Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Matthew Clarke' _publ_contact_author_address ; School of Chemistry University of St. Andrews Purdie Building St. Andrews Fife KY16 9ST UNITED KINGDOM ; _publ_contact_author_email MATTHEW.CLARKE@ST-ANDREWS.AC.UK _publ_section_title ; Evaluation of C4 diphosphine ligands in rhodium catalysed methanol carbonylation under a syngas atmosphere: synthesis, structure, stability and reactivity of rhodium(I) carbonyl and rhodium (III) acetyl intermediates. ; loop_ _publ_author_name 'Matthew Clarke' 'Lesley Key' 'Gareth Lamb' 'Alexandra M. Z. Slawin' 'Bruce Williams' data_6 _database_code_depnum_ccdc_archive 'CCDC 658319' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H32 I O P2 Rh' _chemical_formula_sum 'C45 H32 I O P2 Rh' _chemical_formula_weight 880.46 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' I I -0.4742 1.8119 '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 11.1576(12) _cell_length_b 11.5084(16) _cell_length_c 14.6153(15) _cell_angle_alpha 84.203(7) _cell_angle_beta 71.704(7) _cell_angle_gamma 89.593(10) _cell_volume 1772.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 5733 _cell_measurement_theta_min 2.0220 _cell_measurement_theta_max 28.4800 _exptl_crystal_description Plate _exptl_crystal_colour Orange _exptl_crystal_size_max 0.1000 _exptl_crystal_size_mid 0.0300 _exptl_crystal_size_min 0.0100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 1.480 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8610 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11550 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0958 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.33 _reflns_number_total 6105 _reflns_number_gt 4758 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0271P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6105 _refine_ls_number_parameters 452 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.0865 _refine_ls_wR_factor_gt 0.0781 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh -0.08659(3) 0.27827(4) 0.58537(3) 0.01510(12) Uani 1 1 d . . . I1 I -0.20698(3) 0.32798(3) 0.45383(2) 0.02500(12) Uani 1 1 d . . . P1 P 0.02095(10) 0.21024(12) 0.68461(9) 0.0146(3) Uani 1 1 d . . . P2 P -0.28005(10) 0.23946(11) 0.71281(9) 0.0145(3) Uani 1 1 d . . . C1 C -0.0543(4) 0.0683(4) 0.7416(3) 0.0136(10) Uani 1 1 d . . . C2 C -0.1561(4) 0.0551(4) 0.8265(3) 0.0119(10) Uani 1 1 d . . . C3 C -0.2174(4) -0.0583(4) 0.8607(3) 0.0156(11) Uani 1 1 d . . . C4 C -0.3250(4) -0.0778(4) 0.9443(3) 0.0170(11) Uani 1 1 d . . . H4A H -0.3586 -0.0147 0.9810 0.020 Uiso 1 1 calc R . . C5 C -0.3810(4) -0.1866(5) 0.9726(4) 0.0234(12) Uani 1 1 d . . . H5A H -0.4531 -0.1977 1.0287 0.028 Uiso 1 1 calc R . . C6 C -0.3343(4) -0.2822(5) 0.9205(4) 0.0223(12) Uani 1 1 d . . . H6A H -0.3746 -0.3570 0.9416 0.027 Uiso 1 1 calc R . . C7 C -0.2306(4) -0.2673(4) 0.8393(4) 0.0214(12) Uani 1 1 d . . . H7A H -0.1984 -0.3321 0.8045 0.026 Uiso 1 1 calc R . . C8 C -0.1708(4) -0.1554(4) 0.8069(3) 0.0173(11) Uani 1 1 d . . . C9 C -0.0688(4) -0.1368(4) 0.7194(3) 0.0168(11) Uani 1 1 d . . . H9A H -0.0367 -0.2007 0.6834 0.020 Uiso 1 1 calc R . . C10 C -0.0167(4) -0.0276(5) 0.6867(3) 0.0177(12) Uani 1 1 d . . . H10A H 0.0467 -0.0156 0.6253 0.021 Uiso 1 1 calc R . . C11 C -0.2728(4) 0.2433(4) 0.8373(3) 0.0151(11) Uani 1 1 d . . . C12 C -0.2117(4) 0.1585(4) 0.8792(3) 0.0123(10) Uani 1 1 d . . . C13 C -0.1991(4) 0.1719(4) 0.9733(3) 0.0162(11) Uani 1 1 d . . . C14 C -0.1373(4) 0.0876(4) 1.0196(3) 0.0160(11) Uani 1 1 d . . . H14A H -0.1065 0.0190 0.9899 0.019 Uiso 1 1 calc R . . C15 C -0.1217(4) 0.1048(4) 1.1074(3) 0.0198(12) Uani 1 1 d . . . H15A H -0.0789 0.0487 1.1371 0.024 Uiso 1 1 calc R . . C16 C -0.1693(4) 0.2057(5) 1.1532(3) 0.0198(12) Uani 1 1 d . . . H16A H -0.1587 0.2169 1.2137 0.024 Uiso 1 1 calc R . . C17 C -0.2300(4) 0.2863(4) 1.1110(3) 0.0184(11) Uani 1 1 d . . . H17A H -0.2612 0.3538 1.1424 0.022 Uiso 1 1 calc R . . C18 C -0.2477(4) 0.2716(4) 1.0206(3) 0.0155(11) Uani 1 1 d . . . C19 C -0.3088(4) 0.3556(4) 0.9753(3) 0.0184(11) Uani 1 1 d . . . H19A H -0.3414 0.4229 1.0066 0.022 Uiso 1 1 calc R . . C20 C -0.3219(4) 0.3420(4) 0.8878(3) 0.0168(11) Uani 1 1 d . . . H20A H -0.3647 0.3995 0.8594 0.020 Uiso 1 1 calc R . . C21 C 0.0572(4) 0.3137(5) 0.4796(4) 0.0210(12) Uani 1 1 d . . . O21 O 0.1410(3) 0.3346(3) 0.4107(2) 0.0293(9) Uani 1 1 d . . . C22 C 0.1908(4) 0.1836(4) 0.6291(3) 0.0157(11) Uani 1 1 d . . . C23 C 0.2513(4) 0.0799(5) 0.6422(3) 0.0203(12) Uani 1 1 d . . . H23A H 0.2038 0.0136 0.6796 0.024 Uiso 1 1 calc R . . C24 C 0.3821(4) 0.0733(5) 0.6003(4) 0.0232(12) Uani 1 1 d . . . H24A H 0.4226 0.0015 0.6072 0.028 Uiso 1 1 calc R . . C25 C 0.4530(4) 0.1705(5) 0.5488(3) 0.0246(13) Uani 1 1 d . . . H25A H 0.5417 0.1653 0.5202 0.030 Uiso 1 1 calc R . . C26 C 0.3946(4) 0.2752(5) 0.5390(3) 0.0208(12) Uani 1 1 d . . . H26A H 0.4437 0.3427 0.5057 0.025 Uiso 1 1 calc R . . C27 C 0.2639(4) 0.2821(5) 0.5778(3) 0.0169(11) Uani 1 1 d . . . H27A H 0.2241 0.3538 0.5694 0.020 Uiso 1 1 calc R . . C28 C 0.0371(4) 0.2920(4) 0.7804(3) 0.0158(11) Uani 1 1 d . . . C29 C 0.0936(4) 0.2392(5) 0.8476(3) 0.0166(11) Uani 1 1 d . . . H29A H 0.1136 0.1589 0.8471 0.020 Uiso 1 1 calc R . . C30 C 0.1199(4) 0.3039(5) 0.9143(4) 0.0261(13) Uani 1 1 d . . . H30A H 0.1571 0.2680 0.9599 0.031 Uiso 1 1 calc R . . C31 C 0.0914(4) 0.4217(5) 0.9142(4) 0.0265(13) Uani 1 1 d . . . H31A H 0.1093 0.4665 0.9597 0.032 Uiso 1 1 calc R . . C32 C 0.0370(4) 0.4740(5) 0.8477(4) 0.0265(13) Uani 1 1 d . . . H32A H 0.0187 0.5547 0.8473 0.032 Uiso 1 1 calc R . . C33 C 0.0093(4) 0.4095(5) 0.7821(4) 0.0216(12) Uani 1 1 d . . . H33A H -0.0292 0.4460 0.7376 0.026 Uiso 1 1 calc R . . C34 C -0.3949(4) 0.3513(4) 0.7069(3) 0.0160(11) Uani 1 1 d . . . C35 C -0.3474(4) 0.4647(4) 0.6798(3) 0.0165(11) Uani 1 1 d . . . H35A H -0.2590 0.4788 0.6631 0.020 Uiso 1 1 calc R . . C36 C -0.4248(4) 0.5576(5) 0.6765(3) 0.0207(12) Uani 1 1 d . . . H36A H -0.3907 0.6351 0.6597 0.025 Uiso 1 1 calc R . . C37 C -0.5540(4) 0.5362(5) 0.6981(3) 