# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_3 _database_code_depnum_ccdc_archive 'CCDC 895721' #TrackingRef 'Dalton Trans Bourissou DPPO CIF.cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H41 Au Cl O P3' _chemical_formula_sum 'C30 H41 Au Cl O P3' _chemical_formula_weight 742.96 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 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' '-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 15.4329(3) _cell_length_b 15.7352(3) _cell_length_c 25.7359(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6249.7(2) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 9780 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 27.37 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2960 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.968 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_absorpt_correction_T_min 0.145 _exptl_absorpt_correction_T_max 0.680 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_unetI/netI 0.0328 _diffrn_reflns_number 103280 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 30.71 _diffrn_reflns_theta_full 30.71 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 9682 _reflns_number_gt 6405 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0339P)^2^+13.8798P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 9682 _refine_ls_number_parameters 358 _refine_ls_number_restraints 78 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0929 _refine_ls_wR_factor_gt 0.0753 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.549 _refine_diff_density_min -0.797 _refine_diff_density_rms 0.124 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 0.0565(2) 0.3036(2) 0.51423(15) 0.0304(8) Uani 1 1 d . . . C2 C 0.1081(3) 0.2534(3) 0.54624(19) 0.0490(12) Uani 1 1 d . . . H2 H 0.1543 0.2214 0.5317 0.059 Uiso 1 1 calc R . . C3 C 0.0924(4) 0.2498(4) 0.5990(2) 0.0695(18) Uani 1 1 d . . . H3 H 0.128 0.2154 0.6206 0.083 Uiso 1 1 calc R . . C4 C 0.0259(4) 0.2955(4) 0.62033(19) 0.0630(16) Uani 1 1 d . . . H4 H 0.016 0.2936 0.6567 0.076 Uiso 1 1 calc R . . C5 C -0.0263(4) 0.3440(3) 0.58928(19) 0.0499(12) Uani 1 1 d . . . H5 H -0.0731 0.3747 0.6041 0.06 Uiso 1 1 calc R . . C6 C -0.0113(3) 0.3485(3) 0.53644(17) 0.0379(9) Uani 1 1 d . . . H6 H -0.0477 0.3826 0.5152 0.045 Uiso 1 1 calc R . . C7 C -0.0168(2) 0.3390(2) 0.41346(14) 0.0261(7) Uani 1 1 d . . . C8 C -0.0324(3) 0.4271(2) 0.41438(15) 0.0313(8) Uani 1 1 d . . . H8 H 0.0098 0.4635 0.4296 0.038 Uiso 1 1 calc R . . C9 C -0.1069(3) 0.4627(3) 0.39399(18) 0.0401(10) Uani 1 1 d . . . H9 H -0.1149 0.5225 0.3944 0.048 Uiso 1 1 calc R . . C10 C -0.1686(3) 0.4109(3) 0.3733(2) 0.0494(12) Uani 1 1 d . . . H10 H -0.2206 0.4345 0.3599 0.059 Uiso 1 1 calc R . . C11 C -0.1554(3) 0.3239(3) 0.3719(2) 0.0461(11) Uani 1 1 d . . . H11 H -0.1993 0.2889 0.3573 0.055 Uiso 1 1 calc R . . C12 C -0.0803(2) 0.2855(2) 0.39095(15) 0.0292(8) Uani 1 1 d . . . C13 C 0.1565(2) 0.3974(2) 0.43783(16) 0.0304(8) Uani 1 1 d . . . C14 C 0.1743(3) 0.4482(3) 0.48076(18) 0.0368(9) Uani 1 1 d . . . H14 H 0.1517 0.433 0.5138 0.044 Uiso 1 1 calc R . . C15 C 0.2247(3) 0.5209(3) 0.4760(2) 0.0457(11) Uani 1 1 d . . . H15 H 0.2366 0.5553 0.5055 0.055 Uiso 1 1 calc R . . C16 C 0.2575(3) 0.5426(3) 0.4279(2) 0.0509(13) Uani 1 1 d . . . H16 H 0.2911 0.5928 0.4242 0.061 Uiso 1 1 calc R . . C17 C 0.2416(3) 0.4917(3) 0.3849(2) 0.0439(11) Uani 1 1 d . . . H17 H 0.2656 0.5071 0.3522 0.053 Uiso 1 1 calc R . . C18 C 0.1909(2) 0.4181(2) 0.38856(18) 0.0342(9) Uani 1 1 d . A . C19 C -0.0594(3) 0.1182(3) 0.44334(17) 0.0376(9) Uani 1 1 d . . . H19 H 0.0012 0.1281 0.4557 0.045 Uiso 1 1 calc R . . C20 C -0.1228(4) 0.1566(3) 0.4822(2) 0.0564(13) Uani 1 1 d . . . H20A H -0.1817 0.1534 0.4681 0.085 Uiso 1 1 calc R . . H20B H -0.1075 0.2162 0.4885 0.085 Uiso 1 1 calc R . . H20C H -0.1199 0.125 0.5149 0.085 Uiso 1 1 calc R . . C21 C -0.0755(4) 0.0222(3) 0.4388(2) 0.0552(13) Uani 1 1 d . . . H21A H -0.0702 -0.0041 0.4731 0.083 Uiso 1 1 calc R . . H21B H -0.0327 -0.0028 0.4152 0.083 Uiso 1 1 calc R . . H21C H -0.1339 0.0123 0.4251 0.083 Uiso 1 1 calc R . . C22 C 0.0198(3) 0.1573(2) 0.33678(15) 0.0307(8) Uani 1 1 d . . . H22 H 0.0697 0.1887 0.3524 0.037 Uiso 1 1 calc R . . C23 C 0.0459(3) 0.0642(3) 0.33112(18) 0.0414(10) Uani 1 1 d . . . H23A H -0.0042 0.031 0.3194 0.062 Uiso 1 1 calc R . . H23B H 0.0657 0.0424 0.3647 0.062 Uiso 1 1 calc R . . H23C H 0.0927 0.0593 0.3056 0.062 Uiso 1 1 calc R . . C24 C -0.0011(3) 0.1981(3) 0.28397(17) 0.0439(10) Uani 1 1 d . . . H24A H 0.0476 0.1894 0.2602 0.066 Uiso 1 1 calc R . . H24B H -0.0111 0.2591 0.2887 0.066 Uiso 1 1 calc R . . H24C H -0.0533 0.1717 0.2694 0.066 Uiso 1 1 calc R . . C28 C 0.1538(4) 0.4332(3) 0.27930(19) 0.0603(15) Uani 1 1 d . A . H28 H 0.2076 0.4686 0.2782 0.072 Uiso 1 1 calc R . . C29 C 0.0766(5) 0.4893(4) 0.2912(2) 0.079(2) Uani 1 1 d . . . H29A H 0.0701 0.5318 0.2636 0.119 Uiso 1 1 calc R . . H29B H 0.0857 0.5181 0.3245 0.119 Uiso 1 1 calc R . . H29C H 0.0242 0.4544 0.2931 0.119 Uiso 1 1 calc R . . C30 C 0.1405(5) 0.3899(4) 0.2266(2) 0.077(2) Uani 1 1 d . . . H30A H 0.0865 0.3571 0.2272 0.116 Uiso 1 1 calc R . . H30B H 0.1892 0.3518 0.2195 0.116 Uiso 1 1 calc R . . H30C H 0.1371 0.4332 0.1993 0.116 Uiso 1 1 calc R . . O1 O 0.12235(17) 0.22334(16) 0.43029(11) 0.0311(6) Uani 1 1 d . . . P1 P 0.08414(6) 0.30608(6) 0.44566(4) 0.02517(18) Uani 1 1 d . . . P2 P -0.07424(6) 0.17048(6) 0.37973(4) 0.0288(2) Uani 1 1 d . . . Cl1 Cl -0.31263(7) 0.08742(8) 0.28989(5) 0.0510(3) Uani 1 1 d . . . Au1 Au -0.194253(10) 0.126390(10) 0.337773(6) 0.03408(5) Uani 1 1 d . . . P3 P 0.16385(8) 0.35180(7) 0.33150(5) 0.0399(3) Uani 1 1 d D . . C25 C 0.2633(5) 0.2982(4) 0.3070(3) 0.0376(15) Uani 0.64 1 d PDU A 1 H25 H 0.2481 0.2737 0.2723 0.045 Uiso 0.64 1 calc PR A 1 C26 C 0.2816(5) 0.2231(6) 0.3427(4) 0.053(2) Uani 0.64 1 d PDU A 1 H26A H 0.3289 0.189 0.3282 0.08 Uiso 0.64 1 calc PR A 1 H26B H 0.2294 0.188 0.3458 0.08 Uiso 0.64 1 calc PR A 1 H26C H 0.2983 0.2441 0.3771 0.08 Uiso 0.64 1 calc PR A 1 C27 C 0.3425(7) 0.3541(8) 0.2986(4) 0.055(3) Uani 0.64 1 d PDU A 1 H27A H 0.3628 0.3759 0.3321 0.082 Uiso 0.64 1 calc PR A 1 H27B H 0.3271 0.4018 0.2759 0.082 Uiso 0.64 1 calc PR A 1 H27C H 0.3886 0.3206 0.2823 0.082 Uiso 0.64 1 calc PR A 1 C25' C 0.2778(7) 0.2983(7) 0.3368(6) 0.040(3) Uani 0.36 1 d PDU A 2 H25' H 0.2859 0.2844 0.3744 0.048 Uiso 0.36 1 calc PR A 2 C26' C 0.2741(10) 0.2140(8) 0.3086(7) 0.054(4) Uani 0.36 1 d PDU A 2 H26D H 0.2649 0.224 0.2714 0.082 Uiso 0.36 1 calc PR A 2 H26E H 0.2262 0.1799 0.3224 0.082 Uiso 0.36 1 calc PR A 2 H26F H 0.3288 0.1835 0.3137 0.082 Uiso 0.36 1 calc PR A 2 C27' C 0.3546(12) 0.3535(14) 0.3216(8) 0.056(6) Uani 0.36 1 d PDU A 2 H27D H 0.406 0.3176 0.3172 0.084 Uiso 0.36 1 calc PR A 2 H27E H 0.3654 0.3956 0.3489 0.084 Uiso 0.36 1 calc PR A 2 H27F H 0.3419 0.3826 0.2888 0.084 Uiso 0.36 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0302(19) 0.0278(18) 0.033(2) 0.0025(16) -0.0030(15) -0.0071(15) C2 0.041(2) 0.061(3) 0.045(3) 0.013(2) -0.006(2) 0.004(2) C3 0.057(3) 0.109(5) 0.043(3) 0.028(3) -0.009(3) 0.004(3) C4 0.072(4) 0.090(4) 0.026(2) 0.001(3) 0.003(2) -0.023(3) C5 0.059(3) 0.045(3) 0.046(3) -0.004(2) 0.010(2) -0.009(2) C6 0.047(2) 0.031(2) 0.036(2) -0.0023(17) 0.0029(18) -0.0006(18) C7 0.0257(17) 0.0238(17) 0.0289(18) -0.0003(14) -0.0005(14) 0.0032(14) C8 0.034(2) 0.0256(18) 0.035(2) -0.0031(16) -0.0055(16) 0.0010(15) C9 0.041(2) 0.027(2) 0.052(3) -0.0026(18) -0.012(2) 0.0081(17) C10 0.039(2) 0.038(2) 0.071(3) -0.004(2) -0.024(2) 0.009(2) C11 0.037(2) 0.033(2) 0.068(3) -0.011(2) -0.020(2) 0.0040(18) C12 0.0251(17) 0.0266(18) 0.036(2) -0.0020(15) -0.0016(15) 0.0010(15) C13 0.0223(17) 0.0238(17) 0.045(2) 0.0063(16) -0.0062(16) -0.0004(14) C14 0.031(2) 0.032(2) 0.048(2) 0.0071(18) -0.0097(17) -0.0027(16) C15 0.038(2) 0.031(2) 0.069(3) -0.002(2) -0.017(2) -0.0061(18) C16 0.033(2) 0.032(2) 0.088(4) 0.015(3) -0.010(2) -0.0101(18) C17 0.033(2) 0.030(2) 0.068(3) 0.014(2) 0.001(2) -0.0082(17) C18 0.0236(18) 0.0241(18) 0.055(3) 0.0075(17) 0.0022(17) 0.0018(15) C19 0.037(2) 0.038(2) 0.038(2) 0.0077(18) -0.0013(17) -0.0103(18) C20 0.066(3) 0.053(3) 0.051(3) 0.000(2) 0.019(3) -0.019(3) C21 0.064(3) 0.039(3) 0.062(3) 0.018(2) 0.003(3) -0.003(2) C22 0.0306(19) 0.0263(17) 0.035(2) -0.0011(16) 0.0015(16) 0.0010(15) C23 0.041(2) 0.037(2) 0.047(3) 0.0013(19) 0.0024(19) 0.0123(18) C24 0.055(3) 0.038(2) 0.038(2) 0.0037(19) 0.001(2) 0.001(2) C28 0.107(5) 0.032(2) 0.042(3) 0.003(2) 0.022(3) -0.010(3) C29 0.147(6) 0.051(3) 0.039(3) 0.007(2) -0.005(3) 0.032(4) C30 0.136(6) 0.050(3) 0.045(3) -0.002(2) 0.034(4) -0.015(4) O1 0.0306(14) 0.0231(13) 0.0397(15) 0.0034(11) -0.0004(11) 0.0054(11) P1 0.0231(4) 0.0212(4) 0.0312(5) 0.0024(4) -0.0017(4) -0.0002(3) P2 0.0267(5) 0.0236(4) 0.0361(5) -0.0010(4) -0.0014(4) -0.0009(4) Cl1 0.0402(6) 0.0543(7) 0.0585(7) -0.0088(6) -0.0156(5) -0.0040(5) Au1 