Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name '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_section_title ; Methanol carbonylation catalysed by rhodium complexes of bis-(ditertiarybutylphosphinomethyl)benzene. ; loop_ _publ_author_name D.Cole-Hamilton G.R.Eastham C.Jimenez-Rodriguez P.Pogorzelec ; A.Slawin ; # Attachment 'Rh2Cl2_DTBPMB_COD2.cif' data_Rh2Cl2(DTBPMB)COD2 _database_code_depnum_ccdc_archive 'CCDC 635431' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H68 Cl2 P2 Rh2' _chemical_formula_weight 887.60 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 Monoclinic _symmetry_space_group_name_H-M C2/c 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' '-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 32.30(2) _cell_length_b 9.811(6) _cell_length_c 14.041(10) _cell_angle_alpha 90.00 _cell_angle_beta 111.228(16) _cell_angle_gamma 90.00 _cell_volume 4148(5) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 6707 _cell_measurement_theta_min 2.1827 _cell_measurement_theta_max 26.3714 _exptl_crystal_description Platelet _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.1000 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.0100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 1.028 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4025 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 0.83 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11966 _diffrn_reflns_av_R_equivalents 0.1008 _diffrn_reflns_av_sigmaI/netI 0.1088 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3729 _reflns_number_gt 2763 _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^)+(0.0783P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3729 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0933 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.1669 _refine_ls_wR_factor_gt 0.1517 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.008 _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 0.339852(14) -0.11778(5) 0.64018(4) 0.0191(2) Uani 1 1 d . . . Cl1 Cl 0.36129(5) -0.17713(19) 0.49903(13) 0.0273(4) Uani 1 1 d . . . P1 P 0.40179(5) -0.24961(17) 0.75203(13) 0.0185(4) Uani 1 1 d . . . C1 C 0.3252(2) -0.0028(7) 0.7560(5) 0.0238(15) Uani 1 1 d . . . H1A H 0.3559 -0.0082 0.7964 0.029 Uiso 1 1 calc R . . C2 C 0.2999(2) -0.1243(7) 0.7339(6) 0.0271(17) Uani 1 1 d . . . H2A H 0.3147 -0.2067 0.7626 0.033 Uiso 1 1 calc R . . C3 C 0.2501(2) -0.1329(7) 0.6666(6) 0.0287(17) Uani 1 1 d . . . H3A H 0.2421 -0.2298 0.6502 0.034 Uiso 1 1 calc R . . H3B H 0.2324 -0.0983 0.7062 0.034 Uiso 1 1 calc R . . C4 C 0.2375(2) -0.0526(8) 0.5667(6) 0.0307(18) Uani 1 1 d . . . H4A H 0.2114 -0.0959 0.5146 0.037 Uiso 1 1 calc R . . H4B H 0.2290 0.0413 0.5780 0.037 Uiso 1 1 calc R . . C5 C 0.27557(19) -0.0465(7) 0.5268(5) 0.0261(16) Uani 1 1 d . . . H5A H 0.2782 -0.1192 0.4846 0.031 Uiso 1 1 calc R . . C6 C 0.3068(2) 0.0582(7) 0.5477(6) 0.0285(17) Uani 1 1 d . . . H6A H 0.3281 0.0535 0.5157 0.034 Uiso 1 1 calc R . . C7 C 0.3096(2) 0.1766(8) 0.6158(6) 0.0325(18) Uani 1 1 d . . . H7A H 0.2858 0.2423 0.5797 0.039 Uiso 1 1 calc R . . H7B H 0.3385 0.2229 0.6302 0.039 Uiso 1 1 calc R . . C8 C 0.3051(2) 0.1370(7) 0.7177(6) 0.0284(17) Uani 1 1 d . . . H8A H 0.3201 0.2067 0.7698 0.034 Uiso 1 1 calc R . . H8B H 0.2733 0.1364 0.7088 0.034 Uiso 1 1 calc R . . C9 C 0.3874(2) -0.4408(7) 0.7361(6) 0.0275(16) Uani 1 1 d . . . C10 C 0.4173(2) -0.5368(7) 0.8156(6) 0.0360(19) Uani 1 1 d . . . H10A H 0.4065 -0.6305 0.7991 0.054 Uiso 1 1 calc R . . H10B H 0.4170 -0.5122 0.8830 0.054 Uiso 1 1 calc R . . H10C H 0.4476 -0.5301 0.8161 0.054 Uiso 1 1 calc R . . C11 C 0.3385(2) -0.4567(7) 0.7351(6) 0.0299(17) Uani 1 1 d . . . H11A H 0.3300 -0.5532 0.7275 0.045 Uiso 1 1 calc R . . H11B H 0.3179 -0.4047 0.6779 0.045 Uiso 1 1 calc R . . H11C H 0.3372 -0.4220 0.7995 0.045 Uiso 1 1 calc R . . C12 C 0.3868(2) -0.4876(7) 0.6304(6) 0.0276(16) Uani 1 1 d . . . H12A H 0.3796 -0.5849 0.6213 0.041 Uiso 1 1 calc R . . H12B H 0.4161 -0.4720 0.6264 0.041 Uiso 1 1 calc R . . H12C H 0.3644 -0.4354 0.5766 0.041 Uiso 1 1 calc R . . C13 C 0.4285(2) -0.2064(7) 0.8931(5) 0.0232(15) Uani 1 1 d . . . C14 C 0.4396(2) -0.0507(7) 0.9069(5) 0.0240(15) Uani 1 1 d . . . H14A H 0.4535 -0.0296 0.9799 0.036 Uiso 1 1 calc R . . H14B H 0.4122 0.0022 0.8771 0.036 Uiso 1 1 calc R . . H14C H 0.4602 -0.0273 0.8724 0.036 Uiso 1 1 calc R . . C15 C 0.4736(2) -0.2803(8) 0.9524(5) 0.0280(16) Uani 1 1 d . . . H15A H 0.4847 -0.2508 1.0239 0.042 Uiso 1 1 calc R . . H15B H 0.4953 -0.2571 0.9212 0.042 Uiso 1 1 calc R . . H15C H 0.4688 -0.3791 0.9491 0.042 Uiso 1 1 calc R . . C16 C 0.3956(2) -0.2387(7) 0.9477(5) 0.0258(16) Uani 1 1 d . . . H16A H 0.4094 -0.2159 1.0204 0.039 Uiso 1 1 calc R . . H16B H 0.3881 -0.3359 0.9404 0.039 Uiso 1 1 calc R . . H16C H 0.3685 -0.1847 0.9169 0.039 Uiso 1 1 calc R . . C17 C 0.44917(19) -0.2466(7) 0.7052(5) 0.0200(14) Uani 1 1 d . . . H17A H 0.4694 -0.3231 0.7375 0.024 Uiso 1 1 calc R . . H17B H 0.4372 -0.2632 0.6306 0.024 Uiso 1 1 calc R . . C18 C 0.4766(2) -0.1141(7) 0.7259(5) 0.0200(15) Uani 1 1 d . . . C19 C 0.45456(19) 0.0116(7) 0.6979(5) 0.0214(15) Uani 1 1 d . . . H19A H 0.4234 0.0131 0.6620 0.026 Uiso 1 1 calc R . . C20 C 0.4776(2) 0.1323(7) 0.7219(5) 0.0213(15) Uani 1 1 d . . . H20A H 0.4625 0.2162 0.6994 0.026 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 0.0161(3) 0.0210(3) 0.0245(3) -0.0014(2) 0.0127(2) -0.0018(2) Cl1 0.0243(8) 0.0382(11) 0.0252(9) -0.0021(8) 0.0158(7) -0.0008(7) P1 0.0173(8) 0.0188(9) 0.0252(10) -0.0023(7) 0.0146(7) -0.0011(6) C1 0.024(3) 0.026(4) 0.027(4) -0.005(3) 0.016(3) -0.001(3) C2 0.026(4) 0.022(4) 0.041(4) -0.009(3) 0.021(3) 0.000(3) C3 0.017(3) 0.028(4) 0.049(5) -0.014(4) 0.022(3) -0.006(3) C4 0.015(3) 0.040(5) 0.038(5) -0.006(4) 0.010(3) -0.002(3) C5 0.013(3) 0.029(4) 0.032(4) -0.004(3) 0.003(3) -0.001(3) C6 0.021(3) 0.030(4) 0.038(4) 0.006(3) 0.014(3) 0.008(3) C7 0.028(4) 0.024(4) 0.041(5) 0.004(3) 0.008(3) 0.000(3) C8 0.025(4) 0.022(4) 0.039(5) -0.001(3) 0.014(3) -0.001(3) C9 0.025(4) 0.024(4) 0.044(5) -0.005(3) 0.024(3) -0.006(3) C10 0.034(4) 0.025(4) 0.053(5) 0.001(4) 0.020(4) -0.002(3) C11 0.036(4) 0.023(4) 0.049(5) -0.011(3) 0.037(4) -0.011(3) C12 0.029(4) 0.020(4) 0.043(4) -0.012(3) 0.024(3) -0.009(3) C13 0.024(3) 0.026(4) 0.026(4) 0.001(3) 0.016(3) 0.003(3) C14 0.022(3) 0.030(4) 0.024(4) -0.005(3) 0.014(3) -0.004(3) C15 0.022(3) 0.039(4) 0.024(4) 0.004(3) 0.009(3) -0.001(3) C16 0.029(4) 0.031(4) 0.023(4) 0.002(3) 0.017(3) 0.003(3) C17 0.022(3) 0.025(4) 0.022(4) -0.002(3) 0.018(3) -0.001(3) C18 0.014(3) 0.032(4) 0.020(3) -0.001(3) 0.013(3) -0.003(3) C19 0.014(3) 0.028(4) 0.027(4) 0.005(3) 0.014(3) 0.002(3) C20 0.025(3) 0.020(4) 0.024(4) 0.001(3) 0.015(3) 0.006(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 C2 2.151(7) . ? Rh1 C1 2.168(7) . ? Rh1 C6 2.192(7) . ? Rh1 C5 2.223(6) . ? Rh1 Cl1 2.396(2) . ? Rh1 P1 2.422(2) . ? P1 C17 1.871(6) . ? P1 C13 1.900(7) . ? P1 C9 1.926(7) . ? C1 C2 1.414(9) . ? C1 C8 1.529(9) . ? C2 C3 1.546(9) . ? C3 C4 1.530(11) . ? C4 C5 1.526(9) . ? C5 C6 1.394(9) . ? C6 C7 1.486(11) . ? C7 C8 1.540(11) . ? C9 C10 1.511(10) . ? C9 C12 1.548(10) . ? C9 C11 1.583(8) . ? C13 C16 1.552(9) . ? C13 C14 1.565(10) . ? C13 C15 1.567(9) . ? C17 C18 1.540(9) . ? C18 C19 1.407(9) . ? C18 C18 1.416(12) 2_656 ? C19 C20 1.374(9) . ? C20 C20 1.374(13) 2_656 ? 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 C2 Rh1 C1 38.2(2) . . ? C2 Rh1 C6 96.6(3) . . ? C1 Rh1 C6 80.9(3) . . ? C2 Rh1 C5 80.6(3) . . ? C1 Rh1 C5 88.4(3) . . ? C6 Rh1 C5 36.8(3) . . ? C2 Rh1 Cl1 156.30(19) . . ? C1 Rh1 Cl1 162.58(19) . . ? C6 Rh1 Cl1 85.8(2) . . ? C5 Rh1 Cl1 87.6(2) . . ? C2 Rh1 P1 97.2(2) . . ? C1 Rh1 P1 98.34(19) . . ? C6 Rh1 P1 156.30(18) . . ? C5 Rh1 P1 166.05(19) . . ? Cl1 Rh1 P1 89.33(7) . . ? C17 P1 C13 104.0(3) . . ? C17 P1 C9 99.7(3) . . ? C13 P1 C9 109.7(3) . . ? C17 P1 Rh1 110.6(2) . . ? C13 P1 Rh1 120.9(2) . . ? C9 P1 Rh1 109.7(2) . . ? C2 C1 C8 122.8(6) . . ? C2 C1 Rh1 70.2(4) . . ? C8 C1 Rh1 112.5(5) . . ? C1 C2 C3 124.7(6) . . ? C1 C2 Rh1 71.5(4) . . ? C3 C2 Rh1 110.4(5) . . ? C4 C3 C2 113.9(6) . . ? C5 C4 C3 112.0(6) . . ? C6 C5 C4 124.7(7) . . ? C6 C5 Rh1 70.4(4) . . ? C4 C5 Rh1 113.1(5) . . ? C5 C6 C7 125.6(7) . . ? C5 C6 Rh1 72.8(4) . . ? C7 C6 Rh1 109.4(5) . . ? C6 C7 C8 113.4(6) . . ? C1 C8 C7 112.5(6) . . ? C10 C9 C12 107.8(6) . . ? C10 C9 C11 108.3(6) . . ? C12 C9 C11 107.3(5) . . ? C10 C9 P1 117.3(5) . . ? C12 C9 P1 108.5(5) . . ? C11 C9 P1 107.2(4) . . ? C16 C13 C14 107.8(5) . . ? C16 C13 C15 108.2(5) . . ? C14 C13 C15 105.0(5) . . ? C16 C13 P1 109.6(4) . . ? C14 C13 P1 110.1(5) . . ? C15 C13 P1 115.8(5) . . ? C18 C17 P1 115.8(4) . . ? C19 C18 C18 118.6(4) . 2_656 ? C19 C18 C17 119.3(5) . . ? C18 C18 C17 122.1(3) 2_656 . ? C20 C19 C18 120.8(6) . . ? C20 C20 C19 120.3(4) 2_656 . ? 