0.0232(12) Uani 1 1 d . . . H37A H -0.6079 0.5994 0.6939 0.028 Uiso 1 1 calc R . . C38 C -0.6039(4) 0.4254(5) 0.7252(3) 0.0210(12) Uani 1 1 d . . . H38A H -0.6923 0.4123 0.7404 0.025 Uiso 1 1 calc R . . C39 C -0.5257(4) 0.3308(5) 0.7308(3) 0.0182(11) Uani 1 1 d . . . H39A H -0.5607 0.2539 0.7505 0.022 Uiso 1 1 calc R . . C40 C -0.3533(4) 0.0986(4) 0.7151(3) 0.0160(11) Uani 1 1 d . . . C41 C -0.3004(4) 0.0276(5) 0.6412(4) 0.0201(12) Uani 1 1 d . . . H41A H -0.2289 0.0553 0.5883 0.024 Uiso 1 1 calc R . . C42 C -0.3519(4) -0.0840(5) 0.6442(4) 0.0228(12) Uani 1 1 d . . . H42A H -0.3152 -0.1317 0.5937 0.027 Uiso 1 1 calc R . . C43 C -0.4542(4) -0.1237(5) 0.7194(4) 0.0217(12) Uani 1 1 d . . . H43A H -0.4888 -0.1994 0.7213 0.026 Uiso 1 1 calc R . . C44 C -0.5088(4) -0.0550(4) 0.7936(4) 0.0195(11) Uani 1 1 d . . . H44A H -0.5810 -0.0834 0.8456 0.023 Uiso 1 1 calc R . . C45 C -0.4584(4) 0.0542(4) 0.7919(4) 0.0189(11) Uani 1 1 d . . . H45A H -0.4954 0.1002 0.8435 0.023 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 0.0119(2) 0.0201(3) 0.0130(2) -0.00127(17) -0.00361(14) 0.00117(15) I1 0.01756(18) 0.0411(3) 0.0172(2) -0.00113(16) -0.00731(13) 0.00409(15) P1 0.0107(6) 0.0177(8) 0.0148(7) -0.0022(6) -0.0029(5) 0.0010(5) P2 0.0133(6) 0.0157(8) 0.0146(7) -0.0033(5) -0.0043(5) 0.0015(5) C1 0.016(2) 0.016(3) 0.010(2) -0.001(2) -0.0054(18) 0.0015(19) C2 0.019(2) 0.006(3) 0.014(3) -0.003(2) -0.0097(18) 0.0028(19) C3 0.019(2) 0.016(3) 0.014(3) -0.002(2) -0.0090(19) 0.005(2) C4 0.021(2) 0.012(3) 0.016(3) -0.002(2) -0.0044(19) -0.002(2) C5 0.023(3) 0.029(4) 0.018(3) -0.007(2) -0.005(2) -0.001(2) C6 0.030(3) 0.015(3) 0.022(3) -0.002(2) -0.009(2) -0.006(2) C7 0.029(3) 0.013(3) 0.026(3) -0.002(2) -0.013(2) -0.003(2) C8 0.022(3) 0.016(3) 0.018(3) -0.007(2) -0.011(2) 0.003(2) C9 0.017(2) 0.022(3) 0.017(3) -0.014(2) -0.0086(19) 0.005(2) C10 0.010(2) 0.032(4) 0.015(3) -0.005(2) -0.0069(18) -0.002(2) C11 0.009(2) 0.023(3) 0.012(3) -0.005(2) 0.0002(17) -0.0025(19) C12 0.013(2) 0.009(3) 0.016(3) -0.006(2) -0.0060(18) 0.0032(18) C13 0.018(2) 0.019(3) 0.012(3) -0.002(2) -0.0048(18) 0.001(2) C14 0.013(2) 0.018(3) 0.018(3) -0.003(2) -0.0056(18) 0.0001(19) C15 0.023(3) 0.017(3) 0.019(3) -0.001(2) -0.007(2) 0.000(2) C16 0.020(2) 0.026(3) 0.015(3) -0.003(2) -0.0073(19) -0.007(2) C17 0.025(3) 0.016(3) 0.016(3) -0.012(2) -0.005(2) 0.001(2) C18 0.020(2) 0.013(3) 0.012(3) -0.005(2) -0.0017(18) -0.001(2) C19 0.019(2) 0.015(3) 0.022(3) -0.005(2) -0.007(2) 0.002(2) C20 0.019(2) 0.013(3) 0.018(3) -0.001(2) -0.0050(19) 0.001(2) C21 0.023(3) 0.022(3) 0.026(3) -0.010(2) -0.018(2) 0.002(2) O21 0.0246(18) 0.043(3) 0.017(2) -0.0004(18) -0.0026(15) -0.0109(17) C22 0.012(2) 0.024(3) 0.013(3) -0.007(2) -0.0063(18) 0.004(2) C23 0.015(2) 0.036(4) 0.013(3) -0.002(2) -0.0100(19) 0.003(2) C24 0.020(3) 0.031(4) 0.025(3) -0.007(3) -0.014(2) 0.011(2) C25 0.014(2) 0.045(4) 0.017(3) -0.008(3) -0.0066(19) 0.000(2) C26 0.018(2) 0.027(4) 0.019(3) -0.002(2) -0.0065(19) -0.008(2) C27 0.019(2) 0.024(3) 0.009(2) -0.004(2) -0.0066(19) 0.001(2) C28 0.011(2) 0.022(3) 0.015(3) -0.006(2) -0.0039(18) -0.002(2) C29 0.017(2) 0.018(3) 0.016(3) -0.002(2) -0.0053(19) -0.002(2) C30 0.019(3) 0.041(4) 0.020(3) -0.004(3) -0.008(2) -0.011(2) C31 0.016(2) 0.035(4) 0.029(3) -0.015(3) -0.004(2) -0.005(2) C32 0.025(3) 0.020(3) 0.034(3) -0.011(3) -0.006(2) 0.002(2) C33 0.019(2) 0.021(3) 0.026(3) -0.004(2) -0.007(2) 0.002(2) C34 0.017(2) 0.022(3) 0.008(2) -0.004(2) -0.0019(18) 0.004(2) C35 0.014(2) 0.018(3) 0.018(3) -0.003(2) -0.0043(18) -0.001(2) C36 0.022(3) 0.019(3) 0.018(3) 0.001(2) -0.003(2) 0.001(2) C37 0.030(3) 0.029(4) 0.012(3) -0.008(2) -0.009(2) 0.009(2) C38 0.012(2) 0.032(4) 0.019(3) -0.006(2) -0.0043(19) 0.003(2) C39 0.016(2) 0.020(3) 0.020(3) -0.005(2) -0.0065(19) -0.002(2) C40 0.016(2) 0.023(3) 0.015(3) -0.008(2) -0.0120(19) 0.001(2) C41 0.019(2) 0.025(3) 0.019(3) -0.005(2) -0.010(2) 0.003(2) C42 0.023(3) 0.019(3) 0.029(3) -0.009(2) -0.011(2) 0.010(2) C43 0.018(3) 0.023(3) 0.029(3) -0.005(2) -0.012(2) -0.003(2) C44 0.019(2) 0.017(3) 0.021(3) 0.000(2) -0.005(2) -0.003(2) C45 0.023(3) 0.014(3) 0.020(3) -0.006(2) -0.006(2) -0.002(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 C21 1.858(5) . ? Rh1 P1 2.2374(12) . ? Rh1 P2 2.3769(12) . ? Rh1 I1 2.6863(5) . ? P1 C28 1.818(5) . ? P1 C1 1.837(5) . ? P1 C22 1.850(4) . ? P2 C40 1.813(5) . ? P2 C34 1.825(5) . ? P2 C11 1.851(5) . ? C1 C2 1.389(6) . ? C1 C10 1.414(7) . ? C2 C3 1.444(6) . ? C2 C12 1.507(6) . ? C3 C4 1.419(6) . ? C3 C8 1.431(7) . ? C4 C5 1.369(7) . ? C4 H4A 0.9500 . ? C5 C6 1.404(7) . ? C5 H5A 0.9500 . ? C6 C7 1.370(6) . ? C6 H6A 0.9500 . ? C7 C8 1.421(7) . ? C7 H7A 0.9500 . ? C8 C9 1.418(6) . ? C9 C10 1.365(6) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 C12 1.388(6) . ? C11 C20 1.428(7) . ? C12 C13 1.448(6) . ? C13 C18 1.416(7) . ? C13 C14 1.424(6) . ? C14 C15 1.381(6) . ? C14 H14A 0.9500 . ? C15 C16 1.415(7) . ? C15 H15A 0.9500 . ? C16 C17 1.355(6) . ? C16 H16A 0.9500 . ? C17 C18 1.423(6) . ? C17 H17A 0.9500 . ? C18 C19 1.407(6) . ? C19 C20 1.357(6) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 O21 1.144(5) . ? C22 C23 1.393(7) . ? C22 C27 1.403(6) . ? C23 C24 1.399(6) . ? C23 H23A 0.9500 . ? C24 C25 1.382(7) . ? C24 H24A 0.9500 . ? C25 C26 1.382(7) . ? C25 H25A 0.9500 . ? C26 C27 1.393(6) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C28 C33 1.386(7) . ? C28 C29 1.411(6) . ? C29 C30 1.387(7) . ? C29 H29A 0.9500 . ? C30 C31 1.390(7) . ? C30 H30A 0.9500 . ? C31 C32 1.387(7) . ? C31 H31A 0.9500 . ? C32 C33 1.377(7) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C34 C35 1.383(7) . ? C34 C39 1.406(6) . ? C35 C36 1.376(7) . ? C35 H35A 0.9500 . ? C36 C37 1.393(6) . ? C36 H36A 0.9500 . ? C37 C38 1.365(7) . ? C37 H37A 0.9500 . ? C38 C39 1.402(7) . ? C38 H38A 0.9500 . ? C39 H39A 0.9500 . ? C40 C41 1.398(7) . ? C40 C45 1.401(6) . ? C41 C42 1.402(7) . ? C41 H41A 0.9500 . ? C42 C43 1.356(6) . ? C42 H42A 0.9500 . ? C43 C44 1.387(7) . ? C43 H43A 0.9500 . ? C44 C45 1.375(7) . ? C44 H44A 0.9500 . ? C45 H45A 