Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Evamarie Hey-Hawkins' _publ_contact_author_address ; Department of Inorganic Chemistry Faculty of Chemistry and Mineralogy Johannisallee 29 Leipzig Saxony 04103 GERMANY ; _publ_contact_author_email HEY@RZ.UNI-LEIPZIG.DE _publ_section_title ; Different Transmetallation Behaviour of [M(P4HR4)] Salts toward Rhodium(I) and Copper(I) (M = Na, K; R = Ph, Mes; Mes = 2,4,6-Me3C6H2) ; _publ_requested_category FM loop_ _publ_author_name 'Evamarie Hey-Hawkins' 'Santiago Gomez-Ruiz' 'Robert Wolf' data_x0063fin _database_code_depnum_ccdc_archive 'CCDC 666346' _audit_creation_date 2007-03-12T18:40:00-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C44 H57 P4 Rh' _chemical_formula_weight 812.69 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2250(14) _cell_length_b 11.9022(17) _cell_length_c 21.536(4) _cell_angle_alpha 105.206(14) _cell_angle_beta 94.195(14) _cell_angle_gamma 92.753(13) _cell_volume 2024.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 12348 _cell_measurement_theta_min 2.5844 _cell_measurement_theta_max 32.2698 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plates _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.61 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.92626 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 0.0381206203 _diffrn_orient_matrix_ub_12 0.0268802094 _diffrn_orient_matrix_ub_13 -0.0214237725 _diffrn_orient_matrix_ub_21 -0.0522476259 _diffrn_orient_matrix_ub_22 0.0464034073 _diffrn_orient_matrix_ub_23 0.0075216041 _diffrn_orient_matrix_ub_31 0.0575218286 _diffrn_orient_matrix_ub_32 0.0308804222 _diffrn_orient_matrix_ub_33 0.0256316617 _diffrn_measurement_device_type 'ccd xcalibur s' _diffrn_measurement_method '\w scans and \f scans' _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_unetI/netI 0.0914 _diffrn_reflns_number 38404 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 28.28 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 9977 _reflns_number_gt 6959 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick,1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0361P)^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_number_reflns 9977 _refine_ls_number_parameters 458 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0823 _refine_ls_R_factor_gt 0.043 _refine_ls_wR_factor_ref 0.0843 _refine_ls_wR_factor_gt 0.0731 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.537 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.085 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9207(3) -0.0507(2) 0.17313(12) 0.0168(6) Uani 1 1 d . . . C2 C 1.0918(3) -0.0457(2) 0.17207(12) 0.0180(6) Uani 1 1 d . . . C3 C 1.1689(4) -0.1497(2) 0.15446(13) 0.0213(6) Uani 1 1 d . . . H3 H 1.2845 -0.146 0.1547 0.026 Uiso 1 1 calc R . . C4 C 1.0843(4) -0.2579(2) 0.13677(13) 0.0217(6) Uani 1 1 d . . . C5 C 0.9160(4) -0.2612(2) 0.13642(13) 0.0226(6) Uani 1 1 d . . . H5 H 0.8553 -0.3347 0.1235 0.027 Uiso 1 1 calc R . . C6 C 0.8326(3) -0.1603(2) 0.15436(13) 0.0194(6) Uani 1 1 d . . . C7 C 1.1966(3) 0.0673(2) 0.18903(14) 0.0227(6) Uani 1 1 d . . . H7A H 1.2177 0.0958 0.2361 0.034 Uiso 1 1 calc R . . H7B H 1.1398 0.1254 0.1724 0.034 Uiso 1 1 calc R . . H7C H 1.3006 0.0542 0.1696 0.034 Uiso 1 1 calc R . . C8 C 1.1729(4) -0.3682(3) 0.11807(15) 0.0304(7) Uani 1 1 d . . . H8A H 1.1292 -0.4145 0.0749 0.046 Uiso 1 1 calc R . . H8B H 1.1574 -0.4137 0.1493 0.046 Uiso 1 1 calc R . . H8C H 1.2898 -0.3481 0.1178 0.046 Uiso 1 1 calc R . . C9 C 0.6487(4) -0.1736(3) 0.15286(15) 0.0289(7) Uani 1 1 d . . . H9A H 0.6151 -0.1387 0.1961 0.043 Uiso 1 1 calc R . . H9B H 0.6121 -0.2567 0.1393 0.043 Uiso 1 1 calc R . . H9C H 0.5994 -0.1342 0.1223 0.043 Uiso 1 1 calc R . . C10 C 0.8163(3) 0.0494(2) 0.34447(12) 0.0163(6) Uani 1 1 d . . . C11 C 0.6488(3) 0.0423(2) 0.35385(13) 0.0179(6) Uani 1 1 d . . . C12 C 0.5950(3) -0.0213(2) 0.39479(13) 0.0202(6) Uani 1 1 d . . . H12 H 0.482 -0.0245 0.4012 0.024 Uiso 1 1 calc R . . C13 C 0.6988(4) -0.0804(2) 0.42680(13) 0.0222(6) Uani 1 1 d . . . C14 C 0.8628(4) -0.0753(2) 0.41600(13) 0.0208(6) Uani 1 1 d . . . H14 H 0.9361 -0.116 0.4368 0.025 Uiso 1 1 calc R . . C15 C 0.9231(3) -0.0127(2) 0.37583(13) 0.0184(6) Uani 1 1 d . . . C16 C 0.5205(3) 0.0977(3) 0.32082(14) 0.0252(7) Uani 1 1 d . . . H16A H 0.4157 0.0521 0.3158 0.038 Uiso 1 1 calc R . . H16B H 0.5526 0.0999 0.2782 0.038 Uiso 1 1 calc R . . H16C H 0.5095 0.1775 0.3469 0.038 Uiso 1 1 calc R . . C17 C 0.6331(4) -0.1530(3) 0.46825(15) 0.0332(8) Uani 1 1 d . . . H17A H 0.535 -0.1198 0.4867 0.05 Uiso 1 1 calc R . . H17B H 0.7162 -0.1533 0.5032 0.05 Uiso 1 1 calc R . . H17C H 0.6054 -0.2331 0.4418 0.05 Uiso 1 1 calc R . . C18 C 1.1028(3) -0.0149(3) 0.36647(15) 0.0284(7) Uani 1 1 d . . . H18A H 1.1546 -0.062 0.3924 0.043 Uiso 1 1 calc R . . H18B H 1.1536 0.0649 0.3802 0.043 Uiso 1 1 calc R . . H18C H 1.1172 -0.049 0.3207 0.043 Uiso 1 1 calc R . . C19 C 0.9372(3) 0.4234(2) 0.38085(12) 0.0160(6) Uani 1 1 d . . . C20 C 1.1081(3) 0.4398(2) 0.38187(13) 0.0182(6) Uani 1 1 d . . . C21 C 1.1881(4) 0.5416(2) 0.42068(13) 0.0206(6) Uani 1 1 d . . . H21 H 1.3033 0.552 0.4205 0.025 Uiso 1 1 calc R . . C22 C 1.1075(4) 0.6289(2) 0.45980(13) 0.0210(6) Uani 1 1 d . . . C23 C 0.9410(4) 0.6102(2) 0.46006(13) 0.0201(6) Uani 1 1 d . . . H23 H 0.8839 0.6678 0.4877 0.024 Uiso 1 1 calc R . . C24 C 0.8527(3) 0.5099(2) 0.42138(12) 0.0175(6) Uani 1 1 d . . . C25 C 1.2113(3) 0.3504(3) 0.34276(14) 0.0245(7) Uani 1 1 d . . . H25A H 1.3212 0.3861 0.3428 0.037 Uiso 1 1 calc R . . H25B H 1.1612 0.3228 0.2983 0.037 Uiso 1 1 calc R . . H25C H 1.2184 0.2844 0.3618 0.037 Uiso 1 1 calc R . . C26 C 1.1980(4) 0.7391(3) 0.50033(14) 0.0300(7) Uani 1 1 d . . . H26A H 1.1294 0.7793 0.5334 0.045 Uiso 1 1 calc R . . H26B H 1.2248 0.7901 0.4729 0.045 Uiso 1 1 calc R . . H26C H 1.299 0.7202 0.5212 0.045 Uiso 1 1 calc R . . C27 C 0.6693(3) 0.5022(3) 0.42433(13) 0.0221(6) Uani 1 1 d . . . H27A H 0.641 0.5585 0.4635 0.033 Uiso 1 1 calc R . . H27B H 0.6325 0.4232 0.4252 0.033 Uiso 1 1 calc R . . H27C H 0.6158 0.5201 0.3862 0.033 Uiso 1 1 calc R . . C28 C 0.6948(3) 0.4750(2) 0.24647(12) 0.0161(6) Uani 1 1 d . . . C29 C 0.5252(3) 0.4442(2) 0.23537(12) 0.0171(6) Uani 1 1 d . . . C30 C 0.4179(4) 0.5320(2) 0.24980(13) 0.0213(6) Uani 1 1 d . . . H30 H 0.3036 0.5116 0.2431 0.026 Uiso 1 1 calc R . . C31 C 0.4718(4) 0.6485(2) 0.27358(13) 0.0212(6) Uani 1 1 d . . . C32 C 0.6387(3) 0.6770(2) 0.28152(13) 0.0198(6) Uani 1 1 d . . . H32 H 0.677 0.7569 0.2961 0.024 Uiso 1 1 calc R . . C33 C 0.7518(3) 0.5928(2) 0.26883(12) 0.0170(6) Uani 1 1 d . . . C34 C 0.4555(4) 0.3196(2) 0.21037(14) 0.0233(6) Uani 1 1 d . . . H34A H 0.4755 0.2783 0.2438 0.035 Uiso 1 1 calc R . . H34B H 0.5082 0.281 0.1718 0.035 Uiso 1 1 calc R . . H34C H 0.3376 0.3184 0.1993 0.035 Uiso 1 1 calc R . . C35 C 0.3527(4) 0.7416(3) 0.29086(16) 0.0299(7) Uani 1 1 d . . . H35A H 0.4057 0.8173 0.2912 0.045 Uiso 1 1 calc R . . H35B H 0.3174 0.745 0.3338 0.045 Uiso 1 1 calc R . . H35C H 0.2575 0.7232 0.2589 0.045 Uiso 1 1 calc R . . C36 C 0.9306(3) 0.6340(2) 0.28068(14) 0.0226(6) Uani 1 1 d . . . H36A H 0.9417 0.7193 0.2908 0.034 Uiso 1 1 calc R . . H36B H 0.9858 0.6006 0.2419 0.034 Uiso 1 1 calc R . . H36C H 0.9803 0.6087 0.3171 0.034 Uiso 1 1 calc R . . C37 C 0.7727(4) 0.0807(3) 0.04865(13) 0.0277(7) Uani 1 1 d . . . H37 H 0.7389 0.0017 0.0533 0.033 Uiso 1 1 calc R . . C38 C 