# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1912 data_vk21 # compound 3 in the manuscript _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H20 Cl2 F6 N4 O2 Rh Sb' _chemical_formula_weight 637.86 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' 'F' 'F' 0.0171 0.0103 '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' 'Sb' 'Sb' -0.5866 1.5461 '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 12.293(2) _cell_length_b 10.021(2) _cell_length_c 8.811(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.75(3) _cell_angle_gamma 90.00 _cell_volume 1039.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10.1 _cell_measurement_theta_max 11.8 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.038 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 2.414 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.212 _exptl_absorpt_correction_T_max 0.356 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator filter _diffrn_measurement_device_type CAD4 _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_% .4 _diffrn_reflns_number 1138 _diffrn_reflns_av_R_equivalents 0.0845 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.96 _reflns_number_total 1065 _reflns_number_gt 1065 _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0985P)^2^+0.3958P] 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 1065 _refine_ls_number_parameters 139 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1098 _refine_ls_wR_factor_gt 0.1098 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 Sb Sb 0.5000 0.0000 0.5000 0.0519(3) Uani 1 2 d S . . F1 F 0.4329(4) 0.0351(7) 0.6594(6) 0.0949(18) Uani 1 1 d . . . F2A F 0.6389(13) 0.037(4) 0.6396(19) 0.139(10) Uani 0.50 1 d P . . F2B F 0.629(2) -0.076(5) 0.624(2) 0.187(17) Uani 0.50 1 d P . . F3A F 0.567(3) 0.162(3) 0.552(5) 0.199(14) Uani 0.50 1 d P . . F3B F 0.490(3) 0.1647(15) 0.417(2) 0.130(8) Uani 0.50 1 d P . . Rh Rh 0.0000 0.5000 0.5000 0.0317(2) Uani 1 2 d S . . Cl1 Cl -0.03711(15) 0.5531(2) 0.2334(2) 0.0512(5) Uani 1 1 d . . . O1 O 0.2101(4) 0.6261(5) 0.5002(5) 0.0474(11) Uani 1 1 d . . . N1 N 0.0532(4) 0.6873(5) 0.5666(6) 0.0374(12) Uani 1 1 d . . . N2 N 0.1677(4) 0.4931(5) 0.5134(7) 0.0393(13) Uani 1 1 d . . . C1 C 0.1501(5) 0.7179(6) 0.5527(7) 0.0402(14) Uani 1 1 d . . . C2 C 0.2097(6) 0.8475(7) 0.5885(9) 0.0570(18) Uani 1 1 d . . . C3 C 0.2450(5) 0.4067(7) 0.5253(7) 0.0431(16) Uani 1 1 d . . . C4 C 0.2212(6) 0.2650(8) 0.5542(9) 0.062(2) Uani 1 1 d . . . C5 C 0.3601(6) 0.4405(10) 0.5101(9) 0.063(2) Uani 1 1 d . . . H1 H 0.0409 0.7523 0.6211 0.080 Uiso 1 1 d . . . H21 H 0.1638 0.9069 0.6308 0.080 Uiso 1 1 d . . . H22 H 0.2144 0.8860 0.4906 0.080 Uiso 1 1 d . . . H23 H 0.2832 0.8368 0.6615 0.080 Uiso 1 1 