# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry, 1999 # CCDC Number: 186/1557 data_v3rh # compound 1 in manuscript _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H48 Cl6 N6 O6 Rh2' _chemical_formula_weight 1007.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Rh' 'Rh' -1.1178 0.9187 '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' 'O' 'O' 0.0106 0.0060 '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' '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 11.640(6) _cell_length_b 8.898(5) _cell_length_c 19.75(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.03(4) _cell_angle_gamma 90.00 _cell_volume 2025(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour orange _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.622 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 1.256 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1825 _diffrn_reflns_av_R_equivalents 0.0939 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 27.49 _reflns_number_total 1824 _reflns_number_gt 1558 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0652P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1824 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1075 _refine_ls_wR_factor_gt 0.1018 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh Rh 0.23456(7) 0.15104(9) 0.10893(4) 0.0334(2) Uani 1 d . . . Cl1 Cl 0.0483(2) 0.1269(3) 0.14247(13) 0.0499(7) Uani 1 d . . . Cl2 Cl 0.4174(2) 0.1952(3) 0.07688(13) 0.0464(7) Uani 1 d . . . Cl3 Cl 0.2513(3) 0.3858(3) 0.16484(14) 0.0575(9) Uani 1 d . . . N1 N 0.2135(7) -0.0530(8) 0.0602(4) 0.0347(19) Uani 1 d . . . N2 N 0.3116(7) 0.0549(9) 0.1986(4) 0.040(2) Uani 1 d . . . N3 N 0.1574(7) 0.2553(9) 0.0209(4) 0.040(2) Uani 1 d . . . O1 O 0.0971(5) -0.0804(7) 0.0324(3) 0.0415(17) Uani 1 d . . . O2 O 0.4036(6) 0.1353(9) 0.2338(4) 0.062(2) Uani 1 d . . . O3 O 0.0803(6) 0.3731(7) 0.0328(4) 0.053(2) Uani 1 d . . . C1 C 0.2818(8) -0.1627(11) 0.0489(5) 0.033(2) Uani 1 d . . . C2 C 0.2385(9) -0.3029(10) 0.0106(6) 0.047(3) Uani 1 d . . . H2A H 0.2013 -0.2791 -0.0352 0.056 Uiso 1 calc R . . H2B H 0.1843 -0.3572 0.0346 0.056 Uiso 1 calc R . . C3 C 0.3500(9) -0.3934(11) 0.0087(6) 0.054(3) Uani 1 d . . . H3A H 0.3351 -0.5002 0.0122 0.065 Uiso 1 calc R . . H3B H 0.3814 -0.3747 -0.0335 0.065 Uiso 1 calc R . . C4 C 0.4327(9) -0.3402(12) 0.0692(6) 0.054(3) Uani 1 d . . . H4A H 0.5125 -0.3587 0.0626 0.064 Uiso 1 calc R . . H4B H 0.4177 -0.3899 0.1108 0.064 Uiso 1 calc R . . C5 C 0.4083(8) -0.1716(10) 0.0722(5) 0.042(3) Uani 1 d . . . H5A H 0.4275 -0.1332 0.1183 0.050 Uiso 1 calc R . . H5B H 0.4516 -0.1159 0.0419 0.050 Uiso 1 calc R . . C6 C 0.2924(9) -0.0683(12) 0.2296(5) 0.044(3) Uani 1 d . . . C7 C 0.3604(10) -0.1167(12) 0.2970(6) 0.058(3) Uani 1 d . . . H7A H 0.3510 -0.0451 0.3328 0.069 Uiso 1 calc R . . H7B H 0.4423 -0.1261 0.2932 0.069 Uiso 1 calc R . . C8 C 0.3083(11) -0.2702(14) 0.3119(6) 0.075(4) Uani 1 d . . . H8A H 0.3564 -0.3516 0.2991 0.090 Uiso 1 calc R . . H8B H 0.3009 -0.2797 0.3600 0.090 Uiso 1 calc R . . C9 C 0.1935(10) -0.2720(13) 0.2696(6) 0.060(3) Uani 1 d . . . H9A H 0.1362 -0.2256 0.2942 0.072 Uiso 1 calc R . . H9B H 0.1696 -0.3747 0.2588 0.072 Uiso 1 calc R . . C10 C 0.2030(10) -0.1864(12) 0.2054(6) 0.062(4) Uani 1 d . . . H10A H 0.1295 -0.1412 0.1870 0.075 Uiso 1 calc R . . H10B H 0.2292 -0.2507 0.1709 0.075 Uiso 1 calc R . . C11 C 0.1625(8) 0.2390(11) -0.0430(5) 0.039(3) Uani 1 d . . . C12 C 0.0992(9) 0.3358(13) -0.0988(5) 0.053(3) Uani 1 d . . . H12A H 0.1246 0.4395 -0.0938 0.064 Uiso 1 calc R . . H12B H 0.0160 0.3318 -0.0983 0.064 Uiso 1 calc R . . C13 C 0.1316(11) 0.2669(16) -0.1644(6) 0.075(4) Uani 1 d . . . H13A H 0.0727 0.1964 -0.1840 0.089 Uiso 1 calc R . . H13B H 0.1402 0.3444 -0.1978 0.089 Uiso 1 calc R . . C14 C 0.2454(11) 0.1877(13) -0.1429(6) 0.064(4) Uani 1 d . . . H14A H 