# cif data for compound 1 data_iv63ras _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H29 Cl2 N2 O4 Rh' _chemical_formula_weight 487.22 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 monoclinic _symmetry_space_group_name_H-M 'P 2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.5542(3) _cell_length_b 15.9110(6) _cell_length_c 15.4317(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.138(1) _cell_angle_gamma 90.00 _cell_volume 2053.39(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8776 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 28.04 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 1.114 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7682 _exptl_absorpt_correction_T_max 0.8419 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Buker SMART APEX' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23574 _diffrn_reflns_av_R_equivalents 0.0150 _diffrn_reflns_av_sigmaI/netI 0.0180 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 27.10 _reflns_number_total 8876 _reflns_number_gt 8721 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _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. The structure was refined as a racemic twin with components 0.46(0.015). ; _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^)+(0.0266P)^2^+0.5539P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'NH free with SADI, rigid methyls' _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 0.460(15) _refine_ls_number_reflns 8876 _refine_ls_number_parameters 486 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0193 _refine_ls_R_factor_gt 0.0189 _refine_ls_wR_factor_ref 0.0473 _refine_ls_wR_factor_gt 0.0471 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.002 _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 0.634439(16) 0.608574(8) 0.022180(10) 0.01161(4) Uani 1 1 d . . . Cl1 Cl 0.53103(6) 0.72442(4) 0.09333(4) 0.01991(11) Uani 1 1 d . . . N1 N 0.6419(2) 0.53027(13) 0.13219(13) 0.0146(4) Uani 1 1 d D . . H01 H 0.728(2) 0.5022(17) 0.1455(16) 0.019(7) Uiso 1 1 d D . . N2 N 0.8664(2) 0.64290(14) 0.08848(13) 0.0163(4) Uani 1 1 d D . . H02 H 0.915(3) 0.6047(15) 0.1196(16) 0.021(7) Uiso 1 1 d D . . C1 C 0.4311(2) 0.59540(17) -0.08667(15) 0.0161(5) Uani 1 1 d . . . C2 C 0.5031(3) 0.51510(17) -0.06605(16) 0.0174(5) Uani 1 1 d . . . C3 C 0.6683(3) 0.52039(16) -0.07601(15) 0.0162(5) Uani 1 1 d . . . C4 C 0.6916(2) 0.60349(19) -0.10833(13) 0.0155(4) Uani 1 1 d . . . C5 C 0.5477(2) 0.65018(16) -0.11338(15) 0.0156(5) Uani 1 1 d . . . C6 C 0.2615(2) 0.6182(2) -0.08755(16) 0.0238(5) Uani 1 1 d . . . H6A H 0.1977 0.6127 -0.1480 0.029 Uiso 1 1 calc R . . H6B H 0.2565 0.6763 -0.0673 0.029 Uiso 1 1 calc R . . H6C H 0.2190 0.5804 -0.0480 0.029 Uiso 1 1 calc R . . C7 C 0.4246(3) 0.43877(18) -0.03883(18) 0.0255(5) Uani 1 1 d . . . H7A H 0.3506 0.4553 -0.0013 0.031 Uiso 1 1 calc R . . H7B H 0.5062 0.4010 -0.0056 0.031 Uiso 1 1 calc R . . H7C H 0.3654 0.4098 -0.0917 0.031 Uiso 1 1 calc R . . C8 C 0.7908(3) 0.45165(19) -0.06171(17) 0.0271(6) Uani 1 1 d . . . H8A H 0.8160 0.4359 -0.1186 0.032 Uiso 1 1 calc R . . H8B H 0.7485 0.4027 -0.0357 0.032 Uiso 1 1 calc R . . H8C H 0.8881 0.4714 -0.0215 0.032 Uiso 1 1 calc R . . C9 C 0.8413(3) 0.63323(18) -0.13376(16) 0.0224(5) Uani 1 1 d . . . H9A H 0.8496 0.6081 -0.1906 0.027 Uiso 1 1 calc R . . H9B H 0.9339 0.6165 -0.0881 0.027 Uiso 1 1 calc R . . H9C H 0.8386 0.6946 -0.1393 0.027 Uiso 1 1 calc R . . C10 C 0.5132(3) 0.73837(16) -0.14567(17) 0.0221(6) Uani 1 1 d . . . H10A H 0.6139 0.7672 -0.1471 0.027 Uiso 1 1 calc R . . H10B H 0.4575 0.7683 -0.1056 0.027 Uiso 1 1 calc R . . H10C H 0.4457 0.7373 -0.2054 0.027 Uiso 1 1 calc R . . C11 C 0.3793(3) 0.54676(18) 0.16556(16) 0.0237(5) Uani 1 1 d . . . H11A H 0.3640 0.5863 0.1158 0.028 Uiso 1 1 calc R . . H11B H 0.3689 0.5766 0.2196 0.028 Uiso 1 1 calc R . . H11C H 0.2984 0.5024 0.1528 0.028 Uiso 1 1 calc R . . C12 C 0.5411(3) 0.50880(16) 0.17837(15) 0.0172(5) Uani 1 1 d . . . C13 C 0.5805(3) 0.44340(16) 0.24993(15) 0.0216(5) Uani 1 1 d . . . H13A H 0.6842 0.4179 0.2484 0.026 Uiso 1 1 calc R . . H13B H 0.4975 0.3999 0.2402 0.026 Uiso 1 1 calc R . . H13C H 0.5855 0.4698 0.3078 0.026 Uiso 1 1 calc R . . C14 C 0.8871(3) 0.78558(17) 0.03739(17) 0.0216(5) Uani 1 1 d . . . H14A H 0.7758 0.7761 0.0070 0.026 Uiso 1 1 calc R . . H14B H 0.9526 0.7957 -0.0066 0.026 Uiso 1 1 calc R . . H14C H 0.8927 0.8346 0.0763 0.026 Uiso 1 1 calc R . . C15 C 0.9483(2) 0.70996(18) 0.09132(14) 0.0161(4) Uani 1 1 d . . . C16 C 1.1128(2) 0.7181(2) 0.14924(15) 0.0221(5) Uani 1 1 d . . . H16A H 1.1386 0.6669 0.1847 0.027 Uiso 1 1 calc R . . H16B H 1.1154 0.7666 0.1887 0.027 Uiso 1 1 calc R . . H16C H 1.1913 0.7261 0.1120 0.027 Uiso 1 1 calc R . . Cl3 Cl 1.02018(6) 0.38214(4) 0.19924(4) 0.01929(12) Uani 1 1 d . . . O1 O 1.0118(3) 0.38169(15) 0.29114(13) 0.0406(5) Uani 1 1 d . . . O2 O 1.1769(2) 0.35722(12) 0.18973(14) 0.0353(4) Uani 1 1 d . . . O3 O 0.9023(2) 0.32610(14) 0.15084(15) 0.0468(5) Uani 1 1 d . . . O4 O 0.9876(2) 0.46660(13) 0.16512(13) 0.0319(4) Uani 1 1 d . . . Rh2 Rh 0.624941(17) 0.218097(8) 0.523266(10) 0.01246(4) Uani 1 1 d . . . Cl2 Cl 0.50008(6) 0.10262(5) 0.58393(4) 0.02126(12) Uani 1 1 d . . . N3 N 0.6114(2) 0.29601(14) 0.63071(14) 0.0175(4) Uani 1 1 d D . . H03 H 0.699(2) 0.3197(17) 0.6478(16) 0.018(7) Uiso 1 1 d D . . N4 N 0.8474(2) 0.18292(14) 0.60179(14) 0.0168(4) Uani 1 1 d D . . H04 H 0.897(3) 0.2182(17) 0.6348(19) 0.038(9) Uiso 1 1 d D . . C21 C 0.5681(3) 0.17702(17) 0.38669(15) 0.0163(5) Uani 1 1 d . . . C22 C 0.7112(2) 0.2242(2) 0.40060(14) 0.0176(4) Uani 1 1 d . . . C23 C 0.6798(3) 0.30694(17) 0.43183(15) 0.0178(5) Uani 1 1 d . . . C24 C 0.5107(3) 0.31145(16) 0.42983(15) 0.0171(5) Uani 1 1 d . . . C25 C 0.4421(3) 0.23155(18) 0.40413(16) 0.0183(5) Uani 1 1 d . . . C26 C 0.5409(3) 0.08902(16) 0.35202(17) 0.0222(5) Uani 1 1 d . . . H26A H 0.4831 0.0906 0.2901 0.027 Uiso 1 1 calc R . . H26B H 0.4776 0.0580 0.3875 0.027 Uiso 1 1 calc R . . H26C H 0.6441 0.0610 0.3559 0.027 Uiso 1 1 calc R . . C27 C 0.8700(3) 0.19571(19) 0.38550(17) 0.0266(6) Uani 1 1 d . . . H27A H 0.8658 0.1354 0.3723 0.032 Uiso 1 1 calc R . . H27B H 0.9525 0.2064 0.4389 0.032 Uiso 1 1 calc R . . H27C H 0.8959 0.2267 0.3354 0.032 Uiso 1 1 calc R . . C28 C 0.8010(3) 0.37619(18) 0.45476(17) 0.0248(6) Uani 1 1 d . . . H28A H 0.8261 0.3989 0.4003 0.030 Uiso 1 1 calc R . . H28B H 0.8986 0.3538 0.4926 0.030 Uiso 1 1 calc R . . H28C H 0.7573 0.4209 0.4863 0.030 Uiso 1 1 calc R . . C29 C 0.4204(3) 0.38645(19) 0.44983(19) 0.0273(6) Uani 1 1 d . . . H29A H 0.3801 0.4178 0.3950 0.033 Uiso 1 1 calc R . . H29B H 0.4914 0.4226 0.4923 0.033 Uiso 1 1 calc R . . H29C H 0.3303 0.3683 0.4754 0.033 Uiso 1 1 calc R . . C30 C 0.2696(3) 0.2079(2) 0.39147(17) 0.0265(6) Uani 1 1 d . . . H30A H 0.2193 0.2414 0.4314 0.032 Uiso 1 1 calc R . . H30B H 0.2610 0.1481 0.4048 0.032 Uiso 1 1 calc R . . H30C H 0.2157 0.2188 0.3299 0.032 Uiso 1 1 calc R . . C31 C 0.4992(3) 0.31855(16) 0.66923(15) 0.0200(5) Uani 1 1 d . . . C32 C 0.3361(3) 0.28183(18) 0.6467(2) 0.0317(6) Uani 1 1 d . . . H32A H 0.3319 0.2391 0.6005 0.038 Uiso 1 1 calc R . . H32B H 0.2583 0.3262 0.6250 0.038 Uiso 1 1 calc R . . H32C H 0.3106 0.2559 0.6996 0.038 Uiso 1 1 calc R . . C33 C 0.5268(3) 0.38250(17) 0.74233(16) 0.0250(5) Uani 1 1 d . . . H33A H 0.5340 0.3541 0.7994 0.030 Uiso 1 1 calc R . . H33B H 0.4378 0.4225 0.7328 0.030 Uiso 1 1 calc R . . H33C H 0.6268 0.4126 0.7425 0.030 Uiso 1 1 calc R . . C34 C 0.9306(2) 0.11543(19) 0.60683(14) 0.0179(4) Uani 1 1 d . . . C35 C 0.8778(3) 0.04121(18) 0.55004(17) 0.0236(5) Uani 1 1 d . . . H35A H 0.7675 0.0497 0.5176 0.028 Uiso 1 1 calc R . . H35B H 0.8832 -0.0091 0.5872 0.028 Uiso 1 1 calc R . . H35C H 0.9478 0.0340 0.5078 0.028 Uiso 1 1 calc R . . C36 C 1.0898(2) 0.1076(2) 0.66987(15) 0.0246(5) Uani 1 1 d . . . H36A H 1.1110 0.1586 0.7060 0.030 Uiso 1 1 calc R . . H36B H 1.1739 0.1001 0.6362 0.030 Uiso 1 1 calc R . . H36C H 1.0882 0.0589 0.7086 0.030 Uiso 1 1 calc R . . Cl4 Cl 1.00041(7) 0.44120(4) 0.70453(4) 0.02009(12) Uani 1 1 d . . . O5 O 0.8575(2) 0.49025(14) 0.68277(16) 0.0494(6) Uani 1 1 d . . . O6 O 0.9604(2) 0.35360(13) 0.68849(14) 0.0347(5) Uani 1 1 d . . . O7 O 1.1072(3) 0.46530(13) 0.64981(15) 0.0468(5) Uani 1 1 d . . . O8 O 1.0722(3) 0.45222(18) 0.79528(14) 0.0559(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 Rh1 0.01119(7) 0.00997(9) 0.01391(8) -0.00016(7) 0.00319(6) 0.00000(6) Cl1 0.0240(2) 0.0133(3) 0.0249(3) -0.0036(2) 0.0109(2) 0.0011(2) N1 0.0135(8) 0.0131(10) 0.0163(9) -0.0006(7) 0.0015(7) 0.0011(7) N2 0.0152(9) 0.0175(10) 0.0154(9) 0.0007(8) 0.0014(7) 0.0020(7) C1 0.0146(9) 0.0161(14) 0.0168(10) -0.0034(9) 0.0012(8) -0.0005(9) C2 0.0164(10) 0.0169(14) 0.0186(11) -0.0040(10) 0.0028(8) -0.0033(9) C3 0.0192(10) 0.0140(13) 0.0150(11) -0.0037(9) 0.0030(8) 0.0035(8) C4 0.0160(9) 0.0180(12) 0.0129(9) -0.0016(10) 0.0038(7) -0.0027(9) C5 0.0151(10) 0.0166(13) 0.0142(11) -0.0026(9) 0.0012(8) 0.0000(8) C6 0.0115(9) 0.0291(14) 0.0297(12) 0.0023(11) 0.0020(8) 0.0016(9) C7 0.0301(12) 0.0170(14) 0.0294(13) -0.0031(11) 0.0064(10) -0.0099(10) C8 0.0283(12) 0.0250(15) 0.0269(12) -0.0038(11) 0.0035(10) 0.0113(10) C9 0.0168(10) 0.0295(14) 0.0221(11) -0.0019(9) 0.0071(9) -0.0010(9) C10 0.0235(11) 0.0220(16) 0.0197(11) 0.0048(9) 0.0019(9) 0.0025(9) C11 0.0220(11) 0.0247(13) 0.0270(12) 0.0057(10) 0.0112(9) 0.0018(9) C12 0.0196(10) 0.0147(11) 0.0171(11) -0.0035(9) 0.0035(8) -0.0019(8) C13 0.0269(11) 0.0191(12) 0.0208(11) 0.0027(9) 0.0097(9) 0.0007(9) C14 0.0212(11) 0.0161(13) 0.0275(13) 0.0012(10) 0.0051(10) -0.0044(9) C15 0.0137(9) 0.0184(12) 0.0174(10) -0.0051(9) 0.0059(7) -0.0002(9) C16 0.0163(9) 0.0233(12) 0.0254(11) -0.0044(11) 0.0011(8) -0.0019(10) Cl3 0.0180(2) 0.0164(3) 0.0237(3) -0.0016(2) 0.0050(2) 0.0011(2) O1 0.0550(13) 0.0423(13) 0.0280(10) 0.0042(9) 0.0163(9) 0.0036(10) O2 0.0256(9) 0.0263(9) 0.0586(13) 0.0016(9) 0.0193(9) 0.0077(7) O3 0.0384(11) 0.0403(12) 0.0592(13) -0.0167(10) 0.0046(10) -0.0180(9) O4 