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 Rh1 P1 C17 -171.7(3) . . . . ? C1 Rh1 P1 C17 -133.1(3) . . . . ? C6 Rh1 P1 C17 -46.6(6) . . . . ? C5 Rh1 P1 C17 108.6(8) . . . . ? Cl1 Rh1 P1 C17 31.2(2) . . . . ? C2 Rh1 P1 C13 -49.9(3) . . . . ? C1 Rh1 P1 C13 -11.3(3) . . . . ? C6 Rh1 P1 C13 75.1(6) . . . . ? C5 Rh1 P1 C13 -129.7(8) . . . . ? Cl1 Rh1 P1 C13 153.0(2) . . . . ? C2 Rh1 P1 C9 79.3(3) . . . . ? C1 Rh1 P1 C9 117.9(3) . . . . ? C6 Rh1 P1 C9 -155.7(6) . . . . ? C5 Rh1 P1 C9 -0.5(9) . . . . ? Cl1 Rh1 P1 C9 -77.8(2) . . . . ? C6 Rh1 C1 C2 113.0(4) . . . . ? C5 Rh1 C1 C2 76.7(4) . . . . ? Cl1 Rh1 C1 C2 153.7(5) . . . . ? P1 Rh1 C1 C2 -91.0(4) . . . . ? C2 Rh1 C1 C8 -118.3(6) . . . . ? C6 Rh1 C1 C8 -5.4(4) . . . . ? C5 Rh1 C1 C8 -41.6(5) . . . . ? Cl1 Rh1 C1 C8 35.3(9) . . . . ? P1 Rh1 C1 C8 150.7(4) . . . . ? C8 C1 C2 C3 2.1(11) . . . . ? Rh1 C1 C2 C3 -102.5(7) . . . . ? C8 C1 C2 Rh1 104.6(6) . . . . ? C6 Rh1 C2 C1 -66.2(4) . . . . ? C5 Rh1 C2 C1 -99.5(4) . . . . ? Cl1 Rh1 C2 C1 -160.7(4) . . . . ? P1 Rh1 C2 C1 94.4(4) . . . . ? C1 Rh1 C2 C3 121.1(7) . . . . ? C6 Rh1 C2 C3 54.9(5) . . . . ? C5 Rh1 C2 C3 21.6(5) . . . . ? Cl1 Rh1 C2 C3 -39.6(8) . . . . ? P1 Rh1 C2 C3 -144.5(4) . . . . ? C1 C2 C3 C4 45.8(10) . . . . ? Rh1 C2 C3 C4 -35.4(7) . . . . ? C2 C3 C4 C5 30.8(8) . . . . ? C3 C4 C5 C6 -93.1(8) . . . . ? C3 C4 C5 Rh1 -11.6(7) . . . . ? C2 Rh1 C5 C6 114.5(5) . . . . ? C1 Rh1 C5 C6 76.9(5) . . . . ? Cl1 Rh1 C5 C6 -86.1(4) . . . . ? P1 Rh1 C5 C6 -163.7(7) . . . . ? C2 Rh1 C5 C4 -5.8(5) . . . . ? C1 Rh1 C5 C4 -43.4(5) . . . . ? C6 Rh1 C5 C4 -120.3(7) . . . . ? Cl1 Rh1 C5 C4 153.6(5) . . . . ? P1 Rh1 C5 C4 76.0(10) . . . . ? C4 C5 C6 C7 3.2(11) . . . . ? Rh1 C5 C6 C7 -101.8(7) . . . . ? C4 C5 C6 Rh1 105.1(7) . . . . ? C2 Rh1 C6 C5 -64.6(5) . . . . ? C1 Rh1 C6 C5 -99.6(5) . . . . ? Cl1 Rh1 C6 C5 91.7(4) . . . . ? P1 Rh1 C6 C5 170.3(4) . . . . ? C2 Rh1 C6 C7 57.9(5) . . . . ? C1 Rh1 C6 C7 22.9(5) . . . . ? C5 Rh1 C6 C7 122.5(7) . . . . ? Cl1 Rh1 C6 C7 -145.8(5) . . . . ? P1 Rh1 C6 C7 -67.2(7) . . . . ? C5 C6 C7 C8 45.3(9) . . . . ? Rh1 C6 C7 C8 -37.0(7) . . . . ? C2 C1 C8 C7 -93.1(8) . . . . ? Rh1 C1 C8 C7 -12.8(7) . . . . ? C6 C7 C8 C1 33.5(8) . . . . ? C17 P1 C9 C10 77.2(6) . . . . ? C13 P1 C9 C10 -31.5(6) . . . . ? Rh1 P1 C9 C10 -166.6(5) . . . . ? C17 P1 C9 C12 -45.2(5) . . . . ? C13 P1 C9 C12 -153.9(4) . . . . ? Rh1 P1 C9 C12 71.0(4) . . . . ? C17 P1 C9 C11 -160.8(5) . . . . ? C13 P1 C9 C11 90.5(5) . . . . ? Rh1 P1 C9 C11 -44.6(5) . . . . ? C17 P1 C13 C16 -166.5(4) . . . . ? C9 P1 C13 C16 -60.6(5) . . . . ? Rh1 P1 C13 C16 68.5(5) . . . . ? C17 P1 C13 C14 75.1(5) . . . . ? C9 P1 C13 C14 -179.0(4) . . . . ? Rh1 P1 C13 C14 -49.9(5) . . . . ? C17 P1 C13 C15 -43.8(6) . . . . ? C9 P1 C13 C15 62.1(5) . . . . ? Rh1 P1 C13 C15 -168.7(4) . . . . ? C13 P1 C17 C18 -54.9(5) . . . . ? C9 P1 C17 C18 -168.2(5) . . . . ? Rh1 P1 C17 C18 76.4(5) . . . . ? P1 C17 C18 C19 -50.9(8) . . . . ? P1 C17 C18 C18 127.9(8) . . . 2_656 ? C18 C18 C19 C20 -3.6(11) 2_656 . . . ? C17 C18 C19 C20 175.2(6) . . . . ? C18 C19 C20 C20 -3.2(12) . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.142 _refine_diff_density_min -1.002 _refine_diff_density_rms 0.176 # Attachment 'Rh_DTBPMP__CO_Cl_.cif' data_Rh(DTBPMP)(CO)Cl _database_code_depnum_ccdc_archive 'CCDC 635432' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H44 Cl O P2 Rh' _chemical_formula_weight 560.90 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.476(3) _cell_length_b 10.474(4) _cell_length_c 16.257(6) _cell_angle_alpha 77.071(7) _cell_angle_beta 75.674(7) _cell_angle_gamma 74.635(6) _cell_volume 1329.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 161 _cell_measurement_theta_min 12 _cell_measurement_theta_max 28 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max .14 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 0.878 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.589335 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _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 0.83 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8051 _diffrn_reflns_av_R_equivalents 0.0682 _diffrn_reflns_av_sigmaI/netI 0.2520 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 25.53 _reflns_number_total 4797 _reflns_number_gt 2196 _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^)+(0.0419P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4797 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1202 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1076 _refine_ls_wR_factor_gt 0.0971 _refine_ls_goodness_of_fit_ref 0.764 _refine_ls_restrained_S_all 0.764 _refine_ls_shift/su_max 0.005 _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 0.82656(7) -0.00149(6) 0.71269(4) 0.0254(2) Uani 1 1 d . . . Cl1 Cl 0.9230(2) 0.19157(18) 0.73522(16) 0.0647(8) Uani 1 1 d . . . P1 P 0.5395(2) 0.11872(17) 0.73506(11) 0.0224(5) Uani 1 1 d . . . C1 C 0.3740(7) 0.0273(7) 0.7484(4) 0.0288(18) Uani 1 1 d . . . H1A H 0.2667 0.0946 0.7514 0.035 Uiso 1 1 calc R . . H1B H 0.3932 -0.0100 0.6951 0.035 Uiso 1 1 calc R . . C2 C 0.3500(8) -0.0860(7) 0.8235(4) 0.0257(17) Uani 1 1 d . . . C3 C 0.4567(8) -0.2130(7) 0.8237(4) 0.0201(16) Uani 1 1 d . . . C4 C 0.4214(8) -0.3126(7) 0.8962(4) 0.0291(18) Uani 1 1 d . . . H4A H 0.4932 -0.3995 0.8975 0.035 Uiso 1 1 calc R . . C5 C 0.2907(9) -0.2922(8) 0.9646(4) 0.040(2) Uani 1 1 d . . . H5A H 0.2757 -0.3613 1.0128 0.048 Uiso 1 1 calc R . . C6 C 0.1821(9) -0.1684(8) 0.9611(5) 0.046(2) Uani 1 1 d . . . H6A H 0.0882 -0.1512 1.0065 0.055 Uiso 1 1 calc R . . C7 C 0.2118(9) -0.0686(7) 0.8903(5) 0.042(2) Uani 1 1 d . . . H7A H 0.1338 0.0155 0.8876 0.050 Uiso 1 1 calc R . . C8 C 0.5873(7) -0.2511(7) 0.7477(4) 0.0266(18) Uani 1 1 d . . . H8A H 0.5371 -0.2095 0.6964 0.032 Uiso 1 1 calc R . . H8B H 0.6041 -0.3495 0.7522 0.032 Uiso 1 1 calc R . . P2 P 0.7980(2) -0.21537(17) 0.72166(11) 0.0193(4) Uani 1 1 d . . . C9 C 0.5015(7) 0.2367(6) 0.6330(4) 0.0192(16) Uani 1 1 d . . . C10 C 0.3251(8) 0.3199(8) 0.6355(4) 0.053(3) Uani 1 1 d . . . H10A H 0.3178 0.3780 0.5796 0.079 Uiso 1 1 calc R . . H10B H 0.2958 0.3754 0.6806 0.079 Uiso 1 1 calc R . . H10C H 0.2475 0.2602 0.6480 0.079 Uiso 1 1 calc R . . C11 C 0.6211(11) 0.3334(8) 0.6082(5) 0.065(3) Uani 1 1 d . . . H11A H 0.6017 0.3944 0.5546 0.098 Uiso 1 1 calc R . . H11B H 0.7368 0.2816 0.5999 0.098 Uiso 1 1 calc R . . H11C H 0.6007 0.3857 0.6543 0.098 Uiso 1 1 calc R . . C12 C 0.5501(9) 0.1578(8) 0.5603(4) 0.047(2) Uani 1 1 d . . . H12A H 0.5313 0.2188 0.5066 0.071 Uiso 1 1 calc R . . H12B H 0.4822 0.0906 0.5728 0.071 Uiso 1 1 calc R . . H12C H 0.6684 0.1126 0.5541 0.071 Uiso 1 1 calc R . . C13 C 0.4680(9) 0.2106(7) 0.8296(4) 0.0302(18) Uani 1 1 d . . . C14 C 0.5351(9) 0.1106(7) 0.9035(4) 0.048(2) Uani 1 1 d . . . H14A H 0.5017 0.1518 0.9555 0.072 Uiso 1 1 calc R . . H14B H 0.6572 0.0853 0.8881 0.072 Uiso 1 1 calc R . . H14C H 0.4895 0.0302 0.9144 0.072 Uiso 1 1 calc R . . C15 C 0.2801(9) 0.2566(8) 0.8573(5) 0.060(3) Uani 1 1 d . . . H15A H 0.2552 0.3028 0.9068 0.089 Uiso 1 1 calc R . . H15B H 0.2292 0.1784 0.8736 0.089 Uiso 1 1 calc R . . H15C H 0.2347 0.3182 0.8095 0.089 Uiso 1 1 calc R . . C16 C 0.5365(11) 0.3375(8) 0.8162(5) 0.064(3) Uani 1 1 d . . . H16A H 0.4936 0.3797 0.8678 0.095 Uiso 1 1 calc R . . H16B H 0.5008 0.4007 0.7664 0.095 Uiso 1 1 calc R . . H16C H 0.6587 0.3128 0.8059 0.095 Uiso 1 1 calc R . . C17 C 0.9030(8) -0.3279(6) 0.8096(4) 0.0230(17) Uani 1 1 d . . . C18 C 0.8196(8) -0.2713(7) 0.8926(4) 0.036(2) Uani 1 1 d . . . H18A H 0.8709 -0.3276 0.9401 0.055 Uiso 1 1 calc R . . H18B H 0.7002 -0.2707 0.9056 0.055 Uiso 1 1 calc R . . H18C H 0.8342 -0.1794 0.8853 0.055 Uiso 1 1 calc R . . C19 C 0.8897(8) -0.4734(7) 0.8233(4) 0.0354(19) Uani 1 1 d . . . H19A H 0.9459 -0.5260 0.8700 0.053 Uiso 1 1 calc R . . H19B H 0.9427 -0.5101 0.7702 0.053 Uiso 1 1 calc R . . H19C H 0.7717 -0.4779 0.8385 0.053 Uiso 1 1 calc R . . C20 C 1.0899(7) -0.3281(7) 0.7949(4) 0.034(2) Uani 1 1 d . . . H20A H 1.1372 -0.3879 0.8428 0.051 Uiso 1 1 calc R . . H20B H 1.1025 -0.2368 0.7920 0.051 Uiso 1 1 calc R . . H20C H 1.1487 -0.3599 0.7408 0.051 Uiso 1 1 calc R . . C21 C 0.8768(8) -0.2885(7) 0.6177(4) 0.0258(17) Uani 1 1 d . . . C22 C 0.7994(9) -0.3998(7) 0.6131(4) 0.041(2) Uani 1 1 d . . . H22A H 0.8469 -0.4306 0.5576 0.061 Uiso 1 1 calc R . . H22B H 0.6784 -0.3665 0.6186 0.061 Uiso 1 1 calc R . . H22C H 0.8225 -0.4747 0.6600 0.061 Uiso 1 1 calc R . . C23 C 1.0660(7) -0.3401(7) 0.5987(4) 0.036(2) Uani 1 1 d . . . H23A H 1.1000 -0.3768 0.5450 0.054 Uiso 1 1 calc R . . H23B H 1.0991 -0.4107 0.6461 0.054 Uiso 1 1 calc R . . H23C H 1.1205 -0.2659 0.5928 0.054 Uiso 1 1 calc R . . C24 C 0.8292(8) -0.1709(7) 0.5444(4) 0.0343(19) Uani 1 1 d . . . H24A H 0.8663 -0.2030 0.4891 0.052 Uiso 1 1 calc R . . H24B H 0.8836 -0.0984 0.5428 0.052 Uiso 1 1 calc R . . H24C H 0.7078 -0.1372 0.5552 0.052 Uiso 1 1 calc R . . C25 C 1.0611(10) -0.0556(8) 0.6624(6) 0.031(2) Uani 1 1 d . . . O25 O 1.1731(7) -0.0685(6) 0.6339(4) 0.0437(17) 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 0.0234(3) 0.0166(3) 0.0401(4) -0.0068(3) -0.0100(3) -0.0057(2) Cl1 0.0107(10) 0.0135(11) 0.167(2) -0.0080(13) -0.0244(12) 0.0018(8) P1 0.0244(10) 0.0154(11) 0.0275(12) -0.0051(8) -0.0073(9) -0.0016(8) C1 0.020(4) 0.026(4) 0.039(5) -0.005(3) -0.010(3) 0.000(3) C2 0.021(4) 0.024(5) 0.032(5) -0.006(3) -0.001(3) -0.008(3) C3 0.023(4) 0.024(4) 0.014(4) -0.004(3) 0.004(3) -0.013(3) C4 0.034(4) 0.031(5) 0.025(5) 0.001(3) -0.008(4) -0.015(4) C5 0.052(5) 0.044(6) 0.027(5) -0.004(4) 0.001(4) -0.026(4) C6 0.045(5) 0.040(6) 0.050(6) -0.014(4) 0.018(4) -0.024(4) C7 0.042(5) 0.020(5) 0.056(6) -0.013(4) 0.015(4) -0.012(4) C8 0.024(4) 0.029(4) 0.034(5) -0.001(3) -0.018(4) -0.010(3) P2 0.0219(10) 0.0135(10) 0.0242(11) -0.0030(8) -0.0072(9) -0.0048(8) C9 0.021(4) 0.019(4) 0.017(4) -0.003(3) -0.003(3) -0.005(3) C10 0.045(5) 0.055(6) 0.035(5) 0.011(4) -0.010(4) 0.015(4) C11 0.103(7) 0.066(7) 0.047(6) 0.020(5) -0.026(5) -0.066(6) C12 0.056(5) 0.049(6) 0.027(5) -0.001(4) -0.011(4) 0.002(4) C13 0.048(5) 0.023(4) 0.026(4) -0.008(3) -0.010(4) -0.011(4) C14 0.088(6) 0.033(5) 0.024(5) -0.015(4) -0.021(4) 0.003(4) C15 0.055(6) 0.052(6) 0.057(6) -0.036(5) 0.004(5) 0.019(5) C16 0.115(8) 0.031(6) 0.051(6) -0.027(4) -0.001(5) -0.026(5) C17 0.023(4) 0.013(4) 0.031(4) -0.006(3) -0.002(3) 0.000(3) C18 0.030(4) 0.045(5) 0.028(5) -0.001(4) -0.011(4) 0.002(4) C19 0.037(4) 0.027(5) 0.043(5) 