0.3097 0.2576 -0.1409 0.077 Uiso 1 calc R . . H14B H 0.2567 0.1078 -0.1747 0.077 Uiso 1 calc R . . C15 C 0.2365(9) 0.1242(12) -0.0726(5) 0.051(3) Uani 1 d . . . H15A H 0.1996 0.0262 -0.0757 0.061 Uiso 1 calc R . . H15B H 0.3124 0.1159 -0.0454 0.061 Uiso 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 0.0381(5) 0.0323(4) 0.0308(4) -0.0002(5) 0.0083(3) -0.0022(5) Cl1 0.0439(16) 0.065(2) 0.0439(15) -0.0001(15) 0.0182(13) 0.0055(15) Cl2 0.0432(16) 0.0501(17) 0.0476(16) 0.0000(13) 0.0121(13) -0.0118(13) Cl3 0.087(2) 0.0417(19) 0.0455(17) -0.0109(13) 0.0145(16) -0.0046(15) N1 0.034(5) 0.034(5) 0.035(5) -0.004(4) 0.002(4) -0.004(4) N2 0.041(5) 0.040(5) 0.039(5) -0.005(4) 0.005(4) -0.007(4) N3 0.045(6) 0.032(5) 0.043(5) 0.008(4) 0.008(4) 0.006(4) O1 0.028(4) 0.044(4) 0.049(4) -0.007(3) -0.007(3) -0.003(3) O2 0.060(5) 0.068(6) 0.054(5) 0.001(4) -0.008(4) -0.029(5) O3 0.058(5) 0.031(4) 0.069(5) 0.005(4) 0.005(4) 0.019(4) C1 0.036(5) 0.023(5) 0.040(5) 0.009(5) 0.009(5) 0.005(5) C2 0.050(7) 0.028(6) 0.063(7) -0.013(5) 0.010(6) -0.006(5) C3 0.054(8) 0.038(7) 0.074(8) -0.007(6) 0.019(7) 0.008(5) C4 0.044(7) 0.051(7) 0.069(8) 0.009(7) 0.016(6) 0.011(6) C5 0.025(5) 0.044(7) 0.057(7) 0.006(6) 0.003(5) -0.002(5) C6 0.053(7) 0.041(7) 0.038(6) -0.001(5) 0.011(6) 0.000(6) C7 0.058(8) 0.051(8) 0.058(7) 0.008(6) -0.015(6) -0.013(6) C8 0.082(11) 0.069(9) 0.067(9) 0.023(7) -0.014(8) -0.016(8) C9 0.061(9) 0.052(7) 0.068(8) 0.006(6) 0.013(7) -0.006(6) C10 0.052(8) 0.058(9) 0.071(9) 0.019(7) -0.008(7) -0.014(6) C11 0.032(6) 0.038(6) 0.047(6) 0.011(5) 0.009(5) -0.004(5) C12 0.054(7) 0.057(7) 0.047(6) 0.002(6) 0.005(5) -0.012(6) C13 0.067(9) 0.103(11) 0.051(8) 0.040(8) 0.000(7) -0.005(8) C14 0.093(10) 0.060(8) 0.040(6) -0.003(6) 0.015(7) -0.015(7) C15 0.056(7) 0.055(8) 0.043(6) 0.000(6) 0.011(6) -0.005(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 Rh N1 2.054(8) . ? Rh N2 2.057(10) . ? Rh N3 2.062(10) . ? Rh Cl2 2.337(3) . ? Rh Cl3 2.358(4) . ? Rh Cl1 2.364(3) . ? N1 C1 1.298(11) . ? N1 O1 1.410(9) . ? N2 C6 1.290(12) . ? N2 O2 1.391(9) . ? N3 C11 1.280(13) . ? N3 O3 1.421(9) . ? C1 C5 1.481(12) . ? C1 C2 1.508(13) . ? C2 C3 1.532(13) . ? C3 C4 1.502(14) . ? C4 C5 1.530(14) . ? C6 C7 1.512(14) . ? C6 C10 1.509(14) . ? C7 C8 1.539(14) . ? C8 C9 1.473(14) . ? C9 C10 1.497(15) . ? C11 C15 1.506(13) . ? C11 C12 1.507(13) . ? C12 C13 1.527(15) . ? C13 C14 1.508(15) . ? C14 C15 1.516(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 N1 Rh N2 92.6(4) . . ? N1 Rh N3 89.6(4) . . ? N2 Rh N3 177.8(3) . . ? N1 Rh Cl2 94.3(2) . . ? N2 Rh Cl2 90.0(3) . . ? N3 Rh Cl2 90.1(3) . . ? N1 Rh Cl3 177.9(2) . . ? N2 Rh Cl3 88.1(3) . . ? N3 Rh Cl3 89.7(3) . . ? Cl2 Rh Cl3 87.66(13) . . ? N1 Rh Cl1 89.8(2) . . ? N2 Rh Cl1 91.6(3) . . ? N3 Rh Cl1 88.2(3) . . ? Cl2 Rh Cl1 175.53(10) . . ? Cl3 Rh Cl1 88.19(13) . . ? C1 N1 O1 112.5(7) . . ? C1 N1 Rh 135.2(7) . . ? O1 N1 Rh 112.4(5) . . ? C6 N2 O2 111.9(9) . . ? C6 N2 Rh 132.7(8) . . ? O2 N2 Rh 115.4(6) . . ? C11 N3 O3 111.3(8) . . ? C11 N3 Rh 134.9(7) . . ? O3 N3 Rh 113.8(6) . . ? N1 C1 C5 126.4(9) . . ? N1 C1 C2 122.6(9) . . ? C5 C1 C2 111.1(8) . . ? C1 C2 C3 102.8(8) . . ? C4 C3 C2 105.4(8) . . ? C3 C4 C5 103.8(9) . . ? C1 C5 C4 102.8(8) . . ? N2 C6 C7 123.7(10) . . ? N2 C6 C10 126.8(10) . . ? C7 C6 C10 109.5(9) . . ? C6 C7 C8 104.4(9) . . ? C9 C8 C7 104.6(9) . . ? C8 C9 C10 107.8(10) . . ? C9 C10 C6 102.4(9) . . ? N3 C11 C15 124.6(9) . . ? N3 C11 C12 124.8(9) . . ? C15 C11 C12 110.6(9) . . ? C11 C12 C13 103.7(9) . . ? C14 C13 C12 105.1(10) . . ? C13 C14 C15 105.2(10) . . ? C11 C15 C14 102.6(9) . . ? _diffrn_measured_fraction_theta_max 0.368 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.368 _refine_diff_density_max 0.689 _refine_diff_density_min -0.359 _refine_diff_density_rms 0.101 #===END data_pmb19 # compound 2 in manuscript _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H21 Cl3 N3 O2 Rh' _chemical_formula_weight 448.58 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 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 11.512(2) _cell_length_b 9.724(2) _cell_length_c 15.694(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.06(3) _cell_angle_gamma 90.00 _cell_volume 1679.