# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1794 data_General # MS No. B004167J #============================================================================== _audit_creation_date '19100-04-04' _audit_creation_method 'by teXsan for Windows v1.0' _audit_update_record ; ? ; #============================================================================== # SUBMISSION DETAILS _publ_requested_journal 'Chemical Communications' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name 'Kristin Bowman-James' _publ_contact_author_address ; Department of Chemistry University of Kansas 2010 Malott Hall Lawrence, KS 66045 USA ; _publ_contact_author_phone '1(785)8645673' _publ_contact_author_fax '1(785)8645396' _publ_contact_author_email 'KBowmanJames@chem.ukans.edu' #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER ANY FOOTNOTES TO TITLE ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; #============================================================================== # 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 1.05. 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. 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__crystal_333______________ #============================================================================== _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 12.143(7) _cell_length_b 21.64(1) _cell_length_c 11.97(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3144(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 11 _cell_measurement_theta_min 14.4 _cell_measurement_theta_max 18.9 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x, -y,1/2+z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'Prism' _exptl_crystal_colour 'Clear' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 639.39 _chemical_formula_analytical ? _chemical_formula_sum 'C18 H54 Cl6 N8 O2.75 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1368.00 _exptl_absorpt_coefficient_mu 5.256 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 0.998 _exptl_absorpt_correction_T_min 0.756 _exptl_special_details ; The scan width was (1.57+0.30tan\q)\% with an \w scan speed of 8\% per minute (up to 5 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. ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -6.75 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 4 0 0 2 -6 0 5 0 1 _diffrn_reflns_number 2679 _reflns_number_total 2679 _reflns_number_gt 1630 _reflns_threshold_expression I>1.00\s(I) _diffrn_reflns_av_R_equivalents 0.00000 _diffrn_reflns_av_sigmaI/netI 0.161 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 60.03 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.04958 _diffrn_orient_matrix_UB_12 -0.03184 _diffrn_orient_matrix_UB_13 0.03372 _diffrn_orient_matrix_UB_21 0.05063 _diffrn_orient_matrix_UB_22 0.00359 _diffrn_orient_matrix_UB_23 -0.06559 _diffrn_orient_matrix_UB_31 0.04195 _diffrn_orient_matrix_UB_32 0.03330 _diffrn_orient_matrix_UB_33 0.03931 #------------------------------------------------------------------------------ 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 72 0.017 0.009 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 216 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 32 0.029 0.018 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 24 0.348 0.702 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 11 0.047 0.032 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #============================================================================== # 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 Cl(1) -0.0124(2) 0.1276(1) 0.2656(2) 0.0458(7) 1.000 . Uani d ? Cl(2) 0.2211(3) 0.1195(1) 0.0995(2) 0.063(1) 1.000 . Uani d ? Cl(3) -0.0160(3) 0.3179(1) 0.4396(2) 0.068(1) 1.000 . Uani d ? Cl(4) 0.1162(3) 0.0911(2) 0.7874(3) 0.085(1) 1.000 . Uani d ? Cl(5) 0.1082(3) 0.3761(2) 0.8665(3) 0.090(1) 1.000 . Uani d ? Cl(6) -0.2144(2) -0.0718(2) 0.2389(3) 0.085(1) 1.000 . Uani d ? O(100) -0.0229(8) 0.1741(3) 0.6370(7) 0.084(3) 1.000 . Uani d ? O(200) -0.5736(8) 0.0599(4) 0.3065(7) 0.102(4) 1.000 . Uani d ? O(300) -0.025(1) 0.2929(5) 0.6973(9) 0.099(5) 0.750 S Uani d ? N(1) 0.0786(7) 0.0150(3) 0.4232(7) 0.037(3) 1.000 . Uani d ? N(4) -0.1294(7) 0.0937(4) 0.4813(7) 0.049(3) 1.000 . Uani d ? N(7) -0.2321(6) 0.1890(4) 0.2834(7) 0.046(3) 1.000 . Uani d ? N(10) -0.0892(6) 0.2421(3) 0.0975(6) 0.035(2) 1.000 S Uani d ? N(13) -0.0266(7) 0.1072(3) 0.0030(6) 0.040(2) 1.000 . Uani d ? N(16) 0.0076(7) -0.0075(3) 0.1848(6) 0.039(2) 1.000 . Uani d ? N(21) 0.2243(7) 0.1328(3) 0.3688(7) 0.043(3) 1.000 . Uani d ? N(24) 0.1112(7) 0.2517(3) 0.2439(7) 0.048(3) 1.000 . Uani d ? C(2) 0.007(1) 0.0143(4) 0.5251(8) 0.053(4) 1.000 . Uani d ? C(3) -0.1138(9) 0.0257(5) 0.502(1) 0.056(4) 1.000 . Uani d ? C(5) -0.2431(9) 0.1098(5) 0.439(1) 0.063(4) 1.000 . Uani d ? C(6) -0.2495(9) 0.1781(5) 0.4055(9) 0.055(4) 1.000 . Uani d ? C(8) -0.2331(8) 0.2539(5) 0.244(1) 0.050(4) 1.000 . Uani d ? C(9) -0.2069(9) 0.2576(4) 0.1210(9) 0.051(4) 1.000 . Uani d ? C(11) -0.0748(9) 0.2192(4) -0.0180(9) 0.048(3) 1.000 . Uani d ? C(12) -0.1130(9) 0.1521(4) -0.0301(8) 0.050(3) 1.000 . Uani d ? C(14) -0.0699(9) 0.0426(4) 0.0130(9) 0.050(3) 1.000 . Uani d ? C(15) 0.016(1) -0.0010(4) 0.0631(8) 0.047(3) 1.000 . Uani d ? C(17) 0.0975(8) -0.0404(4) 0.2416(9) 0.047(3) 