Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email DJC@ST-AND.AC.UK _publ_contact_author_name 'Prof David J Cole-Hamilton' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0186 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name D.J.Cole-Hamilton D.F.Foster D.J.Law A.E.C.McConnell ; P.Pogorzelec ; A.Slawin data_9 _database_code_CSD 197739 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H29 I O P Rh' _chemical_formula_sum 'C17 H29 I O P Rh' _chemical_formula_weight 510.18 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 8.0159(2) _cell_length_b 17.77960(10) _cell_length_c 13.6522(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.2430(10) _cell_angle_gamma 90.00 _cell_volume 1940.37(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 70 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max .2 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 2.551 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.857849 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7999 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 23.26 _reflns_number_total 2694 _reflns_number_gt 2088 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0868P)^2^+7.8958P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2694 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1464 _refine_ls_wR_factor_gt 0.1336 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.002 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 0.41628(8) 0.59086(4) 0.76775(5) 0.0316(2) Uani 1 1 d . . . I1 I 0.26717(11) 0.45765(4) 0.72726(7) 0.0719(3) Uani 1 1 d . . . P1 P 0.2786(3) 0.65794(13) 0.64722(17) 0.0378(6) Uani 1 1 d . . . C1 C 0.4433(13) 0.6656(7) 0.5576(8) 0.056(3) Uani 1 1 d . . . H1A H 0.4509 0.6187 0.5220 0.067 Uiso 1 1 calc R . . H1B H 0.4139 0.7052 0.5106 0.067 Uiso 1 1 calc R . . C2 C 0.6088(12) 0.6831(7) 0.6118(8) 0.055(3) Uani 1 1 d . . . H2A H 0.6112 0.7358 0.6302 0.066 Uiso 1 1 calc R . . H2B H 0.6974 0.6747 0.5683 0.066 Uiso 1 1 calc R . . C3 C 0.6423(11) 0.6353(6) 0.7036(7) 0.042(2) Uani 1 1 d . . . C4 C 0.6325(11) 0.6637(5) 0.8044(7) 0.043(2) Uani 1 1 d . . . C5 C 0.6554(11) 0.5986(6) 0.8673(7) 0.047(2) Uani 1 1 d . . . C6 C 0.6699(12) 0.5363(5) 0.8112(8) 0.047(2) Uani 1 1 d . . . C7 C 0.6682(11) 0.5586(6) 0.7080(7) 0.044(2) Uani 1 1 d . . . C8 C 0.6315(15) 0.7444(6) 0.8340(9) 0.061(3) Uani 1 1 d . . . H8A H 0.6135 0.7753 0.7765 0.091 Uiso 1 1 calc R . . H8B H 0.7370 0.7570 0.8678 0.091 Uiso 1 1 calc R . . H8C H 0.5434 0.7528 0.8766 0.091 Uiso 1 1 calc R . . C9 C 0.6670(15) 0.6042(8) 0.9789(8) 0.072(4) Uani 1 1 d . . . H9A H 0.6513 0.6556 0.9979 0.108 Uiso 1 1 calc R . . H9B H 0.7751 0.5872 1.0048 0.108 Uiso 1 1 calc R . . H9C H 0.5819 0.5734 1.0045 0.108 Uiso 1 1 calc R . . C10 C 0.7086(16) 0.4579(7) 0.8478(12) 0.082(4) Uani 1 1 d . . . H10A H 0.7126 0.4244 0.7928 0.123 Uiso 1 1 calc R . . H10B H 0.6231 0.4417 0.8886 0.123 Uiso 1 1 calc R . . H10C H 0.8149 0.4577 0.8851 0.123 Uiso 1 1 calc R . . C11 C 0.6974(16) 0.5059(7) 0.6240(9) 0.070(3) Uani 1 1 d . . . H11A H 0.7112 0.4555 0.6486 0.106 Uiso 1 1 calc R . . H11B H 0.7964 0.5210 0.5937 0.106 Uiso 1 1 calc R . . H11C H 0.6031 0.5078 0.5764 0.106 Uiso 1 1 calc R . . C12 C 0.0999(13) 0.6183(6) 0.5751(7) 0.051(2) Uani 1 1 d . . . H12A H 0.1281 0.5674 0.5565 0.061 Uiso 1 1 calc R . . H12B H 0.0072 0.6149 0.6167 0.061 Uiso 1 1 calc R . . C13 C 0.0411(16) 0.6612(8) 0.4826(9) 0.078(4) Uani 1 1 d . . . H13A H -0.0531 0.6359 0.4500 0.117 Uiso 1 1 calc R . . H13B H 0.1303 0.6637 0.4395 0.117 Uiso 1 1 calc R . . H13C H 0.0091 0.7113 0.4999 0.117 Uiso 1 1 calc R . . C14 C 0.2197(13) 0.7554(5) 0.6677(8) 0.052(3) Uani 1 1 d . . . H14A H 0.3095 0.7791 0.7080 0.062 Uiso 1 1 calc R . . H14B H 0.2114 0.7809 0.6048 0.062 Uiso 1 1 calc R . . C15 C 0.0616(18) 0.7677(8) 0.7149(11) 0.087(4) Uani 1 1 d . . . H15A H 0.0435 0.8207 0.7225 0.131 Uiso 1 1 calc R . . H15B H 0.0685 0.7440 0.7783 0.131 Uiso 1 1 calc R . . H15C H -0.0297 0.7464 0.6747 0.131 Uiso 1 1 calc R . . C21 C 0.2265 0.6269 0.8878 0.049 Uani 1 1 d . . . O21 O 0.2932 0.6703 0.9256 0.067 Uani 1 1 d . . . C22 C 0.0983 0.5931 0.8768 0.062 Uani 1 1 d . . . H22A H 0.0252 0.6086 0.9256 0.093 Uiso 1 1 calc R . . H22B H 0.1201 0.5401 0.8833 0.093 Uiso 1 1 calc R . . H22C H 0.0462 0.6032 0.8126 0.093 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 0.0296(4) 0.0290(4) 0.0363(4) -0.0002(3) 0.0031(3) -0.0028(3) I1 0.0765(6) 0.0431(5) 0.0931(7) 0.0010(4) -0.0128(4) -0.0187(4) P1 0.0335(12) 0.0402(13) 0.0394(13) 0.0019(10) 0.0011(10) -0.0014(10) C1 0.057(7) 0.062(7) 0.050(6) 0.012(5) 0.007(5) 0.004(5) C2 0.037(5) 0.071(7) 0.058(6) 0.022(5) 0.009(5) -0.002(5) C3 0.031(5) 0.054(6) 0.040(5) -0.004(4) 0.007(4) -0.007(4) C4 0.028(5) 0.047(6) 0.054(6) -0.005(5) 0.009(4) -0.006(4) C5 0.030(5) 0.073(7) 0.038(5) 0.001(5) 0.004(4) -0.006(5) C6 0.037(5) 0.039(5) 0.064(7) 0.010(5) 0.004(5) -0.001(4) C7 0.035(5) 0.048(6) 0.050(6) -0.013(5) 0.003(4) -0.002(4) C8 0.063(7) 0.051(6) 0.069(7) -0.018(5) 0.008(6) -0.008(5) C9 0.053(7) 0.120(11) 0.042(6) 0.000(6) -0.004(5) -0.006(7) C10 0.067(8) 0.057(7) 0.121(12) 0.031(7) 0.004(8) 0.016(6) C11 0.068(7) 0.066(7) 0.079(8) -0.034(7) 0.014(6) 0.004(6) C12 0.051(6) 0.050(6) 0.051(6) -0.002(5) -0.001(5) 0.002(5) C13 0.075(9) 0.098(10) 0.057(7) 0.007(7) -0.022(6) 0.004(7) C14 0.056(6) 0.037(5) 0.061(6) 0.002(5) -0.004(5) 0.004(5) C15 0.086(10) 0.080(9) 0.096(10) -0.018(8) 0.005(8) 0.029(8) C21 0.049 0.049 0.049 0.000 0.004 0.000 O21 0.067 0.067 0.067 0.000 0.005 0.000 C22 0.062 0.062 0.062 0.000 0.005 0.000 _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 C4 2.191(9) . ? Rh1 C3 2.215(9) . ? Rh1 P1 2.254(2) . ? Rh1 C5 2.270(9) . ? Rh1 C6 2.291(9) . ? Rh1 C7 2.306(10) . ? Rh1 C21 2.4036(7) . ? Rh1 I1 2.6919(9) . ? P1 C14 1.822(10) . ? P1 C12 1.819(10) . ? P1 C1 1.870(11) . ? C1 C2 1.503(15) . ? C2 C3 1.522(14) . ? C3 C7 1.380(14) . ? C3 C4 1.473(13) . ? C4 C5 1.444(14) . ? C4 C8 1.491(14) . ? C5 C6 1.356(14) . ? C5 C9 1.524(14) . ? C6 C7 1.463(15) . ? C6 C10 1.504(14) . ? C7 C11 1.511(14) . ? C12 C13 1.521(15) . ? C14 C15 1.480(17) . ? C21 O21 1.0533 . ? C21 C22 1.1902 . ? 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 C4 Rh1 C3 39.1(3) . . ? C4 Rh1 P1 101.0(3) . . ? C3 Rh1 P1 83.9(3) . . ? C4 Rh1 C5 37.7(4) . . ? C3 Rh1 C5 62.4(3) . . ? P1 Rh1 C5 138.7(3) . . ? C4 Rh1 C6 61.3(3) . . ? C3 Rh1 C6 61.1(3) . . ? P1 Rh1 C6 142.2(3) . . ? C5 Rh1 C6 34.6(4) . . ? C4 Rh1 C7 61.9(3) . . ? C3 Rh1 C7 35.5(4) . . ? P1 Rh1 C7 105.5(3) . . ? C5 Rh1 C7 60.3(3) . . ? C6 Rh1 C7 37.1(4) . . ? C4 Rh1 C21 102.5(2) . . ? C3 Rh1 C21 138.8(2) . . ? P1 Rh1 C21 93.23(7) . . ? C5 Rh1 C21 97.2(2) . . ? C6 Rh1 C21 122.0(3) . . ? C7 Rh1 C21 157.3(2) . . ? C4 Rh1 I1 153.9(2) . . ? C3 Rh1 I1 126.6(2) . . ? P1 Rh1 I1 97.45(7) . . ? C5 Rh1 I1 121.2(3) . . ? C6 Rh1 I1 93.0(2) . . ? C7 Rh1 I1 95.5(2) . . ? C21 Rh1 I1 94.61(3) . . ? C14 P1 C12 104.4(5) . . ? C14 P1 C1 103.5(5) . . ? C12 P1 C1 103.9(5) . . ? C14 P1 Rh1 120.6(4) . . ? C12 P1 Rh1 120.9(3) . . ? C1 P1 Rh1 100.7(3) . . ? C2 C1 P1 109.5(7) . . ? C1 C2 C3 112.7(8) . . ? C7 C3 C4 108.4(8) . . ? C7 C3 C2 127.2(9) . . ? C4 C3 C2 124.1(9) . . ? C7 C3 Rh1 75.8(6) . . ? C4 C3 Rh1 69.6(5) . . ? C2 C3 Rh1 115.2(6) . . ? C5 C4 C3 105.5(8) . . ? C5 C4 C8 127.8(9) . . ? C3 C4 C8 125.7(9) . . ? C5 C4 Rh1 74.1(5) . . ? C3 C4 Rh1 71.3(5) . . ? C8 C4 Rh1 127.6(7) . . ? C6 C5 C4 109.4(8) . . ? C6 C5 C9 128.1(10) . . ? C4 C5 C9 122.5(10) . . ? C6 C5 Rh1 73.6(6) . . ? C4 C5 Rh1 68.2(5) . . ? C9 C5 Rh1 126.1(7) . . ? C5 C6 C7 109.1(8) . . ? C5 C6 C10 126.4(11) . . ? C7 C6 C10 123.9(10) . . ? C5 C6 Rh1 71.9(6) . . ? C7 C6 Rh1 72.0(5) . . ? C10 C6 Rh1 129.4(8) . . ? C3 C7 C6 107.4(8) . . ? C3 C7 C11 127.6(10) . . ? C6 C7 C11 124.9(10) . . ? C3 C7 Rh1 68.7(5) . . ? C6 C7 Rh1 70.9(5) . . ? C11 C7 Rh1 127.7(7) . . ? C13 C12 P1 116.0(8) . . ? C15 C14 P1 116.6(9) . . ? O21 C21 C22 146.6 . . ? O21 C21 Rh1 101.869(16) . . ? C22 C21 Rh1 111.340(15) . . ? 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 C4 Rh1 P1 C14 -55.0(5) . . . . ? C3 Rh1 P1 C14 -90.3(5) . . . . ? C5 Rh1 P1 C14 -56.3(6) . . . . ? C6 Rh1 P1 C14 -111.7(6) . . . . ? C7 Rh1 P1 C14 -118.7(5) . . . . ? C21 Rh1 P1 C14 48.4(4) . . . . ? I1 Rh1 P1 C14 143.5(4) . . . . ? C4 Rh1 P1 C12 171.2(5) . . . . ? C3 Rh1 P1 C12 135.9(5) . . . . ? C5 Rh1 P1 C12 169.9(6) . . . . ? C6 Rh1 P1 C12 114.5(6) . . . . ? C7 Rh1 P1 C12 107.6(5) . . . . ? C21 Rh1 P1 C12 -85.4(4) . . . . ? I1 Rh1 P1 C12 9.7(4) . . . . ? C4 Rh1 P1 C1 57.8(5) . . . . ? C3 Rh1 P1 C1 22.5(5) . . . . ? C5 Rh1 P1 C1 56.5(6) . . . . ? C6 Rh1 P1 C1 1.1(6) . . . . ? C7 Rh1 P1 C1 -5.9(5) . . . . ? C21 Rh1 P1 C1 161.2(4) . . . . ? I1 Rh1 P1 C1 -103.7(4) . . . . ? C14 P1 C1 C2 82.4(9) . . . . ? C12 P1 C1 C2 -168.7(8) . . . . ? Rh1 P1 C1 C2 -42.9(8) . . . . ? P1 C1 C2 C3 44.7(12) . . . . ? C1 C2 C3 C7 66.7(13) . . . . ? C1 C2 C3 C4 -105.8(11) . . . . ? C1 C2 C3 Rh1 -24.3(12) . . . . ? C4 Rh1 C3 C7 116.2(8) . . . . ? P1 Rh1 C3 C7 -127.9(5) . . . . ? C5 Rh1 C3 C7 76.7(6) . . . . ? C6 Rh1 C3 C7 37.3(6) . . . . ? C21 Rh1 C3 C7 144.2(5) . . . . ? I1 Rh1 C3 C7 -33.2(6) . . . . ? P1 Rh1 C3 C4 115.9(5) . . . . ? C5 Rh1 C3 C4 -39.5(5) . . . . ? C6 Rh1 C3 C4 -78.9(6) . . . . ? C7 Rh1 C3 C4 -116.2(8) . . . . ? C21 Rh1 C3 C4 28.0(7) . . . . ? I1 Rh1 C3 C4 -149.4(4) . . . . ? C4 Rh1 C3 C2 -119.1(10) . . . . ? P1 Rh1 C3 C2 -3.2(7) . . . . ? C5 Rh1 C3 C2 -158.5(9) . . . . ? C6 Rh1 C3 C2 162.0(9) . . . . ? C7 Rh1 C3 C2 124.7(10) . . . . ? C21 Rh1 C3 C2 -91.1(8) . . . . ? I1 Rh1 C3 C2 91.6(8) . . . . ? C7 C3 C4 C5 0.3(10) . . . . ? C2 C3 C4 C5 174.0(8) . . . . ? Rh1 C3 C4 C5 66.8(6) . . . . ? C7 C3 C4 C8 170.1(9) . . . . ? C2 C3 C4 C8 -16.2(14) . . . . ? Rh1 C3 C4 C8 -123.4(10) . . . . ? C7 C3 C4 Rh1 -66.5(6) . . . . ? C2 C3 C4 Rh1 107.2(8) . . . . ? C3 Rh1 C4 C5 -112.9(8) . . . . ? P1 Rh1 C4 C5 -178.6(5) . . . . ? C6 Rh1 C4 C5 -34.3(5) . . . . ? C7 Rh1 C4 C5 -76.8(6) . . . . ? C21 Rh1 C4 C5 85.5(5) . . . . ? I1 Rh1 C4 C5 -44.4(9) . . . . ? P1 Rh1 C4 C3 -65.7(5) . . . . ? C5 Rh1 C4 C3 112.9(8) . . . . ? C6 Rh1 C4 C3 78.6(6) . . . . ? C7 Rh1 C4 C3 36.2(5) . . . . ? C21 Rh1 C4 C3 -161.5(5) . . . . ? I1 Rh1 C4 C3 68.5(8) . . . . ? C3 Rh1 C4 C8 121.2(11) . . . . ? P1 Rh1 C4 C8 55.5(9) . . . . ? C5 Rh1 C4 C8 -125.9(11) . . . . ? C6 Rh1 C4 C8 -160.2(11) . . . . ? C7 Rh1 C4 C8 157.4(11) . . . . ? C21 Rh1 C4 C8 -40.3(9) . . . . ? I1 Rh1 C4 C8 -170.3(6) . . . . ? C3 C4 C5 C6 -2.5(10) . . . . ? C8 C4 C5 C6 -172.0(10) . . . . ? Rh1 C4 C5 C6 62.4(7) . . . . ? C3 C4 C5 C9 175.3(9) . . . . ? C8 C4 C5 C9 5.8(15) . . . . ? Rh1 C4 C5 C9 -119.8(9) . . . . ? C3 C4 C5 Rh1 -64.9(6) . . . . ? C8 C4 C5 Rh1 125.6(10) . . . . ? C4 Rh1 C5 C6 -119.4(8) . . . . ? C3 Rh1 C5 C6 -78.5(6) . . . . ? P1 Rh1 C5 C6 -117.3(6) . . . . ? C7 Rh1 C5 C6 -37.9(6) . . . . ? C21 Rh1 C5 C6 139.4(5) . . . . ? I1 Rh1 C5 C6 39.6(6) . . . . ? C3 Rh1 C5 C4 40.9(5) . . . . ? P1 Rh1 C5 C4 2.0(7) . . . . ? C6 Rh1 C5 C4 119.4(8) . . . . ? C7 Rh1 C5 C4 81.5(6) . . . . ? C21 Rh1 C5 C4 -101.2(5) . . . . ? I1 Rh1 C5 C4 158.9(4) . . . . ? C4 Rh1 C5 C9 115.1(12) . . . . ? C3 Rh1 C5 C9 156.0(12) . . . . ? P1 Rh1 C5 C9 117.1(9) . . . . ? C6 Rh1 C5 C9 -125.5(13) . . . . ? C7 Rh1 C5 C9 -163.4(12) . . . . ? C21 Rh1 C5 C9 13.9(10) . . . . ? I1 Rh1 C5 C9 -86.0(10) . . . . ? C4 C5 C6 C7 3.7(11) . . . . ? C9 C5 C6 C7 -174.0(10) . . . . ? Rh1 C5 C6 C7 