# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'J Vicente' _publ_contact_author_email JVS1@UM.ES loop_ _publ_author_name J.Vicente D.Bautista J.Gil-Rubio J.Guerrero-Leal data_jg360bs _database_code_depnum_ccdc_archive 'CCDC 714350' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H45 F3 I2 P3 Rh' _chemical_formula_weight 1056.40 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' F F 0.0171 0.0103 '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 'P 2(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 10.2462(7) _cell_length_b 17.9511(12) _cell_length_c 22.2871(15) _cell_angle_alpha 90.00 _cell_angle_beta 99.995(2) _cell_angle_gamma 90.00 _cell_volume 4037.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8549 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 28.1 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 2.115 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5248 _exptl_absorpt_correction_T_max 0.8163 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46031 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0176 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 28.22 _reflns_number_total 9381 _reflns_number_gt 9079 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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. The largest feature of residual electron density was 2.46eA^3 at 0.79A of I2,and this large peak may be due to residual absorption or unidentified disorder effects. One iodine and the CF3 ligand are disordered over two positions, 72:28%. ; _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^)+(0.0317P)^2^+7.0485P] 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 'Rigid methyls, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9381 _refine_ls_number_parameters 491 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0750 _refine_ls_wR_factor_gt 0.0742 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.153 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.877881(19) 0.259889(12) 0.183386(9) 0.01667(6) Uani 1 1 d . . . I2 I 0.667052(17) 0.307705(10) 0.088755(8) 0.02180(6) Uani 1 1 d . A . P2 P 0.80884(6) 0.34734(4) 0.25045(3) 0.01606(13) Uani 1 1 d . A . P3 P 0.37633(7) 0.54305(4) 0.10645(3) 0.02295(15) Uani 1 1 d . . . P5 P 0.94427(7) 0.17953(4) 0.10994(3) 0.01656(13) Uani 1 1 d . A . C2 C 1.0431(3) 0.22878(17) 0.24833(14) 0.0266(6) Uani 1 1 d . A . H2A H 1.0321 0.2472 0.2886 0.040 Uiso 1 1 calc R . . H2B H 1.1235 0.2503 0.2372 0.040 Uiso 1 1 calc R . . H2C H 1.0507 0.1744 0.2495 0.040 Uiso 1 1 calc R . . C11 C 0.8471(3) 0.09541(16) 0.08492(12) 0.0203(5) Uani 1 1 d . . . C12 C 0.9029(3) 0.03604(18) 0.05806(14) 0.0280(6) Uani 1 1 d . A . H12 H 0.9945 0.0372 0.0555 0.034 Uiso 1 1 calc R . . C13 C 0.8263(3) -0.02493(18) 0.03497(15) 0.0309(7) Uani 1 1 d . . . H13 H 0.8658 -0.0650 0.0168 0.037 Uiso 1 1 calc R A . C14 C 0.6932(3) -0.02750(17) 0.03836(14) 0.0298(7) Uani 1 1 d . A . H14 H 0.6410 -0.0690 0.0224 0.036 Uiso 1 1 calc R . . C15 C 0.6371(3) 0.03014(18) 0.06483(14) 0.0288(7) Uani 1 1 d . . . H15 H 0.5456 0.0282 0.0675 0.035 Uiso 1 1 calc R A . C16 C 0.7124(3) 0.09200(17) 0.08798(13) 0.0244(6) Uani 1 1 d . A . H16 H 0.6716 0.1319 0.1059 0.029 Uiso 1 1 calc R . . C21 C 1.1119(3) 0.14253(15) 0.12989(12) 0.0185(5) Uani 1 1 d . . . C22 C 1.1368(3) 0.08123(16) 0.16851(13) 0.0227(6) Uani 1 1 d . A . H22 H 1.0659 0.0582 0.1839 0.027 Uiso 1 1 calc R . . C23 C 1.2650(3) 0.05358(17) 0.18465(15) 0.0274(6) Uani 1 1 d . . . H23 H 1.2808 0.0110 0.2102 0.033 Uiso 1 1 calc R A . C24 C 1.3692(3) 0.08758(18) 0.16373(15) 0.0293(7) Uani 1 1 d . A . H24 H 1.4565 0.0685 0.1749 0.035 Uiso 1 1 calc R . . C25 C 1.3464(3) 0.14936(18) 0.12653(16) 0.0308(7) Uani 1 1 d . . . H25 H 1.4183 0.1734 0.1127 0.037 Uiso 1 1 calc R A . C26 C 1.2186(3) 0.17643(17) 0.10936(14) 0.0257(6) Uani 1 1 d . A . H26 H 1.2034 0.2186 0.0833 0.031 Uiso 1 1 calc R . . C31 C 0.9460(3) 0.22084(17) 0.03495(12) 0.0225(6) Uani 1 1 d . . . H31A H 0.9959 0.2677 0.0398 0.034 Uiso 1 1 calc R A . H31B H 0.8549 0.2307 0.0147 0.034 Uiso 1 1 calc R . . H31C H 0.9883 0.1863 0.0102 0.034 Uiso 1 1 calc R . . C41 C 0.9087(3) 0.34811(15) 0.32697(12) 0.0183(5) Uani 1 1 d . . . C42 C 0.8793(3) 0.30181(16) 0.37308(14) 0.0250(6) Uani 1 1 d . A . H42 H 0.8010 0.2724 0.3662 0.030 Uiso 1 1 calc R . . C43 C 0.9638(3) 0.29843(19) 0.42900(14) 0.0323(7) Uani 1 1 d . . . H43 H 0.9430 0.2668 0.4602 0.039 Uiso 1 1 calc R A . C44 C 1.0781(3) 0.3409(2) 0.43953(15) 0.0356(8) Uani 1 1 d . A . H44 H 1.1360 0.3380 0.4777 0.043 Uiso 1 1 calc R . . C45 C 1.1078(3) 0.38733(19) 0.39495(16) 0.0341(8) Uani 1 1 d . . . H45 H 1.1856 0.4171 0.4025 0.041 Uiso 1 1 calc R A . C46 C 1.0239(3) 0.39097(16) 0.33840(14) 0.0250(6) Uani 1 1 d . A . H46 H 1.0456 0.4228 0.3075 0.030 Uiso 1 1 calc R . . C51 C 0.6384(3) 0.34594(15) 0.26574(13) 0.0188(5) Uani 1 1 d . . . C52 C 0.5363(3) 0.30926(15) 0.22713(13) 0.0206(5) Uani 1 1 d . A . H52 H 0.5565 0.2786 0.1953 0.025 Uiso 1 1 calc R . . C53 C 0.4048(3) 0.31743(16) 0.23508(14) 0.0238(6) Uani 1 1 d . . . H53 H 0.3360 0.2928 0.2083 0.029 Uiso 1 1 calc R A . C54 C 0.3743(3) 0.36102(16) 0.28165(14) 0.0253(6) Uani 1 1 d . A . H54 H 0.2846 0.3670 0.2866 0.030 Uiso 1 1 calc R . . C55 C 0.4753(3) 0.39635(16) 0.32151(15) 0.0262(6) Uani 1 1 d . . . H55 H 0.4546 0.4251 0.3544 0.031 Uiso 1 1 calc R A . C56 C 0.6062(3) 0.38972(16) 0.31326(14) 0.0237(6) Uani 1 1 d . A . H56 H 0.6742 0.4150 0.3400 0.028 Uiso 1 1 calc R . . C61 C 0.8139(3) 0.44484(15) 0.22651(14) 0.0233(6) Uani 1 1 d . . . H61A H 0.7806 0.4769 0.2561 0.035 Uiso 1 1 calc R A . H61B H 0.7584 0.4511 0.1864 0.035 Uiso 1 1 calc R . . H61C H 0.9055 0.4587 0.2243 0.035 Uiso 1 1 calc R . . C71 C 0.2994(3) 0.47699(16) 0.05144(14) 0.0235(6) Uani 1 1 d . . . C72 C 0.3270(3) 0.40149(17) 0.05800(14) 0.0275(6) Uani 1 1 d . . . H72 H 0.3858 0.3838 0.0927 0.033 Uiso 1 1 calc R . . C73 C 0.2686(3) 0.35231(18) 0.01396(16) 0.0312(7) Uani 1 1 d . . . H73 H 0.2876 0.3006 0.0182 0.037 Uiso 1 1 calc R . . C74 C 0.1830(3) 0.3778(2) -0.03610(18) 0.0397(8) Uani 1 1 d . . . H74 H 0.1421 0.3433 -0.0659 0.048 Uiso 1 1 calc R . . C75 C 0.1553(3) 0.4532(2) -0.04371(17) 0.0409(8) Uani 1 1 d . . . H75 H 0.0969 0.4703 -0.0788 0.049 Uiso 1 1 calc R . . C76 C 0.2133(3) 0.50319(19) 0.00016(16) 0.0333(7) Uani 1 1 d . . . H76 H 0.1948 0.5549 -0.0045 0.040 Uiso 1 1 calc R . . C81 C 0.2519(3) 0.60432(16) 0.12465(13) 0.0235(6) Uani 1 1 d . . . C82 C 0.1582(3) 0.57616(18) 0.15741(14) 0.0282(6) Uani 1 1 d . . . H82 H 0.1612 0.5254 0.1695 0.034 Uiso 1 1 calc R . . C83 C 0.0609(3) 0.6228(2) 0.17211(15) 0.0330(7) Uani 1 1 d . . . H83 H -0.0023 0.6041 0.1949 0.040 Uiso 1 1 calc R . . C84 C 0.0553(3) 0.69672(19) 0.15369(15) 0.0316(7) Uani 1 1 d . . . H84 H -0.0117 0.7286 0.1637 0.038 Uiso 1 1 calc R . . C85 C 0.1474(3) 0.72382(18) 0.12080(15) 0.0323(7) Uani 1 1 d . . . H85 H 0.1427 0.7744 0.1079 0.039 Uiso 1 1 calc R . . C86 C 0.2464(3) 0.67830(17) 0.10631(14) 0.0279(6) Uani 1 1 d . . . H86 H 0.3100 0.6975 0.0840 0.034 Uiso 1 1 calc R . . C91 C 0.4989(3) 0.59435(19) 0.07552(16) 0.0320(7) Uani 1 1 d . . . H91A H 0.4570 0.6199 0.0383 0.048 Uiso 1 1 calc R . . H91B H 0.5669 0.5601 0.0660 0.048 Uiso 1 1 calc R . . H91C H 0.5400 0.6312 0.1054 0.048 Uiso 1 1 calc R . . C92 C 0.4566(4) 0.4967(2) 0.17351(15) 0.0355(7) Uani 1 1 d . . . H92A H 0.4986 0.5337 0.2031 0.053 Uiso 1 1 calc R . . H92B H 0.5243 0.4628 0.1631 0.053 Uiso 1 1 calc R . . H92C H 0.3911 0.4682 0.1913 0.053 Uiso 1 1 calc R . . I1 I 1.04175(3) 0.364674(15) 0.146324(13) 0.02150(9) Uani 0.7177(9) 1 d P A 1 C1 C 0.7848(5) 0.1759(3) 0.2221(3) 0.0203(10) Uani 0.7177(9) 1 d P A 1 F1 F 0.8406(2) 0.10552(12) 0.22091(10) 0.0218(5) Uani 0.7177(9) 1 d P A 1 F2 F 0.6526(2) 0.16100(13) 0.20067(11) 0.0246(5) Uani 0.7177(9) 1 d P A 1 F3 F 0.7831(3) 0.18327(13) 0.28444(11) 0.0256(5) Uani 0.7177(9) 1 d P A 1 I1' I 0.76710(8) 0.15496(5) 0.24133(4) 0.0201(2) Uani 0.2823(9) 1 d P A 2 C1' C 1.0011(17) 0.3428(10) 0.1589(7) 0.041(4) Uiso 0.2823(9) 1 d P A 2 F1' F 1.1116(6) 0.3201(3) 0.1295(3) 0.0266(13) Uiso 0.2823(9) 1 d P A 2 F2' F 0.9543(6) 0.3987(4) 0.1159(3) 0.0305(14) Uiso 0.2823(9) 1 d P A 2 F3' F 1.0749(6) 0.3889(3) 0.2030(3) 0.0263(13) Uiso 0.2823(9) 1 d P A 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 0.01379(10) 0.01870(11) 0.01627(10) -0.00080(7) -0.00089(7) 0.00426(7) I2 0.01723(9) 0.02582(10) 0.02052(9) 0.00338(7) -0.00181(7) 0.00383(6) P2 0.0124(3) 0.0158(3) 0.0193(3) -0.0010(2) 0.0007(2) 0.0013(2) P3 0.0212(3) 0.0237(4) 0.0223(3) 0.0031(3) -0.0007(3) -0.0010(3) P5 0.0150(3) 0.0179(3) 0.0166(3) 0.0002(2) 0.0021(2) 0.0004(2) C2 0.0228(14) 0.0281(15) 0.0246(14) -0.0054(12) -0.0073(11) 0.0103(12) C11 0.0191(13) 0.0222(13) 0.0191(13) 0.0011(10) 0.0025(10) -0.0041(10) C12 0.0269(15) 0.0293(15) 0.0298(15) -0.0049(12) 0.0102(12) -0.0055(12) C13 0.0361(17) 0.0250(15) 0.0333(16) -0.0052(13) 0.0108(13) -0.0057(13) C14 0.0339(16) 0.0266(15) 0.0259(15) 0.0048(12) -0.0031(12) -0.0144(13) C15 0.0205(14) 0.0358(17) 0.0277(15) 0.0084(13) -0.0026(12) -0.0084(12) C16 0.0197(13) 0.0293(15) 0.0232(14) 0.0031(11) 0.0010(11) -0.0022(11) C21 0.0147(12) 0.0189(12) 0.0216(13) -0.0040(10) 0.0024(10) 0.0003(10) C22 0.0195(13) 0.0231(14) 0.0265(14) -0.0005(11) 0.0070(11) 0.0007(11) C23 0.0233(14) 0.0253(15) 0.0325(16) 0.0013(12) 0.0023(12) 0.0041(11) C24 0.0163(13) 0.0321(16) 0.0384(17) -0.0042(13) 0.0016(12) 0.0062(12) C25 0.0180(14) 0.0333(16) 0.0420(18) -0.0026(14) 0.0078(13) -0.0029(12) C26 0.0220(14) 0.0231(14) 0.0323(16) 0.0019(12) 0.0054(12) -0.0027(11) C31 0.0241(14) 0.0261(14) 0.0179(13) 0.0035(11) 0.0050(11) -0.0004(11) C41 0.0155(12) 0.0161(12) 0.0221(13) -0.0052(10) 0.0003(10) 0.0036(10) C42 0.0250(14) 0.0229(14) 0.0269(15) -0.0012(11) 0.0044(12) 0.0045(11) C43 0.0414(18) 0.0328(17) 0.0233(15) 0.0010(13) 0.0067(13) 0.0155(14) C44 0.0381(18) 0.0372(18) 0.0263(16) -0.0128(14) -0.0085(13) 0.0201(15) C45 0.0214(14) 0.0331(17) 0.0424(19) -0.0145(15) -0.0095(13) 0.0031(12) C46 0.0197(13) 0.0230(14) 0.0305(15) -0.0037(12) -0.0005(11) 0.0007(11) C51 0.0148(12) 0.0173(12) 0.0241(13) 0.0007(10) 0.0035(10) 0.0021(10) C52 0.0182(13) 0.0200(13) 0.0230(13) 0.0002(10) 0.0019(10) 0.0001(10) C53 0.0156(12) 0.0241(14) 0.0302(15) 0.0032(12) 0.0001(11) -0.0038(10) C54 0.0154(12) 0.0248(14) 0.0364(16) 0.0028(12) 0.0062(11) 0.0030(11) C55 0.0243(14) 0.0209(14) 0.0356(16) -0.0039(12) 0.0112(12) 0.0024(11) C56 0.0186(13) 0.0213(14) 0.0312(15) -0.0059(12) 0.0041(11) -0.0009(10) C61 0.0238(14) 0.0168(13) 0.0295(15) 0.0031(11) 0.0053(11) 0.0032(10) C71 0.0189(13) 0.0246(14) 