Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_General _journal_coden_Cambridge 182 #============================================================================== #============================================================================== # SUBMISSION DETAILS _publ_requested_journal ' Chem. Commun' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name 'Hiroyuki Furuta' _publ_contact_author_address ; Department of Chemistry, Graduate School of Science, Kyoto University, Kyoto 606-8502, Japan ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' +81-75-753-4010 ' _publ_contact_author_fax ' +81-75-753-3970' _publ_contact_author_email 'hfuruta@kuchem.kyoto-u.ac.jp ' #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; The First Bis-Rh(I) Metal Complex of N-Confused Porphyrin ; _publ_section_title_footnote ; ENTER ANY FOOTNOTES TO TITLE ; loop_ _publ_author_name #_publ_author_footnote #_publ_author_address ' Furuta, Hiroyuki' 'Osuka, Atsuhiro' 'Srinivasan, Alagar' #============================================================================== # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1997-1998). teXsan for Windows version 1.03. Single Crystal Structure Analysis Software. Version 1.04. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1993). J. Appl. Cryst., 26, 343. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #============================================================================== #============================================================================== data__Rh-TPP _database_code_CSD 164093 _audit_creation_date '19101-06-15' _audit_creation_method 'by teXsan for Windows v1.0' _audit_update_record ; ? ; #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows (MSC, 1997)' _computing_structure_solution ? _computing_structure_refinement 'teXsan for Windows (MSC, 1997)' _computing_publication_material 'teXsan for Windows (MSC, 1997)' #------------------------------------------------------------------------------ _cell_length_a 21.695(2) _cell_length_b 11.1778(7) _cell_length_c 21.600(1) _cell_angle_alpha 90 _cell_angle_beta 120.957(3) _cell_angle_gamma 90 _cell_volume 4492.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 11477 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 27.5 #------------------------------------------------------------------------------ _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' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'prism' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1015.52 _chemical_formula_analytical ? _chemical_formula_sum 'C49 H30 Cl2 N4 O4 Rh2 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2032.00 _exptl_absorpt_coefficient_mu 0.900 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_max 1.052 _exptl_absorpt_correction_T_min 0.947 _exptl_special_details ; ? ; #============================================================================== # EXPERIMENTAL DATA _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 'RAXIS-RAPID' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 5415 _reflns_number_total 5415 _reflns_number_gt 3014 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.04626 _diffrn_reflns_av_sigmaI/netI 0.072 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.04873 _diffrn_orient_matrix_UB_12 0.03766 _diffrn_orient_matrix_UB_13 -0.02375 _diffrn_orient_matrix_UB_21 0.02234 _diffrn_orient_matrix_UB_22 0.07849 _diffrn_orient_matrix_UB_23 0.02265 _diffrn_orient_matrix_UB_31 0.00398 _diffrn_orient_matrix_UB_32 0.02061 _diffrn_orient_matrix_UB_33 -0.04287 #------------------------------------------------------------------------------ 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 0 196 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 120 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 16 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Rh 0 8 -1.287 0.919 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 16 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 8 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Rh(1) 0.75466(7) 0.1510(1) 0.45016(7) 0.0329(3) 1.000 . Uani d ? Cl(1) 0.4832 0.1475 0.6677 0.356(1) 0.500 S Uiso d ? Cl(2) 0.5000 -0.0251 0.7500 0.476(1) 0.500 S Uiso d ? O(1) 0.698(1) -0.093(2) 0.448(1) 0.080(6) 1.000 . Uani d ? O(2) 0.649(1) 0.177(2) 0.2924(8) 0.090(6) 1.000 . Uani d ? N(1) 0.8093(7) 0.304(1) 0.4521(7) 0.033(4) 1.000 . Uani d ? N(2) 0.8376(7) 0.129(1) 0.5562(7) 0.034(4) 1.000 . Uani d ? C(1) 0.787(1) 0.408(2) 0.4124(9) 0.036(5) 1.000 . Uani d ? C(2) 0.848(1) 0.464(2) 0.415(1) 0.040(5) 1.000 . Uani d ? C(3) 0.9061(9) 0.395(2) 0.456(1) 0.038(5) 1.000 . Uani d ? C(4) 0.8832(9) 0.294(2) 0.4803(9) 0.033(4) 1.000 . Uani d ? C(5) 0.9277(9) 0.209(2) 0.5308(9) 0.035(5) 1.000 . Uani d ? C(6) 0.9076(9) 0.138(2) 0.5710(9) 0.036(4) 1.000 . Uani d ? C(7) 0.955(1) 0.074(2) 0.636(1) 0.047(5) 1.000 . Uani d ? C(8) 0.913(1) 0.031(2) 0.662(1) 0.046(5) 1.000 . Uani d ? C(9) 0.8396(9) 0.066(2) 0.6118(9) 0.037(5) 1.000 . Uani d ? C(10) 1.0037(9) 0.201(2) 0.547(1) 0.038(5) 1.000 . Uani d ? C(11) 0.7820(9) 0.042(2) 0.6226(9) 0.035(5) 1.000 . Uani d ? C(12) 1.016(1) 0.157(2) 