62.7(7) . . . . ? C4 C5 C6 C10 174.9(10) . . . . ? C9 C5 C6 C10 -2.8(17) . . . . ? Rh1 C5 C6 C10 -126.1(11) . . . . ? C4 C5 C6 Rh1 -59.0(6) . . . . ? C9 C5 C6 Rh1 123.3(10) . . . . ? C4 Rh1 C6 C5 37.4(6) . . . . ? C3 Rh1 C6 C5 82.3(6) . . . . ? P1 Rh1 C6 C5 106.8(6) . . . . ? C7 Rh1 C6 C5 118.0(8) . . . . ? C21 Rh1 C6 C5 -49.6(6) . . . . ? I1 Rh1 C6 C5 -147.0(6) . . . . ? C4 Rh1 C6 C7 -80.5(6) . . . . ? C3 Rh1 C6 C7 -35.7(5) . . . . ? P1 Rh1 C6 C7 -11.2(8) . . . . ? C5 Rh1 C6 C7 -118.0(8) . . . . ? C21 Rh1 C6 C7 -167.6(4) . . . . ? I1 Rh1 C6 C7 95.1(5) . . . . ? C4 Rh1 C6 C10 160.1(13) . . . . ? C3 Rh1 C6 C10 -155.1(13) . . . . ? P1 Rh1 C6 C10 -130.6(10) . . . . ? C5 Rh1 C6 C10 122.6(14) . . . . ? C7 Rh1 C6 C10 -119.4(14) . . . . ? C21 Rh1 C6 C10 73.0(12) . . . . ? I1 Rh1 C6 C10 -24.3(12) . . . . ? C4 C3 C7 C6 1.8(10) . . . . ? C2 C3 C7 C6 -171.7(9) . . . . ? Rh1 C3 C7 C6 -60.6(6) . . . . ? C4 C3 C7 C11 -175.7(10) . . . . ? C2 C3 C7 C11 10.8(16) . . . . ? Rh1 C3 C7 C11 121.9(10) . . . . ? C4 C3 C7 Rh1 62.4(6) . . . . ? C2 C3 C7 Rh1 -111.1(9) . . . . ? C5 C6 C7 C3 -3.5(11) . . . . ? C10 C6 C7 C3 -174.9(10) . . . . ? Rh1 C6 C7 C3 59.2(6) . . . . ? C5 C6 C7 C11 174.1(10) . . . . ? C10 C6 C7 C11 2.7(16) . . . . ? Rh1 C6 C7 C11 -123.2(10) . . . . ? C5 C6 C7 Rh1 -62.7(7) . . . . ? C10 C6 C7 Rh1 125.9(10) . . . . ? C4 Rh1 C7 C3 -39.8(6) . . . . ? P1 Rh1 C7 C3 54.5(5) . . . . ? C5 Rh1 C7 C3 -83.1(6) . . . . ? C6 Rh1 C7 C3 -118.4(8) . . . . ? C21 Rh1 C7 C3 -90.2(8) . . . . ? I1 Rh1 C7 C3 153.8(5) . . . . ? C4 Rh1 C7 C6 78.6(6) . . . . ? C3 Rh1 C7 C6 118.4(8) . . . . ? P1 Rh1 C7 C6 172.9(5) . . . . ? C5 Rh1 C7 C6 35.3(5) . . . . ? C21 Rh1 C7 C6 28.2(10) . . . . ? I1 Rh1 C7 C6 -87.8(5) . . . . ? C4 Rh1 C7 C11 -161.6(11) . . . . ? C3 Rh1 C7 C11 -121.8(12) . . . . ? P1 Rh1 C7 C11 -67.3(10) . . . . ? C5 Rh1 C7 C11 155.1(11) . . . . ? C6 Rh1 C7 C11 119.8(12) . . . . ? C21 Rh1 C7 C11 148.1(8) . . . . ? I1 Rh1 C7 C11 32.0(10) . . . . ? C14 P1 C12 C13 52.8(10) . . . . ? C1 P1 C12 C13 -55.5(10) . . . . ? Rh1 P1 C12 C13 -167.2(7) . . . . ? C12 P1 C14 C15 56.1(10) . . . . ? C1 P1 C14 C15 164.6(9) . . . . ? Rh1 P1 C14 C15 -84.1(9) . . . . ? C4 Rh1 C21 O21 2.5(3) . . . . ? C3 Rh1 C21 O21 -15.1(4) . . . . ? P1 Rh1 C21 O21 -99.50(6) . . . . ? C5 Rh1 C21 O21 40.4(3) . . . . ? C6 Rh1 C21 O21 66.3(3) . . . . ? C7 Rh1 C21 O21 46.6(7) . . . . ? I1 Rh1 C21 O21 162.75(2) . . . . ? C4 Rh1 C21 C22 178.5(3) . . . . ? C3 Rh1 C21 C22 160.9(4) . . . . ? P1 Rh1 C21 C22 76.52(6) . . . . ? C5 Rh1 C21 C22 -143.5(3) . . . . ? C6 Rh1 C21 C22 -117.7(3) . . . . ? C7 Rh1 C21 C22 -137.4(7) . . . . ? I1 Rh1 C21 C22 -21.23(3) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 2.829 _refine_diff_density_min -1.024 _refine_diff_density_rms 0.148 data_10 _database_code_CSD 197740 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H26 Cl2 P Rh.[C6 H6]0.25' _chemical_formula_sum 'C16.50 H27.50 Cl2 P Rh' _chemical_formula_weight 430.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 30.6515(13) _cell_length_b 8.6919(4) _cell_length_c 28.3619(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7556.2(5) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 42 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max .1 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3528 _exptl_absorpt_coefficient_mu 1.263 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.329558 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31133 _diffrn_reflns_av_R_equivalents 0.3568 _diffrn_reflns_av_sigmaI/netI 0.2141 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 23.37 _reflns_number_total 5421 _reflns_number_gt 2311 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0951P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_number_reflns 5421 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2058 _refine_ls_R_factor_gt 0.0766 _refine_ls_wR_factor_ref 0.2125 _refine_ls_wR_factor_gt 0.1570 _refine_ls_goodness_of_fit_ref 0.917 _refine_ls_restrained_S_all 0.917 _refine_ls_shift/su_max 0.122 _refine_ls_shift/su_mean 0.006 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 0.85593(4) 0.08142(14) 0.62535(4) 0.0312(4) Uani 1 1 d . . . Cl1 Cl 0.92866(13) 0.0623(6) 0.59483(16) 0.0553(13) Uani 1 1 d . . . Cl2 Cl 0.84478(16) 0.3388(5) 0.59603(16) 0.0552(13) Uani 1 1 d . . . P1 P 0.88042(14) 0.1517(5) 0.69731(15) 0.0361(11) Uani 1 1 d . . . C1 C 0.8346(5) 0.0932(19) 0.7358(5) 0.048(5) Uani 1 1 d . . . H1A H 0.8444 0.0844 0.7682 0.058 Uiso 1 1 calc R . . H1B H 0.8114 0.1686 0.7343 0.058 Uiso 1 1 calc R . . C2 C 0.8189(5) -0.0599(19) 0.7179(6) 0.049(5) Uani 1 1 d . . . H2A H 0.7903 -0.0805 0.7311 0.059 Uiso 1 1 calc R . . H2B H 0.8385 -0.1396 0.7290 0.059 Uiso 1 1 calc R . . C3 C 0.8161(5) -0.0682(17) 0.6650(5) 0.034(4) Uani 1 1 d . . . C4 C 0.7892(5) 0.0221(17) 0.6360(5) 0.033(4) Uani 1 1 d . . . C5 C 0.7960(6) -0.0196(19) 0.5878(6) 0.043(5) Uani 1 1 d . . . C6 C 0.8286(5) -0.1281(19) 0.5870(6) 0.039(5) Uani 1 1 d . . . C7 C 0.8421(5) -0.1523(16) 0.6339(5) 0.032(4) Uani 1 1 d . . . C8 C 0.7525(6) 0.129(2) 0.6521(6) 0.062(5) Uani 1 1 d . . . H8A H 0.7393 0.1767 0.6251 0.093 Uiso 1 1 calc R . . H8B H 0.7643 0.2073 0.6724 0.093 Uiso 1 1 calc R . . H8C H 0.7309 0.0709 0.6689 0.093 Uiso 1 1 calc R . . C9 C 0.7724(5) 0.053(2) 0.5465(6) 0.063(6) Uani 1 1 d . . . H9A H 0.7516 0.1260 0.5579 0.094 Uiso 1 1 calc R . . H9B H 0.7576 -0.0260 0.5289 0.094 Uiso 1 1 calc R . . H9C H 0.7932 0.1036 0.5265 0.094 Uiso 1 1 calc R . . C10 C 0.8479(6) -0.209(2) 0.5447(6) 0.063(6) Uani 1 1 d . . . H10A H 0.8702 -0.2789 0.5550 0.094 Uiso 1 1 calc R . . H10B H 0.8603 -0.1342 0.5237 0.094 Uiso 1 1 calc R . . H10C H 0.8254 -0.2651 0.5286 0.094 Uiso 1 1 calc R . . C11 C 0.8755(5) -0.2754(18) 0.6478(6) 0.048(5) Uani 1 1 d . . . H11A H 0.8894 -0.3144 0.6199 0.073 Uiso 1 1 calc R . . H11B H 0.8609 -0.3579 0.6638 0.073 Uiso 1 1 calc R . . H11C H 0.8970 -0.2309 0.6682 0.073 Uiso 1 1 calc R . . C12 C 0.9277(5) 0.0437(19) 0.7190(6) 0.054(5) Uani 1 1 d . . . H12A H 0.9212 -0.0653 0.7172 0.065 Uiso 1 1 calc R . . H12B H 0.9522 0.0635 0.6983 0.065 Uiso 1 1 calc R . . C13 C 0.9411(6) 0.081(2) 0.7687(6) 0.074(6) Uani 1 1 d . . . H13A H 0.9659 0.0197 0.7773 0.111 Uiso 1 1 calc R . . H13B H 0.9174 0.0597 0.7897 0.111 Uiso 1 1 calc R . . H13C H 0.9487 0.1882 0.7708 0.111 Uiso 1 1 calc R . . C14 C 0.8917(5) 0.3538(16) 0.7107(6) 0.043(5) Uani 1 1 d . . . H14A H 0.8677 0.4169 0.6998 0.052 Uiso 1 1 calc R . . H14B H 0.8942 0.3669 0.7446 0.052 Uiso 1 1 calc R . . C15 C 0.9349(5) 0.408(2) 0.6866(7) 0.071(6) Uani 1 1 d . . . H15A H 0.9400 0.5142 0.6940 0.107 Uiso 1 1 calc R . . H15B H 0.9323 0.3961 0.6530 0.107 Uiso 1 1 calc R . . H15C H 0.9588 0.3469 0.6979 0.107 Uiso 1 1 calc R . . Rh21 Rh 0.88327(4) -0.28118(15) 0.86959(4) 0.0359(4) Uani 1 1 d . . . Cl3 Cl 0.89363(15) -0.3132(6) 0.78621(15) 0.0549(13) Uani 1 1 d . . . Cl4 Cl 0.83849(15) -0.0539(5) 0.85939(16) 0.0609(14) Uani 1 1 d . . . P21 P 0.82666(14) -0.4485(6) 0.87306(18) 0.0525(13) Uani 1 1 d . . . C21 C 0.8441(5) -0.590(2) 0.9162(7) 0.070(6) Uani 1 1 d . . . H21A H 0.8188 -0.6282 0.9331 0.084 Uiso 1 1 calc R . . H21B H 0.8575 -0.6761 0.9000 0.084 Uiso 1 1 calc R . . C22 C 0.8761(6) -0.524(2) 0.9511(7) 0.068(6) Uani 1 1 d . . . H22A H 0.8943 -0.6056 0.9635 0.081 Uiso 1 1 calc R . . H22B H 0.8603 -0.4783 0.9772 0.081 Uiso 1 1 calc R . . C23 C 0.9048(6) -0.402(2) 0.9284(6) 0.049(5) Uani 1 1 d . . . C24 C 0.9049(6) -0.242(3) 0.9407(6) 0.057(6) Uani 1 1 d . . . C25 C 0.9362(6) -0.1670(19) 0.9115(6) 0.037(4) Uani 1 1 d . . . C26 C 0.9558(5) -0.277(2) 0.8830(5) 0.041(4) Uani 1 1 d . . . C27 C 0.9356(5) -0.421(2) 0.8923(6) 0.045(5) Uani 1 1 d . . . C28 C 0.8798(6) -0.164(2) 0.9777(6) 0.078(7) Uani 1 1 d . . . H28A H 0.8611 -0.2370 0.9932 0.117 Uiso 1 1 calc R . . H28B H 0.8623 -0.0843 0.9638 0.117 Uiso 1 1 calc R . . H28C H 0.8994 -0.1198 1.0002 0.117 Uiso 1 1 calc R . . C29 C 0.9467(6) 0.009(2) 0.9127(7) 0.080(7) Uani 1 1 d . . . H29A H 0.9283 0.0584 0.9355 0.120 Uiso 1 1 calc R . . H29B H 0.9415 0.0526 0.8821 0.120 Uiso 1 1 calc R . . H29C H 0.9767 0.0237 0.9212 0.120 Uiso 1 1 calc R . . C30 C 0.9917(5) -0.2485(19) 0.8476(6) 0.051(5) Uani 1 1 d . . . H30A H 0.9994 -0.3437 0.8325 0.077 Uiso 1 1 calc R . . H30B H 1.0168 -0.2073 0.8634 0.077 Uiso 1 1 calc R . . H30C H 0.9818 -0.1766 0.8242 0.077 Uiso 1 1 calc R . . C31 C 0.9488(6) -0.573(2) 0.8699(7) 0.068(6) Uani 1 1 d . . . H31A H 0.9303 -0.6540 0.8816 0.102 Uiso 1 1 calc R . . H31B H 0.9786 -0.5960 0.8777 0.102 Uiso 1 1 calc R . . H31C H 0.9458 -0.5665 0.8363 0.102 Uiso 1 1 calc R . . C32 C 0.8132(6) -0.560(2) 0.8218(6) 0.072(6) Uani 1 1 d . . . H32A H 0.8400 -0.5981 0.8079 0.087 Uiso 1 1 calc R . . H32B H 0.7962 -0.6485 0.8316 0.087 Uiso 1 1 calc R . . C33 C 0.7877(7) -0.473(3) 0.7842(9) 0.117(10) Uani 1 1 d . . . H33A H 0.7817 -0.5405 0.7582 0.176 Uiso 1 1 calc R . . H33B H 0.8047 -0.3871 0.7733 0.176 Uiso 1 1 calc R . . H33C H 0.7608 -0.4367 0.7973 0.176 Uiso 1 1 calc R . . C34 C 0.7737(6) -0.381(3) 0.8947(9) 0.095(8) Uani 1 1 d . . . H34A H 0.7626 -0.3059 0.8722 0.114 Uiso 1 1 calc R . . H34B H 0.7537 -0.4672 0.8944 0.114 Uiso 1 1 calc R . . C35 C 0.7719(6) -0.309(3) 0.9425(7) 0.101(9) Uani 1 1 d . . . H35A H 0.7424 -0.2804 0.9496 0.152 Uiso 1 1 calc R . . H35B H 0.7902 -0.2197 0.9432 0.152 Uiso 1 1 calc R . . H35C H 0.7820 -0.3821 0.9655 0.152 Uiso 1 1 calc R . . C41 C 0.984(2) 0.367(7) 0.5154(18) 0.133(17) Uani 1 1 d . . . H41A H 0.9711 0.2768 0.5258 0.160 Uiso 1 1 calc R . . C42 C 0.9698(12) 0.504(13) 0.5304(11) 0.15(2) Uani 1 1 d . . . H42A H 0.9492 0.5026 0.5545 0.181 Uiso 1 1 calc R . . C43 C 0.982(2) 0.641(6) 0.515(3) 0.20(3) Uani 1 1 d . . . H43A H 0.9680 0.7322 0.5234 0.239 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 0.0194(7) 0.0336(7) 0.0406(7) 0.0013(7) 0.0022(7) -0.0005(6) Cl1 0.022(2) 0.084(4) 0.060(3) 0.009(3) 0.011(2) 0.001(3) Cl2 0.063(4) 0.041(3) 0.061(3) 0.010(2) -0.006(3) -0.003(3) P1 0.024(2) 0.037(3) 0.047(3) 0.004(2) 0.004(2) -0.006(2) C1 0.037(10) 0.065(13) 0.043(10) -0.011(10) 0.008(9) 0.001(10) C2 0.028(10) 0.043(12) 0.076(13) 0.013(11) 0.015(9) -0.022(10) C3 0.029(10) 0.028(10) 0.044(10) 0.007(9) 0.015(8) 0.000(9) C4 0.035(10) 0.032(10) 0.031(10) 0.006(8) -0.011(8) 0.017(8) C5 0.039(12) 0.034(11) 0.056(12) 0.004(9) -0.023(10) -0.004(9) C6 0.032(11) 0.040(12) 0.047(11) 0.002(9) -0.002(9) -0.010(9) C7 0.015(8) 0.031(9) 0.048(10) -0.010(9) -0.009(8) 0.005(7) C8 0.039(12) 0.069(13) 0.079(13) 0.002(11) -0.005(11) 0.015(11) C9 0.029(11) 0.110(17) 0.050(11) 0.022(12) -0.023(9) 0.000(11) C10 0.058(14) 0.065(13) 0.065(12) -0.028(11) 0.010(11) 0.008(11) C11 0.022(10) 0.048(10) 0.076(12) 0.014(10) -0.014(9) -0.004(9) C12 0.044(12) 0.051(12) 0.067(13) 0.005(10) -0.009(10) -0.016(10) C13 0.070(15) 0.098(17) 0.054(12) 0.010(13) -0.022(11) -0.007(13) C14 0.054(13) 0.025(9) 0.051(11) 0.002(9) -0.005(9) 0.002(9) C15 0.020(10) 0.092(16) 0.102(16) -0.004(13) -0.004(11) -0.026(11) Rh21 0.0231(7) 0.0466(8) 0.0379(7) 0.0045(7) -0.0034(7) 0.0000(6) Cl3 0.049(3) 0.070(3) 0.047(3) 0.002(3) -0.003(2) -0.001(3) Cl4 0.045(3) 0.071(3) 0.066(3) 0.014(3) 0.008(2) 0.020(3) P21 0.028(3) 0.075(4) 0.055(3) 0.013(3) -0.004(3) -0.007(2) C21 0.026(11) 0.079(15) 0.105(16) 0.020(14) -0.011(11) -0.018(11) C22 0.053(14) 0.079(15) 0.071(14) 0.036(12) -0.015(12) -0.010(12) C23 0.035(11) 0.058(14) 0.055(12) -0.002(11) -0.008(10) -0.015(11) C24 