Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'D. Cole-Hamilton' _publ_contact_author_name 'D. Cole-Hamilton' _publ_contact_author_address ; Chemistry Department St Andrews University St Andrews Fife KY16 9ST UNITED KINGDOM ; _publ_contact_author_email DJC@ST-AND.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Modelling proposed intermediates in the hydrocarbonylation of alkenes catalysed by rhodium complexes of PBui3 and PPri3 ; data_RhCl(CO)(PBui3)2 _database_code_depnum_ccdc_archive 'CCDC 661625' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H54 Cl O P2 Rh' _chemical_formula_sum 'C25 H54 Cl O P2 Rh' _chemical_formula_weight 570.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 9.3678(14) _cell_length_b 12.7401(18) _cell_length_c 13.0138(19) _cell_angle_alpha 90.00 _cell_angle_beta 101.414(2) _cell_angle_gamma 90.00 _cell_volume 1522.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 165 _cell_measurement_theta_min 12 _cell_measurement_theta_max 28 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 0.767 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.86795 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details SHELXTL _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8950 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.40 _reflns_number_total 2776 _reflns_number_gt 2227 _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^)+(0.0625P)^2^+1.6883P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0024(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2776 _refine_ls_number_parameters 152 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1132 _refine_ls_wR_factor_gt 0.1042 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.004 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 0.5000 1.0000 0.0000 0.02621(17) Uani 1 2 d S . . Cl1 Cl 0.4240(4) 1.1725(3) 0.0346(3) 0.0382(10) Uani 0.50 1 d P . . P1 P 0.42726(10) 0.93037(7) 0.14727(7) 0.0286(2) Uani 1 1 d . . . C1 C 0.5789(4) 0.8625(3) 0.2332(3) 0.0336(8) Uani 1 1 d . . . H1A H 0.5530 0.8535 0.3028 0.040 Uiso 1 1 calc R . . H1B H 0.5878 0.7915 0.2042 0.040 Uiso 1 1 calc R . . C2 C 0.7282(4) 0.9155(3) 0.2490(3) 0.0399(9) Uani 1 1 d . . . H2A H 0.7586 0.9182 0.1796 0.048 Uiso 1 1 calc R . . C3 C 0.7287(5) 1.0263(4) 0.2905(4) 0.0533(12) Uani 1 1 d . . . H3A H 0.6576 1.0687 0.2425 0.080 Uiso 1 1 calc R . . H3B H 0.8260 1.0568 0.2960 0.080 Uiso 1 1 calc R . . H3C H 0.7029 1.0253 0.3599 0.080 Uiso 1 1 calc R . . C4 C 0.8386(5) 0.8471(4) 0.3231(4) 0.0556(12) Uani 1 1 d . . . H4A H 0.9350 0.8800 0.3339 0.083 Uiso 1 1 calc R . . H4B H 0.8431 0.7774 0.2921 0.083 Uiso 1 1 calc R . . H4C H 0.8082 0.8403 0.3907 0.083 Uiso 1 1 calc R . . C5 C 0.2911(4) 0.8257(3) 0.1182(3) 0.0361(9) Uani 1 1 d . . . H5A H 0.3289 0.7710 0.0767 0.043 Uiso 1 1 calc R . . H5B H 0.2794 0.7933 0.1852 