0.495(1) 0.054(6) 1.000 . Uani d ? C(13) 1.087(1) 0.148(3) 0.508(1) 0.071(8) 1.000 . Uani d ? C(14) 1.143(1) 0.184(2) 0.574(2) 0.066(8) 1.000 . Uani d ? C(15) 1.131(1) 0.228(2) 0.626(1) 0.055(6) 1.000 . Uani d ? C(16) 1.062(1) 0.237(2) 0.613(1) 0.045(5) 1.000 . Uani d ? C(17) 0.7970(9) -0.049(2) 0.679(1) 0.040(5) 1.000 . Uani d ? C(18) 0.816(1) -0.166(2) 0.674(1) 0.053(6) 1.000 . Uani d ? C(19) 0.831(1) -0.248(2) 0.729(2) 0.072(8) 1.000 . Uani d ? C(20) 0.829(1) -0.214(3) 0.788(1) 0.077(9) 1.000 . Uani d ? C(21) 0.811(2) -0.099(3) 0.794(1) 0.08(1) 1.000 . Uani d ? C(22) 0.795(1) -0.017(2) 0.740(1) 0.058(7) 1.000 . Uani d ? C(23) 0.718(1) 0.001(2) 0.449(1) 0.047(6) 1.000 . Uani d ? C(24) 0.689(1) 0.168(2) 0.353(1) 0.053(6) 1.000 . Uani d ? C(25) 0.4783 0.0148 0.6688 0.109(1) 0.500 S Uiso d ? H(1) 0.8451 0.5428 0.3919 0.031 1.000 . Uiso c ? H(2) 0.9568 0.4100 0.4730 0.031 1.000 . Uiso c ? H(3) 1.0118 0.0788 0.6655 0.031 1.000 . Uiso c ? H(4) 0.9315 -0.0055 0.7089 0.031 1.000 . Uiso c ? H(5) 0.9713 0.1463 0.4480 0.031 1.000 . Uiso c ? H(6) 1.1008 0.1162 0.4664 0.031 1.000 . Uiso c ? H(7) 1.1944 0.1670 0.5860 0.031 1.000 . Uiso c ? H(8) 1.1689 0.2693 0.6707 0.031 1.000 . Uiso c ? H(9) 1.0533 0.2592 0.6563 0.031 1.000 . Uiso c ? H(10) 0.8481 -0.3432 0.7204 0.031 1.000 . Uiso c ? H(11) 0.8166 -0.1876 0.6276 0.031 1.000 . Uiso c ? H(12) 0.8448 -0.2744 0.8308 0.031 1.000 . Uiso c ? H(13) 0.8053 -0.0721 0.8407 0.031 1.000 . Uiso c ? H(14) 0.7797 0.0717 0.7487 0.031 1.000 . Uiso c ? H(15) 0.4306 -0.0101 0.6352 0.263 0.500 S Uiso d ? H(16) 0.5104 -0.0205 0.6565 0.263 0.500 S Uiso 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rh(1) 0.0291(6) 0.0397(7) 0.0271(6) -0.0020(8) 0.0124(5) 0.0010(8) O(1) 0.09(1) 0.05(1) 0.09(1) -0.03(1) 0.04(1) -0.01(1) O(2) 0.08(1) 0.12(2) 0.034(8) -0.02(1) 0.001(8) 0.01(1) N(1) 0.028(7) 0.042(8) 0.026(7) 0.002(6) 0.013(6) 0.005(6) N(2) 0.030(7) 0.04(1) 0.030(7) 0.001(6) 0.014(6) 0.003(6) C(1) 0.04(1) 0.04(1) 0.027(8) -0.004(8) 0.017(8) 0.000(8) C(2) 0.04(1) 0.04(1) 0.04(1) -0.003(9) 0.022(8) 0.006(9) C(3) 0.031(9) 0.04(1) 0.04(1) -0.006(8) 0.018(8) -0.002(8) C(4) 0.033(9) 0.04(1) 0.028(8) -0.002(8) 0.016(7) -0.001(7) C(5) 0.030(8) 0.04(1) 0.029(8) -0.001(8) 0.013(7) -0.001(8) C(6) 0.029(8) 0.04(1) 0.030(8) 0.001(8) 0.010(7) 0.004(8) C(7) 0.03(1) 0.06(1) 0.04(1) 0.006(9) 0.011(8) 0.014(9) C(8) 0.032(9) 0.06(1) 0.033(9) 0.005(9) 0.009(8) 0.016(9) C(9) 0.034(9) 0.04(1) 0.033(9) -0.002(8) 0.017(8) 0.002(8) C(10) 0.031(9) 0.04(1) 0.04(1) 0.001(8) 0.017(8) 0.006(8) C(11) 0.032(9) 0.04(1) 0.029(8) -0.002(8) 0.014(7) 0.002(8) C(12) 0.04(1) 0.07(1) 0.05(1) -0.00(1) 0.024(9) -0.01(1) C(13) 0.06(1) 0.08(2) 0.09(2) -0.01(1) 0.05(1) -0.02(2) C(14) 0.04(1) 0.07(2) 0.10(2) 0.01(1) 0.04(1) -0.00(1) C(15) 0.03(1) 0.06(1) 0.06(1) -0.01(1) 0.01(1) 0.01(1) C(16) 0.032(9) 0.05(1) 0.05(1) -0.003(9) 0.016(8) 0.00(1) C(17) 0.032(9) 0.05(1) 0.036(9) 0.002(9) 0.015(8) 0.012(9) C(18) 0.04(1) 0.06(1) 0.06(1) 0.01(1) 0.024(9) 0.02(1) C(19) 0.05(1) 0.06(2) 0.09(2) 0.00(1) 0.02(1) 0.03(1) C(20) 0.06(2) 0.10(2) 0.06(2) -0.01(2) 0.01(1) 0.04(2) C(21) 0.08(2) 0.11(2) 0.04(1) -0.01(2) 0.03(1) 0.02(2) C(22) 0.06(1) 0.07(2) 0.04(1) 0.00(1) 0.03(1) 0.01(1) C(23) 0.04(1) 0.05(1) 0.05(1) -0.006(9) 0.019(9) -0.01(1) C(24) 0.05(1) 0.07(2) 0.04(1) -0.02(1) 0.018(9) -0.00(1) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details unit _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 3014 _refine_ls_number_parameters 265 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_all 0.0630 _refine_ls_wR_factor_ref 0.0630 _refine_ls_goodness_of_fit_all 0.187 _refine_ls_goodness_of_fit_ref 0.190 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.74 _refine_diff_density_max 2.77 #============================================================================== # MOLECULAR GEOMETRY _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 RH1 N1 2.067(6) . . ? RH1 N2 2.074(6) . . ? RH1 C23 1.850(9) . . ? RH1 C24 1.845(9) . . ? CL1 C25 1.4884(1) . . ? CL2 C25 1.6272(1) . . ? CL2 C25 1.6272(1) . . ? O1 C23 1.13(1) . . ? O2 C24 1.14(1) . . ? N1 C1 1.375(9) . . ? N1 C4 1.394(9) . . ? N2 C6 1.387(9) . . ? N2 C9 1.373(9) . . ? C1 C2 1.44(1) . . ? C1 C11 1.40(1) . . ? C2 C3 1.35(1) . . ? C2 H1 1.00 . . no C3 C4 1.44(1) . . ? C3 H2 0.98 . . no C4 C5 1.39(1) . . ? C5 C6 1.40(1) . . ? C5 C10 1.50(1) . . ? C6 C7 1.43(1) . . ? C7 C8 1.38(1) . . ? C7 H3 1.06 . . no C8 C9 1.44(1) . . ? C8 H4 0.98 . . no C9 C11 1.41(1) . . ? C10 C12 1.39(1) . . ? C10 C16 1.39(1) . . ? C11 C17 1.49(1) . . ? C12 C13 1.40(1) . . ? C12 H5 0.98 . . no C13 C14 1.37(1) . . ? C13 H6 1.15 . . no C14 C15 1.36(1) . . ? C14 H7 1.03 . . no C15 C16 1.38(1) . . ? C15 H8 1.01 . . no C16 H9 1.07 . . no C17 C18 1.39(1) . . ? C17 C22 1.40(1) . . ? C18 C19 1.40(1) . . ? C18 H11 1.04 . . no C19 C20 1.36(2) . . ? C19 H10 1.17 . . no C20 C21 1.36(2) . . ? C20 H12 1.05 . . no C21 C22 1.38(1) . . ? C21 H13 1.11 . . no C22 H14 1.08 . . no C25 H15 0.95 . . no C25 H16 0.95 . . 