0.03040(8) 0.02915(8) 0.04271(9) -0.00303(7) -0.00493(6) -0.00231(6) P3 0.0438(6) 0.0230(5) 0.0529(7) 0.0051(5) 0.0186(5) 0.0003(4) C25 0.044(4) 0.030(3) 0.038(4) -0.004(3) 0.007(3) 0.002(3) C26 0.047(4) 0.051(5) 0.061(6) 0.014(4) 0.011(4) 0.022(4) C27 0.055(6) 0.045(5) 0.064(7) -0.021(5) 0.029(5) -0.010(4) C25' 0.039(6) 0.032(6) 0.050(8) -0.006(6) 0.015(6) -0.001(5) C26' 0.062(9) 0.032(6) 0.069(10) -0.007(7) 0.018(9) -0.005(6) C27' 0.039(8) 0.050(9) 0.080(15) -0.025(11) 0.019(9) -0.013(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C6 1.386(6) . ? C1 C2 1.392(6) . ? C1 P1 1.816(4) . ? C2 C3 1.381(7) . ? C2 H2 0.95 . ? C3 C4 1.368(8) . ? C3 H3 0.95 . ? C4 C5 1.368(8) . ? C4 H4 0.95 . ? C5 C6 1.381(6) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 C8 1.407(5) . ? C7 C12 1.416(5) . ? C7 P1 1.839(4) . ? C8 C9 1.382(5) . ? C8 H8 0.95 . ? C9 C10 1.361(6) . ? C9 H9 0.95 . ? C10 C11 1.385(6) . ? C10 H10 0.95 . ? C11 C12 1.397(6) . ? C11 H11 0.95 . ? C12 P2 1.835(4) . ? C13 C14 1.391(6) . ? C13 C18 1.413(6) . ? C13 P1 1.831(4) . ? C14 C15 1.389(6) . ? C14 H14 0.95 . ? C15 C16 1.379(7) . ? C15 H15 0.95 . ? C16 C17 1.388(7) . ? C16 H16 0.95 . ? C17 C18 1.401(5) . ? C17 H17 0.95 . ? C18 P3 1.849(5) . ? C19 C20 1.524(7) . ? C19 C21 1.535(6) . ? C19 P2 1.847(4) . ? C19 H19 1 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 C23 1.526(6) . ? C22 C24 1.537(6) . ? C22 P2 1.836(4) . ? C22 H22 1 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C28 C29 1.514(8) . ? C28 C30 1.532(8) . ? C28 P3 1.863(5) . ? C28 H28 1 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C30 H30A 0.98 . ? C30 H30B 0.98 . ? C30 H30C 0.98 . ? O1 P1 1.483(3) . ? P2 Au1 2.2534(10) . ? Cl1 Au1 2.2875(11) . ? P3 C25 1.861(7) . ? P3 C25' 1.954(11) . ? C25 C26 1.522(9) . ? C25 C27 1.523(10) . ? C25 H25 1 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C25' C26' 1.514(13) . ? C25' C27' 1.520(14) . ? C25' H25' 1 . ? C26' H26D 0.98 . ? C26' H26E 0.98 . ? C26' H26F 0.98 . ? C27' H27D 0.98 . ? C27' H27E 0.98 . ? C27' H27F 0.98 . ? 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 C6 C1 C2 118.5(4) . . ? C6 C1 P1 124.6(3) . . ? C2 C1 P1 116.9(3) . . ? C3 C2 C1 120.4(5) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C4 C3 C2 120.2(5) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C5 C4 C3 120.1(5) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 120.3(5) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 120.4(4) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C8 C7 C12 118.3(3) . . ? C8 C7 P1 114.5(3) . . ? C12 C7 P1 127.1(3) . . ? C9 C8 C7 122.3(4) . . ? C9 C8 H8 118.8 . . ? C7 C8 H8 118.8 . . ? C10 C9 C8 119.2(4) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C9 C10 C11 120.0(4) . . ? C9 C10 H10 120 . . ? C11 C10 H10 120 . . ? C10 C11 C12 122.6(4) . . ? C10 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? C11 C12 C7 117.5(3) . . ? C11 C12 P2 114.4(3) . . ? C7 C12 P2 128.0(3) . . ? C14 C13 C18 120.4(4) . . ? C14 C13 P1 119.0(3) . . ? C18 C13 P1 120.6(3) . . ? C15 C14 C13 120.9(4) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C16 C15 C14 119.3(5) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C17 120.5(4) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C18 121.5(5) . . ? C16 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? C17 C18 C13 117.4(4) . . ? C17 C18 P3 122.6(4) . . ? C13 C18 P3 119.9(3) . . ? C20 C19 C21 109.7(4) . . ? C20 C19 P2 109.0(3) . . ? C21 C19 P2 110.5(3) . . ? C20 C19 H19 109.2 . . ? C21 C19 H19 109.2 . . ? P2 C19 H19 109.2 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C24 111.8(3) . . ? C23 C22 P2 112.0(3) . . ? C24 C22 P2 108.6(3) . . ? C23 C22 H22 108.1 . . ? C24 C22 H22 108.1 . . ? P2 C22 H22 108.1 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C29 C28 C30 109.4(6) . . ? C29 C28 P3 108.7(4) . . ? C30 C28 P3 110.2(3) . . ? C29 C28 H28 109.5 . . ? C30 C28 H28 109.5 . . ? P3 C28 H28 109.5 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O1 P1 C1 109.51(17) . . ? O1 P1 C13 114.64(17) . . ? C1 P1 C13 105.49(18) . . ? O1 P1 C7 117.65(16) . . ? C1 P1 C7 104.18(17) . . ? C13 P1 C7 104.23(17) . . ? C12 P2 C22 104.26(18) . . ? C12 P2 C19 107.83(19) . . ? C22 P2 C19 112.66(19) . . ? C12 P2 Au1 109.72(12) . . ? C22 P2 Au1 109.04(13) . . ? C19 P2 Au1 112.94(13) . . ? P2 Au1 Cl1 175.68(4) . . ? C18 P3 C25 109.8(3) . . ? C18 P3 C28 101.8(2) . . ? C25 P3 C28 97.8(3) . . ? C18 P3 C25' 89.1(4) . . ? C28 P3 C25' 114.9(5) . . ? C26 C25 C27 112.7(8) . . ? C26 C25 P3 107.5(5) . . ? C27 C25 P3 116.6(6) . . ? C26 C25 H25 106.5 . . ? C27 C25 H25 106.5 . . ? P3 C25 H25 106.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26' C25' C27' 113.9(12) . . ? C26' C25' P3 108.1(10) . . ? C27' C25' P3 116.0(12) . . ? C26' C25' H25' 106 . . ? C27' C25' H25' 106 . . ? P3 C25' H25' 106 . . ? C25' C26' H26D 109.5 . . ? C25' C26' H26E 109.5 . . ? H26D C26' H26E 109.5 . . ? C25' C26' H26F 109.5 . . ? H26D C26' H26F 109.5 . . ? H26E C26' H26F 109.5 . . ? C25' C27' H27D 109.5 . . ? C25' C27' H27E 109.5 . . ? H27D C27' H27E 109.5 . . ? C25' C27' H27F 109.5 . . ? H27D C27' H27F 109.5 . . ? H27E C27' H27F 109.5 . . ? data_5 _database_code_depnum_ccdc_archive 'CCDC 895722' #TrackingRef 'Dalton Trans Bourissou DPPO CIF.cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H41 Ag Cl O P3' _chemical_formula_sum 'C30 H41 Ag Cl O P3' _chemical_formula_weight 653.86 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.832(4) _cell_length_b 18.830(8) _cell_length_c 18.315(8) _cell_angle_alpha 90 _cell_angle_beta 97.935(10) _cell_angle_gamma 90 _cell_volume 3017(2) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5242 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 26.33 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description parallelepiped _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.44 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.937 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_absorpt_correction_T_min 0.9350 _exptl_absorpt_correction_T_max 0.9635 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'Bruker Kappa APEX II Quazar' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_unetI/netI 0.051 _diffrn_reflns_number 20202 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.97 _diffrn_measured_fraction_theta_max 0.97 _reflns_number_total 5976 _reflns_number_gt 4667 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0340P)^2^+0.3289P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5976 _refine_ls_number_parameters 333 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0504 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0703 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.357 _refine_diff_density_min -0.355 _refine_diff_density_rms 0.079 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.7955(3) 0.38685(14) 1.05686(14) 0.0185(6) Uani 1 1 d . . . C2 C 0.9148(3) 0.43571(16) 1.05966(16) 0.0268(7) Uani 1 1 d . . . H2 H 0.9722 0.4388 1.0196 0.032 Uiso 1 1 calc R . . C3 C 0.9509(3) 0.47986(16) 1.12034(16) 0.0296(7) Uani 1 1 d . . . H3 H 1.0309 0.5137 1.1212 0.036 Uiso 1 1 calc R . . C4 C 0.8703(4) 0.47435(17) 1.17905(17) 0.0321(7) Uani 1 1 d . . . H4 H 0.8933 0.5054 1.22 0.039 Uiso 1 1 calc R . . C5 C 0.7556(4) 0.42405(17) 1.17928(16) 0.0311(7) Uani 1 1 d . . . H5 H 0.7029 0.4193 1.2208 0.037 Uiso 1 1 calc R . . C6 C 0.7187(3) 0.38046(16) 1.11777(16) 0.0266(7) Uani 1 1 d . . . H6 H 0.64 0.346 1.1176 0.032 Uiso 1 1 calc R . . C7 C 0.5811(3) 0.28573(15) 0.98134(14) 0.0192(6) Uani 1 1 d . . . C8 C 0.4603(3) 0.33286(16) 0.98847(16) 0.0254(7) Uani 1 1 d . . . H8 H 0.4798 0.3825 0.9901 0.03 Uiso 1 1 calc R . . C9 C 0.3147(3) 0.30885(17) 0.99310(16) 0.0291(7) Uani 1 1 d . . . H9 H 0.2351 0.3416 0.9985 0.035 Uiso 1 1 calc R . . C10 C 0.2855(3) 0.23716(18) 0.98992(16) 0.0316(8) Uani 1 1 d . . . H10 H 0.1852 0.2201 0.9928 0.038 Uiso 1 1 calc R . . C11 C 0.4021(3) 0.18981(16) 0.98247(17) 0.0276(7) Uani 1 1 d . . . H11 H 0.3797 0.1405 0.9802 0.033 Uiso 1 1 calc R . . C12 C 0.5525(3) 0.21206(15) 0.97816(15) 0.0204(6) Uani 1 1 d . . . C13 C 0.5989(3) 0.06397(15) 0.93726(16) 0.0255(7) Uani 1 1 d . . . H13 H 0.5251 0.0529 0.9725 0.031 Uiso 1 1 calc R . . C14 C 0.7134(3) 0.00297(16) 0.93670(18) 0.0318(7) Uani 1 1 d . . . H14A H 0.6603 -0.0394 0.9151 0.048 Uiso 1 1 calc R . . H14B H 0.7597 -0.0074 0.9873 0.048 Uiso 1 1 calc R . . H14C H 0.7934 0.0167 0.9073 0.048 Uiso 1 1 calc R . . C15 C 0.5118(4) 0.07452(18) 0.85958(16) 0.0368(8) Uani 1 1 d . . . H15A H 0.5843 0.0859 0.8253 0.055 Uiso 1 1 calc R . . H15B H 0.4386 0.1136 0.8602 0.055 Uiso 1 1 calc R . . H15C H 0.4568 0.0308 0.8436 0.055 Uiso 1 1 calc R . . C16 C 0.7976(3) 0.13493(15) 1.06166(15) 0.0239(7) Uani 1 1 d . . . H16 H 0.8129 0.1837 1.0831 0.029 Uiso 1 1 calc R . . C17 C 0.7018(4) 0.09455(18) 1.11113(16) 0.0336(8) Uani 1 1 d . . . H17A H 