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 11.3 _cell_measurement_theta_max 12.6 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.90 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 1.500 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.3454 _exptl_absorpt_correction_T_max 0.8645 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator beta-filter _diffrn_measurement_device_type CAD-4 _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% .2 _diffrn_reflns_number 2090 _diffrn_reflns_av_R_equivalents 0.0138 _diffrn_reflns_av_sigmaI/netI 0.0187 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 24.95 _reflns_number_total 1982 _reflns_number_gt 1982 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+0.9685P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1982 _refine_ls_number_parameters 270 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0211 _refine_ls_R_factor_gt 0.0211 _refine_ls_wR_factor_ref 0.0559 _refine_ls_wR_factor_gt 0.0559 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0.039 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh Rh 0.30474(2) 0.10028(2) 0.724883(16) 0.03143(10) Uani 1 d . . . Cl1 Cl 0.29430(9) -0.08414(9) 0.62954(6) 0.0481(2) Uani 1 d . . . Cl2 Cl 0.41131(8) 0.22984(9) 0.64741(6) 0.0419(2) Uani 1 d . . . Cl3 Cl 0.20678(10) -0.02406(10) 0.81239(7) 0.0543(3) Uani 1 d . . . O1 O 0.0523(3) 0.1841(3) 0.69819(19) 0.0617(8) Uani 1 d . . . O2 O 0.4464(2) 0.2146(2) 0.89312(15) 0.0415(6) Uani 1 d . . . N1 N 0.1369(3) 0.1695(3) 0.64830(18) 0.0364(6) Uani 1 d . . . N2 N 0.3439(2) 0.2521(3) 0.81729(17) 0.0357(6) Uani 1 d . . . N3 N 0.4608(3) 0.0352(3) 0.8060(2) 0.0395(7) Uani 1 d . . . C1 C 0.0891(3) 0.2088(4) 0.5694(2) 0.0461(9) Uani 1 d . . . C2 C -0.0366(4) 0.2648(5) 0.5326(3) 0.0562(11) Uani 1 d . . . C3 C -0.0408(5) 0.3111(6) 0.4387(3) 0.0692(13) Uani 1 d . . . C4 C 0.0436(5) 0.2121(6) 0.4128(3) 0.0703(13) Uani 1 d . . . C5 C 0.1515(4) 0.2021(6) 0.4976(3) 0.0607(11) Uani 1 d . . . C6 C 0.3159(3) 0.3776(3) 0.8260(2) 0.0352(7) Uani 1 d . . . C7 C 0.2185(4) 0.4518(4) 0.7572(3) 0.0446(9) Uani 1 d . . . C8 C 0.2473(5) 0.6028(4) 0.7832(3) 0.0550(10) Uani 1 d . . . C9 C 0.3013(5) 0.6005(4) 0.8817(3) 0.0549(11) Uani 1 d . . . C10 C 0.3781(4) 0.4704(4) 0.9015(3) 0.0403(8) Uani 1 d . . . C11 C 0.5045(3) 0.1018(3) 0.8773(2) 0.0387(8) Uani 1 d . . . C12 C 0.6179(5) 0.0754(5) 0.9498(3) 0.0525(11) Uani 1 d . . . H3N H 0.497(4) -0.033(4) 0.805(3) 0.050(12) Uiso 1 d . . . H21 H -0.057(4) 0.323(5) 0.569(3) 0.072(16) Uiso 1 d . . . H22 H -0.090(5) 0.183(6) 0.536(3) 0.086(16) Uiso 1 d . . . H31 H -0.007(6) 0.429(7) 0.450(4) 0.12(2) Uiso 1 d . . . H32 H -0.126(5) 0.313(5) 0.400(3) 0.079(15) Uiso 1 d . . . H41 H 0.076(5) 0.231(6) 0.364(4) 0.101(19) Uiso 1 d . . . H42 H -0.004(5) 0.102(6) 0.392(4) 0.092(17) Uiso 1 d . . . H51 H 0.196(5) 0.102(6) 0.504(4) 0.11(2) Uiso 1 d . . . H52 H 0.194(5) 0.307(6) 0.488(3) 0.088(16) Uiso 1 d . . . H71 H 0.144(4) 0.429(4) 0.764(3) 0.043(11) Uiso 1 d . . . H72 H 0.213(4) 0.430(5) 0.697(3) 0.064(14) Uiso 1 d . . . H81 H 0.175(4) 0.654(5) 0.768(3) 0.060(13) Uiso 1 d . . . H82 H 0.307(4) 0.637(5) 0.760(3) 0.063(14) Uiso 1 d . . . H91 H 0.232(4) 0.589(5) 0.912(3) 0.071(14) Uiso 1 d . . . H92 H 0.342(4) 0.674(5) 0.901(3) 0.060(13) Uiso 1 d . . . H101 H 0.451(4) 0.478(4) 0.896(2) 0.039(11) Uiso 1 d . . . H102 H 0.389(3) 0.427(4) 0.961(3) 0.041(10) Uiso 1 d . . . H121 H 0.636(5) -0.011(6) 0.943(3) 0.074(16) Uiso 1 d . . . H122 H 0.668(5) 0.128(6) 