# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge ? _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Kapil S. Lokare' _publ_contact_author_email klokare@scripps.EDU _publ_section_title ; Rhodium complexes bearing a tetradentate diamine–bis(phenolate) ligands ; loop_ _publ_author_name 'Kapil S. Lokare' 'Xiang Y. Liu' 'Somesh K. Ganesh' 'Jason M. Gonzales' 'Jonas Oxgaard' 'William A. Goddard III' 'Roy A. Periana' # Attachment 'structures.cif' data_c:\frames\irina\periana\rhclco\work\p21c _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H53 Cl N2 O4 Rh' _chemical_formula_weight 740.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Rh' 'Rh' -1.1178 0.9187 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.7408(13) _cell_length_b 17.9422(10) _cell_length_c 15.7257(9) _cell_angle_alpha 90.00 _cell_angle_beta 119.7460(10) _cell_angle_gamma 90.00 _cell_volume 3856.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 7846 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 26.22 _exptl_crystal_description ? _exptl_crystal_colour orange _exptl_crystal_size_max 0.118 _exptl_crystal_size_mid 0.106 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.275 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1556 _exptl_absorpt_coefficient_mu 0.551 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22172 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 26.42 _reflns_number_total 7877 _reflns_number_gt 5832 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+1.2422P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00000(15) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7877 _refine_ls_number_parameters 440 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1237 _refine_ls_wR_factor_gt 0.1132 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 7.894 _refine_ls_shift/su_mean 0.019 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 0.566657(19) 0.833804(13) 0.840705(19) 0.03880(11) Uani 1 1 d . . . Cl1 Cl 0.57968(8) 0.96444(5) 0.82529(8) 0.0622(3) Uani 1 1 d . . . O1 O 0.45440(18) 0.83473(12) 0.69934(17) 0.0453(6) Uani 1 1 d . . . O2 O 0.67535(18) 0.84041(12) 0.97940(18) 0.0513(6) Uani 1 1 d . A . O3 O 0.6588(2) 0.81774(15) 0.7817(2) 0.0677(8) Uani 1 1 d . . . O4 O 0.5650(3) 0.8937(2) 0.6184(3) 0.1045(12) Uiso 1 1 d . . . N1 N 0.55973(19) 0.72162(14) 0.85739(19) 0.0402(6) Uani 1 1 d . . . N2 N 0.4774(2) 0.83931(14) 0.89510(18) 0.0386(6) Uani 1 1 d . . . C1 C 0.4354(3) 0.9017(2) 0.9055(3) 0.0544(10) Uani 1 1 d . . . H1 H 0.4460 0.9468 0.8831 0.065 Uiso 1 1 calc R . . C2 C 0.3775(3) 0.9005(3) 0.9483(3) 0.0741(13) Uani 1 1 d . . . H2 H 0.3505 0.9443 0.9561 0.089 Uiso 1 1 calc R . . C3 C 0.3601(4) 0.8331(3) 0.9794(4) 0.0848(16) Uani 1 1 d . . . H3 H 0.3196 0.8306 1.0067 0.102 Uiso 1 1 calc R . . C4 C 0.4035(3) 0.7699(3) 0.9695(3) 0.0699(12) Uani 1 1 d . . . H4 H 0.3931 0.7243 0.9910 0.084 Uiso 1 1 calc R . . C5 C 0.4626(3) 0.77392(19) 0.9279(2) 0.0444(8) Uani 1 1 d . . . C6 C 0.5194(3) 0.70869(19) 0.9238(3) 0.0472(8) Uani 1 1 d . . . H6A H 0.5728 0.6983 0.9892 0.057 Uiso 1 1 calc R . . H6B H 0.4772 0.6652 0.9016 0.057 Uiso 1 1 calc R . . C7 C 0.3767(3) 0.78996(18) 0.6756(2) 0.0418(8) Uani 1 1 d . . . C8 C 0.2790(3) 0.8142(2) 0.6162(2) 0.0475(9) Uani 1 1 d . . . C9 C 0.2537(3) 0.8936(2) 0.5728(3) 0.0577(10) Uani 1 1 d . . . C10 C 0.3011(4) 0.9107(3) 0.5114(4) 0.0937(17) Uani 1 1 d . . . H10A H 0.2811 0.9592 0.4826 0.141 Uiso 1 1 calc R . . H10B H 0.2813 0.8740 0.4605 0.141 Uiso 1 1 calc R . . H10C H 0.3710 0.9095 0.5521 0.141 Uiso 1 1 calc R . . C11 C 0.2878(4) 0.9497(3) 0.6552(4) 0.0928(17) Uani 1 1 d . . . H11A H 0.3575 0.9462 0.6962 0.139 Uiso 1 1 calc R . . H11B H 0.2568 0.9395 0.6933 0.139 Uiso 1 1 calc R . . H11C H 0.2708 0.9991 0.6284 0.139 Uiso 1 1 calc R . . C12 C 0.1432(4) 0.9037(3) 0.5053(5) 0.115(2) Uani 1 1 d . . . H12A H 0.1104 0.8976 0.5425 0.173 Uiso 1 1 calc R . . H12B H 0.1197 0.8671 0.4540 0.173 Uiso 1 1 calc R . . H12C H 0.1304 0.9527 0.4770 0.173 Uiso 1 1 calc R . . C13 C 0.2044(3) 0.7638(2) 0.5991(3) 0.0511(9) Uani 1 1 d . . . H13 H 0.1401 0.7798 0.5608 0.061 Uiso 1 1 calc R . . C14 C 0.2200(3) 0.6914(2) 0.6355(3) 0.0484(9) Uani 1 1 d . . . C15 C 0.1363(3) 0.6387(2) 0.6197(3) 0.0643(11) Uani 1 1 d . . . C16 C 0.1475(4) 0.6219(3) 0.7205(4) 0.0977(17) Uani 1 1 d . . . H16A H 0.0929 0.5926 0.7124 0.147 Uiso 1 1 calc R . . H16B H 0.1496 0.6678 0.7528 0.147 Uiso 1 1 calc R . . H16C H 0.2070 0.5946 0.7594 0.147 Uiso 1 1 calc R . . C17 C 0.0352(3) 0.6728(3) 0.5567(4) 0.0832(14) Uani 1 1 d . . . H17A H 0.0270 0.6862 0.4940 0.125 Uiso 1 1 calc R . . H17B H 0.0289 0.7165 0.5884 0.125 Uiso 1 1 calc R . . H17C H -0.0139 0.6372 0.5481 0.125 Uiso 1 1 calc R . . C18 C 0.1440(4) 0.5666(3) 0.5720(4) 0.0924(17) Uani 1 1 d . . . H18A H 0.1379 0.5778 0.5095 0.139 Uiso 1 1 calc R . . H18B H 0.0927 0.5332 0.5632 0.139 Uiso 1 1 calc R . . H18C H 0.2063 0.5437 0.6134 0.139 Uiso 1 1 calc R . . C19 C 0.3163(3) 0.66864(19) 0.6893(2) 0.0487(9) Uani 1 1 d . . . H19 H 0.3297 0.6202 0.7135 0.058 Uiso 1 1 calc R . . C20 C 0.3934(3) 0.71563(18) 0.7082(2) 0.0434(8) Uani 1 1 d . . . C21 C 0.4956(3) 0.68716(19) 0.7583(3) 0.0474(9) Uani 1 1 d . . . H21A H 0.5242 0.6968 0.7171 0.057 Uiso 1 1 calc R . . H21B H 0.4944 0.6336 0.7660 0.057 Uiso 1 1 calc R . . C22 C 0.6591(3) 0.68692(19) 0.8985(3) 0.0480(9) Uani 1 1 d . . . H22A H 0.6831 0.6961 0.8534 0.058 Uiso 1 1 calc R . . H22B H 0.6522 0.6334 0.9017 0.058 Uiso 1 1 calc R . . C23 C 0.7349(2) 0.71381(18) 0.9984(2) 0.0441(8) Uani 1 1 d . A . C24 C 0.8086(3) 0.66431(18) 1.0569(3) 0.0489(9) Uani 1 1 d . . . H24 H 0.8071 0.6166 1.0331 0.059 Uiso 1 1 calc R . . C25 C 0.8842(3) 0.68256(19) 1.1488(3) 0.0482(9) Uani 1 1 d . A . C26 C 0.9678(3) 0.6279(2) 1.2095(3) 0.0559(10) Uani 1 1 d . . . C27 C 1.0538(6) 0.6662(4) 1.2945(7) 0.101(3) Uani 0.775(11) 1 d P A 1 H27A H 1.0361 0.6804 1.3425 0.152 Uiso 0.775(11) 1 calc PR A 1 H27B H 1.0714 0.7097 1.2712 0.152 Uiso 0.775(11) 1 calc PR A 1 