#Copyright The Royal Society of Chemistry, 1998 data_JNRHCO2_JN/BTH_19/12/94 #------------------------------------------------------------------------------ _audit_creation_date '1998-01-05' _audit_creation_method 'by teXsan v1.7' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1995)' _computing_structure_solution ? _computing_structure_refinement 'teXsan (MSC, 1995)' _computing_publication_material 'teXsan (MSC, 1995)' #------------------------------------------------------------------------------ _cell_length_a 9.784(6) _cell_length_b 13.59(1) _cell_length_c 7.446(5) _cell_angle_alpha 103.73(5) _cell_angle_beta 93.45(6) _cell_angle_gamma 108.42(7) _cell_volume 902(1) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 18 _cell_measurement_theta_min 3.6 _cell_measurement_theta_max 9.4 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 2.012 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 273.48 _chemical_formula_analytical ? _chemical_formula_sum 'C7 H5 Cl N O2 Rh ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 528.00 _exptl_absorpt_coefficient_mu 2.118 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.742 _exptl_special_details ; The scan width was (1.10+0.30tan\q)\% with an \w scan speed of 4\% per minute (up to 4 scans to achieve I/\s(I) > 6). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -4.60 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 3386 _reflns_number_total 3182 _reflns_number_observed 1768 _reflns_observed_criterion >3.00\s(I) _diffrn_reflns_av_R_equivalents 0.03715 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.01406 _diffrn_orient_matrix_UB_12 -0.07089 _diffrn_orient_matrix_UB_13 -0.04751 _diffrn_orient_matrix_UB_21 -0.10677 _diffrn_orient_matrix_UB_22 -0.03800 _diffrn_orient_matrix_UB_23 -0.00729 _diffrn_orient_matrix_UB_31 -0.01617 _diffrn_orient_matrix_UB_32 0.00455 _diffrn_orient_matrix_UB_33 -0.13123 #------------------------------------------------------------------------------ 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 28 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 20 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 4 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 8 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 4 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Rh 0 4 -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_occupancy _atom_site_refinement_flags _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Rh(1) 0.34260(8) 0.22689(6) 0.9786(1) 0.0467(3) 1.000 . Uani d ? Cl(1) 0.3425(3) 0.3969(2) 1.1444(4) 0.0703(10) 1.000 . Uani d ? O(1) 0.3219(7) 0.0069(6) 0.767(1) 0.068(2) 1.000 . Uani d ? O(2) 0.0272(9) 0.1691(8) 0.861(1) 0.124(4) 1.000 . Uani d ? N(1) 0.5727(7) 0.2772(6) 1.0410(9) 0.043(2) 1.000 . Uiso d ? C(1) 0.334(1) 0.0913(8) 0.846(1) 0.053(3) 1.000 . Uani d ? C(2) 0.148(1) 0.1903(9) 0.913(2) 0.075(4) 1.000 . Uani d ? C(3) 0.6535(10) 0.3769(7) 1.034(1) 0.051(2) 1.000 . Uiso d ? C(4) 0.803(1) 0.4133(8) 1.066(1) 0.059(3) 1.000 . Uiso d ? C(5) 0.871(1) 0.3450(8) 1.106(1) 0.058(3) 1.000 . Uiso d ? C(6) 0.7906(9) 0.2419(7) 1.109(1) 0.047(2) 1.000 . Uiso d ? C(7) 0.6416(9) 0.2121(7) 1.079(1) 0.045(2) 1.000 . Uiso d ? H(1) 0.5993 0.4406 1.0322 0.060 1.000 . Uiso c ? H(2) 0.8810 0.4834 1.0406 0.073 1.000 . Uiso c ? H(3) 0.9776 0.3596 1.0902 0.070 1.000 . Uiso c ? H(4) 0.8504 0.1986 1.1309 0.058 1.000 . Uiso c ? H(5) 0.5724 0.1403 1.0836 0.054 1.000 . Uiso c ? Rh(2) 1.67889(8) 0.81168(6) 1.5770(1) 0.0493(3) 1.000 . Uani d ? Cl(2) 1.6565(3) 0.9755(2) 1.7358(4) 0.0618(9) 1.000 . Uani d ? O(3) 1.7345(10) 0.6137(7) 1.381(1) 0.097(3) 1.000 . Uani d ? O(4) 1.9966(9) 0.9130(8) 1.698(2) 0.159(5) 1.000 . Uani d ? N(2) 1.4511(7) 0.7443(6) 1.4930(10) 0.043(2) 1.000 . Uiso d ? C(8) 1.708(1) 0.6872(9) 1.455(2) 0.068(4) 1.000 . Uani d ? C(9) 1.875(1) 0.875(1) 1.651(2) 0.095(5) 1.000 . Uani d ? C(10) 1.3763(10) 0.8045(7) 1.446(1) 0.047(2) 1.000 . Uiso d ? C(11) 1.230(1) 0.7671(8) 1.395(1) 0.057(3) 1.000 . Uiso d ? C(12) 1.153(1) 0.6631(8) 1.397(1) 0.060(3) 1.000 . Uiso d ? C(13) 1.228(1) 0.5991(8) 1.443(1) 0.059(3) 1.000 . Uiso d ? C(14) 1.3744(10) 0.6419(7) 1.490(1) 0.051(2) 1.000 . Uiso d ? H(6) 1.4310 0.8792 1.4484 0.057 1.000 . Uiso c ? H(7) 1.1803 0.8124 1.3585 0.068 1.000 . Uiso c ? H(8) 1.0472 0.6353 1.3668 0.071 1.000 . Uiso c ? H(9) 1.1749 0.5248 1.4410 0.071 1.000 . Uiso c ? H(10) 1.4270 0.5971 1.5239 0.062 1.000 . Uiso c ? 