d . . . H41 H 0.2890 0.2456 0.6448 0.080 Uiso 1 1 d . . . H42 H 0.2095 0.2046 0.4610 0.080 Uiso 1 1 d . . . H43 H 0.1529 0.2594 0.5856 0.080 Uiso 1 1 d . . . H51 H 0.4091 0.3613 0.5369 0.080 Uiso 1 1 d . . . H52 H 0.3957 0.5066 0.5897 0.080 Uiso 1 1 d . . . H53 H 0.3575 0.4708 0.4078 0.080 Uiso 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 Sb 0.0353(4) 0.0664(5) 0.0584(5) 0.0088(3) 0.0203(3) 0.0124(3) F1 0.073(4) 0.143(5) 0.080(3) -0.012(3) 0.040(3) 0.019(3) F2A 0.047(8) 0.31(3) 0.066(8) -0.024(16) 0.030(7) -0.049(15) F2B 0.114(19) 0.36(4) 0.072(10) 0.009(17) 0.010(11) 0.17(2) F3A 0.22(3) 0.16(2) 0.29(3) -0.16(2) 0.20(3) -0.138(19) F3B 0.25(3) 0.068(9) 0.112(11) 0.036(8) 0.110(14) 0.049(11) Rh 0.0222(4) 0.0298(4) 0.0439(4) 0.0007(3) 0.0110(3) -0.0002(2) Cl1 0.0483(10) 0.0553(10) 0.0477(9) 0.0057(9) 0.0101(7) -0.0090(9) O1 0.032(2) 0.048(3) 0.068(3) 0.000(2) 0.023(2) -0.007(2) N1 0.029(3) 0.034(3) 0.049(3) -0.003(2) 0.011(2) -0.004(2) N2 0.028(3) 0.038(3) 0.052(3) -0.001(2) 0.011(2) -0.003(2) C1 0.034(3) 0.040(3) 0.047(3) -0.001(3) 0.013(3) -0.005(3) C2 0.040(4) 0.047(4) 0.083(5) -0.006(4) 0.017(3) -0.018(3) C3 0.026(3) 0.052(4) 0.047(4) -0.011(3) 0.002(3) 0.006(3) C4 0.046(4) 0.050(5) 0.084(5) -0.005(4) 0.010(4) 0.010(4) C5 0.036(4) 0.091(6) 0.068(4) -0.008(5) 0.023(3) 0.007(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 Sb F3B 1.793(12) . ? Sb F3B 1.793(12) 3_656 ? Sb F2B 1.811(14) 3_656 ? Sb F2B 1.811(14) . ? Sb F3A 1.817(14) 3_656 ? Sb F3A 1.817(14) . ? Sb F2A 1.831(15) 3_656 ? Sb F2A 1.831(15) . ? Sb F1 1.856(5) . ? Sb F1 1.856(5) 3_656 ? F2A F2B 1.14(4) . ? F2A F3A 1.60(3) . ? F2B F3B 1.66(3) 3_656 ? F3A F3B 1.28(3) . ? F3B F2B 1.66(3) 3_656 ? Rh N1 2.019(5) 3_566 ? Rh N1 2.019(5) . ? Rh N2 2.031(5) 3_566 ? Rh N2 2.031(5) . ? Rh Cl1 2.3219(17) 3_566 ? Rh Cl1 2.3219(17) . ? O1 C1 1.342(8) . ? O1 N2 1.449(7) . ? N1 C1 1.269(7) . ? N2 C3 1.268(8) . ? C1 C2 1.480(9) . ? C3 C4 1.486(11) . ? C3 C5 1.498(9) . ? 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 F3B Sb F3B 180.000(2) . 3_656 ? F3B Sb F2B 54.8(11) . 3_656 ? F3B Sb F2B 125.2(12) 3_656 3_656 ? F3B Sb F2B 125.2(12) . . ? F3B Sb F2B 54.8(12) 3_656 . ? F2B Sb F2B 180.000(6) 3_656 . ? F3B Sb F3A 138.3(12) . 3_656 ? F3B Sb F3A 41.7(12) 3_656 3_656 ? F2B Sb F3A 88.2(13) 3_656 3_656 ? F2B Sb F3A 91.8(13) . 3_656 ? F3B Sb F3A 41.7(12) . . ? F3B Sb F3A 138.3(12) 3_656 . ? F2B Sb F3A 91.8(13) 3_656 . ? F2B Sb F3A 88.2(13) . . ? F3A Sb F3A 180(2) 3_656 . ? F3B Sb F2A 88.4(9) . 3_656 ? F3B Sb F2A 91.6(9) 3_656 3_656 ? F2B Sb F2A 36.6(12) 3_656 3_656 ? F2B Sb F2A 143.4(12) . 3_656 ? F3A Sb F2A 51.9(11) 3_656 3_656 ? F3A Sb F2A 128.1(11) . 