# Copyright The Royal society of Chemistry, 1998 data_[Rh4(O2CPrn)4Cl4(CH3CN)4] #------------------------------------------------------------------------------ _audit_creation_date 'Thu Jan 22 13:55:07 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1066.04 _chemical_formula_analytical ? _chemical_formula_sum 'C24 H40 Cl4 N4 O8 Rh4 ' _chemical_formula_moiety 'C24 H40 Cl4 N4 O8 Rh4 ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 10.512(2) _cell_length_b 10.5119 _cell_length_c 15.660(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1730.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 193 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.2 _cell_measurement_theta_max 12.4 #------------------------------------------------------------------------------ _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I -4 ' _symmetry_Int_Tables_number 82 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,z y,-x,-z -y,x,-z 1/2+x,1/2+y,1/2+z 1/2-x,1/2-y,1/2+z 1/2+y,1/2-x,1/2-z 1/2-y,1/2+x,1/2-z _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'dark yellow' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 2.046 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1048.00 _exptl_absorpt_coefficient_mu 2.227 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 193 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.41 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 2175 _reflns_number_total 1039 _reflns_number_observed 962 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_av_sigmaI/netI 0.000 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.04701 _diffrn_orient_matrix_UB_12 -0.07111 _diffrn_orient_matrix_UB_13 -0.02834 _diffrn_orient_matrix_UB_21 -0.04513 _diffrn_orient_matrix_UB_22 -0.06275 _diffrn_orient_matrix_UB_23 0.03722 _diffrn_orient_matrix_UB_31 -0.06930 _diffrn_orient_matrix_UB_32 -0.00738 _diffrn_orient_matrix_UB_33 -0.04346 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Rh 0 8 -1.118 0.919 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 16 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 8 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 8 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 48 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 80 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Rh(1) 0.11784(4) 0.47026(5) 0.14529(3) 0.0268(1) Uani d . 1.00 . Cl(1) 0.1901(1) 0.6038(1) 0.2536(1) 0.0329(4) Uani d . 1.00 . O(1) 0.0690(5) 0.3504(5) 0.0491(3) 0.040(1) Uani d . 1.00 . O(2) -0.1407(5) 0.3904(5) 0.0565(3) 0.038(1) Uani d . 1.00 . N(1) 0.3222(6) 0.4087(6) 0.1224(3) 0.038(2) Uani d . 1.00 . C(1) 0.4199(7) 0.3596(7) 0.1151(4) 0.037(2) Uani d . 