0.043 Uiso 1 1 calc R . . C6 C 0.1401(4) 0.8601(4) 0.0582(3) 0.0446(10) Uani 1 1 d . . . H6A H 0.1157 0.9287 0.0878 0.054 Uiso 1 1 calc R . . C7 C 0.1378(5) 0.8754(4) -0.0576(4) 0.0590(13) Uani 1 1 d . . . H7A H 0.2112 0.9275 -0.0666 0.088 Uiso 1 1 calc R . . H7B H 0.0412 0.8999 -0.0925 0.088 Uiso 1 1 calc R . . H7C H 0.1594 0.8085 -0.0885 0.088 Uiso 1 1 calc R . . C8 C 0.0247(5) 0.7799(5) 0.0738(4) 0.0711(16) Uani 1 1 d . . . H8A H 0.0276 0.7705 0.1489 0.107 Uiso 1 1 calc R . . H8B H 0.0444 0.7127 0.0427 0.107 Uiso 1 1 calc R . . H8C H -0.0718 0.8053 0.0396 0.107 Uiso 1 1 calc R . . C9 C 0.3462(4) 1.0229(3) 0.2283(3) 0.0354(9) Uani 1 1 d . . . H9A H 0.4262 1.0680 0.2652 0.042 Uiso 1 1 calc R . . H9B H 0.2795 1.0689 0.1795 0.042 Uiso 1 1 calc R . . C10 C 0.2609(8) 0.9836(4) 0.3117(5) 0.0667(16) Uani 1 1 d . . . H10A H 0.1782 0.9425 0.2703 0.080 Uiso 1 1 calc R . . C11 C 0.1880(8) 1.0761(5) 0.3526(5) 0.0810(19) Uani 1 1 d . . . H11A H 0.1328 1.0516 0.4046 0.121 Uiso 1 1 calc R . . H11B H 0.1217 1.1101 0.2944 0.121 Uiso 1 1 calc R . . H11C H 0.2622 1.1265 0.3854 0.121 Uiso 1 1 calc R . . C12 C 0.3269(10) 0.9134(6) 0.3915(6) 0.116(3) Uani 1 1 d . . . H12A H 0.2570 0.8953 0.4356 0.175 Uiso 1 1 calc R . . H12B H 0.4124 0.9469 0.4346 0.175 Uiso 1 1 calc R . . H12C H 0.3569 0.8496 0.3595 0.175 Uiso 1 1 calc R . . C21 C 0.4399(15) 1.1265(8) 0.0223(10) 0.029(3) Uani 0.50 1 d P . . O21 O 0.4064(16) 1.2143(7) 0.0411(11) 0.051(3) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0264(2) 0.0264(3) 0.0273(2) -0.00127(16) 0.00861(15) 0.00003(16) Cl1 0.0591(18) 0.019(3) 0.0420(16) -0.005(2) 0.0239(12) 0.004(3) P1 0.0279(5) 0.0303(5) 0.0291(5) 0.0003(4) 0.0089(3) -0.0008(4) C1 0.033(2) 0.0335(19) 0.0351(19) 0.0055(16) 0.0098(15) 0.0042(16) C2 0.030(2) 0.055(3) 0.037(2) 0.0027(19) 0.0113(16) 0.0005(19) C3 0.037(2) 0.063(3) 0.057(3) -0.004(2) 0.004(2) -0.007(2) C4 0.038(2) 0.073(3) 0.053(3) 0.012(2) 0.002(2) 0.006(2) C5 0.037(2) 0.036(2) 0.037(2) -0.0027(16) 0.0111(16) -0.0079(17) C6 0.032(2) 0.047(2) 0.055(3) -0.012(2) 0.0109(18) -0.0061(19) C7 0.040(2) 0.068(3) 0.063(3) 0.017(3) -0.003(2) -0.008(2) C8 0.045(3) 0.109(5) 0.061(3) -0.011(3) 0.015(2) -0.030(3) C9 0.033(2) 0.037(2) 0.036(2) -0.0052(16) 0.0073(16) 0.0016(16) C10 0.098(4) 0.054(3) 0.061(3) 0.002(2) 0.044(3) 0.006(3) C11 0.108(5) 0.075(4) 0.078(4) 0.003(3) 0.064(4) 0.021(4) C12 0.148(7) 0.117(6) 0.114(6) 0.049(5) 0.099(6) 0.042(6) C21 0.049(6) 0.008(7) 0.033(5) -0.011(5) 0.014(4) 0.000(6) O21 0.081(6) 0.016(6) 0.063(5) -0.013(5) 0.030(4) 0.006(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C21 1.750(10) . ? Rh1 C21 1.750(10) 3_675 ? Rh1 P1 2.3326(10) . ? Rh1 P1 2.3326(10) 3_675 ? Rh1 Cl1 2.380(4) . ? Rh1 Cl1 2.380(4) 3_675 ? Cl1 O21 0.569(7) . ? Cl1 C21 0.633(8) . ? P1 C5 1.832(4) . ? P1 C1 1.840(4) . ? P1 C9 1.842(4) . ? C1 C2 