3_656 ? F3B Sb F2A 91.6(9) . . ? F3B Sb F2A 88.4(9) 3_656 . ? F2B Sb F2A 143.4(12) 3_656 . ? F2B Sb F2A 36.6(12) . . ? F3A Sb F2A 128.1(11) 3_656 . ? F3A Sb F2A 51.9(11) . . ? F2A Sb F2A 180.000(3) 3_656 . ? F3B Sb F1 98.1(5) . . ? F3B Sb F1 81.9(5) 3_656 . ? F2B Sb F1 82.9(6) 3_656 . ? F2B Sb F1 97.1(6) . . ? F3A Sb F1 95.0(6) 3_656 . ? F3A Sb F1 85.0(6) . . ? F2A Sb F1 90.8(6) 3_656 . ? F2A Sb F1 89.2(6) . . ? F3B Sb F1 81.9(5) . 3_656 ? F3B Sb F1 98.1(5) 3_656 3_656 ? F2B Sb F1 97.1(6) 3_656 3_656 ? F2B Sb F1 82.9(6) . 3_656 ? F3A Sb F1 85.0(6) 3_656 3_656 ? F3A Sb F1 95.0(6) . 3_656 ? F2A Sb F1 89.2(6) 3_656 3_656 ? F2A Sb F1 90.8(6) . 3_656 ? F1 Sb F1 180.0 . 3_656 ? F2B F2A F3A 133.8(19) . . ? F2B F2A Sb 70.8(13) . . ? F3A F2A Sb 63.6(8) . . ? F2A F2B F3B 128.1(16) . 3_656 ? F2A F2B Sb 72.7(14) . . ? F3B F2B Sb 62.1(8) 3_656 . ? F3B F3A F2A 128.5(14) . . ? F3B F3A Sb 68.2(8) . . ? F2A F3A Sb 64.5(9) . . ? F3A F3B F2B 124.1(14) . 3_656 ? F3A F3B Sb 70.1(12) . . ? F2B F3B Sb 63.2(8) 3_656 . ? N1 Rh N1 180.000(1) 3_566 . ? N1 Rh N2 77.1(2) 3_566 3_566 ? N1 Rh N2 102.9(2) . 3_566 ? N1 Rh N2 102.9(2) 3_566 . ? N1 Rh N2 77.1(2) . . ? N2 Rh N2 180.0 3_566 . ? N1 Rh Cl1 91.91(15) 3_566 3_566 ? N1 Rh Cl1 88.09(15) . 3_566 ? N2 Rh Cl1 88.11(17) 3_566 3_566 ? N2 Rh Cl1 91.89(17) . 3_566 ? N1 Rh Cl1 88.09(15) 3_566 . ? N1 Rh Cl1 91.91(15) . . ? N2 Rh Cl1 91.89(17) 3_566 . ? N2 Rh Cl1 88.11(17) . . ? Cl1 Rh Cl1 180.0 3_566 . ? C1 O1 N2 110.9(4) . . ? C1 N1 Rh 115.5(4) . . ? C3 N2 O1 110.8(5) . . ? C3 N2 Rh 138.8(5) . . ? O1 N2 Rh 110.3(3) . . ? N1 C1 O1 119.5(6) . . ? N1 C1 C2 127.8(6) . . ? O1 C1 C2 112.8(5) . . ? N2 C3 C4 119.1(6) . . ? N2 C3 C5 122.9(7) . . ? C4 C3 C5 118.0(6) . . ? _diffrn_measured_fraction_theta_max 0.522 _diffrn_reflns_theta_full 25.96 _diffrn_measured_fraction_theta_full 0.522 _refine_diff_density_max 2.195 _refine_diff_density_min -1.185 _refine_diff_density_rms 0.165 #===END data_vk02 # compound 5 in the manuscript _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H12 Cl3 N4 O2 Rh' _chemical_formula_weight 357.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0015 0.0009 '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' 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.0998 0.0984 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -2.5280 0.5964 '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 8.483(2) _cell_length_b 8.508(2) _cell_length_c 8.617(2) _cell_angle_alpha 87.86(3) _cell_angle_beta 79.59(3) _cell_angle_gamma 80.42(3) _cell_volume 603.