# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Matthew Clarke' 'Gareth Lamb' 'A Slawin' 'Bruce Williams' _publ_contact_author_name 'Matthew Clarke' _publ_contact_author_email MATTHEW.CLARKE@ST-ANDREWS.AC.UK _publ_section_title ; A mechanistic investigation into the elimination of phosphonium salts from rhodium-TRIPHOS complexes under methanol carbonylation conditions. ; # Attachment 'mechanistic_triphos5a.cif' data_5A _database_code_depnum_ccdc_archive 'CCDC 679097' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H43 I3 O3 P3 Rh' _chemical_formula_sum 'C37 H43 I3 O3 P3 Rh' _chemical_formula_weight 1112.23 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)/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 18.916(3) _cell_length_b 11.4403(17) _cell_length_c 20.007(4) _cell_angle_alpha 90.00 _cell_angle_beta 115.263(8) _cell_angle_gamma 90.00 _cell_volume 3915.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 5275 _cell_measurement_theta_min 1.20 _cell_measurement_theta_max 22.91 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.010 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.887 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 2.959 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7815 _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 22382 _diffrn_reflns_av_R_equivalents 0.0886 _diffrn_reflns_av_sigmaI/netI 0.0685 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 25.34 _reflns_number_total 6829 _reflns_number_gt 5151 _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. 2 solvent water molecules oxygen atoms were located, but not the associated hydrogen atoms. ; _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^)+(0.0517P)^2^+145.6472P] 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 6829 _refine_ls_number_parameters 427 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1165 _refine_ls_R_factor_gt 0.0840 _refine_ls_wR_factor_ref 0.1949 _refine_ls_wR_factor_gt 0.1749 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.141 _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 I1 I 0.16414(5) 0.17063(8) 0.13997(5) 0.0252(2) Uani 1 1 d . . . I2 I 0.01586(5) 0.42075(8) 0.10114(5) 0.0223(2) Uani 1 1 d . . . Rh1 Rh 0.05141(6) 0.22655(9) 0.18265(6) 0.0179(3) Uani 1 1 d . . . P1 P 0.0645(2) 0.0479(3) 0.23601(19) 0.0195(7) Uani 1 1 d . . . C2 C -0.0255(8) 0.0162(12) 0.2446(8) 0.023(3) Uani 1 1 d . . . H2A H -0.0641 -0.0188 0.1980 0.028 Uiso 1 1 calc R . . H2B H -0.0150 -0.0409 0.2849 0.028 Uiso 1 1 calc R . . C3 C -0.0590(8) 0.1284(12) 0.2611(8) 0.022(3) Uani 1 1 d . . . H3A H -0.0265 0.1536 0.3126 0.026 Uiso 1 1 calc R . . H3B H -0.1128 0.1143 0.2556 0.026 Uiso 1 1 calc R . . P4 P -0.0597(2) 0.2403(3) 0.1977(2) 0.0188(7) Uani 1 1 d . . . C5 C -0.0847(8) 0.3655(12) 0.2397(8) 0.021(3) Uani 1 1 d . . . H5A H -0.1225 0.3388 0.2587 0.026 Uiso 1 1 calc R . . H5B H -0.0368 0.3903 0.2829 0.026 Uiso 1 1 calc R . . C6 C -0.1184(9) 0.4703(13) 0.1926(8) 0.026(3) Uani 1 1 d . . . H6A H -0.1735 0.4534 0.1587 0.032 Uiso 1 1 calc R . . H6B H -0.0897 0.4837 0.1619 0.032 Uiso 1 1 calc R . . P7 P -0.1156(2) 0.6012(3) 0.2416(2) 0.0228(8) Uani 1 1 d . . . C8 C -0.1638(10) 0.7101(13) 0.1745(9) 0.037(4) Uani 1 1 d . . . C9 C -0.2339(14) 0.752(2) 0.1654(12) 0.065(6) Uani 1 1 d . . . H9A H -0.2559 0.7270 0.1977 0.078 Uiso 1 1 calc R . . C10 C -0.2741(16) 0.830(2) 0.1095(14) 0.082(8) Uani 1 1 d . . . H10A H -0.3249 0.8564 0.1009 0.098 Uiso 1 1 calc R . . C11 C -0.2370(16) 0.8688(16) 0.0658(11) 0.068(8) Uani 1 1 d . . . H11A H -0.2611 0.9278 0.0298 0.082 Uiso 1 1 calc R . . C12 C -0.1676(12) 0.8234(18) 0.0743(12) 0.067(7) Uani 1 1 d . . . H12A H -0.1460 0.8438 0.0408 0.080 Uiso 1 1 calc R . . C13 C -0.1291(11) 0.7486(15) 0.1308(9) 0.045(5) Uani 1 1 d . . . H13A H -0.0780 0.7228 0.1401 0.054 Uiso 1 1 calc R . . C14 C -0.0182(8) 0.6397(11) 0.2987(8) 0.019(3) Uani 1 1 d . . . C15 C -0.0009(10) 0.7066(14) 0.3618(9) 0.036(4) Uani 1 1 d . . . H15A H -0.0416 0.7283 0.3751 0.043 Uiso 1 1 calc R . . C16 C 0.0736(12) 0.7414(16) 0.4047(10) 0.047(5) Uani 1 1 d . . . H16A H 0.0843 0.7903 0.4462 0.057 Uiso 1 1 calc R . . C17 C 0.1334(9) 0.7056(14) 0.3879(9) 0.033(4) Uani 1 1 d . . . H17A H 0.1857 0.7282 0.4186 0.040 Uiso 1 1 calc R . . C18 C 0.1180(9) 0.6377(14) 0.3273(8) 0.032(4) Uani 1 1 d . . . H18A H 0.1598 0.6119 0.3166 0.038 Uiso 1 1 calc R . . C19 C 0.0437(9) 0.6064(13) 0.2819(9) 0.029(3) Uani 1 1 d . . . H19A H 0.0336 0.5619 0.2387 0.035 Uiso 1 1 calc R . . C20 C -0.1635(9) 0.5801(15) 0.2985(9) 0.032(4) Uani 1 1 d . . . H20A H -0.1341 0.5239 0.3375 0.048 Uiso 1 1 calc R . . H20B H -0.2162 0.5498 0.2690 0.048 Uiso 1 1 calc R . . H20C H -0.1670 0.6547 0.3210 0.048 Uiso 1 1 calc R . . C21 C 0.0717(8) -0.0736(13) 0.1810(7) 0.022(3) Uani 1 1 d . . . C22 C 0.1207(9) -0.1651(12) 0.2084(8) 0.027(3) Uani 1 1 d . . . H22A H 0.1563 -0.1655 0.2591 0.033 Uiso 1 1 calc R . . C23 C 0.1202(10) -0.2585(12) 0.1643(8) 