H27C H 1.1085 0.6326 1.3236 0.152 Uiso 0.775(11) 1 calc PR A 1 C28 C 1.0084(5) 0.5996(4) 1.1431(5) 0.092(3) Uani 0.775(11) 1 d P A 1 H28A H 1.0612 0.5654 1.1793 0.137 Uiso 0.775(11) 1 calc PR A 1 H28B H 1.0319 0.6412 1.1222 0.137 Uiso 0.775(11) 1 calc PR A 1 H28C H 0.9573 0.5749 1.0868 0.137 Uiso 0.775(11) 1 calc PR A 1 C29 C 0.9312(6) 0.5644(5) 1.2406(8) 0.100(3) Uani 0.775(11) 1 d P A 1 H29A H 0.8756 0.5432 1.1846 0.150 Uiso 0.775(11) 1 calc PR A 1 H29B H 0.9124 0.5810 1.2869 0.150 Uiso 0.775(11) 1 calc PR A 1 H29C H 0.9817 0.5275 1.2706 0.150 Uiso 0.775(11) 1 calc PR A 1 C39 C 0.9682(14) 0.5572(11) 1.1560(13) 0.055(6) Uiso 0.225(11) 1 d P A 2 H39A H 1.0240 0.5274 1.1984 0.082 Uiso 0.225(11) 1 calc PR A 2 H39B H 0.9713 0.5702 1.0984 0.082 Uiso 0.225(11) 1 calc PR A 2 H39C H 0.9095 0.5293 1.1375 0.082 Uiso 0.225(11) 1 calc PR A 2 C40 C 1.068(2) 0.6625(15) 1.251(2) 0.074(8) Uiso 0.225(11) 1 d P A 2 H40A H 1.1163 0.6280 1.2956 0.111 Uiso 0.225(11) 1 calc PR A 2 H40B H 1.0704 0.7072 1.2860 0.111 Uiso 0.225(11) 1 calc PR A 2 H40C H 1.0806 0.6743 1.1992 0.111 Uiso 0.225(11) 1 calc PR A 2 C41 C 0.9513(15) 0.5959(12) 1.2992(16) 0.059(6) Uiso 0.225(11) 1 d P A 2 H41A H 0.8892 0.5712 1.2719 0.088 Uiso 0.225(11) 1 calc PR A 2 H41B H 0.9528 0.6367 1.3394 0.088 Uiso 0.225(11) 1 calc PR A 2 H41C H 1.0025 0.5613 1.3383 0.088 Uiso 0.225(11) 1 calc PR A 2 C30 C 0.8781(3) 0.7520(2) 1.1845(3) 0.0499(9) Uani 1 1 d . . . H30 H 0.9256 0.7643 1.2481 0.060 Uiso 1 1 calc R A . C31 C 0.8059(2) 0.80398(19) 1.1316(2) 0.0439(8) Uani 1 1 d . A . C32 C 0.8003(3) 0.8783(2) 1.1763(3) 0.0556(10) Uani 1 1 d . . . C33 C 0.8765(4) 0.8827(3) 1.2859(3) 0.0880(17) Uani 1 1 d . A . H33A H 0.8656 0.8429 1.3201 0.132 Uiso 1 1 calc R . . H33B H 0.8704 0.9297 1.3117 0.132 Uiso 1 1 calc R . . H33C H 0.9410 0.8784 1.2942 0.132 Uiso 1 1 calc R . . C34 C 0.8185(3) 0.9435(2) 1.1240(3) 0.0731(13) Uani 1 1 d . A . H34A H 0.8813 0.9376 1.1286 0.110 Uiso 1 1 calc R . . H34B H 0.8171 0.9896 1.1542 0.110 Uiso 1 1 calc R . . H34C H 0.7685 0.9440 1.0563 0.110 Uiso 1 1 calc R . . C35 C 0.6979(3) 0.8859(2) 1.1658(3) 0.0712(12) Uani 1 1 d . A . H35A H 0.6493 0.8870 1.0976 0.107 Uiso 1 1 calc R . . H35B H 0.6947 0.9312 1.1965 0.107 Uiso 1 1 calc R . . H35C H 0.6860 0.8442 1.1967 0.107 Uiso 1 1 calc R . . C36 C 0.7359(2) 0.78667(18) 1.0327(2) 0.0431(8) Uani 1 1 d . . . C37 C 0.7601(4) 0.8416(3) 0.8360(5) 0.0978(18) Uani 1 1 d . . . H37A H 0.7630 0.8927 0.8554 0.147 Uiso 1 1 calc R . . H37B H 0.7894 0.8368 0.7954 0.147 Uiso 1 1 calc R . . H37C H 0.7950 0.8110 0.8933 0.147 Uiso 1 1 calc R . . C38 C 0.6126(7) 0.9585(4) 0.6137(5) 0.145(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 Rh1 0.04434(17) 0.02945(15) 0.04607(17) 0.00113(11) 0.02505(13) 0.00270(11) Cl1 0.0716(7) 0.0336(5) 0.0850(7) 0.0047(4) 0.0416(6) -0.0019(4) O1 0.0559(15) 0.0419(14) 0.0413(12) 0.0050(10) 0.0265(11) -0.0001(11) O2 0.0497(15) 0.0318(13) 0.0553(14) -0.0063(11) 0.0131(12) 0.0069(10) O3 0.075(2) 0.0542(17) 0.101(2) -0.0020(15) 0.0643(19) 0.0008(14) N1 0.0409(16) 0.0317(14) 0.0438(15) 0.0003(12) 0.0179(13) 0.0041(11) N2 0.0433(16) 0.0386(15) 0.0335(13) 0.0028(12) 0.0188(12) 0.0067(12) C1 0.062(3) 0.048(2) 0.053(2) 0.0072(17) 0.0283(19) 0.0197(18) C2 0.086(3) 0.083(3) 0.068(3) 0.021(2) 0.050(3) 0.042(3) C3 0.086(4) 0.113(4) 0.083(3) 0.033(3) 0.062(3) 0.038(3) C4 0.075(3) 0.076(3) 0.077(3) 0.033(2) 0.051(3) 0.016(2) C5 0.046(2) 0.045(2) 0.0413(18) 0.0066(15) 0.0208(16) 0.0034(15) C6 0.053(2) 0.0361(19) 0.049(2) 0.0063(15) 0.0228(17) 0.0025(15) C7 0.058(2) 0.0345(18) 0.0362(17) -0.0001(14) 0.0260(16) 0.0015(15) C8 0.059(2) 0.044(2) 0.0388(18) 0.0033(15) 0.0235(17) 0.0088(17) C9 0.063(3) 0.050(2) 0.056(2) 0.0151(18) 0.026(2) 0.0143(19) C10 0.110(4) 0.093(4) 0.086(3) 0.048(3) 0.055(3) 0.029(3) C11 0.135(5) 0.055(3) 0.088(3) 0.010(3) 0.055(3) 0.030(3) C12 0.078(4) 0.088(4) 0.135(5) 0.058(4) 0.018(4) 0.027(3) C13 0.046(2) 0.055(2) 0.045(2) 0.0030(17) 0.0175(17) 0.0068(17) C14 0.050(2) 0.045(2) 0.0458(19) -0.0024(16) 0.0202(17) -0.0014(16) C15 0.055(3) 0.059(3) 0.066(3) 0.000(2) 0.020(2) -0.009(2) C16 0.097(4) 0.095(4) 0.106(4) 0.017(3) 0.054(4) -0.020(3) C17 0.060(3) 0.081(4) 0.097(4) -0.001(3) 0.030(3) -0.005(2) C18 0.070(3) 0.062(3) 0.122(4) -0.022(3) 0.029(3) -0.014(2) C19 0.057(2) 0.0382(19) 0.0413(18) 0.0016(15) 0.0167(16) 0.0033(17) C20 0.047(2) 0.0358(18) 0.0393(17) -0.0022(14) 0.0154(15) 0.0014(15) C21 0.053(2) 0.0339(18) 0.0467(19) -0.0069(15) 0.0184(17) 0.0043(15) C22 0.048(2) 0.0338(18) 0.056(2) -0.0040(16) 0.0203(17) 0.0084(15) C23 0.042(2) 0.0352(18) 0.0503(19) -0.0021(15) 0.0193(16) 0.0041(14) C24 0.053(2) 0.0308(18) 0.060(2) -0.0015(16) 0.0259(18) 0.0082(15) C25 0.041(2) 0.041(2) 0.060(2) 0.0014(16) 0.0227(17) 0.0037(15) C26 0.045(2) 0.046(2) 0.064(2) 0.0095(19) 0.0175(19) 0.0113(17) C27 0.076(5) 0.075(5) 0.090(6) 0.010(4) -0.006(4) 0.034(4) C28 0.073(5) 0.085(5) 0.118(6) 0.025(4) 0.049(4) 0.040(4) C29 0.089(5) 0.086(6) 0.140(8) 0.062(6) 0.068(5) 0.047(4) C30 0.045(2) 0.043(2) 0.051(2) 0.0005(16) 0.0158(17) 0.0012(16) C31 0.0415(19) 0.0349(17) 0.051(2) -0.0032(15) 0.0195(16) -0.0008(15) C32 0.052(2) 0.046(2) 0.053(2) -0.0113(17) 0.0135(18) 0.0022(17) C33 0.090(4) 0.063(3) 0.066(3) -0.021(2) 0.004(3) 0.015(3) C34 0.062(3) 0.036(2) 0.098(3) -0.007(2) 0.023(2) -0.0070(19) C35 0.075(3) 0.064(3) 0.080(3) -0.019(2) 0.042(3) 0.006(2) C36 0.0395(19) 0.0340(18) 0.0511(19) 0.0006(15) 0.0190(16) 0.0055(14) C37 0.077(4) 0.099(4) 0.147(5) 0.019(4) 0.078(4) 0.010(3) C38 0.208(8) 0.110(6) 0.106(5) 0.015(4) 0.069(5) 0.003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N2 1.977(3) . ? Rh1 O2 1.999(2) . ? Rh1 N1 2.040(3) . ? Rh1 O1 2.041(2) . ? Rh1 O3 2.093(3) . ? Rh1 Cl1 2.3757(9) . ? O1 C7 1.352(4) . ? O2 C36 1.323(4) . ? O3 C37 1.451(6) . ? O4 C38 1.406(8) . ? N1 C6 1.485(4) . ? N1 C22 1.499(4) . ? N1 C21 1.506(4) . ? N2 C5 1.348(4) . ? N2 C1 1.351(4) . ? C1 C2 1.375(6) . ? C2 C3 1.382(6) . ? C3 C4 1.371(6) . ? C4 C5 