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 8.5 _cell_measurement_theta_max 11 _exptl_crystal_description cube _exptl_crystal_colour yellow _exptl_crystal_size_max .25 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.968 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 352 _exptl_absorpt_coefficient_mu 1.076 _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 0.56083 _diffrn_radiation_type AgK\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_% 0.4 _diffrn_reflns_number 2027 _diffrn_reflns_av_R_equivalents 0.0140 _diffrn_reflns_av_sigmaI/netI 0.0149 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 19.97 _reflns_number_total 1894 _reflns_number_gt 1894 _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^)+(0.0594P)^2^+0.5908P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.022(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1894 _refine_ls_number_parameters 179 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0276 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0780 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.493 _refine_ls_shift/su_mean 0.044 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 0.5000 0.5000 0.01966(16) Uani 1 d S . . Rh2 Rh 0.0000 0.0000 0.0000 0.02050(16) Uani 1 d S . . Cl1 Cl -0.18951(11) -0.03630(10) 0.22459(10) 0.0319(2) Uani 1 d . . . Cl2 Cl -0.09105(11) 0.26247(10) 0.46566(10) 0.0323(2) Uani 1 d . . . Cl3 Cl 0.23140(14) 0.47661(12) -0.02524(11) 0.0417(3) Uani 1 d . . . O1 O 0.3186(3) 0.3440(3) 0.5573(3) 0.0361(6) Uani 1 d . . . O2 O 0.2439(3) 0.0649(3) 0.1767(3) 0.0401(6) Uani 1 d . . . N1 N 0.2047(4) 0.4330(4) 0.3452(4) 0.0264(6) Uani 1 d . . . N2 N 0.1503(4) 0.3878(4) 0.6424(3) 0.0266(6) Uani 1 d . . . N3 N 0.1754(4) -0.1525(4) 0.0794(4) 0.0287(6) Uani 1 d . . . N4 N 0.0980(4) 0.1478(4) 0.1201(4) 0.0278(6) Uani 1 d . . . C1 C 0.3295(4) 0.3676(4) 0.3999(4) 0.0310(8) Uani 1 d . . . C2 C 0.4945(6) 0.3104(8) 0.3129(7) 0.0511(12) Uani 1 d . . . C3 C 0.2692(4) -0.0936(5) 0.1509(5) 0.0347(8) Uani 1 d . . . C4 C 0.4123(6) -0.1790(8) 0.2143(8) 0.0559(13) Uani 1 d . . . H1N1 H 0.224(6) 0.454(6) 0.268(6) 0.045(15) Uiso 1 d . . . H1N2 H 0.162(5) 0.445(5) 0.721(5) 0.033(11) Uiso 1 d . . . H2N2 H 0.127(5) 0.292(5) 0.675(5) 0.030(10) Uiso 1 d . . . H1N3 H 0.195(6) -0.249(6) 0.062(5) 0.042(12) Uiso 1 d . . . H1N4 H 0.048(4) 0.173(4) 0.196(5) 0.012(9) Uiso 1 d . . . H2N4 H 0.137(6) 0.223(6) 0.070(6) 0.036(12) Uiso 1 d . . . H21 H 0.498(10) 0.213(11) 0.311(11) 0.11(3) Uiso 1 d . . . H22 H 0.559(7) 0.357(7) 0.344(7) 0.070(19) Uiso 1 d . . . H23 H 0.507(10) 0.351(9) 0.215(10) 0.10(3) Uiso 1 d . . . H31 H 0.498(7) -0.140(7) 0.180(7) 0.060(16) Uiso 1 d . . . H32 H 0.450(9) -0.278(10) 0.177(9) 0.11(3) Uiso 1 d . . . H33 H 0.417(10) -0.155(10) 0.309(11) 0.12(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 Rh1 0.0251(2) 0.0216(2) 0.0128(2) 0.00211(14) -0.00456(14) -0.00470(15) Rh2 0.0244(2) 0.0157(2) 0.0217(2) 0.00098(14) -0.00395(15) -0.00469(14) Cl1 