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) 0.0503(5) 0.0420(5) 0.0552(6) 0.0251(4) 0.0090(4) 0.0140(5) Cl(1) 0.102(2) 0.051(2) 0.077(2) 0.048(2) 0.026(2) 0.019(2) O(1) 0.061(5) 0.051(5) 0.079(5) 0.019(4) 0.007(4) -0.006(4) O(2) 0.058(6) 0.123(8) 0.18(1) 0.043(6) -0.007(6) 0.005(7) C(1) 0.049(6) 0.046(6) 0.064(7) 0.017(5) 0.004(5) 0.012(6) C(2) 0.056(7) 0.086(9) 0.094(9) 0.044(7) 0.008(7) 0.017(7) Rh(2) 0.0493(5) 0.0440(5) 0.0649(6) 0.0246(4) 0.0134(4) 0.0208(5) Cl(2) 0.060(2) 0.044(2) 0.081(2) 0.020(1) 0.006(1) 0.016(1) O(3) 0.123(7) 0.094(7) 0.100(7) 0.077(6) 0.036(6) 0.017(5) O(4) 0.051(6) 0.126(9) 0.28(2) 0.031(6) -0.001(8) 0.014(9) C(8) 0.075(8) 0.068(8) 0.078(8) 0.042(7) 0.025(6) 0.026(7) C(9) 0.070(9) 0.076(9) 0.15(1) 0.042(8) 0.015(9) 0.024(9) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00022|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 1768 _refine_ls_number_parameters 157 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0394 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0393 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.168 _refine_ls_shift/esd_max 0.0188 _refine_ls_shift/esd_mean 0.0000 _refine_diff_density_min -0.54 _refine_diff_density_max 0.52 #------------------------------------------------------------------------------ _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) Cl(1) 2.347(3) . . yes Rh(1) N(1) 2.122(7) . . yes Rh(1) C(1) 1.84(1) . . yes Rh(1) C(2) 1.81(1) . . yes O(1) C(1) 1.12(1) . . yes O(2) C(2) 1.14(1) . . yes N(1) C(3) 1.35(1) . . yes N(1) C(7) 1.34(1) . . yes C(3) C(4) 1.37(1) . . yes C(3) H(1) 1.15 . . no C(4) C(5) 1.38(2) . . yes C(4) H(2) 1.08 . . no C(5) C(6) 1.38(1) . . yes C(5) H(3) 1.01 . . no C(6) C(7) 1.37(1) . . yes C(6) H(4) 0.98 . . no C(7) H(5) 1.01 . . no Rh(2) Cl(2) 2.344(3) . . yes Rh(2) N(2) 2.114(7) . . yes Rh(2) C(8) 1.84(1) . . yes Rh(2) C(9) 1.83(1) . . yes O(3) C(8) 1.13(2) . . yes O(4) C(9) 1.13(2) . . yes N(2) C(10) 1.35(1) . . yes N(2) C(14) 1.35(1) . . yes C(10) C(11) 1.35(1) . . yes C(10) H(6) 0.98 . . no C(11) C(12) 1.38(1) . . yes C(11) H(7) 0.97 . . no C(12) C(13) 1.39(2) . . yes C(12) H(8) 0.97 . . no C(13) C(14) 1.36(1) . . yes C(13) H(9) 0.97 . . no C(14) H(10) 0.98 . . 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 Cl(1) Rh(1) N(1) 91.3(2) . . . yes Cl(1) Rh(1) C(1) 177.5(3) . . . yes Cl(1) Rh(1) C(2) 87.4(4) . . . yes N(1) Rh(1) C(1) 91.2(4) . . . yes N(1) Rh(1) C(2) 175.7(5) . . . yes C(1) Rh(1) C(2) 90.1(5) . . . yes Rh(1) N(1) C(3) 119.0(7) . . . yes Rh(1) N(1) C(7) 122.5(5) . . . yes C(3) N(1) C(7) 118.5(8) . . . yes Rh(1) C(1) O(1) 176.7(9) . . . yes Rh(1) C(2) O(2) 175(1) . . . yes N(1) C(3) C(4) 122(1) . . . yes N(1) C(3) H(1) 120.0 . . . no C(4) C(3) H(1) 116.6 . . . no C(3) C(4) C(5) 118.4(9) . . . yes C(3) C(4) H(2) 130.1 . . . no C(5) C(4) H(2) 110.3 . . . no C(4) C(5) C(6) 120.3(9) . . . yes C(4) C(5) H(3) 119.6 . . . no C(6) C(5) H(3) 117.1 . . . no C(5) C(6) C(7) 117(1) . . . yes C(5) C(6) H(4) 113.6 . . . no C(7) C(6) H(4) 128.5 . . . no N(1) C(7) C(6) 122.8(8) . . . yes N(1) C(7) H(5) 112.6 . . . no C(6) C(7) H(5) 124.6 . . . no Cl(2) Rh(2) N(2) 90.6(2) . . . yes Cl(2) Rh(2) C(8) 176.6(3) . . . yes Cl(2) Rh(2) C(9) 87.2(5) . . . yes N(2) Rh(2) C(8) 92.8(4) . . . yes N(2) Rh(2) C(9) 177.7(5) . . . yes C(8) Rh(2) C(9) 89.4(6) . . . yes Rh(2) N(2) C(10) 120.3(5) . . . yes Rh(2) N(2) C(14) 122.1(7) . . . yes C(10) N(2) C(14) 117.5(7) . . . yes Rh(2) C(8) O(3) 176.1(9) . . . yes Rh(2) C(9) O(4) 178(1) . . . yes N(2) C(10) C(11) 123.3(9) . . . yes N(2) C(10) H(6) 118.1 . . . no C(11) C(10) H(6) 118.6 . . . no C(10) C(11) C(12) 118(1) . . . yes C(10) C(11) H(7) 120.9 . . . no C(12) C(11) H(7) 120.3 . . . no C(11) C(12) C(13) 118.9(9) . . . yes C(11) C(12) H(8) 120.6 . . . no C(13) C(12) H(8) 120.5 . . . no C(12) C(13) C(14) 118.9(9) . . . yes C(12) C(13) H(9) 120.0 . . . no C(14) C(13) H(9) 121.1 . . . no N(2) C(14) C(13) 122(1) . . . yes N(2) C(14) H(10) 118.5 . . . no C(13) C(14) H(10) 118.9 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? # -- ENTER NON-BONDED CONTACTS HERE, ONE PER LINE -- # e.g. O1 N1 2.841(1) . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Rh(1) N(1) C(3) C(4) . . . . -177.8(7) no Rh(1) N(1) C(7) C(6) . . . . 176.1(6) no Cl(1) Rh(1) N(1) C(3) . . . . -41.0(6) no Cl(1) Rh(1) N(1) C(7) . . . . 142.2(6) no Cl(1) Rh(1) C(1) O(1) . . . . -26(25) no Cl(1) Rh(1) C(2) O(2) . . . . 95(13) no O(1) C(1) Rh(1) N(1) . . . . 153(18) no O(1) C(1) Rh(1) C(2) . . . . -30(18) no O(2) C(2) Rh(1) N(1) . . . . 23(18) no O(2) C(2) Rh(1) C(1) . . . . -84(13) no N(1) C(3) C(4) C(5) . . . . 0(1) no N(1) C(7) C(6) C(5) . . . . 2(1) no C(1) Rh(1) N(1) C(3) . . . . 139.0(7) no C(1) Rh(1) N(1) C(7) . . . . -37.8(7) no C(2) Rh(1) N(1) C(3) . . . . 31(5) no C(2) Rh(1) N(1) C(7) . . . . -145(5) no C(3) N(1) C(7) C(6) . . . . 0(1) no C(3) C(4) C(5) C(6) . . . . 1(1) no C(4) C(3) N(1) C(7) . . . . 0(1) no C(4) C(5) C(6) C(7) . . . . -2(1) no Rh(2) N(2) C(10) C(11) . . . . -178.5(7) no Rh(2) N(2) C(14) C(13) . . . . 177.6(7) no Cl(2) Rh(2) N(2) C(10) . . . . 37.5(6) no Cl(2) Rh(2) N(2) C(14) . . . . -140.0(7) no Cl(2) Rh(2) C(8) O(3) . . . . -9(22) no Cl(2) Rh(2) C(9) O(4) . . . . 134(59) no O(3) C(8) Rh(2) N(2) . . . . 162(16) no O(3) C(8) Rh(2) C(9) . . . . -16(16) no O(4) C(9) Rh(2) N(2) . . . . 154(50) no O(4) C(9) Rh(2) C(8) . . . . -45(59) no N(2) C(10) C(11) C(12) . . . . 2(1) no N(2) C(14) C(13) C(12) . . . . 0(1) no C(8) Rh(2) N(2) C(10) . . . . -142.1(7) no C(8) Rh(2) N(2) C(14) . . . . 40.4(8) no C(9) Rh(2) N(2) C(10) . . . . 18(13) no C(9) Rh(2) N(2) C(14) . . . . -159(13) no C(10) N(2) C(14) C(13) . . . . 0(1) no C(10) C(11) C(12) C(13) . . . . -2(1) no C(11) C(10) N(2) C(14) . . . . 0(1) no C(11) C(12) C(13) C(14) . . . . 1(1) no #------------------------------------------------------------------------------ #=END data_JNRHPY #------------------------------------------------------------------------------ _audit_creation_date '1998-01-05' _audit_creation_method 'by teXsan v1.7' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garcia-Granda, S., Gould, R.O., Smits, J.M.M. and Smykalla, C. (1992). The DIRDIF program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1995)' _computing_structure_solution ; 'DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan (MSC, 1995)' _computing_publication_material 'teXsan (MSC, 1995)' #------------------------------------------------------------------------------ _cell_length_a 11.023(1) _cell_length_b 13.395(1) _cell_length_c 9.012(3) _cell_angle_alpha 91.89(2) _cell_angle_beta 94.05(2) _cell_angle_gamma 71.570(8) _cell_volume 1259.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 153.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.1 _cell_measurement_theta_max 22.1 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.786 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 677.15 _chemical_formula_analytical ? _chemical_formula_sum 'C23 H20 Cl2 N4 O3 Rh2 ' _chemical_formula_moiety 'C23 H20 Cl2 N4 O3 Rh2 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 668.00 _exptl_absorpt_coefficient_mu 1.536 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.883 _exptl_special_details ; The scan width was (0.89+0.30tan\q)\% with an \w scan speed of 4\% per minute (up to 4 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 153.