1.00 . C(2) 0.5405(7) 0.2955(9) 0.1051(6) 0.052(2) Uani d . 1.00 . C(3) -0.0460(7) 0.3326(7) 0.0254(4) 0.035(2) Uani d . 1.00 . C(4) -0.0662(7) 0.2355(8) -0.0443(5) 0.049(2) Uani d . 1.00 . C(5) 0.022(1) 0.241(1) -0.1184(6) 0.075(4) Uani d . 1.00 . C(6) 0.029(2) 0.127(2) -0.1706(9) 0.065(5) Uani d . 0.57 . C(7) -0.016(3) 0.345(3) -0.173(1) 0.085(9) Uani d . 0.43 . H(1) 0.5294 0.2095 0.0858 0.0636 Uiso calc . 1.00 . H(2) 0.5890 0.3375 0.0571 0.0636 Uiso calc . 1.00 . H(3) 0.5904 0.2995 0.1528 0.0636 Uiso calc . 1.00 . H(4) -0.0605 0.1510 -0.0184 0.0557 Uiso calc . 1.00 . H(5) -0.1512 0.2436 -0.0657 0.0557 Uiso calc . 1.00 . H(6) 0.1023 0.2579 -0.0919 0.0887 Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rh(1) 0.0204(2) 0.0285(3) 0.0316(2) 0.0032(2) 0.0005(2) 0.0005(2) Cl(1) 0.0267(7) 0.0323(8) 0.0397(8) -0.0042(6) 0.0025(6) -0.0032(7) O(1) 0.028(3) 0.048(3) 0.043(3) 0.008(2) -0.001(2) -0.013(2) O(2) 0.029(2) 0.045(3) 0.040(3) 0.005(2) -0.005(2) -0.010(2) N(1) 0.034(3) 0.037(3) 0.043(3) 0.001(2) -0.003(2) -0.006(3) C(1) 0.030(4) 0.038(4) 0.042(4) 0.002(3) -0.005(3) -0.007(3) C(2) 0.036(4) 0.057(5) 0.063(5) 0.014(4) -0.003(4) -0.008(4) C(3) 0.025(3) 0.041(4) 0.038(4) 0.001(3) -0.002(3) -0.002(3) C(4) 0.040(4) 0.053(5) 0.054(4) 0.002(3) -0.005(4) -0.029(4) C(5) 0.096(9) 0.079(7) 0.049(6) -0.027(7) 0.015(5) -0.021(5) C(6) 0.055(10) 0.09(1) 0.050(9) -0.004(9) 0.006(7) -0.040(9) C(7) 0.09(2) 0.12(2) 0.05(1) -0.04(2) -0.01(1) 0.02(1) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00003|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 962 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_number_constraints 1 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0234 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0308 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.245 _refine_ls_shift/esd_max 0.2080 _refine_ls_shift/esd_mean 0.0320 _refine_diff_density_min -0.38 _refine_diff_density_max 0.54 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh(1) Rh(1) 2.5552(9) 1_555 2_565 yes Rh(1) Cl(1) 2.330(2) 1_555 1_555 yes Rh(1) Cl(1) 2.317(2) 1_555 7_455 yes Rh(1) O(1) 2.029(5) 1_555 1_555 yes Rh(1) O(2) 2.033(5) 1_555 2_565 yes Rh(1) N(1) 2.272(6) 1_555 1_555 yes O(1) C(3) 1.278(8) 1_555 1_555 yes O(2) C(3) 1.264(8) 1_555 1_555 yes N(1) C(1) 1.155(9) 1_555 1_555 yes C(1) C(2) 1.444(10) 1_555 1_555 yes C(3) C(4) 1.509(10) 1_555 1_555 yes C(4) C(5) 1.49(1) 1_555 1_555 yes C(5) C(6) 1.45(2) 1_555 1_555 yes C(5) C(7) 1.44(3) 1_555 1_555 yes C(2) H(1) 0.96 1_555 1_555 no C(2) H(2) 1.01 1_555 1_555 no C(2) H(3) 0.91 1_555 1_555 no C(4) H(4) 0.98 1_555 1_555 no C(4) H(5) 0.96 1_555 1_555 no C(5) H(6) 0.96 1_555 1_555 no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Rh(1) Rh(1) Cl(1) 