0.946(4) 0.09(2) Uiso 1 d . . . H123 H 0.601(4) 0.076(5) 1.000(4) 0.071(17) Uiso 1 d . . . H1O H 0.0720 0.1061 0.7491 0.050 Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh 0.03811(15) 0.02479(14) 0.02805(15) -0.00216(11) 0.00451(10) -0.00149(12) Cl1 0.0622(6) 0.0328(4) 0.0461(5) -0.0132(4) 0.0107(4) -0.0047(4) Cl2 0.0449(5) 0.0356(4) 0.0456(5) -0.0006(4) 0.0136(4) -0.0065(4) Cl3 0.0687(6) 0.0479(5) 0.0477(5) 0.0092(4) 0.0195(5) -0.0087(5) O1 0.0568(17) 0.085(2) 0.0490(16) 0.0038(15) 0.0235(13) 0.0078(16) O2 0.0506(14) 0.0345(13) 0.0299(12) -0.0036(10) -0.0031(10) 0.0069(11) N1 0.0396(15) 0.0350(15) 0.0333(16) -0.0030(12) 0.0086(12) -0.0027(13) N2 0.0406(15) 0.0317(14) 0.0299(14) -0.0014(11) 0.0028(12) 0.0035(12) N3 0.0449(17) 0.0285(15) 0.0390(17) -0.0002(13) 0.0027(13) 0.0053(14) C1 0.050(2) 0.0388(19) 0.042(2) -0.0014(16) 0.0032(17) -0.0062(18) C2 0.047(2) 0.065(3) 0.049(2) 0.006(2) 0.0012(19) 0.000(2) C3 0.061(3) 0.078(3) 0.057(3) 0.017(2) 0.000(2) 0.001(3) C4 0.075(3) 0.093(4) 0.039(2) 0.008(2) 0.010(2) -0.004(3) C5 0.060(3) 0.077(3) 0.046(2) 0.003(2) 0.017(2) 0.000(3) C6 0.0416(18) 0.0313(18) 0.0348(18) -0.0031(14) 0.0144(14) -0.0002(15) C7 0.049(2) 0.0335(19) 0.045(2) -0.0003(16) 0.0038(18) 0.0070(17) C8 0.067(3) 0.034(2) 0.062(3) 0.0004(19) 0.015(2) 0.009(2) C9 0.073(3) 0.037(2) 0.056(3) -0.0161(19) 0.020(2) 0.002(2) C10 0.048(2) 0.0363(19) 0.037(2) -0.0094(16) 0.0137(17) -0.0041(17) C11 0.0448(19) 0.0296(17) 0.0370(19) 0.0035(15) 0.0048(15) 0.0000(16) C12 0.053(3) 0.047(3) 0.047(3) 0.003(2) -0.004(2) 0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh N3 1.977(3) . ? Rh N2 2.025(3) . ? Rh N1 2.066(3) . ? Rh Cl1 2.3160(9) . ? Rh Cl2 2.3337(10) . ? Rh Cl3 2.3513(11) . ? O1 N1 1.424(4) . ? O2 C11 1.345(4) . ? O2 N2 1.456(3) . ? N1 C1 1.258(4) . ? N2 C6 1.280(4) . ? N3 C11 1.261(5) . ? C1 C2 1.495(6) . ? C1 C5 1.504(6) . ? C2 C3 1.529(6) . ? C3 C4 1.505(8) . ? C4 C5 1.535(6) . ? C6 C10 1.495(5) . ? C6 C7 1.494(5) . ? C7 C8 1.534(6) . ? C8 C9 1.488(6) . ? C9 C10 1.522(6) . ? C11 C12 1.481(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Rh N2 78.61(12) . . ? N3 Rh N1 175.70(12) . . ? N2 Rh N1 98.79(11) . . ? N3 Rh Cl1 91.93(10) . . ? N2 Rh Cl1 170.22(8) . . ? N1 Rh Cl1 90.80(8) . . ? N3 Rh Cl2 89.48(10) . . ? N2 Rh Cl2 86.50(9) . . ? N1 Rh Cl2 93.80(8) . . ? Cl1 Rh Cl2 90.97(4) . . ? N3 Rh Cl3 87.72(10) . . ? N2 Rh Cl3 90.04(9) . . ? N1 Rh Cl3 88.86(9) . . ? Cl1 Rh Cl3 92.08(4) . . ? Cl2 Rh Cl3 175.92(4) . . ? C11 O2 N2 112.4(2) . . ? C1 N1 O1 109.9(3) . . ? C1 N1 Rh 137.3(3) . . ? O1 N1 Rh 112.7(2) . . ? C6 N2 O2 108.7(3) . . ? C6 N2 Rh 139.6(2) . . ? O2 N2 Rh 111.06(18) . . ? C11 N3 Rh 117.2(3) . . ? N1 C1 C2 125.7(4) . . ? N1 C1 C5 123.9(4) . . ? C2 C1 C5 110.4(4) . . ? C1 C2 C3 103.4(4) . . ? C4 C3 C2 103.4(4) . . ? C3 C4 C5 103.2(4) . . ? C1 C5 C4 101.7(4) . . ? N2 C6 C10 125.7(3) . . ? N2 C6 C7 122.9(3) . . ? C10 C6 C7 111.4(3) . . ? C6 C7 C8 102.2(3) . . ? C9 C8 C7 104.7(4) . . ? C8 C9 C10 105.3(3) . . ? C6 C10 C9 103.1(3) . . ? N3 C11 O2 119.4(3) . . ? N3 C11 C12 128.6(4) . . ? O2 C11 C12 111.9(3) . . ? _diffrn_measured_fraction_theta_max 0.631 _diffrn_reflns_theta_full 24.95 _diffrn_measured_fraction_theta_full 0.631 _refine_diff_density_max 0.642 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.063 #===END data_pmb21 # compound 3 in manuscript _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H27 Cl3 N4 O3.50 Rh' _chemical_formula_weight 516.66 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.524(2) _cell_length_b 11.529(2) _cell_length_c 12.116(2) _cell_angle_alpha 67.21(3) _cell_angle_beta 94.35(3) _cell_angle_gamma 82.12(3) _cell_volume 1076.