc R . . H19C H 0.0717 0.8096 -0.0288 0.046 Uiso 1 1 calc R . . C20 C 0.0897(7) 0.2053(16) 0.1204(6) 0.031(3) Uani 1 1 d . . . H20A H 0.1402 0.1765 0.1467 0.047 Uiso 1 1 calc R . . H20B H 0.0674 0.1424 0.0798 0.047 Uiso 1 1 calc R . . H20C H 0.0624 0.1997 0.1515 0.047 Uiso 1 1 calc R . . C21 C -0.0220(5) 0.7652(15) 0.2296(5) 0.024(2) Uani 1 1 d . . . H21 H 0.0034 0.7789 0.2818 0.028 Uiso 1 1 calc R . . C22 C -0.0601(6) 0.6186(17) 0.2145(6) 0.030(3) Uani 1 1 d . . . H22A H -0.0237 0.5437 0.2363 0.037 Uiso 1 1 calc R . . H22B H -0.0815 0.6019 0.1628 0.037 Uiso 1 1 calc R . . C23 C -0.1217(6) 0.6104(17) 0.2451(7) 0.032(3) Uani 1 1 d . . . H23 H -0.0983 0.6253 0.2975 0.039 Uiso 1 1 calc R . . C24 C -0.1766(6) 0.732(2) 0.2142(6) 0.039(4) Uani 1 1 d . . . H24A H -0.2136 0.7301 0.2359 0.047 Uiso 1 1 calc R . . H24B H -0.2021 0.7181 0.1626 0.047 Uiso 1 1 calc R . . C25 C -0.1375(7) 0.879(2) 0.2285(7) 0.038(3) Uani 1 1 d . . . H25A H -0.1158 0.8956 0.2802 0.046 Uiso 1 1 calc R . . H25B H -0.1739 0.9537 0.2069 0.046 Uiso 1 1 calc R . . C26 C -0.0764(6) 0.8880(18) 0.1979(5) 0.031(3) Uani 1 1 d . . . H26 H -0.1000 0.8710 0.1458 0.037 Uiso 1 1 calc R . . C27 C -0.0394(7) 1.0371(17) 0.2082(6) 0.032(3) Uani 1 1 d . . . H27 H 0.0046 1.0260 0.1962 0.038 Uiso 1 1 calc R . . C28 C -0.0888(8) 1.1460(19) 0.1553(7) 0.039(3) Uani 1 1 d . . . H28A H -0.1007 1.1121 0.1069 0.058 Uiso 1 1 calc R . . H28B H -0.0634 1.2366 0.1616 0.058 Uiso 1 1 calc R . . H28C H -0.1338 1.1582 0.1639 0.058 Uiso 1 1 calc R . . C29 C -0.0113(8) 1.0975(16) 0.2865(7) 0.034(3) Uani 1 1 d . . . H29A H -0.0530 1.1171 0.2996 0.051 Uiso 1 1 calc R . . H29B H 0.0160 1.1849 0.2890 0.051 Uiso 1 1 calc R . . H29C H 0.0204 1.0277 0.3192 0.051 Uiso 1 1 calc R . . C30 C -0.1587(7) 0.456(2) 0.2321(9) 0.046(5) Uani 1 1 d . . . H30A H -0.1745 0.4315 0.1819 0.069 Uiso 1 1 calc R . . H30B H -0.2009 0.4570 0.2459 0.069 Uiso 1 1 calc R . . H30C H -0.1233 0.3864 0.2607 0.069 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 0.03189(15) 0.01461(19) 0.01667(13) -0.0001(2) 0.00997(9) -0.0001(3) Cl1 0.0604(16) 0.0112(16) 0.0238(10) -0.0047(9) 0.0162(10) -0.0065(12) P1 0.0224(10) 0.0107(15) 0.0148(8) 0.0001(8) 0.0096(7) 0.0014(9) O1 0.025(3) 0.005(4) 0.016(2) 0.002(2) 0.009(2) -0.004(2) O2 0.024(3) 0.013(4) 0.016(3) -0.003(2) 0.012(2) -0.003(3) O3 0.016(3) 0.040(6) 0.017(3) -0.002(3) 0.008(2) 0.000(3) C1 0.021(4) 0.015(6) 0.012(3) -0.002(3) 0.005(3) -0.001(3) C2 0.028(4) 0.008(6) 0.017(3) 0.001(3) 0.012(3) 0.000(3) C3 0.034(5) 0.016(7) 0.021(4) 0.004(3) 0.009(4) -0.003(3) C4 0.032(4) 0.036(7) 0.018(3) 0.000(7) 0.006(3) 0.007(8) C5 0.024(4) 0.024(8) 0.023(4) 0.003(4) 0.005(3) 0.006(4) C6 0.029(4) 0.014(6) 0.025(4) 0.005(4) 0.012(3) -0.006(4) C7 0.030(5) 0.032(8) 0.022(4) 0.003(4) 0.014(4) -0.006(5) C8 0.042(6) 0.058(12) 0.044(7) 0.013(6) 0.024(6) -0.015(6) C9 0.035(5) 0.052(11) 0.035(5) -0.011(6) 0.023(5) 0.002(6) C10 0.026(5) 0.033(9) 0.046(6) 0.009(6) 0.011(4) 0.006(5) C11 0.021(4) 0.026(7) 0.013(3) -0.005(3) 0.011(3) -0.004(4) C12 0.024(3) 0.026(8) 0.021(3) 0.002(5) 0.013(3) -0.001(6) C13 0.035(5) 0.020(7) 0.025(4) -0.005(4) 0.017(4) 0.006(4) C14 0.036(5) 0.023(8) 0.024(5) -0.005(4) 0.017(4) 0.006(5) C15 0.031(5) 0.024(7) 0.021(4) -0.002(3) 0.016(4) 0.005(4) C16 0.020(4) 0.026(7) 0.016(3) 0.002(4) 0.011(3) 0.000(4) C17 0.028(4) 0.044(9) 0.019(4) 0.004(4) 0.014(3) -0.008(5) C18 0.027(5) 0.066(12) 0.029(5) 0.011(6) 0.016(4) -0.004(5) C19 0.040(6) 0.028(8) 0.035(5) 0.010(5) 0.026(5) 0.005(5) C20 0.044(6) 0.016(8) 0.037(5) -0.001(5) 0.019(5) -0.003(5) C21 0.022(4) 0.036(8) 0.017(3) -0.005(4) 0.012(3) 0.003(4) C22 0.022(4) 0.045(9) 0.026(4) -0.005(5) 0.012(4) -0.001(5) C23 0.031(5) 0.035(9) 0.040(6) -0.004(5) 0.022(4) -0.007(5) C24 0.024(5) 0.062(13) 0.035(5) 0.003(6) 0.016(4) 0.001(5) C25 0.032(5) 0.058(11) 0.033(5) 0.010(6) 0.023(4) 0.017(6) C26 0.018(4) 0.057(10) 0.022(4) 0.004(5) 0.012(4) 0.007(5) C27 0.030(5) 0.034(8) 0.036(5) 0.002(5) 0.019(5) 0.009(5) C28 0.050(7) 0.032(10) 0.037(6) 0.012(5) 0.019(5) 0.016(6) C29 0.047(6) 0.017(8) 0.038(6) -0.003(5) 0.017(5) 0.012(5) C30 0.036(5) 0.026(14) 0.084(9) -0.015(9) 0.033(6) -0.017(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.198(3) . ? Au1 Cl1 2.261(3) . ? P1 O2 1.572(6) . ? P1 O1 1.576(7) . ? P1 O3 1.593(7) . ? O1 C1 1.465(10) . ? O2 C11 1.462(12) . ? O3 C21 1.465(11) . ? C1 C2 1.536(14) . ? C1 C6 1.537(14) . ? C2 C7 1.540(14) . ? C2 C3 1.543(13) . ? C3 C4 1.531(15) . ? C4 C5 1.56(2) . ? C5 C10 1.527(15) . ? C5 C6 1.554(13) . ? C7 C9 1.53(2) . ? C7 C8 1.54(2) . ? C11 C12 1.52(2) . ? C11 C16 1.531(11) . ? C12 C13 1.524(19) . ? C13 C20 1.52(2) . ? C13 C14 1.522(14) . ? C14 C15 1.502(19) . ? C15 C16 1.553(16) . ? C16 C17 1.515(18) . ? C17 C19 1.530(17) . ? C17 C18 1.532(14) . ? C21 C26 1.519(18) . ? C21 C22 1.52(2) . ? C22 C23 1.540(14) . ? C23 C24 1.51(2) . ? C23 C30 1.58(2) . ? C24 C25 1.53(3) . ? C25 C26 1.533(14) . ? C26 C27 1.54(2) . ? C27 C28 1.513(18) . ? C27 C29 1.554(17) . ? 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 Cl1 176.53(9) . . ? O2 P1 O1 108.1(4) . . ? O2 P1 O3 102.2(4) . . ? O1 P1 O3 102.1(4) . . ? O2 P1 Au1 109.4(3) . . ? O1 P1 Au1 117.0(3) . . ? O3 P1 Au1 116.7(4) . . ? C1 O1 P1 122.0(6) . . ? C11 O2 P1 125.0(6) . . ? C21 O3 P1 120.3(5) . . ? O1 C1 C2 106.4(7) . . ? O1 C1 C6 108.4(7) . . ? C2 C1 C6 111.2(8) . . ? C1 C2 C7 113.2(9) . . ? C1 C2 C3 107.7(8) . . ? C7 C2 C3 112.9(8) . . ? C4 C3 C2 110.9(8) . . ? C3 C4 C5 110.2(13) . . ? C10 C5 C6 109.8(9) . . ? C10 C5 C4 111.2(11) . . ? C6 C5 C4 109.3(9) . . ? C1 C6 C5 109.9(8) . . ? C9 C7 C8 112.7(11) . . ? C9 C7 C2 114.6(10) . . ? C8 C7 C2 110.3(12) . . ? O2 C11 C12 111.4(8) . . ? O2 C11 C16 106.4(8) . . ? C12 C11 C16 112.4(9) . . ? C11 C12 C13 110.8(8) . . ? C20 C13 C14 112.0(10) . . ? C20 C13 C12 111.6(10) . . ? C14 C13 C12 110.5(10) . . ? C15 C14 C13 112.8(10) . . ? C14 C15 C16 112.6(8) . . ? C17 C16 C11 114.1(9) . . ? C17 C16 C15 115.2(8) . . ? C11 C16 C15 106.8(8) . . ? C16 C17 C19 113.6(9) . . ? C16 C17 C18 113.6(11) . . ? C19 C17 C18 109.8(9) . . ? O3 C21 C26 109.1(9) . . ? O3 C21 C22 