Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Hansjoerg Grutzmacher' _publ_contact_author_address ; Department of Chemistry and Applied Biosciences ETH Hoenggerberg Wolgang-Pauli Str. CH-8093 Zuerich Switzerland ; _publ_contact_author_email gruetzmacher@inorg.chem.ethz.ch _publ_contact_author_phone ? _publ_contact_author_fax '(+41) 1 633 10 32' loop_ _publ_author_name _publ_author_address C.Meyer ; Department of Chemistry and Applied Biosciences (D-CHAB) ETH Hoenggerberg Wolfgang-Pauli Str. CH-8093 Zuerich Switzerland ; M.Scherer ; Department of Chemistry and Applied Biosciences (D-CHAB) ETH Hoenggerberg Wolfgang-Pauli Str. CH-8093 Zuerich Switzerland ; H.Schonberg ; Department of Chemistry and Applied Biosciences (D-CHAB) ETH Hoenggerberg Wolfgang-Pauli Str. CH-8093 Zuerich Switzerland ; H.Ruegger ; Department of Chemistry and Applied Biosciences (D-CHAB) ETH Hoenggerberg Wolfgang-Pauli Str. CH-8093 Zuerich Switzerland ; S.Loss ; Department of Chemistry and Applied Biosciences (D-CHAB) ETH Hoenggerberg Wolfgang-Pauli Str. CH-8093 Zuerich Switzerland ; V.Gramlich ; Laboratorium fuer Kristallographie ETH Hoenggerberg Wolfgang-Pauli Str. CH-8093 Zuerich Switzerland ; ; H.Grutzmacher ; ; Department of Chemistry and Applied Biosciences (D-CHAB) ETH Hoenggerberg Wolfgang-Pauli Str. CH-8093 Zuerich Switzerland ; _publ_section_title ; Coordination Chemistry of Phosphanyl Amino Acids: Solid state and Solution Structures of Neutral and Cationic Rhodium Complexes ; #============================================================================== _audit_creation_method 'form.cif (version 2.0)' #============================================================================== # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. data_RhCl(cod)(Z_SerArs)_11 _database_code_depnum_ccdc_archive 'CCDC 178294' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C32 H36 As Cl N O4 Rh' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32 H36 As Cl N O4 Rh' _chemical_formula_weight 711.90 _chemical_absolute_configuration R #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 _symmetry_space_group_name_Hall P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 8.3011(2) _cell_length_b 9.7422(3) _cell_length_c 10.7146(3) _cell_angle_alpha 87.2010(10) _cell_angle_beta 76.2770(10) _cell_angle_gamma 68.5070(10) _cell_volume 782.54(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 1 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 362 _exptl_absorpt_coefficient_mu 1.716 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2787 _exptl_absorpt_correction_T_max 0.5469 _exptl_absorpt_process_details 'Blessing, 1995' #============================================================================== # EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens CCD1k' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8075 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0790 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 32.70 _diffrn_measured_fraction_theta_max 0.876 _diffrn_reflns_theta_full 32.70 _diffrn_measured_fraction_theta_full 0.876 _reflns_number_total 6090 _reflns_number_gt 5308 _reflns_threshold_expression >2sigma(I) #============================================================================== # REFINEMENT DATA _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^)+(0.0394P)^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 undef _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.041(9) _refine_ls_number_reflns 6090 _refine_ls_number_parameters 361 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1076 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.068 _refine_diff_density_min -1.015 _refine_diff_density_rms 0.088 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' As As 0.0499 2.0058 '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' _computing_data_collection 'SMART v4' _computing_cell_refinement 'SAINT v4' _computing_data_reduction 'SAINT v4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1994)' _computing_molecular_graphics ? _computing_publication_material ? #============================================================================== # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 0.73462(2) 0.76177(2) 0.53865(2) 0.03537(10) Uani 1 1 d . . . As1 As 0.75413(6) 0.99335(5) 0.59228(4) 0.03622(15) Uani 1 1 d . . . Cl1 Cl 1.03400(17) 0.68718(15) 0.41563(16) 0.0499(3) Uani 1 1 d . . . N1 N 0.8377(7) 0.9920(5) 0.2814(5) 0.0501(11) Uani 1 1 d . . . H1A H 0.9099 0.9039 0.2885 0.060 Uiso 1 1 calc R . . O1 O 1.1062(8) 1.0908(7) 0.1566(5) 0.0829(18) Uani 1 1 d . . . O2 O 1.0123(8) 1.2768(5) 0.2975(5) 0.0699(15) Uani 1 1 d . . . O3 O 0.6053(8) 1.1293(6) 0.1979(7) 0.0829(18) Uani 1 1 d . . . O4 O 0.7137(6) 0.8793(5) 0.1829(5) 0.0547(10) Uani 1 1 d . . . C1 C 1.0076(8) 1.1567(6) 0.2517(5) 0.0465(12) Uani 1 1 d . . . C2 C 0.8571(7) 1.1146(6) 0.3379(5) 0.0423(10) Uani 1 1 d . . . H2A H 0.7450 1.1998 0.3489 0.051 Uiso 1 1 calc R . . C3 C 0.9031(8) 1.0798(7) 0.4689(5) 0.0460(11) Uani 1 1 d . . . H3A H 0.8954 1.1704 0.5079 0.055 Uiso 1 1 calc R . . H3B H 1.0260 1.0122 0.4548 0.055 Uiso 1 1 calc R . . C4 C 1.1544(12) 1.3274(9) 0.2336(9) 0.078(2) Uani 1 1 d . . . H4A H 1.1412 1.4163 0.2767 0.117 Uiso 1 1 calc R . . H4B H 1.1483 1.3467 0.1457 0.117 Uiso 1 1 calc R . . H4C H 1.2675 1.2527 0.2360 0.117 Uiso 1 1 calc R . . C5 C 0.7102(8) 1.0114(6) 0.2179(6) 0.0484(12) Uani 1 1 d . . . C6 C 0.5859(11) 0.8864(8) 0.1090(9) 0.0645(18) Uani 1 1 d . . . H6A H 0.6213 0.9184 0.0231 0.077 Uiso 1 1 calc R . . H6B H 0.4689 0.9560 0.1502 0.077 Uiso 1 1 calc R . . C7 C 0.5814(9) 0.7340(7) 0.1025(6) 0.0547(14) Uani 1 1 d . . . C8 C 0.7345(13) 0.6111(9) 0.0704(10) 0.080(2) Uani 1 1 d . . . H8A H 0.8446 0.6208 0.0569 0.095 Uiso 1 1 calc R . . C9 C 0.7270(16) 0.4720(10) 0.0577(10) 0.097(3) Uani 1 1 d . . . H9A H 0.8316 0.3900 0.0338 0.116 Uiso 1 1 calc R . . C10 C 0.5648(19) 0.4563(11) 0.0807(9) 0.095(3) Uani 1 1 d . . . H10A H 0.5589 0.3636 0.0736 0.114 Uiso 1 1 calc R . . C11 C 0.4085(16) 0.5810(12) 0.1148(9) 0.089(3) Uani 1 1 d . . . H11A H 0.2985 0.5707 0.1301 0.107 Uiso 1 1 calc R . . C12 C 0.4153(11) 0.7189(10) 0.1260(7) 0.0662(17) Uani 1 1 d . . . H12A H 0.3107 0.8012 0.1490 0.079 Uiso 1 1 calc R . . C13 C 0.5330(7) 1.1606(6) 0.6544(6) 0.0437(11) Uani 1 1 d . . . C14 C 0.4347(8) 1.2354(7) 0.5671(8) 0.0595(16) Uani 1 1 d . . . H14A H 0.4762 1.2078 0.4801 0.071 Uiso 1 1 calc R . . C15 C 0.2723(10) 1.3527(9) 0.6114(11) 0.078(3) Uani 1 1 d . . . H15A H 0.2088 1.4051 0.5526 0.094 Uiso 1 1 calc R . . C16 C 0.2078(10) 1.3902(9) 0.7357(12) 0.087(3) Uani 1 1 d . . . H16A H 0.0978 1.4659 0.7634 0.105 Uiso 1 1 calc R . . C17 C 0.3006(12) 1.3194(11) 0.8219(10) 0.091(3) Uani 1 1 d . . . H17A H 0.2554 1.3472 0.9088 0.109 Uiso 1 1 calc R . . C18 C 0.4660(10) 1.2030(9) 0.7810(7) 0.0670(19) Uani 1 1 d . . . H18A H 0.5298 1.1549 0.8411 0.080 Uiso 1 1 calc R . . C19 C 0.8755(7) 0.9695(6) 0.7299(5) 0.0425(11) Uani 1 1 d . . . C20 C 0.9148(12) 1.0812(8) 0.7725(8) 0.072(2) Uani 1 1 d . . . H20A H 0.8773 1.1739 0.7380 0.086 Uiso 1 1 calc R . . C21 C 1.0114(14) 1.0562(10) 0.8680(10) 0.089(3) Uani 1 1 d . . . H21A H 1.0369 1.1326 0.8971 0.107 Uiso 1 1 calc R . . C22 C 1.0671(10) 0.9221(10) 0.9174(7) 0.073(2) Uani 1 1 d . . . H22A H 1.1292 0.9068 0.9817 0.087 Uiso 1 1 calc R . . C23 C 1.0331(11) 0.8073(9) 0.8740(7) 0.0666(19) Uani 1 1 d . . . H23A H 1.0754 0.7142 0.9070 0.080 Uiso 1 1 calc R . . C24 C 0.9362(9) 0.8305(7) 0.7813(6) 0.0524(13) Uani 1 1 d . . . H24A H 0.9112 0.7533 0.7531 0.063 Uiso 1 1 calc R . . C25 C 0.7663(8) 0.5308(6) 0.5588(6) 0.0475(12) Uani 1 1 d . . . H25A H 0.8898 0.4616 0.5328 0.057 Uiso 1 1 calc R . . C26 C 0.6868(9) 0.5820(7) 0.4581(7) 0.0560(16) Uani 1 1 d . . . H26A H 0.7653 0.5434 0.3736 0.067 Uiso 1 1 calc R . . C27 C 0.4919(9) 0.6202(8) 0.4634(8) 0.0627(17) Uani 1 1 d . . . H27A H 0.4459 0.5603 0.5261 0.075 Uiso 1 1 calc R . . H27B H 0.4794 0.5965 0.3801 0.075 Uiso 1 1 calc R . . C28 C 0.3826(9) 0.7814(9) 0.4987(9) 0.0705(19) Uani 1 1 d . . . H28A H 0.3793 0.8359 0.4206 0.085 Uiso 1 1 calc R . . H28B H 0.2614 0.7914 0.5404 0.085 Uiso 1 1 calc R . . C29 C 0.4526(7) 0.8486(7) 0.5859(7) 0.0550(15) Uani 1 1 d . . . H29A H 0.4024 0.9567 0.5896 0.066 Uiso 1 1 calc R . . C30 C 0.5133(8) 0.7898(7) 0.6959(6) 0.0548(15) Uani 1 1 d . . . H30A H 0.4950 0.8635 0.7621 0.066 Uiso 1 1 calc R . . C31 C 0.5023(11) 0.6450(9) 0.7470(8) 0.074(2) Uani 1 1 d . . . H31A H 0.4002 0.6326 0.7273 0.089 Uiso 1 1 calc R . . H31B H 0.4842 0.6483 0.8398 0.089 Uiso 1 1 calc R . . C32 C 0.6718(11) 0.5109(8) 0.6893(8) 0.070(2) Uani 1 1 d . . . H32A H 0.7529 0.4905 0.7457 0.084 Uiso 1 1 calc R . . H32B H 0.6390 0.4254 0.6871 0.084 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 0.02964(18) 0.0320(2) 0.0448(2) 0.00003(15) -0.00736(15) -0.01239(15) As1 0.0348(3) 0.0325(3) 0.0423(4) 0.0011(2) -0.0088(2) -0.0135(2) Cl1 0.0292(6) 0.0425(6) 0.0723(9) -0.0015(6) -0.0043(5) -0.0108(5) N1 0.057(3) 0.040(2) 0.064(3) 0.007(2) -0.029(2) -0.021(2) O1 0.080(4) 0.096(4) 0.069(3) -0.037(3) 0.022(3) -0.048(3) O2 0.079(3) 0.059(3) 0.068(3) -0.021(2) 0.025(2) -0.045(3) O3 0.081(4) 0.045(3) 0.143(6) 0.013(3) -0.070(4) -0.021(2) O4 0.060(3) 0.046(2) 0.072(3) 0.0049(18) -0.033(2) -0.0243(19) C1 0.049(3) 0.045(3) 0.047(3) 0.001(2) -0.009(2) -0.020(2) C2 0.042(3) 0.037(2) 0.049(3) 0.0000(19) -0.011(2) -0.016(2) C3 0.045(3) 0.050(3) 0.052(3) 0.005(2) -0.012(2) -0.027(2) C4 0.082(5) 0.072(5) 0.081(5) -0.009(4) 0.017(4) -0.052(4) C5 0.052(3) 0.047(3) 0.058(3) 0.010(2) -0.022(3) -0.026(2) C6 0.070(4) 0.049(3) 0.091(5) 0.008(3) -0.046(4) -0.024(3) C7 0.065(4) 0.054(3) 0.057(4) 0.009(3) -0.028(3) -0.028(3) C8 0.080(5) 0.059(4) 0.105(7) 0.004(4) -0.023(5) -0.031(4) C9 0.124(9) 0.058(5) 0.118(8) 0.007(5) -0.047(7) -0.032(5) C10 0.173(11) 0.076(6) 0.082(6) 0.026(5) -0.056(7) -0.085(7) C11 0.123(8) 0.106(7) 0.080(6) 0.022(5) -0.032(5) -0.088(7) C12 0.074(5) 0.082(5) 0.057(4) 0.004(3) -0.017(3) -0.044(4) C13 0.042(3) 0.034(2) 0.054(3) 0.003(2) -0.010(2) -0.014(2) C14 0.040(3) 0.055(3) 0.078(4) 0.015(3) -0.012(3) -0.014(3) C15 0.046(4) 0.060(4) 0.130(8) 0.026(5) -0.029(4) -0.018(3) C16 0.043(4) 0.055(4) 0.144(9) -0.020(5) -0.002(5) -0.004(3) C17 0.070(5) 0.088(6) 0.089(6) -0.029(5) 0.008(4) -0.011(5) C18 0.061(4) 0.064(4) 0.062(4) -0.012(3) -0.006(3) -0.010(3) C19 0.037(2) 0.043(3) 0.047(3) -0.004(2) -0.011(2) -0.013(2) C20 0.095(6) 0.051(4) 0.079(5) -0.001(3) -0.046(4) -0.022(4) C21 0.111(7) 0.071(5) 0.099(7) -0.016(4) -0.061(6) -0.025(5) C22 0.066(4) 0.092(6) 0.056(4) -0.007(4) -0.028(3) -0.014(4) C23 0.068(4) 0.072(5) 0.059(4) 0.015(3) -0.024(3) -0.020(4) C24 0.055(3) 0.051(3) 0.054(3) 0.006(2) -0.018(3) -0.022(3) C25 0.043(3) 0.035(2) 0.068(4) 0.000(2) -0.018(3) -0.016(2) C26 0.052(3) 0.051(3) 0.065(4) -0.021(3) 0.001(3) -0.024(3) C27 0.061(4) 0.063(4) 0.082(5) 0.003(3) -0.032(3) -0.035(3) C28 0.045(3) 0.070(5) 0.104(6) 0.001(4) -0.031(4) -0.020(3) C29 0.029(2) 0.045(3) 0.086(5) -0.004(3) -0.005(3) -0.012(2) C30 0.049(3) 0.054(3) 0.053(3) -0.009(2) 0.011(3) -0.022(3) C31 0.077(5) 0.067(4) 0.071(5) 0.011(3) 0.009(4) -0.035(4) C32 0.079(5) 0.053(4) 0.081(5) 0.027(3) -0.018(4) -0.030(4) #============================================================================== # MOLECULAR GEOMETRY _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 C29 2.117(5) . ? Rh1 C30 2.121(6) . ? Rh1 C25 2.174(5) . ? Rh1 C26 2.189(6) . ? Rh1 Cl1 2.3786(13) . ? Rh1 As1 2.4259(5) . ? As1 C19 1.934(5) . ? As1 C13 1.950(5) . ? As1 C3 1.966(5) . ? N1 C5 1.342(7) . ? N1 C2 1.442(7) . ? O1 C1 1.184(8) . ? O2 C1 1.307(8) . ? O2 C4 1.454(8) . ? O3 C5 1.206(7) . ? O4 C5 1.346(7) . ? O4 C6 1.448(8) . ? C1 C2 1.540(8) . ? C2 C3 1.531(8) . ? C6 C7 1.504(10) . ? C7 C8 1.373(12) . ? C7 C12 1.402(10) . ? C8 C9 1.393(13) . ? C9 C10 1.374(15) . ? C10 C11 1.398(16) . ? C11 C12 1.377(13) . ? C13 C18 1.360(9) . ? C13 C14 1.390(9) . ? C14 C15 1.404(10) . ? C15 C16 1.327(14) . ? C16 C17 1.345(14) . ? C17 C18 1.408(11) . ? C19 C20 1.370(9) . ? C19 C24 1.397(8) . ? C20 C21 1.404(11) . ? C21 C22 1.345(12) . ? C22 C23 1.375(13) . ? C23 C24 1.382(10) . ? C25 C26 1.375(10) . ? C25 C32 1.475(10) . ? C26 C27 1.508(9) . ? C27 C28 1.511(10) . ? C28 C29 1.494(10) . ? C29 C30 1.406(10) . ? C30 C31 1.514(9) . ? C31 C32 1.545(11) . ? 