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _exptl_crystal_description plate _exptl_crystal_colour ? _exptl_crystal_size_max .52 _exptl_crystal_size_mid .50 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 526 _exptl_absorpt_coefficient_mu 1.188 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator beta-filter _diffrn_measurement_device_type 'Syntex P-1' _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _diffrn_reflns_number 3103 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0147 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3103 _reflns_number_gt 3094 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 fullcycle _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+0.9751P] 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 refined _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0108(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3103 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0317 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0828 _refine_ls_wR_factor_gt 0.0824 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.750 _refine_ls_shift/su_mean 0.073 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.0000 0.0000 0.5000 0.02750(14) Uani 1 d S . . Rh2 Rh 0.0000 0.0000 0.0000 0.02918(14) Uani 1 d S . . Cl1 Cl 0.10725(11) 0.11850(9) 0.59583(9) 0.0434(2) Uani 1 d . . . Cl2 Cl -0.19164(11) 0.04454(9) -0.16550(8) 0.0448(2) Uani 1 d . . . Cl3 Cl -0.22255(14) 0.36506(10) 0.10285(10) 0.0586(3) Uani 1 d . . . O1 O 0.2736(3) 0.0604(2) 0.3756(2) 0.0348(5) Uani 1 d . . . N1 N 0.2199(3) -0.0472(3) 0.4629(2) 0.0305(6) Uani 1 d . . . N2 N 0.0090(4) 0.1437(3) 0.3385(3) 0.0330(6) Uani 1 d . . . C1 C 0.3219(4) -0.1496(3) 0.4904(3) 0.0323(7) Uani 1 d . . . C2 C 0.4749(4) -0.1618(4) 0.4396(4) 0.0409(8) Uani 1 d . . . C3 C 0.5514(6) -0.3015(4) 0.5109(5) 0.0626(13) Uani 1 d . . . C4 C 0.4134(6) -0.3703(4) 0.5474(5) 0.0615(12) Uani 1 d . . . C5 C 0.2963(5) -0.2769(4) 0.5762(4) 0.0468(9) Uani 1 d . . . C6 C 0.1940(6) 0.2497(4) 0.1996(4) 0.0475(10) Uani 1 d . . . C7 C 0.1467(4) 0.1514(3) 0.3062(3) 0.0343(7) Uani 1 d . . . O1' O -0.2704(3) -0.0799(3) 0.1189(3) 0.0469(6) Uani 1 d . . . N1' N -0.1157(4) -0.1347(3) 0.1018(3) 0.0375(7) Uani 1 d . . . N2' N -0.1618(4) 0.0989(3) 0.0596(3) 0.0359(7) Uani 1 d . . . C1' C -0.0837(5) -0.2542(4) 0.1661(3) 0.0445(9) Uani 1 d . . . C2' C -0.1839(8) -0.3314(5) 0.2532(5) 0.0645(13) Uani 1 d . . . C3' C -0.0813(10) -0.4635(6) 0.3112(7) 0.097(2) Uani 1 d . . . C4' C 0.0840(11) -0.4480(6) 0.2912(7) 0.095(2) Uani 1 d . . . C5' C 0.0712(7) -0.3355(4) 0.1699(5) 0.0580(11) Uani 1 d . . . C6' C -0.4203(6) 0.0958(6) 0.1407(6) 0.0609(13) Uani 1 d . . . C7' C -0.2745(4) 0.0428(4) 0.1039(3) 0.0401(8) Uani 1 d . . . O1W O -0.4518(8) 0.4957(9) -0.1539(5) 0.179(4) Uani 1 d . . . O2W O -0.444(3) 0.300(2) -0.219(3) 0.300(12) Uani 0.50 d P . . H21 H 0.454(5) -0.142(4) 0.351(4) 0.041(10) Uiso 1 d . . . H22 H 0.544(5) -0.108(4) 0.447(3) 0.037(10) Uiso 1 d . . . H31 H 0.617(6) -0.327(4) 0.459(4) 0.063(13) Uiso 1 d . . . H32 H 0.626(8) -0.318(6) 0.598(6) 0.10(2) Uiso 1 d . . . H41 H 0.450(6) -0.462(5) 0.625(5) 0.071(15) Uiso 1 d . . . H42 H 0.360(6) -0.375(5) 0.473(5) 0.072(16) Uiso 1 d . . . H51 H 0.346(5) -0.285(4) 0.661(4) 0.051(12) Uiso 1 d . . . H52 H 0.201(5) -0.288(4) 0.568(4) 0.048(12) Uiso 1 d . . . H61 H 0.117(6) 0.310(5) 0.166(5) 0.069(16) Uiso 1 d . . . H62 H 0.283(7) 0.281(5) 0.225(5) 0.076(16) Uiso 1 d . . . H63 H 0.235(7) 0.209(6) 0.156(6) 0.10(2) Uiso 1 d . . . H1N2 H -0.063(4) 0.196(4) 0.288(3) 0.029(9) Uiso 1 d . . . H21' H -0.279(6) -0.325(5) 0.208(5) 0.070(16) Uiso 1 d . . . H22' H -0.198(6) -0.300(5) 0.313(5) 0.069(15) Uiso 1 d . . . H31' H -0.104(7) -0.493(6) 0.385(6) 0.087(19) Uiso 1 d . . . H32' H -0.045(16) -0.500(11) 0.240(11) 0.23(5) Uiso 1 d . . . H41' H 0.159(9) -0.513(7) 0.307(6) 0.11(2) Uiso 1 d . . . H42' H 0.165(13) -0.433(11) 0.368(10) 0.20(5) Uiso 1 d . . . H51' H 0.155(6) -0.299(5) 0.172(4) 0.055(14) Uiso 1 d . . . H52' H 0.061(6) -0.353(5) 0.097(5) 