1.000 . Uani d ? C(18) 0.0746(9) -0.0457(4) 0.3665(9) 0.048(3) 1.000 . Uani d ? C(19) 0.1921(8) 0.0289(4) 0.4557(9) 0.043(3) 1.000 . Uani d ? C(20) 0.2135(9) 0.0980(5) 0.4753(8) 0.047(3) 1.000 . Uani d ? C(22) 0.2253(9) 0.2002(4) 0.3906(9) 0.043(3) 1.000 . Uani d ? C(23) 0.2257(8) 0.2399(4) 0.2834(9) 0.043(3) 1.000 . Uani d ? C(25) 0.0970(8) 0.2851(4) 0.1340(9) 0.044(3) 1.000 . Uani d ? C(26) -0.022(1) 0.2973(4) 0.1133(8) 0.041(3) 1.000 . Uani d ? H(2) 0.0078 -0.0289 0.5568 0.072 1.000 . Uiso c ? H(2) 0.0253 0.0408 0.5805 0.072 1.000 . Uiso c ? H(3) -0.1643 0.0119 0.5627 0.073 1.000 . Uiso c ? H(3) -0.1420 0.0015 0.4364 0.073 1.000 . Uiso c ? H(4) -0.1110 0.1164 0.5461 0.058 1.000 . Uiso c ? H(4) -0.0765 0.1064 0.4226 0.058 1.000 . Uiso c ? H(5) -0.2929 0.1036 0.5035 0.085 1.000 . Uiso c ? H(5) -0.2632 0.0841 0.3824 0.085 1.000 . Uiso c ? H(6) -0.3176 0.1972 0.4256 0.067 1.000 . Uiso c ? H(6) -0.1913 0.2027 0.4423 0.067 1.000 . Uiso c ? H(7) -0.2939 0.1669 0.2452 0.062 1.000 . Uiso c ? H(7) -0.1672 0.1692 0.2610 0.062 1.000 . Uiso c ? H(8) -0.1732 0.2778 0.2855 0.071 1.000 . Uiso c ? H(8) -0.2992 0.2761 0.2643 0.071 1.000 . Uiso c ? H(9) -0.2285 0.2952 0.0922 0.068 1.000 . Uiso c ? H(9) -0.2555 0.2251 0.0893 0.068 1.000 . Uiso c ? H(11) 0.0029 0.2189 -0.0391 0.059 1.000 . Uiso c ? H(11) -0.1118 0.2445 -0.0724 0.059 1.000 . Uiso c ? H(12) -0.1781 0.1469 0.0205 0.070 1.000 . Uiso c ? H(12) -0.1428 0.1442 -0.1040 0.070 1.000 . Uiso c ? H(13) 0.0072 0.1193 0.0703 0.047 1.000 . Uiso c ? H(13) 0.0307 0.1068 -0.0551 0.047 1.000 . Uiso c ? H(14) -0.1333 0.0413 0.0613 0.060 1.000 . Uiso c ? H(14) -0.0928 0.0256 -0.0584 0.060 1.000 . Uiso c ? H(15) 0.0051 -0.0422 0.0316 0.056 1.000 . Uiso c ? H(15) 0.0860 0.0130 0.0416 0.056 1.000 . Uiso c ? H(16) -0.0622 -0.0250 0.2046 0.050 1.000 . Uiso c ? H(16) 0.0048 0.0357 0.2158 0.050 1.000 . Uiso c ? H(17) 0.1010 -0.0780 0.2086 0.075 1.000 . Uiso c ? H(17) 0.1616 -0.0162 0.2313 0.075 1.000 . Uiso c ? H(18) -0.0020 -0.0609 0.3786 0.065 1.000 . Uiso c ? H(18) 0.1220 -0.0731 0.4005 0.065 1.000 . Uiso c ? H(19) 0.2427 0.0154 0.3944 0.061 1.000 . Uiso c ? H(19) 0.2179 0.0052 0.5203 0.061 1.000 . Uiso c ? H(20) 0.1472 0.1154 0.5133 0.069 1.000 . Uiso c ? H(20) 0.2737 0.1069 0.5231 0.069 1.000 . Uiso c ? H(21) 0.1650 0.1218 0.3184 0.054 1.000 . Uiso c ? H(21) 0.2920 0.1199 0.3313 0.054 1.000 . Uiso c ? H(22) 0.1640 0.2136 0.4343 0.062 1.000 . Uiso c ? H(22) 0.2917 0.2126 0.4357 0.062 1.000 . Uiso c ? H(23) 0.2659 0.2791 0.2934 0.068 1.000 . Uiso c ? H(23) 0.2685 0.2179 0.2259 0.068 1.000 . Uiso c ? H(24) 0.0728 0.2768 0.3000 0.058 1.000 . Uiso c ? H(24) 0.0709 0.2130 