1.379(5) . ? C5 C6 1.494(5) . ? C7 C20 1.406(4) . ? C7 C8 1.414(5) . ? C8 C13 1.397(5) . ? C8 C9 1.545(5) . ? C9 C11 1.514(6) . ? C9 C10 1.516(6) . ? C9 C12 1.534(6) . ? C13 C14 1.392(5) . ? C14 C19 1.381(5) . ? C14 C15 1.539(6) . ? C15 C17 1.523(6) . ? C15 C18 1.530(6) . ? C15 C16 1.536(6) . ? C19 C20 1.383(5) . ? C20 C21 1.488(5) . ? C22 C23 1.505(5) . ? C23 C24 1.387(5) . ? C23 C36 1.411(4) . ? C24 C25 1.380(5) . ? C25 C30 1.389(5) . ? C25 C26 1.536(5) . ? C26 C29 1.465(8) . ? C26 C40 1.51(3) . ? C26 C27 1.516(8) . ? C26 C39 1.524(18) . ? C26 C28 1.555(8) . ? C26 C41 1.66(2) . ? C30 C31 1.385(5) . ? C31 C36 1.424(5) . ? C31 C32 1.531(5) . ? C32 C33 1.536(5) . ? C32 C34 1.537(6) . ? C32 C35 1.542(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Rh1 O2 86.11(11) . . ? N2 Rh1 N1 84.19(11) . . ? O2 Rh1 N1 89.40(10) . . ? N2 Rh1 O1 93.09(10) . . ? O2 Rh1 O1 176.08(9) . . ? N1 Rh1 O1 94.33(10) . . ? N2 Rh1 O3 174.89(11) . . ? O2 Rh1 O3 94.92(12) . . ? N1 Rh1 O3 90.81(11) . . ? O1 Rh1 O3 86.22(11) . . ? N2 Rh1 Cl1 96.35(8) . . ? O2 Rh1 Cl1 88.99(7) . . ? N1 Rh1 Cl1 178.26(8) . . ? O1 Rh1 Cl1 87.29(7) . . ? O3 Rh1 Cl1 88.68(8) . . ? C7 O1 Rh1 118.13(19) . . ? C36 O2 Rh1 127.3(2) . . ? C37 O3 Rh1 120.0(3) . . ? C6 N1 C22 110.5(3) . . ? C6 N1 C21 111.2(3) . . ? C22 N1 C21 107.2(3) . . ? C6 N1 Rh1 108.26(19) . . ? C22 N1 Rh1 110.8(2) . . ? C21 N1 Rh1 108.9(2) . . ? C5 N2 C1 119.1(3) . . ? C5 N2 Rh1 114.7(2) . . ? C1 N2 Rh1 126.1(2) . . ? N2 C1 C2 122.0(4) . . ? C1 C2 C3 118.9(4) . . ? C4 C3 C2 119.1(4) . . ? C3 C4 C5 120.1(4) . . ? N2 C5 C4 120.9(3) . . ? N2 C5 C6 116.3(3) . . ? C4 C5 C6 122.6(3) . . ? N1 C6 C5 112.5(3) . . ? O1 C7 C20 118.9(3) . . ? O1 C7 C8 122.6(3) . . ? C20 C7 C8 118.5(3) . . ? C13 C8 C7 117.6(3) . . ? C13 C8 C9 120.2(3) . . ? C7 C8 C9 122.2(3) . . ? C11 C9 C10 109.5(4) . . ? C11 C9 C12 108.3(4) . . ? C10 C9 C12 106.4(4) . . ? C11 C9 C8 109.3(3) . . ? C10 C9 C8 111.5(3) . . ? C12 C9 C8 111.7(4) . . ? C14 C13 C8 124.3(3) . . ? C19 C14 C13 116.4(3) . . ? C19 C14 C15 120.6(3) . . ? C13 C14 C15 123.0(3) . . ? C17 C15 C18 109.4(4) . . ? C17 C15 C16 107.3(4) . . ? C18 C15 C16 110.1(4) . . ? C17 C15 C14 113.2(4) . . ? C18 C15 C14 109.2(4) . . ? C16 C15 C14 107.7(3) . . ? C14 C19 C20 122.0(3) . . ? C19 C20 C7 121.0(3) . . ? C19 C20 C21 120.5(3) . . ? C7 C20 C21 118.5(3) . . ? C20 C21 N1 113.6(3) . . ? N1 C22 C23 115.8(3) . . ? C24 C23 C36 119.5(3) . . ? C24 C23 C22 117.1(3) . . ? C36 C23 C22 123.3(3) . . ? C25 C24 C23 123.1(3) . . ? C24 C25 C30 116.1(3) . . ? C24 C25 C26 121.8(3) . . ? C30 C25 C26 122.1(3) . . ? C29 C26 C40 132.3(11) . . ? C29 C26 C27 112.6(6) . . ? C40 C26 C27 31.2(9) . . ? C29 C26 C39 69.4(8) . . ? C40 C26 C39 107.2(12) . . ? C27 C26 C39 128.1(8) . . ? C29 C26 C25 110.3(4) . . ? C40 C26 C25 113.3(11) . . ? C27 C26 C25 111.9(4) . . ? C39 C26 C25 115.2(7) . . ? C29 C26 C28 109.4(5) . . ? C40 C26 C28 74.9(10) . . ? C27 C26 C28 104.7(6) . . ? C39 C26 C28 40.8(7) . . ? C25 C26 C28 107.6(4) . . ? C29 C26 C41 36.3(7) . . ? C40 C26 C41 109.9(12) . . ? C27 C26 C41 81.6(8) . . ? C39 C26 C41 103.1(10) . . ? C25 C26 C41 107.6(8) . . ? C28 C26 C41 138.5(8) . . ? C31 C30 C25 124.2(3) . . ? C30 C31 C36 118.0(3) . . ? C30 C31 C32 121.9(3) . . ? C36 C31 C32 120.2(3) . . ? C31 C32 C33 111.7(3) . . ? C31 C32 C34 110.4(3) . . ? C33 C32 C34 108.2(3) . . ? C31 C32 C35 108.8(3) . . ? C33 C32 C35 108.0(4) . . ? C34 C32 C35 109.8(3) . . ? O2 C36 C23 124.4(3) . . ? O2 C36 C31 117.2(3) . . ? C23 C36 C31 118.4(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.367 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.072 #===END data_perianam _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H40 Cl N2 O4 Rh' _chemical_formula_weight 594.97 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' '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 Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.740(3) _cell_length_b 19.505(4) _cell_length_c 24.825(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5685(2) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3815 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 24.98 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2480 _exptl_absorpt_coefficient_mu 0.728 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.580 _exptl_absorpt_correction_T_max 0.645 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30572 _diffrn_reflns_av_R_equivalents 0.0615 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.68 _reflns_number_total 5392 _reflns_number_gt 3725 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0792P)^2^+4.1646P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5392 _refine_ls_number_parameters 325 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0786 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1504 _refine_ls_wR_factor_gt 0.1307 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.46756(3) 1.022356(18) 0.350088(14) 0.04182(16) Uani 1 1 d . . . Cl1 Cl 0.32950(11) 1.10089(7) 0.32056(5) 0.0593(4) Uani 1 1 d . . . O1 O 0.5368(3) 1.10111(17) 0.39360(13) 0.0530(8) Uani 1 1 d . . . O2 O 0.3776(3) 0.94648(16) 0.31535(14) 0.0535(8) Uani 1 1 d . . . O3 O 0.3662(3) 1.00705(18) 0.42013(14) 0.0561(9) Uani 1 1 d . . . N1 N 0.5716(3) 1.03599(18) 0.28626(16) 0.0428(9) Uani 1 1 d . . . N2 N 0.5910(4) 0.9535(2) 0.37802(18) 0.0567(11) Uani 1 1 d . . . C1 C 0.6377(4) 1.1299(2) 0.3823(2) 0.0520(12) Uani 1 1 d . . . C2 C 0.7016(5) 1.1579(2) 0.4250(2) 0.0571(13) Uani 1 1 d . . . C3 C 0.8095(5) 1.1839(3) 0.4131(3) 0.0667(15) Uani 1 1 d . . . H3 H 0.8523 1.2023 0.4411 0.080 Uiso 1 1 calc R . . C4 C 0.8564(5) 1.1838(3) 0.3621(3) 0.0624(14) Uani 1 1 d . . . C5 C 0.7897(4) 1.1582(2) 0.3211(2) 0.0542(12) Uani 1 1 d . . . H5 H 0.8186 1.1579 0.2862 0.065 Uiso 1 1 calc R . . C6 C 0.6817(4) 1.1329(2) 0.3301(2) 0.0493(12) Uani 1 1 d . . . C7 C 0.6551(6) 1.1586(3) 0.4813(2) 0.0829(19) Uani 1 1 d . . . H7A H 0.7145 1.1709 0.5060 0.124 Uiso 1 1 calc R . . H7B H 0.6265 1.1139 0.4901 