99.72(4) 2_565 1_555 1_555 yes Rh(1) Rh(1) Cl(1) 96.69(4) 2_565 1_555 7_455 yes Rh(1) Rh(1) O(1) 84.6(1) 2_565 1_555 1_555 yes Rh(1) Rh(1) O(2) 86.5(1) 2_565 1_555 2_565 yes Rh(1) Rh(1) N(1) 170.6(1) 2_565 1_555 1_555 yes Cl(1) Rh(1) Cl(1) 87.81(3) 1_555 1_555 7_455 yes Cl(1) Rh(1) O(1) 175.6(1) 1_555 1_555 1_555 yes Cl(1) Rh(1) O(2) 91.4(2) 1_555 1_555 2_565 yes Cl(1) Rh(1) N(1) 88.7(1) 1_555 1_555 1_555 yes Cl(1) Rh(1) O(1) 92.2(2) 7_455 1_555 1_555 yes Cl(1) Rh(1) O(2) 176.8(1) 7_455 1_555 2_565 yes Cl(1) Rh(1) N(1) 87.7(2) 7_455 1_555 1_555 yes O(1) Rh(1) O(2) 88.3(2) 1_555 1_555 2_565 yes O(1) Rh(1) N(1) 86.9(2) 1_555 1_555 1_555 yes O(2) Rh(1) N(1) 89.2(2) 2_565 1_555 1_555 yes Rh(1) Cl(1) Rh(1) 107.36(6) 1_555 1_555 8_555 yes Rh(1) O(1) C(3) 123.1(5) 1_555 1_555 1_555 yes Rh(1) O(2) C(3) 121.1(4) 2_565 1_555 1_555 yes Rh(1) N(1) C(1) 169.6(6) 1_555 1_555 1_555 yes N(1) C(1) C(2) 178.6(8) 1_555 1_555 1_555 yes C(1) C(2) H(1) 111.4(7) 1_555 1_555 1_555 no C(1) C(2) H(2) 108.6(8) 1_555 1_555 1_555 no C(1) C(2) H(3) 113.3(8) 1_555 1_555 1_555 no H(1) C(2) H(2) 103.8(8) 1_555 1_555 1_555 no H(1) C(2) H(3) 111.7(9) 1_555 1_555 1_555 no H(2) C(2) H(3) 107.4(8) 1_555 1_555 1_555 no O(1) C(3) O(2) 124.2(7) 1_555 1_555 1_555 yes O(1) C(3) C(4) 116.2(6) 1_555 1_555 1_555 yes O(2) C(3) C(4) 119.6(6) 1_555 1_555 1_555 yes C(3) C(4) C(5) 116.7(7) 1_555 1_555 1_555 yes C(3) C(4) H(4) 107.8(7) 1_555 1_555 1_555 no C(3) C(4) H(5) 108.9(7) 1_555 1_555 1_555 no C(5) C(4) H(4) 108.8(9) 1_555 1_555 1_555 no C(5) C(4) H(5) 107.7(8) 1_555 1_555 1_555 no H(4) C(4) H(5) 106.4(8) 1_555 1_555 1_555 no C(4) C(5) C(6) 115.9(10) 1_555 1_555 1_555 yes C(4) C(5) C(7) 108(1) 1_555 1_555 1_555 yes C(4) C(5) H(6) 102.7(7) 1_555 1_555 1_555 no C(6) C(5) C(7) 107(1) 1_555 1_555 1_555 yes C(6) C(5) H(6) 110(1) 1_555 1_555 1_555 no C(7) C(5) H(6) 111(1) 1_555 1_555 1_555 no #===END data_[Rh4(mhp)4Cl4(PhCN)2] #------------------------------------------------------------------------------ _audit_creation_date 'Fri Jan 23 16:28:59 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1192.16 _chemical_formula_analytical ? _chemical_formula_sum 'C38 H34 Cl4 N6 O4 Rh4 ' _chemical_formula_moiety 'C38 H34 Cl4 N6 O4 Rh4 ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 12.405(4) _cell_length_b 24.119(4) _cell_length_c 14.405(3) _cell_angle_alpha 90 _cell_angle_beta 112.49(2) _cell_angle_gamma 90 _cell_volume 3982(1) _cell_formula_units_Z 4 _cell_measurement_temperature 193 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.2 _cell_measurement_theta_max 12.1 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 1.988 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 