0.075(15) Uiso 1 d . . . H61' H -0.402(7) 0.063(6) 0.227(6) 0.10(2) Uiso 1 d . . . H62' H -0.417(7) 0.177(7) 0.129(6) 0.10(2) Uiso 1 d . . . H63' H -0.500(8) 0.079(7) 0.112(6) 0.10(2) Uiso 1 d . . . H2N' H -0.164(5) 0.167(4) 0.053(3) 0.033(11) Uiso 1 d . . . H1W1 H -0.525(4) 0.406(3) -0.097(3) 0.016(8) Uiso 1 d . . . H2W1 H -0.375(16) 0.489(14) -0.046(13) 0.34(7) Uiso 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 0.0247(2) 0.0290(2) 0.0304(2) -0.01363(16) 0.00712(14) -0.00320(14) Rh2 0.0296(2) 0.0304(2) 0.0296(2) -0.01312(16) 0.00948(15) -0.00580(15) Cl1 0.0439(5) 0.0516(5) 0.0486(5) -0.0314(4) 0.0123(4) -0.0165(4) Cl2 0.0427(5) 0.0543(5) 0.0396(5) -0.0226(4) 0.0021(4) -0.0065(4) Cl3 0.0599(6) 0.0534(6) 0.0545(6) -0.0227(5) -0.0025(5) 0.0126(5) O1 0.0291(12) 0.0332(12) 0.0396(13) -0.0109(10) 0.0096(10) -0.0068(10) N1 0.0295(14) 0.0318(14) 0.0308(14) -0.0126(12) 0.0081(11) -0.0057(12) N2 0.0319(15) 0.0313(15) 0.0325(15) -0.0109(13) 0.0052(13) -0.0003(13) C1 0.0295(17) 0.0354(18) 0.0342(17) -0.0166(15) 0.0061(14) -0.0042(14) C2 0.0303(18) 0.043(2) 0.047(2) -0.0161(18) 0.0101(16) -0.0026(16) C3 0.049(3) 0.048(2) 0.077(3) -0.014(2) 0.024(2) 0.011(2) C4 0.061(3) 0.039(2) 0.079(3) -0.019(2) 0.026(3) 0.005(2) C5 0.043(2) 0.035(2) 0.055(3) -0.0109(18) 0.0163(19) -0.0013(17) C6 0.046(2) 0.038(2) 0.052(2) -0.0098(19) 0.016(2) -0.0061(19) C7 0.0350(18) 0.0325(17) 0.0363(18) -0.0154(15) 0.0072(14) -0.0031(14) O1' 0.0383(14) 0.0494(16) 0.0607(17) -0.0256(14) 0.0218(13) -0.0142(12) N1' 0.0360(16) 0.0399(17) 0.0426(17) -0.0200(14) 0.0170(13) -0.0098(13) N2' 0.0362(16) 0.0359(17) 0.0407(17) -0.0193(14) 0.0135(13) -0.0072(14) C1' 0.061(2) 0.038(2) 0.039(2) -0.0171(17) 0.0145(18) -0.0153(18) C2' 0.091(4) 0.053(3) 0.062(3) -0.024(2) 0.034(3) -0.038(3) C3' 0.136(6) 0.063(4) 0.073(4) 0.000(3) 0.025(4) -0.035(4) C4' 0.120(6) 0.051(3) 0.081(5) 0.005(3) 0.021(4) 0.004(4) C5' 0.073(3) 0.039(2) 0.059(3) -0.017(2) 0.018(2) -0.004(2) C6' 0.042(3) 0.064(3) 0.084(4) -0.035(3) 0.031(3) -0.008(2) C7' 0.0385(19) 0.044(2) 0.041(2) -0.0202(17) 0.0116(16) -0.0054(17) O1W 0.131(5) 0.279(10) 0.082(4) -0.065(5) -0.007(3) 0.076(6) O2W 0.25(2) 0.24(2) 0.42(4) -0.17(2) -0.03(2) -0.015(19) _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 2.013(3) . ? Rh1 N1 2.013(3) 2_556 ? Rh1 N2 2.031(3) 2_556 ? Rh1 N2 2.031(3) . ? Rh1 Cl1 2.3368(11) 2_556 ? Rh1 Cl1 2.3368(11) . ? Rh2 N1' 2.007(3) 2 ? Rh2 N1' 2.007(3) . ? Rh2 N2' 2.020(3) 2 ? Rh2 N2' 2.020(3) . ? Rh2 Cl2 2.3299(13) 2 ? Rh2 Cl2 2.3299(13) . ? O1 C7 1.358(5) . ? O1 N1 1.442(4) . ? N1 C1 1.276(5) . ? N2 C7 1.269(5) . ? C1 C5 1.491(6) . ? C1 C2 1.497(5) . ? C2 C3 1.521(6) . ? C3 C4 1.507(8) . ? C4 C5 1.525(6) . ? C6 C7 1.479(6) . ? O1' C7' 1.349(5) . ? O1' N1' 1.447(4) . ? N1' C1' 1.269(5) . ? N2' C7' 1.268(5) . ? C1' C2' 1.501(6) . ? C1' C5' 1.497(7) . ? C2' C3' 1.513(10) . ? C3' C4' 1.471(12) . ? C4' C5' 1.521(8) . ? C6' C7' 1.484(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 N1 Rh1 N1 180.0 . 2_556 ? N1 Rh1 N2 103.38(12) . 2_556 ? N1 Rh1 N2 76.62(12) 2_556 2_556 ? N1 Rh1 N2 76.62(12) . . ? N1 Rh1 N2 103.38(12) 2_556 . ? N2 Rh1 N2 180.0 2_556 . ? N1 Rh1 Cl1 91.40(9) . 2_556 ? N1 Rh1 Cl1 88.60(9) 2_556 2_556 ? N2 Rh1 Cl1 88.53(9) 2_556 2_556 ? N2 Rh1 Cl1 91.47(9) . 2_556 ? N1 Rh1 Cl1 88.60(9) . . ? N1 Rh1 Cl1 91.40(9) 2_556 . ? N2 Rh1 Cl1 91.47(9) 2_556 . ? N2 Rh1 Cl1 88.53(9) . . ? Cl1 Rh1 Cl1 180.0 2_556 . ? N1' Rh2 N1' 180.0 2 . ? N1' Rh2 N2' 76.97(13) 2 2 ? N1' Rh2 N2' 103.03(13) . 2 ? N1' Rh2 N2' 103.03(13) 2 . ? N1' Rh2 N2' 76.97(13) . . ? N2' Rh2 N2' 180.0 2 . ? N1' Rh2 Cl2 89.10(10) 2 2 ? N1' Rh2 Cl2 90.90(10) . 2 ? N2' Rh2 Cl2 87.85(10) 2 2 ? N2' Rh2 Cl2 92.15(10) . 