0.124 Uiso 1 1 calc R . . H7C H 0.5944 1.1914 0.4837 0.124 Uiso 1 1 calc R . . C8 C 0.9779(5) 1.2070(4) 0.3520(3) 0.086(2) Uani 1 1 d . . . H8A H 1.0255 1.1676 0.3465 0.128 Uiso 1 1 calc R . . H8B H 1.0048 1.2324 0.3826 0.128 Uiso 1 1 calc R . . H8C H 0.9801 1.2356 0.3206 0.128 Uiso 1 1 calc R . . C9 C 0.6089(4) 1.1097(2) 0.28353(19) 0.0476(11) Uani 1 1 d . . . H9A H 0.5416 1.1385 0.2819 0.057 Uiso 1 1 calc R . . H9B H 0.6511 1.1166 0.2504 0.057 Uiso 1 1 calc R . . C10 C 0.5110(4) 1.0207(2) 0.2338(2) 0.0477(12) Uani 1 1 d . . . H10A H 0.4460 1.0511 0.2306 0.057 Uiso 1 1 calc R . . H10B H 0.5622 1.0307 0.2042 0.057 Uiso 1 1 calc R . . C11 C 0.4704(4) 0.9480(2) 0.2284(2) 0.0475(11) Uani 1 1 d . . . C12 C 0.4980(5) 0.9116(3) 0.1819(2) 0.0569(13) Uani 1 1 d . . . H12 H 0.5451 0.9320 0.1564 0.068 Uiso 1 1 calc R . . C13 C 0.4577(5) 0.8460(3) 0.1724(3) 0.0656(15) Uani 1 1 d . . . C14 C 0.3874(5) 0.8178(3) 0.2112(2) 0.0639(15) Uani 1 1 d . . . H14 H 0.3583 0.7741 0.2052 0.077 Uiso 1 1 calc R . . C15 C 0.3583(4) 0.8506(2) 0.2581(2) 0.0574(13) Uani 1 1 d . . . C16 C 0.4034(4) 0.9176(2) 0.2679(2) 0.0482(12) Uani 1 1 d . . . C17 C 0.4943(7) 0.8047(3) 0.1234(3) 0.096(2) Uani 1 1 d . . . H17A H 0.4293 0.7958 0.1011 0.144 Uiso 1 1 calc R . . H17B H 0.5269 0.7620 0.1350 0.144 Uiso 1 1 calc R . . H17C H 0.5499 0.8301 0.1033 0.144 Uiso 1 1 calc R . . C18 C 0.2800(5) 0.8184(3) 0.2994(3) 0.0764(17) Uani 1 1 d . . . H18A H 0.2083 0.8420 0.2994 0.115 Uiso 1 1 calc R . . H18B H 0.3141 0.8218 0.3345 0.115 Uiso 1 1 calc R . . H18C H 0.2681 0.7710 0.2906 0.115 Uiso 1 1 calc R . . C19 C 0.6730(4) 0.9893(2) 0.2908(2) 0.0486(12) Uani 1 1 d . . . H19A H 0.6585 0.9477 0.2706 0.058 Uiso 1 1 calc R . . H19B H 0.7389 1.0116 0.2750 0.058 Uiso 1 1 calc R . . C20 C 0.6975(7) 0.9721(4) 0.3459(3) 0.105(3) Uani 1 1 d U . . H20A H 0.7349 1.0107 0.3630 0.126 Uiso 1 1 calc R . . H20B H 0.7499 0.9336 0.3466 0.126 Uiso 1 1 calc R . . C21 C 0.6263(8) 0.9673(4) 0.4326(3) 0.111(3) Uani 1 1 d . . . H21A H 0.5610 0.9663 0.4559 0.167 Uiso 1 1 calc R . . H21B H 0.6613 1.0118 0.4343 0.167 Uiso 1 1 calc R . . H21C H 0.6800 0.9331 0.4439 0.167 Uiso 1 1 calc R . . C22 C 0.5607(7) 0.8830(4) 0.3746(4) 0.119(3) Uani 1 1 d U . . H22A H 0.6205 0.8555 0.3898 0.178 Uiso 1 1 calc R . . H22B H 0.5499 0.8706 0.3375 0.178 Uiso 1 1 calc R . . H22C H 0.4914 0.8752 0.3942 0.178 Uiso 1 1 calc R . . C23 C 0.2543(5) 0.9783(3) 0.4149(3) 0.0755(17) Uani 1 1 d . . . H23A H 0.2159 0.9991 0.3850 0.113 Uiso 1 1 calc R . . H23B H 0.2119 0.9867 0.4473 0.113 Uiso 1 1 calc R . . H23C H 0.2602 0.9297 0.4091 0.113 Uiso 1 1 calc R . . C25 C 0.9545(6) 1.0283(5) 0.4545(4) 0.098(2) Uani 1 1 d . . . H25 H 0.9238 1.0473 0.4234 0.117 Uiso 1 1 calc R . . C24 C 0.9491(6) 0.9604(5) 0.4626(4) 0.102(3) Uani 1 1 d . . . H24 H 0.9135 0.9329 0.4371 0.122 Uiso 1 1 calc R . . C26 C 0.9951(7) 0.9305(4) 0.5081(4) 0.101(2) Uani 1 1 d . . . H26 H 0.9918 0.8833 0.5132 0.121 Uiso 1 1 calc R . . O4 O 0.3659(4) 0.1338(2) 0.45887(18) 0.0877(13) Uani 1 1 d . . . H4A H 0.4238 0.1446 0.4425 0.132 Uiso 1 1 calc R . . C27 C 0.2802(8) 0.1811(4) 0.4482(3) 0.124(3) Uani 1 1 d . . . H26A H 0.2225 0.1781 0.4755 0.186 Uiso 1 1 calc R . . H26B H 0.2472 0.1715 0.4136 0.186 Uiso 1 1 calc R . . H26C H 0.3119 0.2265 0.4480 0.186 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 0.0350(2) 0.0438(2) 0.0467(3) 0.00040(16) 0.00034(16) 0.00168(16) Cl1 0.0501(7) 0.0662(8) 0.0614(8) 0.0013(6) -0.0013(6) 0.0180(6) O1 0.048(2) 0.060(2) 0.051(2) -0.0080(16) 0.0010(15) -0.0060(17) O2 0.0429(19) 0.0535(19) 0.064(2) -0.0087(18) 0.0058(16) -0.0080(16) O3 0.046(2) 0.069(2) 0.053(2) 0.0052(17) 0.0071(16) -0.0025(17) N1 0.038(2) 0.042(2) 0.048(2) -0.0031(17) -0.0005(18) -0.0006(17) N2 0.050(3) 0.057(2) 0.063(3) 0.015(2) 0.000(2) 0.007(2) C1 0.051(3) 0.047(3) 0.058(3) -0.005(2) -0.005(2) -0.002(2) C2 0.056(3) 0.051(3) 0.065(3) -0.005(2) -0.007(3) -0.005(3) C3 0.064(4) 0.052(3) 0.085(4) -0.009(3) -0.021(3) -0.007(3) C4 0.053(3) 0.046(3) 0.088(4) -0.007(3) -0.005(3) -0.006(3) C5 0.053(3) 0.040(2) 0.069(3) -0.006(2) 0.005(3) -0.002(2) C6 0.049(3) 0.042(3) 0.057(3) -0.005(2) -0.004(2) -0.001(2) C7 0.099(5) 0.090(4) 0.059(4) -0.010(3) -0.012(3) -0.026(4) C8 0.062(4) 0.072(4) 0.123(6) -0.010(4) -0.002(4) -0.017(3) C9 0.050(3) 0.043(2) 0.050(3) -0.003(2) 0.004(2) -0.003(2) C10 0.046(3) 0.051(3) 0.046(3) -0.003(2) 0.000(2) 0.002(2) C11 0.039(3) 0.043(2) 0.060(3) -0.005(2) -0.004(2) 0.004(2) C12 0.053(3) 0.060(3) 0.058(3) -0.014(3) 0.001(2) 0.001(3) C13 0.063(4) 0.059(3) 0.075(4) -0.023(3) -0.006(3) 0.000(3) C14 0.053(3) 0.045(3) 0.094(4) -0.023(3) -0.005(3) -0.004(3) C15 0.044(3) 0.045(3) 0.083(4) 0.001(3) -0.004(3) 0.000(2) C16 0.035(3) 0.048(3) 0.062(3) -0.005(2) -0.004(2) 0.005(2) C17 0.112(6) 0.077(4) 0.099(5) -0.038(4) 0.006(5) -0.007(4) C18 0.066(4) 0.057(3) 0.106(5) -0.001(3) 0.009(4) -0.008(3) C19 0.038(3) 0.047(3) 0.061(3) 0.000(2) 0.004(2) 0.003(2) C20 0.081(5) 0.126(5) 0.107(5) 0.023(4) 0.017(4) 0.031(4) C21 0.122(7) 0.104(5) 0.107(6) 0.010(4) -0.065(5) 0.017(5) C22 0.120(5) 0.067(4) 0.169(6) 0.009(4) -0.057(5) 0.004(4) C23 0.052(3) 0.096(5) 0.078(4) 0.007(3) 0.010(3) -0.011(3) C25 0.077(5) 0.122(7) 0.094(6) 0.019(5) -0.007(4) 0.017(5) C24 0.056(4) 0.138(8) 0.112(7) -0.020(6) -0.015(4) 0.016(5) C26 0.076(5) 0.095(5) 0.131(7) 0.014(6) 0.001(5) 0.006(5) O4 0.089(3) 0.096(3) 0.079(3) -0.018(2) 0.025(2) -0.011(3) C27 0.134(7) 0.094(5) 0.144(7) -0.011(5) 0.052(6) 0.026(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 O2 2.012(3) . ? Rh1 N1 2.019(4) . ? Rh1 O1 2.046(3) . ? Rh1 N2 2.095(4) . ? Rh1 O3 2.128(3) . ? Rh1 Cl1 2.3475(13) . ? O1 C1 1.341(6) . ? O2 C16 1.340(6) . ? O3 C23 1.435(6) . ? N1 C19 1.502(6) . ? N1 C9 1.505(5) . ? N1 C10 1.514(6) . ? N2 C22 1.423(8) . ? N2 C21 1.441(8) . ? N2 C20 1.527(9) . ? C1 C6 1.396(7) . ? C1 C2 1.410(7) . ? C2 C3 1.397(8) . ? C2 C7 1.500(8) . ? C3 C4 1.380(8) . ? C3 H3 0.9300 . ? C4 C5 1.378(7) . ? C4 C8 1.516(8) . ? C5 C6 1.379(7) . ? C5 