0.9375(4) 0.1087(2) 0.05935(13) 0.0263(7) Uani 1 1 d . . . H38 H 1.0022 0.0463 0.0702 0.032 Uiso 1 1 calc R . . C39 C 1.0312(5) 0.1870(3) 0.02767(18) 0.0447(10) Uani 1 1 d . . . H39A H 1.1483 0.1722 0.0326 0.054 Uiso 1 1 calc R . . H39B H 0.9961 0.1625 -0.0191 0.054 Uiso 1 1 calc R . . C40 C 1.0179(6) 0.3103(3) 0.0499(2) 0.0745(16) Uani 1 1 d . . . H40A H 0.999 0.3405 0.0115 0.089 Uiso 1 1 calc R . . H40B H 1.1246 0.3461 0.0723 0.089 Uiso 1 1 calc R . . C41 C 0.8876(5) 0.3524(3) 0.09430(15) 0.0375(9) Uani 1 1 d . . . H41 H 0.9158 0.4311 0.125 0.045 Uiso 1 1 calc R . . C42 C 0.7232(5) 0.3243(3) 0.08086(14) 0.0393(9) Uani 1 1 d . . . H42 H 0.6531 0.3861 0.1032 0.047 Uiso 1 1 calc R . . C43 C 0.6459(7) 0.2472(4) 0.0174(2) 0.0890(19) Uani 1 1 d . . . H43A H 0.5291 0.2632 0.0137 0.107 Uiso 1 1 calc R . . H43B H 0.6972 0.2713 -0.0177 0.107 Uiso 1 1 calc R . . C44 C 0.6545(5) 0.1253(3) 0.00594(19) 0.0568(12) Uani 1 1 d . . . H44A H 0.6814 0.0942 -0.0392 0.068 Uiso 1 1 calc R . . H44B H 0.544 0.0914 0.0089 0.068 Uiso 1 1 calc R . . P1 P 0.80238(9) 0.07963(6) 0.19911(3) 0.01931(17) Uani 1 1 d . . . P2 P 0.92146(9) 0.14011(6) 0.29930(3) 0.01644(16) Uani 1 1 d . . . P3 P 0.80021(9) 0.30583(6) 0.32574(3) 0.01617(16) Uani 1 1 d . . . P4 P 0.83263(9) 0.35611(6) 0.23596(3) 0.01827(16) Uani 1 1 d . . . Rh1 Rh 0.82122(3) 0.21655(2) 0.141489(11) 0.01981(7) Uani 1 1 d . . . H4P H 0.972(3) 0.411(2) 0.2472(12) 0.022(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0207(15) 0.0166(14) 0.0138(13) 0.0051(11) -0.0004(11) 0.0031(12) C2 0.0228(16) 0.0154(14) 0.0155(13) 0.0038(11) 0.0017(12) 0.0007(12) C3 0.0196(16) 0.0242(16) 0.0221(15) 0.0083(13) 0.0040(12) 0.0052(12) C4 0.0304(18) 0.0179(15) 0.0174(14) 0.0051(12) 0.0023(13) 0.0062(13) C5 0.0312(18) 0.0141(14) 0.0200(14) 0.0023(12) -0.0013(13) -0.0037(13) C6 0.0200(16) 0.0185(15) 0.0197(14) 0.0063(12) -0.0011(12) -0.0001(12) C7 0.0167(15) 0.0199(15) 0.0286(16) 0.0022(13) -0.0001(13) -0.0011(12) C8 0.037(2) 0.0212(16) 0.0341(17) 0.0069(14) 0.0069(15) 0.0096(14) C9 0.0229(17) 0.0233(17) 0.0390(18) 0.0081(14) -0.0027(14) -0.0042(13) C10 0.0180(15) 0.0135(14) 0.0164(13) 0.0024(11) 0.0016(11) 0.0011(11) C11 0.0181(15) 0.0148(14) 0.0190(14) 0.0013(11) 0.0004(12) 0.0017(11) C12 0.0171(15) 0.0189(15) 0.0236(15) 0.0028(12) 0.0049(12) 0.0023(12) C13 0.0295(17) 0.0161(15) 0.0210(15) 0.0047(12) 0.0041(13) 0.0017(13) C14 0.0238(16) 0.0186(15) 0.0209(14) 0.0067(12) 0.0002(12) 0.0060(12) C15 0.0176(15) 0.0157(14) 0.0208(14) 0.0030(12) 0.0006(12) 0.0025(12) C16 0.0150(15) 0.0302(17) 0.0335(17) 0.0139(14) 0.0021(13) 0.0024(13) C17 0.037(2) 0.0311(18) 0.0393(18) 0.0187(15) 0.0150(16) 0.0070(15) C18 0.0181(16) 0.0306(18) 0.0420(18) 0.0183(15) 0.0030(14) 0.0081(13) C19 0.0196(15) 0.0136(14) 0.0153(13) 0.0052(11) 0.0012(11) 0.0002(11) C20 0.0167(15) 0.0196(15) 0.0180(14) 0.0047(12) -0.0010(12) 0.0021(12) C21 0.0167(15) 0.0239(16) 0.0215(15) 0.0082(13) -0.0021(12) -0.0015(12) C22 0.0256(17) 0.0180(15) 0.0191(14) 0.0060(12) -0.0018(13) -0.0009(12) C23 0.0276(17) 0.0160(15) 0.0157(14) 0.0025(12) 0.0001(12) 0.0052(12) C24 0.0187(15) 0.0196(15) 0.0154(13) 0.0067(12) 0.0007(12) 0.0039(12) C25 0.0128(15) 0.0268(17) 0.0322(17) 0.0040(14) 0.0045(13) 0.0029(12) C26 0.0350(19) 0.0216(17) 0.0297(17) 0.0026(14) -0.0017(15) -0.0024(14) C27 0.0211(16) 0.0218(16) 0.0220(15) 0.0021(12) 0.0048(12) 0.0046(12) C28 0.0172(15) 0.0159(14) 0.0143(13) 0.0025(11) -0.0008(11) 0.0044(11) C29 0.0206(15) 0.0136(14) 0.0162(13) 0.0038(11) -0.0028(12) 0.0007(11) C30 0.0165(15) 0.0212(15) 0.0252(15) 0.0058(13) -0.0023(12) 0.0007(12) C31 0.0235(16) 0.0174(15) 0.0222(15) 0.0043(12) 0.0002(12) 0.0060(12) C32 0.0205(16) 0.0140(14) 0.0227(15) 0.0022(12) -0.0019(12) -0.0002(12) C33 0.0180(15) 0.0173(14) 0.0155(13) 0.0044(11) 0.0003(11) 0.0015(12) C34 0.0229(16) 0.0162(15) 0.0296(16) 0.0049(13) -0.0020(13) 0.0019(12) C35 0.0223(17) 0.0188(16) 0.0441(19) 0.0007(14) -0.0007(15) 0.0059(13) C36 0.0209(16) 0.0187(15) 0.0286(16) 0.0069(13) 0.0023(13) 0.0011(12) C37 0.043(2) 0.0187(16) 0.0168(15) -0.0023(12) -0.0020(14) 0.0007(14) C38 0.040(2) 0.0164(15) 0.0206(15) -0.0002(12) 0.0081(14) 0.0060(14) C39 0.050(2) 0.0291(19) 0.059(2) 0.0110(18) 0.032(2) 0.0059(17) C40 0.128(4) 0.030(2) 0.078(3) 0.017(2) 0.076(3) 0.019(2) C41 0.069(3) 0.0202(17) 0.0297(18) 0.0120(14) 0.0205(18) 0.0113(17) C42 0.075(3) 0.0236(18) 0.0203(16) 0.0078(14) -0.0037(17) 0.0180(18) C43 0.152(5) 0.051(3) 0.051(3) 0.002(2) -0.053(3) 0.033(3) C44 0.071(3) 0.034(2) 0.053(2) 0.0030(19) -0.035(2) -0.002(2) P1 0.0239(4) 0.0166(4) 0.0176(4) 0.0039(3) 0.0025(3) 0.0058(3) P2 0.0157(4) 0.0156(4) 0.0186(4) 0.0053(3) 0.0013(3) 0.0026(3) P3 0.0160(4) 0.0154(4) 0.0165(3) 0.0030(3) 0.0012(3) 0.0021(3) P4 0.0226(4) 0.0161(4) 0.0162(4) 0.0036(3) 0.0022(3) 0.0059(3) Rh1 0.02946(15) 0.01583(12) 0.01471(11) 0.00384(9) 0.00307(10) 0.00676(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.407(4) . ? C1 C2 1.407(4) . ? C1 P1 1.853(3) . ? C2 C3 1.394(4) . ? C2 C7 1.507(4) . ? C3 C4 1.380(4) . ? C3 H3 0.95 . ? C4 C5 1.382(4) . ? C4 C8 1.509(4) . ? C5 C6 1.391(4) . ? C5 H5 0.95 . ? C6 C9 1.511(4) . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 C11 1.408(4) . ? C10 C15 1.418(4) . ? C10 P2 1.856(3) . ? C11 C12 1.386(4) . ? C11 C16 1.503(4) . ? C12 C13 1.387(4) . ? C12 H12 0.95 . ? C13 C14 1.387(4) . ? C13 C17 1.505(4) . ? C14 C15 1.384(4) . ? C14 H14 0.95 . ? C15 C18 1.507(4) . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 C20 1.407(4) . ? C19 C24 1.411(4) . ? C19 P3 1.849(3) . ? C20 C21 1.382(4) . ? C20 C25 1.511(4) . ? C21 C22 1.385(4) . ? C21 H21 0.95 . ? C22 C23 1.378(4) . ? C22 C26 1.499(4) . ? C23 C24 1.397(4) . ? C23 H23 0.95 . ? C24 C27 1.513(4) . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C28 C33 1.402(4) . ? C28 C29 1.412(4) . ? C28 P4 1.834(3) . ? C29 C30 1.388(4) . ? C29 C34 1.507(4) . ? C30 C31 1.384(4) . ? C30 H30 0.95 . ? C31 C32 1.385(4) . ? C31 C35 1.506(4) . ? C32 C33 1.389(4) . ? C32 H32 0.95 . ? C33 C36 1.509(4) . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 C38 1.369(4) . ? C37 C44 1.499(4) . ? C37 Rh1 2.213(3) . ? C37 H37 1 . ? C38 C39 1.506(4) . ? C38 Rh1 2.206(3) . ? C38 H38 1 . ? C39 C40 1.432(5) . ? C39 H39A 0.99 . ? C39 H39B 0.99 . ? C40 C41 1.506(5) . ? C40 H40A 0.99 . ? C40 H40B 0.99 . ? C41 C42 1.368(5) . ? C41 Rh1 2.192(3) . ? C41 H41 1 . ? C42 C43 1.508(5) . ? C42 Rh1 2.196(3) . ? C42 H42 1 . ? C43 C44 1.413(5) . ? C43 H43A 0.99 . ? C43 H43B 0.99 . ? C44 H44A 0.99 . ? C44 H44B 0.99 . ? P1 P2 2.2228(11) . ? P1 Rh1 2.2989(8) . ? P2 P3 2.2119(10) . ? P3 P4 2.1987(10) . ? P4 Rh1 2.2566(9) . ? P4 H4P 1.26(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 C6 C1 C2 119.0(2) . . ? C6 C1 P1 117.3(2) . . ? C2 C1 P1 123.8(2) . . ? C3 C2 C1 118.9(3) . . ? C3 C2 C7 118.0(3) . . ? C1 C2 C7 123.1(2) . . ? C4 C3 C2 122.8(3) . . ? C4 C3 H3 118.6 . . ? C2 C3 H3 118.6 . . ? C3 C4 C5 117.6(3) . . ? C3 C4 C8 121.0(3) . . ? C5 C4 C8 121.4(3) . . ? C4 C5 C6 122.1(3) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C5 C6 C1 119.6(3) . . ? C5 C6 C9 117.9(3) . . ? C1 C6 C9 122.5(2) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 118.3(2) . . ? C11 C10 P2 127.6(2) . . ? C15 C10 P2 114.0(2) . . ? C12 C11 C10 119.3(2) . . ? C12 C11 C16 116.6(2) . . ? C10 C11 C16 124.1(2) . . ? C11 C12 C13 122.9(3) . . ? C11 C12 H12 118.5 . . ? C13 C12 H12 118.5 . . ? C12 C13 C14 117.3(3) . . ? C12 C13 C17 120.9(3) . . ? C14 C13 C17 121.7(3) . . ? C15 C14 C13 122.1(3) . . ? C15 C14 H14 119 . . ? C13 C14 H14 119 . . ? C14 C15 C10 120.0(3) . . ? C14 C15 C18 117.7(2) . . ? C10 C15 C18 122.3(2) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 118.9(2) . . ? C20 C19 P3 127.5(2) . . ? C24 C19 P3 113.3(2) . . ? C21 C20 C19 119.4(2) . . ? C21 C20 C25 117.4(2) . . ? C19 C20 C25 123.2(2) . . ? C20 C21 C22 122.8(3) . . ? C20 C21 H21 118.6 . . ? C22 C21 H21 118.6 . . ? C23 C22 C21 117.2(3) . . ? C23 C22 C26 121.4(3) . . ? C21 C22 C26 121.3(3) . . ? C22 C23 C24 122.7(3) . . ? C22 C23 H23 118.6 . . ? C24 C23 H23 118.6 . . ? C23 C24 C19 118.9(3) . . ? C23 C24 C27 117.4(2) . . ? C19 C24 C27 123.7(2) . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C33 C28 C29 120.0(2) . . ? C33 C28 P4 122.3(2) . . ? C29 C28 P4 117.5(2) . . ? C30 C29 C28 118.6(2) . . ? C30 C29 C34 118.5(3) . . ? C28 C29 C34 122.8(2) . . ? C31 C30 C29 122.2(3) . . ? C31 C30 H30 118.9 . . ? C29 C30 H30 118.9 . . ? C30 C31 C32 118.1(3) . . ? C30 C31 C35 121.0(3) . . ? C32 C31 C35 120.8(3) . . ? C31 C32 C33 122.2(3) . . ? C31 C32 H32 118.9 . . ? C33 C32 H32 118.9 . . ? C32 C33 C28 118.8(3) . . ? C32 C33 C36 117.6(2) . . ? C28 C33 C36 123.7(2) . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C35 H35A 109.5 . . ? C31 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C31 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C44 126.3(3) . . ? C38 C37 Rh1 71.68(16) . . ? C44 C37 Rh1 108.0(2) . . ? C38 C37 H37 114.1 . . ? C44 C37 H37 114.1 . . ? Rh1 C37 H37 114.1 . . ? C37 C38 C39 125.0(3) . . ? C37 C38 Rh1 72.23(17) . . ? C39 C38 Rh1 109.41(19) . . ? C37 C38 H38 114.1 . . ? C39 C38 H38 114.1 . . ? Rh1 C38 H38 114.1 . . ? C40 C39 C38 118.2(3) . . ? C40 C39 H39A 107.7 . . ? C38 C39 H39A 107.7 . . ? C40 C39 H39B 107.7 . . ? C38 C39 H39B 107.7 . . ? H39A C39 H39B 107.1 . . ? C39 C40 C41 117.7(3) . . ? C39 C40 H40A 107.9 . . ? C41 C40 H40A 107.9 . . ? C39 C40 H40B 107.9 . . ? C41 C40 H40B 107.9 . . ? H40A C40 H40B 107.2 . . ? C42 C41 C40 126.1(4) . . ? C42 C41 Rh1 71.99(19) . . ? C40 C41 Rh1 108.9(2) . . ? C42 C41 H41 113.9 . . ? C40 C41 H41 113.9 . . ? Rh1 C41 H41 113.9 . . ? C41 C42 C43 124.0(4) . . ? C41 C42 Rh1 71.66(18) . . ? C43 C42 Rh1 109.9(2) . . ? C41 C42 H42 114.4 . . ? C43 C42 H42 114.4 . . ? Rh1 C42 H42 114.4 . . ? C44 C43 C42 117.9(3) . . ? C44 C43 H43A 107.8 . . ? C42 C43 H43A 107.8 . . ? C44 C43 H43B 107.8 . . ? C42 C43 H43B 107.8 . . ? H43A C43 H43B 107.2 . . ? C43 C44 C37 118.5(3) . . ? C43 C44 H44A 107.7 . . ? C37 C44 H44A 107.7 . . ? C43 C44 H44B 107.7 . . ? C37 C44 H44B 107.7 . . ? H44A C44 H44B 107.1 . . ? C1 P1 P2 96.43(9) . . ? C1 P1 Rh1 116.75(9) . . ? P2 P1 Rh1 113.75(4) . . ? C10 P2 P3 102.91(9) . . ? C10 P2 P1 104.74(9) . . ? P3 P2 P1 95.91(4) . . ? C19 P3 P4 97.75(9) . . ? C19 P3 P2 111.35(9) . . ? P4 P3 P2 96.80(4) . . ? C28 P4 P3 99.12(9) . . ? C28 P4 Rh1 120.53(9) . . ? P3 P4 Rh1 119.48(4) . . ? C28 P4 H4P 102.1(12) . . ? P3 P4 H4P 103.3(12) . . ? Rh1 P4 H4P 109.7(12) . . ? C41 Rh1 C42 36.35(13) . . ? C41 Rh1 C38 81.02(11) . . ? C42 Rh1 C38 90.86(12) . . ? C41 Rh1 C37 93.07(12) . . ? C42 Rh1 C37 80.71(11) . . ? C38 Rh1 C37 36.10(11) . . ? C41 Rh1 P4 88.56(9) . . ? C42 Rh1 P4 96.14(9) . . ? C38 Rh1 P4 151.79(9) . . ? C37 Rh1 P4 172.02(9) . . ? C41 Rh1 P1 169.12(11) . . ? C42 Rh1 P1 154.47(11) . . ? C38 Rh1 P1 97.16(8) . . ? C37 Rh1 P1 91.61(8) . . ? P4 Rh1 P1 88.16(3) . . ? #============================================================================ data_x0285fin _database_code_depnum_ccdc_archive 'CCDC 666347' _audit_creation_date 2007-09-11T19:53:50-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C47 H67 O P3 Rh2' _chemical_formula_weight 946.74 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.627(5) _cell_length_b 12.941(5) _cell_length_c 15.604(5) _cell_angle_alpha 74.908(5) _cell_angle_beta 84.544(5) _cell_angle_gamma 67.189(5) _cell_volume 2269.3(15) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 10112 _cell_measurement_theta_min 2.5949 _cell_measurement_theta_max 32.2645 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description 'very thin plates' _exptl_crystal_colour orange _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.866 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.951 _exptl_absorpt_correction_T_max 1.000 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 -0.0158626437 _diffrn_orient_matrix_ub_12 -0.0352758704 _diffrn_orient_matrix_ub_13 0.0375449688 _diffrn_orient_matrix_ub_21 0.0322046582 _diffrn_orient_matrix_ub_22 0.0126478886 _diffrn_orient_matrix_ub_23 0.0276728295 _diffrn_orient_matrix_ub_31 -0.0490112743 _diffrn_orient_matrix_ub_32 0.0483404813 _diffrn_orient_matrix_ub_33 0.005681452 _diffrn_measurement_device_type 'ccd xcalibur s' _diffrn_measurement_method '\w scans and \f scans' _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_unetI/netI 0.0915 _diffrn_reflns_number 35456 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 27.1 _diffrn_reflns_theta_full 27.1 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 9985 _reflns_number_gt 6302 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick,1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1022P)^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_number_reflns 9985 _refine_ls_number_parameters 471 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0904 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1728 _refine_ls_wR_factor_gt 0.153 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.156 _refine_diff_density_min -0.866 _refine_diff_density_rms 0.158 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Rh Rh -1.1178 0.9187 '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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.88126(4) 0.36058(4) 0.87060(3) 0.02487(15) Uani 1 1 d . . . Rh2 Rh 0.67586(4) 0.16450(4) 0.87221(3) 0.02034(14) Uani 1 1 d . . . P1 P 0.78657(14) 0.31482(15) 0.99834(11) 0.0287(4) Uani 1 1 d . . . P2 P 0.73494(14) 0.17181(15) 1.00388(11) 0.0256(4) Uani 1 1 d . . . P3 P 0.80341(14) 0.25746(14) 0.80708(11) 0.0234(3) Uani 1 1 d . . . C1 C 0.8633(5) 0.2641(5) 1.1051(4) 0.0222(13) Uani 1 1 d . . . C2 C 0.8151(5) 0.3167(5) 1.1745(4) 0.0258(13) Uani 1 1 d . . . C3 C 0.8726(5) 0.2761(5) 1.2551(4) 0.0274(14) Uani 1 1 d . . . H3 H 0.8384 0.313 1.3016 0.033 Uiso 1 1 calc R . . C4 C 0.9767(5) 0.1851(5) 1.2709(4) 0.0276(14) Uani 1 1 d . . . C5 C 1.0244(5) 0.1321(5) 1.2026(4) 0.0282(14) Uani 1 1 d . . . H5 H 1.0959 0.0683 1.2122 0.034 Uiso 1 1 calc R . . C6 C 0.9711(5) 0.1695(5) 1.1206(4) 0.0260(13) Uani 1 1 d . . . C7 C 0.7006(5) 0.4168(6) 1.1655(5) 0.0324(15) Uani 1 1 d . . . H7A H 0.6774 0.4345 1.2234 0.049 Uiso 1 1 calc R . . H7B H 0.6427 0.3962 1.1441 0.049 Uiso 1 1 calc R . . H7C H 0.7073 0.4847 1.1232 0.049 Uiso 1 1 calc R . . C8 C 1.0370(7) 0.1427(6) 1.3595(5) 0.0413(18) Uani 1 1 d . . . H8A H 1.0095 0.086 1.399 0.062 Uiso 1 1 calc R . . H8B H 1.0208 0.2081 1.386 0.062 Uiso 1 1 calc R . . H8C H 1.1201 0.1064 1.3511 0.062 Uiso 1 1 calc R . . C9 C 1.0304(6) 0.1042(6) 1.0511(5) 0.0371(17) Uani 1 1 d . . . H9A H 1.1129 0.0657 1.0643 0.056 Uiso 1 1 calc R . . H9B H 1.0184 0.1583 0.9925 0.056 Uiso 1 1 calc R . . H9C H 0.9984 0.0461 1.0514 0.056 Uiso 1 1 calc R . . C10 C 0.6358(5) 0.1776(5) 1.0978(4) 0.0239(13) Uani 1 1 d . . . C11 C 0.5270(5) 0.2675(5) 1.0891(5) 0.0263(14) Uani 1 1 d . . . C12 C 0.4555(6) 