Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Woollins, John Derek' 'Clarke, Matthew L.' 'Cole-Hamilton, David' 'Foster, Douglas F.' 'Slawin, A.' _publ_contact_author_name 'Prof John Derek Woollins' _publ_contact_author_address ; Chemistry St Andrews University of St Andrews St Andrews Fife KY16 9ST UNITED KINGDOM ; _publ_contact_author_email 'JDW3@ST-AND.AC.UK' _publ_section_title ; Co-ordination chemistry and metal catalysed carbonylation reactions using 8-(diphenylphosphino)-methylaminoquinoline: A ligand that displays monodentate, bidentate and tridentate co-ordination modes. ; data_4 _database_code_CSD 177445 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H19 N2 P' _chemical_formula_sum 'C22 H19 N2 P' _chemical_formula_weight 342.36 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 8.6824(6) _cell_length_b 25.8218(17) _cell_length_c 8.2049(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1839.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 242 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max .1 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.155 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.737115 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7576 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 23.26 _reflns_number_total 2549 _reflns_number_gt 1915 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0024(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.20(13) _refine_ls_number_reflns 2549 _refine_ls_number_parameters 231 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.0898 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.936 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.003 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 P1 P 0.06750(9) 0.59921(3) 0.41475(13) 0.0539(3) Uani 1 1 d . . . C1 C 0.1965(4) 0.54459(11) 0.3741(4) 0.0514(9) Uani 1 1 d . . . C2 C 0.1583(4) 0.49264(11) 0.3965(5) 0.0653(9) Uani 1 1 d . . . H2A H 0.0627 0.4838 0.4393 0.078 Uiso 1 1 calc R . . C3 C 0.2625(5) 0.45419(13) 0.3551(4) 0.0727(11) Uani 1 1 d . . . H3A H 0.2351 0.4196 0.3686 0.087 Uiso 1 1 calc R . . C4 C 0.4037(5) 0.46604(16) 0.2952(5) 0.0780(12) Uani 1 1 d . . . H4A H 0.4726 0.4398 0.2689 0.094 Uiso 1 1 calc R . . C5 C 0.4446(4) 0.51702(15) 0.2735(6) 0.0843(13) Uani 1 1 d . . . H5A H 0.5416 0.5255 0.2337 0.101 Uiso 1 1 calc R . . C6 C 0.3399(5) 0.55542(13) 0.3116(4) 0.0684(10) Uani 1 1 d . . . H6A H 0.3674 0.5898 0.2944 0.082 Uiso 1 1 calc R . . C7 C 0.0939(4) 0.61092(12) 0.6336(4) 0.0536(9) Uani 1 1 d . . . C8 C 0.0241(4) 0.65351(13) 0.6994(5) 0.0705(11) Uani 1 1 d . . . H8A H -0.0346 0.6748 0.6324 0.085 Uiso 1 1 calc R . . C9 C 0.0383(6) 0.66574(17) 0.8616(6) 0.0907(14) Uani 1 1 d . . . H9A H -0.0123 0.6945 0.9036 0.109 Uiso 1 1 calc R . . C10 C 0.1268(6) 0.6355(2) 0.9610(5) 0.0955(14) Uani 1 1 d . . . H10A H 0.1377 0.6440 1.0705 0.115 Uiso 1 1 calc R . . C11 C 0.1995(5) 0.59262(16) 0.8992(5) 0.0845(11) Uani 1 1 d . . . H11A H 0.2606 0.5721 0.9663 0.101 Uiso 1 1 calc R . . C12 C 0.1814(4) 0.58006(13) 0.7364(4) 0.0654(10) Uani 1 1 d . . . H12A H 0.2286 0.5505 0.6952 0.078 Uiso 1 1 calc R . . C13 C -0.1248(3) 0.56665(11) 0.4223(5) 0.0608(8) Uani 1 1 d . . . H13A H -0.1468 0.5514 0.3167 0.073 Uiso 1 1 calc R . . H13B H -0.1214 0.5389 0.5018 0.073 Uiso 1 1 calc R . . N13 N -0.2458(3) 0.60167(11) 0.4644(3) 0.0627(8) Uani 1 1 d D . . H13N H -0.292(4) 0.6039(13) 0.573(2) 0.085(12) Uiso 1 1 d D . . C14 C -0.3162(4) 0.63606(12) 0.3608(4) 0.0522(9) Uani 1 1 d . . . C15 C -0.2821(4) 0.64079(13) 0.1975(4) 0.0697(11) Uani 1 1 d . . . H15A H -0.2021 0.6215 