0.695 0.0445 1.0964 0.05 Uiso 1 1 calc R . . H17B H 0.5989 0.1151 1.1063 0.05 Uiso 1 1 calc R . . H17C H 0.7499 0.0981 1.1625 0.05 Uiso 1 1 calc R . . C18 C 0.9566(3) 0.10290(17) 1.06373(17) 0.0330(8) Uani 1 1 d . . . H18A H 1.0112 0.1058 1.114 0.05 Uiso 1 1 calc R . . H18B H 1.0134 0.1292 1.0302 0.05 Uiso 1 1 calc R . . H18C H 0.9476 0.053 1.0484 0.05 Uiso 1 1 calc R . . C19 C 0.7262(3) 0.38984(14) 0.89821(15) 0.0189(6) Uani 1 1 d . . . C20 C 0.6713(3) 0.45777(15) 0.91206(16) 0.0249(7) Uani 1 1 d . . . H20 H 0.6603 0.4703 0.9613 0.03 Uiso 1 1 calc R . . C21 C 0.6326(3) 0.50717(16) 0.85680(17) 0.0314(7) Uani 1 1 d . . . H21 H 0.5942 0.5524 0.868 0.038 Uiso 1 1 calc R . . C22 C 0.6505(3) 0.48991(17) 0.78460(17) 0.0326(8) Uani 1 1 d . . . H22 H 0.6245 0.5231 0.7458 0.039 Uiso 1 1 calc R . . C23 C 0.7066(3) 0.42366(16) 0.77036(16) 0.0257(7) Uani 1 1 d . . . H23 H 0.7207 0.4126 0.7211 0.031 Uiso 1 1 calc R . . C24 C 0.7440(3) 0.37184(15) 0.82477(15) 0.0198(6) Uani 1 1 d . . . C25 C 0.6535(3) 0.26461(17) 0.71534(16) 0.0293(7) Uani 1 1 d . . . H25 H 0.6611 0.2989 0.6743 0.035 Uiso 1 1 calc R . . C26 C 0.4975(3) 0.2725(2) 0.7409(2) 0.0467(10) Uani 1 1 d . . . H26A H 0.4182 0.2553 0.7022 0.07 Uiso 1 1 calc R . . H26B H 0.479 0.3226 0.7509 0.07 Uiso 1 1 calc R . . H26C H 0.4949 0.2447 0.7859 0.07 Uiso 1 1 calc R . . C27 C 0.6705(4) 0.18889(18) 0.68677(19) 0.0423(9) Uani 1 1 d . . . H27A H 0.6644 0.1549 0.7268 0.064 Uiso 1 1 calc R . . H27B H 0.7696 0.1841 0.6689 0.064 Uiso 1 1 calc R . . H27C H 0.5883 0.1792 0.6463 0.064 Uiso 1 1 calc R . . C28 C 0.9789(3) 0.31328(15) 0.75286(16) 0.0253(7) Uani 1 1 d . . . H28 H 0.9551 0.3582 0.7245 0.03 Uiso 1 1 calc R . . C29 C 1.1052(3) 0.32751(17) 0.81571(18) 0.0343(8) Uani 1 1 d . . . H29A H 1.1356 0.2828 0.8411 0.051 Uiso 1 1 calc R . . H29B H 1.0686 0.3608 0.8505 0.051 Uiso 1 1 calc R . . H29C H 1.1934 0.3481 0.7963 0.051 Uiso 1 1 calc R . . C30 C 1.0310(4) 0.25690(18) 0.70116(17) 0.0363(8) Uani 1 1 d . . . H30A H 1.1315 0.2699 0.6884 0.054 Uiso 1 1 calc R . . H30B H 0.957 0.2542 0.6561 0.054 Uiso 1 1 calc R . . H30C H 1.0376 0.2106 0.7259 0.054 Uiso 1 1 calc R . . O1 O 0.90072(19) 0.28312(10) 0.97621(10) 0.0215(4) Uani 1 1 d . . . P1 P 0.76517(8) 0.32921(4) 0.97712(4) 0.01716(16) Uani 1 1 d . . . P2 P 0.70232(8) 0.14697(4) 0.96535(4) 0.01942(17) Uani 1 1 d . . . P3 P 0.80683(8) 0.28468(4) 0.79285(4) 0.01944(17) Uani 1 1 d . . . Cl1 Cl 1.08033(8) 0.10261(4) 0.85760(4) 0.03084(19) Uani 1 1 d . . . Ag1 Ag 0.86521(2) 0.183013(11) 0.874396(12) 0.02178(8) 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 0.0194(14) 0.0179(15) 0.0176(14) 0.0002(12) 0.0003(12) 0.0020(11) C2 0.0292(16) 0.0283(17) 0.0244(16) 0.0011(14) 0.0089(14) -0.0050(13) C3 0.0299(17) 0.0285(18) 0.0291(17) -0.0025(14) -0.0009(15) -0.0096(14) C4 0.0417(19) 0.0294(18) 0.0232(17) -0.0058(14) -0.0024(15) 0.0000(15) C5 0.0398(18) 0.038(2) 0.0164(15) -0.0011(14) 0.0074(15) 0.0003(15) C6 0.0244(16) 0.0319(18) 0.0250(16) 0.0013(14) 0.0087(14) -0.0033(13) C7 0.0173(14) 0.0247(16) 0.0156(14) 0.0006(12) 0.0026(12) -0.0007(12) C8 0.0253(16) 0.0236(17) 0.0276(16) -0.0007(13) 0.0044(14) -0.0015(12) C9 0.0192(15) 0.040(2) 0.0284(17) -0.0004(15) 0.0035(14) 0.0069(13) C10 0.0178(15) 0.044(2) 0.0340(19) -0.0006(16) 0.0059(14) -0.0073(14) C11 0.0226(15) 0.0269(17) 0.0338(18) 0.0005(14) 0.0059(14) -0.0065(13) C12 0.0198(14) 0.0252(16) 0.0160(14) 0.0012(12) 0.0016(12) -0.0003(12) C13 0.0285(16) 0.0239(16) 0.0253(16) 0.0004(13) 0.0076(14) -0.0088(12) C14 0.0352(17) 0.0204(17) 0.0404(19) -0.0045(15) 0.0078(16) -0.0046(13) C15 0.043(2) 0.039(2) 0.0281(18) -0.0012(15) 0.0026(16) -0.0150(16) C16 0.0288(16) 0.0205(16) 0.0215(15) 0.0003(13) 0.0002(14) -0.0021(12) C17 0.0379(18) 0.040(2) 0.0231(16) 0.0026(15) 0.0069(15) -0.0035(15) C18 0.0282(17) 0.038(2) 0.0297(17) 0.0046(15) -0.0067(15) -0.0020(14) C19 0.0166(14) 0.0194(15) 0.0211(15) 0.0045(12) 0.0038(12) 0.0003(11) C20 0.0262(16) 0.0249(17) 0.0243(16) 0.0015(13) 0.0058(14) 0.0061(13) C21 0.0342(17) 0.0210(17) 0.0392(19) 0.0031(15) 0.0057(16) 0.0108(13) C22 0.0383(18) 0.0269(18) 0.0314(18) 0.0095(15) 0.0002(16) 0.0092(14) C23 0.0281(16) 0.0308(18) 0.0175(15) 0.0033(13) 0.0011(13) 0.0018(13) C24 0.0168(14) 0.0210(15) 0.0213(15) 0.0011(12) 0.0019(13) 0.0019(11) C25 0.0316(17) 0.0296(18) 0.0246(17) 0.0027(14) -0.0039(14) -0.0037(13) C26 0.0253(18) 0.055(2) 0.057(2) -0.001(2) -0.0063(18) -0.0053(16) C27 0.051(2) 0.041(2) 0.0331(19) -0.0115(16) -0.0003(17) -0.0144(17) C28 0.0283(16) 0.0222(16) 0.0274(16) 0.0063(13) 0.0104(14) -0.0006(13) C29 0.0232(16) 0.039(2) 0.041(2) -0.0030(16) 0.0063(16) -0.0060(14) C30 0.0399(19) 0.039(2) 0.0344(19) -0.0036(16) 0.0203(16) 0.0017(15) O1 0.0184(10) 0.0217(11) 0.0238(11) 0.0005(9) 0.0003(9) 0.0024(8) P1 0.0167(4) 0.0174(4) 0.0174(4) 0.0004(3) 0.0026(3) -0.0006(3) P2 0.0209(4) 0.0168(4) 0.0209(4) 0.0012(3) 0.0042(3) -0.0022(3) P3 0.0208(4) 0.0208(4) 0.0171(4) 0.0001(3) 0.0038(3) -0.0007(3) Cl1 0.0245(4) 0.0334(4) 0.0352(4) -0.0072(4) 0.0061(3) 0.0058(3) Ag1 0.02246(13) 0.02141(13) 0.02208(13) 0.00081(10) 0.00523(10) -0.00083(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C6 1.388(4) . ? C1 C2 1.395(4) . ? C1 P1 1.810(3) . ? C2 C3 1.389(4) . ? C2 H2 0.95 . ? C3 C4 1.373(4) . ? C3 H3 0.95 . ? C4 C5 1.387(4) . ? C4 H4 0.95 . ? C5 C6 1.396(4) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 C8 1.408(4) . ? C7 C12 1.410(4) . ? C7 P1 1.831(3) . ? C8 C9 1.377(4) . ? C8 H8 0.95 . ? C9 C10 1.374(4) . ? C9 H9 0.95 . ? C10 C11 1.383(4) . ? C10 H10 0.95 . ? C11 C12 1.406(4) . ? C11 H11 0.95 . ? C12 P2 1.842(3) . ? C13 C14 1.531(4) . ? C13 C15 1.534(4) . ? C13 P2 1.847(3) . ? C13 H13 1 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 C18 1.524(4) . ? C16 C17 1.526(4) . ? C16 P2 1.861(3) . ? C16 H16 1 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 C20 1.403(4) . ? C19 C24 1.417(4) . ? C19 P1 1.837(3) . ? C20 C21 1.382(4) . ? C20 H20 0.95 . ? C21 C22 1.392(4) . ? C21 H21 0.95 . ? C22 C23 1.380(4) . ? C22 H22 0.95 . ? C23 C24 1.401(4) . ? C23 H23 0.95 . ? C24 P3 1.853(3) . ? C25 C26 1.522(4) . ? C25 C27 1.533(4) . ? C25 P3 1.860(3) . ? C25 H25 1 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C28 C29 1.512(4) . ? C28 C30 1.535(4) . ? C28 P3 1.856(3) . ? C28 H28 1 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C30 H30A 0.98 . ? C30 H30B 0.98 . ? C30 H30C 0.98 . ? O1 P1 1.4806(19) . ? P2 Ag1 2.4428(10) . ? P3 Ag1 2.4389(11) . ? Cl1 Ag1 2.4816(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 C6 C1 C2 118.6(3) . . ? C6 C1 P1 124.2(2) . . ? C2 C1 P1 116.9(2) . . ? C3 C2 C1 120.9(3) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C4 C3 C2 119.7(3) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 120.8(3) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C4 C5 C6 119.2(3) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C1 C6 C5 120.8(3) . . ? C1 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C8 C7 C12 119.4(2) . . ? C8 C7 P1 114.2(2) . . ? C12 C7 P1 126.4(2) . . ? C9 C8 C7 121.7(3) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C10 C9 C8 119.4(3) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 120.0(3) . . ? C9 C10 H10 120 . . ? C11 C10 H10 120 . . ? C10 C11 C12 122.4(3) . . ? C10 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? C11 C12 C7 117.1(3) . . ? C11 C12 P2 120.7(2) . . ? C7 C12 P2 122.2(2) . . ? C14 C13 C15 109.8(3) . . ? C14 C13 P2 109.6(2) . . ? C15 C13 P2 108.3(2) . . ? C14 C13 H13 109.7 . . ? C15 C13 H13 109.7 . . ? P2 C13 H13 109.7 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C18 C16 C17 111.9(2) . . ? C18 C16 P2 111.5(2) . . ? C17 C16 P2 114.1(2) . . ? C18 C16 H16 106.2 . . ? C17 C16 H16 106.2 . . ? P2 C16 H16 106.2 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 118.4(3) . . ? C20 C19 P1 117.1(2) . . ? C24 C19 P1 124.4(2) . . ? C21 C20 C19 122.5(3) . . ? C21 C20 H20 118.7 . . ? C19 C20 H20 118.7 . . ? C20 C21 C22 119.3(3) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C23 C22 C21 118.8(3) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C22 C23 C24 123.4(3) . . ? C22 C23 H23 118.3 . . ? C24 C23 H23 118.3 . . ? C23 C24 C19 117.6(3) . . ? C23 C24 P3 116.3(2) . . ? C19 C24 P3 126.1(2) . . ? C26 C25 C27 109.3(3) . . ? C26 C25 P3 109.9(2) . . ? C27 C25 P3 110.7(2) . . ? C26 C25 H25 108.9 . . ? C27 C25 H25 108.9 . . ? P3 C25 H25 108.9 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C30 109.9(3) . . ? C29 C28 P3 108.0(2) . . ? C30 C28 P3 112.0(2) . . ? C29 C28 H28 109 . . ? C30 C28 H28 109 . . ? P3 C28 H28 109 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O1 P1 C1 109.33(12) . . ? O1 P1 C7 117.53(13) . . ? C1 P1 C7 105.50(12) . . ? O1 P1 C19 114.81(12) . . ? C1 P1 C19 104.66(13) . . ? C7 P1 C19 103.88(12) . . ? C12 P2 C13 105.19(14) . . ? C12 P2 C16 101.50(13) . . ? C13 P2 C16 107.61(13) . . ? C12 P2 Ag1 113.77(9) . . ? C13 P2 Ag1 111.12(10) . . ? C16 