0.0270(14) -0.0011(11) 0.0044(11) -0.0017(11) C72 0.0270(15) 0.0268(15) 0.0311(16) 0.0049(12) 0.0118(12) 0.0021(12) C73 0.0329(16) 0.0239(15) 0.0416(18) -0.0023(13) 0.0194(14) -0.0048(12) C74 0.0325(17) 0.0399(19) 0.046(2) -0.0153(16) 0.0054(15) -0.0116(15) C75 0.0312(17) 0.044(2) 0.041(2) -0.0075(16) -0.0104(15) 0.0041(15) C76 0.0310(16) 0.0277(16) 0.0376(18) -0.0010(14) -0.0039(14) 0.0027(13) C81 0.0234(13) 0.0250(14) 0.0209(13) -0.0010(11) 0.0004(11) -0.0019(11) C82 0.0303(15) 0.0264(15) 0.0273(15) 0.0011(12) 0.0033(12) -0.0045(12) C83 0.0260(15) 0.0420(19) 0.0314(16) -0.0029(14) 0.0058(13) -0.0070(13) C84 0.0291(16) 0.0334(17) 0.0309(16) -0.0099(13) 0.0010(13) 0.0034(13) C85 0.0410(18) 0.0252(15) 0.0293(16) -0.0004(13) 0.0020(14) 0.0004(13) C86 0.0331(16) 0.0253(15) 0.0251(15) 0.0015(12) 0.0041(12) -0.0032(12) C91 0.0252(15) 0.0356(17) 0.0363(17) 0.0008(14) 0.0080(13) -0.0061(13) C92 0.0363(17) 0.0383(18) 0.0276(16) 0.0090(14) -0.0064(13) 0.0042(14) I1 0.01827(14) 0.01887(14) 0.02821(15) 0.00167(10) 0.00639(10) -0.00264(10) C1 0.022(2) 0.017(2) 0.023(3) -0.0005(19) 0.0073(19) -0.0055(18) F1 0.0242(11) 0.0148(10) 0.0258(11) 0.0045(9) 0.0028(9) -0.0003(9) F2 0.0169(11) 0.0236(12) 0.0333(13) 0.0018(10) 0.0044(9) -0.0043(9) F3 0.0375(14) 0.0231(12) 0.0178(12) -0.0008(10) 0.0091(10) -0.0067(10) I1' 0.0192(4) 0.0169(4) 0.0246(5) 0.0019(3) 0.0051(3) -0.0016(3) _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 2.052(6) . ? Rh1 C1' 2.08(2) . ? Rh1 C2 2.103(3) . ? Rh1 P2 2.3591(7) . ? Rh1 P5 2.3684(7) . ? Rh1 I1' 2.6482(10) . ? Rh1 I1 2.7425(4) . ? Rh1 I2 2.8757(3) . ? P2 C41 1.830(3) . ? P2 C61 1.833(3) . ? P2 C51 1.837(3) . ? P3 C92 1.782(3) . ? P3 C81 1.783(3) . ? P3 C71 1.787(3) . ? P3 C91 1.789(3) . ? P5 C21 1.823(3) . ? P5 C31 1.831(3) . ? P5 C11 1.841(3) . ? C11 C12 1.393(4) . ? C11 C16 1.396(4) . ? C12 C13 1.393(4) . ? C13 C14 1.379(5) . ? C14 C15 1.367(5) . ? C15 C16 1.399(4) . ? C21 C22 1.393(4) . ? C21 C26 1.395(4) . ? C22 C23 1.391(4) . ? C23 C24 1.380(4) . ? C24 C25 1.380(5) . ? C25 C26 1.387(4) . ? C41 C42 1.395(4) . ? C41 C46 1.395(4) . ? C42 C43 1.390(4) . ? C43 C44 1.383(5) . ? C44 C45 1.371(5) . ? C45 C46 1.398(4) . ? C51 C52 1.399(4) . ? C51 C56 1.403(4) . ? C52 C53 1.397(4) . ? C53 C54 1.378(4) . ? C54 C55 1.394(4) . ? C55 C56 1.390(4) . ? C71 C72 1.387(4) . ? C71 C76 1.399(4) . ? C72 C73 1.377(5) . ? C73 C74 1.372(5) . ? C74 C75 1.387(5) . ? C75 C76 1.383(5) . ? C81 C86 1.388(4) . ? C81 C82 1.398(4) . ? C82 C83 1.384(5) . ? C83 C84 1.387(5) . ? C84 C85 1.380(5) . ? C85 C86 1.384(5) . ? C1 F2 1.382(5) . ? C1 F1 1.389(6) . ? C1 F3 1.400(6) . ? C1' F3' 1.401(17) . ? C1' F2' 1.413(18) . ? C1' F1' 1.460(18) . ? 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 C1' 168.9(4) . . ? C1 Rh1 C2 83.87(17) . . ? C1' Rh1 C2 85.3(4) . . ? C1 Rh1 P2 90.60(14) . . ? C1' Rh1 P2 87.3(4) . . ? C2 Rh1 P2 91.99(8) . . ? C1 Rh1 P5 93.04(14) . . ? C1' Rh1 P5 89.7(4) . . ? C2 Rh1 P5 91.18(8) . . ? P2 Rh1 P5 175.42(3) . . ? C1 Rh1 I1' 4.28(15) . . ? C1' Rh1 I1' 165.0(4) . . ? C2 Rh1 I1' 80.64(10) . . ? P2 Rh1 I1' 87.90(3) . . ? P5 Rh1 I1' 95.89(3) . . ? C1 Rh1 I1 169.71(15) . . ? C1' Rh1 I1 2.9(4) . . ? C2 Rh1 I1 85.85(9) . . ? P2 Rh1 I1 90.058(19) . . ? P5 Rh1 I1 86.864(19) . . ? I1' Rh1 I1 166.26(2) . . ? C1 Rh1 I2 100.52(15) . . ? C1' Rh1 I2 90.4(4) . . ? C2 Rh1 I2 175.25(9) . . ? P2 Rh1 I2 89.790(18) . . ? P5 Rh1 I2 86.802(18) . . ? I1' Rh1 I2 103.826(19) . . ? I1 Rh1 I2 89.749(10) . . ? C41 P2 C61 102.96(13) . . ? C41 P2 C51 102.87(13) . . ? C61 P2 C51 98.22(13) . . ? C41 P2 Rh1 114.51(8) . . ? C61 P2 Rh1 115.10(10) . . ? C51 P2 Rh1 120.52(9) . . ? C92 P3 C81 109.96(16) . . ? C92 P3 C71 110.50(16) . . ? C81 P3 C71 108.53(13) . . ? C92 P3 C91 108.09(17) . . ? C81 P3 C91 110.35(15) . . ? C71 P3 C91 109.42(15) . . ? C21 P5 C31 102.24(13) . . ? C21 P5 C11 102.23(13) . . ? C31 P5 C11 98.40(13) . . ? C21 P5 Rh1 115.14(9) . . ? C31 P5 Rh1 115.70(10) . . ? C11 P5 Rh1 120.26(9) . . ? C12 C11 C16 118.1(3) . . ? C12 C11 P5 121.1(2) . . ? C16 C11 P5 120.6(2) . . ? C11 C12 C13 120.9(3) . . ? C14 C13 C12 120.4(3) . . ? C15 C14 C13 119.5(3) . . ? C14 C15 C16 120.9(3) . . ? C11 C16 C15 120.3(3) . . ? C22 C21 C26 118.5(3) . . ? C22 C21 P5 120.1(2) . . ? C26 C21 P5 121.3(2) . . ? C23 C22 C21 120.3(3) . . ? C24 C23 C22 120.4(3) . . ? C23 C24 C25 119.9(3) . . ? C24 C25 C26 120.0(3) . . ? C25 C26 C21 120.8(3) . . ? C42 C41 C46 118.6(3) . . ? C42 C41 P2 121.7(2) . . ? C46 C41 P2 119.5(2) . . ? C43 C42 C41 120.4(3) . . ? C44 C43 C42 120.4(3) . . ? C45 C44 C43 120.0(3) . . ? C44 C45 C46 120.2(3) . . ? C41 C46 C45 120.5(3) . . ? C52 C51 C56 118.6(2) . . ? C52 C51 P2 121.7(2) . . ? C56 C51 P2 119.2(2) . . ? C53 C52 C51 120.5(3) . . ? C54 C53 C52 120.3(3) . . ? C53 C54 C55 119.9(3) . . ? C56 C55 C54 120.2(3) . . ? C55 C56 C51 120.4(3) . . ? C72 C71 C76 120.2(3) . . ? C72 C71 P3 121.2(2) . . ? C76 C71 P3 118.5(2) . . ? C73 C72 C71 119.7(3) . . ? C74 C73 C72 120.2(3) . . ? C73 C74 C75 120.8(3) . . ? C76 C75 C74 119.6(3) . . ? C75 C76 C71 119.5(3) . . ? C86 C81 C82 120.2(3) . . ? C86 C81 P3 121.1(2) . . ? C82 C81 P3 118.6(2) . . ? C83 C82 C81 119.6(3) . . ? C82 C83 C84 120.2(3) . . ? C85 C84 C83 119.9(3) . . ? C84 C85 C86 120.8(3) . . ? C85 C86 C81 119.4(3) . . ? F2 C1 F1 101.5(4) . . ? F2 