0.1530 0.084 Uiso 1 1 calc R . . C16 C -0.3662(5) 0.67432(16) 0.0979(5) 0.0861(12) Uani 1 1 d . . . H16A H -0.3421 0.6766 -0.0123 0.103 Uiso 1 1 calc R . . C17 C -0.4827(5) 0.70363(16) 0.1591(5) 0.0826(12) Uani 1 1 d . . . H17A H -0.5388 0.7253 0.0906 0.099 Uiso 1 1 calc R . . C17A C -0.5183(4) 0.70124(13) 0.3258(5) 0.0615(10) Uani 1 1 d . . . C18 C -0.6378(4) 0.73030(12) 0.4001(7) 0.0786(11) Uani 1 1 d . . . H18A H -0.6970 0.7528 0.3375 0.094 Uiso 1 1 calc R . . C19 C -0.6659(5) 0.72556(14) 0.5609(6) 0.0833(13) Uani 1 1 d . . . H19A H -0.7433 0.7449 0.6105 0.100 Uiso 1 1 calc R . . C20 C -0.5764(4) 0.69099(14) 0.6516(5) 0.0737(12) Uani 1 1 d . . . H20A H -0.5970 0.6877 0.7623 0.088 Uiso 1 1 calc R . . N21 N -0.4648(3) 0.66285(10) 0.5893(4) 0.0626(8) Uani 1 1 d . . . C14A C -0.4355(3) 0.66758(9) 0.4255(6) 0.0514(7) 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 P1 0.0590(5) 0.0470(4) 0.0556(5) -0.0004(5) -0.0015(5) 0.0073(4) C1 0.052(2) 0.0493(18) 0.053(2) -0.0023(15) -0.0066(16) 0.0011(15) C2 0.064(2) 0.0538(18) 0.078(3) 0.000(2) 0.012(2) 0.0015(17) C3 0.089(3) 0.0497(19) 0.079(3) -0.0036(17) 0.000(2) 0.008(2) C4 0.070(3) 0.074(3) 0.090(3) -0.028(2) -0.012(2) 0.024(2) C5 0.051(2) 0.077(3) 0.125(4) -0.020(3) 0.010(3) 0.000(2) C6 0.058(2) 0.052(2) 0.095(3) -0.0112(19) 0.001(2) -0.0074(19) C7 0.052(2) 0.0485(19) 0.060(2) -0.0045(16) 0.0030(18) -0.0010(17) C8 0.077(3) 0.060(2) 0.074(3) -0.011(2) 0.007(2) 0.0069(19) C9 0.097(3) 0.091(3) 0.084(4) -0.031(3) 0.019(3) -0.006(3) C10 0.100(4) 0.130(4) 0.056(3) -0.024(3) 0.018(2) -0.029(3) C11 0.088(3) 0.106(3) 0.059(2) 0.006(2) -0.009(3) -0.012(2) C12 0.068(2) 0.065(2) 0.063(2) -0.0012(18) -0.004(2) -0.002(2) C13 0.057(2) 0.0587(17) 0.066(2) -0.004(2) -0.009(2) 0.0148(15) N13 0.0533(17) 0.0704(19) 0.064(2) 0.0025(15) -0.0035(14) 0.0165(16) C14 0.0452(19) 0.0529(18) 0.059(3) -0.0024(15) -0.0097(17) -0.0027(17) C15 0.073(3) 0.072(2) 0.063(3) -0.0020(19) -0.006(2) 0.016(2) C16 0.099(3) 0.095(3) 0.064(3) 0.005(2) -0.006(2) 0.015(3) C17 0.092(3) 0.071(3) 0.085(3) 0.015(2) -0.021(3) 0.013(3) C17A 0.053(2) 0.0470(19) 0.085(3) 0.0064(19) -0.0060(19) 0.0020(19) C18 0.068(2) 0.0472(18) 0.121(4) 0.010(2) 0.001(3) 0.0103(17) C19 0.071(3) 0.051(2) 0.128(4) -0.005(2) 0.023(3) 0.003(2) C20 0.067(3) 0.061(2) 0.093(3) -0.005(2) 0.021(2) -0.009(2) N21 0.0554(19) 0.0521(16) 0.080(2) -0.0040(15) 0.0078(16) -0.0020(15) C14A 0.0455(17) 0.0416(15) 0.067(2) -0.004(2) -0.003(2) -0.0050(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C1 1.832(3) . ? P1 C7 1.835(4) . ? P1 C13 1.870(3) . ? C1 C6 1.375(5) . ? C1 C2 1.394(4) . ? C2 C3 1.385(5) . ? C3 C4 1.356(5) . ? C4 C5 1.375(5) . ? C5 C6 1.380(5) . ? C7 C8 1.367(4) . ? C7 C12 1.387(5) . ? C8 C9 1.373(5) . ? C9 C10 1.365(6) . ? C10 C11 1.372(5) . ? C11 C12 1.384(5) . ? C13 N13 1.429(4) . ? N13 C14 1.373(4) . ? C14 C15 1.378(4) . ? C14 C14A 1.420(4) . ? C15 C16 1.397(5) . ? C16 C17 1.360(6) . ? C17 C17A 1.404(5) . ? C17A C14A 1.393(5) . ? C17A C18 1.418(5) . ? C18 C19 1.347(5) . ? C19 C20 1.398(6) . ? C20 N21 1.315(4) . ? N21 C14A 1.374(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 P1 C7 103.22(14) . . ? C1 P1 C13 101.89(13) . . ? C7 P1 C13 98.81(16) . . ? C6 C1 C2 117.4(3) . . ? C6 C1 P1 117.7(2) . . ? C2 C1 P1 124.8(3) . . ? C3 C2 C1 120.1(3) . . ? C4 C3 C2 121.2(4) . . ? C3 C4 C5 119.7(4) . . ? C4 C5 C6 119.2(4) . . ? C5 C6 C1 122.3(3) . . ? C8 C7 C12 117.7(3) . . ? C8 C7 P1 117.6(3) . . ? C12 C7 P1 124.7(3) . . ? C9 C8 C7 121.9(4) . . ? C10 C9 C8 119.9(4) . . ? C9 C10 C11 120.0(4) . . ? C10 C11 C12 119.6(4) . . ? C11 C12 C7 121.0(3) . . ? N13 