0.0358(5) 0.0277(4) 0.0299(5) 0.0030(3) 0.0020(3) -0.0081(3) Cl2 0.0419(5) 0.0291(4) 0.0280(4) -0.0023(3) -0.0039(4) -0.0136(4) Cl3 0.0670(7) 0.0375(5) 0.0251(4) 0.0026(4) -0.0107(4) -0.0194(4) O1 0.0272(13) 0.0489(16) 0.0314(13) 0.0072(11) -0.0095(11) -0.0010(11) O2 0.0357(14) 0.0436(16) 0.0472(16) 0.0011(12) -0.0194(12) -0.0117(12) N1 0.0314(16) 0.0309(16) 0.0174(14) 0.0035(12) -0.0035(12) -0.0080(12) N2 0.0300(15) 0.0313(16) 0.0187(14) 0.0034(13) -0.0074(11) -0.0029(12) N3 0.0289(15) 0.0241(15) 0.0311(16) 0.0044(12) -0.0038(13) -0.0016(12) N4 0.0338(16) 0.0244(15) 0.0253(16) -0.0014(13) -0.0021(14) -0.0083(13) C1 0.0319(18) 0.0294(18) 0.0323(19) 0.0009(14) -0.0041(15) -0.0085(14) C2 0.034(2) 0.061(3) 0.054(3) -0.005(2) 0.001(2) -0.004(2) C3 0.0290(18) 0.041(2) 0.034(2) 0.0095(16) -0.0059(15) -0.0072(16) C4 0.030(2) 0.065(3) 0.075(4) 0.018(3) -0.023(2) -0.007(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 Rh1 N1 2.002(3) . ? Rh1 N1 2.002(3) 2_566 ? Rh1 N2 2.029(3) 2_566 ? Rh1 N2 2.029(3) . ? Rh1 Cl2 2.3270(10) 2_566 ? Rh1 Cl2 2.3270(10) . ? Rh2 N3 2.006(3) 2 ? Rh2 N3 2.006(3) . ? Rh2 N4 2.025(3) 2 ? Rh2 N4 2.025(3) . ? Rh2 Cl1 2.3284(11) 2 ? Rh2 Cl1 2.3284(11) . ? O1 C1 1.353(5) . ? O1 N2 1.476(4) . ? O2 C3 1.350(5) . ? O2 N4 1.472(4) . ? N1 C1 1.271(5) . ? N3 C3 1.264(5) . ? C1 C2 1.476(6) . ? C3 C4 1.489(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_566 ? N1 Rh1 N2 101.70(12) . 2_566 ? N1 Rh1 N2 78.30(12) 2_566 2_566 ? N1 Rh1 N2 78.30(12) . . ? N1 Rh1 N2 101.70(12) 2_566 . ? N2 Rh1 N2 180.0 2_566 . ? N1 Rh1 Cl2 88.70(9) . 2_566 ? N1 Rh1 Cl2 91.30(9) 2_566 2_566 ? N2 Rh1 Cl2 90.56(10) 2_566 2_566 ? N2 Rh1 Cl2 89.44(10) . 2_566 ? N1 Rh1 Cl2 91.30(9) . . ? N1 Rh1 Cl2 88.70(9) 2_566 . ? N2 Rh1 Cl2 89.44(10) 2_566 . ? N2 Rh1 Cl2 90.56(10) . . ? Cl2 Rh1 Cl2 180.0 2_566 . ? N3 Rh2 N3 180.0 2 . ? N3 Rh2 N4 78.51(13) 2 2 ? N3 Rh2 N4 101.49(13) . 2 ? N3 Rh2 N4 101.49(13) 2 . ? N3 Rh2 N4 78.51(13) . . ? N4 Rh2 N4 180.0 2 . ? N3 Rh2 Cl1 92.15(9) 2 2 ? N3 Rh2 Cl1 87.85(9) . 2 ? N4 Rh2 Cl1 90.40(10) 2 2 ? N4 Rh2 Cl1 89.60(10) . 2 ? N3 Rh2 Cl1 87.85(9) 2 . ? N3 Rh2 Cl1 92.15(9) . . ? N4 Rh2 Cl1 89.60(10) 2 . ? N4 Rh2 Cl1 90.40(10) . . ? Cl1 Rh2 Cl1 180.0 2 . ? C1 O1 N2 111.9(3) . . ? C3 O2 N4 112.3(3) . . ? C1 N1 Rh1 117.5(3) . . ? O1 N2 Rh1 112.08(19) . . ? C3 N3 Rh2 117.1(3) . . ? O2 N4 Rh2 111.8(2) . . ? N1 C1 O1 119.5(3) . . ? N1 C1 C2 128.4(4) . . ? O1 C1 C2 112.1(4) . . ? N3 C3 O2 119.7(3) . . ? N3 C3 C4 127.7(4) . . ? O2 C3 C4 112.5(4) . . ? _diffrn_measured_fraction_theta_max 0.827 _diffrn_reflns_theta_full 19.97 _diffrn_measured_fraction_theta_full 0.827 _refine_diff_density_max 1.271 _refine_diff_density_min -1.368 _refine_diff_density_rms 0.125