106.6(9) . . ? C26 C21 C22 112.1(9) . . ? C21 C22 C23 111.1(10) . . ? C24 C23 C22 109.7(11) . . ? C24 C23 C30 113.6(11) . . ? C22 C23 C30 110.8(11) . . ? C23 C24 C25 111.1(10) . . ? C24 C25 C26 112.5(12) . . ? C21 C26 C25 108.4(10) . . ? C21 C26 C27 113.7(9) . . ? C25 C26 C27 113.1(12) . . ? C28 C27 C26 111.5(11) . . ? C28 C27 C29 110.6(12) . . ? C26 C27 C29 115.3(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Au1 P1 O2 55.7(18) . . . . ? Cl1 Au1 P1 O1 179(100) . . . . ? Cl1 Au1 P1 O3 -59.6(18) . . . . ? O2 P1 O1 C1 105.4(7) . . . . ? O3 P1 O1 C1 -147.3(7) . . . . ? Au1 P1 O1 C1 -18.6(7) . . . . ? O1 P1 O2 C11 73.9(8) . . . . ? O3 P1 O2 C11 -33.3(9) . . . . ? Au1 P1 O2 C11 -157.6(7) . . . . ? O2 P1 O3 C21 164.1(9) . . . . ? O1 P1 O3 C21 52.3(10) . . . . ? Au1 P1 O3 C21 -76.6(9) . . . . ? P1 O1 C1 C2 162.9(6) . . . . ? P1 O1 C1 C6 -77.4(10) . . . . ? O1 C1 C2 C7 -56.1(10) . . . . ? C6 C1 C2 C7 -174.0(8) . . . . ? O1 C1 C2 C3 178.4(8) . . . . ? C6 C1 C2 C3 60.5(10) . . . . ? C1 C2 C3 C4 -60.3(14) . . . . ? C7 C2 C3 C4 174.0(13) . . . . ? C2 C3 C4 C5 59.7(15) . . . . ? C3 C4 C5 C10 -178.4(11) . . . . ? C3 C4 C5 C6 -57.0(14) . . . . ? O1 C1 C6 C5 -176.7(9) . . . . ? C2 C1 C6 C5 -60.0(12) . . . . ? C10 C5 C6 C1 179.0(11) . . . . ? C4 C5 C6 C1 56.8(13) . . . . ? C1 C2 C7 C9 -62.3(12) . . . . ? C3 C2 C7 C9 60.4(13) . . . . ? C1 C2 C7 C8 169.2(10) . . . . ? C3 C2 C7 C8 -68.1(13) . . . . ? P1 O2 C11 C12 -71.0(10) . . . . ? P1 O2 C11 C16 166.2(7) . . . . ? O2 C11 C12 C13 -178.8(7) . . . . ? C16 C11 C12 C13 -59.5(10) . . . . ? C11 C12 C13 C20 179.5(8) . . . . ? C11 C12 C13 C14 54.2(12) . . . . ? C20 C13 C14 C15 -178.0(10) . . . . ? C12 C13 C14 C15 -52.9(14) . . . . ? C13 C14 C15 C16 55.3(12) . . . . ? O2 C11 C16 C17 -51.0(10) . . . . ? C12 C11 C16 C17 -173.1(8) . . . . ? O2 C11 C16 C15 -179.4(8) . . . . ? C12 C11 C16 C15 58.4(10) . . . . ? C14 C15 C16 C17 176.1(8) . . . . ? C14 C15 C16 C11 -56.1(11) . . . . ? C11 C16 C17 C19 -60.7(11) . . . . ? C15 C16 C17 C19 63.3(11) . . . . ? C11 C16 C17 C18 172.7(8) . . . . ? C15 C16 C17 C18 -63.2(11) . . . . ? P1 O3 C21 C26 126.7(9) . . . . ? P1 O3 C21 C22 -112.1(9) . . . . ? O3 C21 C22 C23 -177.4(9) . . . . ? C26 C21 C22 C23 -58.1(11) . . . . ? C21 C22 C23 C24 56.2(13) . . . . ? C21 C22 C23 C30 -177.7(11) . . . . ? C22 C23 C24 C25 -55.5(13) . . . . ? C30 C23 C24 C25 180.0(10) . . . . ? C23 C24 C25 C26 57.2(13) . . . . ? O3 C21 C26 C25 174.4(10) . . . . ? C22 C21 C26 C25 56.6(12) . . . . ? O3 C21 C26 C27 -58.9(11) . . . . ? C22 C21 C26 C27 -176.8(8) . . . . ? C24 C25 C26 C21 -56.1(13) . . . . ? C24 C25 C26 C27 176.9(10) . . . . ? C21 C26 C27 C28 160.0(9) . . . . ? C25 C26 C27 C28 -75.8(12) . . . . ? C21 C26 C27 C29 -72.8(12) . . . . ? C25 C26 C27 C29 51.3(13) . . . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.96 _refine_diff_density_max 5.633 _refine_diff_density_min -2.715 _refine_diff_density_rms 0.255 _database_code_depnum_ccdc_archive 'CCDC 933756' ####################################################################### # # 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_cu_nd259_0m #TrackingRef 'web_deposit_cif_file_6_AntonioM.Echavarren_1365746154.cu_ND259_0mX.cif' _vrf_PLAT_029_global ; PROBLEM: Diffraction measured fraction low ............ 0.85 RESPONSE: The measured sample had a very weak diffraction power and it required a long measurement time what caused ice formation. Therefore all the measured runs could not be used to the refinement and the completeness is lower than the standard requirements. No better crystals could be obtained from this sample. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H47 O4 P Si2' _chemical_formula_weight 955.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.6873(11) _cell_length_b 13.7576(19) _cell_length_c 34.499(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5547.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4971 _cell_measurement_theta_min 4.11 _cell_measurement_theta_max 60.56 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.144 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 1.206 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8889 _exptl_absorpt_correction_T_max 0.9763 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_type CuK\a _diffrn_radiation_source microsource _diffrn_source 'rotating anode X-ray tube' _diffrn_source_power 45 _diffrn_source_current 0.65 _diffrn_source_size '0.2 mm x 0.2 mm fine focus' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 11574 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 4.11 _diffrn_reflns_theta_max 59.04 _reflns_number_total 6083 _reflns_number_gt 5319 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _chemical_absolute_configuration ad _refine_ls_abs_structure_Flack 0.03(3) _refine_ls_number_reflns 6083 _refine_ls_number_parameters 712 _refine_ls_number_restraints 329 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1652 _refine_ls_wR_factor_gt 0.1597 _refine_ls_goodness_of_fit_ref 1.269 _refine_ls_restrained_S_all 1.281 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8831(3) 0.1737(3) 0.81867(10) 0.0561(9) Uani 1 1 d . A . C2 C 0.9711(3) 0.1789(3) 0.79131(10) 0.0568(10) Uani 1 1 d . . . C3 C 0.9379(3) 0.1728(3) 0.75282(10) 0.0591(10) Uani 1 1 d . . . H3 H 0.9940 0.1757 0.7337 0.071 Uiso 1 1 calc R . . C4 C 0.8217(3) 0.1623(3) 0.74117(11) 0.0630(11) Uani 1 1 d . . . C5 C 0.7349(3) 0.1647(3) 0.77017(12) 0.0609(10) Uani 1 1 d . A . C6 C 0.7670(3) 0.1713(3) 0.80990(11) 0.0554(9) Uani 1 1 d . . . C7 C 0.7927(4) 0.1529(3) 0.70166(12) 0.0802(13) Uani 1 1 d . . . H7 H 0.8500 0.1520 0.6830 0.096 Uiso 1 1 calc R . . C8 C 0.6818(5) 0.1452(4) 0.69090(14) 0.0920(15) Uani 1 1 d . . . H8 H 0.6631 0.1396 0.6648 0.110 Uiso 1 1 calc R . . C9 C 0.5940(4) 0.1455(3) 0.71917(14) 0.0892(14) Uani 1 1 d . A . H9 H 0.5180 0.1392 0.7116 0.107 Uiso 1 1 calc R . . C10 C 0.6206(4) 0.1552(3) 0.75748(13) 0.0705(11) Uani 1 1 d . . . H10 H 0.5619 0.1554 0.7757 0.085 Uiso 1 1 calc R A . C11 C 0.6807(3) 0.1111(3) 0.87040(11) 0.0657(11) Uani 1 1 d . . . C12 C 0.6823(6) 0.1732(5) 0.8418(2) 