# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1327 #======================================================== # Coordination and Conformational Isomerism in Bis(tricyclohexylphosphine) # gold(I) halide complexes, [Au(PCy3)2]X. # # Graham A. Bowmaker, Christopher L. Brown, Robert D. Hart, Peter C. Healy # Clifton E. F. Rickard and Allan H. White # # submitted to: J. Chem. Soc. Dalton Transactions, November 1998 # # # CIF files for the crystal structures described in the paper: # # 1. [Au(PCy3)2]Cl - cy2aucl # 2. alpha [Au(PCy3)2Br] - cy2aubra # 3. beta [Au(PCy3)2Br] - cy2aubrb # 4. gamma [Au(PCy3)2Br] - cy2aubrc # 5. [Au(PCy3)2I].PCy3 - cy3aui # 6. [Au(PCy3)2I]- cy2aui # #======================================================= data_cy2aucl _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(tricyclohexylphosphine)gold(I)chloride ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H66 Au Cl P2' _chemical_formula_weight 793.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.45660(10) _cell_length_b 17.3328(3) _cell_length_c 11.5786(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.9340(10) _cell_angle_gamma 90.00 _cell_volume 1805.63(5) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 6817 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description 'Irregular fragment' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 4.259 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2343 _exptl_absorpt_correction_T_max 0.4408 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'Siemens SMART' _diffrn_measurement_method 'Area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10569 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 28.21 _reflns_number_total 4077 _reflns_number_gt 3188 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+1.7351P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4077 _refine_ls_number_parameters 184 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0703 _refine_ls_wR_factor_gt 0.0649 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.119 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au Au 0.5000 0.5000 0.5000 0.02015(6) Uani 1 d S . . P1 P 0.53141(8) 0.49848(4) 0.70659(7) 0.01775(15) Uani 1 d . . . Cl Cl 0.0000 0.5000 0.0000 0.0353(3) Uani 1 d S . . C21 C 0.6603(3) 0.57342(17) 0.7930(3) 0.0204(6) Uani 1 d . . . H211 H 0.7599 0.5493 0.8216 0.024 Uiso 1 calc R . . C22 C 0.6727(4) 0.64166(19) 0.7119(3) 0.0280(7) Uani 1 d . . . H221 H 0.5757 0.6668 0.6798 0.034 Uiso 1 calc R . . H222 H 0.7025 0.6227 0.6430 0.034 Uiso 1 calc R . . C23 C 0.7882(4) 0.7007(2) 0.7848(4) 0.0362(8) Uani 1 d . . . H231 H 0.8868 0.6767 0.8110 0.043 Uiso 1 calc R . . H232 H 0.7920 0.7447 0.7326 0.043 Uiso 1 calc R . . C24 C 0.7485(4) 0.7290(2) 0.8954(4) 0.0383(9) Uani 1 d . . . H242 H 0.8243 0.7655 0.9412 0.046 Uiso 1 calc R . . H241 H 0.6529 0.7561 0.8690 0.046 Uiso 1 calc R . . C25 C 0.7388(4) 0.6614(2) 0.9765(3) 0.0321(8) Uani 1 d . . . H252 H 0.7108 0.6804 1.0461 0.039 Uiso 1 calc R . . H251 H 0.8365 0.6367 1.0074 0.039 Uiso 1 calc R . . C26 C 0.6244(4) 0.60184(19) 0.9072(3) 0.0265(7) Uani 1 d . . . H261 H 0.5251 0.6250 0.8832 0.032 Uiso 1 calc R . . H262 H 0.6242 0.5579 0.9603 0.032 Uiso 1 calc R . . C31 C 0.6046(3) 0.40369(18) 0.7691(3) 0.0211(6) Uani 1 d . . . H311 H 0.5314 0.3646 0.7254 0.025 Uiso 1 calc R . . C32 C 0.6235(4) 0.39392(19) 0.9041(3) 0.0262(7) Uani 1 d . . . H322 H 0.5290 0.4049 0.9191 0.031 Uiso 1 calc R . . H321 H 0.6976 0.4308 0.9510 0.031 Uiso 1 calc R . . C33 C 0.6734(4) 0.3118(2) 0.9456(3) 0.0343(8) Uani 1 d . . . H331 H 0.5966 0.2751 0.9023 0.041 Uiso 1 calc R . . H332 H 0.6869 0.3069 1.0327 0.041 Uiso 1 calc R . . C34 C 0.8201(4) 0.2929(2) 0.9207(4) 0.0360(8) Uani 1 d . . . H341 H 0.8989 0.3268 0.9694 0.043 Uiso 1 calc R . . H342 H 0.8485 0.2395 0.9445 0.043 Uiso 1 calc R . . C35 C 0.8038(4) 0.30348(19) 0.7871(4) 0.0334(8) Uani 1 d . . . H351 H 0.7315 0.2661 0.7392 0.040 Uiso 1 calc R . . H352 H 0.8995 0.2932 0.7737 0.040 Uiso 1 calc R . . C36 C 0.7528(3) 0.38499(19) 0.7439(3) 0.0276(7) Uani 1 d . . . H362 H 0.7388 0.3893 0.6567 0.033 Uiso 1 calc R . . H361 H 0.8290 0.4222 0.7863 0.033 Uiso 1 calc R . . C11 C 0.3520(3) 0.50927(16) 0.7367(3) 0.0208(6) Uani 1 d . . . H111 H 0.3723 0.5119 0.8258 0.025 Uiso 1 calc R . . C12 C 0.2496(3) 0.43972(19) 0.6892(3) 0.0291(7) Uani 1 d . . . H121 H 0.2296 0.4352 0.6013 0.035 Uiso 1 calc R . . H122 H 0.2994 0.3924 0.7271 0.035 Uiso 1 calc R . . C13 C 0.1032(4) 0.4487(2) 0.7174(4) 0.0361(9) Uani 1 d . . . H131 H 0.0372 0.4060 0.6797 0.043 Uiso 1 calc R . . H132 H 0.1227 0.4450 0.8054 0.043 Uiso 1 calc R . . C14 C 0.0243(4) 0.5244(2) 0.6731(4) 0.0330(8) Uani 1 d . . . H142 H -0.0613 0.5297 0.7034 0.040 Uiso 1 calc R . . H141 H -0.0126 0.5244 0.5842 0.040 Uiso 1 calc R . . C15 C 0.1286(4) 0.5927(2) 0.7166(4) 0.0317(8) Uani 1 d . . . H151 H 0.1539 0.5971 0.8050 0.038 Uiso 1 calc R . . H152 H 0.0781 0.6403 0.6805 0.038 Uiso 1 calc R . . C16 C 0.2710(3) 0.58324(19) 0.6819(3) 0.0281(7) Uani 1 d . . . H162 H 0.3361 0.6277 0.7113 0.034 Uiso 1 calc R . . H161 H 0.2464 0.5814 0.5933 0.034 Uiso 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 Au 0.01901(9) 0.02498(10) 0.01617(9) 0.00000(7) 0.00500(6) 0.00063(7) P1 0.0162(3) 0.0214(4) 0.0158(3) -0.0002(3) 0.0051(3) 0.0007(3) Cl 0.0274(5) 0.0345(6) 0.0347(6) -0.0063(5) -0.0042(5) 0.0044(5) C21 0.0175(13) 0.0235(15) 0.0192(15) -0.0017(12) 0.0043(12) -0.0018(11) C22 0.0282(16) 0.0278(16) 0.0271(17) 0.0048(14) 0.0072(14) -0.0018(14) C23 0.0387(19) 0.0282(17) 0.038(2) 0.0059(16) 0.0066(17) -0.0103(15) C24 0.041(2) 0.0235(17) 0.046(2) -0.0062(16) 0.0076(18) -0.0043(15) C25 0.0358(18) 0.0293(17) 0.0298(18) -0.0083(15) 0.0080(15) -0.0047(15) C26 0.0312(16) 0.0267(16) 0.0235(16) -0.0048(13) 0.0115(14) -0.0001(13) C31 0.0184(13) 0.0229(15) 0.0223(15) -0.0002(12) 0.0065(12) 0.0002(12) C32 0.0280(16) 0.0286(16) 0.0227(16) 0.0043(13) 0.0086(13) 0.0045(13) C33 0.0388(19) 0.0311(18) 0.0316(19) 0.0090(15) 0.0088(16) 0.0004(15) C34 0.0323(18) 0.0261(17) 0.044(2) 0.0034(16) 0.0040(17) 0.0061(14) C35 0.0334(17) 0.0261(17) 0.044(2) -0.0002(16) 0.0161(17) 0.0086(15) C36 0.0250(16) 0.0284(17) 0.0322(18) 0.0037(14) 0.0127(15) 0.0053(13) C11 0.0166(13) 0.0253(16) 0.0203(14) 0.0004(12) 0.0055(11) 0.0007(11) C12 0.0192(14) 0.0282(17) 0.040(2) -0.0034(15) 0.0098(14) -0.0013(13) C13 0.0228(16) 0.0327(19) 0.056(2) -0.0027(18) 0.0175(17) -0.0018(14) C14 0.0188(15) 0.0412(18) 0.040(2) -0.0011(17) 0.0096(15) 0.0030(14) C15 0.0252(16) 0.0318(18) 0.042(2) 0.0024(16) 0.0155(15) 0.0069(14) C16 0.0222(15) 0.0282(16) 0.0369(19) 0.0071(14) 0.0134(14) 0.0040(13) _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 Au P 2.3180(8) 3_666 ? Au P 2.3180(8) . ? P C31 1.842(3) . ? P C11 1.844(3) . ? P C21 1.850(3) . ? C21 C22 1.537(4) . ? C21 C26 1.543(4) . ? C22 C23 1.544(5) . ? C23 C24 1.523(6) . ? C24 C25 1.523(5) . ? C25 C26 1.531(4) . ? C31 C32 1.526(4) . ? C31 C36 1.551(4) . ? C32 C33 1.530(4) . ? C33 C34 1.537(5) . ? C34 C35 1.518(5) . ? C35 C36 1.527(4) . ? C11 C16 1.528(4) . ? C11 C12 1.538(4) . ? C12 C13 1.525(4) . ? C13 C14 1.520(5) . ? C14 C15 1.523(5) . ? C15 C16 1.527(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 P Au P 180.0 3_666 . ? C31 P C11 105.81(13) . . ? C31 P C21 107.96(14) . . ? C11 P C21 108.53(14) . . ? C31 P Au 109.21(10) . . ? C11 P Au 111.17(11) . . ? C21 P Au 113.82(10) . . ? C22 C21 C26 110.9(3) . . ? C22 C21 P 111.8(2) . . ? C26 C21 P 113.9(2) . . ? C21 C22 C23 110.5(3) . . ? C24 C13 C22 110.9(3) . . ? C25 C24 C23 110.3(3) . . ? C24 C25 C26 111.3(3) . . ? C25 C26 C21 111.0(3) . . ? C32 C31 C36 110.0(3) . . ? C32 C31 P 114.4(2) . . ? C36 C31 P 111.4(2) . . ? C31 C32 C33 110.7(3) . . ? C32 C33 C34 110.4(3) . . ? C35 C34 C33 110.6(3) . . ? C34 C35 C36 111.6(3) . . ? C35 C36 C31 110.2(3) . . ? C16 C11 C12 109.2(3) . . ? C16 C11 P 112.3(2) . . ? C12 C11 P 111.6(2) . . ? C13 C12 C11 110.9(3) . . ? C14 C13 C12 113.5(3) . . ? C13 C14 C15 111.0(3) . . ? C14 C15 C16 111.3(3) . . ? C15 C16 C11 110.5(3) . . ? _diffrn_measured_fraction_theta_max 0.885 _diffrn_reflns_theta_full 28.21 _diffrn_measured_fraction_theta_full 0.885 _refine_diff_density_max 2.161 _refine_diff_density_min -2.119 _refine_diff_density_rms 0.104 #=======================================================END data_cy2aubra _audit_creation_date 97-11-21 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source dmf_solution _chemical_name_systematic ; bis(tricyclohexylphosphine)gold(I)bromide ; _chemical_name_common ? _chemical_formula_analytical [((C6H11)3P)2AuBr] _chemical_formula_moiety ? _chemical_formula_structural [(Cy3P)2AuBr] _chemical_formula_sum C36_H66_Au_Br_P2 _chemical_formula_weight 837.74 _chemical_melting_point 194-197C _computing_data_collection 'Enraf_Nonius Cad4 software' _computing_cell_refinement 'Enraf_Nonius Cad4 software' _computing_data_reduction xtal_DIFDAT_SORTRF_ADDREF_ABSORB _computing_structure_solution xtal _computing_structure_refinement xtal_CRYLSQ _computing_molecular_graphics xtal _computing_publication_material xtal_BONDLA_CIFIO _cell_length_a 11.600(4) _cell_length_b 17.913(12) _cell_length_c 18.000(16) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 3740(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _cell_measurement_reflns_used 8 _cell_measurement_theta_min 19.5 _cell_measurement_theta_max 19.5 _cell_special_details ; ? ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M C_c_m_21 _symmetry_space_group_name_Hall C_21_-2c loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,1/2+z -x,+y,1/2+z +x,-y,+z 1/2+x,1/2+y,+z 1/2-x,1/2-y,1/2+z 1/2-x,1/2+y,1/2+z 1/2+x,1/2-y,+z _exptl_crystal_description plate _exptl_crystal_preparation ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.23 _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1704 _exptl_absorpt_process_details ? _exptl_absorpt_coefficient_mu 5.1 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.23 _exptl_absorpt_correction_T_max 0.39 _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type xray_tube _diffrn_radiation_source ? _diffrn_radiation_monochromator graphite _diffrn_radiation_detector scintialltion_counter _diffrn_measurement_device CAD4 _diffrn_measurement_method 2theta/theta _diffrn_standards_number 8 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 1hour _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 6 10 10 6 -10 10 6 10 -10 -6 10 10 -6 -10 -10 -8 10 -10 -6 -10 10 6 -10 -10 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale 1 13.54 _diffrn_reflns_number 2901 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_sigmaI/netI 0 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 29.97 _diffrn_reflns_reduction_process equatorial_monochr_Lp loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 144 .002 .002 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 264 0 0 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 Au ? 0 4 -2.688 8.798 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 Br ? 0 4 -.374 2.456 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 P ? 