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 C21 Rh1 P1 94.29(14) . . ? C21 Rh1 P2 175.44(14) . . ? P1 Rh1 P2 90.27(4) . . ? C21 Rh1 I1 83.48(14) . . ? P1 Rh1 I1 170.96(4) . . ? P2 Rh1 I1 92.06(3) . . ? C28 P1 C1 107.5(2) . . ? C28 P1 C22 96.9(2) . . ? C1 P1 C22 106.6(2) . . ? C28 P1 Rh1 121.98(16) . . ? C1 P1 Rh1 105.48(14) . . ? C22 P1 Rh1 117.36(15) . . ? C40 P2 C34 107.7(2) . . ? C40 P2 C11 104.5(2) . . ? C34 P2 C11 102.0(2) . . ? C40 P2 Rh1 114.26(16) . . ? C34 P2 Rh1 111.22(15) . . ? C11 P2 Rh1 116.07(13) . . ? C2 C1 C10 119.7(4) . . ? C2 C1 P1 123.5(4) . . ? C10 C1 P1 116.1(3) . . ? C1 C2 C3 119.6(4) . . ? C1 C2 C12 121.5(4) . . ? C3 C2 C12 118.7(4) . . ? C4 C3 C8 117.9(4) . . ? C4 C3 C2 122.9(5) . . ? C8 C3 C2 119.1(4) . . ? C5 C4 C3 120.6(5) . . ? C5 C4 H4A 119.7 . . ? C3 C4 H4A 119.7 . . ? C4 C5 C6 121.6(5) . . ? C4 C5 H5A 119.2 . . ? C6 C5 H5A 119.2 . . ? C7 C6 C5 119.8(5) . . ? C7 C6 H6A 120.1 . . ? C5 C6 H6A 120.1 . . ? C6 C7 C8 120.3(5) . . ? C6 C7 H7A 119.8 . . ? C8 C7 H7A 119.8 . . ? C9 C8 C7 121.0(5) . . ? C9 C8 C3 119.1(4) . . ? C7 C8 C3 119.8(4) . . ? C10 C9 C8 120.3(5) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C9 C10 C1 121.8(4) . . ? C9 C10 H10A 119.1 . . ? C1 C10 H10A 119.1 . . ? C12 C11 C20 119.3(4) . . ? C12 C11 P2 121.8(4) . . ? C20 C11 P2 118.6(3) . . ? C11 C12 C13 119.3(4) . . ? C11 C12 C2 120.4(4) . . ? C13 C12 C2 120.3(4) . . ? C18 C13 C14 118.6(4) . . ? C18 C13 C12 119.8(4) . . ? C14 C13 C12 121.7(5) . . ? C15 C14 C13 120.6(5) . . ? C15 C14 H14A 119.7 . . ? C13 C14 H14A 119.7 . . ? C14 C15 C16 120.2(4) . . ? C14 C15 H15A 119.9 . . ? C16 C15 H15A 119.9 . . ? C17 C16 C15 120.3(5) . . ? C17 C16 H16A 119.9 . . ? C15 C16 H16A 119.9 . . ? C16 C17 C18 121.1(5) . . ? C16 C17 H17A 119.5 . . ? C18 C17 H17A 119.5 . . ? C19 C18 C13 119.1(4) . . ? C19 C18 C17 121.6(5) . . ? C13 C18 C17 119.3(4) . . ? C20 C19 C18 121.0(5) . . ? C20 C19 H19A 119.5 . . ? C18 C19 H19A 119.5 . . ? C19 C20 C11 121.6(4) . . ? C19 C20 H20A 119.2 . . ? C11 C20 H20A 119.2 . . ? O21 C21 Rh1 175.5(4) . . ? C23 C22 C27 118.9(4) . . ? C23 C22 P1 125.8(4) . . ? C27 C22 P1 115.0(4) . . ? C22 C23 C24 120.0(5) . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C25 C24 C23 120.5(5) . . ? C25 C24 H24A 119.8 . . ? C23 C24 H24A 119.8 . . ? C26 C25 C24 119.9(4) . . ? C26 C25 H25A 120.0 . . ? C24 C25 H25A 120.0 . . ? C25 C26 C27 120.2(5) . . ? C25 C26 H26A 119.9 . . ? C27 C26 H26A 119.9 . . ? C26 C27 C22 120.4(5) . . ? C26 C27 H27A 119.8 . . ? C22 C27 H27A 119.8 . . ? C33 C28 C29 118.8(4) . . ? C33 C28 P1 121.3(4) . . ? C29 C28 P1 119.4(4) . . ? C30 C29 C28 120.4(5) . . ? C30 C29 H29A 119.8 . . ? C28 C29 H29A 119.8 . . ? C29 C30 C31 119.6(5) . . ? C29 C30 H30A 120.2 . . ? C31 C30 H30A 120.2 . . ? C32 C31 C30 120.1(5) . . ? C32 C31 H31A 119.9 . . ? C30 C31 H31A 119.9 . . ? C33 C32 C31 120.4(5) . . ? C33 C32 H32A 119.8 . . ? C31 C32 H32A 119.8 . . ? C32 C33 C28 120.7(5) . . ? C32 C33 H33A 119.7 . . ? C28 C33 H33A 119.7 . . ? C35 C34 C39 118.9(4) . . ? C35 C34 P2 116.1(3) . . ? C39 C34 P2 125.0(4) . . ? C36 C35 C34 121.8(4) . . ? C36 C35 H35A 119.1 . . ? C34 C35 H35A 119.1 . . ? C35 C36 C37 118.9(5) . . ? C35 C36 H36A 120.5 . . ? C37 C36 H36A 120.5 . . ? C38 C37 C36 120.7(5) . . ? C38 C37 H37A 119.6 . . ? C36 C37 H37A 119.6 . . ? C37 C38 C39 120.5(4) . . ? C37 C38 H38A 119.8 . . ? C39 C38 H38A 119.8 . . ? C38 C39 C34 119.2(5) . . ? C38 C39 H39A 120.4 . . ? C34 C39 H39A 120.4 . . ? C41 C40 C45 117.8(5) . . ? C41 C40 P2 119.9(4) . . ? C45 C40 P2 122.3(4) . . ? C40 C41 C42 120.7(4) . . ? C40 C41 H41A 119.6 . . ? C42 C41 H41A 119.6 . . ? C43 C42 C41 119.8(5) . . ? C43 C42 H42A 120.1 . . ? C41 C42 H42A 120.1 . . ? C42 C43 C44 120.8(5) . . ? C42 C43 H43A 119.6 . . ? C44 C43 H43A 119.6 . . ? C45 C44 C43 119.9(4) . . ? C45 C44 H44A 120.0 . . ? C43 C44 H44A 120.0 . . ? C44 C45 C40 121.0(5) . . ? C44 C45 H45A 119.5 . . ? C40 C45 H45A 119.5 . . ? 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 C21 Rh1 P1 C28 106.6(2) . . . . ? P2 Rh1 P1 C28 -73.11(17) . . . . ? C21 Rh1 P1 C1 -130.7(2) . . . . ? P2 Rh1 P1 C1 49.59(17) . . . . ? C21 Rh1 P1 C22 -12.2(2) . . . . ? P2 Rh1 P1 C22 168.08(19) . . . . ? P1 Rh1 P2 C40 -94.11(16) . . . . ? I1 Rh1 P2 C40 77.15(15) . . . . ? P1 Rh1 P2 C34 143.66(18) . . . . ? I1 Rh1 P2 C34 -45.09(17) . . . . ? P1 Rh1 P2 C11 27.71(19) . . . . ? I1 Rh1 P2 C11 -161.04(18) . . . . ? C28 P1 C1 C2 43.1(4) . . . . ? C22 P1 C1 C2 146.1(4) . . . . ? Rh1 P1 C1 C2 -88.4(4) . . . . ? C28 P1 C1 C10 -146.6(3) . . . . ? C22 P1 C1 C10 -43.6(4) . . . . ? Rh1 P1 C1 C10 81.8(3) . . . . ? C10 C1 C2 C3 3.8(6) . . . . ? P1 C1 C2 C3 173.7(3) . . . . ? C10 C1 C2 C12 -170.7(4) . . . . ? P1 C1 C2 C12 -0.8(6) . . . . ? C1 C2 C3 C4 -177.2(4) . . . . ? C12 C2 C3 C4 -2.6(6) . . . . ? C1 C2 C3 C8 0.7(6) . . . . ? C12 C2 C3 C8 175.4(4) . . . . ? C8 C3 C4 C5 0.7(6) . . . . ? C2 C3 C4 C5 178.7(4) . . . . ? C3 C4 C5 C6 0.1(7) . . . . ? C4 C5 C6 C7 -0.1(7) . . . . ? C5 C6 C7 C8 -0.7(7) . . . . ? C6 C7 C8 C9 -175.6(4) . . . . ? C6 C7 C8 C3 1.5(7) . . . . ? C4 C3 C8 C9 175.6(4) . . . . ? C2 C3 C8 C9 -2.4(6) . . . . ? C4 C3 C8 C7 -1.5(6) . . . . ? C2 C3 C8 C7 -179.6(4) . . . . ? C7 C8 C9 C10 176.6(4) . . . . ? C3 C8 C9 C10 -0.5(6) . . . . ? C8 C9 C10 C1 5.3(6) . . . . ? C2 C1 C10 C9 -7.0(6) . . . . ? P1 C1 C10 C9 -177.6(3) . . . . ? C40 P2 C11 C12 57.1(4) . . . . ? C34 P2 C11 C12 169.2(4) . . . . ? Rh1 P2 C11 C12 -69.7(4) . . . . ? C40 P2 C11 C20 -128.5(3) . . . . ? C34 P2 C11 C20 -16.3(4) . . . . ? Rh1 P2 C11 C20 104.7(3) . . . . ? C20 C11 C12 C13 0.0(6) . . . . ? P2 C11 C12 C13 174.3(3) . . . . ? C20 C11 C12 C2 -178.4(4) . . . . ? P2 C11 C12 C2 -4.0(6) . . . . ? C1 C2 C12 C11 66.4(6) . . . . ? C3 C2 C12 C11 -108.1(5) . . . . ? C1 C2 C12 C13 -111.9(5) . . . . ? C3 C2 C12 C13 73.6(5) . . . . ? C11 C12 C13 C18 -0.7(6) . . . . ? C2 C12 C13 C18 177.7(4) . . . . ? C11 C12 C13 C14 -180.0(4) . . . . ? C2 C12 C13 C14 -1.6(6) . . . . ? C18 C13 C14 C15 -2.1(6) . . . . ? C12 C13 C14 C15 177.2(4) . . . . ? C13 C14 C15 C16 1.2(7) . . . . ? C14 C15 C16 C17 -0.3(7) . . . . ? C15 C16 C17 C18 0.3(7) . . . . ? C14 C13 C18 C19 179.9(4) . . . . ? C12 C13 C18 C19 0.6(6) . . . . ? C14 C13 C18 C17 2.0(6) . . . . ? C12 C13 C18 C17 -177.3(4) . . . . ? C16 C17 C18 C19 -179.0(4) . . . . ? C16 C17 C18 C13 -1.1(7) . . . . ? C13 C18 C19 C20 0.3(7) . . . . ? C17 C18 C19 C20 178.1(4) . . . . ? C18 C19 C20 C11 -1.0(7) . . . . ? C12 C11 C20 C19 0.9(7) . . . . ? P2 C11 C20 C19 -173.7(3) . . . . ? C28 P1 C22 C23 101.2(4) . . . . ? C1 P1 C22 C23 -9.4(5) . . . . ? Rh1 P1 C22 C23 -127.2(4) . . . . ? C28 P1 C22 C27 -72.2(4) . . . . ? C1 P1 C22 C27 177.2(4) . . . . ? Rh1 P1 C22 C27 59.3(4) . . . . ? C27 C22 C23 C24 -3.2(7) . . . . ? P1 C22 C23 C24 -176.4(4) . . . . ? C22 C23 C24 C25 2.5(7) . . . . ? C23 C24 C25 C26 0.3(8) . . . . ? C24 C25 C26 C27 -2.3(7) . . . . ? C25 C26 C27 C22 1.6(7) . . . . ? C23 C22 C27 C26 1.2(7) . . . . ? P1 C22 C27 C26 175.1(4) . . . . ? C1 P1 C28 C33 -136.8(4) . . . . ? C22 P1 C28 C33 113.3(4) . . . . ? Rh1 P1 C28 C33 -15.1(4) . . . . ? C1 P1 C28 C29 51.1(4) . . . . ? C22 P1 C28 C29 -58.8(4) . . . . ? Rh1 P1 C28 C29 172.9(3) . . . . ? C33 C28 C29 C30 0.4(6) . . . . ? P1 C28 C29 C30 172.7(3) . . . . ? C28 C29 C30 C31 -0.6(7) . . . . ? C29 C30 C31 C32 0.0(7) . . . . ? C30 C31 C32 C33 0.8(7) . . . . ? C31 C32 C33 C28 -1.0(7) . . . . ? C29 C28 C33 C32 0.4(7) . . . . ? P1 C28 C33 C32 -171.7(4) . . . . ? C40 P2 C34 C35 -164.0(4) . . . . ? C11 P2 C34 C35 86.3(4) . . . . ? Rh1 P2 C34 C35 -38.1(4) . . . . ? C40 P2 C34 C39 18.3(5) . . . . ? C11 P2 C34 C39 -91.4(4) . . . . ? Rh1 P2 C34 C39 144.3(4) . . . . ? C39 C34 C35 C36 0.6(7) . . . . ? P2 C34 C35 C36 -177.3(4) . . . . ? C34 C35 C36 C37 -2.1(7) . . . . ? C35 C36 C37 C38 2.1(7) . . . . ? C36 C37 C38 C39 -0.7(7) . . . . ? C37 C38 C39 C34 -0.8(7) . . . . ? C35 C34 C39 C38 0.9(7) . . . . ? P2 C34 C39 C38 178.5(4) . . . . ? C34 P2 C40 C41 119.3(4) . . . . ? C11 P2 C40 C41 -132.8(4) . . . . ? Rh1 P2 C40 C41 -4.9(4) . . . . ? C34 P2 C40 C45 -64.5(4) . . . . ? C11 P2 C40 C45 43.4(4) . . . . ? Rh1 P2 C40 C45 171.4(3) . . . . ? C45 C40 C41 C42 0.3(7) . . . . ? P2 C40 C41 C42 176.7(3) . . . . ? C40 C41 C42 C43 0.1(7) . . . . ? C41 C42 C43 C44 0.1(7) . . . . ? C42 C43 C44 C45 -0.7(7) . . . . ? C43 C44 C45 C40 1.1(7) . . . . ? C41 C40 C45 C44 -0.9(7) . . . . ? P2 C40 C45 C44 -177.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 0.875 _refine_diff_density_min -1.667 _refine_diff_density_rms 0.134 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 658320' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C3O H31 I2 O P2 Rh.(0.5[C3 H6 O2]0.5)' _chemical_formula_sum 'C31.50 H34 I2 O2 P2 Rh' _chemical_formula_weight 863.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.540(4) _cell_length_b 8.1514(14) _cell_length_c 18.908(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.662(3) _cell_angle_gamma 90.00 _cell_volume 3297.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 7160 _cell_measurement_theta_min 2.0801 _cell_measurement_theta_max 25.3491 _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.0300 _exptl_crystal_size_mid 0.0200 _exptl_crystal_size_min 0.0200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.739 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 2.513 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9265 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 0.83 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22888 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.36 _reflns_number_total 5963 _reflns_number_gt 5162 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. There is half a disordered methyl acetate solvent molecule. ; _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^)+(0.0183P)^2^+4.1813P] 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 5963 _refine_ls_number_parameters 354 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0337 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0519 _refine_ls_wR_factor_gt 0.0486 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.004 _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 0.251863(11) 0.02515(3) 0.758607(13) 0.01082(6) Uani 1 1 d . . . I1 I 0.334288(10) -0.22441(3) 0.773918(12) 0.01853(6) Uani 1 1 d . . . I2 I 0.177494(10) -0.17543(3) 0.672786(12) 0.01719(6) Uani 1 1 d . . . P1 P 0.16820(4) 0.20624(10) 0.74749(4) 0.01202(17) Uani 1 1 d . . . C1 C 0.17854(15) 0.4214(4) 0.77496(17) 0.0171(7) Uani 1 1 d . . . H1A H 0.2186 0.4604 0.7601 0.020 Uiso 1 1 calc R . . H1B H 0.1448 0.4863 0.7481 0.020 Uiso 1 1 calc R . . C2 C 0.17866(16) 0.4607(4) 0.85447(17) 0.0183(7) Uani 1 1 d . . . H2A H 0.1901 0.5775 0.8624 0.022 Uiso 1 1 calc R . . H2B H 0.1358 0.4456 0.8675 0.022 Uiso 1 1 calc R . . C3 C 0.22346(15) 0.3552(4) 0.90348(17) 0.0167(7) Uani 1 1 d . . . H3A H 0.2070 0.2418 0.9034 0.020 Uiso 1 1 calc R . . H3B H 0.2252 0.3980 0.9527 0.020 Uiso 1 1 calc R . . C4 C 0.29038(15) 0.3514(4) 0.88142(18) 0.0167(7) Uani 1 1 d . . . H4A H 0.3204 0.3868 0.9222 0.020 Uiso 1 1 calc R . . H4B H 0.2931 0.4301 0.8420 0.020 Uiso 1 1 calc R . . P2 P 0.31214(4) 0.14665(10) 0.85289(4) 0.01271(18) Uani 1 1 d . . . C5 C 0.29337(15) 0.1674(4) 0.69324(17) 0.0173(7) Uani 1 1 d . . . O5 O 0.30438(11) 0.3096(3) 0.70387(12) 0.0202(5) Uani 1 1 d . . . C6 C 0.30936(19) 0.0784(5) 0.62774(19) 0.0304(9) Uani 1 1 d . . . H6A H 0.2708 0.0501 0.5975 0.046 Uiso 1 1 calc R . . H6B H 0.3325 -0.0220 0.6420 0.046 Uiso 1 1 calc R . . H6C H 0.3352 0.1494 0.6012 0.046 Uiso 1 1 calc R . . C7 C 0.10188(14) 0.1377(4) 0.79164(17) 0.0138(7) Uani 1 1 d . . . C8 C 0.10299(15) -0.0095(4) 0.82921(17) 0.0156(7) Uani 1 1 d . . . H8A H 0.1392 -0.0768 0.8323 0.019 Uiso 1 1 calc R . . C9 C 0.05209(16) -0.0589(4) 0.86204(18) 0.0213(8) Uani 1 1 d . . . H9A H 0.0535 -0.1596 0.8875 0.026 Uiso 1 1 calc R . . C10 C -0.00112(15) 0.0383(4) 0.85790(18) 0.0212(8) Uani 1 1 d . . . H10A H -0.0362 0.0041 0.8803 0.025 Uiso 1 1 calc R . . C11 C -0.00296(15) 0.1850(5) 0.82106(19) 0.0230(8) Uani 1 1 d . . . H11A H -0.0394 0.2516 0.8182 0.028 Uiso 1 1 calc R . . C12 C 0.04823(15) 