0.2407 0.058 1.000 . Uiso c ? H(25) 0.1391 0.3229 0.1317 0.061 1.000 . Uiso c ? H(25) 0.1287 0.2595 0.0723 0.061 1.000 . Uiso c ? H(26) -0.0500 0.3190 0.1739 0.062 1.000 . Uiso c ? H(26) -0.0302 0.3211 0.0459 0.062 1.000 . Uiso c ? H(100) -0.0218 0.2185 0.6600 0.060 1.000 . Uiso c ? H(100) -0.0072 0.1327 0.6878 0.060 1.000 . Uiso c ? H(200) -0.5005 0.0275 0.2747 0.060 1.000 . Uiso c ? H(200) -0.5705 0.1149 0.3145 0.060 1.000 . Uiso c ? H(300) -0.0198 0.3025 0.6135 0.060 1.000 . Uiso c ? H(300) 0.0201 0.3212 0.7507 0.060 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 Cl(1) 0.049(2) 0.035(1) 0.054(2) 0.004(1) 0.001(1) 0.005(1) Cl(2) 0.067(2) 0.067(2) 0.056(2) -0.005(2) 0.005(2) -0.018(2) Cl(3) 0.052(2) 0.098(2) 0.053(2) -0.002(2) 0.003(2) -0.018(2) Cl(4) 0.086(2) 0.101(2) 0.067(2) -0.003(2) 0.001(2) -0.012(2) Cl(5) 0.096(3) 0.085(2) 0.088(2) 0.038(2) 0.016(2) -0.010(2) Cl(6) 0.051(2) 0.124(3) 0.080(2) -0.016(2) -0.005(2) 0.029(2) O(100) 0.109(7) 0.040(4) 0.101(7) 0.015(5) -0.021(6) -0.018(5) O(200) 0.124(9) 0.095(6) 0.088(7) 0.008(6) 0.045(6) -0.010(6) O(300) 0.13(1) 0.086(8) 0.081(9) -0.027(9) -0.028(9) 0.005(7) N(1) 0.043(5) 0.031(4) 0.039(5) 0.007(4) -0.014(5) 0.003(4) N(4) 0.053(6) 0.053(6) 0.042(5) -0.003(5) 0.003(5) -0.004(5) N(7) 0.035(5) 0.051(5) 0.050(6) 0.007(5) 0.009(5) 0.007(5) N(10) 0.038(5) 0.033(5) 0.032(5) -0.007(4) 0.000(4) 0.005(4) N(13) 0.045(5) 0.043(5) 0.032(4) 0.000(5) -0.012(4) -0.010(4) N(16) 0.048(6) 0.033(4) 0.037(5) -0.005(5) -0.001(5) -0.003(4) N(21) 0.050(5) 0.035(5) 0.046(5) 0.010(5) -0.012(5) -0.011(5) N(24) 0.054(6) 0.040(5) 0.049(6) -0.005(5) 0.009(5) -0.006(5) C(2) 0.09(1) 0.043(6) 0.029(6) 0.002(8) -0.006(7) 0.003(5) C(3) 0.055(8) 0.044(7) 0.068(8) -0.009(6) 0.020(7) 0.011(7) C(5) 0.045(7) 0.067(8) 0.076(9) 0.007(7) 0.013(7) 0.014(8) C(6) 0.040(7) 0.086(9) 0.040(7) 0.010(7) 0.008(5) -0.009(7) C(8) 0.037(6) 0.050(7) 0.062(8) -0.000(6) 0.002(6) -0.024(7) C(9) 0.052(7) 0.040(6) 0.060(8) 0.004(6) -0.014(7) 0.010(6) C(11) 0.057(8) 0.037(6) 0.050(7) 0.009(6) -0.011(6) 0.014(6) C(12) 0.060(8) 0.047(6) 0.043(7) 0.008(6) -0.019(6) -0.012(6) C(14) 0.064(8) 0.033(6) 0.054(7) -0.010(6) 0.002(7) -0.012(6) C(15) 0.064(8) 0.033(6) 0.044(6) 0.007(6) 0.007(7) -0.014(5) C(17) 0.039(6) 0.048(6) 0.056(8) 0.001(6) -0.007(6) -0.013(6) C(18) 0.047(7) 0.040(6) 0.058(8) 0.005(6) 0.002(6) -0.007(6) C(19) 0.044(7) 0.034(6) 0.050(7) 0.011(6) -0.016(6) 0.009(5) C(20) 0.046(7) 0.050(7) 0.044(7) -0.009(6) -0.005(6) -0.010(6) C(22) 0.050(7) 0.032(6) 0.047(7) 0.003(6) -0.018(6) -0.007(6) C(23) 0.031(6) 0.036(6) 0.063(7) -0.011(5) -0.006(6) -0.004(6) C(25) 0.034(6) 0.049(7) 0.049(7) -0.010(6) 