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 N1 RH1 N2 84.9(2) . . . ? N1 RH1 C23 170.9(3) . . . ? N1 RH1 C24 92.1(3) . . . ? N2 RH1 C23 91.7(3) . . . ? N2 RH1 C24 173.2(3) . . . ? C23 RH1 C24 90.3(4) . . . ? C25 CL2 C25 148.152(3) . . . ? RH1 N1 C1 132.2(5) . . . ? RH1 N1 C4 117.7(5) . . . ? C1 N1 C4 107.0(6) . . . ? RH1 N2 C6 118.1(5) . . . ? RH1 N2 C9 130.1(5) . . . ? C6 N2 C9 107.3(6) . . . ? N1 C1 C2 108.8(7) . . . ? N1 C1 C11 127.7(7) . . . ? C2 C1 C11 123.4(7) . . . ? C1 C2 C3 107.8(7) . . . ? C1 C2 H1 122.6 . . . no C3 C2 H1 129.4 . . . no C2 C3 C4 107.8(7) . . . ? C2 C3 H2 129.7 . . . no C4 C3 H2 122.0 . . . no N1 C4 C3 108.6(6) . . . ? N1 C4 C5 124.7(7) . . . ? C3 C4 C5 126.3(7) . . . ? C4 C5 C6 124.2(7) . . . ? C4 C5 C10 117.3(7) . . . ? C6 C5 C10 118.3(7) . . . ? N2 C6 C5 123.4(7) . . . ? N2 C6 C7 109.8(7) . . . ? C5 C6 C7 126.5(7) . . . ? C6 C7 C8 106.1(7) . . . ? C6 C7 H3 126.3 . . . no C8 C7 H3 125.7 . . . no C7 C8 C9 108.1(7) . . . ? C7 C8 H4 124.1 . . . no C9 C8 H4 127.2 . . . no N2 C9 C8 108.7(6) . . . ? N2 C9 C11 127.7(7) . . . ? C8 C9 C11 123.5(7) . . . ? C5 C10 C12 118.9(7) . . . ? C5 C10 C16 122.3(7) . . . ? C12 C10 C16 118.8(7) . . . ? C1 C11 C9 128.5(7) 7_656 7_656 7_656 ? C1 C11 C17 116.0(7) 7_656 7_656 7_656 ? C9 C11 C17 115.4(7) . . . ? C10 C12 C13 120.3(8) . . . ? C10 C12 H5 111.8 . . . no C13 C12 H5 127.3 . . . no C12 C13 C14 119.0(9) . . . ? C12 C13 H6 123.9 . . . no C14 C13 H6 117.0 . . . no C13 C14 C15 121.3(9) . . . ? C13 C14 H7 118.7 . . . no C15 C14 H7 119.5 . . . no C14 C15 C16 120.5(9) . . . ? C14 C15 H8 124.1 . . . no C16 C15 H8 114.4 . . . no C10 C16 C15 120.0(8) . . . ? C10 C16 H9 118.9 . . . no C15 C16 H9 120.4 . . . no C11 C17 C18 121.6(7) . . . ? C11 C17 C22 119.9(8) . . . ? C18 C17 C22 118.5(8) . . . ? C17 C18 C19 119.8(9) . . . ? C17 C18 H11 116.6 . . . no C19 C18 H11 123.7 . . . no C18 C19 C20 120(1) . . . ? C18 C19 H10 114.4 . . . no C20 C19 H10 125.1 . . . no C19 C20 C21 120(1) . . . ? C19 C20 H12 119.2 . . . no C21 C20 H12 120.2 . . . no C20 C21 C22 120(1) . . . ? C20 C21 H13 120.8 . . . no C22 C21 H13 118.5 . . . no C17 C22 C21 120(1) . . . ? C17 C22 H14 123.8 . . . no C21 C22 H14 115.8 . . . no RH1 C23 O1 176.3(9) . . . ? RH1 C24 O2 178(1) . . . ? CL1 C25 CL2 107.888(1) . . . ? CL1 C25 H15 109.9 . . . no CL1 C25 H16 109.9 . . . no CL2 C25 H15 109.9 . . . no CL2 C25 H16 109.9 . . . no H15 C25 H16 109.5 . . . 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 O1 C25 3.437(8) . 3_656 no O2 C16 3.46(1) . 8_454 no O2 C15 3.58(1) . 8_454 no O2 C21 3.59(1) . 4_554 no C21 C24 3.56(1) . 4 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag RH1 N1 C1 C2 . . . . -157.7(6) no RH1 N1 C1 C11 . . . . 25(1) no RH1 N1 C4 C3 . . . . 161.2(5) no RH1 N1 C4 C5 . . . . -25.9(9) no RH1 N2 C6 C5 . . . . 30(1) no RH1 N2 C6 C7 . . . . -155.9(6) no RH1 N2 C9 C8 . . . . 153.3(6) no RH1 N2 C9 C11 . . . . -29(1) no CL1 C25 CL2 C25 . . . . 4.4363(4) no O1 C23 RH1 N1 . . . . -18(15) no O1 C23 RH1 N2 . . . . -86(13) no O1 C23 RH1 C24 . . . . 87(13) no O2 C24 RH1 N1 . . . . 90(34) no O2 C24 RH1 N2 . . . . 27(37) no O2 C24 RH1 C23 . . . . -81(34) no N1 RH1 N2 C6 . . . . -49.5(6) no N1 RH1 N2 C9 . . . . 157.5(7) no N1 C1 C2 C3 . . . . -0.7(9) no N1 C1 C11 C9 . . . . 17(1) no N1 C1 C11 C17 . . . . -162.1(7) no N1 C4 C3 C2 . . . . 0.9(9) no N1 C4 C5 C6 . . . . -14(1) no N1 C4 C5 C10 . . . . 171.4(7) no N2 RH1 N1 C1 . . . . -155.6(7) no N2 RH1 N1 C4 . . . . 47.2(5) no N2 C6 C5 C4 . . . . 12(1) no N2 C6 C5 C10 . . . . -173.6(7) no N2 C6 C7 C8 . . . . -2(1) no N2 C9 C8 C7 . . . . 0(1) no N2 C9 C11 C1 . . . . -13(1) no N2 C9 C11 C17 . . . . 168.0(8) no C1 N1 RH1 C23 . . . . 136(2) no C1 N1 RH1 C24 . . . . 30.5(7) no C1 N1 C4 C3 . . . . -1.3(8) no C1 N1 C4 C5 . . . . 171.7(7) no C1 C2 C3 C4 . . . . -0.1(9) no C1 C11 C9 C8 . . . . -164.6(8) no C1 C11 C17 C18 . . . . -119.8(9) no C1 C11 C17 C22 . . . . 62(1) no C2 C1 N1 C4 . . . . 1.2(8) no C2 C1 C11 C9 . . . . -159.6(8) no C2 C1 C11 C17 . . . . 21(1) no C2 C3 C4 C5 . . . . -171.9(8) no C3 C2 C1 C11 . . . . 176.6(7) no C3 C4 C5 C6 . . . . 157.8(8) no C3 C4 C5 C10 . . . . -17(1) no C4 N1 RH1 C23 . . . . -21(2) no C4 N1 RH1 C24 . . . . -126.7(6) no C4 N1 C1 C11 . . . . -176.0(7) no C4 C5 C6 C7 . . . . -161.8(8) no C4 C5 C10 C12 . . . . -69(1) no C4 C5 C10 C16 . . . . 110.0(9) no C5 C6 N2 C9 . . . . -171.7(8) no C5 C6 C7 C8 . . . . 171.8(9) no C5 C10 C12 C13 . . . . -180(1) no C5 C10 C16 C15 . . . . 179.8(8) no C6 N2 RH1 C23 . . . . 122.1(6) no C6 N2 RH1 C24 . . . . 15(3) no C6 N2 C9 C8 . . . . -1.9(9) no C6 N2 C9 C11 . . . . 175.7(8) no C6 C5 C10 C12 . . . . 115.6(9) no C6 C5 C10 C16 . . . . -65(1) no C6 C7 C8 C9 . . . . 1(1) no C7 C6 N2 C9 . . . . 2.7(9) no C7 C6 C5 C10 . . . . 13(1) no C7 C8 C9 C11 . . . . -177.4(8) no C8 C9 C11 C17 . . . . -15(1) no C9 N2 RH1 C23 . . . . -30.9(7) no C9 N2 RH1 C24 . . . . -138(3) no C9 C11 C17 C18 . . . . -61(1) no C9 C11 C17 C22 . . . . 117.1(9) no C10 C12 C13 C14 . . . . -1(2) no C10 C16 C15 C14 . . . . 1(2) no C11 C17 C18 C19 . . . . 178.3(8) no C11 C17 C22 C21 . . . . -177.6(9) no C12 C10 C16 C15 . . . . -1(1) no C12 C13 C14 C15 . . . . 1(2) no C13 C12 C10 C16 . . . . 1(2) no C13 C14 C15 C16 . . . . -0(2) no C17 C18 C19 C20 . . . . -0(2) no C17 C22 C21 C20 . . . . -1(2) no C18 C17 C22 C21 . . . . 