2336.00 _exptl_absorpt_coefficient_mu 1.942 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 193 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 3.23 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 4868 _reflns_number_total 4689 _reflns_number_observed 1157 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.119 _diffrn_reflns_av_sigmaI/netI 0.416 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.08399 _diffrn_orient_matrix_UB_12 0.01122 _diffrn_orient_matrix_UB_13 0.02753 _diffrn_orient_matrix_UB_21 0.01615 _diffrn_orient_matrix_UB_22 -0.02754 _diffrn_orient_matrix_UB_23 -0.04496 _diffrn_orient_matrix_UB_31 -0.01722 _diffrn_orient_matrix_UB_32 0.02890 _diffrn_orient_matrix_UB_33 -0.05353 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 152 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 136 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 16 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 24 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 16 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Rh 0 16 -1.118 0.919 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Rh(1) -0.0083(2) 0.19268(8) 0.6169(2) 0.0304(6) Uani d . 1.00 . Rh(2) 0.1331(2) 0.1185(1) 0.7175(2) 0.0468(8) Uani d . 1.00 . Cl(1) 0.0000 0.2516(4) 0.7500 0.036(3) Uani d . 0.50 S Cl(2) -0.1809(5) 0.1569(3) 0.6233(5) 0.037(2) Uani d . 1.00 . Cl(3) 0.0000 0.0616(4) 0.7500 0.071(4) Uani d . 0.50 S O(1) 0.099(2) 0.0800(9) 0.584(1) 0.086(8) Uani d . 1.00 . O(2) 0.258(1) 0.163(1) 0.695(1) 0.077(8) Uani d . 1.00 . N(1) -0.036(2) 0.1431(8) 0.495(2) 0.034(5) Uiso d . 1.00 . N(2) 0.134(2) 0.2328(9) 0.608(2) 0.037(6) Uiso d . 1.00 . N(3) 0.265(2) 0.058(1) 0.785(2) 0.086(10) Uani d . 1.00 . C(1) 0.020(2) 0.095(1) 0.500(2) 0.034(7) Uiso d . 1.00 . C(2) 0.240(3) 0.213(1) 0.653(3) 0.07(1) Uiso d . 1.00 . C(3) 0.002(3) 0.059(1) 0.418(2) 0.059(9) Uiso d . 1.00 . C(4) 0.348(3) 0.240(2) 0.658(3) 0.08(1) Uiso d . 1.00 . C(5) -0.083(3) 0.072(1) 0.331(2) 0.067(9) Uiso d . 1.00 . C(6) 0.327(3) 0.292(1) 0.620(2) 0.070(10) Uiso d . 1.00 . C(7) -0.149(2) 0.122(1) 0.324(2) 0.044(7) Uiso d . 1.00 . C(8) 0.224(3) 0.317(1) 0.572(2) 0.075(10) Uiso d . 1.00 . C(9) -0.126(2) 0.155(1) 0.402(2) 0.046(8) Uiso d . 1.00 . C(10) 0.118(2) 0.287(1) 0.569(2) 0.053(8) Uiso d . 1.00 . C(11) -0.201(2) 0.206(1) 0.392(2) 0.059(9) Uiso d . 1.00 . C(12) 0.000(3) 0.310(1) 0.519(2) 0.077(9) Uiso d . 1.00 . C(13) 0.352(3) 0.037(1) 0.820(2) 0.062(9) Uiso d . 1.00 . C(14) 0.469(3) 0.012(1) 0.866(2) 0.069(10) Uiso d . 1.00 . C(15) 0.564(3) 0.049(2) 0.887(3) 0.09(1) Uiso d . 1.00 . C(16) 0.675(4) 0.028(2) 0.923(3) 0.12(1) Uiso d . 1.00 . C(17) 0.687(3) -0.027(2) 0.934(3) 0.09(1) Uiso d . 