# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name _publ_author_address 'Steve Westcott' ;Department of Chemistry University of New Brunswick Fredericton, NB E3B 6E2 Canada ; 'Andreas Decken' ;Department of Chemistry Mount Allison University 63C York Street Sackville, NB E4L 1G8 Canada ; 'Christian N. Garon' '' 'Todd Marder' '' 'Daniel I. McIsaac' '' 'Christopher M Vogels' '' ; I.Williams ; '' _publ_contact_author_name 'Steve Westcott' _publ_contact_author_email SWESTCOTT@MTA.CA _publ_section_title ; Synthesis and structure of indenyl rhodium(I) complexes containing unsaturated phosphines: catalyst precursors for alkene hydroboration ; _publ_contact_author_address ;Department of Chemistry University of New Brunswick Fredericton, NB E3B 6E2 Canada ; _publ_contact_author_fax '(506) 453-4981' _publ_contact_author_phone '(506) 453-4875' # Attachment 'sw050640.cif' data_sw050640 _database_code_depnum_ccdc_archive 'CCDC 686222' _publ_section_references ; Bruker (2006). SAINT. Version 7.23A. Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (1999). SMART. Version 5.054. Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2004). SADABS 2004. Bruker AXS Inc., Madison, Wisconsin, USA. ; _publ_section_exptl_refinement ; Hydrogen atoms were included in calculated positions and refined using a riding model. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H45 P2 Rh' _chemical_formula_sum 'C45 H45 P2 Rh' _chemical_formula_weight 750.66 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1 ' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0600(6) _cell_length_b 11.8418(7) _cell_length_c 17.1608(10) _cell_angle_alpha 108.854(1) _cell_angle_beta 92.464(1) _cell_angle_gamma 112.489(1) _cell_volume 1929.21(19) _cell_formula_units_Z 2 _cell_measurement_temperature 198(1) _cell_measurement_reflns_used 8366 _cell_measurement_theta_min 2.3365 _cell_measurement_theta_max 28.2725 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 0.555 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8084 _exptl_absorpt_correction_T_max 0.8971 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2004)' _exptl_special_details ; Crystal decay was monitored by repeating the initial 50 frames at the end of the data collection and analyzing duplicate reflections. ; _diffrn_ambient_temperature 198(1) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type K760 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART1000/P4' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13395 _diffrn_reflns_av_R_equivalents 0.0174 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8406 _reflns_number_gt 7406 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Sheldrick, 2008)' _computing_publication_material 'Bruker SHELXTL (Sheldrick, 2008)' _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^)+(0.0590P)^2^+0.2619P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8406 _refine_ls_number_parameters 439 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0922 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh Rh 0.363449(14) 0.485095(13) 0.263143(9) 0.02624(6) Uani 1 1 d . . . P1 P 0.19817(5) 0.31726(5) 0.16836(3) 0.02518(11) Uani 1 1 d . . . P2 P 0.24132(5) 0.50656(5) 0.36075(3) 0.02800(11) Uani 1 1 d . . . C1 C 0.5230(2) 0.4971(2) 0.18730(15) 0.0361(5) Uani 1 1 d . . . H1 H 0.5173 0.4276 0.1334 0.043 Uiso 1 1 calc R . . C2 C 0.5770(2) 0.5119(2) 0.26877(15) 0.0383(5) Uani 1 1 d . . . H2 H 0.6138 0.4534 0.2816 0.046 Uiso 1 1 calc R . . C3 C 0.5750(2) 0.6265(2) 0.32818(16) 0.0394(5) Uani 1 1 d . . . H3 H 0.6098 0.6620 0.3899 0.047 Uiso 1 1 calc R . . C3A C 0.5401(2) 0.6966(2) 0.28198(16) 0.0380(5) Uani 1 1 d . . . C4 C 0.5346(2) 0.8203(2) 0.30804(19) 0.0478(6) Uani 1 1 d . . . H4 H 0.5566 0.8747 0.3658 0.057 Uiso 1 1 calc R . . C5 C 0.4968(3) 0.8603(2) 0.2483(2) 0.0562(7) Uani 1 1 d . . . H5 H 0.4959 0.9446 0.2649 0.067 Uiso 1 1 calc R . . C6 C 0.4597(3) 0.7798(3) 0.1634(2) 0.0544(7) Uani 1 1 d . . . H6 H 0.4319 0.8097 0.1238 0.065 Uiso 1 1 calc R . . C7 C 0.4623(2) 0.6579(2) 0.13580(17) 0.0427(5) Uani 1 1 d . . . H7 H 0.4352 0.6033 0.0780 0.051 Uiso 1 1 calc R . . C7A C 0.5062(2) 0.6162(2) 0.19529(15) 0.0362(5) Uani 1 1 d . . . C8 C 0.19527(19) 0.3331(2) 0.06536(12) 0.0294(4) Uani 1 1 d . . . C9 C 0.1450(2) 0.4186(2) 0.05198(14) 0.0365(5) Uani 1 1 d . . . H9 H 0.1103 0.4639 0.0948 0.044 Uiso 1 1 calc R . . C10 C 0.1457(3) 0.4375(3) -0.02376(16) 0.0466(6) Uani 1 1 d . . . H10 H 0.1106 0.4950 -0.0326 0.056 Uiso 1 1 calc R . . C11 C 0.1969(2) 0.3734(3) -0.08613(16) 0.0502(6) Uani 1 1 d . . . H11 H 0.1981 0.3876 -0.1376 0.060 Uiso 1 1 calc R . . C12 C 0.2464(2) 0.2884(3) -0.07354(15) 0.0466(6) Uani 1 1 d . . . H12 H 0.2805 0.2431 -0.1168 0.056 Uiso 1 1 calc R . . C13 C 0.2465(2) 0.2688(2) 0.00228(14) 0.0374(5) Uani 1 1 d . . . H13 H 0.2819 0.2113 0.0108 0.045 Uiso 1 1 calc R . . C14 C 0.20168(19) 0.15587(18) 0.14606(12) 0.0268(4) Uani 1 1 d . . . C15 C 0.3181(2) 0.1516(2) 0.17560(14) 0.0354(5) Uani 1 1 d . . . H15 H 0.3941 0.2310 0.2060 0.043 Uiso 1 1 calc R . . C16 C 0.3234(2) 0.0308(2) 0.16060(15) 0.0415(5) Uani 1 1 d . . . H16 H 0.4034 0.0281 0.1806 0.050 Uiso 1 1 calc R . . C17 C 0.2137(2) -0.0846(2) 0.11705(14) 0.0372(5) Uani 1 1 d . . . H17 H 0.2174 -0.1667 0.1080 0.045 Uiso 1 1 calc R . . C18 C 0.0985(2) -0.0809(2) 0.08652(14) 0.0380(5) Uani 1 1 d . . . H18 H 0.0233 -0.1606 0.0554 0.046 Uiso 1 1 calc R . . C19 C 0.0920(2) 0.0390(2) 0.10109(13) 0.0336(4) Uani 1 1 d . . . H19 H 0.0122 0.0409 0.0802 0.040 Uiso 1 1 calc R . . C20 C 0.02781(19) 0.27648(19) 0.17317(12) 0.0286(4) Uani 1 1 d . . . C21 C -0.0892(2) 0.24624(19) 0.16878(13) 0.0305(4) Uani 1 1 d . . . C22 C -0.2347(2) 0.2060(2) 0.15933(14) 0.0327(4) Uani 1 1 d . . . C23 C -0.3057(2) 0.0611(2) 0.10101(16) 0.0476(6) Uani 1 1 d . . . H23A H -0.2775 0.0500 0.0467 0.071 Uiso 1 1 calc R . . H23B H -0.4023 0.0339 0.0929 0.071 Uiso 1 1 calc R . . H23C H -0.2826 0.0069 0.1262 0.071 Uiso 1 1 calc R . . C24 C -0.2758(2) 0.2240(3) 0.24500(15) 0.0479(6) Uani 1 1 d . . . H24A H -0.2592 0.1638 0.2674 0.072 Uiso 1 1 calc R . . H24B H -0.3708 0.2049 0.2389 0.072 Uiso 1 1 calc R . . H24C H -0.2236 0.3148 0.2836 0.072 Uiso 1 1 calc R . . C25 C -0.2710(3) 0.2908(3) 0.1201(2) 0.0577(7) Uani 1 1 d . . . H25A H -0.2224 0.3837 0.1562 0.087 Uiso 1 1 calc R . . H25B H -0.3671 0.2663 0.1145 0.087 Uiso 1 1 calc R . . H25C H -0.2467 0.2767 0.0647 0.087 Uiso 1 1 calc R . . C26 C 0.1170(2) 0.56836(19) 0.34571(12) 0.0296(4) Uani 1 1 d . . . C27 C 0.0076(2) 0.5480(2) 0.38502(13) 0.0362(5) Uani 1 1 d . . . H27 H -0.0058 0.4985 0.4203 0.043 Uiso 1 1 calc R . . C28 C -0.0823(2) 0.5996(2) 0.37302(15) 0.0415(5) Uani 1 1 d . . . H28 H -0.1571 0.5851 0.3999 0.050 Uiso 1 1 calc R . . C29 C -0.0628(2) 0.6718(2) 0.32201(16) 0.0431(5) Uani 1 1 d . . . H29 H -0.1250 0.7060 0.3133 0.052 Uiso 1 1 calc R . . C30 C 0.0465(3) 0.6945(2) 0.28348(16) 0.0449(5) Uani 1 1 d . . . H30 H 0.0609 0.7463 0.2497 0.054 Uiso 1 1 calc R . . C31 C 0.1357(2) 0.6411(2) 0.29427(14) 0.0381(5) Uani 1 1 d . . . H31 H 0.2094 0.6545 0.2664 0.046 Uiso 1 1 calc R . . C32 C 0.3420(2) 0.6248(2) 0.46355(13) 0.0328(4) Uani 1 1 d . . . C33 C 0.3792(3) 0.7582(2) 0.48230(15) 0.0463(6) Uani 1 1 d . . . H33 H 0.3400 0.7865 0.4463 0.056 Uiso 1 1 calc R . . C34 C 0.4732(3) 0.8502(3) 0.55336(16) 0.0541(7) Uani 1 1 d . . . H34 H 0.4984 0.9413 0.5658 0.065 Uiso 1 1 calc R . . C35 C 0.5306(3) 0.8097(3) 0.60637(15) 0.0513(6) Uani 1 1 d . . . H35 H 0.5957 0.8730 0.6548 0.062 Uiso 1 1 calc R . . C36 C 0.4932(3) 0.6778(3) 0.58867(15) 0.0486(6) Uani 1 1 d . . . H36 H 0.5322 0.6499 0.6250 0.058 Uiso 1 1 calc R . . C37 C 0.3989(2) 0.5857(2) 0.51811(14) 0.0408(5) Uani 1 1 d . . . H37 H 0.3726 0.4947 0.5067 0.049 Uiso 1 1 calc R . . C38 C 0.1483(2) 0.3641(2) 0.38153(13) 0.0358(5) Uani 1 1 d . . . C39 C 0.0880(2) 0.2586(2) 0.38523(14) 0.0381(5) Uani 1 1 d . . . C40 C 0.0152(3) 0.1249(2) 0.38610(15) 0.0441(6) Uani 1 1 d . . . C41 C -0.0230(4) 0.0271(3) 0.29541(18) 0.0778(11) Uani 1 1 d . . . H41A H -0.0752 0.0506 0.2610 0.117 Uiso 1 1 calc R . . H41B H -0.0762 -0.0617 0.2938 0.117 Uiso 1 1 calc R . . H41C H 0.0581 0.0299 0.2735 0.117 Uiso 1 1 calc R . . C42 C -0.1096(3) 0.1152(3) 0.42296(17) 0.0533(6) Uani 1 1 d . . . H42A H -0.0841 0.1758 0.4816 0.080 Uiso 1 1 calc R . . H42B H -0.1596 0.0251 0.4202 0.080 Uiso 1 1 calc R . . H42C H -0.1655 0.1384 0.3908 0.080 Uiso 1 1 calc R . . C43 C 0.1084(3) 0.0980(3) 0.4399(2) 0.0611(8) Uani 1 1 d . . . H43A H 0.1920 0.1126 0.4190 0.092 Uiso 1 1 calc R . . H43B H 0.0652 0.0068 0.4365 0.092 Uiso 1 1 calc R . . H43C H 0.1272 0.1576 0.4983 0.092 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 Rh 0.02207(9) 0.02332(9) 0.03654(10) 0.01279(7) 0.00494(6) 0.01137(7) P1 0.0214(2) 0.0257(2) 0.0329(2) 0.01372(19) 0.00598(19) 0.01199(19) P2 0.0302(3) 0.0254(2) 0.0338(2) 0.0140(2) 0.0062(2) 0.0147(2) C1 0.0261(10) 0.0348(11) 0.0565(13) 0.0219(10) 0.0165(9) 0.0170(9) C2 0.0237(10) 0.0338(11) 0.0622(14) 0.0215(10) 0.0050(9) 0.0142(9) C3 0.0260(10) 0.0322(11) 0.0561(13) 0.0159(10) -0.0018(9) 0.0095(9) C3A 0.0229(10) 0.0279(10) 0.0627(14) 0.0183(10) 0.0068(9) 0.0091(8) C4 0.0385(13) 0.0286(11) 0.0749(17) 0.0188(11) 0.0082(12) 0.0129(10) C5 0.0507(15) 0.0336(12) 0.095(2) 0.0322(14) 0.0158(15) 0.0211(12) C6 0.0429(14) 0.0557(16) 0.092(2) 0.0537(16) 0.0225(14) 0.0261(12) C7 0.0287(11) 0.0472(13) 0.0632(14) 0.0335(12) 0.0145(10) 0.0156(10) C7A 0.0230(10) 0.0336(11) 0.0603(13) 0.0256(10) 0.0147(9) 0.0128(8) C8 0.0228(9) 0.0317(10) 0.0361(10) 0.0180(8) 0.0050(8) 0.0091(8) C9 0.0356(11) 0.0346(11) 0.0441(11) 0.0200(9) 0.0056(9) 0.0154(9) C10 0.0424(13) 0.0490(14) 0.0599(14) 0.0369(12) 0.0057(11) 0.0174(11) C11 0.0388(13) 0.0691(17) 0.0496(13) 0.0402(13) 0.0091(11) 0.0145(12) C12 0.0354(12) 0.0671(16) 0.0429(12) 0.0264(12) 0.0167(10) 0.0211(12) C13 0.0273(10) 0.0476(13) 0.0448(11) 0.0224(10) 0.0105(9) 0.0185(10) C14 0.0279(10) 0.0264(9) 0.0306(9) 0.0133(7) 0.0064(7) 0.0133(8) C15 0.0307(11) 0.0261(10) 0.0469(12) 0.0115(9) -0.0017(9) 0.0119(8) C16 0.0388(12) 0.0345(11) 0.0535(13) 0.0133(10) -0.0020(10) 0.0211(10) C17 0.0420(12) 0.0295(10) 0.0437(11) 0.0133(9) 0.0077(9) 0.0189(9) C18 0.0339(11) 0.0256(10) 0.0448(12) 0.0074(9) 0.0020(9) 0.0080(9) C19 0.0279(10) 0.0326(10) 0.0401(11) 0.0126(9) 0.0023(8) 0.0134(9) C20 0.0245(10) 0.0281(9) 0.0342(10) 0.0125(8) 0.0065(8) 0.0110(8) C21 0.0311(11) 0.0277(10) 0.0375(10) 0.0153(8) 0.0087(8) 0.0143(8) C22 0.0240(10) 0.0316(10) 0.0464(11) 0.0165(9) 0.0106(8) 0.0135(8) C23 0.0361(13) 0.0406(13) 0.0536(14) 0.0099(11) 0.0110(11) 0.0093(10) C24 0.0320(12) 0.0540(15) 0.0494(13) 0.0122(11) 0.0144(10) 0.0146(11) C25 0.0431(15) 0.0629(17) 0.091(2) 0.0438(16) 0.0157(14) 0.0331(13) C26 0.0301(10) 0.0274(9) 0.0322(9) 0.0099(8) 0.0035(8) 0.0140(8) C27 0.0359(11) 0.0367(11) 0.0375(10) 0.0130(9) 0.0071(9) 0.0173(9) C28 0.0333(12) 0.0419(12) 0.0474(12) 0.0099(10) 0.0089(10) 