0.007(6) 0.011(6) C(26) 0.057(7) 0.028(6) 0.038(6) -0.013(6) 0.006(6) -0.000(5) #============================================================================== # 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 'w = 1/[\s^2^(Fo) + 0.00010|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 1630 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1555 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_all 0.0690 _refine_ls_wR_factor_ref 0.0590 _refine_ls_goodness_of_fit_all 1.396 _refine_ls_goodness_of_fit_ref 1.570 _refine_ls_shift/su_max 0.0100 _refine_ls_shift/su_mean 0.0024 _refine_diff_density_min -0.32 _refine_diff_density_max 0.40 #============================================================================== # 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 O(100) H(100a 1.00 . . no O(100) H(100b 1.10 . . no O(200) H(200a 1.19 . . no O(200) H(200b 1.19 . . no O(300) H(300a 1.03 . . no O(300) H(300b 1.04 . . no N(1) C(2) 1.50(2) . . ? N(1) C(18) 1.48(1) . . ? N(1) C(19) 1.46(1) . . ? N(4) C(3) 1.50(1) . . ? N(4) C(5) 1.51(2) . . ? N(4) H(4a) 0.94 . . no N(4) H(4b) 0.99 . . no N(7) C(6) 1.50(2) . . ? N(7) C(8) 1.48(2) . . ? N(7) H(7a) 1.00 . . no N(7) H(7b) 0.94 . . no N(10) C(9) 1.49(2) . . ? N(10) C(11) 1.48(2) . . ? N(10) C(26) 1.46(1) . . ? N(13) C(12) 1.49(1) . . ? N(13) C(14) 1.50(1) . . ? N(13) H(13b) 0.94 . . no N(13) H(13a) 0.98 . . no N(16) C(15) 1.47(1) . . ? N(16) C(17) 1.47(1) . . ? N(16) H(16b) 0.96 . . no N(16) H(16a) 1.01 . . no N(21) C(20) 1.49(2) . . ? N(21) C(22) 1.48(1) . . ? N(21) H(21b) 0.97 . . no N(21) H(21a) 0.98 . . no N(24) C(23) 1.49(2) . . ? N(24) C(25) 1.51(1) . . ? N(24) H(24b) 0.98 . . no N(24) H(24a) 0.97 . . no C(2) C(3) 1.51(2) . . ? C(2) H(2a) 1.01 . . no C(2) H(2b) 0.91 . . no C(3) H(3a) 0.99 . . no C(3) H(3b) 1.01 . . no C(5) C(6) 1.53(2) . . ? C(5) H(5a) 0.99 . . no C(5) H(5b) 0.91 . . no C(6) H(6a) 0.95 . . no C(6) H(6b) 0.99 . . no C(8) C(9) 1.51(2) . . ? C(8) H(8a) 1.02 . . no C(8) H(8b) 0.96 . . no C(9) H(9a) 0.92 . . no C(9) H(9b) 0.99 . . no C(11) C(12) 1.53(2) . . ? C(11) H(11a) 0.98 . . no C(11) H(11b) 0.96 . . no C(12) H(12a) 1.00 . . no C(12) H(12b) 0.97 . . no C(14) C(15) 1.53(2) . . ? C(14) H(14b) 0.96 . . no C(14) H(14a) 0.97 . . no C(15) H(15b) 0.98 . . no C(15) H(15a) 0.94 . . no C(17) C(18) 1.52(2) . . ? C(17) H(17b) 0.91 . . no C(17) H(17a) 0.95 . . no C(18) H(18b) 1.00 . . no C(18) H(18a) 0.92 . . no C(19) C(20) 1.54(2) . . ? C(19) H(19b) 1.00 . . no C(19) H(19a) 0.98 . . no C(20) H(20b) 1.00 . . no C(20) H(20a) 0.95 . . no C(22) C(23) 1.54(2) . . ? C(22) H(22b) 0.96 . . no C(22) H(22a) 1.01 . . no C(23) H(23b) 0.99 . . no C(23) H(23a) 0.98 . . no C(25) C(26) 1.48(2) . . ? C(25) H(25b) 0.97 . . no C(25) H(25a) 1.00 . . no C(26) H(26b) 0.93 . . no C(26) H(26a) 0.96 . . 