2 ? N1' Rh2 Cl2 90.90(10) 2 . ? N1' Rh2 Cl2 89.10(10) . . ? N2' Rh2 Cl2 92.15(10) 2 . ? N2' Rh2 Cl2 87.85(10) . . ? Cl2 Rh2 Cl2 180.0 2 . ? C7 O1 N1 110.5(3) . . ? C1 N1 O1 110.4(3) . . ? C1 N1 Rh1 136.8(3) . . ? O1 N1 Rh1 112.61(19) . . ? C7 N2 Rh1 115.9(3) . . ? N1 C1 C5 122.5(3) . . ? N1 C1 C2 126.6(3) . . ? C5 C1 C2 110.9(3) . . ? C1 C2 C3 103.4(3) . . ? C4 C3 C2 105.1(4) . . ? C3 C4 C5 103.9(4) . . ? C1 C5 C4 103.0(4) . . ? N2 C7 O1 119.1(3) . . ? N2 C7 C6 128.9(4) . . ? O1 C7 C6 112.0(3) . . ? C7' O1' N1' 110.9(3) . . ? C1' N1' O1' 110.5(3) . . ? C1' N1' Rh2 137.0(3) . . ? O1' N1' Rh2 111.9(2) . . ? C7' N2' Rh2 115.7(3) . . ? N1' C1' C2' 126.7(4) . . ? N1' C1' C5' 122.4(4) . . ? C2' C1' C5' 110.7(4) . . ? C1' C2' C3' 103.6(5) . . ? C4' C3' C2' 107.0(5) . . ? C3' C4' C5' 105.9(7) . . ? C1' C5' C4' 102.0(5) . . ? N2' C7' O1' 119.2(3) . . ? N2' C7' C6' 128.3(4) . . ? O1' C7' C6' 112.6(4) . . ? _diffrn_measured_fraction_theta_max 0.815 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.815 _refine_diff_density_max 0.969 _refine_diff_density_min -1.325 _refine_diff_density_rms 0.096 #===END data_vk06 # compound 4 in manuscript _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H21 Cl1.50 N2 O2.50 Rh0.50' _chemical_formula_weight 361.96 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 8.866(2) _cell_length_b 10.358(2) _cell_length_c 10.952(2) _cell_angle_alpha 109.58(3) _cell_angle_beta 97.65(3) _cell_angle_gamma 112.09(3) _cell_volume 838.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10 _cell_measurement_theta_max 13 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 374 _exptl_absorpt_coefficient_mu 0.789 _exptl_absorpt_correction_type numeric _exptl_absorpt_correction_T_min 0.846 _exptl_absorpt_correction_T_max 0.965 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator beta-filter _diffrn_measurement_device_type CAD-4 _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 5 _diffrn_reflns_number 1751 _diffrn_reflns_av_R_equivalents 0.0120 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 24.96 _reflns_number_total 1618 _reflns_number_gt 1618 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0775P)^2^+0.2425P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refined _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1618 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0332 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0907 _refine_ls_wR_factor_gt 0.0907 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh Rh 0.5000 0.5000 0.5000 0.0385(2) Uani 1 d S . . Cl1 Cl 0.21684(17) 0.41480(13) 0.38275(14) 0.0536(4) Uani 1 d . . . O1 O 0.3990(5) 0.1818(3) 0.3349(4) 0.0514(9) Uani 1 d . . . N1 N 0.4224(6) 0.3215(4) 0.5515(5) 0.0436(10) Uani 1 d . . . N2 N 0.5084(5) 0.3327(4) 0.3460(4) 0.0445(10) Uani 1 d . . . C1 C 0.3765(6) 0.1903(5) 0.4562(5) 0.0433(12) Uani 1 d . . . C2 C 0.2972(7) 0.0398(5) 0.4600(6) 0.0477(13) Uani 1 d . . . C3 C 0.3130(7) -0.0839(5) 0.3733(7) 0.0544(14) Uani 1 d . . . C4 C 0.2396(8) -0.2232(7) 0.3823(8) 0.0647(17) Uani 1 d . . . C5 C 0.1546(9) -0.2387(7) 0.4763(8) 0.0729(19) Uani 1 d . . . C6 C 0.1347(9) -0.1177(7) 0.5595(8) 0.0721(19) Uani 1 d . . . C7 C 0.2079(8) 0.0233(7) 0.5528(7) 0.0613(16) Uani 1 d . . . C8 C 0.5921(7) 0.3220(6) 0.2593(5) 0.0497(13) Uani 1 d . . . C9 C 0.5851(11) 0.1774(7) 0.1614(8) 0.0671(18) Uani 1 d . . . C10 C 0.7105(13) 0.2292(9) 0.0868(10) 0.103(3) Uani 1 d . . . C11 C 0.8233(10) 0.3954(9) 0.1709(10) 0.084(2) Uani 1 d . . . C12 C 0.7189(9) 0.4589(7) 0.2484(8) 0.0596(16) Uani 1 d . . . Cl2 Cl 0.5215(14) 0.3328(14) -0.1596(9) 0.0851(18) Uani 0.50 d P . . O1W O 0.507(5) 0.364(4) -0.165(3) 0.125(12) Uani 0.50 d P . . O1E O 0.3242(16) 0.3262(13) 0.0168(11) 0.188(4) Uiso 1 d . . . C1E C 0.144(3) 0.215(2) -0.007(2) 0.213(7) Uiso 1 d . . . C2EA C 0.050(3) 0.217(3) -0.100(3) 0.137(8) Uiso 0.50 d P . . C2EB C 0.050(3) 0.112(3) -0.125(3) 0.137(8) Uiso 0.50 d P . . H1N H 0.424(6) 0.319(5) 0.632(6) 0.038(14) Uiso 1 d . . . H3 H 0.372(7) -0.066(5) 