0.026(11) 0.11(2) 0.029(10) -0.013(12) -0.013(9) 0.013(12) C25 0.044(12) 0.031(11) 0.035(10) -0.007(9) -0.019(9) -0.007(9) C26 0.037(11) 0.051(11) 0.037(10) 0.005(10) 0.002(8) -0.001(10) C27 0.032(10) 0.034(11) 0.069(12) 0.003(10) -0.007(9) -0.010(10) C28 0.065(15) 0.13(2) 0.041(11) -0.019(12) -0.023(11) 0.009(14) C29 0.059(15) 0.097(18) 0.085(16) -0.029(14) -0.011(12) -0.011(13) C30 0.009(9) 0.067(13) 0.078(12) 0.019(11) 0.003(8) 0.001(9) C31 0.057(13) 0.059(13) 0.088(14) -0.008(14) -0.015(12) 0.015(11) C32 0.056(14) 0.100(17) 0.060(13) 0.002(13) -0.007(11) -0.043(14) C33 0.049(15) 0.16(3) 0.14(2) -0.01(2) -0.049(16) -0.009(16) C34 0.023(12) 0.12(2) 0.14(2) 0.034(18) -0.001(14) 0.033(13) C35 0.059(16) 0.16(2) 0.082(16) -0.006(17) 0.030(13) 0.045(16) C41 0.10(3) 0.17(5) 0.13(3) 0.04(3) -0.09(3) -0.08(3) C42 0.09(3) 0.31(7) 0.057(18) -0.01(3) -0.039(17) 0.01(5) C43 0.09(4) 0.16(4) 0.35(9) 0.04(4) -0.15(5) -0.01(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 C7 2.089(14) . ? Rh1 C3 2.110(14) . ? Rh1 C4 2.131(16) . ? Rh1 P1 2.259(4) . ? Rh1 C6 2.281(16) . ? Rh1 C5 2.297(16) . ? Rh1 Cl1 2.397(4) . ? Rh1 Cl2 2.411(4) . ? P1 C14 1.830(15) . ? P1 C12 1.833(17) . ? P1 C1 1.848(16) . ? C1 C2 1.50(2) . ? C2 C3 1.50(2) . ? C3 C7 1.397(19) . ? C3 C4 1.406(19) . ? C4 C5 1.43(2) . ? C4 C8 1.53(2) . ? C5 C6 1.37(2) . ? C5 C9 1.51(2) . ? C6 C7 1.41(2) . ? C6 C10 1.51(2) . ? C7 C11 1.532(19) . ? C12 C13 1.50(2) . ? C14 C15 1.56(2) . ? Rh21 C23 2.080(18) . ? Rh21 C27 2.112(17) . ? Rh21 C24 2.148(16) . ? Rh21 C25 2.242(15) . ? Rh21 C26 2.255(16) . ? Rh21 P21 2.266(5) . ? Rh21 Cl3 2.402(4) . ? Rh21 Cl4 2.423(5) . ? P21 C32 1.796(17) . ? P21 C21 1.815(18) . ? P21 C34 1.833(19) . ? C21 C22 1.51(2) . ? C22 C23 1.52(2) . ? C23 C27 1.40(2) . ? C23 C24 1.43(2) . ? C24 C25 1.43(2) . ? C24 C28 1.47(2) . ? C25 C26 1.39(2) . ? C25 C29 1.56(2) . ? C26 C27 1.42(2) . ? C26 C30 1.51(2) . ? C27 C31 1.53(2) . ? C32 C33 1.52(2) . ? C34 C35 1.49(3) . ? C41 C43 1.35(6) 5_766 ? C41 C42 1.34(5) . ? C42 C43 1.32(5) . ? C43 C41 1.35(6) 5_766 ? 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 C7 Rh1 C3 38.9(5) . . ? C7 Rh1 C4 63.5(5) . . ? C3 Rh1 C4 38.7(5) . . ? C7 Rh1 P1 103.0(4) . . ? C3 Rh1 P1 82.9(4) . . ? C4 Rh1 P1 104.9(4) . . ? C7 Rh1 C6 37.3(5) . . ? C3 Rh1 C6 63.2(6) . . ? C4 Rh1 C6 61.4(6) . . ? P1 Rh1 C6 140.3(4) . . ? C7 Rh1 C5 61.3(6) . . ? C3 Rh1 C5 63.2(6) . . ? C4 Rh1 C5 37.4(6) . . ? P1 Rh1 C5 142.0(5) . . ? C6 Rh1 C5 34.9(6) . . ? C7 Rh1 Cl1 99.4(4) . . ? C3 Rh1 Cl1 133.5(4) . . ? C4 Rh1 Cl1 158.0(4) . . ? P1 Rh1 Cl1 92.06(16) . . ? C6 Rh1 Cl1 96.5(4) . . ? C5 Rh1 Cl1 123.3(5) . . ? C7 Rh1 Cl2 156.0(4) . . ? C3 Rh1 Cl2 132.4(4) . . ? C4 Rh1 Cl2 97.9(4) . . ? P1 Rh1 Cl2 96.19(16) . . ? C6 Rh1 Cl2 121.6(4) . . ? C5 Rh1 Cl2 94.7(4) . . ? Cl1 Rh1 Cl2 94.11(17) . . ? C14 P1 C12 105.8(8) . . ? C14 P1 C1 106.6(7) . . ? C12 P1 C1 105.1(8) . . ? C14 P1 Rh1 120.7(5) . . ? C12 P1 Rh1 115.3(6) . . ? C1 P1 Rh1 101.9(5) . . ? C2 C1 P1 106.8(10) . . ? C1 C2 C3 113.4(13) . . ? C7 C3 C4 104.8(13) . . ? C7 C3 C2 128.5(15) . . ? C4 C3 C2 126.3(14) . . ? C7 C3 Rh1 69.8(8) . . ? C4 C3 Rh1 71.5(9) . . ? C2 C3 Rh1 118.0(10) . . ? C3 C4 C5 109.5(13) . . ? C3 C4 C8 126.5(14) . . ? C5 C4 C8 123.2(14) . . ? C3 C4 Rh1 69.8(9) . . ? C5 C4 Rh1 77.6(10) . . ? C8 C4 Rh1 126.9(11) . . ? C6 C5 C4 107.3(14) . . ? C6 C5 C9 128.2(17) . . ? C4 C5 C9 124.4(15) . . ? C6 C5 Rh1 71.9(10) . . ? C4 C5 Rh1 65.0(9) . . ? C9 C5 Rh1 125.6(12) . . ? C5 C6 C7 107.4(14) . . ? C5 C6 C10 128.1(16) . . ? C7 C6 C10 124.4(15) . . ? C5 C6 Rh1 73.2(10) . . ? C7 C6 Rh1 63.9(8) . . ? C10 C6 Rh1 127.4(11) . . ? C3 C7 C6 110.6(14) . . ? C3 C7 C11 125.8(14) . . ? C6 C7 C11 122.8(14) . . ? C3 C7 Rh1 71.4(8) . . ? C6 C7 Rh1 78.7(9) . . ? C11 C7 Rh1 125.0(10) . . ? C13 C12 P1 114.9(13) . . ? C15 C14 P1 111.0(11) . . ? C23 Rh21 C27 39.1(6) . . ? C23 Rh21 C24 39.5(7) . . ? C27 Rh21 C24 64.5(7) . . ? C23 Rh21 C25 64.5(6) . . ? C27 Rh21 C25 62.8(6) . . ? C24 Rh21 C25 37.9(6) . . ? C23 Rh21 C26 63.9(6) . . ? C27 Rh21 C26 37.8(6) . . ? C24 Rh21 C26 62.3(6) . . ? C25 Rh21 C26 35.9(5) . . ? C23 Rh21 P21 83.3(5) . . ? C27 Rh21 P21 101.5(5) . . ? C24 Rh21 P21 107.2(6) . . ? C25 Rh21 P21 144.6(5) . . ? C26 Rh21 P21 139.3(5) . . ? C23 Rh21 Cl3 133.6(6) . . ? C27 Rh21 Cl3 97.6(5) . . ? C24 Rh21 Cl3 154.3(5) . . ? C25 Rh21 Cl3 118.5(5) . . ? C26 Rh21 Cl3 92.2(4) . . ? P21 Rh21 Cl3 93.99(18) . . ? C23 Rh21 Cl4 133.5(6) . . ? C27 Rh21 Cl4 159.2(5) . . ? C24 Rh21 Cl4 99.1(6) . . ? C25 Rh21 Cl4 96.4(5) . . ? C26 Rh21 Cl4 124.4(5) . . ? P21 Rh21 Cl4 95.44(17) . . ? Cl3 Rh21 Cl4 92.97(16) . . ? C32 P21 C21 104.3(9) . . ? C32 P21 C34 104.0(10) . . ? C21 P21 C34 104.7(10) . . ? C32 P21 Rh21 119.2(6) . . ? C21 P21 Rh21 103.8(6) . . ? C34 P21 Rh21 119.1(8) . . ? C22 C21 P21 112.0(13) . . ? C21 C22 C23 111.5(15) . . ? C27 C23 C24 106.7(16) . . ? C27 C23 C22 128.3(18) . . ? C24 C23 C22 125.0(18) . . ? C27 C23 Rh21 71.7(10) . . ? C24 C23 Rh21 72.8(10) . . ? C22 C23 Rh21 120.5(12) . . ? C25 C24 C23 107.8(16) . . ? C25 C24 C28 124(2) . . ? C23 C24 C28 128.5(19) . . ? C25 C24 Rh21 74.6(9) . . ? C23 C24 Rh21 67.6(10) . . ? C28 C24 Rh21 125.6(12) . . ? C26 C25 C24 108.2(15) . . ? C26 C25 C29 126.8(17) . . ? C24 C25 C29 125.0(17) . . ? C26 C25 Rh21 72.6(9) . . ? C24 C25 Rh21 67.5(9) . . ? C29 C25 Rh21 126.4(11) . . ? C25 C26 C27 108.1(15) . . ? C25 C26 C30 126.1(16) . . ? C27 C26 C30 125.7(16) . . ? C25 C26 Rh21 71.6(9) . . ? C27 C26 Rh21 65.7(9) . . ? C30 C26 Rh21 127.5(11) . . ? C23 C27 C26 109.1(16) . . ? C23 C27 C31 125.7(17) . . ? C26 C27 C31 125.0(16) . . ? C23 C27 Rh21 69.2(10) . . ? C26 C27 Rh21 76.6(10) . . ? C31 C27 Rh21 125.0(12) . . ? C33 C32 P21 114.6(16) . . ? C35 C34 P21 118.0(15) . . ? C43 C41 C42 120(4) 5_766 . ? C43 C42 C41 127(5) . . ? C41 C43 C42 112(5) 5_766 . ? 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 C7 Rh1 P1 C14 -173.4(7) . . . . ? C3 Rh1 P1 C14 -139.9(8) . . . . ? C4 Rh1 P1 C14 -107.8(7) . . . . ? C6 Rh1 P1 C14 -170.7(9) . . . . ? C5 Rh1 P1 C14 -113.6(9) . . . . ? Cl1 Rh1 P1 C14 86.5(6) . . . . ? Cl2 Rh1 P1 C14 -7.9(7) . . . . ? C7 Rh1 P1 C12 57.5(7) . . . . ? C3 Rh1 P1 C12 91.0(7) . . . . ? C4 Rh1 P1 C12 123.2(7) . . . . ? C6 Rh1 P1 C12 60.2(9) . . . . ? C5 Rh1 P1 C12 117.3(9) . . . . ? Cl1 Rh1 P1 C12 -42.6(6) . . . . ? Cl2 Rh1 P1 C12 -137.0(6) . . . . ? C7 Rh1 P1 C1 -55.7(7) . . . . ? C3 Rh1 P1 C1 -22.3(7) . . . . ? C4 Rh1 P1 C1 9.9(7) . . . . ? C6 Rh1 P1 C1 -53.1(9) . . . . ? C5 Rh1 P1 C1 4.0(9) . . . . ? Cl1 Rh1 P1 C1 -155.9(6) . . . . ? Cl2 Rh1 P1 C1 109.8(6) . . . . ? C14 P1 C1 C2 168.1(11) . . . . ? C12 P1 C1 C2 -80.0(13) . . . . ? Rh1 P1 C1 C2 40.7(12) . . . . ? P1 C1 C2 C3 -42.7(16) . . . . ? C1 C2 C3 C7 110.0(19) . . . . ? C1 C2 C3 C4 -62(2) . . . . ? C1 C2 C3 Rh1 24.4(18) . . . . ? C4 Rh1 C3 C7 114.3(13) . . . . ? P1 Rh1 C3 C7 -121.1(9) . . . . ? C6 Rh1 C3 C7 37.4(9) . . . . ? C5 Rh1 C3 C7 76.7(10) . . . . ? Cl1 Rh1 C3 C7 -34.9(11) . . . . ? Cl2 Rh1 C3 C7 147.0(7) . . . . ? C7 Rh1 C3 C4 -114.3(13) . . . . ? P1 Rh1 C3 C4 124.6(8) . . . . ? C6 Rh1 C3 C4 -76.9(9) . . . . ? C5 Rh1 C3 C4 -37.6(9) . . . . ? Cl1 Rh1 C3 C4 -149.2(7) . . . . ? Cl2 Rh1 C3 C4 32.7(11) . . . . ? C7 Rh1 C3 C2 123.7(16) . . . . ? C4 Rh1 C3 C2 -121.9(16) . . . . ? P1 Rh1 C3 C2 2.7(11) . . . . ? C6 Rh1 C3 C2 161.2(14) . . . . ? C5 Rh1 C3 C2 -159.5(14) . . . . ? Cl1 Rh1 C3 C2 88.8(13) . . . . ? Cl2 Rh1 C3 C2 -89.3(13) . . . . ? C7 C3 C4 C5 5.9(18) . . . . ? C2 C3 C4 C5 179.7(14) . . . . ? Rh1 C3 C4 C5 68.2(12) . . . . ? C7 C3 C4 C8 176.2(15) . . . . ? C2 C3 C4 C8 -10(3) . . . . ? Rh1 C3 C4 C8 -121.6(16) . . . . ? C7 C3 C4 Rh1 -62.2(10) . . . . ? C2 C3 C4 Rh1 111.6(15) . . . . ? C7 Rh1 C4 C3 39.7(9) . . . . ? P1 Rh1 C4 C3 -57.7(9) . . . . ? C6 Rh1 C4 C3 81.9(10) . . . . ? C5 Rh1 C4 C3 116.4(13) . . . . ? Cl1 Rh1 C4 C3 81.5(13) . . . . ? Cl2 Rh1 C4 C3 -156.2(8) . . . . ? C7 Rh1 C4 C5 -76.7(9) . . . . ? C3 Rh1 C4 C5 -116.4(13) . . . . ? P1 Rh1 C4 C5 -174.0(8) . . . . ? C6 Rh1 C4 C5 -34.4(8) . . . . ? Cl1 Rh1 C4 C5 -34.9(16) . . . . ? Cl2 Rh1 C4 C5 87.4(9) . . . . ? C7 Rh1 C4 C8 160.9(15) . . . . ? C3 Rh1 C4 C8 121.2(17) . . . . ? P1 Rh1 C4 C8 63.5(13) . . . . ? C6 Rh1 C4 C8 -156.9(15) . . . . ? C5 Rh1 C4 C8 -122.5(17) . . . . ? Cl1 Rh1 C4 C8 -157.4(9) . . . . ? Cl2 Rh1 C4 C8 -35.1(13) . . . . ? C3 C4 C5 C6 -3.4(19) . . . . ? C8 C4 C5 C6 -174.0(15) . . . . ? Rh1 C4 C5 C6 59.7(12) . . . . ? C3 C4 C5 C9 179.5(15) . . . . ? C8 C4 C5 C9 9(3) . . . . ? Rh1 C4 C5 C9 -117.3(16) . . . . ? C3 C4 C5 Rh1 -63.1(11) . . . . ? C8 C4 C5 Rh1 126.3(16) . . . . ? C7 Rh1 C5 C6 -36.9(9) . . . . ? C3 Rh1 C5 C6 -81.0(10) . . . . ? C4 Rh1 C5 C6 -119.8(14) . . . . ? P1 Rh1 C5 C6 -110.5(11) . . . . ? Cl1 Rh1 C5 C6 45.3(11) . . . . ? Cl2 Rh1 C5 C6 143.3(9) . . . . ? C7 Rh1 C5 C4 83.0(10) . . . . ? C3 Rh1 C5 C4 38.9(8) . . . . ? P1 Rh1 C5 C4 9.4(13) . . . . ? C6 Rh1 C5 C4 119.8(14) . . . . ? Cl1 Rh1 C5 C4 165.1(7) . . . . ? Cl2 Rh1 C5 C4 -96.9(8) . . . . ? C7 Rh1 C5 C9 -161.4(18) . . . . ? C3 Rh1 C5 C9 154.5(17) . . . . ? C4 Rh1 C5 C9 115.7(19) . . . . ? P1 Rh1 C5 C9 125.1(13) . . . . ? C6 Rh1 C5 C9 -124(2) . . . . ? Cl1 Rh1 C5 C9 -79.2(16) . . . . ? Cl2 Rh1 C5 C9 18.8(15) . . . . ? C4 C5 C6 C7 -0.5(19) . . . . ? C9 C5 C6 C7 176.3(16) . . . . ? Rh1 C5 C6 C7 54.8(11) . . . . ? C4 C5 C6 C10 180.0(16) . . . . ? C9 C5 C6 C10 -3(3) . . . . ? Rh1 C5 C6 C10 -124.7(18) . . . . ? C4 C5 C6 Rh1 -55.4(11) . . . . ? C9 C5 C6 Rh1 121.5(18) . . . . ? C7 Rh1 C6 C5 119.7(14) . . . . ? C3 Rh1 C6 C5 80.7(11) . . . . ? C4 Rh1 C6 C5 36.9(10) . . . . ? P1 Rh1 C6 C5 115.5(10) . . . . ? Cl1 Rh1 C6 C5 -143.3(10) . . . . ? Cl2 Rh1 C6 C5 -44.4(11) . . . . ? C3 Rh1 C6 C7 -39.0(9) . . . . ? C4 Rh1 C6 C7 -82.9(10) . . . . ? P1 Rh1 C6 C7 -4.3(13) . . . . ? C5 Rh1 C6 C7 -119.7(14) . . . . ? Cl1 Rh1 C6 C7 96.9(9) . . . . ? Cl2 Rh1 C6 C7 -164.1(7) . . . . ? C7 Rh1 C6 C10 -114.8(19) . . . . ? C3 Rh1 C6 C10 -153.7(17) . . . . ? C4 Rh1 C6 C10 162.4(17) . . . . ? P1 Rh1 C6 C10 -119.0(13) . . . . ? C5 Rh1 C6 C10 126(2) . . . . ? Cl1 Rh1 C6 C10 -17.8(15) . . . . ? Cl2 Rh1 C6 C10 81.1(15) . . . . ? C4 C3 C7 C6 -6.4(17) . . . . ? C2 C3 C7 C6 -179.9(15) . . . . ? Rh1 C3 C7 C6 -69.7(11) . . . . ? C4 C3 C7 C11 -176.4(14) . . . . ? C2 C3 C7 C11 10(3) . . . . ? Rh1 C3 C7 C11 120.2(15) . . . . ? C4 C3 C7 Rh1 63.4(10) . . . . ? C2 C3 C7 Rh1 -110.2(16) . . . . ? C5 C6 C7 C3 4.4(19) . . . . ? C10 C6 C7 C3 -176.1(15) . . . . ? Rh1 C6 C7 C3 65.0(11) . . . . ? C5 C6 C7 C11 174.8(14) . . . . ? C10 C6 C7 C11 -6(2) . . . . ? Rh1 C6 C7 C11 -124.6(15) . . . . ? C5 C6 C7 Rh1 -60.6(12) . . . . ? C10 C6 C7 Rh1 118.9(16) . . . . ? C4 Rh1 C7 C3 -39.6(9) . . . . ? P1 Rh1 C7 C3 60.8(9) . . . . ? C6 Rh1 C7 C3 -116.4(13) . . . . ? C5 Rh1 C7 C3 -81.9(10) . . . . ? Cl1 Rh1 C7 C3 155.1(8) . . . . ? Cl2 Rh1 C7 C3 -81.5(14) . . . . ? C3 Rh1 C7 C6 116.4(13) . . . . ? C4 Rh1 C7 C6 76.9(9) . . . . ? P1 Rh1 C7 C6 177.2(8) . . . . ? C5 Rh1 C7 C6 34.5(9) . . . . ? Cl1 Rh1 C7 C6 -88.5(9) . . . . ? Cl2 Rh1 C7 C6 34.9(16) . . . . ? C3 Rh1 C7 C11 -121.2(17) . . . . ? C4 Rh1 C7 C11 -160.8(15) . . . . ? P1 Rh1 C7 C11 -60.4(13) . . . . ? C6 Rh1 C7 C11 122.4(18) . . . . ? C5 Rh1 C7 C11 156.9(16) . . . . ? Cl1 Rh1 C7 C11 33.9(14) . . . . ? Cl2 Rh1 C7 C11 157.3(9) . . . . ? C14 P1 C12 C13 49.4(15) . . . . ? C1 P1 C12 C13 -63.2(14) . . . . ? Rh1 P1 C12 C13 -174.6(11) . . . . ? C12 P1 C14 C15 