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC6S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.30 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 4661 _reflns_number_total 4409 _reflns_number_observed 3765 _reflns_observed_criterion >3.00\s(I) _diffrn_reflns_av_R_equivalents 0.01278 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 24.96 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.06150 _diffrn_orient_matrix_UB_12 0.07223 _diffrn_orient_matrix_UB_13 0.01364 _diffrn_orient_matrix_UB_21 0.07334 _diffrn_orient_matrix_UB_22 0.02893 _diffrn_orient_matrix_UB_23 0.01388 _diffrn_orient_matrix_UB_31 -0.00455 _diffrn_orient_matrix_UB_32 0.01176 _diffrn_orient_matrix_UB_33 -0.10953 #------------------------------------------------------------------------------ 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 46 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 40 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 8 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 4 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Rh 0 4 -1.118 0.919 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 6 0.011 0.006 ;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_occupancy _atom_site_refinement_flags _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Rh(1) 0.11613(2) 0.24310(2) 0.13094(2) 0.01754(6) 1.000 . Uani d ? Rh(2) 0.34132(2) 0.25776(2) 0.18744(2) 0.01722(6) 1.000 . Uani d ? Cl(1) 0.05884(8) 0.09088(6) 0.21162(9) 0.0305(2) 1.000 . Uani d ? Cl(2) 0.37344(8) 0.41333(6) 0.31863(9) 0.0270(2) 1.000 . Uani d ? O(1) 0.1963(2) 0.2557(2) 0.4549(2) 0.0287(6) 1.000 . Uani d ? O(2) 0.3287(2) 0.0761(2) -0.0062(3) 0.0310(6) 1.000 . Uani d ? O(3) 0.1596(2) 0.4324(2) 0.0062(3) 0.0284(6) 1.000 . Uani d ? N(1) -0.0624(2) 0.3497(2) 0.2098(3) 0.0221(7) 1.000 . Uani d ? N(2) 0.0247(2) 0.2371(2) -0.0925(3) 0.0210(7) 1.000 . Uani d ? N(3) 0.4776(2) 0.2655(2) 0.0265(3) 0.0214(7) 1.000 . Uani d ? N(4) 0.4992(2) 0.1434(2) 0.3200(3) 0.0225(7) 1.000 . Uani d ? C(1) -0.0665(3) 0.4383(2) 0.2869(4) 0.0273(9) 1.000 . Uani d ? C(2) -0.1762(4) 0.4997(3) 0.3514(4) 0.039(1) 1.000 . Uani d ? C(3) -0.2857(4) 0.4706(3) 0.3338(4) 0.044(1) 1.000 . Uani d ? C(4) -0.2828(3) 0.3815(3) 0.2530(4) 0.042(1) 1.000 . Uani d ? C(5) -0.1705(3) 0.3233(3) 0.1924(4) 0.0306(9) 1.000 . Uani d ? C(6) 0.0380(3) 0.1448(2) -0.1632(4) 0.0257(8) 1.000 . Uani d ? C(7) 0.0012(3) 0.1388(3) -0.3127(4) 0.0283(9) 1.000 . Uani d ? C(8) -0.0515(3) 0.2311(3) -0.3921(4) 0.0305(9) 1.000 . Uani d ? C(9) -0.0702(3) 0.3260(3) -0.3179(4) 0.0306(9) 1.000 . Uani d ? C(10) -0.0305(3) 0.3262(2) -0.1696(4) 0.0253(8) 1.000 . Uani d ? C(11) 0.5734(3) 0.1777(3) -0.0083(4) 0.0293(9) 1.000 . Uani d ? C(12) 0.6657(4) 0.1797(3) -0.1028(4) 0.038(1) 1.000 . Uani d ? C(13) 0.6600(4) 0.2743(3) -0.1638(4) 0.041(1) 1.000 . Uani d ? C(14) 0.5623(4) 0.3637(3) -0.1300(4) 0.0337(10) 1.000 . Uani d ? C(15) 0.4726(3) 0.3563(3) -0.0342(4) 0.0269(9) 1.000 . Uani d ? C(16) 0.5749(3) 0.1770(3) 0.4183(4) 0.0350(10) 1.000 . Uani d ? C(17) 0.6791(4) 0.1082(3) 0.4964(4) 0.044(1) 1.000 . Uani d ? C(18) 0.7059(3) 0.0013(3) 0.4742(4) 0.0370(10) 1.000 . Uani d ? C(19) 0.6284(4) -0.0337(3) 0.3747(4) 0.038(1) 1.000 . Uani d ? C(20) 0.5265(3) 0.0389(3) 0.2993(4) 0.0309(9) 1.000 . Uani d ? C(21) 0.2107(3) 0.2519(2) 0.3289(3) 0.0208(8) 1.000 . Uani d ? C(22) 0.2859(3) 0.1500(2) 0.0679(3) 0.0223(8) 1.000 . Uani d ? C(23) 0.1880(3) 0.3545(2) 0.0726(3) 0.0213(8) 1.000 . Uani d ? H(1) 0.0083 0.4703 0.2980 0.033 1.000 . Uiso c ? H(2) -0.1888 0.5745 0.4058 0.047 1.000 . Uiso c ? H(3) -0.3595 0.5156 0.3934 0.052 1.000 . Uiso c ? H(4) -0.3620 0.3554 0.2253 0.050 1.000 . Uiso c ? H(5) -0.1648 0.2574 0.1265 0.037 1.000 . Uiso c ? H(6) 0.0653 0.0839 -0.1053 0.030 1.000 . Uiso c ? H(7) 0.0097 0.0731 -0.3637 0.034 1.000 . Uiso c ? H(8) -0.0806 0.2262 -0.5063 0.037 1.000 . Uiso c ? H(9) -0.1126 0.3890 -0.3690 0.036 1.000 . Uiso c ? H(10) -0.0468 0.3915 -0.1084 0.032 1.000 . Uiso c ? H(11) 0.5802 0.1038 0.0418 0.035 1.000 . Uiso c ? H(12) 0.7348 0.1159 -0.1215 0.045 1.000 . Uiso c ? H(13) 0.7256 0.2766 -0.2302 0.047 1.000 . Uiso c ? H(14) 0.5592 0.4366 -0.1797 0.040 1.000 . Uiso c ? H(15) 0.4070 0.4193 -0.0009 0.031 1.000 . Uiso c ? H(16) 0.5560 0.2601 0.4316 0.043 1.000 . Uiso c ? H(17) 0.7220 0.1406 0.5845 0.052 1.000 . Uiso c ? H(18) 0.7777 -0.0480 0.5279 0.043 1.000 . Uiso c ? H(19) 0.6397 -0.1137 0.3563 0.045 1.000 . Uiso c ? H(20) 0.4602 0.0122 0.2229 0.037 1.000 . Uiso c ? 