0.031(4) Uani 1 1 d . . . H23A H 0.1548 -0.3224 0.1847 0.037 Uiso 1 1 calc R . . C24 C 0.0707(9) -0.2579(13) 0.0927(8) 0.028(3) Uani 1 1 d . . . H24A H 0.0701 -0.3216 0.0620 0.034 Uiso 1 1 calc R . . C25 C 0.0196(10) -0.1633(14) 0.0627(9) 0.034(4) Uani 1 1 d . . . H25A H -0.0152 -0.1623 0.0117 0.041 Uiso 1 1 calc R . . C26 C 0.0204(9) -0.0730(13) 0.1072(9) 0.031(4) Uani 1 1 d . . . H26A H -0.0146 -0.0093 0.0874 0.037 Uiso 1 1 calc R . . C27 C 0.1440(8) 0.0325(12) 0.3261(8) 0.021(3) Uani 1 1 d . . . C28 C 0.1324(10) 0.0307(15) 0.3888(8) 0.035(4) Uani 1 1 d . . . H28A H 0.0807 0.0377 0.3846 0.042 Uiso 1 1 calc R . . C29 C 0.1926(11) 0.0190(16) 0.4575(9) 0.042(4) Uani 1 1 d . . . H29A H 0.1826 0.0145 0.5000 0.051 Uiso 1 1 calc R . . C30 C 0.2677(10) 0.0139(14) 0.4639(8) 0.035(4) Uani 1 1 d . . . H30A H 0.3106 0.0088 0.5113 0.042 Uiso 1 1 calc R . . C31 C 0.2803(8) 0.0163(13) 0.4009(8) 0.026(3) Uani 1 1 d . . . H31A H 0.3319 0.0105 0.4046 0.031 Uiso 1 1 calc R . . C32 C 0.2201(8) 0.0269(13) 0.3350(8) 0.025(3) Uani 1 1 d . . . H32A H 0.2301 0.0306 0.2924 0.030 Uiso 1 1 calc R . . C33 C -0.1436(8) 0.2095(11) 0.1134(8) 0.023(3) Uani 1 1 d . . . C34 C -0.1345(9) 0.1755(12) 0.0521(8) 0.026(3) Uani 1 1 d . . . H34A H -0.0837 0.1715 0.0536 0.031 Uiso 1 1 calc R . . C35 C -0.1986(9) 0.1473(15) -0.0113(8) 0.034(4) Uani 1 1 d . . . H35A H -0.1920 0.1237 -0.0538 0.041 Uiso 1 1 calc R . . C36 C -0.2714(9) 0.1527(15) -0.0141(9) 0.036(4) Uani 1 1 d . . . H36A H -0.3155 0.1324 -0.0583 0.043 Uiso 1 1 calc R . . C37 C -0.2812(8) 0.1877(13) 0.0472(9) 0.030(3) Uani 1 1 d . . . H37A H -0.3321 0.1918 0.0455 0.036 Uiso 1 1 calc R . . C38 C -0.2183(8) 0.2159(13) 0.1093(8) 0.026(3) Uani 1 1 d . . . H38A H -0.2253 0.2408 0.1514 0.031 Uiso 1 1 calc R . . O39 O 0.0885(6) 0.3000(8) 0.3281(5) 0.027(2) Uani 1 1 d . . . C39 C 0.1093(8) 0.3009(13) 0.2780(8) 0.026(3) Uani 1 1 d . . . C40 C 0.1839(9) 0.3552(14) 0.2852(9) 0.033(4) Uani 1 1 d . . . H40A H 0.2046 0.4060 0.3288 0.049 Uiso 1 1 calc R . . H40B H 0.1742 0.4015 0.2409 0.049 Uiso 1 1 calc R . . H40C H 0.2220 0.2936 0.2906 0.049 Uiso 1 1 calc R . . I3 I -0.14694(6) -0.05678(10) 0.36290(6) 0.0378(3) Uani 1 1 d . . . O41 O -0.0043(10) 0.1708(19) 0.4609(8) 0.091(6) Uani 1 1 d . . . O42 O -0.0042(8) 0.4143(11) 0.4596(10) 0.068(5) 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 I1 0.0209(5) 0.0313(5) 0.0254(5) 0.0044(4) 0.0118(4) 0.0024(4) I2 0.0259(5) 0.0204(5) 0.0215(5) 0.0030(4) 0.0110(4) -0.0004(4) Rh1 