0 8 .09 .095 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Au .83900(4) .50000 .50000 .0479(3) Uani ? ? Br .79361(15) .50000 .70706(12) .0826(13) Uani ? ? P1 .6411(2) .50000 .52118(18) .040(2) Uani ? ? P2 1.0341(3) .50000 .4756(2) .049(2) Uani ? ? C111 .5675(10) .50000 .4310(9) .047(8) Uani ? ? C112 .5918(11) .5704(8) .3855(7) .066(8) Uani ? ? C113 .5195(13) .5693(8) .3145(7) .089(10) Uani ? ? C114 .5461(16) .50000 .2678(11) .085(14) Uani ? ? C121 .5905(9) .4189(6) .5743(6) .047(6) Uani ? ? C122 .4640(8) .3959(6) .5620(6) .055(6) Uani ? ? C123 .4282(10) .3329(7) .6128(7) .069(8) Uani ? ? C124 .5064(14) .2669(5) .6047(10) .086(8) Uani ? ? C125 .6287(11) .2888(7) .6201(11) .104(11) Uani ? ? C126 .6698(9) .3514(6) .5698(7) .066(7) Uani ? ? C211 1.1156(10) .50000 .5635(7) .037(7) Uani ? ? C212 1.0903(12) .4309(6) .6102(7) .054(8) Uani ? ? C213 1.1504(10) .4314(7) .6841(7) .066(7) Uani ? ? C214 1.1243(12) .50000 .7276(8) .059(9) Uani ? ? C221 1.0773(12) .5847(13) .4253(10) .122(14) Uani ? ? C222 1.2029(9) .6022(7) .4217(8) .061(7) Uani ? ? C223 1.2327(14) .6686(12) .3776(12) .153(16) Uani ? ? C224 1.1543(15) .7109(8) .3454(15) .138(16) Uani ? ? C225 1.0326(12) .6908(8) .3429(9) .095(10) Uani ? ? C226 .9987(13) .6228(7) .3860(12) .115(12) Uani ? ? H111 .48544 .50038 .44276 .05120 Uiso ? ? H112a .57571 .61242 .41415 .08300 Uiso ? ? H112b .67251 .56909 .37320 .08300 Uiso ? ? H113a .43971 .56789 .32722 .10400 Uiso ? ? H113b .53547 .61169 .28576 .10400 Uiso ? ? H114a .49823 .50000 .22530 .11100 Uiso ? ? H114b .62444 .50000 .25378 .11100 Uiso ? ? H121 .59428 .43726 .62395 .05550 Uiso ? ? H122a .41631 .43809 .57170 .06700 Uiso ? ? H122b .45481 .38084 .51199 .06700 Uiso ? ? H123a .42954 .34946 .66271 .08300 Uiso ? ? H123b .35178 .31777 .60009 .08300 Uiso ? ? H124a .48592 .22983 .63916 .10200 Uiso ? ? H124b .50076 .24799 .55543 .10200 Uiso ? ? H125a .63617 .30336 .66843 .12700 Uiso ? ? H125b .67619 .24647 .60879 .12700 Uiso ? ? H126a .74425 .36586 .58506 .08130 Uiso ? ? H126b .67138 .33491 .51968 .08130 Uiso ? ? H211 1.19326 .50024 .54931 .05030 Uiso ? ? H212a 1.01081 .42612 .61732 .06250 Uiso ? ? H212b 1.11829 .38808 .58273 .06250 Uiso ? ? H213a 1.12463 .38885 .71153 .08250 Uiso ? ? H213b 1.23084 .42806 .67660 .08250 Uiso ? ? H214a 1.04433 .50000 .74005 .07450 Uiso ? ? H214b 1.16817 .50000 .77254 .07450 Uiso ? ? H221 1.05375 .62656 .46170 .15300 Uiso ? ? H222a 1.23212 .60894 .46989 .05780 Uiso ? ? H222b 1.23652 .55939 .39926 .05780 Uiso ? ? H223a 1.27400 .70002 .40789 .18800 Uiso ? ? H223b 1.27919 .65038 .33734 .18800 Uiso ? ? H224a 1.15723 .75717 .36837 .16200 Uiso ? ? H224b 1.17515 .71471 .29415 .16200 Uiso ? ? H225a .99130 .73133 .36423 .11500 Uiso ? ? H225b 1.01098 .68406 .29314 .11500 Uiso ? ? H226a .93687 .63575 .41522 .13600 Uiso ? ? H226b .97638 .58719 .34855 .13600 Uiso ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au .02105(17) .0678(3) .0550(3) .00000 .0044(4) .00000 Br .0474(9) .1254(17) .0750(13) .00000 -.0232(9) .00000 P1 .0234(14) .0528(17) .042(3) .00000 -.0010(12) .00000 P2 .0213(16) .079(3) .046(2) .00000 .0010(14) .00000 C111 .020(6) .069(10) .053(9) .00000 .002(6) .00000 C112 .066(8) .075(9) .057(8) -.008(7) .005(7) .015(7) C113 .086(10) .122(11) .059(8) .011(9) -.009(8) .030(8) C114 .060(12) .127(16) .068(14) .00000 -.015(10) .00000 C121 .041(5) .060(6) .040(6) -.001(5) -.006(5) .007(5) C122 .042(5) .051(6) .073(7) -.009(4) .003(5) .002(5) C123 .059(7) .067(7) .082(8) -.007(6) .015(6) .006(7) C124 .076(8) .049(6) .132(11) -.006(7) .021(8) .006(8) C125 .060(8) .056(7) .196(18) .018(6) .013(10) .045(10) C126 .044(6) .062(7) .093(8) .013(5) .004(6) .002(6) C211 .026(5) .049(8) .036(7) .00000 .009(5) .00000 C212 .060(9) .049(6) .052(8) -.003(6) .003(6) -.002(6) C213 .059(7) .080(8) .061(7) .019(6) .006(6) .020(6) C214 .032(7) .100(12) .045(9) .00000 .008(6) .00000 C221 .030(6) .22(2) .110(13) -.016(10) -.010(8) .123(15) C222 .038(5) .062(7) .083(8) .003(5) .009(6) -.002(7) C223 .066(9) .21(2) .19(2) -.030(11) .015(11) .146(18) C224 .104(13) .062(9) .25(3) .001(8) -.005(18) .044(13) C225 .075(9) .113(11) .097(11) .018(8) -.015(9) .016(9) C226 .064(8) .059(7) .22(2) -.004(7) -.023(11) .031(10) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details sfls:_F____sigma_weight______full_matrix _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 2061(290) _refine_ls_extinction_expression Eq22_p292_"Cryst._Comp."_Munksgaard_1970 _refine_ls_abs_structure_details 'same R for both chiralities' _refine_ls_abs_structure_Flack 0 _refine_ls_number_reflns 2062 _refine_ls_number_parameters 193 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .058 _refine_ls_R_factor_obs .041 _refine_ls_wR_factor_all .044 _refine_ls_wR_factor_obs .041 _refine_ls_goodness_of_fit_all 1.603 _refine_ls_goodness_of_fit_obs 1.793 _refine_ls_shift/esd_max .091 _refine_ls_shift/esd_mean .002 _refine_diff_density_min -3.018 _refine_diff_density_max 1.396 _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au P1 2.328(3) . . ? Au P2 2.305(3) . . ? P1 C111 1.834(15) . . ? P1 C121 1.835(11) . . ? P1 C121 1.835(11) . 4_565 ? P2 C211 1.844(13) . . ? P2 C221 1.84(2) . . ? P2 C221 1.84(2) . 4_565 ? C111 C112 1.529(16) . . ? C111 H111 .976(12) . . ? C111 C112 1.529(16) . 4_565 ? C112 C113 1.528(19) . . ? C112 H112a .931(13) . . ? C112 H112b .963(13) . . ? C113 C114 1.531(18) . . ? C113 H113a .954(15) . . ? C113 H113b .938(14) . . ? C114 H114a .94(2) . . ? C114 H114b .94(2) . . ? C121 C122 1.539(14) . . ? C121 C126 1.523(15) . . ? C121 H121 .954(10) . . ? C122 C123 1.511(16) . . ? C122 H122a .953(10) . . ? C122 H122b .945(11) . . ? C123 C124 1.498(17) . . ? C123 H123a .946(13) . . ? C123 H123b .955(12) . . ? C124 C125 1.50(2) . . ? C124 H124a .939(14) . . ? C124 H124b .952(17) . . ? C125 C126 1.52(2) . . ? C125 H125a .91(2) . . ? C125 H125b .958(13) . . ? C126 H126a .942(11) . . ? C126 H126b .948(13) . . ? C211 C212 1.525(14) . . ? C211 H211 .936(12) . . ? C211 C212 1.525(14) . 4_565 ? C212 C213 1.502(18) . . ? C212 H212a .934(14) . . ? C212 H212b .969(12) . . ? C213 C214 1.488(15) . . ? C213 H213a .955(12) . . ? C213 H213b .945(11) . . ? C214 H214a .954(14) . . ? C214 H214b .956(15) . . ? C221 C222 1.492(18) . . ? C221 C226 1.34(2) . . ? C221 H221 1.03(2) . . ? C222 C223 1.47(2) . . ? C222 H222a .938(13) . . ? C222 H222b .950(12) . . ? C223 C224 1.32(3) . . ? C223 H223a .92(2) . . ? C223 H223b .96(2) . . ? C224 C225 1.46(2) . . ? C224 H224a .926(18) . . ? C224 H224b .96(3) . . ? C225 C226 1.50(2) . . ? C225 H225a .951(15) . . ? C225 H225b .937(16) . . ? C226 H226a .919(17) . . ? C226 H226b .964(17) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au P2 178.44(13) . . . ? Au P1 C111 108.3(4) . . . ? Au P1 C121 113.6(3) . . . ? Au P1 C121 113.6(3) . . 4_565 ? C111 P1 C121 108.2(4) . . . ? C111 P1 C121 108.2(4) . . 4_565 ? C121 P1 C121 104.7(5) . . 4_565 ? Au P2 C211 109.9(4) . . . ? Au P2 C221 111.2(5) . . . ? Au P2 C221 111.2(5) . . 4_565 ? C211 P2 C221 106.4(6) . . . ? C211 P2 C221 106.4(6) . . 4_565 ? C221 P2 C221 111.4(9) . . 4_565 ? P1 C111 C112 112.8(7) . . . ? P1 C111 H111 105.1(12) . . . ? P1 C111 C112 112.8(7) . . 4_565 ? C112 C111 H111 106.9(8) . . . ? C112 C111 C112 111.1(12) . . 4_565 ? H111 C111 C112 107.6(8) . . 4_565 ? C111 C112 C113 109.6(11) . . . ? C111 C112 H112a 109.5(11) . . . ? C111 C112 H112b 106.4(11) . . . ? C113 C112 H112a 111.3(12) . . . ? C113 C112 H112b 109.9(11) . . . ? H112a C112 H112b 110.0(13) . . . ? C112 C113 C114 111.1(12) . . . ? C112 C113 H113a 109.4(12) . . . ? C112 C113 H113b 110.0(13) . . . ? C114 C113 H113a 107.9(14) . . . ? C114 C113 H113b 108.2(12) . . . ? H113a C113 H113b 110.2(15) . . . ? C113 C114 H114a 109.0(11) . . . ? C113 C114 H114b 110.0(11) . . . ? C113 C114 C113 108.3(14) . . 4_565 ? H114a C114 H114b 111(2) . . . ? H114a C114 C113 109.0(11) . . 4_565 ? H114b C114 C113 110.0(11) . . 4_565 ? P1 C121 C122 116.2(7) . . . ? P1 C121 C126 114.1(7) . . . ? P1 C121 H121 101.6(8) . . . ? C122 C121 C126 110.9(9) . . . ? C122 C121 H121 105.7(9) . . . ? C126 C121 H121 107.2(9) . . . ? C121 C122 C123 112.0(9) . . . ? C121 C122 H122a 108.4(9) . . . ? C121 C122 H122b 108.7(9) . . . ? C123 C122 H122a 108.7(10) . . . ? C123 C122 H122b 109.4(10) . . . ? H122a C122 H122b 109.6(10) . . . ? C122 C123 C124 111.4(11) . . . ? C122 C123 H123a 109.7(10) . . . ? C122 C123 H123b 108.8(11) . . . ? C124 C123 H123a 109.2(12) . . . ? C124 C123 H123b 108.3(11) . . . ? H123a C123 H123b 109.4(12) . . . ? C123 C124 C125 110.4(10) . . . ? C123 C124 H124a 109.9(15) . . . ? C123 C124 H124b 109.3(14) . . . ? C125 C124 H124a 107.6(15) . . . ? C125 C124 H124b 109.3(15) . . . ? H124a C124 H124b 110.3(11) . . . ? C124 C125 C126 112.4(13) . . . ? C124 C125 H125a 109.9(15) . . . ? C124 C125 H125b 107.4(12) . . . ? C126 C125 H125a 109.1(12) . . . ? C126 C125 H125b 106.1(14) . . . ? H125a C125 H125b 112.0(16) . . . ? C121 C126 C125 111.4(10) . . . ? C121 C126 H126a 108.6(10) . . . ? C121 C126 H126b 108.0(10) . . . ? C125 C126 H126a 108.5(11) . . . ? C125 C126 H126b 110.1(11) . . . ? H126a C126 H126b 110.3(11) . . . ? P2 C211 C212 112.0(7) . . . ? P2 C211 H211 105.0(10) . . . ? P2 C211 C212 112.0(7) . . 4_565 ? C212 C211 H211 109.9(8) . . . ? C212 C211 C212 108.5(10) . . 4_565 ? H211 C211 C212 109.4(8) . . 4_565 ? C211 C212 C213 113.2(10) . . . ? C211 C212 H212a 109.9(11) . . . ? C211 C212 H212b 107.2(11) . . . ? C213 C212 H212a 109.7(12) . . . ? C213 C212 H212b 107.5(11) . . . ? H212a C212 H212b 109.1(12) . . . ? C212 C213 C214 112.1(10) . . . ? C212 C213 H213a 107.9(11) . . . ? C212 C213 H213b 109.3(11) . . . ? C214 C213 H213a 108.9(11) . . . ? C214 C213 H213b 109.2(11) . . . ? H213a C213 H213b 109.4(12) . . . ? C213 C214 H214a 108.7(9) . . . ? C213 C214 H214b 109.7(8) . . . ? C213 C214 C213 111.4(12) . . 4_565 ? H214a C214 H214b 108.6(15) . . . ? H214a C214 C213 108.7(9) . . 4_565 ? H214b C214 C213 109.7(8) . . 4_565 ? P2 C221 C222 117.4(12) . . . ? P2 C221 C226 119.7(12) . . . ? P2 C221 H221 102.4(13) . . . ? C222 C221 C226 122.3(17) . . . ? C222 C221 H221 97.7(14) . . . ? C226 C221 H221 77.6(14) . . . ? C221 C222 C223 114.9(13) . . . ? C221 C222 H222a 109.9(12) . . . ? C221 C222 H222b 104.5(12) . . . ? C223 C222 H222a 108.0(12) . . . ? C223 C222 H222b 109.0(13) . . . ? H222a C222 H222b 110.5(12) . . . ? C222 C223 C224 122.7(15) . . . ? C222 C223 H223a 107.3(18) . . . ? C222 C223 H223b 105.3(17) . . . ? C224 C223 H223a 106(2) . . . ? C224 C223 H223b 105(2) . . . ? H223a C223 H223b 111.3(16) . . . ? C223 C224 C225 122.7(16) . . . ? C223 C224 H224a 107(2) . . . ? C223 C224 H224b 106.8(17) . . . ? C225 C224 H224a 105.8(16) . . . ? C225 C224 H224b 103.4(19) . . . ? H224a C224 H224b 110.9(18) . . . ? C224 C225 C226 116.1(14) . . . ? C224 C225 H225a 106.7(14) . . . ? C224 C225 H225b 108.8(16) . . . ? C226 C225 H225a 106.2(14) . . . ? C226 C225 H225b 108.7(14) . . . ? H225a C225 H225b 110.4(15) . . . ? C221 C226 C225 120.6(14) . . . ? C221 C226 H226a 111(2) . . . ? C221 C226 H226b 102.3(14) . . . ? C225 C226 H226a 107.3(12) . . . ? C225 C226 H226b 104.3(17) . . . ? H226a C226 H226b 110.9(15) . . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _reflns_number_total 2901 _reflns_number_observed 2063 _reflns_observed_criterion refl_observed_if_F____>_.000_sigma(F___) _reflns_d_resolution_high .711 _reflns_d_resolution_low 9.737 #=======================================================END data_cy2aubrb _audit_creation_method SHELXL-97 _chemical_name_systematic ; bromobis(tricyclohexylphosphine)gold(I) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H66 Au Br P2' _chemical_formula_weight 837.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P c a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 17.1299(3) _cell_length_b 17.54580(10) _cell_length_c 24.7345(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7434.15(18) _cell_formula_units_Z 8 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 8196 _cell_measurement_theta_min 1 _cell_measurement_theta_max 26 _exptl_crystal_description Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3408 _exptl_absorpt_coefficient_mu 5.141 _exptl_absorpt_correction_type 'Multi-scan (Blessing, 1995)' _exptl_absorpt_correction_T_min 0.2270 _exptl_absorpt_correction_T_max 0.4934 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'Siemens SMART' _diffrn_measurement_method 'Area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 43203 _diffrn_reflns_av_R_equivalents 0.0758 _diffrn_reflns_av_sigmaI/netI 0.0878 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12972 _reflns_number_gt 10052 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS Sheldrick, (1990)' _computing_structure_refinement 'SHELXL-93 Sheldrick, (1993)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL-93' _refine_special_details ; The structure could not be solved in Pbcm but solved and refined satisfactorally in Pca2~1~. One cyclohexyl group, C54 to C58, shows evidence of disorder and has high thermal parameters. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 12972 _refine_ls_number_parameters 721 _refine_ls_number_restraints 109 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1192 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.060 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.31614(2) 0.46362(2) 0.009368(16) 0.02468(9) Uani 1 d . . . Br1 Br 0.45374(7) 0.55790(7) 0.02088(5) 0.0443(3) Uani 1 d . . . P1 P 0.32602(15) 0.43359(16) -0.08160(11) 0.0249(6) Uani 1 d . . . P2 P 0.26706(15) 0.48010(16) 0.09564(11) 0.0235(6) Uani 1 d . . . C131 C 0.3360(7) 0.5208(8) -0.1230(5) 0.039(3) Uani 1 d . . . H131 H 0.3917 0.5353 -0.1202 0.047 Uiso 1 calc R . . C132 C 0.3195(7) 0.5132(8) -0.1845(5) 0.036(3) Uani 1 d . . . H132A H 0.3525 0.4730 -0.1997 0.043 Uiso 1 calc R . . H132B H 0.2649 0.4986 -0.1900 0.043 Uiso 1 calc R . . C133 C 0.3354(7) 0.5871(7) -0.2136(5) 0.038(3) Uani 1 d . . . H133A H 0.3223 0.5812 -0.2520 0.046 Uiso 1 calc R . . H133B H 0.3912 0.5991 -0.2111 0.046 Uiso 1 calc R . . C134 C 0.2881(7) 0.6526(8) -0.1898(5) 0.050(4) Uani 1 d . . . H134A H 0.3013 0.6999 -0.2089 0.060 Uiso 1 calc R . . H134B H 0.2324 0.6427 -0.1953 0.060 Uiso 1 calc R . . C135 C 0.3041(8) 0.6626(7) -0.1302(5) 0.049(3) Uani 1 d . . . H135A H 0.2702 0.7028 -0.1159 0.058 Uiso 1 calc R . . H135B H 0.3584 0.6787 -0.1252 0.058 Uiso 1 calc R . . C136 C 0.2900(7) 0.5889(7) -0.0987(5) 0.039(3) Uani 1 d . . . H136A H 0.2341 0.5770 -0.0990 0.047 Uiso 1 calc R . . H136B H 0.3058 0.5963 -0.0610 0.047 Uiso 1 calc R . . C111 C 0.2411(6) 0.3801(6) -0.1057(4) 0.029(2) Uani 1 d . . . H111 H 0.2460 0.3729 -0.1453 0.035 Uiso 1 calc R . . C112 C 0.2392(7) 0.3010(7) -0.0785(5) 0.042(3) Uani 1 d . . . H112A H 0.2429 0.3075 -0.0392 0.051 Uiso 1 calc R . . H112B H 0.2847 0.2716 -0.0904 0.051 Uiso 1 calc R . . C113 C 0.1632(7) 0.2551(7) -0.0921(6) 0.050(3) Uani 1 d . . . H113A H 0.1635 0.2409 -0.1304 0.060 Uiso 1 calc R . . H113B H 0.1620 0.2081 -0.0707 0.060 Uiso 1 calc R . . C114 C 0.0898(7) 0.3027(7) -0.0799(5) 0.044(3) Uani 1 d . . . H114A H 0.0435 0.2746 -0.0920 0.053 Uiso 1 calc R . . H114B H 0.0855 0.3102 -0.0408 0.053 Uiso 1 calc R . . C115 C 0.0918(6) 0.3787(8) -0.1073(5) 0.046(3) Uani 1 d . . . H115A H 0.0459 0.4082 -0.0962 0.055 Uiso 1 calc R . . H115B H 0.0887 0.3711 -0.1465 0.055 Uiso 1 calc R . . C116 C 0.1648(7) 0.4239(7) -0.0942(5) 0.040(3) Uani 1 d . . . H116A H 0.1636 0.4381 -0.0559 0.048 Uiso 1 calc R . . H116B H 0.1646 0.4710 -0.1154 0.048 Uiso 1 calc R . . C121 C 0.4116(6) 0.3712(6) -0.0977(4) 0.028(2) Uani 1 d . . . H121 H 0.4038 0.3249 -0.0754 0.034 Uiso 1 calc R . . C122 C 0.4181(8) 0.3424(8) -0.1544(5) 0.050(4) Uani 1 d . . . H122A H 0.4268 0.3853 -0.1790 0.060 Uiso 1 calc R . . H122B H 0.3693 0.3172 -0.1648 0.060 Uiso 1 calc R . . C123 C 0.4874(8) 0.2847(9) -0.1591(6) 0.068(5) Uani 1 d . . . H123A H 0.4741 0.2382 -0.1392 0.082 Uiso 1 calc R . . H123B H 0.4944 0.2709 -0.1972 0.082 Uiso 1 calc R . . C124 C 0.5630(7) 0.3159(8) -0.1376(5) 0.051(3) Uani 1 d . . . H124A H 0.6027 0.2757 -0.1385 0.061 Uiso 1 calc R . . H124B H 0.5807 0.3575 -0.1611 0.061 Uiso 1 calc R . . C125 C 0.5555(8) 0.3444(10) -0.0823(6) 0.066(5) Uani 1 d . . . H125A H 0.6052 0.3671 -0.0710 0.079 Uiso 1 calc R . . H125B H 0.5439 0.3018 -0.0580 0.079 Uiso 1 calc R . . C126 C 0.4902(7) 0.4047(8) -0.0779(6) 0.052(4) Uani 1 d . . . H126A H 0.5038 0.4492 -0.0999 0.062 Uiso 1 calc R . . H126B H 0.4851 0.4213 -0.0403 0.062 Uiso 1 calc R . . C211 C 0.2117(6) 0.5702(6) 0.1019(4) 0.028(2) Uani 1 d . . . H211 H 0.1873 0.5719 0.1382 0.034 Uiso 1 calc R . . C212 C 0.1468(7) 0.5738(6) 0.0591(5) 0.037(3) Uani 1 d . . . H212A H 0.1702 0.5719 0.0229 0.045 Uiso 1 calc R . . H212B H 0.1126 0.5294 0.0630 0.045 Uiso 1 calc R . . C213 C 0.0990(7) 0.6456(7) 0.0645(5) 0.042(3) Uani 1 d . . . H213A H 0.0744 0.6472 0.1002 0.050 Uiso 1 calc R . . H213B H 0.0577 0.6461 0.0371 0.050 Uiso 1 calc R . . C214 C 0.1519(8) 0.7159(7) 0.0572(6) 0.058(4) Uani 1 d . . . H214A H 0.1756 0.7153 0.0212 0.070 Uiso 1 calc R . . H214B H 0.1210 0.7626 0.0608 0.070 Uiso 1 calc R . . C215 C 0.2150(7) 0.7138(8) 0.1002(6) 0.057(4) Uani 1 d . . . H215A H 0.1909 0.7162 0.1361 0.069 Uiso 1 calc R . . H215B H 0.2492 0.7582 0.0961 0.069 Uiso 1 calc R . . C216 C 0.2637(6) 0.6403(6) 0.0954(5) 0.034(3) Uani 1 d . . . H216A H 0.2894 0.6388 0.0601 0.041 Uiso 1 calc R . . H216B H 0.3042 0.6400 0.1234 0.041 Uiso 1 calc R . . C221 C 0.3479(7) 0.4902(8) 0.1450(5) 0.037(3) Uani 1 d . . . H221 H 0.3822 0.5319 0.1323 0.045 Uiso 1 calc R . . C222 C 0.3970(6) 0.4159(7) 0.1459(5) 0.039(3) Uani 1 d . . . H222A H 0.3650 0.3741 0.1600 0.047 Uiso 1 calc R . . H222B H 0.4125 0.4028 0.1089 0.047 Uiso 1 calc R . . C223 C 0.4707(7) 0.4250(10) 0.1812(6) 0.061(4) Uani 1 d . . . H223A H 0.4991 0.3766 0.1829 0.073 Uiso 1 calc R . . H223B H 0.5053 0.4635 0.1655 0.073 Uiso 1 calc R . . C224 C 0.4464(10) 0.4488(11) 0.2367(6) 0.085(6) Uani 1 d . . . H224A H 0.4932 0.4581 0.2584 0.102 Uiso 1 calc R . . H224B H 0.4175 0.4068 0.2536 0.102 Uiso 1 calc R . . C225 C 0.3957(8) 0.5199(10) 0.2375(6) 0.068(5) Uani 1 d . . . H225A H 0.3803 0.5314 0.2748 0.081 Uiso 1 calc R . . H225B H 0.4257 0.5633 0.2236 0.081 Uiso 1 calc R . . C226 C 0.3236(8) 0.5087(10) 0.2033(5) 0.048(4) Uani 1 d . . . H226A H 0.2918 0.5551 0.2038 0.057 Uiso 1 calc R . . H226B H 0.2922 0.4668 0.2180 0.057 Uiso 1 calc R . . C231 C 0.2016(5) 0.4028(6) 0.1193(5) 0.026(2) Uani 1 d . . . H231 H 0.2356 0.3637 0.1360 0.032 Uiso 1 calc R . . C232 C 0.1417(7) 0.4269(7) 0.1634(5) 0.039(3) Uani 1 d . . . H232A H 0.1693 0.4497 0.1941 0.047 Uiso 1 calc R . . H232B H 0.1060 0.4652 0.1486 0.047 Uiso 1 calc R . . C233 C 0.0951(7) 0.3578(7) 0.1826(5) 0.045(3) Uani 1 d . . . H233A H 0.0572 0.3740 0.2100 0.054 Uiso 1 calc R . . H233B H 0.1306 0.3210 0.1995 0.054 Uiso 1 calc R . . C234 C 0.0518(8) 0.3190(8) 0.1359(5) 0.051(4) Uani 1 d . . . H234A H 0.0245 0.2737 0.1491 0.061 Uiso 1 calc R . . H234B H 0.0131 0.3541 0.1206 0.061 Uiso 1 calc R . . C235 C 0.1099(7) 0.2966(7) 0.0928(5) 0.043(3) Uani 1 d . . . H235A H 0.0818 0.2748 0.0619 0.051 Uiso 1 calc R . . H235B H 0.1446 0.2572 0.1072 0.051 Uiso 1 calc R . . C236 C 0.1587(6) 0.3635(6) 0.0733(4) 0.030(3) Uani 1 d . . . H236A H 0.1968 0.3453 0.0467 0.037 Uiso 1 calc R . . H236B H 0.1247 0.4005 0.0553 0.037 Uiso 1 calc R . . Au2 Au 0.52920(2) 0.00085(2) 0.12159(2) 0.03057(10) Uani 1 d . . . Br2 Br 0.68172(7) 0.06156(8) 0.10797(6) 0.0514(3) Uani 1 d . . . P3 P 0.52826(17) -0.01968(17) 0.21312(12) 0.0319(7) Uani 1 d . . . P4 P 0.48107(16) 0.00675(15) 0.03481(12) 0.0270(6) Uani 1 d . . . C331 C 0.6193(6) -0.0654(7) 0.2392(5) 0.035(3) Uani 1 d U . . H331 H 0.6584 -0.0240 0.2411 0.042 Uiso 1 calc R . . C332 C 0.6520(7) -0.1239(7) 0.1958(5) 0.043(3) Uani 1 d U . . H332A H 0.6155 -0.1664 0.1915 0.052 Uiso 1 calc R . . H332B H 0.6578 -0.0985 0.1608 0.052 Uiso 1 calc R . . C333 C 0.7309(7) -0.1534(8) 0.2151(6) 0.060(4) Uani 1 d U . . H333A H 0.7689 -0.1117 0.2142 0.072 Uiso 1 calc R . . H333B H 0.7491 -0.1930 0.1901 0.072 Uiso 1 calc R . . C334 C 0.7276(8) -0.1864(9) 0.2722(6) 0.065(4) Uani 1 d U . . H334A H 0.6931 -0.2309 0.2726 0.078 Uiso 1 calc R . . H334B H 0.7799 -0.2032 0.2830 0.078 Uiso 1 calc R . . C335 C 0.6978(9) -0.1279(9) 0.3124(7) 0.064(4) Uani 1 d U . . H335A H 0.7346 -0.0852 0.3145 0.077 Uiso 1 calc R . . H335B H 0.6940 -0.1510 0.3483 0.077 Uiso 1 calc R . . C336 C 0.6156(8) -0.0980(8) 0.2944(5) 0.049(3) Uani 1 d U . . H336A H 0.5780 -0.1401 0.2950 0.058 Uiso 1 calc R . . H336B H 0.5976 -0.0589 0.3198 0.058 Uiso 1 calc R . . C311 C 0.4457(6) -0.0799(7) 0.2369(5) 0.035(3) Uani 1 d U . . H311 H 0.4521 -0.0876 0.2763 0.042 Uiso 1 calc R . . C312 C 0.4465(8) -0.1590(8) 0.2097(6) 0.048(3) Uani 1 d U . . H312A H 0.4476 -0.1521 0.1704 0.058 Uiso 1 calc R . . H312B H 0.4947 -0.1854 0.2201 0.058 Uiso 1 calc R . . C313 C 0.3788(7) -0.2086(8) 0.2238(7) 0.061(4) Uani 1 d U . . H313A H 0.3826 -0.2238 0.2618 0.073 Uiso 1 calc R . . H313B H 0.3806 -0.2550 0.2017 0.073 Uiso 1 calc R . . C314 C 0.3024(7) -0.1689(8) 0.2146(6) 0.049(3) Uani 1 d U . . H314A H 0.2952 -0.1599 0.1758 0.059 Uiso 1 calc R . . H314B H 0.2596 -0.2016 0.2271 0.059 Uiso 1 calc R . . C3115 C 0.2993(7) -0.0943(9) 0.2440(7) 0.067(4) Uani 1 d U . . H315A H 0.3017 -0.1036 0.2831 0.081 Uiso 1 calc R . . H315B H 0.2496 -0.0689 0.2361 0.081 Uiso 1 calc R . . C316 C 0.3666(8) -0.0424(7) 0.2275(7) 0.061(4) Uani 1 d U . . H316A H 0.3613 -0.0293 0.1892 0.073 Uiso 1 calc R . . H316B H 0.3638 0.0050 0.2484 0.073 Uiso 1 calc R . . C321 C 0.5156(9) 0.0696(8) 0.2530(7) 0.062(4) Uani 1 d U . . H321 H 0.4783 0.0570 0.2823 0.075 Uiso 1 calc R . . C322 C 0.4782(14) 0.1290(11) 0.2209(9) 0.117(7) Uani 1 d U . . H322A H 0.4302 0.1089 0.2048 0.140 Uiso 1 calc R . . H322B H 0.5132 0.1442 0.1914 0.140 Uiso 1 calc R . . C323 C 0.4579(15) 0.2014(11) 0.2566(10) 0.134(8) Uani 1 d U . . H323A H 0.4323 0.2404 0.2345 0.161 Uiso 1 calc R . . H323B H 0.4226 0.1871 0.2861 0.161 Uiso 1 calc R . . C324 C 0.5277(11) 0.2291(10) 0.2773(10) 0.112(7) Uani 1 d U . . H324A H 0.5182 0.2766 0.2970 0.134 Uiso 1 calc R . . H324B H 0.5640 0.2400 0.2476 0.134 Uiso 1 calc R . . C325 C 0.5616(15) 0.1728(10) 0.3133(8) 0.110(7) Uani 1 d U . . H325A H 0.5240 0.1595 0.3417 0.132 Uiso 1 calc R . . H325B H 0.6084 0.1937 0.3306 0.132 Uiso 1 calc R . . C326 C 0.5841(13) 0.0980(11) 0.2793(9) 0.106(7) Uani 1 d U . . H326A H 0.6239 0.1106 0.2522 0.127 Uiso 1 calc R . . H326B H 0.6054 0.0590 0.3035 0.127 Uiso 1 calc R . . C431 C 0.5592(6) 0.0262(7) -0.0164(5) 0.036(3) Uani 1 d . . . H431 H 0.5916 0.0672 -0.0006 0.043 Uiso 1 calc R . . C432 C 0.6150(6) -0.0450(7) -0.0214(5) 0.040(3) Uani 1 d . . . H432A H 0.6293 -0.0634 0.0146 0.048 Uiso 1 calc R . . H432B H 0.5882 -0.0863 -0.0406 0.048 Uiso 1 calc R . . C433 C 0.6878(6) -0.0217(7) -0.0523(5) 0.039(3) Uani 1 d . . . H433A H 0.7176 0.0149 -0.0306 0.047 Uiso 1 calc R . . H433B H 0.7208 -0.0667 -0.0580 0.047 Uiso 1 calc R . . C434 C 0.6688(8) 0.0131(9) -0.1056(6) 0.054(4) Uani 1 d . . . H434A H 0.6470 -0.0264 -0.1293 0.065 Uiso 1 calc R . . H434B H 0.7171 0.0314 -0.1223 0.065 Uiso 1 calc R . . C435 C 0.6110(7) 0.0791(8) -0.1023(5) 0.047(3) Uani 1 d . . . H435A H 0.5966 0.0953 -0.1389 0.057 Uiso 1 calc R . . H435B H 0.6356 0.1224 -0.0840 0.057 Uiso 1 calc R . . C436 C 0.5354(6) 0.0545(8) -0.0705(5) 0.043(3) Uani 1 d . . . H436A H 0.5001 0.0981 -0.0666 0.051 Uiso 1 calc R . . H436B H 0.5079 0.0142 -0.0903 0.051 Uiso 1 calc R . . C411 C 0.4145(6) 0.0886(6) 0.0272(4) 0.029(3) Uani 1 d . . . H411 H 0.3972 0.0907 -0.0110 0.035 Uiso 1 calc R . . C412 C 0.3410(6) 0.0824(7) 0.0634(5) 0.037(3) Uani 1 d . . . H412A H 0.3110 0.0374 0.0525 0.045 Uiso 1 calc R . . H412B H 0.3575 0.0749 0.1010 0.045 Uiso 1 calc R . . C413 C 0.2899(7) 0.1503(7) 0.0605(6) 0.044(3) Uani 1 d . . . H413A H 0.2467 0.1442 0.0861 0.053 Uiso 1 calc R . . H413B H 0.2677 0.1539 0.0241 0.053 Uiso 1 calc R . . C414 C 0.3334(7) 0.2238(7) 0.0733(6) 0.054(4) Uani 1 d . . . H414A H 0.2982 0.2673 0.0685 0.065 Uiso 1 calc R . . H414B H 0.3505 0.2231 0.1112 0.065 Uiso 1 calc R . . C415 C 0.4040(7) 0.2329(7) 0.0366(6) 0.049(3) Uani 1 d . . . H415A H 0.4332 0.2786 0.0471 0.059 Uiso 1 calc R . . H415B H 0.3864 0.2396 -0.0008 0.059 Uiso 1 calc R . . C416 C 0.4584(7) 0.1625(6) 0.0399(5) 0.036(3) Uani 1 d . . . H416A H 0.5016 0.1687 0.0143 0.044 Uiso 1 calc R . . H416B H 0.4806 0.1592 0.0764 0.044 Uiso 1 calc R . . C421 C 0.4223(6) -0.0781(5) 0.0199(5) 0.030(3) Uani 1 d . . . H421 H 0.3774 -0.0754 0.0450 0.036 Uiso 1 calc R . . C422 C 0.3860(7) -0.0859(7) -0.0366(5) 0.040(3) Uani 1 d . . . H422A H 0.3593 -0.0384 -0.0463 0.048 Uiso 1 calc R . . H422B H 0.4271 -0.0951 -0.0633 0.048 Uiso 1 calc R . . C423 C 0.3285(8) -0.1509(8) -0.0374(6) 0.053(4) Uani 1 d . . . H423A H 0.3070 -0.1565 -0.0738 0.064 Uiso 1 calc R . . H423B H 0.2853 -0.1396 -0.0127 0.064 Uiso 1 calc R . . C424 C 0.3682(7) -0.2265(7) -0.0201(5) 0.047(3) Uani 1 d . . . H424A H 0.3287 -0.2668 -0.0180 0.056 Uiso 1 calc R . . H424B H 0.4065 -0.2413 -0.0476 0.056 Uiso 1 calc R . . C425 C 0.4084(7) -0.2193(7) 0.0335(5) 0.042(3) Uani 1 d . . . H425A H 0.4366 -0.2666 0.0413 0.050 Uiso 1 calc R . . H425B H 0.3690 -0.2122 0.0619 0.050 Uiso 1 calc R . . C426 C 0.4656(7) -0.1526(6) 0.0350(5) 0.035(3) Uani 1 d . . . H426A H 0.5082 -0.1617 0.0093 0.042 Uiso 1 calc R . . H426B H 0.4881 -0.1479 0.0712 0.042 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.02396(17) 0.02883(18) 0.02123(17) -0.0012(2) 0.00130(19) 0.00019(16) Br1 0.0296(6) 0.0468(7) 0.0566(9) -0.0108(6) 0.0047(5) -0.0127(5) P1 0.0243(15) 0.0268(14) 0.0237(14) -0.0032(11) 0.0022(10) -0.0038(11) P2 0.0199(14) 0.0295(15) 0.0211(14) -0.0032(11) -0.0009(10) 0.0001(11) C131 0.033(6) 0.060(9) 0.024(6) 0.002(6) 0.003(5) -0.009(6) C132 0.031(7) 0.046(8) 0.031(7) 0.004(6) -0.003(5) 0.011(6) C133 0.037(7) 0.044(7) 0.033(7) 0.006(5) 0.006(5) -0.003(5) C134 0.035(7) 0.060(9) 0.056(9) 0.023(7) -0.011(6) -0.008(6) C135 0.055(8) 0.039(7) 0.052(9) -0.002(6) -0.007(6) -0.002(6) C136 0.051(8) 0.033(7) 0.034(7) -0.001(5) 0.001(5) -0.002(5) C111 0.028(6) 0.039(7) 0.021(6) -0.003(5) 0.007(4) -0.002(5) C112 0.038(7) 0.033(7) 0.055(8) -0.011(6) 0.008(6) -0.009(5) C113 0.041(7) 0.041(7) 0.068(10) -0.007(7) 0.001(6) -0.017(6) C114 0.033(7) 0.049(8) 0.051(9) -0.005(6) 0.000(6) -0.016(6) C115 0.016(6) 0.075(10) 0.047(8) 0.001(7) -0.006(5) -0.008(6) C116 0.043(7) 0.039(7) 