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 H(100a O(100) H(100b 128.9 . . . no H(200a O(200) H(200b 125.9 . . . no H(300a O(300) H(300b 116.4 . . . no C(2) N(1) C(18) 110(1) . . . ? C(2) N(1) C(19) 110(1) . . . ? C(18) N(1) C(19) 109.6(9) . . . ? C(3) N(4) C(5) 113(1) . . . ? C(3) N(4) H(4a) 110.0 . . . no C(3) N(4) H(4b) 107.9 . . . no C(5) N(4) H(4a) 111.8 . . . no C(5) N(4) H(4b) 106.8 . . . no H(4a) N(4) H(4b) 106.6 . . . no C(6) N(7) C(8) 117(1) . . . ? C(6) N(7) H(7a) 105.3 . . . no C(6) N(7) H(7b) 109.1 . . . no C(8) N(7) H(7a) 107.7 . . . no C(8) N(7) H(7b) 110.6 . . . no H(7a) N(7) H(7b) 106.3 . . . no C(9) N(10) C(11) 111(1) . . . ? C(9) N(10) C(26) 109(1) . . . ? C(11) N(10) C(26) 109(1) . . . ? C(12) N(13) C(14) 113(1) . . . ? C(12) N(13) H(13b) 110.7 . . . no C(12) N(13) H(13a) 108.4 . . . no C(14) N(13) H(13b) 110.3 . . . no C(14) N(13) H(13a) 107.3 . . . no H(13b) N(13) H(13a) 107.4 . . . no C(15) N(16) C(17) 117(1) . . . ? C(15) N(16) H(16b) 110.1 . . . no C(15) N(16) H(16a) 106.2 . . . no C(17) N(16) H(16b) 110.6 . . . no C(17) N(16) H(16a) 107.7 . . . no H(16b) N(16) H(16a) 104.3 . . . no C(20) N(21) C(22) 110(1) . . . ? C(20) N(21) H(21b) 110.1 . . . no C(20) N(21) H(21a) 108.8 . . . no C(22) N(21) H(21b) 111.0 . . . no C(22) N(21) H(21a) 110.8 . . . no H(21b) N(21) H(21a) 105.6 . . . no C(23) N(24) C(25) 118(1) . . . ? C(23) N(24) H(24b) 108.8 . . . no C(23) N(24) H(24a) 109.6 . . . no C(25) N(24) H(24b) 106.0 . . . no C(25) N(24) H(24a) 108.7 . . . no H(24b) N(24) H(24a) 105.4 . . . no N(1) C(2) C(3) 114(1) . . . ? N(1) C(2) H(2a) 108.0 . . . no N(1) C(2) H(2b) 116.3 . . . no C(3) C(2) H(2a) 103.5 . . . no C(3) C(2) H(2b) 105.6 . . . no H(2a) C(2) H(2b) 108.1 . . . no N(4) C(3) C(2) 108(1) . . . ? N(4) C(3) H(3a) 109.7 . . . no N(4) C(3) H(3b) 109.7 . . . no C(2) C(3) H(3a) 114.5 . . . no C(2) C(3) H(3b) 112.8 . . . no H(3a) C(3) H(3b) 101.7 . . . no N(4) C(5) C(6) 111(1) . . . ? N(4) C(5) H(5a) 105.3 . . . no N(4) C(5) H(5b) 110.7 . . . no C(6) C(5) H(5a) 107.7 . . . no C(6) C(5) H(5b) 112.6 . . . no H(5a) C(5) H(5b) 109.4 . . . no N(7) C(6) C(5) 114(1) . . . ? N(7) C(6) H(6a) 107.5 . . . no N(7) C(6) H(6b) 104.4 . . . no C(5) C(6) H(6a) 113.3 . . . no C(5) C(6) H(6b) 111.5 . . . no H(6a) C(6) H(6b) 106.0 . . . no N(7) C(8) C(9) 111(1) . . . ? N(7) C(8) H(8a) 108.8 . . . no N(7) C(8) H(8b) 113.6 . . . no C(9) C(8) H(8a) 107.2 . . . no C(9) C(8) H(8b) 113.1 . . . no H(8a) C(8) H(8b) 102.9 . . . no