C1 F3 100.4(4) . . ? F1 C1 F3 100.4(4) . . ? F2 C1 Rh1 119.8(4) . . ? F1 C1 Rh1 116.0(3) . . ? F3 C1 Rh1 115.8(3) . . ? F3' C1' F2' 97.7(12) . . ? F3' C1' F1' 96.5(11) . . ? F2' C1' F1' 95.3(12) . . ? F3' C1' Rh1 121.0(11) . . ? F2' C1' Rh1 122.3(10) . . ? F1' C1' Rh1 118.0(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C82 H82 I1 0.95 3.14 3.974(3) 147.4 1_455 _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.457 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.099 #===END data_jgl184si _database_code_depnum_ccdc_archive 'CCDC 714351' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H39 F3 O P3 Rh' _chemical_formula_weight 800.54 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' F F 0.0171 0.0103 '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 Orthorhombic _symmetry_space_group_name_H-M 'P bca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 19.3065(11) _cell_length_b 10.2522(5) _cell_length_c 37.1457(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7352.4(7) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8889 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 28.92 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3280 _exptl_absorpt_coefficient_mu 0.642 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8257 _exptl_absorpt_correction_T_max 0.8987 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 86841 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -50 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 29.09 _reflns_number_total 9488 _reflns_number_gt 8424 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0411P)^2^+5.5359P] 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 'Methyls rigid, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9488 _refine_ls_number_parameters 445 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0849 _refine_ls_wR_factor_gt 0.0821 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _refine_ls_shift/su_max 0.003 _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 0.530658(7) 0.407520(14) 0.124154(4) 0.01418(5) Uani 1 1 d . . . P1 P 0.51878(3) 0.48401(5) 0.183010(13) 0.01567(10) Uani 1 1 d . . . P2 P 0.44917(3) 0.24697(5) 0.105969(13) 0.01686(10) Uani 1 1 d . . . P3 P 0.62090(3) 0.46819(5) 0.085526(13) 0.01634(10) Uani 1 1 d . . . C1 C 0.47978(10) 0.5545(2) 0.10885(5) 0.0173(4) Uani 1 1 d . . . O1 O 0.45159(8) 0.64769(15) 0.10063(4) 0.0242(3) Uani 1 1 d . . . C2 C 0.59475(10) 0.25625(19) 0.14161(5) 0.0196(4) Uani 1 1 d . . . F1 F 0.56567(7) 0.16402(12) 0.16378(4) 0.0283(3) Uani 1 1 d . . . F2 F 0.62347(7) 0.18200(12) 0.11454(3) 0.0274(3) Uani 1 1 d . . . F3 F 0.65242(6) 0.29375(12) 0.16134(3) 0.0241(3) Uani 1 1 d . . . C3 C 0.57475(10) 0.6246(2) 0.19174(5) 0.0183(4) Uani 1 1 d . . . C4 C 0.64636(11) 0.6046(2) 0.19332(5) 0.0242(4) Uani 1 1 d . . . H4 H 0.6642 0.5183 0.1933 0.029 Uiso 1 1 calc R . . C5 C 0.69148(12) 0.7093(3) 0.19487(6) 0.0306(5) Uani 1 1 d . . . H5 H 0.7400 0.6943 0.1960 0.037 Uiso 1 1 calc R . . C6 C 0.66637(13) 0.8356(3) 0.19485(6) 0.0346(5) Uani 1 1 d . . . H6 H 0.6975 0.9073 0.1959 0.041 Uiso 1 1 calc R . . C7 C 0.59540(13) 0.8570(2) 0.19331(6) 0.0301(5) Uani 1 1 d . . . H7 H 0.5778 0.9436 0.1932 0.036 Uiso 1 1 calc R . . C8 C 0.54998(11) 0.7517(2) 0.19190(5) 0.0227(4) Uani 1 1 d . . . H8 H 0.5015 0.7670 0.1910 0.027 Uiso 1 1 calc R . . C11 C 0.43272(10) 0.53982(19) 0.19757(5) 0.0180(4) Uani 1 1 d . . . C12 C 0.37506(11) 0.5270(2) 0.17535(5) 0.0210(4) Uani 1 1 d . . . H12 H 0.3807 0.4941 0.1516 0.025 Uiso 1 1 calc R . . C13 C 0.30915(11) 0.5616(2) 0.18731(6) 0.0256(4) Uani 1 1 d . . . H13 H 0.2703 0.5529 0.1718 0.031 Uiso 1 1 calc R . . C14 C 0.30062(12) 0.6090(2) 0.22208(6) 0.0285(5) Uani 1 1 d . . . H14 H 0.2558 0.6324 0.2304 0.034 Uiso 1 1 calc R . . C15 C 0.35733(12) 0.6222(2) 0.24446(6) 0.0263(4) Uani 1 1 d . . . H15 H 0.3514 0.6548 0.2682 0.032 Uiso 1 1 calc R . . C16 C 0.42301(11) 0.5880(2) 0.23250(5) 0.0221(4) Uani 1 1 d . . . H16 H 0.4617 0.5974 0.2481 0.026 Uiso 1 1 calc R . . C17 C 0.54081(11) 0.3760(2) 0.22033(6) 0.0247(4) Uani 1 1 d . . . H17A H 0.5898 0.3519 0.2188 0.037 Uiso 1 1 calc R . . H17B H 0.5122 0.2972 0.2191 0.037 Uiso 1 1 calc R . . H17C H 0.5322 0.4209 0.2432 0.037 Uiso 1 1 calc R . . C21 C 0.42225(10) 0.1278(2) 0.13996(6) 0.0210(4) Uani 1 1 d . . . C22 C 0.41824(12) -0.0060(2) 0.13379(6) 0.0273(5) Uani 1 1 d . . . H22 H 0.4309 -0.0402 0.1109 0.033 Uiso 1 1 calc R . . C23 C 0.39589(13) -0.0898(2) 0.16079(7) 0.0349(6) Uani 1 1 d . . . H23 H 0.3926 -0.1807 0.1561 0.042 Uiso 1 1 calc R . . C24 C 0.37847(12) -0.0424(3) 0.19424(7) 0.0352(6) Uani 1 1 d . . . H24 H 0.3628 -0.1002 0.2125 0.042 Uiso 1 1 calc R . . C25 C 0.38394(11) 0.0900(2) 0.20121(6) 0.0298(5) Uani 1 1 d . . . H25 H 0.3729 0.1229 0.2244 0.036 Uiso 1 1 calc R . . C26 C 0.40547(11) 0.1744(2) 0.17426(6) 0.0247(4) Uani 1 1 d . . . H26 H 0.4089 0.2651 0.1792 0.030 Uiso 1 1 calc R . . C31 C 0.36552(10) 0.31463(19) 0.09180(5) 0.0177(4) Uani 1 1 d . . . C32 C 0.30244(11) 0.2802(2) 0.10735(6) 0.0259(4) Uani 1 1 d . . . H32 H 0.3010 0.2124 0.1248 0.031 Uiso 1 1 calc R . . C33 C 0.24174(12) 0.3438(2) 0.09769(6) 0.0314(5) Uani 1 1 d . . . H33 H 0.1991 0.3186 0.1084 0.038 Uiso 1 1 calc R . . C34 C 0.24298(12) 0.4435(2) 0.07261(6) 0.0268(4) Uani 1 1 d . . . H34 H 0.2017 0.4896 0.0669 0.032 Uiso 1 1 calc R . . C35 C 0.30481(12) 0.4756(2) 0.05594(6) 0.0265(4) Uani 1 1 d . . . H35 H 0.3057 0.5417 0.0380 0.032 Uiso 1 1 calc R . . C36 C 0.36520(11) 0.4116(2) 0.06529(5) 0.0224(4) Uani 1 1 d . . . H36 H 0.4072 0.4338 0.0535 0.027 Uiso 1 1 calc R . . C37 C 0.47098(11) 0.1442(2) 0.06728(6) 0.0262(4) Uani 1 1 d . . . H37A H 0.5124 0.0928 0.0728 0.039 Uiso 1 1 calc R . . H37B H 0.4799 0.1994 0.0463 0.039 Uiso 1 1 calc R . . H37C H 0.4323 0.0853 0.0621 0.039 Uiso 1 1 calc R . . C41 C 0.62322(10) 0.3760(2) 0.04336(5) 0.0190(4) Uani 1 1 d . . . C42 C 0.56586(11) 0.3828(2) 0.02051(5) 0.0216(4) Uani 1 1 d . . . H42 H 0.5285 0.4389 0.0265 0.026 Uiso 1 1 calc R . . C43 C 0.56249(11) 0.3088(2) -0.01081(5) 0.0246(4) Uani 1 1 d . . . H43 H 0.5234 0.3154 -0.0262 0.030 Uiso 1 1 calc R . . C44 C 0.61659(12) 0.2254(2) -0.01939(6) 0.0262(4) Uani 1 1 d . . . H44 H 0.6145 0.1740 -0.0406 0.031 Uiso 1 1 calc R . . C45 C 0.67372(12) 0.2171(2) 0.00311(6) 0.0282(5) Uani 1 1 d . . . H45 H 0.7107 0.1598 -0.0028 0.034 Uiso 1 1 calc R . . C46 C 0.67736(11) 0.2922(2) 0.03440(5) 0.0232(4) Uani 1 1 d . . . H46 H 0.7168 0.2862 0.0496 0.028 Uiso 1 1 calc R . . C51 C 0.62030(10) 0.6385(2) 0.06998(5) 0.0185(4) Uani 1 1 d . . . C52 C 0.63246(11) 0.6749(2) 0.03433(6) 0.0235(4) Uani 1 1 d . . . H52 H 0.6403 0.6100 0.0165 0.028 Uiso 1 1 calc R . . C53 C 0.63313(11) 0.8063(2) 0.02486(6) 0.0284(5) Uani 1 1 d . . . H53 H 0.6408 0.8306 0.0005 0.034 Uiso 1 1 calc R . . C54 C 0.62277(11) 0.9017(2) 0.05049(7) 0.0278(5) Uani 1 1 d . . . H54 H 0.6230 0.9911 0.0438 0.033 Uiso 1 1 calc R . . C55 C 0.61191(12) 0.8665(2) 0.08624(6) 0.0279(5) Uani 1 1 d . . . H55 H 0.6055 0.9319 0.1041 0.033 Uiso 1 1 calc R . . C56 C 0.61051(11) 0.7355(2) 0.09580(6) 0.0230(4) Uani 1 1 d . . . H56 H 0.6028 0.7118 0.1202 0.028 Uiso 1 1 calc R . . C57 C 0.71032(10) 0.4599(2) 0.10159(6) 0.0233(4) Uani 1 1 d . . . H57A H 0.7214 0.3699 0.1083 0.035 Uiso 1 1 calc R . . H57B H 0.7157 0.5168 0.1226 0.035 Uiso 1 1 calc R . . H57C H 0.7417 0.4887 0.0824 0.035 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 0.01480(8) 0.01604(8) 0.01169(8) 0.00055(5) -0.00027(5) 0.00123(5) P1 0.0171(2) 0.0186(2) 0.0114(2) 0.00097(17) -0.00071(17) 0.00032(18) P2 0.0180(2) 0.0176(2) 0.0150(2) -0.00059(17) 0.00040(18) -0.00078(18) P3 0.0158(2) 0.0196(2) 0.0137(2) -0.00006(17) 0.00076(17) 0.00090(18) C1 0.0175(9) 0.0224(10) 0.0120(8) -0.0012(7) 0.0010(7) -0.0013(7) O1 0.0255(7) 0.0248(8) 0.0223(7) 0.0038(6) -0.0005(6) 0.0055(6) C2 0.0210(9) 0.0189(9) 0.0188(9) 0.0009(7) 0.0003(7) 0.0000(7) F1 0.0269(7) 0.0230(6) 0.0351(7) 0.0121(5) -0.0018(5) 0.0010(5) F2 0.0290(7) 0.0251(6) 0.0281(6) -0.0044(5) -0.0005(5) 0.0088(5) F3 0.0200(6) 0.0275(6) 0.0248(6) 0.0031(5) -0.0051(5) 0.0030(5) C3 0.0218(9) 0.0242(10) 0.0089(8) -0.0005(7) -0.0001(7) -0.0031(8) C4 0.0232(10) 0.0319(12) 0.0173(9) -0.0001(8) -0.0022(8) -0.0007(8) C5 0.0207(10) 0.0467(14) 0.0245(11) -0.0001(10) -0.0019(8) -0.0080(10) C6 0.0353(13) 0.0385(14) 0.0299(12) -0.0035(10) 0.0028(10) -0.0166(11) C7 0.0377(13) 0.0244(11) 0.0283(11) -0.0022(9) 0.0050(9) -0.0057(9) C8 0.0239(10) 0.0254(10) 0.0188(9) -0.0015(8) 0.0020(8) -0.0013(8) C11 0.0184(9) 0.0175(9) 0.0180(9) 0.0000(7) 0.0018(7) -0.0011(7) C12 0.0223(10) 0.0237(10) 0.0169(9) -0.0005(7) 0.0014(7) -0.0012(8) C13 0.0195(10) 0.0329(12) 0.0244(10) -0.0019(9) 0.0004(8) -0.0017(8) C14 0.0228(11) 0.0325(12) 0.0303(12) -0.0054(9) 0.0079(9) -0.0004(9) C15 0.0281(11) 0.0292(11) 0.0217(10) -0.0081(8) 0.0091(8) -0.0056(9) C16 0.0217(10) 0.0272(11) 0.0174(9) -0.0030(8) 0.0016(7) -0.0050(8) C17 0.0291(11) 0.0272(11) 0.0179(9) 0.0066(8) -0.0026(8) 0.0012(9) C21 0.0179(9) 0.0215(10) 0.0236(10) 0.0048(8) -0.0036(7) -0.0024(8) C22 0.0294(11) 0.0228(10) 0.0297(11) 0.0038(9) -0.0121(9) -0.0028(9) C23 0.0385(13) 0.0258(12) 0.0405(14) 0.0137(10) -0.0212(11) -0.0084(10) C24 0.0263(12) 0.0425(14) 0.0367(13) 0.0249(11) -0.0146(10) -0.0132(10) C25 0.0216(11) 0.0432(14) 0.0247(11) 0.0134(9) -0.0018(8) -0.0032(9) C26 0.0234(10) 0.0278(11) 0.0229(10) 0.0044(8) 0.0004(8) -0.0027(8) C31 0.0205(9) 0.0184(9) 0.0143(8) -0.0022(7) -0.0018(7) -0.0009(7) C32 0.0236(10) 0.0322(12) 0.0219(10) 0.0053(9) 0.0017(8) -0.0003(9) C33 0.0211(11) 0.0461(15) 0.0271(11) 0.0019(10) 0.0042(8) 0.0021(10) C34 0.0251(11) 0.0300(11) 0.0254(10) -0.0051(9) -0.0059(8) 0.0065(9) C35 0.0297(11) 0.0255(11) 0.0241(10) 0.0026(8) -0.0086(8) -0.0029(9) C36 0.0212(10) 0.0277(11) 0.0184(9) 0.0031(8) -0.0027(7) -0.0051(8) C37 0.0288(11) 0.0245(11) 0.0252(11) -0.0056(8) 0.0029(8) 0.0000(8) C41 0.0205(9) 0.0213(9) 0.0154(9) 0.0007(7) 0.0041(7) -0.0010(7) C42 0.0186(10) 0.0272(11) 0.0189(9) 0.0004(8) 0.0029(7) -0.0004(8) C43 0.0253(11) 0.0320(11) 0.0166(9) 0.0003(8) 0.0010(8) -0.0040(9) C44 0.0357(12) 0.0254(11) 0.0175(9) -0.0037(8) 0.0048(8) -0.0021(9) C45 0.0354(12) 0.0260(11) 0.0232(10) -0.0027(8) 0.0074(9) 0.0069(9) C46 0.0250(10) 0.0260(11) 0.0187(9) 0.0017(8) 0.0025(8) 0.0038(8) C51 0.0152(9) 0.0221(9) 0.0182(9) 0.0025(7) 0.0000(7) -0.0013(7) C52 0.0221(10) 0.0295(11) 0.0190(10) 0.0010(8) 0.0008(8) -0.0027(8) C53 0.0257(11) 0.0350(12) 0.0247(11) 0.0114(9) -0.0010(8) -0.0040(9) C54 0.0238(11) 0.0229(11) 0.0367(12) 0.0093(9) -0.0006(9) -0.0025(8) C55 0.0265(11) 0.0228(10) 