0.0188(10) C29 0.0371(12) 0.0422(12) 0.0545(13) 0.0136(10) 0.0018(10) 0.0255(10) C30 0.0462(14) 0.0451(13) 0.0578(14) 0.0271(11) 0.0103(11) 0.0269(11) C31 0.0376(12) 0.0404(12) 0.0480(12) 0.0239(10) 0.0113(10) 0.0216(10) C32 0.0353(11) 0.0350(11) 0.0336(10) 0.0129(8) 0.0063(8) 0.0202(9) C33 0.0557(15) 0.0392(12) 0.0456(12) 0.0125(10) -0.0016(11) 0.0253(11) C34 0.0633(17) 0.0375(13) 0.0523(14) 0.0044(11) -0.0015(12) 0.0232(12) C35 0.0509(15) 0.0606(16) 0.0361(11) 0.0053(11) 0.0013(11) 0.0280(13) C36 0.0500(15) 0.0660(17) 0.0376(11) 0.0206(11) 0.0035(10) 0.0317(13) C37 0.0480(14) 0.0444(13) 0.0403(11) 0.0195(10) 0.0094(10) 0.0264(11) C38 0.0425(12) 0.0351(11) 0.0390(11) 0.0189(9) 0.0116(9) 0.0209(10) C39 0.0466(13) 0.0358(11) 0.0394(11) 0.0190(9) 0.0117(10) 0.0202(10) C40 0.0602(16) 0.0318(11) 0.0449(12) 0.0221(10) 0.0143(11) 0.0169(11) C41 0.138(3) 0.0357(14) 0.0512(16) 0.0187(12) 0.0262(18) 0.0252(18) C42 0.0485(15) 0.0491(14) 0.0594(15) 0.0299(12) 0.0080(12) 0.0095(12) C43 0.0670(19) 0.0636(17) 0.087(2) 0.0564(17) 0.0292(16) 0.0376(15) _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 Rh P1 2.1938(5) . ? Rh P2 2.2083(5) . ? Rh C1 2.226(2) . ? Rh C2 2.253(2) . ? Rh C3 2.257(2) . ? Rh C7A 2.390(2) . ? Rh C3A 2.423(2) . ? P1 C20 1.770(2) . ? P1 C8 1.837(2) . ? P1 C14 1.8401(19) . ? P2 C38 1.768(2) . ? P2 C26 1.831(2) . ? P2 C32 1.832(2) . ? C1 C2 1.425(3) . ? C1 C7A 1.456(3) . ? C1 H1 1.0000 . ? C2 C3 1.419(3) . ? C2 H2 1.0000 . ? C3 C3A 1.452(3) . ? C3 H3 1.0000 . ? C3A C4 1.414(3) . ? C3A C7A 1.423(3) . ? C4 C5 1.371(4) . ? C4 H4 0.9500 . ? C5 C6 1.396(4) . ? C5 H5 0.9500 . ? C6 C7 1.379(4) . ? C6 H6 0.9500 . ? C7 C7A 1.410(3) . ? C7 H7 0.9500 . ? C8 C13 1.387(3) . ? C8 C9 1.399(3) . ? C9 C10 1.388(3) . ? C9 H9 0.9500 . ? C10 C11 1.377(4) . ? C10 H10 0.9500 . ? C11 C12 1.383(4) . ? C11 H11 0.9500 . ? C12 C13 1.393(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C19 1.388(3) . ? C14 C15 1.389(3) . ? C15 C16 1.395(3) . ? C15 H15 0.9500 . ? C16 C17 1.375(3) . ? C16 H16 0.9500 . ? C17 C18 1.379(3) . ? C17 H17 0.9500 . ? C18 C19 1.391(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.195(3) . ? C21 C22 1.478(3) . ? C22 C24 1.530(3) . ? C22 C25 1.531(3) . ? C22 C23 1.534(3) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.389(3) . ? C26 C31 1.391(3) . ? C27 C28 1.391(3) . ? C27 H27 0.9500 . ? C28 C29 1.379(4) . ? C28 H28 0.9500 . ? C29 C30 1.381(4) . ? C29 H29 0.9500 . ? C30 C31 1.394(3) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.390(3) . ? C32 C37 1.393(3) . ? C33 C34 1.386(4) . ? C33 H33 0.9500 . ? C34 C35 1.388(4) . ? C34 H34 0.9500 . ? C35 C36 1.376(4) . ? C35 H35 0.9500 . ? C36 C37 1.382(3) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C39 1.195(3) . ? C39 C40 1.481(3) . ? C40 C42 1.524(4) . ? C40 C41 1.532(4) . ? C40 C43 1.541(4) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Rh P2 94.30(2) . . ? P1 Rh C1 98.13(6) . . ? P2 Rh C1 167.49(6) . . ? P1 Rh C2 122.92(6) . . ? P2 Rh C2 132.44(6) . . ? C1 Rh C2 37.11(9) . . ? P1 Rh C3 159.00(7) . . ? P2 Rh C3 105.46(7) . . ? C1 Rh C3 62.03(9) . . ? C2 Rh C3 36.68(8) . . ? P1 Rh C7A 108.98(6) . . ? P2 Rh C7A 138.72(6) . . ? C1 Rh C7A 36.56(7) . . ? C2 Rh C7A 59.93(8) . . ? C3 Rh C7A 59.89(8) . . ? P1 Rh C3A 141.36(6) . . ? P2 Rh C3A 110.35(6) . . ? C1 Rh C3A 59.84(8) . . ? C2 Rh C3A 59.28(8) . . ? C3 Rh C3A 35.92(8) . . ? C7A Rh C3A 34.37(8) . . ? C20 P1 C8 98.32(9) . . ? C20 P1 C14 100.47(9) . . ? C8 P1 C14 103.27(9) . . ? C20 P1 Rh 124.04(7) . . ? C8 P1 Rh 111.69(7) . . ? C14 P1 Rh 115.93(6) . . ? C38 P2 C26 102.99(10) . . ? C38 P2 C32 103.36(10) . . ? C26 P2 C32 102.40(9) . . ? C38 P2 Rh 116.87(7) . . ? C26 P2 Rh 116.93(7) . . ? C32 P2 Rh 112.40(7) . . ? C2 C1 C7A 107.4(2) . . ? C2 C1 Rh 72.47(13) . . ? C7A C1 Rh 77.86(12) . . ? C2 C1 H1 125.7 . . ? C7A C1 H1 125.7 . . ? Rh C1 H1 125.7 . . ? C3 C2 C1 108.61(19) . . ? C3 C2 Rh 71.83(12) . . ? C1 C2 Rh 70.42(12) . . ? C3 C2 H2 125.7 . . ? C1 C2 H2 125.7 . . ? Rh C2 H2 125.7 . . ? C2 C3 C3A 107.6(2) . . ? C2 C3 Rh 71.50(12) . . ? C3A C3 Rh 78.30(12) . . ? C2 C3 H3 125.6 . . ? C3A C3 H3 125.6 . . ? Rh C3 H3 125.6 . . ? C4 C3A C7A 119.9(2) . . ? C4 C3A C3 132.3(2) . . ? C7A C3A C3 107.78(19) . . ? C4 C3A Rh 127.94(16) . . ? C7A C3A Rh 71.52(12) . . ? C3 C3A Rh 65.78(11) . . ? C5 C4 C3A 118.6(3) . . ? C5 C4 H4 120.7 . . ? C3A C4 H4 120.7 . . ? C4 C5 C6 121.5(2) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C7 C6 C5 121.5(2) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C6 C7 C7A 118.4(3) . . ? C6 C7 H7 120.8 . . ? C7A C7 H7 120.8 . . ? C7 C7A C3A 119.9(2) . . ? C7 C7A C1 132.3(2) . . ? C3A C7A C1 107.7(2) . . ? C7 C7A Rh 124.77(15) . . ? C3A C7A Rh 74.11(12) . . ? C1 C7A Rh 65.58(11) . . ? C13 C8 C9 119.03(19) . . ? C13 C8 P1 122.66(16) . . ? C9 C8 P1 118.24(16) . . ? C10 C9 C8 120.2(2) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C11 C10 C9 120.5(2) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C12 119.7(2) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C11 C12 C13 120.3(2) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C8 C13 C12 120.2(2) . . ? C8 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C19 C14 C15 119.25(18) . . ? C19 C14 P1 122.20(15) . . ? C15 C14 P1 118.56(15) . . ? C14 C15 C16 119.9(2) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 C16 C15 120.5(2) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 119.8(2) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C17 C18 C19 120.2(2) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C14 C19 C18 120.3(2) . . ? C14 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C21 C20 P1 174.09(18) . . ? C20 C21 C22 177.5(2) . . ? C21 C22 C24 110.05(18) . . ? C21 C22 C25 108.55(18) . . ? C24 C22 C25 110.1(2) . . ? C21 C22 C23 108.65(18) . . ? C24 C22 C23 109.96(19) . . ? C25 C22 C23 109.5(2) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C31 119.3(2) . . ? C27 C26 P2 122.61(16) . . ? C31 C26 P2 118.12(16) . . ? C26 C27 C28 120.4(2) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C29 C28 C27 119.9(2) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 120.3(2) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C29 C30 C31 119.9(2) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C26 C31 C30 120.2(2) . . ? C26 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C33 C32 C37 118.9(2) . . ? C33 C32 P2 119.47(16) . . ? C37 C32 P2 120.92(17) . . ? C34 C33 C32 120.2(2) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C35 120.2(2) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C36 C35 C34 119.8(2) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C37 120.1(2) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C36 C37 C32 120.7(2) . . ? C36 C37 H37 119.7 . . ? C32 C37 H37 119.7 . . ? C39 C38 P2 171.1(2) . . ? C38 C39 C40 177.3(2) . . ? C39 C40 C42 110.2(2) . . ? C39 C40 C41 107.8(2) . . ? C42 C40 C41 110.0(3) . . ? C39 C40 C43 108.4(2) . . ? C42 C40 C43 109.9(2) . . ? C41 C40 C43 110.5(3) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.473 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.081 # Attachment 'sw051112.cif' data_sw051112 _database_code_depnum_ccdc_archive 'CCDC 686223' _publ_section_references ; Bruker (2006). SAINT. Version 7.23A. Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (1999). SMART. Version 5.054. Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2004). SADABS 2004. Bruker AXS Inc., Madison, Wisconsin, USA. ; _publ_section_exptl_refinement ; Hydrogen atoms were included in calculated positions and refined using a riding model. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H35 Rh' _chemical_formula_sum 'C25 H35 Rh' _chemical_formula_weight 438.44 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' Rh Rh -1.1178 0.9187 '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 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_int_tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.3306(6) _cell_length_b 13.4620(12) _cell_length_c 20.7134(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2044.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 5932 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 28.1765 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 0.841 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6322 _exptl_absorpt_correction_T_max 0.8667 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2004)' _exptl_special_details ; Crystal decay was monitored by repeating the initial 50 frames at the end of the data collection and analyzing duplicate reflections. ; _diffrn_ambient_temperature 173(1) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type K760 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART1000/P4' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14137 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4575 _reflns_number_gt 4429 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Sheldrick, 2008)' _computing_publication_material 'Bruker SHELXTL (Sheldrick, 2008)' _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^)+(0.0306P)^2^+0.3037P] 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 constr _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 -0.011(19) _refine_ls_number_reflns 4575 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0211 _refine_ls_R_factor_gt 0.0195 _refine_ls_wR_factor_ref 0.0497 _refine_ls_wR_factor_gt 0.0488 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh Rh 0.769368(17) 0.400318(9) 0.104482(6) 0.01619(5) Uani 1 1 d . . . C1A C 0.4835(2) 0.41932(15) 0.16089(10) 0.0212(4) Uani 1 1 d . . . C1 C 0.5256(3) 0.31829(17) 0.14068(11) 0.0253(5) Uani 1 1 d . . . H1 H 0.5289 0.2590 0.1697 0.030 Uiso 1 1 calc R . . C2 C 0.5221(3) 0.31528(17) 0.07233(11) 0.0278(5) Uani 1 1 d . . . H2 H 0.5224 0.2539 0.0451 0.033 Uiso 1 1 calc R . . C3 C 0.5079(3) 0.41416(17) 0.04936(10) 0.0249(4) Uani 1 1 d . . . H3 H 0.4976 0.4339 0.0030 0.030 Uiso 1 1 calc R . . C3A C 0.4732(2) 0.47878(14) 0.10400(11) 0.0216(4) Uani 1 1 d . . . C4 C 0.4365(2) 0.58112(15) 0.10871(11) 0.0266(4) Uani 1 1 d . . . H4 H 0.4320 0.6215 0.0711 0.032 Uiso 1 1 calc R . . C5 C 0.4073(3) 0.62160(16) 0.16868(11) 0.0298(5) Uani 1 1 d . . . H5 H 0.3810 0.6905 0.1724 0.036 Uiso 1 1 calc R . . C6 C 0.4158(3) 0.56292(17) 0.22465(11) 0.0314(5) Uani 1 1 d . . . H6 H 0.3938 0.5928 0.2655 0.038 Uiso 1 1 calc R . . C7 C 0.4550(3) 0.46377(16) 0.22172(10) 0.0256(4) Uani 1 1 d . . . H7 H 0.4628 0.4253 0.2601 0.031 Uiso 1 1 calc R . . C8 C 0.9545(3) 0.51190(15) 0.06927(9) 0.0202(4) Uani 1 1 d . . . H8 H 1.0729 0.5136 0.0933 0.024 Uiso 1 1 calc R . . C9 C 0.9441(3) 0.43401(15) 0.02406(9) 0.0209(4) Uani 1 1 d . . . H9 H 1.0567 0.3921 0.0233 0.025 Uiso 1 1 calc R . . C10 C 0.8606(3) 0.44714(16) -0.04225(10) 0.0256(4) Uani 1 1 d . . . H10A H 0.7636 0.4982 -0.0404 0.031 Uiso 1 1 calc R . . H10B H 0.8049 0.3839 -0.0565 0.031 Uiso 1 1 calc R . . C11 C 1.0084(4) 