0(1) no C18 C19 C20 C21 . . . . -0(2) no C19 C18 C17 C22 . . . . 0(1) no C19 C20 C21 C22 . . . . 1(2) no #------------------------------------------------------------------------------ #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data__Rh2-NCTPP _database_code_CSD 164093 _audit_creation_date '19101-06-19' _audit_creation_method 'by teXsan for Windows v1.0' _audit_update_record ; ? ; #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows (MSC, 1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan for Windows (MSC, 1997)' _computing_publication_material 'teXsan for Windows (MSC, 1997)' #------------------------------------------------------------------------------ _cell_length_a 18.0381(3) _cell_length_b 31.4290(5) _cell_length_c 17.1686(3) _cell_angle_alpha 90 _cell_angle_beta 111.3050(6) _cell_angle_gamma 90 _cell_volume 9068.0(2) _cell_formula_units_Z 8 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 51987 _cell_measurement_theta_min 1.3 _cell_measurement_theta_max 27.5 #------------------------------------------------------------------------------ _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' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'prism' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.90 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1018.52 _chemical_formula_analytical ? _chemical_formula_sum 'C48.50 H31 Cl2 N4 O4.50 Rh2 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 4080.00 _exptl_absorpt_coefficient_mu 0.893 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #============================================================================== # EXPERIMENTAL DATA _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 'RAXIS-RAPID' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 10611 _reflns_number_total 10420 _reflns_number_gt 7278 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.03440 _diffrn_reflns_av_sigmaI/netI 0.049 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.05019 _diffrn_orient_matrix_UB_12 0.01683 _diffrn_orient_matrix_UB_13 -0.02465 _diffrn_orient_matrix_UB_21 0.03196 _diffrn_orient_matrix_UB_22 0.02627 _diffrn_orient_matrix_UB_23 0.00212 _diffrn_orient_matrix_UB_31 -0.00082 _diffrn_orient_matrix_UB_32 -0.00626 _diffrn_orient_matrix_UB_33 -0.05742 #------------------------------------------------------------------------------ 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 0 388 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 248 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 32 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Rh 0 16 -1.287 0.919 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 36 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 16 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Rh(1) -0.19165(6) 0.17807(3) -0.65456(6) 0.0485(3) 1.000 . Uani d ? Rh(2) -0.28859(5) -0.01434(3) -0.72296(5) 0.0389(2) 1.000 . Uani d ? Cl(1) -0.0815(2) 0.1928(1) -0.5326(3) 0.078(1) 1.000 . Uani d ? Cl(2) 0.6198 0.2511 -0.0578 0.590(2) 0.500 S Uiso d ? Cl(3) 0.7816 0.2262 0.0771 0.629(2) 0.500 S Uiso d ? O(1) -0.1965(8) 0.2711(3) -0.6875(9) 0.105(5) 1.000 . Uani d ? O(2) -0.3289(8) 0.1633(4) -0.8118(8) 0.110(5) 1.000 . Uani d ? O(3) -0.2405(7) -0.0453(4) -0.8627(6) 0.087(4) 1.000 . Uani d ? O(4) -0.3526(7) 0.0647(4) -0.8208(7) 0.095(4) 1.000 . Uani d ? O(6) 0.5000 0.2425 0.7500 0.443(2) 0.500 S Uiso d ? N(1) -0.1677(5) 0.1131(3) -0.6279(6) 0.042(2) 1.000 . Uani d ? N(2) -0.0981(5) -0.0368(3) -0.6416(6) 0.039(2) 1.000 . Uani d ? N(3) -0.2616(5) -0.0727(3) -0.6595(6) 0.040(2) 1.000 . Uani d ? N(4) -0.3221(5) 0.0056(3) -0.6252(6) 0.039(2) 1.000 . Uani d ? C(1) -0.2067(6) 0.0783(3) -0.6051(6) 0.038(3) 1.000 . Uani d ? C(2) -0.1569(6) 0.0426(3) -0.5910(6) 0.037(3) 1.000 . Uani d ? C(3) -0.0997(6) 0.0985(3) -0.6283(7) 0.043(3) 1.000 . Uani d ? C(4) -0.0879(6) 0.0540(3) -0.6063(6) 0.038(3) 1.000 . Uani d ? C(5) -0.0222(6) 0.0295(3) -0.6089(6) 0.038(3) 1.000 . Uani d ? C(6) -0.0277(6) -0.0144(3) -0.6218(6) 0.039(3) 1.000 . Uani d ? C(7) 0.0303(6) -0.0450(4) -0.6239(7) 0.046(3) 1.000 . Uani d ? C(8) -0.0063(7) -0.0832(4) -0.6480(7) 0.048(3) 1.000 . Uani d ? C(9) -0.0889(6) -0.0783(3) -0.6601(7) 0.041(3) 1.000 . Uani d ? C(10) -0.1472(6) -0.1099(3) -0.6808(7) 0.042(3) 1.000 . Uani d ? C(11) -0.2229(6) -0.1079(3) -0.6751(7) 0.041(3) 1.000 . Uani d ? C(12) -0.2681(7) -0.1458(3) -0.6740(8) 0.049(3) 1.000 . Uani d ? C(13) -0.3307(7) -0.1340(4) -0.6535(8) 0.050(3) 1.000 . Uani d ? C(14) -0.3271(6) -0.0883(3) -0.6426(7) 0.041(3) 1.000 . Uani d ? C(15) -0.3784(6) -0.0644(3) -0.6162(7) 0.041(3) 1.000 . Uani d ? C(16) -0.3716(6) -0.0204(3) -0.6018(7) 0.043(3) 1.000 . Uani d ? C(17) -0.4110(7) 0.0044(4) -0.5582(8) 0.054(4) 1.000 . Uani d ? C(18) -0.3860(7) 0.0452(4) -0.5562(8) 0.052(4) 1.000 . Uani d ? C(19) -0.3288(6) 0.0463(3) -0.5971(7) 0.042(3) 1.000 . Uani d ? C(20) -0.2823(6) 0.0822(3) -0.5991(7) 0.040(3) 1.000 . Uani d ? C(21) 0.0512(6) 0.0526(4) -0.6047(6) 0.042(3) 1.000 . Uani d ? C(22) 0.0894(7) 0.0436(4) -0.6606(7) 0.051(3) 1.000 . Uani d ? C(23) 0.1549(8) 0.0672(5) -0.6581(9) 0.068(5) 1.000 . Uani d ? C(24) 0.1845(8) 0.0992(6) -0.601(1) 0.076(5) 1.000 . Uani d ? C(25) 0.1477(9) 0.1083(5) -0.5451(9) 0.074(5) 1.000 . Uani d ? C(26) 0.0817(7) 0.0854(4) -0.5470(7) 0.053(4) 1.000 . Uani d ? C(27) -0.1237(6) -0.1533(4) -0.7031(7) 0.046(3) 1.000 . Uani d ? C(28) -0.1333(8) -0.1620(4) -0.7853(8) 0.060(4) 1.000 . Uani d ? C(29) -0.1159(9) -0.2020(5) -0.807(1) 0.077(5) 1.000 . Uani d ? C(30) -0.0908(9) -0.2331(5) -0.748(1) 0.077(5) 1.000 . Uani d ? C(31) -0.0790(9) -0.2247(4) -0.666(1) 0.075(5) 1.000 . Uani d ? C(32) -0.0943(8) -0.1844(4) -0.6433(9) 0.064(4) 1.000 . Uani d ? C(33) -0.4412(6) -0.0878(3) -0.5960(7) 0.040(3) 1.000 . Uani d ? C(34) -0.4225(8) -0.1152(6) -0.5288(9) 0.084(5) 1.000 . Uani d ? C(35) -0.4812(9) -0.1384(6) -0.513(1) 0.099(6) 1.000 . Uani d ? C(36) -0.5585(8) -0.1345(4) -0.5652(9) 0.062(4) 1.000 . Uani d ? C(37) -0.5781(7) -0.1071(5) -0.6301(9) 0.068(4) 1.000 . Uani d ? C(38) -0.5198(7) -0.0833(5) -0.6451(8) 0.062(4) 1.000 . Uani d ? C(39) -0.3147(7) 0.1243(3) -0.5891(7) 0.042(3) 1.000 . Uani d ? C(40) -0.3933(7) 0.1352(4) -0.6373(8) 0.051(3) 1.000 . Uani d ? C(41) -0.4240(8) 0.1740(4) -0.6252(9) 0.062(4) 1.000 . Uani d ? C(42) -0.378(1) 0.2021(4) -0.566(1) 0.066(5) 1.000 . Uani d ? C(43) -0.3007(9) 0.1921(4) -0.5192(9) 0.059(4) 1.000 . Uani d ? C(44) -0.2683(7) 0.1533(4) -0.5301(8) 0.049(3) 1.000 . Uani d ? C(45) -0.1970(9) 0.2361(4) -0.676(1) 0.068(5) 1.000 . Uani d ? C(46) -0.2772(9) 0.1686(4) -0.752(1) 0.067(4) 1.000 . Uani d ? C(47) -0.2596(7) -0.0339(4) -0.8103(8) 0.055(4) 1.000 . Uani d ? C(48) -0.3266(7) 0.0357(4) -0.7826(8) 0.056(4) 1.000 . Uani d ? C(49) 0.6861 0.2266 0.0343 0.199(3) 0.500 S Uiso d ? H(1) -0.1467 -0.0249 -0.6422 0.047 1.000 . Uiso c ? H(2) -0.1679 0.0153 -0.5740 0.044 1.000 . Uiso c ? H(3) -0.0623 0.1154 -0.6417 0.051 1.000 . Uiso c ? H(4) 0.0853 -0.0396 -0.6106 0.056 1.000 . Uiso c ? H(5) 0.0186 -0.1087 -0.6555 0.057 1.000 . Uiso c ? H(6) -0.2559 -0.1739 -0.6857 0.059 1.000 . Uiso c ? H(7) -0.3700 -0.1524 -0.6473 0.060 1.000 . Uiso c ? H(8) -0.4480 -0.0059 -0.5350 0.065 1.000 . Uiso c ? H(9) -0.4029 0.0687 -0.5322 0.063 1.000 . Uiso c ? H(10) 0.0702 0.0213 -0.7003 0.062 1.000 . Uiso c ? H(11) 0.1800 0.0611 -0.6969 0.082 1.000 . Uiso c ? H(12) 0.2299 0.1149 -0.5993 0.091 1.000 . Uiso c ? H(13) 0.1678 0.1304 -0.5052 0.088 1.000 . Uiso c ? H(14) 0.0566 0.0921 -0.5085 0.064 1.000 . Uiso c ? H(15) -0.1519 -0.1405 -0.8268 0.072 1.000 . Uiso c ? H(16) -0.1214 -0.2077 -0.8630 0.092 1.000 . Uiso c ? H(17) -0.0812 -0.2609 -0.7643 0.092 1.000 . Uiso c ? H(18) -0.0605 -0.2465 -0.6254 0.090 1.000 . Uiso c ? H(19) -0.0844 -0.1782 -0.5863 0.077 1.000 . Uiso c ? H(20) -0.3686 -0.1183 -0.4925 0.101 1.000 . Uiso c ? H(21) -0.4674 -0.1569 -0.4665 0.119 1.000 . Uiso c ? H(22) -0.5985 -0.1511 -0.5557 0.074 1.000 . Uiso c ? H(23) -0.6322 -0.1041 -0.6658 0.082 1.000 . Uiso c ? H(24) -0.5348 -0.0636 -0.6901 0.075 1.000 . Uiso c ? H(25) -0.4256 0.1159 -0.6783 0.061 1.000 . Uiso c ? H(26) -0.4774 0.1812 -0.6581 0.075 1.000 . Uiso c ? H(27) -0.3997 0.2285 -0.5575 0.079 1.000 . Uiso c ? H(28) -0.2689 0.2118 -0.4789 0.071 1.000 . Uiso c ? H(29) -0.2146 0.1466 -0.4973 0.059 1.000 . Uiso c ? H(30) 0.4979 0.2117 0.7834 0.043 1.000 . Uiso c ? H(31) 0.6696 0.2374 0.0771 0.222 0.500 S Uiso d ? H(32) 0.6727 0.1973 0.0259 0.222 0.500 S Uiso 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rh(1) 0.0510(5) 0.0374(5) 0.0602(6) 0.0019(4) 0.0237(5) 0.0053(4) Rh(2) 0.0359(4) 0.0405(4) 0.0419(4) 0.0009(4) 0.0162(3) -0.0042(4) Cl(1) 0.066(2) 0.062(2) 0.090(3) -0.006(2) 0.010(2) -0.017(2) O(1) 0.12(1) 0.046(6) 0.16(1) 0.008(6) 0.054(9) 0.029(7) O(2) 0.11(1) 0.099(9) 0.079(8) 0.002(8) -0.014(7) 0.002(7) O(3) 0.099(8) 0.114(9) 0.061(6) 0.009(7) 0.044(6) -0.018(6) O(4) 0.111(9) 0.085(8) 0.085(8) 0.033(7) 0.031(7) 0.036(7) N(1) 0.044(5) 0.035(4) 0.049(5) 0.000(4) 0.021(4) -0.000(4) N(2) 0.031(4) 0.039(5) 0.051(5) 0.002(4) 0.018(4) -0.005(4) N(3) 0.038(5) 0.036(5) 0.050(5) 0.000(4) 0.021(4) -0.006(4) N(4) 0.037(4) 0.034(4) 0.053(5) -0.001(4) 0.024(4) -0.007(4) C(1) 0.040(5) 0.032(5) 0.042(6) -0.001(4) 0.016(5) -0.003(4) C(2) 0.038(5) 0.033(5) 0.041(5) -0.001(4) 0.016(4) -0.003(4) C(3) 0.043(6) 0.041(6) 0.048(6) -0.004(5) 0.021(5) -0.003(5) C(4) 0.036(5) 0.042(6) 0.036(5) -0.002(4) 0.013(4) -0.003(4) C(5) 0.032(5) 0.047(6) 0.033(5) -0.002(4) 0.012(4) -0.002(4) C(6) 0.034(5) 0.046(6) 0.037(5) 0.002(5) 0.014(4) -0.003(5) C(7) 0.035(5) 0.056(7) 0.051(7) 0.003(5) 0.019(5) -0.005(5) C(8) 0.044(6) 0.048(6) 0.054(7) 0.008(5) 0.022(5) -0.006(5) C(9) 0.041(6) 0.042(6) 0.044(6) 0.004(5) 0.019(5) -0.005(5) C(10) 0.043(6) 0.039(6) 0.045(6) 0.003(5) 0.018(5) -0.009(5) C(11) 0.043(6) 0.035(5) 0.047(6) 0.002(4) 0.018(5) -0.008(5) C(12) 0.046(6) 0.038(6) 0.065(8) -0.001(5) 0.021(6) -0.012(5) C(13) 0.046(6) 0.038(6) 0.068(8) -0.006(5) 0.023(6) -0.006(5) C(14) 0.037(5) 0.037(5) 0.051(6) -0.002(4) 0.017(5) -0.005(5) C(15) 0.035(5) 0.039(5) 0.051(6) -0.001(4) 0.019(5) -0.003(5) C(16) 0.039(6) 0.039(6) 0.056(7) -0.002(4) 0.024(5) -0.005(5) C(17) 0.056(7) 0.048(7) 0.074(8) -0.005(5) 0.044(7) -0.008(6) C(18) 0.056(7) 0.044(6) 0.072(8) -0.000(5) 0.041(7) -0.009(6) C(19) 