P2 Ag1 116.64(10) . . ? C24 P3 C28 99.49(13) . . ? C24 P3 C25 101.68(13) . . ? C28 P3 C25 107.90(14) . . ? C24 P3 Ag1 123.32(9) . . ? C28 P3 Ag1 110.73(10) . . ? C25 P3 Ag1 112.21(10) . . ? P3 Ag1 P2 122.75(3) . . ? P3 Ag1 Cl1 120.25(3) . . ? P2 Ag1 Cl1 116.62(3) . . ? data_6 _database_code_depnum_ccdc_archive 'CCDC 895723' #TrackingRef 'Dalton Trans Bourissou DPPO CIF.cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C37 H49 Cl O P3 Rh' _chemical_formula_sum 'C37 H49 Cl O P3 Rh' _chemical_formula_weight 741.03 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4107(2) _cell_length_b 10.5382(2) _cell_length_c 17.9760(3) _cell_angle_alpha 75.4240(10) _cell_angle_beta 74.6830(10) _cell_angle_gamma 71.3380(10) _cell_volume 1771.69(6) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 9858 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 30.51 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.721 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_absorpt_correction_T_min 0.850 _exptl_absorpt_correction_T_max 0.952 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_unetI/netI 0.0212 _diffrn_reflns_number 40865 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 30.51 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 10728 _reflns_number_gt 9708 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0374P)^2^+0.7523P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 10728 _refine_ls_number_parameters 412 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0296 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0707 _refine_ls_wR_factor_gt 0.068 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.753 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.061 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.72354(19) 0.33467(16) 0.06193(9) 0.0337(3) Uani 1 1 d . . . H1 H 0.8013 0.3703 0.0489 0.04 Uiso 1 1 calc R . . C2 C 0.59767(18) 0.38313(17) 0.10869(10) 0.0361(4) Uani 1 1 d . . . H2 H 0.5716 0.459 0.1342 0.043 Uiso 1 1 calc R . . C3 C 0.50715(18) 0.29068(19) 0.11183(11) 0.0389(4) Uani 1 1 d . . . H3 H 0.4049 0.3262 0.1296 0.047 Uiso 1 1 calc R . . C4 C 0.58090(16) 0.15717(17) 0.16012(9) 0.0317(3) Uani 1 1 d . . . H4 H 0.5461 0.1158 0.2118 0.038 Uiso 1 1 calc R . . C5 C 0.70967(17) 0.10890(16) 0.11262(9) 0.0295(3) Uani 1 1 d . . . H5 H 0.7802 0.0287 0.1257 0.035 Uiso 1 1 calc R . . C6 C 0.71365(19) 0.21202(17) 0.03504(9) 0.0359(3) Uani 1 1 d . . . H6 H 0.7836 0.1813 -0.0116 0.043 Uiso 1 1 calc R . . C7 C 0.5595(2) 0.2566(2) 0.02883(11) 0.0447(4) Uani 1 1 d . . . H7A H 0.5371 0.3371 -0.0128 0.054 Uiso 1 1 calc R . . H7B H 0.5276 0.1817 0.0225 0.054 Uiso 1 1 calc R . . C8 C 0.78270(17) -0.10127(18) 0.32586(10) 0.0341(3) Uani 1 1 d . . . H8 H 0.8807 -0.1455 0.3028 0.041 Uiso 1 1 calc R . . C9 C 0.7658(3) -0.1599(3) 0.41370(12) 0.0562(6) Uani 1 1 d . . . H9A H 0.6682 -0.1312 0.439 0.084 Uiso 1 1 calc R . . H9B H 0.8212 -0.1263 0.4368 0.084 Uiso 1 1 calc R . . H9C H 0.7973 -0.2595 0.4216 0.084 Uiso 1 1 calc R . . C10 C 0.6947(2) -0.1475(2) 0.28756(13) 0.0502(5) Uani 1 1 d . . . H10A H 0.7156 -0.2471 0.2996 0.075 Uiso 1 1 calc R . . H10B H 0.7156 -0.1171 0.2306 0.075 Uiso 1 1 calc R . . H10C H 0.5964 -0.1079 0.3079 0.075 Uiso 1 1 calc R . . C11 C 0.62723(16) 0.1565(2) 0.38158(10) 0.0412(4) Uani 1 1 d . . . H11 H 0.651 0.1046 0.4332 0.049 Uiso 1 1 calc R . . C12 C 0.6064(2) 0.3072(2) 0.37933(12) 0.0543(6) Uani 1 1 d . . . H12A H 0.5746 0.3608 0.3313 0.081 Uiso 1 1 calc R . . H12B H 0.6942 0.3221 0.3801 0.081 Uiso 1 1 calc R . . H12C H 0.5371 0.3356 0.4251 0.081 Uiso 1 1 calc R . . C13 C 0.49048(19) 0.1358(4) 0.37635(13) 0.0688(8) Uani 1 1 d . . . H13A H 0.4158 0.1762 0.4168 0.103 Uiso 1 1 calc R . . H13B H 0.4993 0.0381 0.3844 0.103 Uiso 1 1 calc R . . H13C H 0.4692 0.1799 0.3244 0.103 Uiso 1 1 calc R . . C14 C 0.92816(13) 0.08577(14) 0.32749(8) 0.0210(2) Uani 1 1 d . . . C15 C 0.92022(15) 0.12173(17) 0.39851(9) 0.0283(3) Uani 1 1 d . . . H15 H 0.8336 0.1377 0.4341 0.034 Uiso 1 1 calc R . . C16 C 1.03413(16) 0.13498(19) 0.41913(10) 0.0343(3) Uani 1 1 d . . . H16 H 1.0251 0.1594 0.468 0.041 Uiso 1 1 calc R . . C17 C 1.16007(16) 0.1124(2) 0.36823(11) 0.0376(4) Uani 1 1 d . . . H17 H 1.2379 0.1249 0.3807 0.045 Uiso 1 1 calc R . . C18 C 1.17282(14) 0.07123(17) 0.29831(9) 0.0294(3) Uani 1 1 d . . . H18 H 1.2608 0.0531 0.2641 0.035 Uiso 1 1 calc R . . C19 C 1.05965(13) 0.05588(13) 0.27719(8) 0.0203(2) Uani 1 1 d . . . C20 C 1.10476(14) 0.13522(14) 0.10537(8) 0.0225(2) Uani 1 1 d . . . C21 C 1.14192(18) 0.24929(16) 0.10770(10) 0.0344(3) Uani 1 1 d . . . H21 H 1.1604 0.2588 0.1547 0.041 Uiso 1 1 calc R . . C22 C 1.1520(2) 0.34941(18) 0.04111(12) 0.0433(4) Uani 1 1 d . . . H22 H 1.1793 0.4264 0.0426 0.052 Uiso 1 1 calc R . . C23 C 1.12288(18) 0.33851(18) -0.02735(10) 0.0407(4) Uani 1 1 d . . . H23 H 1.1292 0.4081 -0.0724 0.049 Uiso 1 1 calc R . . C24 C 1.08453(18) 0.22577(19) -0.03000(10) 0.0384(4) Uani 1 1 d . . . H24 H 1.0646 0.2176 -0.0769 0.046 Uiso 1 1 calc R . . C25 C 1.07524(16) 0.12437(16) 0.03630(9) 0.0303(3) Uani 1 1 d . . . H25 H 1.0486 0.0472 0.0345 0.036 Uiso 1 1 calc R . . C26 C 1.27668(13) -0.11296(14) 0.17924(8) 0.0214(2) Uani 1 1 d . . . C27 C 1.38261(15) -0.06650(15) 0.12399(9) 0.0264(3) Uani 1 1 d . . . H27 H 1.3604 0.0193 0.0903 0.032 Uiso 1 1 calc R . . C28 C 1.51986(15) -0.14424(17) 0.11783(9) 0.0295(3) Uani 1 1 d . . . H28 H 1.5909 -0.1109 0.0808 0.035 Uiso 1 1 calc R . . C29 C 1.55229(15) -0.26986(17) 0.16573(9) 0.0308(3) Uani 1 1 d . . . H29 H 1.6456 -0.3238 0.1613 0.037 Uiso 1 1 calc R . . C30 C 1.44813(16) -0.31730(16) 0.22039(9) 0.0304(3) Uani 1 1 d . . . H30 H 1.4716 -0.4044 0.2527 0.036 Uiso 1 1 calc R . . C31 C 1.30936(14) -0.24036(14) 0.22922(8) 0.0239(2) Uani 1 1 d . . . C32 C 1.2698(2) -0.3833(2) 0.38708(10) 0.0415(4) Uani 1 1 d . . . H32 H 1.3559 -0.4526 0.3679 0.05 Uiso 1 1 calc R . . C33 C 1.3094(3) -0.2754(3) 0.41187(13) 0.0614(6) Uani 1 1 d . . . H33A H 1.2258 -0.2041 0.4275 0.092 Uiso 1 1 calc R . . H33B H 1.3716 -0.2353 0.3678 0.092 Uiso 1 1 calc R . . H33C H 1.3564 -0.3174 0.4562 0.092 Uiso 1 1 calc R . . C34 C 1.1809(3) -0.4539(3) 0.45726(13) 0.0679(7) Uani 1 1 d . . . H34A H 1.227 -0.4841 0.5022 0.102 Uiso 1 1 calc R . . H34B H 1.1687 -0.5329 0.4434 0.102 Uiso 1 1 calc R . . H34C H 1.0903 -0.3899 0.471 0.102 Uiso 1 1 calc R . . P3 P 1.17302(4) -0.30121(4) 0.30592(2) 0.02700(8) Uani 1 1 d D B . C35 C 1.1682(2) -0.45056(19) 0.26880(12) 0.0461(4) Uani 1 1 d D . . H35 H 1.2443 -0.5314 0.2846 0.055 Uiso 1 1 calc R A 1 C36 C 1.1868(10) -0.4208(17) 0.1794(5) 0.0485(17) Uani 0.55 1 d PDU B 1 H36A H 1.1613 -0.4896 0.1626 0.073 Uiso 0.55 1 calc PR B 1 H36B H 1.2837 -0.4236 0.1556 0.073 Uiso 0.55 1 calc PR B 1 H36C H 1.1274 -0.3303 0.1625 0.073 Uiso 0.55 1 calc PR B 1 C37 C 1.029(2) -0.483(3) 0.3050(13) 0.093(4) Uani 0.55 1 d PDU B 1 H37A H 0.954 -0.404 0.2897 0.14 Uiso 0.55 1 calc PR B 1 H37B H 1.0172 -0.5038 0.3622 0.14 Uiso 0.55 1 calc PR B 1 H37C H 1.0271 -0.5617 0.2861 0.14 Uiso 0.55 1 calc PR B 1 C36' C 1.1503(15) -0.413(2) 0.1842(6) 0.053(2) Uani 0.45 1 d PDU B 2 H36D H 1.2335 -0.3906 0.1499 0.079 Uiso 0.45 1 calc PR B 2 H36E H 1.07 -0.3337 0.1786 0.079 Uiso 0.45 1 calc PR B 2 H36F H 1.1358 -0.4899 0.1694 0.079 Uiso 0.45 1 calc PR B 2 C37' C 1.045(3) -0.503(4) 0.3187(16) 0.095(4) Uani 0.45 1 d PDU B 2 H37D H 0.96 -0.4279 0.318 0.142 Uiso 0.45 1 calc PR B 2 H37E H 1.0589 -0.5368 0.3729 0.142 Uiso 0.45 1 calc PR B 2 H37F H 1.0379 -0.5763 0.2974 0.142 Uiso 0.45 1 calc PR B 2 O1 O 1.00207(11) -0.08121(10) 0.17857(6) 0.0264(2) Uani 1 1 d . . . P1 P 0.76779(3) 0.08510(4) 0.30192(2) 0.02391(7) Uani 1 1 d . . . P2 P 1.09745(3) -0.00742(3) 0.185562(19) 0.01929(6) Uani 1 1 d . . . Cl1 Cl 0.81998(4) 0.38958(4) 0.21061(3) 0.03598(9) Uani 1 1 d . . . Rh1 Rh 0.729367(11) 0.230854(11) 0.183653(6) 0.02284(4) 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 0.0464(9) 0.0279(7) 0.0256(7) 0.0036(6) -0.0144(6) -0.0091(6) C2 0.0448(9) 0.0276(8) 0.0363(8) -0.0081(6) -0.0239(7) 0.0043(6) C3 0.0336(8) 0.0448(10) 0.0409(9) -0.0125(7) -0.0210(7) 0.0005(7) C4 0.0318(7) 0.0395(8) 0.0290(7) -0.0054(6) -0.0129(6) -0.0119(6) C5 0.0362(7) 0.0261(7) 0.0284(7) -0.0047(5) -0.0124(6) -0.0068(6) C6 0.0494(9) 0.0323(8) 0.0243(7) -0.0055(6) -0.0113(6) -0.0055(7) C7 0.0600(11) 0.0432(10) 0.0375(9) -0.0069(7) -0.0301(8) -0.0070(8) C8 0.0354(8) 0.0400(9) 0.0300(7) 0.0093(6) -0.0120(6) -0.0219(7) C9 0.0712(14) 0.0656(14) 0.0362(10) 0.0211(9) -0.0222(10) -0.0389(12) C10 0.0621(12) 0.0508(11) 0.0521(11) 0.0112(9) -0.0277(10) -0.0373(10) C11 0.0197(6) 0.0747(13) 0.0254(7) -0.0112(8) -0.0033(5) -0.0073(7) C12 0.0396(9) 0.0698(14) 0.0373(10) -0.0203(9) -0.0103(8) 0.0170(9) C13 0.0214(8) 0.146(3) 0.0415(11) -0.0293(14) 0.0014(7) -0.0234(11) C14 0.0186(5) 0.0246(6) 0.0194(6) -0.0019(5) -0.0064(4) -0.0050(4) C15 0.0226(6) 0.0389(8) 0.0229(6) -0.0088(6) -0.0061(5) -0.0040(5) C16 