58.8(13) . . . . ? C1 P1 C14 C15 170.3(12) . . . . ? Rh1 P1 C14 C15 -74.4(13) . . . . ? C23 Rh21 P21 C32 -125.7(10) . . . . ? C27 Rh21 P21 C32 -90.9(9) . . . . ? C24 Rh21 P21 C32 -157.6(10) . . . . ? C25 Rh21 P21 C32 -149.7(11) . . . . ? C26 Rh21 P21 C32 -90.3(10) . . . . ? Cl3 Rh21 P21 C32 7.7(8) . . . . ? Cl4 Rh21 P21 C32 101.1(8) . . . . ? C23 Rh21 P21 C21 -10.3(9) . . . . ? C27 Rh21 P21 C21 24.5(9) . . . . ? C24 Rh21 P21 C21 -42.2(9) . . . . ? C25 Rh21 P21 C21 -34.3(11) . . . . ? C26 Rh21 P21 C21 25.1(10) . . . . ? Cl3 Rh21 P21 C21 123.1(7) . . . . ? Cl4 Rh21 P21 C21 -143.5(7) . . . . ? C23 Rh21 P21 C34 105.5(10) . . . . ? C27 Rh21 P21 C34 140.3(10) . . . . ? C24 Rh21 P21 C34 73.6(10) . . . . ? C25 Rh21 P21 C34 81.5(12) . . . . ? C26 Rh21 P21 C34 140.9(11) . . . . ? Cl3 Rh21 P21 C34 -121.1(9) . . . . ? Cl4 Rh21 P21 C34 -27.7(9) . . . . ? C32 P21 C21 C22 152.1(15) . . . . ? C34 P21 C21 C22 -98.9(16) . . . . ? Rh21 P21 C21 C22 26.6(16) . . . . ? P21 C21 C22 C23 -33(2) . . . . ? C21 C22 C23 C27 -65(3) . . . . ? C21 C22 C23 C24 115(2) . . . . ? C21 C22 C23 Rh21 25(2) . . . . ? C24 Rh21 C23 C27 -114.8(15) . . . . ? C25 Rh21 C23 C27 -77.5(11) . . . . ? C26 Rh21 C23 C27 -37.5(10) . . . . ? P21 Rh21 C23 C27 117.6(11) . . . . ? Cl3 Rh21 C23 C27 28.4(13) . . . . ? Cl4 Rh21 C23 C27 -151.2(9) . . . . ? C27 Rh21 C23 C24 114.8(15) . . . . ? C25 Rh21 C23 C24 37.3(10) . . . . ? C26 Rh21 C23 C24 77.3(11) . . . . ? P21 Rh21 C23 C24 -127.6(11) . . . . ? Cl3 Rh21 C23 C24 143.3(9) . . . . ? Cl4 Rh21 C23 C24 -36.4(13) . . . . ? C27 Rh21 C23 C22 -124(2) . . . . ? C24 Rh21 C23 C22 121(2) . . . . ? C25 Rh21 C23 C22 158.2(18) . . . . ? C26 Rh21 C23 C22 -161.8(19) . . . . ? P21 Rh21 C23 C22 -6.6(15) . . . . ? Cl3 Rh21 C23 C22 -95.8(16) . . . . ? Cl4 Rh21 C23 C22 84.5(16) . . . . ? C27 C23 C24 C25 -0.2(19) . . . . ? C22 C23 C24 C25 -179.9(15) . . . . ? Rh21 C23 C24 C25 -64.4(11) . . . . ? C27 C23 C24 C28 -177.4(16) . . . . ? C22 C23 C24 C28 3(3) . . . . ? Rh21 C23 C24 C28 118.5(17) . . . . ? C27 C23 C24 Rh21 64.2(12) . . . . ? C22 C23 C24 Rh21 -115.6(17) . . . . ? C23 Rh21 C24 C25 117.1(15) . . . . ? C27 Rh21 C24 C25 77.8(11) . . . . ? C26 Rh21 C24 C25 35.4(9) . . . . ? P21 Rh21 C24 C25 172.6(9) . . . . ? Cl3 Rh21 C24 C25 28(2) . . . . ? Cl4 Rh21 C24 C25 -88.8(10) . . . . ? C27 Rh21 C24 C23 -39.3(10) . . . . ? C25 Rh21 C24 C23 -117.1(15) . . . . ? C26 Rh21 C24 C23 -81.7(11) . . . . ? P21 Rh21 C24 C23 55.5(11) . . . . ? Cl3 Rh21 C24 C23 -88.8(18) . . . . ? Cl4 Rh21 C24 C23 154.1(10) . . . . ? C23 Rh21 C24 C28 -122(2) . . . . ? C27 Rh21 C24 C28 -162(2) . . . . ? C25 Rh21 C24 C28 121(2) . . . . ? C26 Rh21 C24 C28 156(2) . . . . ? P21 Rh21 C24 C28 -67(2) . . . . ? Cl3 Rh21 C24 C28 149.0(13) . . . . ? Cl4 Rh21 C24 C28 31.9(19) . . . . ? C23 C24 C25 C26 -1.6(18) . . . . ? C28 C24 C25 C26 175.7(15) . . . . ? Rh21 C24 C25 C26 -61.5(11) . . . . ? C23 C24 C25 C29 179.4(15) . . . . ? C28 C24 C25 C29 -3(3) . . . . ? Rh21 C24 C25 C29 119.6(16) . . . . ? C23 C24 C25 Rh21 59.9(11) . . . . ? C28 C24 C25 Rh21 -122.8(16) . . . . ? C23 Rh21 C25 C26 80.1(10) . . . . ? C27 Rh21 C25 C26 36.3(9) . . . . ? C24 Rh21 C25 C26 119.0(14) . . . . ? P21 Rh21 C25 C26 106.7(11) . . . . ? Cl3 Rh21 C25 C26 -47.5(10) . . . . ? Cl4 Rh21 C25 C26 -144.4(9) . . . . ? C23 Rh21 C25 C24 -38.9(11) . . . . ? C27 Rh21 C25 C24 -82.7(11) . . . . ? C26 Rh21 C25 C24 -119.0(14) . . . . ? P21 Rh21 C25 C24 -12.3(16) . . . . ? Cl3 Rh21 C25 C24 -166.5(10) . . . . ? Cl4 Rh21 C25 C24 96.6(11) . . . . ? C23 Rh21 C25 C29 -156.7(18) . . . . ? C27 Rh21 C25 C29 159.5(18) . . . . ? C24 Rh21 C25 C29 -118(2) . . . . ? C26 Rh21 C25 C29 123(2) . . . . ? P21 Rh21 C25 C29 -130.1(13) . . . . ? Cl3 Rh21 C25 C29 75.7(16) . . . . ? Cl4 Rh21 C25 C29 -21.2(16) . . . . ? C24 C25 C26 C27 2.8(18) . . . . ? C29 C25 C26 C27 -178.3(16) . . . . ? Rh21 C25 C26 C27 -55.5(11) . . . . ? C24 C25 C26 C30 -178.3(15) . . . . ? C29 C25 C26 C30 1(3) . . . . ? Rh21 C25 C26 C30 123.4(16) . . . . ? C24 C25 C26 Rh21 58.3(11) . . . . ? C29 C25 C26 Rh21 -122.8(17) . . . . ? C23 Rh21 C26 C25 -81.9(11) . . . . ? C27 Rh21 C26 C25 -120.7(14) . . . . ? C24 Rh21 C26 C25 -37.3(10) . . . . ? P21 Rh21 C26 C25 -121.8(10) . . . . ? Cl3 Rh21 C26 C25 139.6(9) . . . . ? Cl4 Rh21 C26 C25 44.5(10) . . . . ? C23 Rh21 C26 C27 38.8(10) . . . . ? C24 Rh21 C26 C27 83.4(12) . . . . ? C25 Rh21 C26 C27 120.7(14) . . . . ? P21 Rh21 C26 C27 -1.0(13) . . . . ? Cl3 Rh21 C26 C27 -99.7(10) . . . . ? Cl4 Rh21 C26 C27 165.2(9) . . . . ? C23 Rh21 C26 C30 156.2(18) . . . . ? C27 Rh21 C26 C30 117(2) . . . . ? C24 Rh21 C26 C30 -159.2(19) . . . . ? C25 Rh21 C26 C30 -122(2) . . . . ? P21 Rh21 C26 C30 116.4(14) . . . . ? Cl3 Rh21 C26 C30 17.7(15) . . . . ? Cl4 Rh21 C26 C30 -77.4(16) . . . . ? C24 C23 C27 C26 1.9(19) . . . . ? C22 C23 C27 C26 -178.4(16) . . . . ? Rh21 C23 C27 C26 66.8(12) . . . . ? C24 C23 C27 C31 176.2(15) . . . . ? C22 C23 C27 C31 -4(3) . . . . ? Rh21 C23 C27 C31 -118.9(17) . . . . ? C24 C23 C27 Rh21 -64.9(12) . . . . ? C22 C23 C27 Rh21 114.8(18) . . . . ? C25 C26 C27 C23 -3.0(19) . . . . ? C30 C26 C27 C23 178.1(15) . . . . ? Rh21 C26 C27 C23 -62.0(12) . . . . ? C25 C26 C27 C31 -177.3(15) . . . . ? C30 C26 C27 C31 4(3) . . . . ? Rh21 C26 C27 C31 123.6(17) . . . . ? C25 C26 C27 Rh21 59.1(12) . . . . ? C30 C26 C27 Rh21 -119.8(16) . . . . ? C24 Rh21 C27 C23 39.8(11) . . . . ? C25 Rh21 C27 C23 82.2(11) . . . . ? C26 Rh21 C27 C23 116.7(15) . . . . ? P21 Rh21 C27 C23 -63.9(11) . . . . ? Cl3 Rh21 C27 C23 -159.6(10) . . . . ? Cl4 Rh21 C27 C23 80.3(18) . . . . ? C23 Rh21 C27 C26 -116.7(15) . . . . ? C24 Rh21 C27 C26 -76.9(11) . . . . ? C25 Rh21 C27 C26 -34.5(9) . . . . ? P21 Rh21 C27 C26 179.3(9) . . . . ? Cl3 Rh21 C27 C26 83.6(10) . . . . ? Cl4 Rh21 C27 C26 -36(2) . . . . ? C23 Rh21 C27 C31 120(2) . . . . ? C24 Rh21 C27 C31 159.5(18) . . . . ? C25 Rh21 C27 C31 -158.1(17) . . . . ? C26 Rh21 C27 C31 -124(2) . . . . ? P21 Rh21 C27 C31 55.7(15) . . . . ? Cl3 Rh21 C27 C31 -39.9(15) . . . . ? Cl4 Rh21 C27 C31 -160.1(10) . . . . ? C21 P21 C32 C33 166.5(15) . . . . ? C34 P21 C32 C33 57.0(17) . . . . ? Rh21 P21 C32 C33 -78.4(16) . . . . ? C32 P21 C34 C35 168.2(18) . . . . ? C21 P21 C34 C35 59(2) . . . . ? Rh21 P21 C34 C35 -56(2) . . . . ? C43 C41 C42 C43 9(8) 5_766 . . . ? C41 C42 C43 C41 -8(7) . . . 5_766 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 23.37 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.971 _refine_diff_density_min -0.947 _refine_diff_density_rms 0.159 data_11 _database_code_CSD 197741 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H26 I2 P Rh' _chemical_formula_sum 'C15 H26 I2 P Rh' _chemical_formula_weight 594.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 12.1284(13) _cell_length_b 13.5763(15) _cell_length_c 11.9212(13) _cell_angle_alpha 90.00 _cell_angle_beta 92.718(8) _cell_angle_gamma 90.00 _cell_volume 1960.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 76 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max .18 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.012 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 4.090 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.638782 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4132 _diffrn_reflns_av_R_equivalents 0.1082 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 23.29 _reflns_number_total 2662 _reflns_number_gt 2473 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0572P)^2^+3.6741P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00182(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 2662 _refine_ls_number_parameters 182 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0842 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.002 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 -0.27808(5) 0.23815(4) -0.07303(5) 0.03400(19) Uani 1 1 d . . . I1 I -0.12400(5) 0.35969(5) 0.01907(5) 0.0594(2) Uani 1 1 d . . . I2 I -0.12799(5) 0.10891(5) -0.14471(6) 0.0619(2) Uani 1 1 d . . . P1 P -0.29933(17) 0.31694(16) -0.24082(18) 0.0402(5) Uani 1 1 d . . . C1 C -0.4363(8) 0.3728(8) -0.2302(10) 0.057(3) Uani 1 1 d . . . H1A H -0.4300 0.4334 -0.1873 0.069 Uiso 1 1 calc R . . H1B H -0.4672 0.3884 -0.3046 0.069 Uiso 1 1 calc R . . C2 C -0.5112(7) 0.3011(9) -0.1727(9) 0.058(2) Uani 1 1 d . . . H2A H -0.5733 0.3370 -0.1445 0.069 Uiso 1 1 calc R . . H2B H -0.5400 0.2537 -0.2274 0.069 Uiso 1 1 calc R . . C3 C -0.4536(6) 0.2473(7) -0.0776(8) 0.045(2) Uani 1 1 d . . . C4 C -0.4122(7) 0.2902(7) 0.0268(8) 0.045(2) Uani 1 1 d . . . C5 C -0.3590(8) 0.2130(9) 0.0914(7) 0.054(2) Uani 1 1 d . . . C6 C -0.3648(9) 0.1247(8) 0.0302(8) 0.056(2) Uani 1 1 d . . . C7 C -0.4229(8) 0.1453(7) -0.0767(9) 0.048(2) Uani 1 1 d . . . C8 C -0.4359(9) 0.3921(9) 0.0656(11) 0.071(3) Uani 1 1 d . . . H8A H -0.5014 0.3917 0.1078 0.106 Uiso 1 1 calc R . . H8B H -0.4468 0.4347 0.0017 0.106 Uiso 1 1 calc R . . H8C H -0.3748 0.4156 0.1123 0.106 Uiso 1 1 calc R . . C9 C -0.3134(10) 0.2242(12) 0.2118(9) 0.083(4) Uani 1 1 d G . . H9A H -0.3697 0.2078 0.2625 0.125 Uiso 1 1 calc R . . H9B H -0.2902 0.2911 0.2244 0.125 Uiso 1 1 calc R . . H9C H -0.2515 0.1809 0.2244 0.125 Uiso 1 1 calc R . . C10 C -0.3273(10) 0.0263(9) 0.0652(11) 0.075(3) Uani 1 1 d G . . H10A H -0.3825 -0.0043 0.1085 0.113 Uiso 1 1 calc R . . H10B H -0.2597 0.0318 0.1100 0.113 Uiso 1 1 calc R . . H10C H -0.3151 -0.0129 -0.0001 0.113 Uiso 1 1 calc R . . C11 C -0.4558(9) 0.0681(8) -0.1611(10) 0.066(3) Uani 1 1 d G . . H11A H -0.5242 0.0387 -0.1415 0.099 Uiso 1 1 calc R . . H11B H -0.3996 0.0184 -0.1620 0.099 Uiso 1 1 calc R . . H11C H -0.4648 0.0977 -0.2342 0.099 Uiso 1 1 calc R . . C12 C -0.2123(8) 0.4167(8) -0.2797(9) 0.059(2) Uani 1 1 d . . . H12A H -0.2470 0.4515 -0.3430 0.071 Uiso 1 1 calc R . . H12B H -0.2037 0.4626 -0.2175 0.071 Uiso 1 1 calc R . . C13 C -0.0969(9) 0.3793(10) -0.3115(11) 0.067(3) Uani 1 1 d . . . H13A H -0.0522 0.4343 -0.3319 0.100 Uiso 1 1 calc R . . H13B H -0.1051 0.3348 -0.3739 0.100 Uiso 1 1 calc R . . H13C H -0.0619 0.3457 -0.2485 0.100 Uiso 1 1 calc R . . C14 C -0.3113(11) 0.2384(9) -0.3633(9) 0.066(3) Uani 1 1 d . . . H14A H -0.2438 0.2002 -0.3664 0.079 Uiso 1 1 calc R . . H14B H -0.3710 0.1923 -0.3530 0.079 Uiso 1 1 calc R . . C15 C -0.3317(15) 0.2883(14) -0.4753(12) 0.107(5) Uani 1 1 d . . . H15D H -0.3361 0.2396 -0.5337 0.160 Uiso 1 1 calc R . . H15A H -0.2721 0.3329 -0.4883 0.160 Uiso 1 1 calc R . . H15B H -0.3998 0.3243 -0.4752 0.160 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 0.0319(3) 0.0369(3) 0.0331(3) 0.0011(3) 0.0006(2) -0.0030(2) I1 0.0500(4) 0.0719(4) 0.0555(4) -0.0105(3) -0.0046(3) -0.0216(3) I2 0.0568(4) 0.0557(4) 0.0741(5) 0.0027(3) 0.0117(3) 0.0173(3) P1 0.0383(11) 0.0427(12) 0.0393(12) 0.0087(9) -0.0011(8) -0.0013(9) C1 0.045(5) 0.057(6) 0.069(7) 0.018(5) 0.005(4) 0.019(4) C2 0.033(4) 0.085(7) 0.056(6) 0.011(5) 0.006(4) -0.004(4) C3 0.023(4) 0.057(5) 0.054(6) -0.005(4) 0.003(4) -0.005(3) C4 0.030(4) 0.057(5) 0.050(5) -0.009(4) 0.009(3) -0.006(4) C5 0.048(5) 0.090(7) 0.025(4) 0.005(4) 0.007(3) -0.026(5) C6 0.061(6) 0.070(7) 0.039(5) 0.006(5) 0.003(4) -0.012(5) C7 0.044(5) 0.050(5) 0.052(6) 0.003(4) 0.015(4) -0.009(4) C8 0.057(6) 0.077(8) 0.081(8) -0.027(6) 0.028(5) -0.006(5) C9 0.066(7) 0.153(13) 0.032(6) -0.002(6) 0.005(5) -0.042(7) C10 0.071(7) 0.076(7) 0.078(8) 0.035(6) 0.011(5) 0.006(6) C11 0.076(7) 0.058(6) 0.064(6) -0.008(5) 0.002(5) -0.033(5) C12 