0.0270(9) 0.0234(10) 0.0450(11) 0.0127(8) 0.0072(8) 0.0072(7) Rh2 0.01234(8) 0.01075(9) 0.01477(8) 0.00044(7) 0.00396(6) -0.00026(6) Cl2 0.0269(3) 0.0147(3) 0.0250(3) 0.0016(2) 0.0118(2) -0.0030(2) N3 0.0183(9) 0.0142(10) 0.0203(10) -0.0010(8) 0.0048(8) -0.0036(7) N4 0.0169(9) 0.0141(10) 0.0186(10) -0.0010(8) 0.0022(7) -0.0004(7) C21 0.0161(10) 0.0178(13) 0.0148(11) 0.0016(9) 0.0024(8) 0.0016(9) C22 0.0169(9) 0.0216(12) 0.0145(10) 0.0048(10) 0.0036(7) -0.0019(10) C23 0.0193(11) 0.0202(14) 0.0142(11) 0.0047(9) 0.0041(8) 0.0000(9) C24 0.0208(11) 0.0145(13) 0.0162(11) 0.0023(10) 0.0045(9) 0.0004(9) C25 0.0141(10) 0.0203(15) 0.0203(11) 0.0031(10) 0.0030(8) 0.0010(9) C26 0.0286(12) 0.0165(14) 0.0207(11) -0.0028(9) 0.0032(9) -0.0010(9) C27 0.0186(11) 0.0359(16) 0.0289(13) 0.0048(11) 0.0131(10) 0.0061(10) C28 0.0274(12) 0.0212(14) 0.0253(12) 0.0054(10) 0.0042(10) -0.0100(10) C29 0.0316(13) 0.0188(14) 0.0337(14) 0.0046(11) 0.0118(11) 0.0076(10) C30 0.0151(10) 0.0285(15) 0.0345(13) 0.0034(11) 0.0020(9) 0.0011(10) C31 0.0294(12) 0.0130(11) 0.0199(11) 0.0031(9) 0.0100(9) 0.0017(9) C32 0.0275(13) 0.0268(14) 0.0461(16) -0.0093(12) 0.0197(12) -0.0034(10) C33 0.0381(13) 0.0174(12) 0.0219(11) -0.0008(9) 0.0116(10) -0.0011(10) C34 0.0179(9) 0.0183(12) 0.0174(10) 0.0065(10) 0.0033(8) -0.0018(9) C35 0.0217(11) 0.0185(13) 0.0291(13) 0.0009(10) 0.0017(10) 0.0037(9) C36 0.0183(10) 0.0259(13) 0.0277(12) 0.0054(12) 0.0004(8) 0.0005(10) Cl4 0.0211(3) 0.0175(3) 0.0219(3) -0.0012(2) 0.0050(2) -0.0025(2) O5 0.0363(11) 0.0389(12) 0.0717(15) 0.0035(11) 0.0085(10) 0.0176(9) O6 0.0303(10) 0.0198(9) 0.0529(13) -0.0051(9) 0.0064(8) -0.0060(7) O7 0.0513(12) 0.0330(11) 0.0678(15) 0.0143(10) 0.0391(11) -0.0031(10) O8 0.0789(17) 0.0539(15) 0.0265(11) -0.0107(10) -0.0079(11) -0.0050(13) _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 N1 2.096(2) . ? Rh1 N2 2.1045(19) . ? Rh1 C3 2.129(2) . ? Rh1 C1 2.159(2) . ? Rh1 C2 2.165(2) . ? Rh1 C5 2.171(2) . ? Rh1 C4 2.172(2) . ? Rh1 Cl1 2.4070(7) . ? N1 C12 1.275(3) . ? N2 C15 1.272(3) . ? C1 C2 1.425(4) . ? C1 C5 1.448(3) . ? C1 C6 1.493(3) . ? C2 C3 1.456(3) . ? C2 C7 1.490(3) . ? C3 C4 1.442(4) . ? C3 C8 1.498(3) . ? C4 C5 1.426(3) . ? C4 C9 1.493(3) . ? C5 C10 1.498(4) . ? C11 C12 1.485(3) . ? C12 C13 1.503(3) . ? C14 C15 1.494(4) . ? C15 C16 1.506(3) . ? Cl3 O3 1.4329(19) . ? Cl3 O2 1.4349(17) . ? Cl3 O1 1.435(2) . ? Cl3 O4 1.449(2) . ? Rh2 N3 2.093(2) . ? Rh2 N4 2.1056(19) . ? Rh2 C23 2.118(2) . ? Rh2 C24 2.156(2) . ? Rh2 C25 2.159(2) . ? Rh2 C21 2.162(2) . ? Rh2 C22 2.174(2) . ? Rh2 Cl2 2.4112(7) . ? N3 C31 1.282(3) . ? N4 C34 1.281(3) . ? C21 C22 1.413(3) . ? C21 C25 1.453(3) . ? C21 C26 1.500(4) . ? C22 C23 1.447(4) . ? C22 C27 1.496(3) . ? C23 C24 1.442(3) . ? C23 C28 1.503(3) . ? C24 C25 1.421(4) . ? C24 C29 1.489(3) . ? C25 C30 1.495(3) . ? C31 C32 1.484(3) . ? C31 C33 1.501(3) . ? C34 C35 1.483(4) . ? C34 C36 1.503(3) . ? Cl4 O8 1.417(2) . ? Cl4 O7 1.4210(19) . ? Cl4 O5 1.4297(19) . ? Cl4 O6 1.444(2) . ? 