0.2765(6) 1.1616(5) 0.0323(15) Uani 1 1 d . . . H12 H 0.3828 0.3387 1.1552 0.039 Uiso 1 1 calc R . . C13 C 0.4853(6) 0.1991(6) 1.2423(5) 0.0365(17) Uani 1 1 d . . . C14 C 0.5934(6) 0.1080(6) 1.2510(4) 0.0332(15) Uani 1 1 d . . . H14 H 0.6151 0.0536 1.3067 0.04 Uiso 1 1 calc R . . C15 C 0.6682(6) 0.0954(5) 1.1815(4) 0.0297(14) Uani 1 1 d . . . C16 C 0.4851(5) 0.3568(5) 1.0038(5) 0.0327(15) Uani 1 1 d . . . H16A H 0.5006 0.3188 0.9547 0.049 Uiso 1 1 calc R . . H16B H 0.525 0.4105 0.9934 0.049 Uiso 1 1 calc R . . H16C H 0.4022 0.3996 1.0074 0.049 Uiso 1 1 calc R . . C17 C 0.4063(7) 0.2086(8) 1.3219(5) 0.053(2) Uani 1 1 d . . . H17A H 0.3946 0.2799 1.3391 0.08 Uiso 1 1 calc R . . H17B H 0.4412 0.1419 1.3715 0.08 Uiso 1 1 calc R . . H17C H 0.3322 0.2102 1.3064 0.08 Uiso 1 1 calc R . . C18 C 0.7836(6) -0.0020(6) 1.1961(5) 0.0440(19) Uani 1 1 d . . . H18A H 0.8441 0.0295 1.1868 0.066 Uiso 1 1 calc R . . H18B H 0.7935 -0.0496 1.1541 0.066 Uiso 1 1 calc R . . H18C H 0.7887 -0.0496 1.2569 0.066 Uiso 1 1 calc R . . C19 C 0.7702(5) 0.3261(5) 0.6891(4) 0.0228(13) Uani 1 1 d . . . C20 C 0.8336(5) 0.2816(5) 0.6194(4) 0.0286(14) Uani 1 1 d . . . C21 C 0.8007(6) 0.3429(6) 0.5327(5) 0.0418(18) Uani 1 1 d . . . H21 H 0.8452 0.3141 0.4853 0.05 Uiso 1 1 calc R . . C22 C 0.7043(7) 0.4458(6) 0.5128(5) 0.0437(19) Uani 1 1 d . . . C23 C 0.6430(6) 0.4873(5) 0.5816(5) 0.0351(16) Uani 1 1 d . . . H23 H 0.5774 0.5574 0.569 0.042 Uiso 1 1 calc R . . C24 C 0.6732(5) 0.4308(5) 0.6685(5) 0.0289(14) Uani 1 1 d . . . C25 C 0.9393(6) 0.1704(5) 0.6322(5) 0.0361(16) Uani 1 1 d . . . H25A H 0.9955 0.1741 0.6694 0.054 Uiso 1 1 calc R . . H25B H 0.9733 0.1606 0.5743 0.054 Uiso 1 1 calc R . . H25C H 0.9174 0.1048 0.6613 0.054 Uiso 1 1 calc R . . C26 C 0.6697(9) 0.5067(8) 0.4174(6) 0.073(3) Uani 1 1 d . . . H26A H 0.6258 0.5892 0.4128 0.109 Uiso 1 1 calc R . . H26B H 0.6223 0.4734 0.3966 0.109 Uiso 1 1 calc R . . H26C H 0.7388 0.4972 0.3807 0.109 Uiso 1 1 calc R . . C27 C 0.6033(6) 0.4812(6) 0.7414(5) 0.0354(16) Uani 1 1 d . . . H27A H 0.542 0.5551 0.7156 0.053 Uiso 1 1 calc R . . H27B H 0.6529 0.4939 0.7789 0.053 Uiso 1 1 calc R . . H27C H 0.5695 0.4277 0.7774 0.053 Uiso 1 1 calc R . . C28 C 0.9078(6) 0.4733(6) 0.7477(5) 0.0370(17) Uani 1 1 d . . . H28 H 0.8545 0.4882 0.6985 0.044 Uiso 1 1 calc R . . C29 C 0.9975(6) 0.3694(7) 0.7603(5) 0.0394(18) Uani 1 1 d . . . H29 H 0.997 0.3227 0.7184 0.047 Uiso 1 1 calc R . . C30 C 1.1155(6) 0.3442(7) 0.7921(6) 0.048(2) Uani 1 1 d . . . H30A H 1.1563 0.3801 0.7437 0.057 Uiso 1 1 calc R . . H30B H 1.1591 0.2596 0.8064 0.057 Uiso 1 1 calc R . . C31 C 1.1134(6) 0.3889(7) 0.8736(6) 0.048(2) Uani 1 1 d . . . H31A H 1.1112 0.4688 0.8539 0.057 Uiso 1 1 calc R . . H31B H 1.1854 0.3407 0.9078 0.057 Uiso 1 1 calc R . . C32 C 1.0111(6) 0.3884(6) 0.9350(5) 0.0357(16) Uani 1 1 d . . . H32 H 1.0317 0.3409 0.9972 0.043 Uiso 1 1 calc R . . C33 C 0.9116(6) 0.4854(6) 0.9262(5) 0.0392(17) Uani 1 1 d . . . H33 H 0.8712 0.4953 0.9836 0.047 Uiso 1 1 calc R . . C34 C 0.8884(7) 0.5979(6) 0.8563(6) 0.053(2) Uani 1 1 d . . . H34A H 0.9336 0.6387 0.8711 0.063 Uiso 1 1 calc R . . H34B H 0.8061 0.6475 0.8581 0.063 Uiso 1 1 calc R . . C35 C 0.9185(7) 0.5821(6) 0.7603(6) 0.050(2) Uani 1 1 d . . . H35A H 0.8664 0.6505 0.7179 0.06 Uiso 1 1 calc R . . H35B H 0.9981 0.5778 0.7468 0.06 Uiso 1 1 calc R . . C36 C 0.5753(5) 0.2100(6) 0.7518(4) 0.0289(14) Uani 1 1 d . . . H36 H 0.5829 0.276 0.7048 0.035 Uiso 1 1 calc R . . C37 C 0.6637(5) 0.1057(6) 0.7542(4) 0.0282(14) Uani 1 1 d . . . H37 H 0.7246 0.1105 0.7092 0.034 Uiso 1 1 calc R . . C38 C 0.6529(6) -0.0109(6) 0.7793(5) 0.0354(16) Uani 1 1 d . . . H38A H 0.7093 -0.0619 0.7448 0.043 Uiso 1 1 calc R . . H38B H 0.5752 -0.0007 0.7625 0.043 Uiso 1 1 calc R . . C39 C 0.6730(6) -0.0711(5) 0.8798(5) 0.0333(16) Uani 1 1 d . . . H39A H 0.6285 -0.1216 0.8972 0.04 Uiso 1 1 calc R . . H39B H 0.7553 -0.1208 0.8899 0.04 Uiso 1 1 calc R . . C40 C 0.6392(5) 0.0117(5) 0.9371(4) 0.0263(14) Uani 1 1 d . . . H40 H 0.6702 -0.0241 0.999 0.032 Uiso 1 1 calc R . . C41 C 0.5369(5) 0.1076(5) 0.9305(4) 0.0254(13) Uani 1 1 d . . . H41 H 0.5086 0.1276 0.9885 0.031 Uiso 1 1 calc R . . C42 C 0.4423(5) 0.1389(5) 0.8648(4) 0.0278(14) Uani 1 1 d . . . H42A H 0.3669 0.172 0.8925 0.033 Uiso 1 1 calc R . . H42B H 0.446 0.0681 0.8493 0.033 Uiso 1 1 calc R . . C43 C 0.4523(6) 0.2264(6) 0.7799(5) 0.0338(15) Uani 1 1 d . . . H43A H 0.412 0.2203 0.7311 0.041 Uiso 1 1 calc R . . H43B H 0.4126 0.3052 0.7891 0.041 Uiso 1 1 calc R . . H3P H 0.895(5) 0.175(5) 0.799(4) 0.031(18) Uiso 1 1 d . . . H2P H 0.810(6) 0.090(6) 1.030(5) 0.05(2) Uiso 1 1 d . . . O1 O 0.4122(14) 0.8037(12) 0.4904(9) 0.203(4) Uani 1 1 d D . . C101 C 0.3785(19) 0.9342(15) 0.4685(13) 0.203(4) Uani 1 1 d D . . H10A H 0.4472 0.9514 0.4733 0.243 Uiso 1 1 calc R . . H10B H 0.3502 0.9676 0.4065 0.243 Uiso 1 1 calc R . . C102 C 0.2954(19) 0.9850(13) 0.5238(14) 0.203(4) Uani 1 1 d D . . H10C H 0.2386 1.0589 0.4905 0.243 Uiso 1 1 calc R . . H10D H 0.3296 1 0.5715 0.243 Uiso 1 1 calc R . . C103 C 0.2431(17) 0.9035(15) 0.5594(13) 0.203(4) Uani 1 1 d D . . H10E H 0.1867 0.9089 0.517 0.243 Uiso 1 1 calc R . . H10F H 0.2035 0.917 0.6157 0.243 Uiso 1 1 calc R . . C104 C 0.3362(18) 0.7925(15) 0.5746(12) 0.203(4) Uani 1 1 d D . . H10G H 0.3077 0.7299 0.5797 0.243 Uiso 1 1 calc R . . H10H H 0.3796 0.7771 0.6292 0.243 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0287(3) 0.0306(3) 0.0242(3) -0.0090(2) 0.0010(2) -0.0193(2) Rh2 0.0240(3) 0.0231(2) 0.0190(3) -0.00542(19) 0.00016(19) -0.0141(2) P1 0.0266(9) 0.0442(10) 0.0223(9) -0.0101(8) -0.0006(7) -0.0193(8) P2 0.0241(8) 0.0361(9) 0.0207(9) -0.0085(7) 0.0010(7) -0.0149(7) P3 0.0274(8) 0.0270(8) 0.0203(8) -0.0057(7) 0.0010(7) -0.0154(7) C1 0.022(3) 0.022(3) 0.026(3) -0.012(3) 0.002(3) -0.009(2) C2 0.024(3) 0.022(3) 0.032(4) -0.011(3) 0.000(3) -0.007(3) C3 0.034(3) 0.029(3) 0.024(3) -0.011(3) 0.002(3) -0.015(3) C4 0.031(3) 0.024(3) 0.026(4) -0.002(3) -0.008(3) -0.009(3) C5 0.028(3) 0.027(3) 0.030(4) -0.006(3) -0.002(3) -0.010(3) C6 0.026(3) 0.028(3) 0.028(4) -0.013(3) -0.001(3) -0.011(3) C7 0.026(3) 0.042(4) 0.029(4) -0.016(3) 0.002(3) -0.008(3) C8 0.052(5) 0.043(4) 0.025(4) -0.005(3) -0.013(3) -0.013(4) C9 0.029(4) 0.036(4) 0.043(4) -0.025(3) -0.006(3) 0.002(3) C10 0.026(3) 0.029(3) 0.021(3) -0.009(3) 0.001(3) -0.014(3) C11 0.026(3) 0.023(3) 0.035(4) -0.014(3) 0.001(3) -0.010(3) C12 0.029(3) 0.036(4) 0.042(4) -0.024(3) 0.008(3) -0.017(3) C13 0.041(4) 0.052(4) 0.037(4) -0.029(4) 0.013(3) -0.031(4) C14 0.043(4) 0.043(4) 0.021(4) -0.005(3) 0.002(3) -0.027(3) C15 0.033(4) 0.034(3) 0.028(4) -0.007(3) -0.002(3) -0.018(3) C16 0.026(3) 0.024(3) 0.044(4) -0.008(3) -0.003(3) -0.004(3) C17 0.071(6) 0.075(6) 0.040(5) -0.032(4) 0.026(4) -0.050(5) C18 0.039(4) 0.033(4) 0.039(5) 0.010(3) -0.005(3) -0.003(3) C19 0.025(3) 0.026(3) 0.023(3) -0.006(3) 0.003(3) -0.017(3) C20 0.030(3) 0.029(3) 0.029(4) -0.007(3) -0.002(3) -0.014(3) C21 0.045(4) 0.049(4) 0.029(4) -0.015(3) 0.010(3) -0.014(4) C22 0.051(5) 0.037(4) 0.027(4) 0.003(3) -0.007(3) -0.005(4) C23 0.033(4) 0.024(3) 0.037(4) 0.000(3) -0.002(3) -0.004(3) C24 0.031(3) 0.032(3) 0.031(4) -0.013(3) 0.006(3) -0.018(3) C25 0.036(4) 0.031(3) 0.040(4) -0.012(3) 0.000(3) -0.009(3) C26 0.078(7) 0.077(7) 0.031(5) 0.003(5) -0.001(5) -0.005(5) C27 0.036(4) 0.031(4) 0.036(4) -0.009(3) 0.002(3) -0.009(3) C28 0.053(4) 0.047(4) 0.027(4) -0.002(3) -0.002(3) -0.039(4) C29 