1.530(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.511(6) . ? C2 C4 1.538(6) . ? C2 H2A 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.538(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.515(6) . ? C6 C8 1.530(6) . ? C6 H6A 1.0000 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.553(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C12 1.416(9) . ? C10 C11 1.510(7) . ? C10 H10A 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C21 O21 1.200(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 Rh1 C21 180.000(2) . 3_675 ? C21 Rh1 P1 93.3(4) . . ? C21 Rh1 P1 86.7(4) 3_675 . ? C21 Rh1 P1 86.7(4) . 3_675 ? C21 Rh1 P1 93.3(4) 3_675 3_675 ? P1 Rh1 P1 180.00(4) . 3_675 ? C21 Rh1 Cl1 1.7(4) . . ? C21 Rh1 Cl1 178.3(4) 3_675 . ? P1 Rh1 Cl1 92.79(8) . . ? P1 Rh1 Cl1 87.21(8) 3_675 . ? C21 Rh1 Cl1 178.3(4) . 3_675 ? C21 Rh1 Cl1 1.7(4) 3_675 3_675 ? P1 Rh1 Cl1 87.21(8) . 3_675 ? P1 Rh1 Cl1 92.79(8) 3_675 3_675 ? Cl1 Rh1 Cl1 180.0 . 3_675 ? O21 Cl1 C21 173.8(15) . . ? O21 Cl1 Rh1 177.5(16) . . ? C5 P1 C1 101.86(18) . . ? C5 P1 C9 103.56(18) . . ? C1 P1 C9 107.99(18) . . ? C5 P1 Rh1 114.33(13) . . ? C1 P1 Rh1 111.22(12) . . ? C9 P1 Rh1 116.57(14) . . ? C2 C1 P1 116.7(3) . . ? C2 C1 H1A 108.1 . . ? P1 C1 H1A 108.1 . . ? C2 C1 H1B 108.1 . . ? P1 C1 H1B 108.1 . . ? H1A C1 H1B 107.3 . . ? C3 C2 C1 113.5(3) . . ? C3 C2 C4 110.5(4) . . ? C1 C2 C4 108.5(3) . . ? C3 C2 H2A 108.0 . . ? C1 C2 H2A 108.0 . . ? C4 C2 H2A 108.0 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 P1 115.5(3) . . ? C6 C5 H5A 108.4 . . ? P1 C5 H5A 108.4 . . ? C6 C5 H5B 108.4 . . ? P1 C5 H5B 108.4 . . ? H5A C5 H5B 107.5 . . ? C7 C6 C8 110.2(4) . . ? C7 C6 C5 111.9(3) . . ? C8 C6 C5 110.2(4) . . ? C7 C6 H6A 108.1 . . ? C8 C6 H6A 108.1 . . ? C5 C6 H6A 108.1 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 P1 121.5(3) . . ? C10 C9 H9A 107.0 . . ? P1 C9 H9A 107.0 . . ? C10 C9 H9B 107.0 . . ? P1 C9 H9B 107.0 . . ? H9A C9 H9B 106.7 . . ? C12 C10 C11 113.3(5) . . ? C12 C10 C9 120.4(5) . . ? C11 C10 C9 109.1(4) . . ? C12 C10 H10A 104.1 . . ? C11 C10 H10A 104.1 . . ? C9 C10 H10A 104.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Cl1 C21 Rh1 173.7(17) . . ? O21 C21 Rh1 176.3(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 P1 Rh1 Cl1 C21 -109(15) . . . . ? P1 Rh1 Cl1 C21 71(15) 3_675 . . . ? C21 Rh1 P1 C5 119.4(5) . . . . ? C21 Rh1 P1 C5 -60.6(5) 3_675 . . . ? Cl1 Rh1 P1 C5 120.99(17) . . . . ? Cl1 Rh1 P1 C5 -59.01(17) 3_675 . . . ? C21 Rh1 P1 C1 -125.9(5) . . . . ? C21 Rh1 P1 C1 54.1(5) 3_675 . . . ? Cl1 Rh1 P1 C1 -124.32(16) . . . . ? Cl1 Rh1 P1 C1 55.68(16) 3_675 . . . ? C21 Rh1 P1 C9 -1.5(5) . . . . ? C21 Rh1 P1 C9 178.5(5) 3_675 . . . ? Cl1 Rh1 P1 C9 0.06(17) . . . . ? Cl1 Rh1 P1 C9 -179.94(17) 3_675 . . . ? C5 P1 C1 C2 163.3(3) . . . . ? C9 P1 C1 C2 -88.1(3) . . . . ? Rh1 P1 