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 N1 Rh1 N2 84.00(8) . . ? N1 Rh1 C3 101.49(9) . . ? N2 Rh1 C3 105.15(8) . . ? N1 Rh1 C1 117.05(8) . . ? N2 Rh1 C1 157.87(8) . . ? C3 Rh1 C1 65.82(9) . . ? N1 Rh1 C2 91.40(9) . . ? N2 Rh1 C2 142.74(8) . . ? C3 Rh1 C2 39.64(8) . . ? C1 Rh1 C2 38.48(10) . . ? N1 Rh1 C5 155.20(8) . . ? N2 Rh1 C5 119.06(8) . . ? C3 Rh1 C5 65.50(9) . . ? C1 Rh1 C5 39.06(8) . . ? C2 Rh1 C5 64.93(9) . . ? N1 Rh1 C4 138.99(10) . . ? N2 Rh1 C4 95.01(7) . . ? C3 Rh1 C4 39.15(10) . . ? C1 Rh1 C4 64.94(8) . . ? C2 Rh1 C4 65.13(9) . . ? C5 Rh1 C4 38.34(8) . . ? N1 Rh1 Cl1 92.14(6) . . ? N2 Rh1 Cl1 88.79(6) . . ? C3 Rh1 Cl1 161.32(7) . . ? C1 Rh1 Cl1 96.67(7) . . ? C2 Rh1 Cl1 128.40(6) . . ? C5 Rh1 Cl1 97.01(7) . . ? C4 Rh1 Cl1 128.87(8) . . ? C12 N1 Rh1 134.67(16) . . ? C15 N2 Rh1 133.66(17) . . ? C2 C1 C5 108.22(19) . . ? C2 C1 C6 126.4(2) . . ? C5 C1 C6 125.3(2) . . ? C2 C1 Rh1 70.97(13) . . ? C5 C1 Rh1 70.91(12) . . ? C6 C1 Rh1 127.29(16) . . ? C1 C2 C3 107.9(2) . . ? C1 C2 C7 126.5(2) . . ? C3 C2 C7 125.6(2) . . ? C1 C2 Rh1 70.55(13) . . ? C3 C2 Rh1 68.87(13) . . ? C7 C2 Rh1 126.00(17) . . ? C4 C3 C2 107.3(2) . . ? C4 C3 C8 125.3(2) . . ? C2 C3 C8 127.3(2) . . ? C4 C3 Rh1 72.01(13) . . ? C2 C3 Rh1 71.49(13) . . ? C8 C3 Rh1 124.88(17) . . ? C5 C4 C3 108.44(19) . . ? C5 C4 C9 126.8(3) . . ? C3 C4 C9 124.8(2) . . ? C5 C4 Rh1 70.80(12) . . ? C3 C4 Rh1 68.83(12) . . ? C9 C4 Rh1 127.21(16) . . ? C4 C5 C1 108.0(2) . . ? C4 C5 C10 127.8(2) . . ? C1 C5 C10 124.0(2) . . ? C4 C5 Rh1 70.86(12) . . ? C1 C5 Rh1 70.03(13) . . ? C10 C5 Rh1 127.58(17) . . ? N1 C12 C11 122.5(2) . . ? N1 C12 C13 121.5(2) . . ? C11 C12 C13 115.98(19) . . ? N2 C15 C14 122.1(2) . . ? N2 C15 C16 122.1(2) . . ? C14 C15 C16 115.8(2) . . ? O3 Cl3 O2 110.19(12) . . ? O3 Cl3 O1 109.63(13) . . ? O2 Cl3 O1 109.99(13) . . ? O3 Cl3 O4 109.10(13) . . ? O2 Cl3 O4 109.36(11) . . ? O1 Cl3 O4 108.54(13) . . ? N3 Rh2 N4 84.00(8) . . ? N3 Rh2 C23 100.92(10) . . ? N4 Rh2 C23 105.11(9) . . ? N3 Rh2 C24 91.66(9) . . ? N4 Rh2 C24 142.73(8) . . ? C23 Rh2 C24 39.42(8) . . ? N3 Rh2 C25 117.70(9) . . ? N4 Rh2 C25 157.15(9) . . ? C23 Rh2 C25 65.73(9) . . ? C24 Rh2 C25 38.46(10) . . ? N3 Rh2 C21 155.89(9) . . ? N4 Rh2 C21 118.12(8) . . ? C23 Rh2 C21 65.69(9) . . ? C24 Rh2 C21 65.10(9) . . ? C25 Rh2 C21 39.28(9) . . ? N3 Rh2 C22 138.52(10) . . ? N4 Rh2 C22 94.69(8) . . ? C23 Rh2 C22 39.37(11) . . ? C24 Rh2 C22 64.92(10) . . ? C25 Rh2 C22 64.65(8) . . ? C21 Rh2 C22 38.03(9) . . ? N3 Rh2 Cl2 92.35(6) . . ? N4 Rh2 Cl2 89.68(6) . . ? C23 Rh2 Cl2 160.97(7) . . ? C24 Rh2 Cl2 127.53(6) . . ? C25 Rh2 Cl2 96.05(7) . . ? C21 Rh2 Cl2 96.95(7) . . ? C22 Rh2 Cl2 129.14(8) . . ? C31 N3 Rh2 134.80(18) . . ? C34 N4 Rh2 132.91(17) . . ? C22 C21 C25 107.9(2) . . ? C22 C21 C26 127.9(2) . . ? C25 C21 C26 123.9(2) . . ? C22 C21 Rh2 71.43(13) . . ? C25 C21 Rh2 70.26(13) . . ? C26 C21 Rh2 128.05(17) . . ? C21 C22 C23 108.6(2) . . ? C21 C22 C27 127.0(3) . . ? C23 C22 C27 124.4(2) . . ? C21 C22 Rh2 70.54(12) . . ? C23 C22 Rh2 68.25(13) . . ? C27 C22 Rh2 127.44(17) . . ? C24 C23 C22 107.1(2) . . ? C24 C23 C28 127.4(2) . . ? C22 C23 C28 125.3(2) . . ? C24 C23 Rh2 71.69(13) . . ? C22 C23 Rh2 72.37(14) . . ? C28 C23 Rh2 124.80(17) . . ? C25 C24 C23 108.4(2) . . ? C25 C24 C29 125.0(2) . . ? C23 C24 C29 126.7(2) . . ? C25 C24 Rh2 70.91(14) . . ? C23 C24 Rh2 68.89(13) . . ? C29 C24 Rh2 126.56(17) . . ? C24 C25 C21 107.87(19) . . ? C24 C25 C30 126.9(2) . . ? C21 C25 C30 125.2(2) . . ? C24 C25 Rh2 70.64(13) . . ? C21 C25 Rh2 70.46(13) . . ? C30 C25 Rh2 127.20(17) . . ? N3 C31 C32 122.6(2) . . ? N3 C31 C33 121.5(2) . . ? C32 C31 C33 115.8(2) . . ? N4 C34 C35 122.4(2) . . ? N4 C34 C36 121.7(2) . . ? C35 C34 C36 116.0(2) . . ? O8 Cl4 O7 110.79(16) . . ? O8 Cl4 O5 109.64(15) . . ? O7 Cl4 O5 109.76(14) . . ? O8 Cl4 O6 109.07(15) . . ? O7 Cl4 O6 108.51(13) . . ? O5 Cl4 O6 109.04(13) . . ? 