C13 P1 112.35(19) . . ? C14 N13 C13 126.0(3) . . ? N13 C14 C15 124.3(3) . . ? N13 C14 C14A 117.6(3) . . ? C15 C14 C14A 118.0(3) . . ? C14 C15 C16 120.7(4) . . ? C17 C16 C15 121.2(4) . . ? C16 C17 C17A 119.9(4) . . ? C14A C17A C17 119.1(4) . . ? C14A C17A C18 117.1(4) . . ? C17 C17A C18 123.8(4) . . ? C19 C18 C17A 120.4(4) . . ? C18 C19 C20 118.6(4) . . ? N21 C20 C19 123.8(4) . . ? C20 N21 C14A 117.9(3) . . ? N21 C14A C17A 122.3(3) . . ? N21 C14A C14 116.7(3) . . ? C17A C14A C14 121.0(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 P1 C1 C6 -97.5(3) . . . . ? C13 P1 C1 C6 160.4(3) . . . . ? C7 P1 C1 C2 84.9(3) . . . . ? C13 P1 C1 C2 -17.2(3) . . . . ? C6 C1 C2 C3 -0.5(5) . . . . ? P1 C1 C2 C3 177.2(3) . . . . ? C1 C2 C3 C4 1.2(6) . . . . ? C2 C3 C4 C5 -0.6(6) . . . . ? C3 C4 C5 C6 -0.7(6) . . . . ? C4 C5 C6 C1 1.4(6) . . . . ? C2 C1 C6 C5 -0.8(5) . . . . ? P1 C1 C6 C5 -178.6(3) . . . . ? C1 P1 C7 C8 173.2(3) . . . . ? C13 P1 C7 C8 -82.3(3) . . . . ? C1 P1 C7 C12 -5.8(3) . . . . ? C13 P1 C7 C12 98.8(3) . . . . ? C12 C7 C8 C9 -0.3(5) . . . . ? P1 C7 C8 C9 -179.4(3) . . . . ? C7 C8 C9 C10 1.4(7) . . . . ? C8 C9 C10 C11 -0.9(7) . . . . ? C9 C10 C11 C12 -0.6(6) . . . . ? C10 C11 C12 C7 1.6(5) . . . . ? C8 C7 C12 C11 -1.2(5) . . . . ? P1 C7 C12 C11 177.8(3) . . . . ? C1 P1 C13 N13 176.0(3) . . . . ? C7 P1 C13 N13 70.4(3) . . . . ? P1 C13 N13 C14 79.5(4) . . . . ? C13 N13 C14 C15 1.8(5) . . . . ? C13 N13 C14 C14A 179.6(3) . . . . ? N13 C14 C15 C16 175.7(3) . . . . ? C14A C14 C15 C16 -2.2(5) . . . . ? C14 C15 C16 C17 0.8(6) . . . . ? C15 C16 C17 C17A 1.2(6) . . . . ? C16 C17 C17A C14A -1.7(6) . . . . ? C16 C17 C17A C18 -179.9(4) . . . . ? C14A C17A C18 C19 1.1(5) . . . . ? C17 C17A C18 C19 179.4(4) . . . . ? C17A C18 C19 C20 -0.9(6) . . . . ? C18 C19 C20 N21 0.5(6) . . . . ? C19 C20 N21 C14A -0.5(5) . . . . ? C20 N21 C14A C17A 0.8(5) . . . . ? C20 N21 C14A C14 -178.9(3) . . . . ? C17 C17A C14A N21 -179.4(3) . . . . ? C18 C17A C14A N21 -1.1(5) . . . . ? C17 C17A C14A C14 0.2(5) . . . . ? C18 C17A C14A C14 178.5(3) . . . . ? N13 C14 C14A N21 3.4(4) . . . . ? C15 C14 C14A N21 -178.6(3) . . . . ? N13 C14 C14A C17A -176.3(3) . . . . ? C15 C14 C14A C17A 1.8(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N13 H13N N21 0.977(5) 2.14(3) 2.676(4) 113(3) . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.136 _refine_diff_density_min -0.108 _refine_diff_density_rms 0.030 data_5 _database_code_CSD 177446 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H34 Cl2 N2 P Rh' _chemical_formula_sum 'C32 H34 Cl2 N2 P Rh' _chemical_formula_weight 651.39 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 21.779(2) _cell_length_b 8.4708(8) _cell_length_c 16.3038(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3007.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 87 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max .25 _exptl_crystal_size_mid .14 _exptl_crystal_size_min .1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 0.822 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.805519 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12242 _diffrn_reflns_av_R_equivalents 0.0596 _diffrn_reflns_av_sigmaI/netI 0.0689 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 23.27 _reflns_number_total 4269 _reflns_number_gt 2870 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00008(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.47(5) _refine_ls_number_reflns 4269 _refine_ls_number_parameters 348 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0865 _refine_ls_wR_factor_gt 0.0743 _refine_ls_goodness_of_fit_ref 0.912 _refine_ls_restrained_S_all 0.911 _refine_ls_shift/su_max 0.127 _refine_ls_shift/su_mean 0.007 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 0.90071(2) 0.75346(5) 0.53196(5) 0.03886(14) Uani 1 1 d . . . Cl1 Cl 0.89454(9) 0.5468(3) 0.43042(16) 0.0552(6) Uani 1 1 d . . . Cl2 Cl 0.91396(9) 0.5644(3) 0.64132(15) 0.0537(6) Uani 1 1 d . . . P1 P 0.79560(8) 0.72580(19) 0.55098(9) 0.0392(6) Uani 1 1 d . . . C1 C 0.7632(3) 0.7915(8) 0.6471(5) 0.0406(18) Uani 1 1 d . . . C2 C 0.8005(4) 0.8214(9) 0.7144(5) 0.054(2) Uani 1 1 d . . . H2A H 0.8429 0.8221 0.7069 0.065 Uiso 1 1 calc R . . C3 C 0.7782(4) 0.8494(10) 0.7904(5) 0.070(2) Uani 1 1 d . . . H3A H 0.8047 0.8697 0.8339 0.085 Uiso 1 1 calc R . . C4 C 0.7172(5) 0.8474(10) 0.8022(5) 0.069(2) Uani 1 1 d . . . H4A H 0.7019 0.8645 0.8547 0.082 Uiso 1 1 calc R . . C5 C 0.6767(4) 0.8211(11) 0.7394(6) 0.071(3) Uani 1 1 d . . . H5A H 0.6345 0.8224 0.7483 0.085 Uiso 1 1 calc R . . C6 C 0.7008(4) 0.7921(9) 0.6616(5) 0.065(2) Uani 1 1 d . . . H6A H 0.6741 0.7725 0.6183 0.078 Uiso 1 1 calc R . . C7 C 0.7492(3) 0.8110(9) 0.4694(5) 0.0430(18) Uani 1 1 d . . . C8 C 0.7133(3) 0.9457(9) 0.4797(4) 0.056(2) Uani 1 1 d . . . H8A H 0.7128 0.9975 0.5300 0.068 Uiso 1 1 calc R . . C9 C 0.6780(4) 1.0030(10) 0.4148(6) 0.081(3) Uani 1 1 d . . . H9A H 0.6552 1.0950 0.4213 0.097 Uiso 1 1 calc R . . C10 C 0.6769(4) 0.9248(12) 0.3424(6) 0.077(3) Uani 1 1 d . . . H10A H 0.6524 0.9617 0.2998 0.092 Uiso 1 1 calc R . . C11 C 0.7113(4) 0.7933(10) 0.3317(5) 0.067(2) Uani 1 1 d . . . H11A H 0.7102 0.7405 0.2817 0.080 Uiso 1 1 calc R . . C12 C 0.7483(4) 0.7362(9) 0.3950(4) 0.049(2) Uani 1 1 d . . . H12A H 0.7725 0.6471 0.3865 0.059 Uiso 1 1 calc R . . N13 N 0.7065(3) 0.4952(6) 0.5357(5) 0.0577(15) Uani 1 1 d D . . H13N H 0.694(4) 0.521(9) 0.4795(18) 0.10(3) Uiso 1 1 d D . . C13 C 0.7714(3) 0.5141(7) 0.5508(5) 0.050(2) Uani 1 1 d . . . H13A H 0.7942 0.4579 0.5089 0.060 Uiso 1 1 calc R . . H13B H 0.7815 0.4673 0.6035 0.060 Uiso 1 1 calc R . . C14 C 0.6693(3) 0.3907(8) 0.5765(5) 0.0477(19) Uani 1 1 d . . . C14A C 0.6168(3) 0.3324(7) 0.5328(7) 0.0459(15) Uani 1 1 d . . . C15 C 0.6785(4) 0.3372(9) 0.6542(5) 0.066(2) Uani 1 1 d . . . H15A H 0.7128 0.3704 0.6834 0.079 Uiso 1 1 calc R . . C16 C 0.6363(5) 0.2311(11) 0.6914(5) 0.080(3) Uani 1 1 d . . . H16A H 0.6436 0.1965 0.7446 0.097 Uiso 1 1 calc R . . C17 C 0.5856(5) 0.1788(11) 0.6513(7) 0.081(3) Uani 1 1 d . . . H17A H 0.5585 0.1104 0.6775 0.097 Uiso 1 1 calc R . . C17A C 0.5739(4) 0.2279(9) 0.5704(5) 0.060(2) Uani 1 1 d . . . C18 C 0.5258(4) 0.1755(9) 0.5225(9) 0.076(2) Uani 1 1 d . . . H18A H 0.4970 0.1065 0.5446 0.091 Uiso 1 1 calc R . . C19 C 0.5201(4) 0.2233(10) 0.4440(7) 0.085(3) Uani 1 1 d . . . H19A H 0.4881 0.1870 0.4112 0.102 Uiso 1 1 calc R . . C20 C 0.5624(4) 0.3261(10) 0.4144(6) 0.065(2) Uani 1 1 d . . . H20A H 0.5575 0.3596 0.3605 0.078 Uiso 1 1 calc R . . N21 N 0.6098(3) 0.3828(6) 0.4549(4) 0.0555(16) Uani 1 1 d . . . C31 C 0.9498(5) 0.9484(11) 0.5883(5) 0.063(3) Uani 1 1 d . . . C32 C 0.9070(3) 1.0088(6) 0.5301(9) 0.0527(16) Uani 1 1 d . . . C33 C 0.9222(4) 0.9481(10) 0.4529(5) 0.060(2) Uani 1 1 d . . . C34 C 0.9768(4) 0.8616(10) 0.4608(6) 0.068(3) Uani 1 1 d . . . C35 C 0.9939(3) 0.8576(9) 0.5414(7) 0.063(2) Uani 1 1 d . . . C36 C 0.9576(5) 0.9818(14) 0.6786(5) 0.133(5) Uani 1 1 d . . . H36A H 0.9239 1.0450 0.6976 0.199 Uiso 1 1 calc R . . H36B H 0.9954 1.0377 0.6873 0.199 Uiso 1 1 calc R . . H36C H 0.9585 0.8841 0.7083 0.199 Uiso 1 1 calc R . . C37 C 0.8579(4) 1.1270(8) 0.5531(8) 0.103(4) Uani 1 1 d . . . H37A H 0.8587 1.1442 