0.47904(18) -0.09064(10) 0.0365(5) Uani 1 1 d . . . H11A H 1.0887 0.4214 -0.0992 0.044 Uiso 1 1 calc R . . H11B H 0.9483 0.4968 -0.1319 0.044 Uiso 1 1 calc R . . C12 C 1.1267(3) 0.56609(19) -0.06937(13) 0.0402(6) Uani 1 1 d . . . H12A H 1.2138 0.5815 -0.1045 0.048 Uiso 1 1 calc R . . H12B H 1.1988 0.5452 -0.0313 0.048 Uiso 1 1 calc R . . C13 C 1.0233(4) 0.66121(18) -0.05208(13) 0.0385(6) Uani 1 1 d . . . H13A H 0.9003 0.6573 -0.0717 0.046 Uiso 1 1 calc R . . H13B H 1.0872 0.7179 -0.0724 0.046 Uiso 1 1 calc R . . C14 C 1.0003(3) 0.68428(16) 0.02034(11) 0.0293(5) Uani 1 1 d . . . H14A H 1.1223 0.6828 0.0408 0.035 Uiso 1 1 calc R . . H14B H 0.9524 0.7527 0.0247 0.035 Uiso 1 1 calc R . . C15 C 0.8741(3) 0.61373(15) 0.05782(10) 0.0235(4) Uani 1 1 d . . . H15A H 0.8447 0.6442 0.1001 0.028 Uiso 1 1 calc R . . H15B H 0.7585 0.6063 0.0336 0.028 Uiso 1 1 calc R . . C16 C 0.9892(2) 0.30924(16) 0.13959(9) 0.0198(4) Uani 1 1 d . . . H16 H 1.1068 0.3216 0.1165 0.024 Uiso 1 1 calc R . . C17 C 0.9503(2) 0.38192(14) 0.18629(10) 0.0209(4) Uani 1 1 d . . . H17 H 1.0458 0.4348 0.1892 0.025 Uiso 1 1 calc R . . C18 C 0.8671(3) 0.35584(15) 0.25087(9) 0.0225(4) Uani 1 1 d . . . H18A H 0.7879 0.2967 0.2461 0.027 Uiso 1 1 calc R . . H18B H 0.7906 0.4117 0.2661 0.027 Uiso 1 1 calc R . . C19 C 1.0176(3) 0.33415(17) 0.30089(10) 0.0283(5) Uani 1 1 d . . . H19A H 1.0782 0.3975 0.3122 0.034 Uiso 1 1 calc R . . H19B H 0.9595 0.3082 0.3406 0.034 Uiso 1 1 calc R . . C20 C 1.1636(3) 0.26033(15) 0.27915(10) 0.0263(4) Uani 1 1 d . . . H20A H 1.2510 0.2510 0.3151 0.032 Uiso 1 1 calc R . . H20B H 1.2316 0.2901 0.2427 0.032 Uiso 1 1 calc R . . C21 C 1.0942(3) 0.15734(15) 0.25797(10) 0.0271(4) Uani 1 1 d . . . H21A H 1.1732 0.1060 0.2777 0.033 Uiso 1 1 calc R . . H21B H 0.9695 0.1479 0.2753 0.033 Uiso 1 1 calc R . . C22 C 1.0894(3) 0.14032(15) 0.18485(11) 0.0282(4) Uani 1 1 d . . . H22A H 1.0683 0.0687 0.1770 0.034 Uiso 1 1 calc R . . H22B H 1.2111 0.1568 0.1672 0.034 Uiso 1 1 calc R . . C23 C 0.9453(3) 0.19942(15) 0.14658(10) 0.0249(4) Uani 1 1 d . . . H23A H 0.9335 0.1699 0.1030 0.030 Uiso 1 1 calc R . . H23B H 0.8259 0.1925 0.1685 0.030 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 Rh 0.01639(6) 0.01527(7) 0.01692(7) 0.00029(5) -0.00007(5) -0.00093(5) C1A 0.0147(7) 0.0222(11) 0.0267(10) 0.0015(8) 0.0016(7) -0.0022(7) C1 0.0193(9) 0.0223(11) 0.0344(12) 0.0012(9) 0.0018(8) -0.0062(8) C2 0.0219(9) 0.0267(12) 0.0349(12) -0.0082(9) -0.0039(9) -0.0046(9) C3 0.0207(8) 0.0313(12) 0.0227(10) -0.0024(9) -0.0039(7) -0.0003(9) C3A 0.0144(7) 0.0251(9) 0.0253(9) 0.0007(9) -0.0034(9) 0.0005(7) C4 0.0187(7) 0.0266(10) 0.0344(11) 0.0053(9) 0.0009(8) 0.0017(7) C5 0.0209(8) 0.0231(11) 0.0454(13) -0.0051(9) 0.0040(9) 0.0029(8) C6 0.0228(9) 0.0382(12) 0.0333(12) -0.0130(10) 0.0048(9) 0.0002(9) C7 0.0178(8) 0.0337(11) 0.0254(10) 0.0011(9) 0.0016(8) 0.0014(8) C8 0.0176(8) 0.0227(10) 0.0204(9) 0.0039(8) 0.0014(7) -0.0032(7) C9 0.0222(8) 0.0217(10) 0.0189(9) 0.0021(8) 0.0052(8) -0.0005(7) C10 0.0341(10) 0.0238(10) 0.0189(10) -0.0010(8) 0.0016(8) -0.0010(9) C11 0.0508(13) 0.0343(12) 0.0244(12) 0.0007(9) 0.0131(10) 0.0007(11) C12 0.0406(12) 0.0415(14) 0.0384(13) 0.0089(11) 0.0158(11) 0.0026(11) C13 0.0433(13) 0.0306(12) 0.0418(14) 0.0128(11) 0.0098(11) -0.0021(11) C14 0.0328(10) 0.0196(10) 0.0354(12) 0.0066(9) 0.0017(9) -0.0035(9) C15 0.0259(8) 0.0206(10) 0.0239(10) -0.0006(8) 0.0022(7) -0.0005(8) C16 0.0189(8) 0.0209(10) 0.0196(10) 0.0054(8) 0.0010(7) 0.0020(8) C17 0.0201(8) 0.0208(10) 0.0218(9) 0.0041(8) -0.0046(7) -0.0019(7) C18 0.0234(9) 0.0237(10) 0.0203(10) -0.0014(8) -0.0009(7) 0.0034(8) C19 0.0320(10) 0.0302(11) 0.0227(11) 0.0013(9) -0.0058(9) 0.0009(9) C20 0.0245(9) 0.0274(10) 0.0270(11) 0.0077(8) -0.0041(8) 0.0014(8) C21 0.0260(10) 0.0245(11) 0.0307(11) 0.0085(9) -0.0008(9) 0.0045(8) C22 0.0324(10) 0.0206(10) 0.0317(11) 0.0021(9) -0.0007(9) 0.0058(8) C23 0.0292(9) 0.0201(10) 0.0254(10) -0.0021(8) -0.0025(8) 0.0020(8) _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 Rh C9 2.1495(19) . ? Rh C16 2.1513(19) . ? Rh C8 2.1520(19) . ? Rh C17 2.1659(19) . ? Rh C1 2.230(2) . ? Rh C3 2.2385(19) . ? Rh C2 2.245(2) . ? Rh C1A 2.4126(18) . ? Rh C3A 2.4148(17) . ? C1A C7 1.411(3) . ? C1A C3A 1.427(3) . ? C1A C1 1.456(3) . ? C1 C2 1.417(3) . ? C1 H1 1.0000 . ? C2 C3 1.417(3) . ? C2 H2 1.0000 . ? C3 C3A 1.450(3) . ? C3 H3 1.0000 . ? C3A C4 1.407(3) . ? C4 C5 1.373(3) . ? C4 H4 0.9500 . ? C5 C6 1.404(3) . ? C5 H5 0.9500 . ? C6 C7 1.367(3) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.408(3) . ? C8 C15 1.511(3) . ? C8 H8 1.0000 . ? C9 C10 1.514(3) . ? C9 H9 1.0000 . ? C10 C11 1.537(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.523(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.531(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.541(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.537(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.405(3) . ? C16 C23 1.520(3) . ? C16 H16 1.0000 . ? C17 C18 1.511(3) . ? C17 H17 1.0000 . ? C18 C19 1.542(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.528(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.541(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.532(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.542(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 Rh C16 86.33(7) . . ? C9 Rh C8 38.21(7) . . ? C16 Rh C8 92.29(7) . . ? C9 Rh C17 105.40(8) . . ? C16 Rh C17 37.98(8) . . ? C8 Rh C17 87.63(7) . . ? C9 Rh C1 147.38(8) . . ? C16 Rh C1 101.78(7) . . ? C8 Rh C1 164.78(7) . . ? C17 Rh C1 99.84(8) . . ? C9 Rh C3 95.58(8) . . ? C16 Rh C3 149.43(8) . . ? C8 Rh C3 108.00(8) . . ? C17 Rh C3 158.86(7) . . ? C1 Rh C3 61.76(8) . . ? C9 Rh C2 111.02(8) . . ? C16 Rh C2 114.48(9) . . ? C8 Rh C2 139.88(8) . . ? C17 Rh C2 131.92(8) . . ? C1 Rh C2 36.91(8) . . ? C3 Rh C2 36.86(8) . . ? C9 Rh C1A 150.50(7) . . ? C16 Rh C1A 123.17(7) . . ? C8 Rh C1A 129.64(7) . . ? C17 Rh C1A 99.50(7) . . ? C1 Rh C1A 36.28(7) . . ? C3 Rh C1A 59.65(7) . . ? C2 Rh C1A 59.77(8) . . ? C9 Rh C3A 116.12(7) . . ? C16 Rh C3A 157.54(7) . . ? C8 Rh C3A 105.10(7) . . ? C17 Rh C3A 127.14(7) . . ? C1 Rh C3A 59.84(7) . . ? C3 Rh C3A 36.07(7) . . ? C2 Rh C3A 59.72(7) . . ? C1A Rh C3A 34.38(7) . . ? C7 C1A C3A 119.46(19) . . ? C7 C1A C1 133.2(2) . . ? C3A C1A C1 107.34(18) . . ? C7 C1A Rh 127.34(13) . . ? C3A C1A Rh 72.89(10) . . ? C1 C1A Rh 65.02(10) . . ? C2 C1 C1A 108.1(2) . . ? C2 C1 Rh 72.10(13) . . ? C1A C1 Rh 78.69(11) . . ? C2 C1 H1 125.3 . . ? C1A C1 H1 125.3 . . ? Rh C1 H1 125.3 . . ? C1 C2 C3 108.1(2) . . ? C1 C2 Rh 70.99(12) . . ? C3 C2 Rh 71.33(11) . . ? C1 C2 H2 125.9 . . ? C3 C2 H2 125.9 . . ? Rh C2 H2 125.9 . . ? C2 C3 C3A 108.31(19) . . ? C2 C3 Rh 71.81(11) . . ? C3A C3 Rh 78.60(11) . . ? C2 C3 H3 125.3 . . ? C3A C3 H3 125.3 . . ? Rh C3 H3 125.3 . . ? C4 C3A C1A 120.2(2) . . ? C4 C3A C3 132.5(2) . . ? C1A C3A C3 107.38(17) . . ? C4 C3A Rh 126.86(12) . . ? C1A C3A Rh 72.73(10) . . ? C3 C3A Rh 65.33(10) . . ? C5 C4 C3A 118.7(2) . . ? C5 C4 H4 120.6 . . ? C3A C4 H4 120.6 . . ? C4 C5 C6 121.1(2) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C7 C6 C5 121.5(2) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C6 C7 C1A 119.0(2) . . ? C6 C7 H7 120.5 . . ? C1A C7 H7 120.5 . . ? C9 C8 C15 123.36(17) . . ? C9 C8 Rh 70.80(11) . . ? C15 C8 Rh 116.12(13) . . ? C9 C8 H8 113.3 . . ? C15 C8 H8 113.3 . . ? Rh C8 H8 113.3 . . ? C8 C9 C10 122.59(18) . . ? C8 C9 Rh 70.99(11) . . ? C10 C9 Rh 119.15(14) . . ? C8 C9 H9 112.7 . . ? C10 C9 H9 112.7 . . ? Rh C9 H9 112.7 . . ? C9 C10 C11 109.85(18) . . ? C9 C10 H10A 109.7 . . ? C11 C10 H10A 109.7 . . ? C9 C10 H10B 109.7 . . ? C11 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? C12 C11 C10 115.32(19) . . ? C12 C11 H11A 108.4 . . ? C10 C11 H11A 108.4 . . ? C12 C11 H11B 108.4 . . ? C10 C11 H11B 108.4 . . ? H11A C11 H11B 107.5 . . ? C11 C12 C13 115.4(2) . . ? C11 C12 H12A 108.4 . . ? C13 C12 H12A 108.4 . . ? C11 C12 H12B 108.4 . . ? C13 C12 H12B 108.4 . . ? H12A C12 H12B 107.5 . . ? C12 C13 C14 116.8(2) . . ? C12 C13 H13A 108.1 . . ? C14 C13 H13A 108.1 . . ? C12 C13 H13B 108.1 . . ? C14 C13 H13B 108.1 . . ? H13A C13 H13B 107.3 . . ? C15 C14 C13 115.66(18) . . ? C15 C14 H14A 108.4 . . ? C13 C14 H14A 108.4 . . ? C15 C14 H14B 108.4 . . ? C13 C14 H14B 108.4 . . ? H14A C14 H14B 107.4 . . ? C8 C15 C14 113.89(16) . . ? C8 C15 H15A 108.8 . . ? C14 C15 H15A 108.8 . . ? C8 C15 H15B 108.8 . . ? C14 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C17 C16 C23 124.67(18) . . ? C17 C16 Rh 71.57(11) . . ? C23 C16 Rh 115.35(13) . . ? C17 C16 H16 112.9 . . ? C23 C16 H16 112.9 . . ? Rh C16 H16 112.9 . . ? C16 C17 C18 121.97(17) . . ? C16 C17 Rh 70.45(11) . . ? C18 C17 Rh 118.17(13) . . ? C16 C17 H17 113.2 . . ? C18 C17 H17 113.2 . . ? Rh C17 H17 113.2 . . ? C17 C18 C19 110.50(16) . . ? C17 C18 H18A 109.5 . . ? C19 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C20 C19 C18 115.23(17) . . ? C20 C19 H19A 108.5 . . ? C18 C19 H19A 108.5 . . ? C20 C19 H19B 108.5 . . ? C18 C19 H19B 108.5 . . ? H19A C19 H19B 107.5 . . ? C19 C20 C21 115.97(17) . . ? C19 C20 H20A 108.3 . . ? C21 C20 H20A 108.3 . . ? C19 C20 H20B 108.3 . . ? C21 C20 H20B 108.3 . . ? H20A C20 H20B 107.4 . . ? C22 C21 C20 115.08(17) . . ? C22 C21 H21A 108.5 . . ? C20 C21 H21A 108.5 . . ? C22 C21 H21B 108.5 . . ? C20 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? C21 C22 C23 116.55(17) . . ? C21 C22 H22A 108.2 . . ? C23 C22 H22A 108.2 . . ? C21 C22 H22B 108.2 . . ? C23 C22 H22B 108.2 . . ? H22A C22 H22B 107.3 . . ? C16 C23 C22 113.96(16) . . ? C16 C23 H23A 108.8 . . ? C22 C23 H23A 108.8 . . ? C16 C23 H23B 108.8 . . ? C22 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.795 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.056 # Attachment 'sw071089.cif' data_sw071089 _database_code_depnum_ccdc_archive 'CCDC 686224' _publ_section_references ; Bruker (2006). SAINT. Version 7.23A. Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (1999). SMART. Version 5.054. Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2004). SADABS 2004. Bruker AXS Inc., Madison, Wisconsin, USA. ; _publ_section_exptl_refinement ; ? ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H33 P2 Rh' _chemical_formula_sum 'C37 H33 P2 Rh' _chemical_formula_weight 642.48 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' Rh Rh -1.1178 0.9187 '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' _symmetry_space_group_name_Hall '-P 2ybc ' _symmetry_int_tables_number 14 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 17.385(4) _cell_length_b 10.162(2) _cell_length_c 17.492(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.055(4) _cell_angle_gamma 90.00 _cell_volume 3010.