H5 0.9300 . ? C6 C9 1.507(6) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.502(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C16 1.389(7) . ? C11 C12 1.395(7) . ? C12 C13 1.383(7) . ? C12 H12 0.9300 . ? C13 C14 1.384(8) . ? C13 C17 1.520(8) . ? C14 C15 1.372(7) . ? C14 H14 0.9300 . ? C15 C16 1.430(6) . ? C15 C18 1.514(8) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.438(8) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C25 C24 1.341(11) . ? C25 C26 1.361(11) 5_776 ? C25 H25 0.9300 . ? C24 C26 1.381(11) . ? C24 H24 0.9300 . ? C26 C25 1.361(11) 5_776 ? C26 H26 0.9300 . ? O4 C27 1.391(9) . ? O4 H4A 0.8200 . ? C27 H26A 0.9600 . ? C27 H26B 0.9600 . ? C27 H26C 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 O2 Rh1 N1 94.48(14) . . ? O2 Rh1 O1 170.68(13) . . ? N1 Rh1 O1 94.31(14) . . ? O2 Rh1 N2 91.90(16) . . ? N1 Rh1 N2 85.73(16) . . ? O1 Rh1 N2 91.83(16) . . ? O2 Rh1 O3 87.35(14) . . ? N1 Rh1 O3 176.73(14) . . ? O1 Rh1 O3 84.02(13) . . ? N2 Rh1 O3 91.51(15) . . ? O2 Rh1 Cl1 89.07(11) . . ? N1 Rh1 Cl1 94.98(11) . . ? O1 Rh1 Cl1 87.09(10) . . ? N2 Rh1 Cl1 178.75(13) . . ? O3 Rh1 Cl1 87.75(10) . . ? C1 O1 Rh1 123.7(3) . . ? C16 O2 Rh1 124.6(3) . . ? C23 O3 Rh1 119.6(3) . . ? C19 N1 C9 110.6(4) . . ? C19 N1 C10 108.5(3) . . ? C9 N1 C10 106.6(3) . . ? C19 N1 Rh1 109.9(3) . . ? C9 N1 Rh1 109.7(3) . . ? C10 N1 Rh1 111.4(3) . . ? C22 N2 C21 108.0(5) . . ? C22 N2 C20 113.8(6) . . ? C21 N2 C20 102.2(6) . . ? C22 N2 Rh1 115.3(4) . . ? C21 N2 Rh1 112.9(4) . . ? C20 N2 Rh1 104.0(3) . . ? O1 C1 C6 122.6(4) . . ? O1 C1 C2 118.4(5) . . ? C6 C1 C2 119.0(5) . . ? C3 C2 C1 117.7(5) . . ? C3 C2 C7 121.6(5) . . ? C1 C2 C7 120.7(5) . . ? C4 C3 C2 123.8(5) . . ? C4 C3 H3 118.1 . . ? C2 C3 H3 118.1 . . ? C5 C4 C3 116.8(5) . . ? C5 C4 C8 121.3(6) . . ? C3 C4 C8 121.7(5) . . ? C4 C5 C6 122.2(5) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C5 C6 C1 120.4(5) . . ? C5 C6 C9 120.3(5) . . ? C1 C6 C9 119.3(4) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 C6 114.6(4) . . ? N1 C9 H9A 108.6 . . ? C6 C9 H9A 108.6 . . ? N1 C9 H9B 108.6 . . ? C6 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? C11 C10 N1 114.3(4) . . ? C11 C10 H10A 108.7 . . ? N1 C10 H10A 108.7 . . ? C11 C10 H10B 108.7 . . ? N1 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C16 C11 C12 119.9(5) . . ? C16 C11 C10 121.3(4) . . ? C12 C11 C10 118.7(4) . . ? C13 C12 C11 122.2(5) . . ? C13 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C12 C13 C14 116.9(5) . . ? C12 C13 C17 122.0(6) . . ? C14 C13 C17 121.0(5) . . ? C15 C14 C13 123.7(5) . . ? C15 C14 H14 118.2 . . ? C13 C14 H14 118.2 . . ? C14 C15 C16 118.6(5) . . ? C14 C15 C18 122.2(5) . . ? C16 C15 C18 119.2(5) . . ? O2 C16 C11 124.6(4) . . ? O2 C16 C15 116.8(4) . . ? C11 C16 C15 118.6(5) . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 N1 111.8(5) . . ? C20 C19 H19A 109.3 . . ? N1 C19 H19A 109.3 . . ? C20 C19 H19B 109.3 . . ? N1 C19 H19B 109.3 . . ? H19A C19 H19B 107.9 . . ? C19 C20 N2 112.9(6) . . ? C19 C20 H20A 109.0 . . ? N2 C20 H20A 109.0 . . ? C19 C20 H20B 109.0 . . ? N2 C20 H20B 109.0 . . ? H20A C20 H20B 107.8 . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O3 C23 H23A 109.5 . . ? O3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C24 C25 C26 120.1(8) . 5_776 ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 5_776 . ? C25 C24 C26 121.4(8) . . ? C25 C24 H24 119.3 . . ? C26 C24 H24 119.3 . . ? C25 C26 C24 118.5(8) 5_776 . ? C25 C26 H26 120.7 5_776 . ? C24 C26 H26 120.7 . . ? C27 O4 H4A 109.5 . . ? O4 C27 H26A 109.5 . . ? O4 C27 H26B 109.5 . . ? H26A C27 H26B 109.5 . . ? O4 C27 H26C 109.5 . . ? H26A C27 H26C 109.5 . . ? H26B C27 H26C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.660 _refine_diff_density_min -0.720 _refine_diff_density_rms 0.092 #===END data_rhnnoom _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H27 Cl N2 O4 Rh' _chemical_formula_weight 545.84 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' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2566(18) _cell_length_b 9.2615(18) _cell_length_c 13.978(3) _cell_angle_alpha 76.053(3) _cell_angle_beta 77.247(3) _cell_angle_gamma 81.376(3) _cell_volume 1128.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 2655 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description ? _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 558 _exptl_absorpt_coefficient_mu 0.909 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6872 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0845 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.54 _reflns_number_total 4846 _reflns_number_gt 3590 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1729P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4846 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0970 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.2514 _refine_ls_wR_factor_gt 0.1880 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.034 _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 Rh1 Rh 0.78545(6) 0.59573(7) 0.61925(4) 0.0230(2) Uani 1 1 d . . . Cl1 Cl 0.7139(2) 0.5617(2) 0.47323(14) 0.0285(4) Uani 1 1 d . . . O1 O 0.8632(7) 0.6328(7) 0.7323(4) 0.0360(14) Uani 1 1 d . . . O2 O 0.9878(6) 0.6637(8) 0.5340(4) 0.0386(15) Uani 1 1 d . . . H2 H 1.0009 0.6426 0.4773 0.058 Uiso 1 1 calc R . . O3 O 0.8829(6) 0.3893(6) 0.6392(4) 0.0284(12) Uani 1 1 d . . . O4 O 0.0766(14) 0.8368(17) 0.6719(11) 0.134(5) Uani 1 1 d . . . N1 N 0.5852(7) 0.5455(7) 0.7060(5) 0.0245(14) Uani 1 1 d . . . N2 N 0.6822(7) 0.7981(7) 0.6062(4) 0.0247(14) Uani 1 1 d . . . C1 C 0.4742(8) 0.6588(9) 0.6618(6) 0.0282(17) Uani 1 1 d . . . H1A H 0.3793 0.6614 0.7110 0.034 Uiso 1 1 calc R . . H1B H 0.4551 0.6326 0.6015 0.034 Uiso 1 1 calc R . . C2 C 0.5314(10) 0.8070(10) 0.6341(6) 0.0330(19) Uani 1 1 d . . . C3 C 0.4442(11) 0.9403(10) 0.6378(6) 0.039(2) Uani 1 1 d . . . H3 H 0.3396 0.9421 0.6609 0.047 Uiso 1 1 calc R . . C4 C 0.5133(14) 1.0751(10) 0.6063(6) 