0.6113 0.155 Uiso 1 1 calc R . . H37B H 0.8184 1.0868 0.5374 0.155 Uiso 1 1 calc R . . H37C H 0.8655 1.2249 0.5252 0.155 Uiso 1 1 calc R . . C38 C 0.8887(5) 0.9980(14) 0.3761(6) 0.125(5) Uani 1 1 d . . . H38A H 0.8527 1.0570 0.3907 0.188 Uiso 1 1 calc R . . H38B H 0.8769 0.9060 0.3455 0.188 Uiso 1 1 calc R . . H38C H 0.9152 1.0626 0.3431 0.188 Uiso 1 1 calc R . . C39 C 1.0101(5) 0.7805(12) 0.3906(7) 0.122(5) Uani 1 1 d . . . H39A H 0.9891 0.8019 0.3401 0.182 Uiso 1 1 calc R . . H39B H 1.0109 0.6686 0.4001 0.182 Uiso 1 1 calc R . . H39C H 1.0514 0.8196 0.3874 0.182 Uiso 1 1 calc R . . C40 C 1.0495(4) 0.7748(11) 0.5766(8) 0.126(5) Uani 1 1 d . . . H40A H 1.0506 0.7898 0.6350 0.188 Uiso 1 1 calc R . . H40B H 1.0861 0.8180 0.5527 0.188 Uiso 1 1 calc R . . H40C H 1.0472 0.6640 0.5646 0.188 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0296(2) 0.0387(2) 0.0483(3) 0.0014(4) -0.0017(3) -0.0004(3) Cl1 0.0474(11) 0.0538(13) 0.0644(14) -0.0135(11) 0.0021(10) 0.0032(10) Cl2 0.0458(12) 0.0528(13) 0.0627(14) 0.0124(12) 0.0019(11) 0.0056(10) P1 0.0302(10) 0.0402(10) 0.0471(16) -0.0008(9) -0.0023(8) -0.0009(8) C1 0.038(4) 0.034(4) 0.050(5) 0.000(4) 0.000(4) 0.002(3) C2 0.051(5) 0.057(4) 0.055(5) -0.006(4) -0.010(4) 0.004(4) C3 0.071(7) 0.083(6) 0.057(6) -0.029(5) -0.001(5) 0.004(5) C4 0.084(7) 0.067(6) 0.055(6) -0.002(4) 0.012(5) 0.005(6) C5 0.060(6) 0.087(6) 0.065(6) -0.002(5) 0.022(5) 0.010(6) C6 0.043(5) 0.080(6) 0.073(6) -0.006(5) 0.005(4) -0.007(4) C7 0.031(4) 0.045(4) 0.053(5) -0.002(4) 0.000(3) -0.004(4) C8 0.053(5) 0.052(5) 0.065(5) 0.007(4) 0.003(4) 0.007(5) C9 0.092(7) 0.067(6) 0.083(7) -0.002(5) -0.013(5) 0.031(5) C10 0.058(6) 0.097(7) 0.075(7) 0.029(6) -0.017(5) 0.008(6) C11 0.073(6) 0.071(6) 0.056(5) 0.004(4) -0.009(5) -0.002(5) C12 0.054(5) 0.053(5) 0.040(4) -0.003(4) -0.004(4) 0.014(5) N13 0.057(4) 0.054(3) 0.062(4) 0.009(4) -0.017(4) -0.018(3) C13 0.043(5) 0.034(3) 0.072(7) -0.006(4) -0.002(4) -0.003(3) C14 0.047(5) 0.044(4) 0.053(5) -0.003(4) 0.004(4) 0.001(4) C14A 0.039(4) 0.035(3) 0.063(5) -0.002(6) 0.005(6) 0.005(3) C15 0.076(6) 0.064(5) 0.057(6) 0.005(5) -0.005(5) -0.011(5) C16 0.106(8) 0.081(7) 0.055(5) 0.006(5) 0.019(5) 0.015(7) C17 0.079(7) 0.068(6) 0.096(8) 0.007(6) 0.023(6) -0.014(5) C17A 0.053(5) 0.048(5) 0.080(5) 0.004(4) 0.018(4) 0.003(4) C18 0.044(5) 0.048(4) 0.135(8) -0.011(8) 0.011(7) -0.008(4) C19 0.043(6) 0.081(7) 0.132(9) -0.005(7) -0.016(6) -0.006(5) C20 0.042(5) 0.062(5) 0.091(7) 0.000(5) -0.008(5) 0.001(5) N21 0.044(4) 0.046(3) 0.077(5) -0.001(3) 0.001(3) -0.003(3) C31 0.080(7) 0.070(6) 0.039(5) 0.012(5) -0.010(5) -0.055(6) C32 0.043(4) 0.032(3) 0.084(5) -0.002(7) 0.003(5) -0.010(3) C33 0.066(6) 0.047(5) 0.068(7) 0.009(5) -0.009(5) -0.027(5) C34 0.057(6) 0.063(6) 0.083(7) -0.012(5) 0.034(5) -0.021(5) C35 0.037(4) 0.064(5) 0.088(8) 0.039(6) -0.003(5) -0.014(4) C36 0.159(11) 0.175(11) 0.064(7) -0.024(7) -0.003(6) -0.120(10) C37 0.086(7) 0.040(4) 0.185(13) -0.018(6) 0.010(7) -0.010(4) C38 0.163(11) 0.132(9) 0.081(7) 0.059(7) -0.055(7) -0.066(8) C39 0.093(9) 0.117(10) 0.155(11) -0.003(8) 0.078(8) -0.019(7) C40 0.050(6) 0.094(8) 0.233(13) 0.074(8) -0.040(7) -0.021(6) _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 C33 2.144(8) . ? Rh1 C32 2.168(5) . ? Rh1 C31 2.171(8) . ? Rh1 C34 2.221(7) . ? Rh1 C35 2.219(7) . ? Rh1 P1 2.3220(17) . ? Rh1 Cl1 2.413(3) . ? Rh1 Cl2 2.414(3) . ? P1 C1 1.806(8) . ? P1 C7 1.820(7) . ? P1 C13 1.869(6) . ? C1 C6 1.378(10) . ? C1 C2 1.390(10) . ? C2 C3 1.352(10) . ? C3 C4 1.343(11) . ? C4 C5 1.369(11) . ? C5 C6 1.395(11) . ? C7 C12 1.369(10) . ? C7 C8 1.393(9) . ? C8 