0.305(5) 0.040(13) Uiso 1 d . . . H4 H 0.252(9) -0.299(8) 0.328(7) 0.07(2) Uiso 1 d . . . H5 H 0.101(8) -0.333(7) 0.492(6) 0.062(16) Uiso 1 d . . . H6 H 0.079(9) -0.140(8) 0.625(7) 0.09(2) Uiso 1 d . . . H7 H 0.189(7) 0.100(6) 0.611(5) 0.047(15) Uiso 1 d . . . H91 H 0.460(12) 0.102(10) 0.123(8) 0.11(3) Uiso 1 d . . . H92 H 0.583(9) 0.127(7) 0.202(7) 0.06(2) Uiso 1 d . . . H101 H 0.755(9) 0.153(8) 0.042(7) 0.09(2) Uiso 1 d . . . H102 H 0.625(18) 0.260(15) -0.017(14) 0.23(6) Uiso 1 d . . . H111 H 0.890(9) 0.450(8) 0.139(7) 0.07(2) Uiso 1 d . . . H112 H 0.884(16) 0.392(13) 0.277(13) 0.19(5) Uiso 1 d . . . H121 H 0.775(7) 0.551(7) 0.330(6) 0.048(14) Uiso 1 d . . . H122 H 0.660(10) 0.480(8) 0.205(8) 0.08(3) Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh 0.0427(4) 0.0253(3) 0.0442(4) 0.0147(3) 0.0113(3) 0.0125(3) Cl1 0.0479(9) 0.0410(7) 0.0638(9) 0.0216(7) 0.0081(7) 0.0151(6) O1 0.064(2) 0.0270(16) 0.056(2) 0.0165(16) 0.0207(19) 0.0130(16) N1 0.048(3) 0.035(2) 0.048(3) 0.022(2) 0.014(2) 0.0153(19) N2 0.051(3) 0.0268(18) 0.049(2) 0.0143(17) 0.013(2) 0.0118(18) C1 0.040(3) 0.032(2) 0.058(3) 0.021(2) 0.013(2) 0.015(2) C2 0.043(3) 0.033(2) 0.064(3) 0.022(2) 0.009(3) 0.014(2) C3 0.052(3) 0.032(3) 0.071(4) 0.018(3) 0.014(3) 0.016(2) C4 0.059(4) 0.036(3) 0.092(5) 0.024(3) 0.017(4) 0.020(3) C5 0.063(4) 0.040(3) 0.109(5) 0.038(4) 0.012(4) 0.015(3) C6 0.076(5) 0.053(4) 0.093(5) 0.045(4) 0.032(4) 0.020(3) C7 0.061(4) 0.045(3) 0.081(4) 0.032(3) 0.025(3) 0.021(3) C8 0.049(3) 0.040(3) 0.046(3) 0.010(2) 0.012(3) 0.013(2) C9 0.082(5) 0.049(3) 0.067(4) 0.017(3) 0.032(4) 0.029(4) C10 0.108(7) 0.063(4) 0.122(7) 0.015(4) 0.074(6) 0.030(4) C11 0.066(5) 0.065(4) 0.104(6) 0.024(4) 0.043(5) 0.018(4) C12 0.061(4) 0.049(3) 0.065(4) 0.023(3) 0.024(3) 0.019(3) Cl2 0.091(4) 0.107(5) 0.069(3) 0.044(3) 0.029(3) 0.049(4) O1W 0.135(18) 0.123(17) 0.142(17) 0.073(12) 0.026(12) 0.072(12) _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 N2 2.006(4) 2_666 ? Rh N2 2.006(4) . ? Rh N1 2.014(4) . ? Rh N1 2.014(4) 2_666 ? Rh Cl1 2.3337(17) 2_666 ? Rh Cl1 2.3337(17) . ? O1 C1 1.349(6) . ? O1 N2 1.449(5) . ? N1 C1 1.274(6) . ? N2 C8 1.282(7) . ? C1 C2 1.467(6) . ? C2 C3 1.384(8) . ? C2 C7 1.384(8) . ? C3 C4 1.386(7) . ? C4 C5 1.371(10) . ? C5 C6 1.370(10) . ? C6 C7 1.390(8) . ? C8 C9 1.494(8) . ? C8 C12 1.496(8) . ? C9 C10 1.509(11) . ? C10 C11 1.487(10) . ? C11 C12 1.518(10) . ? O1E C1E 1.50(2) . ? C1E C2EA 1.24(3) . ? C1E C2EB 1.28(3) . ? C2EA C2EB 1.04(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 N2 Rh N2 180.0 2_666 . ? N2 Rh N1 103.25(17) 2_666 . ? N2 Rh N1 76.75(17) . . ? N2 Rh N1 76.75(17) 2_666 2_666 ? N2 Rh N1 103.25(17) . 2_666 ? N1 Rh N1 180.0 . 2_666 ? N2 Rh Cl1 88.75(14) 2_666 2_666 ? N2 Rh Cl1 91.25(14) . 2_666 ? N1 Rh Cl1 91.26(13) . 2_666 ? N1 Rh Cl1 88.74(13) 2_666 2_666 ? N2 Rh Cl1 91.25(14) 2_666 . ? N2 Rh Cl1 88.75(14) . . ? N1 Rh Cl1 88.74(13) . . ? N1 Rh Cl1 91.26(13) 2_666 . ? Cl1 Rh Cl1 180.0 2_666 . ? C1 O1 N2 110.3(3) . . ? C1 N1 Rh 115.8(4) . . ? C8 N2 O1 110.4(4) . . ? C8 N2 Rh 137.5(3) . . ? O1 N2 Rh 111.8(3) . . ? N1 C1 O1 119.0(4) . . ? N1 C1 C2 127.6(5) . . ? O1 C1 C2 113.4(4) . . ? C3 C2 C7 120.3(5) . . ? C3 C2 C1 120.6(5) . . ? C7 C2 C1 119.1(5) . . ? C2 C3 C4 118.8(6) . . ? C5 C4 C3 121.0(6) . . ? C6 C5 C4 120.3(6) . . ? C5 C6 C7 119.7(7) . . ? C2 C7 C6 119.9(6) . . ? N2 C8 C9 126.3(5) . . ? N2 C8 C12 122.9(5) . . ? C9 C8 C12 110.7(5) . . ? C8 C9 C10 104.8(6) . . ? C11 C10 C9 106.6(7) . . ? C10 C11 C12 106.7(6) . . ? C8 C12 C11 103.0(5) . . ? C2EA C1E C2EB 48.6(16) . . ? C2EA C1E O1E 109(2) . . ? C2EB C1E O1E 121(2) . . ? C2EB C2EA C1E 68(2) . . ? C2EA C2EB C1E 64(2) . . ? _diffrn_measured_fraction_theta_max 0.550 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.550 _refine_diff_density_max 0.690 _refine_diff_density_min -0.575 _refine_diff_density_rms 0.073