0.049(4) 0.061(5) 0.032(4) -0.021(4) 0.014(3) -0.042(4) C30 0.033(4) 0.057(5) 0.066(6) -0.030(4) 0.012(4) -0.024(4) C31 0.035(4) 0.051(5) 0.066(6) -0.021(4) -0.004(4) -0.021(4) C32 0.032(4) 0.044(4) 0.041(4) -0.017(3) -0.001(3) -0.021(3) C33 0.048(4) 0.045(4) 0.041(4) -0.016(3) 0.000(3) -0.032(4) C34 0.051(5) 0.039(4) 0.076(7) -0.018(4) -0.011(4) -0.019(4) C35 0.064(5) 0.041(4) 0.057(6) 0.004(4) -0.017(4) -0.037(4) C36 0.033(3) 0.036(4) 0.024(3) -0.004(3) -0.011(3) -0.021(3) C37 0.032(3) 0.041(4) 0.024(3) -0.015(3) 0.005(3) -0.024(3) C38 0.038(4) 0.041(4) 0.041(4) -0.022(3) 0.010(3) -0.024(3) C39 0.035(4) 0.027(3) 0.046(4) -0.014(3) 0.009(3) -0.021(3) C40 0.028(3) 0.029(3) 0.024(3) -0.004(3) 0.002(3) -0.015(3) C41 0.029(3) 0.033(3) 0.022(3) -0.007(3) 0.008(3) -0.021(3) C42 0.026(3) 0.034(3) 0.028(4) -0.007(3) 0.005(3) -0.018(3) C43 0.031(4) 0.038(4) 0.037(4) -0.008(3) -0.005(3) -0.018(3) O1 0.277(12) 0.164(7) 0.126(7) 0.038(6) -0.062(7) -0.072(8) C101 0.277(12) 0.164(7) 0.126(7) 0.038(6) -0.062(7) -0.072(8) C102 0.277(12) 0.164(7) 0.126(7) 0.038(6) -0.062(7) -0.072(8) C103 0.277(12) 0.164(7) 0.126(7) 0.038(6) -0.062(7) -0.072(8) C104 0.277(12) 0.164(7) 0.126(7) 0.038(6) -0.062(7) -0.072(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C29 2.163(7) . ? Rh1 C28 2.173(7) . ? Rh1 C33 2.187(7) . ? Rh1 C32 2.188(6) . ? Rh1 P1 2.2878(18) . ? Rh1 P3 2.3708(17) . ? Rh2 C40 2.175(6) . ? Rh2 C36 2.188(6) . ? Rh2 C41 2.191(6) . ? Rh2 C37 2.206(6) . ? Rh2 P2 2.2878(18) . ? Rh2 P3 2.3724(17) . ? P1 C1 1.842(6) . ? P1 P2 2.168(2) . ? P2 C10 1.832(6) . ? P2 H2P 1.11(7) . ? P3 C19 1.833(6) . ? P3 H3P 1.26(6) . ? C1 C2 1.394(8) . ? C1 C6 1.423(8) . ? C2 C3 1.384(9) . ? C2 C7 1.510(8) . ? C3 C4 1.373(9) . ? C3 H3 0.95 . ? C4 C5 1.381(9) . ? C4 C8 1.508(9) . ? C5 C6 1.384(9) . ? C5 H5 0.95 . ? C6 C9 1.511(8) . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 C11 1.404(8) . ? C10 C15 1.430(9) . ? C11 C12 1.379(9) . ? C11 C16 1.499(9) . ? C12 C13 1.369(10) . ? C12 H12 0.95 . ? C13 C14 1.405(10) . ? C13 C17 1.516(10) . ? C14 C15 1.368(9) . ? C14 H14 0.95 . ? C15 C18 1.502(9) . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 C20 1.399(9) . ? C19 C24 1.414(9) . ? C20 C21 1.388(10) . ? C20 C25 1.517(9) . ? C21 C22 1.396(10) . ? C21 H21 0.95 . ? C22 C23 1.363(10) . ? C22 C26 1.508(11) . ? C23 C24 1.373(9) . ? C23 H23 0.95 . ? C24 C27 1.499(9) . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C28 C29 1.361(10) . ? C28 C35 1.528(9) . ? C28 H28 1 . ? C29 C30 1.501(10) . ? C29 H29 1 . ? C30 C31 1.522(11) . ? C30 H30A 0.99 . ? C30 H30B 0.99 . ? C31 C32 1.534(10) . ? C31 H31A 0.99 . ? C31 H31B 0.99 . ? C32 C33 1.376(10) . ? C32 H32 1 . ? C33 C34 1.516(11) . ? C33 H33 1 . ? C34 C35 1.555(12) . ? C34 H34A 0.99 . ? C34 H34B 0.99 . ? C35 H35A 0.99 . ? C35 H35B 0.99 . ? C36 C37 1.371(9) . ? C36 C43 1.522(9) . ? C36 H36 1 . ? C37 C38 1.514(9) . ? C37 H37 1 . ? C38 C39 1.555(10) . ? C38 H38A 0.99 . ? C38 H38B 0.99 . ? C39 C40 1.484(9) . ? C39 H39A 0.99 . ? C39 H39B 0.99 . ? C40 C41 1.391(9) . ? C40 H40 1 . ? C41 C42 1.511(9) . ? C41 H41 1 . ? C42 C43 1.532(9) . ? C42 H42A 0.99 . ? C42 H42B 0.99 . ? C43 H43A 0.99 . ? C43 H43B 0.99 . ? O1 C101 1.523(17) . ? O1 C104 1.561(18) . ? C101 C102 1.365(16) . ? C101 H10A 0.99 . ? C101 H10B 0.99 . ? C102 C103 1.421(17) . ? C102 H10C 0.99 . ? C102 H10D 0.99 . ? C103 C104 1.438(17) . ? C103 H10E 0.99 . ? C103 H10F 0.99 . ? C104 H10G 0.99 . ? C104 H10H 0.99 . ? 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 C29 Rh1 C28 36.6(3) . . ? C29 Rh1 C33 95.5(3) . . ? C28 Rh1 C33 81.2(3) . . ? C29 Rh1 C32 81.1(3) . . ? C28 Rh1 C32 89.3(3) . . ? C33 Rh1 C32 36.7(3) . . ? C29 Rh1 P1 168.3(2) . . ? C28 Rh1 P1 155.1(2) . . ? C33 Rh1 P1 88.2(2) . . ? C32 Rh1 P1 95.6(2) . . ? C29 Rh1 P3 91.12(19) . . ? C28 Rh1 P3 97.45(18) . . ? C33 Rh1 P3 166.5(2) . . ? C32 Rh1 P3 156.71(19) . . ? P1 Rh1 P3 87.67(6) . . ? C40 Rh2 C36 96.4(2) . . ? C40 Rh2 C41 37.2(2) . . ? C36 Rh2 C41 81.0(2) . . ? C40 Rh2 C37 80.7(2) . . ? C36 Rh2 C37 36.4(2) . . ? C41 Rh2 C37 87.9(2) . . ? C40 Rh2 P2 91.06(18) . . ? C36 Rh2 P2 161.30(18) . . ? C41 Rh2 P2 94.99(18) . . ? C37 Rh2 P2 162.31(18) . . ? C40 Rh2 P3 152.23(17) . . ? C36 Rh2 P3 96.20(17) . . ? C41 Rh2 P3 170.52(17) . . ? C37 Rh2 P3 95.26(16) . . ? P2 Rh2 P3 84.76(6) . . ? C1 P1 P2 100.31(19) . . ? C1 P1 Rh1 118.81(19) . . ? P2 P1 Rh1 113.13(9) . . ? C10 P2 P1 102.7(2) . . ? C10 P2 Rh2 118.4(2) . . ? P1 P2 Rh2 115.72(9) . . ? C10 P2 H2P 102(4) . . ? P1 P2 H2P 107(4) . . ? Rh2 P2 H2P 109(4) . . ? C19 P3 Rh1 110.92(18) . . ? C19 P3 Rh2 111.16(18) . . ? Rh1 P3 Rh2 128.31(8) . . ? C19 P3 H3P 98(3) . . ? Rh1 P3 H3P 99(3) . . ? Rh2 P3 H3P 104(3) . . ? C2 C1 C6 117.9(6) . . ? C2 C1 P1 120.2(4) . . ? C6 C1 P1 121.9(4) . . ? C3 C2 C1 119.6(6) . . ? C3 C2 C7 118.2(6) . . ? C1 C2 C7 122.2(6) . . ? C4 C3 C2 123.2(6) . . ? C4 C3 H3 118.4 . . ? C2 C3 H3 118.4 . . ? C3 C4 C5 117.5(6) . . ? C3 C4 C8 121.9(6) . . ? C5 C4 C8 120.6(6) . . ? C4 C5 C6 121.8(6) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C5 C6 C1 120.0(6) . . ? C5 C6 C9 117.3(6) . . ? C1 C6 C9 122.7(6) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 118.8(6) . . ? C11 C10 P2 119.6(5) . . ? C15 C10 P2 121.6(5) . . ? C12 C11 C10 119.6(6) . . ? C12 C11 C16 117.8(6) . . ? C10 C11 C16 122.6(6) . . ? C13 C12 C11 122.4(6) . . ? C13 C12 H12 118.8 . . ? C11 C12 H12 118.8 . . ? C12 C13 C14 118.2(6) . . ? C12 C13 C17 122.4(7) . . ? C14 C13 C17 119.4(7) . . ? C15 C14 C13 121.8(6) . . ? C15 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? C14 C15 C10 119.1(6) . . ? C14 C15 C18 119.0(6) . . ? C10 C15 C18 121.8(6) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 118.7(6) . . ? C20 C19 P3 124.4(5) . . ? C24 C19 P3 116.8(5) . . ? C21 C20 C19 118.9(6) . . ? C21 C20 C25 117.0(6) . . ? C19 C20 C25 124.1(6) . . ? C20 C21 C22 122.1(7) . . ? C20 C21 H21 119 . . ? C22 C21 H21 119 . . ? C23 C22 C21 118.2(7) . . ? C23 C22 C26 121.9(7) . . ? C21 C22 C26 119.9(7) . . ? C22 C23 C24 121.9(6) . . ? C22 C23 H23 119 . . ? C24 C23 H23 119 . . ? C23 C24 C19 120.2(6) . . ? C23 C24 C27 119.6(6) . . ? C19 C24 C27 120.2(6) . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C35 122.8(7) . . ? C29 C28 Rh1 71.3(4) . . ? C35 C28 Rh1 113.7(5) . . ? C29 C28 H28 114 . . ? C35 C28 H28 114 . . ? Rh1 C28 H28 114 . . ? C28 C29 C30 125.8(6) . . ? C28 C29 Rh1 72.1(4) . . ? C30 C29 Rh1 110.9(5) . . ? C28 C29 H29 113.5 . . ? C30 C29 H29 113.5 . . ? Rh1 C29 H29 113.5 . . ? C29 C30 C31 112.8(6) . . ? C29 C30 H30A 109 . . ? C31 C30 H30A 109 . . ? C29 C30 H30B 109 . . ? C31 C30 H30B 109 . . ? H30A C30 H30B 107.8 . . ? C30 C31 C32 113.8(6) . . ? C30 C31 H31A 108.8 . . ? C32 C31 H31A 108.8 . . ? C30 C31 H31B 108.8 . . ? C32 C31 H31B 108.8 . . ? H31A C31 H31B 107.7 . . ? C33 C32 C31 120.5(7) . . ? C33 C32 Rh1 71.7(4) . . ? C31 C32 Rh1 111.4(5) . . ? C33 C32 H32 115.2 . . ? C31 C32 H32 115.2 . . ? Rh1 C32 H32 115.2 . . ? C32 C33 C34 125.8(7) . . ? C32 C33 Rh1 71.7(4) . . ? C34 C33 Rh1 109.9(5) . . ? C32 C33 H33 113.8 . . ? C34 C33 H33 113.8 . . ? Rh1 C33 H33 113.8 . . ? C33 C34 C35 113.9(6) . . ? C33 C34 H34A 108.8 . . ? C35 C34 H34A 108.8 . . ? C33 C34 H34B 108.8 . . ? C35 C34 H34B 108.8 . . ? H34A C34 H34B 107.7 . . ? C28 C35 C34 112.4(6) . . ? C28 C35 H35A 109.1 . . ? C34 C35 H35A 109.1 . . ? C28 C35 H35B 109.1 . . ? C34 C35 H35B 109.1 . . ? H35A C35 H35B 107.8 . . ? C37 C36 C43 125.4(6) . . ? C37 