0.0343(12) -0.0018(9) 0.0019(9) -0.0037(9) C56 0.0235(10) 0.0254(10) 0.0200(10) -0.0002(8) 0.0020(8) -0.0020(8) C57 0.0160(9) 0.0316(11) 0.0224(10) 0.0011(8) -0.0012(7) 0.0010(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 1.886(2) . ? Rh1 C2 2.087(2) . ? Rh1 P1 2.3339(5) . ? Rh1 P3 2.3412(5) . ? Rh1 P2 2.3750(5) . ? P1 C17 1.825(2) . ? P1 C3 1.830(2) . ? P1 C11 1.839(2) . ? P2 C37 1.831(2) . ? P2 C21 1.832(2) . ? P2 C31 1.835(2) . ? P3 C57 1.828(2) . ? P3 C41 1.830(2) . ? P3 C51 1.839(2) . ? C1 O1 1.142(2) . ? C2 F1 1.374(2) . ? C2 F2 1.378(2) . ? C2 F3 1.387(2) . ? C3 C8 1.388(3) . ? C3 C4 1.399(3) . ? C4 C5 1.383(3) . ? C5 C6 1.383(4) . ? C6 C7 1.389(4) . ? C7 C8 1.392(3) . ? C11 C12 1.392(3) . ? C11 C16 1.401(3) . ? C12 C13 1.394(3) . ? C13 C14 1.390(3) . ? C14 C15 1.381(3) . ? C15 C16 1.388(3) . ? C21 C22 1.393(3) . ? C21 C26 1.399(3) . ? C22 C23 1.389(3) . ? C23 C24 1.376(4) . ? C24 C25 1.386(4) . ? C25 C26 1.387(3) . ? C31 C32 1.393(3) . ? C31 C36 1.399(3) . ? C32 C33 1.388(3) . ? C33 C34 1.383(3) . ? C34 C35 1.385(3) . ? C35 C36 1.382(3) . ? C41 C46 1.393(3) . ? C41 C42 1.397(3) . ? C42 C43 1.390(3) . ? C43 C44 1.387(3) . ? C44 C45 1.387(3) . ? C45 C46 1.396(3) . ? C51 C56 1.395(3) . ? C51 C52 1.396(3) . ? C52 C53 1.393(3) . ? C53 C54 1.379(3) . ? C54 C55 1.392(3) . ? C55 C56 1.390(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Rh1 C2 174.75(8) . . ? C1 Rh1 P1 87.87(6) . . ? C2 Rh1 P1 90.96(6) . . ? C1 Rh1 P3 89.46(6) . . ? C2 Rh1 P3 86.94(6) . . ? P1 Rh1 P3 123.912(18) . . ? C1 Rh1 P2 97.05(6) . . ? C2 Rh1 P2 88.06(6) . . ? P1 Rh1 P2 115.735(18) . . ? P3 Rh1 P2 120.184(18) . . ? C17 P1 C3 101.88(10) . . ? C17 P1 C11 100.13(10) . . ? C3 P1 C11 103.67(9) . . ? C17 P1 Rh1 119.00(8) . . ? C3 P1 Rh1 111.87(6) . . ? C11 P1 Rh1 117.96(6) . . ? C37 P2 C21 102.85(10) . . ? C37 P2 C31 101.24(9) . . ? C21 P2 C31 101.54(9) . . ? C37 P2 Rh1 118.02(7) . . ? C21 P2 Rh1 117.00(7) . . ? C31 P2 Rh1 113.74(6) . . ? C57 P3 C41 103.43(10) . . ? C57 P3 C51 98.77(9) . . ? C41 P3 C51 102.82(9) . . ? C57 P3 Rh1 119.36(7) . . ? C41 P3 Rh1 113.92(7) . . ? C51 P3 Rh1 116.10(6) . . ? O1 C1 Rh1 176.11(18) . . ? F1 C2 F2 102.80(15) . . ? F1 C2 F3 101.65(15) . . ? F2 C2 F3 102.46(15) . . ? F1 C2 Rh1 117.09(13) . . ? F2 C2 Rh1 114.99(13) . . ? F3 C2 Rh1 115.72(13) . . ? C8 C3 C4 118.53(19) . . ? C8 C3 P1 122.46(16) . . ? C4 C3 P1 118.41(16) . . ? C5 C4 C3 120.7(2) . . ? C6 C5 C4 120.4(2) . . ? C5 C6 C7 119.6(2) . . ? C6 C7 C8 120.0(2) . . ? C3 C8 C7 120.8(2) . . ? C12 C11 C16 118.38(18) . . ? C12 C11 P1 121.26(15) . . ? C16 C11 P1 120.20(15) . . ? C11 C12 C13 121.15(19) . . ? C14 C13 C12 119.6(2) . . ? C15 C14 C13 120.0(2) . . ? C14 C15 C16 120.5(2) . . ? C15 C16 C11 120.49(19) . . ? C22 C21 C26 118.3(2) . . ? C22 C21 P2 123.98(17) . . ? C26 C21 P2 117.75(16) . . ? C23 C22 C21 120.5(2) . . ? C24 C23 C22 120.6(2) . . ? C23 C24 C25 119.7(2) . . ? C24 C25 C26 119.9(2) . . ? C25 C26 C21 120.9(2) . . ? C32 C31 C36 117.89(19) . . ? C32 C31 P2 123.69(15) . . ? C36 C31 P2 118.32(15) . . ? C33 C32 C31 120.8(2) . . ? C34 C33 C32 120.4(2) . . ? C33 C34 C35 119.5(2) . . ? C36 C35 C34 120.1(2) . . ? C35 C36 C31 121.2(2) . . ? C46 C41 C42 118.72(19) . . ? C46 C41 P3 122.77(16) . . ? C42 C41 P3 118.34(15) . . ? C43 C42 C41 121.22(19) . . ? C44 C43 C42 119.6(2) . . ? C45 C44 C43 119.9(2) . . ? C44 C45 C46 120.5(2) . . ? C41 C46 C45 120.1(2) . . ? C56 C51 C52 118.95(19) . . ? C56 C51 P3 117.54(15) . . ? C52 C51 P3 123.43(16) . . ? C53 C52 C51 120.0(2) . . ? C54 C53 C52 120.7(2) . . ? C53 C54 C55 119.8(2) . . ? C56 C55 C54 119.8(2) . . ? C55 C56 C51 120.7(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C7 H7 F1 0.95 2.52 3.382(3) 150.7 1_565 _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.289 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.087 #===END data_jgl2382s _database_code_depnum_ccdc_archive 'CCDC 714352' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H34 F7 I N P2 Rh' _chemical_formula_weight 821.32 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 11.4084(5) _cell_length_b 11.6334(5) _cell_length_c 13.1497(6) _cell_angle_alpha 88.019(2) _cell_angle_beta 76.668(2) _cell_angle_gamma 69.908(2) _cell_volume 1592.92(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6798 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 28.11 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 1.667 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6711 _exptl_absorpt_correction_T_max 0.7881 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18039 _diffrn_reflns_av_R_equivalents 0.0154 _diffrn_reflns_av_sigmaI/netI 0.0188 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 28.18 _reflns_number_total 7093 _reflns_number_gt 6838 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0234P)^2^+0.8200P] 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 'rigid methyls, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7093 _refine_ls_number_parameters 377 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0201 _refine_ls_R_factor_gt 0.0191 _refine_ls_wR_factor_ref 0.0474 _refine_ls_wR_factor_gt 0.0469 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.003 _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 0.679280(11) 0.111052(10) 0.260489(9) 