0.048(3) Uani 1 1 d . . . H4 H 0.4561 1.1693 0.6064 0.058 Uiso 1 1 calc R . . C5 C 0.6659(14) 1.0655(11) 0.5754(7) 0.050(3) Uani 1 1 d . . . H5 H 0.7147 1.1543 0.5538 0.059 Uiso 1 1 calc R . . C6 C 0.7480(12) 0.9296(11) 0.5756(7) 0.043(2) Uani 1 1 d . . . H6 H 0.8530 0.9260 0.5540 0.051 Uiso 1 1 calc R . . C7 C 0.8423(9) 0.5257(10) 0.8182(6) 0.0315(18) Uani 1 1 d . . . C8 C 0.9641(10) 0.4577(13) 0.8644(7) 0.049(3) Uani 1 1 d . . . C9 C 0.9373(11) 0.3465(15) 0.9516(7) 0.059(3) Uani 1 1 d . . . H9 H 1.0183 0.2998 0.9834 0.071 Uiso 1 1 calc R . . C10 C 0.7961(10) 0.3018(11) 0.9936(7) 0.041(2) Uani 1 1 d . . . C11 C 0.6809(9) 0.3723(9) 0.9490(6) 0.0277(17) Uani 1 1 d . . . H11 H 0.5833 0.3449 0.9781 0.033 Uiso 1 1 calc R . . C12 C 0.7015(9) 0.4823(8) 0.8630(5) 0.0244(16) Uani 1 1 d . . . C13 C 1.1183(12) 0.5060(19) 0.8183(8) 0.083(5) Uani 1 1 d . . . H13A H 1.1891 0.4503 0.8602 0.125 Uiso 1 1 calc R . . H13B H 1.1167 0.6133 0.8143 0.125 Uiso 1 1 calc R . . H13C H 1.1488 0.4857 0.7507 0.125 Uiso 1 1 calc R . . C14 C 0.7776(12) 0.1732(13) 1.0841(7) 0.053(3) Uani 1 1 d . . . H14A H 0.6738 0.1784 1.1199 0.080 Uiso 1 1 calc R . . H14B H 0.8430 0.1795 1.1290 0.080 Uiso 1 1 calc R . . H14C H 0.8039 0.0783 1.0620 0.080 Uiso 1 1 calc R . . C15 C 0.5732(9) 0.5615(9) 0.8130(6) 0.0273(17) Uani 1 1 d . . . H15A H 0.5654 0.6692 0.8131 0.033 Uiso 1 1 calc R . . H15B H 0.4799 0.5224 0.8539 0.033 Uiso 1 1 calc R . . C16 C 0.5569(8) 0.3913(9) 0.7041(6) 0.0260(16) Uani 1 1 d . . . H16A H 0.5564 0.3881 0.6338 0.031 Uiso 1 1 calc R . . H16B H 0.4562 0.3725 0.7438 0.031 Uiso 1 1 calc R . . C17 C 0.6665(8) 0.2662(8) 0.7437(5) 0.0208(14) Uani 1 1 d . . . C18 C 0.6129(9) 0.1413(9) 0.8140(6) 0.0286(17) Uani 1 1 d . . . H18 H 0.5085 0.1404 0.8377 0.034 Uiso 1 1 calc R . . C19 C 0.7047(10) 0.0216(9) 0.8492(6) 0.0327(19) Uani 1 1 d . . . C20 C 0.8559(12) 0.0268(12) 0.8168(8) 0.059(3) Uani 1 1 d . . . H20 H 0.9211 -0.0553 0.8429 0.071 Uiso 1 1 calc R . . C21 C 0.9172(10) 0.1477(11) 0.7473(7) 0.048(3) Uani 1 1 d . . . C22 C 0.8221(9) 0.2708(9) 0.7093(6) 0.0292(17) Uani 1 1 d . . . C23 C 0.6464(11) -0.1118(10) 0.9250(7) 0.043(2) Uani 1 1 d . . . H23A H 0.5374 -0.1006 0.9368 0.065 Uiso 1 1 calc R . . H23B H 0.6793 -0.1192 0.9882 0.065 Uiso 1 1 calc R . . H23C H 0.6846 -0.2027 0.8995 0.065 Uiso 1 1 calc R . . C24 C 1.0833(16) 0.1576(17) 0.7144(11) 0.081(4) Uiso 1 1 d . . . H24A H 1.1146 0.1472 0.6445 0.122 Uiso 1 1 calc R . . H24B H 1.1363 0.0773 0.7574 0.122 Uiso 1 1 calc R . . H24C H 1.1066 0.2547 0.7200 0.122 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 0.0152(4) 0.0320(4) 0.0212(3) -0.0052(2) -0.0004(2) -0.0058(2) Cl1 0.0208(10) 0.0415(11) 0.0239(9) -0.0106(8) -0.0026(7) -0.0025(8) O1 0.036(3) 0.049(4) 0.024(3) 0.005(3) -0.007(2) -0.024(3) O2 0.021(3) 0.066(4) 0.028(3) -0.016(3) 0.011(2) -0.018(3) O3 0.014(3) 0.032(3) 0.030(3) 0.005(2) -0.004(2) 0.010(2) O4 0.106(10) 0.158(13) 0.146(12) -0.035(10) -0.019(9) -0.044(9) N1 0.019(3) 0.033(3) 0.024(3) -0.013(3) 0.000(2) -0.003(3) N2 0.030(4) 0.025(3) 0.018(3) 0.005(2) -0.017(3) 0.006(3) C1 0.020(4) 0.036(4) 0.026(4) -0.007(3) -0.001(3) 0.000(3) C2 0.038(5) 0.041(5) 0.024(4) -0.017(4) 0.000(3) -0.005(4) C3 0.049(6) 0.038(5) 0.029(4) -0.014(4) -0.009(4) 0.012(4) C4 0.088(9) 0.037(5) 0.025(4) -0.009(4) -0.032(5) 0.012(5) C5 0.077(8) 0.039(5) 0.042(5) -0.012(4) -0.021(5) -0.018(5) C6 0.061(7) 0.044(5) 0.028(4) -0.007(4) -0.009(4) -0.024(5) C7 0.029(4) 0.046(5) 0.020(4) -0.005(3) -0.003(3) -0.012(4) C8 0.026(5) 0.088(8) 0.030(5) 0.004(5) -0.009(4) -0.016(5) C9 0.023(5) 0.116(10) 0.030(5) 0.006(5) -0.009(4) -0.011(5) C10 0.030(5) 0.060(6) 0.028(4) 0.001(4) -0.009(4) 0.001(4) C11 0.024(4) 0.037(4) 0.023(4) -0.009(3) -0.003(3) -0.006(3) C12 0.026(4) 0.028(4) 0.020(4) -0.004(3) -0.007(3) -0.002(3) C13 0.032(6) 0.171(15) 0.039(6) 0.014(7) -0.014(5) -0.038(8) C14 0.045(6) 0.070(7) 0.036(5) 0.004(5) -0.004(4) -0.007(5) C15 0.026(4) 0.032(4) 0.023(4) -0.009(3) -0.001(3) 0.000(3) C16 0.019(4) 0.032(4) 0.029(4) -0.009(3) 0.000(3) -0.008(3) C17 0.016(4) 0.025(4) 0.019(3) -0.003(3) -0.002(3) -0.002(3) C18 0.024(4) 0.031(4) 0.032(4) -0.010(3) 0.000(3) -0.008(3) C19 0.035(5) 0.028(4) 0.026(4) 0.006(3) -0.004(3) 0.003(3) C20 0.044(6) 0.058(7) 0.052(6) 0.005(5) 0.016(5) 0.006(5) C21 0.023(5) 0.049(6) 0.047(6) 0.022(4) 0.002(4) 0.013(4) C22 0.023(4) 0.038(4) 0.021(4) -0.005(3) 0.004(3) 0.000(3) C23 0.048(6) 0.033(5) 0.039(5) -0.003(4) 0.003(4) 0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N2 1.958(6) . ? Rh1 O3 1.971(5) . ? Rh1 O1 1.992(6) . ? Rh1 N1 2.029(6) . ? Rh1 O2 2.081(5) . ? Rh1 Cl1 2.3821(19) . ? O1 C7 1.358(10) . ? O3 C22 1.380(10) . ? N1 C1 1.478(10) . ? N1 C16 1.498(10) . ? N1 C15 1.516(9) . ? N2 C2 1.360(11) . ? N2 C6 1.376(11) . ? C1 C2 1.478(12) . ? C2 C3 1.375(11) . ? C3 C4 1.418(14) . ? C4 C5 1.379(15) . ? C5 C6 1.369(14) . ? C7 C12 1.389(11) . ? C7 C8 1.413(12) . ? C8 C9 1.395(14) . ? C8 C13 1.517(14) . ? C9 C10 1.390(13) . ? C10 C11 1.357(12) . ? C10 C14 1.512(13) . ? C11 C12 1.374(11) . ? C12 C15 1.514(10) . ? C16 C17 1.505(10) . ? C17 C18 1.399(11) . ? C17 C22 1.418(10) . ? C18 C19 1.353(11) . ? C19 C20 1.377(14) . ? C19 C23 1.503(12) . ? C20 C21 1.393(14) . ? C21 C22 1.404(11) . ? C21 C24 1.515(17) . ? 