C1 C2 41.0(3) . . . . ? P1 C1 C2 C3 56.4(4) . . . . ? P1 C1 C2 C4 179.7(3) . . . . ? C1 P1 C5 C6 172.4(3) . . . . ? C9 P1 C5 C6 60.4(3) . . . . ? Rh1 P1 C5 C6 -67.5(3) . . . . ? P1 C5 C6 C7 77.9(4) . . . . ? P1 C5 C6 C8 -159.1(3) . . . . ? C5 P1 C9 C10 38.8(4) . . . . ? C1 P1 C9 C10 -68.7(4) . . . . ? Rh1 P1 C9 C10 165.3(4) . . . . ? P1 C9 C10 C12 55.4(8) . . . . ? P1 C9 C10 C11 -171.1(4) . . . . ? Rh1 Cl1 C21 O21 -158(18) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.250 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.087 # Attachment 'RhCl_CO__PPri3_2.cif' data_RhCl(CO)(PPri3)2 _database_code_depnum_ccdc_archive 'CCDC 661626' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H42 Cl O P2 Rh' _chemical_formula_sum 'C19 H42 Cl O P2 Rh' _chemical_formula_weight 486.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 8.0534(16) _cell_length_b 8.875(2) _cell_length_c 16.440(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.301(7) _cell_angle_gamma 90.00 _cell_volume 1174.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 3478 _cell_measurement_theta_min 2.2934 _cell_measurement_theta_max 25.3491 _exptl_crystal_description Platelet _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.1000 _exptl_crystal_size_mid 0.0500 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 512 _exptl_absorpt_coefficient_mu 0.982 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8964 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6740 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0706 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 25.35 _reflns_number_total 2056 _reflns_number_gt 1665 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0846P)^2^+0.4531P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2056 _refine_ls_number_parameters 124 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.1098 _refine_ls_wR_factor_gt 0.0975 _refine_ls_goodness_of_fit_ref 0.807 _refine_ls_restrained_S_all 0.807 _refine_ls_shift/su_max 3.032 _refine_ls_shift/su_mean 0.149 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 1.0000 0.0000 1.0000 0.01179(6) Uani 1 2 d S . . Cl1 Cl 1.01242(13) -0.20107(12) 1.09968(6) 0.0301(3) Uani 0.50 1 d P . . P1 P 1.12429(5) 0.16455(5) 1.09647(3) 0.01220(11) Uani 1 1 d . . . C1 C 0.9670(2) 0.2536(2) 1.15997(11) 0.0150(5) Uani 1 1 d . . . H1A H 1.0263 0.3154 1.2029 0.018 Uiso 1 1 calc R . . C2 C 0.8642(2) 0.1338(2) 1.20194(12) 0.0226(5) Uani 1 1 d . . . H2A H 0.7821 0.1831 1.2354 0.034 Uiso 1 1 calc R . . H2B H 0.9377 0.0708 1.2366 0.034 Uiso 1 1 calc R . . H2C H 0.8068 0.0708 1.1607 0.034 Uiso 1 1 calc R . . C3 C 0.8524(2) 0.3577(2) 1.10905(12) 0.0248(5) Uani 1 1 d . . . H3A H 0.7710 0.4038 1.1441 0.037 Uiso 1 1 calc R . . H3B H 0.7943 0.2991 1.0662 0.037 Uiso 1 1 calc R . . H3C H 0.9186 0.4368 1.0843 0.037 Uiso 1 1 calc R . . C4 