0.01112(4) Uani 1 1 d . . . I2 I 0.763303(10) 0.269480(9) 0.121106(8) 0.01588(4) Uani 1 1 d . . . P3 P 0.60854(4) 0.25494(4) 0.40253(3) 0.01375(8) Uani 1 1 d . . . P4 P 0.73898(4) -0.03656(4) 0.12138(3) 0.01617(9) Uani 1 1 d . . . F1 F 0.96136(9) 0.01700(9) 0.21028(8) 0.0204(2) Uani 1 1 d . . . F2 F 0.88351(9) 0.11956(9) 0.36028(8) 0.0199(2) Uani 1 1 d . . . F3 F 0.86568(10) -0.16859(9) 0.31189(9) 0.0240(2) Uani 1 1 d . . . F4 F 0.83083(10) -0.06291(10) 0.45705(8) 0.0249(2) Uani 1 1 d . . . F5 F 1.05013(12) -0.23490(11) 0.42620(11) 0.0366(3) Uani 1 1 d . . . F6 F 1.11122(12) -0.19634(12) 0.26593(11) 0.0414(3) Uani 1 1 d . . . F7 F 1.08830(12) -0.06810(11) 0.38924(12) 0.0404(3) Uani 1 1 d . . . C1 C 0.59122(16) 0.00694(15) 0.36598(13) 0.0175(3) Uani 1 1 d . . . H1A H 0.4992 0.0530 0.3895 0.026 Uiso 1 1 calc R . . H1B H 0.6301 -0.0097 0.4265 0.026 Uiso 1 1 calc R . . H1C H 0.6036 -0.0707 0.3308 0.026 Uiso 1 1 calc R . . C2 C 0.85965(16) 0.03851(15) 0.29797(13) 0.0163(3) Uani 1 1 d . . . C3 C 0.89676(17) -0.08248(15) 0.35578(14) 0.0196(3) Uani 1 1 d . . . C4 C 1.03940(18) -0.14518(17) 0.35894(17) 0.0281(4) Uani 1 1 d . . . C5 C 0.51226(15) 0.18372(14) 0.22140(12) 0.0141(3) Uani 1 1 d . . . N1 N 0.41417(13) 0.22660(13) 0.19983(11) 0.0165(3) Uani 1 1 d . . . C11 C 0.29464(16) 0.28684(15) 0.17612(13) 0.0168(3) Uani 1 1 d . . . C12 C 0.28355(17) 0.38564(16) 0.11056(14) 0.0193(3) Uani 1 1 d . . . C13 C 0.16374(18) 0.44373(18) 0.08854(16) 0.0264(4) Uani 1 1 d . . . H13 H 0.1518 0.5117 0.0450 0.032 Uiso 1 1 calc R . . C14 C 0.06185(19) 0.4039(2) 0.12920(17) 0.0304(4) Uani 1 1 d . . . H14 H -0.0185 0.4436 0.1120 0.036 Uiso 1 1 calc R . . C15 C 0.07601(18) 0.30654(19) 0.19479(16) 0.0273(4) Uani 1 1 d . . . H15 H 0.0050 0.2808 0.2224 0.033 Uiso 1 1 calc R . . C16 C 0.19305(17) 0.24608(17) 0.22063(14) 0.0206(3) Uani 1 1 d . . . C17 C 0.39467(18) 0.42777(18) 0.06744(15) 0.0247(4) Uani 1 1 d . . . H17A H 0.3705 0.4927 0.0188 0.037 Uiso 1 1 calc R . . H17B H 0.4680 0.3587 0.0304 0.037 Uiso 1 1 calc R . . H17C H 0.4182 0.4595 0.1249 0.037 Uiso 1 1 calc R . . C18 C 0.2089(2) 0.1435(2) 0.29491(17) 0.0297(4) Uani 1 1 d . . . H18A H 0.1263 0.1319 0.3213 0.045 Uiso 1 1 calc R . . H18B H 0.2389 0.1640 0.3536 0.045 Uiso 1 1 calc R . . H18C H 0.2719 0.0678 0.2581 0.045 Uiso 1 1 calc R . . C21 C 0.43785(16) 0.34219(15) 0.42345(13) 0.0167(3) Uani 1 1 d . . . C22 C 0.39816(17) 0.43392(16) 0.35458(14) 0.0203(3) Uani 1 1 d . . . H22 H 0.4604 0.4512 0.3007 0.024 Uiso 1 1 calc R . . C23 C 0.26925(18) 0.49984(17) 0.36404(16) 0.0254(4) Uani 1 1 d . . . H23 H 0.2435 0.5618 0.3167 0.030 Uiso 1 1 calc R . . C24 C 0.17809(18) 0.47583(18) 0.44202(19) 0.0323(5) Uani 1 1 d . . . H24 H 0.0896 0.5212 0.4485 0.039 Uiso 1 1 calc R . . C25 C 0.21604(19) 0.38522(19) 0.51103(19) 0.0353(5) Uani 1 1 d . . . H25 H 0.1533 0.3689 0.5650 0.042 Uiso 1 1 calc R . . C26 C 0.34569(18) 0.31803(17) 0.50167(16) 0.0250(4) Uani 1 1 d . . . H26 H 0.3710 0.2557 0.5489 0.030 Uiso 1 1 calc R . . C27 C 0.67830(17) 0.37497(16) 0.39374(15) 0.0212(4) Uani 1 1 d . . . H27A H 0.6641 0.4210 0.3312 0.032 Uiso 1 1 calc R . . H27B H 0.7707 0.3381 0.3891 0.032 Uiso 1 1 calc R . . H27C H 0.6378 0.4305 0.4561 0.032 Uiso 1 1 calc R . . C28 C 0.62454(18) 0.19904(17) 0.53136(13) 0.0211(4) Uani 1 1 d . . . H28A H 0.5848 0.2677 0.5835 0.032 Uiso 1 1 calc R . . H28B H 0.7157 0.1608 0.5311 0.032 Uiso 1 1 calc R . . H28C H 0.5817 0.1385 0.5488 0.032 Uiso 1 1 calc R . . C31 C 0.67044(18) -0.15769(16) 0.14889(13) 0.0195(3) Uani 1 1 d . . . C32 C 0.53941(19) -0.12930(18) 0.15759(15) 0.0255(4) Uani 1 1 d . . . H32 H 0.4878 -0.0477 0.1485 0.031 Uiso 1 1 calc R . . C33 C 0.4833(2) -0.2186(2) 0.17938(16) 0.0339(5) Uani 1 1 d . . . H33 H 0.3940 -0.1986 0.1844 0.041 Uiso 1 1 calc R . . C34 C 0.5585(2) -0.3375(2) 0.19384(16) 0.0360(5) Uani 1 1 d . . . H34 H 0.5206 -0.3992 0.2083 0.043 Uiso 1 1 calc R . . C35 C 0.6873(2) -0.36639(18) 0.18728(17) 0.0344(5) Uani 1 1 d . . . H35 H 0.7380 -0.4477 0.1981 0.041 Uiso 1 1 calc R . . C36 C 0.7438(2) -0.27718(17) 0.16482(15) 0.0272(4) Uani 1 1 d . . . H36 H 0.8331 -0.2978 0.1603 0.033 Uiso 1 1 calc R . . C37 C 0.90661(18) -0.11885(18) 0.06157(16) 0.0273(4) Uani 1 1 d . . . H37A H 0.9491 -0.1652 0.1145 0.041 Uiso 1 1 calc R . . H37B H 0.9485 -0.0603 0.0324 0.041 Uiso 1 1 calc R . . H37C H 0.9127 -0.1754 0.0055 0.041 Uiso 1 1 calc R . . C38 C 0.6823(2) 0.02663(18) 0.00562(14) 0.0268(4) Uani 1 1 d . . . H38A H 0.7218 0.0873 -0.0224 0.040 Uiso 1 1 calc R . . H38B H 0.5887 0.0660 0.0246 0.040 Uiso 1 1 calc R . . H38C H 0.7059 -0.0395 -0.0475 0.040 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 0.01163(6) 0.01000(6) 0.01208(6) 0.00139(4) -0.00289(5) -0.00419(5) I2 0.01627(6) 0.01407(6) 0.01782(6) 0.00393(4) -0.00278(4) -0.00693(4) P3 0.01458(19) 0.01276(18) 0.01399(19) 0.00017(15) -0.00365(15) -0.00457(15) P4 0.0206(2) 0.01344(19) 0.0146(2) -0.00055(15) -0.00161(16) -0.00750(16) F1 0.0137(5) 0.0194(5) 0.0247(5) 0.0031(4) -0.0010(4) -0.0038(4) F2 0.0187(5) 0.0161(5) 0.0280(5) 0.0003(4) -0.0112(4) -0.0061(4) F3 0.0283(6) 0.0144(5) 0.0319(6) 0.0040(4) -0.0113(5) -0.0082(4) F4 0.0278(6) 0.0248(5) 0.0213(5) 0.0076(4) -0.0071(4) -0.0077(4) F5 0.0338(6) 0.0230(6) 0.0525(8) 0.0177(5) -0.0207(6) -0.0037(5) F6 0.0246(6) 0.0345(7) 