0.0305(7) 0.0478(9) 0.0305(7) -0.0181(7) -0.0107(6) -0.0065(6) C17 0.0260(7) 0.0540(10) 0.0433(9) -0.0225(8) -0.0102(6) -0.0120(7) C18 0.0199(6) 0.0382(8) 0.0342(7) -0.0138(6) -0.0036(5) -0.0093(5) C19 0.0196(5) 0.0211(6) 0.0211(6) -0.0035(4) -0.0055(4) -0.0056(4) C20 0.0215(5) 0.0193(6) 0.0226(6) -0.0020(5) -0.0022(5) -0.0028(4) C21 0.0454(9) 0.0259(7) 0.0325(8) -0.0007(6) -0.0070(7) -0.0148(6) C22 0.0519(10) 0.0263(8) 0.0450(10) 0.0044(7) -0.0031(8) -0.0153(7) C23 0.0363(8) 0.0317(8) 0.0319(8) 0.0085(6) 0.0048(6) 0.0003(6) C24 0.0382(8) 0.0411(9) 0.0236(7) 0.0004(6) -0.0059(6) 0.0007(7) C25 0.0330(7) 0.0281(7) 0.0262(7) -0.0025(5) -0.0080(6) -0.0037(6) C26 0.0217(6) 0.0209(6) 0.0205(6) -0.0055(5) -0.0036(4) -0.0033(5) C27 0.0255(6) 0.0263(7) 0.0256(6) -0.0051(5) -0.0021(5) -0.0068(5) C28 0.0238(6) 0.0353(8) 0.0301(7) -0.0124(6) -0.0004(5) -0.0079(6) C29 0.0234(6) 0.0342(8) 0.0321(7) -0.0128(6) -0.0052(5) 0.0006(5) C30 0.0303(7) 0.0255(7) 0.0298(7) -0.0052(6) -0.0072(6) 0.0009(5) C31 0.0264(6) 0.0226(6) 0.0212(6) -0.0049(5) -0.0047(5) -0.0038(5) C32 0.0427(9) 0.0427(10) 0.0266(8) 0.0023(7) -0.0077(7) -0.0006(7) C33 0.0691(14) 0.0899(18) 0.0335(10) -0.0114(11) -0.0177(10) -0.0267(13) C34 0.0831(17) 0.0668(15) 0.0357(11) 0.0182(10) -0.0092(11) -0.0194(13) P3 0.02969(17) 0.02136(17) 0.02570(17) 0.00049(13) -0.00459(14) -0.00567(13) C35 0.0663(12) 0.0276(8) 0.0485(11) -0.0026(7) -0.0179(9) -0.0165(8) C36 0.059(5) 0.040(2) 0.0549(18) -0.0163(15) -0.021(3) -0.012(4) C37 0.127(5) 0.096(8) 0.086(7) -0.018(6) 0.000(5) -0.086(6) C36' 0.068(6) 0.041(2) 0.0562(19) -0.0143(16) -0.022(3) -0.014(4) C37' 0.129(5) 0.096(8) 0.087(7) -0.016(6) 0.001(5) -0.085(6) O1 0.0296(5) 0.0248(5) 0.0290(5) -0.0025(4) -0.0099(4) -0.0114(4) P1 0.01769(14) 0.03541(19) 0.01885(15) -0.00150(13) -0.00530(11) -0.00884(13) P2 0.02013(14) 0.01828(15) 0.01936(15) -0.00236(11) -0.00426(11) -0.00569(11) Cl1 0.04050(19) 0.02914(18) 0.0448(2) -0.00485(15) -0.01896(17) -0.01121(15) Rh1 0.02323(5) 0.02388(6) 0.02224(6) -0.00249(4) -0.00899(4) -0.00527(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C2 1.375(3) . ? C1 C6 1.530(2) . ? C1 Rh1 2.1934(15) . ? C1 H1 0.95 . ? C2 C3 1.540(3) . ? C2 Rh1 2.1795(15) . ? C2 H2 0.95 . ? C3 C7 1.538(3) . ? C3 C4 1.539(2) . ? C3 H3 1 . ? C4 C5 1.401(2) . ? C4 Rh1 2.1094(15) . ? C4 H4 0.95 . ? C5 C6 1.537(2) . ? C5 Rh1 2.1112(15) . ? C5 H5 0.95 . ? C6 C7 1.547(3) . ? C6 H6 1 . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 C9 1.529(2) . ? C8 C10 1.529(2) . ? C8 P1 1.8659(17) . ? C8 H8 1 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 C12 1.524(3) . ? C11 C13 1.537(3) . ? C11 P1 1.8680(17) . ? C11 H11 1 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 C15 1.3956(19) . ? C14 C19 1.4157(18) . ? C14 P1 1.8476(13) . ? C15 C16 1.388(2) . ? C15 H15 0.95 . ? C16 C17 1.374(2) . ? C16 H16 0.95 . ? C17 C18 1.391(2) . ? C17 H17 0.95 . ? C18 C19 1.3955(18) . ? C18 H18 0.95 . ? C19 P2 1.8318(14) . ? C20 C21 1.388(2) . ? C20 C25 1.394(2) . ? C20 P2 1.8077(14) . ? C21 C22 1.388(2) . ? C21 H21 0.95 . ? C22 C23 1.382(3) . ? C22 H22 0.95 . ? C23 C24 1.384(3) . ? C23 H23 0.95 . ? C24 C25 1.391(2) . ? C24 H24 0.95 . ? C25 H25 0.95 . ? C26 C27 1.4015(19) . ? C26 C31 1.4098(19) . ? C26 P2 1.8317(13) . ? C27 C28 1.392(2) . ? C27 H27 0.95 . ? C28 C29 1.379(2) . ? C28 H28 0.95 . ? C29 C30 1.388(2) . ? C29 H29 0.95 . ? C30 C31 1.401(2) . ? C30 H30 0.95 . ? C31 P3 1.8521(15) . ? C32 C33 1.521(3) . ? C32 C34 1.534(3) . ? C32 P3 1.8644(18) . ? C32 H32 1 . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? P3 C35 1.8769(19) . ? C35 C36' 1.518(10) . ? C35 C37' 1.530(11) . ? C35 C37 1.530(11) . ? C35 C36 1.530(8) . ? C35 H35 1 . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C36' H36D 0.98 . ? C36' H36E 0.98 . ? C36' H36F 0.98 . ? C37' H37D 0.98 . ? C37' H37E 0.98 . ? C37' H37F 0.98 . ? O1 P2 1.4885(10) . ? P1 Rh1 2.3347(4) . ? Cl1 Rh1 2.3626(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 106.50(15) . . ? C2 C1 Rh1 71.13(9) . . ? C6 C1 Rh1 94.87(9) . . ? C2 C1 H1 126.8 . . ? C6 C1 H1 126.8 . . ? Rh1 C1 H1 101.5 . . ? C1 C2 C3 106.79(15) . . ? C1 C2 Rh1 72.22(9) . . ? C3 C2 Rh1 94.52(10) . . ? C1 C2 H2 126.6 . . ? C3 C2 H2 126.6 . . ? Rh1 C2 H2 101 . . ? C7 C3 C4 100.54(14) . . ? C7 C3 C2 100.46(16) . . ? C4 C3 C2 100.79(12) . . ? C7 C3 H3 117.3 . . ? C4 C3 H3 117.3 . . ? C2 C3 H3 117.3 . . ? C5 C4 C3 106.18(14) . . ? C5 C4 Rh1 70.68(9) . . ? C3 C4 Rh1 97.37(11) . . ? C5 C4 H4 126.9 . . ? C3 C4 H4 126.9 . . ? Rh1 C4 H4 99.7 . . ? C4 C5 C6 106.03(14) . . ? C4 C5 Rh1 70.54(9) . . ? C6 C5 Rh1 97.98(10) . . ? C4 C5 H5 127 . . ? C6 C5 H5 127 . . ? Rh1 C5 H5 99.3 . . ? C1 C6 C5 100.63(12) . . ? C1 C6 C7 100.87(14) . . ? C5 C6 C7 100.73(14) . . ? C1 C6 H6 117.2 . . ? C5 C6 H6 117.2 . . ? C7 C6 H6 117.2 . . ? C3 C7 C6 93.87(12) . . ? C3 C7 H7A 112.9 . . ? C6 C7 H7A 112.9 . . ? C3 C7 H7B 112.9 . . ? C6 C7 H7B 112.9 . . ? H7A C7 H7B 110.4 . . ? C9 C8 C10 111.43(14) . . ? C9 C8 P1 113.59(15) . . ? C10 C8 P1 115.42(12) . . ? C9 C8 H8 105.1 . . ? C10 C8 H8 105.1 . . ? P1 C8 H8 105.1 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C13 108.86(18) . . ? C12 C11 P1 113.98(13) . . ? C13 C11 P1 109.20(14) . . ? C12 C11 H11 108.2 . . ? C13 C11 H11 108.2 . . ? P1 C11 H11 108.2 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 117.70(12) . . ? C15 C14 P1 119.07(10) . . ? C19 C14 P1 123.19(10) . . ? C16 C15 C14 122.47(13) . . ? C16 C15 H15 118.8 . . ? C14 C15 H15 118.8 . . ? C17 C16 C15 119.46(14) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 119.54(14) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C17 C18 C19 121.63(13) . . ? C17 C18 H18 119.2 . . ? C19 C18 H18 119.2 . . ? C18 C19 C14 119.06(12) . . ? C18 C19 P2 115.61(10) . . ? C14 C19 P2 125.31(10) . . ? C21 C20 C25 119.31(13) . . ? C21 C20 P2 124.58(11) . . ? C25 C20 P2 116.07(11) . . ? C22 C21 C20 119.80(16) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C23 C22 C21 120.84(17) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C22 C23 C24 119.74(15) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C23 C24 C25 119.80(16) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C24 C25 C20 120.49(16) . . ? C24 C25 H25 119.8 . . ? C20 C25 H25 119.8 . . ? C27 C26 C31 119.61(12) . . ? C27 C26 P2 119.58(10) . . ? C31 C26 P2 120.81(10) . . ? C28 C27 C26 120.94(14) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C29 C28 C27 119.74(14) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 119.83(14) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C29 C30 C31 121.86(14) . . ? C29 C30 H30 119.1 . . ? C31 C30 H30 119.1 . . ? C30 C31 C26 118.00(13) . . ? C30 C31 P3 121.28(11) . . ? C26 C31 P3 120.70(10) . . ? C33 C32 C34 109.89(19) . . ? C33 C32 P3 109.20(14) . . ? C34 C32 P3 110.46(16) . . ? C33 C32 H32 109.1 . . ? C34 C32 H32 109.1 . . ? P3 C32 H32 109.1 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 P3 C32 100.11(8) . . ? C31 P3 C35 101.27(8) . . ? C32 P3 C35 102.99(9) . . ? C36' C35 C37' 107.7(12) . . ? C36' C35 C37 96.7(13) . . ? C37' C35 C36 119.3(14) . . ? C37 C35 C36 109.0(9) . . ? C36' C35 P3 112.2(8) . . ? C37' C35 P3 108.9(12) . . ? C37 C35 P3 109.5(10) . . ? C36 C35 P3 111.2(6) . . ? C36' C35 H35 119.4 . . ? C37' C35 H35 98.3 . . ? C37 C35 H35 109 . . ? C36 C35 H35 109 . . ? P3 C35 H35 109 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C36' H36D 109.5 . . ? C35 C36' H36E 109.5 . . ? H36D C36' H36E 109.5 . . ? C35 C36' H36F 109.5 . . ? H36D C36' H36F 109.5 . . ? H36E C36' H36F 109.5 . . ? C35 C37' H37D 109.5 . . ? C35 C37' H37E 109.5 . . ? H37D C37' H37E 109.5 . . ? C35 C37' H37F 109.5 . . ? H37D C37' H37F 109.5 . . ? H37E C37' H37F 109.5 . . ? C14 P1 C8 100.42(7) . . ? C14 P1 C11 104.03(7) . . ? C8 P1 C11 104.39(9) . . ? C14 P1 Rh1 112.16(4) . . ? C8 P1 Rh1 126.34(5) . . ? C11 P1 Rh1 107.31(6) . . ? O1 P2 C20 110.67(6) . . ? O1 P2 C26 112.86(6) . . ? C20 P2 C26 104.84(6) . . ? O1 P2 C19 116.38(6) . . ? C20 P2 C19 107.77(6) . . ? C26 P2 C19 103.47(6) . . ? C4 Rh1 C5 38.77(6) . . ? C4 Rh1 C2 67.14(7) . . ? C5 Rh1 C2 79.31(6) . . ? C4 Rh1 C1 79.35(6) . . ? C5 Rh1 C1 66.47(6) . . ? C2 Rh1 C1 36.65(7) . . ? C4 Rh1 P1 99.69(5) . . ? C5 Rh1 P1 105.66(4) . . ? C2 Rh1 P1 152.94(5) . . ? C1 Rh1 P1 168.63(5) . . ? C4 Rh1 Cl1 157.35(5) . . ? C5 Rh1 Cl1 154.40(5) . . ? C2 Rh1 Cl1 94.39(5) . . ? C1 Rh1 Cl1 93.66(5) . . ? P1 Rh1 Cl1 91.274(14) . . ? data_8 _database_code_depnum_ccdc_archive 'CCDC 895724' #TrackingRef 'Dalton Trans Bourissou DPPO CIF.cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C31 H41 O2 P3 Rh, C F3 O3 S' _chemical_formula_sum 'C32 H41 F3 O5 P3 Rh S' _chemical_formula_weight 790.54 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1191(5) _cell_length_b 19.9268(12) _cell_length_c 23.3037(15) _cell_angle_alpha 68.072(3) _cell_angle_beta 85.812(3) _cell_angle_gamma 85.295(3) _cell_volume 3482.