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 C29 Rh1 C30 38.7(3) . . ? C29 Rh1 C25 96.6(2) . . ? C30 Rh1 C25 82.1(2) . . ? C29 Rh1 C26 80.8(3) . . ? C30 Rh1 C26 90.0(3) . . ? C25 Rh1 C26 36.7(3) . . ? C29 Rh1 Cl1 160.6(2) . . ? C30 Rh1 Cl1 160.6(2) . . ? C25 Rh1 Cl1 89.26(17) . . ? C26 Rh1 Cl1 93.39(18) . . ? C29 Rh1 As1 93.19(18) . . ? C30 Rh1 As1 92.32(18) . . ? C25 Rh1 As1 156.13(17) . . ? C26 Rh1 As1 167.1(2) . . ? Cl1 Rh1 As1 88.62(4) . . ? C19 As1 C13 103.2(2) . . ? C19 As1 C3 97.6(2) . . ? C13 As1 C3 103.8(2) . . ? C19 As1 Rh1 110.66(16) . . ? C13 As1 Rh1 118.21(17) . . ? C3 As1 Rh1 120.34(18) . . ? C5 N1 C2 121.8(5) . . ? C1 O2 C4 118.4(5) . . ? C5 O4 C6 114.7(5) . . ? O1 C1 O2 123.9(6) . . ? O1 C1 C2 125.4(6) . . ? O2 C1 C2 110.6(5) . . ? N1 C2 C3 112.2(4) . . ? N1 C2 C1 111.2(5) . . ? C3 C2 C1 106.8(5) . . ? C2 C3 As1 116.3(4) . . ? O3 C5 N1 125.2(6) . . ? O3 C5 O4 125.0(5) . . ? N1 C5 O4 109.7(5) . . ? O4 C6 C7 107.4(5) . . ? C8 C7 C12 119.6(7) . . ? C8 C7 C6 121.9(7) . . ? C12 C7 C6 118.5(7) . . ? C7 C8 C9 120.8(9) . . ? C10 C9 C8 119.9(10) . . ? C9 C10 C11 119.4(8) . . ? C12 C11 C10 120.9(9) . . ? C11 C12 C7 119.4(9) . . ? C18 C13 C14 118.3(6) . . ? C18 C13 As1 122.7(5) . . ? C14 C13 As1 119.0(5) . . ? C13 C14 C15 119.5(8) . . ? C16 C15 C14 121.2(8) . . ? C15 C16 C17 120.4(7) . . ? C16 C17 C18 120.2(8) . . ? C13 C18 C17 120.5(8) . . ? C20 C19 C24 118.8(5) . . ? C20 C19 As1 122.4(5) . . ? C24 C19 As1 118.6(5) . . ? C19 C20 C21 120.2(7) . . ? C22 C21 C20 120.1(8) . . ? C21 C22 C23 120.7(7) . . ? C22 C23 C24 119.9(7) . . ? C23 C24 C19 120.2(7) . . ? C26 C25 C32 124.8(6) . . ? C26 C25 Rh1 72.2(4) . . ? C32 C25 Rh1 109.1(4) . . ? C25 C26 C27 125.2(6) . . ? C25 C26 Rh1 71.0(4) . . ? C27 C26 Rh1 111.9(4) . . ? C26 C27 C28 112.5(6) . . ? C29 C28 C27 113.7(5) . . ? C30 C29 C28 128.3(6) . . ? C30 C29 Rh1 70.8(3) . . ? C28 C29 Rh1 110.5(5) . . ? C29 C30 C31 121.4(7) . . ? C29 C30 Rh1 70.5(3) . . ? C31 C30 Rh1 113.1(4) . . ? C30 C31 C32 112.5(5) . . ? C25 C32 C31 114.4(5) . . ? #============================================================================== # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. #============================================================================== #============================================================================== # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. data_RhCl(cod)(Z_AlaSerPhos)_10 _database_code_depnum_ccdc_archive 'CCDC 178295' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H40 Cl N2 O5 P Rh' _chemical_formula_sum 'C35 H40 Cl N2 O5 P Rh' _chemical_formula_weight 738.02 #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7543(3) _cell_length_b 11.7575(2) _cell_length_c 16.8367(4) _cell_angle_alpha 104.3120(10) _cell_angle_beta 91.8730(10) _cell_angle_gamma 112.6490(10) _cell_volume 1884.17(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irregular shaped crystal' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 762 _exptl_absorpt_coefficient_mu 0.606 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Blessing, 1995' #============================================================================== # EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens CCD1k' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15731 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 28.28 _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.976 _reflns_number_total 9127 _reflns_number_gt 7771 _reflns_threshold_expression >2sigma(I) #============================================================================== # REFINEMENT DATA _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^)+(0.0784P)^2^+2.6008P] 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 undef _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9127 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0688 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1714 _refine_ls_wR_factor_gt 0.1590 _refine_ls_goodness_of_fit_ref 1.188 _refine_ls_restrained_S_all 1.188 _refine_ls_shift/su_max 0.066 _refine_ls_shift/su_mean 0.003 _refine_diff_density_max 1.301 _refine_diff_density_min -0.766 _refine_diff_density_rms 0.126 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _computing_data_collection 'SMART v4' _computing_cell_refinement 'SAINT v4' _computing_data_reduction 'SAINT v4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1994)' _computing_molecular_graphics ? _computing_publication_material ? #============================================================================== # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 -0.23368(3) 1.03730(3) 0.334793(18) 0.03570(11) Uani 1 1 d . . . P1 P -0.06487(9) 1.08105(10) 0.25031(6) 0.0348(2) Uani 1 1 d . . . Cl1 Cl -0.37800(12) 1.07046(13) 0.24231(7) 0.0518(3) Uani 1 1 d . . . N1 N -0.3043(4) 0.8492(3) 0.1160(2) 0.0432(8) Uani 1 1 d . . . H1A H -0.3337 0.8866 0.1569 0.052 Uiso 1 1 calc R . . C1 C -0.3475(5) 1.0808(7) 0.4363(3) 0.0626(14) Uani 1 1 d . . . H1B H -0.3999 1.1292 0.4261 0.075 Uiso 1 1 calc R . . O1 O -0.3261(4) 0.6660(4) 0.0271(3) 0.0699(11) Uani 1 1 d . . . N2 N -0.5024(5) 0.5291(4) 0.1217(3) 0.0642(12) Uani 1 1 d . A . H2A H -0.5697 0.4586 0.0959 0.077 Uiso 1 1 calc R . . C2 C -0.4110(5) 0.9503(6) 0.3970(4) 0.0660(15) Uani 1 1 d . . . H2B H -0.4997 0.9234 0.3643 0.079 Uiso 1 1 calc R . . O2 O -0.3107(5) 0.6230(5) 0.2144(3) 0.0919(15) Uani 1 1 d . . . O3 O -0.4133(6) 0.4074(4) 0.1600(4) 0.0975(16) Uani 1 1 d . . . C3 C -0.3938(8) 0.8476(9) 0.4275(7) 0.116(3) Uani 1 1 d . . . H3A H -0.4284 0.8494 0.4801 0.139 Uiso 1 1 calc R . . H3B H -0.4508 0.7653 0.3888 0.139 Uiso 1 1 calc R . . O4 O -0.1607(5) 0.9254(6) -0.0575(3) 0.0887(14) Uani 1 1 d . . . C4 C -0.2556(8) 0.8532(9) 0.4389(6) 0.098(3) Uani 1 1 d . . . H4A H -0.2593 0.7676 0.4158 0.118 Uiso 1 1 calc R . . H4B H -0.2245 0.8784 0.4979 0.118 Uiso 1 1 calc R . . O5 O -0.3452(5) 0.9400(5) -0.0090(2) 0.0776(12) Uani 1 1 d . . . C5 C -0.1523(6) 0.9437(6) 0.4004(3) 0.0627(14) Uani 1 1 d . . . H5A H -0.0949 0.9064 0.3696 0.075 Uiso 1 1 calc R . . C6 C -0.0875(5) 1.0750(7) 0.4357(3) 0.0623(14) Uani 1 1 d . . . H6A H 0.0071 1.1130 0.4257 0.075 Uiso 1 1 calc R . . C7 C -0.1181(7) 1.1488(9) 0.5148(4) 0.100(3) Uani 1 1 d . . . H7A H -0.0941 1.1200 0.5600 0.120 Uiso 1 1 calc R . . H7B H -0.0582 1.2388 0.5255 0.120 Uiso 1 1 calc R . . C8 C -0.2569(8) 1.1395(10) 0.5178(4) 0.103(3) Uani 1 1 d . . . H8A H -0.2532 1.2251 0.5410 0.124 Uiso 1 1 calc R . . H8B H -0.2977 1.0891 0.5552 0.124 Uiso 1 1 calc R . . C9 C 0.0440(5) 1.2521(4) 0.2790(3) 0.0456(9) Uani 1 1 d . . . C10 C 0.0092(6) 1.3372(5) 0.3377(4) 0.0683(15) Uani 1 1 d . . . H10A H -0.0662 1.3066 0.3642 0.082 Uiso 1 1 calc R . . C11 C 0.0891(9) 1.4692(7) 0.3564(6) 0.101(3) Uani 1 1 d . . . H11A H 0.0643 1.5262 0.3943 0.122 Uiso 1 1 calc R . . C12 C 0.2007(9) 1.5154(6) 0.3206(5) 0.101(3) Uani 1 1 d . . . H12A H 0.2538 1.6033 0.3350 0.121 Uiso 1 1 calc R . . C13 C 0.2368(7) 1.4316(6) 0.2622(5) 0.0813(19) Uani 1 1 d . . . H13A H 0.3140 1.4638 0.2374 0.098 Uiso 1 1 calc R . . C14 C 0.1588(5) 1.3009(5) 0.2404(3) 0.0589(12) Uani 1 1 d . . . H14A H 0.1824 1.2455 0.2003 0.071 Uiso 1 1 calc R . . C15 C 0.0476(4) 0.9988(4) 0.2530(2) 0.0399(8) Uani 1 1 d . . . C16 C -0.0090(5) 0.8662(5) 0.2242(3) 0.0565(12) Uani 1 1 d . . . H16A H -0.1009 0.8229 0.2028 0.068 Uiso 1 1 calc R . . C17 C 0.0702(8) 0.7966(7) 0.2269(4) 0.0743(17) Uani 1 1 d . . . H17A H 0.0314 0.7074 0.2076 0.089 Uiso 1 1 calc R . . C18 C 0.2073(7) 0.8617(8) 0.2587(4) 0.0759(18) Uani 1 1 d . . . H18A H 0.2612 0.8160 0.2590 0.091 Uiso 1 1 calc R . . C19 C 0.2633(6) 0.9911(7) 0.2894(4) 0.0684(16) Uani 1 1 d . . . H19A H 0.3546 1.0338 0.3122 0.082 Uiso 1 1 calc R . . C20 C 0.1842(4) 1.0607(5) 0.2868(3) 0.0521(11) Uani 1 1 d . . . H20A H 0.2234 1.1497 0.3081 0.063 Uiso 1 1 calc R . . C21 C -0.1146(4) 1.0604(4) 0.1400(2) 0.0396(8) Uani 1 1 d . . . H21A H -0.1732 1.1051 0.1371 0.047 Uiso 1 1 calc R . . H21B H -0.0330 1.1030 0.1176 0.047 Uiso 1 1 calc R . . C22 C -0.1876(4) 0.9233(4) 0.0835(2) 0.0405(8) Uani 1 1 d . . . H22A H -0.1238 0.8817 0.0792 0.049 Uiso 1 1 calc R . . C23 C -0.2284(5) 0.9291(5) -0.0028(3) 0.0505(10) Uani 1 1 d . . . C24 C -0.3925(11) 0.9467(12) -0.0887(5) 0.126(4) Uani 1 1 d . . . H24A H -0.4775 0.9555 -0.0865 0.189 Uiso 1 1 calc R . . H24B H -0.4049 0.8695 -0.1306 0.189 Uiso 1 1 calc R . . H24C H -0.3264 1.0194 -0.1019 0.189 Uiso 1 1 calc R . . C25 C -0.3670(5) 0.7224(4) 0.0827(3) 0.0481(10) Uani 1 1 d . A . C26 C -0.4970(6) 0.6510(6) 0.1158(5) 0.0709(16) Uani 1 1 d . . . C27 C -0.5415(14) 0.7126(11) 0.1771(9) 0.072(4) Uani 0.474(14) 1 d P A 1 H27A H -0.6235 0.6531 0.1896 0.107 Uiso 0.474(14) 1 calc PR A 1 H27B H -0.5599 0.7781 0.1610 0.107 Uiso 0.474(14) 1 calc PR A 1 H27C H -0.4735 0.7514 0.2252 0.107 Uiso 0.474(14) 1 calc PR A 1 C27A C -0.6209(12) 0.6569(12) 0.0813(10) 0.084(5) Uani 0.526(14) 1 d P A 2 H27D H -0.6968 0.6104 0.1056 0.125 Uiso 0.526(14) 1 calc PR A 2 H27E H -0.6377 0.6193 0.0224 0.125 Uiso 0.526(14) 1 calc PR A 2 H27F H -0.6093 0.7449 0.0934 0.125 Uiso 0.526(14) 1 calc PR A 2 C28 C -0.3988(7) 0.5287(6) 0.1690(4) 0.0697(15) Uani 1 1 d . A . C29 C -0.3044(13) 0.4083(11) 0.2229(8) 0.071(3) Uani 0.582(5) 1 d P B 1 H29A H -0.2929 0.3285 