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 N2 Rh1 O3 177.1(2) . . ? N2 Rh1 O1 87.7(3) . . ? O3 Rh1 O1 91.1(2) . . ? N2 Rh1 N1 81.2(3) . . ? O3 Rh1 N1 96.3(2) . . ? O1 Rh1 N1 93.6(2) . . ? N2 Rh1 O2 94.9(3) . . ? O3 Rh1 O2 87.6(2) . . ? O1 Rh1 O2 83.8(2) . . ? N1 Rh1 O2 175.4(2) . . ? N2 Rh1 Cl1 92.18(18) . . ? O3 Rh1 Cl1 89.32(17) . . ? O1 Rh1 Cl1 174.26(17) . . ? N1 Rh1 Cl1 92.05(18) . . ? O2 Rh1 Cl1 90.53(17) . . ? C7 O1 Rh1 115.1(5) . . ? C22 O3 Rh1 123.8(4) . . ? C1 N1 C16 110.8(6) . . ? C1 N1 C15 107.2(6) . . ? C16 N1 C15 110.8(6) . . ? C1 N1 Rh1 105.5(5) . . ? C16 N1 Rh1 110.4(4) . . ? C15 N1 Rh1 112.0(5) . . ? C2 N2 C6 117.8(7) . . ? C2 N2 Rh1 115.9(6) . . ? C6 N2 Rh1 126.3(6) . . ? N1 C1 C2 109.3(7) . . ? N2 C2 C3 122.8(8) . . ? N2 C2 C1 112.5(7) . . ? C3 C2 C1 124.7(8) . . ? C2 C3 C4 118.8(9) . . ? C5 C4 C3 118.1(8) . . ? C6 C5 C4 120.8(9) . . ? C5 C6 N2 121.7(10) . . ? O1 C7 C12 120.9(7) . . ? O1 C7 C8 120.3(8) . . ? C12 C7 C8 118.7(8) . . ? C9 C8 C7 118.1(9) . . ? C9 C8 C13 122.2(9) . . ? C7 C8 C13 119.7(9) . . ? C10 C9 C8 122.1(9) . . ? C11 C10 C9 118.3(9) . . ? C11 C10 C14 122.6(9) . . ? C9 C10 C14 119.1(8) . . ? C10 C11 C12 121.8(8) . . ? C11 C12 C7 120.9(7) . . ? C11 C12 C15 122.0(7) . . ? C7 C12 C15 117.1(7) . . ? C12 C15 N1 115.2(6) . . ? N1 C16 C17 115.8(6) . . ? C18 C17 C22 119.6(7) . . ? C18 C17 C16 119.0(7) . . ? C22 C17 C16 121.3(7) . . ? C19 C18 C17 122.2(8) . . ? C18 C19 C20 118.2(8) . . ? C18 C19 C23 121.9(8) . . ? C20 C19 C23 119.8(8) . . ? C19 C20 C21 122.7(9) . . ? C20 C21 C22 119.2(9) . . ? C20 C21 C24 123.2(9) . . ? C22 C21 C24 117.5(9) . . ? O3 C22 C21 119.1(7) . . ? O3 C22 C17 122.8(7) . . ? C21 C22 C17 118.1(7) . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 1.573 _refine_diff_density_min -2.497 _refine_diff_density_rms 0.253 #===END data_rhn2o2m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H34 N2 O5 Rh' _chemical_formula_weight 617.51 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' '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 P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.3395(14) _cell_length_b 14.753(2) _cell_length_c 23.961(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3654.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 5491 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 22.65 _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.122 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1276 _exptl_absorpt_coefficient_mu 0.500 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20150 _diffrn_reflns_av_R_equivalents 0.0598 _diffrn_reflns_av_sigmaI/netI 0.0783 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.68 _reflns_number_total 6911 _reflns_number_gt 4981 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1509P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.47(8) _refine_ls_number_reflns 6911 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1005 _refine_ls_R_factor_gt 0.0690 _refine_ls_wR_factor_ref 0.2348 _refine_ls_wR_factor_gt 0.2131 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.25316(7) 0.20809(4) 0.14226(2) 0.0374(2) Uani 1 1 d . . . O1 O 0.1034(6) 0.2729(4) 0.1063(2) 0.0392(15) Uani 1 1 d . . . O2 O 0.2657(6) 0.3178(4) 0.2018(2) 0.0488(14) Uani 1 1 d . . . O3 O 0.1178(6) 0.1480(5) 0.1962(3) 0.0507(17) Uani 1 1 d . . . O4 O 0.9609(8) 0.0116(6) 0.1663(4) 0.084(2) Uani 1 1 d . . . O5 O 0.1041(10) 0.4432(7) 0.2319(4) 0.098(3) Uiso 1 1 d . . . N1 N 0.3899(7) 0.2686(5) 0.0931(3) 0.0381(19) Uani 1 1 d . . . N2 N 0.4109(8) 0.1521(6) 0.1786(3) 0.045(2) Uani 1 1 d . . . C1 C 0.3405(8) 0.2809(6) 0.0358(3) 0.041(2) Uani 1 1 d . . . H1A H 0.4109 0.3053 0.0121 0.050 Uiso 1 1 calc R . . H1B H 0.3159 0.2209 0.0205 0.050 Uiso 1 1 calc R . . C2 C 0.2287(9) 0.3418(5) 0.0322(3) 0.042(2) Uani 1 1 d . . . C3 C 0.2329(10) 0.4102(6) -0.0083(3) 0.047(2) Uani 1 1 d . . . H3 H 0.3078 0.4153 -0.0310 0.056 Uiso 1 1 calc R . . C4 C 0.1312(11) 0.4715(7) -0.0167(4) 0.054(2) Uani 1 1 d . . . C5 C 0.0187(10) 0.4605(7) 0.0153(4) 0.051(2) Uani 1 1 d . . . H5 H -0.0526 0.5002 0.0100 0.061 Uiso 1 1 calc R . . C6 C 0.0113(9) 0.3902(6) 0.0556(3) 0.044(2) Uani 1 1 d . . . C7 C 0.1183(8) 0.3327(6) 0.0654(3) 0.0386(19) Uani 1 1 d . . . C8 C 0.1403(12) 0.5462(7) -0.0578(5) 0.070(3) Uani 1 1 d . . . H8A H 0.1664 0.6021 -0.0388 0.106 Uiso 1 1 calc R . . H8B H 0.0559 0.5552 -0.0756 0.106 Uiso 1 1 calc R . . H8C H 0.2046 0.5307 -0.0863 0.106 Uiso 1 1 calc R . . C9 C -0.1079(9) 0.3781(8) 0.0890(4) 0.060(3) Uani 1 1 d . . . H9A H -0.1512 0.3219 0.0778 0.090 Uiso 1 1 calc R . . H9B H -0.1660 0.4296 0.0827 0.090 Uiso 1 1 calc R . . H9C H -0.0854 0.3749 0.1287 0.090 Uiso 1 1 calc R . . C10 C 0.4291(9) 0.3593(7) 0.1146(4) 0.050(2) Uani 1 1 d . . . H10A H 0.3539 0.4007 0.1121 0.060 Uiso 1 1 calc R . . H10B H 0.4979 0.3839 0.0901 0.060 Uiso 1 1 calc R . . C11 C 0.4781(9) 0.3590(6) 0.1745(4) 0.045(2) Uani 1 1 d . . . C12 C 0.6049(9) 0.3761(7) 0.1872(4) 0.054(2) Uani 1 1 d . . . H12 H 0.6655 0.3887 0.1584 0.065 Uiso 1 1 calc R . . C13 C 0.6451(10) 0.3747(7) 0.2445(4) 0.057(3) Uani 1 1 d . . . C14 C 0.5538(10) 0.3569(7) 0.2844(4) 0.056(3) Uani 1 1 d . . . H14 H 0.5796 0.3573 0.3224 0.067 Uiso 1 1 calc R . . C15 C 0.4269(9) 0.3386(7) 0.2723(4) 0.050(2) Uani 1 1 d . . . C16 C 0.3866(8) 0.3396(6) 0.2167(4) 0.043(2) Uani 1 1 d . . . C17 C 0.7839(9) 0.3953(9) 0.2599(5) 0.075(3) Uani 1 1 d . . . H17A H 0.7859 0.4339 0.2931 0.112 Uiso 1 1 calc R . . H17B H 0.8262 0.4267 0.2288 0.112 Uiso 1 1 calc R . . H17C H 0.8298 0.3385 0.2676 0.112 Uiso 1 1 calc R . . C18 C 0.3278(11) 0.3149(8) 0.3168(4) 0.066(3) Uani 1 1 d . . . H18A H 0.3694 0.3153 0.3535 0.099 Uiso 1 1 calc R . . H18B H 0.2923 0.2545 0.3093 0.099 Uiso 1 1 calc R . . H18C H 0.2578 0.3597 0.3162 0.099 Uiso 1 1 calc R . . C19 C 0.5036(8) 0.2065(7) 0.0933(4) 0.044(2) Uani 1 1 d . . . H19A H 0.5826 0.2411 0.0839 0.053 Uiso 1 1 calc R . . H19B H 0.4916 0.1590 0.0646 0.053 Uiso 1 1 calc R . . C20 C 0.5202(9) 0.1619(7) 0.1507(4) 0.047(2) Uani 1 1 d . . . C21 C 0.6359(10) 0.1289(7) 0.1702(4) 0.057(3) Uani 1 1 d . . . H21 H 0.7131 0.1372 0.1494 0.068 Uiso 1 1 calc R . . C22 C 0.6384(11) 0.0857(8) 0.2181(6) 0.073(3) Uani 1 1 d . . . H22 H 0.7177 0.0609 0.2311 0.088 Uiso 1 1 calc R . . C23 C 0.5245(12) 0.0752(7) 0.2511(5) 0.069(3) Uani 1 1 d . . . H23 H 0.5260 0.0465 0.2866 0.082 Uiso 1 1 calc R . . C24 C 0.4135(11) 0.1091(7) 0.2285(5) 0.058(3) Uani 1 1 d . . . H24 H 0.3348 0.1022 0.2486 0.070 Uiso 1 1 calc R . . C25 C 0.2247(7) 0.0985(6) 0.0920(3) 0.040(2) Uani 1 1 d . . . C26 C 0.2870(9) 0.0149(6) 0.1040(4) 0.049(2) Uani 1 1 d . . . H26 H 0.3500 0.0121 0.1328 0.059 Uiso 1 1 calc R . . C27 C 0.2563(14) -0.0630(6) 0.0738(4) 