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 7674 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 23.37 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.742 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_absorpt_correction_T_min 0.960 _exptl_absorpt_correction_T_max 0.985 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'Bruker Kappa APEX II Quazar' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0709 _diffrn_reflns_av_unetI/netI 0.0857 _diffrn_reflns_number 52047 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 5.1 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 14095 _reflns_number_gt 9446 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0543P)^2^+4.8826P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 14095 _refine_ls_number_parameters 827 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1047 _refine_ls_R_factor_gt 0.0602 _refine_ls_wR_factor_ref 0.1396 _refine_ls_wR_factor_gt 0.1232 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.047 _refine_diff_density_min -0.887 _refine_diff_density_rms 0.103 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Rh1 Rh 0.34221(5) 0.17044(2) 0.496712(19) 0.02508(12) Uani 1 1 d . . . P3 P 0.31926(16) 0.08904(7) 0.59754(7) 0.0267(3) Uani 1 1 d . . . P2 P 0.31360(16) 0.27517(7) 0.41013(6) 0.0284(3) Uani 1 1 d . . . P1 P 0.09271(15) 0.25376(7) 0.54712(6) 0.0224(3) Uani 1 1 d . . . O2 O 0.6911(5) 0.1325(2) 0.4703(2) 0.0571(13) Uani 1 1 d . . . C1 C -0.1175(6) 0.2792(3) 0.5623(2) 0.0231(11) Uani 1 1 d . . . C18 C 0.2718(6) 0.1444(3) 0.6449(2) 0.0279(12) Uani 1 1 d . . . C29 C 0.6456(7) 0.0637(3) 0.6347(3) 0.0441(15) Uani 1 1 d . . . H29A H 0.7361 0.0281 0.653 0.066 Uiso 1 1 calc R . . H29B H 0.6201 0.0942 0.6593 0.066 Uiso 1 1 calc R . . H29C H 0.6787 0.0941 0.5922 0.066 Uiso 1 1 calc R . . C11 C 0.3076(6) 0.4186(3) 0.4040(3) 0.0315(12) Uani 1 1 d . . . H11 H 0.3558 0.428 0.3635 0.038 Uiso 1 1 calc R . . C8 C 0.1586(6) 0.3956(3) 0.5182(2) 0.0285(12) Uani 1 1 d . . . H8 H 0.1037 0.388 0.5574 0.034 Uiso 1 1 calc R . . C2 C -0.2028(6) 0.2388(3) 0.6167(3) 0.0327(13) Uani 1 1 d . . . H2 H -0.1484 0.1984 0.6469 0.039 Uiso 1 1 calc R . . C6 C -0.1994(6) 0.3376(3) 0.5183(3) 0.0294(12) Uani 1 1 d . . . H6 H -0.1424 0.3644 0.4806 0.035 Uiso 1 1 calc R . . C14 C 0.1544(6) 0.2525(3) 0.6614(2) 0.0289(12) Uani 1 1 d . . . H14 H 0.0945 0.2982 0.647 0.035 Uiso 1 1 calc R . . C22 C 0.4867(7) 0.3067(3) 0.3523(3) 0.0398(14) Uani 1 1 d . . . H22 H 0.448 0.3535 0.3199 0.048 Uiso 1 1 calc R . . C7 C 0.1847(6) 0.3373(3) 0.4981(2) 0.0237(11) Uani 1 1 d . . . C15 C 0.2103(6) 0.2258(3) 0.7206(3) 0.0346(13) Uani 1 1 d . . . H15 H 0.1931 0.2541 0.7458 0.042 Uiso 1 1 calc R . . C17 C 0.3197(6) 0.1189(3) 0.7056(3) 0.0314(12) Uani 1 1 d . . . H17 H 0.3749 0.0722 0.722 0.038 Uiso 1 1 calc R . . C28 C 0.4941(7) 0.0247(3) 0.6341(3) 0.0379(14) Uani 1 1 d . . . H28 H 0.459 -0.004 0.678 0.045 Uiso 1 1 calc R . . C3 C -0.3673(7) 0.2579(3) 0.6267(3) 0.0425(15) Uani 1 1 d . . . H3 H -0.4263 0.2301 0.6636 0.051 Uiso 1 1 calc R . . C4 C -0.4461(6) 0.3175(3) 0.5829(3) 0.0388(14) Uani 1 1 d . . . H4 H -0.5582 0.331 0.5904 0.047 Uiso 1 1 calc R . . C9 C 0.2107(6) 0.4642(3) 0.4826(3) 0.0327(13) Uani 1 1 d . . . H9 H 0.1963 0.5025 0.4978 0.039 Uiso 1 1 calc R . . C12 C 0.2646(6) 0.3489(3) 0.4394(2) 0.0265(11) Uani 1 1 d . . . C5 C -0.3637(6) 0.3571(3) 0.5287(3) 0.0404(15) Uani 1 1 d . . . H5 H -0.4184 0.3975 0.4987 0.048 Uiso 1 1 calc R . . C10 C 0.2829(6) 0.4752(3) 0.4254(3) 0.0342(13) Uani 1 1 d . . . H10 H 0.3167 0.522 0.3999 0.041 Uiso 1 1 calc R . . C13 C 0.1838(5) 0.2139(3) 0.6221(2) 0.0232(11) Uani 1 1 d . . . C16 C 0.2903(6) 0.1588(3) 0.7433(3) 0.0338(13) Uani 1 1 d . . . H16 H 0.3256 0.1397 0.7846 0.041 Uiso 1 1 calc R . . C23 C 0.6363(7) 0.3208(4) 0.3803(3) 0.0510(17) Uani 1 1 d . . . H23A H 0.6795 0.2754 0.4112 0.076 Uiso 1 1 calc R . . H23B H 0.6043 0.3558 0.4002 0.076 Uiso 1 1 calc R . . H23C H 0.7219 0.3405 0.3477 0.076 Uiso 1 1 calc R . . C31 C 0.5553(7) 0.1474(3) 0.4806(3) 0.0347(13) Uani 1 1 d . . . C26 C 0.0942(8) 0.0141(3) 0.5606(3) 0.0499(17) Uani 1 1 d . . . H26A H 0.1812 -0.021 0.5562 0.075 Uiso 1 1 calc R . . H26B H 0.0905 0.0569 0.5221 0.075 Uiso 1 1 calc R . . H26C H -0.0128 -0.008 0.5691 0.075 Uiso 1 1 calc R . . C25 C 0.1311(7) 0.0365(3) 0.6140(3) 0.0358(13) Uani 1 1 d . . . H25 H 0.0367 0.0707 0.6171 0.043 Uiso 1 1 calc R . . S2 S 0.89705(18) 0.52483(8) 0.33792(7) 0.0392(4) Uani 1 1 d . . . F4 F 0.6041(5) 0.5876(3) 0.3426(3) 0.0955(17) Uani 1 1 d . . . F6 F 0.7138(6) 0.6118(3) 0.2505(2) 0.0959(16) Uani 1 1 d . . . F5 F 0.6103(5) 0.5076(2) 0.3023(2) 0.0801(13) Uani 1 1 d . . . O10 O 0.9611(5) 0.5839(2) 0.3471(2) 0.0484(11) Uani 1 1 d . . . O9 O 0.9815(6) 0.5031(3) 0.2924(2) 0.0659(14) Uani 1 1 d . . . O8 O 0.8531(7) 0.4666(3) 0.3946(2) 0.0757(16) Uani 1 1 d . . . C64 C 0.6894(7) 0.5595(3) 0.3068(3) 0.0384(14) Uani 1 1 d . . . Rh2 Rh 0.69260(5) 0.33350(2) 1.000675(19) 0.02695(12) Uani 1 1 d . . . P4 P 0.50423(15) 0.24617(7) 0.95178(6) 0.0212(3) Uani 1 1 d . . . P5 P 0.68163(16) 0.22781(7) 1.08707(6) 0.0267(3) Uani 1 1 d . . . P6 P 0.67655(16) 0.41299(7) 0.89912(7) 0.0269(3) Uani 1 1 d . . . C44 C 0.6093(6) 0.2854(3) 0.8766(2) 0.0220(10) Uani 1 1 d . . . C49 C 0.6755(6) 0.3554(2) 0.8531(2) 0.0235(11) Uani 1 1 d . . . C41 C 0.7464(6) 0.0272(3) 1.0729(3) 0.0304(12) Uani 1 1 d . . . H41 H 0.791 -0.0192 1.0982 0.037 Uiso 1 1 calc R . . C45 C 0.6147(6) 0.2456(3) 0.8388(2) 0.0291(12) Uani 1 1 d . . . H45 H 0.5689 0.1995 0.8542 0.035 Uiso 1 1 calc R . . C48 C 0.7404(6) 0.3802(3) 0.7919(2) 0.0303(12) Uani 1 1 d . . . H48 H 0.7829 0.4269 0.7749 0.036 Uiso 1 1 calc R . . C40 C 0.6876(6) 0.0369(3) 1.0170(3) 0.0311(12) Uani 1 1 d . . . H40 H 0.6938 -0.0019 1.0025 0.037 Uiso 1 1 calc R . . C38 C 0.6120(5) 0.1632(3) 1.0003(2) 0.0219(11) Uani 1 1 d . . . C37 C 0.2368(6) 0.1598(3) 0.9792(3) 0.0307(12) Uani 1 1 d . . . H37 H 0.2903 0.1321 1.0164 0.037 Uiso 1 1 calc R . . C56 C 0.4724(7) 0.4653(3) 0.8807(3) 0.0359(13) Uani 1 1 d . . . H56 H 0.3935 0.4304 0.8786 0.043 Uiso 1 1 calc R . . C32 C 0.3110(5) 0.2193(2) 0.9367(2) 0.0204(10) Uani 1 1 d . . . C43 C 0.6791(5) 0.1538(3) 1.0579(2) 0.0235(11) Uani 1 1 d . . . C33 C 0.2307(6) 0.2606(3) 0.8828(3) 0.0339(13) Uani 1 1 d . . . H33 H 0.2801 0.3018 0.8531 0.041 Uiso 1 1 calc R . . C57 C 0.4032(8) 0.4905(4) 0.9327(3) 0.0538(18) Uani 1 1 d . . . H57A H 0.4743 0.5263 0.9359 0.081 Uiso 1 1 calc R . . H57B H 0.4001 0.4488 0.972 0.081 Uiso 1 1 calc R . . H57C H 0.2911 0.5125 0.9235 0.081 Uiso 1 1 calc R . . C47 C 0.7448(6) 0.3391(3) 0.7553(2) 0.0317(13) Uani 1 1 d . . . H47 H 0.789 0.3579 0.7139 0.038 Uiso 1 1 calc R . . C39 C 0.6184(6) 0.1046(3) 0.9815(3) 0.0282(12) Uani 1 1 d . . . H39 H 0.5741 0.111 0.9431 0.034 Uiso 1 1 calc R . . C35 C 0.0086(6) 0.1806(3) 0.9146(3) 0.0391(14) Uani 1 1 d . . . H35 H -0.0937 0.1668 0.9063 0.047 Uiso 1 1 calc R . . C42 C 0.7419(6) 0.0844(3) 1.0931(3) 0.0332(13) Uani 1 1 d . . . H42 H 0.7831 0.0761 1.1325 0.04 Uiso 1 1 calc R . . C46 C 0.6853(6) 0.2713(3) 0.7790(2) 0.0314(12) Uani 1 1 d . . . H46 H 0.6922 0.242 0.7546 0.038 Uiso 1 1 calc R . . C59 C 0.8385(7) 0.4771(3) 0.8619(3) 0.0333(13) Uani 1 1 d . . . H59 H 0.812 0.504 0.8176 0.04 Uiso 1 1 calc R . . C50 C 0.4816(7) 0.2193(3) 1.1324(3) 0.0332(13) Uani 1 1 d . . . H50 H 0.4007 0.2066 1.1082 0.04 Uiso 1 1 calc R . . C34 C 0.0795(7) 0.2414(4) 0.8727(3) 0.0426(15) Uani 1 1 d . . . H34 H 0.0234 0.2703 0.8365 0.051 Uiso 1 1 calc R . . C51 C 0.4809(8) 0.1594(3) 1.1954(3) 0.0473(16) Uani 1 1 d . . . H51A H 0.5549 0.1702 1.2218 0.071 Uiso 1 1 calc R . . H51B H 0.519 0.1134 1.1913 0.071 Uiso 1 1 calc R . . H51C H 0.3683 0.1556 1.2142 0.071 Uiso 1 1 calc R . . O4 O 1.0025(6) 0.3820(3) 1.0277(2) 0.0643(14) Uani 1 1 d . . . C36 C 0.0864(6) 0.1396(3) 0.9688(3) 0.0394(14) Uani 1 1 d . . . H36 H 0.0371 0.0983 0.9983 0.047 Uiso 1 1 calc R . . C53 C 0.8462(7) 0.2001(3) 1.1432(3) 0.0382(14) Uani 1 1 d . . . H53 H 0.8191 0.1525 1.176 0.046 Uiso 1 1 calc R . . C52 C 0.4145(8) 0.2921(3) 1.1363(3) 0.0521(17) Uani 1 1 d . . . H52A H 0.3081 0.2856 1.1598 0.078 Uiso 1 1 calc R . . H52B H 0.3994 0.328 1.0944 0.078 Uiso 1 1 calc R . . H52C H 0.4934 0.3089 1.1571 0.078 Uiso 1 1 calc R . . C54 C 1.0163(7) 0.1901(3) 1.1133(3) 0.0441(15) Uani 1 1 d . . . H54A H 1.0462 0.2363 1.0812 0.066 Uiso 1 1 calc R . . H54B H 1.0122 0.1537 1.0946 0.066 Uiso 1 1 calc R . . H54C H 1.0992 0.1739 1.1449 0.066 Uiso 1 1 calc R . . C58 C 0.4722(8) 0.5267(3) 0.8182(3) 0.0484(16) Uani 1 1 d . . . H58A H 0.3584 0.5463 0.8088 0.073 Uiso 1 1 calc R . . H58B H 0.5184 0.5085 0.7863 0.073 Uiso 1 1 calc R . . H58C H 0.5395 0.5649 0.819 0.073 Uiso 1 1 calc R . . C61 C 0.8414(8) 0.5317(3) 0.8931(3) 0.0494(17) Uani 1 1 d . . . H61A H 0.8634 0.5061 0.937 0.074 Uiso 1 1 calc R . . H61B H 0.7341 0.559 0.8894 0.074 Uiso 1 1 calc R . . H61C H 0.9285 0.5652 0.8731 0.074 