0.2041 0.085 Uiso 0.582(5) 1 calc PR B 1 H29B H -0.2183 0.4777 0.2229 0.085 Uiso 0.582(5) 1 calc PR B 1 C30 C -0.3344(10) 0.4234(8) 0.3085(7) 0.062(2) Uani 0.582(5) 1 d P B 1 C31 C -0.4569(11) 0.3510(12) 0.3296(7) 0.076(3) Uani 0.582(5) 1 d P B 1 H31A H -0.5290 0.2960 0.2880 0.092 Uiso 0.582(5) 1 calc PR B 1 C32 C -0.4739(14) 0.3585(13) 0.4084(8) 0.086(3) Uani 0.582(5) 1 d P B 1 H32A H -0.5549 0.3042 0.4212 0.103 Uiso 0.582(5) 1 calc PR B 1 C33 C -0.3732(19) 0.4452(16) 0.4703(9) 0.102(5) Uani 0.582(5) 1 d P B 1 H33A H -0.3850 0.4521 0.5255 0.122 Uiso 0.582(5) 1 calc PR B 1 C34 C -0.2557(18) 0.5210(15) 0.4499(10) 0.109(5) Uani 0.582(5) 1 d P B 1 H34A H -0.1868 0.5802 0.4923 0.131 Uiso 0.582(5) 1 calc PR B 1 C35 C -0.2342(14) 0.5151(13) 0.3732(9) 0.093(4) Uani 0.582(5) 1 d P B 1 H35A H -0.1530 0.5713 0.3617 0.112 Uiso 0.582(5) 1 calc PR B 1 C29A C -0.315(3) 0.363(3) 0.1764(17) 0.114(8) Uiso 0.418(5) 1 d P B 2 H29C H -0.3616 0.2786 0.1848 0.137 Uiso 0.418(5) 1 calc PR B 2 H29D H -0.2586 0.4194 0.2282 0.137 Uiso 0.418(5) 1 calc PR B 2 C30A C -0.2178(16) 0.3510(17) 0.1091(10) 0.111(7) Uiso 0.418(5) 1 d PG B 2 C31A C -0.2646(13) 0.2704(16) 0.0289(11) 0.127(8) Uiso 0.418(5) 1 d PG B 2 H31B H -0.3575 0.2302 0.0098 0.152 Uiso 0.418(5) 1 calc PR B 2 C32A C -0.1726(18) 0.2500(15) -0.0229(8) 0.145(10) Uiso 0.418(5) 1 d PG B 2 H32B H -0.2039 0.1961 -0.0766 0.173 Uiso 0.418(5) 1 calc PR B 2 C33A C -0.0337(16) 0.3101(16) 0.0056(10) 0.108(6) Uiso 0.418(5) 1 d PG B 2 H33B H 0.0278 0.2965 -0.0290 0.130 Uiso 0.418(5) 1 calc PR B 2 C34A C 0.0131(13) 0.3907(16) 0.0859(11) 0.130(8) Uiso 0.418(5) 1 d PG B 2 H34B H 0.1060 0.4309 0.1050 0.156 Uiso 0.418(5) 1 calc PR B 2 C35A C -0.0789(18) 0.4111(16) 0.1376(8) 0.143(10) Uiso 0.418(5) 1 d PG B 2 H35B H -0.0476 0.4650 0.1913 0.171 Uiso 0.418(5) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.03040(16) 0.04943(19) 0.03211(16) 0.01232(12) 0.00727(11) 0.02056(13) P1 0.0287(4) 0.0425(5) 0.0311(4) 0.0086(4) 0.0047(3) 0.0133(4) Cl1 0.0496(6) 0.0750(7) 0.0484(6) 0.0227(5) 0.0084(4) 0.0404(6) N1 0.0414(18) 0.0454(18) 0.0382(17) 0.0111(14) 0.0079(14) 0.0131(15) C1 0.052(3) 0.106(4) 0.046(2) 0.021(3) 0.021(2) 0.049(3) O1 0.068(2) 0.0506(19) 0.066(2) -0.0031(17) 0.0102(19) 0.0091(17) N2 0.066(3) 0.045(2) 0.066(3) 0.017(2) 0.007(2) 0.006(2) C2 0.044(3) 0.099(4) 0.076(4) 0.050(3) 0.030(3) 0.034(3) O2 0.083(3) 0.080(3) 0.092(3) 0.028(3) -0.011(3) 0.011(3) O3 0.105(4) 0.064(3) 0.132(5) 0.043(3) 0.024(3) 0.034(3) C3 0.074(5) 0.137(7) 0.176(9) 0.120(7) 0.041(5) 0.036(5) O4 0.082(3) 0.138(4) 0.048(2) 0.029(2) 0.027(2) 0.042(3) C4 0.101(5) 0.128(6) 0.129(6) 0.097(6) 0.059(5) 0.072(5) O5 0.086(3) 0.125(4) 0.049(2) 0.032(2) 0.0082(19) 0.067(3) C5 0.061(3) 0.103(4) 0.061(3) 0.047(3) 0.021(2) 0.056(3) C6 0.043(2) 0.106(5) 0.043(2) 0.022(3) 0.0047(19) 0.035(3) C7 0.065(4) 0.168(8) 0.042(3) -0.011(4) -0.005(3) 0.048(5) C8 0.093(5) 0.172(8) 0.046(3) -0.011(4) 0.003(3) 0.080(6) C9 0.042(2) 0.046(2) 0.043(2) 0.0096(18) 0.0042(17) 0.0150(18) C10 0.068(3) 0.054(3) 0.071(3) 0.005(3) 0.018(3) 0.019(3) C11 0.113(6) 0.056(4) 0.112(6) -0.006(4) 0.029(5) 0.027(4) C12 0.104(6) 0.050(3) 0.109(6) 0.009(4) 0.017(5) -0.003(3) C13 0.069(4) 0.064(4) 0.090(5) 0.030(3) 0.018(3) 0.000(3) C14 0.053(3) 0.056(3) 0.056(3) 0.014(2) 0.014(2) 0.011(2) C15 0.0351(19) 0.053(2) 0.0355(18) 0.0113(17) 0.0098(15) 0.0220(17) C16 0.052(3) 0.055(3) 0.061(3) 0.007(2) -0.001(2) 0.026(2) C17 0.096(5) 0.076(4) 0.067(3) 0.012(3) 0.006(3) 0.057(4) C18 0.088(4) 0.115(5) 0.066(3) 0.033(4) 0.027(3) 0.077(4) C19 0.046(3) 0.115(5) 0.067(3) 0.043(3) 0.020(2) 0.045(3) C20 0.034(2) 0.072(3) 0.055(3) 0.025(2) 0.0083(18) 0.021(2) C21 0.0385(19) 0.047(2) 0.0324(18) 0.0133(16) 0.0068(15) 0.0151(17) C22 0.0359(19) 0.049(2) 0.0355(19) 0.0106(16) 0.0051(15) 0.0165(17) C23 0.056(3) 0.059(3) 0.0290(19) 0.0112(18) 0.0066(18) 0.017(2) C24 0.151(8) 0.214(11) 0.057(4) 0.050(5) -0.001(5) 0.114(8) C25 0.046(2) 0.046(2) 0.046(2) 0.0106(19) 0.0033(18) 0.0134(19) C26 0.048(3) 0.060(3) 0.105(5) 0.038(3) 0.022(3) 0.013(2) C27 0.075(8) 0.047(6) 0.097(10) 0.025(6) 0.049(7) 0.024(5) C27A 0.051(6) 0.072(7) 0.121(12) 0.021(7) 0.025(7) 0.021(5) C28 0.076(4) 0.058(3) 0.072(4) 0.027(3) 0.021(3) 0.018(3) C29 0.092(8) 0.056(5) 0.078(7) 0.023(5) 0.016(6) 0.040(5) C30 0.063(5) 0.044(4) 0.092(7) 0.028(4) 0.004(5) 0.029(4) C31 0.062(6) 0.083(7) 0.073(7) 0.021(6) 0.007(5) 0.019(5) C32 0.088(8) 0.084(8) 0.082(8) 0.016(6) 0.021(7) 0.035(7) C33 0.137(14) 0.108(10) 0.079(8) 0.027(8) -0.003(8) 0.070(10) C34 0.111(12) 0.090(9) 0.100(11) 0.020(8) -0.033(9) 0.020(8) C35 0.076(8) 0.095(9) 0.097(9) 0.025(7) -0.023(7) 0.026(7) #============================================================================== # MOLECULAR GEOMETRY _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 C6 2.114(5) . ? Rh1 C5 2.116(5) . ? Rh1 C1 2.206(4) . ? Rh1 C2 2.223(5) . ? Rh1 P1 2.3228(10) . ? Rh1 Cl1 2.3650(10) . ? P1 C9 1.821(5) . ? P1 C15 1.822(4) . ? P1 C21 1.845(4) . ? N1 C25 1.334(6) . ? N1 C22 1.440(5) . ? C1 C2 1.386(9) . ? C1 C8 1.494(8) . ? O1 C25 1.205(6) . ? N2 C28 1.350(8) . ? N2 C26 1.441(7) . ? C2 C3 1.492(9) . ? O2 C28 1.199(7) . ? O3 C28 1.342(7) . ? O3 C29A 1.40(3) . ? O3 C29 1.549(13) . ? C3 C4 1.467(10) . ? O4 C23 1.195(6) . ? C4 C5 1.505(8) . ? O5 C23 1.314(6) . ? O5 C24 1.451(7) . ? C5 C6 1.383(9) . ? C6 C7 1.521(8) . ? C7 C8 1.457(9) . ? C9 C10 1.393(7) . ? C9 C14 1.403(7) . ? C10 C11 1.401(9) . ? C11 C12 1.344(11) . ? C12 C13 1.389(11) . ? C13 C14 1.382(8) . ? C15 C16 1.382(7) . ? C15 C20 1.389(6) . ? C16 C17 1.396(7) . ? C17 C18 1.387(10) . ? C18 C19 1.353(10) . ? C19 C20 1.395(7) . ? C21 C22 1.529(6) . ? C22 C23 1.529(6) . ? C25 C26 1.533(7) . ? C26 C27 1.322(13) . ? C26 C27A 1.468(14) . ? C29 C30 1.470(16) . ? C30 C31 1.379(15) . ? C30 C35 1.399(15) . ? C31 C32 1.332(17) . ? C32 C33 1.359(19) . ? C33 C34 1.35(2) . ? C34 C35 1.31(2) . ? C29A C30A 1.58(3) . ? C30A C31A 1.3900 . ? C30A C35A 1.3900 . ? C31A C32A 1.3900 . ? C32A C33A 1.3900 . ? C33A C34A 1.3900 . ? C34A C35A 1.3900 . ? 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 C6 Rh1 C5 38.2(2) . . ? C6 Rh1 C1 81.56(19) . . ? C5 Rh1 C1 91.4(2) . . ? C6 Rh1 C2 94.4(2) . . ? C5 Rh1 C2 80.8(2) . . ? C1 Rh1 C2 36.5(2) . . ? C6 Rh1 P1 90.51(14) . . ? C5 Rh1 P1 95.91(14) . . ? C1 Rh1 P1 156.55(18) . . ? C2 Rh1 P1 166.99(18) . . ? C6 Rh1 Cl1 160.38(19) . . ? C5 Rh1 Cl1 160.81(19) . . ? C1 Rh1 Cl1 90.19(14) . . ? C2 Rh1 Cl1 89.29(15) . . ? P1 Rh1 Cl1 90.13(4) . . ? C9 P1 C15 106.4(2) . . ? C9 P1 C21 97.8(2) . . ? C15 P1 C21 106.39(19) . . ? C9 P1 Rh1 110.85(15) . . ? C15 P1 Rh1 114.85(14) . . ? C21 P1 Rh1 118.67(13) . . ? C25 N1 C22 120.0(4) . . ? C2 C1 C8 125.1(6) . . ? C2 C1 Rh1 72.4(3) . . ? C8 C1 Rh1 110.9(4) . . ? C28 N2 C26 118.2(5) . . ? C1 C2 C3 125.2(7) . . ? C1 C2 Rh1 71.1(3) . . ? C3 C2 Rh1 108.9(4) . . ? C28 O3 C29A 128.9(13) . . ? C28 O3 C29 108.8(6) . . ? C29A O3 C29 31.3(11) . . ? C4 C3 C2 117.3(6) . . ? C3 C4 C5 115.3(5) . . ? C23 O5 C24 116.1(5) . . ? C6 C5 C4 124.2(6) . . ? C6 C5 Rh1 70.8(3) . . ? C4 C5 Rh1 113.9(4) . . ? C5 C6 C7 124.9(6) . . ? C5 C6 Rh1 71.0(3) . . ? C7 C6 Rh1 110.0(4) . . ? C8 C7 C6 117.9(5) . . ? C7 C8 C1 115.3(5) . . ? C10 C9 C14 119.1(5) . . ? C10 C9 P1 119.4(4) . . ? C14 C9 P1 121.4(4) . . ? C9 C10 C11 119.3(6) . . ? C12 C11 C10 121.4(7) . . ? C11 C12 C13 119.9(6) . . ? C14 C13 C12 120.6(6) . . ? C13 C14 C9 119.7(5) . . ? C16 C15 C20 118.3(4) . . ? C16 C15 P1 117.7(3) . . ? C20 C15 P1 123.8(4) . . ? C15 C16 C17 120.8(5) . . ? C18 C17 C16 119.4(6) . . ? C19 C18 C17 120.5(5) . . ? C18 C19 C20 120.1(5) . . ? C15 C20 C19 120.8(5) . . ? C22 C21 P1 117.7(3) . . ? N1 C22 C21 111.7(3) . . ? N1 C22 C23 111.1(3) . . ? C21 C22 C23 108.8(4) . . ? O4 C23 O5 124.4(5) . . ? O4 C23 C22 123.6(5) . . ? O5 C23 C22 112.0(4) . . ? O1 C25 N1 121.9(4) . . ? O1 C25 C26 120.9(5) . . ? N1 C25 C26 117.2(4) . . ? C27 C26 N2 115.0(7) . . ? C27 C26 C27A 72.2(9) . . ? N2 C26 C27A 118.8(7) . . ? C27 C26 C25 121.0(7) . . ? N2 C26 C25 110.5(5) . . ? C27A C26 C25 115.1(7) . . ? O2 C28 O3 125.6(7) . . ? O2 C28 N2 124.4(6) . . ? O3 C28 N2 109.9(6) . . ? C30 C29 O3 115.4(9) . . ? C31 C30 C35 117.2(12) . . ? C31 C30 C29 123.7(10) . . ? C35 C30 C29 119.1(11) . . ? C32 C31 C30 121.2(12) . . ? C31 C32 C33 120.3(14) . . ? C34 C33 C32 118.6(15) . . ? C35 C34 C33 123.0(14) . . ? C34 C35 C30 119.4(14) . . ? O3 C29A C30A 117.7(19) . . ? C31A C30A C35A 120.0 . . ? C31A C30A C29A 123.2(15) . . ? C35A C30A C29A 116.1(15) . . ? C30A C31A C32A 120.0 . . ? C31A C32A C33A 120.0 . . ? C34A C33A C32A 120.0 . . ? C33A C34A C35A 120.0 . . ? C34A C35A C30A 120.0 . . ? data_RhCl(cod)(Z-SerPhos)_8 _database_code_depnum_ccdc_archive 'CCDC 283233' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H36 Cl N O4 P Rh' _chemical_formula_sum 'C32 H36 Cl N O4 P Rh' _chemical_formula_weight 667.95 #============================================================================== # CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.339(16) _cell_length_b 30.582(15) _cell_length_c 9.520(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.55(5) _cell_angle_gamma 90.00 _cell_volume 6212(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 16 _cell_measurement_theta_min 20 _cell_measurement_theta_max 25 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2752 _exptl_absorpt_coefficient_mu 6.015 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.3792 _exptl_absorpt_correction_T_max 0.5846 #============================================================================== # EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'PICKER 4-circle Stoe upgrade' _diffrn_measurement_method ' \w scans' _diffrn_standards_number 1 _diffrn_standards_interval_count 120 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4357 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 42.50 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 42.50 _diffrn_measured_fraction_theta_full 0.993 _reflns_number_total 4357 _reflns_number_gt 2811 _reflns_threshold_expression >2sigma(I) #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0873P)^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 undef _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4357 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0743 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1216 _refine_ls_wR_factor_gt 0.1067 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.563 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.077 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'PICKER STOE DIF4' _computing_cell_refinement 'STOE DIF4' _computing_data_reduction 'STOE REDU4' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXLTL-Plus _computing_publication_material SHELXL-93 #============================================================================== # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Rh Rh 0.17277(3) 0.14943(2) 0.06417(7) 0.0541(3) Uani 1 1 d . . . Cl Cl 0.12551(13) 0.21912(8) 0.0864(3) 0.0807(8) Uani 1 1 d . . . P P 0.18470(11) 0.14791(7) 0.3040(2) 0.0467(7) Uani 1 1 d . . . C2 C 0.0586(4) 0.1518(3) 0.4048(10) 0.053(3) Uani 1 1 d . . . H2A H 0.0604 0.1245 0.4543 0.080 Uiso 1 1 d R . . N N 0.0377(4) 0.1443(3) 0.2627(8) 0.061(2) Uani 1 1 d . . . H0A H 0.0558 0.1588 0.1915 0.080 Uiso 1 1 d R . . C1 C 0.1233(4) 0.1728(3) 0.4119(8) 0.050(2) Uani 1 1 d . . . H1A H 0.1183 0.2025 0.3807 0.080 Uiso 1 1 d R . . H1B H 0.1378 0.1737 0.5077 0.080 Uiso 1 1 d R . . C28 C 0.2092(7) 0.1669(4) -0.1455(9) 0.076(3) Uani 1 1 d . . . H28A H 0.2107 0.1977 -0.1632 0.080 Uiso 1 1 d R . . C19 C 0.2522(3) 0.1798(2) 0.3485(9) 0.055(3) Uani 1 1 d G . . C20 C 0.2566(4) 0.2049(3) 0.4713(8) 0.094(4) Uani 1 1 d G . . H20A H 0.2216 0.2061 0.5337 0.080 Uiso 1 1 d G . . C21 C 0.3116(5) 0.2283(2) 0.5046(8) 0.123(5) Uani 1 1 d G . . H21A H 0.3136 0.2460 0.5877 0.080 Uiso 1 1 d G . . C22 C 0.3640(4) 0.2254(2) 0.4148(12) 0.105(4) Uani 1 1 d G . . H22A H 0.4019 0.2409 0.4378 0.080 Uiso 1 1 d G . . C23 C 0.3608(3) 0.2000(3) 0.2928(10) 0.094(4) Uani 1 1 d G . . H23A H 0.3963 0.1979 0.2322 0.080 Uiso 1 1 d G . . C24 C 0.3044(4) 0.1775(2) 0.2592(6) 0.069(3) Uani 1 1 d G . . H24A H 0.3017 0.1604 0.1746 0.080 Uiso 1 1 d G . . C5' C 0.4308(3) 0.4252(4) 0.9895(7) 0.067(3) Uani 1 1 d G . . C6' C 0.4378(3) 0.4685(3) 1.0330(13) 0.083(3) Uani 1 1 d G . . H6'A H 0.4404 0.4915 0.9646 0.080 Uiso 1 1 d G . . C7' C 0.4408(3) 0.4784(3) 1.1760(15) 0.101(4) Uani 1 1 d G . . H7'A H 0.4456 0.5082 1.2059 0.080 Uiso 1 1 d G . . C8' C 0.4369(4) 0.4450(5) 1.2754(8) 0.101(4) Uani 1 1 d G . . H8'A H 0.4390 0.4518 1.3737 0.080 Uiso 1 1 d G . . C9' C 0.4300(4) 0.4017(4) 1.2318(12) 0.111(5) Uani 1 1 d G . . H9'A H 0.4273 0.3787 1.3002 0.080 Uiso 1 1 d G . . C10' C 0.4269(3) 0.3918(3) 1.0889(14) 0.096(4) Uani 1 1 d G . . H10A H 0.4221 0.3620 1.0590 0.080 Uiso 1 1 d G . . Rh' Rh 0.67813(3) 0.34845(2) 0.84681(7) 0.0525(3) Uani 1 1 d . . . P' P 0.68679(11) 0.35325(7) 0.6072(2) 0.0458(7) Uani 1 1 d . . . Cl' Cl 0.63051(13) 0.27933(8) 0.8170(2) 0.0773(8) Uani 1 1 d . . . O4' O 0.5298(3) 0.3155(2) 0.2890(8) 0.0644(18) Uani 1 1 d . . . N1 N 0.5401(4) 0.3557(3) 0.6445(7) 0.056(2) Uani 1 1 d . . . H0B H 0.5585 0.3414 0.7166 0.080 Uiso 1 1 d R . . C2' C 0.5606(4) 0.3470(3) 0.5012(9) 0.050(2) Uani 1 1 d . . . H2'A H 0.5618 0.3743 0.4518 0.080 Uiso 1 1 d R . . C19' C 0.6988(4) 0.40647(18) 0.5220(6) 0.046(2) Uani 1 1 d G . . C20' C 0.7539(3) 0.4170(3) 0.4521(8) 0.062(3) Uani 1 1 d G . . H20B H 0.7881 0.3966 0.4508 0.080 Uiso 1 1 d G . . C21' C 0.7594(3) 0.4572(3) 0.3841(7) 0.080(3) Uani 1 1 d G . . H21B H 0.7974 0.4644 0.3360 0.080 Uiso 1 1 d G . . C22' C 0.7098(5) 0.48686(19) 0.3860(7) 0.086(4) Uani 1 1 d G . . H22B H 0.7136 0.5145 0.3392 0.080 Uiso 1 1 d G . . C23' C 0.6547(4) 0.4764(2) 0.4558(8) 0.078(3) Uani 1 1 d G . . H23B H 0.6205 0.4968 0.4571 0.080 Uiso 1 1 d G . . C24' C 0.6491(3) 0.4362(3) 0.5238(6) 0.060(3) Uani 1 1 d G . . H24B H 0.6112 0.4289 0.5719 0.080 Uiso 1 1 d G . . O3' O 0.4738(4) 0.2961(3) 0.4774(7) 0.089(2) Uani 1 1 d . . . C13' C 0.7565(3) 0.3224(2) 0.5582(9) 0.057(3) Uani 1 1 d G . . C14' C 0.7601(4) 0.2994(3) 0.4319(8) 0.071(3) Uani 1 1 d G . . H14A H 0.7250 0.2991 0.3681 0.080 Uiso 1 1 d G . . C15' C 0.8147(5) 0.2767(2) 0.3985(8) 0.097(4) Uani 1 1 d G . . H15A H 0.8171 0.2609 0.3116 0.080 Uiso 1 1 d G . . C16' C 0.8656(4) 0.2770(2) 0.4913(12) 0.091(4) Uani 1 1 d G . . H16A H 0.9032 0.2614 0.4683 0.080 Uiso 1 1 d G . . C17' C 0.8621(3) 0.3000(3) 0.6175(10) 0.095(4) Uani 1 1 d G . . H17A H 0.8972 0.3002 0.6814 0.080 Uiso 1 1 d G . . C18' C 0.8075(5) 0.3226(2) 0.6510(6) 0.069(3) Uani 1 1 d G . . H18A H 0.8050 0.3385 0.7379 0.080 Uiso 1 1 d G . . C11' C 0.5159(5) 0.3167(3) 0.4269(12) 0.055(3) Uani 1 1 d . . . C1' C 0.6254(4) 0.3273(3) 0.4992(8) 0.052(3) Uani 1 1 d . . . H1'A H 0.6209 0.2978 0.5320 0.080 Uiso 1 1 d R . . H1'B H 0.6396 0.3260 0.4040 0.080 Uiso 1 1 d R . . C29' C 0.7371(6) 0.4022(3) 0.8803(10) 0.063(3) Uani 1 1 d . . . H29A H 0.7582 0.4119 0.7974 0.080 Uiso 1 1 d R . . C25' C 0.6595(7) 0.3460(4) 1.0770(10) 0.077(3) Uani 1 1 d . . . H25A H 0.6290 0.3243 1.1020 0.080 Uiso 1 1 d R . . C12' C 0.4955(5) 0.2853(3) 0.2024(10) 0.084(3) Uani 1 1 d . . . H12A H 0.5093 0.2876 0.1071 0.080 Uiso 1 1 d R . . H12B H 0.5029 0.2561 0.2361 0.080 Uiso 1 1 d R . . H12C H 0.4515 0.2916 0.2065 0.080 Uiso 1 1 d R . . C27' C 0.6413(6) 0.4247(4) 1.0223(12) 0.102(4) Uani 1 1 d . . . H27A H 0.5980 0.4274 0.9951 0.080 Uiso 1 1 d R . . H27B H 0.6548 0.4522 1.0606 0.080 Uiso 1 1 d R . . O2' O 0.4791(3) 0.3865(2) 0.8037(8) 0.076(2) Uani 1 1 d . . . O1' O 0.4681(4) 0.4061(3) 0.5787(8) 0.110(3) Uani 1 1 d . . . C32 C 0.1717(6) 0.0819(3) 0.0316(10) 0.073(3) Uani 1 1 d . . . H32A H 0.1593 0.0661 0.1138 0.080 Uiso 1 1 d R . . C28' C 0.6760(6) 0.4156(3) 0.8885(10) 0.062(3) Uani 1 1 d . . . H28B H 0.6630 0.4325 0.8083 0.080 Uiso 1 1 d R . . C4' C 0.4277(5) 0.4155(4) 0.8359(10) 0.084(3) Uani 1 1 d . . . H4'A H 0.4304 0.4421 0.7826 0.080 Uiso 1 1 d R . . H4'B H 0.3887 0.4013 0.8141 0.080 Uiso 1 1 d R . . C32' C 0.7163(7) 0.3288(4) 1.0521(10) 0.081(4) Uani 1 1 d . . . H32B H 0.7198 0.2977 1.0625 0.080 Uiso 1 1 d R . . C29 C 0.1509(7) 0.1488(4) -0.1649(10) 0.078(3) Uani 1 1 d . . . H29B H 0.1185 0.1688 -0.1933 0.080 Uiso 1 1 d R . . C31' C 0.7779(6) 0.3523(4) 1.0724(12) 0.095(4) Uani 1 1 d . . . H31A H 0.8112 0.3347 1.0356 0.080 Uiso 1 1 d R . . H31B H 0.7853 0.3556 1.1715 0.080 Uiso 1 1 d R . . C3' C 0.4936(6) 0.3843(4) 0.6648(13) 0.066(3) Uani 1 1 d . . . C31 C 0.1350(6) 0.0702(4) -0.0996(13) 0.105(4) Uani 1 1 d . . . H31C H 0.0917 0.0678 -0.0742 0.080 Uiso 1 1 d R . . H31D H 0.1485 0.0420 -0.1311 0.080 Uiso 1 1 d R . . C30' C 0.7810(6) 0.3960(4) 1.0040(13) 0.106(4) Uani 1 1 d . . . H30A H 0.7687 0.4176 1.0715 0.080 Uiso 1 1 d R . . H30B H 0.8236 0.4020 0.9785 0.080 Uiso 1 1 d R . . C30 C 0.1404(6) 0.1033(5) -0.2153(12) 0.108(4) Uani 1 1 d . . . H30C H 0.1749 0.0949 -0.2732 0.080 Uiso 1 1 d R . . H30D H 0.1030 0.1021 -0.2720 0.080 Uiso 1 1 d R . . C27 C 0.2705(6) 0.1433(4) -0.1636(12) 0.102(4) Uani 1 1 d . . . H27C H 0.3032 0.1615 -0.1254 0.080 Uiso 1 1 d R . . H27D H 0.2785 0.1398 -0.2620 0.080 Uiso 1 1 d R . . C26' C 0.6463(6) 0.3906(4) 1.1314(12) 0.104(4) Uani 1 1 d . . . H26A H 0.6799 0.3985 1.1942 0.080 Uiso 1 1 d R . . H26B H 0.6084 0.3898 1.1851 0.080 Uiso 1 1 d R . . O2 O -0.0232(3) 0.1152(3) 0.1008(10) 0.102(3) Uani 1 1 d . . . O1 O -0.0339(4) 0.0937(3) 0.3226(10) 0.115(3) Uani 1 1 d . . . C5 C -0.0672(4) 0.0721(6) -0.0801(9) 0.086(4) Uani 1 1 d G . . C6 C -0.0714(4) 0.1035(3) -0.1862(18) 0.114(4) Uani 1 1 d G . . H6A H -0.0836 0.1329 -0.1641 0.080 Uiso 1 1 d G . . C7 C -0.0576(5) 0.0921(5) -0.3245(14) 0.155(8) Uani 1 1 d G . . H7A H -0.0604 0.1137 -0.3975 0.080 Uiso 1 1 d G . . C8 C -0.0397(4) 0.0494(6) -0.3566(11) 0.147(8) Uani 1 1 d G . . H8A H -0.0303 0.0416 -0.4518 0.080 Uiso 1 1 d G . . C9 C -0.0356(4) 0.0181(3) -0.251(2) 0.146(7) Uani 1 1 d G . . H9A H -0.0233 -0.0113 -0.2726 0.080 Uiso 1 1 d G . . C10 C -0.0494(4) 0.0294(5) -0.1123(16) 0.121(5) Uani 1 1 d G . . H10B H -0.0466 0.0079 -0.0393 0.080 Uiso 1 1 d G . . C13 C 0.1992(4) 0.09548(18) 0.3937(6) 0.044(2) Uani 1 1 d G . . C14 C 0.2560(3) 0.0885(2) 0.4636(7) 0.055(3) Uani 1 1 d G . . H14B H 0.2879 0.1106 0.4625 0.080 Uiso 1 1 d G . . C15 C 0.2666(3) 0.0493(3) 0.5349(6) 0.069(3) Uani 1 1 d G . . H15B H 0.3057 0.0444 0.5830 0.080 Uiso 1 1 d G . . C16 C 0.2202(5) 0.01709(19) 0.5364(7) 0.070(3) Uani 1 1 d G . . H16B H 0.2275 -0.0099 0.5854 0.080 Uiso 1 1 d G . . C17 C 0.1634(4) 0.0241(2) 0.4665(8) 0.071(3) Uani 1 1 d G . . H17B H 0.1315 0.0020 0.4675 0.080 Uiso 1 1 d G . . C18 C 0.1528(3) 0.0633(3) 0.3951(6) 0.056(3) Uani 1 1 d G . . H18B H 0.1137 0.0682 0.3471 0.080 Uiso 1 1 d G . . C25 C 0.2326(6) 0.0960(3) 0.0380(10) 0.071(3) Uani 1 1 d . . . H25B H 0.2545 0.0876 0.1223 0.080 Uiso 1 1 d R . . C3 C -0.0090(6) 0.1158(5) 0.2381(14) 0.077(3) Uani 1 1 d . . . C26 C 0.2755(6) 0.1005(4) -0.0890(12) 0.100(4) Uani 1 1 d . . . H26C H 0.3183 0.0947 -0.0629 0.080 Uiso 1 1 d R . . H26D H 0.2626 0.0785 -0.1551 0.080 Uiso 1 1 d R . . C4 C -0.0751(6) 0.0879(5) 0.0620(13) 0.136(6) Uani 1 1 d . . . H4A H -0.1139 0.1036 0.0702 0.080 Uiso 1 1 d R . . H4B H -0.0760 0.0628 0.1223 0.080 Uiso 1 1 d R . . O4 O 0.0286(3) 0.1830(2) 0.6194(8) 0.0682(19) Uani 1 1 d . . . C12 C -0.0063(5) 0.2127(3) 0.7054(10) 0.081(3) Uani 1 1 d . . . H12D H 0.0075 0.2100 0.8013 0.080 Uiso 1 1 d R . . H12E H 0.0013 0.2420 0.6733 0.080 Uiso 1 1 d R . . H12F H -0.0503 0.2065 0.6989 0.080 Uiso 1 1 d R . . O3 O -0.0292(4) 0.2027(3) 0.4289(8) 0.090(3) Uani 1 1 d . . . C11 C 0.0132(5) 0.1822(3) 0.4820(13) 0.062(3) 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 Rh 0.0622(6) 0.0537(6) 0.0463(5) 0.0015(4) 0.0020(4) 0.0090(4) Cl 0.105(2) 0.0605(17) 0.0772(18) 0.0150(14) 0.0148(16) 0.0245(16) P 0.0463(16) 0.0444(16) 0.0493(15) -0.0023(12) -0.0003(12) 0.0023(13) C2 0.056(7) 0.054(6) 0.051(7) -0.016(5) -0.002(6) 0.006(6) N 0.050(6) 0.079(6) 0.056(7) -0.021(5) 0.004(4) -0.003(5) C1 0.051(7) 0.056(6) 0.042(6) -0.007(4) -0.001(5) 0.003(5) C28 0.103(10) 0.085(9) 0.042(7) 0.012(6) 0.018(7) 0.009(9) C19 0.063(8) 0.045(6) 0.057(7) 0.012(6) 0.000(6) 0.001(5) C20 0.076(9) 0.109(10) 0.096(10) -0.045(8) -0.012(7) -0.025(8) C21 0.104(12) 0.103(11) 0.161(14) -0.038(9) -0.033(12) -0.019(10) C22 0.100(13) 0.083(10) 0.131(12) 0.019(9) -0.045(10) -0.046(8) C23 0.060(10) 0.100(9) 0.122(12) 0.030(8) -0.007(8) -0.018(8) C24 0.065(8) 0.074(8) 0.067(7) 0.014(6) -0.006(7) -0.017(7) C5' 0.048(7) 0.095(10) 0.060(9) 0.001(9) 0.018(6) 0.018(7) C6' 0.086(9) 0.081(11) 0.082(11) 0.009(7) 0.017(7) -0.005(7) C7' 0.083(9) 0.109(12) 0.112(12) -0.034(12) 0.018(8) -0.010(8) C8' 0.107(10) 0.139(13) 0.056(8) 0.001(11) 0.015(7) 0.034(10) C9' 0.126(11) 0.116(14) 0.090(14) 0.015(8) 0.023(8) 0.073(10) C10' 0.109(10) 0.099(11) 0.078(10) -0.001(10) 0.011(8) 0.031(8) Rh' 0.0652(6) 0.0475(5) 0.0448(5) 0.0012(4) 0.0004(4) -0.0061(4) P' 0.0479(16) 0.0433(15) 0.0462(14) -0.0018(12) 0.0018(12) -0.0014(13) Cl' 0.102(2) 0.0571(17) 0.0723(17) 0.0084(13) -0.0134(15) -0.0208(15) O4' 0.066(5) 0.072(5) 0.056(5) -0.011(4) -0.012(4) -0.009(4) N1 0.046(5) 0.078(6) 0.046(6) -0.003(4) -0.002(4) 0.009(5) C2' 0.049(7) 0.053(6) 0.048(7) -0.001(5) 0.004(5) -0.001(6) C19' 0.062(7) 0.040(6) 0.035(5) -0.001(4) -0.009(5) 0.005(7) C20' 0.050(8) 0.066(8) 0.071(7) 0.010(6) 0.010(6) -0.007(6) C21' 0.090(10) 0.074(9) 0.075(8) 0.014(7) 0.007(6) -0.024(8) C22' 0.128(11) 0.042(8) 0.089(9) 0.012(6) -0.008(8) -0.014(9) C23' 0.098(10) 0.053(9) 0.082(8) -0.019(7) 0.004(7) -0.001(7) C24' 