N(10) C(9) C(8) 112(1) . . . ? N(10) C(9) H(9a) 113.6 . . . no N(10) C(9) H(9b) 109.7 . . . no C(8) C(9) H(9a) 110.6 . . . no C(8) C(9) H(9b) 102.2 . . . no H(9a) C(9) H(9b) 108.1 . . . no N(10) C(11) C(12) 112(1) . . . ? N(10) C(11) H(11a) 111.0 . . . no N(10) C(11) H(11b) 112.6 . . . no C(12) C(11) H(11a) 105.2 . . . no C(12) C(11) H(11b) 109.6 . . . no H(11a) C(11) H(11b) 106.3 . . . no N(13) C(12) C(11) 112(1) . . . ? N(13) C(12) H(12a) 108.7 . . . no N(13) C(12) H(12b) 113.0 . . . no C(11) C(12) H(12a) 106.9 . . . no C(11) C(12) H(12b) 111.5 . . . no H(12a) C(12) H(12b) 103.6 . . . no N(13) C(14) C(15) 112(1) . . . ? N(13) C(14) H(14b) 110.9 . . . no N(13) C(14) H(14a) 112.7 . . . no C(15) C(14) H(14b) 106.9 . . . no C(15) C(14) H(14a) 107.8 . . . no H(14b) C(14) H(14a) 106.6 . . . no N(16) C(15) C(14) 114(1) . . . ? N(16) C(15) H(15b) 106.7 . . . no N(16) C(15) H(15a) 111.5 . . . no C(14) C(15) H(15b) 108.7 . . . no C(14) C(15) H(15a) 108.1 . . . no H(15b) C(15) H(15a) 108.1 . . . no N(16) C(17) C(18) 111(1) . . . ? N(16) C(17) H(17b) 105.6 . . . no N(16) C(17) H(17a) 106.4 . . . no C(18) C(17) H(17b) 111.6 . . . no C(18) C(17) H(17a) 108.6 . . . no H(17b) C(17) H(17a) 113.7 . . . no N(1) C(18) C(17) 112(1) . . . ? N(1) C(18) H(18b) 104.9 . . . no N(1) C(18) H(18a) 110.4 . . . no C(17) C(18) H(18b) 109.8 . . . no C(17) C(18) H(18a) 111.5 . . . no H(18b) C(18) H(18a) 107.8 . . . no N(1) C(19) C(20) 114(1) . . . ? N(1) C(19) H(19b) 108.9 . . . no N(1) C(19) H(19a) 113.8 . . . no C(20) C(19) H(19b) 107.0 . . . no C(20) C(19) H(19a) 109.6 . . . no H(19b) C(19) H(19a) 103.3 . . . no N(21) C(20) C(19) 112(1) . . . ? N(21) C(20) H(20b) 105.7 . . . no N(21) C(20) H(20a) 110.3 . . . no C(19) C(20) H(20b) 107.5 . . . no C(19) C(20) H(20a) 114.8 . . . no H(20b) C(20) H(20a) 105.6 . . . no N(21) C(22) C(23) 114(1) . . . ? N(21) C(22) H(22b) 112.9 . . . no N(21) C(22) H(22a) 111.3 . . . no C(23) C(22) H(22b) 106.8 . . . no C(23) C(22) H(22a) 107.2 . . . no H(22b) C(22) H(22a) 104.4 . . . no N(24) C(23) C(22) 111(1) . . . ? N(24) C(23) H(23b) 110.7 . . . no N(24) C(23) H(23a) 110.8 . . . no C(22) C(23) H(23b) 112.3 . . . no C(22) C(23) H(23a) 108.3 . . . no H(23b) C(23) H(23a) 103.8 . . . no N(24) C(25) C(26) 110(1) . . . ? N(24) C(25) H(25b) 111.7 . . . no N(24) C(25) H(25a) 109.4 . . . no C(26) C(25) H(25b) 111.0 . . . no C(26) C(25) H(25a) 110.4 . . . no H(25b) C(25) H(25a) 104.2 . . . no N(10) C(26) C(25) 115(1) . . . ? N(10) C(26) H(26b) 107.7 . . . no N(10) C(26) H(26a) 105.5 . . . no C(25) C(26) H(26b) 108.7 . . . no C(25) C(26) H(26a) 109.9 . . . no H(26b) C(26) H(26a) 110.0 . . . 