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) 0.0181(1) 0.0153(1) 0.0186(1) -0.0044(1) 0.00053(9) 0.00143(9) Rh(2) 0.0176(1) 0.0149(1) 0.0184(1) -0.00374(9) 0.00202(9) 0.00053(9) Cl(1) 0.0383(5) 0.0250(4) 0.0326(4) -0.0165(4) -0.0020(4) 0.0081(3) Cl(2) 0.0325(4) 0.0218(4) 0.0290(4) -0.0114(3) 0.0065(3) -0.0054(3) O(1) 0.031(1) 0.037(1) 0.018(1) -0.011(1) 0.0044(10) 0.0027(10) O(2) 0.031(1) 0.022(1) 0.034(1) -0.001(1) 0.001(1) -0.009(1) O(3) 0.028(1) 0.020(1) 0.036(1) -0.0048(10) -0.001(1) 0.008(1) N(1) 0.020(1) 0.024(1) 0.020(1) -0.003(1) 0.002(1) 0.003(1) N(2) 0.019(1) 0.021(1) 0.023(1) -0.006(1) 0.001(1) 0.001(1) N(3) 0.023(1) 0.020(1) 0.022(1) -0.008(1) 0.005(1) -0.001(1) N(4) 0.020(1) 0.023(1) 0.022(1) -0.003(1) 0.000(1) 0.004(1) C(1) 0.035(2) 0.021(2) 0.022(2) -0.003(1) 0.001(1) 0.003(1) C(2) 0.046(2) 0.036(2) 0.024(2) 0.003(2) 0.000(2) 0.000(2) C(3) 0.031(2) 0.061(3) 0.023(2) 0.009(2) 0.006(2) 0.001(2) C(4) 0.026(2) 0.064(3) 0.031(2) -0.008(2) 0.002(2) 0.004(2) C(5) 0.025(2) 0.040(2) 0.025(2) -0.008(2) 0.000(1) 0.000(1) C(6) 0.026(2) 0.023(2) 0.029(2) -0.009(1) -0.001(1) 0.002(1) C(7) 0.028(2) 0.031(2) 0.027(2) -0.012(1) 0.003(1) -0.008(1) C(8) 0.031(2) 0.048(2) 0.020(2) -0.023(2) 0.003(1) 0.002(1) C(9) 0.035(2) 0.032(2) 0.027(2) -0.015(2) -0.006(1) 0.011(1) C(10) 0.025(2) 0.023(2) 0.027(2) -0.008(1) -0.002(1) 0.004(1) C(11) 0.030(2) 0.024(2) 0.033(2) -0.006(1) 0.008(1) -0.001(1) C(12) 0.033(2) 0.035(2) 0.042(2) -0.003(2) 0.017(2) -0.006(2) C(13) 0.038(2) 0.046(2) 0.044(2) -0.019(2) 0.019(2) -0.005(2) C(14) 0.039(2) 0.037(2) 0.032(2) -0.020(2) 0.006(2) 0.003(2) C(15) 0.028(2) 0.026(2) 0.028(2) -0.010(1) 0.005(1) 0.001(1) C(16) 0.035(2) 0.031(2) 0.038(2) -0.011(2) -0.009(2) 0.004(2) C(17) 0.039(2) 0.051(2) 0.042(2) -0.016(2) -0.012(2) 0.008(2) C(18) 0.028(2) 0.043(2) 0.032(2) 0.001(2) -0.002(2) 0.012(2) C(19) 0.043(2) 0.029(2) 0.033(2) 0.000(2) 0.000(2) 0.008(2) C(20) 0.035(2) 0.027(2) 0.026(2) -0.003(1) -0.003(1) 0.002(1) C(21) 0.021(2) 0.014(1) 0.027(2) -0.004(1) 0.001(1) 0.001(1) C(22) 0.024(2) 0.021(2) 0.021(2) -0.006(1) -0.001(1) 0.004(1) C(23) 0.021(2) 0.021(2) 0.021(2) -0.004(1) 0.005(1) -0.002(1) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00022|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 3765 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0216 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0281 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.255 _refine_ls_shift/esd_max 0.0191 _refine_ls_shift/esd_mean 0.0000 _refine_diff_density_min -0.42 _refine_diff_density_max 0.37 #------------------------------------------------------------------------------ _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) 2.5657(5) . . yes Rh(1) Cl(1) 2.462(1) . . yes Rh(1) N(1) 2.184(2) . . yes Rh(1) N(2) 2.198(2) . . yes Rh(1) C(21) 2.021(3) . . yes Rh(1) C(22) 2.002(3) . . yes Rh(1) C(23) 1.997(4) . . yes Rh(2) Cl(2) 2.4719(9) . . yes Rh(2) N(3) 2.188(3) . . yes Rh(2) N(4) 2.223(2) . . yes Rh(2) C(21) 2.011(3) . . yes Rh(2) C(22) 1.995(3) . . yes Rh(2) C(23) 2.016(3) . . yes O(1) C(21) 1.155(4) . . yes O(2) C(22) 1.164(4) . . yes O(3) C(23) 1.164(4) . . yes N(1) C(1) 1.345(4) . . yes N(1) C(5) 1.344(5) . . yes N(2) C(6) 1.343(4) . . yes N(2) C(10) 1.347(4) . . yes N(3) C(11) 1.354(4) . . yes N(3) C(15) 1.334(4) . . yes N(4) C(16) 1.339(5) . . yes N(4) C(20) 1.345(4) . . yes C(1) C(2) 1.384(5) . . yes C(1) H(1) 1.04 . . no C(2) C(3) 1.379(6) . . yes C(2) H(2) 1.07 . . no C(3) C(4) 1.370(6) . . yes C(3) H(3) 1.02 . . no C(4) C(5) 1.377(5) . . yes C(4) H(4) 1.05 . . no C(5) H(5) 1.03 . . no C(6) C(7) 1.386(4) . . yes C(6) H(6) 0.94 . . no C(7) C(8) 1.387(5) . . yes C(7) H(7) 0.96 . . no C(8) C(9) 1.380(5) . . yes C(8) H(8) 1.06 . . no C(9) C(10) 1.376(4) . . yes C(9) H(9) 0.94 . . no C(10) H(10) 0.99 . . no C(11) C(12) 1.380(6) . . yes C(11) H(11) 1.08 . . no C(12) C(13) 1.380(6) . . yes C(12) H(12) 0.97 . . no C(13) C(14) 1.375(5) . . yes C(13) H(13) 0.98 . . no C(14) C(15) 1.386(5) . . yes C(14) H(14) 1.08 . . no C(15) H(15) 0.98 . . no C(16) C(17) 1.387(5) . . yes C(16) H(16) 1.07 . . no C(17) C(18) 1.377(6) . . yes C(17) H(17) 1.05 . . no C(18) C(19) 1.368(6) . . yes C(18) H(18) 0.97 . . no C(19) C(20) 1.383(4) . . yes C(19) H(19) 1.05 . . no C(20) H(20) 1.10 . . 