C36 Rh2 72.5(4) . . ? C43 C36 Rh2 107.5(4) . . ? C37 C36 H36 114.3 . . ? C43 C36 H36 114.3 . . ? Rh2 C36 H36 114.3 . . ? C36 C37 C38 125.5(6) . . ? C36 C37 Rh2 71.1(4) . . ? C38 C37 Rh2 111.8(5) . . ? C36 C37 H37 113.6 . . ? C38 C37 H37 113.6 . . ? Rh2 C37 H37 113.6 . . ? C37 C38 C39 113.6(5) . . ? C37 C38 H38A 108.8 . . ? C39 C38 H38A 108.8 . . ? C37 C38 H38B 108.8 . . ? C39 C38 H38B 108.8 . . ? H38A C38 H38B 107.7 . . ? C40 C39 C38 113.2(5) . . ? C40 C39 H39A 108.9 . . ? C38 C39 H39A 108.9 . . ? C40 C39 H39B 108.9 . . ? C38 C39 H39B 108.9 . . ? H39A C39 H39B 107.8 . . ? C41 C40 C39 125.6(6) . . ? C41 C40 Rh2 72.0(3) . . ? C39 C40 Rh2 110.7(4) . . ? C41 C40 H40 113.7 . . ? C39 C40 H40 113.7 . . ? Rh2 C40 H40 113.7 . . ? C40 C41 C42 123.8(6) . . ? C40 C41 Rh2 70.8(3) . . ? C42 C41 Rh2 112.9(4) . . ? C40 C41 H41 114 . . ? C42 C41 H41 114 . . ? Rh2 C41 H41 114 . . ? C41 C42 C43 111.8(5) . . ? C41 C42 H42A 109.3 . . ? C43 C42 H42A 109.3 . . ? C41 C42 H42B 109.3 . . ? C43 C42 H42B 109.3 . . ? H42A C42 H42B 107.9 . . ? C36 C43 C42 114.1(5) . . ? C36 C43 H43A 108.7 . . ? C42 C43 H43A 108.7 . . ? C36 C43 H43B 108.7 . . ? C42 C43 H43B 108.7 . . ? H43A C43 H43B 107.6 . . ? C101 O1 C104 97.7(15) . . ? C102 C101 O1 112.2(14) . . ? C102 C101 H10A 109.2 . . ? O1 C101 H10A 109.2 . . ? C102 C101 H10B 109.2 . . ? O1 C101 H10B 109.2 . . ? H10A C101 H10B 107.9 . . ? C101 C102 C103 104.6(12) . . ? C101 C102 H10C 110.8 . . ? C103 C102 H10C 110.8 . . ? C101 C102 H10D 110.8 . . ? C103 C102 H10D 110.8 . . ? H10C C102 H10D 108.9 . . ? C102 C103 C104 105.1(12) . . ? C102 C103 H10E 110.7 . . ? C104 C103 H10E 110.7 . . ? C102 C103 H10F 110.7 . . ? C104 C103 H10F 110.7 . . ? H10E C103 H10F 108.8 . . ? C103 C104 O1 103.3(12) . . ? C103 C104 H10G 111.1 . . ? O1 C104 H10G 111.1 . . ? C103 C104 H10H 111.1 . . ? O1 C104 H10H 111.1 . . ? H10G C104 H10H 109.1 . . ? #============================================================================ data_x0163fin _database_code_depnum_ccdc_archive 'CCDC 666348' _audit_creation_date 2007-03-06T18:41:04-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C90 H108 Cu4 P12' _chemical_formula_weight 1815.56 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 14.208(5) _cell_length_b 18.536(5) _cell_length_c 16.923(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 107.519(5) _cell_angle_gamma 90.000(5) _cell_volume 4250(2) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 29072 _cell_measurement_theta_min 2.506 _cell_measurement_theta_max 32.4146 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.258 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.95685 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 0.0095447304 _diffrn_orient_matrix_ub_12 0.0314367444 _diffrn_orient_matrix_ub_13 0.0248696973 _diffrn_orient_matrix_ub_21 -0.0506801414 _diffrn_orient_matrix_ub_22 0.0090171812 _diffrn_orient_matrix_ub_23 -0.0141692375 _diffrn_orient_matrix_ub_31 -0.0079922809 _diffrn_orient_matrix_ub_32 -0.019696465 _diffrn_orient_matrix_ub_33 0.0331822145 _diffrn_measurement_device_type 'ccd xcalibur s' _diffrn_measurement_method '\w scans and \f scans' _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_unetI/netI 0.0397 _diffrn_reflns_number 99893 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 27.1 _diffrn_reflns_theta_full 27.1 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 9374 _reflns_number_gt 6901 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick,1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+0.6759P] 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_number_reflns 9374 _refine_ls_number_parameters 486 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0786 _refine_ls_wR_factor_gt 0.066 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.797 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.073 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu 0.3201 1.2651 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu2 Cu 1.22136(2) 0.002281(15) 0.638875(17) 0.01736(7) Uani 1 1 d . . . Cu1 Cu 1.05320(2) 0.058691(15) 0.429431(17) 0.01636(7) Uani 1 1 d . . . P6 P 1.35456(5) -0.00981(3) 0.74843(4) 0.01914(14) Uani 1 1 d . . . P3 P 1.03724(5) 0.14798(3) 0.60515(4) 0.01683(13) Uani 1 1 d . . . P4 P 1.15035(4) 0.09876(3) 0.55906(4) 0.01606(13) Uani 1 1 d . . . P2 P 0.92379(4) 0.06528(3) 0.55349(4) 0.01534(13) Uani 1 1 d . . . P1 P 0.89176(4) 0.08401(3) 0.42048(4) 0.01603(13) Uani 1 1 d . . . P5 P 1.12770(5) 0.09686(4) 0.33865(4) 0.02288(15) Uani 1 1 d . . . C36 C 1.42339(18) 0.07167(13) 0.79194(15) 0.0237(5) Uani 1 1 d . . . H36 H 1.4788 0.0582 0.8421 0.028 Uiso 1 1 calc R . . C23 C 1.3707(2) 0.21810(15) 0.51602(15) 0.0285(6) Uani 1 1 d . . . H23 H 1.4244 0.2078 0.4954 0.034 Uiso 1 1 calc R . . C4 C 0.8016(2) 0.32402(14) 0.37494(16) 0.0321(7) Uani 1 1 d . . . H4 H 0.7821 0.3729 0.3639 0.039 Uiso 1 1 calc R . . C12 C 0.8230(2) 0.15727(14) 0.63704(16) 0.0291(6) Uani 1 1 d . . . H12 H 0.8832 0.1828 0.6587 0.035 Uiso 1 1 calc R . . C16 C 1.13660(19) 0.10665(14) 0.88790(15) 0.0250(6) Uani 1 1 d . . . H16 H 1.158 0.0996 0.9462 0.03 Uiso 1 1 calc R . . C25 C 1.08520(19) 0.09361(13) 0.22626(15) 0.0235(5) Uani 1 1 d . . . C45 C 1.44473(19) -0.07233(14) 0.72791(16) 0.0259(6) Uani 1 1 d . . . H45 H 1.4168 -0.1219 0.7277 0.031 Uiso 1 1 calc R . . C3 C 0.8918(2) 0.30146(14) 0.36991(17) 0.0333(7) Uani 1 1 d . . . H3 H 0.9347 0.3347 0.3554 0.04 Uiso 1 1 calc R . . C11 C 0.7402(2) 0.17861(16) 0.65799(17) 0.0366(7) Uani 1 1 d . . . H11 H 0.7443 0.2182 0.6945 0.044 Uiso 1 1 calc R . . C17 C 1.09965(19) 0.04963(14) 0.83592(15) 0.0252(6) Uani 1 1 d . . . H17 H 1.0945 0.0033 0.8584 0.03 Uiso 1 1 calc R . . C21 C 1.2774(2) 0.30201(13) 0.56859(15) 0.0273(6) Uani 1 1 d . . . H21 H 1.2668 0.3497 0.5846 0.033 Uiso 1 1 calc R . . C7 C 0.81895(18) 0.09898(13) 0.58469(14) 0.0200(5) Uani 1 1 d . . . C10 C 0.6528(2) 0.14312(16) 0.62652(18) 0.0379(7) Uani 1 1 d . . . H10 H 0.5957 0.1591 0.6396 0.045 Uiso 1 1 calc R . . C28 C 1.0238(2) 0.09163(19) 0.05473(18) 0.0437(8) Uani 1 1 d . . . H28 H 1.0033 0.0911 -0.0041 0.052 Uiso 1 1 calc R . . C1 C 0.85826(18) 0.17989(12) 0.40593(14) 0.0186(5) Uani 1 1 d . . . C20 C 1.21385(19) 0.24700(13) 0.57566(15) 0.0221(5) Uani 1 1 d . . . H20 H 1.16 0.2577 0.596 0.027 Uiso 1 1 calc R . . C18 C 1.06976(18) 0.05957(13) 0.75059(14) 0.0221(5) Uani 1 1 d . . . H18 H 1.0452 0.0198 0.715 0.027 Uiso 1 1 calc R . . C22 C 1.3554(2) 0.28805(15) 0.53865(15) 0.0297(6) Uani 1 1 d . . . H22 H 1.3984 0.3259 0.5335 0.036 Uiso 1 1 calc R . . C13 C 1.07546(17) 0.12708(13) 0.71690(14) 0.0183(5) Uani 1 1 d . . . C2 C 0.9201(2) 0.22991(13) 0.38613(15) 0.0256(6) Uani 1 1 d . . . H2 H 0.9831 0.215 0.3836 0.031 Uiso 1 1 calc R . . C15 C 1.1426(2) 0.17416(14) 0.85534(15) 0.0264(6) Uani 1 1 d . . . H15 H 1.168 0.2136 0.8913 0.032 Uiso 1 1 calc R . . C8 C 0.73039(19) 0.06217(14) 0.55582(16) 0.0265(6) Uani 1 1 d . . . H8 H 0.7266 0.021 0.5216 0.032 Uiso 1 1 calc R . . C5 C 0.7397(2) 0.27578(14) 0.39587(16) 0.0306(6) Uani 1 1 d . . . H5 H 0.678 0.2917 0.4004 0.037 Uiso 1 1 calc R . . C6 C 0.76678(19) 0.20418(13) 0.41032(15) 0.0255(6) Uani 1 1 d . . . H6 H 0.7226 0.1711 0.4234 0.031 Uiso 1 1 calc R . . C41 C 1.4553(2) -0.06041(15) 0.64131(16) 0.0330(6) Uani 1 1 d . . . H41A H 1.3977 -0.0802 0.598 0.04 Uiso 1 1 calc R . . H41B H 1.4616 -0.0084 0.6305 0.04 Uiso 1 1 calc R . . C35 C 1.4059(2) -0.0540(2) 0.91987(18) 