0.039(7) 0.007(6) -0.010(6) -0.018(6) C121 0.029(6) 0.032(6) 0.023(6) -0.006(5) 0.006(4) -0.010(5) C122 0.039(7) 0.076(10) 0.036(8) -0.018(7) -0.001(5) 0.015(7) C123 0.041(9) 0.083(12) 0.080(12) -0.035(9) 0.004(7) 0.005(8) C124 0.038(8) 0.058(9) 0.057(9) -0.004(7) 0.012(6) 0.010(6) C125 0.032(7) 0.098(13) 0.066(11) -0.030(9) -0.011(7) 0.004(8) C126 0.032(7) 0.065(9) 0.059(9) -0.036(7) -0.011(6) -0.005(6) C211 0.025(6) 0.028(6) 0.031(6) -0.002(5) -0.001(4) 0.008(5) C212 0.031(6) 0.034(6) 0.047(8) 0.001(6) -0.003(5) 0.000(5) C213 0.028(7) 0.041(7) 0.056(8) 0.005(6) -0.006(5) 0.012(5) C214 0.057(9) 0.038(7) 0.080(11) 0.016(7) 0.013(7) 0.023(7) C215 0.037(8) 0.034(7) 0.100(13) -0.010(7) 0.010(7) 0.008(6) C216 0.028(6) 0.022(6) 0.053(8) -0.007(5) -0.001(5) 0.004(5) C221 0.028(6) 0.055(8) 0.028(6) -0.001(6) -0.002(5) -0.010(6) C222 0.026(6) 0.043(7) 0.048(7) 0.002(6) -0.013(5) 0.006(5) C223 0.037(8) 0.087(12) 0.059(10) 0.002(8) -0.013(6) 0.010(7) C224 0.049(9) 0.145(18) 0.061(11) 0.031(11) -0.033(8) 0.000(10) C225 0.033(7) 0.136(15) 0.035(8) -0.019(8) -0.004(6) -0.001(8) C226 0.049(9) 0.071(11) 0.022(7) -0.018(7) 0.002(5) 0.005(8) C231 0.027(5) 0.028(5) 0.024(6) -0.002(5) -0.004(5) 0.002(4) C232 0.036(7) 0.046(7) 0.035(7) 0.000(6) 0.020(5) -0.003(6) C233 0.033(7) 0.058(9) 0.044(8) 0.016(6) 0.011(6) 0.010(6) C234 0.041(7) 0.061(9) 0.051(9) 0.025(7) -0.003(6) -0.023(7) C235 0.044(8) 0.039(7) 0.045(8) 0.000(6) -0.001(6) -0.016(6) C236 0.035(6) 0.026(6) 0.030(6) 0.009(5) 0.003(5) -0.009(5) Au2 0.03234(19) 0.02975(19) 0.0296(2) 0.00034(19) -0.0030(2) 0.00101(18) Br2 0.0339(7) 0.0548(8) 0.0655(10) -0.0010(7) -0.0083(6) -0.0136(6) P3 0.0351(17) 0.0288(15) 0.0317(16) -0.0037(12) -0.0039(12) 0.0016(12) P4 0.0238(15) 0.0261(14) 0.0311(15) -0.0019(11) -0.0002(11) 0.0016(11) C331 0.024(6) 0.039(6) 0.041(7) 0.012(5) -0.013(5) -0.002(5) C332 0.035(7) 0.044(7) 0.051(8) 0.014(6) -0.008(5) 0.005(6) C333 0.027(7) 0.055(9) 0.098(12) 0.003(8) -0.011(7) 0.001(6) C334 0.047(9) 0.070(10) 0.078(11) 0.002(8) -0.035(7) 0.011(7) C335 0.063(10) 0.060(9) 0.069(10) 0.009(8) -0.033(8) 0.003(7) C336 0.050(8) 0.043(7) 0.052(8) 0.004(6) -0.021(6) 0.003(6) C311 0.024(6) 0.051(8) 0.028(6) -0.002(5) -0.013(5) 0.008(5) C312 0.036(7) 0.049(8) 0.060(9) -0.002(7) 0.012(7) -0.002(6) C313 0.031(7) 0.053(8) 0.097(11) 0.026(8) 0.006(7) 0.003(6) C314 0.022(6) 0.056(8) 0.069(9) 0.016(7) -0.009(6) 0.003(6) C315 0.029(7) 0.067(10) 0.105(13) -0.019(9) 0.001(7) 0.012(6) C316 0.039(8) 0.046(8) 0.097(11) -0.013(8) -0.017(7) 0.026(6) C321 0.066(9) 0.036(8) 0.085(11) -0.021(7) -0.012(8) 0.019(7) C322 0.152(17) 0.067(11) 0.132(16) -0.037(11) -0.059(13) 0.055(12) C323 0.177(19) 0.062(12) 0.164(19) -0.039(12) -0.065(16) 0.052(13) C324 0.076(13) 0.046(10) 0.21(2) -0.005(12) -0.051(13) -0.007(9) C325 0.165(17) 0.062(11) 0.104(14) -0.038(10) -0.065(13) 0.022(12) C326 0.116(15) 0.070(12) 0.131(16) -0.037(11) -0.052(12) 0.015(11) C431 0.015(5) 0.044(7) 0.050(7) 0.008(6) 0.006(5) 0.000(5) C432 0.020(6) 0.052(8) 0.048(8) 0.004(6) 0.005(5) 0.008(5) C433 0.020(5) 0.046(7) 0.051(8) -0.001(6) 0.003(5) 0.007(5) C434 0.044(8) 0.076(10) 0.043(9) 0.001(7) 0.011(6) 0.003(7) C435 0.036(7) 0.071(9) 0.035(7) 0.017(6) 0.005(5) 0.005(6) C436 0.026(7) 0.062(9) 0.040(7) -0.002(6) 0.002(5) 0.003(5) C411 0.020(5) 0.029(6) 0.038(7) -0.002(4) -0.004(4) -0.003(4) C412 0.024(6) 0.038(7) 0.050(8) -0.001(6) 0.005(5) 0.001(5) C413 0.030(7) 0.032(7) 0.070(10) -0.010(6) 0.007(6) 0.002(5) C414 0.037(8) 0.037(7) 0.089(11) -0.015(7) 0.009(7) 0.012(6) C415 0.045(8) 0.030(7) 0.072(9) -0.002(6) 0.002(7) -0.002(6) C416 0.033(7) 0.031(6) 0.045(7) 0.000(5) -0.003(5) 0.000(5) C421 0.019(5) 0.028(5) 0.043(8) 0.003(5) -0.002(4) -0.001(4) C422 0.044(7) 0.040(7) 0.037(7) 0.000(5) -0.010(6) 0.001(6) C423 0.048(8) 0.046(8) 0.066(9) -0.014(7) -0.015(7) 0.005(6) C424 0.040(8) 0.039(7) 0.061(9) -0.008(6) -0.001(6) -0.003(6) C425 0.039(7) 0.031(7) 0.055(8) 0.000(5) -0.010(6) -0.011(6) C426 0.043(7) 0.020(6) 0.042(7) -0.004(5) -0.007(5) 0.001(5) _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P2 2.312(3) . ? Au1 P1 2.317(3) . ? Au1 Br1 2.8937(12) . ? P1 C111 1.832(11) . ? P1 C131 1.848(13) . ? P1 C121 1.873(11) . ? P2 C211 1.850(10) . ? P2 C231 1.855(11) . ? P2 C221 1.855(12) . ? C131 C132 1.553(17) . ? C131 C136 1.553(17) . ? C132 C133 1.507(17) . ? C133 C134 1.525(18) . ? C134 C135 1.510(18) . ? C135 C136 1.530(17) . ? C111 C116 1.543(16) . ? C111 C112 1.542(17) . ? C112 C113 1.568(15) . ? C113 C114 1.539(17) . ? C114 C115 1.495(17) . ? C115 C116 1.516(15) . ? C121 C122 1.494(14) . ? C121 C126 1.547(14) . ? C122 C123 1.564(18) . ? C123 C124 1.503(18) . ? C124 C125 1.462(18) . ? C125 C126 1.544(19) . ? C211 C216 1.526(15) . ? C211 C212 1.538(15) . ? C212 C213 1.508(15) . ? C213 C214 1.540(17) . ? C214 C215 1.516(19) . ? C215 C216 1.540(16) . ? C221 C226 1.535(17) . ? C221 C222 1.551(17) . ? C222 C223 1.544(16) . ? C223 C224 1.49(2) . ? C224 C225 1.52(2) . ? C225 C226 1.510(18) . ? C231 C236 1.519(15) . ? C231 C232 1.558(15) . ? C232 C233 1.528(16) . ? C233 C234 1.532(17) . ? C234 C235 1.510(17) . ? C235 C236 1.519(15) . ? Au2 P3 2.292(3) . ? Au2 P4 2.302(3) . ? Au2 Br2 2.8415(12) . ? P3 C311 1.860(12) . ? P3 C331 1.868(11) . ? P3 C321 1.864(14) . ? P4 C421 1.834(10) . ? P4 C411 1.843(10) . ? P4 C431 1.873(11) . ? C331 C336 1.481(16) . ? C331 C332 1.586(17) . ? C332 C333 1.524(16) . ? C333 C334 1.53(2) . ? C334 C335 1.52(2) . ? C335 C336 1.568(18) . ? C311 C316 1.526(15) . ? C311 C312 1.542(18) . ? C312 C313 1.492(17) . ? C313 C314 1.500(16) . ? C314 C315 1.50(2) . ? C315 C316 1.53(2) . ? C321 C326 1.43(2) . ? C321 C322 1.46(2) . ? C322 C323 1.59(2) . ? C323 C324 1.39(3) . ? C324 C325 1.45(2) . ? C325 C326 1.61(2) . ? C431 C416 1.484(16) . ? C431 C432 1.578(16) . ? C432 C433 1.519(16) . ? C433 C434 1.490(19) . ? C434 C435 1.526(18) . ? C435 C436 1.576(15) . ? C411 C412 1.532(14) . ? C411 C416 1.550(15) . ? C412 C413 1.480(16) . ? C413 C414 1.523(17) . ? C414 C415 1.522(18) . ? C415 C416 1.549(16) . ? C421 C422 1.536(15) . ? C421 C426 1.548(14) . ? C422 C423 1.507(17) . ? C423 C424 1.550(18) . ? C424 C425 1.501(16) . ? C425 C426 1.527(15) . ? 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 P2 Au1 P1 162.06(9) . . ? P2 Au1 Br1 97.69(7) . . ? P1 Au1 Br1 99.56(7) . . ? C111 P1 C131 108.5(5) . . ? C111 P1 C121 104.7(5) . . ? C131 P1 C121 107.1(5) . . ? C111 P1 Au1 112.0(3) . . ? C131 P1 Au1 110.9(4) . . ? C121 P1 Au1 113.3(3) . . ? C211 P2 C231 106.8(5) . . ? C211 P2 C221 104.2(5) . . ? C231 P2 C221 108.3(5) . . ? C211 P2 Au1 111.8(4) . . ? C231 P2 Au1 114.8(4) . . ? C221 P2 Au1 110.4(4) . . ? C132 C131 C136 110.6(10) . . ? C132 C131 P1 117.1(9) . . ? C136 C131 P1 112.1(8) . . ? C133 C132 C131 111.2(11) . . ? C132 C133 C134 111.6(10) . . ? C135 C134 C133 111.6(10) . . ? C134 C135 C136 111.8(11) . . ? C135 C136 C131 111.9(10) . . ? C116 C111 C112 110.5(9) . . ? C116 C111 P1 110.9(8) . . ? C112 C111 P1 109.6(8) . . ? C111 C112 C113 112.7(10) . . ? C114 C113 C112 110.9(10) . . ? C115 C114 C113 112.1(10) . . ? C114 C115 C116 112.9(10) . . ? C115 C116 C111 113.5(10) . . ? C121 C122 C126 111.1(9) . . ? C122 C121 P1 117.0(8) . . ? C126 C121 P1 113.1(7) . . ? C121 C122 C123 110.2(11) . . ? C124 C123 C122 113.0(12) . . ? C125 C124 C123 112.4(11) . . ? C124 C125 C126 111.3(12) . . ? C125 C126 C121 110.3(10) . . ? C216 C211 C212 108.4(9) . . ? C216 C211 P2 112.4(7) . . ? C212 C211 P2 110.3(8) . . ? C213 C212 C211 111.4(10) . . ? C212 C213 C214 109.8(10) . . ? C215 C214 C213 108.5(11) . . ? C214 C215 C216 110.7(11) . . ? C211 C216 C215 110.5(9) . . ? C226 C221 C222 108.2(11) . . ? C226 C221 P2 115.8(9) . . ? C222 C221 P2 109.4(8) . . ? C223 C222 C221 111.3(11) . . ? C224 C223 C222 108.7(11) . . ? C223 C224 C225 113.6(12) . . ? C226 C225 C224 110.6(13) . . ? C225 C226 C221 109.3(11) . . ? C236 C231 C232 109.2(9) . . ? C236 C231 P2 112.8(8) . . ? C232 C231 P2 114.9(7) . . ? C233 C232 C231 110.3(10) . . ? C232 C233 C234 111.7(10) . . ? C235 C234 C233 109.3(10) . . ? C234 C235 C236 112.6(10) . . ? C231 C236 C235 112.3(9) . . ? P3 Au2 P4 157.75(11) . . ? P3 Au2 Br2 100.51(8) . . ? P4 Au2 Br2 101.65(8) . . ? C311 P3 C331 106.3(5) . . ? C311 P3 C321 102.8(7) . . ? C331 P3 C321 106.0(6) . . ? C311 P3 Au2 114.0(4) . . ? C331 P3 Au2 113.7(4) . . ? C321 P3 Au2 113.1(5) . . ? C421 P4 C411 105.8(5) . . ? C421 P4 C431 113.8(5) . . ? C411 P4 C431 103.3(5) . . ? C421 P4 Au2 110.3(4) . . ? C411 P4 Au2 110.6(4) . . ? C431 P4 Au2 112.5(4) . . ? C336 C331 C332 112.8(10) . . ? C336 C331 P3 116.6(9) . . ? C332 C331 P3 109.8(7) . . ? C333 C332 C331 108.9(10) . . ? C332 C333 C334 112.6(11) . . ? C335 C334 C333 111.3(13) . . ? C334 C335 C336 110.0(11) . . ? C331 C336 C335 110.6(12) . . ? C316 C311 C312 109.3(10) . . ? C316 C311 P3 112.4(9) . . ? C312 C311 P3 111.6(8) . . ? C313 C312 C311 114.6(11) . . ? C312 C313 C314 111.9(12) . . ? C315 C314 C313 111.3(11) . . ? C314 C315 C316 111.4(11) . . ? C311 C316 C315 111.9(11) . . ? C326 C321 C322 110.9(17) . . ? C326 C321 P3 115.8(12) . . ? C322 C321 P3 111.3(11) . . ? C321 C322 C323 111.4(16) . . ? C324 C323 C322 107(2) . . ? C323 C324 C325 109.4(18) . . ? C324 C325 C326 109.3(17) . . ? C321 C326 C325 108.8(16) . . ? C436 C431 C432 111.0(10) . . ? C436 C431 P4 118.3(8) . . ? C432 C431 P4 110.0(8) . . ? C433 C432 C431 108.9(10) . . ? C434 C433 C432 112.1(10) . . ? C433 C434 C435 113.9(11) . . ? C434 C435 C436 110.6(11) . . ? C431 C436 C435 108.5(9) . . ? C416 C411 C412 109.8(9) . . ? C416 C411 P4 109.6(7) . . ? C412 C411 P4 112.8(7) . . ? C413 C412 C411 113.3(10) . . ? C412 C413 C414 112.5(10) . . ? C415 C414 C4113 110.7(11) . . ? C414 C415 C416 111.2(10) . . ? C411 C416 C415 111.6(9) . . ? C422 C421 C422 109.8(9) . . ? C422 C421 P4 118.5(8) . . ? C426 C421 P4 111.9(7) . . ? C423 C422 C421 110.0(10) . . ? C422 C423 C424 111.0(10) . . ? C425 C424 C423 111.8(11) . . ? C424 C425 C426 112.3(10) . . ? C425 C426 C421 109.5(9) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.833 _refine_diff_density_min -1.315 _refine_diff_density_rms 0.168 #=======================================================END data_cy2aubrc #-------------------------------------------------------------------- _audit_creation_date '1998-11-07' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #-------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ? _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #-------------------------------------------------------------------- _cell_length_a 18.01(1) _cell_length_b 9.198(4) _cell_length_c 22.485(7) _cell_angle_alpha 90 _cell_angle_beta 95.63(3) _cell_angle_gamma 90 _cell_volume 3707(3) _cell_formula_units_Z 4 _cell_measurement_temperature 568.4 _cell_measurement_reflns_used 14 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 2.8 #-------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2+y, +z' ' -x, +y,1/2-z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2-x,1/2-y, -z' ' +x, -y,1/2+z' '1/2+x,1/2-y,1/2+z' #-------------------------------------------------------------------- _exptl_crystal_description 'plate' _exptl_crystal_colour 'clear' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 837.74 _chemical_formula_analytical ? _chemical_formula_sum 'C36 H66 Au Br P2 ' _chemical_formula_moiety 'C36 H66 Au Br P2 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1704.00 _exptl_absorpt_coefficient_mu 5.172 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 0.60 _exptl_absorpt_correction_T_min 0.42 _exptl_special_details ; The scan width was (1.15+0.35tan\q)\% with an \w scan speed of 16\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #-------------------------------------------------------------------- _diffrn_special_details ; ? ; _diffrn_ambient_temperature 568.4 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku Rigaku_AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.68 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -1 4 1 1 4 -2 0 6 _diffrn_reflns_number 3602 _reflns_number_total 3478 _reflns_number_gt 2309 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.00039 _diffrn_reflns_av_sigmaI/netI 0.090 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.01179 _diffrn_orient_matrix_UB_12 0.03523 _diffrn_orient_matrix_UB_13 0.04009 _diffrn_orient_matrix_UB_21 -0.00743 _diffrn_orient_matrix_UB_22 -0.10265 _diffrn_orient_matrix_UB_23 0.01281 _diffrn_orient_matrix_UB_31 0.05403 _diffrn_orient_matrix_UB_32 -0.00644 _diffrn_orient_matrix_UB_33 0.01504 #-------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 144 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 264 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Au 0 4 -2.688 8.798 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Br 0 4 -0.374 2.456 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P 0 8 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #-------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Au 0.00 0.28409(6) 0.25 0.0403(1) 0.5 ST Uani d ? Br 0.00 0.5860(2) 0.25 0.0744(6) 0.5 ST Uani d ? P(1) 0.0641(1) 0.2133(3) 0.34005(9) 0.0376(6) 1.0 . Uani d ? C(11) 0.0077(4) 0.0884(9) 0.3816(3) 0.037(2) 1.0 . Uani d ? C(12) -0.0646(5) 0.159(1) 0.3951(4) 0.054(3) 1.0 . Uani d ? C(13) -0.1124(5) 0.057(1) 0.4295(4) 0.058(3) 1.0 . Uani d ? C(14) -0.1268(6) -0.085(1) 0.3976(4) 0.062(3) 1.0 . Uani d ? C(15) -0.0554(6) -0.157(1) 0.3838(5) 0.063(3) 1.0 . Uani d ? C(16) -0.0086(5) -0.056(1) 0.3495(4) 0.052(3) 1.0 . Uani d ? C(21) 0.0872(5) 0.3626(9) 0.3936(4) 0.046(3) 1.0 . Uani d ? C(22) 0.1452(5) 0.467(1) 0.3725(4) 0.063(3) 1.0 . Uani d ? C(23) 0.1502(6) 0.603(1) 0.4111(5) 0.079(4) 1.0 . Uani d ? C(24) 0.1679(6) 0.570(1) 0.4760(5) 0.074(4) 1.0 . Uani d ? C(25) 0.1138(6) 0.465(1) 0.4975(4) 0.074(4) 1.0 . Uani d ? C(26) 0.1066(6) 0.328(1) 0.4591(4) 0.061(3) 1.0 . Uani d ? C(31) 0.1486(5) 0.1085(9) 0.3251(4) 0.041(3) 1.0 . Uani d ? C(32) 0.1970(5) 0.184(1) 0.2836(4) 0.057(3) 1.0 . Uani d ? C(33) 0.2588(6) 0.085(1) 0.2651(5) 0.065(3) 1.0 . Uani d ? C(34) 0.3041(5) 0.020(1) 0.3178(5) 0.063(3) 1.0 . Uani d ? C(35) 0.2563(5) -0.059(1) 0.3573(4) 0.058(3) 1.0 . Uani d ? C(36) 0.1958(5) 0.041(1) 0.3782(4) 0.053(3) 1.0 . Uani d ? H(11) 0.04 0.07 0.42 0.0 1.0 . Uiso c ? H(21) 0.04 0.42 0.39 0.0 1.0 . Uiso c ? H(31) 0.13 0.03 0.30 0.0 1.0 . Uiso c ? H(121) -0.09 0.19 0.36 0.0 1.0 . Uiso c ? H(122) -0.05 0.24 0.42 0.0 1.0 . Uiso c ? H(131) -0.09 0.04 0.47 0.0 1.0 . Uiso c ? H(132) -0.16 0.10 0.43 0.0 1.0 . Uiso c ? H(141) -0.16 -0.07 0.36 0.0 1.0 . Uiso c ? H(142) -0.15 -0.15 0.42 0.0 1.0 . Uiso c ? H(151) -0.03 -0.18 0.42 0.0 1.0 . Uiso c ? H(152) -0.07 -0.24 0.36 0.0 1.0 . Uiso c ? H(161) -0.04 -0.04 0.31 0.0 1.0 . Uiso c ? H(162) 0.04 -0.10 0.34 0.0 1.0 . Uiso c ? H(221) 0.19 0.42 0.38 0.0 1.0 . Uiso c ? H(222) 0.13 0.49 0.33 0.0 1.0 . Uiso c ? H(231) 0.10 0.65 0.41 0.0 1.0 . Uiso c ? H(232) 0.19 0.67 0.40 0.0 1.0 . Uiso c ? H(241) 0.22 0.53 0.48 0.0 1.0 . Uiso c ? H(242) 0.17 0.66 0.50 0.0 1.0 . Uiso c ? H(251) 0.07 0.51 0.50 0.0 1.0 . Uiso c ? H(252) 0.13 0.44 0.54 0.0 1.0 . Uiso c ? H(261) 0.15 0.28 0.46 0.0 1.0 . Uiso c ? H(262) 0.07 0.27 0.47 0.0 1.0 . Uiso c ? H(321) 0.22 0.27 0.30 0.0 1.0 . Uiso c ? H(322) 0.17 0.22 0.25 0.0 1.0 . Uiso c ? H(331) 0.24 0.01 0.24 0.0 1.0 . Uiso c ? H(332) 0.29 0.14 0.24 0.0 1.0 . Uiso c ? H(341) 0.33 0.10 0.34 0.0 1.0 . Uiso c ? H(342) 0.34 -0.05 0.30 0.0 1.0 . Uiso c ? H(351) 0.23 -0.14 0.34 0.0 1.0 . Uiso c ? H(352) 0.29 -0.10 0.39 0.0 1.0 . Uiso c ? H(361) 0.22 0.12 0.40 0.0 1.0 . Uiso c ? H(362) 0.16 -0.01 0.40 0.0 1.0 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au 0.0417(3) 0.0463(3) 0.0327(3) 0.00 0.0029(2) 0.00 Br 0.085(1) 0.0424(9) 0.094(1) 0.00 -0.001(1) 0.00 P(1) 0.042(1) 0.038(1) 0.033(1) -0.007(1) 0.0023(9) 0.002(1) C(11) 0.039(5) 0.042(5) 0.029(4) -0.006(4) 0.003(4) 0.001(4) C(12) 0.060(6) 0.054(6) 0.048(6) -0.014(5) 0.013(5) -0.007(5) C(13) 0.049(6) 0.064(7) 0.066(7) -0.004(5) 0.020(5) 0.004(6) C(14) 0.063(7) 0.064(7) 0.060(7) -0.029(6) 0.009(5) 0.012(5) C(15) 0.064(7) 0.052(6) 0.073(7) -0.022(5) 0.010(6) -0.004(6) C(16) 0.045(5) 0.052(6) 0.060(6) -0.002(5) 0.012(5) 0.001(5) C(21) 0.054(6) 0.047(6) 0.037(5) -0.010(5) 0.008(4) -0.007(4) C(22) 0.072(7) 0.069(8) 0.048(6) -0.013(6) 0.002(5) -0.001(5) C(23) 0.092(9) 0.055(7) 0.088(9) -0.025(6) 0.006(7) 0.007(6) C(24) 0.083(8) 0.073(8) 0.065(7) -0.023(6) 0.005(6) -0.028(6) C(25) 0.078(8) 0.10(1) 0.043(6) -0.021(7) 0.016(5) -0.016(6) C(26) 0.077(7) 0.070(7) 0.038(5) -0.029(6) 0.008(5) -0.003(5) C(31) 0.045(5) 0.037(5) 0.042(5) -0.005(4) 0.001(4) 0.001(4) C(32) 0.061(6) 0.061(7) 0.050(6) 0.004(5) 0.018(5) 0.010(5) C(33) 0.072(7) 0.064(7) 0.062(7) 0.002(6) 0.027(6) -0.004(5) C(34) 0.048(6) 0.054(7) 0.087(8) -0.001(5) 0.007(5) -0.017(6) C(35) 0.046(6) 0.056(6) 0.071(7) 0.009(5) -0.003(5) 0.005(5) C(36) 0.053(6) 0.059(7) 0.048(6) -0.012(5) 0.002(5) 0.010(5) #-------------------------------------------------------------------- _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.000000305(8) _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2309 _refine_ls_number_parameters 183 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_all 0.0412 _refine_ls_wR_factor_ref 0.0412 _refine_ls_goodness_of_fit_all 1.695 _refine_ls_goodness_of_fit_ref 1.695 _refine_ls_shift/su_max 0.0051 _refine_ls_shift/su_mean 0.0005 _refine_diff_density_min -0.74 _refine_diff_density_max 1.01 #-------------------------------------------------------------------- _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag AU BR 2.777(2) . . yes AU P1 2.323(2) . . yes AU P1 2.323(2) . 2 yes P1 C11 1.847(8) . . yes P1 C21 1.847(8) . . yes P1 C31 1.860(9) . . yes C11 C12 1.51(1) . . yes C11 C16 1.53(1) . . yes C11 H11 0.95 . . no C12 C13 1.54(1) . . yes C12 H121 0.96 . . no C12 H122 0.95 . . no C13 C14 1.50(1) . . yes C13 H131 0.96 . . no C13 H132 0.95 . . no C14 C15 1.51(1) . . yes C14 H141 0.96 . . no C14 H142 0.95 . . no C15 C16 1.52(1) . . yes C15 H151 0.95 . . no C15 H152 0.96 . . no C16 H161 0.96 . . no C16 H162 0.95 . . no C21 C22 1.53(1) . . yes C21 C26 1.51(1) . . yes C21 H21 0.95 . . no C22 C23 1.52(1) . . yes C22 H221 0.96 . . no C22 H222 0.95 . . no C23 C24 1.49(1) . . yes C23 H231 0.95 . . no C23 H232 0.96 . . no C24 C25 1.49(1) . . yes C24 H241 0.96 . . no C24 H242 0.95 . . no C25 C26 1.53(1) . . yes C25 H251 0.95 . . no C25 H252 0.96 . . no C26 H261 0.96 . . no C26 H262 0.95 . . no C31 C32 1.51(1) . . yes C31 C36 1.53(1) . . yes C31 H31 0.96 . . no C32 C33 1.53(1) . . yes C32 H321 0.95 . . no C32 H322 0.95 . . no C33 C34 1.50(1) . . yes C33 H331 0.96 . . no C33 H332 0.95 . . no C34 C35 1.49(1) . . yes C34 H341 0.95 . . no C34 H342 0.96 . . no C35 C36 1.53(1) . . yes C35 H351 0.95 . . no C35 H352 0.95 . . no C36 H361 0.95 . . no C36 H362 0.96 . . no #-------------------------------------------------------------------- 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag BR AU P1 106.27(6) . . . yes BR AU P1 106.27(6) . . 2 yes P1 AU P1 147.5(1) . . 2 yes AU P1 C11 111.4(3) . . . yes AU P1 C21 114.9(3) . . . yes AU P1 C31 109.4(3) . . . yes C11 P1 C21 103.5(4) . . . yes C11 P1 C31 105.6(4) . . . yes C21 P1 C31 111.5(4) . . . yes P1 C11 C12 111.2(6) . . . yes P1 C11 C16 113.1(6) . . . yes P1 C11 H11 107.6 . . . no C12 C11 C16 109.8(7) . . . yes C12 C11 H11 107.4 . . . no C16 C11 H11 107.4 . . . no C11 C12 C13 112.1(8) . . . yes C11 C12 H121 109.0 . . . no C11 C12 H122 109.4 . . . no C13 C12 H121 108.5 . . . no C13 C12 H122 109.1 . . . no H121 C12 H122 108.8 . . . no C12 C13 C14 111.8(8) . . . yes C12 C13 H131 108.8 . . . no C12 C13 H132 109.4 . . . no C14 C13 H131 108.8 . . . no C14 C13 H132 109.3 . . . no H131 C13 H132 108.7 . . . no C13 C14 C15 111.8(8) . . . yes C13 C14 H141 108.9 . . . no C13 C14 H142 109.6 . . . no C15 C14 H141 108.6 . . . no C15 C14 H142 109.4 . . . no H141 C14 H142 108.5 . . . no C14 C15 C16 111.3(8) . . . yes C14 C15 H151 108.9 . . . no C14 C15 H152 109.5 . . . no C16 C15 H151 109.1 . . . no C16 C15 H152 109.5 . . . no H151 C15 H152 108.5 . . . no C11 C16 C15 112.6(8) . . . yes C11 C16 H161 108.7 . . . no C11 C16 H162 109.0 . . . no C15 C16 H161 108.5 . . . no C15 C16 H162 109.1 . . . no H161 C16 H162 108.8 . . . no P1 C21 C22 112.5(6) . . . yes P1 C21 C26 119.5(7) . . . yes P1 C21 H21 105.0 . . . no C22 C21 C26 109.7(7) . . . yes C22 C21 H21 104.4 . . . no C26 C21 H21 104.2 . . . no C21 C22 C23 110.1(8) . . . yes C21 C22 H221 109.5 . . . no C21 C22 H222 109.5 . . . no C23 C22 H221 109.5 . . . no C23 C22 H222 109.7 . . . no H221 C22 H222 108.5 . . . no C22 C23 C24 112.9(9) . . . yes C22 C23 H231 109.0 . . . no C22 C23 H232 109.0 . . . no C24 C23 H231 108.5 . . . no C24 C23 H232 108.8 . . . no H231 C23 H232 108.6 . . . no C23 C24 C25 111.3(9) . . . yes C23 C24 H241 108.7 . . . no C23 C24 H242 109.1 . . . no C25 C24 H241 109.5 . . . no C25 C24 H242 109.7 . . . no H241 C24 H242 108.6 . . . no C24 C25 C26 112.2(8) . . . yes C24 C25 H251 108.9 . . . no C24 C25 H252 108.8 . . . no C26 C25 H251 108.9 . . . no C26 C25 H252 109.1 . . . no H251 C25 H252 108.8 . . . no C21 C26 C25 111.9(8) . . . yes C21 C26 H261 108.8 . . . no C21 C26 H262 109.1 . . . no C25 C26 H261 109.0 . . . no C25 C26 H262 109.4 . . . no H261 C26 H262 108.5 . . . no P1 C31 C32 114.0(6) . . . yes P1 C31 C36 118.2(6) . . . yes P1 C31 H31 104.0 . . . no C32 C31 C36 111.1(7) . . . yes C32 C31 H31 104.0 . . . no C36 C31 H31 103.7 . . . no C31 C32 C33 112.0(8) . . . yes C31 C32 H321 108.9 . . . no C31 C32 H322 109.0 . . . no C33 C32 H321 108.7 . . . no C33 C32 H322 109.1 . . . no H321 C32 H322 109.0 . . . no C32 C33 C34 112.2(8) . . . yes C32 C33 H331 108.8 . . . no C32 C33 H332 109.3 . . . no C34 C33 H331 108.8 . . . no C34 C33 H332 109.4 . . . no H331 C33 H332 108.3 . . . no C33 C34 C35 111.4(8) . . . yes C33 C34 H341 108.8 . . . no C33 C34 H342 109.3 . . . no C35 C34 H341 109.3 . . . no C35 C34 H342 109.3 . . . no H341 C34 H342 108.7 . . . no C34 C35 C36 111.2(8) . . . yes C34 C35 H351 109.1 . . . no C34 C35 H352 109.5 . . . no C36 C35 H351 108.9 . . . no C36 C35 H352 109.1 . . . no H351 C35 H352 109.0 . . . no C31 C36 C35 111.2(7) . . . yes C31 C36 H361 108.9 . . . no C31 C36 H362 109.2 . . . no C35 C36 H361 109.3 . . . no C35 C36 H362 109.4 . . . no H361 C36 H362 108.9 . . . no #========================================================END data_cy3aui _audit_creation_method SHELXL-97 _chemical_name_systematic ; [P(cyclohexyl03]2AuI.(P(cyclohexyl)3) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H49.50 Au0.50 I0.50 P1.50' _chemical_formula_weight 582.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.3435(3) _cell_length_b 17.6264(3) _cell_length_c 17.6136(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.8380(10) _cell_angle_gamma 90.00 _cell_volume 5593.42(15) _cell_formula_units_Z 8 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 7911 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2400 _exptl_absorpt_coefficient_mu 3.300 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.3311 _exptl_absorpt_correction_T_max 0.7782 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'Siemens SMART' _diffrn_measurement_method 'Area detector w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 33840 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9820 _reflns_number_gt 7393 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS Sheldrick, (1990)' _computing_structure_refinement 'SHELXL-97 Sheldrick, (1997)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL-97' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+79.4972P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9820 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0938 _refine_ls_R_factor_gt 0.0703 _refine_ls_wR_factor_ref 0.1764 _refine_ls_wR_factor_gt 0.1664 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au Au 0.26843(2) 0.26466(3) 0.95054(3) 0.04299(14) Uani 1 d . . . I I 0.28275(6) 0.19571(7) 1.10887(6) 0.0774(3) Uani 1 d . . . P2 P 0.38791(17) 0.25327(16) 0.92775(17) 0.0430(7) Uani 1 d . . . P1 P 0.14188(15) 0.28757(16) 0.92633(16) 0.0384(6) Uani 1 d . . . C231 C 0.4077(8) 0.3245(8) 0.8574(8) 0.066(4) Uani 1 d . . . H231 H 0.3729 0.3094 0.8097 0.080 Uiso 1 calc R . . C232 C 0.3832(9) 0.4018(8) 0.8700(10) 0.079(5) Uani 1 d . . . H232A H 0.4146 0.4221 0.9168 0.095 Uiso 1 calc R . . H232B H 0.3323 0.3997 0.8793 0.095 Uiso 1 calc R . . C233 C 0.3855(9) 0.4555(9) 0.8046(10) 0.083(5) Uani 1 d . . . H233A H 0.3450 0.4431 0.7617 0.100 Uiso 1 calc R . . H233B H 0.3774 0.5073 0.8215 0.100 Uiso 1 calc R . . C234 C 0.4565(10) 0.4527(10) 0.7768(12) 0.099(6) Uani 1 d . . . H234A H 0.4503 0.4795 0.7272 0.119 Uiso 1 calc R . . H234B H 0.4940 0.4801 0.8136 0.119 Uiso 1 calc R . . C235 C 0.4838(10) 0.3770(9) 0.7667(10) 0.086(5) Uani 1 d . . . H235A H 0.5356 0.3810 0.7600 0.104 Uiso 1 calc R . . H235B H 0.4551 0.3558 0.7188 0.104 Uiso 1 calc R . . C236 C 0.4804(7) 0.3213(8) 0.8324(8) 0.063(4) Uani 1 d . . . H236A H 0.4890 0.2698 0.8152 0.075 Uiso 