0.0615(9) Uani 0.4875(18) 1 d PDU A 1 C13 C 0.6021(5) 0.2520(4) 0.84631(19) 0.0689(8) Uani 0.4875(18) 1 d PDU A 1 C14 C 0.5252(5) 0.2491(4) 0.87778(19) 0.0719(9) Uani 0.4875(18) 1 d PDU A 1 C15 C 0.5253(6) 0.1667(4) 0.9023(2) 0.0685(10) Uani 0.4875(18) 1 d PDU A 1 H15A H 0.4683 0.1619 0.9210 0.082 Uiso 0.4875(18) 1 calc PR A 1 C16 C 0.6051(6) 0.0928(5) 0.9001(2) 0.0629(11) Uani 0.4875(18) 1 d PDU A 1 C17 C 0.6082(6) 0.3360(4) 0.8239(2) 0.0779(10) Uani 0.4875(18) 1 d PDU A 1 H17A H 0.6635 0.3402 0.8045 0.093 Uiso 0.4875(18) 1 calc PR A 1 C18 C 0.5352(6) 0.4125(5) 0.8293(2) 0.0858(11) Uani 0.4875(18) 1 d PDU A 1 H18A H 0.5389 0.4673 0.8136 0.103 Uiso 0.4875(18) 1 calc PR A 1 C19 C 0.4539(6) 0.4060(5) 0.8596(3) 0.0877(12) Uani 0.4875(18) 1 d PDU A 1 H19A H 0.4013 0.4559 0.8630 0.105 Uiso 0.4875(18) 1 calc PR A 1 C20 C 0.4515(6) 0.3303(5) 0.8830(2) 0.0814(11) Uani 0.4875(18) 1 d PDU A 1 H20A H 0.4001 0.3300 0.9036 0.098 Uiso 0.4875(18) 1 calc PR A 1 C12' C 0.6781(6) 0.1844(5) 0.8404(2) 0.0615(9) Uani 0.5125(18) 1 d PDU A 2 C13' C 0.5964(5) 0.2626(5) 0.8386(2) 0.0689(8) Uani 0.5125(18) 1 d PDU A 2 C14' C 0.5084(5) 0.2658(5) 0.8665(2) 0.0719(9) Uani 0.5125(18) 1 d PDU A 2 C15' C 0.5053(6) 0.1938(5) 0.8957(2) 0.0685(10) Uani 0.5125(18) 1 d PDU A 2 H15' H 0.4460 0.1961 0.9137 0.082 Uiso 0.5125(18) 1 calc PR A 2 C16' C 0.5850(6) 0.1201(5) 0.8993(2) 0.0629(11) Uani 0.5125(18) 1 d PDU A 2 C17' C 0.5991(6) 0.3341(5) 0.8100(2) 0.0779(10) Uani 0.5125(18) 1 d PDU A 2 H17' H 0.6558 0.3315 0.7911 0.093 Uiso 0.5125(18) 1 calc PR A 2 C18' C 0.5206(6) 0.4079(5) 0.8089(3) 0.0858(11) Uani 0.5125(18) 1 d PDU A 2 H18' H 0.5261 0.4569 0.7904 0.103 Uiso 0.5125(18) 1 calc PR A 2 C19' C 0.4311(6) 0.4082(5) 0.8365(3) 0.0877(12) Uani 0.5125(18) 1 d PDU A 2 H19' H 0.3740 0.4551 0.8350 0.105 Uiso 0.5125(18) 1 calc PR A 2 C20' C 0.4276(6) 0.3427(5) 0.8644(3) 0.0814(11) Uani 0.5125(18) 1 d PDU A 2 H20' H 0.3708 0.3470 0.8831 0.098 Uiso 0.5125(18) 1 calc PR A 2 C21 C 1.1884(3) 0.2821(3) 0.76576(11) 0.0608(10) Uani 1 1 d . . . C22 C 1.3041(4) 0.2809(4) 0.75855(17) 0.1024(17) Uani 1 1 d . . . H22 H 1.3493 0.2342 0.7706 0.123 Uiso 1 1 calc R . . C23 C 1.3550(5) 0.3467(5) 0.73405(19) 0.129(2) Uani 1 1 d . . . H23 H 1.4338 0.3453 0.7304 0.155 Uiso 1 1 calc R . . C24 C 1.2893(5) 0.4148(4) 0.71487(16) 0.1041(17) Uani 1 1 d . . . H24 H 1.3230 0.4581 0.6976 0.125 Uiso 1 1 calc R . . C25 C 1.1754(4) 0.4178(3) 0.72152(14) 0.0848(13) Uani 1 1 d . . . H25 H 1.1300 0.4636 0.7090 0.102 Uiso 1 1 calc R . . C26 C 1.1274(4) 0.3529(3) 0.74678(12) 0.0718(11) Uani 1 1 d . . . H26 H 1.0491 0.3570 0.7514 0.086 Uiso 1 1 calc R . . C27 C 1.2073(3) 0.0854(3) 0.80511(12) 0.0652(11) Uani 1 1 d . . . C28 C 1.1714(4) 0.0043(3) 0.78535(14) 0.0854(14) Uani 1 1 d . . . H28 H 1.1021 0.0063 0.7721 0.103 Uiso 1 1 calc R . . C29 C 1.2351(6) -0.0799(4) 0.7846(2) 0.127(2) Uani 1 1 d . . . H29 H 1.2072 -0.1344 0.7717 0.153 Uiso 1 1 calc R . . C30 C 1.3401(5) -0.0838(5) 0.8029(3) 0.136(2) Uani 1 1 d . . . H30 H 1.3840 -0.1401 0.8021 0.163 Uiso 1 1 calc R . . C32 C 1.3133(4) 0.0796(4) 0.82324(15) 0.0889(15) Uani 1 1 d . . . H32 H 1.3414 0.1333 0.8365 0.107 Uiso 1 1 calc R . . C33 C 1.3777(4) -0.0047(4) 0.8218(2) 0.118(2) Uani 1 1 d . . . H33 H 1.4483 -0.0067 0.8342 0.142 Uiso 1 1 calc R . . C34 C 1.1399(2) 0.2685(2) 0.85145(7) 0.0739(12) Uani 1 1 d G . . C35 C 1.1286(3) 0.3690(2) 0.85130(10) 0.0999(16) Uani 1 1 d G . . H35A H 1.1165 0.4018 0.8281 0.120 Uiso 1 1 calc R . . C36 C 1.1353(4) 0.4206(2) 0.88587(13) 0.153(3) Uani 1 1 d G . . H36A H 1.1277 0.4879 0.8858 0.184 Uiso 1 1 calc R . . C37 C 1.1533(4) 0.3717(4) 0.92058(10) 0.156(3) Uani 1 1 d G . . H37A H 1.1577 0.4062 0.9437 0.188 Uiso 1 1 calc R . . C38 C 1.1646(3) 0.2711(4) 0.92072(7) 0.122(2) Uani 1 1 d G . . H38A H 1.1766 0.2383 0.9439 0.146 Uiso 1 1 calc R . . C39 C 1.1579(3) 0.2195(2) 0.88616(9) 0.0935(15) Uani 1 1 d G . . H39A H 1.1655 0.1522 0.8863 0.112 Uiso 1 1 calc R . . Si2 Si 0.6055(2) -0.0149(3) 0.93583(8) 0.0714(9) Uani 0.4875(18) 1 d P A 1 C40 C 0.4766(4) -0.0045(6) 0.96835(17) 0.095(4) Uani 0.4875(18) 1 d PG A 1 C41 C 0.3680(5) 0.0013(7) 0.95203(18) 0.121(3) Uani 0.4875(18) 1 d PG A 1 H41A H 0.3598 0.0050 0.9253 0.145 Uiso 0.4875(18) 1 calc PR A 1 C42 C 0.2719(4) 0.0017(8) 0.9757(3) 0.151(4) Uani 0.4875(18) 1 d PG A 1 H42A H 0.1992 0.0056 0.9648 0.182 Uiso 0.4875(18) 1 calc PR A 1 C43 C 0.2842(6) -0.0038(9) 1.0157(2) 0.153(5) Uani 0.4875(18) 1 d PG A 1 H43A H 0.2198 -0.0035 1.0316 0.183 Uiso 0.4875(18) 1 calc PR A 1 C44 C 0.3927(7) -0.0096(9) 1.03206(17) 0.170(5) Uani 0.4875(18) 1 d PG A 1 H44A H 0.4010 -0.0132 1.0588 0.204 Uiso 0.4875(18) 1 calc PR A 1 C45 C 0.4889(5) -0.0099(8) 1.00837(18) 0.133(4) Uani 0.4875(18) 1 d PG A 1 H45A H 0.5615 -0.0138 1.0193 0.160 Uiso 0.4875(18) 1 calc PR A 1 Si2' Si 0.5895(3) 0.0367(3) 0.94167(9) 0.0794(10) Uani 0.5125(18) 1 d P A 2 C40' C 0.4580(2) 0.0607(3) 0.97180(9) 0.095(4) Uani 0.5125(18) 1 d PG A 2 C41' C 0.35629(19) 0.0170(3) 0.96035(10) 0.121(3) Uani 0.5125(18) 1 d PG A 2 H41B H 0.3543 -0.0212 0.9381 0.145 Uiso 0.5125(18) 1 calc PR A 2 C42' C 0.2575(2) 0.0304(4) 0.98212(12) 0.151(4) Uani 0.5125(18) 1 d PG A 2 H42B H 0.1894 0.0011 0.9745 0.182 Uiso 0.5125(18) 1 calc PR A 2 C43' C 0.2604(2) 0.0875(4) 1.01535(12) 0.153(5) Uani 0.5125(18) 1 d PG A 2 H43B H 0.1943 0.0964 1.0299 0.183 Uiso 0.5125(18) 1 calc PR A 2 C44' C 0.3621(3) 0.1312(4) 1.02680(11) 0.170(5) Uani 0.5125(18) 1 d PG A 2 H44B H 0.3641 0.1694 1.0490 0.204 Uiso 0.5125(18) 1 calc PR A 2 C45' C 0.4610(2) 0.1178(3) 1.00503(9) 0.133(4) Uani 0.5125(18) 1 d PG A 2 H45B H 0.5290 0.1471 1.0127 0.160 Uiso 0.5125(18) 1 calc PR A 2 C46 C 0.5971(2) -0.1382(2) 0.91181(9) 0.1086(18) Uani 0.4875(18) 1 d PGU A 1 C47 C 0.5620(3) -0.2132(2) 0.93608(12) 0.1158(18) Uani 0.4875(18) 1 d PGU A 1 H47A H 0.5410 -0.1998 0.9615 0.139 Uiso 0.4875(18) 1 calc PR A 1 C48 C 0.5583(3) -0.3081(2) 0.92232(15) 0.1173(18) Uani 0.4875(18) 1 d PGU A 1 H48A H 0.5348 -0.3582 0.9386 0.141 Uiso 0.4875(18) 1 calc PR A 1 C49 C 0.5898(4) -0.3280(3) 0.88429(15) 0.1165(18) Uani 0.4875(18) 1 d PGU A 1 H49A