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 N1 H01 O4 0.847(16) 2.252(17) 3.066(2) 161(3) . N2 H02 O4 0.831(16) 2.350(19) 3.135(3) 158(3) . N3 H03 O6 0.831(16) 2.257(17) 3.070(3) 166(3) . N4 H04 O6 0.813(17) 2.33(2) 3.091(3) 156(3) . C28 H28A O1 0.98 2.56 3.398(3) 143.4 . C10 H10A O2 0.98 2.49 3.438(3) 163.8 2_755 C16 H16B O6 0.98 2.54 3.460(3) 156.4 2_756 C35 H35B O1 0.98 2.58 3.517(4) 160.6 2_746 C33 H33A Cl1 0.98 2.77 3.678(3) 153.7 2_646 C13 H13C Cl2 0.98 2.88 3.770(3) 151.0 2_656 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.456 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.063 # END # cif data for compound 2 data_calle _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H29 Cl2 N2 Rh' _chemical_formula_weight 423.22 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.5331(6) _cell_length_b 12.0370(4) _cell_length_c 22.7027(8) _cell_angle_alpha 90.00 _cell_angle_beta 94.644(4) _cell_angle_gamma 90.00 _cell_volume 3686.1(2) _cell_formula_units_Z 8 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 7231 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 30.49 _exptl_crystal_description rhomb _exptl_crystal_colour orange _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 1.213 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7774 _exptl_absorpt_correction_T_max 0.8883 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 'Bruker SMART 1000 CCD' _diffrn_measurement_method '\w- & \f-scan' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43299 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 30.50 _reflns_number_total 5620 _reflns_number_gt 4569 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _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^)+(0.0272P)^2^+4.2156P] 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 'NH free, rigid methyls, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5620 _refine_ls_number_parameters 210 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0607 _refine_ls_wR_factor_gt 0.0559 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.002 _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 Rh Rh 0.336581(10) 0.818746(11) 0.340633(6) 0.01083(4) Uani 1 1 d . . . Cl1 Cl 0.36416(3) 0.71569(4) 0.25257(2) 0.01817(9) Uani 1 1 d . . . Cl2 Cl 0.12192(4) 0.55211(4) 0.40221(2) 0.02342(11) Uani 1 1 d . . . N1 N 0.33279(12) 0.66435(13) 0.38202(7) 0.0142(3) Uani 1 1 d . . . H01 H 0.2791(17) 0.6425(19) 0.3877(9) 0.014(5) Uiso 1 1 d . . . N2 N 0.49537(12) 0.81762(14) 0.35831(7) 0.0139(3) Uani 1 1 d . . . H02 H 0.5177(16) 0.7987(18) 0.3264(10) 0.014(6) Uiso 1 1 d . . . H03 H 0.5162(16) 0.881(2) 0.3677(10) 0.019(6) Uiso 1 1 d . . . C1 C 0.38164(15) 0.48211(16) 0.42105(9) 0.0195(4) Uani 1 1 d . . . H1A H 0.3100 0.4717 0.4220 0.023 Uiso 1 1 calc R . . H1B H 0.4137 0.4757 0.4612 0.023 Uiso 1 1 calc R . . H1C H 0.4081 0.4251 0.3958 0.023 Uiso 1 1 calc R . . C2 C 0.40181(14) 0.59527(15) 0.39669(8) 0.0141(3) Uani 1 1 d . . . C3 C 0.50852(14) 0.62294(16) 0.38968(9) 0.0172(4) Uani 1 1 d . . . H3A H 0.5219 0.6087 0.3481 0.021 Uiso 1 1 calc R . . H3B H 0.5506 0.5715 0.4148 