0.007(4) -0.015(4) -0.014(4) C20 0.030(4) 0.033(5) 0.035(5) 0.008(4) -0.018(4) -0.002(3) C21 0.031(4) 0.020(4) 0.025(4) -0.009(3) 0.006(3) -0.009(3) C22 0.054(5) 0.032(5) 0.038(5) -0.020(4) 0.004(4) -0.014(4) C23 0.029(4) 0.038(5) 0.038(5) -0.021(4) 0.009(4) -0.005(4) C24 0.057(5) 0.025(5) 0.020(4) -0.007(3) -0.006(4) -0.008(4) C25 0.053(6) 0.012(4) 0.033(6) -0.011(4) -0.026(5) 0.006(5) O25 0.075(5) 0.036(4) 0.035(4) -0.005(3) -0.018(4) -0.031(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 C25 1.936(8) . ? Rh1 P2 2.285(2) . ? Rh1 P1 2.4043(19) . ? Rh1 Cl1 2.499(2) . ? P1 C1 1.844(6) . ? P1 C9 1.876(6) . ? P1 C13 1.883(7) . ? C1 C2 1.515(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C7 1.389(8) . ? C2 C3 1.397(8) . ? C3 C4 1.417(8) . ? C3 C8 1.491(8) . ? C4 C5 1.371(8) . ? C4 H4A 0.9500 . ? C5 C6 1.376(9) . ? C5 H5A 0.9500 . ? C6 C7 1.392(9) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 P2 1.850(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? P2 C17 1.882(6) . ? P2 C21 1.908(7) . ? C9 C12 1.506(9) . ? C9 C10 1.514(8) . ? C9 C11 1.541(9) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.519(9) . ? C13 C14 1.525(8) . ? C13 C16 1.539(9) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C19 1.521(8) . ? C17 C18 1.528(8) . ? C17 C20 1.541(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.505(9) . ? C21 C23 1.527(8) . ? C21 C24 1.554(8) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 O25 0.936(7) . ? 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 C25 Rh1 P2 89.5(3) . . ? C25 Rh1 P1 161.9(3) . . ? P2 Rh1 P1 101.20(7) . . ? C25 Rh1 Cl1 81.4(3) . . ? P2 Rh1 Cl1 160.97(6) . . ? P1 Rh1 Cl1 92.09(7) . . ? C1 P1 C9 98.3(3) . . ? C1 P1 C13 103.1(3) . . ? C9 P1 C13 110.7(3) . . ? C1 P1 Rh1 119.2(2) . . ? C9 P1 Rh1 108.6(2) . . ? C13 P1 Rh1 115.6(2) . . ? C2 C1 P1 120.7(4) . . ? C2 C1 H1A 107.2 . . ? P1 C1 H1A 107.2 . . ? C2 C1 H1B 107.2 . . ? P1 C1 H1B 107.2 . . ? H1A C1 H1B 106.8 . . ? C7 C2 C3 118.4(6) . . ? C7 C2 C1 120.2(6) . . ? C3 C2 C1 121.1(6) . . ? C2 C3 C4 116.7(6) . . ? C2 C3 C8 123.0(6) . . ? C4 C3 C8 119.7(6) . . ? C5 C4 C3 124.4(7) . . ? C5 C4 H4A 117.8 . . ? C3 C4 H4A 117.8 . . ? C4 C5 C6 118.0(7) . . ? C4 C5 H5A 121.0 . . ? C6 C5 H5A 121.0 . . ? C5 C6 C7 119.1(7) . . ? C5 C6 H6A 120.5 . . ? C7 C6 H6A 120.5 . . ? C2 C7 C6 123.2(7) . . ? C2 C7 H7A 118.4 . . ? C6 C7 H7A 118.4 . . ? C3 C8 P2 124.0(5) . . ? C3 C8 H8A 106.3 . . ? P2 C8 H8A 106.3 . . ? C3 C8 H8B 106.3 . . ? P2 C8 H8B 106.3 . . ? H8A C8 H8B 106.4 . . ? C8 P2 C17 104.0(3) . . ? C8 P2 C21 97.1(3) . . ? C17 P2 C21 110.3(3) . . ? C8 P2 Rh1 119.8(2) . . ? C17 P2 Rh1 108.6(2) . . ? C21 P2 Rh1 116.0(2) . . ? C12 C9 C10 109.4(5) . . ? C12 C9 C11 104.6(6) . . ? C10 C9 C11 108.1(6) . . ? C12 C9 P1 108.9(5) . . ? C10 C9 P1 115.6(4) . . ? C11 C9 P1 109.6(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C14 108.6(6) . . ? C15 C13 C16 105.1(6) . . ? C14 C13 C16 108.2(6) . . ? C15 C13 P1 115.4(5) . . ? C14 C13 P1 104.9(5) . . ? C16 C13 P1 114.3(5) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 C18 109.1(5) . . ? C19 C17 C20 107.2(5) . . ? C18 C17 C20 106.1(5) . . ? C19 C17 P2 113.7(5) . . ? C18 C17 P2 107.0(4) . . ? C20 C17 P2 113.3(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C23 107.5(6) . . ? C22 C21 C24 106.9(5) . . ? C23 C21 C24 108.3(5) . . ? C22 C21 P2 115.2(4) . . ? C23 C21 P2 112.7(5) . . ? C24 C21 P2 105.9(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O25 C25 Rh1 171.5(10) . . ? 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 C25 Rh1 P1 C1 122.8(9) . . . . ? P2 Rh1 P1 C1 -2.4(2) . . . . ? Cl1 Rh1 P1 C1 -168.8(2) . . . . ? C25 Rh1 P1 C9 11.6(9) . . . . ? P2 Rh1 P1 C9 -113.6(2) . . . . ? Cl1 Rh1 P1 C9 80.1(2) . . . . ? C25 Rh1 P1 C13 -113.4(9) . . . . ? P2 Rh1 P1 C13 121.3(2) . . . . ? Cl1 Rh1 P1 C13 -45.0(2) . . . . ? C9 P1 C1 C2 179.0(5) . . . . ? C13 P1 C1 C2 -67.3(6) . . . . ? Rh1 P1 C1 C2 62.3(6) . . . . ? P1 C1 C2 C7 108.8(6) . . . . ? P1 C1 C2 C3 -77.0(8) . . . . ? C7 C2 C3 C4 -4.4(10) . . . . ? C1 C2 C3 C4 -178.8(6) . . . . ? C7 C2 C3 C8 167.1(6) . . . . ? C1 C2 C3 C8 -7.2(10) . . . . ? C2 C3 C4 C5 0.3(10) . . . . ? C8 C3 C4 C5 -171.5(6) . . . . ? C3 C4 C5 C6 2.9(11) . . . . ? C4 C5 C6 C7 -1.9(11) . . . . ? C3 C2 C7 C6 5.6(11) . . . . ? C1 C2 C7 C6 180.0(7) . . . . ? C5 C6 C7 C2 -2.3(12) . . . . ? C2 C3 C8 P2 84.3(7) . . . . ? C4 C3 C8 P2 -104.4(7) . . . . ? C3 C8 P2 C17 68.8(6) . . . . ? C3 C8 P2 C21 -178.2(5) . . . . ? C3 C8 P2 Rh1 -52.7(6) . . . . ? C25 Rh1 P2 C8 -168.7(3) . . . . ? P1 Rh1 P2 C8 -3.4(2) . . . . ? Cl1 Rh1 P2 C8 130.1(3) . . . . ? C25 Rh1 P2 C17 72.1(3) . . . . ? P1 Rh1 P2 C17 -122.6(2) . . . . ? Cl1 Rh1 P2 C17 10.9(3) . . . . ? C25 Rh1 P2 C21 -52.7(3) . . . . ? P1 Rh1 P2 C21 112.6(2) . . . . ? Cl1 Rh1 P2 C21 -113.9(3) . . . . ? C1 P1 C9 C12 -68.9(5) . . . . ? C13 P1 C9 C12 -176.4(5) . . . . ? Rh1 P1 C9 C12 55.7(5) . . . . ? C1 P1 C9 C10 54.7(6) . . . . ? C13 P1 C9 C10 -52.8(6) . . . . ? Rh1 P1 C9 C10 179.4(5) . . . . ? C1 P1 C9 C11 177.2(5) . . . . ? C13 P1 C9 C11 69.7(6) . . . . ? Rh1 P1 C9 C11 -58.2(5) . . . . ? C1 P1 C13 C15 -33.5(6) . . . . ? C9 P1 C13 C15 70.8(6) . . . . ? Rh1 P1 C13 C15 -165.3(4) . . . . ? C1 P1 C13 C14 86.1(5) . . . . ? C9 P1 C13 C14 -169.7(4) . . . . ? Rh1 P1 C13 C14 -45.8(5) . . . . ? C1 P1 C13 C16 -155.6(5) . . . . ? C9 P1 C13 C16 -51.3(6) . . . . ? Rh1 P1 C13 C16 72.6(5) . . . . ? C8 P2 C17 C19 50.1(5) . . . . ? C21 P2 C17 C19 -53.1(5) . . . . ? Rh1 P2 C17 C19 178.8(4) . . . . ? C8 P2 C17 C18 -70.5(5) . . . . ? C21 P2 C17 C18 -173.7(4) . . . . ? Rh1 P2 C17 C18 58.2(5) . . . . ? C8 P2 C17 C20 172.8(5) . . . . ? C21 P2 C17 C20 69.6(5) . . . . ? Rh1 P2 C17 C20 -58.4(5) . . . . ? C8 P2 C21 C22 -28.2(5) . . . . ? C17 P2 C21 C22 79.7(5) . . . . ? Rh1 P2 C21 C22 -156.4(4) . . . . ? C8 P2 C21 C23 -152.0(5) . . . . ? C17 P2 C21 C23 -44.1(5) . . . . ? Rh1 P2 C21 C23 79.8(5) . . . . ? C8 P2 C21 C24 89.8(5) . . . . ? C17 P2 C21 C24 -162.4(4) . . . . ? Rh1 P2 C21 C24 -38.5(5) . . . . ? P2 Rh1 C25 O25 151(7) . . . . ? P1 Rh1 C25 O25 24(8) . . . . ? Cl1 Rh1 C25 O25 -46(7) . . . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 25.53 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.046 _refine_diff_density_min -1.336 _refine_diff_density_rms 0.127 # Attachment 'Rh_DTBPMP__CO_I.cif' data_Rh(DTBPMP)(CO)I _database_code_depnum_ccdc_archive 'CCDC 635433' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H44 I O P2 Rh' _chemical_formula_weight 652.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2158(12) _cell_length_b 12.7064(13) _cell_length_c 19.6855(19) _cell_angle_alpha 102.122(2) _cell_angle_beta 106.790(2) _cell_angle_gamma 100.582(2) _cell_volume 2760.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 132 _cell_measurement_theta_min 12 _cell_measurement_theta_max 28 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max .1 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 1.867 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.746379 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _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 0.83 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16256 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.44 _reflns_number_total 9905 _reflns_number_gt 7581 _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^)+(0.0684P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9905 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1070 _refine_ls_wR_factor_gt 0.0997 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _refine_ls_shift/su_max 0.010 _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 1.50513(4) 0.16237(3) 0.23804(2) 0.01376(10) Uani 1 1 d . . . I1 I 1.73766(3) 0.26746(3) 0.313956(18) 0.02012(10) Uani 1 1 d . . . P1 P 1.44231(12) 0.19512(11) 0.34600(7) 0.0142(3) Uani 1 1 d . . . C1 C 1.3018(5) 0.1046(4) 0.3427(3) 0.0174(11) Uani 1 1 d . . . H1A H 1.3150 0.0296 0.3404 0.021 Uiso 1 1 calc R . . H1B H 1.2933 0.1322 0.3914 0.021 Uiso 1 1 calc R . . C2 C 1.1820(5) 0.0870(4) 0.2856(3) 0.0169(11) Uani 1 1 d . . . C3 C 1.1466(5) 0.0135(4) 0.2145(3) 0.0168(11) Uani 1 1 d . . . C4 C 1.0270(5) -0.0144(5) 0.1696(3) 0.0246(12) Uani 1 1 d . . . H4A H 1.0020 -0.0665 0.1223 0.029 Uiso 1 1 calc R . . C5 C 0.9441(5) 0.0313(5) 0.1919(3) 0.0282(13) Uani 1 1 d . . . H5A H 0.8639 0.0117 0.1602 0.034 Uiso 1 1 calc R . . C6 C 0.9804(5) 0.1069(5) 0.2619(3) 0.0285(13) Uani 1 1 d . . . H6A H 0.9256 0.1405 0.2781 0.034 Uiso 1 1 calc R . . C7 C 1.0965(5) 0.1320(4) 0.3072(3) 0.0228(12) Uani 1 1 d . . . H7A H 1.1199 0.1819 0.3552 0.027 Uiso 1 1 calc R . . C8 C 1.2300(5) -0.0445(4) 0.1883(3) 0.0182(11) Uani 1 1 d . . . H8A H 1.1800 -0.1114 0.1475 0.022 Uiso 1 1 calc R . . H8B H 1.2721 -0.0718 0.2293 0.022 Uiso 1 1 calc R . . P2 P 1.34461(12) 0.02451(11) 0.15569(7) 0.0158(3) Uani 1 1 d . . . C9 C 1.5415(5) 0.1746(5) 0.4353(3) 0.0213(12) Uani 1 1 d . . . C10 C 1.4776(5) 0.1498(5) 0.4896(3) 0.0278(13) Uani 1 1 d . . . H10A H 1.5341 0.1403 0.5332 0.042 Uiso 1 1 calc R . . H10B H 1.4133 0.0813 0.4653 0.042 Uiso 1 1 calc R . . H10C H 1.4448 0.2120 0.5047 0.042 Uiso 1 1 calc R . . C11 C 1.6479(5) 0.2766(5) 0.4794(3) 0.0244(12) Uani 1 1 d . . . H11A H 1.6955 0.2620 0.5241 0.037 Uiso 1 1 calc R . . H11B H 1.6191 0.3422 0.4933 0.037 Uiso 1 1 calc R . . H11C H 1.6966 0.2904 0.4489 0.037 Uiso 1 1 calc R . . C12 C 1.5866(5) 0.0741(5) 0.4099(3) 0.0242(12) Uani 1 1 d . . . H12A H 1.6382 0.0589 0.4531 0.036 Uiso 1 1 calc R . . H12B H 1.6315 0.0901 0.3776 0.036 Uiso 1 1 calc R . . H12C H 1.5192 0.0088 0.3827 0.036 Uiso 1 1 calc R . . C13 C 1.4181(5) 0.3400(4) 0.3615(3) 0.0193(11) Uani 1 1 d . . . C14 C 1.3317(5) 0.3427(5) 0.2877(3) 