0.043(6) 0.036(5) 0.053(6) 0.002(4) 0.025(5) -0.004(5) C(20) 0.043(6) 0.036(5) 0.044(6) -0.000(4) 0.021(5) -0.004(4) C(21) 0.033(5) 0.053(6) 0.038(6) -0.001(5) 0.013(4) -0.000(5) C(22) 0.039(6) 0.068(8) 0.050(7) -0.001(6) 0.019(5) -0.004(6) C(23) 0.044(7) 0.10(1) 0.068(9) -0.003(7) 0.030(7) 0.008(8) C(24) 0.046(8) 0.11(1) 0.07(1) -0.025(8) 0.021(7) 0.004(9) C(25) 0.063(9) 0.09(1) 0.057(8) -0.035(8) 0.008(7) -0.010(8) C(26) 0.050(7) 0.064(8) 0.044(6) -0.014(6) 0.015(5) -0.006(6) C(27) 0.039(6) 0.043(6) 0.060(7) 0.000(5) 0.023(5) -0.017(5) C(28) 0.068(8) 0.059(8) 0.058(8) 0.004(6) 0.028(7) -0.016(6) C(29) 0.08(1) 0.08(1) 0.07(1) 0.005(8) 0.033(8) -0.037(9) C(30) 0.069(9) 0.055(8) 0.10(1) 0.011(7) 0.026(9) -0.034(8) C(31) 0.07(1) 0.053(8) 0.10(1) 0.023(7) 0.029(9) -0.003(8) C(32) 0.072(9) 0.054(8) 0.066(9) 0.021(7) 0.025(7) -0.005(6) C(33) 0.037(5) 0.038(5) 0.051(6) -0.001(4) 0.021(5) -0.000(5) C(34) 0.039(7) 0.14(1) 0.07(1) -0.006(8) 0.012(7) 0.04(1) C(35) 0.057(9) 0.15(2) 0.09(1) 0.00(1) 0.031(9) 0.07(1) C(36) 0.053(7) 0.063(8) 0.080(9) -0.007(6) 0.036(7) 0.010(7) C(37) 0.038(7) 0.10(1) 0.065(9) -0.011(7) 0.014(6) 0.012(8) C(38) 0.045(7) 0.076(9) 0.062(8) -0.001(6) 0.015(6) 0.025(7) C(39) 0.049(6) 0.032(5) 0.056(7) 0.003(5) 0.031(5) 0.001(5) C(40) 0.051(7) 0.047(6) 0.060(7) 0.006(5) 0.027(6) 0.005(6) C(41) 0.067(8) 0.053(8) 0.08(1) 0.022(7) 0.046(8) 0.025(7) C(42) 0.09(1) 0.035(6) 0.10(1) 0.014(7) 0.068(9) 0.015(7) C(43) 0.09(1) 0.035(6) 0.076(9) -0.007(6) 0.053(8) -0.008(6) C(44) 0.056(7) 0.040(6) 0.061(7) -0.004(5) 0.033(6) -0.003(5) C(45) 0.067(9) 0.050(8) 0.09(1) 0.006(7) 0.036(8) 0.012(7) C(46) 0.07(1) 0.052(8) 0.067(9) 0.008(7) 0.018(8) 0.007(7) C(47) 0.053(7) 0.064(8) 0.050(7) 0.002(6) 0.020(6) -0.006(6) C(48) 0.052(7) 0.064(8) 0.053(7) 0.005(6) 0.022(6) 0.007(6) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details unit _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 7278 _refine_ls_number_parameters 536 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_all 0.0720 _refine_ls_wR_factor_ref 0.0720 _refine_ls_goodness_of_fit_all 0.490 _refine_ls_goodness_of_fit_ref 0.490 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.40 _refine_diff_density_max 2.33 #============================================================================== # MOLECULAR GEOMETRY _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 RH1 CL1 2.349(3) . . ? RH1 N1 2.104(6) . . ? RH1 C45 1.857(9) . . ? RH1 C46 1.84(1) . . ? RH2 N3 2.099(6) . . ? RH2 N4 2.077(6) . . ? RH2 C47 1.863(9) . . ? RH2 C48 1.867(9) . . ? CL2 CL3 2.052 . . ? CL2 C49 1.775 . . ? CL3 C49 1.609 . . ? O1 C45 1.12(1) . . ? O2 C46 1.12(1) . . ? O3 C47 1.13(1) . . ? O4 C48 1.12(1) . . ? O6 H30 1.13 . . no O6 H30 1.13 . . no N1 C1 1.431(9) . . ? N1 C3 1.310(9) . . ? N2 C6 1.383(9) . . ? N2 C9 1.367(9) . . ? N2 H1 0.95 . . no N3 C11 1.383(9) . . ? N3 C14 1.403(9) . . ? N4 C16 1.372(9) . . ? N4 C19 1.389(9) . . ? C1 C2 1.402(9) . . ? C1 C20 1.41(1) . . ? C2 C4 1.408(9) . . ? C2 H2 0.95 . . no C3 C4 1.44(1) . . ? C3 H3 0.95 . . no C4 C5 1.43(1) . . ? C5 C6 1.39(1) . . ? C5 C21 1.49(1) . . ? C6 C7 1.43(1) . . ? C7 C8 1.36(1) . . ? C7 H4 0.95 . . no C8 C9 1.44(1) . . ? C8 H5 0.95 . . no C9 C10 1.40(1) . . ? C10 C11 1.41(1) . . ? C10 C27 1.52(1) . . ? C11 C12 1.45(1) . . ? C12 C13 1.35(1) . . ? C12 H6 0.95 . . no C13 C14 1.45(1) . . ? C13 H7 0.95 . . no C14 C15 1.39(1) . . ? C15 C16 1.40(1) . . ? C15 C33 1.49(1) . . ? C16 C17 1.43(1) . . ? C17 C18 1.36(1) . . ? C17 H8 0.95 . . no C18 C19 1.44(1) . . ? C18 H9 0.95 . . no C19 C20 1.41(1) . . ? C20 C39 1.483(9) . . ? C21 C22 1.40(1) . . ? C21 C26 1.40(1) . . ? C22 C23 1.38(1) . . ? C22 H10 0.95 . . no C23 C24 1.37(1) . . ? C23 H11 0.95 . . no C24 C25 1.37(1) . . ? C24 H12 0.95 . . no C25 C26 1.38(1) . . ? C25 H13 0.95 . . no C26 H14 0.95 . . no C27 C28 1.39(1) . . ? C27 C32 1.38(1) . . ? C28 C29 1.38(1) . . ? C28 H15 0.95 . . no C29 C30 1.36(2) . . ? C29 H16 0.95 . . no C30 C31 1.37(1) . . ? C30 H17 0.95 . . no C31 C32 1.38(1) . . ? C31 H18 0.95 . . no C32 H19 0.95 . . no C33 C34 1.38(1) . . ? C33 C38 1.37(1) . . ? C34 C35 1.39(1) . . ? C34 H20 0.95 . . no C35 C36 1.36(1) . . ? C35 H21 0.95 . . no C36 C37 1.35(1) . . ? C36 H22 0.95 . . no C37 C38 1.39(1) . . ? C37 H23 0.95 . . no C38 H24 0.95 . . no C39 C40 1.40(1) . . ? C39 C44 1.39(1) . . ? C40 C41 1.39(1) . . ? C40 H25 0.95 . . no C41 C42 1.38(1) . . ? C41 H26 0.95 . . no C42 C43 1.37(1) . . ? C42 H27 0.95 . . no C43 C44 1.39(1) . . ? C43 H28 0.95 . . no C44 H29 0.95 . . no C49 H31 0.95 . . no C49 H32 0.95 . . 