0.0570(10) Uani 1 1 d . . . H35A H 1.4684 -0.0681 0.9096 0.068 Uiso 1 1 calc R . . H35B H 1.4166 -0.0088 0.9525 0.068 Uiso 1 1 calc R . . C14 C 1.11168(18) 0.18439(13) 0.77060(14) 0.0227(5) Uani 1 1 d . . . H14 H 1.1152 0.2311 0.7487 0.027 Uiso 1 1 calc R . . C26 C 1.1237(2) 0.04337(16) 0.18320(17) 0.0331(6) Uani 1 1 d . . . H26 H 1.1712 0.0092 0.2125 0.04 Uiso 1 1 calc R . . C29 C 0.9837(2) 0.14092(16) 0.09536(17) 0.0394(7) Uani 1 1 d . . . H29 H 0.9361 0.1747 0.0651 0.047 Uiso 1 1 calc R . . C19 C 1.22816(17) 0.17631(12) 0.55330(13) 0.0179(5) Uani 1 1 d . . . C37 C 1.3575(2) 0.12696(15) 0.8169(2) 0.0382(7) Uani 1 1 d . . . H37A H 1.2916 0.1294 0.7752 0.046 Uiso 1 1 calc R . . H37B H 1.3494 0.1149 0.8715 0.046 Uiso 1 1 calc R . . C44 C 1.5511(2) -0.07541(18) 0.78537(19) 0.0402(7) Uani 1 1 d . . . H44A H 1.569 -0.0298 0.8167 0.048 Uiso 1 1 calc R . . H44B H 1.5594 -0.1158 0.8252 0.048 Uiso 1 1 calc R . . C27 C 1.0924(2) 0.04348(18) 0.09727(19) 0.0440(8) Uani 1 1 d . . . H27 H 1.1192 0.0095 0.0679 0.053 Uiso 1 1 calc R . . C38 C 1.4131(3) 0.19763(17) 0.8208(2) 0.0527(9) Uani 1 1 d . . . H38A H 1.3671 0.2391 0.8121 0.063 Uiso 1 1 calc R . . H38B H 1.4639 0.2031 0.8752 0.063 Uiso 1 1 calc R . . C31 C 1.32360(19) -0.04498(14) 0.83874(15) 0.0253(6) Uani 1 1 d . . . H31 H 1.2779 -0.0084 0.8507 0.03 Uiso 1 1 calc R . . C30 C 1.0133(2) 0.14102(14) 0.18164(16) 0.0291(6) Uani 1 1 d . . . H30 H 0.9839 0.1739 0.2102 0.035 Uiso 1 1 calc R . . C9 C 0.6473(2) 0.08418(17) 0.57590(18) 0.0367(7) Uani 1 1 d . . . H9 H 0.5869 0.0587 0.5548 0.044 Uiso 1 1 calc R . . C24 C 1.30805(19) 0.16352(14) 0.52341(15) 0.0250(6) Uani 1 1 d . . . H24 H 1.3196 0.1159 0.5077 0.03 Uiso 1 1 calc R . . C39 C 1.4601(2) 0.19370(15) 0.75282(18) 0.0411(8) Uani 1 1 d . . . H39A H 1.5271 0.215 0.7713 0.049 Uiso 1 1 calc R . . H39B H 1.4201 0.2205 0.7036 0.049 Uiso 1 1 calc R . . C32 C 1.2664(3) -0.11561(16) 0.82580(18) 0.0426(8) Uani 1 1 d . . . H32A H 1.1966 -0.1081 0.793 0.051 Uiso 1 1 calc R . . H32B H 1.2964 -0.1517 0.7975 0.051 Uiso 1 1 calc R . . C33 C 1.2750(4) -0.1389(2) 0.9136(2) 0.0716(13) Uani 1 1 d . . . H33A H 1.2212 -0.1175 0.9318 0.086 Uiso 1 1 calc R . . H33B H 1.271 -0.1921 0.9168 0.086 Uiso 1 1 calc R . . C34 C 1.3693(3) -0.1138(3) 0.9647(3) 0.108(2) Uani 1 1 d . . . H34A H 1.4171 -0.1541 0.977 0.13 Uiso 1 1 calc R . . H34B H 1.3631 -0.0953 1.0178 0.13 Uiso 1 1 calc R . . C42 C 1.5478(3) -0.10034(18) 0.6435(2) 0.0504(9) Uani 1 1 d . . . H42A H 1.5346 -0.1526 0.6338 0.06 Uiso 1 1 calc R . . H42B H 1.5765 -0.0814 0.6011 0.06 Uiso 1 1 calc R . . C40 C 1.4656(2) 0.11364(14) 0.73181(17) 0.0303(6) Uani 1 1 d . . . H40A H 1.5348 0.0992 0.7392 0.036 Uiso 1 1 calc R . . H40B H 1.4262 0.1041 0.6737 0.036 Uiso 1 1 calc R . . C43 C 1.6147(3) -0.0869(2) 0.7283(2) 0.0687(12) Uani 1 1 d . . . H43A H 1.6557 -0.0437 0.7285 0.082 Uiso 1 1 calc R . . H43B H 1.6591 -0.1288 0.7474 0.082 Uiso 1 1 calc R . . H1P H 1.155(2) 0.1641(16) 0.3502(18) 0.051(9) Uiso 1 1 d . . . H2P H 1.215(2) 0.0702(15) 0.3478(16) 0.041(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu2 0.01701(15) 0.01922(14) 0.01512(14) -0.00001(11) 0.00376(11) -0.00081(12) Cu1 0.01810(15) 0.01804(14) 0.01359(14) -0.00005(11) 0.00574(11) 0.00018(12) P6 0.0170(3) 0.0224(3) 0.0170(3) 0.0008(2) 0.0036(2) -0.0003(2) P3 0.0193(3) 0.0171(3) 0.0141(3) -0.0012(2) 0.0050(2) -0.0015(2) P4 0.0172(3) 0.0166(3) 0.0145(3) -0.0007(2) 0.0049(2) -0.0018(2) P2 0.0164(3) 0.0167(3) 0.0137(3) -0.0004(2) 0.0056(2) -0.0002(2) P1 0.0172(3) 0.0167(3) 0.0139(3) 0.0000(2) 0.0043(2) 0.0000(2) P5 0.0242(4) 0.0282(3) 0.0170(3) 0.0023(3) 0.0072(3) -0.0050(3) C36 0.0188(13) 0.0266(13) 0.0252(13) -0.0029(11) 0.0058(11) -0.0021(10) C23 0.0248(15) 0.0402(16) 0.0232(13) -0.0027(12) 0.0112(11) -0.0091(12) C4 0.0427(18) 0.0188(13) 0.0311(15) 0.0016(11) 0.0055(13) 0.0078(12) C12 0.0300(15) 0.0323(14) 0.0265(14) -0.0043(11) 0.0108(12) 0.0025(12) C16 0.0271(14) 0.0340(14) 0.0142(12) -0.0004(10) 0.0067(11) 0.0010(11) C25 0.0270(14) 0.0270(13) 0.0193(12) -0.0014(10) 0.0115(11) -0.0115(11) C45 0.0261(14) 0.0227(13) 0.0304(14) 0.0035(11) 0.0106(12) 0.0005(11) C3 0.0386(17) 0.0230(14) 0.0388(16) 0.0052(12) 0.0122(14) -0.0014(12) C11 0.0439(19) 0.0392(16) 0.0336(16) -0.0025(13) 0.0219(14) 0.0125(14) C17 0.0266(14) 0.0282(13) 0.0231(13) 0.0060(11) 0.0107(11) -0.0018(11) C21 0.0315(15) 0.0202(13) 0.0247(13) 0.0007(10) 0.0001(12) -0.0043(11) C7 0.0216(13) 0.0236(12) 0.0171(12) 0.0047(10) 0.0094(10) 0.0054(10) C10 0.0343(17) 0.0502(18) 0.0387(17) 0.0084(14) 0.0252(14) 0.0162(14) C28 0.050(2) 0.060(2) 0.0226(15) -0.0043(15) 0.0141(15) -0.0254(17) C1 0.0197(13) 0.0220(12) 0.0125(11) -0.0015(9) 0.0024(10) -0.0005(10) C20 0.0214(13) 0.0257(13) 0.0179(12) 0.0008(10) 0.0038(10) -0.0028(10) C18 0.0243(13) 0.0241(13) 0.0182(12) -0.0029(10) 0.0069(11) -0.0046(10) C22 0.0294(15) 0.0330(15) 0.0230(14) 0.0028(11) 0.0024(12) -0.0155(12) C13 0.0153(12) 0.0246(12) 0.0154(11) -0.0014(10) 0.0054(10) 0.0013(10) C2 0.0257(14) 0.0234(13) 0.0288(14) 0.0003(11) 0.0099(12) 0.0006(11) C15 0.0302(15) 0.0290(14) 0.0189(13) -0.0091(11) 0.0054(11) 0.0007(11) C8 0.0248(14) 0.0268(13) 0.0310(14) 0.0007(11) 0.0133(12) -0.0008(11) C5 0.0319(16) 0.0294(14) 0.0308(15) 0.0016(12) 0.0100(12) 0.0114(12) C6 0.0249(14) 0.0242(13) 0.0268(14) 0.0025(11) 0.0072(11) 0.0028(11) C41 0.0383(17) 0.0359(16) 0.0279(15) -0.0074(12) 0.0148(13) 0.0012(13) C35 0.0368(19) 0.104(3) 0.0234(16) 0.0214(17) -0.0004(14) -0.0148(19) C14 0.0258(14) 0.0223(12) 0.0194(12) -0.0025(10) 0.0059(11) 0.0020(10) C26 0.0310(16) 0.0389(16) 0.0325(15) -0.0063(13) 0.0143(13) -0.0078(13) C29 0.0435(19) 0.0385(17) 0.0292(15) 0.0091(13) 0.0006(14) -0.0169(14) C19 0.0185(12) 0.0210(12) 0.0122(11) 0.0001(9) 0.0018(9) -0.0036(10) C37 0.0294(16) 0.0363(16) 0.0523(19) -0.0184(14) 0.0176(14) -0.0063(13) C44 0.0285(16) 0.0516(19) 0.0393(17) 0.0111(14) 0.0083(13) 0.0150(14) C27 0.046(2) 0.061(2) 0.0347(17) -0.0173(16) 0.0262(16) -0.0170(17) C38 0.061(2) 0.0340(18) 0.066(2) -0.0108(16) 0.025(2) -0.0059(16) C31 0.0220(14) 0.0355(15) 0.0183(12) 0.0020(11) 0.0058(11) -0.0046(11) C30 0.0340(16) 0.0280(14) 0.0243(14) -0.0012(11) 0.0071(12) -0.0075(12) C9 0.0216(15) 0.0482(18) 0.0444(17) 0.0081(14) 0.0163(13) 0.0020(13) C24 0.0273(15) 0.0279(13) 0.0202(13) -0.0039(10) 0.0079(11) -0.0048(11) C39 0.048(2) 0.0306(16) 0.0375(17) -0.0027(13) 0.0022(15) -0.0078(14) C32 0.057(2) 0.0430(18) 0.0313(16) 0.0019(13) 0.0184(15) -0.0197(16) C33 0.112(4) 0.063(2) 0.041(2) 0.0074(18) 0.025(2) -0.037(2) C34 0.052(3) 0.192(6) 0.065(3) 0.084(3) -0.006(2) -0.035(3) C42 0.060(2) 0.0475(19) 0.055(2) 0.0091(16) 0.0351(19) 0.0217(17) C40 0.0285(15) 0.0280(14) 0.0355(15) 0.0020(12) 0.0111(13) -0.0043(11) C43 0.031(2) 0.105(3) 0.075(3) -0.021(2) 0.0219(19) 0.012(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu2 P6 2.2264(9) . ? Cu2 P1 2.2756(8) 3_756 ? Cu2 P4 2.2847(8) . ? Cu1 P5 2.2272(8) . ? Cu1 P1 2.3012(10) . ? Cu1 P2 2.3267(9) 3_756 ? Cu1 P4 2.3338(8) . ? P6 C36 1.829(3) . ? P6 C31 1.833(2) . ? P6 C45 1.836(3) . ? P3 C13 1.845(2) . ? P3 P4 2.1858(10) . ? P3 P2 2.2054(10) . ? P4 C19 1.834(2) . ? P2 C7 1.833(2) . ? P2 P1 2.1858(10) . ? P2 Cu1 2.3267(9) 3_756 ? P1 C1 1.837(2) . ? P1 Cu2 2.2756(8) 3_756 ? P5 C25 1.815(2) . ? P5 H1P 1.30(3) . ? P5 H2P 1.30(3) . ? C36 C37 1.531(4) . ? C36 C40 1.539(4) . ? C36 H36 1 . ? C23 C24 1.378(3) . ? C23 C22 1.387(4) . ? C23 H23 0.95 . ? C4 C3 