0.2353(4) 0.78828(18) 0.0190(7) Uani 1 1 d . . . H12A H 0.0468 0.3367 0.7634 0.023 Uiso 1 1 calc R . . C13 C 0.13533(14) 0.2374(4) 0.65464(16) 0.0131(7) Uani 1 1 d . . . C14 C 0.08173(15) 0.1539(4) 0.62487(18) 0.0180(7) Uani 1 1 d . . . H14A H 0.0606 0.0818 0.6535 0.022 Uiso 1 1 calc R . . C15 C 0.05954(16) 0.1764(4) 0.55369(19) 0.0221(8) Uani 1 1 d . . . H15A H 0.0229 0.1206 0.5339 0.027 Uiso 1 1 calc R . . C16 C 0.09046(18) 0.2796(5) 0.51137(19) 0.0265(9) Uani 1 1 d . . . H16A H 0.0755 0.2925 0.4624 0.032 Uiso 1 1 calc R . . C17 C 0.14285(17) 0.3637(4) 0.54010(18) 0.0229(8) Uani 1 1 d . . . H17A H 0.1637 0.4354 0.5110 0.027 Uiso 1 1 calc R . . C18 C 0.16533(15) 0.3439(4) 0.61162(18) 0.0187(7) Uani 1 1 d . . . H18A H 0.2012 0.4031 0.6313 0.022 Uiso 1 1 calc R . . C19 C 0.39561(15) 0.1717(4) 0.84760(18) 0.0192(8) Uani 1 1 d . . . C20 C 0.41861(17) 0.3102(5) 0.81645(19) 0.0250(8) Uani 1 1 d . . . H20A H 0.3906 0.3930 0.7971 0.030 Uiso 1 1 calc R . . C21 C 0.48283(18) 0.3277(6) 0.8136(2) 0.0343(10) Uani 1 1 d . . . H21A H 0.4984 0.4224 0.7923 0.041 Uiso 1 1 calc R . . C22 C 0.52373(18) 0.2071(6) 0.8419(2) 0.0367(11) Uani 1 1 d . . . H22A H 0.5673 0.2189 0.8397 0.044 Uiso 1 1 calc R . . C23 C 0.50117(16) 0.0699(5) 0.8731(2) 0.0325(10) Uani 1 1 d . . . H23A H 0.5293 -0.0125 0.8926 0.039 Uiso 1 1 calc R . . C24 C 0.43729(16) 0.0523(5) 0.87586(18) 0.0225(8) Uani 1 1 d . . . H24A H 0.4220 -0.0426 0.8973 0.027 Uiso 1 1 calc R . . C25 C 0.30793(14) 0.0299(4) 0.93471(17) 0.0132(7) Uani 1 1 d . . . C26 C 0.34224(15) 0.0827(4) 0.99804(17) 0.0175(7) Uani 1 1 d . . . H26A H 0.3699 0.1734 0.9976 0.021 Uiso 1 1 calc R . . C27 C 0.33585(15) 0.0028(4) 1.06134(18) 0.0186(7) Uani 1 1 d . . . H27A H 0.3595 0.0386 1.1041 0.022 Uiso 1 1 calc R . . C28 C 0.29563(15) -0.1283(4) 1.06310(18) 0.0204(8) Uani 1 1 d . . . H28A H 0.2912 -0.1814 1.1070 0.024 Uiso 1 1 calc R . . C29 C 0.26165(16) -0.1824(4) 1.00084(19) 0.0215(8) Uani 1 1 d . . . H29A H 0.2342 -0.2734 1.0018 0.026 Uiso 1 1 calc R . . C30 C 0.26786(14) -0.1029(4) 0.93667(18) 0.0169(7) Uani 1 1 d . . . H30A H 0.2445 -0.1400 0.8940 0.020 Uiso 1 1 calc R . . O31 O 0.4441(3) -0.6054(8) 1.0238(3) 0.0500(17) Uani 0.50 1 d P A 1 C31 C 0.46771(16) -0.4993(4) 1.00036(18) 0.0381(8) Uani 0.50 1 d P . 1 C32 C 0.4394(3) -0.3498(6) 0.9686(3) 0.0597(16) Uani 1 1 d . B 1 H32A H 0.4416 -0.3511 0.9171 0.090 Uiso 1 1 calc R B 1 H32B H 0.4620 -0.2540 0.9896 0.090 Uiso 1 1 calc R B 1 H32C H 0.3955 -0.3440 0.9777 0.090 Uiso 1 1 calc R B 1 O32 O 0.46771(16) -0.4993(4) 1.00036(18) 0.0381(8) Uani 0.50 1 d P . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01058(12) 0.01050(13) 0.01147(13) 0.00103(10) 0.00166(9) 0.00036(10) I1 0.01779(11) 0.01839(12) 0.01895(12) -0.00110(9) 0.00011(9) 0.00718(9) I2 0.01404(11) 0.01313(12) 0.02388(12) -0.00421(9) -0.00004(9) -0.00009(9) P1 0.0119(4) 0.0119(4) 0.0122(4) 0.0011(3) 0.0013(3) 0.0008(3) C1 0.0173(17) 0.0139(18) 0.0200(18) 0.0031(14) 0.0022(14) 0.0021(14) C2 0.0222(18) 0.0110(17) 0.0225(19) -0.0054(14) 0.0059(14) -0.0021(15) C3 0.0215(17) 0.0162(18) 0.0125(17) -0.0002(13) 0.0025(14) 0.0003(15) C4 0.0195(17) 0.0146(18) 0.0155(17) 0.0026(14) -0.0010(14) -0.0024(14) P2 0.0121(4) 0.0149(4) 0.0109(4) 0.0017(3) 0.0002(3) -0.0014(3) C5 0.0155(16) 0.021(2) 0.0151(17) 0.0042(14) 0.0000(13) -0.0002(15) O5 0.0235(13) 0.0176(14) 0.0195(13) 0.0030(10) 0.0032(10) -0.0037(11) C6 0.050(3) 0.022(2) 0.023(2) -0.0005(16) 0.0200(18) -0.0062(19) C7 0.0152(16) 0.0135(17) 0.0124(16) -0.0011(13) 0.0011(13) 0.0011(14) C8 0.0127(16) 0.0161(18) 0.0177(17) 0.0001(14) 0.0008(13) 0.0017(14) C9 0.0237(18) 0.021(2) 0.0187(18) -0.0016(15) 0.0023(14) -0.0059(16) C10 0.0149(17) 0.028(2) 0.0210(18) -0.0074(16) 0.0041(14) -0.0078(16) C11 0.0125(17) 0.029(2) 0.027(2) -0.0061(16) 0.0024(15) 0.0045(16) C12 0.0185(17) 0.0174(19) 0.0200(19) 0.0006(14) -0.0021(14) 0.0027(15) C13 0.0125(15) 0.0154(17) 0.0110(16) -0.0008(13) -0.0004(12) 0.0063(14) C14 0.0195(17) 0.0141(18) 0.0200(18) -0.0015(14) 0.0010(14) 0.0036(15) C15 0.0215(18) 0.0182(19) 0.025(2) -0.0075(15) -0.0059(15) 0.0046(16) C16 0.036(2) 0.029(2) 0.0134(18) -0.0006(16) -0.0026(16) 0.0127(18) C17 0.029(2) 0.024(2) 0.0165(18) 0.0060(15) 0.0055(15) 0.0063(17) C18 0.0162(17) 0.0152(18) 0.0246(19) 0.0006(14) 0.0023(14) 0.0042(14) C19 0.0148(16) 0.027(2) 0.0158(17) -0.0015(15) 0.0009(14) -0.0053(15) C20 0.0224(19) 0.032(2) 0.0206(19) 0.0056(16) 0.0007(15) -0.0046(17) C21 0.026(2) 0.048(3) 0.030(2) 0.0053(19) 0.0073(17) -0.017(2) C22 0.0154(18) 0.062(3) 0.033(2) 0.002(2) 0.0062(17) -0.008(2) C23 0.0143(18) 0.049(3) 0.034(2) 0.000(2) 0.0027(16) 0.0017(18) C24 0.0198(18) 0.029(2) 0.0199(19) 0.0007(16) 0.0064(14) -0.0012(16) C25 0.0107(15) 0.0144(17) 0.0153(16) 0.0023(13) 0.0040(13) 0.0039(13) C26 0.0158(16) 0.0197(19) 0.0168(17) -0.0025(14) 0.0008(13) 0.0023(15) C27 0.0182(17) 0.0225(19) 0.0149(17) 0.0008(14) 0.0008(13) 0.0085(15) C28 0.0224(18) 0.024(2) 0.0151(17) 0.0099(15) 0.0032(14) 0.0081(16) C29 0.0222(18) 0.0212(19) 0.0216(19) 0.0065(15) 0.0051(15) -0.0015(16) C30 0.0131(16) 0.0197(18) 0.0177(18) 0.0004(14) 0.0009(13) 0.0015(14) O31 0.058(4) 0.040(4) 0.054(4) -0.004(3) 0.015(3) -0.023(3) C31 0.046(2) 0.030(2) 0.035(2) -0.0002(16) -0.0075(17) 0.0008(19) C32 0.075(4) 0.042(3) 0.054(3) -0.006(2) -0.030(3) 0.027(3) O32 0.046(2) 0.030(2) 0.035(2) -0.0002(16) -0.0075(17) 0.0008(19) _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 C5 1.982(3) . ? Rh1 P2 2.3039(9) . ? Rh1 P1 2.3202(9) . ? Rh1 I1 2.6934(5) . ? Rh1 I2 2.6962(4) . ? P1 C7 1.824(3) . ? P1 C13 1.833(3) . ? P1 C1 1.835(3) . ? C1 C2 1.537(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.524(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.547(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 P2 1.832(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? P2 C19 1.824(3) . ? P2 C25 1.827(3) . ? C5 O5 1.196(4) . ? C5 C6 1.509(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.393(5) . ? C7 C12 1.398(5) . ? C8 C9 1.381(4) . ? C8 H8A 0.9500 . ? C9 C10 1.388(5) . ? C9 H9A 0.9500 . ? C10 C11 1.382(5) . ? C10 H10A 0.9500 . ? C11 C12 1.388(5) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C18 1.398(5) . ? C13 C14 1.401(5) . ? C14 C15 1.387(5) . ? C14 H14A 0.9500 . ? C15 C16 1.384(5) . ? C15 H15A 0.9500 . ? C16 C17 1.377(5) . ? C16 H16A 0.9500 . ? C17 C18 1.392(5) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C24 1.389(5) . ? C19 C20 1.391(5) . ? C20 C21 1.398(5) . ? C20 H20A 0.9500 . ? C21 C22 1.385(6) . ? C21 H21A 0.9500 . ? C22 C23 1.379(6) . ? C22 H22A 0.9500 . ? C23 C24 1.391(5) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C30 1.388(5) . ? C25 C26 1.400(4) . ? C26 C27 1.384(5) . ? C26 H26A 0.9500 . ? C27 C28 1.378(5) . ? C27 H27A 0.9500 . ? C28 C29 1.384(5) . ? C28 H28A 0.9500 . ? C29 C30 1.396(5) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? O31 C31 1.121(6) . ? C31 C31 1.393(7) 3_647 ? C31 C32 1.461(5) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? O32 O32 1.393(7) 3_647 ? 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 C5 Rh1 P2 88.66(10) . . ? C5 Rh1 P1 88.46(10) . . ? P2 Rh1 P1 99.13(3) . . ? C5 Rh1 I1 99.75(10) . . ? P2 Rh1 I1 86.34(2) . . ? P1 Rh1 I1 170.28(2) . . ? C5 Rh1 I2 105.01(10) . . ? P2 Rh1 I2 165.59(2) . . ? P1 Rh1 I2 86.00(3) . . ? I1 Rh1 I2 86.842(16) . . ? C7 P1 C13 104.17(14) . . ? C7 P1 C1 103.82(15) . . ? C13 P1 C1 99.17(15) . . ? C7 P1 Rh1 113.90(11) . . ? C13 P1 Rh1 112.62(10) . . ? C1 P1 Rh1 120.98(11) . . ? C2 C1 P1 117.5(2) . . ? C2 C1 H1A 107.9 . . ? P1 C1 H1A 107.9 . . ? C2 C1 H1B 107.9 . . ? P1 C1 H1B 107.9 . . ? H1A C1 H1B 107.2 . . ? C3 C2 C1 114.0(3) . . ? C3 C2 H2A 108.8 . . ? C1 C2 H2A 108.8 . . ? C3 C2 H2B 108.8 . . ? C1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C2 C3 C4 113.0(3) . . ? C2 C3 H3A 109.0 . . ? C4 C3 H3A 109.0 . . ? C2 C3 H3B 109.0 . . ? C4 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C3 C4 P2 112.1(2) . . ? C3 C4 H4A 109.2 . . ? P2 C4 H4A 109.2 . . ? C3 C4 H4B 109.2 . . ? P2 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C19 P2 C25 104.52(15) . . ? C19 P2 C4 101.64(16) . . ? C25 P2 C4 100.71(15) . . ? C19 P2 Rh1 118.45(11) . . ? C25 P2 Rh1 110.63(11) . . ? C4 P2 Rh1 118.63(11) . . ? O5 C5 C6 123.0(3) . . ? O5 C5 Rh1 123.9(3) . . ? C6 C5 Rh1 113.2(2) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C12 118.6(3) . . ? C8 C7 P1 121.9(2) . . ? C12 C7 P1 119.5(3) . . ? C9 C8 C7 120.8(3) . . ? C9 C8 H8A 119.6 . . ? C7 C8 H8A 119.6 . . ? C8 C9 C10 120.1(3) . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C11 C10 C9 119.8(3) . . ? C11 C10 H10A 120.1 . . ? C9 C10 H10A 120.1 . . ? C10 C11 C12 120.2(3) . . ? C10 C11 H11A 119.9 . . ? C12 C11 H11A 119.9 . . ? C11 C12 C7 120.5(3) . . ? C11 C12 H12A 119.8 . . ? C7 C12 H12A 119.8 . . ? C18 C13 C14 118.9(3) . . ? C18 C13 P1 119.3(2) . . ? C14 C13 P1 121.8(3) . . ? C15 C14 C13 120.1(3) . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C16 C15 C14 120.4(3) . . ? C16 C15 H15A 119.8 . . ? C14 C15 H15A 119.8 . . ? C17 C16 C15 120.1(3) . . ? C17 C16 H16A 119.9 . . ? C15 C16 H16A 119.9 . . ? C16 C17 C18 120.2(3) . . ? C16 C17 H17A 119.9 . . ? C18 C17 H17A 119.9 . . ? C17 C18 C13 120.3(3) . . ? C17 C18 H18A 119.8 . . ? C13 C18 H18A 119.8 . . ? C24 C19 C20 119.1(3) . . ? C24 C19 P2 119.9(3) . . ? C20 C19 P2 121.1(3) . . ? C19 C20 C21 120.1(4) . . ? C19 C20 H20A 119.9 . . ? C21 C20 H20A 119.9 . . ? C22 C21 C20 120.0(4) . . ? C22 C21 H21A 120.0 . . ? C20 C21 H21A 120.0 . . ? C23 C22 C21 120.0(3) . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C22 C23 C24 120.0(4) . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C19 C24 C23 120.8(4) . . ? C19 C24 H24A 119.6 . . ? C23 C24 H24A 119.6 . . ? C30 C25 C26 119.0(3) . . ? C30 C25 P2 121.4(2) . . ? C26 C25 P2 119.4(2) . . ? C27 C26 C25 120.0(3) . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C28 C27 C26 120.8(3) . . ? C28 C27 H27A 119.6 . . ? C26 C27 H27A 119.6 . . ? C27 C28 C29 119.9(3) . . ? C27 C28 H28A 120.1 . . ? C29 C28 H28A 120.1 . . ? C28 C29 C30 119.8(3) . . ? C28 C29 H29A 120.1 . . ? C30 C29 H29A 120.1 . . ? C25 C30 C29 120.5(3) . . ? C25 C30 H30A 119.7 . . ? C29 C30 H30A 119.7 . . ? O31 C31 C31 119.8(5) . 3_647 ? O31 C31 C32 128.3(5) . . ? C31 C31 C32 111.9(5) 3_647 . ? 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 C5 Rh1 P1 C7 174.34(15) . . . . ? P2 Rh1 P1 C7 -97.27(12) . . . . ? I2 Rh1 P1 C7 69.18(11) . . . . ? C5 Rh1 P1 C13 56.00(15) . . . . ? P2 Rh1 P1 C13 144.39(12) . . . . ? I2 Rh1 P1 C13 -49.17(12) . . . . ? C5 Rh1 P1 C1 -60.85(16) . . . . ? P2 Rh1 P1 C1 27.55(13) . . . . ? I2 Rh1 P1 C1 -166.01(13) . . . . ? C7 P1 C1 C2 47.5(3) . . . . ? C13 P1 C1 C2 154.6(2) . . . . ? Rh1 P1 C1 C2 -81.9(3) . . . . ? P1 C1 C2 C3 51.2(4) . . . . ? C1 C2 C3 C4 50.8(4) . . . . ? C2 C3 C4 P2 -114.5(3) . . . . ? C3 C4 P2 C19 -169.5(2) . . . . ? C3 C4 P2 C25 -62.0(2) . . . . ? C3 C4 P2 Rh1 58.8(2) . . . . ? C5 Rh1 P2 C19 -46.28(17) . . . . ? P1 Rh1 P2 C19 -134.51(14) . . . . ? I1 Rh1 P2 C19 53.58(13) . . . . ? I2 Rh1 P2 C19 115.51(15) . . . . ? C5 Rh1 P2 C25 -166.85(14) . . . . ? P1 Rh1 P2 C25 104.92(11) . . . . ? I1 Rh1 P2 C25 -66.99(11) . . . . ? I2 Rh1 P2 C25 -5.07(16) . . . . ? C5 Rh1 P2 C4 77.57(16) . . . . ? P1 Rh1 P2 C4 -10.66(13) . . . . ? I1 Rh1 P2 C4 177.43(13) . . . . ? I2 Rh1 P2 C4 -120.64(14) . . . . ? P2 Rh1 C5 O5 -42.0(3) . . . . ? P1 Rh1 C5 O5 57.2(3) . . . . ? I1 Rh1 C5 O5 -128.1(3) . . . . ? I2 Rh1 C5 O5 142.6(3) . . . . ? P2 Rh1 C5 C6 138.6(2) . . . . ? P1 Rh1 C5 C6 -122.3(2) . . . . ? I1 Rh1 C5 C6 52.5(3) . . . . ? I2 Rh1 C5 C6 -36.8(3) . . . . ? C13 P1 C7 C8 124.0(3) . . . . ? C1 P1 C7 C8 -132.6(3) . . . . ? Rh1 P1 C7 C8 0.9(3) . . . . ? C13 P1 C7 C12 -56.3(3) . . . . ? C1 P1 C7 C12 47.1(3) . . . . ? Rh1 P1 C7 C12 -179.4(2) . . . . ? C12 C7 C8 C9 0.5(5) . . . . ? P1 C7 C8 C9 -179.8(3) . . . . ? C7 C8 C9 C10 0.0(5) . . . . ? C8 C9 C10 C11 -0.2(5) . . . . ? C9 C10 C11 C12 0.0(5) . . . . ? C10 C11 C12 C7 0.5(5) . . . . ? C8 C7 C12 C11 -0.7(5) . . . . ? P1 C7 C12 C11 179.5(3) . . . . ? C7 P1 C13 C18 156.6(3) . . . . ? C1 P1 C13 C18 49.8(3) . . . . ? Rh1 P1 C13 C18 -79.5(3) . . . . ? C7 P1 C13 C14 -25.1(3) . . . . ? C1 P1 C13 C14 -132.0(3) . . . . ? Rh1 P1 C13 C14 98.8(3) . . . . ? C18 C13 C14 C15 0.6(5) . . . . ? P1 C13 C14 C15 -177.7(3) . . . . ? C13 C14 C15 C16 0.8(5) . . . . ? C14 C15 C16 C17 -1.4(5) . . . . ? C15 C16 C17 C18 0.7(5) . . . . ? C16 C17 C18 C13 0.6(5) . . . . ? C14 C13 C18 C17 -1.3(5) . . . . ? P1 C13 C18 C17 177.0(3) . . . . ? C25 P2 C19 C24 30.6(3) . . . . ? C4 P2 C19 C24 135.1(3) . . . . ? Rh1 P2 C19 C24 -93.0(3) . . . . ? C25 P2 C19 C20 -148.5(3) . . . . ? C4 P2 C19 C20 -44.1(3) . . . . ? Rh1 P2 C19 C20 87.9(3) . . . . ? C24 C19 C20 C21 0.2(5) . . . . ? P2 C19 C20 C21 179.4(3) . . . . ? C19 C20 C21 C22 0.0(6) . . . . ? C20 C21 C22 C23 -0.3(6) . . . . ? C21 C22 C23 C24 0.3(6) . . . . ? C20 C19 C24 C23 -0.2(5) . . . . ? P2 C19 C24 C23 -179.3(3) . . . . ? C22 C23 C24 C19 -0.1(6) . . . . ? C19 P2 C25 C30 -134.4(3) . . . . ? C4 P2 C25 C30 120.4(3) . . . . ? Rh1 P2 C25 C30 -5.9(3) . . . . ? C19 P2 C25 C26 50.5(3) . . . . ? C4 P2 C25 C26 -54.6(3) . . . . ? Rh1 P2 C25 C26 179.1(2) . . . . ? C30 C25 C26 C27 0.0(5) . . . . ? P2 C25 C26 C27 175.1(2) . . . . ? C25 C26 C27 C28 -0.4(5) . . . . ? C26 C27 C28 C29 0.8(5) . . . . ? C27 C28 C29 C30 -0.6(5) . . . . ? C26 C25 C30 C29 0.2(5) . . . . ? P2 C25 C30 C29 -174.9(3) . . . . ? C28 C29 C30 C25 0.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.670 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.102 #===END data_8 _database_code_depnum_ccdc_archive 'CCDC 658321' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H32 Cl3 I2 O P2 Rh' _chemical_formula_sum 'C35 H32 Cl3 I2 O P2 Rh' _chemical_formula_weight 993.61 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 24.241(4) _cell_length_b 18.209(3) _cell_length_c 8.1431(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3594.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 8576 _cell_measurement_theta_min 1.6800 _cell_measurement_theta_max 28.4010 _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.1100 _exptl_crystal_size_mid 0.0300 _exptl_crystal_size_min 0.0300 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.836 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 2.533 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7255 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(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 ? _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21819 _diffrn_reflns_av_R_equivalents 0.1380 _diffrn_reflns_av_sigmaI/netI 0.1189 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.31 _reflns_number_total 3338 _reflns_number_gt 2388 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0417P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3338 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1037 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1305 _refine_ls_wR_factor_gt 0.1177 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.37241(4) 0.2500 0.04921(10) 0.0217(2) Uani 1 2 d S . . I1 I 0.39853(2) 0.14927(3) 0.27957(6) 0.0294(2) Uani 1 1 d . . . P1 P 0.33886(9) 0.34734(11) -0.1025(2) 0.0223(5) Uani 1 1 d . . . C1 C 0.4372(5) 0.2500 -0.0994(15) 0.026(3) Uani 1 2 d S . . O1 O 0.4358(3) 0.2500 -0.2479(10) 0.0279(19) Uani 1 2 d S . . C2 C 0.4929(5) 0.2500 -0.0058(16) 0.043(3) Uani 1 2 d S . . H2A H 0.5234 0.2500 -0.0849 0.064 Uiso 1 2 calc SR . . H2B H 0.4952 0.2061 0.0633 0.064 Uiso 1 1 calc R . . C3 C 0.3200(3) 0.3311(4) -0.3212(9) 0.0267(19) Uani 1 1 d . . . H3A H 0.3159 0.3793 -0.3762 0.032 Uiso 1 1 calc R . . H3B H 0.3509 0.3050 -0.3753 0.032 Uiso 1 1 calc R . . C4 C 0.2680(3) 0.2876(4) -0.3482(9) 0.0238(18) Uani 1 1 d . . . C5 C 0.2189(4) 0.3252(5) -0.3827(10) 0.032(2) Uani 1 1 d . . . H5A H 0.2190 0.3773 -0.3839 0.038 Uiso 1 1 calc R . . C6 C 0.1702(3) 0.2877(5) -0.4151(10) 0.036(2) Uani 1 1 d . . . H6A H 0.1372 0.3139 -0.4372 0.043 Uiso 1 1 calc R . . C7 C 0.3867(3) 0.4237(5) -0.1266(10) 0.029(2) Uani 1 1 d . . . C8 C 0.4277(3) 0.4223(5) -0.2502(9) 0.0260(19) Uani 1 1 d . . . H8A H 0.4300 0.3815 -0.3226 0.031 Uiso 1 1 calc R . . C9 C 0.4642(3) 0.4796(5) -0.2662(10) 0.030(2) Uani 1 1 d . . . H9A H 0.4914 0.4780 -0.3501 0.036 Uiso 1 1 calc R . . C10 C 0.4620(4) 0.5402(5) -0.1610(12) 0.040(2) Uani 1 1 d . . . H10A H 0.4876 0.5793 -0.1717 0.048 Uiso 1 1 calc R . . C11 C 0.4222(4) 0.5420(5) -0.0427(12) 0.039(2) Uani 1 1 d . . . H11A H 0.4204 0.5829 0.0297 0.046 Uiso 1 1 calc R . . C12 C 0.3840(3) 0.4851(4) -0.0255(10) 0.0275(19) Uani 1 1 d . . . H12A H 0.3560 0.4884 0.0558 0.033 Uiso 1 1 calc R . . C13 C 0.2763(3) 0.3884(4) -0.0199(9) 0.0231(18) Uani 1 1 d . . . C14 C 0.2479(3) 0.3560(5) 0.1114(10) 0.031(2) Uani 1 1 d . . . H14A H 0.2641 0.3163 0.1697 0.037 Uiso 1 1 calc R . . C15 C 0.1966(4) 0.3815(5) 0.1561(11) 0.036(2) Uani 1 1 d . . . H15A H 0.1768 0.3572 0.2407 0.044 Uiso 1 1 calc R . . C16 C 0.1742(4) 0.4408(5) 0.0812(11) 0.041(2) Uani 1 1 d . . . H16A H 0.1394 0.4588 0.1168 0.050 Uiso 1 1 calc R . . C17 C 0.2016(3) 0.4759(5) -0.0482(11) 0.036(2) Uani 1 1 d . . . H17A H 0.1860 0.5173 -0.1015 0.043 Uiso 1 1 calc R . . C18 C 0.2519(3) 0.4484(5) -0.0954(9) 0.030(2) Uani 1 1 d . . . H18A H 0.2709 0.4715 -0.1834 0.036 Uiso 1 1 calc R . . C20 C 0.5391(6) 0.2500 -0.5215(16) 0.043(3) Uani 1 2 d S . . H20A H 0.4995 0.2500 -0.5562 0.052 Uiso 1 2 calc SR . . Cl1 Cl 0.58309(17) 0.2500 -0.6960(5) 0.0668(12) Uani 1 2 d S . . Cl2 Cl 0.55442(12) 0.33021(16) -0.4057(3) 0.0600(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0197(5) 0.0206(5) 0.0249(5) 0.000 0.0023(4) 0.000 I1 0.0332(4) 0.0272(4) 0.0277(4) 0.0039(2) -0.0012(2) 0.0004(3) P1 0.0177(12) 0.0193(12) 0.0298(12) 0.0010(8) 0.0021(9) 0.0006(9) C1 0.032(8) 0.013(6) 0.032(8) 0.000 -0.006(5) 0.000 O1 0.020(5) 0.032(5) 0.031(5) 0.000 0.004(4) 0.000 C2 0.013(7) 0.061(10) 0.054(9) 0.000 -0.001(6) 0.000 C3 0.035(5) 0.022(5) 0.023(5) 0.001(3) -0.005(4) 0.003(4) C4 0.021(4) 0.034(5) 0.017(5) -0.003(3) -0.001(3) 0.001(4) C5 0.042(6) 0.017(5) 0.037(5) -0.005(3) -0.010(4) -0.004(4) C6 0.014(4) 0.051(6) 0.042(6) 0.004(4) -0.001(4) 0.005(4) C7 0.027(5) 