0.0242(12) Uani 1 1 d . . . H14A H 1.3164 0.4165 0.2928 0.036 Uiso 1 1 calc R . . H14B H 1.2572 0.2860 0.2744 0.036 Uiso 1 1 calc R . . H14C H 1.3668 0.3274 0.2489 0.036 Uiso 1 1 calc R . . C15 C 1.3680(6) 0.3701(5) 0.4238(3) 0.0280(13) Uani 1 1 d . . . H15A H 1.3581 0.4459 0.4294 0.042 Uiso 1 1 calc R . . H15B H 1.4228 0.3663 0.4701 0.042 Uiso 1 1 calc R . . H15C H 1.2911 0.3174 0.4117 0.042 Uiso 1 1 calc R . . C16 C 1.5327(5) 0.4297(4) 0.3778(3) 0.0228(12) Uani 1 1 d . . . H16A H 1.5170 0.5035 0.3857 0.034 Uiso 1 1 calc R . . H16B H 1.5609 0.4158 0.3357 0.034 Uiso 1 1 calc R . . H16C H 1.5933 0.4271 0.4222 0.034 Uiso 1 1 calc R . . C17 C 1.2538(5) 0.0559(5) 0.0694(3) 0.0260(13) Uani 1 1 d . . . C18 C 1.2057(7) 0.1559(5) 0.0958(3) 0.0421(18) Uani 1 1 d . . . H18A H 1.1582 0.1746 0.0529 0.063 Uiso 1 1 calc R . . H18B H 1.2722 0.2204 0.1265 0.063 Uiso 1 1 calc R . . H18C H 1.1563 0.1360 0.1249 0.063 Uiso 1 1 calc R . . C19 C 1.1493(6) -0.0416(5) 0.0182(3) 0.0372(16) Uani 1 1 d . . . H19A H 1.1068 -0.0201 -0.0250 0.056 Uiso 1 1 calc R . . H19B H 1.0955 -0.0614 0.0447 0.056 Uiso 1 1 calc R . . H19C H 1.1784 -0.1059 0.0019 0.056 Uiso 1 1 calc R . . C20 C 1.3289(7) 0.0940(10) 0.0240(4) 0.084(4) Uani 1 1 d . . . H20A H 1.2780 0.1086 -0.0197 0.127 Uiso 1 1 calc R . . H20B H 1.3659 0.0355 0.0084 0.127 Uiso 1 1 calc R . . H20C H 1.3905 0.1624 0.0543 0.127 Uiso 1 1 calc R . . C21 C 1.4035(5) -0.1018(5) 0.1291(3) 0.0257(13) Uani 1 1 d . . . C22 C 1.3101(7) -0.2111(6) 0.0869(4) 0.064(3) Uani 1 1 d . . . H22A H 1.3489 -0.2703 0.0757 0.096 Uiso 1 1 calc R . . H22B H 1.2588 -0.2034 0.0407 0.096 Uiso 1 1 calc R . . H22C H 1.2624 -0.2302 0.1171 0.096 Uiso 1 1 calc R . . C23 C 1.4819(12) -0.0822(8) 0.0838(7) 0.129(6) Uani 1 1 d . . . H23A H 1.5108 -0.1482 0.0714 0.193 Uiso 1 1 calc R . . H23B H 1.5494 -0.0175 0.1124 0.193 Uiso 1 1 calc R . . H23C H 1.4366 -0.0681 0.0383 0.193 Uiso 1 1 calc R . . C24 C 1.4762(7) -0.1182(6) 0.2005(4) 0.054(2) Uani 1 1 d . . . H24A H 1.5088 -0.1822 0.1896 0.082 Uiso 1 1 calc R . . H24B H 1.4259 -0.1321 0.2301 0.082 Uiso 1 1 calc R . . H24C H 1.5412 -0.0511 0.2281 0.082 Uiso 1 1 calc R . . C25 C 1.5609(5) 0.1789(5) 0.1621(3) 0.0266(13) Uani 1 1 d . . . O25 O 1.6023(4) 0.1997(4) 0.1208(2) 0.0492(13) Uani 1 1 d . . . Rh31 Rh 2.02312(4) 0.70226(3) 0.29843(2) 0.01585(11) Uani 1 1 d . . . I31 I 2.24627(3) 0.71979(3) 0.29153(2) 0.03025(11) Uani 1 1 d . . . P31 P 1.92167(12) 0.54202(11) 0.18921(7) 0.0143(3) Uani 1 1 d . . . C31 C 1.7730(4) 0.4558(4) 0.1742(3) 0.0158(11) Uani 1 1 d . . . H31A H 1.7514 0.3968 0.1273 0.019 Uiso 1 1 calc R . . H31B H 1.7834 0.4177 0.2138 0.019 Uiso 1 1 calc R . . C32 C 1.6649(5) 0.4981(4) 0.1707(3) 0.0184(11) Uani 1 1 d . . . C33 C 1.6493(4) 0.5564(4) 0.2346(3) 0.0172(11) Uani 1 1 d . . . C34 C 1.5382(5) 0.5784(5) 0.2277(3) 0.0239(12) Uani 1 1 d . . . H34A H 1.5246 0.6146 0.2707 0.029 Uiso 1 1 calc R . . C35 C 1.4479(5) 0.5486(5) 0.1597(3) 0.0287(14) Uani 1 1 d . . . H35A H 1.3749 0.5669 0.1564 0.034 Uiso 1 1 calc R . . C36 C 1.4645(5) 0.4928(5) 0.0977(3) 0.0311(14) Uani 1 1 d . . . H36A H 1.4029 0.4718 0.0511 0.037 Uiso 1 1 calc R . . C37 C 1.5713(5) 0.4669(5) 0.1030(3) 0.0240(12) Uani 1 1 d . . . H37A H 1.5816 0.4270 0.0597 0.029 Uiso 1 1 calc R . . C38 C 1.7411(5) 0.5820(4) 0.3107(3) 0.0170(11) Uani 1 1 d . . . H38A H 1.7690 0.5139 0.3126 0.020 Uiso 1 1 calc R . . H38B H 1.6983 0.5910 0.3463 0.020 Uiso 1 1 calc R . . P32 P 1.87500(12) 0.70015(11) 0.34803(7) 0.0152(3) Uani 1 1 d . . . C39 C 1.9982(5) 0.4224(4) 0.1850(3) 0.0192(11) Uani 1 1 d . . . C40 C 1.9165(5) 0.3068(5) 0.1387(3) 0.0278(13) Uani 1 1 d . . . H40A H 1.9628 0.2514 0.1395 0.042 Uiso 1 1 calc R . . H40B H 1.8804 0.3082 0.0876 0.042 Uiso 1 1 calc R . . H40C H 1.8542 0.2869 0.1594 0.042 Uiso 1 1 calc R . . C41 C 2.1026(5) 0.4427(5) 0.1557(3) 0.0260(13) Uani 1 1 d . . . H41A H 2.1378 0.3793 0.1546 0.039 Uiso 1 1 calc R . . H41B H 2.1625 0.5109 0.1883 0.039 Uiso 1 1 calc R . . H41C H 2.0736 0.4508 0.1057 0.039 Uiso 1 1 calc R . . C42 C 2.0452(5) 0.4188(5) 0.2657(3) 0.0215(12) Uani 1 1 d . . . H42A H 2.0858 0.3593 0.2683 0.032 Uiso 1 1 calc R . . H42B H 1.9789 0.4042 0.2839 0.032 Uiso 1 1 calc R . . H42C H 2.1009 0.4905 0.2962 0.032 Uiso 1 1 calc R . . C43 C 1.8986(5) 0.5919(4) 0.1031(3) 0.0183(11) Uani 1 1 d . . . C44 C 1.8219(5) 0.6746(5) 0.1075(3) 0.0246(13) Uani 1 1 d . . . H44A H 1.8080 0.7022 0.0636 0.037 Uiso 1 1 calc R . . H44B H 1.8630 0.7374 0.1519 0.037 Uiso 1 1 calc R . . H44C H 1.7460 0.6370 0.1096 0.037 Uiso 1 1 calc R . . C45 C 1.8390(5) 0.4950(4) 0.0318(3) 0.0229(12) Uani 1 1 d . . . H45A H 1.8288 0.5243 -0.0112 0.034 Uiso 1 1 calc R . . H45B H 1.7614 0.4560 0.0311 0.034 Uiso 1 1 calc R . . H45C H 1.8889 0.4429 0.0302 0.034 Uiso 1 1 calc R . . C46 C 2.0164(5) 0.6569(5) 0.1014(3) 0.0240(12) Uani 1 1 d . . . H46A H 2.0021 0.6815 0.0564 0.036 Uiso 1 1 calc R . . H46B H 2.0705 0.6086 0.1020 0.036 Uiso 1 1 calc R . . H46C H 2.0519 0.7221 0.1448 0.036 Uiso 1 1 calc R . . C47 C 1.8120(5) 0.8265(4) 0.3529(3) 0.0218(12) Uani 1 1 d . . . C48 C 1.7575(5) 0.8279(5) 0.2726(3) 0.0287(14) Uani 1 1 d . . . H48A H 1.7233 0.8917 0.2715 0.043 Uiso 1 1 calc R . . H48B H 1.6954 0.7587 0.2451 0.043 Uiso 1 1 calc R . . H48C H 1.8192 0.8341 0.2499 0.043 Uiso 1 1 calc R . . C49 C 1.7211(6) 0.8235(6) 0.3922(4) 0.0420(17) Uani 1 1 d . . . H49A H 1.6920 0.8906 0.3933 0.063 Uiso 1 1 calc R . . H49B H 1.7582 0.8209 0.4429 0.063 Uiso 1 1 calc R . . H49C H 1.6546 0.7573 0.3657 0.063 Uiso 1 1 calc R . . C50 C 1.9073(6) 0.9381(5) 0.3905(3) 0.0329(15) Uani 1 1 d . . . H50A H 1.8693 0.9997 0.3916 0.049 Uiso 1 1 calc R . . H50B H 1.9618 0.9457 0.3627 0.049 Uiso 1 1 calc R . . H50C H 1.9515 0.9400 0.4411 0.049 Uiso 1 1 calc R . . C51 C 1.9364(5) 0.6775(4) 0.4439(3) 0.0193(11) Uani 1 1 d . . . C52 C 1.8414(5) 0.6275(5) 0.4735(3) 0.0274(13) Uani 1 1 d . . . H52A H 1.8797 0.6187 0.5223 0.041 Uiso 1 1 calc R . . H52B H 1.7940 0.5546 0.4395 0.041 Uiso 1 1 calc R . . H52C H 1.7898 0.6774 0.4775 0.041 Uiso 1 1 calc R . . C53 C 2.0142(6) 0.7860(5) 0.5027(3) 0.0296(14) Uani 1 1 d . . . H53A H 2.0433 0.7708 0.5505 0.044 Uiso 1 1 calc R . . H53B H 1.9673 0.8405 0.5064 0.044 Uiso 1 1 calc R . . H53C H 2.0815 0.8160 0.4886 0.044 Uiso 1 1 calc R . . C54 C 2.0113(5) 0.5953(5) 0.4361(3) 0.0234(12) Uani 1 1 d . . . H54A H 2.0446 0.5808 0.4838 0.035 Uiso 1 1 calc R . . H54B H 2.0757 0.6267 0.4200 0.035 Uiso 1 1 calc R . . H54C H 1.9616 0.5253 0.3993 0.035 Uiso 1 1 calc R . . C55 C 2.1146(7) 0.8395(5) 0.3684(3) 0.0289(14) Uani 1 1 d . . . O55 O 2.1697(4) 0.9175(4) 0.4050(2) 0.0370(11) 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 0.0101(2) 0.0166(2) 0.0132(2) 0.00407(15) 0.00241(16) 0.00283(16) I1 0.01135(19) 0.0263(2) 0.02152(18) 0.00835(14) 0.00303(14) 0.00419(15) P1 0.0100(7) 0.0185(7) 0.0128(6) 0.0054(5) 0.0016(5) 0.0031(5) C1 0.014(3) 0.019(3) 0.016(3) 0.005(2) 0.002(2) 0.001(2) C2 0.014(3) 0.018(3) 0.021(3) 0.010(2) 0.006(2) 0.003(2) C3 0.014(3) 0.017(3) 0.018(3) 0.008(2) 0.004(2) 0.002(2) C4 0.014(3) 0.035(3) 0.023(3) 0.012(2) 0.003(2) 0.004(3) C5 0.015(3) 0.045(4) 0.026(3) 0.016(3) 0.002(3) 0.010(3) C6 0.019(3) 0.031(3) 0.042(4) 0.016(3) 0.013(3) 0.013(3) C7 0.016(3) 0.024(3) 0.027(3) 0.006(2) 0.005(2) 0.004(2) C8 0.016(3) 0.017(3) 0.021(3) 0.004(2) 0.006(2) 0.001(2) P2 0.0108(7) 0.0196(7) 0.0137(6) 0.0028(5) 0.0015(5) 0.0021(6) C9 0.021(3) 0.029(3) 0.013(3) 0.010(2) 0.002(2) 0.006(2) C10 0.020(3) 0.043(4) 0.021(3) 0.016(3) 0.005(3) 0.007(3) C11 0.017(3) 0.037(3) 0.016(3) 0.008(2) 0.001(2) 0.004(3) C12 0.020(3) 0.028(3) 0.026(3) 0.013(2) 0.004(3) 0.008(3) C13 0.019(3) 0.018(3) 0.021(3) 0.006(2) 0.005(2) 0.006(2) C14 0.017(3) 0.023(3) 0.029(3) 0.007(2) 0.001(2) 0.005(2) C15 0.030(4) 0.023(3) 0.029(3) 0.000(2) 0.015(3) 0.004(3) C16 0.020(3) 0.020(3) 0.029(3) 0.008(2) 0.007(3) 0.007(2) C17 0.025(3) 0.037(3) 0.013(3) 0.007(2) 0.003(2) 0.007(3) C18 0.060(5) 0.030(4) 0.033(4) 0.016(3) 0.003(3) 0.018(3) C19 0.026(4) 0.038(4) 0.027(3) -0.001(3) -0.016(3) 0.013(3) C20 0.037(5) 0.194(11) 0.047(5) 0.083(6) 0.019(4) 0.026(6) C21 0.022(3) 0.027(3) 0.028(3) 0.004(2) 0.010(3) 0.007(3) C22 0.058(6) 0.026(4) 0.063(5) -0.020(3) -0.028(4) 0.019(4) C23 0.232(16) 0.066(6) 0.227(14) 0.082(8) 0.213(14) 0.103(9) C24 0.050(5) 0.060(5) 0.049(4) 0.000(4) -0.001(4) 0.049(4) C25 0.019(3) 0.033(3) 0.017(3) 0.003(2) 0.004(3) -0.009(3) O25 0.043(3) 0.059(3) 0.026(2) -0.005(2) 0.016(2) -0.021(2) Rh31 0.0112(2) 0.0195(2) 0.0148(2) 0.00633(16) 0.00149(17) 0.00207(17) I31 0.0145(2) 0.0460(3) 0.0264(2) 0.01100(17) 0.00344(16) 0.00343(17) P31 0.0094(7) 0.0187(7) 0.0135(6) 0.0043(5) 0.0017(5) 0.0041(5) C31 0.009(3) 0.016(3) 0.015(3) -0.001(2) -0.001(2) 0.000(2) C32 0.010(3) 0.022(3) 0.021(3) 0.009(2) 0.003(2) -0.002(2) C33 0.006(3) 0.020(3) 0.021(3) 0.006(2) -0.001(2) 0.001(2) C34 0.017(3) 0.027(3) 0.031(3) 0.010(2) 0.010(3) 0.008(2) C35 0.011(3) 0.040(4) 0.036(3) 0.017(3) 0.001(3) 0.014(3) C36 0.014(3) 0.045(4) 0.032(3) 0.017(3) 0.002(3) 0.006(3) C37 0.017(3) 0.033(3) 0.016(3) 0.006(2) -0.001(2) 0.005(3) C38 0.013(3) 0.021(3) 0.014(2) 0.003(2) 0.003(2) 0.002(2) P32 0.0138(7) 0.0167(7) 0.0133(6) 0.0041(5) 0.0021(5) 0.0039(6) C39 0.018(3) 0.022(3) 0.022(3) 0.006(2) 0.008(2) 0.012(2) C40 0.030(4) 0.025(3) 0.028(3) 0.004(2) 0.008(3) 0.014(3) C41 0.022(3) 0.036(3) 0.026(3) 0.011(3) 0.010(3) 0.016(3) C42 0.016(3) 0.029(3) 0.023(3) 0.014(2) 0.005(2) 0.009(2) C43 0.019(3) 0.023(3) 0.012(2) 0.006(2) 0.003(2) 0.006(2) C44 0.024(3) 0.033(3) 0.024(3) 0.017(3) 0.011(3) 0.011(3) C45 0.019(3) 0.025(3) 0.019(3) 0.007(2) 0.000(2) 0.003(2) C46 0.023(3) 0.030(3) 0.020(3) 0.010(2) 0.007(2) 0.004(3) C47 0.021(3) 