H 0.5873 -0.3915 0.8751 0.140 Uiso 0.4875(18) 1 calc PR A 1 C50 C 0.6249(3) -0.2531(3) 0.86002(13) 0.1115(18) Uani 0.4875(18) 1 d PGU A 1 H50A H 0.6459 -0.2665 0.8346 0.134 Uiso 0.4875(18) 1 calc PR A 1 C51 C 0.6286(3) -0.1582(3) 0.87378(10) 0.1094(19) Uani 0.4875(18) 1 d PGU A 1 H51A H 0.6521 -0.1081 0.8575 0.131 Uiso 0.4875(18) 1 calc PR A 1 C46' C 0.5901(2) -0.0971(2) 0.92947(9) 0.100(4) Uani 0.5125(18) 1 d PG A 2 C47' C 0.5901(2) -0.1619(2) 0.96039(10) 0.155(6) Uani 0.5125(18) 1 d PG A 2 H47B H 0.5864 -0.1387 0.9857 0.186 Uiso 0.5125(18) 1 calc PR A 2 C48' C 0.5957(3) -0.2613(2) 0.95351(13) 0.197(8) Uani 0.5125(18) 1 d PG A 2 H48B H 0.5957 -0.3046 0.9742 0.236 Uiso 0.5125(18) 1 calc PR A 2 C49' C 0.6012(3) -0.2960(2) 0.91571(14) 0.234(11) Uani 0.5125(18) 1 d PG A 2 H49B H 0.6049 -0.3625 0.9111 0.280 Uiso 0.5125(18) 1 calc PR A 2 C50' C 0.6012(3) -0.2312(3) 0.88479(12) 0.162(6) Uani 0.5125(18) 1 d PG A 2 H50B H 0.6048 -0.2544 0.8595 0.194 Uiso 0.5125(18) 1 calc PR A 2 C51' C 0.5956(3) -0.1318(3) 0.89167(9) 0.124(5) Uani 0.5125(18) 1 d PG A 2 H51B H 0.5955 -0.0884 0.8710 0.149 Uiso 0.5125(18) 1 calc PR A 2 C52 C 0.74089(19) -0.0035(3) 0.96475(7) 0.099(3) Uani 0.4875(18) 1 d PG A 1 C53 C 0.7700(2) 0.0831(3) 0.98297(8) 0.098(3) Uani 0.4875(18) 1 d PG A 1 H53A H 0.7202 0.1358 0.9820 0.118 Uiso 0.4875(18) 1 calc PR A 1 C54 C 0.8735(2) 0.0911(4) 1.00257(9) 0.161(4) Uani 0.4875(18) 1 d PG A 1 H54A H 0.8929 0.1490 1.0148 0.194 Uiso 0.4875(18) 1 calc PR A 1 C55 C 0.9479(2) 0.0123(4) 1.00396(9) 0.161(4) Uani 0.4875(18) 1 d PG A 1 H55A H 1.0171 0.0176 1.0171 0.194 Uiso 0.4875(18) 1 calc PR A 1 C56 C 0.9188(2) -0.0744(4) 0.98575(10) 0.139(5) Uani 0.4875(18) 1 d PG A 1 H56A H 0.9685 -0.1271 0.9867 0.167 Uiso 0.4875(18) 1 calc PR A 1 C57 C 0.8153(2) -0.0823(3) 0.96615(9) 0.101(4) Uani 0.4875(18) 1 d PG A 1 H57A H 0.7958 -0.1403 0.9540 0.121 Uiso 0.4875(18) 1 calc PR A 1 C52' C 0.7237(2) 0.0731(3) 0.96784(7) 0.098(3) Uani 0.5125(18) 1 d PG A 2 C53' C 0.7455(3) 0.1721(3) 0.97107(9) 0.105(4) Uani 0.5125(18) 1 d PG A 2 H53B H 0.6935 0.2169 0.9612 0.126 Uiso 0.5125(18) 1 calc PR A 2 C54' C 0.8451(3) 0.2041(3) 0.98905(10) 0.139(5) Uani 0.5125(18) 1 d PG A 2 H54B H 0.8597 0.2704 0.9912 0.167 Uiso 0.5125(18) 1 calc PR A 2 C55' C 0.9228(2) 0.1372(4) 1.00379(10) 0.161(4) Uani 0.5125(18) 1 d PG A 2 H55B H 0.9894 0.1586 1.0158 0.194 Uiso 0.5125(18) 1 calc PR A 2 C56' C 0.9010(2) 0.0382(4) 1.00056(9) 0.161(4) Uani 0.5125(18) 1 d PG A 2 H56B H 0.9530 -0.0066 1.0104 0.194 Uiso 0.5125(18) 1 calc PR A 2 C57' C 0.80143(19) 0.0061(3) 0.98259(8) 0.099(3) Uani 0.5125(18) 1 d PG A 2 H57B H 0.7868 -0.0601 0.9804 0.118 Uiso 0.5125(18) 1 calc PR A 2 C58 C 1.0118(5) -0.07634(14) 0.88150(6) 0.1034(17) Uani 0.4875(18) 1 d PDU A 1 C59 C 0.9329(7) -0.14042(19) 0.89925(8) 0.1166(18) Uani 0.4875(18) 1 d PDU A 1 H59 H 0.8542 -0.1303 0.8994 0.140 Uiso 0.4875(18) 1 calc PR A 1 C60 C 0.9905(10) -0.2282(4) 0.91826(12) 0.1224(17) Uani 0.4875(18) 1 d PDU A 1 H60 H 0.9487 -0.2761 0.9310 0.147 Uiso 0.4875(18) 1 calc PR A 1 C61 C 1.1092(11) -0.2323(4) 0.91543(11) 0.1222(15) Uani 0.4875(18) 1 d PDU A 1 C62 C 1.1714(5) -0.1758(3) 0.90001(9) 0.1097(13) Uani 1 1 d DU . . H62 H 1.2502 -0.1853 0.8997 0.132 Uiso 0.4875(18) 1 calc PR A 1 H62' H 1.2462 -0.1755 0.9092 0.132 Uiso 0.5125(18) 1 calc PR A 2 C63 C 1.1217(5) -0.0948(3) 0.88240(9) 0.1004(12) Uani 1 1 d DU A . H63 H 1.1704 -0.0506 0.8704 0.120 Uiso 0.4875(18) 1 calc PR A 1 H63' H 1.1687 -0.0431 0.8755 0.120 Uiso 0.5125(18) 1 calc PR A 2 C64 C 1.2749(13) -0.3283(6) 0.93294(19) 0.148(4) Uani 0.4875(18) 1 d PDU A 1 H64A H 1.3089 -0.2863 0.9519 0.222 Uiso 0.4875(18) 1 calc PR A 1 H64B H 1.3005 -0.3099 0.9075 0.222 Uiso 0.4875(18) 1 calc PR A 1 H64C H 1.2970 -0.3943 0.9381 0.222 Uiso 0.4875(18) 1 calc PR A 1 O4 O 1.1484(9) -0.3199(5) 0.93498(15) 0.137(2) Uani 0.4875(18) 1 d PDU A 1 C58' C 1.0111(2) -0.0882(5) 0.87504(10) 0.0772(18) Uani 0.5125(18) 1 d PDU A 2 C59' C 0.9502(4) -0.1678(6) 0.87465(12) 0.0952(17) Uani 0.5125(18) 1 d PDU A 2 H59' H 0.8762 -0.1660 0.8648 0.114 Uiso 0.5125(18) 1 calc PR A 2 C60' C 0.9933(6) -0.2546(7) 0.88864(14) 0.1090(17) Uani 0.5125(18) 1 d PDU A 2 H60' H 0.9478 -0.3100 0.8880 0.131 Uiso 0.5125(18) 1 calc PR A 2 C61' C 1.0985(7) -0.2604(8) 0.90301(13) 0.1164(18) Uani 0.5125(18) 1 d PDU A 2 C64' C 1.2441(12) -0.3649(11) 0.9322(3) 0.143(4) Uani 0.5125(18) 1 d PDU A 2 H64D H 1.2635 -0.3101 0.9481 0.215 Uiso 0.5125(18) 1 calc PR A 2 H64E H 1.2988 -0.3708 0.9115 0.215 Uiso 0.5125(18) 1 calc PR A 2 H64F H 1.2450 -0.4230 0.9476 0.215 Uiso 0.5125(18) 1 calc PR A 2 O4' O 1.1290(8) -0.3508(6) 0.91567(16) 0.131(2) Uani 0.5125(18) 1 d PDU A 2 O1 O 0.9117(2) 0.17380(19) 0.85776(7) 0.0646(7) Uani 1 1 d . . . O2 O 0.7683(2) 0.0409(2) 0.87132(8) 0.0692(7) Uani 1 1 d . A . O3 O 0.9676(2) 0.0016(2) 0.85975(8) 0.0827(9) Uani 1 1 d . . . P1 P 0.89709(9) 0.07998(9) 0.88545(3) 0.0720(3) Uani 1 1 d . A . Si1 Si 1.12587(8) 0.20204(7) 0.80400(3) 0.0558(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.056(2) 0.058(2) 0.0545(19) 0.0026(16) 0.0029(17) 0.0002(18) C2 0.058(2) 0.055(2) 0.058(2) 0.0051(17) 0.0082(17) -0.0003(17) C3 0.066(2) 0.053(3) 0.059(2) 0.0043(18) 0.0081(18) -0.0021(18) C4 0.066(2) 0.061(3) 0.062(2) 0.0053(19) -0.0079(19) -0.0041(19) C5 0.061(2) 0.047(2) 0.075(3) 0.0137(19) -0.0087(19) 0.0005(17) C6 0.0479(18) 0.050(2) 0.068(2) 0.0011(18) 0.0023(17) 0.0000(16) C7 0.091(3) 0.088(3) 0.061(3) 0.003(2) -0.006(2) -0.005(2) C8 0.113(4) 0.087(3) 0.076(3) 0.008(2) -0.032(3) -0.007(3) C9 0.093(3) 0.079(3) 0.096(3) 0.012(3) -0.032(3) 0.009(3) C10 0.062(2) 0.059(3) 0.091(3) 0.011(2) -0.008(2) -0.0028(19) C11 0.0491(19) 0.083(3) 0.065(2) -0.002(2) 0.0037(18) -0.016(2) C12 0.0478(16) 0.058(2) 0.079(2) -0.0010(18) 0.0069(16) -0.0039(14) C13 0.0542(14) 0.0626(16) 0.0900(17) -0.0006(14) 0.0049(14) -0.0001(13) C14 0.0522(15) 0.0685(17) 0.0950(18) -0.0047(15) 0.0078(15) 0.0043(13) C15 0.0482(18) 0.070(2) 0.088(2) -0.0059(16) 0.0108(17) 0.0036(16) C16 0.043(2) 0.066(2) 0.080(2) -0.006(2) 0.0097(19) -0.0010(17) C17 0.0674(18) 0.0677(18) 0.099(2) 0.0029(17) 