1 calc R . . H236B H 0.5200 0.3334 0.8764 0.075 Uiso 1 calc R . . C211 C 0.4012(7) 0.1610(7) 0.8830(7) 0.055(3) Uani 1 d . . . H211 H 0.4517 0.1606 0.8706 0.065 Uiso 1 calc R . . C212 C 0.3962(9) 0.0952(7) 0.9376(9) 0.069(4) Uani 1 d . . . H212A H 0.3477 0.0963 0.9534 0.083 Uiso 1 calc R . . H212B H 0.4346 0.1009 0.9841 0.083 Uiso 1 calc R . . C213 C 0.4060(12) 0.0193(9) 0.8996(12) 0.099(6) Uani 1 d . . . H213A H 0.4563 0.0163 0.8886 0.119 Uiso 1 calc R . . H213B H 0.4005 -0.0217 0.9357 0.119 Uiso 1 calc R . . C214 C 0.3514(13) 0.0079(10) 0.8265(14) 0.117(8) Uani 1 d . . . H214A H 0.3012 0.0051 0.8379 0.140 Uiso 1 calc R . . H214B H 0.3618 -0.0402 0.8027 0.140 Uiso 1 calc R . . C215 C 0.3558(11) 0.0733(10) 0.7701(10) 0.099(6) Uani 1 d . . . H215A H 0.3168 0.0670 0.7241 0.118 Uiso 1 calc R . . H215B H 0.4039 0.0719 0.7535 0.118 Uiso 1 calc R . . C216 C 0.3463(8) 0.1509(8) 0.8080(8) 0.069(4) Uani 1 d . . . H216A H 0.3533 0.1916 0.7721 0.083 Uiso 1 calc R . . H216B H 0.2957 0.1549 0.8182 0.083 Uiso 1 calc R . . C221 C 0.4582(6) 0.2568(7) 1.0177(7) 0.054(3) Uani 1 d . . . H221 H 0.4421 0.2171 1.0507 0.064 Uiso 1 calc R . . C222 C 0.4555(9) 0.3291(8) 1.0629(8) 0.069(4) Uani 1 d . . . H222A H 0.4038 0.3405 1.0661 0.083 Uiso 1 calc R . . H222B H 0.4744 0.3712 1.0358 0.083 Uiso 1 calc R . . C223 C 0.5017(10) 0.3224(10) 1.1449(9) 0.089(5) Uani 1 d . . . H223A H 0.5031 0.3716 1.1710 0.106 Uiso 1 calc R . . H223B H 0.4786 0.2856 1.1746 0.106 Uiso 1 calc R . . C224 C 0.5810(10) 0.2970(13) 1.1419(11) 0.112(7) Uani 1 d . . . H224A H 0.6063 0.3374 1.1187 0.135 Uiso 1 calc R . . H224B H 0.6082 0.2888 1.1947 0.135 Uiso 1 calc R . . C225 C 0.5825(8) 0.2246(11) 1.0955(8) 0.081(5) Uani 1 d . . . H225A H 0.5616 0.1828 1.1212 0.098 Uiso 1 calc R . . H225B H 0.6340 0.2117 1.0929 0.098 Uiso 1 calc R . . C226 C 0.5376(7) 0.2349(9) 1.0136(8) 0.067(4) Uani 1 d . . . H226A H 0.5602 0.2746 0.9867 0.081 Uiso 1 calc R . . H226B H 0.5378 0.1875 0.9845 0.081 Uiso 1 calc R . . C131 C 0.0890(7) 0.1982(7) 0.9021(7) 0.051(3) Uani 1 d . . . H131 H 0.0454 0.2108 0.8617 0.062 Uiso 1 calc R . . C132 C 0.1356(8) 0.1410(8) 0.8665(9) 0.074(4) Uani 1 d . . . H132A H 0.1790 0.1261 0.9051 0.089 Uiso 1 calc R . . H132B H 0.1532 0.1643 0.8228 0.089 Uiso 1 calc R . . C133 C 0.0878(11) 0.0689(9) 0.8382(10) 0.098(6) Uani 1 d . . . H133A H 0.0456 0.0832 0.7979 0.117 Uiso 1 calc R . . H133B H 0.1180 0.0319 0.8163 0.117 Uiso 1 calc R . . C134 C 0.0606(10) 0.0347(9) 0.9051(10) 0.087(5) Uani 1 d . . . H134A H 0.0304 -0.0101 0.8877 0.105 Uiso 1 calc R . . H134B H 0.1031 0.0182 0.9440 0.105 Uiso 1 calc R . . C135 C 0.0158(10) 0.0895(9) 0.9405(11) 0.087(5) Uani 1 d . . . H135A H -0.0009 0.0652 0.9843 0.104 Uiso 1 calc R . . H135B H -0.0284 0.1033 0.9024 0.104 Uiso 1 calc R . . C136 C 0.0592(8) 0.1621(8) 0.9688(8) 0.067(4) Uani 1 d . . . H136A H 0.0265 0.1979 0.9887 0.080 Uiso 1 calc R . . H136B H 0.1005 0.1496 1.0109 0.080 Uiso 1 calc R . . C121 C 0.1083(6) 0.3290(7) 1.0085(6) 0.045(3) Uani 1 d . . . H121 H 0.1069 0.2864 1.0449 0.054 Uiso 1 calc R . . C122 C 0.0298(7) 0.3600(9) 0.9917(8) 0.066(4) Uani 1 d . . . H122A H -0.0042 0.3208 0.9666 0.079 Uiso 1 calc R . . H122B H 0.0273 0.4031 0.9561 0.079 Uiso 1 calc R . . C123 C 0.0055(9) 0.3859(11) 1.0667(10) 0.093(6) Uani 1 d . . . H123A H -0.0445 0.4077 1.0539 0.112 Uiso 1 calc R . . H123B H 0.0033 0.3417 1.1000 0.112 Uiso 1 calc R . . C124 C 0.0582(10) 0.4443(11) 1.1104(10) 0.096(6) Uani 1 d . . . H124A H 0.0577 0.4903 1.0791 0.116 Uiso 1 calc R . . H124B H 0.0421 0.4579 1.1586 0.116 Uiso 1 calc R . . C125 C 0.1347(10) 0.4122(9) 1.1278(8) 0.079(5) Uani 1 d . . . H125A H 0.1356 0.3685 1.1624 0.094 Uiso 1 calc R . . H125B H 0.1689 0.4505 1.1546 0.094 Uiso 1 calc R . . C126 C 0.1614(7) 0.3870(8) 1.0535(7) 0.059(3) Uani 1 d . . . H126A H 0.1647 0.4313 1.0208 0.071 Uiso 1 calc R . . H126B H 0.2111 0.3646 1.0673 0.071 Uiso 1 calc R . . C111 C 0.1089(6) 0.3487(7) 0.8411(6) 0.047(3) Uani 1 d . . . H111 H 0.0545 0.3545 0.8358 0.057 Uiso 1 calc R . . C112 C 0.1241(8) 0.3124(8) 0.7666(7) 0.059(3) Uani 1 d . . . H112A H 0.0965 0.2646 0.7575 0.071 Uiso 1 calc R . . H112B H 0.1771 0.3006 0.7729 0.071 Uiso 1 calc R . . C113 C 0.1013(9) 0.3648(9) 0.6959(8) 0.073(4) Uani 1 d . . . H113A H 0.1163 0.3414 0.6507 0.087 Uiso 1 calc R . . H113B H 0.0472 0.3702 0.6848 0.087 Uiso 1 calc R . . C114 C 0.1361(9) 0.4420(10) 0.7087(9) 0.083(5) Uani 1 d . . . H114A H 0.1900 0.4373 0.7131 0.100 Uiso 1 calc R . . H114B H 0.1174 0.4742 0.6639 0.100 Uiso 1 calc R . . C115 C 0.1196(10) 0.4782(9) 0.7795(9) 0.084(5) Uani 1 d . . . H115A H 0.0663 0.4884 0.7724 0.101 Uiso 1 calc R . . H115B H 0.1458 0.5268 0.7877 0.101 Uiso 1 calc R . . C116 C 0.1432(9) 0.4276(7) 0.8512(8) 0.068(4) Uani 1 d . . . H116A H 0.1974 0.4229 0.8620 0.081 Uiso 1 calc R . . H116B H 0.1284 0.4522 0.8959 0.081 Uiso 1 calc R . . P3 P -0.1811(3) 0.2632(3) 0.9102(3) 0.0874(13) Uani 1 d . . . C321 C -0.2322(11) 0.3510(10) 0.9315(9) 0.087(5) Uani 1 d . . . H321 H -0.1976 0.3930 0.9265 0.105 Uiso 1 calc R . . C322 C -0.2390(13) 0.3527(14) 1.0141(10) 0.122(8) Uani 1 d . . . H322A H -0.1905 0.3424 1.0465 0.147 Uiso 1 calc R . . H322B H -0.2734 0.3128 1.0239 0.147 Uiso 1 calc R . . C323 C -0.2672(15) 0.4292(12) 1.0356(11) 0.126(9) Uani 1 d . . . H323A H -0.2755 0.4273 1.0889 0.151 Uiso 1 calc R . . H323B H -0.2294 0.4679 1.0329 0.151 Uiso 1 calc R . . C324 C -0.3388(14) 0.4513(12) 0.9821(14) 0.124(8) Uani 1 d . . . H324A H -0.3783 0.4158 0.9887 0.148 Uiso 1 calc R . . H324B H -0.3538 0.5022 0.9954 0.148 Uiso 1 calc R . . C325 C -0.3289(13) 0.4502(12) 0.9031(12) 0.119(7) Uani 1 d . . . H325A H -0.2925 0.4889 0.8961 0.143 Uiso 1 calc R . . H325B H -0.3761 0.4632 0.8694 0.143 Uiso 1 calc R . . C326 C -0.3026(10) 0.3728(10) 0.8789(9) 0.091(5) Uani 1 d . . . H326A H -0.3408 0.3344 0.8812 0.109 Uiso 1 calc R . . H326B H -0.2944 0.3755 0.8255 0.109 Uiso 1 calc R . . C331 C -0.2470(10) 0.1835(10) 0.9166(12) 0.095(6) Uani 1 d . . . H331 H -0.2715 0.2023 0.9584 0.114 Uiso 1 calc R . . C332 C -0.2092(12) 0.1172(13) 0.9536(14) 0.128(8) Uani 1 d . . . H332A H -0.1790 0.1324 1.0033 0.154 Uiso 1 calc R . . H332B H -0.1755 0.0976 0.9212 0.154 Uiso 1 calc R . . C333 C -0.2624(12) 0.0525(11) 0.9680(12) 0.114(7) Uani 1 d . . . H333A H -0.2341 0.0052 0.9770 0.136 Uiso 1 calc R . . H333B H -0.2814 0.0641 1.0151 0.136 Uiso 1 calc R . . C334 C -0.3253(13) 0.0405(12) 0.9048(16) 0.137(9) Uani 1 d . . . H334A H -0.3081 0.0115 0.8641 0.164 Uiso 1 calc R . . H334B H -0.3622 0.0093 0.9241 0.164 Uiso 1 calc R . . C335 C -0.3612(11) 0.1077(11) 0.8712(13) 0.113(7) Uani 1 d . . . H335A H -0.3931 0.1269 0.9057 0.135 Uiso 1 calc R . . H335B H -0.3935 0.0937 0.8224 0.135 Uiso 1 calc R . . C336 C -0.3115(10) 0.1719(9) 0.8550(10) 0.087(5) Uani 1 d . . . H336A H -0.2943 0.1613 0.8067 0.104 Uiso 1 calc R . . H336B H -0.3406 0.2189 0.8477 0.104 Uiso 1 calc R . . C311 C -0.1829(9) 0.2718(8) 0.8058(9) 0.073(4) Uani 1 d . . . H311 H -0.2353 0.2742 0.7786 0.088 Uiso 1 calc R . . C312 C -0.1423(14) 0.3448(11) 0.7869(11) 0.118(7) Uani 1 d . . . H312A H -0.1694 0.3893 0.8002 0.142 Uiso 1 calc R . . H312B H -0.0925 0.3459 0.8189 0.142 Uiso 1 calc R . . C313 C -0.1362(15) 0.3493(12) 0.7065(13) 0.136(9) Uani 1 d . . . H313A H -0.1058 0.3936 0.6994 0.164 Uiso 1 calc R . . H313B H -0.1857 0.3575 0.6754 0.164 Uiso 1 calc R . . C314 C -0.1026(11) 0.2802(11) 0.6766(12) 0.101(6) Uani 1 d . . . H314A H -0.1088 0.2839 0.6203 0.121 Uiso 1 calc R . . H314B H -0.0493 0.2793 0.6979 0.121 Uiso 1 calc R . . C315 C -0.1353(15) 0.2099(13) 0.6962(14) 0.132(8) Uani 1 d . . . H315A H -0.1833 0.2031 0.6616 0.159 Uiso 1 calc R . . H315B H -0.1032 0.1678 0.6870 0.159 Uiso 1 calc R . . C316 C -0.1461(15) 0.2065(11) 0.7750(17) 0.155(12) Uani 1 d . . . H316A H -0.0974 0.1995 0.8082 0.185 Uiso 1 calc R . . H316B H -0.1754 0.1609 0.7804 0.185 Uiso 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 Au 0.0393(2) 0.0419(2) 0.0500(3) -0.0029(2) 0.01392(18) -0.0002(2) I 0.0804(7) 0.0981(8) 0.0575(6) 0.0276(5) 0.0226(5) 0.0083(6) P2 0.0449(16) 0.0406(17) 0.0463(16) -0.0004(13) 0.0159(13) -0.0007(12) P1 0.0380(15) 0.0389(15) 0.0396(15) 0.0022(12) 0.0110(12) 0.0010(12) C231 0.079(10) 0.061(9) 0.066(9) 0.004(7) 0.034(8) -0.004(7) C232 0.081(11) 0.056(9) 0.111(13) 0.017(9) 0.046(10) 0.017(8) C233 0.093(12) 0.058(9) 0.104(13) 0.028(9) 0.032(10) 0.012(8) C234 0.100(14) 0.088(13) 0.119(15) 0.044(11) 0.043(12) 0.007(10) C235 0.103(13) 0.083(11) 0.087(11) 0.008(9) 0.056(10) -0.007(10) C236 0.059(8) 0.069(9) 0.066(8) 0.017(7) 0.027(7) 0.010(7) C211 0.052(7) 0.054(8) 0.060(8) -0.011(6) 0.017(6) -0.003(6) C212 0.089(11) 0.049(8) 0.075(10) -0.002(7) 0.028(8) 0.000(7) C213 0.131(17) 0.045(9) 0.134(17) -0.018(10) 0.059(14) -0.003(10) C214 0.140(19) 0.063(12) 0.16(2) -0.045(13) 0.059(17) -0.017(12) C215 0.114(15) 0.087(13) 0.089(12) -0.040(11) 0.003(11) 0.002(11) C216 0.064(9) 0.072(10) 0.068(9) -0.012(7) 0.004(7) 0.017(7) C221 0.044(6) 0.057(8) 0.064(8) 0.006(6) 0.021(6) 0.001(6) C222 0.081(10) 0.068(9) 0.057(8) -0.014(7) 0.005(7) -0.005(8) C223 0.105(14) 0.089(12) 0.067(10) -0.017(9) 0.003(9) -0.020(10) C224 0.079(13) 0.17(2) 0.074(12) -0.003(13) -0.013(10) -0.035(13) C225 0.046(8) 0.133(15) 0.062(9) 0.005(10) 0.001(7) 0.009(9) C226 0.053(8) 0.090(10) 0.061(8) 0.004(8) 0.013(6) 0.012(7) C131 0.050(7) 0.047(7) 0.055(7) 0.005(6) 0.005(6) -0.008(6) C132 0.078(10) 0.061(9) 0.090(11) -0.030(8) 0.028(8) -0.028(8) C133 0.130(16) 0.071(11) 0.101(13) -0.027(10) 0.047(12) -0.040(11) C134 0.107(13) 0.053(9) 0.101(13) -0.002(9) 0.016(11) -0.025(9) C135 0.093(12) 0.067(10) 0.107(13) 0.008(9) 0.036(10) -0.026(9) C136 0.074(9) 0.064(9) 0.067(9) 0.000(7) 0.026(7) -0.004(7) C121 0.043(6) 0.055(7) 0.040(6) 0.010(5) 0.013(5) 0.005(5) C122 0.053(8) 0.083(10) 0.063(8) 0.008(7) 0.017(7) 0.010(7) C123 0.074(11) 0.121(15) 0.096(13) -0.001(11) 0.046(10) 0.027(11) C124 0.111(14) 0.109(14) 0.078(11) -0.010(10) 0.042(11) 0.043(12) C125 0.109(13) 0.079(10) 0.054(8) -0.006(7) 0.031(9) 0.014(9) C126 0.065(8) 0.063(8) 0.051(7) -0.014(6) 0.013(6) 0.002(7) C111 0.042(6) 0.059(8) 0.044(6) 0.011(6) 0.015(5) 0.009(5) C112 0.071(9) 0.065(9) 0.044(7) 0.000(6) 0.016(6) 0.000(7) C113 0.087(11) 0.087(11) 0.046(8) 0.015(7) 0.018(7) 0.007(9) C114 0.077(11) 0.104(13) 0.073(10) 0.035(9) 0.027(9) 0.009(9) C115 0.116(14) 0.061(9) 0.078(11) 0.024(8) 0.024(10) 0.013(9) C116 0.084(10) 0.052(8) 0.062(8) 0.015(7) 0.000(7) 0.001(7) P3 0.073(3) 0.086(3) 0.099(3) 0.010(3) 0.006(2) -0.013(2) C321 0.120(15) 0.072(11) 0.072(11) -0.005(8) 0.027(10) 0.003(10) C322 0.142(19) 0.15(2) 0.069(12) 0.016(13) -0.004(12) -0.028(16) C323 0.20(3) 0.093(15) 0.077(13) -0.031(11) 0.017(15) -0.044(16) C324 0.16(2) 0.098(15) 0.119(18) -0.007(14) 0.056(17) 0.017(15) C325 0.15(2) 0.093(15) 0.111(17) 0.008(12) 0.021(15) 0.018(14) C326 0.111(14) 0.093(13) 0.069(10) -0.021(9) 0.020(10) -0.023(11) C331 0.083(12) 0.072(11) 0.120(15) 0.022(10) -0.004(10) -0.017(9) C332 0.106(16) 0.120(18) 0.14(2) 0.021(15) -0.019(14) -0.008(14) C333 0.130(18) 0.078(13) 0.125(17) 0.039(12) 0.004(14) -0.017(12) C334 0.122(19) 0.090(16) 0.19(3) 0.045(16) 0.012(18) -0.019(14) C335 0.083(13) 0.101(15) 0.150(19) -0.029(14) 0.012(13) -0.024(11) C336 0.107(14) 0.071(10) 0.078(11) 0.000(9) 0.006(10) -0.015(10) C311 0.066(9) 0.063(9) 0.092(11) -0.008(8) 0.019(8) -0.011(8) C312 0.18(2) 0.081(13) 0.099(14) -0.009(11) 0.050(15) -0.033(14) C313 0.21(3) 0.103(16) 0.115(17) 0.012(13) 0.085(18) -0.010(17) C314 0.103(14) 0.098(15) 0.112(15) -0.005(12) 0.046(12) 0.000(11) C315 0.17(2) 0.106(17) 0.129(19) -0.022(14) 0.058(18) 0.002(16) C316 0.20(3) 0.078(13) 0.23(3) -0.029(16) 0.16(2) -0.023(15) _geom_special_details ; ? ; 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 Au P2 2.310(3) . ? Au P1 2.316(3) . ? Au I 3.0080(10) . ? P2 C211 1.844(12) . ? P2 C221 1.846(13) . ? P2 C231 1.847(13) . ? P1 C121 1.828(11) . ? P1 C111 1.855(11) . ? P1 C131 1.857(12) . ? C231 C232 1.465(19) . ? C231 C236 1.483(18) . ? C232 C233 1.499(19) . ? C233 C234 1.47(2) . ? C234 C235 1.45(2) . ? C235 C236 1.527(19) . ? C211 C216 1.514(18) . ? C211 C212 1.520(18) . ? C212 C213 1.522(19) . ? C213 C214 1.49(3) . ? C214 C215 1.53(3) . ? C215 C216 1.55(2) . ? C221 C222 1.509(18) . ? C221 C226 1.521(16) . ? C222 C223 1.54(2) . ? C223 C224 1.53(2) . ? C224 C225 1.52(3) . ? C225 C226 1.532(18) . ? C221 C226 1.525(17) . ? C131 C132 1.531(18) . ? C132 C133 1.571(19) . ? C133 C134 1.49(2) . ? C134 C135 1.48(2) . ? C135 C136 1.54(2) . ? C121 