C9 1.395(10) . ? C9 C10 1.353(11) . ? C10 C11 1.353(11) . ? C11 C12 1.396(11) . ? N13 C14 1.372(9) . ? N13 C13 1.444(8) . ? C14 C15 1.362(10) . ? C14 C14A 1.435(10) . ? C14A N21 1.349(11) . ? C14A C17A 1.425(10) . ? C15 C16 1.421(11) . ? C16 C17 1.356(12) . ? C17 C17A 1.406(13) . ? C17A C18 1.381(12) . ? C18 C19 1.349(15) . ? C19 C20 1.357(11) . ? C20 N21 1.316(9) . ? C31 C32 1.425(13) . ? C31 C35 1.449(12) . ? C31 C36 1.509(11) . ? C32 C33 1.399(14) . ? C32 C37 1.511(10) . ? C33 C34 1.403(11) . ? C33 C38 1.510(11) . ? C34 C35 1.366(13) . ? C34 C39 1.519(11) . ? C35 C40 1.512(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 C33 Rh1 C32 37.9(4) . . ? C33 Rh1 C31 64.0(3) . . ? C32 Rh1 C31 38.4(4) . . ? C33 Rh1 C34 37.4(3) . . ? C32 Rh1 C34 62.2(3) . . ? C31 Rh1 C34 62.6(3) . . ? C33 Rh1 C35 62.4(3) . . ? C32 Rh1 C35 63.0(3) . . ? C31 Rh1 C35 38.5(3) . . ? C34 Rh1 C35 35.9(3) . . ? C33 Rh1 P1 111.9(3) . . ? C32 Rh1 P1 99.49(19) . . ? C31 Rh1 P1 120.4(3) . . ? C34 Rh1 P1 147.9(3) . . ? C35 Rh1 P1 158.9(3) . . ? C33 Rh1 Cl1 99.1(3) . . ? C32 Rh1 Cl1 135.9(4) . . ? C31 Rh1 Cl1 150.4(3) . . ? C34 Rh1 Cl1 89.0(2) . . ? C35 Rh1 Cl1 112.8(3) . . ? P1 Rh1 Cl1 87.91(6) . . ? C33 Rh1 Cl2 158.1(2) . . ? C32 Rh1 Cl2 131.7(4) . . ? C31 Rh1 Cl2 97.7(2) . . ? C34 Rh1 Cl2 124.8(3) . . ? C35 Rh1 Cl2 95.9(2) . . ? P1 Rh1 Cl2 87.27(6) . . ? Cl1 Rh1 Cl2 91.84(6) . . ? C1 P1 C7 107.1(4) . . ? C1 P1 C13 100.7(3) . . ? C7 P1 C13 102.9(3) . . ? C1 P1 Rh1 118.1(2) . . ? C7 P1 Rh1 114.2(2) . . ? C13 P1 Rh1 112.0(2) . . ? C6 C1 C2 116.1(7) . . ? C6 C1 P1 122.4(6) . . ? C2 C1 P1 120.8(6) . . ? C3 C2 C1 123.0(8) . . ? C4 C3 C2 119.1(8) . . ? C3 C4 C5 122.1(8) . . ? C4 C5 C6 117.8(8) . . ? C1 C6 C5 121.9(8) . . ? C12 C7 C8 118.5(7) . . ? C12 C7 P1 118.2(6) . . ? C8 C7 P1 123.3(6) . . ? C7 C8 C9 120.2(7) . . ? C10 C9 C8 120.0(8) . . ? C11 C10 C9 120.4(8) . . ? C10 C11 C12 120.6(8) . . ? C7 C12 C11 120.2(8) . . ? C14 N13 C13 124.6(7) . . ? N13 C13 P1 112.5(4) . . ? C15 C14 N13 125.4(8) . . ? C15 C14 C14A 117.7(7) . . ? N13 C14 C14A 116.9(7) . . ? N21 C14A C17A 121.9(7) . . ? N21 C14A C14 116.6(7) . . ? C17A C14A C14 121.4(9) . . ? C14 C15 C16 120.8(8) . . ? C17 C16 C15 121.9(8) . . ? C16 C17 C17A 120.1(9) . . ? C18 C17A C17 125.0(9) . . ? C18 C17A C14A 116.9(8) . . ? C17 C17A C14A 118.0(8) . . ? C19 C18 C17A 120.8(9) . . ? C18 C19 C20 117.9(8) . . ? N21 C20 C19 126.1(9) . . ? C20 N21 C14A 116.4(7) . . ? C32 C31 C35 105.9(8) . . ? C32 C31 C36 131.0(12) . . ? C35 C31 C36 122.6(10) . . ? C32 C31 Rh1 70.7(4) . . ? C35 C31 Rh1 72.5(5) . . ? C36 C31 Rh1 127.7(6) . . ? C33 C32 C31 108.2(7) . . ? C33 C32 C37 129.4(11) . . ? C31 C32 C37 122.3(12) . . ? C33 C32 Rh1 70.2(4) . . ? C31 C32 Rh1 70.9(4) . . ? C37 C32 Rh1 127.8(5) . . ? C34 C33 C32 108.1(8) . . ? C34 C33 C38 129.2(10) . . ? C32 C33 C38 121.9(10) . . ? C34 C33 Rh1 74.2(5) . . ? C32 C33 Rh1 72.0(4) . . ? C38 C33 Rh1 127.5(6) . . ? C35 C34 C33 109.4(7) . . ? C35 C34 C39 125.7(10) . . ? C33 C34 C39 124.9(10) . . ? C35 C34 Rh1 72.0(4) . . ? C33 C34 Rh1 68.3(4) . . ? C39 C34 Rh1 124.3(6) . . ? C34 C35 C31 108.2(7) . . ? C34 C35 C40 126.5(10) . . ? C31 C35 C40 125.2(10) . . ? C34 C35 Rh1 72.2(5) . . ? C31 C35 Rh1 69.0(4) . . ? C40 C35 Rh1 125.1(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 C33 Rh1 P1 C1 -103.7(4) . . . . ? C32 Rh1 P1 C1 -66.4(5) . . . . ? C31 Rh1 P1 C1 -31.9(4) . . . . ? C34 Rh1 P1 C1 -117.9(5) . . . . ? C35 Rh1 P1 C1 -33.9(8) . . . . ? Cl1 Rh1 P1 C1 157.4(3) . . . . ? Cl2 Rh1 P1 C1 65.4(3) . . . . ? C33 Rh1 P1 C7 23.5(4) . . . . ? C32 Rh1 P1 C7 60.8(5) . . . . ? C31 Rh1 P1 C7 