0.0170(5) 0.0199(6) 0.0163(5) 0.0013(4) 0.0065(4) -0.0006(4) P1 0.0215(18) 0.0217(19) 0.0152(17) 0.0023(14) 0.0076(15) 0.0024(15) C2 0.024(8) 0.022(7) 0.032(8) 0.004(6) 0.020(7) -0.001(6) C3 0.027(8) 0.026(8) 0.020(7) 0.000(6) 0.016(6) -0.001(6) P4 0.0164(17) 0.0209(18) 0.0199(18) -0.0009(14) 0.0085(15) 0.0003(14) C5 0.030(8) 0.021(7) 0.020(7) 0.003(6) 0.017(6) 0.003(6) C6 0.030(8) 0.033(8) 0.015(7) 0.001(6) 0.009(6) 0.003(7) P7 0.025(2) 0.0210(19) 0.024(2) 0.0001(15) 0.0126(17) 0.0041(15) C8 0.050(11) 0.020(8) 0.027(9) -0.001(7) 0.004(8) 0.005(7) C9 0.081(16) 0.075(15) 0.047(12) 0.019(11) 0.036(12) 0.044(13) C10 0.10(2) 0.059(15) 0.076(17) 0.002(13) 0.025(15) 0.056(14) C11 0.12(2) 0.017(9) 0.028(10) -0.005(8) -0.008(12) -0.003(11) C12 0.038(11) 0.051(13) 0.067(15) 0.042(11) -0.020(10) -0.013(10) C13 0.045(11) 0.041(10) 0.030(9) 0.023(8) -0.004(8) -0.007(8) C14 0.025(7) 0.003(6) 0.025(7) 0.003(5) 0.007(6) 0.002(5) C15 0.041(10) 0.030(9) 0.037(10) -0.015(7) 0.018(8) 0.001(7) C16 0.063(13) 0.036(10) 0.038(10) -0.011(8) 0.018(10) -0.004(9) C17 0.023(8) 0.035(9) 0.037(10) 0.003(7) 0.008(7) -0.004(7) C18 0.027(8) 0.042(9) 0.027(8) 0.011(7) 0.013(7) -0.003(7) C19 0.027(8) 0.033(9) 0.030(8) -0.015(7) 0.015(7) -0.008(7) C20 0.026(8) 0.047(10) 0.028(8) -0.012(7) 0.017(7) -0.004(7) C21 0.020(7) 0.033(8) 0.015(7) 0.002(6) 0.008(6) -0.005(6) C22 0.037(9) 0.016(7) 0.024(8) -0.005(6) 0.009(7) -0.003(6) C23 0.046(10) 0.014(7) 0.022(8) -0.001(6) 0.006(7) -0.005(7) C24 0.034(9) 0.024(8) 0.028(8) -0.009(6) 0.014(7) -0.015(7) C25 0.038(9) 0.029(9) 0.031(9) -0.006(7) 0.010(7) -0.006(7) C26 0.029(8) 0.025(8) 0.033(9) 0.007(7) 0.008(7) 0.012(7) C27 0.029(8) 0.018(7) 0.018(7) 0.001(5) 0.012(6) -0.003(6) C28 0.031(9) 0.052(11) 0.019(8) -0.001(7) 0.008(7) 0.017(8) C29 0.058(12) 0.051(11) 0.023(9) -0.002(8) 0.022(8) 0.005(9) C30 0.042(10) 0.039(9) 0.016(8) -0.002(7) 0.003(7) 0.004(8) C31 0.018(7) 0.031(8) 0.024(8) 0.005(6) 0.005(6) 0.006(6) C32 0.025(8) 0.028(8) 0.015(7) 0.007(6) 0.002(6) 0.000(6) C33 0.021(7) 0.010(7) 0.037(9) 0.001(6) 0.013(7) 0.000(5) C34 0.029(8) 0.024(8) 0.031(8) -0.002(6) 0.019(7) -0.001(6) C35 0.032(9) 0.048(10) 0.021(8) 0.000(7) 0.010(7) -0.008(8) C36 0.019(8) 0.042(10) 0.030(9) 0.002(7) -0.004(7) 0.002(7) C37 0.017(7) 0.027(8) 0.035(9) 0.006(7) 0.002(7) 0.002(6) C38 0.027(8) 0.025(8) 0.031(8) 0.000(6) 0.019(7) -0.004(6) O39 0.030(6) 0.026(6) 0.020(5) 0.001(4) 0.007(5) -0.003(4) C39 0.024(8) 0.027(8) 0.018(8) 