# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2000 # CCDC Number: 440/178 #======================================================================= data_global #======================================================================= _audit_creation_date 11-01-99 # 1. SUBMISSION DETAILS _publ_contact_author_name # Name of author for correspondance ; Prof. Jean Fischer ; _publ_contact_author_address # Address of author for correspondance ; Universite Louis Pasteur Laboratoire de Cristallochimie et de Chimie Structurale UMR 7513 4, rue Blaise Pascal 67070 Strasbourg cedex France ; _publ_contact_author_phone '+33 (0)3 88 41 60 58' _publ_contact_author_fax '+33 (0)3 88 41 53 63' _publ_contact_author_email fischer@chimie.u-strasbg.fr _publ_requested_journal 'NJC' _publ_contact_letter ; ; _publ_requested_category FM #======================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Oxidative Addition of Iodine, Iodomethane and Iodobenzene to the Rhodium Phosphino Enolate Complex (Rh(Ph2PCH...C(...O)Ph)(CO)(PPh3)) and Carbon Monoxide Insertion into the resulting Rh-Carbon Bond of (Rh(Ph2PCH...C(...O)Ph)Me(I)(CO)(PPh3)). ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Braunstein Pierre' ; Laboratoire de Chimie de Coordination UMR 7513 Universite Louis Pasteur 4, rue Blaise Pascal 67070 Strasbourg cedex France ; 'Fischer Jean' ; Laboratoire de Cristallochimie et de Chimie Structurale UMR 7513 Universite Louis Pasteur 4, rue Blaise Pascal 67070 Strasbourg cedex France ; 'Chauvin Yves' ; Institut Francais du Petrole BP 311 92506 Rueil-Malmaison France ; 'Olivier Helene' ; Institut Francais du Petrole BP 311 92506 Rueil-Malmaison France ; 'Strohmann Carsten' ; Institut fur Anorganishe Chemie Universitat Wurtzburg Am Hubland 97074 Wurtzburg Germany ; 'Toronto Dawn V.' ; Institut Francais du Petrole BP 311 92506 Rueil-Malmaison France ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. OpenMoleN, Interactive Intelligent Structure solution (1997) Nonius B.V., Delft, The Netherlands. North, A.C.T., Phillips, D.C., Mathews, F.S. (1968). Acta Cryst., A24, 351-359. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #======================================================================= data_st732 #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C40 H34 I O2 P2 Rh' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C40 H34 I O2 P2 Rh' _chemical_formula_weight 838.47 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 I ? -0.726 1.812 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 Rh ? -1.287 0.919 International_Tables_Vol_IV_Table_2.3.1 #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 12.054(3) _cell_length_b 24.130(3) _cell_length_c 12.213(3) _cell_angle_alpha 90 _cell_angle_beta 92.25(2) _cell_angle_gamma 90 _cell_volume 3549(2) _cell_formula_units_Z 4 _cell_measurement_temperature 294 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 18.0 _cell_measurement_theta_max 19.5 _cell_special_details ; ? ; _exptl_crystal_description prism _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.57 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 1.475 _exptl_absorpt_correction_type psi_scan_(North,_Phillips,_Mathews,_1968) _exptl_absorpt_correction_T_min 0.7414 _exptl_absorpt_correction_T_max 1.0000 #======================================================================= # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 294 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 0 -6 1 1 -5 2 4 -1 _diffrn_reflns_number 8297 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7930 _reflns_number_gt 4991 _reflns_threshold_expression >3.0\s(I) _computing_data_collection 'CAD4_(Enraf-Nonius,_1994)' _computing_cell_refinement CAD4_(Enraf-Nonius,_1994) _computing_data_reduction 'process_OpenMoleN_(_1997)' _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #======================================================================= # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4991 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.091 _refine_ls_R_factor_gt 0.039 _refine_ls_wR_factor_all 0.149 _refine_ls_wR_factor_ref 0.055 _refine_ls_goodness_of_fit_all 2.970 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_shift/su_max 0.003 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 1.259 _refine_diff_density_min -0.215 #======================================================================= # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol RH 0.06662(3) 0.10259(2) 0.26465(3) 0.0355(2) Uani ? ? Rh O1 0.0651(3) 0.1176(2) 0.4322(2) 0.045(2) Uani ? ? O C1 -0.0298(4) 0.1314(2) 0.4742(4) 0.044(3) Uani ? ? C C2 -0.1278(4) 0.1339(3) 0.4141(4) 0.049(3) Uani ? ? C C3 -0.0237(4) 0.1433(2) 0.5940(4) 0.046(3) Uani ? ? C C4 0.0513(5) 0.1154(2) 0.6622(4) 0.053(3) Uani ? ? C C5 0.0547(6) 0.1255(3) 0.7737(5) 0.066(4) Uani ? ? C C6 -0.0150(6) 0.1649(3) 0.8194(5) 0.070(4) Uani ? ? C C7 -0.0877(5) 0.1928(3) 0.7505(4) 0.066(4) Uani ? ? C C8 -0.0935(5) 0.1827(3) 0.6392(4) 0.059(3) Uani ? ? C P1 -0.1229(1) 0.11630(6) 0.2761(1) 0.0426(7) Uani ? ? P C9 -0.1940(4) 0.1682(2) 0.1917(4) 0.045(3) Uani ? ? C C10 -0.2604(6) 0.2074(3) 0.2382(5) 0.077(4) Uani ? ? C C11 -0.3238(7) 0.2427(3) 