0.020(3) 0.027(3) 0.007(2) 0.006(3) 0.014(2) C48 0.025(3) 0.022(3) 0.031(3) 0.008(2) -0.004(3) 0.006(3) C49 0.047(5) 0.038(4) 0.056(4) 0.014(3) 0.033(4) 0.022(3) C50 0.039(4) 0.020(3) 0.029(3) 0.005(3) -0.002(3) 0.005(3) C51 0.015(3) 0.025(3) 0.015(3) 0.006(2) 0.002(2) 0.004(2) C52 0.026(3) 0.035(3) 0.022(3) 0.010(3) 0.008(3) 0.005(3) C53 0.033(4) 0.026(3) 0.018(3) 0.003(2) -0.006(3) 0.004(3) C54 0.019(3) 0.030(3) 0.021(3) 0.014(2) 0.000(2) 0.007(3) C55 0.053(5) 0.027(3) 0.016(3) 0.013(3) 0.015(3) 0.020(3) O55 0.020(2) 0.045(3) 0.037(3) 0.021(2) 0.002(2) -0.012(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C25 1.847(5) . ? Rh1 P2 2.2915(14) . ? Rh1 P1 2.4426(13) . ? Rh1 I1 2.7205(6) . ? P1 C1 1.859(5) . ? P1 C13 1.894(5) . ? P1 C9 1.925(5) . ? C1 C2 1.510(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.403(7) . ? C2 C7 1.404(7) . ? C3 C4 1.405(8) . ? C3 C8 1.506(7) . ? C4 C5 1.387(8) . ? C4 H4A 0.9500 . ? C5 C6 1.397(8) . ? C5 H5A 0.9500 . ? C6 C7 1.375(8) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 P2 1.856(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? P2 C17 1.906(5) . ? P2 C21 1.912(6) . ? C9 C12 1.529(8) . ? C9 C11 1.542(8) . ? C9 C10 1.543(7) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.532(7) . ? C13 C16 1.537(8) . ? C13 C14 1.541(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C19 1.527(8) . ? C17 C20 1.539(9) . ? C17 C18 1.551(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C23 1.508(9) . ? C21 C24 1.509(8) . ? C21 C22 1.519(9) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 O25 1.125(7) . ? Rh31 C55 1.890(7) . ? Rh31 P32 2.2896(14) . ? Rh31 P31 2.4493(14) . ? Rh31 I31 2.7390(6) . ? P31 C31 1.847(5) . ? P31 C43 1.897(5) . ? P31 C39 1.924(5) . ? C31 C32 1.503(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C37 1.404(7) . ? C32 C33 1.404(7) . ? C33 C34 1.410(7) . ? C33 C38 1.515(7) . ? C34 C35 1.390(8) . ? C34 H34A 0.9500 . ? C35 C36 1.366(8) . ? C35 H35A 0.9500 . ? C36 C37 1.384(8) . ? C36 H36A 0.9500 . ? C37 H37A 0.9500 . ? C38 P32 1.847(5) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? P32 C47 1.900(5) . ? P32 C51 1.924(5) . ? C39 C40 1.536(8) . ? C39 C42 1.539(7) . ? C39 C41 1.547(7) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C46 1.535(8) . ? C43 C44 1.536(7) . ? C43 C45 1.539(7) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C49 1.526(8) . ? C47 C48 1.532(7) . ? C47 C50 1.539(8) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C54 1.522(7) . ? C51 C53 1.535(7) . ? C51 C52 1.538(8) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 O55 1.063(7) . ? 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 C25 Rh1 P2 89.87(17) . . ? C25 Rh1 P1 164.52(19) . . ? P2 Rh1 P1 100.28(5) . . ? C25 Rh1 I1 78.65(17) . . ? P2 Rh1 I1 157.42(4) . . ? P1 Rh1 I1 95.32(3) . . ? C1 P1 C13 104.3(2) . . ? C1 P1 C9 96.5(2) . . ? C13 P1 C9 111.6(2) . . ? C1 P1 Rh1 119.42(17) . . ? C13 P1 Rh1 106.63(16) . . ? C9 P1 Rh1 117.62(18) . . ? C2 C1 P1 124.8(4) . . ? C2 C1 H1A 106.1 . . ? P1 C1 H1A 106.1 . . ? C2 C1 H1B 106.1 . . ? P1 C1 H1B 106.1 . . ? H1A C1 H1B 106.3 . . ? C3 C2 C7 118.1(5) . . ? C3 C2 C1 122.2(5) . . ? C7 C2 C1 119.0(5) . . ? C2 C3 C4 118.5(5) . . ? C2 C3 C8 121.9(5) . . ? C4 C3 C8 119.3(5) . . ? C5 C4 C3 122.4(5) . . ? C5 C4 H4A 118.8 . . ? C3 C4 H4A 118.8 . . ? C4 C5 C6 118.8(5) . . ? C4 C5 H5A 120.6 . . ? C6 C5 H5A 120.6 . . ? C7 C6 C5 119.2(6) . . ? C7 C6 H6A 120.4 . . ? C5 C6 H6A 120.4 . . ? C6 C7 C2 122.8(5) . . ? C6 C7 H7A 118.6 . . ? C2 C7 H7A 118.6 . . ? C3 C8 P2 123.2(4) . . ? C3 C8 H8A 106.5 . . ? P2 C8 H8A 106.5 . . ? C3 C8 H8B 106.5 . . ? P2 C8 H8B 106.5 . . ? H8A C8 H8B 106.5 . . ? C8 P2 C17 103.3(3) . . ? C8 P2 C21 97.4(2) . . ? C17 P2 C21 110.4(3) . . ? C8 P2 Rh1 119.90(17) . . ? C17 P2 Rh1 117.94(19) . . ? C21 P2 Rh1 105.95(19) . . ? C12 C9 C11 109.3(5) . . ? C12 C9 C10 108.4(4) . . ? C11 C9 C10 106.4(4) . . ? C12 C9 P1 105.2(3) . . ? C11 C9 P1 112.6(3) . . ? C10 C9 P1 114.8(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C16 108.8(4) . . ? C15 C13 C14 110.3(5) . . ? C16 C13 C14 106.2(4) . . ? C15 C13 P1 113.3(4) . . ? C16 C13 P1 111.7(4) . . ? C14 C13 P1 106.3(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 C20 108.4(6) . . ? C19 C17 C18 108.7(5) . . ? C20 C17 C18 105.9(6) . . ? C19 C17 P2 113.7(4) . . ? C20 C17 P2 112.9(4) . . ? C18 C17 P2 107.0(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C23 C21 C24 108.7(7) . . ? C23 C21 C22 107.3(7) . . ? C24 C21 C22 106.7(6) . . ? C23 C21 P2 111.6(4) . . ? C24 C21 P2 106.5(4) . . ? C22 C21 P2 115.7(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O25 C25 Rh1 172.6(5) . . ? C55 Rh31 P32 91.1(2) . . ? C55 Rh31 P31 167.41(17) . . ? P32 Rh31 P31 98.76(5) . . ? C55 Rh31 I31 75.8(2) . . ? P32 Rh31 I31 159.39(4) . . ? P31 Rh31 I31 96.70(4) . . ? C31 P31 C43 103.1(2) . . ? C31 P31 C39 96.5(2) . . ? C43 P31 C39 111.7(2) . . ? C31 P31 Rh31 121.05(16) . . ? C43 P31 Rh31 109.13(17) . . ? C39 P31 Rh31 114.38(17) . . ? C32 C31 P31 125.5(4) . . ? C32 C31 H31A 106.0 . . ? P31 C31 H31A 106.0 . . ? C32 C31 H31B 106.0 . . ? P31 C31 H31B 106.0 . . ? H31A C31 H31B 106.3 . . ? C37 C32 C33 119.0(5) . . ? C37 C32 C31 118.9(5) . . ? C33 C32 C31 121.6(4) . . ? C32 C33 C34 117.8(5) . . ? C32 C33 C38 122.0(5) . . ? C34 C33 C38 119.7(5) . . ? C35 C34 C33 121.9(5) . . ? C35 C34 H34A 119.1 . . ? C33 C34 H34A 119.1 . . ? C36 C35 C34 119.8(5) . . ? C36 C35 H35A 120.1 . . ? C34 C35 H35A 120.1 . . ? C35 C36 C37 119.7(5) . . ? C35 C36 H36A 120.1 . . ? C37 C36 H36A 120.1 . . ? C36 C37 C32 121.7(5) . . ? C36 C37 H37A 119.1 . . ? C32 C37 H37A 119.1 . . ? C33 C38 P32 123.6(4) . . ? C33 C38 H38A 106.4 . . ? P32 C38 H38A 106.4 . . ? C33 C38 H38B 106.4 . . ? P32 C38 H38B 106.4 . . ? H38A C38 H38B 106.5 . . ? C38 P32 C47 103.1(2) . . ? C38 P32 C51 97.5(2) . . ? C47 P32 C51 111.7(2) . . ? C38 P32 Rh31 120.65(17) . . ? C47 P32 Rh31 116.06(18) . . ? C51 P32 Rh31 106.44(17) . . ? C40 C39 C42 107.6(4) . . ? C40 C39 C41 106.9(4) . . ? C42 C39 C41 109.5(4) . . ? C40 C39 P31 115.1(4) . . ? C42 C39 P31 104.4(3) . . ? C41 C39 P31 113.1(4) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C46 C43 C44 106.5(4) . . ? C46 C43 C45 109.1(4) . . ? C44 C43 C45 110.7(4) . . ? C46 C43 P31 111.1(4) . . ? C44 C43 P31 107.1(3) . . ? C45 C43 P31 112.2(4) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C49 C47 C48 111.6(5) . . ? C49 C47 C50 108.0(5) . . ? C48 C47 C50 104.9(4) . . ? C49 C47 P32 113.0(4) . . ? C48 C47 P32 105.7(4) . . ? C50 C47 P32 113.4(4) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C47 C50 H50A 109.5 . . ? C47 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C47 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C54 C51 C53 109.1(5) . . ? C54 C51 C52 107.5(4) . . ? C53 C51 C52 106.9(4) . . ? C54 C51 P32 106.4(3) . . ? C53 C51 P32 112.2(4) . . ? C52 C51 P32 114.6(4) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O55 C55 Rh31 175.7(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 C25 Rh1 P1 C1 135.2(7) . . . . ? P2 Rh1 P1 C1 4.94(19) . . . . ? I1 Rh1 P1 C1 -158.66(19) . . . . ? C25 Rh1 P1 C13 17.6(7) . . . . ? P2 Rh1 P1 C13 -112.68(19) . . . . ? I1 Rh1 P1 C13 83.71(18) . . . . ? C25 Rh1 P1 C9 -108.6(7) . . . . ? P2 Rh1 P1 C9 121.1(2) . . . . ? I1 Rh1 P1 C9 -42.5(2) . . . . ? C13 P1 C1 C2 62.7(5) . . . . ? C9 P1 C1 C2 177.0(4) . . . . ? Rh1 P1 C1 C2 -56.2(5) . . . . ? P1 C1 C2 C3 79.7(6) . . . . ? P1 C1 C2 C7 -110.2(5) . . . . ? C7 C2 C3 C4 -2.2(7) . . . . ? C1 C2 C3 C4 168.0(5) . . . . ? C7 C2 C3 C8 -176.0(5) . . . . ? C1 C2 C3 C8 -5.8(7) . . . . ? C2 C3 C4 C5 2.6(8) . . . . ? C8 C3 C4 C5 176.6(5) . . . . ? C3 C4 C5 C6 -0.8(8) . . . . ? C4 C5 C6 C7 -1.3(8) . . . . ? C5 C6 C7 C2 1.6(8) . . . . ? C3 C2 C7 C6 0.1(8) . . . . ? C1 C2 C7 C6 -170.4(5) . . . . ? C2 C3 C8 P2 -79.0(6) . . . . ? C4 C3 C8 P2 107.2(5) . . . . ? C3 C8 P2 C17 -64.2(5) . . . . ? C3 C8 P2 C21 -177.3(4) . . . . ? C3 C8 P2 Rh1 69.4(5) . . . . ? C25 Rh1 P2 C8 -179.2(3) . . . . ? P1 Rh1 P2 C8 -11.0(2) . . . . ? I1 Rh1 P2 C8 122.0(2) . . . . ? C25 Rh1 P2 C17 -52.0(3) . . . . ? P1 Rh1 P2 C17 116.2(2) . . . . ? I1 Rh1 P2 C17 -110.8(2) . . . . ? C25 Rh1 P2 C21 72.2(3) . . . . ? P1 Rh1 P2 C21 -119.56(18) . . . . ? I1 Rh1 P2 C21 13.4(2) . . . . ? C1 P1 C9 C12 90.5(4) . . . . ? C13 P1 C9 C12 -161.3(4) . . . . ? Rh1 P1 C9 C12 -37.6(4) . . . . ? C1 P1 C9 C11 -150.5(4) . . . . ? C13 P1 C9 C11 -42.3(5) . . . . ? Rh1 P1 C9 C11 81.4(4) . . . . ? C1 P1 C9 C10 -28.5(4) . . . . ? C13 P1 C9 C10 79.7(4) . . . . ? Rh1 P1 C9 C10 -156.6(3) . . . . ? C1 P1 C13 C15 47.9(4) . . . . ? C9 P1 C13 C15 -55.2(5) . . . . ? Rh1 P1 C13 C15 175.1(4) . . . . ? C1 P1 C13 C16 171.2(4) . . . . ? C9 P1 C13 C16 68.1(4) . . . . ? Rh1 P1 C13 C16 -61.6(4) . . . . ? C1 P1 C13 C14 -73.4(4) . . . . ? C9 P1 C13 C14 -176.5(4) . . . . ? Rh1 P1 C13 C14 53.8(4) . . . . ? C8 P2 C17 C19 -45.4(5) . . . . ? C21 P2 C17 C19 57.8(5) . . . . ? Rh1 P2 C17 C19 179.8(4) . . . . ? C8 P2 C17 C20 -169.3(6) . . . . ? C21 P2 C17 C20 -66.1(6) . . . . ? Rh1 P2 C17 C20 55.9(6) . . . . ? C8 P2 C17 C18 74.6(5) . . . . ? C21 P2 C17 C18 177.8(4) . . . . ? Rh1 P2 C17 C18 -60.2(5) . . . . ? C8 P2 C21 C23 167.2(7) . . . . ? C17 P2 C21 C23 60.1(8) . . . . ? Rh1 P2 C21 C23 -68.7(7) . . . . ? C8 P2 C21 C24 -74.2(5) . . . . ? C17 P2 C21 C24 178.6(5) . . . . ? Rh1 P2 C21 C24 49.8(5) . . . . ? C8 P2 C21 C22 44.1(5) . . . . ? C17 P2 C21 C22 -63.1(6) . . . . ? Rh1 P2 C21 C22 168.2(5) . . . . ? P2 Rh1 C25 O25 162(5) . . . . ? P1 Rh1 C25 O25 31(5) . . . . ? I1 Rh1 C25 O25 -37(5) . . . . ? C55 Rh31 P31 C31 -146.0(9) . . . . ? P32 Rh31 P31 C31 -4.7(2) . . . . ? I31 Rh31 P31 C31 161.60(19) . . . . ? C55 Rh31 P31 C43 -26.7(9) . . . . ? P32 Rh31 P31 C43 114.54(18) . . . . ? I31 Rh31 P31 C43 -79.13(18) . . . . ? C55 Rh31 P31 C39 99.3(9) . . . . ? P32 Rh31 P31 C39 -119.45(18) . . . . ? I31 Rh31 P31 C39 46.87(18) . . . . ? C43 P31 C31 C32 -65.5(5) . . . . ? C39 P31 C31 C32 -179.7(4) . . . . ? Rh31 P31 C31 C32 56.7(5) . . . . ? P31 C31 C32 C37 111.8(5) . . . . ? P31 C31 C32 C33 -76.0(6) . . . . ? C37 C32 C33 C34 1.6(7) . . . . ? C31 C32 C33 C34 -170.7(5) . . . . ? C37 C32 C33 C38 173.4(5) . . . . ? C31 C32 C33 C38 1.1(8) . . . . ? C32 C33 C34 C35 -3.0(8) . . . . ? C38 C33 C34 C35 -175.0(5) . . . . ? C33 C34 C35 C36 2.4(9) . . . . ? C34 C35 C36 C37 -0.4(9) . . . . ? C35 C36 C37 C32 -1.0(9) . . . . ? C33 C32 C37 C36 0.3(8) . . . . ? C31 C32 C37 C36 172.8(5) . . . . ? C32 C33 C38 P32 81.6(6) . . . . ? C34 C33 C38 P32 -106.8(5) . . . . ? C33 C38 P32 C47 63.2(5) . . . . ? C33 C38 P32 C51 177.7(4) . . . . ? C33 C38 P32 Rh31 -68.2(5) . . . . ? C55 Rh31 P32 C38 -178.2(2) . . . . ? P31 Rh31 P32 C38 9.62(19) . . . . ? I31 Rh31 P32 C38 -128.6(2) . . . . ? C55 Rh31 P32 C47 56.2(3) . . . . ? P31 Rh31 P32 C47 -116.0(2) . . . . ? I31 Rh31 P32 C47 105.9(2) . . . . ? C55 Rh31 P32 C51 -68.8(2) . . . . ? P31 Rh31 P32 C51 119.01(18) . . . . ? I31 Rh31 P32 C51 -19.2(2) . . . . ? C31 P31 C39 C40 27.0(4) . . . . ? C43 P31 C39 C40 -79.9(4) . . . . ? Rh31 P31 C39 C40 155.5(3) . . . . ? C31 P31 C39 C42 -90.7(4) . . . . ? C43 P31 C39 C42 162.3(3) . . . . ? Rh31 P31 C39 C42 37.7(4) . . . . ? C31 P31 C39 C41 150.4(4) . . . . ? C43 P31 C39 C41 43.4(5) . . . . ? Rh31 P31 C39 C41 -81.2(4) . . . . ? C31 P31 C43 C46 -174.5(4) . . . . ? C39 P31 C43 C46 -71.9(4) . . . . ? Rh31 P31 C43 C46 55.6(4) . . . . ? C31 P31 C43 C44 69.5(4) . . . . ? C39 P31 C43 C44 172.1(4) . . . . ? Rh31 P31 C43 C44 -60.4(4) . . . . ? C31 P31 C43 C45 -52.1(4) . . . . ? C39 P31 C43 C45 50.5(5) . . . . ? Rh31 P31 C43 C45 178.0(3) . . . . ? C38 P32 C47 C49 50.6(5) . . . . ? C51 P32 C47 C49 -53.0(5) . . . . ? Rh31 P32 C47 C49 -175.3(4) . . . . ? C38 P32 C47 C48 -71.7(4) . . . . ? C51 P32 C47 C48 -175.3(4) . . . . ? Rh31 P32 C47 C48 62.4(4) . . . . ? C38 P32 C47 C50 173.9(4) . . . . ? C51 P32 C47 C50 70.3(5) . . . . ? Rh31 P32 C47 C50 -52.0(4) . . . . ? C38 P32 C51 C54 87.0(4) . . . . ? C47 P32 C51 C54 -165.7(4) . . . . ? Rh31 P32 C51 C54 -38.1(4) . . . . ? C38 P32 C51 C53 -153.8(4) . . . . ? C47 P32 C51 C53 -46.5(5) . . . . ? Rh31 P32 C51 C53 81.2(4) . . . . ? C38 P32 C51 C52 -31.6(4) . . . . ? C47 P32 C51 C52 75.7(4) . . . . ? Rh31 P32 C51 C52 -156.7(4) . . . . ? P32 Rh31 C55 O55 -161(8) . . . . ? P31 Rh31 C55 O55 -20(8) . . . . ? I31 Rh31 C55 O55 35(8) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.44 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.461 _refine_diff_density_min -1.973 _refine_diff_density_rms 0.153 # Attachment 'Rh_DTBPMB_Me2_I3_2.cif' data_Rh(DTBPMB)Me2(I3)2 _database_code_depnum_ccdc_archive 'CCDC 635434' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H50 I6 P2' _chemical_formula_weight 1186.00 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9029(12) _cell_length_b 11.3875(14) _cell_length_c 34.978(4) _cell_angle_alpha 87.539(2) _cell_angle_beta 86.579(2) _cell_angle_gamma 76.306(2) _cell_volume 3823.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 162 _cell_measurement_theta_min 12 _cell_measurement_theta_max 28 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max .1 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.060 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2216 _exptl_absorpt_coefficient_mu 4.972 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.551918 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _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 0.83 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23048 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0680 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.63 _reflns_number_total 13740 _reflns_number_gt 10354 _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^)+(0.0454P)^2^+9.1565P] 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 13740 _refine_ls_number_parameters 617 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1135 _refine_ls_wR_factor_gt 0.1058 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.85353(6) 0.93620(5) 0.311192(17) 0.02605(14) Uani 1 1 d . . . I2 I 0.58941(5) 1.06777(5) 0.276960(16) 0.02231(13) Uani 1 1 d . . . I3 I 0.34876(6) 1.22472(6) 0.245717(19) 0.03312(15) Uani 1 1 d . . . I4 I 0.71799(7) 0.52854(6) 0.55370(2) 0.04386(18) Uani 1 1 d . . . I5 I 0.43746(7) 0.66559(6) 0.539581(18) 0.03380(16) Uani 1 1 d . . . I6 I 0.15626(7) 0.81851(7) 0.53027(2) 0.0474(2) Uani 1 1 d . . . I31 I 0.65107(8) 0.17445(6) -0.016256(19) 0.04487(19) Uani 1 1 d . . . I32 I 0.80103(6) -0.08354(6) -0.004148(18) 0.03501(16) Uani 1 1 d . . . I33 I 0.96260(7) -0.32810(7) 0.00620(2) 0.04401(18) Uani 1 1 d . . . I34 I 1.45675(7) -0.30680(7) 0.23127(2) 0.04479(19) Uani 1 1 d . . . I35 I 1.20962(6) -0.39787(6) 0.220379(18) 0.03359(16) Uani 1 1 d . . . I36 I 0.96328(7) -0.48241(6) 0.20224(2) 0.04220(18) Uani 1 1 d . . . P1 P 0.3983(2) 0.8817(2) 0.39831(6) 0.0196(5) Uani 1 1 d . . . C1 C 0.5722(8) 0.8401(8) 0.3737(2) 0.0224(19) Uani 1 1 d . . . H1A H 0.5706 0.7819 0.3536 0.027 Uiso 1 1 calc R . . H1B H 0.5934 0.9134 0.3608 0.027 Uiso 1 1 calc R . . C2 C 0.6885(8) 0.7840(8) 0.4005(2) 0.0193(18) Uani 1 1 d . . . C3 C 0.7270(8) 0.6610(8) 0.4093(3) 0.0226(19) Uani 1 1 d . . . C4 C 0.8105(9) 0.6181(8) 0.4400(3) 0.027(2) Uani 1 1 d . . . H4A H 0.8267 0.5353 0.4479 0.032 Uiso 1 1 calc R . . C5 C 0.8708(9) 0.6973(9) 0.4592(3) 0.031(2) Uani 1 1 d . . . H5A H 0.9299 0.6682 0.4797 0.038 Uiso 1 1 calc R . . C6 C 0.8423(8) 0.8193(9) 0.4478(3) 0.027(2) Uani 1 1 d . . . H6A H 0.8847 0.8737 0.4598 0.033 Uiso 1 1 calc R . . C7 C 0.7537(8) 0.8595(8) 0.4194(3) 0.025(2) Uani 1 1 d . . . H7A H 0.7352 0.9428 0.4120 0.031 Uiso 1 1 calc R . . C8 C 0.6789(8) 0.5648(8) 0.3875(2) 0.0212(19) Uani 1 1 d . . . H8A H 0.5806 0.5984 0.3815 0.025 Uiso 1 1 calc R . . H8B H 0.6809 0.4943 0.4052 0.025 Uiso 1 1 calc R . . P2 P 0.7751(2) 0.5091(2) 0.34282(7) 0.0214(5) Uani 1 1 d . . . C9 C 0.3673(8) 1.0358(8) 0.4184(3) 0.030(2) Uani 1 1 d . . . C10 C 0.4399(10) 1.0243(9) 0.4565(3) 0.037(2) Uani 1 1 d . . . H10A H 0.4243 1.1043 0.4676 0.056 Uiso 1 1 calc R . . H10B H 0.5400 0.9912 0.4518 0.056 Uiso 1 1 calc R . . H10C H 0.4016 0.9702 0.4742 0.056 Uiso 1 1 calc R . . C11 C 0.4250(10) 1.1206(8) 0.3897(3) 0.032(2) Uani 1 1 d . . . H11A H 0.4080 1.2013 0.4004 0.048 Uiso 1 1 calc R . . H11B H 0.3782 1.1258 0.3656 0.048 Uiso 1 1 calc R . . H11C H 0.5252 1.0887 0.3850 0.048 Uiso 1 1 calc R . . C12 C 0.2097(9) 1.0873(9) 0.4276(3) 0.036(2) Uani 1 1 d . . . H12A H 0.1952 1.1680 0.4381 0.055 Uiso 1 1 calc R . . H12B H 0.1751 1.0337 0.4464 0.055 Uiso 1 1 calc R . . H12C H 0.1593 1.0929 0.4041 0.055 Uiso 1 1 calc R . . C13 C 0.2666(8) 0.8623(9) 0.3648(3) 0.027(2) Uani 1 1 d . . . C14 C 0.2436(10) 0.9659(11) 0.3337(3) 0.048(3) Uani 1 1 d . . . H14A H 0.1739 0.9547 0.3163 0.071 Uiso 1 1 calc R . . H14B H 0.3316 0.9645 0.3191 0.071 Uiso 1 1 calc R . . H14C H 0.2110 1.0439 0.3460 0.071 Uiso 1 1 calc R . . C15 C 0.1288(8) 0.8575(10) 0.3873(3) 0.034(2) Uani 1 1 d . . . H15A H 0.0602 0.8469 0.3695 0.051 Uiso 1 1 calc R . . H15B H 0.0932 0.9330 0.4009 0.051 Uiso 1 1 calc R . . H15C H 0.1455 0.7894 0.4059 0.051 Uiso 1 1 calc R . . C16 C 0.3182(9) 0.7412(10) 0.3452(3) 0.039(3) Uani 1 1 d . . . H16A H 0.2488 0.7303 0.3276 0.058 Uiso 1 1 calc R . . H16B H 0.3325 0.6754 0.3646 0.058 Uiso 1 1 calc R . . H16C H 0.4062 0.7403 0.3307 0.058 Uiso 1 1 calc R . . C17 C 0.9666(9) 0.4591(8) 0.3489(3) 0.027(2) Uani 1 1 d . . . C18 C 1.0245(9) 0.5715(9) 0.3523(3) 0.036(2) Uani 1 1 d . . . H18A H 1.1249 0.5467 0.3556 0.054 Uiso 1 1 calc R . . H18B H 0.9786 0.6174 0.3745 0.054 Uiso 1 1 calc R . . H18C H 1.0070 0.6223 0.3290 0.054 Uiso 1 1 calc R . . C19 C 0.9963(10) 0.3772(9) 0.3854(3) 0.036(2) Uani 1 1 d . . . H19A H 1.0970 0.3519 0.3882 0.055 Uiso 1 1 calc R . . H19B H 0.9587 0.3057 0.3832 0.055 Uiso 1 1 calc R . . H19C H 0.9520 0.4222 0.4079 0.055 Uiso 1 1 calc R . . C20 C 1.0400(9) 0.3865(9) 0.3137(3) 0.038(2) Uani 1 1 d . . . H20A H 1.1402 0.3607 0.3173 0.057 Uiso 1 1 calc R . . H20B H 1.0239 0.4380 0.2904 0.057 Uiso 1 1 calc R . . H20C H 1.0022 0.3153 0.3112 0.057 Uiso 1 1 calc R . . C21 C 0.6920(10) 0.3904(9) 0.3261(3) 0.031(2) Uani 1 1 d . . . C22 C 0.7406(11) 0.2710(9) 0.3491(3) 0.040(3) Uani 1 1 d . . . H22A H 0.6963 0.2099 0.3400 0.059 Uiso 1 1 calc R . . H22B H 0.7145 0.2842 0.3764 0.059 Uiso 1 1 calc R . . H22C H 0.8419 0.2430 0.3458 0.059 Uiso 1 1 calc R . . C23 C 0.7244(10) 0.3734(8) 0.2826(2) 0.029(2) Uani 1 1 d . . . H23A H 0.6812 0.3108 0.2741 0.044 Uiso 1 1 calc R . . H23B H 0.8253 0.3490 0.2775 0.044 Uiso 1 1 calc R . . H23C H 0.6871 0.4498 0.2688 0.044 Uiso 1 1 calc R . . C24 C 0.5330(9) 0.4335(9) 0.3323(3) 0.035(2) Uani 1 1 d . . . H24A H 0.4886 0.3717 0.3237 0.052 Uiso 1 1 calc R . . H24B H 0.5004 0.5090 0.3176 0.052 Uiso 1 1 calc R . . H24C H 0.5089 0.4473 0.3596 0.052 Uiso 1 1 calc R . . C25 C 0.3949(9) 0.7749(8) 0.4376(2) 0.026(2) Uani 1 1 d . . . H25A H 0.4035 0.6943 0.4276 0.039 Uiso 1 1 calc R . . H25B H 0.3069 0.7990 0.4527 0.039 Uiso 1 1 calc R . . H25C H 0.4726 0.7733 0.4538 0.039 Uiso 1 1 calc R . . C26 C 0.7512(9) 0.6286(8) 0.3070(2) 0.026(2) Uani 1 1 d . . . H26A H 0.6560 0.6448 0.2985 0.040 Uiso 1 1 calc R . . H26B H 0.8173 0.6045 0.2852 0.040 Uiso 1 1 calc R . . H26C H 0.7672 0.7017 0.3179 0.040 Uiso 1 1 calc R . . C31 C 0.6353(8) 0.2422(7) 0.0920(2) 0.0192(18) Uani 1 1 d . . . H31A H 0.6271 0.2425 0.0639 