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 Cl(1) N(7) 2.99(1) . . no Cl(1) N(4) 3.04(1) . . no Cl(1) N(24) 3.09(1) . . no Cl(1) N(16) 3.088(9) . . no Cl(1) N(21) 3.13(1) . . no Cl(1) N(13) 3.18(1) . . no Cl(1) N(1) 3.27(1) . . no Cl(1) N(10) 3.32(1) . . no Cl(1) Cl(2) 3.467(5) . . no Cl(1) C(6) 3.51(1) . . no Cl(1) C(5) 3.51(1) . . no Cl(2) N(13) 3.23(1) . . no Cl(2) N(21) 3.24(1) . . no Cl(2) C(23) 3.41(1) . . no Cl(2) N(24) 3.60(1) . . no Cl(3) O(300) 3.13(2) . . no Cl(3) N(24) 3.15(1) . . no Cl(4) O(100) 3.05(1) . . no Cl(4) N(13) 3.13(1) . 1_556 no Cl(4) O(200) 3.32(1) . 2_455 no Cl(5) N(7) 2.99(1) . 3_556 no Cl(5) O(300) 3.16(1) . . no Cl(5) O(200) 3.33(1) . 3_556 no Cl(5) C(2) 3.55(1) . 4_556 no Cl(6) N(16) 3.10(1) . . no O(100) O(300) 2.67(2) . . no O(100) N(4) 2.86(1) . . no O(200) N(21) 3.01(2) . 1_455 no O(200) O(300) 3.24(2) . 3_456 no O(200) C(20) 3.38(2) . 1_455 no O(200) C(15) 3.40(2) . 2_455 no O(200) C(19) 3.42(2) . 1_455 no O(300) C(23) 3.11(2) . 3_456 no O(300) C(22) 3.21(2) . 3_456 no O(300) N(21) 3.53(2) . 3_456 no O(300) N(7) 3.59(2) . 3_556 no C(18) C(26) 3.47(2) . 4_545 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 N(1) C(2) C(3) N(4) . . . . -76(1) no N(1) C(18) C(17) N(16) . . . . -68(1) no N(1) C(19) C(20) N(21) . . . . -77(2) no N(4) C(5) C(6) N(7) . . . . 96(1) no N(7) C(8) C(9) N(10) . . . . -70(1) no N(10) C(11) C(12) N(13) . . . . -84(1) no N(10) C(26) C(25) N(24) . . . . -65(1) no N(13) C(14) C(15) N(16) . . . . 93(1) no N(21) C(22) C(23) N(24) . . . . 88(1) no C(2) N(1) C(18) C(17) . . . . 153(1) no C(2) N(1) C(19) C(20) . . . . -80(1) no C(2) C(3) N(4) C(5) . . . . 171(1) no C(3) N(4) C(5) C(6) . . . . -173(1) no C(3) C(2) N(1) C(18) . . . . -82(1) no C(3) C(2) N(1) C(19) . . . . 157(1) no C(5) C(6) N(7) C(8) . . . . -178(1) no C(6) N(7) C(8) C(9) . . . . 176(1) no C(8) C(9) N(10) C(11) . . . . 155(1) no C(8) C(9) N(10) C(26) . . . . -84(1) no C(9) N(10) C(11) C(12) . . . . -77(1) no C(9) N(10) C(26) C(25) . . . . 159(1) no C(11) N(10) C(26) C(25) . . . . -79(1) no C(11) C(12) N(13) C(14) . . . . 169(1) no C(12) N(13) C(14) C(15) . . . . -172(1) no C(12) C(11) N(10) C(26) . . . . 162(1) no C(14) C(15) N(16) C(17) . . . . -170.4(9) no C(15) N(16) C(17) C(18) . . . . -178(1) no C(17) C(18) N(1) C(19) . . . . -86(1) no C(18) N(1) C(19) C(20) . . . . 159(1) no C(19) C(20) N(21) C(22) . . . . 170(1) no C(20) N(21) C(22) C(23) . . . . -175(1) no C(22) C(23) N(24) C(25) . . . . -174.7(9) no C(23) N(24) C(25) C(26) . . . . -175(1) 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 #==============================================================================