0.1736(6) 0.103(5) Uani ? ? C C12 -0.3173(5) 0.2424(3) 0.0616(5) 0.063(3) Uani ? ? C C13 -0.2483(5) 0.2054(3) 0.0149(5) 0.063(3) Uani ? ? C C14 -0.1865(5) 0.1691(3) 0.0797(5) 0.064(3) Uani ? ? C C15 -0.2126(4) 0.0560(2) 0.2495(4) 0.043(2) Uani ? ? C C16 -0.2250(6) 0.0314(3) 0.1473(5) 0.071(4) Uani ? ? C C17 -0.2964(6) -0.0127(3) 0.1295(5) 0.079(4) Uani ? ? C C18 -0.3595(5) -0.0314(3) 0.2122(6) 0.073(4) Uani ? ? C C19 -0.3485(6) -0.0077(3) 0.3121(5) 0.088(4) Uani ? ? C C20 -0.2763(5) 0.0361(3) 0.3337(5) 0.070(4) Uani ? ? C C21 0.0378(5) 0.0203(2) 0.3128(5) 0.055(3) Uani ? ? C C22 0.0560(4) 0.0825(2) 0.1206(4) 0.047(3) Uani ? ? C O2 0.0474(4) 0.0672(2) 0.0339(3) 0.070(3) Uani ? ? O P2 0.2655(1) 0.08963(5) 0.2643(1) 0.0393(6) Uani ? ? P C23 0.3364(4) 0.1103(2) 0.1409(4) 0.045(3) Uani ? ? C C24 0.2906(5) 0.1476(3) 0.0655(5) 0.062(3) Uani ? ? C C25 0.3518(6) 0.1658(3) -0.0213(5) 0.074(4) Uani ? ? C C26 0.4546(6) 0.1473(3) -0.0350(5) 0.081(4) Uani ? ? C C27 0.4995(5) 0.1082(4) 0.0356(6) 0.081(4) Uani ? ? C C28 0.4423(5) 0.0901(3) 0.1233(6) 0.073(4) Uani ? ? C C29 0.3047(4) 0.0166(2) 0.2762(4) 0.041(2) Uani ? ? C C30 0.3559(5) -0.0064(2) 0.3684(5) 0.056(3) Uani ? ? C C31 0.3760(5) -0.0625(2) 0.3767(5) 0.061(3) Uani ? ? C C32 0.3450(5) -0.0967(3) 0.2911(6) 0.069(4) Uani ? ? C C33 0.2931(6) -0.0753(3) 0.1998(5) 0.067(4) Uani ? ? C C34 0.2728(5) -0.0191(2) 0.1895(5) 0.059(3) Uani ? ? C C35 0.3414(4) 0.1249(2) 0.3759(5) 0.051(3) Uani ? ? C C36 0.4277(6) 0.1605(3) 0.3591(6) 0.078(4) Uani ? ? C C37 0.4810(7) 0.1874(3) 0.4459(7) 0.108(5) Uani ? ? C C38 0.4460(7) 0.1802(3) 0.5490(6) 0.102(4) Uani ? ? C C39 0.3593(6) 0.1452(3) 0.5701(5) 0.097(4) Uani ? ? C C40 0.3069(5) 0.1172(3) 0.4802(5) 0.067(3) Uani ? ? C I 0.09763(3) 0.21656(1) 0.24651(3) 0.0514(2) Uani ? ? I H1 -0.1951 0.1447 0.4460 0.0667 Uiso calc C2 H H2 0.1007 0.0892 0.6324 0.0704 Uiso calc C4 H H3 0.1052 0.1054 0.8202 0.0887 Uiso calc C5 H H4 -0.0120 0.1721 0.8959 0.0942 Uiso calc C6 H H5 -0.1354 0.2198 0.7799 0.0873 Uiso calc C7 H H6 -0.1451 0.2025 0.5932 0.0766 Uiso calc C8 H H7 -0.2623 0.2102 0.3157 0.1009 Uiso calc C10 H H8 -0.3731 0.2677 0.2069 0.1351 Uiso calc C11 H H9 -0.3601 0.2675 0.0176 0.0828 Uiso calc C12 H H10 -0.2427 0.2046 -0.0624 0.0842 Uiso calc C13 H H11 -0.1373 0.1441 0.0461 0.0825 Uiso calc C14 H H12 -0.1835 0.0450 0.0885 0.0927 Uiso calc C16 H H13 -0.3018 -0.0299 0.0596 0.1049 Uiso calc C17 H H14 -0.4106 -0.0609 0.1995 0.0959 Uiso calc C18 H H15 -0.3916 -0.0214 0.3696 0.1166 Uiso calc C19 H H16 -0.2705 0.0523 0.4047 0.0924 Uiso calc C20 H H17 0.1061 0.0006 0.3167 0.0733 Uiso calc C21 H H18 0.0058 0.0201 0.3826 0.0733 Uiso calc C21 H H19 -0.0115 0.0030 0.2607 0.0733 Uiso calc C21 H H20 0.2170 0.1607 0.0733 0.0805 Uiso calc C24 H H21 0.3200 0.1918 -0.0718 0.0981 Uiso calc C25 H H22 0.4967 0.1611 -0.0932 0.1053 Uiso calc C26 H H23 0.5711 0.0936 0.0233 0.1113 Uiso calc C27 H H24 0.4750 0.0636 0.1723 0.1010 Uiso calc C28 H H25 0.3780 0.0170 0.4279 0.0725 Uiso calc C30 H H26 0.4110 -0.0775 0.4412 0.0806 Uiso calc C31 H H27 0.3597 -0.1353 0.2956 0.0939 Uiso calc C32 H H28 0.2703 -0.0994 0.1418 0.0929 Uiso calc C33 H H29 0.2377 -0.0047 0.1246 0.0774 Uiso calc C34 H H30 0.4511 0.1668 0.2867 0.1047 Uiso calc C36 H H31 0.5423 0.2111 0.4334 0.1557 Uiso calc C37 H H32 0.4820 0.1997 0.6079 0.1416 Uiso calc C38 H H33 0.3353 0.1399 0.6426 0.1304 Uiso calc C39 H H34 0.2469 0.0927 0.4924 0.0878 Uiso calc C40 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol RH 0.0339(2) 0.0347(2) 0.0382(2) 0.0015(2) 0.0016(1) 0.0017(2) Rh O1 0.044(2) 0.055(2) 0.038(2) 0.002(2) 0.002(1) -0.001(2) O C1 0.055(3) 0.046(3) 0.033(2) -0.001(2) 0.001(2) 0.001(2) C C2 0.043(3) 0.073(4) 0.039(2) -0.001(3) 0.008(2) -0.005(2) C C3 0.053(3) 0.045(3) 0.041(2) -0.010(2) 0.004(2) -0.002(2) C C4 0.068(3) 0.046(3) 0.048(3) -0.000(3) 0.002(3) 0.005(2) C C5 0.090(4) 0.061(3) 0.053(3) -0.016(3) -0.002(3) 0.013(3) C C6 0.093(4) 0.080(4) 0.046(3) -0.022(4) 0.017(3) -0.013(3) C C7 0.079(4) 0.071(4) 0.052(3) -0.006(3) 0.017(3) -0.013(3) C C8 0.059(3) 0.065(4) 0.054(3) -0.006(3) 0.012(3) -0.007(3) C P1 0.0371(6) 0.0497(7) 0.0418(6) 0.0005(6) 0.0034(5) -0.0025(6) P C9 0.032(2) 0.052(3) 0.054(3) 0.001(2) -0.001(2) -0.001(2) C C10 0.092(4) 0.079(4) 0.063(3) 0.043(3) 0.014(3) -0.007(3) C C11 0.123(5) 0.107(5) 0.082(4) 0.069(4) 0.010(4) -0.012(4) C C12 0.061(3) 0.065(4) 0.063(3) 0.015(3) -0.011(3) 0.006(3) C C13 0.075(4) 0.071(4) 0.048(3) 0.011(3) -0.006(3) 0.016(3) C C14 0.059(3) 0.073(4) 0.059(3) 0.022(3) 0.016(3) 0.003(3) C C15 0.035(2) 0.049(3) 0.047(2) -0.000(2) 0.002(2) 0.003(2) C C16 0.081(4) 0.076(4) 0.058(3) -0.025(3) 0.012(3) -0.002(3) C C17 0.103(5) 0.072(4) 0.068(4) -0.031(4) 0.007(4) -0.018(3) C C18 0.062(3) 0.073(4) 0.085(4) -0.031(3) -0.005(3) -0.002(3) C C19 0.081(4) 0.117(5) 0.072(4) -0.058(3) 0.012(3) 0.001(4) C C20 0.062(3) 0.094(5) 0.057(3) -0.020(3) 0.008(3) 0.003(3) C C21 0.057(3) 0.041(3) 0.071(3) 0.002(3) 0.002(3) 0.006(3) C C22 0.042(3) 0.057(3) 0.044(2) 0.002(2) 0.005(2) -0.000(2) C O2 0.080(3) 0.100(3) 0.043(2) 0.006(3) 0.004(2) -0.014(2) O P2 0.0364(6) 0.0380(7) 0.0437(6) 0.0017(5) -0.0005(5) 0.0022(5) P C23 0.040(3) 0.045(3) 0.051(3) -0.005(2) 0.005(2) 0.001(2) C