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 5228 _cell_measurement_theta_min 2.333 _cell_measurement_theta_max 28.245 _exptl_crystal_description Irregular _exptl_crystal_colour Orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.025 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.698 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7675 _exptl_absorpt_correction_T_max 0.9828 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2004)' _exptl_special_details ; Crystal decay was monitored by repeating the initial 50 frames at the end of the data collection and analyzing duplicate reflections. ; _diffrn_ambient_temperature 173(1) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type K760 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART1000/P4' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 19545 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0715 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6710 _reflns_number_gt 4557 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Sheldrick, 2008)' _computing_publication_material 'Bruker SHELXTL (Sheldrick, 2008)' _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^)+(0.0447P)^2^+8.3225P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6710 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1374 _refine_ls_wR_factor_gt 0.1055 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.25582(2) 0.36084(3) 0.31514(2) 0.02079(12) Uani 1 1 d . . . P1 P 0.23500(7) 0.57629(11) 0.32027(7) 0.0226(3) Uani 1 1 d . . . P2 P 0.25336(7) 0.35371(10) 0.18779(7) 0.0208(2) Uani 1 1 d . . . C1 C 0.2706(3) 0.3055(5) 0.4413(3) 0.0270(10) Uani 1 1 d . . . H1 H 0.2762 0.3687 0.4860 0.032 Uiso 1 1 calc R . . C2 C 0.3340(3) 0.2509(5) 0.4128(3) 0.0326(11) Uani 1 1 d . . . H2 H 0.3914 0.2685 0.4344 0.039 Uiso 1 1 calc R . . C3 C 0.3024(3) 0.1606(4) 0.3518(3) 0.0299(11) Uani 1 1 d . . . H3 H 0.3340 0.1047 0.3232 0.036 Uiso 1 1 calc R . . C3A C 0.2199(3) 0.1416(4) 0.3514(3) 0.0260(10) Uani 1 1 d . . . C4 C 0.1618(3) 0.0583(5) 0.3080(3) 0.0346(12) Uani 1 1 d . . . H4 H 0.1739 0.0005 0.2696 0.041 Uiso 1 1 calc R . . C5 C 0.0874(3) 0.0617(5) 0.3217(3) 0.0380(13) Uani 1 1 d . . . H5 H 0.0481 0.0042 0.2932 0.046 Uiso 1 1 calc R . . C6 C 0.0678(3) 0.1478(5) 0.3767(3) 0.0378(12) Uani 1 1 d . . . H6 H 0.0156 0.1476 0.3849 0.045 Uiso 1 1 calc R . . C7 C 0.1231(3) 0.2332(5) 0.4193(3) 0.0331(11) Uani 1 1 d . . . H7 H 0.1092 0.2921 0.4561 0.040 Uiso 1 1 calc R . . C7A C 0.2001(3) 0.2316(4) 0.4073(3) 0.0273(10) Uani 1 1 d . . . C8 C 0.1711(3) 0.6318(4) 0.3842(3) 0.0261(10) Uani 1 1 d . . . C9 C 0.1025(3) 0.5609(5) 0.3825(3) 0.0351(12) Uani 1 1 d . . . H9 H 0.0916 0.4846 0.3505 0.042 Uiso 1 1 calc R . . C10 C 0.0497(3) 0.5999(6) 0.4271(3) 0.0431(14) Uani 1 1 d . . . H10 H 0.0031 0.5501 0.4259 0.052 Uiso 1 1 calc R . . C11 C 0.0653(4) 0.7124(6) 0.4734(3) 0.0449(14) Uani 1 1 d . . . H11 H 0.0294 0.7395 0.5040 0.054 Uiso 1 1 calc R . . C12 C 0.1323(4) 0.7839(5) 0.4749(3) 0.0415(13) Uani 1 1 d . . . H12 H 0.1428 0.8606 0.5066 0.050 Uiso 1 1 calc R . . C13 C 0.1854(3) 0.7446(5) 0.4301(3) 0.0353(12) Uani 1 1 d . . . H13 H 0.2316 0.7953 0.4311 0.042 Uiso 1 1 calc R . . C14 C 0.3273(3) 0.6667(4) 0.3573(3) 0.0237(10) Uani 1 1 d . . . C15 C 0.3460(3) 0.7838(5) 0.3234(3) 0.0323(11) Uani 1 1 d . . . H15 H 0.3076 0.8252 0.2834 0.039 Uiso 1 1 calc R . . C16 C 0.4204(3) 0.8399(5) 0.3481(3) 0.0365(12) Uani 1 1 d . . . H16 H 0.4329 0.9182 0.3239 0.044 Uiso 1 1 calc R . . C17 C 0.4762(3) 0.7829(5) 0.4075(3) 0.0376(13) Uani 1 1 d . . . H17 H 0.5269 0.8218 0.4243 0.045 Uiso 1 1 calc R . . C18 C 0.4577(3) 0.6687(5) 0.4424(3) 0.0369(12) Uani 1 1 d . . . H18 H 0.4958 0.6297 0.4838 0.044 Uiso 1 1 calc R . . C19 C 0.3846(3) 0.6111(5) 0.4175(3) 0.0327(11) Uani 1 1 d . . . H19 H 0.3730 0.5323 0.4419 0.039 Uiso 1 1 calc R . . C20 C 0.1936(3) 0.6683(4) 0.2311(3) 0.0288(11) Uani 1 1 d . . . H20 H 0.2212 0.6635 0.1901 0.035 Uiso 1 1 calc R . . C21 C 0.1293(3) 0.7409(5) 0.2179(3) 0.0351(12) Uani 1 1 d . . . H21A H 0.0997 0.7489 0.2571 0.042 Uiso 1 1 calc R . . H21B H 0.1125 0.7853 0.1692 0.042 Uiso 1 1 calc R . . C22 C 0.3223(3) 0.4580(4) 0.1495(3) 0.0243(10) Uani 1 1 d . . . C23 C 0.3854(3) 0.5161(4) 0.2036(3) 0.0297(11) Uani 1 1 d . . . H23 H 0.3912 0.5008 0.2582 0.036 Uiso 1 1 calc R . . C24 C 0.4389(3) 0.5955(5) 0.1776(3) 0.0351(12) Uani 1 1 d . . . H24 H 0.4808 0.6355 0.2147 0.042 Uiso 1 1 calc R . . C25 C 0.4321(3) 0.6172(5) 0.0984(3) 0.0369(12) Uani 1 1 d . . . H25 H 0.4690 0.6721 0.0811 0.044 Uiso 1 1 calc R . . C26 C 0.3713(3) 0.5587(5) 0.0444(3) 0.0372(12) Uani 1 1 d . . . H26 H 0.3668 0.5725 -0.0101 0.045 Uiso 1 1 calc R . . C27 C 0.3168(3) 0.4798(5) 0.0696(3) 0.0311(11) Uani 1 1 d . . . H27 H 0.2751 0.4402 0.0321 0.037 Uiso 1 1 calc R . . C28 C 0.2780(3) 0.1902(4) 0.1543(3) 0.0243(10) Uani 1 1 d . . . C29 C 0.3560(3) 0.1530(5) 0.1602(3) 0.0315(11) Uani 1 1 d . . . H29 H 0.3972 0.2146 0.1785 0.038 Uiso 1 1 calc R . . C30 C 0.3745(3) 0.0268(5) 0.1397(3) 0.0398(13) Uani 1 1 d . . . H30 H 0.4281 0.0024 0.1443 0.048 Uiso 1 1 calc R . . C31 C 0.3152(4) -0.0632(5) 0.1126(3) 0.0415(14) Uani 1 1 d . . . H31 H 0.3280 -0.1493 0.0983 0.050 Uiso 1 1 calc R . . C32 C 0.2377(4) -0.0282(5) 0.1064(3) 0.0387(13) Uani 1 1 d . . . H32 H 0.1970 -0.0905 0.0879 0.046 Uiso 1 1 calc R . . C33 C 0.2183(3) 0.0981(5) 0.1270(3) 0.0311(11) Uani 1 1 d . . . H33 H 0.1645 0.1215 0.1224 0.037 Uiso 1 1 calc R . . C34 C 0.1598(3) 0.3840(4) 0.1200(3) 0.0300(11) Uani 1 1 d . . . H34 H 0.1584 0.3930 0.0656 0.036 Uiso 1 1 calc R . . C35 C 0.0943(3) 0.3936(5) 0.1439(4) 0.0452(15) Uani 1 1 d . . . H35A H 0.0949 0.3848 0.1981 0.054 Uiso 1 1 calc R . . H35B H 0.0459 0.4096 0.1071 0.054 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 0.0267(2) 0.01938(16) 0.01692(19) -0.00104(14) 0.00621(13) -0.00102(14) P1 0.0281(6) 0.0209(5) 0.0189(6) -0.0011(5) 0.0059(5) -0.0016(4) P2 0.0251(6) 0.0217(5) 0.0161(6) -0.0017(4) 0.0054(4) -0.0004(4) C1 0.041(3) 0.032(2) 0.007(2) -0.0004(18) 0.0038(19) -0.010(2) C2 0.031(3) 0.031(2) 0.033(3) 0.009(2) 0.002(2) 0.003(2) C3 0.036(3) 0.027(2) 0.028(3) 0.0024(19) 0.008(2) 0.009(2) C3A 0.037(3) 0.0189(19) 0.022(2) -0.0003(18) 0.007(2) 0.0020(19) C4 0.050(3) 0.024(2) 0.031(3) -0.002(2) 0.014(2) -0.004(2) C5 0.040(3) 0.036(3) 0.037(3) 0.000(2) 0.008(2) -0.014(2) C6 0.034(3) 0.041(3) 0.043(3) 0.009(2) 0.019(2) -0.002(2) C7 0.046(3) 0.032(2) 0.025(3) 0.006(2) 0.017(2) 0.003(2) C7A 0.036(3) 0.026(2) 0.021(2) 0.0051(19) 0.010(2) 0.0010(19) C8 0.033(3) 0.027(2) 0.018(2) 0.0028(19) 0.0047(19) 0.0023(19) C9 0.037(3) 0.034(2) 0.034(3) 0.002(2) 0.010(2) 0.005(2) C10 0.037(3) 0.054(3) 0.044(3) 0.009(3) 0.021(3) 0.004(3) C11 0.049(4) 0.056(3) 0.035(3) 0.004(3) 0.021(3) 0.022(3) C12 0.057(4) 0.037(3) 0.033(3) -0.005(2) 0.014(3) 0.013(3) C13 0.045(3) 0.031(2) 0.034(3) -0.001(2) 0.015(2) 0.004(2) C14 0.027(2) 0.022(2) 0.024(2) -0.0075(18) 0.0095(19) -0.0042(17) C15 0.036(3) 0.027(2) 0.035(3) 0.000(2) 0.011(2) 0.001(2) C16 0.039(3) 0.030(2) 0.045(3) -0.003(2) 0.018(3) -0.009(2) C17 0.030(3) 0.035(3) 0.049(4) -0.014(2) 0.012(2) -0.008(2) C18 0.033(3) 0.039(3) 0.034(3) -0.007(2) -0.002(2) -0.001(2) C19 0.039(3) 0.029(2) 0.028(3) -0.002(2) 0.004(2) -0.003(2) C20 0.035(3) 0.027(2) 0.025(3) -0.0024(19) 0.008(2) -0.0061(19) C21 0.039(3) 0.033(3) 0.030(3) 0.003(2) 0.003(2) 0.002(2) C22 0.026(2) 0.022(2) 0.025(3) -0.0032(18) 0.0071(19) 0.0029(17) C23 0.034(3) 0.029(2) 0.027(3) -0.001(2) 0.010(2) 0.000(2) C24 0.033(3) 0.032(2) 0.042(3) -0.006(2) 0.011(2) -0.004(2) C25 0.038(3) 0.032(3) 0.046(3) 0.010(2) 0.022(3) 0.000(2) C26 0.047(3) 0.037(3) 0.031(3) 0.011(2) 0.016(2) 0.008(2) C27 0.037(3) 0.029(2) 0.027(3) 0.000(2) 0.007(2) 0.000(2) C28 0.037(3) 0.026(2) 0.012(2) 0.0006(17) 0.0096(19) 0.0010(19) C29 0.033(3) 0.035(2) 0.025(3) 0.001(2) 0.005(2) 0.003(2) C30 0.046(3) 0.037(3) 0.037(3) 0.001(2) 0.010(3) 0.016(2) C31 0.070(4) 0.027(2) 0.031(3) 0.000(2) 0.020(3) 0.008(3) C32 0.058(4) 0.028(2) 0.031(3) -0.007(2) 0.011(3) -0.008(2) C33 0.039(3) 0.035(2) 0.023(3) 0.000(2) 0.012(2) -0.002(2) C34 0.034(3) 0.031(2) 0.022(2) -0.0066(19) -0.001(2) 0.000(2) C35 0.031(3) 0.050(3) 0.049(4) -0.022(3) -0.001(3) 0.003(2) _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 P2 2.2194(13) . ? Rh1 P1 2.2243(13) . ? Rh1 C2 2.228(5) . ? Rh1 C3 2.230(4) . ? Rh1 C1 2.235(4) . ? Rh1 C3A 2.435(4) . ? Rh1 C7A 2.443(5) . ? P1 C20 1.822(5) . ? P1 C8 1.834(5) . ? P1 C14 1.834(5) . ? P2 C34 1.810(5) . ? P2 C22 1.837(5) . ? P2 C28 1.844(5) . ? C1 C2 1.421(7) . ? C1 C7A 1.446(7) . ? C1 H1 1.0000 . ? C2 C3 1.420(7) . ? C2 H2 1.0000 . ? C3 C3A 1.444(7) . ? C3 H3 1.0000 . ? C3A C4 1.403(7) . ? C3A C7A 1.436(6) . ? C4 C5 1.368(8) . ? C4 H4 0.9500 . ? C5 C6 1.398(8) . ? C5 H5 0.9500 . ? C6 C7 1.383(7) . ? C6 H6 0.9500 . ? C7 C7A 1.400(7) . ? C7 H7 0.9500 . ? C8 C9 1.388(7) . ? C8 C13 1.390(7) . ? C9 C10 1.391(8) . ? C9 H9 0.9500 . ? C10 C11 1.392(8) . ? C10 H10 0.9500 . ? C11 C12 1.368(8) . ? C11 H11 0.9500 . ? C12 C13 1.398(8) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C19 1.396(7) . ? C14 C15 1.400(6) . ? C15 C16 1.391(7) . ? C15 H15 0.9500 . ? C16 C17 1.378(8) . ? C16 H16 0.9500 . ? C17 C18 1.382(7) . ? C17 H17 0.9500 . ? C18 C19 1.378(7) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.315(7) . ? C20 H20 0.9500 . ? C21 H21A 0.9500 . ? C21 H21B 0.9500 . ? C22 C27 1.396(7) . ? C22 C23 1.406(6) . ? C23 C24 1.383(7) . ? C23 H23 0.9500 . ? C24 C25 1.382(8) . ? C24 H24 0.9500 . ? C25 C26 1.383(8) . ? C25 H25 0.9500 . ? C26 C27 1.386(7) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.389(7) . ? C28 C33 1.400(7) . ? C29 C30 1.389(7) . ? C29 H29 0.9500 . ? C30 C31 1.380(8) . ? C30 H30 0.9500 . ? C31 C32 1.373(8) . ? C31 H31 0.9500 . ? C32 C33 1.395(7) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.303(8) . ? C34 H34 0.9500 . ? C35 H35A 0.9500 . ? C35 H35B 0.9500 . ? 