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(2) Rh(1) Cl(1) 121.62(2) . . . yes Rh(2) Rh(1) N(1) 126.41(8) . . . yes Rh(2) Rh(1) N(2) 125.39(7) . . . yes Rh(2) Rh(1) C(21) 50.31(10) . . . yes Rh(2) Rh(1) C(22) 49.94(10) . . . yes Rh(2) Rh(1) C(23) 50.58(8) . . . yes Cl(1) Rh(1) N(1) 90.24(8) . . . yes Cl(1) Rh(1) N(2) 91.79(8) . . . yes Cl(1) Rh(1) C(21) 91.75(10) . . . yes Cl(1) Rh(1) C(22) 91.6(1) . . . yes Cl(1) Rh(1) C(23) 171.97(8) . . . yes N(1) Rh(1) N(2) 91.19(9) . . . yes N(1) Rh(1) C(21) 91.4(1) . . . yes N(1) Rh(1) C(22) 176.3(1) . . . yes N(1) Rh(1) C(23) 96.5(1) . . . yes N(2) Rh(1) C(21) 175.6(1) . . . yes N(2) Rh(1) C(22) 92.0(1) . . . yes N(2) Rh(1) C(23) 92.4(1) . . . yes C(21) Rh(1) C(22) 85.3(1) . . . yes C(21) Rh(1) C(23) 83.8(1) . . . yes C(22) Rh(1) C(23) 81.4(1) . . . yes Rh(1) Rh(2) Cl(2) 121.19(2) . . . yes Rh(1) Rh(2) N(3) 127.18(7) . . . yes Rh(1) Rh(2) N(4) 125.07(8) . . . yes Rh(1) Rh(2) C(21) 50.65(9) . . . yes Rh(1) Rh(2) C(22) 50.18(8) . . . yes Rh(1) Rh(2) C(23) 49.9(1) . . . yes Cl(2) Rh(2) N(3) 89.58(7) . . . yes Cl(2) Rh(2) N(4) 94.04(7) . . . yes Cl(2) Rh(2) C(21) 91.39(9) . . . yes Cl(2) Rh(2) C(22) 169.83(8) . . . yes Cl(2) Rh(2) C(23) 88.89(9) . . . yes N(3) Rh(2) N(4) 89.70(9) . . . yes N(3) Rh(2) C(21) 177.8(1) . . . yes N(3) Rh(2) C(22) 92.9(1) . . . yes N(3) Rh(2) C(23) 94.4(1) . . . yes N(4) Rh(2) C(21) 92.2(1) . . . yes N(4) Rh(2) C(22) 95.8(1) . . . yes N(4) Rh(2) C(23) 175.0(1) . . . yes C(21) Rh(2) C(22) 85.8(1) . . . yes C(21) Rh(2) C(23) 83.6(1) . . . yes C(22) Rh(2) C(23) 81.1(1) . . . yes Rh(1) N(1) C(1) 122.0(2) . . . yes Rh(1) N(1) C(5) 119.9(2) . . . yes C(1) N(1) C(5) 117.9(3) . . . yes Rh(1) N(2) C(6) 120.9(2) . . . yes Rh(1) N(2) C(10) 120.3(2) . . . yes C(6) N(2) C(10) 118.1(3) . . . yes Rh(2) N(3) C(11) 120.0(2) . . . yes Rh(2) N(3) C(15) 121.5(2) . . . yes C(11) N(3) C(15) 118.5(3) . . . yes Rh(2) N(4) C(16) 120.6(2) . . . yes Rh(2) N(4) C(20) 121.8(2) . . . yes C(16) N(4) C(20) 117.6(3) . . . yes N(1) C(1) C(2) 122.1(4) . . . yes N(1) C(1) H(1) 124.4 . . . no C(2) C(1) H(1) 113.4 . . . no C(1) C(2) C(3) 119.2(4) . . . yes C(1) C(2) H(2) 125.9 . . . no C(3) C(2) H(2) 114.5 . . . no C(2) C(3) C(4) 119.0(3) . . . yes C(2) C(3) H(3) 114.3 . . . no C(4) C(3) H(3) 126.4 . . . no C(3) C(4) C(5) 119.1(4) . . . yes C(3) C(4) H(4) 125.5 . . . no C(5) C(4) H(4) 115.3 . . . no N(1) C(5) C(4) 122.7(3) . . . yes N(1) C(5) H(5) 115.3 . . . no C(4) C(5) H(5) 121.9 . . . no N(2) C(6) C(7) 122.2(3) . . . yes N(2) C(6) H(6) 117.3 . . . no C(7) C(6) H(6) 120.3 . . . no C(6) C(7) C(8) 119.1(3) . . . yes C(6) C(7) H(7) 122.6 . . . no C(8) C(7) H(7) 118.3 . . . no C(7) C(8) C(9) 118.7(3) . . . yes C(7) C(8) H(8) 118.9 . . . no C(9) C(8) H(8) 122.4 . . . no C(8) C(9) C(10) 119.1(3) . . . yes C(8) C(9) H(9) 119.2 . . . no C(10) C(9) H(9) 121.6 . . . no N(2) C(10) C(9) 122.7(3) . . . yes N(2) C(10) H(10) 114.1 . . . no C(9) C(10) H(10) 122.9 . . . no N(3) C(11) C(12) 122.1(3) . . . yes N(3) C(11) H(11) 119.4 . . . no C(12) C(11) H(11) 118.4 . . . no C(11) C(12) C(13) 118.9(3) . . . yes C(11) C(12) H(12) 119.6 . . . no C(13) C(12) H(12) 121.5 . . . no C(12) C(13) C(14) 119.3(4) . . . yes C(12) C(13) H(13) 119.4 . . . no C(14) C(13) H(13) 121.3 . . . no C(13) C(14) C(15) 119.0(4) . . . yes C(13) C(14) H(14) 118.1 . . . no C(15) C(14) H(14) 122.9 . . . no N(3) C(15) C(14) 122.3(3) . . . yes N(3) C(15) H(15) 116.7 . . . no C(14) C(15) H(15) 120.8 . . . no N(4) C(16) C(17) 122.3(3) . . . yes N(4) C(16) H(16) 117.8 . . . no C(17) C(16) H(16) 119.8 . . . no C(16) C(17) C(18) 119.5(4) . . . yes C(16) C(17) H(17) 116.5 . . . no C(18) C(17) H(17) 122.9 . . . no C(17) C(18) C(19) 118.6(3) . . . yes C(17) C(18) H(18) 120.8 . . . no C(19) C(18) H(18) 120.6 . . . no C(18) C(19) C(20) 119.2(3) . . . yes C(18) C(19) H(19) 122.9 . . . no C(20) C(19) H(19) 117.8 . . . no N(4) C(20) C(19) 122.9(3) . . . yes N(4) C(20) H(20) 116.8 . . . no C(19) C(20) H(20) 120.2 . . . no Rh(1) C(21) Rh(2) 79.0(1) . . . yes Rh(1) C(21) O(1) 140.7(3) . . . yes Rh(2) C(21) O(1) 140.1(3) . . . yes Rh(1) C(22) Rh(2) 79.9(1) . . . yes Rh(1) C(22) O(2) 140.0(3) . . . yes Rh(2) C(22) O(2) 139.9(3) . . . yes Rh(1) C(23) Rh(2) 79.5(1) . . . yes Rh(1) C(23) O(3) 141.1(3) . . . yes Rh(2) C(23) O(3) 139.4(3) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? # -- ENTER NON-BONDED CONTACTS HERE, ONE PER LINE -- # e.g. O1 N1 2.841(1) . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Rh(1) Rh(2) N(3) C(11) . . . . -98.7(2) no Rh(1) Rh(2) N(3) C(15) . . . . 84.5(3) no Rh(1) Rh(2) N(4) C(16) . . . . -138.6(2) no Rh(1) Rh(2) N(4) C(20) . . . . 45.0(3) no Rh(1) Rh(2) C(21) O(1) . . . . -177.3(4) no Rh(1) Rh(2) C(22) O(2) . . . . 175.9(4) no Rh(1) Rh(2) C(23) O(3) . . . . -178.8(4) no Rh(1) N(1) C(1) C(2) . . . . -172.5(2) no Rh(1) N(1) C(5) C(4) . . . . 173.1(3) no Rh(1) N(2) C(6) C(7) . . . . -168.4(3) no Rh(1) N(2) C(10) C(9) . . . . 169.0(3) no Rh(1) C(21) Rh(2) Cl(2) . . . . 130.54(7) no Rh(1) C(21) Rh(2) N(3) . . . . 14(2) no Rh(1) C(21) Rh(2) N(4) . . . . -135.36(9) no Rh(1) C(21) Rh(2) C(22) . . . . -39.69(10) no Rh(1) C(21) Rh(2) C(23) . . . . 41.8(1) no Rh(1) C(22) Rh(2) Cl(2) . . . . -34.0(6) no Rh(1) C(22) Rh(2) N(3) . . . . -138.17(9) no Rh(1) C(22) Rh(2) N(4) . . . . 131.84(10) no Rh(1) C(22) Rh(2) C(21) . . . . 40.0(1) no Rh(1) C(22) Rh(2) C(23) . . . . -44.1(1) no Rh(1) C(23) Rh(2) Cl(2) . . . . -133.88(7) no Rh(1) C(23) Rh(2) N(3) . . . . 136.63(10) no Rh(1) C(23) Rh(2) N(4) . . . . -8(1) no Rh(1) C(23) Rh(2) C(21) . . . . -42.4(1) no Rh(1) C(23) Rh(2) C(22) . . . . 44.3(1) no Rh(2) Rh(1) N(1) C(1) . . . . 5.5(3) no Rh(2) Rh(1) N(1) C(5) . . . . -168.9(2) no Rh(2) Rh(1) N(2) C(6) . . . . 90.2(3) no Rh(2) Rh(1) N(2) C(10) . . . . -80.4(2) no Rh(2) Rh(1) C(21) O(1) . . . . 177.2(4) no Rh(2) Rh(1) C(22) O(2) . . . . -175.9(5) no Rh(2) Rh(1) C(23) O(3) . . . . 178.7(4) no Rh(2) N(3) C(11) C(12) . . . . -176.4(3) no Rh(2) N(3) C(15) C(14) . . . . 176.4(3) no Rh(2) N(4) C(16) C(17) . . . . -176.0(3) no Rh(2) N(4) C(20) C(19) . . . . 176.5(3) no Rh(2) C(21) Rh(1) Cl(1) . . . . 131.02(7) no Rh(2) C(21) Rh(1) N(1) . . . . -138.7(1) no Rh(2) C(21) Rh(1) N(2) . . . . -12(1) no Rh(2) C(21) Rh(1) C(22) . . . . 39.5(1) no Rh(2) C(21) Rh(1) C(23) . . . . -42.28(10) no Rh(2) C(22) Rh(1) Cl(1) . . . . -131.43(8) no Rh(2) C(22) Rh(1) N(1) . . . . -11(1) no Rh(2) C(22) Rh(1) N(2) . . . . 136.7(1) no Rh(2) C(22) Rh(1) C(21) . . . . -39.8(1) no Rh(2) C(22) Rh(1) C(23) . . . . 44.6(1) no Rh(2) C(23) Rh(1) Cl(1) . . . . -14.5(7) no Rh(2) C(23) Rh(1) N(1) . . . . 132.79(9) no Rh(2) C(23) Rh(1) N(2) . . . . -135.74(9) no Rh(2) C(23) Rh(1) C(21) . . . . 42.08(10) no Rh(2) C(23) Rh(1) C(22) . . . . -44.1(1) no Cl(1) Rh(1) Rh(2) Cl(2) . . . . -124.96(3) no Cl(1) Rh(1) Rh(2) N(3) . . . . 118.39(8) no Cl(1) Rh(1) Rh(2) N(4) . . . . -3.24(8) no Cl(1) Rh(1) Rh(2) C(21) . . . . -62.3(1) no Cl(1) Rh(1) Rh(2) C(22) . . . . 61.7(1) no Cl(1) Rh(1) Rh(2) C(23) . . . . 177.6(1) no Cl(1) Rh(1) N(1) C(1) . . . . 136.4(2) no Cl(1) Rh(1) N(1) C(5) . . . . -38.1(2) no Cl(1) Rh(1) N(2) C(6) . . . . -41.6(3) no Cl(1) Rh(1) N(2) C(10) . . . . 147.9(2) no Cl(1) Rh(1) C(21) O(1) . . . . -51.7(4) no Cl(1) Rh(1) C(22) O(2) . . . . 52.7(4) no Cl(1) Rh(1) C(23) O(3) . . . . 164.2(4) no Cl(2) Rh(2) Rh(1) N(1) . . . . -7.55(9) no Cl(2) Rh(2) Rh(1) N(2) . . . . 116.19(8) no Cl(2) Rh(2) Rh(1) C(21) . . . . -62.6(1) no Cl(2) Rh(2) Rh(1) C(22) . . . . 173.4(1) no Cl(2) Rh(2) Rh(1) C(23) . . . . 57.4(1) no Cl(2) Rh(2) N(3) C(11) . . . . 131.2(2) no Cl(2) Rh(2) N(3) C(15) . . . . -45.6(2) no Cl(2) Rh(2) N(4) C(16) . . . . -5.4(3) no Cl(2) Rh(2) N(4) C(20) . . . . 178.2(3) no Cl(2) Rh(2) C(21) O(1) . . . . -46.7(3) no Cl(2) Rh(2) C(22) O(2) . . . . 141.9(4) no Cl(2) Rh(2) C(23) O(3) . . . . 47.3(4) no O(1) C(21) Rh(1) N(1) . . . . 38.6(4) no O(1) C(21) Rh(1) N(2) . . . . 164(1) no O(1) C(21) Rh(1) C(22) . . . . -143.2(4) no O(1) C(21) Rh(1) C(23) . . . . 135.0(4) no O(1) C(21) Rh(2) N(3) . . . . -162(2) no O(1) C(21) Rh(2) N(4) . . . . 47.4(4) no O(1) C(21) Rh(2) C(22) . . . . 