C24 0.063(3) 0.065(4) 0.058(3) 0.009(3) 0.012(3) 0.016(3) C C25 0.095(5) 0.074(4) 0.058(3) -0.002(4) 0.014(3) 0.012(3) C C26 0.074(4) 0.100(5) 0.071(4) -0.029(4) 0.028(3) 0.002(4) C C27 0.052(3) 0.119(6) 0.088(4) -0.007(4) 0.026(3) 0.014(4) C C28 0.042(3) 0.087(5) 0.105(5) 0.004(3) 0.015(3) 0.023(4) C C29 0.034(2) 0.038(2) 0.053(3) 0.001(2) 0.009(2) 0.003(2) C C30 0.053(3) 0.056(3) 0.058(3) 0.012(3) 0.004(2) 0.002(3) C C31 0.069(4) 0.045(3) 0.073(3) 0.015(3) 0.009(3) 0.009(3) C C32 0.070(4) 0.044(3) 0.104(4) 0.013(3) 0.027(3) 0.010(3) C C33 0.079(4) 0.041(3) 0.094(4) 0.002(3) 0.006(4) -0.020(3) C C34 0.067(3) 0.048(3) 0.064(3) 0.007(3) 0.001(3) -0.006(3) C C35 0.049(3) 0.042(3) 0.064(3) 0.011(2) -0.017(2) -0.004(3) C C36 0.094(5) 0.061(4) 0.084(4) -0.020(3) -0.031(4) 0.011(3) C C37 0.128(5) 0.059(4) 0.165(6) -0.023(4) -0.085(4) 0.012(5) C C38 0.136(5) 0.066(4) 0.118(4) 0.021(4) -0.083(3) -0.037(3) C C39 0.112(5) 0.106(5) 0.078(3) 0.054(4) -0.055(3) -0.045(3) C C40 0.057(3) 0.077(4) 0.067(3) 0.021(3) -0.018(3) -0.022(3) C I 0.0524(2) 0.0376(2) 0.0690(2) 0.0017(2) -0.0036(2) 0.0037(2) I # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag RH O1 2.079(3) . . ? RH P1 2.318(1) . . ? RH C21 2.104(6) . . ? RH C22 1.824(5) . . ? RH P2 2.418(1) . . ? RH I 2.7854(5) . . ? O1 C1 1.314(6) . . ? C1 C2 1.368(7) . . ? C1 C3 1.490(7) . . ? C2 P1 1.741(5) . . ? C3 C4 1.381(8) . . ? C3 C8 1.397(8) . . ? C4 C5 1.383(8) . . ? C5 C6 1.40(1) . . ? C6 C7 1.37(1) . . ? C7 C8 1.380(8) . . ? P1 C9 1.816(6) . . ? P1 C15 1.834(6) . . ? C9 C10 1.376(8) . . ? C9 C14 1.375(8) . . ? C10 C11 1.37(1) . . ? C11 C12 1.373(9) . . ? C12 C13 1.360(9) . . ? C13 C14 1.379(8) . . ? C15 C16 1.386(8) . . ? C15 C20 1.393(8) . . ? C16 C17 1.379(9) . . ? C17 C18 1.364(9) . . ? C18 C19 1.35(1) . . ? C19 C20 1.388(9) . . ? C22 O2 1.123(6) . . ? P2 C23 1.830(5) . . ? P2 C29 1.829(5) . . ? P2 C35 1.822(6) . . ? C23 C24 1.387(8) . . ? C23 C28 1.392(8) . . ? C24 C25 1.386(9) . . ? C25 C26 1.33(1) . . ? C26 C27 1.37(1) . . ? C27 C28 1.368(9) . . ? C29 C30 1.380(7) . . ? C29 C34 1.406(8) . . ? C30 C31 1.379(8) . . ? C31 C32 1.37(1) . . ? C32 C33 1.36(1) . . ? C33 C34 1.383(9) . . ? C35 C36 1.371(9) . . ? C35 C40 1.368(9) . . ? C36 C37 1.38(1) . . ? C37 C38 1.35(1) . . ? C38 C39 1.38(1) . . ? C39 C40 1.416(9) . . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 RH P1 82.5(1) . . . ? O1 RH C21 83.2(2) . . . ? O1 RH C22 173.0(2) . . . ? O1 RH P2 94.1(1) . . . ? O1 RH I 85.0(1) . . . ? P1 RH C21 86.8(2) . . . ? P1 RH C22 93.7(2) . . . ? P1 RH P2 176.53(5) . . . ? P1 RH I 89.98(4) . . . ? C21 RH C22 90.7(2) . . . ? C21 RH P2 93.0(2) . . . ? C21 RH I 168.1(2) . . . ? C22 RH P2 89.8(2) . . . ? C22 RH I 101.0(2) . . . ? P2 RH I 89.51(3) . . . ? O1 C1 C2 123.3(4) . . . ? O1 C1 C3 115.0(4) . . . ? C2 C1 C3 121.7(5) . . . ? C1 C2 P1 116.5(4) . . . ? C1 C3 C4 120.2(5) . . . ? C1 C3 C8 120.8(5) . . . ? C4 C3 C8 118.9(5) . . . ? C3 C4 C5 120.0(6) . . . ? C4 C5 C6 121.2(6) . . . ? C5 C6 C7 118.0(6) . . . ? C6 C7 C8 121.7(6) . . . ? C3 C8 C7 120.1(6) . . . ? C2 P1 C9 110.4(3) . . . ? C2 P1 C15 108.8(3) . . . ? C9 P1 C15 100.6(2) . . . ? P1 C9 C10 120.6(5) . . . ? P1 C9 C14 121.9(4) . . . ? C10 C9 C14 117.5(5) . . . ? C9 C10 C11 120.6(6) . . . ? C10 C11 C12 121.2(6) . . . ? C11 C12 C13 118.7(6) . . . ? C12 C13 C14 120.1(6) . . . ? C9 C14 C13 121.7(6) . . . ? P1 C15 C16 122.8(4) . . . ? P1 C15 C20 118.7(4) . . . ? C16 C15 C20 118.3(5) . . . ? C15 C16 C17 121.1(6) . . . ? C16 C17 C18 120.1(6) . . . ? C17 C18 C19 119.4(6) . . . ? C18 C19 C20 122.3(6) . . . ? C15 C20 C19 118.8(6) . . . ? C23 P2 C29 101.6(2) . . . ? C23 P2 C35 104.6(3) . . . ? C29 P2 C35 105.7(2) . . . ? P2 C23 C24 122.5(4) . . . ? P2 C23 C28 119.5(5) . . . ? C24 C23 C28 117.9(5) . . . ? C23 C24 C25 120.2(6) . . . ? C24 C25 C26 121.0(7) . . . ? C25 C26 C27 119.7(6) . . . ? C26 C27 C28 120.8(7) . . . ? C23 C28 C27 120.2(7) . . . ? P2 C29 C30 123.9(4) . . . ? P2 C29 C34 117.9(4) . . . ? C30 C29 C34 118.0(5) . . . ? C29 C30 C31 121.8(6) . . . ? C30 C31 C32 119.5(6) . . . ? C31 C32 C33 120.0(6) . . . ? C32 C33 C34 121.5(6) . . . ? C29 C34 C33 119.3(6) . . . ? P2 C35 C36 122.8(5) . . . ? P2 C35 C40 118.1(5) . . . ? C36 C35 C40 119.0(6) . . . ? C35 C36 C37 120.8(8) . . . ? C36 C37 C38 120.1(9) . . . ? C37 C38 C39 121.3(7) . . . ? C38 C39 C40 117.8(8) . . . ? C35 C40 C39 121.0(8) . . . ? #======================================================================= data_st799 #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C45 H36 I O2 P2 Rh' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C45 H36 I O2 P2 Rh' _chemical_formula_weight 900.54 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 I ? -0.726 1.812 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 Rh ? -1.287 0.919 International_Tables_Vol_IV_Table_2.3.1 #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall ' P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,-y,1/2+z 1/2+x,1/2-y,+z 1/2-x,1/2+y,1/2+z _cell_length_a 17.887(5) _cell_length_b 18.538(5) _cell_length_c 11.515(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3818(3) _cell_formula_units_Z 4 _cell_measurement_temperature 294 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 