0.0022(19) 0.0042(15) C18 0.078(2) 0.073(2) 0.106(2) 0.004(2) 0.001(2) 0.0109(17) C19 0.075(2) 0.077(2) 0.111(3) 0.001(2) 0.003(2) 0.0159(19) C20 0.062(2) 0.076(2) 0.106(2) -0.0014(19) 0.005(2) 0.0116(17) C12' 0.0478(16) 0.058(2) 0.079(2) -0.0010(18) 0.0069(16) -0.0039(14) C13' 0.0542(14) 0.0626(16) 0.0900(17) -0.0006(14) 0.0049(14) -0.0001(13) C14' 0.0522(15) 0.0685(17) 0.0950(18) -0.0047(15) 0.0078(15) 0.0043(13) C15' 0.0482(18) 0.070(2) 0.088(2) -0.0059(16) 0.0108(17) 0.0036(16) C16' 0.043(2) 0.066(2) 0.080(2) -0.006(2) 0.0097(19) -0.0010(17) C17' 0.0674(18) 0.0677(18) 0.099(2) 0.0029(17) 0.0022(19) 0.0042(15) C18' 0.078(2) 0.073(2) 0.106(2) 0.004(2) 0.001(2) 0.0109(17) C19' 0.075(2) 0.077(2) 0.111(3) 0.001(2) 0.003(2) 0.0159(19) C20' 0.062(2) 0.076(2) 0.106(2) -0.0014(19) 0.005(2) 0.0116(17) C21 0.059(2) 0.054(3) 0.069(2) 0.0015(19) 0.0036(19) 0.0001(18) C22 0.067(3) 0.096(4) 0.144(4) 0.047(3) 0.027(3) 0.005(3) C23 0.083(3) 0.134(5) 0.171(5) 0.074(4) 0.057(3) 0.010(3) C24 0.117(4) 0.077(3) 0.119(4) 0.038(3) 0.044(3) 0.012(3) C25 0.097(3) 0.057(3) 0.100(3) 0.007(3) 0.008(3) 0.003(2) C26 0.068(2) 0.068(3) 0.079(3) 0.019(2) 0.003(2) 0.000(2) C27 0.056(2) 0.061(3) 0.079(2) 0.005(2) 0.012(2) 0.0006(18) C28 0.079(3) 0.073(3) 0.104(3) -0.009(3) 0.010(3) 0.008(2) C29 0.120(4) 0.056(3) 0.205(7) -0.023(4) 0.049(4) 0.001(3) C30 0.089(4) 0.085(4) 0.234(7) 0.015(5) 0.054(4) 0.023(3) C32 0.064(3) 0.077(3) 0.125(4) 0.024(3) 0.004(3) 0.001(2) C33 0.060(3) 0.091(4) 0.205(6) 0.041(4) 0.020(3) 0.013(3) C34 0.052(2) 0.092(3) 0.077(3) -0.011(2) 0.0061(19) -0.008(2) C35 0.089(3) 0.097(4) 0.114(4) -0.036(3) -0.005(3) 0.020(3) C36 0.148(6) 0.160(6) 0.151(5) -0.088(5) -0.021(5) 0.015(5) C37 0.109(5) 0.230(8) 0.131(5) -0.099(5) 0.003(4) 0.027(5) C38 0.093(4) 0.207(7) 0.065(3) -0.030(4) 0.009(3) -0.024(4) C39 0.066(3) 0.143(4) 0.072(3) 0.005(3) 0.001(2) -0.014(3) Si2 0.0524(13) 0.098(3) 0.0638(14) 0.0121(16) 0.0079(11) -0.0073(15) C40 0.068(3) 0.147(11) 0.071(3) -0.002(5) 0.012(3) -0.029(5) C41 0.069(3) 0.190(7) 0.104(5) 0.004(5) 0.004(3) -0.036(4) C42 0.053(3) 0.258(11) 0.143(6) 0.020(7) 0.013(4) -0.019(5) C43 0.090(5) 0.258(17) 0.111(6) 0.008(10) 0.044(5) -0.019(9) C44 0.092(6) 0.334(16) 0.085(5) 0.015(8) 0.019(5) -0.010(9) C45 0.065(4) 0.253(11) 0.082(4) 0.001(7) -0.002(4) 0.010(6) Si2' 0.0593(15) 0.104(3) 0.0747(17) 0.0244(17) -0.0006(12) -0.0069(15) C40' 0.068(3) 0.147(11) 0.071(3) -0.002(5) 0.012(3) -0.029(5) C41' 0.069(3) 0.190(7) 0.104(5) 0.004(5) 0.004(3) -0.036(4) C42' 0.053(3) 0.258(11) 0.143(6) 0.020(7) 0.013(4) -0.019(5) C43' 0.090(5) 0.258(17) 0.111(6) 0.008(10) 0.044(5) -0.019(9) C44' 0.092(6) 0.334(16) 0.085(5) 0.015(8) 0.019(5) -0.010(9) C45' 0.065(4) 0.253(11) 0.082(4) 0.001(7) -0.002(4) 0.010(6) C46 0.109(4) 0.098(3) 0.119(3) 0.028(3) 0.013(3) 0.000(3) C47 0.121(4) 0.102(3) 0.124(3) 0.030(3) 0.017(3) -0.003(4) C48 0.121(4) 0.102(3) 0.129(3) 0.029(3) 0.017(3) -0.006(4) C49 0.115(4) 0.103(3) 0.131(3) 0.022(3) 0.010(4) -0.003(3) C50 0.107(4) 0.104(3) 0.123(3) 0.021(3) 0.009(3) -0.002(4) C51 0.105(4) 0.103(3) 0.120(3) 0.025(3) 0.011(3) -0.001(4) C46' 0.069(5) 0.069(7) 0.163(10) 0.059(7) -0.012(6) -0.020(5) C47' 0.208(14) 0.132(10) 0.124(9) 0.046(8) -0.018(10) -0.071(10) C48' 0.231(19) 0.148(13) 0.212(16) 0.095(13) 0.006(15) -0.002(14) C49' 0.31(2) 0.129(14) 0.26(2) 0.049(14) 0.15(2) -0.034(15) C50' 0.160(13) 0.168(14) 0.157(12) 0.013(11) 0.017(11) -0.030(11) C51' 0.089(7) 0.069(7) 0.215(14) 0.042(8) -0.013(9) -0.031(6) C52 0.081(5) 0.145(7) 0.070(5) 0.024(5) -0.009(3) -0.031(5) C53 0.073(5) 0.132(6) 0.090(6) 0.007(5) 0.027(5) -0.020(5) C54 0.095(5) 0.290(12) 0.100(3) 0.013(6) -0.014(3) -0.050(6) C55 0.095(5) 0.290(12) 0.100(3) 0.013(6) -0.014(3) -0.050(6) C56 0.075(7) 0.239(16) 0.103(8) 0.021(9) 0.016(6) 0.039(9) C57 0.083(6) 0.143(10) 0.078(6) 0.026(6) -0.016(5) -0.004(6) C52' 0.073(5) 0.132(6) 0.090(6) 0.007(5) 0.027(5) -0.020(5) C53' 0.066(5) 0.183(11) 0.067(5) -0.029(6) 0.017(4) -0.023(6) C54' 0.100(8) 0.199(14) 0.118(9) -0.009(9) 0.014(7) 0.009(9) C55' 0.095(5) 0.290(12) 0.100(3) 0.013(6) -0.014(3) -0.050(6) C56' 0.095(5) 0.290(12) 0.100(3) 0.013(6) -0.014(3) -0.050(6) C57' 0.081(5) 0.145(7) 0.070(5) 0.024(5) -0.009(3) -0.031(5) C58 0.087(3) 0.093(3) 0.130(3) 0.038(3) 0.004(3) -0.003(3) C59 0.099(3) 0.105(3) 0.146(4) 0.041(3) 0.006(3) -0.007(3) C60 0.111(3) 0.107(3) 0.149(4) 0.052(3) 0.004(3) -0.010(3) C61 0.113(3) 0.103(3) 0.150(3) 0.052(3) -0.011(3) -0.001(2) C62 0.095(2) 0.095(3) 0.139(3) 0.032(2) -0.005(2) 0.003(2) C63 0.088(2) 0.085(2) 0.128(3) 0.032(2) 0.003(2) 0.000(2) C64 0.138(4) 0.117(7) 0.190(8) 0.064(7) -0.026(7) 0.016(5) O4 0.134(3) 0.113(4) 0.165(4) 0.059(3) -0.022(4) 0.003(3) C58' 0.082(4) 0.081(3) 0.069(4) 0.018(3) -0.031(3) -0.020(3) C59' 0.102(3) 0.088(3) 0.096(3) 0.013(3) -0.027(3) -0.025(3) C60' 0.125(3) 0.086(3) 0.116(4) 0.014(3) -0.030(3) -0.019(3) C61' 0.139(3) 0.086(3) 0.125(4) 0.016(3) -0.039(3) -0.006(3) C64' 0.149(6) 0.109(7) 0.172(8) 0.035(6) -0.033(6) 0.008(6) O4' 0.157(4) 0.090(4) 0.146(4) 0.019(3) -0.043(4) -0.001(3) O1 0.0588(14) 0.0812(19) 0.0536(14) -0.0010(12) 0.0021(12) -0.0088(13) O2 0.0595(14) 0.0791(19) 0.0689(16) 0.0140(14) -0.0052(12) -0.0106(14) O3 0.0703(16) 0.104(2) 0.0737(17) 0.0216(16) -0.0078(14) 0.0122(16) P1 0.0567(5) 0.1015(8) 0.0579(5) 0.0139(6) -0.0026(5) -0.0121(6) Si1 0.0504(5) 0.0556(7) 0.0615(6) 0.0026(5) 0.0070(5) 0.0000(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.389(4) . ? C1 C6 1.391(5) . ? C1 C2 1.398(5) . ? C2 C3 1.386(5) . ? C2 Si1 1.888(4) . ? C3 C4 1.423(5) . ? C4 C7 1.411(6) . ? C4 C5 1.426(5) . ? C5 C10 1.412(5) . ? C5 C6 1.424(5) . ? C6 C12 1.482(7) . ? C6 C12' 1.491(7) . ? C7 C8 1.353(6) . ? C8 C9 1.416(7) . ? C9 C10 1.364(6) . ? C11 C12 1.304(8) . ? C11 C16 1.377(8) . ? C11 O2 1.409(5) . ? C11 C12' 1.444(8) . ? C11 C16' 1.503(8) . ? C12 C13 1.441(6) . ? C13 C17 1.393(7) . ? C13 C14 1.410(6) . ? C14 C15 1.414(7) . ? C14 C20 1.422(7) . ? C15 C16 1.381(7) . ? C16 Si2 1.927(7) . ? C17 C18 1.368(7) . ? C18 C19 1.415(9) . ? C19 C20 1.319(9) . ? C12' C13' 1.440(6) . ? C13' C17' 