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 Rh1 P1 96.10(4) . . ? P2 Rh1 C2 128.54(14) . . ? P1 Rh1 C2 122.64(13) . . ? P2 Rh1 C3 100.51(13) . . ? P1 Rh1 C3 159.78(13) . . ? C2 Rh1 C3 37.14(18) . . ? P2 Rh1 C1 162.65(13) . . ? P1 Rh1 C1 101.03(13) . . ? C2 Rh1 C1 37.14(19) . . ? C3 Rh1 C1 62.15(18) . . ? P2 Rh1 C3A 106.46(11) . . ? P1 Rh1 C3A 146.74(12) . . ? C2 Rh1 C3A 59.30(17) . . ? C3 Rh1 C3A 35.72(17) . . ? C1 Rh1 C3A 59.46(16) . . ? P2 Rh1 C7A 136.39(12) . . ? P1 Rh1 C7A 114.22(11) . . ? C2 Rh1 C7A 59.24(18) . . ? C3 Rh1 C7A 59.45(17) . . ? C1 Rh1 C7A 35.65(16) . . ? C3A Rh1 C7A 34.24(15) . . ? C20 P1 C8 100.8(2) . . ? C20 P1 C14 100.9(2) . . ? C8 P1 C14 103.5(2) . . ? C20 P1 Rh1 120.47(15) . . ? C8 P1 Rh1 116.99(15) . . ? C14 P1 Rh1 111.70(15) . . ? C34 P2 C22 103.1(2) . . ? C34 P2 C28 100.6(2) . . ? C22 P2 C28 100.7(2) . . ? C34 P2 Rh1 117.58(18) . . ? C22 P2 Rh1 118.76(15) . . ? C28 P2 Rh1 113.29(14) . . ? C2 C1 C7A 107.8(4) . . ? C2 C1 Rh1 71.2(3) . . ? C7A C1 Rh1 80.0(3) . . ? C2 C1 H1 125.4 . . ? C7A C1 H1 125.4 . . ? Rh1 C1 H1 125.4 . . ? C3 C2 C1 108.4(4) . . ? C3 C2 Rh1 71.5(3) . . ? C1 C2 Rh1 71.7(3) . . ? C3 C2 H2 125.7 . . ? C1 C2 H2 125.7 . . ? Rh1 C2 H2 125.7 . . ? C2 C3 C3A 107.8(4) . . ? C2 C3 Rh1 71.4(3) . . ? C3A C3 Rh1 79.9(3) . . ? C2 C3 H3 125.4 . . ? C3A C3 H3 125.4 . . ? Rh1 C3 H3 125.4 . . ? C4 C3A C7A 119.8(5) . . ? C4 C3A C3 132.6(5) . . ? C7A C3A C3 107.6(4) . . ? C4 C3A Rh1 127.3(3) . . ? C7A C3A Rh1 73.2(2) . . ? C3 C3A Rh1 64.4(2) . . ? C5 C4 C3A 119.0(5) . . ? C5 C4 H4 120.5 . . ? C3A C4 H4 120.5 . . ? C4 C5 C6 121.5(5) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C7 C6 C5 121.1(5) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C7A 118.9(5) . . ? C6 C7 H7 120.5 . . ? C7A C7 H7 120.5 . . ? C7 C7A C3A 119.6(4) . . ? C7 C7A C1 133.0(5) . . ? C3A C7A C1 107.4(4) . . ? C7 C7A Rh1 128.8(3) . . ? C3A C7A Rh1 72.6(3) . . ? C1 C7A Rh1 64.3(2) . . ? C9 C8 C13 118.8(5) . . ? C9 C8 P1 117.6(4) . . ? C13 C8 P1 123.5(4) . . ? C8 C9 C10 120.9(5) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C9 C10 C11 119.6(5) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 120.1(5) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 120.3(5) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C8 C13 C12 120.3(5) . . ? C8 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C19 C14 C15 117.9(4) . . ? C19 C14 P1 118.8(3) . . ? C15 C14 P1 123.0(4) . . ? C16 C15 C14 120.5(5) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C16 C15 120.5(5) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 119.5(5) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C19 C18 C17 120.5(5) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C14 121.1(5) . . ? C18 C19 H19 119.4 . . ? C14 C19 H19 119.4 . . ? C21 C20 P1 126.4(4) . . ? C21 C20 H20 116.8 . . ? P1 C20 H20 116.8 . . ? C20 C21 H21A 120.0 . . ? C20 C21 H21B 120.0 . . ? H21A C21 H21B 120.0 . . ? C27 C22 C23 118.3(5) . . ? C27 C22 P2 123.6(4) . . ? C23 C22 P2 118.1(4) . . ? C24 C23 C22 120.3(5) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C25 C24 C23 120.7(5) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 119.7(5) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C25 C26 C27 120.3(5) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C26 C27 C22 120.8(5) . . ? C26 C27 H27 119.6 . . ? C22 C27 H27 119.6 . . ? C29 C28 C33 118.7(4) . . ? C29 C28 P2 120.9(4) . . ? C33 C28 P2 120.2(4) . . ? C28 C29 C30 120.7(5) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C31 C30 C29 120.2(5) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C32 C31 C30 119.9(5) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 C33 120.6(5) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C32 C33 C28 120.0(5) . . ? C32 C33 H33 120.0 . . ? C28 C33 H33 120.0 . . ? C35 C34 P2 121.6(4) . . ? C35 C34 H34 119.2 . . ? P2 C34 H34 119.2 . . ? C34 C35 H35A 120.0 . . ? C34 C35 H35B 120.0 . . ? H35A C35 H35B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.514 _refine_diff_density_min -1.284 _refine_diff_density_rms 0.134 # Attachment '08srv426_compl.cif' data_08srv426 _database_code_depnum_ccdc_archive 'CCDC 708194' _audit_creation_method SHELXL-97 _chemical_name_systematic ;bis(\m~2~-1,2-bis(Diphenylphosphino)ethyne)- bis(\h^5^-indenyl)-di-rodium ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C70 H54 P4 Rh2' _chemical_formula_sum 'C70 H54 P4 Rh2' _chemical_formula_weight 1224.83 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.6644(2) _cell_length_b 13.4814(2) _cell_length_c 19.1415(3) _cell_angle_alpha 102.0975(5) _cell_angle_beta 92.9700(6) _cell_angle_gamma 106.4690(5) _cell_volume 2802.52(8) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9882 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 29.98 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 0.746 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8926 _exptl_absorpt_correction_T_max 0.9618 _exptl_absorpt_process_details 'SADABS 2006/1 (Bruker AXS)' _exptl_special_details ; The collected data covered more than one hemisphere of the reciprocal space. A combination of 5 sets of \w scans were used. each set at different \w or 2\q angles and each scan 0.3 deg in \w. ; _diffrn_ambient_temperature 120(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 'Bruker SMART 6K CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 5.6 _diffrn_standards_number 0 _diffrn_reflns_number 43145 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12873 _reflns_number_gt 10611 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART version 5.049 (Bruker, 1998)' _computing_cell_refinement 'SAINT version 7.46A (Bruker, 2007)' _computing_data_reduction 'SAINT version 7.46A (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXTL version 6.14 (Bruker, 2003)' _computing_molecular_graphics 'SHELXTL version 6.14 (Bruker, 2003)' _computing_publication_material 'SHELXTL version 6.14 (Bruker, 2003)' _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. ; _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^)+(0.0349P)^2^+2.0246P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12873 _refine_ls_number_parameters 685 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0406 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0757 _refine_ls_wR_factor_gt 0.0698 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.374958(15) 0.638171(13) 0.157536(9) 0.01510(5) Uani 1 1 d . . . Rh1B Rh 0.043034(14) 0.243712(13) 0.300141(9) 0.01533(5) Uani 1 1 d . . . P1 P 0.20032(5) 0.62729(4) 0.19822(3) 0.01511(11) Uani 1 1 d . . . P1B P 0.22882(5) 0.33198(4) 0.35023(3) 0.01577(11) Uani 1 1 d . . . P2 P 0.07792(5) 0.26468(4) 0.19191(3) 0.01507(11) Uani 1 1 d . . . P2B P 0.46153(5) 0.61086(4) 0.25438(3) 0.01561(11) Uani 1 1 d . . . C1 C 0.3313(2) 0.66025(19) 0.04935(12) 0.0231(5) Uani 1 1 d . . . H1 H 0.2493 0.6542 0.0367 0.028 Uiso 1 1 calc R . . C1B C -0.1500(2) 0.1510(2) 0.28004(13) 0.0247(5) Uani 1 1 d . . . H1B H -0.1866 0.1395 0.2323 0.030 Uiso 1 1 calc R . . C2 C 0.3822(2) 0.5751(2) 0.03978(12) 0.0249(5) Uani 1 1 d . . . H2 H 0.3431 0.5039 0.0140 0.030 Uiso 1 1 calc R . . C2B C -0.1361(2) 0.2422(2) 0.33670(13) 0.0248(5) Uani 1 1 d . . . H2B H -0.1707 0.2977 0.3353 0.030 Uiso 1 1 calc R . . C3 C 0.5009(2) 0.61445(19) 0.07515(12) 0.0234(5) Uani 1 1 d . . . H3 H 0.5515 0.5727 0.0830 0.028 Uiso 1 1 calc R . . C3A C 0.5324(2) 0.72899(19) 0.09731(12) 0.0208(5) Uani 1 1 d . . . C3B C -0.0625(2) 0.2362(2) 0.39510(13) 0.0278(5) Uani 1 1 d . . . H3B H -0.0300 0.2911 0.4373 0.033 Uiso 1 1 calc R . . C3AB C -0.0444(2) 0.1320(2) 0.38012(13) 0.0258(5) Uani 1 1 d . . . C4 C 0.6401(2) 0.8082(2) 0.12738(13) 0.0249(5) Uani 1 1 d . . . H4 H 0.7113 0.7899 0.1370 0.030 Uiso 1 1 calc R . . C4B C 0.0115(3) 0.0806(2) 0.42157(16) 0.0373(7) Uani 1 1 d . . . H4B H 0.0471 0.1151 0.4695 0.045 Uiso 1 1 calc R . . C5 C 0.6416(2) 0.9134(2) 0.14287(14) 0.0299(6) Uani 1 1 d . . . H5 H 0.7150 0.9678 0.1619 0.036 Uiso 1 1 calc R . . C5B C 0.0138(3) -0.0205(3) 0.39147(18) 0.0423(7) Uani 1 1 d . . . H5B H 0.0495 -0.0566 0.4196 0.051 Uiso 1 1 calc R . . C6 C 0.5365(2) 0.9411(2) 0.13092(15) 0.0320(6) Uani 1 1 d . . . H6 H 0.5396 1.0139 0.1434 0.038 Uiso 1 1 calc R . . C6B C -0.0350(3) -0.0715(2) 0.32043(19) 0.0421(7) Uani 1 1 d . . . H6B H -0.0296 -0.1406 0.3009 0.050 Uiso 1 1 calc R . . C7 C 0.4290(2) 0.8655(2) 0.10162(13) 0.0265(5) Uani 1 1 d . . . H7 H 0.3579 0.8853 0.0949 0.032 Uiso 1 1 calc R . . C7A C 0.4262(2) 0.75836(19) 0.08184(12) 0.0212(5) Uani 1 1 d . . . C7B C -0.0908(2) -0.0235(2) 0.27796(16) 0.0326(6) Uani 1 1 d . . . H7B H -0.1230 -0.0587 0.2296 0.039 Uiso 1 1 calc R . . C7AB C -0.0988(2) 0.0788(2) 0.30784(14) 0.0251(5) Uani 1 1 d . . . C8 C 0.0968(2) 0.67247(18) 0.14658(12) 0.0188(4) Uani 1 1 d . . . C8B C 0.23872(19) 0.39774(18) 0.44482(12) 0.0191(4) Uani 1 1 d . . . C9 C 0.1061(2) 0.7802(2) 0.16108(14) 0.0281(5) Uani 1 1 d . . . H9 H 0.1608 0.8284 0.2002 0.034 Uiso 1 1 calc R . . C9B C 0.2494(2) 0.3448(2) 0.49821(13) 0.0301(6) Uani 1 1 d . . . H9B H 0.2601 0.2763 0.4859 0.036 Uiso 1 1 calc R . . C10 C 0.0355(3) 0.8176(2) 0.11848(16) 0.0390(7) Uani 1 1 d . . . H10 H 0.0423 0.8912 0.1289 0.047 Uiso 1 1 calc R . . C10B C 0.2445(3) 0.3910(2) 0.56984(14) 0.0365(6) Uani 1 1 d . . . H10B H 0.2521 0.3538 0.6060 0.044 Uiso 1 1 calc R . . C11 C -0.0443(3) 0.7487(2) 0.06130(15) 0.0358(6) Uani 1 1 d . . . H11 H -0.0918 0.7749 0.0322 0.043 Uiso 1 1 calc R . . C11B C 0.2290(3) 0.4895(2) 0.58817(14) 0.0386(7) Uani 1 1 d . . . H11B H 0.2255 0.5210 0.6370 0.046 Uiso 1 1 calc R . . C12 C -0.0546(2) 0.6415(2) 0.04668(14) 0.0323(6) Uani 1 1 d . . . H12 H -0.1096 0.5938 0.0075 0.039 Uiso 1 1 calc R . . C12B C 0.2184(3) 0.5433(3) 0.53492(16) 0.0458(8) Uani 1 1 d . . . H12B H 0.2078 0.6119 0.5475 0.055 Uiso 1 1 calc R . . C13 C 0.0153(2) 0.6030(2) 0.08921(13) 0.0253(5) Uani 1 1 d . . . H13 H 0.0074 0.5291 0.0790 0.030 Uiso 1 1 calc R . . C13B C 0.2231(3) 0.4976(2) 0.46357(14) 0.0344(6) Uani 1 1 d . . . H13B H 0.2156 0.5348 0.4274 0.041 Uiso 1 1 calc R . . C14 C 0.18679(19) 0.68594(17) 0.29148(12) 0.0177(4) Uani 1 1 d . . . C14B C 0.3342(2) 0.25349(18) 0.34869(12) 0.0200(4) Uani 1 1 d . . . C15 C 0.0962(2) 0.6393(2) 0.32962(13) 0.0235(5) Uani 1 1 d . . . H15 H 0.0372 0.5739 0.3072 0.028 Uiso 1 1 calc R . . C15B C 0.4587(2) 0.2986(2) 0.35546(16) 0.0315(6) Uani 1 1 d . . . H15B H 0.4928 0.3737 0.3651 0.038 Uiso 1 1 calc R . . C16 C 0.0922(2) 0.6886(2) 0.40052(14) 0.0297(6) Uani 1 1 d . . . H16 H 0.0301 0.6569 0.4264 0.036 Uiso 1 1 calc R . . C16B C 0.5328(3) 0.2334(3) 0.34800(18) 0.0426(7) Uani 1 1 d . . . H16B H 0.6175 0.2643 0.3516 0.051 Uiso 1 1 calc R . . C17 C 0.1781(2) 0.7835(2) 0.43359(13) 0.0295(5) Uani 1 1 d . . . H17 H 0.1753 0.8167 0.4821 0.035 Uiso 1 1 calc R . . C17B C 0.4850(3) 0.1245(3) 0.33543(17) 0.0421(7) Uani 1 1 d . . . H17B H 0.5363 0.0805 0.3301 0.051 Uiso 1 1 calc R . . C18 C 0.2682(2) 0.83003(19) 0.39597(13) 0.0266(5) Uani 1 1 d . . . H18 H 0.3273 0.8953 0.4187 0.032 Uiso 1 1 calc R . . C18B C 0.3619(3) 0.0798(2) 0.33064(15) 0.0352(6) Uani 1 1 d . . . H18B H 0.3285 0.0049 0.3230 0.042 Uiso 1 1 calc R . . C19 C 0.2726(2) 0.78171(18) 0.32502(13) 0.0215(5) Uani 1 1 d . . . H19 H 0.3344 0.8142 0.2993 0.026 Uiso 1 1 calc R . . C19B C 0.2867(2) 0.14383(19) 0.33699(13) 0.0249(5) Uani 1 1 d . . . H19B H 0.2021 0.1124 0.3333 0.030 Uiso 1 1 calc R . . C20 C 0.12135(19) 0.49125(18) 0.18948(12) 0.0181(4) Uani 1 1 d . . . C20B C 0.31499(19) 0.43950(17) 0.31693(12) 0.0174(4) Uani 1 1 d . . . C21 C 0.09288(19) 0.39690(17) 0.18566(11) 0.0178(4) Uani 1 1 d . . . C21B C 0.37464(19) 0.51150(18) 0.29406(12) 0.0184(4) Uani 1 1 d . . . C22 C 0.21022(19) 0.24358(17) 0.15131(11) 0.0173(4) Uani 1 1 d . . . C22B C 0.5221(2) 0.72257(18) 0.33268(12) 0.0195(4) Uani 1 1 d . . . C23 C 0.2495(2) 0.16090(19) 0.16557(13) 0.0228(5) Uani 1 1 d . . . H23 H 0.2090 0.1189 0.1962 0.027 Uiso 1 1 calc R . . C23B C 0.5811(2) 0.82144(19) 0.31959(14) 0.0252(5) Uani 1 1 d . . . H23B H 0.5845 0.8293 0.2715 0.030 Uiso 1 1 calc R . . C24 C 0.3484(2) 0.1396(2) 0.13503(14) 0.0305(6) Uani 1 1 d . . . H24 H 0.3757 0.0836 0.1453 0.037 Uiso 1 1 calc