18.0 _cell_measurement_theta_max 19.5 _cell_special_details ; ? ; _exptl_crystal_description prism _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.57 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 1.377 _exptl_absorpt_correction_type psi_scan_(North,_Phillips,_Mathews,_1968) _exptl_absorpt_correction_T_min 0.9622 _exptl_absorpt_correction_T_max 1.0000 #======================================================================= # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 294 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 7 4 0 3 2 1 1 3 1 _diffrn_reflns_number 6390 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 30.41 _reflns_number_total 6390 _reflns_number_gt 5141 _reflns_threshold_expression >3.0\s(I) _computing_data_collection 'CAD4_(Enraf-Nonius,_1994)' _computing_cell_refinement CAD4_(Enraf-Nonius,_1994) _computing_data_reduction 'process_OpenMoleN_(_1997)' _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #======================================================================= # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0009 Fo^4^)' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack -0.08(3) _refine_ls_number_reflns 5141 _refine_ls_number_parameters 459 _refine_ls_number_restraints 1 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39,876-881' _refine_ls_R_factor_all 0.038 _refine_ls_R_factor_gt 0.022 _refine_ls_wR_factor_all 0.037 _refine_ls_wR_factor_ref 0.027 _refine_ls_goodness_of_fit_all 1.408 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_shift/su_max 0.004 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.254 _refine_diff_density_min -0.095 #======================================================================= # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol RH 0.23957(1) 0.95994(1) 0.7232 0.02737(7) Uani ? ? Rh I 0.36884(1) 0.90898(1) 0.82829(3) 0.04346(9) Uani ? ? I P1 0.29142(4) 1.07488(4) 0.71033(7) 0.0310(3) Uani ? ? P C1 0.3347(2) 1.0651(2) 0.5751(3) 0.038(1) Uani ? ? C C2 0.3217(2) 1.0023(2) 0.5167(3) 0.033(1) Uani ? ? C O1 0.2834(1) 0.9485(1) 0.5596(2) 0.033(1) Uani ? ? O C3 0.3596(2) 1.1035(1) 0.8176(3) 0.036(1) Uani ? ? C C4 0.3405(2) 1.1173(2) 0.9315(3) 0.046(2) Uani ? ? C C5 0.3941(3) 1.1375(2) 1.0116(3) 0.053(2) Uani ? ? C C6 0.4677(2) 1.1427(2) 0.9783(4) 0.057(2) Uani ? ? C C7 0.4874(2) 1.1287(2) 0.8666(4) 0.056(2) Uani ? ? C C8 0.4347(2) 1.1097(2) 0.7853(4) 0.046(2) Uani ? ? C C9 0.2265(2) 1.1509(2) 0.6988(3) 0.036(1) Uani ? ? C C10 0.2206(2) 1.1875(2) 0.5945(4) 0.054(2) Uani ? ? C C11 0.1711(3) 1.2456(2) 0.5844(4) 0.063(2) Uani ? ? C C12 0.1283(2) 1.2658(2) 0.6760(5) 0.056(2) Uani ? ? C C13 0.1326(2) 1.2286(2) 0.7798(5) 0.063(2) Uani ? ? C C14 0.1822(2) 1.1709(2) 0.7910(4) 0.051(2) Uani ? ? C C15 0.3459(2) 0.9931(2) 0.3945(3) 0.037(1) Uani ? ? C C16 0.3021(2) 0.9508(2) 0.3208(3) 0.047(2) Uani ? ? C C17 0.3212(3) 0.9453(2) 0.2042(3) 0.056(2) Uani ? ? C C18 0.3839(3) 0.9797(2) 0.1618(4) 0.060(2) Uani ? ? C C19 0.4272(2) 1.0203(2) 0.2336(4) 0.060(2) Uani ? ? C C20 0.4087(2) 1.0271(2) 0.3499(3) 0.045(2) Uani ? ? C C21 0.1397(2) 0.9995(2) 0.6565(3) 0.038(1) Uani ? ? C C22 0.0744(2) 1.0000(2) 0.7237(4) 0.053(2) Uani ? ? C C23 0.0074(2) 1.0255(2) 0.6755(5) 0.066(2) Uani ? ? C C24 0.0056(2) 1.0514(2) 0.5635(6) 0.073(3) Uani ? ? C C25 0.0690(3) 1.0515(2) 0.4996(5) 0.071(2) Uani ? ? C C26 0.1358(2) 1.0252(2) 0.5447(4) 0.052(2) Uani ? ? C C27 0.2058(2) 0.9742(2) 0.8742(3) 0.043(2) Uani ? ? C O2 0.1876(2) 0.9864(2) 0.9659(2) 0.062(2) Uani ? ? O P2 0.19129(4) 0.84014(4) 0.68840(7) 0.0282(3) Uani ? ? P C28 0.1431(2) 0.8336(1) 0.5492(3) 0.032(1) Uani ? ? C C29 0.1785(2) 0.8037(2) 0.4533(3) 0.042(2) Uani ? ? C C30 0.1440(2) 0.8014(2) 0.3456(3) 0.049(2) Uani ? ? C C31 0.0719(2) 0.8280(2) 0.3342(4) 0.052(2) Uani ? ? C C32 0.0361(2) 0.8579(2) 0.4265(3) 0.048(2) Uani ? ? C C33 0.0711(2) 0.8611(2) 0.5343(3) 0.039(1) Uani ? ? C C34 0.2597(2) 0.7663(2) 0.6801(3) 0.033(1) Uani ? ? C C35 0.3258(2) 0.7766(2) 0.6196(3) 0.040(1) Uani ? ? C C36 0.3758(2) 0.7194(2) 0.6066(4) 0.052(2) Uani ? ? C C37 0.3601(2) 0.6529(2) 0.6537(5) 0.063(2) Uani ? ? C C38 0.2953(2) 0.6430(2) 0.7157(5) 0.060(2) Uani ? ? C C39 0.2445(2) 0.6994(2) 0.7279(5) 0.047(2) Uani ? ? C C40 0.1278(2) 0.8081(2) 0.8005(3) 0.034(1) Uani ? ? C C41 0.1539(2) 0.8109(2) 0.9138(3) 0.044(2) Uani ? ? C C42 0.1122(3) 0.7830(3) 1.0046(4) 0.059(2) Uani ? ? C C43 0.0436(3) 0.7523(3) 0.9815(4) 0.074(2) Uani ? ? C C44 0.0171(2) 0.7496(3) 0.8700(5) 0.073(2) Uani ? ? C C45 0.0584(2) 0.7765(2) 0.7780(4) 0.054(2) Uani ? ? C H1 0.3659 1.1018 0.5437 0.0501 Uiso calc C1 H H2 0.2898 1.1129 0.9552 0.0598 Uiso calc C4 H H3 0.3801 1.1478 1.0895 0.0705 Uiso calc C5 H H4 0.5048 1.1560 1.0334 0.0757 Uiso calc C6 H H5 0.5385 1.1321 0.8443 0.0746 Uiso calc C7 H H6 0.4492 1.1009 0.7072 0.0599 Uiso calc C8 H H7 0.2501 1.1732 0.5298 0.0703 Uiso calc C10 H H8 0.1674 1.2710 0.5130 0.0829 Uiso calc C11 H H9 0.0953 1.3057 0.6689 0.0770 Uiso calc C12 H H10 0.1018 1.2422 0.8433 0.0824 Uiso calc C13 H H11 0.1854 1.1454 0.8624 0.0671 Uiso calc C14 H H12 0.2596 0.9260 0.3502 0.0630 Uiso calc C16 H H13 0.2908 0.9176 0.1533 0.0770 Uiso calc C17 H H14 0.3970 0.9750 0.0822 0.0838 Uiso calc