0.005(6) 0.000(6) 0.010(6) C40 0.023(8) 0.035(9) 0.035(9) -0.001(7) 0.007(7) -0.005(7) I3 0.0373(6) 0.0431(6) 0.0409(6) 0.0089(5) 0.0244(5) 0.0014(5) O41 0.085(12) 0.145(17) 0.041(9) -0.011(10) 0.026(9) 0.006(12) O42 0.044(8) 0.030(7) 0.145(15) 0.038(8) 0.056(9) 0.010(6) _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 I1 Rh1 2.6906(14) . ? I2 Rh1 2.6667(14) . ? Rh1 C39 1.945(15) . ? Rh1 P4 2.252(4) . ? Rh1 P1 2.270(4) . ? P1 C27 1.796(14) . ? P1 C21 1.812(15) . ? P1 C2 1.820(13) . ? C2 C3 1.528(19) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 P4 1.798(14) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? P4 C33 1.791(15) . ? P4 C5 1.822(14) . ? C5 C6 1.490(19) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 P7 1.778(15) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? P7 C20 1.748(14) . ? P7 C14 1.760(14) . ? P7 C8 1.772(16) . ? C8 C9 1.35(3) . ? C8 C13 1.37(3) . ? C9 C10 1.38(3) . ? C9 H9A 0.9500 . ? C10 C11 1.41(4) . ? C10 H10A 0.9500 . ? C11 C12 1.35(3) . ? C11 H11A 0.9500 . ? C12 C13 1.36(2) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.39(2) . ? C14 C19 1.401(19) . ? C15 C16 1.36(2) . ? C15 H15A 0.9500 . ? C16 C17 1.37(2) . ? C16 H16A 0.9500 . ? C17 C18 1.36(2) . ? C17 H17A 0.9500 . ? C18 C19 1.36(2) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.35(2) . ? C21 C26 1.38(2) . ? C22 C23 1.38(2) . ? C22 H22A 0.9500 . ? C23 C24 1.34(2) . ? C23 H23A 0.9500 . ? C24 C25 1.40(2) . ? C24 H24A 0.9500 . ? C25 C26 1.36(2) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C28 1.36(2) . ? C27 C32 1.38(2) . ? C28 C29 1.37(2) . ? C28 H28A 0.9500 . ? C29 C30 1.37(2) . ? C29 H29A 0.9500 . ? C30 C31 1.38(2) . ? C30 H30A 0.9500 . ? C31 C32 1.329(19) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C34 1.37(2) . ? C33 C38 1.381(19) . ? C34 C35 1.37(2) . ? C34 H34A 0.9500 . ? C35 C36 1.36(2) . ? C35 H35A 0.9500 . ? C36 C37 1.37(2) . ? C36 H36A 0.9500 . ? C37 C38 1.34(2) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? O39 C39 1.222(18) . ? C39 C40 1.49(2) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C39 Rh1 P4 90.3(5) . . ? C39 Rh1 P1 91.7(4) . . ? P4 Rh1 P1 85.46(13) . . ? C39 Rh1 I2 97.2(4) . . ? P4 Rh1 I2 91.01(10) . . ? P1 Rh1 I2 170.46(11) . . ? C39 Rh1 I1 103.0(4) . . ? P4 Rh1 I1 165.98(11) . . ? P1 Rh1 I1 89.58(10) . . ? I2 Rh1 I1 91.79(4) . . ? C27 P1 C21 106.7(6) . . ? C27 P1 C2 107.6(7) . . ? C21 P1 C2 102.7(6) . . ? C27 P1 Rh1 115.9(5) . . ? C21 P1 Rh1 115.2(5) . . ? C2 