R . . C24B C 0.6346(3) 0.9082(2) 0.37640(16) 0.0349(6) Uani 1 1 d . . . H24B H 0.6780 0.9745 0.3673 0.042 Uiso 1 1 calc R . . C25 C 0.4066(2) 0.1997(2) 0.08994(15) 0.0337(6) Uani 1 1 d . . . H25 H 0.4730 0.1842 0.0684 0.040 Uiso 1 1 calc R . . C25B C 0.6246(3) 0.8975(2) 0.44640(16) 0.0395(7) Uani 1 1 d . . . H25B H 0.6609 0.9570 0.4853 0.047 Uiso 1 1 calc R . . C26 C 0.3683(2) 0.2826(2) 0.07606(14) 0.0321(6) Uani 1 1 d . . . H26 H 0.4090 0.3241 0.0453 0.038 Uiso 1 1 calc R . . C26B C 0.5623(3) 0.8011(2) 0.46031(14) 0.0355(6) Uani 1 1 d . . . H26B H 0.5533 0.7949 0.5084 0.043 Uiso 1 1 calc R . . C27 C 0.2708(2) 0.3054(2) 0.10681(12) 0.0243(5) Uani 1 1 d . . . H27 H 0.2454 0.3629 0.0976 0.029 Uiso 1 1 calc R . . C27B C 0.5130(2) 0.7135(2) 0.40319(13) 0.0265(5) Uani 1 1 d . . . H27B H 0.4725 0.6467 0.4125 0.032 Uiso 1 1 calc R . . C28 C -0.04541(19) 0.18878(17) 0.12064(11) 0.0175(4) Uani 1 1 d . . . C28B C 0.5925(2) 0.56257(18) 0.23832(11) 0.0183(4) Uani 1 1 d . . . C29 C -0.0526(2) 0.08601(18) 0.08453(12) 0.0221(5) Uani 1 1 d . . . H29 H 0.0116 0.0579 0.0927 0.027 Uiso 1 1 calc R . . C29B C 0.5792(2) 0.45429(19) 0.21920(13) 0.0237(5) Uani 1 1 d . . . H29B H 0.5029 0.4041 0.2182 0.028 Uiso 1 1 calc R . . C30 C -0.1535(2) 0.02418(19) 0.03645(13) 0.0269(5) Uani 1 1 d . . . H30 H -0.1574 -0.0458 0.0116 0.032 Uiso 1 1 calc R . . C30B C 0.6775(2) 0.4193(2) 0.20161(15) 0.0320(6) Uani 1 1 d . . . H30B H 0.6680 0.3452 0.1887 0.038 Uiso 1 1 calc R . . C31 C -0.2483(2) 0.0638(2) 0.02451(13) 0.0267(5) Uani 1 1 d . . . H31 H -0.3181 0.0207 -0.0073 0.032 Uiso 1 1 calc R . . C31B C 0.7895(2) 0.4920(2) 0.20270(15) 0.0336(6) Uani 1 1 d . . . H31B H 0.8565 0.4678 0.1907 0.040 Uiso 1 1 calc R . . C32 C -0.2399(2) 0.1679(2) 0.05981(13) 0.0264(5) Uani 1 1 d . . . H32 H -0.3034 0.1965 0.0510 0.032 Uiso 1 1 calc R . . C32B C 0.8027(2) 0.5995(2) 0.22136(14) 0.0290(5) Uani 1 1 d . . . H32B H 0.8789 0.6494 0.2217 0.035 Uiso 1 1 calc R . . C33 C -0.1397(2) 0.22930(19) 0.10752(13) 0.0240(5) Uani 1 1 d . . . H33 H -0.1351 0.2998 0.1316 0.029 Uiso 1 1 calc R . . C33B C 0.7055(2) 0.63529(19) 0.23966(13) 0.0234(5) Uani 1 1 d . . . H33B H 0.7158 0.7095 0.2532 0.028 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 0.01641(9) 0.01698(9) 0.01361(8) 0.00477(6) 0.00356(6) 0.00650(7) Rh1B 0.01388(8) 0.01760(9) 0.01413(8) 0.00329(6) 0.00234(6) 0.00434(6) P1 0.0161(3) 0.0157(3) 0.0152(3) 0.0048(2) 0.0027(2) 0.0063(2) P1B 0.0154(3) 0.0173(3) 0.0152(3) 0.0050(2) 0.0015(2) 0.0050(2) P2 0.0155(3) 0.0150(3) 0.0148(3) 0.0034(2) 0.0012(2) 0.0051(2) P2B 0.0154(3) 0.0171(3) 0.0157(3) 0.0058(2) 0.0028(2) 0.0055(2) C1 0.0243(12) 0.0292(13) 0.0144(10) 0.0082(9) 0.0020(9) 0.0040(10) C1B 0.0135(10) 0.0315(13) 0.0264(12) 0.0065(10) 0.0030(9) 0.0027(9) C2 0.0297(13) 0.0243(12) 0.0177(11) 0.0025(9) 0.0077(9) 0.0040(10) C2B 0.0159(11) 0.0322(13) 0.0272(12) 0.0059(10) 0.0104(9) 0.0079(10) C3 0.0283(12) 0.0257(12) 0.0201(11) 0.0069(9) 0.0117(9) 0.0115(10) C3A 0.0218(11) 0.0266(12) 0.0163(11) 0.0085(9) 0.0079(9) 0.0075(9) C3B 0.0235(12) 0.0354(14) 0.0207(12) 0.0029(10) 0.0092(10) 0.0043(10) C3AB 0.0202(11) 0.0335(13) 0.0233(12) 0.0129(10) 0.0086(9) 0.0022(10) C4 0.0209(11) 0.0311(13) 0.0248(12) 0.0123(10) 0.0050(9) 0.0067(10) C4B 0.0324(14) 0.0525(18) 0.0323(14) 0.0258(13) 0.0100(11) 0.0085(13) C5 0.0281(13) 0.0265(13) 0.0302(13) 0.0105(11) -0.0001(10) -0.0018(10) C5B 0.0361(15) 0.0473(18) 0.0561(19) 0.0372(16) 0.0125(14) 0.0130(14) C6 0.0377(15) 0.0206(12) 0.0379(15) 0.0110(11) 0.0009(12) 0.0066(11) C6B 0.0392(16) 0.0270(14) 0.064(2) 0.0192(14) 0.0129(15) 0.0095(12) C7 0.0280(13) 0.0272(13) 0.0285(13) 0.0128(10) 0.0027(10) 0.0105(10) C7A 0.0221(11) 0.0259(12) 0.0177(11) 0.0103(9) 0.0031(9) 0.0067(9) C7B 0.0261(13) 0.0263(13) 0.0418(16) 0.0072(12) 0.0049(11) 0.0029(11) C7AB 0.0179(11) 0.0272(12) 0.0290(13) 0.0105(10) 0.0055(9) 0.0017(9) C8 0.0190(11) 0.0238(11) 0.0183(11) 0.0094(9) 0.0052(8) 0.0102(9) C8B 0.0151(10) 0.0228(11) 0.0172(10) 0.0038(9) -0.0004(8) 0.0034(9) C9 0.0345(14) 0.0252(13) 0.0287(13) 0.0093(10) -0.0015(11) 0.0142(11) C9B 0.0366(14) 0.0369(14) 0.0223(12) 0.0104(11) 0.0045(11) 0.0171(12) C10 0.0499(18) 0.0321(15) 0.0438(17) 0.0163(13) 0.0010(14) 0.0215(13) C10B 0.0412(16) 0.0514(18) 0.0210(13) 0.0126(12) 0.0029(11) 0.0173(14) C11 0.0389(15) 0.0497(17) 0.0323(14) 0.0204(13) 0.0010(12) 0.0271(14) C11B 0.0458(17) 0.0477(17) 0.0181(12) -0.0020(12) 0.0031(11) 0.0145(14) C12 0.0288(13) 0.0455(16) 0.0255(13) 0.0091(12) -0.0024(10) 0.0159(12) C12B 0.069(2) 0.0403(17) 0.0294(15) -0.0020(13) 0.0065(14) 0.0268(16) C13 0.0267(12) 0.0262(12) 0.0246(12) 0.0054(10) -0.0013(10) 0.0116(10) C13B 0.0519(17) 0.0322(14) 0.0233(13) 0.0049(11) 0.0047(12) 0.0202(13) C14 0.0184(10) 0.0201(11) 0.0175(10) 0.0055(9) 0.0027(8) 0.0094(9) C14B 0.0219(11) 0.0233(11) 0.0193(11) 0.0086(9) 0.0035(9) 0.0113(9) C15 0.0196(11) 0.0274(12) 0.0223(12) 0.0051(10) 0.0038(9) 0.0055(9) C15B 0.0213(12) 0.0314(14) 0.0473(16) 0.0178(12) 0.0054(11) 0.0101(11) C16 0.0299(13) 0.0364(14) 0.0250(13) 0.0098(11) 0.0108(10) 0.0100(11) C16B 0.0228(13) 0.0524(19) 0.063(2) 0.0258(16) 0.0096(13) 0.0184(13) C17 0.0388(14) 0.0342(14) 0.0190(12) 0.0043(10) 0.0073(10) 0.0171(12) C17B 0.0438(17) 0.0484(18) 0.0512(18) 0.0178(15) 0.0099(14) 0.0353(15) C18 0.0321(13) 0.0206(12) 0.0237(12) -0.0018(10) 0.0034(10) 0.0078(10) C18B 0.0499(17) 0.0275(14) 0.0349(15) 0.0103(11) 0.0057(13) 0.0197(13) C19 0.0227(11) 0.0196(11) 0.0234(12) 0.0052(9) 0.0067(9) 0.0075(9) C19B 0.0282(12) 0.0246(12) 0.0230(12) 0.0080(10) 0.0030(10) 0.0080(10) C20 0.0159(10) 0.0214(11) 0.0174(10) 0.0039(9) 0.0010(8) 0.0070(9) C20B 0.0147(10) 0.0208(11) 0.0174(10) 0.0039(9) 0.0006(8) 0.0072(9) C21 0.0172(10) 0.0199(11) 0.0159(10) 0.0044(8) -0.0012(8) 0.0053(9) C21B 0.0172(10) 0.0232(11) 0.0174(10) 0.0052(9) 0.0016(8) 0.0099(9) C22 0.0177(10) 0.0196(11) 0.0129(10) 0.0009(8) 0.0016(8) 0.0052(9) C22B 0.0198(11) 0.0201(11) 0.0191(11) 0.0021(9) 0.0020(9) 0.0086(9) C23 0.0227(11) 0.0257(12) 0.0209(11) 0.0035(9) 0.0019(9) 0.0100(10) C23B 0.0255(12) 0.0247(12) 0.0258(12) 0.0049(10) 0.0048(10) 0.0086(10) C24 0.0297(13) 0.0323(14) 0.0299(13) -0.0031(11) -0.0001(11) 0.0182(11) C24B 0.0358(15) 0.0223(13) 0.0423(16) 0.0018(11) 0.0035(12) 0.0065(11) C25 0.0203(12) 0.0401(15) 0.0329(14) -0.0081(12) 0.0061(10) 0.0082(11) C25B 0.0462(17) 0.0317(15) 0.0331(15) -0.0082(12) -0.0046(13) 0.0129(13) C26 0.0275(13) 0.0383(15) 0.0251(13) 0.0033(11) 0.0109(10) 0.0032(11) C26B 0.0463(16) 0.0391(16) 0.0210(13) -0.0001(11) -0.0002(11) 0.0186(13) C27 0.0254(12) 0.0275(12) 0.0198(11) 0.0065(10) 0.0038(9) 0.0066(10) C27B 0.0316(13) 0.0280(13) 0.0225(12) 0.0064(10) 0.0024(10) 0.0131(11) C28 0.0179(10) 0.0182(11) 0.0151(10) 0.0048(8) 0.0014(8) 0.0027(8) C28B 0.0181(10) 0.0239(11) 0.0149(10) 0.0049(9) 0.0024(8) 0.0092(9) C29 0.0224(11) 0.0204(11) 0.0229(12) 0.0043(9) -0.0001(9) 0.0067(9) C29B 0.0211(11) 0.0220(12) 0.0253(12) 0.0004(9) 0.0014(9) 0.0062(9) C30 0.0312(13) 0.0191(12) 0.0263(13) 0.0015(10) -0.0007(10) 0.0047(10) C30B 0.0275(13) 0.0268(13) 0.0399(15) -0.0014(11) 0.0049(11) 0.0119(11) C31 0.0287(13) 0.0279(13) 0.0214(12) 0.0064(10) -0.0030(10) 0.0059(10) C31B 0.0217(12) 0.0374(15) 0.0415(16) -0.0014(12) 0.0052(11) 0.0159(11) C32 0.0225(12) 0.0286(13) 0.0282(13) 0.0072(10) -0.0032(10) 0.0085(10) C32B 0.0195(12) 0.0309(13) 0.0356(14) 0.0046(11) 0.0070(10) 0.0077(10) C33 0.0240(12) 0.0220(12) 0.0252(12) 0.0015(9) -0.0020(9) 0.0095(10) C33B 0.0214(11) 0.0217(12) 0.0284(12) 0.0067(10) 0.0046(9) 0.0075(9) _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 P1 2.1956(6) . ? Rh1 C1 2.207(2) . ? Rh1 P2B 2.2124(6) . ? Rh1 C3 2.246(2) . ? Rh1 C2 2.251(2) . ? Rh1 C7A 2.368(2) . ? Rh1 C3A 2.395(2) . ? Rh1B P2 2.1920(6) . ? Rh1B P1B 2.2081(6) . ? Rh1B C1B 2.212(2) . ? Rh1B C2B 2.234(2) . ? Rh1B C3B 2.251(2) . ? Rh1B C7AB 2.404(2) . ? Rh1B C3AB 2.431(2) . ? P1 C20 1.771(2) . ? P1 C14 1.829(2) . ? P1 C8 1.831(2) . ? P1B C20B 1.773(2) . ? P1B C8B 1.823(2) . ? P1B C14B 1.833(2) . ? P2 C21 1.771(2) . ? P2 C22 1.829(2) . ? P2 C28 1.832(2) . ? P2B C21B 1.771(2) . ? P2B C22B 1.832(2) . ? P2B C28B 1.838(2) . ? C1 C2 1.419(3) . ? C1 C7A 1.455(3) . ? C1 H1 0.9500 . ? C1B C2B 1.422(3) . ? C1B C7AB 1.450(3) . ? C1B H1B 0.9500 . ? C2 C3 1.412(3) . ? C2 H2 0.9500 . ? C2B C3B 1.404(4) . ? C2B H2B 0.9500 . ? C3 C3A 1.445(3) . ? C3 H3 0.9500 . ? C3A C4 1.399(3) . ? C3A C7A 1.438(3) . ? C3B C3AB 1.450(4) . ? C3B H3B 0.9500 . ? C3AB C4B 1.404(4) . ? C3AB C7AB 1.438(3) . ? C4 C5 1.382(4) . ? C4 H4 0.9500 . ? C4B C5B 1.372(4) . ? C4B H4B 0.9500 . ? C5 C6 1.400(4) . ? C5 H5 0.9500 . ? C5B C6B 1.397(5) . ? C5B H5B 0.9500 . ? C6 C7 1.375(4) . ? C6 H6 0.9500 . ? C6B C7B 1.381(4) . ? C6B H6B 0.9500 . ? C7 C7A 1.405(3) . ? C7 H7 0.9500 . ? C7B C7AB 1.409(4) . ? C7B H7B 0.9500 . ? C8 C9 1.391(3) . ? C8 C13 1.394(3) . ? C8B C9B 1.382(3) . ? C8B C13B 1.384(3) . ? C9 C10 1.391(4) . ? C9 H9 0.9500 . ? C9B C10B 1.393(4) . ? C9B H9B 0.9500 . ? C10 C11 1.380(4) . ? C10 H10 0.9500 . ? C10B C11B 1.367(4) . ? C10B H10B 0.9500 . ? C11 C12 1.382(4) . ? C11 H11 0.9500 . ? C11B C12B 1.389(4) . ? C11B H11B 0.9500 . ? C12 C13 1.395(3) . ? C12 H12 0.9500 . ? C12B C13B 1.387(4) . ? C12B H12B 0.9500 . ? C13 H13 0.9500 . ? C13B H13B 0.9500 . ? C14 C19 1.391(3) . ? C14 C15 1.393(3) . ? C14B C19B 1.388(3) . ? C14B C15B 1.393(3) . ? C15 C16 1.390(3) . ? C15 H15 0.9500 . ? C15B C16B 1.389(4) . ? C15B H15B 0.9500 . ? C16 C17 1.382(4) . ? C16 H16 0.9500 . ? C16B C17B 1.377(4) . ? C16B H16B 0.9500 . ? C17 C18 1.382(4) . ? C17 H17 0.9500 . ? C17B C18B 1.381(4) . ? C17B H17B 0.9500 . ? C18 C19 1.388(3) . ? C18 H18 0.9500 . ? C18B C19B 1.387(4) . ? C18B H18B 0.9500 . ? C19 H19 0.9500 . ? C19B H19B 0.9500 . ? C20 C21 1.205(3) . ? C20B C21B 1.202(3) . ? C22 C23 1.390(3) . ? C22 C27 1.395(3) . ? C22B C27B 1.387(3) . ? C22B C23B 1.397(3) . ? C23 C24 1.393(3) . ? C23 H23 0.9500 . ? C23B C24B 1.387(4) . ? C23B H23B 0.9500 . ? C24 C25 1.380(4) . ? C24 H24 0.9500 . ? C24B C25B 1.385(4) . ? C24B H24B 0.9500 . ? C25 C26 1.383(4) . ? C25 H25 0.9500 . ? C25B C26B 1.385(4) . ? C25B H25B 0.9500 . ? C26 C27 1.388(3) . ? C26 H26 0.9500 . ? C26B C27B 1.389(4) . ? C26B H26B 0.9500 . ? C27 H27 0.9500 . ? C27B H27B 0.9500 . ? C28 C29 1.390(3) . ? C28 C33 1.394(3) . ? C28B C29B 1.390(3) . ? C28B C33B 1.398(3) . ? C29 C30 1.392(3) . ? C29 H29 0.9500 . ? C29B C30B 1.389(3) . ? C29B H29B 0.9500 . ? C30 C31 1.385(4) . ? C30 H30 0.9500 . ? C30B C31B 1.389(4) . ? C30B H30B 0.9500 . ? C31 C32 1.398(3) . ? C31 H31 0.9500 . ? C31B C32B 1.379(4) . ? C31B H31B 0.9500 . ? C32 C33 1.382(3) . ? C32 H32 0.9500 . ? C32B C33B 1.386(3) . ? C32B H32B 0.9500 . ? C33 H33 0.9500 . ? C33B H33B 0.9500 . ? 