0.078(9) 0.042(7) 0.060(7) 0.010(6) 0.003(5) -0.013(7) O3' 0.070(5) 0.115(6) 0.081(5) 0.003(4) 0.006(4) -0.050(5) C13' 0.063(8) 0.049(7) 0.059(7) 0.014(6) 0.009(7) 0.007(5) C14' 0.060(8) 0.078(8) 0.076(9) -0.025(6) 0.006(6) 0.016(7) C15' 0.102(11) 0.086(9) 0.104(10) -0.023(7) 0.032(10) 0.023(8) C16' 0.089(11) 0.085(9) 0.101(10) 0.035(8) 0.033(9) 0.045(8) C17' 0.069(10) 0.121(11) 0.095(11) 0.037(8) 0.010(7) 0.023(9) C18' 0.062(8) 0.078(8) 0.067(8) -0.005(6) 0.006(8) 0.018(7) C11' 0.048(8) 0.056(7) 0.061(9) -0.013(6) -0.006(7) -0.004(6) C1' 0.048(7) 0.061(6) 0.047(6) 0.000(5) 0.007(5) -0.008(5) C29' 0.089(9) 0.057(7) 0.044(6) 0.004(5) -0.033(7) -0.003(6) C25' 0.115(11) 0.072(10) 0.044(7) 0.002(6) 0.010(7) -0.011(8) C12' 0.081(8) 0.094(8) 0.076(7) -0.031(7) -0.031(7) -0.002(7) C27' 0.147(12) 0.089(9) 0.071(9) -0.007(8) 0.017(8) 0.026(8) O2' 0.069(5) 0.109(6) 0.051(5) -0.004(4) 0.010(4) 0.031(5) O1' 0.119(7) 0.148(8) 0.062(5) 0.026(5) 0.005(5) 0.075(6) C32 0.094(10) 0.068(8) 0.058(8) -0.014(6) 0.007(7) -0.012(7) C28' 0.092(9) 0.048(7) 0.045(7) -0.006(5) -0.017(6) 0.012(6) C4' 0.077(9) 0.112(9) 0.064(9) -0.019(7) 0.024(6) 0.026(8) C32' 0.135(12) 0.065(8) 0.042(7) 0.015(5) -0.027(7) 0.005(10) C29 0.102(11) 0.084(10) 0.048(7) -0.005(6) -0.022(7) 0.035(8) C31' 0.098(10) 0.091(10) 0.094(9) 0.016(7) -0.041(7) -0.017(8) C3' 0.058(9) 0.080(9) 0.060(11) -0.006(7) 0.007(7) 0.006(8) C31 0.130(12) 0.096(10) 0.088(10) -0.036(8) 0.017(9) -0.020(8) C30' 0.123(12) 0.082(10) 0.112(11) 0.004(8) -0.003(9) -0.041(8) C30 0.111(11) 0.147(14) 0.066(9) -0.011(10) -0.009(7) 0.007(9) C27 0.096(11) 0.127(12) 0.084(9) -0.001(8) 0.041(7) 0.001(9) C26' 0.139(12) 0.114(11) 0.060(8) -0.008(9) 0.028(7) -0.008(9) O2 0.066(6) 0.152(8) 0.089(7) -0.042(5) -0.012(5) -0.028(5) O1 0.114(8) 0.128(8) 0.104(7) -0.011(6) 0.012(6) -0.059(6) C5 0.064(8) 0.092(10) 0.102(13) -0.014(11) -0.023(7) -0.004(8) C6 0.118(11) 0.083(10) 0.141(14) 0.003(13) -0.014(11) -0.040(8) C7 0.152(15) 0.22(2) 0.095(14) 0.004(11) 0.029(10) -0.113(15) C8 0.119(13) 0.201(18) 0.120(15) -0.120(17) 0.032(10) -0.035(14) C9 0.135(14) 0.130(14) 0.171(18) -0.046(15) -0.061(15) 0.027(11) C10 0.099(11) 0.17(2) 0.093(13) 0.016(10) -0.054(9) -0.019(11) C13 0.050(7) 0.049(7) 0.034(5) -0.010(4) 0.001(5) 0.009(6) C14 0.055(8) 0.056(8) 0.054(6) 0.014(5) 0.004(6) 0.005(6) C15 0.063(8) 0.071(8) 0.072(8) -0.010(7) -0.003(6) 0.006(8) C16 0.100(10) 0.058(8) 0.052(7) 0.005(5) -0.014(7) 0.011(8) C17 0.084(10) 0.047(8) 0.082(8) 0.010(6) -0.008(7) -0.010(6) C18 0.054(7) 0.055(7) 0.059(7) -0.006(6) 0.002(5) -0.018(7) C25 0.103(10) 0.076(8) 0.036(7) 0.001(5) 0.020(7) 0.013(7) C3 0.061(10) 0.104(11) 0.066(11) -0.027(9) -0.003(8) 0.002(9) C26 0.113(10) 0.090(10) 0.098(10) 0.003(8) 0.009(8) 0.035(8) C4 0.081(11) 0.222(17) 0.106(11) -0.082(11) 0.000(9) -0.043(11) O4 0.070(5) 0.087(5) 0.048(5) -0.017(4) 0.011(4) 0.012(4) C12 0.069(8) 0.087(8) 0.087(8) -0.021(7) 0.025(6) 0.003(7) O3 0.067(5) 0.112(6) 0.092(6) -0.011(5) -0.003(4) 0.055(5) C11 0.056(8) 0.059(8) 0.073(10) -0.019(7) 0.018(7) -0.003(7) #============================================================================== # MOLECULAR GEOMETRY _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 Rh C32 2.088(10) . ? Rh C25 2.091(10) . ? Rh C28 2.214(9) . ? Rh C29 2.226(10) . ? Rh P 2.295(3) . ? Rh Cl 2.368(3) . ? P C19 1.788(6) . ? P C1 1.838(8) . ? P C13 1.841(6) . ? C2 N 1.439(11) . ? C2 C1 1.524(11) . ? C2 C11 1.535(13) . ? C2 H2A 0.9601 . ? N C3 1.344(14) . ? N H0A 0.9000 . ? C1 H1A 0.9600 . ? C1 H1B 0.9601 . ? C28 C29 1.373(14) . ? C28 C27 1.505(15) . ? C28 H28A 0.9601 . ? C19 C20 1.4002 . ? C19 C24 1.4084 . ? C20 C21 1.4080 . ? C20 H20A 0.9601 . ? C21 C22 1.4167 . ? C21 H21A 0.9600 . ? C22 C23 1.3978 . ? C22 H22A 0.9602 . ? C23 C24 1.4214 . ? C23 H23A 0.9601 . ? C24 H24A 0.9600 . ? C5' C10' 1.3949 . ? C5' C6' 1.3950 . ? C5' C4' 1.493(10) . ? C6' C7' 1.3949 . ? C6' H6'A 0.9603 . ? C7' C8' 1.3948 . ? C7' H7'A 0.9604 . ? C8' C9' 1.3950 . ? C8' H8'A 0.9599 . ? C9' C10' 1.3950 . ? C9' H9'A 0.9599 . ? C10' H10A 0.9597 . ? Rh' C29' 2.093(10) . ? Rh' C28' 2.094(9) . ? Rh' C32' 2.194(9) . ? Rh' C25' 2.233(9) . ? Rh' P' 2.295(3) . ? Rh' Cl' 2.361(3) . ? P' C13' 1.827(6) . ? P' C19' 1.838(6) . ? P' C1' 1.838(8) . ? O4' C11' 1.349(11) . ? O4' C12' 1.435(10) . ? N1 C3' 1.338(12) . ? N1 C2' 1.461(10) . ? N1 H0B 0.9001 . ? C2' C11' 1.502(12) . ? C2' C1' 1.508(11) . ? C2' H2'A 0.9600 . ? C19' C20' 1.3948 . ? C19' C24' 1.3951 . ? C20' C21' 1.3950 . ? C20' H20B 0.9599 . ? C21' C22' 1.3947 . ? C21' H21B 0.9600 . ? C22' C23' 1.3950 . ? C22' H22B 0.9601 . ? C23' C24' 1.3947 . ? C23' H23B 0.9599 . ? C24' H24B 0.9601 . ? O3' C11' 1.201(10) . ? C13' C18' 1.3949 . ? C13' C14' 1.3951 . ? C14' C15' 1.3948 . ? C14' H14A 0.9601 . ? C15' C16' 1.3948 . ? C15' H15A 0.9600 . ? C16' C17' 1.3951 . ? C16' H16A 0.9602 . ? C17' C18' 1.3948 . ? C17' H17A 0.9602 . ? C18' H18A 0.9599 . ? C1' H1'A 0.9599 . ? C1' H1'B 0.9600 . ? C29' C28' 1.369(13) . ? C29' C30' 1.510(13) . ? C29' H29A 0.9600 . ? C25' C32' 1.345(14) . ? C25' C26' 1.487(14) . ? C25' H25A 0.9599 . ? C12' H12A 0.9600 . ? C12' H12B 0.9600 . ? C12' H12C 0.9599 . ? C27' C26' 1.475(14) . ? C27' C28' 1.505(13) . ? C27' H27A 0.9600 . ? C27' H27B 0.9600 . ? O2' C3' 1.363(11) . ? O2' C4' 1.446(11) . ? O1' C3' 1.185(12) . ? C32 C25 1.369(13) . ? C32 C31 1.512(14) . ? C32 H32A 0.9600 . ? C28' H28B 0.9599 . ? C4' H4'A 0.9599 . ? C4' H4'B 0.9599 . ? C32' C31' 1.508(15) . ? C32' H32B 0.9600 . ? C29 C30 1.487(14) . ? C29 H29B 0.9601 . ? C31' C30' 1.490(13) . ? C31' H31A 0.9601 . ? C31' H31B 0.9600 . ? C31 C30 1.502(15) . ? C31 H31C 0.9599 . ? C31 H31D 0.9600 . ? C30' H30A 0.9599 . ? C30' H30B 0.9600 . ? C30 H30C 0.9599 . ? C30 H30D 0.9599 . ? C27 C26 1.493(13) . ? C27 H27C 0.9601 . ? C27 H27D 0.9600 . ? C26' H26A 0.9600 . ? C26' H26B 0.9601 . ? O2 C3 1.338(12) . ? O2 C4 1.433(13) . ? O1 C3 1.181(13) . ? C5 C10 1.3948 . ? C5 C6 1.3949 . ? C5 C4 1.449(12) . ? C6 C7 1.3951 . ? C6 H6A 0.9599 . ? C7 C8 1.3949 . ? C7 H7A 0.9601 . ? C8 C9 1.3951 . ? C8 H8A 0.9600 . ? C9 C10 1.3949 . ? C9 H9A 0.9598 . ? C10 H10B 0.9598 . ? C13 C18 1.3948 . ? C13 C14 1.3948 . ? C14 C15 1.3951 . ? C14 H14B 0.9601 . ? C15 C16 1.3951 . ? C15 H15B 0.9599 . ? C16 C17 1.3952 . ? C16 H16B 0.9597 . ? C17 C18 1.3950 . ? C17 H17B 0.9601 . ? C18 H18B 0.9598 . ? C25 C26 1.530(14) . ? C25 H25B 0.9599 . ? C26 H26C 0.9601 . ? C26 H26D 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9599 . ? O4 C11 1.345(12) . ? O4 C12 1.438(10) . ? C12 H12D 0.9600 . ? C12 H12E 0.9601 . ? C12 H12F 0.9600 . ? O3 C11 1.208(11) . ? 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 C32 Rh C25 38.3(4) . . ? C32 Rh C28 96.2(4) . . ? C25 Rh C28 82.0(4) . . ? C32 Rh C29 81.0(4) . . ? C25 Rh C29 89.9(4) . . ? C28 Rh C29 36.0(4) . . ? C32 Rh P 97.4(3) . . ? C25 Rh P 92.3(3) . . ? C28 Rh P 149.9(4) . . ? C29 Rh P 174.0(4) . . ? C32 Rh Cl 154.1(4) . . ? C25 Rh Cl 167.3(4) . . ? C28 Rh Cl 91.0(3) . . ? C29 Rh Cl 90.6(3) . . ? P Rh Cl 88.43(9) . . ? C19 P C1 102.6(4) . . ? C19 P C13 103.5(4) . . ? C1 P C13 102.7(4) . . ? C19 P Rh 107.8(3) . . ? C1 P Rh 118.4(3) . . ? C13 P Rh 119.7(2) . . ? N C2 C1 112.4(8) . . ? N C2 C11 110.8(8) . . ? C1 C2 C11 107.4(7) . . ? N C2 H2A 109.5 . . ? C1 C2 H2A 108.3 . . ? C11 C2 H2A 108.3 . . ? C3 N C2 119.3(9) . . ? C3 N H0A 120.8 . . ? C2 N H0A 119.9 . . ? C2 C1 P 116.8(6) . . ? C2 C1 H1A 106.7 . . ? P C1 H1A 107.2 . . ? C2 C1 H1B 109.6 . . ? P C1 H1B 108.6 . . ? H1A C1 H1B 107.5 . . ? C29 C28 C27 125.5(11) . . ? C29 C28 Rh 72.5(6) . . ? C27 C28 Rh 107.5(7) . . ? C29 C28 H28A 113.8 . . ? C27 C28 H28A 114.8 . . ? Rh C28 H28A 114.0 . . ? C20 C19 C24 119.1 . . ? C20 C19 P 122.9(6) . . ? C24 C19 P 117.9(6) . . ? C19 C20 C21 121.0 . . ? C19 C20 H20A 119.5 . . ? C21 C20 H20A 119.5 . . ? C20 C21 C22 119.6 . . ? C20 C21 H21A 120.2 . . ? C22 C21 H21A 120.2 . . ? C23 C22 C21 120.1 . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 119.9 . . ? C22 C23 C24 119.5 . . ? C22 C23 H23A 120.3 . . ? C24 C23 H23A 120.3 . . ? C19 C24 C23 120.7 . . ? C19 C24 H24A 119.6 . . ? C23 C24 H24A 119.7 . . ? C10' C5' C6' 120.0 . . ? C10' C5' C4' 121.1(11) . . ? C6' C5' C4' 118.9(11) . . ? C7' C6' C5' 120.0 . . ? C7' C6' H6'A 120.0 . . ? C5' C6' H6'A 120.0 . . ? C8' C7' C6' 120.0 . . ? C8' C7' H7'A 120.0 . . ? C6' C7' H7'A 120.0 . . ? C7' C8' C9' 120.0 . . ? C7' C8' H8'A 120.0 . . ? C9' C8' H8'A 120.0 . . ? C8' C9' C10' 120.0 . . ? C8' C9' H9'A 120.0 . . ? C10' C9' H9'A 120.0 . . ? C5' C10' C9' 120.0 . . ? C5' C10' H10A 120.0 . . ? C9' C10' H10A 120.0 . . ? C29' Rh' C28' 38.2(3) . . ? C29' Rh' C32' 82.1(4) . . ? C28' Rh' C32' 96.2(4) . . ? C29' Rh' C25' 89.4(4) . . ? C28' Rh' C25' 80.9(4) . . ? C32' Rh' C25' 35.4(4) . . ? C29' Rh' P' 92.7(3) . . ? C28' Rh' P' 97.3(3) . . ? C32' Rh' P' 150.5(4) . . ? C25' Rh' P' 174.1(4) . . ? C29' Rh' Cl' 168.2(3) . . ? C28' Rh' Cl' 153.0(3) . . ? C32' Rh' Cl' 91.0(3) . . ? C25' Rh' Cl' 90.4(3) . . ? P' Rh' Cl' 88.65(8) . . ? C13' P' C19' 103.2(4) . . ? C13' P' C1' 102.2(4) . . ? C19' P' C1' 103.7(4) . . ? C13' P' Rh' 107.1(3) . . ? C19' P' Rh' 120.6(2) . . ? C1' P' Rh' 117.7(3) . . ? C11' O4' C12' 117.4(8) . . ? C3' N1 C2' 118.9(8) . . ? C3' N1 H0B 121.7 . . ? C2' N1 H0B 119.4 . . ? N1 C2' C11' 110.9(8) . . ? N1 C2' C1' 111.6(7) . . ? C11' C2' C1' 109.1(7) . . ? N1 C2' H2'A 108.0 . . ? C11' C2' H2'A 109.0 . . ? C1' C2' H2'A 108.2 . . ? C20' C19' C24' 120.0 . . ? C20' C19' P' 122.4(6) . . ? C24' C19' P' 117.5(6) . . ? C19' C20' C21' 120.0 . . ? C19' C20' H20B 120.0 . . ? C21' C20' H20B 120.0 . . ? C22' C21' C20' 120.0 . . ? C22' C21' H21B 120.0 . . ? C20' C21' H21B 120.0 . . ? C21' C22' C23' 120.0 . . ? C21' C22' H22B 120.0 . . ? C23' C22' H22B 120.0 . . ? C24' C23' C22' 120.0 . . ? C24' C23' H23B 120.0 . . ? C22' C23' H23B 120.0 . . ? C23' C24' C19' 120.0 . . ? C23' C24' H24B 120.0 . . ? C19' C24' H24B 120.0 . . ? C18' C13' C14' 120.0 . . ? C18' C13' P' 117.8(7) . . ? C14' C13' P' 122.1(7) . . ? C15' C14' C13' 120.0 . . ? C15' C14' H14A 120.0 . . ? C13' C14' H14A 120.0 . . ? C14' C15' C16' 120.0 . . ? C14' C15' H15A 120.0 . . ? C16' C15' H15A 120.0 . . ? C15' C16' C17' 120.0 . . ? C15' C16' H16A 120.0 . . ? C17' C16' H16A 120.0 . . ? C18' C17' C16' 120.0 . . ? C18' C17' H17A 120.0 . . ? C16' C17' H17A 120.0 . . ? C17' C18' C13' 120.0 . . ? C17' C18' H18A 120.0 . . ? C13' C18' H18A 120.0 . . ? O3' C11' O4' 123.2(9) . . ? O3' C11' C2' 127.5(10) . . ? O4' C11' C2' 109.3(9) . . ? C2' C1' P' 118.0(6) . . ? C2' C1' H1'A 106.1 . . ? P' C1' H1'A 107.3 . . ? C2' C1' H1'B 109.0 . . ? P' C1' H1'B 108.4 . . ? H1'A C1' H1'B 107.5 . . ? C28' C29' C30' 125.3(10) . . ? C28' C29' Rh' 70.9(6) . . ? C30' C29' Rh' 112.8(6) . . ? C28' C29' H29A 114.1 . . ? C30' C29' H29A 112.8 . . ? Rh' C29' H29A 113.8 . . ? C32' C25' C26' 126.4(11) . . ? C32' C25' Rh' 70.8(6) . . ? C26' C25' Rh' 110.3(7) . . ? C32' C25' H25A 112.8 . . ? C26' C25' H25A 114.6 . . ? Rh' C25' H25A 113.2 . . ? O4' C12' H12A 109.6 . . ? O4' C12' H12B 109.0 . . ? H12A C12' H12B 109.5 . . ? O4' C12' H12C 109.8 . . ? H12A C12' H12C 109.5 . . ? H12B C12' H12C 109.5 . . ? C26' C27' C28' 115.7(9) . . ? C26' C27' H27A 108.4 . . ? C28' C27' H27A 105.5 . . ? C26' C27' H27B 109.4 . . ? C28' C27' H27B 109.5 . . ? H27A C27' H27B 108.0 . . ? C3' O2' C4' 114.6(8) . . ? C25 C32 C31 126.6(10) . . ? C25 C32 Rh 71.0(6) . . ? C31 C32 Rh 111.2(7) . . ? C25 C32 H32A 113.1 . . ? C31 C32 H32A 114.1 . . ? Rh C32 H32A 112.4 . . ? C29' C28' C27' 125.4(10) . . ? C29' C28' Rh' 70.9(6) . . ? C27' C28' Rh' 110.6(7) . . ? C29' C28' H28B 112.6 . . ? C27' C28' H28B 115.7 . . ? Rh' C28' H28B 112.5 . . ? O2' C4' C5' 107.6(8) . . ? O2' C4' H4'A 111.0 . . ? C5' C4' H4'A 110.3 . . ? O2' C4' H4'B 109.5 . . ? C5' C4' H4'B 109.4 . . ? H4'A C4' H4'B 109.0 . . ? C25' C32' C31' 125.3(11) . . ? C25' C32' Rh' 73.9(6) . . ? C31' C32' Rh' 107.4(7) . . ? C25' C32' H32B 116.0 . . ? C31' C32' H32B 113.1 . . ? Rh' C32' H32B 113.0 . . ? C28 C29 C30 123.6(11) . . ? C28 C29 Rh 71.5(6) . . ? C30 C29 Rh 110.7(7) . . ? C28 C29 H29B 115.4 . . ? C30 C29 H29B 113.6 . . ? Rh C29 H29B 114.5 . . ? C30' C31' C32' 114.5(9) . . ? C30' C31' H31A 108.0 . . ? C32' C31' H31A 109.4 . . ? C30' C31' H31B 109.2 . . ? C32' C31' H31B 108.1 . . ? H31A C31' H31B 107.5 . . ? O1' C3' N1 127.2(11) . . ? O1' C3' O2' 122.4(11) . . ? N1 C3' O2' 110.4(11) . . ? C30 C31 C32 113.8(10) . . ? C30 C31 H31C 108.5 . . ? C32 C31 H31C 107.6 . . ? C30 C31 H31D 110.6 . . ? C32 C31 H31D 108.4 . . ? H31C C31 H31D 107.7 . . ? C31' C30' C29' 115.1(9) . . ? C31' C30' H30A 108.1 . . ? C29' C30' H30A 105.3 . . ? C31' C30' H30B 109.1 . . ? C29' C30' H30B 111.2 . . ? H30A C30' H30B 107.7 . . ? C29 C30 C31 114.0(9) . . ? C29 C30 H30C 108.8 . . ? C31 C30 H30C 107.7 . . ? C29 C30 H30D 109.9 . . ? C31 C30 H30D 108.4 . . ? H30C C30 H30D 107.8 . . ? C26 C27 C28 115.0(9) . . ? C26 C27 H27C 106.2 . . ? C28 C27 H27C 107.9 . . ? C26 C27 H27D 110.7 . . ? C28 C27 H27D 109.1 . . ? H27C C27 H27D 107.5 . . ? C27' C26' C25' 114.6(9) . . ? C27' C26' H26A 108.0 . . ? C25' C26' H26A 107.7 . . ? C27' C26' H26B 109.6 . . ? C25' C26' H26B 109.1 . . ? H26A C26' H26B 107.6 . . ? C3 O2 C4 115.2(10) . . ? C10 C5 C6 120.0 . . ? C10 C5 C4 123.5(15) . . ? C6 C5 C4 116.1(15) . . ? C5 C6 C7 120.0 . . ? C5 C6 H6A 120.0 . . ? C7 C6 H6A 120.0 . . ? C8 C7 C6 120.0 . . ? C8 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? C7 C8 C9 120.0 . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? C10 C9 C8 120.0 . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C5 C10 C9 120.0 . . ? C5 C10 H10B 120.0 . . ? C9 C10 H10B 120.0 . . ? C18 C13 C14 120.0 . . ? C18 C13 P 120.2(6) . . ? C14 C13 P 119.8(6) . . ? C13 C14 C15 120.0 . . ? C13 C14 H14B 120.0 . . ? C15 C14 H14B 120.0 . . ? C16 C15 C14 120.0 . . ? C16 C15 H15B 120.0 . . ? C14 C15 H15B 120.0 . . ? C15 C16 C17 120.0 . . ? C15 C16 H16B 120.0 . . ? C17 C16 H16B 120.0 . . ? C18 C17 C16 120.0 . . ? C18 C17 H17B 120.0 . . ? C16 C17 H17B 120.0 . . ? C13 C18 C17 120.0 . . ? C13 C18 H18B 120.0 . . ? C17 C18 H18B 120.0 . . ? C32 C25 C26 124.6(10) . . ? C32 C25 Rh 70.8(6) . . ? C26 C25 Rh 113.2(7) . . ? C32 C25 H25B 114.1 . . ? C26 C25 H25B 113.2 . . ? Rh C25 H25B 113.8 . . ? O1 C3 O2 124.0(14) . . ? O1 C3 N 126.2(12) . . ? O2 C3 N 109.8(12) . . ? C27 C26 C25 114.5(9) . . ? C27 C26 H26C 110.3 . . ? C25 C26 H26C 110.7 . . ? C27 C26 H26D 106.5 . . ? C25 C26 H26D 106.5 . . ? H26C C26 H26D 107.9 . . ? O2 C4 C5 109.8(10) . . ? O2 C4 H4A 110.7 . . ? C5 C4 H4A 110.5 . . ? O2 C4 H4B 109.4 . . ? C5 C4 H4B 107.1 . . ? H4A C4 H4B 109.2 . . ? C11 O4 C12 116.2(8) . . ? O4 C12 H12D 109.4 . . ? O4 C12 H12E 108.6 . . ? H12D C12 H12E 109.5 . . ? O4 C12 H12F 110.4 . . ? H12D C12 H12F 109.5 . . ? H12E C12 H12F 109.5 . . ? O3 C11 O4 125.0(9) . . ? O3 C11 C2 126.0(11) . . ? O4 C11 C2 109.0(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 C32 Rh P C19 125.1(4) . . . . ? C25 Rh P C19 87.0(4) . . . . ? C28 Rh P C19 9.1(7) . . . . ? Cl Rh P C19 -80.2(3) . . . . ? C32 Rh P C1 -119.2(5) . . . . ? C25 Rh P C1 -157.3(5) . . . . ? C28 Rh P C1 124.7(7) . . . . ? Cl Rh P C1 35.5(3) . . . . ? C32 Rh P C13 7.3(5) . . . . ? C25 Rh P C13 -30.8(5) . . . . ? C28 Rh P C13 -108.8(7) . . . . ? Cl Rh P C13 161.9(3) . . . . ? C1 C2 N C3 161.7(8) . . . . ? C11 C2 N C3 -78.1(10) . . . . ? N C2 C1 P -48.5(9) . . . . ? C11 C2 C1 P -170.6(7) . . . . ? C19 P C1 C2 -177.2(6) . . . . ? C13 P C1 C2 -70.0(7) . . . . ? Rh P C1 C2 64.3(7) . . . . ? C32 Rh C28 C29 65.4(7) . . . . ? C25 Rh C28 C29 101.1(7) . . . . ? P Rh C28 C29 -178.2(5) . . . . ? Cl Rh C28 C29 -89.6(7) . . . . ? C32 Rh C28 C27 -57.1(9) . . . . ? C25 Rh C28 C27 -21.5(9) . . . . ? C29 Rh C28 C27 -122.6(11) . . . . ? P Rh C28 C27 59.2(11) . . . . ? Cl Rh C28 C27 147.8(8) . . . . ? C1 P C19 C20 19.9(5) . . . . ? C13 P C19 C20 -86.6(4) . . . . ? Rh P C19 C20 145.6(3) . . . . ? C1 P C19 C24 -163.8(4) . . . . ? C13 P C19 C24 89.7(4) . . . . ? Rh P C19 C24 -38.1(4) . . . . ? C24 C19 C20 C21 1.4 . . . . ? P C19 C20 C21 177.6(5) . . . . ? C19 C20 C21 C22 -1.9 . . . . ? C20 C21 C22 C23 1.0 . . . . ? C21 C22 C23 C24 0.5 . . . . ? C20 C19 C24 C23 0.1 . . . . ? P C19 C24 C23 -176.4(4) . . . . ? C22 C23 C24 C19 -1.0 . . . . ? C10' C5' C6' C7' 0.0 . . . . ? C4' C5' C6' C7' -180.0(7) . . . . ? C5' C6' C7' C8' 0.0 . . . . ? C6' C7' C8' C9' 0.0 . . . . ? C7' C8' C9' C10' 0.0 . . . . ? C6' C5' C10' C9' 0.0 . . . . ? C4' C5' C10' C9' 180.0(7) . . . . ? C8' C9' C10' C5' 0.0 . . . . ? C29' Rh' P' C13' 86.5(4) . . . . ? C28' Rh' P' C13' 124.6(4) . . . . ? C32' Rh' P' C13' 7.9(7) . . . . ? Cl' Rh' P' C13' -81.8(3) . . . . ? C29' Rh' P' C19' -30.8(5) . . . . ? C28' Rh' P' C19' 7.2(5) . . . . ? C32' Rh' P' C19' -109.5(7) . . . . ? Cl' Rh' P' C19' 160.9(4) . . . . ? C29' Rh' P' C1' -159.2(5) . . . . ? C28' Rh' P' C1' -121.1(5) . . . . ? C32' Rh' P' C1' 122.2(7) . . . . ? Cl' Rh' P' C1' 32.5(3) . . . . ? C3' N1 C2' C11' -78.0(10) . . . . ? C3' N1 C2' C1' 160.2(8) . . . . ? C13' P' C19' C20' -5.6(5) . . . . ? C1' P' C19' C20' -111.9(4) . . . . ? Rh' P' C19' C20' 113.7(3) . . . . ? C13' P' C19' C24' 171.7(4) . . . . ? C1' P' C19' C24' 65.4(4) . . . . ? Rh' P' C19' C24' -68.9(4) . . . . ? C24' C19' C20' C21' 0.0 . . . . ? P' C19' C20' C21' 177.3(4) . . . . ? C19' C20' C21' C22' 0.0 . . . . ? C20' C21' C22' C23' 0.0 . . . . ? C21' C22' C23' C24' 0.0 . . . . ? C22' C23' C24' C19' 0.0 . . . . ? C20' C19' C24' C23' 0.0 . . . . ? P' C19' C24' C23' -177.4(4) . . . . ? C19' P' C13' C18' 93.8(4) . . . . ? C1' P' C13' C18' -158.8(4) . . . . ? Rh' P' C13' C18' -34.5(4) . . . . ? C19' P' C13' C14' -85.5(4) . . . . ? C1' P' C13' C14' 22.0(5) . . . . ? Rh' P' C13' C14' 146.3(3) . . . . ? C18' C13' C14' C15' 0.0 . . . . ? P' C13' C14' C15' 179.2(5) . . . . ? C13' C14' C15' C16' 0.0 . . . . ? C14' C15' C16' C17' 0.0 . . . . ? C15' C16' C17' C18' 0.0 . . . . ? C16' C17' C18' C13' 0.0 . . . . ? C14' C13' C18' C17' 0.0 . . . . ? P' C13' C18' C17' -179.3(4) . . . . ? C12' O4' C11' O3' -5.2(13) . . . . ? C12' O4' C11' C2' 174.6(7) . . . . ? N1 C2' C11' O3' -11.0(13) . . . . ? C1' C2' C11' O3' 112.3(11) . . . . ? N1 C2' C11' O4' 169.2(7) . . . . ? C1' C2' C11' O4' -67.5(9) . . . . ? N1 C2' C1' P' -47.5(9) . . . . ? C11' C2' C1' P' -170.4(7) . . . . ? C13' P' C1' C2' -174.6(6) . . . . ? C19' P' C1' C2' -67.5(7) . . . . ? Rh' P' C1' C2' 68.4(7) . . . . ? C32' Rh' C29' C28' -110.8(7) . . . . ? C25' Rh' C29' C28' -76.0(7) . . . . ? P' Rh' C29' C28' 98.4(6) . . . . ? Cl' Rh' C29' C28' -165.1(11) . . . . ? C28' Rh' C29' C30' 121.2(12) . . . . ? C32' Rh' C29' C30' 10.4(9) . . . . ? C25' Rh' C29' C30' 45.1(10) . . . . ? P' Rh' C29' C30' -140.4(9) . . . . ? Cl' Rh' C29' C30' -44(2) . . . . ? C29' Rh' C25' C32' -77.0(7) . . . . ? C28' Rh' C25' C32' -114.4(8) . . . . ? Cl' Rh' C25' C32' 91.2(7) . . . . ? C29' Rh' C25' C26' 45.7(9) . . . . ? C28' Rh' C25' C26' 8.3(9) . . . . ? C32' Rh' C25' C26' 122.8(12) . . . . ? Cl' Rh' C25' C26' -146.0(9) . . . . ? C28 Rh C32 C25 68.7(7) . . . . ? C29 Rh C32 C25 101.5(7) . . . . ? P Rh C32 C25 -84.4(6) . . . . ? Cl Rh C32 C25 173.9(5) . . . . ? C25 Rh C32 C31 -122.9(11) . . . . ? C28 Rh C32 C31 -54.2(9) . . . . ? C29 Rh C32 C31 -21.4(8) . . . . ? P Rh C32 C31 152.8(8) . . . . ? Cl Rh C32 C31 51.0(12) . . . . ? C30' C29' C28' C27' -2.8(16) . . . . ? Rh' C29' C28' C27' 102.2(10) . . . . ? C30' C29' C28' Rh' -105.0(9) . . . . ? C26' C27' C28' C29' -48.6(16) . . . . ? C26' C27' C28' Rh' 32.1(14) . . . . ? C32' Rh' C28' C29' 68.7(7) . . . . ? C25' Rh' C28' C29' 100.7(7) . . . . ? P' Rh' C28' C29' -85.0(6) . . . . ? Cl' Rh' C28' C29' 173.4(5) . . . . ? C29' Rh' C28' C27' -121.7(11) . . . . ? C32' Rh' C28' C27' -53.0(9) . . . . ? C25' Rh' C28' C27' -21.0(9) . . . . ? P' Rh' C28' C27' 153.3(8) . . . . ? Cl' Rh' C28' C27' 51.7(11) . . . . ? C3' O2' C4' C5' -162.4(9) . . . . ? C10' C5' C4' O2' -59.7(9) . . . . ? C6' C5' C4' O2' 120.3(7) . . . . ? C26' C25' C32' C31' -1.3(17) . . . . ? Rh' C25' C32' C31' 100.2(10) . . . . ? C26' C25' C32' Rh' -101.5(10) . . . . ? C29' Rh' C32' C25' 100.3(8) . . . . ? C28' Rh' C32' C25' 64.7(8) . . . . ? P' Rh' C32' C25' -178.3(5) . . . . ? Cl' Rh' C32' C25' -89.3(7) . . . . ? C29' Rh' C32' C31' -22.4(9) . . . . ? C28' Rh' C32' C31' -57.9(9) . . . . ? C25' Rh' C32' C31' -122.7(11) . . . . ? P' Rh' C32' C31' 59.0(11) . . . . ? Cl' Rh' C32' C31' 148.1(8) . . . . ? C27 C28 C29 C30 -3.7(16) . . . . ? Rh C28 C29 C30 -103.1(10) . . . . ? C27 C28 C29 Rh 99.4(10) . . . . ? C32 Rh C29 C28 -113.7(7) . . . . ? C25 Rh C29 C28 -76.4(7) . . . . ? Cl Rh C29 C28 90.9(7) . . . . ? C32 Rh C29 C30 6.1(9) . . . . ? C25 Rh C29 C30 43.5(9) . . . . ? C28 Rh C29 C30 119.8(12) . . . . ? Cl Rh C29 C30 -149.2(9) . . . . ? C25' C32' C31' C30' -50.9(15) . . . . ? Rh' C32' C31' C30' 31.4(13) . . . . ? C2' N1 C3' O1' -4.4(16) . . . . ? C2' N1 C3' O2' 177.1(7) . . . . ? C4' O2' C3' O1' 3.6(14) . . . . ? C4' O2' C3' N1 -177.9(8) . . . . ? C25 C32 C31 C30 -47.2(16) . . . . ? Rh C32 C31 C30 34.3(13) . . . . ? C32' C31' C30' C29' -24.7(16) . . . . ? C28' C29' C30' C31' 86.4(14) . . . . ? Rh' C29' C30' C31' 4.2(14) . . . . ? C28 C29 C30 C31 91.8(14) . . . . ? Rh C29 C30 C31 10.7(14) . . . . ? C32 C31 C30 C29 -29.5(16) . . . . ? C29 C28 C27 C26 -50.0(15) . . . . ? Rh C28 C27 C26 30.6(13) . . . . ? C28' C27' C26' C25' -25.5(17) . . . . ? C32' C25' C26' C27' 87.2(15) . . . . ? Rh' C25' C26' C27' 6.6(14) . . . . ? C10 C5 C6 C7 0.0 . . . . ? C4 C5 C6 C7 172.9(8) . . . . ? C5 C6 C7 C8 0.0 . . . . ? C6 C7 C8 C9 0.0 . . . . ? C7 C8 C9 C10 0.0 . . . . ? C6 C5 C10 C9 0.0 . . . . ? C4 C5 C10 C9 -172.4(9) . . . . ? C8 C9 C10 C5 0.0 . . . . ? C19 P C13 C18 173.3(4) . . . . ? C1 P C13 C18 66.8(4) . . . . ? Rh P C13 C18 -66.7(4) . . . . ? C19 P C13 C14 -5.0(5) . . . . ? C1 P C13 C14 -111.4(4) . . . . ? Rh P C13 C14 115.0(3) . . . . ? C18 C13 C14 C15 0.0 . . . . ? P C13 C14 C15 178.3(4) . . . . ? C13 C14 C15 C16 0.0 . . . . ? C14 C15 C16 C17 0.0 . . . . ? C15 C16 C17 C18 0.0 . . . . ? C14 C13 C18 C17 0.0 . . . . ? P C13 C18 C17 -178.3(4) . . . . ? C16 C17 C18 C13 0.0 . . . . ? C31 C32 C25 C26 -2.7(18) . . . . ? Rh C32 C25 C26 -105.4(10) . . . . ? C31 C32 C25 Rh 102.7(11) . . . . ? C28 Rh C25 C32 -110.7(7) . . . . ? C29 Rh C25 C32 -75.5(7) . . . . ? P Rh C25 C32 99.0(6) . . . . ? Cl Rh C25 C32 -167.8(10) . . . . ? C32 Rh C25 C26 120.3(12) . . . . ? C28 Rh C25 C26 9.6(9) . . . . ? C29 Rh C25 C26 44.8(9) . . . . ? P Rh C25 C26 -140.7(9) . . . . ? Cl Rh C25 C26 -47.5(18) . . . . ? C4 O2 C3 O1 4.6(17) . . . . ? C4 O2 C3 N -176.4(10) . . . . ? C2 N C3 O1 -4.0(17) . . . . ? C2 N C3 O2 177.0(8) . . . . ? C28 C27 C26 C25 -24.5(16) . . . . ? C32 C25 C26 C27 86.6(14) . . . . ? Rh C25 C26 C27 4.6(14) . . . . ? C3 O2 C4 C5 -151.0(12) . . . . ? C10 C5 C4 O2 105.0(11) . . . . ? C6 C5 C4 O2 -67.7(12) . . . . ? C12 O4 C11 O3 -3.9(14) . . . . ? C12 O4 C11 C2 175.1(7) . . . . ? N C2 C11 O3 -10.4(14) . . . . ? C1 C2 C11 O3 112.7(11) . . . . ? N C2 C11 O4 170.5(7) . . . . ? C1 C2 C11 O4 -66.4(9) . . . . ? #============================================================================== # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. data_RhCl(cod)(Boc_SerPhos)_9 _database_code_depnum_ccdc_archive 'CCDC 283234' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H38 Cl N1 O4 P Rh, 0.5 C2H3N' _chemical_formula_sum 'C30 H39.50 Cl N1.50 O4 P Rh' _chemical_formula_weight 654.46 #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.575(8) _cell_length_b 10.255(5) _cell_length_c 19.572(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.06(4) _cell_angle_gamma 90.00 _cell_volume 3126(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 16 _cell_measurement_theta_min 20 _cell_measurement_theta_max 25 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1356 _exptl_absorpt_coefficient_mu 5.965 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.3817 _exptl_absorpt_correction_T_max 0.5869 #============================================================================== # EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'PICKER 4-circle Stoe upgrade' _diffrn_measurement_method ' \w scans' _diffrn_standards_number 1 _diffrn_standards_interval_count 120 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2998 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 49.98 _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 49.98 _diffrn_measured_fraction_theta_full 0.934 _reflns_number_total 2998 _reflns_number_gt 2345 _reflns_threshold_expression >2sigma(I) #============================================================================== # REFINEMENT DATA _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^)+(0.0775P)^2^+1.8616P] 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 undef _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2998 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0664 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1193 _refine_ls_wR_factor_gt 0.1099 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.002 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.080 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'PICKER STOE DIF4' _computing_cell_refinement 'STOE DIF4' _computing_data_reduction 'STOE REDU4' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXLTL-Plus _computing_publication_material SHELXL-93 #============================================================================== # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Rh Rh 0.14664(3) 0.06953(5) 0.23585(3) 0.0460(2) Uani 1 1 d . . . Cl Cl 0.08984(12) -0.12899(16) 0.28061(9) 0.0588(5) Uani 1 1 d . . . P P 0.13195(11) 0.15276(16) 0.34355(8) 0.0412(5) Uani 1 1 d . . . O3 O 0.3337(4) -0.1291(7) 0.4695(3) 0.096(2) Uani 1 1 d . . . O4 O 0.3692(5) 0.0837(8) 0.4790(4) 0.113(2) Uani 1 1 d . . . O5 O 0.4315(4) -0.0928(5) 0.3296(3) 0.0752(16) Uani 1 1 d . . . O6 O 0.3451(3) -0.2359(6) 0.2715(3) 0.0771(16) Uani 1 1 d . . . N N 0.2861(4) -0.0864(5) 0.3365(3) 0.0565(16) Uani 1 1 d . . . H0A H 0.2191 -0.1231 0.3235 0.085 Uiso 1 1 d R . . C1 C 0.1935(4) 0.0532(6) 0.4053(3) 0.0471(18) Uani 1 1 d . . . H1A H 0.1634 -0.0275 0.4123 0.071 Uiso 1 1 d R . . H1B H 0.1953 0.0983 0.4482 0.071 Uiso 1 1 d R . . C2 C 0.2858(4) 0.0198(7) 0.3843(3) 0.0490(18) Uani 1 1 d . . . H2A H 0.3119 0.0951 0.3639 0.074 Uiso 1 1 d R . . C3 C 0.3339(5) -0.0154(10) 0.4489(4) 0.064(2) Uani 1 1 d . . . C4 C 0.4099(13) 0.074(2) 0.5427(9) 0.106(8) Uani 0.50 1 d P . . H4A H 0.4333 0.1560 0.5568 0.159 Uiso 0.50 1 d PR . . H4B H 0.3675 0.0458 0.5752 0.159 Uiso 0.50 1 d PR . . H4C H 0.4550 0.0100 0.5404 0.159 Uiso 0.50 1 d PR . . C5 C 0.3624(6) -0.1334(8) 0.3136(4) 0.060(2) Uani 1 1 d . . . C6 C 0.4140(5) -0.3267(8) 0.2503(4) 0.069(2) Uani 1 1 d . . . C7 C 0.3639(7) -0.4327(10) 0.2139(6) 0.115(4) Uani 1 1 d . . . H7A H 0.3366 -0.3973 0.1740 0.173 Uiso 1 1 d R . . H7B H 0.4021 -0.5017 0.2007 0.173 Uiso 1 1 d R . . H7C H 0.3211 -0.4663 0.2444 0.173 Uiso 1 1 d R . . C8 C 0.4756(7) -0.2595(11) 0.2037(5) 0.117(4) Uani 1 1 d . . . H8A H 0.5056 -0.1936 0.2291 0.176 Uiso 1 1 d R . . H8B H 0.5162 -0.3214 0.1860 0.176 Uiso 1 1 d R . . H8C H 0.4450 -0.2197 0.1666 0.176 Uiso 1 1 d R . . C9 C 0.4572(6) -0.3802(10) 0.3129(5) 0.096(3) Uani 1 1 d . . . H9A H 0.4891 -0.3126 0.3354 0.144 Uiso 1 1 d R . . H9B H 0.4144 -0.4137 0.3435 0.144 Uiso 1 1 d R . . H9C H 0.4954 -0.4492 0.2998 0.144 Uiso 1 1 d R . . C10 C 0.0252(5) 0.1475(6) 0.3797(4) 0.0451(18) Uani 1 1 d . . . C11 C -0.0444(5) 0.1120(7) 0.3410(4) 0.058(2) Uani 1 1 d . . . H11A H -0.0360 0.0892 0.2939 0.086 Uiso 1 1 d R . . C12 C -0.1261(6) 0.1081(9) 0.3690(6) 0.081(3) Uani 1 1 d . . . H12A H -0.1737 0.0785 0.3420 0.121 Uiso 1 1 d R . . C13 C -0.1379(6) 0.1468(9) 0.4358(6) 0.082(3) Uani 1 1 d . . . H13A H -0.1946 0.1472 0.4548 0.123 Uiso 1 1 d R . . C14 C -0.0709(7) 0.1837(9) 0.4737(5) 0.081(3) Uani 1 1 d . . . H14A H -0.0794 0.2099 0.5203 0.122 Uiso 1 1 d R . . C15 C 0.0097(5) 0.1856(8) 0.4472(4) 0.067(2) Uani 1 1 d . . . H15A H 0.0573 0.2133 0.4749 0.100 Uiso 1 1 d R . . C16 C 0.1651(5) 0.3197(6) 0.3628(3) 0.0424(17) Uani 1 1 d . . . C17 C 0.2364(5) 0.3525(7) 0.4016(4) 0.058(2) Uani 1 1 d . . . H17A H 0.2720 0.2837 0.4190 0.087 Uiso 1 1 d R . . C18 C 0.2569(5) 0.4813(8) 0.4157(4) 0.069(2) Uani 1 1 d . . . H18A H 0.3065 0.5025 0.4427 0.103 Uiso 1 1 d R . . C19 C 0.2066(7) 0.5791(8) 0.3899(5) 0.077(3) Uani 1 1 d . . . H19A H 0.2202 0.6687 0.3989 0.116 Uiso 1 1 d R . . C20 C 0.1353(6) 0.5488(8) 0.3508(5) 0.075(3) Uani 1 1 d . . . H20A H 0.1003 0.6179 0.3330 0.112 Uiso 1 1 d R . . C21 C 0.1142(5) 0.4215(7) 0.3379(4) 0.060(2) Uani 1 1 d . . . H21A H 0.0641 0.4003 0.3115 0.090 Uiso 1 1 d R . . C22 C 0.2314(6) 0.2177(8) 0.2056(4) 0.068(2) Uani 1 1 d . . . H22A H 0.2514 0.2709 0.2427 0.102 Uiso 1 1 d R . . C23 C 0.1494(7) 0.2481(7) 0.1834(4) 0.071(3) Uani 1 1 d . . . H23A H 0.1235 0.3181 0.2086 0.106 Uiso 1 1 d R . . C24 C 0.1179(9) 0.2364(10) 0.1113(4) 0.119(4) Uani 1 1 d . . . H24A H 0.1571 0.2837 0.0827 0.179 Uiso 1 1 d R . . H24B H 0.0634 0.2800 0.1088 0.179 Uiso 1 1 d R . . C25 C 0.1078(7) 0.1072(9) 0.0830(5) 0.089(3) Uani 1 1 d . . . H25A H 0.1433 0.1005 0.0430 0.133 Uiso 1 1 d R . . H25B H 0.0493 0.0974 0.0684 0.133 Uiso 1 1 d R . . C26 C 0.1292(6) -0.0056(8) 0.1302(4) 0.062(2) Uani 1 1 d . . . H26A H 0.0927 -0.0808 0.1266 0.094 Uiso 1 1 d R . . C27 C 0.2113(7) -0.0343(8) 0.1512(4) 0.074(3) Uani 1 1 d . . . H27A H 0.2217 -0.1245 0.1613 0.111 Uiso 1 1 d R . . C28 C 0.2903(7) 0.0386(11) 0.1318(6) 0.103(3) Uani 1 1 d . . . H28A H 0.2907 0.0456 0.0829 0.154 Uiso 1 1 d R . . H28B H 0.3392 -0.0128 0.1447 0.154 Uiso 1 1 d R . . C29 C 0.3012(7) 0.1672(13) 0.1597(7) 0.146(5) Uani 1 1 d . . . H29A H 0.3544 0.1691 0.1845 0.219 Uiso 1 1 d R . . H29B H 0.3064 0.2276 0.1224 0.219 Uiso 1 1 d R . . C1N C 0.5020(16) 0.4435(18) 0.4981(12) 0.201(9) Uani 0.50 1 d P . . N1N N 0.5020(16) 0.4435(18) 0.4981(12) 0.201(9) Uani 0.50 1 d P . . C2N C 0.498(3) 0.306(3) 0.4982(17) 0.194(16) Uani 0.50 1 d P . . H2NA H 0.5431 0.2711 0.4700 0.291 Uiso 0.50 1 d PR . . H2NB H 0.5041 0.2729 0.5438 0.291 Uiso 0.50 1 d PR . . H2NC H 0.4435 0.2816 0.4800 0.291 Uiso 0.50 1 d PR . . C4' C 0.3689(17) -0.185(3) 0.5235(13) 0.153(10) Uiso 0.50 1 d P . . H4'A H 0.3553 -0.2765 0.5216 0.230 Uiso 0.50 1 d PR . . H4'B H 0.4301 -0.1744 0.5241 0.230 Uiso 0.50 1 d PR . . H4'C H 0.3448 -0.1481 0.5642 0.230 Uiso 0.50 1 d PR . . 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 Rh 0.0537(4) 0.0346(3) 0.0497(4) -0.0007(3) 0.0012(2) -0.0010(3) Cl 0.0663(14) 0.0338(9) 0.0762(12) 0.0005(9) -0.0058(9) -0.0049(9) P 0.0456(12) 0.0298(9) 0.0483(10) 0.0024(8) -0.0003(8) 0.0006(8) O3 0.087(5) 0.104(5) 0.097(5) 0.050(4) 0.009(4) 0.031(4) O4 0.096(6) 0.120(6) 0.123(6) -0.040(5) -0.047(4) 0.017(4) O5 0.047(4) 0.072(4) 0.106(4) -0.014(3) 0.003(3) -0.006(3) O6 0.058(4) 0.078(4) 0.096(4) -0.026(3) -0.004(3) 0.020(3) N 0.047(4) 0.048(4) 0.074(4) -0.005(3) 0.001(3) 0.009(3) C1 0.056(5) 0.038(4) 0.047(4) 0.009(3) -0.001(3) 0.008(3) C2 0.045(5) 0.040(4) 0.063(5) 0.003(4) -0.002(4) 0.005(3) C3 0.045(5) 0.074(6) 0.073(6) 0.006(5) 0.001(4) 0.014(5) C4 0.084(15) 0.16(2) 0.070(12) -0.037(13) -0.045(11) 0.033(14) C5 0.059(7) 0.050(5) 0.070(5) 0.001(4) 0.006(5) 0.011(5) C6 0.059(6) 0.056(5) 0.092(6) -0.011(5) 0.000(5) 0.015(4) C7 0.095(8) 0.108(8) 0.142(10) -0.057(7) -0.019(7) 0.024(6) C8 0.129(9) 0.105(8) 0.118(8) -0.002(7) 0.057(7) 0.024(7) C9 0.070(7) 0.088(7) 0.130(9) -0.001(6) -0.007(6) 0.024(5) C10 0.041(5) 0.033(4) 0.061(5) 0.008(3) -0.003(4) 0.002(3) C11 0.047(6) 0.049(5) 0.077(5) 0.001(4) -0.002(5) 0.007(4) C12 0.051(6) 0.067(6) 0.123(9) 0.009(6) -0.013(6) -0.003(4) C13 0.060(7) 0.075(6) 0.111(8) 0.023(6) 0.024(6) 0.000(5) C14 0.073(8) 0.097(7) 0.073(6) 0.006(5) 0.027(6) 0.001(6) C15 0.057(6) 0.088(6) 0.056(5) -0.008(4) 0.002(4) 0.003(4) C16 0.045(5) 0.032(4) 0.050(4) 0.005(3) -0.001(4) 0.000(3) C17 0.059(6) 0.045(5) 0.071(5) -0.001(4) -0.006(4) -0.008(4) C18 0.072(6) 0.059(6) 0.075(5) -0.010(5) -0.003(4) -0.020(5) C19 0.097(8) 0.039(5) 0.096(7) -0.006(5) 0.016(6) -0.017(5) C20 0.091(7) 0.039(5) 0.094(6) 0.004(4) 0.008(6) 0.008(5) C21 0.063(5) 0.041(5) 0.077(5) -0.004(4) 0.003(4) 0.004(4) C22 0.080(7) 0.050(5) 0.074(5) -0.002(4) 0.020(5) -0.024(5) C23 0.125(9) 0.036(4) 0.052(5) 0.006(4) 0.002(5) 0.000(5) C24 0.228(14) 0.068(7) 0.061(6) 0.003(5) -0.031(7) 0.011(7) C25 0.106(8) 0.090(7) 0.070(6) -0.006(5) -0.019(5) 0.006(6) C26 