1.395(7) . ? C13' C14' 1.409(6) . ? C14' C15' 1.414(7) . ? C14' C20' 1.420(7) . ? C15' C16' 1.381(7) . ? C16' Si2' 1.861(8) . ? C17' C18' 1.369(7) . ? C18' C19' 1.414(9) . ? C19' C20' 1.318(9) . ? C21 C26 1.374(6) . ? C21 C22 1.375(6) . ? C21 Si1 1.868(4) . ? C22 C23 1.373(7) . ? C23 C24 1.380(7) . ? C24 C25 1.352(7) . ? C25 C26 1.367(6) . ? C27 C28 1.373(6) . ? C27 C32 1.390(6) . ? C27 Si1 1.867(4) . ? C28 C29 1.377(7) . ? C29 C30 1.382(9) . ? C30 C33 1.342(9) . ? C32 C33 1.384(7) . ? C34 C35 1.3900 . ? C34 C39 1.3900 . ? C34 Si1 1.882(3) . ? C35 C36 1.3900 . ? C36 C37 1.3900 . ? C37 C38 1.3900 . ? C38 C39 1.3900 . ? Si2 C52 1.878(4) . ? Si2 C40 1.884(6) . ? Si2 C46 1.890(5) . ? C40 C41 1.3900 . ? C40 C45 1.3900 . ? C41 C42 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? Si2' C52' 1.878(4) . ? Si2' C40' 1.884(4) . ? Si2' C46' 1.888(5) . ? C40' C41' 1.3900 . ? C40' C45' 1.3900 . ? C41' C42' 1.3900 . ? C42' C43' 1.3900 . ? C43' C44' 1.3900 . ? C44' C45' 1.3900 . ? C46 C47 1.3900 . ? C46 C51 1.3900 . ? C47 C48 1.3900 . ? C48 C49 1.3900 . ? C49 C50 1.3900 . ? C50 C51 1.3900 . ? C46' C47' 1.3900 . ? C46' C51' 1.3900 . ? C47' C48' 1.3900 . ? C48' C49' 1.3900 . ? C49' C50' 1.3900 . ? C50' C51' 1.3900 . ? C52 C53 1.3900 . ? C52 C57 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C56 C57 1.3900 . ? C52' C53' 1.3900 . ? C52' C57' 1.3900 . ? C53' C54' 1.3900 . ? C54' C55' 1.3900 . ? C55' C56' 1.3900 . ? C56' C57' 1.3900 . ? C58 C63 1.310(8) . ? C58 O3 1.406(4) . ? C58 C59 1.415(7) . ? C59 C60 1.531(8) . ? C60 C61 1.391(17) . ? C61 C62 1.190(10) . ? C61 O4 1.455(10) . ? C62 C63 1.396(6) . ? C62 C61' 1.445(11) . ? C63 C58' 1.321(6) . ? C64 O4 1.484(18) . ? C58' C59' 1.306(9) . ? C58' O3 1.435(7) . ? C59' C60' 1.384(12) . ? C60' C61' 1.327(11) . ? C61' O4' 1.366(13) . ? C64' O4' 1.473(16) . ? O1 P1 1.615(3) . ? O2 P1 1.671(3) . ? O3 P1 1.621(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 O1 C1 C6 116.5(3) . . ? O1 C1 C2 118.6(3) . . ? C6 C1 C2 124.9(3) . . ? C3 C2 C1 115.9(3) . . ? C3 C2 Si1 120.1(3) . . ? C1 C2 Si1 123.9(3) . . ? C2 C3 C4 123.0(3) . . ? C7 C4 C3 120.7(4) . . ? C7 C4 C5 120.6(4) . . ? C3 C4 C5 118.6(3) . . ? C10 C5 C6 123.6(4) . . ? C10 C5 C4 117.0(4) . . ? C6 C5 C4 119.3(3) . . ? C1 C6 C5 117.9(3) . . ? C1 C6 C12 119.3(4) . . ? C5 C6 C12 122.7(4) . . ? C1 C6 C12' 121.6(5) . . ? C5 C6 C12' 120.3(4) . . ? C12 C6 C12' 6.5(3) . . ? C8 C7 C4 120.2(4) . . ? C7 C8 C9 120.4(4) . . ? C10 C9 C8 120.2(4) . . ? C9 C10 C5 121.7(4) . . ? C12 C11 C16 133.8(5) . . ? C12 C11 O2 117.1(4) . . ? C16 C11 O2 108.9(4) . . ? C12 C11 C12' 3.9(4) . . ? C16 C11 C12' 130.3(5) . . ? O2 C11 C12' 120.7(4) . . ? C12 C11 C16' 117.2(4) . . ? C16 C11 C16' 17.1(3) . . ? O2 C11 C16' 125.7(4) . . ? C12' C11 C16' 113.6(4) . . ? C11 C12 C13 113.7(5) . . ? C11 C12 C6 124.1(4) . . ? C13 C12 C6 121.8(5) . . ? C17 C13 C14 118.9(4) . . ? C17 C13 C12 122.1(5) . . ? C14 C13 C12 118.4(5) . . ? C13 C14 C15 118.8(4) . . ? C13 C14 C20 117.5(5) . . ? C15 C14 C20 123.6(5) . . ? C16 C15 C14 123.9(5) . . ? C11 C16 C15 109.8(5) . . ? C11 C16 Si2 128.0(4) . . ? C15 C16 Si2 122.2(5) . . ? C18 C17 C13 122.0(6) . . ? C17 C18 C19 118.1(6) . . ? C20 C19 C18 121.2(6) . . ? C19 C20 C14 122.0(6) . . ? C13' C12' C11 124.5(5) . . ? C13' C12' C6 121.5(5) . . ? C11 C12' C6 114.0(4) . . ? C17' C13' C14' 118.7(5) . . ? C17' C13' C12' 122.8(5) . . ? C14' C13' C12' 118.5(5) . . ? C13' C14' C15' 119.0(5) . . ? C13' C14' C20' 118.2(5) . . ? C15' C14' C20' 122.9(5) . . ? C16' C15' C14' 124.0(5) . . ? C15' C16' C11 120.3(5) . . ? C15' C16' Si2' 122.8(5) . . ? C11 C16' Si2' 116.7(4) . . ? C18' C17' C13' 121.7(6) . . ? C17' C18' C19' 118.7(6) . . ? C20' C19' C18' 120.8(6) . . ? C19' C20' C14' 121.8(6) . . ? C26 C21 C22 115.6(4) . . ? C26 C21 Si1 123.5(3) . . ? C22 C21 Si1 120.4(3) . . ? C23 C22 C21 121.9(5) . . ? C22 C23 C24 120.1(5) . . ? C25 C24 C23 119.1(5) . . ? C24 C25 C26 119.5(5) . . ? C25 C26 C21 123.6(4) . . ? C28 C27 C32 116.8(4) . . ? C28 C27 Si1 122.1(3) . . ? C32 C27 Si1 120.8(3) . . ? C27 C28 C29 121.8(5) . . ? C28 C29 C30 120.3(6) . . ? C33 C30 C29 118.8(5) . . ? C33 C32 C27 121.1(5) . . ? C30 C33 C32 121.2(6) . . ? C35 C34 C39 120.0 . . ? C35 C34 Si1 118.17(17) . . ? C39 C34 Si1 121.81(17) . . ? C34 C35 C36 120.0 . . ? C37 C36 C35 120.0 . . ? C36 C37 C38 120.0 . . ? C39 C38 C37 120.0 . . ? C38 C39 C34 120.0 . . ? C52 Si2 C40 110.6(2) . . ? C52 Si2 C46 110.6(2) . . ? C40 Si2 C46 106.8(3) . . ? C52 Si2 C16 106.1(3) . . ? C40 Si2 C16 108.7(3) . . ? C46 Si2 C16 114.2(3) . . ? C41 C40 C45 120.0 . . ? C41 C40 Si2 119.5(3) . . ? C45 C40 Si2 120.3(3) . . ? C40 C41 C42 120.0 . . ? C41 C42 C43 120.0 . . ? C44 C43 C42 120.0 . . ? C45 C44 C43 120.0 . . ? C44 C45 C40 120.0 . . ? C16' Si2' C52' 103.7(3) . . ? C16' Si2' C40' 107.6(3) . . ? C52' Si2' C40' 111.7(2) . . ? C16' Si2' C46' 115.2(3) . . ? C52' Si2' C46' 111.4(2) . . ? C40' Si2' C46' 107.3(2) . . ? C41' C40' C45' 120.0 . . ? C41' C40' Si2' 117.70(14) . . ? C45' C40' Si2' 122.28(14) . . ? C42' C41' C40' 120.0 . . ? C41' C42' C43' 120.0 . . ? C44' C43' C42' 120.0 . . ? C45' C44' C43' 120.0 . . ? C44' C45' C40' 120.0 . . ? C47 C46 C51 120.0 . . ? C47 C46 Si2 114.63(11) . . ? C51 C46 Si2 125.27(11) . . ? C46 C47 C48 120.0 . . ? C49 C48 C47 120.0 . . ? C48 C49 C50 120.0 . . ? C49 C50 C51 120.0 . . ? C50 C51 C46 120.0 . . ? C47' C46' C51' 120.0 . . ? C47' C46' Si2' 116.99(12) . . ? C51' C46' Si2' 122.95(12) . . ? C46' C47' C48' 120.0 . . ? C47' C48' C49' 120.0 . . ? C50' C49' C48' 120.0 . . ? C51' C50' C49' 120.0 . . ? C50' C51' C46' 120.0 . . ? C53 C52 C57 120.0 . . ? C53 C52 Si2 121.21(14) . . ? C57 C52 Si2 118.71(14) . . ? C54 C53 C52 120.0 . . ? C55 C54 C53 120.0 . . ? C56 C55 C54 120.0 . . ? C57 C56 C55 120.0 . . ? C56 C57 C52 120.0 . . ? C53' C52' C57' 120.0 . . ? C53' C52' Si2' 116.94(14) . . ? C57' C52' Si2' 123.03(15) . . ? C54' C53' C52' 120.0 . . ? C53' C54' C55' 120.0 . . ? C56' C55' C54' 120.0 . . ? C55' C56' C57' 120.0 . . ? C56' C57' C52' 120.0 . . ? C63 C58 O3 121.4(4) . . ? C63 C58 C59 120.5(4) . . ? O3 C58 C59 117.8(5) . . ? C58 C59 C60 