P1 Rh1 107.7(5) . . ? C3 C2 P1 110.1(9) . . ? C3 C2 H2A 109.6 . . ? P1 C2 H2A 109.6 . . ? C3 C2 H2B 109.6 . . ? P1 C2 H2B 109.6 . . ? H2A C2 H2B 108.2 . . ? C2 C3 P4 109.0(9) . . ? C2 C3 H3A 109.9 . . ? P4 C3 H3A 109.9 . . ? C2 C3 H3B 109.9 . . ? P4 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? C33 P4 C3 105.1(7) . . ? C33 P4 C5 106.8(7) . . ? C3 P4 C5 99.2(6) . . ? C33 P4 Rh1 111.3(5) . . ? C3 P4 Rh1 108.6(5) . . ? C5 P4 Rh1 123.9(5) . . ? C6 C5 P4 117.8(10) . . ? C6 C5 H5A 107.9 . . ? P4 C5 H5A 107.9 . . ? C6 C5 H5B 107.9 . . ? P4 C5 H5B 107.9 . . ? H5A C5 H5B 107.2 . . ? C5 C6 P7 115.1(10) . . ? C5 C6 H6A 108.5 . . ? P7 C6 H6A 108.5 . . ? C5 C6 H6B 108.5 . . ? P7 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? C20 P7 C14 107.6(7) . . ? C20 P7 C8 110.4(8) . . ? C14 P7 C8 111.9(7) . . ? C20 P7 C6 109.9(8) . . ? C14 P7 C6 110.2(7) . . ? C8 P7 C6 106.8(7) . . ? C9 C8 C13 120.8(17) . . ? C9 C8 P7 120.7(15) . . ? C13 C8 P7 118.5(14) . . ? C8 C9 C10 121(2) . . ? C8 C9 H9A 119.7 . . ? C10 C9 H9A 119.7 . . ? C9 C10 C11 117(2) . . ? C9 C10 H10A 121.3 . . ? C11 C10 H10A 121.3 . . ? C12 C11 C10 121.1(19) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C11 C12 C13 120(2) . . ? C11 C12 H12A 120.2 . . ? C13 C12 H12A 120.2 . . ? C12 C13 C8 120(2) . . ? C12 C13 H13A 119.9 . . ? C8 C13 H13A 119.9 . . ? C15 C14 C19 118.0(13) . . ? C15 C14 P7 120.2(11) . . ? C19 C14 P7 121.8(11) . . ? C16 C15 C14 120.9(15) . . ? C16 C15 H15A 119.5 . . ? C14 C15 H15A 119.5 . . ? C15 C16 C17 119.9(16) . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C18 C17 C16 120.1(15) . . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C19 C18 C17 120.9(15) . . ? C19 C18 H18A 119.6 . . ? C17 C18 H18A 119.6 . . ? C18 C19 C14 120.1(14) . . ? C18 C19 H19A 120.0 . . ? C14 C19 H19A 120.0 . . ? P7 C20 H20A 109.5 . . ? P7 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? P7 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C26 119.0(14) . . ? C22 C21 P1 124.4(11) . . ? C26 C21 P1 116.5(11) . . ? C21 C22 C23 121.6(14) . . ? C21 C22 H22A 119.2 . . ? C23 C22 H22A 119.2 . . ? C24 C23 C22 119.4(15) . . ? C24 C23 H23A 120.3 . . ? C22 C23 H23A 120.3 . . ? C23 C24 C25 120.1(14) . . ? C23 C24 H24A 119.9 . . ? C25 C24 H24A 119.9 . . ? C26 C25 C24 119.5(15) . . ? C26 C25 H25A 120.2 . . ? C24 C25 H25A 120.2 . . ? C25 C26 C21 120.2(14) . . ? C25 C26 H26A 119.9 . . ? C21 C26 H26A 119.9 . . ? C28 C27 C32 116.8(14) . . ? C28 C27 P1 122.1(12) . . ? C32 