1.375(4) . ? C4 C5 1.373(4) . ? C4 H4 0.95 . ? C12 C11 1.384(4) . ? C12 C7 1.387(3) . ? C12 H12 0.95 . ? C16 C17 1.374(3) . ? C16 C15 1.380(4) . ? C16 H16 0.95 . ? C25 C30 1.386(4) . ? C25 C26 1.392(4) . ? C45 C44 1.532(4) . ? C45 C41 1.533(4) . ? C45 H45 1 . ? C3 C2 1.389(3) . ? C3 H3 0.95 . ? C11 C10 1.364(4) . ? C11 H11 0.95 . ? C17 C18 1.389(3) . ? C17 H17 0.95 . ? C21 C22 1.375(4) . ? C21 C20 1.391(3) . ? C21 H21 0.95 . ? C7 C8 1.385(4) . ? C10 C9 1.376(4) . ? C10 H10 0.95 . ? C28 C27 1.357(5) . ? C28 C29 1.367(4) . ? C28 H28 0.95 . ? C1 C2 1.386(3) . ? C1 C6 1.398(3) . ? C20 C19 1.395(3) . ? C20 H20 0.95 . ? C18 C13 1.388(3) . ? C18 H18 0.95 . ? C22 H22 0.95 . ? C13 C14 1.392(3) . ? C2 H2 0.95 . ? C15 C14 1.381(3) . ? C15 H15 0.95 . ? C8 C9 1.384(4) . ? C8 H8 0.95 . ? C5 C6 1.383(3) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C41 C42 1.500(4) . ? C41 H41A 0.99 . ? C41 H41B 0.99 . ? C35 C34 1.520(5) . ? C35 C31 1.521(4) . ? C35 H35A 0.99 . ? C35 H35B 0.99 . ? C14 H14 0.95 . ? C26 C27 1.387(4) . ? C26 H26 0.95 . ? C29 C30 1.392(4) . ? C29 H29 0.95 . ? C19 C24 1.395(3) . ? C37 C38 1.521(4) . ? C37 H37A 0.99 . ? C37 H37B 0.99 . ? C44 C43 1.524(4) . ? C44 H44A 0.99 . ? C44 H44B 0.99 . ? C27 H27 0.95 . ? C38 C39 1.495(4) . ? C38 H38A 0.99 . ? C38 H38B 0.99 . ? C31 C32 1.522(4) . ? C31 H31 1 . ? C30 H30 0.95 . ? C9 H9 0.95 . ? C24 H24 0.95 . ? C39 C40 1.533(4) . ? C39 H39A 0.99 . ? C39 H39B 0.99 . ? C32 C33 1.516(4) . ? C32 H32A 0.99 . ? C32 H32B 0.99 . ? C33 C34 1.436(5) . ? C33 H33A 0.99 . ? C33 H33B 0.99 . ? C34 H34A 0.99 . ? C34 H34B 0.99 . ? C42 C43 1.485(5) . ? C42 H42A 0.99 . ? C42 H42B 0.99 . ? C40 H40A 0.99 . ? C40 H40B 0.99 . ? C43 H43A 0.99 . ? C43 H43B 0.99 . ? 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 P6 Cu2 P1 127.39(3) . 3_756 ? P6 Cu2 P4 133.20(3) . . ? P1 Cu2 P4 99.31(3) 3_756 . ? P5 Cu1 P1 124.13(3) . . ? P5 Cu1 P2 108.74(3) . 3_756 ? P1 Cu1 P2 108.03(2) . 3_756 ? P5 Cu1 P4 106.14(3) . . ? P1 Cu1 P4 107.02(3) . . ? P2 Cu1 P4 100.15(2) 3_756 . ? C36 P6 C31 101.03(12) . . ? C36 P6 C45 106.16(12) . . ? C31 P6 C45 106.83(12) . . ? C36 P6 Cu2 118.00(9) . . ? C31 P6 Cu2 111.90(9) . . ? C45 P6 Cu2 111.87(9) . . ? C13 P3 P4 104.89(8) . . ? C13 P3 P2 102.41(8) . . ? P4 P3 P2 95.54(4) . . ? C19 P4 P3 102.21(8) . . ? C19 P4 Cu2 118.62(8) . . ? P3 P4 Cu2 110.92(3) . . ? C19 P4 Cu1 113.26(7) . . ? P3 P4 Cu1 100.25(4) . . ? Cu2 P4 Cu1 109.73(3) . . ? C7 P2 P1 107.88(8) . . ? C7 P2 P3 102.08(9) . . ? P1 P2 P3 101.46(3) . . ? C7 P2 Cu1 113.37(8) . 3_756 ? P1 P2 Cu1 105.23(3) . 3_756 ? P3 P2 Cu1 125.35(4) . 3_756 ? C1 P1 P2 104.88(7) . . ? C1 P1 Cu2 120.05(8) . 3_756 ? P2 P1 Cu2 104.09(3) . 3_756 ? C1 P1 Cu1 114.77(8) . . ? P2 P1 Cu1 90.31(3) . . ? Cu2 P1 Cu1 116.31(3) 3_756 . ? C25 P5 Cu1 129.42(8) . . ? C25 P5 H1P 100.4(12) . . ? Cu1 P5 H1P 112.6(12) . . ? C25 P5 H2P 96.7(12) . . ? Cu1 P5 H2P 115.6(12) . . ? H1P P5 H2P 96.3(18) . . ? C37 C36 C40 103.7(2) . . ? C37 C36 P6 111.51(18) . . ? C40 C36 P6 114.76(18) . . ? C37 C36 H36 108.9 . . ? C40 C36 H36 108.9 . . ? P6 C36 H36 108.9 . . ? C24 C23 C22 120.2(3) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C3 C4 C5 119.9(2) . . ? C3 C4 H4 120 . . ? C5 C4 H4 120 . . ? C11 C12 C7 120.7(3) . . ? C11 C12 H12 119.6 . . ? C7 C12 H12 119.6 . . ? C17 C16 C15 120.0(2) . . ? C17 C16 H16 120 . . ? C15 C16 H16 120 . . ? C30 C25 C26 118.7(2) . . ? C30 C25 P5 120.5(2) . . ? C26 C25 P5 120.8(2) . . ? C44 C45 C41 104.5(2) . . ? C44 C45 P6 121.0(2) . . ? C41 C45 P6 111.36(18) . . ? C44 C45 H45 106.4 . . ? C41 C45 H45 106.4 . . ? P6 C45 H45 106.4 . . ? C4 C3 C2 119.9(3) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C10 C11 C12 120.4(3) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C16 C17 C18 120.1(2) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C22 C21 C20 120.7(2) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C8 C7 C12 117.9(2) . . ? C8 C7 P2 117.47(19) . . ? C12 C7 P2 124.6(2) . . ? C11 C10 C9 120.0(3) . . ? C11 C10 H10 120 . . ? C9 C10 H10 120 . . ? C27 C28 C29 120.9(3) . . ? C27 C28 H28 119.5 . . ? C29 C28 H28 119.5 . . ? C2 C1 C6 117.7(2) . . ? C2 C1 P1 121.46(19) . . ? C6 C1 P1 120.78(18) . . ? C21 C20 C19 120.9(2) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C13 C18 C17 120.6(2) . . ? C13 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C21 C22 C23 119.2(2) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C18 C13 C14 118.4(2) . . ? C18 C13 P3 125.10(18) . . ? C14 C13 P3 116.48(18) . . ? C1 C2 C3 121.3(3) . . ? C1 C2 H2 119.4 . . ? C3 C2 H2 119.4 . . ? C16 C15 C14 120.0(2) . . ? C16 C15 H15 120 . . ? C14 C15 H15 120 . . ? C9 C8 C7 121.3(3) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C4 C5 C6 120.4(3) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 120.9(2) . . ? C5 C6 H6 119.6 . . ? C1 C6 H6 119.6 . . ? C42 C41 C45 104.1(2) . . ? C42 C41 H41A 110.9 . . ? C45 C41 H41A 110.9 . . ? C42 C41 H41B 110.9 . . ? C45 C41 H41B 110.9 . . ? H41A C41 H41B 109 . . ? C34 C35 C31 104.2(3) . . ? C34 C35 H35A 110.9 . . ? C31 C35 H35A 110.9 . . ? C34 C35 H35B 110.9 . . ? C31 C35 H35B 110.9 . . ? H35A C35 H35B 108.9 . . ? C15 C14 C13 120.8(2) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C27 C26 C25 119.7(3) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C28 C29 C30 119.2(3) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C20 C19 C24 117.3(2) . . ? C20 C19 P4 125.60(19) . . ? C24 C19 P4 117.09(18) . . ? C38 C37 C36 103.6(2) . . ? C38 C37 H37A 111 . . ? C36 C37 H37A 111 . . ? C38 C37 H37B 111 . . ? C36 C37 H37B 111 . . ? H37A C37 H37B 109 . . ? C43 C44 C45 105.2(2) . . ? C43 C44 H44A 110.7 . . ? C45 C44 H44A 110.7 . . ? C43 C44 H44B 110.7 . . ? C45 C44 H44B 110.7 . . ? H44A C44 H44B 108.8 . . ? C28 C27 C26 120.6(3) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C39 C38 C37 105.8(3) . . ? C39 C38 H38A 110.6 . . ? C37 C38 H38A 110.6 . . ? C39 C38 H38B 110.6 . . ? C37 C38 H38B 110.6 . . ? H38A C38 H38B 108.7 . . ? C32 C31 C35 105.5(2) . . ? C32 C31 P6 115.96(18) . . ? C35 C31 P6 118.66(19) . . ? C32 C31 H31 105.1 . . ? C35 C31 H31 105.1 . . ? P6 C31 H31 105.1 . . ? C25 C30 C29 120.7(3) . . ? C25 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C10 C9 C8 119.6(3) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C23 C24 C19 121.8(2) . . ? C23 C24 H24 119.1 . . ? C19 C24 H24 119.1 . . ? C38 C39 C40 106.9(2) . . ? C38 C39 H39A 110.3 . . ? C40 C39 H39A 110.3 . . ? C38 C39 H39B 110.3 . . ? C40 C39 H39B 110.3 . . ? H39A C39 H39B 108.6 . . ? C33 C32 C31 102.8(2) . . ? C33 C32 H32A 111.2 . . ? C31 C32 H32A 111.2 . . ? C33 C32 H32B 111.2 . . ? C31 C32 H32B 111.2 . . ? H32A C32 H32B 109.1 . . ? C34 C33 C32 106.5(3) . . ? C34 C33 H33A 110.4 . . ? C32 C33 H33A 110.4 . . ? C34 C33 H33B 110.4 . . ? C32 C33 H33B 110.4 . . ? H33A C33 H33B 108.6 . . ? C33 C34 C35 109.4(3) . . ? C33 C34 H34A 109.8 . . ? C35 C34 H34A 109.8 . . ? C33 C34 H34B 109.8 . . ? C35 C34 H34B 109.8 . . ? H34A C34 H34B 108.2 . . ? C43 C42 C41 104.0(3) . . ? C43 C42 H42A 110.9 . . ? C41 C42 H42A 110.9 . . ? C43 C42 H42B 110.9 . . ? C41 C42 H42B 110.9 . . ? H42A C42 H42B 109 . . ? C39 C40 C36 106.2(2) . . ? C39 C40 H40A 110.5 . . ? C36 C40 H40A 110.5 . . ? C39 C40 H40B 110.5 . . ? C36 C40 H40B 110.5 . . ? H40A C40 H40B 108.7 . . ? C42 C43 C44 107.9(3) . . ? C42 C43 H43A 110.1 . . ? C44 C43 H43A 110.1 . . ? C42 C43 H43B 110.1 . . ? C44 C43 H43B 110.1 . . ? H43A C43 H43B 108.4 . . ?