0.053(5) 0.055(6) 0.067(6) 0.026(5) -0.001(4) -0.014(5) C13 0.060(7) 0.078(7) 0.063(7) 0.011(5) 0.013(5) -0.003(6) C14 0.074(7) 0.076(7) 0.047(6) -0.001(5) 0.004(5) -0.009(6) C15 0.116(12) 0.151(15) 0.052(8) 0.016(9) -0.017(7) -0.034(11) _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 C3 2.131(8) . ? Rh1 C7 2.161(9) . ? Rh1 C4 2.178(8) . ? Rh1 C5 2.260(9) . ? Rh1 C6 2.261(10) . ? Rh1 P1 2.272(2) . ? Rh1 I1 2.6881(8) . ? Rh1 I2 2.6964(8) . ? P1 C12 1.791(9) . ? P1 C14 1.808(11) . ? P1 C1 1.835(9) . ? C1 C2 1.517(15) . ? C2 C3 1.494(14) . ? C3 C7 1.435(14) . ? C3 C4 1.442(13) . ? C4 C5 1.436(15) . ? C4 C8 1.491(15) . ? C5 C6 1.404(16) . ? C5 C9 1.520(13) . ? C6 C7 1.453(14) . ? C6 C10 1.465(16) . ? C7 C11 1.494(15) . ? C12 C13 1.553(16) . ? C14 C15 1.507(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 C3 Rh1 C7 39.1(4) . . ? C3 Rh1 C4 39.1(3) . . ? C7 Rh1 C4 64.7(4) . . ? C3 Rh1 C5 63.7(4) . . ? C7 Rh1 C5 62.8(4) . . ? C4 Rh1 C5 37.7(4) . . ? C3 Rh1 C6 64.1(4) . . ? C7 Rh1 C6 38.3(4) . . ? C4 Rh1 C6 63.0(4) . . ? C5 Rh1 C6 36.2(4) . . ? C3 Rh1 P1 83.0(3) . . ? C7 Rh1 P1 101.5(3) . . ? C4 Rh1 P1 105.8(3) . . ? C5 Rh1 P1 143.0(3) . . ? C6 Rh1 P1 139.8(3) . . ? C3 Rh1 I1 130.5(2) . . ? C7 Rh1 I1 156.2(3) . . ? C4 Rh1 I1 95.8(2) . . ? C5 Rh1 I1 93.5(2) . . ? C6 Rh1 I1 121.9(2) . . ? P1 Rh1 I1 96.79(6) . . ? C3 Rh1 I2 136.0(2) . . ? C7 Rh1 I2 100.0(3) . . ? C4 Rh1 I2 156.5(3) . . ? C5 Rh1 I2 120.3(3) . . ? C6 Rh1 I2 93.9(3) . . ? P1 Rh1 I2 94.44(6) . . ? I1 Rh1 I2 93.56(3) . . ? C12 P1 C14 105.2(6) . . ? C12 P1 C1 104.6(5) . . ? C14 P1 C1 105.2(6) . . ? C12 P1 Rh1 122.7(4) . . ? C14 P1 Rh1 115.7(4) . . ? C1 P1 Rh1 101.5(4) . . ? C2 C1 P1 109.3(7) . . ? C3 C2 C1 112.8(8) . . ? C7 C3 C4 107.7(8) . . ? C7 C3 C2 126.2(9) . . ? C4 C3 C2 126.0(9) . . ? C7 C3 Rh1 71.6(5) . . ? C4 C3 Rh1 72.2(5) . . ? C2 C3 Rh1 118.6(6) . . ? C3 C4 C5 107.3(8) . . ? C3 C4 C8 125.3(9) . . ? C5 C4 C8 126.8(10) . . ? C3 C4 Rh1 68.7(5) . . ? C5 C4 Rh1 74.2(5) . . ? C8 C4 Rh1 129.1(7) . . ? C6 C5 C4 109.5(8) . . ? C6 C5 C9 125.7(11) . . ? C4 C5 C9 124.6(11) . . ? C6 C5 Rh1 72.0(5) . . ? C4 C5 Rh1 68.1(5) . . ? C9 C5 Rh1 130.6(7) . . ? C5 C6 C7 107.6(9) . . ? C5 C6 C10 128.5(10) . . ? C7 C6 C10 123.8(10) . . ? C5 C6 Rh1 71.9(5) . . ? C7 C6 Rh1 67.1(5) . . ? C10 C6 Rh1 129.0(8) . . ? C3 C7 C6 107.9(9) . . ? C3 C7 C11 127.7(10) . . ? C6 C7 C11 124.0(10) . . ? C3 C7 Rh1 69.3(5) . . ? C6 C7 Rh1 74.6(6) . . ? C11 C7 Rh1 127.8(7) . . ? C13 C12 P1 111.4(8) . . ? C15 C14 P1 117.0(11) . . ? 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 C3 Rh1 P1 C12 137.4(5) . . . . ? C7 Rh1 P1 C12 172.0(5) . . . . ? C4 Rh1 P1 C12 105.3(5) . . . . ? C5 Rh1 P1 C12 112.4(6) . . . . ? C6 Rh1 P1 C12 171.8(6) . . . . ? I1 Rh1 P1 C12 7.3(5) . . . . ? I2 Rh1 P1 C12 -86.8(5) . . . . ? C3 Rh1 P1 C14 -91.6(5) . . . . ? C7 Rh1 P1 C14 -57.0(5) . . . . ? C4 Rh1 P1 C14 -123.7(5) . . . . ? C5 Rh1 P1 C14 -116.7(6) . . . . ? C6 Rh1 P1 C14 -57.2(7) . . . . ? I1 Rh1 P1 C14 138.3(5) . . . . ? I2 Rh1 P1 C14 44.2(5) . . . . ? C3 Rh1 P1 C1 21.6(5) . . . . ? C7 Rh1 P1 C1 56.2(5) . . . . ? C4 Rh1 P1 C1 -10.5(5) . . . . ? C5 Rh1 P1 C1 -3.5(6) . . . . ? C6 Rh1 P1 C1 56.0(6) . . . . ? I1 Rh1 P1 C1 -108.5(4) . . . . ? I2 Rh1 P1 C1 157.4(4) . . . . ? C12 P1 C1 C2 -167.4(8) . . . . ? C14 P1 C1 C2 82.0(9) . . . . ? Rh1 P1 C1 C2 -38.9(8) . . . . ? P1 C1 C2 C3 39.7(12) . . . . ? C1 C2 C3 C7 -108.2(11) . . . . ? C1 C2 C3 C4 67.2(12) . . . . ? C1 C2 C3 Rh1 -20.9(12) . . . . ? C4 Rh1 C3 C7 -116.3(8) . . . . ? C5 Rh1 C3 C7 -78.5(6) . . . . ? C6 Rh1 C3 C7 -38.1(6) . . . . ? P1 Rh1 C3 C7 118.0(5) . . . . ? I1 Rh1 C3 C7 -149.0(5) . . . . ? I2 Rh1 C3 C7 28.8(7) . . . . ? C7 Rh1 C3 C4 116.3(8) . . . . ? C5 Rh1 C3 C4 37.7(6) . . . . ? C6 Rh1 C3 C4 78.2(6) . . . . ? P1 Rh1 C3 C4 -125.8(5) . . . . ? I1 Rh1 C3 C4 -32.8(7) . . . . ? I2 Rh1 C3 C4 145.1(5) . . . . ? C7 Rh1 C3 C2 -121.8(10) . . . . ? C4 Rh1 C3 C2 121.9(10) . . . . ? C5 Rh1 C3 C2 159.7(9) . . . . ? C6 Rh1 C3 C2 -159.9(9) . . . . ? P1 Rh1 C3 C2 -3.8(7) . . . . ? I1 Rh1 C3 C2 89.2(8) . . . . ? I2 Rh1 C3 C2 -93.0(8) . . . . ? C7 C3 C4 C5 -1.4(9) . . . . ? C2 C3 C4 C5 -177.6(8) . . . . ? Rh1 C3 C4 C5 -64.7(6) . . . . ? C7 C3 C4 C8 -173.1(9) . . . . ? C2 C3 C4 C8 10.7(13) . . . . ? Rh1 C3 C4 C8 123.6(9) . . . . ? C7 C3 C4 Rh1 63.3(6) . . . . ? C2 C3 C4 Rh1 -112.9(8) . . . . ? C7 Rh1 C4 C3 -38.7(6) . . . . ? C5 Rh1 C4 C3 -116.2(8) . . . . ? C6 Rh1 C4 C3 -81.5(6) . . . . ? P1 Rh1 C4 C3 56.8(6) . . . . ? I1 Rh1 C4 C3 155.5(5) . . . . ? I2 Rh1 C4 C3 -91.6(7) . . . . ? C3 Rh1 C4 C5 116.2(8) . . . . ? C7 Rh1 C4 C5 77.6(6) . . . . ? C6 Rh1 C4 C5 34.8(5) . . . . ? P1 Rh1 C4 C5 173.0(5) . . . . ? I1 Rh1 C4 C5 -88.2(5) . . . . ? I2 Rh1 C4 C5 24.7(9) . . . . ? C3 Rh1 C4 C8 -118.8(12) . . . . ? C7 Rh1 C4 C8 -157.5(11) . . . . ? C5 Rh1 C4 C8 124.9(12) . . . . ? C6 Rh1 C4 C8 159.7(11) . . . . ? P1 Rh1 C4 C8 -62.0(10) . . . . ? I1 Rh1 C4 C8 36.7(10) . . . . ? I2 Rh1 C4 C8 149.6(8) . . . . ? C3 C4 C5 C6 0.9(10) . . . . ? C8 C4 C5 C6 172.4(8) . . . . ? Rh1 C4 C5 C6 -60.2(7) . . . . ? C3 C4 C5 C9 -173.9(8) . . . . ? C8 C4 C5 C9 -2.4(15) . . . . ? Rh1 C4 C5 C9 125.0(9) . . . . ? C3 C4 C5 Rh1 61.1(6) . . . . ? C8 C4 C5 Rh1 -127.4(9) . . . . ? C3 Rh1 C5 C6 81.5(6) . . . . ? C7 Rh1 C5 C6 37.6(6) . . . . ? C4 Rh1 C5 C6 120.6(8) . . . . ? P1 Rh1 C5 C6 109.5(7) . . . . ? I1 Rh1 C5 C6 -144.4(6) . . . . ? I2 Rh1 C5 C6 -48.3(6) . . . . ? C3 Rh1 C5 C4 -39.1(5) . . . . ? C7 Rh1 C5 C4 -83.1(6) . . . . ? C6 Rh1 C5 C4 -120.6(8) . . . . ? P1 Rh1 C5 C4 -11.2(8) . . . . ? I1 Rh1 C5 C4 94.9(5) . . . . ? I2 Rh1 C5 C4 -168.9(4) . . . . ? C3 Rh1 C5 C9 -156.6(14) . . . . ? C7 Rh1 C5 C9 159.5(14) . . . . ? C4 Rh1 C5 C9 -117.4(15) . . . . ? C6 Rh1 C5 C9 121.9(15) . . . . ? P1 Rh1 C5 C9 -128.6(11) . . . . ? I1 Rh1 C5 C9 -22.5(13) . . . . ? I2 Rh1 C5 C9 73.7(13) . . . . ? C4 C5 C6 C7 0.1(10) . . . . ? C9 C5 C6 C7 174.8(9) . . . . ? Rh1 C5 C6 C7 -57.8(6) . . . . ? C4 C5 C6 C10 -176.3(10) . . . . ? C9 C5 C6 C10 -1.6(16) . . . . ? Rh1 C5 C6 C10 125.9(11) . . . . ? C4 C5 C6 Rh1 57.9(6) . . . . ? C9 C5 C6 Rh1 -127.4(9) . . . . ? C3 Rh1 C6 C5 -80.1(6) . . . . ? C7 Rh1 C6 C5 -118.9(9) . . . . ? C4 Rh1 C6 C5 -36.2(6) . . . . ? P1 Rh1 C6 C5 -118.7(5) . . . . ? I1 Rh1 C6 C5 43.1(7) . . . . ? I2 Rh1 C6 C5 139.8(6) . . . . ? C3 Rh1 C6 C7 38.8(6) . . . . ? C4 Rh1 C6 C7 82.7(6) . . . . ? C5 Rh1 C6 C7 118.9(9) . . . . ? P1 Rh1 C6 C7 0.2(8) . . . . ? I1 Rh1 C6 C7 162.1(5) . . . . ? I2 Rh1 C6 C7 -101.3(5) . . . . ? C3 Rh1 C6 C10 154.6(11) . . . . ? C7 Rh1 C6 C10 115.8(12) . . . . ? C4 Rh1 C6 C10 -161.5(11) . . . . ? C5 Rh1 C6 C10 -125.3(13) . . . . ? P1 Rh1 C6 C10 116.0(10) . . . . ? I1 Rh1 C6 C10 -82.2(10) . . . . ? I2 Rh1 C6 C10 14.4(10) . . . . ? C4 C3 C7 C6 1.5(9) . . . . ? C2 C3 C7 C6 177.6(8) . . . . ? Rh1 C3 C7 C6 65.2(6) . . . . ? C4 C3 C7 C11 173.9(9) . . . . ? C2 C3 C7 C11 -10.0(15) . . . . ? Rh1 C3 C7 C11 -122.5(10) . . . . ? C4 C3 C7 Rh1 -63.7(6) . . . . ? C2 C3 C7 Rh1 112.5(8) . . . . ? C5 C6 C7 C3 -1.0(10) . . . . ? C10 C6 C7 C3 175.6(9) . . . . ? Rh1 C6 C7 C3 -61.7(6) . . . . ? C5 C6 C7 C11 -173.7(9) . . . . ? C10 C6 C7 C11 2.9(15) . . . . ? Rh1 C6 C7 C11 125.6(9) . . . . ? C5 C6 C7 Rh1 60.8(6) . . . . ? C10 C6 C7 Rh1 -122.7(10) . . . . ? C4 Rh1 C7 C3 38.7(6) . . . . ? C5 Rh1 C7 C3 80.9(6) . . . . ? C6 Rh1 C7 C3 116.4(8) . . . . ? P1 Rh1 C7 C3 -63.5(5) . . . . ? I1 Rh1 C7 C3 76.0(9) . . . . ? I2 Rh1 C7 C3 -160.1(5) . . . . ? C3 Rh1 C7 C6 -116.4(8) . . . . ? C4 Rh1 C7 C6 -77.7(6) . . . . ? C5 Rh1 C7 C6 -35.5(6) . . . . ? P1 Rh1 C7 C6 -179.8(5) . . . . ? I1 Rh1 C7 C6 -40.4(10) . . . . ? I2 Rh1 C7 C6 83.5(6) . . . . ? C3 Rh1 C7 C11 122.3(12) . . . . ? C4 Rh1 C7 C11 161.0(11) . . . . ? C5 Rh1 C7 C11 -156.9(11) . . . . ? C6 Rh1 C7 C11 -121.4(12) . . . . ? P1 Rh1 C7 C11 58.8(10) . . . . ? I1 Rh1 C7 C11 -161.8(7) . . . . ? I2 Rh1 C7 C11 -37.9(10) . . . . ? C14 P1 C12 C13 -60.1(9) . . . . ? C1 P1 C12 C13 -170.6(8) . . . . ? Rh1 P1 C12 C13 75.1(9) . . . . ? C12 P1 C14 C15 -44.4(13) . . . . ? C1 P1 C14 C15 65.7(12) . . . . ? Rh1 P1 C14 C15 176.7(10) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.704 _refine_diff_density_min -0.836 _refine_diff_density_rms 0.113 data_2 _database_code_CSD 197742 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H26 O P Rh' _chemical_formula_sum 'C24 H26 O P Rh' _chemical_formula_weight 464.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 8.8431(9) _cell_length_b 24.718(3) _cell_length_c 9.8846(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.548(2) _cell_angle_gamma 90.00 _cell_volume 2116.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 93 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max .1 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 0.893 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.906288 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10327 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 23.27 _reflns_number_total 2989 _reflns_number_gt 2406 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0323P)^2^+2.2787P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00050(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2989 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0689 _refine_ls_wR_factor_gt 0.0632 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.969 _refine_ls_shift/su_max 0.007 _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 0.23481(3) 0.092556(11) 0.81757(3) 0.03296(12) Uani 1 1 d . . . P1 P 0.31565(11) 0.17049(4) 0.74300(10) 0.0323(2) Uani 1 1 d . . . C1 C 0.2747(5) 0.16101(15) 0.5531(4) 0.0432(10) Uani 1 1 d . . . H1A H 0.1674 0.1693 0.5155 0.052 Uiso 1 1 calc R . . H1B H 0.3385 0.1853 0.5115 0.052 Uiso 1 1 calc R . . C2 C 0.3091(5) 0.10218(16) 0.5199(4) 0.0481(11) Uani 1 1 d . . . H2A H 0.2654 0.0948 0.4236 0.058 Uiso 1 1 calc R . . H2B H 0.4199 0.0971 0.5339 0.058 Uiso 1 1 calc R . . C3 C 0.2427(4) 0.06267(15) 0.6103(4) 0.0382(9) Uani 1 1 d . . . C4 C 0.0830(4) 0.05788(16) 0.6217(4) 0.0418(10) Uani 1 1 d . . . C5 C 0.0777(5) 0.02164(16) 0.7302(4) 0.0447(10) Uani 1 1 d . . . C6 C 0.2304(5) 0.00096(15) 0.7816(4) 0.0446(10) Uani 1 1 d . . . C7 C 0.3313(5) 0.02408(16) 0.7022(4) 0.0409(10) Uani 1 1 d . . . C8 C -0.0538(5) 0.08375(18) 0.5308(5) 0.0624(13) Uani 1 1 d . . . H8A H -0.0948 0.0598 0.4560 0.094 Uiso 1 1 calc R . . H8B H -0.0227 0.1170 0.4943 0.094 Uiso 1 1 calc R . . H8C H -0.1315 0.0910 0.5836 0.094 Uiso 1 1 calc R . . C9 C -0.0666(5) 0.0021(2) 0.7740(6) 0.0722(15) Uani 1 1 d . . . H9A H -0.1079 -0.0283 0.7184 0.108 Uiso 1 1 calc R . . H9B H -0.1416 0.0307 0.7623 0.108 Uiso 1 1 calc R . . H9C H -0.0422 -0.0085 0.8694 0.108 Uiso 1 1 calc R . . C10 C 0.2700(6) -0.04280(18) 0.8877(5) 0.0656(14) Uani 1 1 d . . . H10A H 0.2579 -0.0775 0.8430 0.098 Uiso 1 1 calc R . . H10B H 0.2025 -0.0405 0.9524 0.098 Uiso 1 1 calc R . . H10C H 0.3750 -0.0385 0.9356 0.098 Uiso 1 1 calc R . . C11 C 0.4964(5) 0.00808(19) 0.7084(5) 0.0580(12) Uani 1 1 d . . . H11A H 0.5000 -0.0223 0.6485 0.087 Uiso 1 1 calc R . . H11B H 0.5431 -0.0017 0.8014 0.087 Uiso 1 1 calc R . . H11C H 0.5515 0.0379 0.6792 0.087 Uiso 1 1 calc R . . C12 C 0.2264(6) 0.11276(18) 0.9935(5) 0.0555(12) Uani 1 1 d . . . O12 O 0.2180(6) 0.12717(16) 1.1031(4) 0.0994(15) Uani 1 1 d . . . C13 C 0.2324(4) 0.23637(14) 0.7696(4) 0.0331(9) Uani 1 1 d . . . C14 C 0.2443(5) 0.25550(16) 0.9034(4) 0.0426(10) Uani 1 1 d . . . H14A H 