113.0(7) . . ? C61 C60 C59 116.1(6) . . ? C62 C61 C60 127.9(7) . . ? C62 C61 O4 123.8(11) . . ? C60 C61 O4 108.4(7) . . ? C61 C62 C63 117.5(7) . . ? C61 C62 C61' 23.4(2) . . ? C63 C62 C61' 115.4(5) . . ? C58 C63 C58' 12.0(2) . . ? C58 C63 C62 125.0(4) . . ? C58' C63 C62 123.1(5) . . ? C61 O4 C64 110.9(8) . . ? C59' C58' C63 118.5(6) . . ? C59' C58' O3 121.6(4) . . ? C63 C58' O3 118.5(5) . . ? C58' C59' C60' 121.4(5) . . ? C61' C60' C59' 121.3(9) . . ? C60' C61' O4' 114.6(9) . . ? C60' C61' C62 118.1(9) . . ? O4' C61' C62 127.0(7) . . ? C61' O4' C64' 118.8(9) . . ? C1 O1 P1 123.3(2) . . ? C11 O2 P1 116.1(2) . . ? C58 O3 C58' 11.09(19) . . ? C58 O3 P1 113.7(2) . . ? C58' O3 P1 123.5(2) . . ? O1 P1 O3 98.90(14) . . ? O1 P1 O2 100.36(14) . . ? O3 P1 O2 94.82(16) . . ? C27 Si1 C21 108.79(17) . . ? C27 Si1 C34 110.81(17) . . ? C21 Si1 C34 107.08(16) . . ? C27 Si1 C2 110.40(17) . . ? C21 Si1 C2 108.10(17) . . ? C34 Si1 C2 111.54(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 176.4(3) . . . . ? C6 C1 C2 C3 -5.7(6) . . . . ? O1 C1 C2 Si1 -8.1(5) . . . . ? C6 C1 C2 Si1 169.9(3) . . . . ? C1 C2 C3 C4 0.2(5) . . . . ? Si1 C2 C3 C4 -175.5(3) . . . . ? C2 C3 C4 C7 -177.7(4) . . . . ? C2 C3 C4 C5 4.4(6) . . . . ? C7 C4 C5 C10 1.4(6) . . . . ? C3 C4 C5 C10 179.3(3) . . . . ? C7 C4 C5 C6 178.1(4) . . . . ? C3 C4 C5 C6 -3.9(5) . . . . ? O1 C1 C6 C5 -175.9(3) . . . . ? C2 C1 C6 C5 6.0(6) . . . . ? O1 C1 C6 C12 2.6(5) . . . . ? C2 C1 C6 C12 -175.5(4) . . . . ? O1 C1 C6 C12' 9.6(6) . . . . ? C2 C1 C6 C12' -168.4(4) . . . . ? C10 C5 C6 C1 175.6(4) . . . . ? C4 C5 C6 C1 -0.9(5) . . . . ? C10 C5 C6 C12 -2.8(6) . . . . ? C4 C5 C6 C12 -179.4(4) . . . . ? C10 C5 C6 C12' -9.9(6) . . . . ? C4 C5 C6 C12' 173.6(4) . . . . ? C3 C4 C7 C8 -178.5(4) . . . . ? C5 C4 C7 C8 -0.6(7) . . . . ? C4 C7 C8 C9 -0.6(7) . . . . ? C7 C8 C9 C10 1.0(7) . . . . ? C8 C9 C10 C5 -0.2(7) . . . . ? C6 C5 C10 C9 -177.6(4) . . . . ? C4 C5 C10 C9 -1.0(6) . . . . ? C16 C11 C12 C13 15.3(12) . . . . ? O2 C11 C12 C13 -170.3(5) . . . . ? C12' C11 C12 C13 -15(9) . . . . ? C16' C11 C12 C13 10.3(9) . . . . ? C16 C11 C12 C6 -171.7(7) . . . . ? O2 C11 C12 C6 2.7(10) . . . . ? C12' C11 C12 C6 158(10) . . . . ? C16' C11 C12 C6 -176.8(6) . . . . ? C1 C6 C12 C11 -55.5(9) . . . . ? C5 C6 C12 C11 122.9(7) . . . . ? C12' C6 C12 C11 -167(6) . . . . ? C1 C6 C12 C13 116.9(7) . . . . ? C5 C6 C12 C13 -64.7(9) . . . . ? C12' C6 C12 C13 5(5) . . . . ? C11 C12 C13 C17 165.4(7) . . . . ? C6 C12 C13 C17 -7.7(12) . . . . ? C11 C12 C13 C14 -6.0(10) . . . . ? C6 C12 C13 C14 -179.1(6) . . . . ? C17 C13 C14 C15 -175.3(7) . . . . ? C12 C13 C14 C15 -3.6(11) . . . . ? C17 C13 C14 C20 4.6(11) . . . . ? C12 C13 C14 C20 176.3(7) . . . . ? C13 C14 C15 C16 7.6(12) . . . . ? C20 C14 C15 C16 -172.3(8) . . . . ? C12 C11 C16 C15 -11.6(12) . . . . ? O2 C11 C16 C15 173.7(6) . . . . ? C12' C11 C16 C15 -9.0(11) . . . . ? C16' C11 C16 C15 3.8(17) . . . . ? C12 C11 C16 Si2 170.2(7) . . . . ? O2 C11 C16 Si2 -4.5(8) . . . . ? C12' C11 C16 Si2 172.8(6) . . . . ? C16' C11 C16 Si2 -174(3) . . . . ? C14 C15 C16 C11 -1.3(11) . . . . ? C14 C15 C16 Si2 177.0(6) . . . . ? C14 C13 C17 C18 -5.6(12) . . . . ? C12 C13 C17 C18 -177.0(8) . . . . ? C13 C17 C18 C19 1.9(12) . . . . ? C17 C18 C19 C20 2.9(13) . . . . ? C18 C19 C20 C14 -3.8(13) . . . . ? C13 C14 C20 C19 0.0(12) . . . . ? C15 C14 C20 C19 179.9(8) . . . . ? C12 C11 C12' C13' 159(10) . . . . ? C16 C11 C12' C13' 7.2(12) . . . . ? O2 C11 C12' C13' -175.8(7) . . . . ? C16' C11 C12' C13' 3.1(10) . . . . ? C12 C11 C12' C6 -20(9) . . . . ? C16 C11 C12' C6 -171.2(6) . . . . ? O2 C11 C12' C6 5.8(8) . . . . ? C16' C11 C12' C6 -175.3(6) . . . . ? C1 C6 C12' C13' 120.2(7) . . . . ? C5 C6 C12' C13' -54.1(9) . . . . ? C12 C6 C12' C13' -168(6) . . . . ? C1 C6 C12' C11 -61.4(8) . . . . ? C5 C6 C12' C11 124.3(6) . . . . ? C12 C6 C12' C11 10(5) . . . . ? C11 C12' C13' C17' 177.6(8) . . . . ? C6 C12' C13' C17' -4.1(13) . . . . ? C11 C12' C13' C14' -3.9(12) . . . . ? C6 C12' C13' C14' 174.4(7) . . . . ? C17' C13' C14' C15' -179.8(8) . . . . ? C12' C13' C14' C15' 1.7(12) . . . . ? C17' C13' C14' C20' -1.0(12) . . . . ? C12' C13' C14' C20' -179.5(8) . . . . ? C13' C14' C15' C16' 1.0(12) . . . . ? C20' C14' C15' C16' -177.7(8) . . . . ? C14' C15' C16' C11 -1.7(13) . . . . ? C14' C15' C16' Si2' 171.7(7) . . . . ? C12 C11 C16' C15' -2.1(10) . . . . ? C16 C11 C16' C15' -170(3) . . . . ? O2 C11 C16' C15' 178.5(6) . . . . ? C12' C11 C16' C15' -0.3(10) . . . . ? C12 C11 C16' Si2' -175.9(6) . . . . ? C16 C11 C16' Si2' 16.5(17) . . . . ? O2 C11 C16' Si2' 4.8(8) . . . . ? C12' C11 C16' Si2' -174.1(5) . . . . ? C14' C13' C17' C18' 1.7(13) . . . . ? C12' C13' C17' C18' -179.9(9) . . . . ? C13' C17' C18' C19' -3.4(13) . . . . ? C17' C18' C19' C20' 4.7(14) . . . . ? C18' C19' C20' C14' -4.2(14) . . . . ? C13' C14' C20' C19' 2.3(13) . . . . ? C15' C14' C20' C19' -178.9(9) . . . . ? C26 C21 C22 C23 0.2(8) . . . . ? Si1 C21 C22 C23 -172.1(5) . . . . ? C21 C22 C23 C24 -2.0(10) . . . . ? C22 C23 C24 C25 2.1(10) . . . . ? C23 C24 C25 C26 -0.5(8) . . . . ? C24 C25 C26 C21 -1.3(7) . . . . ? C22 C21 C26 C25 1.4(7) . . . . ? Si1 C21 C26 C25 173.5(4) . . . . ? C32 C27 C28 C29 2.3(7) . . . . ? Si1 C27 C28 C29 176.5(4) . . . . ? C27 C28 C29 C30 -2.3(9) . . . . ? C28 C29 C30 C33 1.1(10) . . . . ? C28 C27 C32 C33 -1.2(7) . . . . ? Si1 C27 C32 C33 -175.4(4) . . . . ? C29 C30 C33 C32 0.0(10) . . . . ? C27 C32 C33 C30 0.0(9) . . . . ? C39 C34 C35 C36 0.0 . . . . ? Si1 C34 C35 C36 178.25(19) . . . . ? C34 C35 C36 C37 0.0 . . . . ? C35 C36 C37 C38 0.0 . . . . ? C36 C37 C38 C39 0.0 . . . . ? C37 C38 C39 C34 0.0 . . . . ? C35 C34 C39 C38 0.0 . . . . ? Si1 C34 C39 C38 -178.19(19) . . . . ? C11 C16 Si2 C52 64.0(8) . . . . ? C15 C16 Si2 C52 -114.0(7) . . . . ? C11 C16 Si2 C40 -177.1(7) . . . . ? C15 C16 Si2 C40 4.9(8) . . . . ? C11 C16 Si2 C46 -58.0(8) . . . . ? C15 C16 Si2 C46 123.9(7) . . . . ? C52 Si2 C40 C41 171.9(4) . . . . ? C46 Si2 C40 C41 -67.8(5) . . . . ? C16 Si2 C40 C41 55.8(6) . . . . ? C52 Si2 C40 C45 -13.0(6) . . . . ? C46 Si2 C40 C45 107.4(5) . . . . ? C16 