Uiso 1 1 calc R . . C55 C 0.8527(8) 0.2553(4) 1.1746(3) 0.0491(16) Uani 1 1 d . . . H55A H 0.94 0.2394 1.2046 0.074 Uiso 1 1 calc R . . H55B H 0.746 0.2589 1.1961 0.074 Uiso 1 1 calc R . . H55C H 0.8763 0.3028 1.1432 0.074 Uiso 1 1 calc R . . C60 C 1.0100(7) 0.4372(3) 0.8638(3) 0.0462(16) Uani 1 1 d . . . H60A H 1.0923 0.4723 0.8415 0.069 Uiso 1 1 calc R . . H60B H 1.0066 0.4017 0.8441 0.069 Uiso 1 1 calc R . . H60C H 1.0402 0.4123 0.9069 0.069 Uiso 1 1 calc R . . C62 C 0.8825(7) 0.3629(3) 1.0167(3) 0.0379(14) Uani 1 1 d . . . S1 S 0.66231(19) 0.02204(8) 0.83701(7) 0.0408(4) Uani 1 1 d . . . O5 O 0.5759(5) 0.0815(2) 0.8475(2) 0.0540(12) Uani 1 1 d . . . F2 F 0.9651(5) 0.0021(3) 0.7988(2) 0.0927(16) Uani 1 1 d . . . F1 F 0.9354(5) 0.0797(3) 0.8415(3) 0.1081(19) Uani 1 1 d . . . F3 F 0.8467(6) 0.1086(3) 0.7504(2) 0.0993(17) Uani 1 1 d . . . C27 C 0.1289(8) -0.0271(3) 0.6758(3) 0.0522(17) Uani 1 1 d . . . H27A H 0.0172 -0.0447 0.6859 0.078 Uiso 1 1 calc R . . H27B H 0.1615 -0.0114 0.7083 0.078 Uiso 1 1 calc R . . H27C H 0.2067 -0.0662 0.6731 0.078 Uiso 1 1 calc R . . C30 C 0.5310(8) -0.0274(3) 0.6003(3) 0.0529(18) Uani 1 1 d . . . H30A H 0.5651 -0.0002 0.5571 0.079 Uiso 1 1 calc R . . H30B H 0.4315 -0.0527 0.6017 0.079 Uiso 1 1 calc R . . H30C H 0.6203 -0.0628 0.6204 0.079 Uiso 1 1 calc R . . O3 O 0.4716(4) 0.30035(17) 0.98347(16) 0.0269(8) Uani 1 1 d . . . O1 O 0.0982(4) 0.19985(18) 0.51490(16) 0.0264(8) Uani 1 1 d . . . C24 C 0.5297(8) 0.2525(4) 0.3207(3) 0.0549(18) Uani 1 1 d . . . H24A H 0.6221 0.2693 0.2904 0.082 Uiso 1 1 calc R . . H24B H 0.4333 0.2483 0.2995 0.082 Uiso 1 1 calc R . . H24C H 0.5614 0.2051 0.3518 0.082 Uiso 1 1 calc R . . O6 O 0.5992(6) 0.0027(3) 0.7908(2) 0.0651(14) Uani 1 1 d . . . O7 O 0.7037(7) -0.0387(3) 0.8925(2) 0.089(2) Uani 1 1 d . . . C63 C 0.8677(8) 0.0553(3) 0.8048(3) 0.0410(14) Uani 1 1 d . . . C19 C 0.1284(7) 0.2782(3) 0.3674(3) 0.0421(15) Uani 1 1 d . . . H19 H 0.0319 0.2877 0.393 0.051 Uiso 1 1 calc R . . C20 C 0.1162(9) 0.3385(4) 0.3040(3) 0.0557(18) Uani 1 1 d . . . H20A H 0.2047 0.3305 0.2759 0.084 Uiso 1 1 calc R . . H20B H 0.1276 0.3852 0.3079 0.084 Uiso 1 1 calc R . . H20C H 0.0086 0.3387 0.2875 0.084 Uiso 1 1 calc R . . C21 C 0.1021(9) 0.2038(4) 0.3633(3) 0.0588(19) Uani 1 1 d . . . H21A H -0.0062 0.2055 0.3467 0.088 Uiso 1 1 calc R . . H21B H 0.1068 0.1659 0.4047 0.088 Uiso 1 1 calc R . . H21C H 0.1891 0.1931 0.336 0.088 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 Rh1 0.0215(2) 0.0284(2) 0.0281(2) -0.01496(19) -0.00133(17) 0.00541(16) P3 0.0215(7) 0.0272(7) 0.0331(8) -0.0139(6) -0.0039(6) 0.0040(5) P2 0.0265(7) 0.0340(8) 0.0274(8) -0.0159(7) 0.0032(6) 0.0011(6) P1 0.0167(6) 0.0255(7) 0.0257(7) -0.0109(6) -0.0013(5) 0.0018(5) O2 0.032(2) 0.066(3) 0.071(3) -0.027(3) 0.006(2) 0.015(2) C1 0.022(3) 0.025(3) 0.025(3) -0.011(2) -0.002(2) -0.003(2) C18 0.023(3) 0.030(3) 0.032(3) -0.013(2) 0.000(2) -0.002(2) C29 0.028(3) 0.055(4) 0.049(4) -0.020(3) -0.013(3) 0.012(3) C11 0.025(3) 0.034(3) 0.032(3) -0.011(3) 0.004(2) 0.001(2) C8 0.024(3) 0.031(3) 0.031(3) -0.013(2) 0.000(2) 0.002(2) C2 0.023(3) 0.037(3) 0.035(3) -0.010(3) -0.006(2) 0.001(2) C6 0.020(3) 0.032(3) 0.032(3) -0.008(3) -0.005(2) 0.005(2) C14 0.027(3) 0.029(3) 0.033(3) -0.014(3) -0.004(2) 0.003(2) C22 0.041(3) 0.044(3) 0.034(3) -0.016(3) 0.010(3) 0.001(3) C7 0.018(2) 0.024(3) 0.027(3) -0.008(2) -0.002(2) 0.0030(19) C15 0.034(3) 0.042(3) 0.033(3) -0.020(3) -0.002(2) -0.004(3) C17 0.024(3) 0.035(3) 0.034(3) -0.012(3) -0.006(2) 0.006(2) C28 0.035(3) 0.035(3) 0.047(4) -0.019(3) -0.016(3) 0.016(2) C3 0.027(3) 0.063(4) 0.034(3) -0.014(3) 0.005(3) -0.012(3) C4 0.014(3) 0.059(4) 0.051(4) -0.030(3) -0.002(3) 0.002(3) C9 0.026(3) 0.025(3) 0.050(4) -0.018(3) -0.002(3) 0.005(2) C12 0.022(3) 0.031(3) 0.025(3) -0.010(2) 0.000(2) 0.004(2) C5 0.024(3) 0.036(3) 0.057(4) -0.013(3) -0.009(3) 0.004(2) C10 0.026(3) 0.030(3) 0.039(3) -0.005(3) 0.004(2) -0.001(2) C13 0.015(2) 0.026(3) 0.028(3) -0.008(2) -0.002(2) -0.0006(19) C16 0.024(3) 0.051(4) 0.025(3) -0.012(3) -0.006(2) 0.003(2) C23 0.027(3) 0.058(4) 0.065(5) -0.022(4) 0.010(3) -0.002(3) C31 0.038(3) 0.036(3) 0.029(3) -0.013(3) 0.001(3) 0.003(3) C26 0.042(4) 0.047(4) 0.073(5) -0.036(4) -0.008(3) -0.002(3) C25 0.038(3) 0.034(3) 0.038(3) -0.017(3) 0.002(3) 0.002(2) S2 0.0407(8) 0.0363(8) 0.0399(9) -0.0136(7) 0.0003(7) -0.0031(6) F4 0.042(2) 0.140(4) 0.138(5) -0.096(4) 0.011(3) 0.004(3) F6 0.100(4) 0.077(3) 0.070(3) 0.019(3) -0.022(3) 0.016(3) F5 0.073(3) 0.090(3) 0.086(3) -0.035(3) -0.028(2) -0.024(2) O10 0.038(2) 0.048(2) 0.070(3) -0.033(2) 0.003(2) -0.0125(19) O9 0.066(3) 0.069(3) 0.077(4) -0.048(3) 0.013(3) 0.007(2) O8 0.092(4) 0.062(3) 0.043(3) 0.023(3) -0.019(3) -0.027(3) C64 0.046(4) 0.033(3) 0.034(3) -0.011(3) 0.007(3) -0.005(3) Rh2 0.0269(2) 0.0289(2) 0.0296(3) -0.0152(2) -0.00260(18) -0.00434(17) P4 0.0179(6) 0.0229(6) 0.0239(7) -0.0094(6) -0.0032(5) -0.0004(5) P5 0.0239(7) 0.0343(8) 0.0257(8) -0.0153(6) -0.0040(6) -0.0006(6) P6 0.0261(7) 0.0251(7) 0.0328(8) -0.0135(6) -0.0027(6) -0.0045(5) C44 0.018(2) 0.028(3) 0.023(3) -0.013(2) -0.004(2) -0.002(2) C49 0.022(3) 0.022(2) 0.027(3) -0.008(2) -0.005(2) -0.002(2) C41 0.029(3) 0.023(3) 0.035(3) -0.005(2) -0.008(2) 0.000(2) C45 0.023(3) 0.031(3) 0.036(3) -0.014(3) -0.005(2) -0.004(2) C48 0.029(3) 0.030(3) 0.026(3) -0.003(2) 0.001(2) -0.009(2) C40 0.021(3) 0.029(3) 0.045(4) -0.018(3) -0.003(2) 0.003(2) C38 0.015(2) 0.027(3) 0.023(3) -0.008(2) -0.002(2) -0.0028(19) C37 0.023(3) 0.037(3) 0.030(3) -0.011(3) 0.002(2) -0.002(2) C56 0.037(3) 0.033(3) 0.041(4) -0.018(3) -0.005(3) 0.000(2) C32 0.019(2) 0.023(2) 0.022(3) -0.012(2) -0.001(2) 0.0004(19) C43 0.015(2) 0.033(3) 0.026(3) -0.014(2) -0.002(2) -0.001(2) C33 0.022(3) 0.044(3) 0.030(3) -0.008(3) -0.002(2) -0.004(2) C57 0.048(4) 0.055(4) 0.068(5) -0.036(4) -0.008(3) 0.012(3) C47 0.027(3) 0.047(3) 0.022(3) -0.015(3) 0.003(2) -0.003(2) C39 0.022(3) 0.029(3) 0.034(3) -0.012(2) -0.004(2) -0.003(2) C35 0.020(3) 0.055(4) 0.051(4) -0.029(3) -0.004(3) 0.001(3) C42 0.027(3) 0.041(3) 0.033(3) -0.015(3) -0.005(2) -0.003(2) C46 0.033(3) 0.039(3) 0.024(3) -0.013(3) -0.001(2) -0.002(2) C59 0.039(3) 0.027(3) 0.036(3) -0.012(3) -0.001(3) -0.015(2) C50 0.033(3) 0.039(3) 0.030(3) -0.015(3) 0.000(2) -0.002(2) C34 0.023(3) 0.066(4) 0.035(3) -0.017(3) -0.010(3) 0.011(3) C51 0.046(4) 0.053(4) 0.044(4) -0.020(3) 0.009(3) -0.007(3) O4 0.055(3) 0.076(3) 0.068(3) -0.027(3) -0.019(2) -0.029(3) C36 0.020(3) 0.044(3) 0.054(4) -0.017(3) 0.008(3) -0.009(2) C53 0.033(3) 0.052(4) 0.039(4) -0.026(3) -0.007(3) -0.006(3) C52 0.057(4) 0.047(4) 0.057(4) -0.029(3) 0.012(3) 0.003(3) C54 0.029(3) 0.054(4) 0.058(4) -0.028(3) -0.014(3) 0.002(3) C58 0.051(4) 0.044(4) 0.050(4) -0.015(3) -0.011(3) -0.002(3) C61 0.055(4) 0.032(3) 0.068(5) -0.023(3) 0.000(3) -0.021(3) C55 0.049(4) 0.072(5) 0.041(4) -0.036(4) -0.011(3) -0.005(3) C60 0.028(3) 0.057(4) 0.060(4) -0.028(3) 0.002(3) -0.014(3) C62 0.047(4) 0.037(3) 0.033(3) -0.013(3) -0.007(3) -0.012(3) S1 0.0427(9) 0.0380(8) 0.0393(9) -0.0125(7) -0.0029(7) 0.0025(7) O5 0.049(3) 0.052(3) 0.072(3) -0.037(3) -0.014(2) 0.016(2) F2 0.059(3) 0.104(4) 0.100(4) -0.029(3) 0.017(3) 0.023(3) F1 0.052(3) 0.157(5) 0.154(5) -0.096(5) -0.023(3) -0.015(3) F3 0.097(4) 0.085(3) 0.077(3) 0.017(3) 0.006(3) -0.030(3) C27 0.052(4) 0.043(4) 0.058(4) -0.014(3) 0.000(3) -0.006(3) C30 0.046(4) 0.046(4) 0.073(5) -0.033(4) -0.010(3) 0.020(3) O3 0.0259(18) 0.0280(18) 0.030(2) -0.0159(17) -0.0003(15) 0.0016(15) O1 0.0191(17) 0.0295(19) 0.033(2) -0.0147(17) -0.0027(15) 0.0031(14) C24 0.062(4) 0.062(4) 0.044(4) -0.029(4) 0.022(3) 0.000(3) O6 0.071(3) 0.065(3) 0.081(4) -0.047(3) -0.019(3) -0.008(3) O7 0.098(4) 0.070(3) 0.045(3) 0.028(3) 0.011(3) 0.027(3) C63 0.046(4) 0.039(3) 0.038(4) -0.013(3) -0.010(3) 0.006(3) C19 0.044(4) 0.047(4) 0.040(4) -0.021(3) -0.009(3) 0.006(3) C20 0.064(5) 0.060(4) 0.042(4) -0.019(4) -0.015(3) 0.013(3) C21 0.063(5) 0.061(4) 0.060(5) -0.027(4) -0.020(4) -0.008(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Rh1 C31 1.802(6) . ? Rh1 O1 2.079(3) . ? Rh1 P2 2.3074(15) . ? Rh1 P3 2.3078(15) . ? P3 C18 1.835(5) . ? P3 C28 1.857(5) . ? P3 C25 1.859(6) . ? P2 C12 1.843(5) . ? P2 C19 1.849(6) . ? P2 C22 1.850(6) . ? P1 O1 1.520(4) . ? P1 C1 1.788(5) . ? P1 C13 1.814(5) . ? P1 C7 1.814(5) . ? O2 C31 1.150(6) . ? C1 C6 1.387(7) . ? C1 C2 1.393(7) . ? C18 C17 1.386(7) . ? C18 C13 1.433(7) . ? C29 C28 1.511(8) . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C11 C12 1.382(7) . ? C11 C10 1.390(7) . ? C11 H11 0.95 . ? C8 C9 1.390(7) . ? C8 C7 1.404(7) . ? C8 H8 0.95 . ? C2 C3 1.386(7) . ? C2 H2 0.95 . ? C6 C5 1.388(7) . ? C6 H6 0.95 . ? C14 C15 1.376(7) . ? C14 C13 1.396(7) . ? C14 H14 0.95 . ? C22 C23 1.514(8) . ? C22 C24 1.525(8) . ? C22 H22 1 . ? C7 C12 1.415(7) . ? C15 C16 1.366(7) . ? C15 H15 0.95 . ? C17 C16 1.386(7) . ? C17 H17 0.95 . ? C28 C30 1.522(8) . ? C28 H28 1 . ? C3 C4 1.389(8) . ? C3 H3 0.95 . ? C4 C5 1.372(8) . ? C4 H4 0.95 . ? C9 C10 1.364(8) . ? C9 H9 0.95 . ? C5 H5 0.95 . ? C10 H10 0.95 . ? C16 H16 0.95 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C26 C25 1.525(8) . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C25 C27 1.523(8) . ? C25 H25 1 . ? S2 O9 1.404(5) . ? S2 O10 1.416(4) . ? S2 O8 1.439(4) . ? S2 C64 1.860(6) . ? F4 C64 1.301(7) . ? F6 C64 1.349(7) . ? F5 C64 1.300(7) . ? Rh2 C62 1.804(6) . ? Rh2 O3 2.077(3) . ? Rh2 P5 2.3097(14) . ? Rh2 P6 2.3105(15) . ? P4 O3 1.517(3) . ? P4 C32 1.797(5) . ? P4 C44 1.809(5) . ? P4 C38 1.813(5) . ? P5 C43 1.842(5) . ? P5 C53 1.843(6) . ? P5 C50 1.855(5) . ? P6 C49 1.841(5) . ? P6 C59 1.842(5) . ? P6 C56 1.871(6) . ? C44 C45 1.385(7) . ? C44 C49 1.429(6) . ? C49 C48 1.402(7) . ? C41 C40 1.359(8) . ? C41 C42 1.385(7) . ? C41 H41 0.95 . ? C45 C46 1.391(7) . ? C45 H45 0.95 . ? C48 C47 1.380(7) . ? C48 H48 0.95 . ? C40 C39 1.389(7) . ? C40 H40 0.95 . ? C38 C39 1.387(7) . ? C38 C43 1.429(7) . ? C37 C32 1.380(7) . ? C37 C36 1.382(7) . ? C37 H37 0.95 . ? C56 C58 1.513(8) . ? C56 C57 1.532(8) . ? C56 H56 1 . ? C32 C33 1.393(7) . ? C43 C42 1.393(7) . ? C33 C34 1.376(7) . ? C33 H33 0.95 . ? C57 H57A 0.98 . ? C57 H57B 0.98 . ? C57 H57C 0.98 . ? C47 C46 1.369(7) . ? C47 H47 0.95 . ? C39 H39 0.95 . ? C35 C34 1.378(8) . ? C35 C36 1.387(8) . ? C35 H35 0.95 . ? C42 H42 0.95 . ? C46 H46 0.95 . ? C59 C61 1.519(8) . ? C59 C60 1.541(8) . ? C59 H59 1 . ? C50 C51 1.509(8) . ? C50 C52 1.539(8) . ? C50 H50 1 . ? C34 H34 0.95 . ? C51 H51A 0.98 . ? C51 H51B 0.98 . ? C51 H51C 0.98 . ? O4 C62 1.153(6) . ? C36 H36 0.95 . ? C53 C54 1.534(8) . ? C53 C55 1.539(8) . ? C53 H53 1 . ? C52 H52A 0.98 . ? C52 H52B 0.98 . ? C52 H52C 0.98 . ? C54 H54A 0.98 . ? C54 H54B 0.98 . ? C54 H54C 0.98 . ? C58 H58A 0.98 . ? C58 H58B 0.98 . ? C58 H58C 0.98 . ? C61 H61A 0.98 . ? C61 H61B 0.98 . ? C61 H61C 0.98 . ? C55 H55A 0.98 . ? C55 H55B 0.98 . ? C55 H55C 0.98 . ? C60 H60A 0.98 . ? C60 H60B 0.98 . ? C60 H60C 0.98 . ? S1 O6 1.411(5) . ? S1 O5 1.417(4) . ? S1 O7 1.442(5) . ? S1 C63 1.846(6) . ? F2 C63 1.313(7) . ? F1 C63 1.303(7) . ? F3 C63 1.327(7) . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C30 H30A 0.98 . ? C30 H30B 0.98 . ? C30 H30C 0.98 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C19 C20 1.520(8) . ? C19 C21 1.552(8) . ? C19 H19 1 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? 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 C31 Rh1 O1 178.4(2) . . ? C31 Rh1 P2 96.81(18) . . ? O1 Rh1 P2 82.20(10) . . ? C31 Rh1 P3 97.68(18) . . ? O1 Rh1 P3 83.04(10) . . ? P2 Rh1 P3 161.26(5) . . ? C18 P3 C28 106.0(3) . . ? C18 P3 C25 101.1(2) . . ? C28 P3 C25 107.5(3) . . ? C18 P3 Rh1 105.48(17) . . ? C28 P3 Rh1 121.5(2) . . ? C25 P3 Rh1 113.10(19) . . ? C12 P2 C19 102.8(2) . . ? C12 P2 C22 104.9(2) . . ? C19 P2 C22 107.4(3) . . ? C12 P2 Rh1 105.81(17) . . ? C19 P2 Rh1 112.7(2) . . ? C22 P2 Rh1 121.4(2) . . ? O1 P1 C1 109.8(2) . . ? O1 P1 C13 111.5(2) . . ? C1 P1 C13 105.7(2) . . ? O1 P1 C7 111.5(2) . . ? C1 P1 C7 105.6(2) . . ? C13 P1 C7 112.4(2) . . ? C6 C1 C2 119.4(5) . . ? C6 C1 P1 120.1(4) . . ? C2 C1 P1 120.5(4) . . ? C17 C18 C13 117.5(5) . . ? C17 C18 P3 119.9(4) . . ? C13 C18 P3 122.6(4) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C12 C11 C10 122.4(5) . . ? C12 C11 H11 118.8 . . ? C10 C11 H11 118.8 . . ? C9 C8 C7 122.0(5) . . ? C9 C8 H8 119 . . ? C7 C8 H8 119 . . ? C3 C2 C1 119.7(5) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C1 C6 C5 120.8(5) . . ? C1 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C15 C14 C13 121.6(5) . . ? C15 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? C23 C22 C24 111.6(5) . . ? C23 C22 P2 112.2(4) . . ? C24 C22 P2 109.9(4) . . ? C23 C22 H22 107.6 . . ? C24 C22 H22 107.6 . . ? P2 C22 H22 107.6 . . ? C8 C7 C12 118.9(4) . . ? C8 C7 P1 116.1(4) . . ? C12 C7 P1 124.7(4) . . ? C16 C15 C14 120.2(5) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C18 C17 C16 122.5(5) . . ? C18 C17 H17 118.7 . . ? C16 C17 H17 118.7 . . ? C29 C28 C30 111.4(5) . . ? C29 C28 P3 111.8(4) . . ? C30 C28 P3 108.9(4) . . ? C29 C28 H28 108.2 . . ? C30 C28 H28 108.2 . . ? P3 C28 H28 108.2 . . ? C2 C3 C4 120.1(5) . . ? C2 C3 H3 120 . . ? C4 C3 H3 120 . . ? C5 C4 C3 120.6(5) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C10 C9 C8 118.4(5) . . ? C10 C9 H9 120.8 . . ? C8 C9 H9 120.8 . . ? C11 C12 C7 117.6(5) . . ? C11 C12 P2 120.1(4) . . ? C7 C12 P2 122.4(4) . . ? C4 C5 C6 119.4(5) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C9 C10 C11 120.7(5) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C14 C13 C18 118.6(5) . . ? C14 C13 P1 116.4(4) . . ? C18 C13 P1 124.8(4) . . ? C15 C16 C17 119.5(5) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O2 C31 Rh1 179.7(6) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C27 C25 C26 112.0(5) . . ? C27 C25 P3 114.2(4) . . ? C26 C25 P3 112.5(4) . . ? C27 C25 H25 105.8 . . ? C26 C25 H25 105.8 . . ? P3 C25 H25 105.8 . . ? O9 S2 O10 115.7(3) . . ? O9 S2 O8 115.1(3) . . ? O10 S2 O8 113.7(3) . . ? O9 S2 C64 104.4(3) . . ? O10 S2 C64 104.8(3) . . ? O8 S2 C64 100.9(3) . . ? F5 C64 F4 109.7(5) . . ? F5 C64 F6 110.6(6) . . ? F4 C64 F6 108.9(5) . . ? F5 C64 S2 110.6(4) . . ? F4 C64 S2 110.0(5) . . ? F6 C64 S2 107.0(4) . . ? C62 Rh2 O3 178.9(2) . . ? C62 Rh2 P5 97.14(18) . . ? O3 Rh2 P5 82.63(10) . . ? C62 Rh2 P6 97.31(18) . . ? O3 Rh2 P6 83.17(10) . . ? P5 Rh2 P6 160.49(5) . . ? O3 P4 C32 109.6(2) . . ? O3 P4 C44 112.0(2) . . ? C32 P4 C44 105.2(2) . . ? O3 P4 C38 112.3(2) . . ? C32 P4 C38 105.5(2) . . ? C44 P4 C38 111.7(2) . . ? C43 P5 C53 105.5(2) . . ? C43 P5 C50 101.8(2) . . ? C53 P5 C50 106.9(3) . . ? C43 P5 Rh2 106.13(17) . . ? C53 P5 Rh2 121.1(2) . . ? C50 P5 Rh2 113.43(18) . . ? C49 P6 C59 105.7(2) . . ? C49 P6 C56 101.2(2) . . ? C59 P6 C56 107.1(3) . . ? C49 P6 Rh2 105.30(16) . . ? C59 P6 Rh2 121.11(19) . . ? C56 P6 Rh2 114.17(19) . . ? C45 C44 C49 119.1(4) . . ? C45 C44 P4 116.3(4) . . ? C49 C44 P4 124.5(4) . . ? C48 C49 C44 117.1(5) . . ? C48 C49 P6 119.8(4) . . ? C44 C49 P6 123.1(4) . . ? C40 C41 C42 120.5(5) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C44 C45 C46 121.9(5) . . ? C44 C45 H45 119.1 . . ? C46 C45 H45 119.1 . . ? C47 C48 C49 122.5(5) . . ? C47 C48 H48 118.8 . . ? C49 C48 H48 118.8 . . ? C41 C40 C39 118.9(5) . . ? C41 C40 H40 120.6 . . ? C39 C40 H40 120.6 . . ? C39 C38 C43 119.0(4) . . ? C39 C38 P4 117.1(4) . . ? C43 C38 P4 123.8(4) . . ? C32 C37 C36 121.4(5) . . ? C32 C37 H37 119.3 . . ? C36 C37 H37 119.3 . . ? C58 C56 C57 112.0(5) . . ? C58 C56 P6 114.0(4) . . ? C57 C56 P6 112.2(4) . . ? C58 C56 H56 106 . . ? C57 C56 H56 106 . . ? P6 C56 H56 106 . . ? C37 C32 C33 119.1(5) . . ? C37 C32 P4 120.8(4) . . ? C33 C32 P4 120.0(4) . . ? C42 C43 C38 116.9(5) . . ? C42 C43 P5 120.0(4) . . ? C38 C43 P5 123.0(4) . . ? C34 C33 C32 119.7(5) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C46 C47 C48 119.8(5) . . ? C46 C47 H47 120.1 . . ? C48 C47 H47 120.1 . . ? C38 C39 C40 122.2(5) . . ? C38 C39 H39 118.9 . . ? C40 C39 H39 118.9 . . ? C34 C35 C36 120.0(5) . . ? C34 C35 H35 120 . . ? C36 C35 H35 120 . . ? C41 C42 C43 122.4(5) . . ? C41 C42 H42 118.8 . . ? C43 C42 H42 118.8 . . ? C47 C46 C45 119.5(5) . . ? C47 C46 H46 120.2 . . ? C45 C46 H46 120.2 . . ? C61 C59 C60 110.0(5) . . ? C61 C59 P6 110.4(4) . . ? C60 C59 P6 111.3(4) . . ? C61 C59 H59 108.4 . . ? C60 C59 H59 108.4 . . ? P6 C59 H59 108.4 . . ? C51 C50 C52 111.3(5) . . ? C51 C50 P5 115.0(4) . . ? C52 C50 P5 111.9(4) . . ? C51 C50 H50 106 . . ? C52 C50 H50 106 . . ? P5 C50 H50 106 . . ? C33 C34 C35 120.8(5) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C37 C36 C35 119.0(5) . . ? C37 C36 H36 120.5 . . ? C35 C36 H36 120.5 . . ? C54 C53 C55 109.9(5) . . ? C54 C53 P5 112.2(4) . . ? C55 C53 P5 110.7(4) . . ? C54 C53 H53 108 . . ? C55 C53 H53 108 . . ? P5 C53 H53 108 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 C58 H58A 109.5 . . ? C56 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C56 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C59 C61 H61A 109.5 . . ? C59 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C59 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O4 C62 Rh2 178.9(6) . . ? O6 S1 O5 115.2(3) . . ? O6 S1 O7 114.2(4) . . ? O5 S1 O7 114.6(3) . . ? O6 S1 C63 104.3(3) . . ? O5 S1 C63 104.4(3) . . ? O7 S1 C63 102.2(3) . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? P4 O3 Rh2 110.65(17) . . ? P1 O1 Rh1 110.05(18) . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? F1 C63 F2 108.3(6) . . ? F1 C63 F3 109.4(6) . . ? F2 C63 F3 111.0(6) . . ? F1 C63 S1 110.5(5) . . ? F2 C63 S1 109.8(4) . . ? F3 C63 S1 107.9(4) . . ? C20 C19 C21 110.7(5) . . ? C20 C19 P2 116.0(5) . . ? C21 C19 P2 112.2(4) . . ? C20 C19 H19 105.7 . . ? C21 C19 H19 105.7 . . ? P2 C19 H19 105.7 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? #===END