0.0482(8) 0.0053(6) -0.0025(6) 0.0066(5) F7 0.0306(6) 0.0286(6) 0.0728(10) 0.0149(6) -0.0336(7) -0.0109(5) C1 0.0188(8) 0.0181(8) 0.0173(8) 0.0034(6) -0.0033(6) -0.0095(7) C2 0.0163(8) 0.0133(7) 0.0187(8) 0.0014(6) -0.0037(6) -0.0049(6) C3 0.0190(8) 0.0161(8) 0.0236(9) 0.0033(7) -0.0073(7) -0.0046(7) C4 0.0232(9) 0.0202(9) 0.0393(11) 0.0085(8) -0.0124(8) -0.0028(7) C5 0.0175(8) 0.0132(7) 0.0122(7) 0.0008(6) -0.0016(6) -0.0074(6) N1 0.0170(7) 0.0174(7) 0.0174(7) 0.0014(5) -0.0047(5) -0.0082(6) C11 0.0142(8) 0.0196(8) 0.0174(8) -0.0003(6) -0.0063(6) -0.0049(6) C12 0.0202(8) 0.0204(8) 0.0182(8) 0.0013(7) -0.0067(7) -0.0070(7) C13 0.0253(9) 0.0270(9) 0.0272(10) 0.0050(8) -0.0130(8) -0.0050(8) C14 0.0193(9) 0.0375(11) 0.0342(11) 0.0009(9) -0.0133(8) -0.0049(8) C15 0.0175(9) 0.0363(11) 0.0312(10) -0.0016(8) -0.0067(8) -0.0122(8) C16 0.0187(8) 0.0240(9) 0.0217(9) 0.0003(7) -0.0058(7) -0.0101(7) C17 0.0258(9) 0.0293(10) 0.0239(9) 0.0093(8) -0.0096(7) -0.0140(8) C18 0.0270(10) 0.0357(11) 0.0324(11) 0.0118(9) -0.0074(8) -0.0188(9) C21 0.0172(8) 0.0131(7) 0.0187(8) -0.0021(6) -0.0045(6) -0.0032(6) C22 0.0227(9) 0.0162(8) 0.0188(8) -0.0002(6) -0.0030(7) -0.0037(7) C23 0.0260(9) 0.0187(8) 0.0293(10) 0.0010(7) -0.0109(8) -0.0021(7) C24 0.0164(9) 0.0233(9) 0.0529(13) 0.0039(9) -0.0082(9) -0.0014(7) C25 0.0187(9) 0.0282(10) 0.0521(14) 0.0092(10) 0.0018(9) -0.0066(8) C26 0.0209(9) 0.0190(8) 0.0323(10) 0.0078(7) -0.0040(8) -0.0055(7) C27 0.0229(9) 0.0184(8) 0.0241(9) -0.0038(7) -0.0033(7) -0.0101(7) C28 0.0232(9) 0.0245(9) 0.0144(8) 0.0000(7) -0.0063(7) -0.0053(7) C31 0.0290(9) 0.0174(8) 0.0142(8) -0.0020(6) -0.0021(7) -0.0121(7) C32 0.0328(10) 0.0250(9) 0.0249(9) 0.0019(7) -0.0106(8) -0.0155(8) C33 0.0416(12) 0.0463(12) 0.0280(10) 0.0019(9) -0.0098(9) -0.0317(10) C34 0.0635(15) 0.0343(11) 0.0228(10) 0.0031(8) -0.0043(10) -0.0365(11) C35 0.0539(14) 0.0193(9) 0.0306(11) 0.0015(8) -0.0038(10) -0.0173(9) C36 0.0355(11) 0.0186(9) 0.0264(10) 0.0002(7) -0.0018(8) -0.0112(8) C37 0.0246(9) 0.0244(9) 0.0278(10) -0.0080(8) 0.0061(8) -0.0090(8) C38 0.0442(12) 0.0238(9) 0.0160(8) 0.0020(7) -0.0095(8) -0.0146(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C5 1.9810(16) . ? Rh1 C2 2.1061(16) . ? Rh1 C1 2.1160(16) . ? Rh1 P3 2.3526(4) . ? Rh1 P4 2.3660(4) . ? Rh1 I2 2.80090(18) . ? P3 C27 1.8184(18) . ? P3 C28 1.8196(17) . ? P3 C21 1.8200(17) . ? P4 C37 1.8146(19) . ? P4 C31 1.8219(17) . ? P4 C38 1.8237(19) . ? F1 C2 1.3936(19) . ? F2 C2 1.4025(19) . ? F3 C3 1.357(2) . ? F4 C3 1.354(2) . ? F5 C4 1.336(2) . ? F6 C4 1.332(2) . ? F7 C4 1.321(2) . ? C2 C3 1.550(2) . ? C3 C4 1.548(2) . ? C5 N1 1.155(2) . ? N1 C11 1.404(2) . ? C11 C16 1.399(2) . ? C11 C12 1.401(2) . ? C12 C13 1.394(2) . ? C12 C17 1.498(2) . ? C13 C14 1.385(3) . ? C14 C15 1.387(3) . ? C15 C16 1.393(3) . ? C16 C18 1.504(3) . ? C21 C26 1.388(2) . ? C21 C22 1.398(2) . ? C22 C23 1.383(3) . ? C23 C24 1.378(3) . ? C24 C25 1.387(3) . ? C25 C26 1.394(3) . ? C31 C36 1.392(3) . ? C31 C32 1.393(3) . ? C32 C33 1.387(3) . ? C33 C34 1.388(3) . ? C34 C35 1.373(3) . ? C35 C36 1.390(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Rh1 C2 177.70(6) . . ? C5 Rh1 C1 86.58(6) . . ? C2 Rh1 C1 95.71(6) . . ? C5 Rh1 P3 90.46(5) . . ? C2 Rh1 P3 89.62(5) . . ? C1 Rh1 P3 84.89(5) . . ? C5 Rh1 P4 87.40(5) . . ? C2 Rh1 P4 92.63(5) . . ? C1 Rh1 P4 92.25(5) . . ? P3 Rh1 P4 176.529(15) . . ? C5 Rh1 I2 86.37(5) . . ? C2 Rh1 I2 91.33(4) . . ? C1 Rh1 I2 172.52(5) . . ? P3 Rh1 I2 92.650(11) . . ? P4 Rh1 I2 89.943(12) . . ? C27 P3 C28 101.48(9) . . ? C27 P3 C21 102.38(8) . . ? C28 P3 C21 103.03(8) . . ? C27 P3 Rh1 117.84(6) . . ? C28 P3 Rh1 118.35(6) . . ? C21 P3 Rh1 111.58(6) . . ? C37 P4 C31 103.50(9) . . ? C37 P4 C38 99.95(10) . . ? C31 P4 C38 101.48(9) . . ? C37 P4 Rh1 120.98(7) . . ? C31 P4 Rh1 114.84(6) . . ? C38 P4 Rh1 113.39(6) . . ? F1 C2 F2 102.12(12) . . ? F1 C2 C3 103.12(13) . . ? F2 C2 C3 102.51(13) . . ? F1 C2 Rh1 112.67(11) . . ? F2 C2 Rh1 113.29(10) . . ? C3 C2 Rh1 120.94(11) . . ? F4 C3 F3 107.70(14) . . ? F4 C3 C4 105.50(14) . . ? F3 C3 C4 105.13(14) . . ? F4 C3 C2 109.76(14) . . ? F3 C3 C2 110.31(14) . . ? C4 C3 C2 117.89(15) . . ? F7 C4 F6 108.34(17) . . ? F7 C4 F5 107.80(16) . . ? F6 C4 F5 107.01(15) . . ? F7 C4 C3 112.37(15) . . ? F6 C4 C3 111.56(16) . . ? F5 C4 C3 109.56(16) . . ? N1 C5 Rh1 179.19(15) . . ? C5 N1 C11 175.92(16) . . ? C16 C11 C12 123.77(16) . . ? C16 C11 N1 118.17(15) . . ? C12 C11 N1 118.04(15) . . ? C13 C12 C11 116.75(16) . . ? C13 C12 C17 121.69(16) . . ? C11 C12 C17 121.55(16) . . ? C14 C13 C12 121.02(18) . . ? C13 C14 C15 120.63(17) . . ? C14 C15 C16 120.85(18) . . ? C15 C16 C11 116.95(17) . . ? C15 C16 C18 121.61(17) . . ? C11 C16 C18 121.42(16) . . ? C26 C21 C22 118.91(16) . . ? C26 C21 P3 122.88(13) . . ? C22 C21 P3 118.15(13) . . ? C23 C22 C21 120.71(17) . . ? C24 C23 C22 120.18(18) . . ? C23 C24 C25 119.75(18) . . ? C24 C25 C26 120.39(19) . . ? C21 C26 C25 120.05(17) . . ? C36 C31 C32 118.69(17) . . ? C36 C31 P4 122.22(15) . . ? C32 C31 P4 119.06(14) . . ? C33 C32 C31 120.86(19) . . ? C32 C33 C34 119.5(2) . . ? C35 C34 C33 120.30(19) . . ? C34 C35 C36 120.3(2) . . ? C35 C36 C31 120.4(2) . . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.510 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.073 #===END