0.023 Uiso 1 1 calc R . . H31B H 0.7354 0.2296 0.0966 0.023 Uiso 1 1 calc R . . P31 P 0.5468(2) 0.3927(2) 0.10864(6) 0.0205(5) Uani 1 1 d . . . C32 C 0.5864(7) 0.1344(7) 0.1093(2) 0.0187(18) Uani 1 1 d . . . C33 C 0.6266(7) 0.0810(7) 0.1446(2) 0.0183(18) Uani 1 1 d . . . C34 C 0.5627(7) -0.0085(7) 0.1608(2) 0.0183(18) Uani 1 1 d . . . H34A H 0.5815 -0.0382 0.1862 0.022 Uiso 1 1 calc R . . C35 C 0.4724(8) -0.0540(8) 0.1400(3) 0.027(2) Uani 1 1 d . . . H35A H 0.4306 -0.1152 0.1511 0.033 Uiso 1 1 calc R . . C36 C 0.4435(9) -0.0100(8) 0.1034(3) 0.028(2) Uani 1 1 d . . . H36A H 0.3860 -0.0439 0.0884 0.033 Uiso 1 1 calc R . . C37 C 0.4989(9) 0.0839(8) 0.0884(3) 0.028(2) Uani 1 1 d . . . H37A H 0.4769 0.1151 0.0634 0.033 Uiso 1 1 calc R . . C38 C 0.7412(7) 0.1128(7) 0.1659(2) 0.0180(18) Uani 1 1 d . . . H38A H 0.7051 0.1335 0.1924 0.022 Uiso 1 1 calc R . . H38B H 0.7633 0.1862 0.1534 0.022 Uiso 1 1 calc R . . P32 P 0.9047(2) -0.00561(19) 0.16844(6) 0.0180(5) Uani 1 1 d . . . C39 C 0.3622(9) 0.4282(8) 0.0962(3) 0.027(2) Uani 1 1 d . . . C40 C 0.2842(9) 0.3556(9) 0.1243(3) 0.037(3) Uani 1 1 d . . . H40A H 0.1861 0.3725 0.1181 0.055 Uiso 1 1 calc R . . H40B H 0.2911 0.3793 0.1505 0.055 Uiso 1 1 calc R . . H40C H 0.3259 0.2690 0.1219 0.055 Uiso 1 1 calc R . . C41 C 0.3481(9) 0.3965(10) 0.0547(3) 0.035(2) Uani 1 1 d . . . H41A H 0.2494 0.4158 0.0490 0.053 Uiso 1 1 calc R . . H41B H 0.3878 0.3099 0.0514 0.053 Uiso 1 1 calc R . . H41C H 0.3979 0.4433 0.0373 0.053 Uiso 1 1 calc R . . C42 C 0.2950(9) 0.5650(8) 0.1014(3) 0.037(3) Uani 1 1 d . . . H42A H 0.1974 0.5825 0.0947 0.055 Uiso 1 1 calc R . . H42B H 0.3454 0.6133 0.0847 0.055 Uiso 1 1 calc R . . H42C H 0.2997 0.5852 0.1282 0.055 Uiso 1 1 calc R . . C43 C 0.6537(9) 0.4972(8) 0.0881(3) 0.028(2) Uani 1 1 d . . . C44 C 0.6379(10) 0.5156(9) 0.0451(3) 0.033(2) Uani 1 1 d . . . H44A H 0.6949 0.5704 0.0348 0.050 Uiso 1 1 calc R . . H44B H 0.5400 0.5507 0.0401 0.050 Uiso 1 1 calc R . . H44C H 0.6686 0.4375 0.0327 0.050 Uiso 1 1 calc R . . C45 C 0.6114(11) 0.6195(8) 0.1080(3) 0.038(2) Uani 1 1 d . . . H45A H 0.6682 0.6735 0.0970 0.057 Uiso 1 1 calc R . . H45B H 0.6263 0.6066 0.1355 0.057 Uiso 1 1 calc R . . H45C H 0.5129 0.6562 0.1043 0.057 Uiso 1 1 calc R . . C46 C 0.8090(9) 0.4394(9) 0.0952(3) 0.033(2) Uani 1 1 d . . . H46A H 0.8667 0.4931 0.0844 0.050 Uiso 1 1 calc R . . H46B H 0.8372 0.3612 0.0827 0.050 Uiso 1 1 calc R . . H46C H 0.8212 0.4274 0.1228 0.050 Uiso 1 1 calc R . . C47 C 0.9635(8) -0.0743(8) 0.1212(3) 0.0234(19) Uani 1 1 d . . . C48 C 0.9514(9) 0.0210(8) 0.0889(3) 0.030(2) Uani 1 1 d . . . H48A H 0.9837 -0.0185 0.0646 0.045 Uiso 1 1 calc R . . H48B H 1.0087 0.0775 0.0939 0.045 Uiso 1 1 calc R . . H48C H 0.8540 0.0653 0.0874 0.045 Uiso 1 1 calc R . . C49 C 0.8737(9) -0.1646(8) 0.1129(3) 0.028(2) Uani 1 1 d . . . H49A H 0.9043 -0.2011 0.0881 0.042 Uiso 1 1 calc R . . H49B H 0.7756 -0.1214 0.1124 0.042 Uiso 1 1 calc R . . H49C H 0.8845 -0.2281 0.1331 0.042 Uiso 1 1 calc R . . C50 C 1.1157(9) -0.1490(8) 0.1232(3) 0.030(2) Uani 1 1 d . . . H50A H 1.1473 -0.1851 0.0983 0.045 Uiso 1 1 calc R . . H50B H 1.1206 -0.2132 0.1430 0.045 Uiso 1 1 calc R . . H50C H 1.1755 -0.0960 0.1295 0.045 Uiso 1 1 calc R . . C51 C 1.0291(8) 0.0681(7) 0.1903(2) 0.0203(18) Uani 1 1 d . . . C52 C 1.1443(8) -0.0274(8) 0.2091(3) 0.028(2) Uani 1 1 d . . . H52A H 1.2091 0.0126 0.2204 0.043 Uiso 1 1 calc R . . H52B H 1.1947 -0.0833 0.1897 0.043 Uiso 1 1 calc R . . H52C H 1.1027 -0.0725 0.2292 0.043 Uiso 1 1 calc R . . C53 C 0.9504(8) 0.1520(8) 0.2219(3) 0.027(2) Uani 1 1 d . . . H53A H 1.0150 0.1914 0.2335 0.040 Uiso 1 1 calc R . . H53B H 0.9105 0.1043 0.2415 0.040 Uiso 1 1 calc R . . H53C H 0.8756 0.2136 0.2106 0.040 Uiso 1 1 calc R . . C54 C 1.0908(8) 0.1476(8) 0.1608(3) 0.026(2) Uani 1 1 d . . . H54A H 1.1557 0.1849 0.1732 0.040 Uiso 1 1 calc R . . H54B H 1.0157 0.2109 0.1505 0.040 Uiso 1 1 calc R . . H54C H 1.1405 0.0976 0.1399 0.040 Uiso 1 1 calc R . . C55 C 0.5497(9) 0.3950(8) 0.1599(2) 0.029(2) Uani 1 1 d . . . H55A H 0.5076 0.3314 0.1715 0.044 Uiso 1 1 calc R . . H55B H 0.4970 0.4739 0.1689 0.044 Uiso 1 1 calc R . . H55C H 0.6462 0.3809 0.1674 0.044 Uiso 1 1 calc R . . C56 C 0.8751(8) -0.1237(7) 0.2012(2) 0.0227(19) Uani 1 1 d . . . H56A H 0.8039 -0.1600 0.1915 0.034 Uiso 1 1 calc R . . H56B H 0.8435 -0.0899 0.2263 0.034 Uiso 1 1 calc R . . H56C H 0.9619 -0.1858 0.2035 0.034 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 I1 0.0256(3) 0.0250(3) 0.0286(3) 0.0047(2) -0.0056(2) -0.0081(2) I2 0.0233(3) 0.0221(3) 0.0231(3) -0.0023(2) 0.0006(2) -0.0086(2) I3 0.0264(3) 0.0315(4) 0.0395(4) -0.0025(3) -0.0056(3) -0.0018(3) I4 0.0542(4) 0.0357(4) 0.0461(4) 0.0076(3) -0.0171(3) -0.0174(3) I5 0.0480(4) 0.0349(4) 0.0250(3) 0.0022(3) -0.0029(3) -0.0231(3) I6 0.0385(4) 0.0609(5) 0.0410(4) -0.0064(3) 0.0123(3) -0.0109(3) I31 0.0772(5) 0.0319(4) 0.0253(4) -0.0044(3) 0.0018(3) -0.0127(4) I32 0.0392(3) 0.0395(4) 0.0299(4) -0.0054(3) 0.0017(3) -0.0167(3) I33 0.0369(3) 0.0426(4) 0.0521(5) -0.0113(3) -0.0018(3) -0.0070(3) I34 0.0423(4) 0.0489(5) 0.0371(4) 0.0024(3) -0.0111(3) 0.0029(3) I35 0.0419(3) 0.0226(3) 0.0278(3) 0.0026(3) 0.0016(3) 0.0080(3) I36 0.0594(4) 0.0271(4) 0.0398(4) -0.0029(3) 0.0084(3) -0.0121(3) P1 0.0177(10) 0.0194(12) 0.0212(12) -0.0008(9) 0.0004(8) -0.0038(8) C1 0.019(4) 0.024(5) 0.021(5) 0.003(4) 0.002(3) -0.001(3) C2 0.015(4) 0.023(5) 0.020(5) -0.005(3) 0.004(3) -0.004(3) C3 0.024(4) 0.016(5) 0.031(5) -0.004(4) 0.001(4) -0.010(3) C4 0.032(5) 0.022(5) 0.028(5) 0.002(4) -0.006(4) -0.007(4) C5 0.024(4) 0.037(6) 0.030(6) -0.006(4) -0.011(4) 0.001(4) C6 0.023(4) 0.034(6) 0.027(5) -0.009(4) -0.002(4) -0.011(4) C7 0.019(4) 0.024(5) 0.032(5) -0.002(4) 0.006(4) -0.004(4) C8 0.025(4) 0.021(5) 0.022(5) 0.004(4) -0.002(3) -0.014(4) P2 0.0252(11) 0.0151(12) 0.0244(13) -0.0007(9) -0.0016(9) -0.0058(9) C9 0.022(4) 0.025(5) 0.039(6) -0.003(4) 0.004(4) 0.001(4) C10 0.039(5) 0.040(6) 0.029(6) -0.009(4) 0.001(4) -0.002(5) C11 0.041(5) 0.017(5) 0.038(6) -0.009(4) 0.002(4) -0.006(4) C12 0.035(5) 0.026(6) 0.044(6) -0.006(4) 0.006(4) 0.002(4) C13 0.013(4) 0.043(6) 0.029(5) 0.003(4) -0.007(3) -0.013(4) C14 0.028(5) 0.080(9) 0.039(7) 0.026(6) -0.013(4) -0.024(5) C15 0.022(4) 0.053(7) 0.033(6) 0.003(5) -0.005(4) -0.020(4) C16 0.027(5) 0.049(7) 0.046(7) -0.008(5) -0.006(4) -0.018(5) C17 0.028(4) 0.020(5) 0.033(6) -0.006(4) -0.002(4) -0.001(4) C18 0.025(4) 0.030(6) 0.054(7) 0.002(5) -0.007(4) -0.006(4) C19 0.037(5) 0.027(6) 0.040(6) 0.008(4) -0.012(4) 0.003(4) C20 0.033(5) 0.032(6) 0.042(6) -0.009(5) -0.004(4) 0.006(4) C21 0.041(5) 0.028(6) 0.026(5) 0.000(4) 0.002(4) -0.013(4) C22 0.060(6) 0.026(6) 0.031(6) 0.001(4) 0.001(5) -0.010(5) C23 0.048(5) 0.020(5) 0.025(5) -0.006(4) -0.002(4) -0.017(4) C24 0.042(5) 0.030(6) 0.039(6) -0.013(4) -0.004(4) -0.020(4) C25 0.027(4) 0.028(5) 0.023(5) -0.001(4) 0.007(4) -0.008(4) C26 0.038(5) 0.016(5) 0.024(5) -0.001(4) -0.001(4) -0.005(4) C31 0.018(4) 0.023(5) 0.017(4) -0.002(3) -0.002(3) -0.005(3) P31 0.0274(11) 0.0133(11) 0.0187(12) -0.0008(9) -0.0005(9) -0.0010(9) C32 0.012(3) 0.018(5) 0.027(5) -0.005(3) -0.002(3) -0.005(3) C33 0.014(4) 0.016(4) 0.024(5) -0.008(3) 0.001(3) -0.001(3) C34 0.018(4) 0.010(4) 0.025(5) -0.005(3) 0.003(3) -0.001(3) C35 0.027(4) 0.022(5) 0.034(6) -0.007(4) 0.003(4) -0.009(4) C36 0.025(4) 0.022(5) 0.037(6) -0.012(4) 0.002(4) -0.008(4) C37 0.035(5) 0.018(5) 0.025(5) -0.005(4) -0.004(4) 0.004(4) C38 0.018(4) 0.008(4) 0.027(5) 0.001(3) -0.005(3) 0.000(3) P32 0.0181(9) 0.0125(11) 0.0221(12) -0.0002(9) -0.0006(8) -0.0013(8) C39 0.027(4) 0.021(5) 0.030(5) 0.004(4) 0.002(4) -0.002(4) C40 0.023(4) 0.033(6) 0.052(7) 0.005(5) 0.004(4) -0.003(4) C41 0.027(5) 0.045(7) 0.030(6) -0.005(4) -0.006(4) 0.000(4) C42 0.034(5) 0.027(6) 0.040(6) 0.012(4) 0.005(4) 0.007(4) C43 0.032(5) 0.017(5) 0.035(6) -0.002(4) -0.005(4) -0.006(4) C44 0.043(5) 0.028(6) 0.029(6) 0.002(4) -0.002(4) -0.007(4) C45 0.058(6) 0.015(5) 0.044(7) -0.006(4) -0.001(5) -0.011(5) C46 0.035(5) 0.024(5) 0.042(6) 0.001(4) -0.004(4) -0.010(4) C47 0.024(4) 0.016(5) 0.027(5) -0.003(4) 0.004(4) 0.002(3) C48 0.029(5) 0.027(5) 0.030(5) -0.003(4) 0.003(4) 0.003(4) C49 0.033(5) 0.023(5) 0.029(5) -0.014(4) 0.003(4) -0.008(4) C50 0.029(5) 0.023(5) 0.037(6) -0.007(4) 0.005(4) -0.002(4) C51 0.020(4) 0.011(4) 0.028(5) -0.002(3) -0.003(3) -0.001(3) C52 0.022(4) 0.022(5) 0.042(6) -0.001(4) -0.011(4) -0.004(4) C53 0.023(4) 0.020(5) 0.035(6) -0.004(4) 0.000(4) -0.001(4) C54 0.023(4) 0.027(5) 0.032(5) -0.005(4) 0.001(4) -0.013(4) C55 0.040(5) 0.022(5) 0.019(5) -0.002(4) -0.006(4) 0.008(4) C56 0.028(4) 0.018(5) 0.020(5) -0.001(3) 0.000(4) -0.001(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 I1 I2 2.9806(8) . ? I2 I3 2.8626(8) . ? I4 I5 2.9055(10) . ? I5 I6 2.9422(10) . ? I31 I32 2.9863(10) . ? I32 I33 2.8844(10) . ? I34 I35 2.9252(11) . ? I35 I36 2.9376(11) . ? P1 C25 1.799(8) . ? P1 C1 1.845(8) . ? P1 C13 1.862(9) . ? P1 C9 1.870(10) . ? C1 C2 1.532(11) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.388(11) . ? C2 C7 1.398(12) . ? C3 C4 1.395(12) . ? C3 C8 1.540(12) . ? C4 C5 1.406(13) . ? C4 H4A 0.9500 . ? C5 C6 1.397(13) . ? C5 H5A 0.9500 . ? C6 C7 1.356(12) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 P2 1.836(8) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? P2 C26 1.791(8) . ? P2 C17 1.868(9) . ? P2 C21 1.870(10) . ? C9 C10 1.535(13) . ? C9 C11 1.541(12) . ? C9 C12 1.551(11) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C16 1.530(14) . ? C13 C15 1.546(11) . ? C13 C14 1.556(13) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.533(13) . ? C17 C19 1.547(12) . ? C17 C20 