0.021 Uiso 1 1 calc R . . C4 C 0.54048(13) 0.74250(15) 0.40543(8) 0.0150(3) Uani 1 1 d . . . C5 C 0.65446(14) 0.74832(18) 0.40692(9) 0.0218(4) Uani 1 1 d . . . H5A H 0.6761 0.7201 0.3696 0.026 Uiso 1 1 calc R . . H5B H 0.6837 0.7030 0.4397 0.026 Uiso 1 1 calc R . . H5C H 0.6760 0.8256 0.4124 0.026 Uiso 1 1 calc R . . C6 C 0.50724(15) 0.77965(17) 0.46479(8) 0.0194(4) Uani 1 1 d . . . H6A H 0.5308 0.8554 0.4733 0.023 Uiso 1 1 calc R . . H6B H 0.5348 0.7294 0.4959 0.023 Uiso 1 1 calc R . . H6C H 0.4347 0.7781 0.4634 0.023 Uiso 1 1 calc R . . C11 C 0.22562(13) 0.89714(15) 0.38976(8) 0.0136(3) Uani 1 1 d . . . C12 C 0.18341(13) 0.87081(15) 0.33136(8) 0.0145(3) Uani 1 1 d . . . C13 C 0.23713(14) 0.93261(15) 0.29014(8) 0.0148(3) Uani 1 1 d . . . C14 C 0.31361(14) 0.99352(15) 0.32247(9) 0.0161(4) Uani 1 1 d . . . C15 C 0.30604(13) 0.97281(15) 0.38495(8) 0.0143(3) Uani 1 1 d . . . C16 C 0.18889(15) 0.85417(17) 0.44588(8) 0.0193(4) Uani 1 1 d . . . H16A H 0.1312 0.8976 0.4556 0.023 Uiso 1 1 calc R . . H16B H 0.2415 0.8607 0.4780 0.023 Uiso 1 1 calc R . . H16C H 0.1699 0.7760 0.4408 0.023 Uiso 1 1 calc R . . C17 C 0.09127(14) 0.80400(16) 0.31642(9) 0.0205(4) Uani 1 1 d . . . H17A H 0.0332 0.8528 0.3157 0.025 Uiso 1 1 calc R . . H17B H 0.0858 0.7460 0.3463 0.025 Uiso 1 1 calc R . . H17C H 0.0946 0.7695 0.2775 0.025 Uiso 1 1 calc R . . C18 C 0.21456(16) 0.93341(17) 0.22484(8) 0.0223(4) Uani 1 1 d . . . H18A H 0.1619 0.9874 0.2143 0.027 Uiso 1 1 calc R . . H18B H 0.1927 0.8593 0.2115 0.027 Uiso 1 1 calc R . . H18C H 0.2742 0.9541 0.2057 0.027 Uiso 1 1 calc R . . C19 C 0.38383(16) 1.07350(17) 0.29747(10) 0.0239(4) Uani 1 1 d . . . H19A H 0.3946 1.0518 0.2569 0.029 Uiso 1 1 calc R . . H19B H 0.4472 1.0725 0.3217 0.029 Uiso 1 1 calc R . . H19C H 0.3557 1.1485 0.2975 0.029 Uiso 1 1 calc R . . C20 C 0.36511(15) 1.02942(17) 0.43441(9) 0.0202(4) Uani 1 1 d . . . H20A H 0.3382 1.1039 0.4400 0.024 Uiso 1 1 calc R . . H20B H 0.4343 1.0354 0.4250 0.024 Uiso 1 1 calc R . . H20C H 0.3617 0.9862 0.4708 0.024 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 Rh 0.01074(6) 0.01081(7) 0.01087(6) 0.00089(5) 0.00044(4) 0.00021(5) Cl1 0.0198(2) 0.0202(2) 0.0148(2) -0.00267(17) 0.00263(17) -0.00032(17) Cl2 0.0175(2) 0.0213(2) 0.0315(3) 0.0022(2) 0.00223(19) -0.00557(18) N1 0.0134(7) 0.0149(8) 0.0145(7) 0.0008(6) 0.0019(6) -0.0017(6) N2 0.0139(7) 0.0133(7) 0.0146(7) -0.0001(6) 0.0018(6) -0.0009(6) C1 0.0229(9) 0.0132(9) 0.0219(9) 0.0041(7) -0.0010(8) -0.0008(7) C2 0.0164(8) 0.0140(8) 0.0117(8) -0.0013(7) 0.0001(7) -0.0015(7) C3 0.0158(8) 0.0147(9) 0.0210(9) 0.0016(7) 0.0007(7) 0.0033(7) C4 0.0133(8) 0.0155(8) 0.0158(8) 0.0020(7) -0.0010(7) 0.0004(7) C5 0.0134(9) 0.0248(10) 0.0266(10) 0.0029(8) -0.0018(8) 0.0003(8) C6 0.0212(9) 0.0216(9) 0.0149(9) -0.0008(8) -0.0021(7) -0.0022(8) C11 0.0119(8) 0.0147(8) 0.0142(8) -0.0001(7) 0.0012(6) 0.0033(7) C12 0.0135(8) 0.0140(8) 0.0158(8) -0.0004(7) -0.0007(7) 0.0030(7) C13 0.0169(8) 0.0130(8) 0.0143(8) 0.0018(7) -0.0009(7) 0.0041(7) C14 0.0170(8) 0.0122(8) 0.0189(9) 0.0037(7) 0.0015(7) 0.0029(7) C15 0.0147(8) 0.0115(8) 0.0166(8) -0.0007(7) -0.0002(7) 0.0018(7) C16 0.0192(9) 0.0219(9) 0.0172(9) 0.0014(8) 0.0045(8) 0.0034(8) C17 0.0155(9) 0.0214(10) 0.0238(10) -0.0023(8) -0.0043(7) -0.0028(7) C18 0.0284(11) 0.0233(10) 0.0143(9) 0.0029(8) -0.0035(8) 0.0039(8) C19 