0.2945 0.2346 0.9771 0.051 Uiso 1 1 calc R . . C15 C 0.1831(5) 0.30472(17) 0.9289(4) 0.0477(10) Uani 1 1 d . . . H15A H 0.1928 0.3172 1.0190 0.057 Uiso 1 1 calc R . . C16 C 0.1068(5) 0.33563(17) 0.8193(5) 0.0517(11) Uani 1 1 d . . . H16A H 0.0650 0.3689 0.8360 0.062 Uiso 1 1 calc R . . C17 C 0.0928(5) 0.31760(17) 0.6872(4) 0.0488(11) Uani 1 1 d . . . H17A H 0.0412 0.3386 0.6144 0.059 Uiso 1 1 calc R . . C18 C 0.1549(5) 0.26805(16) 0.6602(4) 0.0443(10) Uani 1 1 d . . . H18A H 0.1449 0.2560 0.5698 0.053 Uiso 1 1 calc R . . C19 C 0.5226(4) 0.18595(14) 0.7808(4) 0.0341(9) Uani 1 1 d . . . C20 C 0.6258(4) 0.14649(17) 0.8381(4) 0.0453(10) Uani 1 1 d . . . H20A H 0.5892 0.1132 0.8616 0.054 Uiso 1 1 calc R . . C21 C 0.7838(5) 0.15574(19) 0.8611(5) 0.0583(12) Uani 1 1 d . . . H21A H 0.8530 0.1288 0.8985 0.070 Uiso 1 1 calc R . . C22 C 0.8365(5) 0.2055(2) 0.8275(5) 0.0593(13) Uani 1 1 d . . . H22A H 0.9421 0.2121 0.8418 0.071 Uiso 1 1 calc R . . C23 C 0.7347(5) 0.24547(19) 0.7732(4) 0.0529(12) Uani 1 1 d . . . H23A H 0.7713 0.2791 0.7525 0.063 Uiso 1 1 calc R . . C24 C 0.5790(5) 0.23592(16) 0.7494(4) 0.0436(10) Uani 1 1 d . . . H24A H 0.5105 0.2631 0.7120 0.052 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 0.03458(17) 0.02856(17) 0.03605(18) -0.00307(15) 0.00778(12) -0.00414(14) P1 0.0357(5) 0.0298(5) 0.0312(5) -0.0009(4) 0.0063(4) -0.0031(4) C1 0.060(3) 0.035(2) 0.034(2) -0.0007(18) 0.0084(19) -0.0024(19) C2 0.063(3) 0.047(3) 0.036(2) -0.006(2) 0.015(2) -0.005(2) C3 0.047(2) 0.033(2) 0.035(2) -0.0087(18) 0.0074(18) -0.0055(18) C4 0.037(2) 0.041(2) 0.044(2) -0.016(2) -0.0012(19) -0.0016(18) C5 0.044(2) 0.037(2) 0.055(3) -0.015(2) 0.016(2) -0.0124(19) C6 0.059(3) 0.027(2) 0.048(3) -0.0047(18) 0.014(2) -0.0036(19) C7 0.045(2) 0.035(2) 0.043(2) -0.0100(19) 0.0106(19) 0.0024(18) C8 0.055(3) 0.059(3) 0.066(3) -0.021(3) -0.008(2) 0.010(2) C9 0.062(3) 0.067(3) 0.094(4) -0.027(3) 0.031(3) -0.026(3) C10 0.094(4) 0.038(3) 0.070(3) 0.006(2) 0.029(3) 0.007(2) C11 0.050(3) 0.059(3) 0.064(3) -0.007(2) 0.009(2) 0.015(2) C12 0.071(3) 0.048(3) 0.051(3) -0.007(2) 0.020(2) -0.023(2) O12 0.159(4) 0.093(3) 0.058(2) -0.031(2) 0.051(3) -0.054(3) C13 0.034(2) 0.030(2) 0.035(2) -0.0006(17) 0.0067(17) -0.0045(16) C14 0.050(2) 0.037(2) 0.039(2) -0.0010(19) 0.0039(19) -0.0005(19) C15 0.057(3) 0.043(2) 0.045(2) -0.007(2) 0.015(2) -0.008(2) C16 0.060(3) 0.035(2) 0.065(3) -0.002(2) 0.025(2) 0.001(2) C17 0.054(3) 0.043(3) 0.050(3) 0.010(2) 0.012(2) 0.011(2) C18 0.050(2) 0.043(2) 0.040(2) 0.003(2) 0.010(2) 0.002(2) C19 0.035(2) 0.034(2) 0.034(2) -0.0029(17) 0.0093(16) -0.0046(17) C20 0.039(2) 0.044(2) 0.052(3) 0.001(2) 0.0063(19) -0.0015(19) C21 0.037(2) 0.061(3) 0.076(3) -0.004(3) 0.009(2) 0.004(2) C22 0.036(2) 0.085(4) 0.060(3) -0.015(3) 0.017(2) -0.022(3) C23 0.060(3) 0.056(3) 0.046(3) -0.008(2) 0.018(2) -0.022(2) C24 0.050(3) 0.042(2) 0.040(2) -0.0046(19) 0.0130(19) -0.0055(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 C12 1.825(5) . ? Rh1 C3 2.192(4) . ? Rh1 P1 2.2306(10) . ? Rh1 C4 2.290(4) . ? Rh1 C6 2.291(4) . ? Rh1 C5 2.295(4) . ? Rh1 C7 2.298(4) . ? P1 C13 1.828(4) . ? P1 C19 1.833(4) . ? P1 C1 1.854(4) . ? C1 C2 1.534(5) . ? C2 C3 1.519(6) . ? C3 C7 1.437(6) . ? C3 C4 1.444(5) . ? C4 C5 1.406(6) . ? C4 C8 1.498(6) . ? C5 C6 1.438(6) . ? C5 C9 1.506(6) . ? C6 C7 1.421(6) . ? C6 C10 1.498(6) . ? C7 C11 1.502(6) . ? C12 O12 1.157(5) . ? C13 C14 1.389(5) . ? C13 C18 1.398(5) . ? C14 C15 1.375(6) . ? C15 C16 1.386(6) . ? C16 C17 1.361(6) . ? C17 C18 1.390(6) . ? C19 C20 1.378(5) . ? C19 C24 1.390(5) . ? C20 C21 1.389(6) . ? C21 C22 1.380(6) . ? C22 C23 1.371(6) . ? C23 C24 1.370(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 Rh1 C3 176.16(17) . . ? C12 Rh1 P1 98.94(14) . . ? C3 Rh1 P1 84.83(10) . . ? C12 Rh1 C4 141.18(18) . . ? C3 Rh1 C4 37.50(14) . . ? P1 Rh1 C4 102.49(11) . . ? C12 Rh1 C6 114.55(18) . . ? C3 Rh1 C6 61.63(14) . . ? P1 Rh1 C6 143.02(11) . . ? C4 Rh1 C6 60.67(14) . . ? C12 Rh1 C5 115.48(17) . . ? C3 Rh1 C5 61.40(14) . . ? P1 Rh1 C5 138.17(11) . . ? C4 Rh1 C5 35.71(15) . . ? C6 Rh1 C5 36.56(15) . . ? C12 Rh1 C7 139.84(18) . . ? C3 Rh1 C7 37.23(14) . . ? P1 Rh1 C7 107.26(11) . . ? C4 Rh1 C7 61.19(14) . . ? C6 Rh1 C7 36.08(14) . . ? C5 Rh1 C7 60.53(14) . . ? C13 P1 C19 101.50(16) . . ? C13 P1 C1 104.80(17) . . ? C19 P1 C1 102.54(18) . . ? C13 P1 Rh1 123.85(12) . . ? C19 P1 Rh1 119.06(12) . . ? C1 P1 Rh1 102.41(13) . . ? C2 C1 P1 109.2(3) . . ? C3 C2 C1 111.5(3) . . ? C7 C3 C4 108.3(3) . . ? C7 C3 C2 124.9(4) . . ? C4 C3 C2 126.7(4) . . ? C7 C3 Rh1 75.4(2) . . ? C4 C3 Rh1 74.9(2) . . ? C2 C3 Rh1 114.9(2) . . ? C5 C4 C3 107.1(3) . . ? C5 C4 C8 125.7(4) . . ? C3 C4 C8 127.1(4) . . ? C5 C4 Rh1 72.4(2) . . ? C3 C4 Rh1 67.6(2) . . ? C8 C4 Rh1 127.9(3) . . ? C4 C5 C6 108.9(4) . . ? C4 C5 C9 125.7(4) . . ? C6 C5 C9 125.0(4) . . ? C4 C5 Rh1 71.9(2) . . ? C6 C5 Rh1 71.5(2) . . ? C9 C5 Rh1 128.4(3) . . ? C7 C6 C5 108.1(4) . . ? C7 C6 C10 126.3(4) . . ? C5 C6 C10 125.1(4) . . ? C7 C6 Rh1 72.2(2) . . ? C5 C6 Rh1 71.9(2) . . ? C10 C6 Rh1 127.6(3) . . ? C6 C7 C3 107.0(3) . . ? C6 C7 C11 125.8(4) . . ? C3 C7 C11 127.1(4) . . ? C6 C7 Rh1 71.7(2) . . ? C3 C7 Rh1 67.4(2) . . ? C11 C7 Rh1 128.9(3) . . ? O12 C12 Rh1 177.5(5) . . ? C14 C13 C18 118.5(4) . . ? C14 C13 P1 119.0(3) . . ? C18 C13 P1 122.5(3) . . ? C15 C14 C13 121.2(4) . . ? C14 C15 C16 119.5(4) . . ? C17 C16 C15 120.4(4) . . ? C16 C17 C18 120.6(4) . . ? C17 C18 C13 119.8(4) . . ? C20 C19 C24 118.9(4) . . ? C20 C19 P1 119.2(3) . . ? C24 C19 P1 121.9(3) . . ? C19 C20 C21 120.8(4) . . ? C22 C21 C20 119.0(4) . . ? C23 C22 C21 120.6(4) . . ? C22 C23 C24 120.1(4) . . ? C23 C24 C19 120.5(4) . . ? 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 C12 Rh1 P1 C13 -46.8(2) . . . . ? C3 Rh1 P1 C13 133.92(17) . . . . ? C4 Rh1 P1 C13 100.64(17) . . . . ? C6 Rh1 P1 C13 158.0(2) . . . . ? C5 Rh1 P1 C13 99.2(2) . . . . ? C7 Rh1 P1 C13 164.02(17) . . . . ? C12 Rh1 P1 C19 83.5(2) . . . . ? C3 Rh1 P1 C19 -95.74(17) . . . . ? C4 Rh1 P1 C19 -129.03(17) . . . . ? C6 Rh1 P1 C19 -71.7(2) . . . . ? C5 Rh1 P1 C19 -130.5(2) . . . . ? C7 Rh1 P1 C19 -65.65(17) . . . . ? C12 Rh1 P1 C1 -164.3(2) . . . . ? C3 Rh1 P1 C1 16.37(17) . . . . ? C4 Rh1 P1 C1 -16.91(18) . . . . ? C6 Rh1 P1 C1 40.4(2) . . . . ? C5 Rh1 P1 C1 -18.4(2) . . . . ? C7 Rh1 P1 C1 46.47(18) . . . . ? C13 P1 C1 C2 -168.3(3) . . . . ? C19 P1 C1 C2 86.1(3) . . . . ? Rh1 P1 C1 C2 -37.9(3) . . . . ? P1 C1 C2 C3 45.6(4) . . . . ? C1 C2 C3 C7 -120.8(4) . . . . ? C1 C2 C3 C4 57.8(5) . . . . ? C1 C2 C3 Rh1 -31.6(4) . . . . ? C12 Rh1 C3 C7 -42(3) . . . . ? P1 Rh1 C3 C7 127.7(2) . . . . ? C4 Rh1 C3 C7 -114.0(3) . . . . ? C6 Rh1 C3 C7 -36.1(2) . . . . ? C5 Rh1 C3 C7 -78.0(2) . . . . ? C12 Rh1 C3 C4 72(3) . . . . ? P1 Rh1 C3 C4 -118.3(2) . . . . ? C6 Rh1 C3 C4 77.8(2) . . . . ? C5 Rh1 C3 C4 36.0(2) . . . . ? C7 Rh1 C3 C4 114.0(3) . . . . ? C12 Rh1 C3 C2 -164(3) . . . . ? P1 Rh1 C3 C2 5.6(3) . . . . ? C4 Rh1 C3 C2 123.9(4) . . . . ? C6 Rh1 C3 C2 -158.2(3) . . . . ? C5 Rh1 C3 C2 159.9(3) . . . . ? C7 Rh1 C3 C2 -122.1(4) . . . . ? C7 C3 C4 C5 6.7(4) . . . . ? C2 C3 C4 C5 -172.0(4) . . . . ? Rh1 C3 C4 C5 -61.9(3) . . . . ? C7 C3 C4 C8 -170.0(4) . . . . ? C2 C3 C4 C8 11.2(6) . . . . ? Rh1 C3 C4 C8 121.3(4) . . . . ? C7 C3 C4 Rh1 68.6(3) . . . . ? C2 C3 C4 Rh1 -110.1(4) . . . . ? C12 Rh1 C4 C5 -56.4(4) . . . . ? C3 Rh1 C4 C5 117.8(3) . . . . ? P1 Rh1 C4 C5 -178.3(2) . . . . ? C6 Rh1 C4 C5 37.2(2) . . . . ? C7 Rh1 C4 C5 78.7(3) . . . . ? C12 Rh1 C4 C3 -174.2(3) . . . . ? P1 Rh1 C4 C3 63.9(2) . . . . ? C6 Rh1 C4 C3 -80.6(2) . . . . ? C5 Rh1 C4 C3 -117.8(3) . . . . ? C7 Rh1 C4 C3 -39.1(2) . . . . ? C12 Rh1 C4 C8 65.5(5) . . . . ? C3 Rh1 C4 C8 -120.3(5) . . . . ? P1 Rh1 C4 C8 -56.5(4) . . . . ? C6 Rh1 C4 C8 159.0(5) . . . . ? C5 Rh1 C4 C8 121.9(5) . . . . ? C7 Rh1 C4 C8 -159.5(5) . . . . ? C3 C4 C5 C6 -3.6(4) . . . . ? C8 C4 C5 C6 173.2(4) . . . . ? Rh1 C4 C5 C6 -62.4(3) . . . . ? C3 C4 C5 C9 -176.4(4) . . . . ? C8 C4 C5 C9 0.4(6) . . . . ? Rh1 C4 C5 C9 124.7(4) . . . . ? C3 C4 C5 Rh1 58.9(2) . . . . ? C8 C4 C5 Rh1 -124.4(4) . . . . ? C12 Rh1 C5 C4 144.7(3) . . . . ? C3 Rh1 C5 C4 -37.8(2) . . . . ? P1 Rh1 C5 C4 2.4(3) . . . . ? C6 Rh1 C5 C4 -117.8(3) . . . . ? C7 Rh1 C5 C4 -80.7(3) . . . . ? C12 Rh1 C5 C6 -97.5(3) . . . . ? C3 Rh1 C5 C6 80.0(3) . . . . ? P1 Rh1 C5 C6 120.3(2) . . . . ? C4 Rh1 C5 C6 117.8(3) . . . . ? C7 Rh1 C5 C6 37.2(2) . . . . ? C12 Rh1 C5 C9 23.0(5) . . . . ? C3 Rh1 C5 C9 -159.5(5) . . . . ? P1 Rh1 C5 C9 -119.2(4) . . . . ? C4 Rh1 C5 C9 -121.7(5) . . . . ? C6 Rh1 C5 C9 120.5(5) . . . . ? C7 Rh1 C5 C9 157.7(5) . . . . ? C4 C5 C6 C7 -0.9(4) . . . . ? C9 C5 C6 C7 172.0(4) . . . . ? Rh1 C5 C6 C7 -63.6(3) . . . . ? C4 C5 C6 C10 -173.6(4) . . . . ? C9 C5 C6 C10 -0.7(7) . . . . ? Rh1 C5 C6 C10 123.7(4) . . . . ? C4 C5 C6 Rh1 62.7(3) . . . . ? C9 C5 C6 Rh1 -124.4(4) . . . . ? C12 Rh1 C6 C7 -143.1(3) . . . . ? C3 Rh1 C6 C7 37.3(2) . . . . ? P1 Rh1 C6 C7 9.9(3) . . . . ? C4 Rh1 C6 C7 80.4(2) . . . . ? C5 Rh1 C6 C7 116.6(3) . . . . ? C12 Rh1 C6 C5 100.2(3) . . . . ? C3 Rh1 C6 C5 -79.3(3) . . . . ? P1 Rh1 C6 C5 -106.8(3) . . . . ? C4 Rh1 C6 C5 -36.3(2) . . . . ? C7 Rh1 C6 C5 -116.6(3) . . . . ? C12 Rh1 C6 C10 -20.6(5) . . . . ? C3 Rh1 C6 C10 159.9(4) . . . . ? P1 Rh1 C6 C10 132.4(3) . . . . ? C4 Rh1 C6 C10 -157.1(4) . . . . ? C5 Rh1 C6 C10 -120.8(5) . . . . ? C7 Rh1 C6 C10 122.6(5) . . . . ? C5 C6 C7 C3 5.1(4) . . . . ? C10 C6 C7 C3 177.6(4) . . . . ? Rh1 C6 C7 C3 -58.3(3) . . . . ? C5 C6 C7 C11 -171.4(4) . . . . ? C10 C6 C7 C11 1.2(7) . . . . ? Rh1 C6 C7 C11 125.3(4) . . . . ? C5 C6 C7 Rh1 63.4(3) . . . . ? C10 C6 C7 Rh1 -124.1(4) . . . . ? C4 C3 C7 C6 -7.3(4) . . . . ? C2 C3 C7 C6 171.5(3) . . . . ? Rh1 C3 C7 C6 61.1(3) . . . . ? C4 C3 C7 C11 169.1(4) . . . . ? C2 C3 C7 C11 -12.1(6) . . . . ? Rh1 C3 C7 C11 -122.6(4) . . . . ? C4 C3 C7 Rh1 -68.3(3) . . . . ? C2 C3 C7 Rh1 110.4(4) . . . . ? C12 Rh1 C7 C6 57.8(4) . . . . ? C3 Rh1 C7 C6 -118.2(3) . . . . ? P1 Rh1 C7 C6 -173.8(2) . . . . ? C4 Rh1 C7 C6 -78.8(3) . . . . ? C5 Rh1 C7 C6 -37.7(2) . . . . ? C12 Rh1 C7 C3 176.0(3) . . . . ? P1 Rh1 C7 C3 -55.6(2) . . . . ? C4 Rh1 C7 C3 39.4(2) . . . . ? C6 Rh1 C7 C3 118.2(3) . . . . ? C5 Rh1 C7 C3 80.5(2) . . . . ? C12 Rh1 C7 C11 -63.8(5) . . . . ? C3 Rh1 C7 C11 120.2(5) . . . . ? P1 Rh1 C7 C11 64.6(4) . . . . ? C4 Rh1 C7 C11 159.6(4) . . . . ? C6 Rh1 C7 C11 -121.6(5) . . . . ? C5 Rh1 C7 C11 -159.3(4) . . . . ? C3 Rh1 C12 O12 -140(9) . . . . ? P1 Rh1 C12 O12 51(10) . . . . ? C4 Rh1 C12 O12 -72(10) . . . . ? C6 Rh1 C12 O12 -145(10) . . . . ? C5 Rh1 C12 O12 -105(10) . . . . ? C7 Rh1 C12 O12 -179(100) . . . . ? C19 P1 C13 C14 -73.5(3) . . . . ? C1 P1 C13 C14 -179.9(3) . . . . ? Rh1 P1 C13 C14 63.7(3) . . . . ? C19 P1 C13 C18 107.5(3) . . . . ? C1 P1 C13 C18 1.1(4) . . . . ? Rh1 P1 C13 C18 -115.3(3) . . . . ? C18 C13 C14 C15 -0.7(6) . . . . ? P1 C13 C14 C15 -179.8(3) . . . . ? C13 C14 C15 C16 0.7(6) . . . . ? C14 C15 C16 C17 -0.2(6) . . . . ? C15 C16 C17 C18 -0.1(7) . . . . ? C16 C17 C18 C13 0.0(6) . . . . ? C14 C13 C18 C17 0.4(6) . . . . ? P1 C13 C18 C17 179.4(3) . . . . ? C13 P1 C19 C20 148.2(3) . . . . ? C1 P1 C19 C20 -103.6(3) . . . . ? Rh1 P1 C19 C20 8.5(4) . . . . ? C13 P1 C19 C24 -33.7(4) . . . . ? C1 P1 C19 C24 74.5(3) . . . . ? Rh1 P1 C19 C24 -173.5(3) . . . . ? C24 C19 C20 C21 -1.7(6) . . . . ? P1 C19 C20 C21 176.4(3) . . . . ? C19 C20 C21 C22 0.9(7) . . . . ? C20 C21 C22 C23 0.5(7) . . . . ? C21 C22 C23 C24 -1.2(7) . . . . ? C22 C23 C24 C19 0.4(6) . . . . ? C20 C19 C24 C23 1.0(6) . . . . ? P1 C19 C24 C23 -177.