0.088(7) 0.047(5) 0.053(5) -0.013(4) -0.005(4) 0.003(5) C27 0.096(8) 0.066(6) 0.059(5) -0.016(4) 0.017(5) 0.009(5) C28 0.089(8) 0.104(9) 0.115(8) -0.012(7) 0.037(6) 0.009(6) C29 0.109(10) 0.125(10) 0.204(13) -0.045(10) 0.083(9) -0.033(8) C1N 0.192(13) 0.24(3) 0.173(12) -0.01(2) -0.031(10) 0.11(2) N1N 0.192(13) 0.24(3) 0.173(12) -0.01(2) -0.031(10) 0.11(2) C2N 0.31(5) 0.13(2) 0.15(2) -0.03(2) -0.03(3) 0.08(3) #============================================================================== # MOLECULAR GEOMETRY _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 Rh C22 2.098(7) . ? Rh C23 2.100(7) . ? Rh C27 2.212(8) . ? Rh C26 2.224(7) . ? Rh P 2.286(2) . ? Rh Cl 2.387(2) . ? P C10 1.808(7) . ? P C16 1.827(7) . ? P C1 1.849(6) . ? O3 C3 1.235(10) . ? O3 C4' 1.32(3) . ? O4 C3 1.297(10) . ? O4 C4 1.401(17) . ? O5 C5 1.196(9) . ? O6 C5 1.362(10) . ? O6 C6 1.480(9) . ? N C5 1.360(9) . ? N C2 1.436(9) . ? N H0A 1.1370 . ? C1 C2 1.535(9) . ? C1 H1A 0.9600 . ? C1 H1B 0.9599 . ? C2 C3 1.511(10) . ? C2 H2A 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C6 C8 1.493(12) . ? C6 C9 1.501(12) . ? C6 C7 1.515(12) . ? C7 H7A 0.9600 . ? C7 H7B 0.9601 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9599 . ? C9 H9C 0.9600 . ? C10 C11 1.371(10) . ? C10 C15 1.400(10) . ? C11 C12 1.385(11) . ? C11 H11A 0.9600 . ? C12 C13 1.378(13) . ? C12 H12A 0.9600 . ? C13 C14 1.335(12) . ? C13 H13A 0.9599 . ? C14 C15 1.359(11) . ? C14 H14A 0.9600 . ? C15 H15A 0.9601 . ? C16 C17 1.386(9) . ? C16 C21 1.399(10) . ? C17 C18 1.387(11) . ? C17 H17A 0.9600 . ? C18 C19 1.369(12) . ? C18 H18A 0.9601 . ? C19 C20 1.383(12) . ? C19 H19A 0.9600 . ? C20 C21 1.369(10) . ? C20 H20A 0.9600 . ? C21 H21A 0.9601 . ? C22 C23 1.384(11) . ? C22 C29 1.504(13) . ? C22 H22A 0.9600 . ? C23 C24 1.498(11) . ? C23 H23A 0.9601 . ? C24 C25 1.445(13) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C25 C26 1.517(12) . ? C25 H25A 0.9599 . ? C25 H25B 0.9600 . ? C26 C27 1.376(11) . ? C26 H26A 0.9600 . ? C27 C28 1.490(13) . ? C27 H27A 0.9600 . ? C28 C29 1.437(14) . ? C28 H28A 0.9600 . ? C28 H28B 0.9599 . ? C29 H29A 0.9600 . ? C29 H29B 0.9601 . ? C1N N1N 1.16(4) 3_666 ? C1N C1N 1.16(4) 3_666 ? C1N C2N 1.41(3) . ? N1N N1N 1.16(4) 3_666 ? N1N C1N 1.16(4) 3_666 ? N1N C2N 1.41(3) . ? C2N H2NA 0.9600 . ? C2N H2NB 0.9600 . ? C2N H2NC 0.9600 . ? C4' H4'A 0.9600 . ? C4' H4'B 0.9601 . ? C4' H4'C 0.9600 . ? 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 C22 Rh C23 38.5(3) . . ? C22 Rh C27 81.4(3) . . ? C23 Rh C27 92.5(3) . . ? C22 Rh C26 93.7(3) . . ? C23 Rh C26 81.4(3) . . ? C27 Rh C26 36.1(3) . . ? C22 Rh P 93.1(2) . . ? C23 Rh P 97.3(2) . . ? C27 Rh P 156.4(3) . . ? C26 Rh P 167.1(3) . . ? C22 Rh Cl 162.7(3) . . ? C23 Rh Cl 158.6(3) . . ? C27 Rh Cl 91.9(2) . . ? C26 Rh Cl 90.0(2) . . ? P Rh Cl 86.71(7) . . ? C10 P C16 101.9(3) . . ? C10 P C1 101.8(3) . . ? C16 P C1 103.7(3) . . ? C10 P Rh 116.3(2) . . ? C16 P Rh 120.8(2) . . ? C1 P Rh 110.1(2) . . ? C3 O3 C4' 132.2(15) . . ? C3 O4 C4 122.6(12) . . ? C5 O6 C6 120.8(6) . . ? C5 N C2 119.1(7) . . ? C5 N H0A 127.6 . . ? C2 N H0A 113.2 . . ? C2 C1 P 115.7(5) . . ? C2 C1 H1A 107.6 . . ? P C1 H1A 108.5 . . ? C2 C1 H1B 108.3 . . ? P C1 H1B 108.7 . . ? H1A C1 H1B 107.8 . . ? N C2 C3 111.2(6) . . ? N C2 C1 110.3(6) . . ? C3 C2 C1 107.1(6) . . ? N C2 H2A 109.6 . . ? C3 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? O3 C3 O4 126.3(9) . . ? O3 C3 C2 119.8(8) . . ? O4 C3 C2 113.8(8) . . ? O4 C4 H4A 111.2 . . ? O4 C4 H4B 107.5 . . ? H4A C4 H4B 109.5 . . ? O4 C4 H4C 109.7 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O5 C5 N 125.3(8) . . ? O5 C5 O6 127.2(7) . . ? N C5 O6 107.5(8) . . ? O6 C6 C8 110.3(7) . . ? O6 C6 C9 108.9(7) . . ? C8 C6 C9 112.3(8) . . ? O6 C6 C7 102.2(7) . . ? C8 C6 C7 112.0(8) . . ? C9 C6 C7 110.6(8) . . ? C6 C7 H7A 109.9 . . ? C6 C7 H7B 109.7 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 108.8 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 108.8 . . ? C6 C8 H8B 109.8 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.8 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 110.0 . . ? C6 C9 H9B 109.3 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.2 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 117.3(7) . . ? C11 C10 P 121.3(6) . . ? C15 C10 P 121.3(6) . . ? C10 C11 C12 121.0(8) . . ? C10 C11 H11A 119.1 . . ? C12 C11 H11A 119.9 . . ? C13 C12 C11 119.3(9) . . ? C13 C12 H12A 120.6 . . ? C11 C12 H12A 120.1 . . ? C14 C13 C12 120.3(8) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 119.5 . . ? C13 C14 C15 120.9(9) . . ? C13 C14 H14A 119.9 . . ? C15 C14 H14A 119.2 . . ? C14 C15 C10 121.1(8) . . ? C14 C15 H15A 120.1 . . ? C10 C15 H15A 118.8 . . ? C17 C16 C21 117.6(6) . . ? C17 C16 P 124.5(5) . . ? C21 C16 P 117.9(6) . . ? C16 C17 C18 121.6(7) . . ? C16 C17 H17A 118.6 . . ? C18 C17 H17A 119.8 . . ? C19 C18 C17 119.5(8) . . ? C19 C18 H18A 119.8 . . ? C17 C18 H18A 120.7 . . ? C18 C19 C20 119.9(7) . . ? C18 C19 H19A 120.5 . . ? C20 C19 H19A 119.6 . . ? C21 C20 C19 120.6(8) . . ? C21 C20 H20A 120.0 . . ? C19 C20 H20A 119.4 . . ? C20 C21 C16 120.7(8) . . ? C20 C21 H21A 120.7 . . ? C16 C21 H21A 118.6 . . ? C23 C22 C29 123.9(9) . . ? C23 C22 Rh 70.8(4) . . ? C29 C22 Rh 112.0(6) . . ? C23 C22 H22A 114.1 . . ? C29 C22 H22A 114.4 . . ? Rh C22 H22A 113.7 . . ? C22 C23 C24 125.3(9) . . ? C22 C23 Rh 70.7(4) . . ? C24 C23 Rh 112.6(6) . . ? C22 C23 H23A 113.3 . . ? C24 C23 H23A 114.0 . . ? Rh C23 H23A 113.1 . . ? C25 C24 C23 118.0(8) . . ? C25 C24 H24A 107.9 . . ? C23 C24 H24A 107.5 . . ? C25 C24 H24B 108.2 . . ? C23 C24 H24B 107.5 . . ? H24A C24 H24B 107.3 . . ? C24 C25 C26 116.2(7) . . ? C24 C25 H25A 108.4 . . ? C26 C25 H25A 108.4 . . ? C24 C25 H25B 108.2 . . ? C26 C25 H25B 108.0 . . ? H25A C25 H25B 107.4 . . ? C27 C26 C25 123.3(8) . . ? C27 C26 Rh 71.5(4) . . ? C25 C26 Rh 109.2(5) . . ? C27 C26 H26A 113.6 . . ? C25 C26 H26A 116.0 . . ? Rh C26 H26A 114.7 . . ? C26 C27 C28 125.8(9) . . ? C26 C27 Rh 72.4(5) . . ? C28 C27 Rh 109.1(6) . . ? C26 C27 H27A 115.1 . . ? C28 C27 H27A 113.4 . . ? Rh C27 H27A 112.8 . . ? C29 C28 C27 117.4(8) . . ? C29 C28 H28A 108.0 . . ? C27 C28 H28A 107.4 . . ? C29 C28 H28B 108.1 . . ? C27 C28 H28B 108.2 . . ? H28A C28 H28B 107.4 . . ? C28 C29 C22 117.3(8) . . ? C28 C29 H29A 108.2 . . ? C22 C29 H29A 108.3 . . ? C28 C29 H29B 108.3 . . ? C22 C29 H29B 107.0 . . ? H29A C29 H29B 107.3 . . ? N1N C1N C2N 173(4) 3_666 . ? C1N C1N C2N 173(4) 3_666 . ? N1N N1N C2N 173(4) 3_666 . ? C1N N1N C2N 173(4) 3_666 . ? N1N C2N H2NA 110.2 . . ? C1N C2N H2NA 110.2 . . ? N1N C2N H2NB 110.8 . . ? C1N C2N H2NB 110.8 . . ? H2NA C2N H2NB 109.5 . . ? N1N C2N H2NC 107.4 . . ? C1N C2N H2NC 107.4 . . ? H2NA C2N H2NC 109.5 . . ? H2NB C2N H2NC 109.5 . . ? O3 C4' H4'A 107.5 . . ? O3 C4' H4'B 111.7 . . ? H4'A C4' H4'B 109.5 . . ? O3 C4' H4'C 109.2 . . ? H4'A C4' H4'C 109.5 . . ? H4'B C4' H4'C 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 C22 Rh P C10 140.1(4) . . . . ? C23 Rh P C10 101.7(4) . . . . ? C27 Rh P C10 -144.5(6) . . . . ? C26 Rh P C10 18.4(10) . . . . ? Cl Rh P C10 -57.2(2) . . . . ? C22 Rh P C16 15.9(4) . . . . ? C23 Rh P C16 -22.5(4) . . . . ? C27 Rh P C16 91.3(6) . . . . ? C26 Rh P C16 -105.8(10) . . . . ? Cl Rh P C16 178.6(3) . . . . ? C22 Rh P C1 -104.9(4) . . . . ? C23 Rh P C1 -143.3(4) . . . . ? C27 Rh P C1 -29.4(6) . . . . ? C26 Rh P C1 133.4(10) . . . . ? Cl Rh P C1 57.8(2) . . . . ? C10 P C1 C2 171.2(5) . . . . ? C16 P C1 C2 -83.2(5) . . . . ? Rh P C1 C2 47.3(5) . . . . ? C5 N C2 C3 -59.1(8) . . . . ? C5 N C2 C1 -177.7(6) . . . . ? P C1 C2 N -79.4(6) . . . . ? P C1 C2 C3 159.5(6) . . . . ? C4' O3 C3 O4 -2(2) . . . . ? C4' O3 C3 C2 -179.2(17) . . . . ? C4 O4 C3 O3 -3.0(16) . . . . ? C4 O4 C3 C2 174.0(11) . . . . ? N C2 C3 O3 -32.3(9) . . . . ? C1 C2 C3 O3 88.3(8) . . . . ? N C2 C3 O4 150.6(7) . . . . ? C1 C2 C3 O4 -88.9(8) . . . . ? C2 N C5 O5 -0.6(11) . . . . ? C2 N C5 O6 177.6(6) . . . . ? C6 O6 C5 O5 11.9(12) . . . . ? C6 O6 C5 N -166.3(6) . . . . ? C5 O6 C6 C8 -68.8(10) . . . . ? C5 O6 C6 C9 54.9(10) . . . . ? C5 O6 C6 C7 172.0(7) . . . . ? C16 P C10 C11 124.9(6) . . . . ? C1 P C10 C11 -128.2(6) . . . . ? Rh P C10 C11 -8.5(6) . . . . ? C16 P C10 C15 -51.9(6) . . . . ? C1 P C10 C15 55.0(6) . . . . ? Rh P C10 C15 174.7(5) . . . . ? C15 C10 C11 C12 -3.0(11) . . . . ? P C10 C11 C12 180.0(6) . . . . ? C10 C11 C12 C13 3.2(12) . . . . ? C11 C12 C13 C14 -2.1(14) . . . . ? C12 C13 C14 C15 1.0(14) . . . . ? C13 C14 C15 C10 -0.9(14) . . . . ? C11 C10 C15 C14 1.9(11) . . . . ? P C10 C15 C14 178.8(7) . . . . ? C10 P C16 C17 120.7(6) . . . . ? C1 P C16 C17 15.3(7) . . . . ? Rh P C16 C17 -108.6(6) . . . . ? C10 P C16 C21 -57.9(6) . . . . ? C1 P C16 C21 -163.3(5) . . . . ? Rh P C16 C21 72.8(6) . . . . ? C21 C16 C17 C18 0.2(10) . . . . ? P C16 C17 C18 -178.5(6) . . . . ? C16 C17 C18 C19 -1.1(12) . . . . ? C17 C18 C19 C20 0.9(13) . . . . ? C18 C19 C20 C21 0.2(13) . . . . ? C19 C20 C21 C16 -1.2(13) . . . . ? C17 C16 C21 C20 1.0(11) . . . . ? P C16 C21 C20 179.7(6) . . . . ? C27 Rh C22 C23 105.2(5) . . . . ? C26 Rh C22 C23 71.2(5) . . . . ? P Rh C22 C23 -97.9(4) . . . . ? Cl Rh C22 C23 173.3(6) . . . . ? C23 Rh C22 C29 -119.8(10) . . . . ? C27 Rh C22 C29 -14.6(9) . . . . ? C26 Rh C22 C29 -48.6(9) . . . . ? P Rh C22 C29 142.3(9) . . . . ? Cl Rh C22 C29 53.5(13) . . . . ? C29 C22 C23 C24 -0.3(13) . . . . ? Rh C22 C23 C24 -104.5(8) . . . . ? C29 C22 C23 Rh 104.2(8) . . . . ? C27 Rh C23 C22 -72.7(5) . . . . ? C26 Rh C23 C22 -107.2(5) . . . . ? P Rh C23 C22 85.7(4) . . . . ? Cl Rh C23 C22 -174.6(5) . . . . ? C22 Rh C23 C24 121.2(10) . . . . ? C27 Rh C23 C24 48.5(8) . . . . ? C26 Rh C23 C24 14.0(8) . . . . ? P Rh C23 C24 -153.1(8) . . . . ? Cl Rh C23 C24 -53.4(11) . . . . ? C22 C23 C24 C25 68.9(14) . . . . ? Rh C23 C24 C25 -12.8(14) . . . . ? C23 C24 C25 C26 1.0(16) . . . . ? C24 C25 C26 C27 -69.6(12) . . . . ? C24 C25 C26 Rh 10.4(12) . . . . ? C22 Rh C26 C27 69.9(6) . . . . ? C23 Rh C26 C27 106.5(6) . . . . ? P Rh C26 C27 -168.4(8) . . . . ? Cl Rh C26 C27 -93.2(5) . . . . ? C22 Rh C26 C25 -49.8(7) . . . . ? C23 Rh C26 C25 -13.2(7) . . . . ? C27 Rh C26 C25 -119.7(9) . . . . ? P Rh C26 C25 71.8(13) . . . . ? Cl Rh C26 C25 147.1(6) . . . . ? C25 C26 C27 C28 0.0(12) . . . . ? Rh C26 C27 C28 -101.2(8) . . . . ? C25 C26 C27 Rh 101.2(7) . . . . ? C22 Rh C27 C26 -108.6(6) . . . . ? C23 Rh C27 C26 -71.6(6) . . . . ? P Rh C27 C26 173.6(4) . . . . ? Cl Rh C27 C26 87.4(5) . . . . ? C22 Rh C27 C28 14.0(7) . . . . ? C23 Rh C27 C28 51.0(8) . . . . ? C26 Rh C27 C28 122.6(10) . . . . ? P Rh C27 C28 -63.8(10) . . . . ? Cl Rh C27 C28 -150.0(7) . . . . ? C26 C27 C28 C29 70.4(14) . . . . ? Rh C27 C28 C29 -11.3(14) . . . . ? C27 C28 C29 C22 -0.6(18) . . . . ? C23 C22 C29 C28 -68.0(16) . . . . ? Rh C22 C29 C28 13.1(16) . . . . ?