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 CL1 RH1 N1 87.6(2) . . . ? CL1 RH1 C45 87.0(3) . . . ? CL1 RH1 C46 177.6(3) . . . ? N1 RH1 C45 171.5(4) . . . ? N1 RH1 C46 94.5(3) . . . ? C45 RH1 C46 90.8(4) . . . ? N3 RH2 N4 85.7(2) . . . ? N3 RH2 C47 92.8(3) . . . ? N3 RH2 C48 172.5(3) . . . ? N4 RH2 C47 178.2(3) . . . ? N4 RH2 C48 91.9(3) . . . ? C47 RH2 C48 89.5(4) . . . ? CL3 CL2 C49 87.272(1) 7_655 7_655 7_655 ? CL2 CL3 C49 140.4406(8) 7_655 7_655 7_655 ? H30 O6 H30 62.7 . . . no RH1 N1 C1 136.0(5) . . . ? RH1 N1 C3 117.2(5) . . . ? C1 N1 C3 106.7(6) . . . ? C6 N2 C9 111.5(6) . . . ? C6 N2 H1 124.3 . . . no C9 N2 H1 124.3 . . . no RH2 N3 C11 129.5(5) . . . ? RH2 N3 C14 111.0(5) . . . ? C11 N3 C14 106.4(6) . . . ? RH2 N4 C16 118.0(5) . . . ? RH2 N4 C19 130.2(5) . . . ? C16 N4 C19 107.3(6) . . . ? N1 C1 C2 108.1(6) . . . ? N1 C1 C20 122.6(6) . . . ? C2 C1 C20 129.3(7) . . . ? C1 C2 C4 108.5(6) . . . ? C1 C2 H2 125.7 . . . no C4 C2 H2 125.8 . . . no N1 C3 C4 112.7(6) . . . ? N1 C3 H3 123.6 . . . no C4 C3 H3 123.6 . . . no C2 C4 C3 103.9(6) . . . ? C2 C4 C5 131.9(7) . . . ? C3 C4 C5 124.0(7) . . . ? C4 C5 C6 121.8(6) . . . ? C4 C5 C21 118.0(7) . . . ? C6 C5 C21 120.1(6) . . . ? N2 C6 C5 123.3(6) . . . ? N2 C6 C7 105.3(6) . . . ? C5 C6 C7 131.2(7) . . . ? C6 C7 C8 108.9(7) . . . ? C6 C7 H4 125.6 . . . no C8 C7 H4 125.5 . . . no C7 C8 C9 108.2(7) . . . ? C7 C8 H5 125.9 . . . no C9 C8 H5 125.9 . . . no N2 C9 C8 106.0(6) . . . ? N2 C9 C10 126.5(7) . . . ? C8 C9 C10 127.4(7) . . . ? C9 C10 C11 127.7(7) . . . ? C9 C10 C27 116.7(6) . . . ? C11 C10 C27 115.2(7) . . . ? N3 C11 C10 128.4(7) . . . ? N3 C11 C12 109.2(6) . . . ? C10 C11 C12 122.0(7) . . . ? C11 C12 C13 107.8(7) . . . ? C11 C12 H6 126.1 . . . no C13 C12 H6 126.1 . . . no C12 C13 C14 107.7(7) . . . ? C12 C13 H7 126.2 . . . no C14 C13 H7 126.2 . . . no N3 C14 C13 108.7(6) . . . ? N3 C14 C15 126.1(7) . . . ? C13 C14 C15 125.1(7) . . . ? C14 C15 C16 124.4(7) . . . ? C14 C15 C33 117.4(6) . . . ? C16 C15 C33 118.1(6) . . . ? N4 C16 C15 123.9(6) . . . ? N4 C16 C17 109.2(6) . . . ? C15 C16 C17 126.8(7) . . . ? C16 C17 C18 107.6(7) . . . ? C16 C17 H8 126.2 . . . no C18 C17 H8 126.2 . . . no C17 C18 C19 107.5(7) . . . ? C17 C18 H9 126.2 . . . no C19 C18 H9 126.3 . . . no N4 C19 C18 108.3(6) . . . ? N4 C19 C20 126.8(6) . . . ? C18 C19 C20 124.5(7) . . . ? C1 C20 C19 122.0(6) . . . ? C1 C20 C39 121.3(6) . . . ? C19 C20 C39 116.6(6) . . . ? C5 C21 C22 121.2(7) . . . ? C5 C21 C26 120.6(7) . . . ? C22 C21 C26 118.1(7) . . . ? C21 C22 C23 119.9(8) . . . ? C21 C22 H10 120.0 . . . no C23 C22 H10 120.1 . . . no C22 C23 C24 121.2(9) . . . ? C22 C23 H11 119.4 . . . no C24 C23 H11 119.4 . . . no C23 C24 C25 119.4(9) . . . ? C23 C24 H12 120.3 . . . no C25 C24 H12 120.3 . . . no C24 C25 C26 120.3(9) . . . ? C24 C25 H13 119.9 . . . no C26 C25 H13 119.8 . . . no C21 C26 C25 121.0(8) . . . ? C21 C26 H14 119.5 . . . no C25 C26 H14 119.5 . . . no C10 C27 C28 119.5(8) . . . ? C10 C27 C32 121.1(7) . . . ? C28 C27 C32 119.3(8) . . . ? C27 C28 C29 119.9(9) . . . ? C27 C28 H15 120.1 . . . no C29 C28 H15 120.0 . . . no C28 C29 C30 120.4(9) . . . ? C28 C29 H16 119.8 . . . no C30 C29 H16 119.8 . . . no C29 C30 C31 120.4(9) . . . ? C29 C30 H17 119.8 . . . no C31 C30 H17 119.8 . . . no C30 C31 C32 120(1) . . . ? C30 C31 H18 120.1 . . . no C32 C31 H18 120.2 . . . no C27 C32 C31 120.0(9) . . . ? C27 C32 H19 120.0 . . . no C31 C32 H19 120.0 . . . no C15 C33 C34 121.8(7) . . . ? C15 C33 C38 120.6(7) . . . ? C34 C33 C38 117.6(7) . . . ? C33 C34 C35 121.1(9) . . . ? C33 C34 H20 119.5 . . . no C35 C34 H20 119.5 . . . no C34 C35 C36 120.0(9) . . . ? C34 C35 H21 120.0 . . . no C36 C35 H21 120.0 . . . no C35 C36 C37 119.7(8) . . . ? C35 C36 H22 120.2 . . . no C37 C36 H22 120.1 . . . no C36 C37 C38 120.5(8) . . . ? C36 C37 H23 119.7 . . . no C38 C37 H23 119.7 . . . no C33 C38 C37 121.0(8) . . . ? C33 C38 H24 119.5 . . . no C37 C38 H24 119.5 . . . no C20 C39 C40 120.4(7) . . . ? C20 C39 C44 120.6(7) . . . ? C40 C39 C44 118.9(7) . . . ? C39 C40 C41 120.1(8) . . . ? C39 C40 H25 120.0 . . . no C41 C40 H25 120.0 . . . no C40 C41 C42 120.5(9) . . . ? C40 C41 H26 119.8 . . . no C42 C41 H26 119.7 . . . no C41 C42 C43 120.0(8) . . . ? C41 C42 H27 120.1 . . . no C43 C42 H27 120.0 . . . no C42 C43 C44 120.6(9) . . . ? C42 C43 H28 119.7 . . . no C44 C43 H28 119.7 . . . no C39 C44 C43 119.9(8) . . . ? C39 C44 H29 120.1 . . . no C43 C44 H29 120.1 . . . no RH1 C45 O1 177(1) . . . ? RH1 C46 O2 179(1) . . . ? RH2 C47 O3 178.4(9) . . . ? RH2 C48 O4 176.6(9) . . . ? CL2 C49 CL3 132.2733(5) . . . ? CL2 C49 H31 103.5 . . . no CL2 C49 H32 103.5 . . . no CL3 C49 H31 103.5 . . . no CL3 C49 H32 103.5 . . . no H31 C49 H32 109.5 . . . 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 O1 C12 3.43(1) . 6_453 no O1 C29 3.45(1) . 6_453 no O1 C30 3.59(1) . 6_453 no O2 C49 3.394(9) . 1_454 no O3 C18 3.40(1) . 4_554 no N2 C26 3.49(1) . 3_554 no N3 C25 3.55(1) . 3_554 no C2 C7 3.57(1) . 3_554 no C3 C23 3.57(1) . 2_553 no C8 C8 3.59(2) . 2_553 no C9 C26 3.52(1) . 3_554 no C11 C25 3.52(1) . 3_554 no C13 C37 3.58(1) . 2_453 no C22 C22 3.55(2) . 2_553 no C30 C30 3.30(2) . 2_553 no C35 C41 3.58(1) . 3_454 no C36 C42 3.57(1) . 3_454 no C37 C47 3.57(1) . 2_453 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag RH1 N1 C1 C2 . . . . -176.6(5) no RH1 N1 C1 C20 . . . . 3(1) no RH1 N1 C3 C4 . . . . 177.8(5) no RH2 N3 C11 C10 . . . . 55(1) no RH2 N3 C11 C12 . . . . -132.4(6) no RH2 N3 C14 C13 . . . . 141.8(6) no RH2 N3 C14 C15 . . . . -40.8(9) no RH2 N4 C16 C15 . . . . 24(1) no RH2 N4 C16 C17 . . . . -158.5(6) no RH2 N4 C19 C18 . . . . 154.2(6) no RH2 N4 C19 C20 . . . . -32(1) no CL1 RH1 N1 C1 . . . . 113.7(7) no CL1 RH1 N1 C3 . . . . -63.5(6) no CL1 RH1 C45 O1 . . . . 