C122 1.516(16) . ? C121 C126 1.528(17) . ? C122 C123 1.541(19) . ? C123 C124 1.52(2) . ? C124 C125 1.49(2) . ? C125 C126 1.547(17) . ? C111 C116 1.523(18) . ? C111 C112 1.531(16) . ? C112 C113 1.545(17) . ? C113 C114 1.50(2) . ? C114 C115 1.48(2) . ? C115 C116 1.540(18) . ? P3 C311 1.839(16) . ? P3 C331 1.872(16) . ? P3 C321 1.883(17) . ? C321 C322 1.48(2) . ? C321 C326 1.49(2) . ? C322 C323 1.52(3) . ? C323 C324 1.52(3) . ? C324 C325 1.44(3) . ? C325 C326 1.53(2) . ? C331 C332 1.45(2) . ? C331 C336 1.46(2) . ? C332 C333 1.55(3) . ? C333 C334 1.46(3) . ? C334 C335 1.43(3) . ? C335 C336 1.51(2) . ? C311 C316 1.49(2) . ? C311 C312 1.55(2) . ? C312 C313 1.44(2) . ? C313 C314 1.50(3) . ? C314 C315 1.45(3) . ? C315 C316 1.44(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au P2 159.11(10) . . ? P2 Au I 101.87(8) . . ? P1 Au I 98.68(7) . . ? C211 P2 C221 105.6(6) . . ? C211 P2 C231 104.7(6) . . ? C221 P2 C231 111.1(6) . . ? C211 P2 Au 110.9(4) . . ? C221 P2 Au 112.4(4) . . ? C231 P2 Au 111.7(5) . . ? C121 P1 C111 107.6(5) . . ? C121 P1 C131 106.3(5) . . ? C111 P1 C131 103.3(6) . . ? C121 P1 Au 113.5(4) . . ? C111 P1 Au 114.4(4) . . ? C31 P1 Au 110.9(4) . . ? C232 C231 C236 113.4(12) . . ? C232 C231 P2 115.2(10) . . ? C236 C231 P2 118.4(10) . . ? C231 C232 C233 114.6(13) . . ? C234 C233 C232 112.9(14) . . ? C235 C234 C233 114.8(15) . . ? C234 C235 C236 115.7(13) . . ? C231 C236 C235 111.6(12) . . ? C216 C211 C212 110.7(12) . . ? C216 C211 P2 110.9(9) . . ? C212 C211 P2 111.9(9) . . ? C211 C212 C213 111.5(12) . . ? C214 C213 C212 112.5(16) . . ? C213 C214 C215 110.5(16) . . ? C214 C215 C216 111.2(14) . . ? C211 C216 C215 111.7(12) . . ? C222 C221 C226 111.5(12) . . ? C222 C221 P2 113.2(9) . . ? C226 C221 P2 118.1(9) . . ? C221 C222 C223 111.3(13) . . ? C224 C223 C222 110.5(14) . . ? C225 C224 C223 112.2(14) . . ? C224 C225 C226 110.3(14) . . ? C221 C226 C225 109.6(11) . . ? C136 C131 C132 110.4(11) . . ? C136 C131 P1 115.1(9) . . ? C132 C131 P1 110.2(8) . . ? C131 C132 C133 110.0(12) . . ? C134 C133 C132 109.0(13) . . ? C135 C134 C133 111.3(14) . . ? C134 C135 C136 112.6(13) . . ? C131 C136 C135 109.6(12) . . ? C122 C121 C126 110.4(11) . . ? C122 C121 P1 116.0(8) . . ? C126 C121 P1 113.6(8) . . ? C121 C122 C123 110.9(12) . . ? C124 C123 C122 112.0(14) . . ? C125 C124 C123 109.4(14) . . ? C124 C125 C126 111.7(13) . . ? C121 C126 C125 111.0(11) . . ? C116 C111 C112 110.2(10) . . ? C116 C111 P1 111.8(8) . . ? C112 C111 P1 111.5(8) . . ? C111 C112 C113 112.1(11) . . ? C114 C113 C112 112.2(12) . . ? C115 C114 C113 111.6(13) . . ? C114 C115 C116 111.8(13) . . ? C111 C116 C115 112.7(12) . . ? C311 P3 C331 103.4(8) . . ? C311 P3 C321 102.4(7) . . ? C331 P3 C321 104.7(9) . . ? C322 C321 C326 112.4(16) . . ? C322 C321 P3 110.4(14) . . ? C326 C321 P3 119.6(12) . . ? C321 C322 C323 110.9(17) . . ? C324 C323 C322 111.7(16) . . ? C325 C324 C323 110(2) . . ? C324 C325 C326 112.7(17) . . ? C321 C326 C325 109.7(15) . . ? C332 C331 C336 118.3(16) . . ? C332 C331 P3 111.9(13) . . ? C336 C331 P3 120.1(13) . . ? C331 C332 C333 113.7(17) . . ? C334 C333 C332 114.4(17) . . ? C335 C334 C333 116(2) . . ? C334 C335 C336 116.9(17) . . ? C331 C336 C335 113.3(15) . . ? C316 C311 C312 107.1(14) . . ? C316 C311 P3 112.1(15) . . ? C312 C311 P3 111.3(11) . . ? C313 C312 C311 112.7(17) . . ? C312 C313 C314 114.2(19) . . ? C315 C314 C313 113.3(17) . . ? C316 C315 C314 113.8(19) . . ? C315 C316 C311 118(2) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 2.531 _refine_diff_density_min -1.493 _refine_diff_density_rms 0.153 #===============================================END data_cy2aui _audit_creation_date 97-11-21 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source dmf_solution _chemical_name_systematic ; Iodobis(tricyclohexylphosphine)gold(I) ; _chemical_name_common ? _chemical_formula_analytical [((C6H11)3P)2AuI] _chemical_formula_moiety ? _chemical_formula_structural [Cy3P)2AuI] _chemical_formula_sum C36_H66_Au_P2_I _chemical_formula_weight 884.74 _chemical_melting_point ? _computing_data_collection 'Enraf-Nonius cad4 software' _computing_cell_refinement 'Enraf_Nonius cad4 software' _computing_data_reduction xtal_DIFDAT_SORTRF_ADDREF_ABSORB _computing_structure_solution xtal _computing_structure_refinement xtal_CRYLSQ _computing_molecular_graphics xtal _computing_publication_material xtal_BONDLA_CIFIO _cell_length_a 9.211(6) _cell_length_b 9.727(4) _cell_length_c 23.216(3) _cell_angle_alpha 94.01(2) _cell_angle_beta 97.61(4) _cell_angle_gamma 114.88(5) _cell_volume 1852.0(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293 _cell_measurement_reflns_used 6 _cell_measurement_theta_min 17.5 _cell_measurement_theta_max 21.9 _cell_special_details ; ? ; _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -P_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _exptl_crystal_description prism _exptl_crystal_preparation ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 888 _exptl_absorpt_process_details ? _exptl_absorpt_coefficient_mu 4.9 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.32 _exptl_absorpt_correction_T_max 0.57 _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type xray_tube _diffrn_radiation_source ? _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device CAD4 _diffrn_measurement_method 2theta/theta _diffrn_standards_number 6 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 1hour _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 7 0 0 -7 0 0 0 9 0 0 -9 0 0 0 24 0 0 -24 loop_ _diffrn_attenuator_code _diffrn_attenuator_scale 1 13.54 _diffrn_reflns_number 8827 _diffrn_reflns_av_R_equivalents .015 _diffrn_reflns_av_sigmaI/netI .03 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 2 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_reduction_process equatorial_monochr_Lp loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 74 .002 .002 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 132 0 0 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 Au ? 0 2 -2.688 8.798 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 I ? 0 2 -.726 1.812 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 P ? 0 4 .09 .095 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Au .06893(4) .34044(4) .250951(15) .03209(15) Uani ? ? I -.24556(8) .34219(8) .24768(3) .0533(3) Uani ? ? P1 .1328(3) .2704(2) .34204(9) .0302(8) Uani ? ? P2 .1559(3) .3900(2) .16173(10) .0316(9) Uani ? ? C121 .1519(10) .0907(8) .3287(4) .033(3) Uani ? ? C122 .0086(11) -.0303(10) .2844(4) .044(4) Uani ? ? C123 .0394(12) -.1708(10) .2679(5) .059(5) Uani ? ? C124 .0830(12) -.2405(10) .3231(5) .054(5) Uani ? ? C125 .2265(12) -.1174(11) .3643(5) .051(5) Uani ? ? C126 .1957(11) .0237(10) .3826(4) .047(4) Uani ? ? C111 .3321(9) .4039(9) .3851(4) .032(3) Uani ? ? C112 .4728(10) .4150(10) .3545(4) .046(4) Uani ? ? C113 .6369(11) .5326(12) .3892(5) .060(5) Uani ? ? C114 .6431(12) .6921(11) .4016(5) .055(5) Uani ? ? C115 .5039(12) .6816(10) .4330(5) .054(5) Uani ? ? C116 .3397(10) .5660(10) .3976(4) .044(4) Uani ? ? C131 -.0099(10) .2583(8) .3924(4) .033(3) Uani ? ? C132 .0459(11) .2662(11) .4569(4) .051(4) Uani ? ? C133 -.0806(13) .2712(12) .4928(5) .064(5) Uani ? ? C134 -.2467(13) .1344(13) .4733(5) .069(6) Uani ? ? C135 -.2998(12) .1325(13) .4066(5) .063(5) Uani ? ? C136 -.1753(11) .1235(10) .3709(4) .044(4) Uani ? ? C211 .0228(10) .4247(10) .1038(4) .035(4) Uani ? ? C212 -.1412(11) .2817(10) .0853(4) .043(4) Uani ? ? C213 -.2520(12) .3172(13) .0385(4) .058(5) Uani ? ? C214 -.2716(13) .4631(14) .0584(5) .065(6) Uani ? ? C215 -.1098(12) .5999(11) .0764(5) .051(5) Uani ? ? C216 .0011(11) .5698(10) .1228(4) .044(4) Uani ? ? C231 .3607(10) .5518(10) .1717(4) .039(4) Uani ? ? C232 .4140(12) .6280(10) .1152(4) .050(4) Uani ? ? C233 .5899(13) .7445(12) .1291(5) .065(6) Uani ? ? C234 .6181(13) .8681(11) .1789(5) .062(5) Uani ? ? C235 .5644(13) .8040(12) .2316(5) .068(6) Uani ? ? C236 .3880(12) .6767(11) .2209(4) .053(5) Uani ? ? C221 .1747(10) .2219(9) .1286(4) .035(4) Uani ? ? C222 .2227(14) .2198(11) .0697(4) .053(5) Uani ? ? C223 .2201(17) .0712(13) .0454(5) .070(6) Uani ? ? C224 .3292(16) .0312(13) .0871(5) .071(6) Uani ? ? C225 .2764(14) .0212(12) .1490(5) .064(6) Uani ? ? C226 .2850(13) .1792(12) .1701(4) .055(5) Uani ? ? H121 .24779 .12013 .31097 .04020 Uiso ? ? H111 .34610 .36642 .42135 .03900 Uiso ? ? H131 -.01564 .35424 .39090 .04010 Uiso ? ? H122a -.08759 -.06405 .30244 .04250 Uiso ? ? H122b -.01231 .01365 .25062 .04250 Uiso ? ? H123a -.05075 -.24776 .24054 .06670 Uiso ? ? H123b .13245 -.13838 .24635 .06670 Uiso ? ? H124a -.00836 -.27852 .34266 .06630 Uiso ? ? H124b .10662 -.32556 .31181 .06630 Uiso ? ? H125a .25620 -.15669 .39866 .06650 Uiso ? ? H125b .32173 -.08174 .34496 .06650 Uiso ? ? H126a .10630 -.01061 .40398 .05320 Uiso ? ? H126b .28886 .09967 .40881 .05320 Uiso ? ? H112a .47296 .31584 .34920 .05360 Uiso ? ? H112b .45816 .44445 .31656 .05360 Uiso ? ? H113a .65720 .49486 .42554 .06500 Uiso ? ? H113b .72120 .53622 .36757 .06500 Uiso ? ? H114a .74612 .76006 .42650 .06030 Uiso ? ? H114b .63548 .73291 .36630 .06030 Uiso ? ? H115a .51817 .64808 .47087 .05940 Uiso ? ? H115b .50337 .77874 .43969 .05940 Uiso ? ? H116a .25349 .55864 .41941 .04960 Uiso ? ? H116b .31871 .60093 .36171 .04960 Uiso ? ? H132a .06411 .17692 .46363 .05630 Uiso ? ? H132b .14758 .35432 .47071 .05630 Uiso ? ? H133a -.04318 .27087 .53341 .07370 Uiso ? ? H133b -.09098 .36257 .48869 .07370 Uiso ? ? H134a -.24153 .04114 .47988 .07760 Uiso ? ? H134b -.32486 .14522 .49464 .07760 Uiso ? ? H135a -.40532 .04284 .39255 .08370 Uiso ? ? H135b -.31666 .22013 .40004 .08370 Uiso ? ? H136a -.16797 .02823 .37498 .05130 Uiso ? ? H136b -.21287 .12107 .33005 .05130 Uiso ? ? H211 .07671 .44609 .06946 .04610 Uiso ? ? H231 .43155 .50383 .18213 .04870 Uiso ? ? H221 .06235 .14453 .12031 .04630 Uiso ? ? H212a -.12420 .19648 .07041 .05100 Uiso ? ? H212b -.19095 .25704 .11924 .05100 Uiso ? ? H213a -.20737 .32969 .00343 .06660 Uiso ? ? H213b -.35771 .22829 .02933 .06660 Uiso ? ? H214a -.34074 .48099 .02911 .08680 Uiso ? ? H214b -.32763 .44394 .09297 .08680 Uiso ? ? H215a -.06012 .62201 .04283 .07170 Uiso ? ? H215b -.12508 .68708 .09101 .07170 Uiso ? ? H216a .10457 .65734 .13326 .05560 Uiso ? ? H216b -.04610 .55393 .15856 .05560 Uiso ? ? H232a .39327 .55034 .08410 .06070 Uiso ? ? H232b .34441 .67799 .10419 .06070 Uiso ? ? H233a .65679 .69338 .14175 .08400 Uiso ? ? H233b .62369 .78834 .09514 .08400 Uiso ? ? H234a .72982 .94163 .18704 .06960 Uiso ? ? H234b .55462 .92264 .16585 .06960 Uiso ? ? H235a .63436 .75361 .24657 .07360 Uiso ? ? H235b .57865 .87904 .26272 .07360 Uiso ? ? H236a .35997 .63375 .25576 .06110 Uiso ? ? H236b .31705 .72425 .20931 .06110 Uiso ? ? H222a .15716 .24992 .04200 .07120 Uiso ? ? H222b .33516 .30243 .07338 .07120 Uiso ? ? H223a .11162 -.00801 .03999 .09500 Uiso ? ? H223b .25501 .07656 .00795 .09500 Uiso ? ? H224a .32637 -.06670 .07323 .09610 Uiso ? ? H224b .43996 .10601 .09220 .09610 Uiso ? ? H225a .16717 -.05770 .14516 .08600 Uiso ? ? H225b .34560 -.00478 .17614 .08600 Uiso ? ? H226a .25155 .17366 .20855 .07530 Uiso ? ? H226b .39335 .25320 .17518 .07530 Uiso ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Au .0358(2) .03134(17) .02915(18) .01568(14) .00242(14) .00333(12) I .0405(4) .0746(5) .0542(4) .0329(3) .0108(3) .0116(3) P1 .0290(11) .0292(10) .0292(12) .0108(9) .0010(9) .0040(9) P2 .0341(12) .0324(11) .0296(12) .0170(9) .0018(10) .0040(9) C121 .034(5) .027(4) .034(5) .011(4) .002(4) .008(3) C122 .044(5) .037(5) .047(6) .018(4) -.006(5) -.004(4) C123 .057(7) .042(5) .068(7) .021(5) -.005(6) -.019(5) C124 .053(6) .037(5) .069(7) .020(5) .002(5) .003(5) C125 .054(6) .046(5) .058(7) .027(5) .005(5) .007(5) C126 .046(6) .040(5) .048(6) .020(4) -.011(5) -.006(4) C111 .028(4) .034(4) .031(5) .012(4) -.001(4) .003(3) C112 .030(5) .049(5) .052(6) .015(4) .002(4) -.012(4) C113 .024(5) .069(7) .075(8) .016(5) .000(5) -.019(6) C114 .040(6) .041(5) .066(7) .003(4) .001(5) .005(5) C115 .047(6) .043(5) .058(7) .015(5) -.003(5) -.014(5) C116 .033(5) .040(5) .053(6) .015(4) .000(4) -.008(4) C131 .035(5) .028(4) .032(5) .009(4) .006(4) .005(3) C132 .041(6) .055(6) .045(6) .010(5) .006(5) .000(5) C133 .057(7) .070(7) .050(7) .012(6) .021(5) -.011(5) C134 .047(6) .076(8) .067(8) .010(6) .026(6) -.010(6) C135 .029(5) .075(7) .071(8) .011(5) .014(5) .002(6) C136 .036(5) .045(5) .042(6) .010(4) .003(4) .006(4) C211 .037(5) .050(5) .024(4) .026(4) .003(4) -.002(4) C212 .041(5) .048(5) .035(5) .019(4) -.004(4) -.002(4) C213 .040(6) .087(8) .040(6) .029(6) -.005(5) -.010(5) C214 .055(7) .096(9) .062(8) .052(7) .006(6) .011(6) C215 .052(6) .059(6) .059(7) .037(5) .013(5) .023(5) C216 .043(5) .040(5) .052(6) .023(4) .004(5) .004(4) C231 .032(5) .044(5) .042(5) .020(4) -.002(4) -.001(4) C232 .059(6) .040(5) .046(6) .014(5) .016(5) .002(4) C233 .060(7) .059(7) .079(9) .021(6) .030(6) .027(6) C234 .050(6) .041(6) .078(8) .005(5) .006(6) .020(5) C235 .046(6) .062(7) .075(8) .014(5) -.016(6) -.020(6) C236 .046(6) .054(6) .046(6) .014(5) .000(5) -.008(5) C221 .042(5) .033(4) .035(5) .020(4) .004(4) .005(4) C222 .084(8) .053(6) .037(6) .043(6) .015(5) .009(4) C223 .122(11) .067(7) .045(6) .063(7) .021(7) .007(5) C224 .096(9) .066(7) .073(8) .057(7) .019(7) .001(6) C225 .080(8) .068(7) .066(8) .058(6) .007(6) .003(6) C226 .072(7) .069(7) .044(6) .054(6) -.001(5) .000(5) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details sfls:_F____sigma_weight______full_matrix _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef .00000 _refine_ls_extinction_expression ? _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack 0 _refine_ls_number_reflns 5767 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .038 _refine_ls_R_factor_obs .031 _refine_ls_wR_factor_all .055 _refine_ls_wR_factor_obs .054 _refine_ls_goodness_of_fit_all 2.164 _refine_ls_goodness_of_fit_obs 2.317 _refine_ls_shift/esd_max .001 _refine_ls_shift/esd_mean . _refine_diff_density_min -.681 _refine_diff_density_max .693 _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au I 2.895(2) . . ? Au P1 2.344(2) . . ? Au P2 2.328(2) . . ? P1 C121 1.838(10) . . ? P1 C111 1.839(7) . . ? P1 C131 1.845(10) . . ? P2 C211 1.844(10) . . ? P2 C231 1.850(7) . . ? P2 C221 1.843(10) . . ? C121 C122 1.532(10) . . ? C121 C126 1.534(14) . . ? C121 H121 .965(9) . . ? C122 C123 1.542(16) . . ? C122 H122a .970(10) . . ? C122 H122b .955(10) . . ? C123 C124 1.574(16) . . ? C123 H123a .961(8) . . ? C123 H123b .996(12) . . ? C124 C125 1.507(12) . . ? C124 H124a .956(11) . . ? C124 H124b .968(12) . . ? C125 C126 1.556(16) . . ? C125 H125a .964(11) . . ? C125 H125b .981(11) . . ? C126 H126a .968(10) . . ? C126 H126b .958(8) . . ? C111 C112 1.527(14) . . ? C111 C116 1.553(14) . . ? C111 H111 .955(9) . . ? C112 C113 1.528(11) . . ? C112 H112a .964(11) . . ? C112 H112b .956(10) . . ? C113 C114 1.534(17) . . ? C113 H113a .969(12) . . ? C113 H113b .970(12) . . ? C114 C115 1.528(17) . . ? C114 H114a .972(8) . . ? C114 H114b .942(11) . . ? C115 C116 1.529(11) . . ? C115 H115a .970(11) . . ? C115 H115b .949(11) . . ? C116 H116a .978(10) . . ? C116 H116b .949(10) . . ? C131 C132 1.504(13) . . ? C131 C136 1.522(10) . . ? C131 H131 .959(9) . . ? C132 C133 1.535(17) . . ? C132 H132a .971(12) . . ? C132 H132b .960(8) . . ? C133 C134 1.528(13) . . ? C133 H133a .961(11) . . ? C133 H133b .943(13) . . ? C134 C135 1.559(17) . . ? C134 H134a .950(14) . . ? C134 H134b .962(14) . . ? C135 C136 1.528(17) . . ? C135 H135a .987(8) . . ? C135 H135b .947(13) . . ? C136 H136a .967(11) . . ? C136 H136b .960(9) . . ? C211 C212 1.542(10) . . ? C211 C216 1.550(15) . . ? C211 H211 .982(9) . . ? C212 C213 1.549(16) . . ? C212 H212a .957(11) . . ? C212 H212b .957(10) . . ? C213 C214 1.55(2) . . ? C213 H213a .952(11) . . ? C213 H213b .975(9) . . ? C214 C215 1.502(12) . . ? C214 H214a .945(13) . . ? C214 H214b .997(12) . . ? C215 C216 1.514(16) . . ? C215 H215a .947(11) . . ? C215 H215b .963(12) . . ? C216 H216a .959(7) . . ? C216 H216b .980(10) . . ? C231 C232 1.584(14) . . ? C231 C236 1.523(14) . . ? C231 H231 .965(11) . . ? C232 C233 1.510(13) . . ? C232 H232a .946(10) . . ? C232 H232b .974(12) . . ? C233 C234 1.520(17) . . ? C233 H233a .972(14) . . ? C233 H233b .949(12) . . ? C234 C235 1.463(18) . . ? C234 H234a .957(9) . . ? C234 H234b .976(13) . . ? C235 C236 1.547(12) . . ? C235 H235a 1.003(14) . . ? C235 H235b .944(12) . . ? C236 H236a .952(10) . . ? C236 H236b .969(12) . . ? C221 C222 1.491(14) . . ? C221 C226 1.512(16) . . ? C221 H221 .973(7) . . ? C222 C223 1.504(18) . . ? C222 H222a .968(12) . . ? C222 H222b .997(10) . . ? C223 C224 1.49(2) . . ? C223 H223a .956(11) . . ? C223 H223b .963(12) . . ? C224 C225 1.574(18) . . ? C224 H224a .973(14) . . ? C224 H224b .957(11) . . ? C225 C226 1.546(18) . . ? C225 H225a .962(10) . . ? C225 H225b .958(13) . . ? C226 H226a .980(11) . . ? C226 H226b .938(9) . . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I Au P1 106.26(7) . . . ? I Au P2 110.45(7) . . . ? P1 Au P2 143.07(10) . . . ? Au P1 C121 108.1(3) . . . ? Au P1 C111 114.3(3) . . . ? Au P1 C131 114.3(3) . . . ? C111 P1 C121 103.7(4) . . . ? C121 P1 C131 112.3(4) . . . ? C111 P1 C131 103.6(4) . . . ? Au P2 C211 117.8(3) . . . ? Au P2 C231 111.7(3) . . . ? Au P2 C221 108.8(3) . . . ? C211 P2 C231 107.6(4) . . . ? C211 P2 C221 104.1(4) . . . ? C221 P2 C231 106.0(4) . . . ? P1 C121 C122 112.5(7) . . . ? P1 C121 C126 117.3(6) . . . ? P1 C121 H121 103.5(6) . . . ? C122 C121 C126 112.1(7) . . . ? C122 C121 H121 107.7(8) . . . ? C126 C121 H121 102.4(8) . . . ? C121 C122 C123 111.2(8) . . . ? C121 C122 H122a 108.4(8) . . . ? C121 C122 H122b 110.1(7) . . . ? C123 C122 H122a 108.0(8) . . . ? C123 C122 H122b 111.7(9) . . . ? H122a C122 H122b 107.4(10) . . . ? C122 C123 C124 112.7(9) . . . ? C122 C123 H123a 111.5(11) . . . ? C122 C123 H123b 108.3(8) . . . ? C124 C123 H123a 110.9(8) . . . ? C124 C123 H123b 108.2(10) . . . ? H123a C123 H123b 104.8(11) . . . ? C123 C124 C125 109.3(8) . . . ? C123 C124 H124a 109.0(10) . . . ? C123 C124 H124b 111.3(10) . . . ? C125 C124 H124a 109.3(10) . . . ? C125 C124 H124b 110.3(10) . . . ? H124a C124 H124b 107.5(9) . . . ? C124 C125 C126 112.2(9) . . . ? C124 C125 H125a 111.3(8) . . . ? C124 C125 H125b 109.5(9) . . . ? C126 C125 H125a 110.2(9) . . . ? C126 C125 H125b 107.6(8) . . . ? H125a C125 H125b 105.8(11) . . . ? C121 C126 C125 111.3(8) . . . ? C121 C126 H126a 109.6(10) . . . ? C121 C126 H126b 110.9(8) . . . ? C125 C126 H126a 107.3(8) . . . ? C125 C126 H126b 110.3(10) . . . ? H116a C126 H126b 107.2(10) . . . ? P1 C111 C112 112.6(6) . . . ? P1 C111 C116 110.4(6) . . . ? P1 C111 H111 108.0(5) . . . ? C112 C111 C116 109.1(7) . . . ? C112 C111 H111 107.3(9) . . . ? C116 C111 H111 109.4(8) . . . ? C111 C112 C113 112.0(8) . . . ? C111 C112 H112a 109.3(8) . . . ? C111 C112 H112b 109.6(9) . . . ? C113 C112 H112a 109.8(10) . . . ? C113 C112 H112b 108.3(8) . . . ? H112a C112 H112b 107.8(10) . . . ? C112 C113 C114 112.7(9) . . . ? C112 C113 H113a 107.7(8) . . . ? C112 C113 H113b 108.5(10) . . . ? C114 C113 H113a 110.8(10) . . . ? C114 C113 H113b 110.6(9) . . . ? H113a C113 H113b 106.3(11) . . . ? C113 C114 C115 109.5(8) . . . ? C113 C114 H114a 109.4(10) . . . ? C113 C114 H114b 110.4(10) . . . ? C115 C114 H114a 109.1(10) . . . ? C115 C114 H114b 110.1(11) . . . ? H114a C114 H114b 108.3(9) . . . ? C114 C115 C116 111.0(8) . . . ? C114 C115 H115a 109.5(11) . . . ? C114 C115 H115b 110.7(8) . . . ? C116 C115 H115a 108.0(8) . . . ? C116 C115 H115b 109.6(10) . . . ? H115a C115 H115b 107.9(10) . . . ? C111 C116 C115 112.4(9) . . . ? C111 C116 H116a 108.4(7) . . . ? C111 C116 H116b 109.8(8) . . . ? C115 C116 H116a 109.3(8) . . . ? C115 C116 H116b 109.6(8) . . . ? H116a C116 H116b 107.3(10) . . . ? P1 C131 C132 118.4(7) . . . ? P1 C131 C136 111.4(6) . . . ? P1 C131 H31 101.7(6) . . . ? C132 C131 C136 111.0(7) . . . ? C132 C131 H131 101.7(8) . . . ? C136 C131 H131 111.7(9) . . . ? C131 C132 C133 111.5(9) . . . ? C131 C132 H132a 109.3(9) . . . ? C131 C132 H132b 110.8(9) . . . ? C133 C132 H132a 108.8(9) . . . ? C133 C132 H132b 109.3(9) . . . ? H132a C132 H132b 106.9(11) . . . ? C132 C133 C134 112.5(9) . . . ? C132 C133 H133a 109.0(11) . . . ? C132 C133 H133b 108.4(10) . . . ? C134 C133 H133a 108.2(10) . . . ? C134 C133 H133b 109.5(11) . . . ? H133a C133 H133b 109.2(11) . . . ? C133 C134 C135 107.1(9) . . . ? C133 C134 H134a 111.3(11) . . . ? C133 C134 H134b 110.2(10) . . . ? C135 C134 H134a 110.1(11) . . . ? C135 C134 H134b 109.6(11) . . . ? H134a C134 H134b 108.5(11) . . . ? C134 C135 C136 111.8(9) . . . ? C134 C135 H135a 108.7(10) . . . ? C134 C135 H135b 110.6(11) . . . ? C136 C135 H135a 109.1(10) . . . ? C136 C135 H135b 109.8(10) . . . ? H135a C135 H135b 106.6(11) . . . ? C131 C136 C135 110.4(8) . . . ? C131 C136 H136a 110.2(9) . . . ? C131 C136 H136b 111.0(8) . . . ? C135 C136 H136a 108.5(9) . . . ? C135 C136 H136b 109.4(10) . . . ? H136a C136 H136b 107.2(9) . . . ? P2 C211 C212 110.5(6) . . . ? P2 C211 C216 111.4(5) . . . ? P2 C211 H211 108.3(8) . . . ? C212 C211 C216 112.3(8) . . . ? C212 C211 H211 108.4(7) . . . ? C216 C211 H211 105.7(8) . . . ? C211 C212 C213 109.0(8) . . . ? C211 C212 H212a 110.2(9) . . . ? C211 C212 H212b 108.6(7) . . . ? C213 C212 H212a 110.8(8) . . . ? C213 C212 H212b 109.9(10) . . . ? H212a C212 H212b 108.3(9) . . . ? C212 C213 C214 113.0(8) . . . ? C212 C213 H213a 108.9(11) . . . ? C212 C213 H213b 108.0(10) . . . ? C214 C213 H213a 109.1(11) . . . ? C214 C213 H213b 110.5(11) . . . ? H213a C213 H213b 107.2(9) . . . ? C213 C214 C215 111.6(10) . . . ? C213 C214 H214a 111.0(10) . . . ? C213 C214 H214b 107.7(11) . . . ? C215 C214 H214a 111.8(11) . . . ? C215 C214 H214b 108.6(9) . . . ? H214a C214 H214b 106.0(13) . . . ? C214 C215 C216 111.5(9) . . . ? C214 C215 H215a 108.3(9) . . . ? C214 C215 H215b 109.9(11) . . . ? C216 C215 H215a 108.8(11) . . . ? C216 C215 H215b 109.6(9) . . . ? H215a C215 H215b 108.7(10) . . . ? C211 C216 C215 112.6(7) . . . ? C211 C216 H216a 110.7(10) . . . ? C211 C216 H216b 107.3(8) . . . ? C215 C216 H216a 110.6(9) . . . ? C215 C216 H216b 109.2(10) . . . ? H216a C216 H216b 106.3(8) . . . ? P2 C231 C232 116.7(6) . . . ? P2 C231 C236 112.6(7) . . . ? P2 C231 H231 102.7(6) . . . ? C232 C231 C236 108.9(7) . . . ? C232 C231 H231 105.5(9) . . . ? C236 C231 H231 109.9(8) . . . ? C231 C232 C233 110.1(8) . . . ? C231 C232 H232a 109.2(8) . . . ? C231 C232 H232b 106.8(10) . . . ? C233 C232 H232a 112.8(11) . . . ? C233 C232 H232b 110.0(9) . . . ? H232a C232 H232b 107.7(9) . . . ? C232 C233 C234 111.3(10) . . . ? C232 C233 H233a 108.8(10) . . . ? C232 C233 H233b 110.6(10) . . . ? C234 C233 H233a 107.5(10) . . . ? C234 C233 H233b 110.7(10) . . . ? H233a C233 H233b 107.8(13) . . . ? C233 C234 C235 112.1(9) . . . ? C233 C234 H234a 110.5(12) . . . ? C233 C234 H234b 107.9(10) . . . ? C235 C234 H234a 111.4(10) . . . ? C235 C234 H234b 107.9(12) . . . ? H234a C234 H234b 106.7(10) . . . ? C234 C235 C236 114.3(9) . . . ? C234 C235 H235a 108.0(11) . . . ? C234 C235 H235b 113.3(10) . . . ? C236 C235 H235a 105.3(9) . . . ? C236 C235 H235b 109.8(11) . . . ? H235a C235 H235b 105.6(11) . . . ? C231 C236 C235 111.4(9) . . . ? C231 C236 H236a 110.4(9) . . . ? C231 C236 H236b 108.5(8) . . . ? C235 C236 H236a 111.7(9) . . . ? C235 C236 H236b 106.9(9) . . . ? H236a C236 H236b 107.7(11) . . . ? P2 C221 C222 120.3(7) . . . ? P2 C221 C226 111.3(6) . . . ? P2 C221 H221 102.2(8) . . . ? C222 C221 C226 107.7(9) . . . ? C222 C221 H221 101.8(7) . . . ? C226 C221 H221 113.2(8) . . . ? C221 C222 C223 115.1(9) . . . ? C221 C222 H222a 110.4(12) . . . ? C221 C222 H222b 107.4(7) . . . ? C223 C222 H222a 110.5(9) . . . ? C223 C222 H222b 108.6(12) . . . ? H222a C222 H222b 104.3(9) . . . ? C222 C223 C224 109.7(9) . . . ? C222 C223 H223a 109.3(14) . . . ? C222 C223 H223b 111.9(11) . . . ? C224 C223 H223a 109.2(11) . . . ? C224 C223 H223b 108.7(15) . . . ? H223a C223 H223b 107.9(9) . . . ? C223 C224 C225 110.5(12) . . . ? C223 C224 H224a 111.5(10) . . . ? C223 C224 H224b 111.5(11) . . . ? C225 C224 H224a 108.1(11) . . . ? C225 C224 H224b 108.0(10) . . . ? H224a C224 H224b 107.0(15) . . . ? C224 C225 C226 106.7(9) . . . ? C224 C225 H225a 109.3(9) . . . ? C224 C225 H225b 111.1(13) . . . ? C226 C225 H225a 110.7(13) . . . ? C226 C225 H225b 111.4(9) . . . ? H225a C225 H225b 107.8(11) . . . ? C221 C226 C225 112.5(8) . . . ? C221 C226 H226a 109.2(11) . . . ? C221 C226 H226b 110.9(10) . . . ? C225 C226 H226a 107.2(10) . . . ? C225 C226 H226b 109.0(12) . . . ? H226a C226 H226b 107.9(9) . . . ? _reflns_limit_h_min 0 _reflns_limit_h_max 10 _reflns_limit_k_min -11 _reflns_limit_k_max 11 _reflns_limit_l_min -27 _reflns_limit_l_max 27 _reflns_number_total 6761 _reflns_number_observed 5767 _reflns_observed_criterion refl_observed_if_F____>_.000_sigma(F___) _reflns_d_resolution_high .771 _reflns_d_resolution_low 11.367 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? 2.353 #========END