Si2 C40 C45 -129.0(6) . . . . ? C45 C40 C41 C42 0.0 . . . . ? Si2 C40 C41 C42 175.2(6) . . . . ? C40 C41 C42 C43 0.0 . . . . ? C41 C42 C43 C44 0.0 . . . . ? C42 C43 C44 C45 0.0 . . . . ? C43 C44 C45 C40 0.0 . . . . ? C41 C40 C45 C44 0.0 . . . . ? Si2 C40 C45 C44 -175.1(6) . . . . ? C15' C16' Si2' C52' -110.1(7) . . . . ? C11 C16' Si2' C52' 63.5(6) . . . . ? C15' C16' Si2' C40' 8.3(8) . . . . ? C11 C16' Si2' C40' -178.1(5) . . . . ? C15' C16' Si2' C46' 127.9(7) . . . . ? C11 C16' Si2' C46' -58.5(6) . . . . ? C16' Si2' C40' C41' 81.7(3) . . . . ? C52' Si2' C40' C41' -165.08(14) . . . . ? C46' Si2' C40' C41' -42.8(2) . . . . ? C16' Si2' C40' C45' -99.9(3) . . . . ? C52' Si2' C40' C45' 13.3(3) . . . . ? C46' Si2' C40' C45' 135.52(13) . . . . ? C45' C40' C41' C42' 0.0 . . . . ? Si2' C40' C41' C42' 178.37(15) . . . . ? C40' C41' C42' C43' 0.0 . . . . ? C41' C42' C43' C44' 0.0 . . . . ? C42' C43' C44' C45' 0.0 . . . . ? C43' C44' C45' C40' 0.0 . . . . ? C41' C40' C45' C44' 0.0 . . . . ? Si2' C40' C45' C44' -178.29(16) . . . . ? C52 Si2 C46 C47 79.46(17) . . . . ? C40 Si2 C46 C47 -40.9(3) . . . . ? C16 Si2 C46 C47 -161.0(2) . . . . ? C52 Si2 C46 C51 -96.94(17) . . . . ? C40 Si2 C46 C51 142.7(2) . . . . ? C16 Si2 C46 C51 22.6(3) . . . . ? C51 C46 C47 C48 0.0 . . . . ? Si2 C46 C47 C48 -176.61(12) . . . . ? C46 C47 C48 C49 0.0 . . . . ? C47 C48 C49 C50 0.0 . . . . ? C48 C49 C50 C51 0.0 . . . . ? C49 C50 C51 C46 0.0 . . . . ? C47 C46 C51 C50 0.0 . . . . ? Si2 C46 C51 C50 176.22(14) . . . . ? C16' Si2' C46' C47' -178.2(3) . . . . ? C52' Si2' C46' C47' 64.0(2) . . . . ? C40' Si2' C46' C47' -58.5(2) . . . . ? C16' Si2' C46' C51' 4.8(3) . . . . ? C52' Si2' C46' C51' -113.03(16) . . . . ? C40' Si2' C46' C51' 124.52(14) . . . . ? C51' C46' C47' C48' 0.0 . . . . ? Si2' C46' C47' C48' -177.12(13) . . . . ? C46' C47' C48' C49' 0.0 . . . . ? C47' C48' C49' C50' 0.0 . . . . ? C48' C49' C50' C51' 0.0 . . . . ? C49' C50' C51' C46' 0.0 . . . . ? C47' C46' C51' C50' 0.0 . . . . ? Si2' C46' C51' C50' 176.94(14) . . . . ? C40 Si2 C52 C53 -66.4(3) . . . . ? C46 Si2 C52 C53 175.62(9) . . . . ? C16 Si2 C52 C53 51.3(3) . . . . ? C40 Si2 C52 C57 116.8(3) . . . . ? C46 Si2 C52 C57 -1.2(2) . . . . ? C16 Si2 C52 C57 -125.5(3) . . . . ? C57 C52 C53 C54 0.0 . . . . ? Si2 C52 C53 C54 -176.78(13) . . . . ? C52 C53 C54 C55 0.0 . . . . ? C53 C54 C55 C56 0.0 . . . . ? C54 C55 C56 C57 0.0 . . . . ? C55 C56 C57 C52 0.0 . . . . ? C53 C52 C57 C56 0.0 . . . . ? Si2 C52 C57 C56 176.86(13) . . . . ? C16' Si2' C52' C53' 42.0(3) . . . . ? C40' Si2' C52' C53' -73.6(2) . . . . ? C46' Si2' C52' C53' 166.50(12) . . . . ? C16' Si2' C52' C57' -136.0(3) . . . . ? C40' Si2' C52' C57' 108.4(2) . . . . ? C46' Si2' C52' C57' -11.5(3) . . . . ? C57' C52' C53' C54' 0.0 . . . . ? Si2' C52' C53' C54' -178.04(14) . . . . ? C52' C53' C54' C55' 0.0 . . . . ? C53' C54' C55' C56' 0.0 . . . . ? C54' C55' C56' C57' 0.0 . . . . ? C55' C56' C57' C52' 0.0 . . . . ? C53' C52' C57' C56' 0.0 . . . . ? Si2' C52' C57' C56' 177.92(15) . . . . ? C63 C58 C59 C60 -0.03(5) . . . . ? O3 C58 C59 C60 173.6(2) . . . . ? C58 C59 C60 C61 -0.01(5) . . . . ? C59 C60 C61 C62 -0.01(14) . . . . ? C59 C60 C61 O4 179.99(6) . . . . ? C60 C61 C62 C63 0.06(17) . . . . ? O4 C61 C62 C63 -179.94(10) . . . . ? C60 C61 C62 C61' -90.7(16) . . . . ? O4 C61 C62 C61' 89.3(16) . . . . ? O3 C58 C63 C58' -88.2(13) . . . . ? C59 C58 C63 C58' 85.3(13) . . . . ? O3 C58 C63 C62 -173.4(2) . . . . ? C59 C58 C63 C62 0.08(12) . . . . ? C61 C62 C63 C58 -0.10(16) . . . . ? C61' C62 C63 C58 26.0(3) . . . . ? C61 C62 C63 C58' -14.5(3) . . . . ? C61' C62 C63 C58' 11.6(4) . . . . ? C62 C61 O4 C64 0.01(16) . . . . ? C60 C61 O4 C64 -179.99(8) . . . . ? C58 C63 C58' C59' -121.2(14) . . . . ? C62 C63 C58' C59' -18.3(5) . . . . ? C58 C63 C58' O3 72.1(14) . . . . ? C62 C63 C58' O3 174.9(2) . . . . ? C63 C58' C59' C60' 12.2(4) . . . . ? O3 C58' C59' C60' 178.6(3) . . . . ? C58' C59' C60' C61' 0.00(7) . . . . ? C59' C60' C61' O4' -179.99(8) . . . . ? C59' C60' C61' C62 -6.3(4) . . . . ? C61 C62 C61' C60' 101.9(18) . . . . ? C63 C62 C61' C60' 0.9(5) . . . . ? C61 C62 C61' O4' -85.3(17) . . . . ? C63 C62 C61' O4' 173.6(2) . . . . ? C60' C61' O4' C64' -179.98(11) . . . . ? C62 C61' O4' C64' 7.0(4) . . . . ? C6 C1 O1 P1 71.5(4) . . . . ? C2 C1 O1 P1 -110.3(3) . . . . ? C12 C11 O2 P1 75.2(6) . . . . ? C16 C11 O2 P1 -109.1(5) . . . . ? C12' C11 O2 P1 73.3(5) . . . . ? C16' C11 O2 P1 -105.4(5) . . . . ? C63 C58 O3 C58' 85.7(14) . . . . ? C59 C58 O3 C58' -87.9(14) . . . . ? C63 C58 O3 P1 -121.3(2) . . . . ? C59 C58 O3 P1 65.1(3) . . . . ? C59' C58' O3 C58 119.6(15) . . . . ? C63 C58' O3 C58 -74.0(15) . . . . ? C59' C58' O3 P1 89.8(4) . . . . ? C63 C58' O3 P1 -103.9(3) . . . . ? C1 O1 P1 O3 53.3(3) . . . . ? C1 O1 P1 O2 -43.3(3) . . . . ? C58 O3 P1 O1 155.6(3) . . . . ? C58' O3 P1 O1 161.6(3) . . . . ? C58 O3 P1 O2 -103.1(3) . . . . ? C58' O3 P1 O2 -97.1(3) . . . . ? C11 O2 P1 O1 -50.3(3) . . . . ? C11 O2 P1 O3 -150.3(3) . . . . ? C28 C27 Si1 C21 -95.5(4) . . . . ? C32 C27 Si1 C21 78.5(4) . . . . ? C28 C27 Si1 C34 147.0(3) . . . . ? C32 C27 Si1 C34 -39.0(4) . . . . ? C28 C27 Si1 C2 23.0(4) . . . . ? C32 C27 Si1 C2 -163.1(3) . . . . ? C26 C21 Si1 C27 153.5(3) . . . . ? C22 C21 Si1 C27 -34.8(4) . . . . ? C26 C21 Si1 C34 -86.6(4) . . . . ? C22 C21 Si1 C34 85.0(4) . . . . ? C26 C21 Si1 C2 33.6(4) . . . . ? C22 C21 Si1 C2 -154.7(4) . . . . ? C35 C34 Si1 C27 153.41(19) . . . . ? C39 C34 Si1 C27 -28.4(2) . . . . ? C35 C34 Si1 C21 34.9(2) . . . . ? C39 C34 Si1 C21 -146.88(19) . . . . ? C35 C34 Si1 C2 -83.2(2) . . . . ? C39 C34 Si1 C2 95.0(2) . . . . ? C3 C2 Si1 C27 -85.5(3) . . . . ? C1 C2 Si1 C27 99.1(3) . . . . ? C3 C2 Si1 C21 33.4(4) . . . . ? C1 C2 Si1 C21 -142.0(3) . . . . ? C3 C2 Si1 C34 150.9(3) . . . . ? C1 C2 Si1 C34 -24.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.850 _diffrn_reflns_theta_full 59.04 _diffrn_measured_fraction_theta_full 0.850 _refine_diff_density_max 0.249 _refine_diff_density_min -0.301 _refine_diff_density_rms 0.057 _database_code_depnum_ccdc_archive 'CCDC 933757'