95.4(4) . . . . ? C34 Rh1 P1 C7 9.4(5) . . . . ? C35 Rh1 P1 C7 93.3(7) . . . . ? Cl1 Rh1 P1 C7 -75.4(3) . . . . ? Cl2 Rh1 P1 C7 -167.3(3) . . . . ? C33 Rh1 P1 C13 140.0(4) . . . . ? C32 Rh1 P1 C13 177.3(6) . . . . ? C31 Rh1 P1 C13 -148.2(4) . . . . ? C34 Rh1 P1 C13 125.8(5) . . . . ? C35 Rh1 P1 C13 -150.3(7) . . . . ? Cl1 Rh1 P1 C13 41.0(3) . . . . ? Cl2 Rh1 P1 C13 -50.9(3) . . . . ? C7 P1 C1 C6 44.0(7) . . . . ? C13 P1 C1 C6 -63.2(7) . . . . ? Rh1 P1 C1 C6 174.6(6) . . . . ? C7 P1 C1 C2 -145.9(6) . . . . ? C13 P1 C1 C2 106.9(6) . . . . ? Rh1 P1 C1 C2 -15.3(7) . . . . ? C6 C1 C2 C3 0.1(11) . . . . ? P1 C1 C2 C3 -170.6(6) . . . . ? C1 C2 C3 C4 0.5(12) . . . . ? C2 C3 C4 C5 -1.3(13) . . . . ? C3 C4 C5 C6 1.5(14) . . . . ? C2 C1 C6 C5 0.1(12) . . . . ? P1 C1 C6 C5 170.6(6) . . . . ? C4 C5 C6 C1 -0.8(13) . . . . ? C1 P1 C7 C12 -155.5(6) . . . . ? C13 P1 C7 C12 -49.8(7) . . . . ? Rh1 P1 C7 C12 71.8(6) . . . . ? C1 P1 C7 C8 22.6(7) . . . . ? C13 P1 C7 C8 128.3(6) . . . . ? Rh1 P1 C7 C8 -110.1(6) . . . . ? C12 C7 C8 C9 -0.8(11) . . . . ? P1 C7 C8 C9 -178.9(6) . . . . ? C7 C8 C9 C10 2.3(13) . . . . ? C8 C9 C10 C11 -1.9(15) . . . . ? C9 C10 C11 C12 0.0(14) . . . . ? C8 C7 C12 C11 -1.0(11) . . . . ? P1 C7 C12 C11 177.2(6) . . . . ? C10 C11 C12 C7 1.5(13) . . . . ? C14 N13 C13 P1 -138.3(6) . . . . ? C1 P1 C13 N13 72.6(6) . . . . ? C7 P1 C13 N13 -38.0(6) . . . . ? Rh1 P1 C13 N13 -161.1(5) . . . . ? C13 N13 C14 C15 27.7(12) . . . . ? C13 N13 C14 C14A -151.7(7) . . . . ? C15 C14 C14A N21 -177.8(6) . . . . ? N13 C14 C14A N21 1.7(9) . . . . ? C15 C14 C14A C17A 2.9(10) . . . . ? N13 C14 C14A C17A -177.7(6) . . . . ? N13 C14 C15 C16 178.7(7) . . . . ? C14A C14 C15 C16 -1.9(11) . . . . ? C14 C15 C16 C17 0.1(14) . . . . ? C15 C16 C17 C17A 0.8(14) . . . . ? C16 C17 C17A C18 176.2(8) . . . . ? C16 C17 C17A C14A 0.2(13) . . . . ? N21 C14A C17A C18 2.3(10) . . . . ? C14 C14A C17A C18 -178.4(7) . . . . ? N21 C14A C17A C17 178.7(7) . . . . ? C14 C14A C17A C17 -2.0(11) . . . . ? C17 C17A C18 C19 -176.6(8) . . . . ? C14A C17A C18 C19 -0.5(12) . . . . ? C17A C18 C19 C20 -1.1(14) . . . . ? C18 C19 C20 N21 1.2(14) . . . . ? C19 C20 N21 C14A 0.5(12) . . . . ? C17A C14A N21 C20 -2.3(10) . . . . ? C14 C14A N21 C20 178.4(6) . . . . ? C33 Rh1 C31 C32 36.9(6) . . . . ? C34 Rh1 C31 C32 79.0(6) . . . . ? C35 Rh1 C31 C32 114.5(7) . . . . ? P1 Rh1 C31 C32 -64.3(6) . . . . ? Cl1 Rh1 C31 C32 96.7(9) . . . . ? Cl2 Rh1 C31 C32 -155.7(6) . . . . ? C33 Rh1 C31 C35 -77.6(5) . . . . ? C32 Rh1 C31 C35 -114.5(7) . . . . ? C34 Rh1 C31 C35 -35.5(5) . . . . ? P1 Rh1 C31 C35 -178.8(4) . . . . ? Cl1 Rh1 C31 C35 -17.7(8) . . . . ? Cl2 Rh1 C31 C35 89.9(5) . . . . ? C33 Rh1 C31 C36 164.4(13) . . . . ? C32 Rh1 C31 C36 127.4(14) . . . . ? C34 Rh1 C31 C36 -153.5(12) . . . . ? C35 Rh1 C31 C36 -118.1(13) . . . . ? P1 Rh1 C31 C36 63.1(11) . . . . ? Cl1 Rh1 C31 C36 -135.8(9) . . . . ? Cl2 Rh1 C31 C36 -28.2(11) . . . . ? C35 C31 C32 C33 3.9(7) . . . . ? C36 C31 C32 C33 175.8(8) . . . . ? Rh1 C31 C32 C33 -60.6(5) . . . . ? C35 C31 C32 C37 -172.3(6) . . . . ? C36 C31 C32 C37 -0.4(12) . . . . ? Rh1 C31 C32 C37 123.2(7) . . . . ? C35 C31 C32 Rh1 64.5(5) . . . . ? C36 C31 C32 Rh1 -123.6(9) . . . . ? C31 Rh1 C32 C33 118.4(7) . . . . ? C34 Rh1 C32 C33 38.3(5) . . . . ? C35 Rh1 C32 C33 78.9(6) . . . . ? P1 Rh1 C32 C33 -113.7(5) . . . . ? Cl1 Rh1 C32 C33 -16.8(6) . . . . ? Cl2 Rh1 C32 C33 151.5(5) . . . . ? C33 Rh1 C32 C31 -118.4(7) . . . . ? C34 Rh1 C32 C31 -80.0(5) . . . . ? C35 Rh1 C32 C31 -39.5(5) . . . . ? P1 Rh1 C32 C31 128.0(5) . . . . ? Cl1 Rh1 C32 C31 -135.2(6) . . . . ? Cl2 Rh1 C32 C31 