42(19) no CL1 RH1 C46 O2 . . . . 9(68) no O1 C45 RH1 N1 . . . . -8(21) no O1 C45 RH1 C46 . . . . -137(19) no O2 C46 RH1 N1 . . . . -141(61) no O2 C46 RH1 C45 . . . . 33(61) no O3 C47 RH2 N3 . . . . -105(32) no O3 C47 RH2 N4 . . . . -138(27) no O3 C47 RH2 C48 . . . . 82(32) no O4 C48 RH2 N3 . . . . -30(16) no O4 C48 RH2 N4 . . . . -101(15) no O4 C48 RH2 C47 . . . . 78(15) no N1 C1 C2 C4 . . . . -1.2(8) no N1 C1 C20 C19 . . . . 164.1(7) no N1 C1 C20 C39 . . . . -20(1) no N1 C3 C4 C2 . . . . -0.6(9) no N1 C3 C4 C5 . . . . 174.4(7) no N2 C6 C5 C4 . . . . 7(1) no N2 C6 C5 C21 . . . . -167.9(6) no N2 C6 C7 C8 . . . . 2.9(9) no N2 C9 C8 C7 . . . . -0.6(9) no N2 C9 C10 C11 . . . . -10(1) no N2 C9 C10 C27 . . . . 177.1(7) no N3 RH2 N4 C16 . . . . -48.5(5) no N3 RH2 N4 C19 . . . . 158.4(7) no N3 C11 C10 C9 . . . . 10(1) no N3 C11 C10 C27 . . . . -177.0(7) no N3 C11 C12 C13 . . . . -3(1) no N3 C14 C13 C12 . . . . 2(1) no N3 C14 C15 C16 . . . . -0(1) no N3 C14 C15 C33 . . . . -175.8(7) no N4 RH2 N3 C11 . . . . -171.0(6) no N4 RH2 N3 C14 . . . . 53.8(5) no N4 C16 C15 C14 . . . . 11(1) no N4 C16 C15 C33 . . . . -173.2(7) no N4 C16 C17 C18 . . . . 1(1) no N4 C19 C18 C17 . . . . 2(1) no N4 C19 C20 C1 . . . . -21(1) no N4 C19 C20 C39 . . . . 162.7(7) no C1 N1 RH1 C45 . . . . 164(3) no C1 N1 RH1 C46 . . . . -67.5(8) no C1 N1 C3 C4 . . . . -0.1(9) no C1 C2 C4 C3 . . . . 1.1(8) no C1 C2 C4 C5 . . . . -173.4(7) no C1 C20 C19 C18 . . . . 151.5(8) no C1 C20 C39 C40 . . . . 134.3(8) no C1 C20 C39 C44 . . . . -48(1) no C2 C1 N1 C3 . . . . 0.8(8) no C2 C1 C20 C19 . . . . -16(1) no C2 C1 C20 C39 . . . . 159.8(8) no C2 C4 C5 C6 . . . . 21(1) no C2 C4 C5 C21 . . . . -164.2(7) no C3 N1 RH1 C45 . . . . -13(3) no C3 N1 RH1 C46 . . . . 115.3(6) no C3 N1 C1 C20 . . . . -179.3(7) no C3 C4 C5 C6 . . . . -152.7(7) no C3 C4 C5 C21 . . . . 22(1) no C4 C2 C1 C20 . . . . 179.0(7) no C4 C5 C6 C7 . . . . -177.5(7) no C4 C5 C21 C22 . . . . -132.4(8) no C4 C5 C21 C26 . . . . 44(1) no C5 C6 N2 C9 . . . . 173.1(7) no C5 C6 C7 C8 . . . . -173.2(8) no C5 C21 C22 C23 . . . . 176.4(8) no C5 C21 C26 C25 . . . . -177.0(8) no C6 N2 C9 C8 . . . . 2.6(9) no C6 N2 C9 C10 . . . . 178.5(7) no C6 C5 C21 C22 . . . . 43(1) no C6 C5 C21 C26 . . . . -140.5(8) no C6 C7 C8 C9 . . . . -1.4(9) no C7 C6 N2 C9 . . . . -3.4(8) no C7 C6 C5 C21 . . . . 8(1) no C7 C8 C9 C10 . . . . -176.5(8) no C8 C9 C10 C11 . . . . 164.8(8) no C8 C9 C10 C27 . . . . -8(1) no C9 C10 C11 C12 . . . . -161.0(8) no C9 C10 C27 C28 . . . . -89(1) no C9 C10 C27 C32 . . . . 92(1) no C10 C11 N3 C14 . . . . -167.9(8) no C10 C11 C12 C13 . . . . 169.4(8) no C10 C27 C28 C29 . . . . -176.8(9) no C10 C27 C32 C31 . . . . 175.1(9) no C11 N3 RH2 C47 . . . . 10.0(7) no C11 N3 RH2 C48 . . . . 117(2) no C11 N3 C14 C13 . . . . -3.6(9) no C11 N3 C14 C15 . . . . 173.7(8) no C11 C10 C27 C28 . . . . 97.7(9) no C11 C10 C27 C32 . . . . -81(1) no C11 C12 C13 C14 . . . . 1(1) no C12 C11 N3 C14 . . . . 4.3(9) no C12 C11 C10 C27 . . . . 12(1) no C12 C13 C14 C15 . . . . -175.8(8) no C13 C14 C15 C16 . . . . 176.5(8) no C13 C14 C15 C33 . . . . 1(1) no C14 N3 RH2 C47 . . . . -125.2(5) no C14 N3 RH2 C48 . . . . -18(3) no C14 C15 C16 C17 . . . . -165.7(8) no C14 C15 C33 C34 . . . . 67(1) no C14 C15 C33 C38 . . . . -111.8(9) no C15 C16 N4 C19 . . . . -177.2(8) no C15 C16 C17 C18 . . . . 178.1(8) no C15 C33 C34 C35 . . . . -177(1) no C15 C33 C38 C37 . . . . 175.7(9) no C16 N4 RH2 C47 . . . . -15(10) no C16 N4 RH2 C48 . . . . 124.3(6) no C16 N4 C19 C18 . . . . -1.1(9) no C16 N4 C19 C20 . . . . 172.5(8) no C16 C15 C33 C34 . . . . -109(1) no C16 C15 C33 C38 . . . . 72(1) no C16 C17 C18 C19 . . . . -1(1) no C17 C16 N4 C19 . . . . 0.3(9) no C17 C16 C15 C33 . . . . 10(1) no C17 C18 C19 C20 . . . . -172.3(8) no C18 C19 C20 C39 . . . . -25(1) no C19 N4 RH2 C47 . . . . -168(10) no C19 N4 RH2 C48 . . . . -28.8(7) no C19 C20 C39 C40 . . . . -50(1) no C19 C20 C39 C44 . . . . 128.6(8) no C20 C39 C40 C41 . . . . 177.5(7) no C20 C39 C44 C43 . . . . -177.4(7) no C21 C22 C23 C24 . . . . 1(2) no C21 C26 C25 C24 . . . . 0(2) no C22 C21 C26 C25 . . . . -0(1) no C22 C23 C24 C25 . . . . -1(2) no C23 C22 C21 C26 . . . . -0(1) no C23 C24 C25 C26 . . . . 0(2) no C27 C28 C29 C30 . . . . 1(2) no C27 C32 C31 C30 . . . . 2(2) no C28 C27 C32 C31 . . . . -4(1) no C28 C29 C30 C31 . . . . -3(2) no C29 C28 C27 C32 . . . . 2(1) no C29 C30 C31 C32 . . . . 1(2) no C33 C34 C35 C36 . . . . 0(2) no C33 C38 C37 C36 . . . . 2(2) no C34 C33 C38 C37 . . . . -3(2) no C34 C35 C36 C37 . . . . -2(2) no C35 C34 C33 C38 . . . . 2(2) no C35 C36 C37 C38 . . . . 1(2) no C39 C40 C41 C42 . . . . -0(1) no C39 C44 C43 C42 . . . . 0(1) no C40 C39 C44 C43 . . . . 1(1) no C40 C41 C42 C43 . . . . 1(1) no C41 C40 C39 C44 . . . . -1(1) no C41 C42 C43 C44 . . . . -1(1) no #------------------------------------------------------------------------------ #============================================================================== #============================================================================== # End of CIF #==============================================================================