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.292 _refine_diff_density_min -0.259 _refine_diff_density_rms 0.059 data_3 _database_code_CSD 197743 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H18 O P Rh' _chemical_formula_sum 'C12 H18 O P Rh' _chemical_formula_weight 312.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 12.3029(4) _cell_length_b 9.5500(3) _cell_length_c 11.1065(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1304.93(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 62 _cell_measurement_theta_min 12 _cell_measurement_theta_max 158 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max .08 _exptl_crystal_size_mid .08 _exptl_crystal_size_min .1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 1.404 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.897745 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5187 _diffrn_reflns_av_R_equivalents 0.0163 _diffrn_reflns_av_sigmaI/netI 0.0178 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 23.25 _reflns_number_total 1841 _reflns_number_gt 1572 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0311P)^2^+0.5219P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0052(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(7) _refine_ls_number_reflns 1841 _refine_ls_number_parameters 137 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0297 _refine_ls_R_factor_gt 0.0229 _refine_ls_wR_factor_ref 0.0596 _refine_ls_wR_factor_gt 0.0562 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.050 _refine_ls_shift/su_mean 0.009 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 0.54722(2) 0.06575(3) 0.3979(3) 0.06262(17) Uani 1 1 d . . . C1 C 0.6983(5) -0.1810(5) 0.3115(7) 0.0982(19) Uani 1 1 d . . . H1A H 0.6732 -0.1677 0.2295 0.118 Uiso 1 1 calc R . . H1B H 0.7650 -0.2349 0.3110 0.118 Uiso 1 1 calc R . . P1 P 0.71629(9) -0.00379(12) 0.3948(7) 0.1041(5) Uani 1 1 d . . . C2 C 0.6059(4) -0.2538(4) 0.3950(17) 0.1011(18) Uani 1 1 d . . . H2A H 0.5831 -0.3413 0.3586 0.121 Uiso 1 1 calc R . . H2B H 0.6360 -0.2745 0.4737 0.121 Uiso 1 1 calc R . . C3 C 0.5103(5) -0.1596(5) 0.4085(14) 0.0650(17) Uani 1 1 d . . . C4 C 0.4490(9) -0.0940(17) 0.2923(15) 0.083(4) Uani 1 1 d . . . H4A H 0.4631 -0.1183 0.2127 0.100 Uiso 1 1 calc R . . C5 C 0.3812(13) -0.0075(16) 0.3250(16) 0.105(5) Uani 1 1 d . . . H5A H 0.3401 0.0494 0.2746 0.125 Uiso 1 1 calc R . . C6 C 0.3763(10) -0.0092(14) 0.4491(16) 0.093(4) Uani 1 1 d . . . H6A H 0.3297 0.0442 0.4963 0.112 Uiso 1 1 calc R . . C7 C 0.4605(9) -0.1134(16) 0.4958(12) 0.078(4) Uani 1 1 d . . . H7A H 0.4720 -0.1375 0.5759 0.093 Uiso 1 1 calc R . . C8 C 0.8031(6) -0.0313(8) 0.5000(8) 0.110(2) Uani 1 1 d . . . H8A H 0.7755 -0.1004 0.5562 0.132 Uiso 1 1 calc R . . H8B H 0.8708 -0.0658 0.4664 0.132 Uiso 1 1 calc R . . C9 C 0.8198(13) 0.0947(14) 0.5576(15) 0.155(7) Uani 1 1 d . . . H9A H 0.8716 0.0822 0.6214 0.232 Uiso 1 1 calc R . . H9B H 0.7523 0.1276 0.5905 0.232 Uiso 1 1 calc R . . H9C H 0.8473 0.1620 0.5011 0.232 Uiso 1 1 calc R . . C10 C 0.8059(11) 0.0912(11) 0.2478(14) 0.127(5) Uani 1 1 d . . . H10A H 0.7579 0.1009 0.1790 0.152 Uiso 1 1 calc R . . H10B H 0.8286 0.1844 0.2718 0.152 Uiso 1 1 calc R . . C11 C 0.8996(7) 0.0131(11) 0.2123(9) 0.139(3) Uani 1 1 d . . . H11A H 0.9355 0.0604 0.1472 0.209 Uiso 1 1 calc R . . H11B H 0.8778 -0.0786 0.1865 0.209 Uiso 1 1 calc R . . H11C H 0.9485 0.0050 0.2793 0.209 Uiso 1 1 calc R . . C20 C 0.5849(4) 0.2479(5) 0.401(2) 0.1002(18) Uani 1 1 d . . . O20 O 0.6161(4) 0.3626(4) 0.4151(17) 0.159(4) 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 0.0558(2) 0.04135(19) 0.0907(3) -0.0033(7) 0.0008(7) -0.00097(13) C1 0.087(4) 0.048(3) 0.160(5) -0.018(3) 0.021(4) 0.007(3) P1 0.0583(6) 0.0459(6) 0.2082(16) -0.009(3) 0.011(3) 0.0031(5) C2 0.095(3) 0.0425(19) 0.166(5) 0.018(9) 0.028(11) -0.002(2) C3 0.079(2) 0.046(2) 0.070(5) 0.002(5) 0.010(6) -0.0145(18) C4 0.092(8) 0.063(6) 0.095(8) 0.017(5) -0.010(6) -0.016(5) C5 0.091(9) 0.074(7) 0.149(12) 0.030(7) -0.047(8) -0.033(6) C6 0.057(6) 0.067(6) 0.156(11) -0.008(5) 0.011(5) 0.000(5) C7 0.091(7) 0.052(5) 0.090(8) 0.012(6) 0.015(6) -0.020(5) C8 0.082(4) 0.109(5) 0.138(6) -0.001(5) -0.029(4) 0.019(4) C9 0.129(11) 0.150(11) 0.185(14) -0.064(9) 0.053(10) -0.024(9) C10 0.106(7) 0.077(6) 0.197(14) -0.048(7) -0.012(8) 0.021(6) C11 0.089(5) 0.161(8) 0.167(8) 0.019(7) 0.031(6) 0.014(6) C20 0.063(2) 0.048(2) 0.190(5) -0.029(8) 0.010(11) 0.000(2) O20 0.100(3) 0.0527(19) 0.324(12) -0.045(6) 0.029(8) -0.0120(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 C20 1.800(4) . ? Rh1 P1 2.1838(11) . ? Rh1 C3 2.203(4) . ? Rh1 C4 2.272(15) . ? Rh1 C7 2.291(12) . ? Rh1 C6 2.292(13) . ? Rh1 C5 2.305(13) . ? C1 C2 1.623(12) . ? C1 P1 1.941(6) . ? P1 C8 1.605(8) . ? P1 C10 2.169(16) . ? C2 C3 1.488(8) . ? C3 C7 1.229(18) . ? C3 C4 1.62(2) . ? C4 C5 1.23(2) . ? C5 C6 1.379(10) . ? C6 C7 1.527(19) . ? C8 C9 1.378(15) . ? C10 C11 1.428(15) . ? C20 O20 1.171(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C20 Rh1 P1 92.81(14) . . ? C20 Rh1 C3 174.7(7) . . ? P1 Rh1 C3 84.28(16) . . ? C20 Rh1 C4 142.9(7) . . ? P1 Rh1 C4 107.1(4) . . ? C3 Rh1 C4 42.4(5) . . ? C20 Rh1 C7 146.2(7) . . ? P1 Rh1 C7 103.0(4) . . ? C3 Rh1 C7 31.7(5) . . ? C4 Rh1 C7 59.7(2) . . ? C20 Rh1 C6 122.1(4) . . ? P1 Rh1 C6 141.5(4) . . ? C3 Rh1 C6 59.5(4) . . ? C4 Rh1 C6 55.3(6) . . ? C7 Rh1 C6 38.9(5) . . ? C20 Rh1 C5 121.9(5) . . ? P1 Rh1 C5 138.2(5) . . ? C3 Rh1 C5 62.6(4) . . ? C4 Rh1 C5 31.1(5) . . ? C7 Rh1 C5 61.8(5) . . ? C6 Rh1 C5 34.9(3) . . ? C2 C1 P1 100.5(6) . . ? C8 P1 C1 106.3(4) . . ? C8 P1 C10 106.1(5) . . ? C1 P1 C10 93.7(4) . . ? C8 P1 Rh1 132.3(5) . . ? C1 P1 Rh1 99.4(2) . . ? C10 P1 Rh1 111.6(4) . . ? C3 C2 C1 110.6(6) . . ? C7 C3 C2 133.7(14) . . ? C7 C3 C4 104.9(6) . . ? C2 C3 C4 121.4(13) . . ? C7 C3 Rh1 78.1(7) . . ? C2 C3 Rh1 115.0(3) . . ? C4 C3 Rh1 71.1(6) . . ? C5 C4 C3 109.9(15) . . ? C5 C4 Rh1 75.9(10) . . ? C3 C4 Rh1 66.5(5) . . ? C4 C5 C6 108.5(17) . . ? C4 C5 Rh1 72.9(9) . . ? C6 C5 Rh1 72.0(10) . . ? C5 C6 C7 108.5(16) . . ? C5 C6 Rh1 73.1(10) . . ? C7 C6 Rh1 70.5(6) . . ? C3 C7 C6 107.7(13) . . ? C3 C7 Rh1 70.2(6) . . ? C6 C7 Rh1 70.6(7) . . ? C9 C8 P1 107.1(10) . . ? C11 C10 P1 113.5(8) . . ? O20 C20 Rh1 172.4(17) . . ? 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 C2 C1 P1 C8 85.7(6) . . . . ? C2 C1 P1 C10 -166.3(6) . . . . ? C2 C1 P1 Rh1 -53.6(6) . . . . ? C20 Rh1 P1 C8 85.2(8) . . . . ? C3 Rh1 P1 C8 -90.4(6) . . . . ? C4 Rh1 P1 C8 -126.6(6) . . . . ? C7 Rh1 P1 C8 -64.7(6) . . . . ? C6 Rh1 P1 C8 -71.3(9) . . . . ? C5 Rh1 P1 C8 -126.6(8) . . . . ? C20 Rh1 P1 C1 -152.5(8) . . . . ? C3 Rh1 P1 C1 31.9(5) . . . . ? C4 Rh1 P1 C1 -4.3(6) . . . . ? C7 Rh1 P1 C1 57.6(5) . . . . ? C6 Rh1 P1 C1 51.0(9) . . . . ? C5 Rh1 P1 C1 -4.3(8) . . . . ? C20 Rh1 P1 C10 -54.7(8) . . . . ? C3 Rh1 P1 C10 129.7(6) . . . . ? C4 Rh1 P1 C10 93.5(6) . . . . ? C7 Rh1 P1 C10 155.4(5) . . . . ? C6 Rh1 P1 C10 148.8(8) . . . . ? C5 Rh1 P1 C10 93.5(7) . . . . ? P1 C1 C2 C3 53.4(12) . . . . ? C1 C2 C3 C7 -126.5(12) . . . . ? C1 C2 C3 C4 53.3(12) . . . . ? C1 C2 C3 Rh1 -29.0(15) . . . . ? C20 Rh1 C3 C7 70(5) . . . . ? P1 Rh1 C3 C7 126.3(8) . . . . ? C4 Rh1 C3 C7 -110.5(5) . . . . ? C6 Rh1 C3 C7 -40.1(9) . . . . ? C5 Rh1 C3 C7 -80.0(9) . . . . ? C20 Rh1 C3 C2 -63(6) . . . . ? P1 Rh1 C3 C2 -6.6(11) . . . . ? C4 Rh1 C3 C2 116.6(15) . . . . ? C7 Rh1 C3 C2 -132.9(16) . . . . ? C6 Rh1 C3 C2 -173.0(14) . . . . ? C5 Rh1 C3 C2 147.1(14) . . . . ? C20 Rh1 C3 C4 -180(31) . . . . ? P1 Rh1 C3 C4 -123.2(7) . . . . ? C7 Rh1 C3 C4 110.5(5) . . . . ? C6 Rh1 C3 C4 70.4(8) . . . . ? C5 Rh1 C3 C4 30.5(7) . . . . ? C7 C3 C4 C5 7.6(9) . . . . ? C2 C3 C4 C5 -172.2(9) . . . . ? Rh1 C3 C4 C5 -64.0(11) . . . . ? C7 C3 C4 Rh1 71.6(6) . . . . ? C2 C3 C4 Rh1 -108.3(5) . . . . ? C20 Rh1 C4 C5 -60.6(15) . . . . ? P1 Rh1 C4 C5 180.0(11) . . . . ? C3 Rh1 C4 C5 119.4(14) . . . . ? C7 Rh1 C4 C5 84.7(12) . . . . ? C6 Rh1 C4 C5 38.5(9) . . . . ? C20 Rh1 C4 C3 180.0(8) . . . . ? P1 Rh1 C4 C3 60.6(7) . . . . ? C7 Rh1 C4 C3 -34.7(6) . . . . ? C6 Rh1 C4 C3 -81.0(8) . . . . ? C5 Rh1 C4 C3 -119.4(14) . . . . ? C3 C4 C5 C6 -5.6(18) . . . . ? Rh1 C4 C5 C6 -63.7(13) . . . . ? C3 C4 C5 Rh1 58.1(8) . . . . ? C20 Rh1 C5 C4 141.7(13) . . . . ? P1 Rh1 C5 C4 0.0(15) . . . . ? C3 Rh1 C5 C4 -41.5(11) . . . . ? C7 Rh1 C5 C4 -77.4(9) . . . . ? C6 Rh1 C5 C4 -116.7(17) . . . . ? C20 Rh1 C5 C6 -101.7(13) . . . . ? P1 Rh1 C5 C6 116.6(12) . . . . ? C3 Rh1 C5 C6 75.2(11) . . . . ? C4 Rh1 C5 C6 116.7(17) . . . . ? C7 Rh1 C5 C6 39.3(10) . . . . ? C4 C5 C6 C7 2(2) . . . . ? Rh1 C5 C6 C7 -62.0(10) . . . . ? C4 C5 C6 Rh1 64.3(12) . . . . ? C20 Rh1 C6 C5 101.0(13) . . . . ? P1 Rh1 C6 C5 -107.0(13) . . . . ? C3 Rh1 C6 C5 -84.8(12) . . . . ? C4 Rh1 C6 C5 -34.2(10) . . . . ? C7 Rh1 C6 C5 -117.4(15) . . . . ? C20 Rh1 C6 C7 -141.6(11) . . . . ? P1 Rh1 C6 C7 10.4(14) . . . . ? C3 Rh1 C6 C7 32.5(8) . . . . ? C4 Rh1 C6 C7 83.2(7) . . . . ? C5 Rh1 C6 C7 117.4(15) . . . . ? C2 C3 C7 C6 174.3(7) . . . . ? C4 C3 C7 C6 -5.5(8) . . . . ? Rh1 C3 C7 C6 61.0(9) . . . . ? C2 C3 C7 Rh1 113.3(8) . . . . ? C4 C3 C7 Rh1 -66.5(5) . . . . ? C5 C6 C7 C3 2.9(17) . . . . ? Rh1 C6 C7 C3 -60.7(8) . . . . ? C5 C6 C7 Rh1 63.6(12) . . . . ? C20 Rh1 C7 C3 -171.1(8) . . . . ? P1 Rh1 C7 C3 -55.4(8) . . . . ? C4 Rh1 C7 C3 47.0(7) . . . . ? C6 Rh1 C7 C3 118.0(13) . . . . ? C5 Rh1 C7 C3 82.8(10) . . . . ? C20 Rh1 C7 C6 70.9(13) . . . . ? P1 Rh1 C7 C6 -173.4(9) . . . . ? C3 Rh1 C7 C6 -118.0(13) . . . . ? C4 Rh1 C7 C6 -71.0(10) . . . . ? C5 Rh1 C7 C6 -35.2(8) . . . . ? C1 P1 C8 C9 178.0(7) . . . . ? C10 P1 C8 C9 79.1(8) . . . . ? Rh1 P1 C8 C9 -62.3(9) . . . . ? C8 P1 C10 C11 52.8(10) . . . . ? C1 P1 C10 C11 -55.3(10) . . . . ? Rh1 P1 C10 C11 -157.0(8) . . . . ? P1 Rh1 C20 O20 -56(9) . . . . ? C3 Rh1 C20 O20 1(13) . . . . ? C4 Rh1 C20 O20 -179(100) . . . . ? C7 Rh1 C20 O20 63(8) . . . . ? C6 Rh1 C20 O20 107(8) . . . . ? C5 Rh1 C20 O20 149(9) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.239 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.046 data_1 _database_code_CSD 197744 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H26 O P Rh' _chemical_formula_sum 'C16 H26 O P Rh' _chemical_formula_weight 368.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 7.2206(6) _cell_length_b 16.6210(13) _cell_length_c 14.3525(12) _cell_angle_alpha 90.00 _cell_angle_beta 102.160(2) _cell_angle_gamma 90.00 _cell_volume 1683.