0.067(3) Uani 1 1 d . . . H27 H 0.2971 -0.1188 0.0829 0.080 Uiso 1 1 calc R . . C28 C 0.1668(10) -0.0599(7) 0.0307(4) 0.060(3) Uani 1 1 d . . . H28 H 0.1462 -0.1126 0.0097 0.072 Uiso 1 1 calc R . . C29 C 0.1082(12) 0.0229(8) 0.0191(5) 0.074(3) Uani 1 1 d . . . H29 H 0.0471 0.0270 -0.0104 0.089 Uiso 1 1 calc R . . C30 C 0.1368(11) 0.0971(7) 0.0492(4) 0.056(3) Uani 1 1 d . . . H30 H 0.0935 0.1519 0.0402 0.067 Uiso 1 1 calc R . . C31 C 0.0114(14) 0.2055(11) 0.2182(6) 0.094(4) Uani 1 1 d . . . H31A H 0.0407 0.2369 0.2519 0.141 Uiso 1 1 calc R . . H31B H -0.0633 0.1674 0.2272 0.141 Uiso 1 1 calc R . . H31C H -0.0134 0.2503 0.1899 0.141 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 0.0374(3) 0.0423(3) 0.0325(3) 0.0021(2) 0.0005(4) -0.0001(4) O1 0.035(3) 0.044(4) 0.038(3) 0.011(3) -0.005(3) 0.002(3) O2 0.045(4) 0.053(3) 0.048(3) -0.010(2) 0.016(3) 0.008(3) O3 0.048(4) 0.063(5) 0.041(4) 0.017(3) 0.009(3) -0.004(3) O4 0.059(5) 0.096(6) 0.098(6) 0.022(5) -0.003(4) -0.018(4) N1 0.044(4) 0.044(5) 0.026(4) -0.001(3) -0.002(3) 0.005(3) N2 0.058(5) 0.050(5) 0.028(4) 0.006(3) -0.003(3) -0.006(4) C1 0.038(4) 0.050(5) 0.037(4) -0.005(4) 0.005(4) -0.003(4) C2 0.054(6) 0.037(4) 0.035(4) -0.001(3) -0.006(4) -0.012(4) C3 0.053(6) 0.052(5) 0.035(4) -0.001(3) -0.009(4) -0.005(5) C4 0.078(7) 0.050(6) 0.033(5) 0.001(4) -0.004(5) -0.008(5) C5 0.061(6) 0.056(6) 0.036(5) 0.000(4) -0.010(4) 0.005(5) C6 0.044(5) 0.049(5) 0.039(5) -0.004(4) -0.002(4) 0.002(4) C7 0.039(5) 0.049(5) 0.028(4) -0.010(4) 0.000(4) 0.005(4) C8 0.092(9) 0.054(6) 0.065(7) 0.018(5) -0.018(6) 0.001(6) C9 0.042(5) 0.091(8) 0.046(6) 0.007(5) 0.009(4) 0.024(5) C10 0.048(5) 0.057(6) 0.046(5) 0.006(4) 0.004(4) -0.007(5) C11 0.044(5) 0.046(5) 0.046(5) -0.014(4) 0.001(4) -0.001(4) C12 0.041(5) 0.067(7) 0.054(6) -0.010(5) 0.003(4) -0.007(5) C13 0.052(6) 0.055(6) 0.064(7) -0.010(5) -0.020(5) -0.006(5) C14 0.070(7) 0.052(6) 0.045(6) -0.018(5) 0.004(5) -0.008(5) C15 0.057(6) 0.056(6) 0.036(5) -0.011(4) 0.003(4) -0.005(5) C16 0.038(5) 0.042(5) 0.048(5) -0.008(4) 0.001(4) -0.002(4) C17 0.048(7) 0.091(9) 0.085(8) -0.025(7) -0.013(5) 0.008(5) C18 0.077(7) 0.076(8) 0.045(6) -0.008(5) 0.004(5) -0.015(6) C19 0.038(5) 0.052(5) 0.043(5) 0.001(4) 0.005(4) 0.003(4) C20 0.041(5) 0.053(5) 0.046(5) -0.012(4) -0.010(4) -0.003(4) C21 0.061(6) 0.063(6) 0.046(6) -0.005(5) -0.016(5) 0.007(5) C22 0.043(6) 0.081(8) 0.094(9) -0.011(7) -0.021(6) 0.017(6) C23 0.089(9) 0.045(6) 0.072(8) 0.008(5) -0.038(7) -0.001(6) C24 0.062(6) 0.053(6) 0.060(6) -0.013(5) -0.024(5) -0.001(5) C25 0.034(6) 0.047(5) 0.037(4) 0.013(3) 0.000(3) -0.007(4) C26 0.050(6) 0.046(5) 0.051(5) 0.002(4) -0.013(4) -0.003(4) C27 0.081(7) 0.044(5) 0.075(6) 0.003(4) -0.028(8) -0.003(7) C28 0.063(6) 0.053(6) 0.065(7) -0.017(5) -0.011(5) -0.007(5) C29 0.077(8) 0.075(8) 0.071(7) 0.010(6) -0.034(6) -0.016(6) C30 0.073(7) 0.044(6) 0.050(6) -0.006(5) -0.013(5) -0.003(5) C31 0.093(10) 0.115(11) 0.074(9) 0.024(8) 0.006(7) -0.022(9) _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 O1 2.013(6) . ? Rh1 N2 2.025(8) . ? Rh1 C25 2.037(9) . ? Rh1 N1 2.045(8) . ? Rh1 O3 2.101(6) . ? Rh1 O2 2.161(6) . ? O1 C7 1.329(10) . ? O2 C16 1.339(11) . ? O3 C31 1.486(16) . ? N1 C1 1.476(10) . ? N1 C19 1.490(11) . ? N1 C10 1.490(12) . ? N2 C20 1.319(12) . ? N2 C24 1.355(12) . ? C1 C2 1.467(12) . ? C2 C7 1.397(12) . ? C2 C3 1.401(11) . ? C3 C4 1.401(14) . ? C4 C5 1.403(14) . ? C4 C8 1.481(14) . ? C5 C6 1.418(13) . ? C6 C7 1.414(12) . ? C6 C9 1.481(12) . ? C10 C11 1.522(12) . ? C11 C12 1.369(13) . ? C11 C16 1.415(13) . ? C12 C13 1.436(13) . ? C13 C14 1.367(14) . ? C13 C17 1.513(14) . ? C14 C15 1.370(13) . ? C15 C16 1.395(12) . ? C15 C18 1.520(13) . ? C19 C20 1.534(12) . ? C20 C21 1.374(13) . ? C21 C22 1.312(16) . ? C22 C23 1.426(17) . ? C23 C24 1.364(15) . ? C25 C30 1.371(12) . ? C25 C26 1.420(12) . ? C26 C27 1.394(12) . ? C27 C28 1.389(14) . ? C28 C29 1.391(16) . ? C29 C30 1.343(14) . ? 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 O1 Rh1 N2 175.6(3) . . ? O1 Rh1 C25 90.7(3) . . ? N2 Rh1 C25 92.7(3) . . ? O1 Rh1 N1 94.5(2) . . ? N2 Rh1 N1 82.4(3) . . ? C25 Rh1 N1 96.1(3) . . ? O1 Rh1 O3 87.2(3) . . ? N2 Rh1 O3 95.8(3) . . ? C25 Rh1 O3 86.1(3) . . ? N1 Rh1 O3 177.2(3) . . ? O1 Rh1 O2 88.5(2) . . ? N2 Rh1 O2 88.5(3) . . ? C25 Rh1 O2 173.2(3) . . ? N1 Rh1 O2 90.7(3) . . ? O3 Rh1 O2 87.1(3) . . ? C7 O1 Rh1 122.9(5) . . ? C16 O2 Rh1 114.3(5) . . ? C31 O3 Rh1 118.1(7) . . ? C1 N1 C19 110.6(7) . . ? C1 N1 C10 107.8(7) . . ? C19 N1 C10 109.6(7) . . ? C1 N1 Rh1 110.5(5) . . ? C19 N1 Rh1 106.0(5) . . ? C10 N1 Rh1 112.4(5) . . ? C20 N2 C24 118.7(9) . . ? C20 N2 Rh1 115.4(6) . . ? C24 N2 Rh1 125.9(7) . . ? C2 C1 N1 113.7(7) . . ? C7 C2 C3 119.2(9) . . ? C7 C2 C1 123.5(7) . . ? C3 C2 C1 117.2(8) . . ? C2 C3 C4 122.8(9) . . ? C3 C4 C5 118.0(8) . . ? C3 C4 C8 121.9(9) . . ? C5 C4 C8 120.2(10) . . ? C4 C5 C6 120.1(9) . . ? C7 C6 C5 120.6(8) . . ? C7 C6 C9 119.3(8) . . ? C5 C6 C9 120.1(9) . . ? O1 C7 C2 125.3(8) . . ? O1 C7 C6 115.5(7) . . ? C2 C7 C6 119.2(8) . . ? N1 C10 C11 114.5(8) . . ? C12 C11 C16 121.2(8) . . ? C12 C11 C10 121.9(8) . . ? C16 C11 C10 116.9(8) . . ? C11 C12 C13 119.2(9) . . ? C14 C13 C12 118.1(9) . . ? C14 C13 C17 121.6(9) . . ? C12 C13 C17 120.3(10) . . ? C13 C14 C15 123.4(9) . . ? C14 C15 C16 119.1(9) . . ? C14 C15 C18 122.8(9) . . ? C16 C15 C18 118.1(8) . . ? O2 C16 C15 122.1(8) . . ? O2 C16 C11 118.8(8) . . ? C15 C16 C11 119.0(8) . . ? N1 C19 C20 110.8(7) . . ? N2 C20 C21 122.3(9) . . ? N2 C20 C19 113.8(8) . . ? C21 C20 C19 123.7(9) . . ? C22 C21 C20 119.1(10) . . ? C21 C22 C23 121.4(10) . . ? C24 C23 C22 115.8(10) . . ? N2 C24 C23 122.6(11) . . ? C30 C25 C26 116.0(8) . . ? C30 C25 Rh1 123.4(7) . . ? C26 C25 Rh1 120.3(6) . . ? C27 C26 C25 120.5(8) . . ? C28 C27 C26 120.7(9) . . ? C27 C28 C29 117.8(9) . . ? C30 C29 C28 120.9(10) . . ? C29 C30 C25 124.0(10) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.445 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.255