C18 H H15 0.4702 1.0441 0.2039 0.0813 Uiso calc C19 H H16 0.4394 1.0553 0.3996 0.0606 Uiso calc C20 H H17 0.0755 0.9831 0.8016 0.0703 Uiso calc C22 H H18 -0.0371 1.0250 0.7205 0.0959 Uiso calc C23 H H19 -0.0398 1.0691 0.5314 0.1048 Uiso calc C24 H H20 0.0679 1.0697 0.4225 0.0939 Uiso calc C25 H H21 0.1794 1.0251 0.4975 0.0694 Uiso calc C26 H H22 0.2275 0.7845 0.4616 0.0543 Uiso calc C29 H H23 0.1694 0.7818 0.2804 0.0656 Uiso calc C30 H H24 0.0474 0.8252 0.2612 0.0701 Uiso calc C31 H H25 -0.0130 0.8767 0.4173 0.0622 Uiso calc C32 H H26 0.0457 0.8822 0.5983 0.0503 Uiso calc C33 H H27 0.3371 0.8224 0.5870 0.0519 Uiso calc C35 H H28 0.4211 0.7264 0.5650 0.0684 Uiso calc C36 H H29 0.3940 0.6140 0.6434 0.0854 Uiso calc C37 H H30 0.2850 0.5975 0.7503 0.0828 Uiso calc C38 H H31 0.1993 0.6920 0.7693 0.0619 Uiso calc C39 H H32 0.2012 0.8322 0.9293 0.0575 Uiso calc C41 H H33 0.1307 0.7850 1.0819 0.0800 Uiso calc C42 H H34 0.0146 0.7330 1.0432 0.0962 Uiso calc C43 H H35 -0.0306 0.7289 0.8555 0.0969 Uiso calc C44 H H36 0.0398 0.7736 0.7008 0.0704 Uiso calc C45 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol RH 0.02841(7) 0.02566(7) 0.02812(7) -0.00089(7) 0.0007(1) -0.0015(1) Rh I 0.04240(8) 0.03733(8) 0.0519(1) 0.00215(8) -0.01514(9) -0.0010(1) I P1 0.0355(3) 0.0255(3) 0.0328(4) -0.0025(3) 0.0019(3) -0.0030(3) P C1 0.042(1) 0.035(1) 0.039(2) -0.007(1) 0.008(1) -0.003(1) C C2 0.033(1) 0.032(1) 0.035(1) 0.003(1) -0.000(1) 0.001(1) C O1 0.042(1) 0.0295(9) 0.0300(9) -0.0013(8) 0.0021(9) -0.0019(8) O C3 0.041(1) 0.023(1) 0.048(2) -0.003(1) -0.002(1) -0.005(1) C C4 0.049(2) 0.046(2) 0.042(2) 0.005(2) -0.004(2) -0.004(2) C C5 0.069(2) 0.050(2) 0.044(2) 0.004(2) -0.012(2) -0.014(2) C C6 0.058(2) 0.047(2) 0.070(2) -0.008(2) -0.023(2) -0.006(2) C C7 0.043(2) 0.055(2) 0.074(3) -0.013(2) -0.010(2) -0.001(2) C C8 0.040(2) 0.043(2) 0.055(2) -0.008(1) 0.004(2) -0.001(2) C C9 0.038(1) 0.029(1) 0.042(2) -0.002(1) -0.001(1) -0.000(1) C C10 0.063(2) 0.049(2) 0.051(2) 0.011(2) 0.001(2) 0.009(2) C C11 0.073(3) 0.049(2) 0.069(2) 0.008(2) -0.008(2) 0.021(2) C C12 0.050(2) 0.041(2) 0.087(3) 0.008(1) -0.010(2) -0.001(2) C C13 0.057(2) 0.060(2) 0.073(3) 0.020(2) 0.001(2) -0.007(2) C C14 0.057(2) 0.051(2) 0.047(2) 0.014(2) -0.002(2) -0.002(2) C C15 0.045(1) 0.034(1) 0.032(1) -0.000(1) 0.001(1) 0.000(1) C C16 0.065(2) 0.041(1) 0.039(2) -0.004(2) 0.000(2) -0.005(2) C C17 0.088(3) 0.051(2) 0.039(2) 0.002(2) -0.006(2) -0.007(2) C C18 0.097(3) 0.060(2) 0.037(2) 0.002(2) 0.013(2) -0.003(2) C C19 0.079(2) 0.069(2) 0.040(2) -0.007(2) 0.020(2) 0.006(2) C C20 0.054(2) 0.054(2) 0.033(2) -0.006(2) 0.007(1) -0.001(1) C C21 0.035(1) 0.028(1) 0.055(2) 0.001(1) -0.009(1) -0.007(1) C C22 0.039(1) 0.054(2) 0.069(2) 0.006(1) -0.003(2) -0.020(2) C C23 0.038(2) 0.066(2) 0.118(4) 0.013(2) -0.008(2) -0.041(2) C C24 0.050(2) 0.059(2) 0.132(4) 0.019(2) -0.041(2) -0.017(3) C C25 0.069(2) 0.055(2) 0.093(3) 0.001(2) -0.037(2) 0.012(2) C C26 0.045(2) 0.046(2) 0.069(2) -0.004(1) -0.016(2) 0.011(2) C C27 0.047(2) 0.044(2) 0.039(2) -0.005(1) 0.003(1) -0.006(1) C O2 0.078(2) 0.075(2) 0.041(1) -0.006(2) 0.018(1) -0.014(1) O P2 0.0294(3) 0.0270(3) 0.0284(3) -0.0012(3) 0.0002(3) -0.0011(3) P C28 0.038(1) 0.026(1) 0.035(1) -0.003(1) -0.004(1) -0.000(1) C C29 0.048(2) 0.041(2) 0.036(2) 0.004(1) -0.003(1) -0.001(1) C C30 0.065(2) 0.053(2) 0.033(2) 0.006(2) -0.004(2) -0.006(2) C C31 0.074(2) 0.049(2) 0.039(2) -0.004(2) -0.018(2) 0.003(2) C C32 0.044(2) 0.047(2) 0.053(2) 0.002(1) -0.017(2) -0.000(2) C C33 0.039(1) 0.036(1) 0.041(2) 0.001(1) -0.005(1) -0.004(1) C C34 0.034(1) 0.030(1) 0.035(1) 0.003(1) -0.003(1) -0.004(1) C C35 0.037(1) 0.037(1) 0.046(2) -0.000(1) 0.000(1) -0.003(1) C C36 0.040(2) 0.053(2) 0.065(2) 0.011(1) -0.000(2) -0.010(2) C C37 0.061(2) 0.045(2) 0.092(3) 0.024(2) -0.004(2) -0.004(2) C C38 0.072(2) 0.036(1) 0.083(3) 0.015(2) 0.002(3) 0.008(2) C C39 0.051(2) 0.036(1) 0.055(2) 0.003(1) 0.005(2) 0.003(2) C C40 0.035(1) 0.032(1) 0.035(1) -0.000(1) 0.006(1) 0.003(1) C C41 0.048(2) 0.047(2) 0.037(2) -0.001(1) 0.005(1) 0.002(1) C C42 0.076(2) 0.071(2) 0.038(2) 0.008(2) 0.015(2) 0.011(2) C C43 0.072(2) 0.083(3) 0.068(2) -0.007(2) 0.033(2) 0.025(2) C C44 0.055(2) 0.080(3) 0.089(3) -0.027(2) 0.017(2) 0.016(2) C C45 0.045(2) 0.059(2) 0.058(2) -0.019(1) -0.001(2) 0.010(2) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag RH I 2.7752(3) . . ? RH P1 2.3285(8) . . ? RH O1 2.052(2) . . ? RH C21 2.078(3) . . ? RH C27 1.859(4) . . ? RH P2 2.4164(8) . . ? P1 C1 1.749(4) . . ? P1 C3 1.815(4) . . ? P1 C9 1.832(3) . . ? C1 C2 1.364(5) . . ? C2 O1 1.308(4) . . ? C2 C15 1.482(5) . . ? C3 C4 1.380(6) . . ? C3 C8 1.398(5) . . ? C4 C5 1.382(6) . . ? C5 C6 1.375(7) . . ? C6 C7 1.359(7) . . ? C7 C8 1.375(6) . . ? C9 C10 1.383(5) . . ? C9 C14 1.376(5) . . ? C10 C11 1.398(6) . . ? C11 C12 1.357(7) . . ? C12 C13 1.382(8) . . ? C13 C14 1.396(6) . . ? C15 C16 1.396(5) . . ? C15 C20 1.387(5) . . ? C16 C17 1.389(6) . . ? C17 C18 1.381(7) . . ? C18 C19 1.359(7) . . ? C19 C20 1.385(6) . . ? C21 C22 1.401(6) . . ? C21 C26 1.375(6) . . ? C22 C23 1.404(6) . . ? C23 C24 1.376(9) . . ? C24 C25 1.352(9) . . ? C25 C26 1.390(6) . . ? C27 O2 1.128(5) . . ? P2 C28 1.824(3) . . ? P2 C34 1.839(3) . . ? P2 C40 1.819(3) . . ? C28 C29 1.389(5) . . ? C28 C33 1.396(5) . . ? C29 C30 1.385(5) . . ? C30 C31 1.386(6) . . ? C31 C32 1.359(6) . . ? C32 C33 1.392(5) . . ? C34 C35 1.386(5) . . ? C34 C39 1.383(5) . . ? C35 C36 1.395(5) . . ? C36 C37 1.374(7) . . ? C37 C38 1.376(7) . . ? C38 C39 1.392(5) . . ? C40 C41 1.386(5) . . ? C40 C45 1.397(5) . . ? C41 C42 1.385(6) . . ? C42 C43 1.378(8) . . ? C43 C44 1.371(8) . . ? C44 C45 1.385(6) . . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I RH P1 90.43(2) . . . ? I RH O1 92.67(7) . . . ? I RH C21 175.9(1) . . . ? I RH C27 84.9(1) . . . ? I RH P2 93.28(2) . . . ? P1 RH O1 83.34(6) . . . ? P1 RH C21 89.75(9) . . . ? P1 RH C27 93.4(1) . . . ? P1 RH P2 166.59(3) . . . ? O1 RH C21 91.5(1) . . . ? O1 RH C27 175.9(1) . . . ? O1 RH P2 83.61(6) . . . ? C21 RH C27 90.9(2) . . . ? C21 RH P2 87.48(9) . . . ? C27 RH P2 99.8(1) . . . ? C1 P1 C3 109.8(2) . . . ? C1 P1 C9 107.2(2) . . . ? C3 P1 C9 104.5(1) . . . ? P1 C1 C2 116.8(3) . . . ? C1 C2 O1 123.7(3) . . . ? C1 C2 C15 121.1(3) . . . ? O1 C2 C15 115.0(3) . . . ? P1 C3 C4 122.3(3) . . . ? P1 C3 C8 119.3(3) . . . ? C4 C3 C8 118.4(4) . . . ? C3 C4 C5 120.8(4) . . . ? C4 C5 C6 119.9(4) . . . ? C5 C6 C7 119.9(4) . . . ? C6 C7 C8 121.0(4) . . . ? C3 C8 C7 120.0(4) . . . ? P1 C9 C10 119.3(3) . . . ? P1 C9 C14 121.0(3) . . . ? C10 C9 C14 119.7(3) . . . ? C9 C10 C11 119.9(4) . . . ? C10 C11 C12 120.4(4) . . . ? C11 C12 C13 120.2(4) . . . ? C12 C13 C14 119.9(4) . . . ? C9 C14 C13 120.0(4) . . . ? C2 C15 C16 118.6(3) . . . ? C2 C15 C20 122.4(3) . . . ? C16 C15 C20 119.0(3) . . . ? C15 C16 C17 119.5(4) . . . ? C16 C17 C18 120.5(4) . . . ? C17 C18 C19 120.3(4) . . . ? C18 C19 C20 120.2(4) . . . ? C15 C20 C19 120.7(4) . . . ? C22 C21 C26 118.2(4) . . . ? C21 C22 C23 119.7(5) . . . ? C22 C23 C24 120.5(5) . . . ? C23 C24 C25 119.4(5) . . . ? C24 C25 C26 121.2(6) . . . ? C21 C26 C25 121.0(5) . . . ? C28 P2 C34 102.7(2) . . . ? C28 P2 C40 107.9(2) . . . ? C34 P2 C40 102.1(2) . . . ? P2 C28 C29 120.6(3) . . . ? P2 C28 C33 121.3(3) . . . ? C29 C28 C33 118.0(3) . . . ? C28 C29 C30 121.3(3) . . . ? C29 C30 C31 119.3(4) . . . ? C30 C31 C32 120.6(4) . . . ? C31 C32 C33 120.2(3) . . . ? C28 C33 C32 120.6(3) . . . ? P2 C34 C35 119.5(3) . . . ? P2 C34 C39 121.1(3) . . . ? C35 C34 C39 119.4(3) . . . ? C34 C35 C36 119.7(3) . . . ? C35 C36 C37 120.6(4) . . . ? C36 C37 C38 119.8(4) . . . ? C37 C38 C39 120.1(4) . . . ? C34 C39 C38 120.4(4) . . . ? P2 C40 C41 116.5(3) . . . ? P2 C40 C45 124.0(3) . . . ? C41 C40 C45 119.3(3) . . . ? C40 C41 C42 121.1(4) . . . ? C41 C42 C43 119.2(4) . . . ? C42 C43 C44 120.3(4) . . . ? C43 C44 C45 121.2(4) . . . ? C40 C45 C44 118.9(4) . . . ? data_shelx834 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C41 H36 O2.50 P2 Rh' _chemical_formula_weight 733.55 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoklinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.864(3) _cell_length_b 8.859(2) _cell_length_c 29.696(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.27(3) _cell_angle_gamma 90.00 _cell_volume 3577.0(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 13 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max .4 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method ? _exptl_crystal_F_000 1508 _exptl_absorpt_coefficient_mu 0.602 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ' Siemens Stoe AED2' _diffrn_measurement_method ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% 0 _diffrn_reflns_number 25660 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 26.06 _reflns_number_total 6624 _reflns_number_observed 5690 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+2.5140P] 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 'riding model, H3 isotropic' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6619 _refine_ls_number_parameters 429 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_obs 0.0365 _refine_ls_wR_factor_all 0.1066 _refine_ls_wR_factor_obs 0.0916 _refine_ls_goodness_of_fit_all 1.053 _refine_ls_goodness_of_fit_obs 1.077 _refine_ls_restrained_S_all 1.156 _refine_ls_restrained_S_obs 1.077 _refine_ls_shift/esd_max -0.004 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Rh Rh 0.463344(15) 0.12482(3) 0.137712(7) 0.04333(8) Uani 1 d . . P1 P 0.60998(5) 0.02939(8) 0.11961(2) 0.0408(2) Uani 1 d . . P2 P 0.33173(5) 0.20505(9) 0.16678(3) 0.0479(2) Uani 1 d . . O1 O 0.51175(14) 0.0520(3) 0.20413(7) 0.0542(5) Uani 1 d . . O2 O 0.3698(2) 0.2433(4) 0.04675(9) 0.0950(10) Uani 1 d . . C1 C 0.4099(2) 0.1955(4) 0.08143(12) 0.0604(8) Uani 1 d . . C2 C 0.4568(2) 0.0792(3) 0.23485(10) 0.0496(7) Uani 1 d . . C3 C 0.3651(2) 0.1409(4) 0.22381(11) 0.0569(8) Uani 1 d . . H3 H 0.3283(23) 0.1565(34) 0.2455(12) 0.052(9) Uiso 1 d . . C4 C 0.5062(2) 0.0478(4) 0.28319(10) 0.0532(7) Uani 1 d . . C5 C 0.6039(3) 0.0073(5) 0.29322(13) 0.0734(10) Uani 1 d . . H5 H 0.6367(3) -0.0108(5) 0.26925(13) 0.088 Uiso 1 calc R . C6 C 0.6548(3) -0.0072(6) 0.3380(2) 0.0871(13) Uani 1 d . . H6 H 0.7210(3) -0.0333(6) 0.3439(2) 0.105 Uiso 1 calc R . C7 C 0.6081(4) 0.0166(6) 0.37319(14) 0.0913(13) Uani 1 d . . H7 H 0.6419(4) 0.0060(6) 0.40332(14) 0.110 Uiso 1 calc R . C8 C 0.5102(4) 0.0567(8) 