C 1.2300(2) 0.3263(2) 1.04993(11) 0.0164(5) Uani 1 1 d . . . H4A H 1.1434 0.3741 1.0131 0.020 Uiso 1 1 calc R . . C5 C 1.2917(3) 0.4533(2) 1.10665(13) 0.0273(6) Uani 1 1 d . . . H5A H 1.3438 0.5322 1.0746 0.041 Uiso 1 1 calc R . . H5B H 1.3732 0.4130 1.1468 0.041 Uiso 1 1 calc R . . H5C H 1.1975 0.4960 1.1348 0.041 Uiso 1 1 calc R . . C6 C 1.3672(2) 0.2776(3) 0.99390(13) 0.0301(6) Uani 1 1 d . . . H6A H 1.4184 0.3670 0.9705 0.045 Uiso 1 1 calc R . . H6B H 1.3194 0.2144 0.9500 0.045 Uiso 1 1 calc R . . H6C H 1.4517 0.2202 1.0253 0.045 Uiso 1 1 calc R . . C7 C 1.2671(2) 0.0683(2) 1.17116(11) 0.0181(5) Uani 1 1 d . . . H7A H 1.1976 -0.0092 1.1980 0.022 Uiso 1 1 calc R . . C8 C 1.3420(3) 0.1640(2) 1.24043(12) 0.0265(6) Uani 1 1 d . . . H8A H 1.4139 0.1011 1.2759 0.040 Uiso 1 1 calc R . . H8B H 1.2526 0.2065 1.2721 0.040 Uiso 1 1 calc R . . H8C H 1.4075 0.2459 1.2179 0.040 Uiso 1 1 calc R . . C9 C 1.4022(3) -0.0202(2) 1.12932(15) 0.0321(7) Uani 1 1 d . . . H9A H 1.4744 -0.0698 1.1706 0.048 Uiso 1 1 calc R . . H9B H 1.4683 0.0488 1.0972 0.048 Uiso 1 1 calc R . . H9C H 1.3505 -0.0964 1.0934 0.048 Uiso 1 1 calc R . . C10 C 0.9982(5) -0.1442(5) 1.0731(3) 0.0255(12) Uani 0.50 1 d P . . O10 O 1.0279(4) -0.2361(4) 1.1180(2) 0.0419(10) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01402(11) 0.01131(11) 0.00999(11) -0.00096(7) -0.00030(9) -0.00123(7) Cl1 0.0437(6) 0.0194(5) 0.0254(5) -0.0004(5) -0.0227(4) 0.0016(4) P1 0.0123(2) 0.0118(2) 0.0125(2) -0.00124(19) -0.00007(17) -0.00097(17) C1 0.0152(8) 0.0162(10) 0.0136(9) -0.0018(8) 0.0007(7) -0.0006(7) C2 0.0205(9) 0.0215(11) 0.0265(10) -0.0043(9) 0.0121(8) -0.0015(8) C3 0.0214(9) 0.0299(12) 0.0233(10) -0.0010(9) 0.0025(8) 0.0084(8) C4 0.0234(9) 0.0106(9) 0.0155(9) -0.0030(8) 0.0058(7) -0.0046(7) C5 0.0407(12) 0.0193(10) 0.0220(11) -0.0037(10) 0.0018(9) -0.0122(10) C6 0.0281(10) 0.0298(12) 0.0338(11) 0.0015(10) 0.0180(9) -0.0018(9) C7 0.0201(9) 0.0187(10) 0.0153(9) 0.0017(8) -0.0019(7) 0.0030(8) C8 0.0294(10) 0.0257(11) 0.0235(10) -0.0028(9) -0.0120(8) -0.0005(9) C9 0.0276(12) 0.0378(13) 0.0307(13) 0.0019(10) -0.0006(10) 0.0197(9) C10 0.023(2) 0.025(3) 0.028(2) 0.000(2) -0.0088(18) 0.0060(18) O10 0.0491(18) 0.037(2) 0.0369(19) -0.0036(17) -0.0378(15) 0.0185(15) _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 C10 1.756(5) 3_757 ? Rh1 C10 1.756(5) . ? Rh1 P1 2.3500(6) . ? Rh1 P1 2.3500(6) 3_757 ? Rh1 Cl1 2.4222(12) 3_757 ? Rh1 Cl1 2.4222(12) . ? Cl1 C10 0.675(4) . ? P1 C1 1.8504(18) . ? P1 C4 1.8504(19) . ? P1 C7 1.8564(19) . ? C1 C2 1.529(3) . ? C1 C3 1.531(3) . ? C1 H1A 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C6 1.529(3) . ? C4 C5 1.533(3) . ? C4 H4A 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.525(3) . ? C7 C9 1.528(3) . ? C7 H7A 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 O10 1.119(5) . ? 