1.00 . C(18) 0.599(3) -0.065(2) 0.916(3) 0.10(1) Uiso d . 1.00 . C(19) 0.474(3) -0.045(1) 0.866(3) 0.08(1) Uiso d . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rh(1) 0.027(1) 0.030(1) 0.035(1) -0.001(1) 0.0129(9) -0.001(1) Rh(2) 0.040(1) 0.054(2) 0.033(1) 0.021(1) -0.001(1) -0.011(1) Cl(1) 0.036(5) 0.033(6) 0.047(6) 0.0000 0.023(5) 0.0000 Cl(2) 0.029(4) 0.045(5) 0.033(4) -0.004(3) 0.007(3) 0.005(4) Cl(3) 0.068(8) 0.023(6) 0.089(9) 0.0000 -0.005(7) 0.0000 O(1) 0.09(2) 0.09(2) 0.05(1) 0.07(1) -0.01(1) -0.03(1) O(2) 0.03(1) 0.15(2) 0.05(1) 0.02(1) 0.01(1) -0.02(2) N(3) 0.07(2) 0.11(2) 0.04(2) 0.06(2) -0.02(1) -0.05(2) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00004|Fo|^2^]' _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.00017(6) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1157 _refine_ls_number_parameters 150 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0688 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0697 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.364 _refine_ls_shift/esd_max 0.0190 _refine_ls_shift/esd_mean 0.0030 _refine_diff_density_min -0.84 _refine_diff_density_max 0.96 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh(1) Rh(2) 2.537(3) 1_555 1_555 yes Rh(1) Cl(1) 2.356(6) 1_555 1_555 yes Rh(1) Cl(2) 2.343(7) 1_555 1_555 yes Rh(1) N(1) 2.04(2) 1_555 1_555 yes Rh(1) N(2) 2.06(2) 1_555 1_555 yes Rh(2) Cl(2) 2.329(7) 1_555 2_556 yes Rh(2) Cl(3) 2.328(7) 1_555 1_555 yes Rh(2) O(1) 2.02(2) 1_555 1_555 yes Rh(2) O(2) 2.02(2) 1_555 1_555 yes Rh(2) N(3) 2.13(2) 1_555 1_555 yes O(1) C(1) 1.29(3) 1_555 1_555 yes O(2) C(2) 1.33(3) 1_555 1_555 yes N(1) C(1) 1.34(3) 1_555 1_555 yes N(1) C(9) 1.41(3) 1_555 1_555 yes N(2) C(2) 1.31(4) 1_555 1_555 yes N(2) C(10) 1.40(3) 1_555 1_555 yes N(3) C(13) 1.12(3) 1_555 1_555 yes C(1) C(3) 1.41(3) 1_555 1_555 yes C(2) C(4) 1.47(4) 1_555 1_555 yes C(3) C(5) 1.33(4) 1_555 1_555 yes C(4) C(6) 1.34(4) 1_555 1_555 yes C(5) C(7) 1.43(4) 1_555 1_555 yes C(6) C(8) 1.35(4) 1_555 1_555 yes C(7) C(9) 1.32(3) 1_555 1_555 yes C(8) C(10) 1.49(4) 1_555 1_555 yes C(9) C(11) 1.52(3) 1_555 1_555 yes C(10) C(12) 1.47(4) 1_555 1_555 yes C(13) C(14) 1.48(4) 1_555 1_555 yes C(14) C(15) 1.41(4) 1_555 1_555 yes C(14) C(19) 1.37(4) 1_555 1_555 yes C(15) C(16) 1.36(5) 1_555 1_555 yes C(16) C(17) 1.35(4) 1_555 1_555 yes C(17) C(18) 1.37(4) 1_555 1_555 yes C(18) C(19) 1.52(4) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Rh(2) Rh(1) Cl(1) 98.9(2) 1_555 1_555 1_555 yes Rh(2) Rh(1) Cl(2) 99.2(2) 1_555 1_555 1_555 yes Rh(2) Rh(1) N(1) 86.0(6) 1_555 1_555 1_555 yes Rh(2) Rh(1) N(2) 86.8(6) 1_555 1_555 1_555 yes Cl(1) Rh(1) Cl(2) 86.9(2) 1_555 1_555 1_555 yes Cl(1) Rh(1) N(1) 173.2(5) 