1.559(13) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C24 1.539(12) . ? C21 C22 1.539(13) . ? C21 C23 1.547(12) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C31 C32 1.513(11) . ? C31 P31 1.832(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? P31 C55 1.797(9) . ? P31 C39 1.851(9) . ? P31 C43 1.867(9) . ? C32 C33 1.391(11) . ? C32 C37 1.399(12) . ? C33 C34 1.405(11) . ? C33 C38 1.515(11) . ? C34 C35 1.386(12) . ? C34 H34A 0.9500 . ? C35 C36 1.379(12) . ? C35 H35A 0.9500 . ? C36 C37 1.383(12) . ? C36 H36A 0.9500 . ? C37 H37A 0.9500 . ? C38 P32 1.849(7) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? P32 C56 1.794(8) . ? P32 C47 1.860(9) . ? P32 C51 1.862(9) . ? C39 C41 1.531(13) . ? C39 C40 1.546(12) . ? C39 C42 1.556(12) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.522(12) . ? C43 C45 1.541(13) . ? C43 C46 1.553(12) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.524(12) . ? C47 C50 1.549(11) . ? C47 C49 1.556(12) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.536(11) . ? C51 C54 1.537(11) . ? C51 C53 1.540(12) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I3 I2 I1 171.86(3) . . ? I4 I5 I6 175.14(3) . . ? I33 I32 I31 176.26(3) . . ? I34 I35 I36 174.90(3) . . ? C25 P1 C1 107.5(4) . . ? C25 P1 C13 107.0(4) . . ? C1 P1 C13 108.6(4) . . ? C25 P1 C9 108.1(4) . . ? C1 P1 C9 110.5(4) . . ? C13 P1 C9 114.9(4) . . ? C2 C1 P1 113.5(5) . . ? C2 C1 H1A 108.9 . . ? P1 C1 H1A 108.9 . . ? C2 C1 H1B 108.9 . . ? P1 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? C3 C2 C7 117.4(8) . . ? C3 C2 C1 123.1(8) . . ? C7 C2 C1 119.4(8) . . ? C2 C3 C4 120.4(8) . . ? C2 C3 C8 123.6(8) . . ? C4 C3 C8 116.0(7) . . ? C3 C4 C5 120.1(8) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C6 C5 C4 118.9(8) . . ? C6 C5 H5A 120.5 . . ? C4 C5 H5A 120.5 . . ? C7 C6 C5 119.5(9) . . ? C7 C6 H6A 120.2 . . ? C5 C6 H6A 120.2 . . ? C6 C7 C2 123.0(9) . . ? C6 C7 H7A 118.5 . . ? C2 C7 H7A 118.5 . . ? C3 C8 P2 118.6(5) . . ? C3 C8 H8A 107.7 . . ? P2 C8 H8A 107.7 . . ? C3 C8 H8B 107.7 . . ? P2 C8 H8B 107.7 . . ? H8A C8 H8B 107.1 . . ? C26 P2 C8 109.6(4) . . ? C26 P2 C17 106.5(4) . . ? C8 P2 C17 112.1(4) . . ? C26 P2 C21 107.3(4) . . ? C8 P2 C21 106.1(4) . . ? C17 P2 C21 115.2(4) . . ? C10 C9 C11 110.8(8) . . ? C10 C9 C12 107.1(8) . . ? C11 C9 C12 110.4(7) . . ? C10 C9 P1 108.2(6) . . ? C11 C9 P1 109.8(6) . . ? C12 C9 P1 110.4(7) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C16 C13 C15 106.9(8) . . ? C16 C13 C14 109.0(9) . . ? C15 C13 C14 111.2(7) . . ? C16 C13 P1 109.2(6) . . ? C15 C13 P1 110.0(6) . . ? C14 C13 P1 110.4(7) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C19 109.8(8) . . ? C18 C17 C20 109.2(8) . . ? C19 C17 C20 108.6(8) . . ? C18 C17 P2 108.5(6) . . ? C19 C17 P2 110.5(6) . . ? C20 C17 P2 110.3(7) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C24 C21 C22 108.5(8) . . ? C24 C21 C23 107.2(8) . . ? C22 C21 C23 111.7(8) . . ? C24 C21 P2 108.9(6) . . ? C22 C21 P2 110.6(7) . . ? C23 C21 P2 109.7(6) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? P1 C25 H25A 109.5 . . ? P1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? P1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? P2 C26 H26A 109.5 . . ? P2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? P2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C32 C31 P31 118.0(5) . . ? C32 C31 H31A 107.8 . . ? P31 C31 H31A 107.8 . . ? C32 C31 H31B 107.8 . . ? P31 C31 H31B 107.8 . . ? H31A C31 H31B 107.1 . . ? C55 P31 C31 109.7(4) . . ? C55 P31 C39 107.5(4) . . ? C31 P31 C39 109.9(4) . . ? C55 P31 C43 107.5(5) . . ? C31 P31 C43 105.7(4) . . ? C39 P31 C43 116.4(4) . . ? C33 C32 C37 118.1(8) . . ? C33 C32 C31 123.2(7) . . ? C37 C32 C31 118.6(8) . . ? C32 C33 C34 119.5(8) . . ? C32 C33 C38 122.2(7) . . ? C34 C33 C38 118.3(7) . . ? C35 C34 C33 120.6(8) . . ? C35 C34 H34A 119.7 . . ? C33 C34 H34A 119.7 . . ? C36 C35 C34 119.9(8) . . ? C36 C35 H35A 120.1 . . ? C34 C35 H35A 120.1 . . ? C35 C36 C37 119.4(9) . . ? C35 C36 H36A 120.3 . . ? C37 C36 H36A 120.3 . . ? C36 C37 C32 121.9(9) . . ? C36 C37 H37A 119.1 . . ? C32 C37 H37A 119.1 . . ? C33 C38 P32 116.0(6) . . ? C33 C38 H38A 108.3 . . ? P32 C38 H38A 108.3 . . ? C33 C38 H38B 108.3 . . ? P32 C38 H38B 108.3 . . ? H38A C38 H38B 107.4 . . ? C56 P32 C38 108.6(4) . . ? C56 P32 C47 107.7(4) . . ? C38 P32 C47 112.2(4) . . ? C56 P32 C51 107.4(4) . . ? C38 P32 C51 105.1(4) . . ? C47 P32 C51 115.6(4) . . ? C41 C39 C40 110.5(8) . . ? C41 C39 C42 109.0(7) . . ? C40 C39 C42 107.8(7) . . ? C41 C39 P31 111.3(6) . . ? C40 C39 P31 107.9(6) . . ? C42 C39 P31 110.3(7) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C45 110.4(7) . . ? C44 C43 C46 108.4(7) . . ? C45 C43 C46 108.6(8) . . ? C44 C43 P31 110.6(6) . . ? C45 C43 P31 110.3(6) . . ? C46 C43 P31 108.4(6) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 C50 110.5(7) . . ? C48 C47 C49 109.2(8) . . ? C50 C47 C49 106.8(7) . . ? C48 C47 P32 111.8(6) . . ? C50 C47 P32 109.2(6) . . ? C49 C47 P32 109.1(5) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C47 C50 H50A 109.5 . . ? C47 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C47 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 C54 111.1(7) . . ? C52 C51 C53 107.8(7) . . ? C54 C51 C53 107.0(7) . . ? C52 C51 P32 110.3(6) . . ? C54 C51 P32 111.6(6) . . ? C53 C51 P32 108.8(5) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? P31 C55 H55A 109.5 . . ? P31 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? P31 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? P32 C56 H56A 109.5 . . ? P32 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? P32 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C25 P1 C1 C2 -32.2(8) . . . . ? C13 P1 C1 C2 -147.6(6) . . . . ? C9 P1 C1 C2 85.5(7) . . . . ? P1 C1 C2 C3 88.3(9) . . . . ? P1 C1 C2 C7 -87.3(8) . . . . ? C7 C2 C3 C4 10.0(11) . . . . ? C1 C2 C3 C4 -165.7(7) . . . . ? C7 C2 C3 C8 -172.0(7) . . . . ? C1 C2 C3 C8 12.3(12) . . . . ? C2 C3 C4 C5 -8.1(12) . . . . ? C8 C3 C4 C5 173.7(7) . . . . ? C3 C4 C5 C6 1.8(13) . . . . ? C4 C5 C6 C7 2.3(13) . . . . ? C5 C6 C7 C2 -0.2(13) . . . . ? C3 C2 C7 C6 -5.9(12) . . . . ? C1 C2 C7 C6 169.9(7) . . . . ? C2 C3 C8 P2 83.7(9) . . . . ? C4 C3 C8 P2 -98.2(8) . . . . ? C3 C8 P2 C26 -66.9(7) . . . . ? C3 C8 P2 C17 51.1(7) . . . . ? C3 C8 P2 C21 177.6(6) . . . . ? C25 P1 C9 C10 36.6(7) . . . . ? C1 P1 C9 C10 -80.8(7) . . . . ? C13 P1 C9 C10 155.9(6) . . . . ? C25 P1 C9 C11 157.7(6) . . . . ? C1 P1 C9 C11 40.3(7) . . . . ? C13 P1 C9 C11 -83.0(7) . . . . ? C25 P1 C9 C12 -80.4(7) . . . . ? C1 P1 C9 C12 162.3(6) . . . . ? C13 P1 C9 C12 39.0(8) . . . . ? C25 P1 C13 C16 -70.2(7) . . . . ? C1 P1 C13 C16 45.6(7) . . . . ? C9 P1 C13 C16 169.8(6) . . . . ? C25 P1 C13 C15 46.9(8) . . . . ? C1 P1 C13 C15 162.6(6) . . . . ? C9 P1 C13 C15 -73.1(7) . . . . ? C25 P1 C13 C14 170.0(7) . . . . ? C1 P1 C13 C14 -74.2(8) . . . . ? C9 P1 C13 C14 50.1(8) . . . . ? C26 P2 C17 C18 46.7(7) . . . . ? C8 P2 C17 C18 -73.1(7) . . . . ? C21 P2 C17 C18 165.5(6) . . . . ? C26 P2 C17 C19 167.1(7) . . . . ? C8 P2 C17 C19 47.3(8) . . . . ? C21 P2 C17 C19 -74.2(8) . . . . ? C26 P2 C17 C20 -72.9(7) . . . . ? C8 P2 C17 C20 167.3(6) . . . . ? C21 P2 C17 C20 45.9(8) . . . . ? C26 P2 C21 C24 -76.0(7) . . . . ? C8 P2 C21 C24 41.1(7) . . . . ? C17 P2 C21 C24 165.6(6) . . . . ? C26 P2 C21 C22 164.8(6) . . . . ? C8 P2 C21 C22 -78.2(7) . . . . ? C17 P2 C21 C22 46.4(8) . . . . ? C26 P2 C21 C23 41.1(7) . . . . ? C8 P2 C21 C23 158.2(6) . . . . ? C17 P2 C21 C23 -77.2(7) . . . . ? C32 C31 P31 C55 54.4(7) . . . . ? C32 C31 P31 C39 -63.6(7) . . . . ? C32 C31 P31 C43 170.1(6) . . . . ? P31 C31 C32 C33 -80.8(9) . . . . ? P31 C31 C32 C37 100.6(8) . . . . ? C37 C32 C33 C34 -9.6(11) . . . . ? C31 C32 C33 C34 171.8(7) . . . . ? C37 C32 C33 C38 168.3(7) . . . . ? C31 C32 C33 C38 -10.3(12) . . . . ? C32 C33 C34 C35 7.6(11) . . . . ? C38 C33 C34 C35 -170.3(7) . . . . ? C33 C34 C35 C36 -0.8(12) . . . . ? C34 C35 C36 C37 -3.6(12) . . . . ? C35 C36 C37 C32 1.4(13) . . . . ? C33 C32 C37 C36 5.3(12) . . . . ? C31 C32 C37 C36 -176.1(7) . . . . ? C32 C33 C38 P32 -109.8(8) . . . . ? C34 C33 C38 P32 68.1(9) . . . . ? C33 C38 P32 C56 -72.5(7) . . . . ? C33 C38 P32 C47 46.4(7) . . . . ? C33 C38 P32 C51 172.8(6) . . . . ? C55 P31 C39 C41 -165.1(7) . . . . ? C31 P31 C39 C41 -45.7(7) . . . . ? C43 P31 C39 C41 74.3(8) . . . . ? C55 P31 C39 C40 -43.8(8) . . . . ? C31 P31 C39 C40 75.6(7) . . . . ? C43 P31 C39 C40 -164.4(6) . . . . ? C55 P31 C39 C42 73.7(7) . . . . ? C31 P31 C39 C42 -166.9(6) . . . . ? C43 P31 C39 C42 -46.9(7) . . . . ? C55 P31 C43 C44 -171.1(6) . . . . ? C31 P31 C43 C44 71.7(7) . . . . ? C39 P31 C43 C44 -50.5(7) . . . . ? C55 P31 C43 C45 -48.6(7) . . . . ? C31 P31 C43 C45 -165.8(6) . . . . ? C39 P31 C43 C45 72.0(8) . . . . ? C55 P31 C43 C46 70.1(7) . . . . ? C31 P31 C43 C46 -47.0(7) . . . . ? C39 P31 C43 C46 -169.3(6) . . . . ? C56 P32 C47 C48 163.5(6) . . . . ? C38 P32 C47 C48 44.0(7) . . . . ? C51 P32 C47 C48 -76.5(7) . . . . ? C56 P32 C47 C50 -73.9(7) . . . . ? C38 P32 C47 C50 166.6(6) . . . . ? C51 P32 C47 C50 46.1(7) . . . . ? C56 P32 C47 C49 42.5(7) . . . . ? C38 P32 C47 C49 -77.0(6) . . . . ? C51 P32 C47 C49 162.5(5) . . . . ? C56 P32 C51 C52 41.2(7) . . . . ? C38 P32 C51 C52 156.7(6) . . . . ? C47 P32 C51 C52 -79.0(7) . . . . ? C56 P32 C51 C54 165.3(6) . . . . ? C38 P32 C51 C54 -79.2(6) . . . . ? C47 P32 C51 C54 45.1(7) . . . . ? C56 P32 C51 C53 -76.9(6) . . . . ? C38 P32 C51 C53 38.6(6) . . . . ? C47 P32 C51 C53 162.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 25.63 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 2.411 _refine_diff_density_min -1.251 _refine_diff_density_rms 0.189