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 64 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max .1 _exptl_crystal_size_mid .03 _exptl_crystal_size_min .03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 1.101 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.575936 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7070 _diffrn_reflns_av_R_equivalents 0.1767 _diffrn_reflns_av_sigmaI/netI 0.1439 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 23.39 _reflns_number_total 2382 _reflns_number_gt 1456 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0499P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2382 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0908 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1041 _refine_ls_wR_factor_gt 0.0838 _refine_ls_goodness_of_fit_ref 0.865 _refine_ls_restrained_S_all 0.865 _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 0.21159(8) 0.05195(3) 0.21301(3) 0.0379(2) Uani 1 1 d . . . P1 P 0.0872(3) 0.16156(11) 0.26290(11) 0.0455(5) Uani 1 1 d . . . C1 C -0.0723(12) 0.1210(4) 0.3361(5) 0.062(2) Uani 1 1 d . . . H1A H -0.0043 0.1178 0.4019 0.075 Uiso 1 1 calc R . . H1B H -0.1778 0.1577 0.3333 0.075 Uiso 1 1 calc R . . C2 C -0.1481(11) 0.0386(4) 0.3036(4) 0.0518(19) Uani 1 1 d . . . H2A H -0.1877 0.0116 0.3561 0.062 Uiso 1 1 calc R . . H2B H -0.2587 0.0446 0.2524 0.062 Uiso 1 1 calc R . . C3 C -0.0047(11) -0.0128(4) 0.2695(4) 0.0437(17) Uani 1 1 d . . . C4 C -0.0209(11) -0.0440(4) 0.1738(4) 0.0483(19) Uani 1 1 d . . . C5 C 0.1537(12) -0.0812(4) 0.1721(5) 0.0478(19) Uani 1 1 d . . . C6 C 0.2730(11) -0.0789(4) 0.2668(4) 0.050(2) Uani 1 1 d . . . C7 C 0.1735(11) -0.0406(4) 0.3265(4) 0.0439(17) Uani 1 1 d . . . C8 C -0.1912(12) -0.0397(4) 0.0955(4) 0.062(2) Uani 1 1 d . . . H8A H -0.2895 -0.0107 0.1167 0.093 Uiso 1 1 calc R . . H8B H -0.2343 -0.0932 0.0771 0.093 Uiso 1 1 calc R . . H8C H -0.1599 -0.0125 0.0418 0.093 Uiso 1 1 calc R . . C9 C 0.2021(13) -0.1241(4) 0.0872(5) 0.070(2) Uani 1 1 d . . . H9A H 0.3289 -0.1448 0.1042 0.105 Uiso 1 1 calc R . . H9B H 0.1930 -0.0869 0.0352 0.105 Uiso 1 1 calc R . . H9C H 0.1152 -0.1677 0.0683 0.105 Uiso 1 1 calc R . . C10 C 0.4630(12) -0.1197(5) 0.2953(5) 0.070(2) Uani 1 1 d . . . H10A H 0.5001 -0.1405 0.2396 0.106 Uiso 1 1 calc R . . H10B H 0.4543 -0.1630 0.3384 0.106 Uiso 1 1 calc R . . H10C H 0.5555 -0.0814 0.3262 0.106 Uiso 1 1 calc R . . C11 C 0.2353(12) -0.0336(5) 0.4343(4) 0.068(2) Uani 1 1 d . . . H11A H 0.1402 -0.0053 0.4590 0.102 Uiso 1 1 calc R . . H11B H 0.3529 -0.0048 0.4501 0.102 Uiso 1 1 calc R . . H11C H 0.2517 -0.0865 0.4618 0.102 Uiso 1 1 calc R . . C12 C 0.2349(13) 0.2351(5) 0.3395(5) 0.070(2) Uani 1 1 d . . . H12A H 0.2983 0.2682 0.3001 0.084 Uiso 1 1 calc R . . H12B H 0.1530 0.2700 0.3670 0.084 Uiso 1 1 calc R . . C13 C 0.3800(14) 0.2006(5) 0.4178(5) 0.091(3) Uani 1 1 d . . . H13A H 0.4509 0.2434 0.4537 0.137 Uiso 1 1 calc R . . H13B H 0.4641 0.1669 0.3916 0.137 Uiso 1 1 calc R . . H13C H 0.3190 0.1693 0.4589 0.137 Uiso 1 1 calc R . . C14 C -0.0634(13) 0.2252(5) 0.1752(5) 0.071(2) Uani 1 1 d . . . H14A H -0.1663 0.1926 0.1402 0.085 Uiso 1 1 calc R . . H14B H -0.1187 0.2663 0.2088 0.085 Uiso 1 1 calc R . . C15 C 0.0330(13) 0.2655(5) 0.1052(5) 0.079(3) Uani 1 1 d . . . H15A H -0.0574 0.2973 0.0619 0.118 Uiso 1 1 calc R . . H15B H 0.0858 0.2254 0.0702 0.118 Uiso 1 1 calc R . . H15C H 0.1324 0.2996 0.1387 0.118 Uiso 1 1 calc R . . C20 C 0.3742(11) 0.1061(4) 0.1550(5) 0.0521(19) Uani 1 1 d . . . O20 O 0.4724(9) 0.1461(3) 0.1198(4) 0.0859(18) 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 0.0419(4) 0.0309(3) 0.0426(3) 0.0003(3) 0.0129(2) -0.0018(3) P1 0.0514(14) 0.0336(10) 0.0548(10) -0.0035(8) 0.0189(9) -0.0035(9) C1 0.054(6) 0.055(5) 0.085(5) -0.012(4) 0.032(4) -0.006(4) C2 0.048(5) 0.055(5) 0.058(4) -0.003(3) 0.023(3) -0.005(4) C3 0.045(5) 0.047(4) 0.042(4) 0.000(3) 0.016(3) -0.009(4) C4 0.065(6) 0.035(4) 0.041(3) 0.001(3) 0.003(3) -0.012(4) C5 0.063(6) 0.020(3) 0.064(4) 0.000(3) 0.022(4) -0.002(3) C6 0.058(6) 0.028(4) 0.064(5) 0.012(3) 0.016(4) 0.004(3) C7 0.054(5) 0.034(4) 0.042(3) 0.007(3) 0.008(3) -0.001(4) C8 0.080(7) 0.050(5) 0.052(4) 0.000(3) 0.004(4) -0.016(4) C9 0.087(7) 0.052(5) 0.080(5) -0.019(4) 0.037(5) -0.005(5) C10 0.063(6) 0.043(5) 0.109(6) 0.011(4) 0.027(5) 0.001(4) C11 0.074(7) 0.072(6) 0.051(4) 0.015(4) -0.004(4) -0.008(5) C12 0.085(7) 0.054(5) 0.073(5) -0.020(4) 0.025(5) -0.016(5) C13 0.116(9) 0.084(7) 0.068(5) -0.015(5) 0.005(5) -0.024(6) C14 0.063(6) 0.057(5) 0.092(5) -0.003(4) 0.013(4) 0.009(5) C15 0.085(8) 0.063(6) 0.081(5) 0.023(4) 0.001(5) 0.003(5) C20 0.047(5) 0.046(5) 0.065(4) 0.003(4) 0.017(4) 0.003(4) O20 0.074(5) 0.081(4) 0.112(4) 0.034(4) 0.042(3) -0.008(4) _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 C20 1.814(8) . ? Rh1 C3 2.188(7) . ? Rh1 P1 2.2157(19) . ? Rh1 C4 2.298(7) . ? Rh1 C7 2.298(6) . ? Rh1 C5 2.306(6) . ? Rh1 C6 2.320(7) . ? P1 C14 1.818(8) . ? P1 C12 1.829(7) . ? P1 C1 1.842(7) . ? C1 C2 1.513(9) . ? C2 C3 1.501(9) . ? C3 C4 1.449(8) . ? C3 C7 1.447(9) . ? C4 C5 1.410(10) . ? C4 C8 1.483(10) . ? C5 C6 1.449(10) . ? C5 C9 1.515(8) . ? C6 C7 1.384(9) . ? C6 C10 1.507(10) . ? C7 C11 1.522(8) . ? C12 C13 1.481(11) . ? C14 C15 1.496(10) . ? C20 O20 1.163(8) . ? 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 C20 Rh1 C3 174.3(3) . . ? C20 Rh1 P1 94.9(2) . . ? C3 Rh1 P1 85.11(19) . . ? C20 Rh1 C4 137.9(3) . . ? C3 Rh1 C4 37.6(2) . . ? P1 Rh1 C4 108.9(2) . . ? C20 Rh1 C7 147.4(3) . . ? C3 Rh1 C7 37.5(2) . . ? P1 Rh1 C7 101.77(17) . . ? C4 Rh1 C7 61.2(2) . . ? C20 Rh1 C5 117.4(3) . . ? C3 Rh1 C5 61.1(2) . . ? P1 Rh1 C5 143.9(2) . . ? C4 Rh1 C5 35.7(2) . . ? C7 Rh1 C5 59.7(2) . . ? C20 Rh1 C6 121.4(3) . . ? C3 Rh1 C6 61.1(3) . . ? P1 Rh1 C6 136.52(17) . . ? C4 Rh1 C6 60.6(3) . . ? C7 Rh1 C6 34.9(2) . . ? C5 Rh1 C6 36.5(2) . . ? C14 P1 C12 102.4(4) . . ? C14 P1 C1 104.6(4) . . ? C12 P1 C1 104.9(3) . . ? C14 P1 Rh1 118.6(3) . . ? C12 P1 Rh1 121.2(3) . . ? C1 P1 Rh1 103.2(2) . . ? C2 C1 P1 112.6(5) . . ? C3 C2 C1 112.7(6) . . ? C4 C3 C7 107.8(6) . . ? C4 C3 C2 126.1(6) . . ? C7 C3 C2 126.1(5) . . ? C4 C3 Rh1 75.3(4) . . ? C7 C3 Rh1 75.4(4) . . ? C2 C3 Rh1 115.9(5) . . ? C5 C4 C3 106.2(6) . . ? C5 C4 C8 127.5(6) . . ? C3 C4 C8 126.2(7) . . ? C5 C4 Rh1 72.5(4) . . ? C3 C4 Rh1 67.1(3) . . ? C8 C4 Rh1 126.8(5) . . ? C4 C5 C6 109.2(6) . . ? C4 C5 C9 125.4(7) . . ? C6 C5 C9 125.1(7) . . ? C4 C5 Rh1 71.9(4) . . ? C6 C5 Rh1 72.3(4) . . ? C9 C5 Rh1 126.6(5) . . ? C7 C6 C5 108.0(7) . . ? C7 C6 C10 126.9(6) . . ? C5 C6 C10 124.8(6) . . ? C7 C6 Rh1 71.7(4) . . ? C5 C6 Rh1 71.2(3) . . ? C10 C6 Rh1 127.7(5) . . ? C6 C7 C3 108.3(5) . . ? C6 C7 C11 125.8(7) . . ? C3 C7 C11 125.8(6) . . ? C6 C7 Rh1 73.4(4) . . ? C3 C7 Rh1 67.1(3) . . ? C11 C7 Rh1 128.1(5) . . ? C13 C12 P1 115.3(6) . . ? C15 C14 P1 115.5(6) . . ? O20 C20 Rh1 174.8(6) . . ? 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 C20 Rh1 P1 C14 70.2(4) . . . . ? C3 Rh1 P1 C14 -104.1(4) . . . . ? C4 Rh1 P1 C14 -74.6(4) . . . . ? C7 Rh1 P1 C14 -138.0(4) . . . . ? C5 Rh1 P1 C14 -84.0(4) . . . . ? C6 Rh1 P1 C14 -141.5(4) . . . . ? C20 Rh1 P1 C12 -57.9(4) . . . . ? C3 Rh1 P1 C12 127.7(3) . . . . ? C4 Rh1 P1 C12 157.3(3) . . . . ? C7 Rh1 P1 C12 93.9(3) . . . . ? C5 Rh1 P1 C12 147.9(4) . . . . ? C6 Rh1 P1 C12 90.3(4) . . . . ? C20 Rh1 P1 C1 -174.8(4) . . . . ? C3 Rh1 P1 C1 10.9(3) . . . . ? C4 Rh1 P1 C1 40.5(3) . . . . ? C7 Rh1 P1 C1 -22.9(3) . . . . ? C5 Rh1 P1 C1 31.1(4) . . . . ? C6 Rh1 P1 C1 -26.5(4) . . . . ? C14 P1 C1 C2 95.9(6) . . . . ? C12 P1 C1 C2 -156.7(6) . . . . ? Rh1 P1 C1 C2 -28.8(6) . . . . ? P1 C1 C2 C3 36.6(8) . . . . ? C1 C2 C3 C4 -117.2(7) . . . . ? C1 C2 C3 C7 63.4(8) . . . . ? C1 C2 C3 Rh1 -26.9(7) . . . . ? C20 Rh1 C3 C4 39(3) . . . . ? P1 Rh1 C3 C4 130.2(4) . . . . ? C7 Rh1 C3 C4 -113.3(6) . . . . ? C5 Rh1 C3 C4 -36.4(4) . . . . ? C6 Rh1 C3 C4 -78.3(4) . . . . ? C20 Rh1 C3 C7 153(3) . . . . ? P1 Rh1 C3 C7 -116.6(3) . . . . ? C4 Rh1 C3 C7 113.3(6) . . . . ? C5 Rh1 C3 C7 76.8(4) . . . . ? C6 Rh1 C3 C7 34.9(3) . . . . ? C20 Rh1 C3 C2 -84(3) . . . . ? P1 Rh1 C3 C2 6.8(4) . . . . ? C4 Rh1 C3 C2 -123.3(7) . . . . ? C7 Rh1 C3 C2 123.4(6) . . . . ? C5 Rh1 C3 C2 -159.8(6) . . . . ? C6 Rh1 C3 C2 158.3(6) . . . . ? C7 C3 C4 C5 -6.6(7) . . . . ? C2 C3 C4 C5 173.9(6) . . . . ? Rh1 C3 C4 C5 62.4(5) . . . . ? C7 C3 C4 C8 171.3(6) . . . . ? C2 C3 C4 C8 -8.2(11) . . . . ? Rh1 C3 C4 C8 -119.8(6) . . . . ? C7 C3 C4 Rh1 -69.0(5) . . . . ? C2 C3 C4 Rh1 111.6(7) . . . . ? C20 Rh1 C4 C5 68.5(5) . . . . ? C3 Rh1 C4 C5 -116.9(5) . . . . ? P1 Rh1 C4 C5 -170.5(3) . . . . ? C7 Rh1 C4 C5 -77.2(4) . . . . ? C6 Rh1 C4 C5 -37.1(4) . . . . ? C20 Rh1 C4 C3 -174.6(5) . . . . ? P1 Rh1 C4 C3 -53.6(4) . . . . ? C7 Rh1 C4 C3 39.7(4) . . . . ? C5 Rh1 C4 C3 116.9(5) . . . . ? C6 Rh1 C4 C3 79.8(4) . . . . ? C20 Rh1 C4 C8 -55.7(8) . . . . ? C3 Rh1 C4 C8 119.0(8) . . . . ? P1 Rh1 C4 C8 65.3(6) . . . . ? C7 Rh1 C4 C8 158.6(7) . . . . ? C5 Rh1 C4 C8 -124.2(8) . . . . ? C6 Rh1 C4 C8 -161.3(7) . . . . ? C3 C4 C5 C6 4.2(7) . . . . ? C8 C4 C5 C6 -173.7(6) . . . . ? Rh1 C4 C5 C6 63.0(5) . . . . ? C3 C4 C5 C9 178.7(6) . . . . ? C8 C4 C5 C9 0.9(11) . . . . ? Rh1 C4 C5 C9 -122.4(7) . . . . ? C3 C4 C5 Rh1 -58.9(4) . . . . ? C8 C4 C5 Rh1 123.3(7) . . . . ? C20 Rh1 C5 C4 -135.4(4) . . . . ? C3 Rh1 C5 C4 38.4(4) . . . . ? P1 Rh1 C5 C4 15.4(5) . . . . ? C7 Rh1 C5 C4 81.8(4) . . . . ? C6 Rh1 C5 C4 118.0(6) . . . . ? C20 Rh1 C5 C6 106.7(4) . . . . ? C3 Rh1 C5 C6 -79.5(4) . . . . ? P1 Rh1 C5 C6 -102.6(5) . . . . ? C4 Rh1 C5 C6 -118.0(6) . . . . ? C7 Rh1 C5 C6 -36.1(4) . . . . ? C20 Rh1 C5 C9 -14.3(8) . . . . ? C3 Rh1 C5 C9 159.5(8) . . . . ? P1 Rh1 C5 C9 136.5(6) . . . . ? C4 Rh1 C5 C9 121.1(8) . . . . ? C7 Rh1 C5 C9 -157.1(8) . . . . ? C6 Rh1 C5 C9 -120.9(9) . . . . ? C4 C5 C6 C7 -0.1(8) . . . . ? C9 C5 C6 C7 -174.7(6) . . . . ? Rh1 C5 C6 C7 62.7(5) . . . . ? C4 C5 C6 C10 173.9(7) . . . . ? C9 C5 C6 C10 -0.7(11) . . . . ? Rh1 C5 C6 C10 -123.3(7) . . . . ? C4 C5 C6 Rh1 -62.8(5) . . . . ? C9 C5 C6 Rh1 122.7(7) . . . . ? C20 Rh1 C6 C7 148.3(4) . . . . ? C3 Rh1 C6 C7 -37.6(4) . . . . ? P1 Rh1 C6 C7 6.1(6) . . . . ? C4 Rh1 C6 C7 -80.9(5) . . . . ? C5 Rh1 C6 C7 -117.1(7) . . . . ? C20 Rh1 C6 C5 -94.6(5) . . . . ? C3 Rh1 C6 C5 79.5(5) . . . . ? P1 Rh1 C6 C5 123.2(4) . . . . ? C4 Rh1 C6 C5 36.2(4) . . . . ? C7 Rh1 C6 C5 117.1(7) . . . . ? C20 Rh1 C6 C10 25.3(7) . . . . ? C3 Rh1 C6 C10 -160.5(7) . . . . ? P1 Rh1 C6 C10 -116.8(6) . . . . ? C4 Rh1 C6 C10 156.2(7) . . . . ? C7 Rh1 C6 C10 -122.9(8) . . . . ? C5 Rh1 C6 C10 119.9(8) . . . . ? C5 C6 C7 C3 -4.1(8) . . . . ? C10 C6 C7 C3 -177.9(7) . . . . ? Rh1 C6 C7 C3 58.3(5) . . . . ? C5 C6 C7 C11 172.3(6) . . . . ? C10 C6 C7 C11 -1.5(12) . . . . ? Rh1 C6 C7 C11 -125.4(7) . . . . ? C5 C6 C7 Rh1 -62.4(5) . . . . ? C10 C6 C7 Rh1 123.8(8) . . . . ? C4 C3 C7 C6 6.7(7) . . . . ? C2 C3 C7 C6 -173.8(7) . . . . ? Rh1 C3 C7 C6 -62.3(5) . . . . ? C4 C3 C7 C11 -169.7(6) . . . . ? C2 C3 C7 C11 9.8(11) . . . . ? Rh1 C3 C7 C11 121.4(6) . . . . ? C4 C3 C7 Rh1 69.0(4) . . . . ? C2 C3 C7 Rh1 -111.6(7) . . . . ? C20 Rh1 C7 C6 -56.4(7) . . . . ? C3 Rh1 C7 C6 118.7(6) . . . . ? P1 Rh1 C7 C6 -175.7(4) . . . . ? C4 Rh1 C7 C6 79.0(5) . . . . ? C5 Rh1 C7 C6 37.8(5) . . . . ? C20 Rh1 C7 C3 -175.2(5) . . . . ? P1 Rh1 C7 C3 65.5(3) . . . . ? C4 Rh1 C7 C3 -39.7(4) . . . . ? C5 Rh1 C7 C3 -80.9(4) . . . . ? C6 Rh1 C7 C3 -118.7(6) . . . . ? C20 Rh1 C7 C11 66.4(8) . . . . ? C3 Rh1 C7 C11 -118.5(8) . . . . ? P1 Rh1 C7 C11 -52.9(7) . . . . ? C4 Rh1 C7 C11 -158.2(7) . . . . ? C5 Rh1 C7 C11 160.6(8) . . . . ? C6 Rh1 C7 C11 122.8(9) . . . . ? C14 P1 C12 C13 -178.1(7) . . . . ? C1 P1 C12 C13 72.9(7) . . . . ? Rh1 P1 C12 C13 -43.1(7) . . . . ? C12 P1 C14 C15 71.3(6) . . . . ? C1 P1 C14 C15 -179.5(6) . . . . ? Rh1 P1 C14 C15 -65.2(7) . . . . ? C3 Rh1 C20 O20 88(8) . . . . ? P1 Rh1 C20 O20 -2(7) . . . . ? C4 Rh1 C20 O20 123(7) . . . . ? C7 Rh1 C20 O20 -123(7) . . . . ? C5 Rh1 C20 O20 161(7) . . . . ? C6 Rh1 C20 O20 -157(7) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 23.39 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.567 _refine_diff_density_min -1.883 _refine_diff_density_rms 0.166