1_555 1_555 1_555 yes Cl(1) Rh(1) N(2) 89.8(6) 1_555 1_555 1_555 yes Cl(2) Rh(1) N(1) 87.7(6) 1_555 1_555 1_555 yes Cl(2) Rh(1) N(2) 173.6(6) 1_555 1_555 1_555 yes N(1) Rh(1) N(2) 95.2(8) 1_555 1_555 1_555 yes Rh(1) Rh(2) Cl(2) 98.2(2) 1_555 1_555 2_556 yes Rh(1) Rh(2) Cl(3) 98.2(2) 1_555 1_555 1_555 yes Rh(1) Rh(2) O(1) 86.2(5) 1_555 1_555 1_555 yes Rh(1) Rh(2) O(2) 86.4(6) 1_555 1_555 1_555 yes Rh(1) Rh(2) N(3) 170.8(8) 1_555 1_555 1_555 yes Cl(2) Rh(2) Cl(3) 88.3(2) 2_556 1_555 1_555 yes Cl(2) Rh(2) O(1) 175.6(6) 2_556 1_555 1_555 yes Cl(2) Rh(2) O(2) 91.4(6) 2_556 1_555 1_555 yes Cl(2) Rh(2) N(3) 87.7(6) 2_556 1_555 1_555 yes Cl(3) Rh(2) O(1) 90.7(7) 1_555 1_555 1_555 yes Cl(3) Rh(2) O(2) 175.4(7) 1_555 1_555 1_555 yes Cl(3) Rh(2) N(3) 89.1(9) 1_555 1_555 1_555 yes O(1) Rh(2) O(2) 89.3(9) 1_555 1_555 1_555 yes O(1) Rh(2) N(3) 88.1(7) 1_555 1_555 1_555 yes O(2) Rh(2) N(3) 86(1) 1_555 1_555 1_555 yes Rh(1) Cl(1) Rh(1) 105.9(3) 1_555 1_555 2_556 yes Rh(1) Cl(2) Rh(2) 107.0(2) 1_555 1_555 2_556 yes Rh(2) Cl(3) Rh(2) 107.7(4) 1_555 1_555 2_556 yes Rh(2) O(1) C(1) 125(1) 1_555 1_555 1_555 yes Rh(2) O(2) C(2) 123(2) 1_555 1_555 1_555 yes Rh(1) N(1) C(1) 123(1) 1_555 1_555 1_555 yes Rh(1) N(1) C(9) 121(1) 1_555 1_555 1_555 yes C(1) N(1) C(9) 114(2) 1_555 1_555 1_555 yes Rh(1) N(2) C(2) 121(2) 1_555 1_555 1_555 yes Rh(1) N(2) C(10) 117(1) 1_555 1_555 1_555 yes C(2) N(2) C(10) 119(2) 1_555 1_555 1_555 yes Rh(2) N(3) C(13) 162(3) 1_555 1_555 1_555 yes O(1) C(1) N(1) 118(2) 1_555 1_555 1_555 yes O(1) C(1) C(3) 116(2) 1_555 1_555 1_555 yes N(1) C(1) C(3) 125(2) 1_555 1_555 1_555 yes O(2) C(2) N(2) 121(3) 1_555 1_555 1_555 yes O(2) C(2) C(4) 112(3) 1_555 1_555 1_555 yes N(2) C(2) C(4) 125(3) 1_555 1_555 1_555 yes C(1) C(3) C(5) 118(2) 1_555 1_555 1_555 yes C(2) C(4) C(6) 111(3) 1_555 1_555 1_555 yes C(3) C(5) C(7) 118(2) 1_555 1_555 1_555 yes C(4) C(6) C(8) 129(3) 1_555 1_555 1_555 yes C(5) C(7) C(9) 120(2) 1_555 1_555 1_555 yes C(6) C(8) C(10) 115(3) 1_555 1_555 1_555 yes N(1) C(9) C(7) 122(2) 1_555 1_555 1_555 yes N(1) C(9) C(11) 118(2) 1_555 1_555 1_555 yes C(7) C(9) C(11) 119(2) 1_555 1_555 1_555 yes N(2) C(10) C(8) 117(2) 1_555 1_555 1_555 yes N(2) C(10) C(12) 120(2) 1_555 1_555 1_555 yes C(8) C(10) C(12) 121(2) 1_555 1_555 1_555 yes N(3) C(13) C(14) 177(3) 1_555 1_555 1_555 yes C(13) C(14) C(15) 115(3) 1_555 1_555 1_555 yes C(13) C(14) C(19) 116(3) 1_555 1_555 1_555 yes C(15) C(14) C(19) 127(3) 1_555 1_555 1_555 yes C(14) C(15) C(16) 118(3) 1_555 1_555 1_555 yes C(15) C(16) C(17) 117(4) 1_555 1_555 1_555 yes C(16) C(17) C(18) 125(4) 1_555 1_555 1_555 yes C(17) C(18) C(19) 119(3) 1_555 1_555 1_555 yes C(14) C(19) C(18) 110(3) 1_555 1_555 1_555 yes #===END