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 Rh1 C1 99.23(7) . . ? P1 Rh1 P2B 95.41(2) . . ? C1 Rh1 P2B 165.13(7) . . ? P1 Rh1 C3 156.45(7) . . ? C1 Rh1 C3 62.00(9) . . ? P2B Rh1 C3 103.18(7) . . ? P1 Rh1 C2 119.87(7) . . ? C1 Rh1 C2 37.11(9) . . ? P2B Rh1 C2 130.91(7) . . ? C3 Rh1 C2 36.60(9) . . ? P1 Rh1 C7A 113.94(6) . . ? C1 Rh1 C7A 36.87(8) . . ? P2B Rh1 C7A 136.55(6) . . ? C3 Rh1 C7A 60.46(8) . . ? C2 Rh1 C7A 60.47(8) . . ? P1 Rh1 C3A 148.12(6) . . ? C1 Rh1 C3A 60.44(8) . . ? P2B Rh1 C3A 107.28(6) . . ? C3 Rh1 C3A 36.10(8) . . ? C2 Rh1 C3A 59.73(8) . . ? C7A Rh1 C3A 35.13(8) . . ? P2 Rh1B P1B 94.82(2) . . ? P2 Rh1B C1B 100.71(7) . . ? P1B Rh1B C1B 164.46(7) . . ? P2 Rh1B C2B 119.70(7) . . ? P1B Rh1B C2B 132.14(7) . . ? C1B Rh1B C2B 37.31(9) . . ? P2 Rh1B C3B 155.97(7) . . ? P1B Rh1B C3B 103.30(7) . . ? C1B Rh1B C3B 61.79(9) . . ? C2B Rh1B C3B 36.48(9) . . ? P2 Rh1B C7AB 116.76(6) . . ? P1B Rh1B C7AB 134.04(6) . . ? C1B Rh1B C7AB 36.31(9) . . ? C2B Rh1B C7AB 60.03(9) . . ? C3B Rh1B C7AB 59.80(9) . . ? P2 Rh1B C3AB 150.63(6) . . ? P1B Rh1B C3AB 105.85(6) . . ? C1B Rh1B C3AB 59.79(9) . . ? C2B Rh1B C3AB 59.36(9) . . ? C3B Rh1B C3AB 35.82(9) . . ? C7AB Rh1B C3AB 34.59(8) . . ? C20 P1 C14 102.14(10) . . ? C20 P1 C8 102.91(10) . . ? C14 P1 C8 103.03(10) . . ? C20 P1 Rh1 108.46(7) . . ? C14 P1 Rh1 122.65(7) . . ? C8 P1 Rh1 115.29(7) . . ? C20B P1B C8B 100.24(10) . . ? C20B P1B C14B 100.16(10) . . ? C8B P1B C14B 104.42(10) . . ? C20B P1B Rh1B 119.89(7) . . ? C8B P1B Rh1B 113.71(7) . . ? C14B P1B Rh1B 116.00(8) . . ? C21 P2 C22 100.86(10) . . ? C21 P2 C28 101.50(10) . . ? C22 P2 C28 102.65(10) . . ? C21 P2 Rh1B 111.22(7) . . ? C22 P2 Rh1B 122.79(7) . . ? C28 P2 Rh1B 114.98(7) . . ? C21B P2B C22B 101.78(10) . . ? C21B P2B C28B 100.18(10) . . ? C22B P2B C28B 101.81(10) . . ? C21B P2B Rh1 117.23(7) . . ? C22B P2B Rh1 119.00(8) . . ? C28B P2B Rh1 114.03(7) . . ? C2 C1 C7A 108.2(2) . . ? C2 C1 Rh1 73.13(13) . . ? C7A C1 Rh1 77.58(13) . . ? C2 C1 H1 125.9 . . ? C7A C1 H1 125.9 . . ? Rh1 C1 H1 115.5 . . ? C2B C1B C7AB 108.1(2) . . ? C2B C1B Rh1B 72.15(13) . . ? C7AB C1B Rh1B 79.06(13) . . ? C2B C1B H1B 126.0 . . ? C7AB C1B H1B 126.0 . . ? Rh1B C1B H1B 115.0 . . ? C3 C2 C1 108.2(2) . . ? C3 C2 Rh1 71.49(13) . . ? C1 C2 Rh1 69.76(13) . . ? C3 C2 H2 125.9 . . ? C1 C2 H2 125.9 . . ? Rh1 C2 H2 124.5 . . ? C3B C2B C1B 108.4(2) . . ? C3B C2B Rh1B 72.44(13) . . ? C1B C2B Rh1B 70.54(13) . . ? C3B C2B H2B 125.8 . . ? C1B C2B H2B 125.8 . . ? Rh1B C2B H2B 122.9 . . ? C2 C3 C3A 108.4(2) . . ? C2 C3 Rh1 71.91(13) . . ? C3A C3 Rh1 77.58(13) . . ? C2 C3 H3 125.8 . . ? C3A C3 H3 125.8 . . ? Rh1 C3 H3 116.7 . . ? C4 C3A C7A 119.7(2) . . ? C4 C3A C3 132.8(2) . . ? C7A C3A C3 107.5(2) . . ? C4 C3A Rh1 128.59(16) . . ? C7A C3A Rh1 71.41(12) . . ? C3 C3A Rh1 66.32(12) . . ? C2B C3B C3AB 108.5(2) . . ? C2B C3B Rh1B 71.08(13) . . ? C3AB C3B Rh1B 78.86(13) . . ? C2B C3B H3B 125.8 . . ? C3AB C3B H3B 125.8 . . ? Rh1B C3B H3B 116.3 . . ? C4B C3AB C7AB 120.2(3) . . ? C4B C3AB C3B 132.6(3) . . ? C7AB C3AB C3B 107.2(2) . . ? C4B C3AB Rh1B 128.71(17) . . ? C7AB C3AB Rh1B 71.69(13) . . ? C3B C3AB Rh1B 65.32(13) . . ? C5 C4 C3A 119.1(2) . . ? C5 C4 H4 120.5 . . ? C3A C4 H4 120.5 . . ? C5B C4B C3AB 118.7(3) . . ? C5B C4B H4B 120.7 . . ? C3AB C4B H4B 120.7 . . ? C4 C5 C6 121.0(2) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C4B C5B C6B 121.6(3) . . ? C4B C5B H5B 119.2 . . ? C6B C5B H5B 119.2 . . ? C7 C6 C5 121.6(2) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C7B C6B C5B 121.4(3) . . ? C7B C6B H6B 119.3 . . ? C5B C6B H6B 119.3 . . ? C6 C7 C7A 118.6(2) . . ? C6 C7 H7 120.7 . . ? C7A C7 H7 120.7 . . ? C7 C7A C3A 119.9(2) . . ? C7 C7A C1 133.2(2) . . ? C3A C7A C1 106.8(2) . . ? C7 C7A Rh1 123.83(16) . . ? C3A C7A Rh1 73.46(13) . . ? C1 C7A Rh1 65.55(12) . . ? C6B C7B C7AB 118.6(3) . . ? C6B C7B H7B 120.7 . . ? C7AB C7B H7B 120.7 . . ? C7B C7AB C3AB 119.4(2) . . ? C7B C7AB C1B 133.5(2) . . ? C3AB C7AB C1B 107.1(2) . . ? C7B C7AB Rh1B 125.45(17) . . ? C3AB C7AB Rh1B 73.72(13) . . ? C1B C7AB Rh1B 64.63(12) . . ? C9 C8 C13 119.0(2) . . ? C9 C8 P1 119.28(18) . . ? C13 C8 P1 121.54(17) . . ? C9B C8B C13B 119.0(2) . . ? C9B C8B P1B 120.71(19) . . ? C13B C8B P1B 119.98(18) . . ? C10 C9 C8 120.3(2) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C8B C9B C10B 120.7(3) . . ? C8B C9B H9B 119.6 . . ? C10B C9B H9B 119.6 . . ? C11 C10 C9 120.6(3) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C11B C10B C9B 120.2(3) . . ? C11B C10B H10B 119.9 . . ? C9B C10B H10B 119.9 . . ? C10 C11 C12 119.5(2) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C10B C11B C12B 119.5(3) . . ? C10B C11B H11B 120.2 . . ? C12B C11B H11B 120.2 . . ? C11 C12 C13 120.4(2) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C13B C12B C11B 120.4(3) . . ? C13B C12B H12B 119.8 . . ? C11B C12B H12B 119.8 . . ? C8 C13 C12 120.2(2) . . ? C8 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C8B C13B C12B 120.2(3) . . ? C8B C13B H13B 119.9 . . ? C12B C13B H13B 119.9 . . ? C19 C14 C15 119.4(2) . . ? C19 C14 P1 117.27(17) . . ? C15 C14 P1 123.32(17) . . ? C19B C14B C15B 119.0(2) . . ? C19B C14B P1B 117.97(18) . . ? C15B C14B P1B 122.92(18) . . ? C16 C15 C14 119.9(2) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C16B C15B C14B 119.8(3) . . ? C16B C15B H15B 120.1 . . ? C14B C15B H15B 120.1 . . ? C17 C16 C15 120.3(2) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C17B C16B C15B 120.9(3) . . ? C17B C16B H16B 119.6 . . ? C15B C16B H16B 119.6 . . ? C16 C17 C18 119.9(2) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C16B C17B C18B 119.5(3) . . ? C16B C17B H17B 120.3 . . ? C18B C17B H17B 120.3 . . ? C17 C18 C19 120.2(2) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C17B C18B C19B 120.3(3) . . ? C17B C18B H18B 119.9 . . ? C19B C18B H18B 119.9 . . ? C18 C19 C14 120.2(2) . . ? C18 C19 H19 119.9 . . ? C14 C19 H19 119.9 . . ? C18B C19B C14B 120.5(2) . . ? C18B C19B H19B 119.7 . . ? C14B C19B H19B 119.7 . . ? C21 C20 P1 165.5(2) . . ? C21B C20B P1B 179.0(2) . . ? C20 C21 P2 168.5(2) . . ? C20B C21B P2B 175.9(2) . . ? C23 C22 C27 119.6(2) . . ? C23 C22 P2 117.36(17) . . ? C27 C22 P2 123.00(18) . . ? C27B C22B C23B 119.1(2) . . ? C27B C22B P2B 123.58(18) . . ? C23B C22B P2B 117.30(17) . . ? C22 C23 C24 120.0(2) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C24B C23B C22B 120.4(2) . . ? C24B C23B H23B 119.8 . . ? C22B C23B H23B 119.8 . . ? C25 C24 C23 120.1(2) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C25B C24B C23B 119.6(3) . . ? C25B C24B H24B 120.2 . . ? C23B C24B H24B 120.2 . . ? C24 C25 C26 120.0(2) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C24B C25B C26B 120.8(3) . . ? C24B C25B H25B 119.6 . . ? C26B C25B H25B 119.6 . . ? C25 C26 C27 120.4(2) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C25B C26B C27B 119.3(3) . . ? C25B C26B H26B 120.4 . . ? C27B C26B H26B 120.4 . . ? C26 C27 C22 119.8(2) . . ? C26 C27 H27 120.1 . . ? C22 C27 H27 120.1 . . ? C22B C27B C26B 120.8(2) . . ? C22B C27B H27B 119.6 . . ? C26B C27B H27B 119.6 . . ? C29 C28 C33 119.2(2) . . ? C29 C28 P2 120.46(17) . . ? C33 C28 P2 120.00(17) . . ? C29B C28B C33B 119.2(2) . . ? C29B C28B P2B 120.94(17) . . ? C33B C28B P2B 119.68(17) . . ? C28 C29 C30 120.2(2) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C30B C29B C28B 120.1(2) . . ? C30B C29B H29B 119.9 . . ? C28B C29B H29B 119.9 . . ? C31 C30 C29 120.5(2) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C29B C30B C31B 120.5(2) . . ? C29B C30B H30B 119.8 . . ? C31B C30B H30B 119.8 . . ? C30 C31 C32 119.2(2) . . ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? C32B C31B C30B 119.5(2) . . ? C32B C31B H31B 120.2 . . ? C30B C31B H31B 120.2 . . ? C33 C32 C31 120.3(2) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C31B C32B C33B 120.5(2) . . ? C31B C32B H32B 119.7 . . ? C33B C32B H32B 119.7 . . ? C32 C33 C28 120.6(2) . . ? C32 C33 H33 119.7 . . ? C28 C33 H33 119.7 . . ? C32B C33B C28B 120.2(2) . . ? C32B C33B H33B 119.9 . . ? C28B C33B H33B 119.9 . . ? 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 C1 Rh1 P1 C20 99.55(10) . . . . ? P2B Rh1 P1 C20 -77.87(8) . . . . ? C3 Rh1 P1 C20 64.38(18) . . . . ? C2 Rh1 P1 C20 66.52(11) . . . . ? C7A Rh1 P1 C20 135.00(10) . . . . ? C3A Rh1 P1 C20 146.31(13) . . . . ? C1 Rh1 P1 C14 -141.95(11) . . . . ? P2B Rh1 P1 C14 40.63(9) . . . . ? C3 Rh1 P1 C14 -177.13(17) . . . . ? C2 Rh1 P1 C14 -174.98(11) . . . . ? C7A Rh1 P1 C14 -106.51(11) . . . . ? C3A Rh1 P1 C14 -95.19(14) . . . . ? C1 Rh1 P1 C8 -15.17(11) . . . . ? P2B Rh1 P1 C8 167.42(8) . . . . ? C3 Rh1 P1 C8 -50.34(18) . . . . ? C2 Rh1 P1 C8 -48.19(11) . . . . ? C7A Rh1 P1 C8 20.28(11) . . . . ? C3A Rh1 P1 C8 31.60(14) . . . . ? P2 Rh1B P1B C20B 32.17(9) . . . . ? C1B Rh1B P1B C20B -147.6(3) . . . . ? C2B Rh1B P1B C20B -106.14(12) . . . . ? C3B Rh1B P1B C20B -131.94(11) . . . . ? C7AB Rh1B P1B C20B 167.42(12) . . . . ? C3AB Rh1B P1B C20B -168.91(11) . . . . ? P2 Rh1B P1B C8B 150.62(8) . . . . ? C1B Rh1B P1B C8B -29.1(3) . . . . ? C2B Rh1B P1B C8B 12.31(13) . . . . ? C3B Rh1B P1B C8B -13.49(11) . . . . ? C7AB Rh1B P1B C8B -74.13(12) . . . . ? C3AB Rh1B P1B C8B -50.46(11) . . . . ? P2 Rh1B P1B C14B -88.27(8) . . . . ? C1B Rh1B P1B C14B 92.0(3) . . . . ? C2B Rh1B P1B C14B 133.42(12) . . . . ? C3B Rh1B P1B C14B 107.62(11) . . . . ? C7AB Rh1B P1B C14B 46.98(12) . . . . ? C3AB Rh1B P1B C14B 70.65(10) . . . . ? P1B Rh1B P2 C21 -73.60(8) . . . . ? C1B Rh1B P2 C21 106.33(10) . . . . ? C2B Rh1B P2 C21 71.82(11) . . . . ? C3B Rh1B P2 C21 65.55(19) . . . . ? C7AB Rh1B P2 C21 140.93(10) . . . . ? C3AB Rh1B P2 C21 151.27(14) . . . . ? P1B Rh1B P2 C22 45.78(9) . . . . ? C1B Rh1B P2 C22 -134.29(11) . . . . ? C2B Rh1B P2 C22 -168.81(11) . . . . ? C3B Rh1B P2 C22 -175.08(18) . . . . ? C7AB Rh1B P2 C22 -99.69(11) . . . . ? C3AB Rh1B P2 C22 -89.35(15) . . . . ? P1B Rh1B P2 C28 171.77(8) . . . . ? C1B Rh1B P2 C28 -8.31(11) . . . . ? C2B Rh1B P2 C28 -42.82(11) . . . . ? C3B Rh1B P2 C28 -49.09(19) . . . . ? C7AB Rh1B P2 C28 26.30(11) . . . . ? C3AB Rh1B P2 C28 36.64(15) . . . . ? P1 Rh1 P2B C21B 41.75(9) . . . . ? C1 Rh1 P2B C21B -128.3(3) . . . . ? C3 Rh1 P2B C21B -123.70(10) . . . . ? C2 Rh1 P2B C21B -96.33(12) . . . . ? C7A Rh1 P2B C21B 175.59(12) . . . . ? C3A Rh1 P2B C21B -160.93(10) . . . . ? P1 Rh1 P2B C22B -81.47(9) . . . . ? C1 Rh1 P2B C22B 108.5(3) . . . . ? C3 Rh1 P2B C22B 113.09(11) . . . . ? C2 Rh1 P2B C22B 140.45(12) . . . . ? C7A Rh1 P2B C22B 52.37(12) . . . . ? C3A Rh1 P2B C22B 75.86(10) . . . . ? P1 Rh1 P2B C28B 158.30(8) . . . . ? C1 Rh1 P2B C28B -11.7(3) . . . . ? C3 Rh1 P2B C28B -7.14(10) . . . . ? C2 Rh1 P2B C28B 20.22(12) . . . . ? C7A Rh1 P2B C28B -67.86(12) . . . . ? C3A Rh1 P2B C28B -44.37(10) . . . . ? P1 Rh1 C1 C2 -128.43(13) . . . . ? P2B Rh1 C1 C2 41.5(3) . . . . ? C3 Rh1 C1 C2 36.46(14) . . . . ? C7A Rh1 C1 C2 113.6(2) . . . . ? C3A Rh1 C1 C2 77.83(15) . . . . ? P1 Rh1 C1 C7A 117.93(13) . . . . ? P2B Rh1 C1 C7A -72.1(3) . . . . ? C3 Rh1 C1 C7A -77.18(15) . . . . ? C2 Rh1 C1 C7A -113.6(2) . . . . ? C3A Rh1 C1 C7A -35.82(13) . . . . ? P2 Rh1B C1B C2B -125.70(14) . . . . ? P1B Rh1B C1B C2B 