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 C10 Rh1 C10 180.000(1) 3_757 . ? C10 Rh1 P1 89.65(14) 3_757 . ? C10 Rh1 P1 90.35(14) . . ? C10 Rh1 P1 90.35(14) 3_757 3_757 ? C10 Rh1 P1 89.65(14) . 3_757 ? P1 Rh1 P1 180.0 . 3_757 ? C10 Rh1 Cl1 2.94(14) 3_757 3_757 ? C10 Rh1 Cl1 177.06(14) . 3_757 ? P1 Rh1 Cl1 90.21(3) . 3_757 ? P1 Rh1 Cl1 89.79(3) 3_757 3_757 ? C10 Rh1 Cl1 177.06(14) 3_757 . ? C10 Rh1 Cl1 2.94(14) . . ? P1 Rh1 Cl1 89.79(3) . . ? P1 Rh1 Cl1 90.21(3) 3_757 . ? Cl1 Rh1 Cl1 180.0 3_757 . ? C1 P1 C4 103.81(9) . . ? C1 P1 C7 104.07(8) . . ? C4 P1 C7 110.33(9) . . ? C1 P1 Rh1 111.31(6) . . ? C4 P1 Rh1 113.18(6) . . ? C7 P1 Rh1 113.35(7) . . ? C2 C1 C3 109.90(15) . . ? C2 C1 P1 110.69(13) . . ? C3 C1 P1 111.13(13) . . ? C2 C1 H1A 108.3 . . ? C3 C1 H1A 108.3 . . ? P1 C1 H1A 108.3 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C6 C4 C5 110.50(16) . . ? C6 C4 P1 112.67(14) . . ? C5 C4 P1 117.53(13) . . ? C6 C4 H4A 105.0 . . ? C5 C4 H4A 105.0 . . ? P1 C4 H4A 105.0 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C9 110.80(16) . . ? C8 C7 P1 116.98(14) . . ? C9 C7 P1 111.85(14) . . ? C8 C7 H7A 105.4 . . ? C9 C7 H7A 105.4 . . ? P1 C7 H7A 105.4 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Cl1 C10 Rh1 169.4(5) . . ? O10 C10 Rh1 167.1(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 P1 Rh1 Cl1 C10 101(3) . . . . ? P1 Rh1 Cl1 C10 -79(3) 3_757 . . . ? C10 Rh1 P1 C1 96.28(15) 3_757 . . . ? C10 Rh1 P1 C1 -83.72(15) . . . . ? Cl1 Rh1 P1 C1 93.40(7) 3_757 . . . ? Cl1 Rh1 P1 C1 -86.60(7) . . . . ? C10 Rh1 P1 C4 -20.20(15) 3_757 . . . ? C10 Rh1 P1 C4 159.80(15) . . . . ? Cl1 Rh1 P1 C4 -23.08(7) 3_757 . . . ? Cl1 Rh1 P1 C4 156.92(7) . . . . ? C10 Rh1 P1 C7 -146.81(15) 3_757 . . . ? C10 Rh1 P1 C7 33.19(15) . . . . ? P1 Rh1 P1 C7 56(100) 3_757 . . . ? Cl1 Rh1 P1 C7 -149.70(7) 3_757 . . . ? Cl1 Rh1 P1 C7 30.30(7) . . . . ? C4 P1 C1 C2 178.69(12) . . . . ? C7 P1 C1 C2 -65.82(14) . . . . ? Rh1 P1 C1 C2 56.61(13) . . . . ? C4 P1 C1 C3 56.27(14) . . . . ? C7 P1 C1 C3 171.76(13) . . . . ? Rh1 P1 C1 C3 -65.81(14) . . . . ? C1 P1 C4 C6 -179.93(13) . . . . ? C7 P1 C4 C6 69.09(15) . . . . ? Rh1 P1 C4 C6 -59.10(14) . . . . ? C1 P1 C4 C5 49.85(16) . . . . ? C7 P1 C4 C5 -61.12(17) . . . . ? Rh1 P1 C4 C5 170.68(13) . . . . ? C1 P1 C7 C8 -53.84(16) . . . . ? C4 P1 C7 C8 56.97(16) . . . . ? Rh1 P1 C7 C8 -174.92(12) . . . . ? C1 P1 C7 C9 176.86(14) . . . . ? C4 P1 C7 C9 -72.33(16) . . . . ? Rh1 P1 C7 C9 55.79(15) . . . . ? Rh1 Cl1 C10 O10 -38(7) . . . . ? P1 Rh1 C10 Cl1 -79(3) . . . . ? P1 Rh1 C10 Cl1 101(3) 3_757 . . . ? P1 Rh1 C10 O10 -71.1(18) . . . . ? P1 Rh1 C10 O10 108.9(18) 3_757 . . . ? Cl1 Rh1 C10 O10 -172.2(16) 3_757 . . . ? Cl1 Rh1 C10 O10 7.8(16) . . . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 1.125 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.114