143.0(4) no O(1) C(21) Rh(2) C(23) . . . . -135.5(4) no O(2) C(22) Rh(1) N(1) . . . . 172(1) no O(2) C(22) Rh(1) N(2) . . . . -39.2(4) no O(2) C(22) Rh(1) C(21) . . . . 144.3(4) no O(2) C(22) Rh(1) C(23) . . . . -131.3(4) no O(2) C(22) Rh(2) N(3) . . . . 37.7(4) no O(2) C(22) Rh(2) N(4) . . . . -52.3(4) no O(2) C(22) Rh(2) C(21) . . . . -144.1(4) no O(2) C(22) Rh(2) C(23) . . . . 131.8(4) no O(3) C(23) Rh(1) N(1) . . . . -48.5(4) no O(3) C(23) Rh(1) N(2) . . . . 43.0(4) no O(3) C(23) Rh(1) C(21) . . . . -139.2(4) no O(3) C(23) Rh(1) C(22) . . . . 134.6(4) no O(3) C(23) Rh(2) N(3) . . . . -42.2(4) no O(3) C(23) Rh(2) N(4) . . . . 172.9(10) no O(3) C(23) Rh(2) C(21) . . . . 138.9(4) no O(3) C(23) Rh(2) C(22) . . . . -134.4(4) no N(1) Rh(1) Rh(2) N(3) . . . . -124.2(1) no N(1) Rh(1) Rh(2) N(4) . . . . 114.2(1) no N(1) Rh(1) Rh(2) C(21) . . . . 55.1(1) no N(1) Rh(1) Rh(2) C(22) . . . . 179.1(1) no N(1) Rh(1) Rh(2) C(23) . . . . -64.9(1) no N(1) Rh(1) N(2) C(6) . . . . -131.8(3) no N(1) Rh(1) N(2) C(10) . . . . 57.6(3) no N(1) C(1) C(2) C(3) . . . . -1.4(5) no N(1) C(5) C(4) C(3) . . . . 0.4(5) no N(2) Rh(1) Rh(2) N(3) . . . . -0.5(1) no N(2) Rh(1) Rh(2) N(4) . . . . -122.1(1) no N(2) Rh(1) Rh(2) C(21) . . . . 178.8(1) no N(2) Rh(1) Rh(2) C(22) . . . . -57.2(1) no N(2) Rh(1) Rh(2) C(23) . . . . 58.8(1) no N(2) Rh(1) N(1) C(1) . . . . -131.8(2) no N(2) Rh(1) N(1) C(5) . . . . 53.7(2) no N(2) C(6) C(7) C(8) . . . . -0.2(5) no N(2) C(10) C(9) C(8) . . . . -0.9(6) no N(3) Rh(2) Rh(1) C(21) . . . . -179.3(1) no N(3) Rh(2) Rh(1) C(22) . . . . 56.7(1) no N(3) Rh(2) Rh(1) C(23) . . . . -59.2(1) no N(3) Rh(2) N(4) C(16) . . . . 84.1(3) no N(3) Rh(2) N(4) C(20) . . . . -92.3(3) no N(3) C(11) C(12) C(13) . . . . -0.1(6) no N(3) C(15) C(14) C(13) . . . . -0.1(5) no N(4) Rh(2) Rh(1) C(21) . . . . 59.1(1) no N(4) Rh(2) Rh(1) C(22) . . . . -64.9(1) no N(4) Rh(2) Rh(1) C(23) . . . . 179.1(1) no N(4) Rh(2) N(3) C(11) . . . . 37.1(3) no N(4) Rh(2) N(3) C(15) . . . . -139.7(3) no N(4) C(16) C(17) C(18) . . . . -0.6(6) no N(4) C(20) C(19) C(18) . . . . -0.4(6) no C(1) N(1) Rh(1) C(21) . . . . 44.7(3) no C(1) N(1) Rh(1) C(22) . . . . 16(1) no C(1) N(1) Rh(1) C(23) . . . . -39.2(2) no C(1) N(1) C(5) C(4) . . . . -1.6(5) no C(1) C(2) C(3) C(4) . . . . 0.2(5) no C(2) C(1) N(1) C(5) . . . . 2.1(5) no C(2) C(3) C(4) C(5) . . . . 0.3(5) no C(5) N(1) Rh(1) C(21) . . . . -129.8(2) no C(5) N(1) Rh(1) C(22) . . . . -158(1) no C(5) N(1) Rh(1) C(23) . . . . 146.3(2) no C(6) N(2) Rh(1) C(21) . . . . 102(1) no C(6) N(2) Rh(1) C(22) . . . . 50.1(3) no C(6) N(2) Rh(1) C(23) . . . . 131.6(3) no C(6) N(2) C(10) C(9) . . . . -1.8(5) no C(6) C(7) C(8) C(9) . . . . -2.6(5) no C(7) C(6) N(2) C(10) . . . . 2.3(5) no C(7) C(8) C(9) C(10) . . . . 3.1(6) no C(10) N(2) Rh(1) C(21) . . . . -68(1) no C(10) N(2) Rh(1) C(22) . . . . -120.4(3) no C(10) N(2) Rh(1) C(23) . . . . -39.0(3) no C(11) N(3) Rh(2) C(21) . . . . -113(2) no C(11) N(3) Rh(2) C(22) . . . . -58.7(3) no C(11) N(3) Rh(2) C(23) . . . . -140.0(3) no C(11) N(3) C(15) C(14) . . . . -0.5(5) no C(11) C(12) C(13) C(14) . . . . -0.5(6) no C(12) C(11) N(3) C(15) . . . . 0.6(5) no C(12) C(13) C(14) C(15) . . . . 0.6(6) no C(15) N(3) Rh(2) C(21) . . . . 70(2) no C(15) N(3) Rh(2) C(22) . . . . 124.5(3) no C(15) N(3) Rh(2) C(23) . . . . 43.2(3) no C(16) N(4) Rh(2) C(21) . . . . -97.0(3) no C(16) N(4) Rh(2) C(22) . . . . 177.0(3) no C(16) N(4) Rh(2) C(23) . . . . -130(1) no C(16) N(4) C(20) C(19) . . . . 0.0(5) no C(16) C(17) C(18) C(19) . . . . 0.1(6) no C(17) C(16) N(4) C(20) . . . . 0.5(5) no C(17) C(18) C(19) C(20) . . . . 0.4(6) no C(20) N(4) Rh(2) C(21) . . . . 86.6(3) no C(20) N(4) Rh(2) C(22) . . . . 0.6(3) no C(20) N(4) Rh(2) C(23) . . . . 52(1) no C(21) Rh(1) Rh(2) C(22) . . . . 124.0(2) no C(21) Rh(1) Rh(2) C(23) . . . . -120.0(1) no C(21) Rh(2) Rh(1) C(22) . . . . -124.0(2) no C(21) Rh(2) Rh(1) C(23) . . . . 120.0(1) no C(22) Rh(1) Rh(2) C(23) . . . . 116.0(2) no C(22) Rh(2) Rh(1) C(23) . . . . -116.0(2) no #------------------------------------------------------------------------------