0.0235(10) 0.0186(10) 0.0300(11) 0.0079(8) 0.0057(9) -0.0019(8) C20 0.0187(9) 0.0189(9) 0.0224(10) -0.0059(8) -0.0021(8) 0.0004(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh N1 2.0851(16) . ? Rh N2 2.1539(16) . ? Rh C11 2.1588(17) . ? Rh C12 2.1595(18) . ? Rh C14 2.1614(18) . ? Rh C15 2.1654(18) . ? Rh C13 2.1804(18) . ? Rh Cl1 2.4074(5) . ? N1 C2 1.274(2) . ? N2 C4 1.493(2) . ? C1 C2 1.503(3) . ? C2 C3 1.503(3) . ? C3 C4 1.537(3) . ? C4 C6 1.522(3) . ? C4 C5 1.542(3) . ? C11 C15 1.430(3) . ? C11 C12 1.436(3) . ? C11 C16 1.497(3) . ? C12 C13 1.438(3) . ? C12 C17 1.499(3) . ? C13 C14 1.423(3) . ? C13 C18 1.489(3) . ? C14 C15 1.452(3) . ? C14 C19 1.496(3) . ? C15 C20 1.490(3) . ? 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 N1 Rh N2 88.34(6) . . ? N1 Rh C11 96.50(6) . . ? N2 Rh C11 129.18(7) . . ? N1 Rh C12 104.13(7) . . ? N2 Rh C12 162.81(7) . . ? C11 Rh C12 38.84(7) . . ? N1 Rh C14 160.93(7) . . ? N2 Rh C14 99.65(7) . . ? C11 Rh C14 65.03(7) . . ? C12 Rh C14 64.97(7) . . ? N1 Rh C15 122.78(6) . . ? N2 Rh C15 98.27(7) . . ? C11 Rh C15 38.63(7) . . ? C12 Rh C15 65.10(7) . . ? C14 Rh C15 39.21(7) . . ? N1 Rh C13 139.51(7) . . ? N2 Rh C13 131.76(7) . . ? C11 Rh C13 64.61(7) . . ? C12 Rh C13 38.70(7) . . ? C14 Rh C13 38.26(7) . . ? C15 Rh C13 64.73(7) . . ? N1 Rh Cl1 85.76(4) . . ? N2 Rh Cl1 86.11(5) . . ? C11 Rh Cl1 144.62(5) . . ? C12 Rh Cl1 106.30(5) . . ? C14 Rh Cl1 111.88(5) . . ? C15 Rh Cl1 151.08(5) . . ? C13 Rh Cl1 91.02(5) . . ? C2 N1 Rh 130.92(14) . . ? C4 N2 Rh 118.77(11) . . ? N1 C2 C3 121.19(17) . . ? N1 C2 C1 122.42(17) . . ? C3 C2 C1 116.39(16) . . ? C2 C3 C4 115.95(15) . . ? N2 C4 C6 108.87(15) . . ? N2 C4 C3 108.02(15) . . ? C6 C4 C3 112.55(15) . . ? N2 C4 C5 109.79(15) . . ? C6 C4 C5 109.52(16) . . ? C3 C4 C5 108.05(15) . . ? C15 C11 C12 108.57(16) . . ? C15 C11 C16 126.31(17) . . ? C12 C11 C16 125.10(17) . . ? C15 C11 Rh 70.94(10) . . ? C12 C11 Rh 70.61(10) . . ? C16 C11 Rh 125.56(13) . . ? C11 C12 C13 107.60(16) . . ? C11 C12 C17 126.06(17) . . ? C13 C12 C17 125.82(17) . . ? C11 C12 Rh 70.55(10) . . ? C13 C12 Rh 71.44(10) . . ? C17 C12 Rh 129.83(13) . . ? C14 C13 C12 108.40(16) . . ? C14 C13 C18 126.32(17) . . ? C12 C13 C18 125.27(17) . . ? C14 C13 Rh 70.15(10) . . ? C12 C13 Rh 69.86(10) . . ? C18 C13 Rh 126.56(13) . . ? C13 C14 C15 108.04(16) . . ? C13 C14 C19 126.41(18) . . ? C15 C14 C19 125.33(18) . . ? C13 C14 Rh 71.59(10) . . ? C15 C14 Rh 70.54(10) . . ? C19 C14 Rh 127.78(14) . . ? C11 C15 C14 107.35(16) . . ? C11 C15 C20 126.81(17) . . ? C14 C15 C20 125.58(17) . . ? C11 C15 Rh 70.43(10) . . ? C14 C15 Rh 70.25(10) . . ? C20 C15 Rh 129.13(13) . . ? 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 N1 H01 Cl2 0.79(2) 2.43(2) 3.2234(17) 173(2) . N2 H02 Cl1 0.84(2) 2.69(2) 3.4974(17) 162(2) 2_655 N2 H03 Cl2 0.84(2) 2.59(2) 3.4084(18) 166(2) 3 C5 H5A Cl1 0.98 2.78 3.631(2) 145.2 2_655 C18 H18A Cl1 0.98 2.88 3.610(2) 132.2 4 C1 H1A Cl2 0.98 2.73 3.606(2) 149.7 . C5 H5C Cl2 0.98 2.83 3.684(2) 146.3 3 C16 H16C Cl2 0.98 2.89 3.857(2) 168.9 . C17 H17B Cl2 0.98 2.68 3.609(2) 157.8 . C19 H19B Cl2 0.98 2.88 3.855(2) 173.1 3 C20 H20B Cl2 0.98 2.64 3.619(2) 178.7 3 C20 H20C Cl2 0.98 2.91 3.827(2) 156.0 7_566 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.765 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.095 # end