33.1(7) . . . . ? C33 Rh1 C32 C37 125.0(14) . . . . ? C31 Rh1 C32 C37 -116.6(15) . . . . ? C34 Rh1 C32 C37 163.3(13) . . . . ? C35 Rh1 C32 C37 -156.1(13) . . . . ? P1 Rh1 C32 C37 11.4(12) . . . . ? Cl1 Rh1 C32 C37 108.2(11) . . . . ? Cl2 Rh1 C32 C37 -83.5(11) . . . . ? C31 C32 C33 C34 -4.9(8) . . . . ? C37 C32 C33 C34 170.9(7) . . . . ? Rh1 C32 C33 C34 -66.0(5) . . . . ? C31 C32 C33 C38 -175.5(7) . . . . ? C37 C32 C33 C38 0.3(12) . . . . ? Rh1 C32 C33 C38 123.4(8) . . . . ? C31 C32 C33 Rh1 61.1(5) . . . . ? C37 C32 C33 Rh1 -123.1(7) . . . . ? C32 Rh1 C33 C34 115.5(7) . . . . ? C31 Rh1 C33 C34 78.1(5) . . . . ? C35 Rh1 C33 C34 34.8(5) . . . . ? P1 Rh1 C33 C34 -167.6(5) . . . . ? Cl1 Rh1 C33 C34 -76.3(5) . . . . ? Cl2 Rh1 C33 C34 42.7(10) . . . . ? C31 Rh1 C33 C32 -37.4(5) . . . . ? C34 Rh1 C33 C32 -115.5(7) . . . . ? C35 Rh1 C33 C32 -80.8(6) . . . . ? P1 Rh1 C33 C32 76.8(5) . . . . ? Cl1 Rh1 C33 C32 168.2(5) . . . . ? Cl2 Rh1 C33 C32 -72.8(10) . . . . ? C32 Rh1 C33 C38 -116.8(12) . . . . ? C31 Rh1 C33 C38 -154.2(12) . . . . ? C34 Rh1 C33 C38 127.6(12) . . . . ? C35 Rh1 C33 C38 162.4(11) . . . . ? P1 Rh1 C33 C38 -40.0(10) . . . . ? Cl1 Rh1 C33 C38 51.4(10) . . . . ? Cl2 Rh1 C33 C38 170.4(7) . . . . ? C32 C33 C34 C35 4.1(9) . . . . ? C38 C33 C34 C35 173.7(8) . . . . ? Rh1 C33 C34 C35 -60.5(6) . . . . ? C32 C33 C34 C39 -178.0(7) . . . . ? C38 C33 C34 C39 -8.3(13) . . . . ? Rh1 C33 C34 C39 117.5(8) . . . . ? C32 C33 C34 Rh1 64.5(5) . . . . ? C38 C33 C34 Rh1 -125.8(9) . . . . ? C33 Rh1 C34 C35 120.4(7) . . . . ? C32 Rh1 C34 C35 81.6(6) . . . . ? C31 Rh1 C34 C35 38.1(5) . . . . ? P1 Rh1 C34 C35 142.3(5) . . . . ? Cl1 Rh1 C34 C35 -133.2(6) . . . . ? Cl2 Rh1 C34 C35 -41.7(6) . . . . ? C32 Rh1 C34 C33 -38.8(5) . . . . ? C31 Rh1 C34 C33 -82.3(5) . . . . ? C35 Rh1 C34 C33 -120.4(7) . . . . ? P1 Rh1 C34 C33 21.9(8) . . . . ? Cl1 Rh1 C34 C33 106.4(5) . . . . ? Cl2 Rh1 C34 C33 -162.1(4) . . . . ? C33 Rh1 C34 C39 -118.3(12) . . . . ? C32 Rh1 C34 C39 -157.0(11) . . . . ? C31 Rh1 C34 C39 159.4(11) . . . . ? C35 Rh1 C34 C39 121.3(13) . . . . ? P1 Rh1 C34 C39 -96.4(10) . . . . ? Cl1 Rh1 C34 C39 -11.9(9) . . . . ? Cl2 Rh1 C34 C39 79.6(10) . . . . ? C33 C34 C35 C31 -1.6(9) . . . . ? C39 C34 C35 C31 -179.5(8) . . . . ? Rh1 C34 C35 C31 -59.8(5) . . . . ? C33 C34 C35 C40 179.1(7) . . . . ? C39 C34 C35 C40 1.1(13) . . . . ? Rh1 C34 C35 C40 120.9(8) . . . . ? C33 C34 C35 Rh1 58.2(6) . . . . ? C39 C34 C35 Rh1 -119.7(8) . . . . ? C32 C31 C35 C34 -1.5(8) . . . . ? C36 C31 C35 C34 -174.2(8) . . . . ? Rh1 C31 C35 C34 61.8(6) . . . . ? C32 C31 C35 C40 177.9(7) . . . . ? C36 C31 C35 C40 5.2(12) . . . . ? Rh1 C31 C35 C40 -118.8(7) . . . . ? C32 C31 C35 Rh1 -63.3(5) . . . . ? C36 C31 C35 Rh1 124.0(8) . . . . ? C33 Rh1 C35 C34 -36.3(5) . . . . ? C32 Rh1 C35 C34 -79.1(6) . . . . ? C31 Rh1 C35 C34 -118.4(7) . . . . ? P1 Rh1 C35 C34 -115.6(9) . . . . ? Cl1 Rh1 C35 C34 52.2(6) . . . . ? Cl2 Rh1 C35 C34 146.7(5) . . . . ? C33 Rh1 C35 C31 82.1(5) . . . . ? C32 Rh1 C35 C31 39.3(5) . . . . ? C34 Rh1 C35 C31 118.4(7) . . . . ? P1 Rh1 C35 C31 2.9(10) . . . . ? Cl1 Rh1 C35 C31 170.6(4) . . . . ? Cl2 Rh1 C35 C31 -94.9(5) . . . . ? C33 Rh1 C35 C40 -158.8(11) . . . . ? C32 Rh1 C35 C40 158.4(12) . . . . ? C31 Rh1 C35 C40 119.0(12) . . . . ? C34 Rh1 C35 C40 -122.5(13) . . . . ? P1 Rh1 C35 C40 121.9(8) . . . . ? Cl1 Rh1 C35 C40 -70.4(10) . . . . ? Cl2 Rh1 C35 C40 24.1(10) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N13 H13N N21 0.980(4) 2.21(8) 2.661(9) 106(6) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.419 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.058