54.0(3) . . . . ? C3B Rh1B C1B C2B 36.73(15) . . . . ? C7AB Rh1B C1B C2B 113.2(2) . . . . ? C3AB Rh1B C1B C2B 77.94(16) . . . . ? P2 Rh1B C1B C7AB 121.09(13) . . . . ? P1B Rh1B C1B C7AB -59.2(3) . . . . ? C2B Rh1B C1B C7AB -113.2(2) . . . . ? C3B Rh1B C1B C7AB -76.48(16) . . . . ? C3AB Rh1B C1B C7AB -35.27(14) . . . . ? C7A C1 C2 C3 8.9(3) . . . . ? Rh1 C1 C2 C3 -61.47(16) . . . . ? C7A C1 C2 Rh1 70.35(15) . . . . ? P1 Rh1 C2 C3 -178.56(12) . . . . ? C1 Rh1 C2 C3 118.3(2) . . . . ? P2B Rh1 C2 C3 -48.65(17) . . . . ? C7A Rh1 C2 C3 79.18(15) . . . . ? C3A Rh1 C2 C3 38.44(13) . . . . ? P1 Rh1 C2 C1 63.09(15) . . . . ? P2B Rh1 C2 C1 -167.00(11) . . . . ? C3 Rh1 C2 C1 -118.3(2) . . . . ? C7A Rh1 C2 C1 -39.17(13) . . . . ? C3A Rh1 C2 C1 -79.91(15) . . . . ? C7AB C1B C2B C3B 8.7(3) . . . . ? Rh1B C1B C2B C3B -62.95(16) . . . . ? C7AB C1B C2B Rh1B 71.65(16) . . . . ? P2 Rh1B C2B C3B -175.71(13) . . . . ? P1B Rh1B C2B C3B -45.43(18) . . . . ? C1B Rh1B C2B C3B 117.6(2) . . . . ? C7AB Rh1B C2B C3B 78.65(16) . . . . ? C3AB Rh1B C2B C3B 38.38(15) . . . . ? P2 Rh1B C2B C1B 66.72(15) . . . . ? P1B Rh1B C2B C1B -163.00(12) . . . . ? C3B Rh1B C2B C1B -117.6(2) . . . . ? C7AB Rh1B C2B C1B -38.92(14) . . . . ? C3AB Rh1B C2B C1B -79.20(16) . . . . ? C1 C2 C3 C3A -9.3(3) . . . . ? Rh1 C2 C3 C3A -69.70(16) . . . . ? C1 C2 C3 Rh1 60.38(16) . . . . ? P1 Rh1 C3 C2 3.1(3) . . . . ? C1 Rh1 C3 C2 -36.97(14) . . . . ? P2B Rh1 C3 C2 144.36(13) . . . . ? C7A Rh1 C3 C2 -79.22(15) . . . . ? C3A Rh1 C3 C2 -114.3(2) . . . . ? P1 Rh1 C3 C3A 117.43(16) . . . . ? C1 Rh1 C3 C3A 77.34(14) . . . . ? P2B Rh1 C3 C3A -101.33(13) . . . . ? C2 Rh1 C3 C3A 114.3(2) . . . . ? C7A Rh1 C3 C3A 35.08(13) . . . . ? C2 C3 C3A C4 -172.6(2) . . . . ? Rh1 C3 C3A C4 121.5(3) . . . . ? C2 C3 C3A C7A 6.2(3) . . . . ? Rh1 C3 C3A C7A -59.75(16) . . . . ? C2 C3 C3A Rh1 65.91(16) . . . . ? P1 Rh1 C3A C4 95.4(2) . . . . ? C1 Rh1 C3A C4 151.1(2) . . . . ? P2B Rh1 C3A C4 -38.0(2) . . . . ? C3 Rh1 C3A C4 -126.8(3) . . . . ? C2 Rh1 C3A C4 -165.8(3) . . . . ? C7A Rh1 C3A C4 113.5(3) . . . . ? P1 Rh1 C3A C7A -18.2(2) . . . . ? C1 Rh1 C3A C7A 37.60(14) . . . . ? P2B Rh1 C3A C7A -151.55(12) . . . . ? C3 Rh1 C3A C7A 119.7(2) . . . . ? C2 Rh1 C3A C7A 80.67(15) . . . . ? P1 Rh1 C3A C3 -137.82(13) . . . . ? C1 Rh1 C3A C3 -82.06(15) . . . . ? P2B Rh1 C3A C3 88.78(13) . . . . ? C2 Rh1 C3A C3 -38.99(14) . . . . ? C7A Rh1 C3A C3 -119.7(2) . . . . ? C1B C2B C3B C3AB -9.0(3) . . . . ? Rh1B C2B C3B C3AB -70.74(16) . . . . ? C1B C2B C3B Rh1B 61.74(16) . . . . ? P2 Rh1B C3B C2B 9.2(3) . . . . ? P1B Rh1B C3B C2B 147.13(14) . . . . ? C1B Rh1B C3B C2B -37.57(15) . . . . ? C7AB Rh1B C3B C2B -79.33(16) . . . . ? C3AB Rh1B C3B C2B -114.1(2) . . . . ? P2 Rh1B C3B C3AB 123.31(17) . . . . ? P1B Rh1B C3B C3AB -98.74(14) . . . . ? C1B Rh1B C3B C3AB 76.56(15) . . . . ? C2B Rh1B C3B C3AB 114.1(2) . . . . ? C7AB Rh1B C3B C3AB 34.80(14) . . . . ? C2B C3B C3AB C4B -173.6(3) . . . . ? Rh1B C3B C3AB C4B 120.8(3) . . . . ? C2B C3B C3AB C7AB 5.8(3) . . . . ? Rh1B C3B C3AB C7AB -59.71(16) . . . . ? C2B C3B C3AB Rh1B 65.53(16) . . . . ? P2 Rh1B C3AB C4B 98.0(3) . . . . ? P1B Rh1B C3AB C4B -35.0(3) . . . . ? C1B Rh1B C3AB C4B 151.5(3) . . . . ? C2B Rh1B C3AB C4B -165.0(3) . . . . ? C3B Rh1B C3AB C4B -125.9(3) . . . . ? C7AB Rh1B C3AB C4B 114.4(3) . . . . ? P2 Rh1B C3AB C7AB -16.4(2) . . . . ? P1B Rh1B C3AB C7AB -149.44(13) . . . . ? C1B Rh1B C3AB C7AB 37.04(14) . . . . ? C2B Rh1B C3AB C7AB 80.58(16) . . . . ? C3B Rh1B C3AB C7AB 119.7(2) . . . . ? P2 Rh1B C3AB C3B -136.08(14) . . . . ? P1B Rh1B C3AB C3B 90.88(14) . . . . ? C1B Rh1B C3AB C3B -82.64(16) . . . . ? C2B Rh1B C3AB C3B -39.10(14) . . . . ? C7AB Rh1B C3AB C3B -119.7(2) . . . . ? C7A C3A C4 C5 1.2(3) . . . . ? C3 C3A C4 C5 179.9(2) . . . . ? Rh1 C3A C4 C5 -87.9(3) . . . . ? C7AB C3AB C4B C5B 0.5(4) . . . . ? C3B C3AB C4B C5B 179.9(3) . . . . ? Rh1B C3AB C4B C5B -89.5(3) . . . . ? C3A C4 C5 C6 1.9(4) . . . . ? C3AB C4B C5B C6B 1.8(4) . . . . ? C4 C5 C6 C7 -1.8(4) . . . . ? C4B C5B C6B C7B -1.8(4) . . . . ? C5 C6 C7 C7A -1.5(4) . . . . ? C6 C7 C7A C3A 4.6(3) . . . . ? C6 C7 C7A C1 -179.0(2) . . . . ? C6 C7 C7A Rh1 94.0(3) . . . . ? C4 C3A C7A C7 -4.5(3) . . . . ? C3 C3A C7A C7 176.5(2) . . . . ? Rh1 C3A C7A C7 119.9(2) . . . . ? C4 C3A C7A C1 178.3(2) . . . . ? C3 C3A C7A C1 -0.7(2) . . . . ? Rh1 C3A C7A C1 -57.27(15) . . . . ? C4 C3A C7A Rh1 -124.5(2) . . . . ? C3 C3A C7A Rh1 56.58(15) . . . . ? C2 C1 C7A C7 178.3(2) . . . . ? Rh1 C1 C7A C7 -114.3(3) . . . . ? C2 C1 C7A C3A -5.0(2) . . . . ? Rh1 C1 C7A C3A 62.36(16) . . . . ? C2 C1 C7A Rh1 -67.34(15) . . . . ? P1 Rh1 C7A C7 54.4(2) . . . . ? C1 Rh1 C7A C7 126.9(3) . . . . ? P2B Rh1 C7A C7 -73.9(2) . . . . ? C3 Rh1 C7A C7 -151.3(2) . . . . ? C2 Rh1 C7A C7 166.4(2) . . . . ? C3A Rh1 C7A C7 -115.3(3) . . . . ? P1 Rh1 C7A C3A 169.63(11) . . . . ? C1 Rh1 C7A C3A -117.8(2) . . . . ? P2B Rh1 C7A C3A 41.41(17) . . . . ? C3 Rh1 C7A C3A -36.05(13) . . . . ? C2 Rh1 C7A C3A -78.36(15) . . . . ? P1 Rh1 C7A C1 -72.58(14) . . . . ? P2B Rh1 C7A C1 159.20(11) . . . . ? C3 Rh1 C7A C1 81.75(15) . . . . ? C2 Rh1 C7A C1 39.43(14) . . . . ? C3A Rh1 C7A C1 117.8(2) . . . . ? C5B C6B C7B C7AB -0.5(4) . . . . ? C6B C7B C7AB C3AB 2.7(4) . . . . ? C6B C7B C7AB C1B -179.7(3) . . . . ? C6B C7B C7AB Rh1B 93.1(3) . . . . ? C4B C3AB C7AB C7B -2.8(3) . . . . ? C3B C3AB C7AB C7B 177.7(2) . . . . ? Rh1B C3AB C7AB C7B 121.9(2) . . . . ? C4B C3AB C7AB C1B 179.1(2) . . . . ? C3B C3AB C7AB C1B -0.5(3) . . . . ? Rh1B C3AB C7AB C1B -56.19(15) . . . . ? C4B C3AB C7AB Rh1B -124.7(2) . . . . ? C3B C3AB C7AB Rh1B 55.74(15) . . . . ? C2B C1B C7AB C7B 177.3(3) . . . . ? Rh1B C1B C7AB C7B -115.8(3) . . . . ? C2B C1B C7AB C3AB -5.0(3) . . . . ? Rh1B C1B C7AB C3AB 61.97(16) . . . . ? C2B C1B C7AB Rh1B -66.96(15) . . . . ? P2 Rh1B C7AB C7B 56.2(2) . . . . ? P1B Rh1B C7AB C7B -72.0(2) . . . . ? C1B Rh1B C7AB C7B 126.7(3) . . . . ? C2B Rh1B C7AB C7B 166.7(3) . . . . ? C3B Rh1B C7AB C7B -150.9(3) . . . . ? C3AB Rh1B C7AB C7B -114.8(3) . . . . ? P2 Rh1B C7AB C3AB 171.08(12) . . . . ? P1B Rh1B C7AB C3AB 42.87(17) . . . . ? C1B Rh1B C7AB C3AB -118.5(2) . . . . ? C2B Rh1B C7AB C3AB -78.45(16) . . . . ? C3B Rh1B C7AB C3AB -36.04(15) . . . . ? P2 Rh1B C7AB C1B -70.45(15) . . . . ? P1B Rh1B C7AB C1B 161.34(12) . . . . ? C2B Rh1B C7AB C1B 40.02(14) . . . . ? C3B Rh1B C7AB C1B 82.43(16) . . . . ? C3AB Rh1B C7AB C1B 118.5(2) . . . . ? C20 P1 C8 C9 157.27(19) . . . . ? C14 P1 C8 C9 51.3(2) . . . . ? Rh1 P1 C8 C9 -84.86(19) . . . . ? C20 P1 C8 C13 -28.0(2) . . . . ? C14 P1 C8 C13 -133.9(2) . . . . ? Rh1 P1 C8 C13 89.89(19) . . . . ? C20B P1B C8B C9B -142.3(2) . . . . ? C14B P1B C8B C9B -38.9(2) . . . . ? Rh1B P1B C8B C9B 88.5(2) . . . . ? C20B P1B C8B C13B 44.4(2) . . . . ? C14B P1B C8B C13B 147.8(2) . . . . ? Rh1B P1B C8B C13B -84.8(2) . . . . ? C13 C8 C9 C10 -0.4(4) . . . . ? P1 C8 C9 C10 174.4(2) . . . . ? C13B C8B C9B C10B 0.0(4) . . . . ? P1B C8B C9B C10B -173.4(2) . . . . ? C8 C9 C10 C11 -0.2(4) . . . . ? C8B C9B C10B C11B 0.1(4) . . . . ? C9 C10 C11 C12 0.5(5) . . . . ? C9B C10B C11B C12B -0.1(5) . . . . ? C10 C11 C12 C13 -0.2(4) . . . . ? C10B C11B C12B C13B 0.2(5) . . . . ? C9 C8 C13 C12 0.7(4) . . . . ? P1 C8 C13 C12 -174.05(19) . . . . ? C11 C12 C13 C8 -0.4(4) . . . . ? C9B C8B C13B C12B 0.0(4) . . . . ? P1B C8B C13B C12B 173.5(2) . . . . ? C11B C12B C13B C8B -0.1(5) . . . . ? C20 P1 C14 C19 157.03(18) . . . . ? C8 P1 C14 C19 -96.45(19) . . . . ? Rh1 P1 C14 C19 35.5(2) . . . . ? C20 P1 C14 C15 -22.7(2) . . . . ? C8 P1 C14 C15 83.8(2) . . . . ? Rh1 P1 C14 C15 -144.17(17) . . . . ? C20B P1B C14B C19B -149.32(19) . . . . ? C8B P1B C14B C19B 107.23(19) . . . . ? Rh1B P1B C14B C19B -18.7(2) . . . . ? C20B P1B C14B C15B 27.7(2) . . . . ? C8B P1B C14B C15B -75.8(2) . . . . ? Rh1B P1B C14B C15B 158.29(19) . . . . ? C19 C14 C15 C16 0.0(3) . . . . ? P1 C14 C15 C16 179.76(19) . . . . ? C19B C14B C15B C16B 2.2(4) . . . . ? P1B C14B C15B C16B -174.8(2) . . . . ? C14 C15 C16 C17 -0.4(4) . . . . ? C14B C15B C16B C17B -1.4(5) . . . . ? C15 C16 C17 C18 0.3(4) . . . . ? C15B C16B C17B C18B -0.4(5) . . . . ? C16 C17 C18 C19 0.0(4) . . . . ? C16B C17B C18B C19B 1.3(5) . . . . ? C17 C18 C19 C14 -0.3(4) . . . . ? C15 C14 C19 C18 0.3(3) . . . . ? P1 C14 C19 C18 -179.43(18) . . . . ? C17B C18B C19B C14B -0.4(4) . . . . ? C15B C14B C19B C18B -1.3(4) . . . . ? P1B C14B C19B C18B 175.82(19) . . . . ? C14 P1 C20 C21 -100.6(8) . . . . ? C8 P1 C20 C21 152.8(8) . . . . ? Rh1 P1 C20 C21 30.2(8) . . . . ? P1 C20 C21 P2 30.2(17) . . . . ? C22 P2 C21 C20 -63.9(10) . . . . ? C28 P2 C21 C20 -169.3(10) . . . . ? Rh1B P2 C21 C20 67.9(11) . . . . ? C21 P2 C22 C23 161.19(18) . . . . ? C28 P2 C22 C23 -94.27(18) . . . . ? Rh1B P2 C22 C23 37.0(2) . . . . ? C21 P2 C22 C27 -19.6(2) . . . . ? C28 P2 C22 C27 84.9(2) . . . . ? Rh1B P2 C22 C27 -143.80(16) . . . . ? C21B P2B C22B C27B 10.2(2) . . . . ? C28B P2B C22B C27B -93.0(2) . . . . ? Rh1 P2B C22B C27B 140.72(18) . . . . ? C21B P2B C22B C23B -170.23(18) . . . . ? C28B P2B C22B C23B 86.59(19) . . . . ? Rh1 P2B C22B C23B -39.7(2) . . . . ? C27 C22 C23 C24 -0.5(3) . . . . ? P2 C22 C23 C24 178.74(18) . . . . ? C27B C22B C23B C24B 3.0(4) . . . . ? P2B C22B C23B C24B -176.6(2) . . . . ? C22 C23 C24 C25 -0.7(4) . . . . ? C22B C23B C24B C25B -3.0(4) . . . . ? C23 C24 C25 C26 1.2(4) . . . . ? C23B C24B C25B C26B 0.4(4) . . . . ? C24 C25 C26 C27 -0.5(4) . . . . ? C24B C25B C26B C27B 2.2(4) . . . . ? C25 C26 C27 C22 -0.8(4) . . . . ? C23 C22 C27 C26 1.2(3) . . . . ? P2 C22 C27 C26 -177.96(18) . . . . ? C23B C22B C27B C26B -0.4(4) . . . . ? P2B C22B C27B C26B 179.1(2) . . . . ? C25B C26B C27B C22B -2.1(4) . . . . ? C21 P2 C28 C29 150.67(19) . . . . ? C22 P2 C28 C29 46.6(2) . . . . ? Rh1B P2 C28 C29 -89.18(19) . . . . ? C21 P2 C28 C33 -36.2(2) . . . . ? C22 P2 C28 C33 -140.27(19) . . . . ? Rh1B P2 C28 C33 83.93(19) . . . . ? C21B P2B C28B C29B 35.3(2) . . . . ? C22B P2B C28B C29B 139.72(19) . . . . ? Rh1 P2B C28B C29B -90.82(19) . . . . ? C21B P2B C28B C33B -149.88(19) . . . . ? C22B P2B C28B C33B -45.4(2) . . . . ? Rh1 P2B C28B C33B 84.03(19) . . . . ? C33 C28 C29 C30 -0.7(3) . . . . ? P2 C28 C29 C30 172.49(18) . . . . ? C33B C28B C29B C30B -0.1(4) . . . . ? P2B C28B C29B C30B 174.8(2) . . . . ? C28 C29 C30 C31 -0.6(4) . . . . ? C28B C29B C30B C31B -0.2(4) . . . . ? C29 C30 C31 C32 1.8(4) . . . . ? C29B C30B C31B C32B -0.1(4) . . . . ? C30 C31 C32 C33 -1.8(4) . . . . ? C30B C31B C32B C33B 0.7(4) . . . . ? C31 C32 C33 C28 0.5(4) . . . . ? C29 C28 C33 C32 0.7(4) . . . . ? P2 C28 C33 C32 -172.48(19) . . . . ? C31B C32B C33B C28B -1.0(4) . . . . ? C29B C28B C33B C32B 0.7(4) . . . . ? P2B C28B C33B C32B -174.24(19) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.261 _refine_diff_density_min -0.654 _refine_diff_density_rms 0.078 _exptl_crystal_recrystallization_method 'Diffusion of hexane into a solution in benzene at rt.'