C27 P1 121.0(10) . . ? C27 C28 C29 122.3(16) . . ? C27 C28 H28A 118.8 . . ? C29 C28 H28A 118.8 . . ? C28 C29 C30 119.0(15) . . ? C28 C29 H29A 120.5 . . ? C30 C29 H29A 120.5 . . ? C29 C30 C31 119.2(15) . . ? C29 C30 H30A 120.4 . . ? C31 C30 H30A 120.4 . . ? C32 C31 C30 120.0(14) . . ? C32 C31 H31A 120.0 . . ? C30 C31 H31A 120.0 . . ? C31 C32 C27 122.6(14) . . ? C31 C32 H32A 118.7 . . ? C27 C32 H32A 118.7 . . ? C34 C33 C38 118.7(14) . . ? C34 C33 P4 120.0(11) . . ? C38 C33 P4 121.3(12) . . ? C33 C34 C35 119.9(14) . . ? C33 C34 H34A 120.1 . . ? C35 C34 H34A 120.1 . . ? C36 C35 C34 120.7(15) . . ? C36 C35 H35A 119.7 . . ? C34 C35 H35A 119.7 . . ? C35 C36 C37 119.9(15) . . ? C35 C36 H36A 120.1 . . ? C37 C36 H36A 120.1 . . ? C38 C37 C36 119.4(14) . . ? C38 C37 H37A 120.3 . . ? C36 C37 H37A 120.3 . . ? C37 C38 C33 121.5(15) . . ? C37 C38 H38A 119.3 . . ? C33 C38 H38A 119.3 . . ? O39 C39 C40 123.2(14) . . ? O39 C39 Rh1 123.9(12) . . ? C40 C39 Rh1 112.9(11) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? 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 C39 Rh1 P1 C27 -21.8(7) . . . . ? P4 Rh1 P1 C27 -112.0(5) . . . . ? I1 Rh1 P1 C27 81.2(5) . . . . ? C39 Rh1 P1 C21 -147.4(7) . . . . ? P4 Rh1 P1 C21 122.5(5) . . . . ? I1 Rh1 P1 C21 -44.4(5) . . . . ? C39 Rh1 P1 C2 98.7(7) . . . . ? P4 Rh1 P1 C2 8.5(5) . . . . ? I1 Rh1 P1 C2 -158.3(5) . . . . ? C27 P1 C2 C3 90.5(11) . . . . ? C21 P1 C2 C3 -157.2(10) . . . . ? Rh1 P1 C2 C3 -35.1(11) . . . . ? P1 C2 C3 P4 48.0(12) . . . . ? C2 C3 P4 C33 79.2(11) . . . . ? C2 C3 P4 C5 -170.6(10) . . . . ? C2 C3 P4 Rh1 -40.0(11) . . . . ? C39 Rh1 P4 C33 167.8(6) . . . . ? P1 Rh1 P4 C33 -100.5(5) . . . . ? I2 Rh1 P4 C33 70.6(5) . . . . ? I1 Rh1 P4 C33 -30.9(7) . . . . ? C39 Rh1 P4 C3 -77.0(7) . . . . ? P1 Rh1 P4 C3 14.7(5) . . . . ? I2 Rh1 P4 C3 -174.2(5) . . . . ? I1 Rh1 P4 C3 84.3(7) . . . . ? C39 Rh1 P4 C5 38.4(7) . . . . ? P1 Rh1 P4 C5 130.1(6) . . . . ? I2 Rh1 P4 C5 -58.8(5) . . . . ? I1 Rh1 P4 C5 -160.3(6) . . . . ? C33 P4 C5 C6 -50.4(13) . . . . ? C3 P4 C5 C6 -159.3(11) . . . . ? Rh1 P4 C5 C6 80.8(12) . . . . ? P4 C5 C6 P7 -162.9(8) . . . . ? C5 C6 P7 C20 -56.7(13) . . . . ? C5 C6 P7 C14 61.7(13) . . . . ? C5 C6 P7 C8 -176.5(12) . . . . ? C20 P7 C8 C9 -9.7(19) . . . . ? C14 P7 C8 C9 -129.5(16) . . . . ? C6 P7 C8 C9 109.8(17) . . . . ? C20 P7 C8 C13 172.1(14) . . . . ? C14 P7 C8 C13 52.3(16) . . . . ? C6 P7 C8 C13 -68.4(15) . . . . ? C13 C8 C9 C10 3(3) . . . . ? P7 C8 C9 C10 -175.1(18) . . . . ? C8 C9 C10 C11 -4(4) . . . . ? C9 C10 C11 C12 6(3) . . . . ? C10 C11 C12 C13 -7(3) . . . . ? C11 C12 C13 C8 7(3) . . . . ? C9 C8 C13 C12 -5(3) . . . . ? P7 C8 C13 C12 173.7(16) . . . . ? C20 P7 C14 C15 -34.4(14) . . . . ? C8 P7 C14 C15 87.1(14) . . . . ? C6 P7 C14 C15 -154.2(12) . . . . ? C20 P7 C14 C19 146.7(12) . . . . ? C8 P7 C14 C19 -91.8(13) . . . . ? C6 P7 C14 C19 26.9(14) . . . . ? C19 C14 C15 C16 2(2) . . . . ? P7 C14 C15 C16 -177.1(14) . . . . ? C14 C15 C16 C17 -3(3) . . . . ? C15 C16 C17 C18 2(3) . . . . ? C16 C17 C18 C19 1(3) . . . . ? C17 C18 C19 C14 -3(2) . . . . ? C15 C14 C19 C18 1(2) . . . . ? P7 C14 C19 C18 -179.9(12) . . . . ? C27 P1 C21 C22 9.2(14) . . . . ? C2 P1 C21 C22 -103.8(13) . . . . ? Rh1 P1 C21 C22 139.4(11) . . . . ? C27 P1 C21 C26 -174.0(11) . . . . ? C2 P1 C21 C26 73.0(12) . . . . ? Rh1 P1 C21 C26 -43.8(12) . . . . ? C26 C21 C22 C23 0(2) . . . . ? P1 C21 C22 C23 176.2(12) . . . . ? C21 C22 C23 C24 1(2) . . . . ? C22 C23 C24 C25 0(2) . . . . ? C23 C24 C25 C26 -1(2) . . . . ? C24 C25 C26 C21 1(2) . . . . ? C22 C21 C26 C25 0(2) . . . . ? P1 C21 C26 C25 -177.3(12) . . . . ? C21 P1 C27 C28 -126.0(13) . . . . ? C2 P1 C27 C28 -16.4(15) . . . . ? Rh1 P1 C27 C28 104.2(13) . . . . ? C21 P1 C27 C32 56.7(13) . . . . ? C2 P1 C27 C32 166.3(12) . . . . ? Rh1 P1 C27 C32 -73.1(13) . . . . ? C32 C27 C28 C29 -3(2) . . . . ? P1 C27 C28 C29 180.0(14) . . . . ? C27 C28 C29 C30 3(3) . . . . ? C28 C29 C30 C31 -2(3) . . . . ? C29 C30 C31 C32 2(2) . . . . ? C30 C31 C32 C27 -2(2) . . . . ? C28 C27 C32 C31 2(2) . . . . ? P1 C27 C32 C31 179.5(12) . . . . ? C3 P4 C33 C34 -113.6(12) . . . . ? C5 P4 C33 C34 141.7(11) . . . . ? Rh1 P4 C33 C34 3.8(13) . . . . ? C3 P4 C33 C38 64.4(13) . . . . ? C5 P4 C33 C38 -40.3(13) . . . . ? Rh1 P4 C33 C38 -178.2(10) . . . . ? C38 C33 C34 C35 -1(2) . . . . ? P4 C33 C34 C35 177.2(12) . . . . ? C33 C34 C35 C36 0(2) . . . . ? C34 C35 C36 C37 0(3) . . . . ? C35 C36 C37 C38 0(2) . . . . ? C36 C37 C38 C33 -1(2) . . . . ? C34 C33 C38 C37 1(2) . . . . ? P4 C33 C38 C37 -176.9(11) . . . . ? P4 Rh1 C39 O39 24.3(12) . . . . ? P1 Rh1 C39 O39 -61.1(12) . . . . ? I2 Rh1 C39 O39 115.4(12) . . . . ? I1 Rh1 C39 O39 -151.1(11) . . . . ? P4 Rh1 C39 C40 -158.2(10) . . . . ? P1 Rh1 C39 C40 116.3(10) . . . . ? I2 Rh1 C39 C40 -67.1(10) . . . . ? I1 Rh1 C39 C40 26.4(11) . . . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.766 _refine_diff_density_min -2.592 _refine_diff_density_rms 0.274