0.3643(2) 0.117(2) Uani 1 d . . H8 H 0.4780(4) 0.0732(8) 0.3886(2) 0.141 Uiso 1 calc R . C9 C 0.4598(3) 0.0723(6) 0.31986(13) 0.0908(14) Uani 1 d . . H9 H 0.3938(3) 0.0998(6) 0.31433(13) 0.109 Uiso 1 calc R . C10 C 0.3179(2) 0.4093(4) 0.16941(10) 0.0511(7) Uani 1 d . . C11 C 0.3626(2) 0.4905(4) 0.20789(12) 0.0646(9) Uani 1 d . . H11 H 0.3951(2) 0.4391(4) 0.23373(12) 0.077 Uiso 1 calc R . C12 C 0.3596(3) 0.6469(5) 0.20845(15) 0.0763(10) Uani 1 d . . H12 H 0.3908(3) 0.6994(5) 0.23436(15) 0.092 Uiso 1 calc R . C13 C 0.3111(3) 0.7236(5) 0.1711(2) 0.0792(11) Uani 1 d . . H13 H 0.3093(3) 0.8286(5) 0.1715(2) 0.095 Uiso 1 calc R . C14 C 0.2649(3) 0.6463(5) 0.13303(15) 0.0802(11) Uani 1 d . . H14 H 0.2307(3) 0.6990(5) 0.10781(15) 0.096 Uiso 1 calc R . C15 C 0.2687(3) 0.4892(4) 0.13181(12) 0.0646(9) Uani 1 d . . H15 H 0.2380(3) 0.4378(4) 0.10560(12) 0.078 Uiso 1 calc R . C16 C 0.2078(2) 0.1390(4) 0.14244(12) 0.0575(8) Uani 1 d . . C17 C 0.1918(3) 0.0394(5) 0.1066(2) 0.0774(11) Uani 1 d . . H17 H 0.2433(3) 0.0115(5) 0.0925(2) 0.093 Uiso 1 calc R . C18 C 0.0979(3) -0.0203(6) 0.0913(2) 0.111(2) Uani 1 d . . H18 H 0.0871(3) -0.0882(6) 0.0670(2) 0.133 Uiso 1 calc R . C19 C 0.0225(3) 0.0198(6) 0.1118(3) 0.119(2) Uani 1 d . . H19 H -0.0389(3) -0.0244(6) 0.1023(3) 0.143 Uiso 1 calc R . C20 C 0.0363(3) 0.1254(7) 0.1463(2) 0.112(2) Uani 1 d . . H20 H -0.0165(3) 0.1572(7) 0.1590(2) 0.135 Uiso 1 calc R . C21 C 0.1296(3) 0.1841(6) 0.1620(2) 0.0903(13) Uani 1 d . . H21 H 0.1397(3) 0.2541(6) 0.1858(2) 0.108 Uiso 1 calc R . C22 C 0.7135(2) 0.0321(3) 0.16825(9) 0.0459(6) Uani 1 d . . C23 C 0.7216(2) 0.1512(4) 0.19902(12) 0.0639(9) Uani 1 d . . H23 H 0.6745(2) 0.2273(4) 0.19467(12) 0.077 Uiso 1 calc R . C24 C 0.7995(3) 0.1580(5) 0.23629(14) 0.0789(11) Uani 1 d . . H24 H 0.8051(3) 0.2398(5) 0.25629(14) 0.095 Uiso 1 calc R . C25 C 0.8678(3) 0.0456(5) 0.24371(13) 0.0789(11) Uani 1 d . . H25 H 0.9190(3) 0.0494(5) 0.26908(13) 0.095 Uiso 1 calc R . C26 C 0.8606(3) -0.0725(5) 0.2138(2) 0.0791(11) Uani 1 d . . H26 H 0.9077(3) -0.1487(5) 0.2188(2) 0.095 Uiso 1 calc R . C27 C 0.7837(2) -0.0804(4) 0.17585(13) 0.0618(8) Uani 1 d . . H27 H 0.7796(2) -0.1615(4) 0.15566(13) 0.074 Uiso 1 calc R . C28 C 0.5975(2) -0.1698(3) 0.10399(10) 0.0439(6) Uani 1 d . . C29 C 0.6349(2) -0.2331(4) 0.06785(11) 0.0570(7) Uani 1 d . . H29 H 0.6682(2) -0.1730(4) 0.05024(11) 0.068 Uiso 1 calc R . C30 C 0.6224(3) -0.3855(4) 0.05835(13) 0.0695(9) Uani 1 d . . H30 H 0.6469(3) -0.4273(4) 0.03416(13) 0.083 Uiso 1 calc R . C31 C 0.5738(3) -0.4756(4) 0.08443(14) 0.0704(9) Uani 1 d . . H31 H 0.5663(3) -0.5782(4) 0.07808(14) 0.085 Uiso 1 calc R . C32 C 0.5363(3) -0.4138(4) 0.11988(14) 0.0703(10) Uani 1 d . . H32 H 0.5027(3) -0.4743(4) 0.13727(14) 0.084 Uiso 1 calc R . C33 C 0.5485(2) -0.2625(4) 0.12960(11) 0.0568(7) Uani 1 d . . H33 H 0.5234(2) -0.2217(4) 0.15377(11) 0.068 Uiso 1 calc R . C34 C 0.6599(2) 0.1148(3) 0.07275(9) 0.0433(6) Uani 1 d . . C35 C 0.5989(2) 0.1350(4) 0.03037(11) 0.0558(7) Uani 1 d . . H35 H 0.5331(2) 0.1071(4) 0.02629(11) 0.067 Uiso 1 calc R . C36 C 0.6347(3) 0.1964(5) -0.00617(12) 0.0708(10) Uani 1 d . . H36 H 0.5932(3) 0.2081(5) -0.03460(12) 0.085 Uiso 1 calc R . C37 C 0.7307(3) 0.2394(5) -0.00028(13) 0.0814(11) Uani 1 d . . H37 H 0.7548(3) 0.2805(5) -0.02472(13) 0.098 Uiso 1 calc R . C38 C 0.7917(3) 0.2222(6) 0.04160(14) 0.0860(13) Uani 1 d . . H38 H 0.8571(3) 0.2524(6) 0.04552(14) 0.103 Uiso 1 calc R . C39 C 0.7569(2) 0.1600(4) 0.07826(12) 0.0654(9) Uani 1 d . . H39 H 0.7989(2) 0.1488(4) 0.10658(12) 0.079 Uiso 1 calc R . C200 C 0.5520(18) 0.1028(38) -0.4982(9) 0.345(22) Uani 1 d . . H20A H 0.5977(18) 0.0193(38) -0.4912(9) 0.414 Uiso 1 calc R . H20B H 0.5352(18) 0.1275(38) -0.4689(9) 0.414 Uiso 1 calc R . C300 C 0.6093(11) 0.2015(27) -0.5001(6) 0.366(16) Uani 1 d . . H30A H 0.6592(96) 0.1661(84) -0.5158(71) 0.548 Uiso 1 calc R . H30B H 0.6392(125) 0.2323(182) -0.4696(6) 0.548 Uiso 1 calc R . H30C H 0.5757(32) 0.2859(102) -0.5164(69) 0.548 Uiso 1 calc R . O3 O 0.4939(28) 0.0470(55) -0.5116(5) 0.236(16) Uani 0.50 d P . 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 0.03904(13) 0.05259(15) 0.03977(12) 0.00098(9) 0.01120(9) 0.00464(9) P1 0.0371(3) 0.0476(4) 0.0391(3) -0.0027(3) 0.0111(3) 0.0009(3) P2 0.0386(4) 0.0613(5) 0.0461(4) 0.0063(3) 0.0140(3) 0.0081(3) O1 0.0460(10) 0.0741(14) 0.0447(11) 0.0079(10) 0.0144(9) 0.0146(10) O2 0.085(2) 0.147(3) 0.0516(15) 0.025(2) 0.0103(13) 0.033(2) C1 0.051(2) 0.079(2) 0.053(2) -0.001(2) 0.0148(14) 0.011(2) C2 0.050(2) 0.054(2) 0.046(2) 0.0082(12) 0.0126(13) 0.0022(12) C3 0.050(2) 0.078(2) 0.048(2) 0.0133(15) 0.0220(14) 0.0130(15) C4 0.056(2) 0.057(2) 0.046(2) 0.0091(13) 0.0113(13) 0.0002(14) C5 0.067(2) 0.097(3) 0.056(2) 0.016(2) 0.011(2) 0.026(2) C6 0.073(2) 0.111(3) 0.071(3) 0.014(2) -0.003(2) 0.020(2) C7 0.102(3) 0.116(4) 0.049(2) 0.013(2) -0.004(2) 0.011(3) C8 0.098(3) 0.203(6) 0.053(2) 0.022(3) 0.020(2) 0.021(4) C9 0.070(2) 0.154(4) 0.051(2) 0.022(2) 0.017(2) 0.017(3) C10 0.0423(14) 0.066(2) 0.049(2) 0.0054(13) 0.0173(12) 0.0085(13) C11 0.060(2) 0.076(2) 0.055(2) 0.000(2) 0.008(2) 0.007(2) C12 0.082(3) 0.073(3) 0.075(2) -0.017(2) 0.019(2) -0.001(2) C13 0.091(3) 0.063(2) 0.091(3) 0.000(2) 0.034(2) 