0.024(5) 0.034(5) 0.005(4) -0.004(4) -0.006(4) C8 0.028(5) 0.024(5) 0.026(5) 0.006(3) -0.003(4) -0.001(4) C9 0.017(5) 0.030(5) 0.045(6) 0.009(4) 0.002(4) 0.001(4) C10 0.023(5) 0.026(6) 0.070(7) 0.008(4) -0.002(5) -0.005(4) C11 0.033(6) 0.026(5) 0.057(6) -0.002(4) -0.008(5) -0.002(4) C12 0.022(5) 0.019(5) 0.042(5) 0.003(3) -0.009(4) -0.001(4) C13 0.010(4) 0.028(5) 0.031(5) -0.001(3) 0.003(3) -0.004(4) C14 0.021(5) 0.022(5) 0.051(6) -0.005(4) 0.006(4) -0.007(4) C15 0.027(5) 0.028(5) 0.055(6) -0.007(4) 0.016(4) -0.003(4) C16 0.028(5) 0.042(6) 0.054(7) -0.015(5) 0.012(4) -0.008(5) C17 0.025(5) 0.027(5) 0.056(6) -0.008(4) -0.013(4) 0.007(4) C18 0.032(5) 0.034(5) 0.025(5) -0.003(3) 0.005(4) 0.005(4) C20 0.039(9) 0.038(9) 0.053(9) 0.000 -0.003(7) 0.000 Cl1 0.052(3) 0.090(4) 0.058(3) 0.000 0.0007(18) 0.000 Cl2 0.0580(19) 0.0509(18) 0.0710(19) -0.0060(13) 0.0122(14) -0.0083(14) _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 C1 1.982(12) . ? Rh1 P1 2.309(2) 7_565 ? Rh1 P1 2.309(2) . ? Rh1 I1 2.6988(9) 7_565 ? Rh1 I1 2.6988(9) . ? P1 C7 1.820(8) . ? P1 C13 1.820(8) . ? P1 C3 1.862(8) . ? C1 O1 1.210(13) . ? C1 C2 1.550(16) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C3 C4 1.507(11) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C4 1.368(15) 7_565 ? C4 C5 1.400(11) . ? C5 C6 1.389(11) . ? C5 H5A 0.9500 . ? C6 C6 1.371(18) 7_565 ? C6 H6A 0.9500 . ? C7 C12 1.391(11) . ? C7 C8 1.415(11) . ? C8 C9 1.375(11) . ? C8 H8A 0.9500 . ? C9 C10 1.398(13) . ? C9 H9A 0.9500 . ? C10 C11 1.363(12) . ? C10 H10A 0.9500 . ? C11 C12 1.396(11) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C18 1.386(11) . ? C13 C14 1.401(11) . ? C14 C15 1.376(11) . ? C14 H14A 0.9500 . ? C15 C16 1.355(13) . ? C15 H15A 0.9500 . ? C16 C17 1.400(12) . ? C16 H16A 0.9500 . ? C17 C18 1.373(11) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C20 Cl1 1.777(14) . ? C20 Cl2 1.778(8) 7_565 ? C20 Cl2 1.778(8) . ? C20 H20A 1.0000 . ? 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 Rh1 P1 87.3(2) . 7_565 ? C1 Rh1 P1 87.3(2) . . ? P1 Rh1 P1 100.31(11) 7_565 . ? C1 Rh1 I1 103.8(2) . 7_565 ? P1 Rh1 I1 167.53(6) 7_565 7_565 ? P1 Rh1 I1 86.15(5) . 7_565 ? C1 Rh1 I1 103.8(2) . . ? P1 Rh1 I1 86.15(5) 7_565 . ? P1 Rh1 I1 167.53(6) . . ? I1 Rh1 I1 85.63(4) 7_565 . ? C7 P1 C13 104.9(4) . . ? C7 P1 C3 100.0(4) . . ? C13 P1 C3 102.4(4) . . ? C7 P1 Rh1 114.8(3) . . ? C13 P1 Rh1 114.3(3) . . ? C3 P1 Rh1 118.4(3) . . ? O1 C1 C2 121.0(11) . . ? O1 C1 Rh1 126.1(9) . . ? C2 C1 Rh1 112.9(8) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C3 P1 115.4(5) . . ? C4 C3 H3A 108.4 . . ? P1 C3 H3A 108.4 . . ? C4 C3 H3B 108.4 . . ? P1 C3 H3B 108.4 . . ? H3A C3 H3B 107.5 . . ? C4 C4 C5 119.3(5) 7_565 . ? C4 C4 C3 121.8(4) 7_565 . ? C5 C4 C3 118.9(7) . . ? C6 C5 C4 121.3(8) . . ? C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? C6 C6 C5 119.5(5) 7_565 . ? C6 C6 H6A 120.3 7_565 . ? C5 C6 H6A 120.3 . . ? C12 C7 C8 117.9(8) . . ? C12 C7 P1 121.4(7) . . ? C8 C7 P1 120.7(6) . . ? C9 C8 C7 120.5(8) . . ? C9 C8 H8A 119.8 . . ? C7 C8 H8A 119.8 . . ? C8 C9 C10 121.0(8) . . ? C8 C9 H9A 119.5 . . ? C10 C9 H9A 119.5 . . ? C11 C10 C9 118.7(8) . . ? C11 C10 H10A 120.6 . . ? C9 C10 H10A 120.6 . . ? C10 C11 C12 121.4(9) . . ? C10 C11 H11A 119.3 . . ? C12 C11 H11A 119.3 . . ? C7 C12 C11 120.5(8) . . ? C7 C12 H12A 119.8 . . ? C11 C12 H12A 119.8 . . ? C18 C13 C14 117.5(7) . . ? C18 C13 P1 121.0(6) . . ? C14 C13 P1 121.2(6) . . ? C15 C14 C13 120.2(8) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C16 C15 C14 120.9(9) . . ? C16 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? C15 C16 C17 120.7(9) . . ? C15 C16 H16A 119.6 . . ? C17 C16 H16A 119.6 . . ? C18 C17 C16 117.8(9) . . ? C18 C17 H17A 121.1 . . ? C16 C17 H17A 121.1 . . ? C17 C18 C13 122.8(8) . . ? C17 C18 H18A 118.6 . . ? C13 C18 H18A 118.6 . . ? Cl1 C20 Cl2 107.4(5) . 7_565 ? Cl1 C20 Cl2 107.4(5) . . ? Cl2 C20 Cl2 110.5(7) 7_565 . ? Cl1 C20 H20A 110.5 . . ? Cl2 C20 H20A 110.5 7_565 . ? Cl2 C20 H20A 110.5 . . ? 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 C7 -52.6(4) . . . . ? P1 Rh1 P1 C7 -139.4(3) 7_565 . . . ? I1 Rh1 P1 C7 51.4(3) 7_565 . . . ? I1 Rh1 P1 C7 100.2(4) . . . . ? C1 Rh1 P1 C13 -173.9(4) . . . . ? P1 Rh1 P1 C13 99.3(3) 7_565 . . . ? I1 Rh1 P1 C13 -69.9(3) 7_565 . . . ? I1 Rh1 P1 C13 -21.1(4) . . . . ? C1 Rh1 P1 C3 65.3(4) . . . . ? P1 Rh1 P1 C3 -21.4(3) 7_565 . . . ? I1 Rh1 P1 C3 169.3(3) 7_565 . . . ? I1 Rh1 P1 C3 -141.9(4) . . . . ? P1 Rh1 C1 O1 50.23(6) 7_565 . . . ? P1 Rh1 C1 O1 -50.23(6) . . . . ? I1 Rh1 C1 O1 -135.59(6) 7_565 . . . ? I1 Rh1 C1 O1 135.59(6) . . . . ? P1 Rh1 C1 C2 -129.77(6) 7_565 . . . ? P1 Rh1 C1 C2 129.77(6) . . . . ? I1 Rh1 C1 C2 44.41(6) 7_565 . . . ? I1 Rh1 C1 C2 -44.41(6) . . . . ? C7 P1 C3 C4 -161.7(6) . . . . ? C13 P1 C3 C4 -53.9(7) . . . . ? Rh1 P1 C3 C4 72.8(6) . . . . ? P1 C3 C4 C4 -85.0(6) . . . 7_565 ? P1 C3 C4 C5 98.4(8) . . . . ? C4 C4 C5 C6 0.7(9) 7_565 . . . ? C3 C4 C5 C6 177.4(7) . . . . ? C4 C5 C6 C6 -0.7(10) . . . 7_565 ? C13 P1 C7 C12 29.0(8) . . . . ? C3 P1 C7 C12 134.8(7) . . . . ? Rh1 P1 C7 C12 -97.3(7) . . . . ? C13 P1 C7 C8 -150.7(7) . . . . ? C3 P1 C7 C8 -44.9(7) . . . . ? Rh1 P1 C7 C8 83.0(7) . . . . ? C12 C7 C8 C9 1.3(12) . . . . ? P1 C7 C8 C9 -179.0(6) . . . . ? C7 C8 C9 C10 0.3(12) . . . . ? C8 C9 C10 C11 -0.9(13) . . . . ? C9 C10 C11 C12 -0.2(13) . . . . ? C8 C7 C12 C11 -2.4(12) . . . . ? P1 C7 C12 C11 177.9(6) . . . . ? C10 C11 C12 C7 1.9(13) . . . . ? C7 P1 C13 C18 51.9(7) . . . . ? C3 P1 C13 C18 -52.2(7) . . . . ? Rh1 P1 C13 C18 178.5(6) . . . . ? C7 P1 C13 C14 -134.8(7) . . . . ? C3 P1 C13 C14 121.1(7) . . . . ? Rh1 P1 C13 C14 -8.2(7) . . . . ? C18 C13 C14 C15 3.2(12) . . . . ? P1 C13 C14 C15 -170.4(6) . . . . ? C13 C14 C15 C16 -4.0(13) . . . . ? C14 C15 C16 C17 2.6(14) . . . . ? C15 C16 C17 C18 -0.4(13) . . . . ? C16 C17 C18 C13 -0.4(13) . . . . ? C14 C13 C18 C17 -1.0(12) . . . . ? P1 C13 C18 C17 172.5(6) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.230 _refine_diff_density_min -1.355 _refine_diff_density_rms 0.174 #===END