0.005(2) C14 0.098(3) 0.075(3) 0.069(2) 0.018(2) 0.019(2) 0.017(2) C15 0.077(2) 0.064(2) 0.053(2) 0.0048(15) 0.012(2) 0.010(2) C16 0.044(2) 0.063(2) 0.066(2) 0.013(2) 0.0096(14) 0.0069(13) C17 0.053(2) 0.071(2) 0.106(3) -0.011(2) 0.008(2) 0.002(2) C18 0.065(3) 0.094(3) 0.161(5) -0.034(3) -0.009(3) -0.002(2) C19 0.049(2) 0.101(4) 0.198(7) 0.002(4) 0.000(3) -0.012(2) C20 0.052(2) 0.142(5) 0.147(5) 0.000(4) 0.028(3) -0.008(3) C21 0.051(2) 0.133(4) 0.091(3) -0.003(3) 0.026(2) -0.004(2) C22 0.0395(13) 0.057(2) 0.0420(14) 0.0004(12) 0.0107(11) -0.0028(12) C23 0.056(2) 0.073(2) 0.062(2) -0.020(2) 0.009(2) -0.001(2) C24 0.065(2) 0.103(3) 0.065(2) -0.026(2) 0.003(2) -0.010(2) C25 0.057(2) 0.114(3) 0.059(2) 0.001(2) -0.006(2) -0.014(2) C26 0.056(2) 0.085(3) 0.088(3) 0.012(2) -0.008(2) 0.006(2) C27 0.051(2) 0.064(2) 0.067(2) -0.002(2) 0.0023(15) 0.0052(14) C28 0.0387(13) 0.049(2) 0.0441(14) -0.0030(11) 0.0080(11) -0.0019(11) C29 0.065(2) 0.055(2) 0.056(2) -0.0057(14) 0.0224(15) -0.0008(14) C30 0.086(2) 0.055(2) 0.071(2) -0.018(2) 0.024(2) 0.005(2) C31 0.078(2) 0.048(2) 0.082(3) -0.009(2) 0.011(2) -0.006(2) C32 0.072(2) 0.057(2) 0.084(3) 0.006(2) 0.021(2) -0.016(2) C33 0.057(2) 0.059(2) 0.057(2) -0.0027(14) 0.0184(14) -0.0088(14) C34 0.0471(14) 0.0426(15) 0.0416(14) -0.0034(11) 0.0124(11) -0.0007(11) C35 0.053(2) 0.070(2) 0.045(2) -0.0019(14) 0.0104(13) -0.0049(14) C36 0.077(2) 0.095(3) 0.040(2) 0.005(2) 0.011(2) -0.001(2) C37 0.095(3) 0.100(3) 0.056(2) 0.009(2) 0.031(2) -0.020(2) C38 0.066(2) 0.128(4) 0.068(2) 0.010(2) 0.023(2) -0.033(2) C39 0.050(2) 0.095(3) 0.051(2) 0.007(2) 0.0108(14) -0.013(2) C200 0.226(29) 0.584(64) 0.259(30) 0.180(36) 0.131(27) 0.065(30) C300 0.204(16) 0.529(38) 0.320(24) -0.255(27) -0.055(14) 0.041(17) O3 0.265(33) 0.349(36) 0.076(10) -0.041(14) -0.013(15) 0.019(24) _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 C1 1.803(3) . ? Rh O1 2.059(2) . ? Rh P2 2.2793(9) . ? Rh P1 2.3588(8) . ? P1 C28 1.824(3) . ? P1 C22 1.826(3) . ? P1 C34 1.834(3) . ? P2 C3 1.761(3) . ? P2 C10 1.823(3) . ? P2 C16 1.825(3) . ? O1 C2 1.320(4) . ? O2 C1 1.151(4) . ? C2 C3 1.363(4) . ? C2 C4 1.491(4) . ? C4 C5 1.377(5) . ? C4 C9 1.385(5) . ? C5 C6 1.385(5) . ? C6 C7 1.348(6) . ? C7 C8 1.378(6) . ? C8 C9 1.375(6) . ? C10 C15 1.384(4) . ? C10 C11 1.390(5) . ? C11 C12 1.386(5) . ? C12 C13 1.360(6) . ? C13 C14 1.370(6) . ? C14 C15 1.393(5) . ? C16 C17 1.367(5) . ? C16 C21 1.385(5) . ? C17 C18 1.396(5) . ? C18 C19 1.354(8) . ? C19 C20 1.374(8) . ? C20 C21 1.389(6) . ? C22 C27 1.381(4) . ? C22 C23 1.386(4) . ? C23 C24 1.388(5) . ? C24 C25 1.362(6) . ? C25 C26 1.363(6) . ? C26 C27 1.395(5) . ? C28 C33 1.384(4) . ? C28 C29 1.398(4) . ? C29 C30 1.383(5) . ? C30 C31 1.377(5) . ? C31 C32 1.376(6) . ? C32 C33 1.375(5) . ? C34 C39 1.381(4) . ? C34 C35 1.384(4) . ? C35 C36 1.389(5) . ? C36 C37 1.362(5) . ? C37 C38 1.369(6) . ? C38 C39 1.389(5) . ? C200 O3 0.96(5) . ? C200 C300 1.19(3) . ? C200 O3 1.52(5) 3_654 ? O3 O3 1.07(8) 3_654 ? O3 C200 1.52(5) 3_654 ? 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 C1 Rh O1 174.16(11) . . ? C1 Rh P2 91.61(10) . . ? O1 Rh P2 82.54(6) . . ? C1 Rh P1 97.46(10) . . ? O1 Rh P1 88.38(6) . . ? P2 Rh P1 170.92(3) . . ? C28 P1 C22 103.58(13) . . ? C28 P1 C34 103.73(13) . . ? C22 P1 C34 103.88(13) . . ? C28 P1 Rh 111.19(9) . . ? C22 P1 Rh 113.20(9) . . ? C34 P1 Rh 119.65(9) . . ? C3 P2 C10 106.8(2) . . ? C3 P2 C16 109.1(2) . . ? C10 P2 C16 103.67(14) . . ? C3 P2 Rh 100.61(11) . . ? C10 P2 Rh 115.12(9) . . ? C16 P2 Rh 120.77(12) . . ? C2 O1 Rh 118.7(2) . . ? O2 C1 Rh 175.1(3) . . ? O1 C2 C3 122.9(3) . . ? O1 C2 C4 114.4(2) . . ? C3 C2 C4 122.5(3) . . ? C2 C3 P2 114.7(2) . . ? C5 C4 C9 117.3(3) . . ? C5 C4 C2 120.3(3) . . ? C9 C4 C2 122.1(3) . . ? C4 C5 C6 121.8(4) . . ? C7 C6 C5 119.9(4) . . ? C6 C7 C8 119.8(4) . . ? C9 C8 C7 120.4(4) . . ? C8 C9 C4 120.8(4) . . ? C15 C10 C11 117.9(3) . . ? C15 C10 P2 120.8(3) . . ? C11 C10 P2 121.1(2) . . ? C12 C11 C10 121.2(4) . . ? C13 C12 C11 120.1(4) . . ? C12 C13 C14 120.0(4) . . ? C13 C14 C15 120.5(4) . . ? C10 C15 C14 120.3(4) . . ? C17 C16 C21 119.5(3) . . ? C17 C16 P2 120.8(3) . . ? C21 C16 P2 119.6(3) . . ? C16 C17 C18 119.8(4) . . ? C19 C18 C17 120.5(5) . . ? C18 C19 C20 120.5(4) . . ? C19 C20 C21 119.3(5) . . ? C16 C21 C20 120.3(5) . . ? C27 C22 C23 118.6(3) . . ? C27 C22 P1 122.6(2) . . ? C23 C22 P1 118.8(2) . . ? C22 C23 C24 120.6(3) . . ? C25 C24 C23 120.3(4) . . ? C24 C25 C26 119.8(3) . . ? C25 C26 C27 120.8(4) . . ? C22 C27 C26 120.0(3) . . ? C33 C28 C29 118.7(3) . . ? C33 C28 P1 117.8(2) . . ? C29 C28 P1 123.5(2) . . ? C30 C29 C28 119.8(3) . . ? C31 C30 C29 120.5(3) . . ? C30 C31 C32 119.9(3) . . ? C33 C32 C31 120.0(3) . . ? C32 C33 C28 121.1(3) . . ? C39 C34 C35 118.5(3) . . ? C39 C34 P1 122.2(2) . . ? C35 C34 P1 119.3(2) . . ? C34 C35 C36 120.8(3) . . ? C37 C36 C35 119.9(3) . . ? C36 C37 C38 120.0(3) . . ? C37 C38 C39 120.5(3) . . ? C34 C39 C38 120.1(3) . . ? O3 C200 C300 150.6(50) . . ? O3 C200 O3 44.3(34) . 3_654 ? C300 C200 O3 163.0(34) . 3_654 ? C200 O3 O3 96.9(32) . 3_654 ? C200 O3 C200 135.7(34) . 3_654 ? O3 O3 C200 38.8(34) 3_654 3_654 ? _refine_diff_density_max 0.406 _refine_diff_density_min -0.653 _refine_diff_density_rms 0.055