Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_contact_author_name ' Keita Tani ' _publ_contact_author_address ; Division of Natural Science Osaka Kyoiku University Asahigaoka Kashiwara Osaka 582 8582 JAPAN ; _publ_contact_author_email ' ktani@cc.osaka-kyoiku.ac.jp ' _publ_contact_author_fax ' +81-729-78-3554 ' _publ_contact_author_phone ' +81-729-78-3648 ' _publ_contact_letter ;? ; _publ_requested_journal 'Chemical Communications ' _publ_requested_category ' CO' _publ_requested_coeditor_name ' Hideo Ohkita, Masahide Yamamoto ' _publ_section_title ; Synthesis and Photophysical Properties of [3.3](3,9)Carbazolophanes ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name #_publ_author_address 'Ito, Shinzaburo' 'Ohkita, Hideo' 'Takemura, Hiroyuki' 'Tani, Keita' 'Tohda, Yasuo' 'Yamamoto, Masahide' _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; data_syn-[3.3](3,9)carbazolophane _database_code_CSD 151872 #--------------------------------------------------------------------------- _audit_creation_date 'Tue Sep 13 10:50:12 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #--------------------------------------------------------------------------- _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SIR88 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #--------------------------------------------------------------------------- _chemical_compound_source ? _chemical_name_common 'syn-[3.3](3,9)carbazolophane' _chemical_formula_weight 479.60 _chemical_formula_analytical ? _chemical_formula_sum 'C33 H27 N4 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point 270-271 C #--------------------------------------------------------------------------- _cell_length_a 14.035(5) _cell_length_b 11.706(4) _cell_length_c 15.041(4) _cell_angle_alpha 90 _cell_angle_beta 92.14(3) _cell_angle_gamma 90 _cell_volume 2469(1) _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.1 _cell_measurement_theta_max 12.4 #--------------------------------------------------------------------------- #-- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z #--------------------------------------------------------------------------- #-- _exptl_crystal_description 'column' _exptl_crystal_colour 'pale' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012.00 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details '(Walker & Stuart, 1983)' _exptl_absorpt_correction_T_min 0.789 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; #--------------------------------------------------------------------------- #-- _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.50 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 1 3 -3 1 1 -3 0 0 _diffrn_reflns_number 5906 _reflns_number_total 5680 _reflns_number_gt 1675 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_av_sigmaI/netI 0.216 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.06310 _diffrn_orient_matrix_UB_12 -0.03471 _diffrn_orient_matrix_UB_13 0.01309 _diffrn_orient_matrix_UB_21 0.02320 _diffrn_orient_matrix_UB_22 -0.01566 _diffrn_orient_matrix_UB_23 0.06248 _diffrn_orient_matrix_UB_31 -0.02387 _diffrn_orient_matrix_UB_32 0.07647 _diffrn_orient_matrix_UB_33 0.01874 #--------------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #--------------------------------------------------------------------------- loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N(1) N 0.2133(2) -0.0065(3) 0.2647(2) 0.051(1) Uani 1.00 d . . . N(2) N 0.0924(2) -0.0083(3) 0.0767(2) 0.052(1) Uani 1.00 d . . . N(3) N 0.2289(2) -0.5105(3) 0.1208(2) 0.063(1) Uani 1.00 d . . . N(4) N 0.0988(3) -0.6100(3) 0.1965(3) 0.106(2) Uani 1.00 d . . . C(1) C 0.2289(3) -0.1226(4) 0.2561(2) 0.046(1) Uani 1.00 d . . . C(2) C 0.3176(3) -0.1391(4) 0.2156(2) 0.047(1) Uani 1.00 d . . . C(3) C 0.3441(3) -0.2500(4) 0.1920(3) 0.054(1) Uani 1.00 d . . . C(4) C 0.2857(3) -0.3407(4) 0.2115(3) 0.056(1) Uani 1.00 d . . . C(5) C 0.2031(3) -0.3226(4) 0.2601(3) 0.058(2) Uani 1.00 d . . . C(6) C 0.1738(3) -0.2145(4) 0.2815(2) 0.053(1) Uani 1.00 d . . . C(7) C 0.2912(3) 0.0525(4) 0.2338(2) 0.050(1) Uani 1.00 d . . . C(8) C 0.3575(3) -0.0277(4) 0.2027(2) 0.050(1) Uani 1.00 d . . . C(9) C 0.4430(3) 0.0119(4) 0.1702(3) 0.064(2) Uani 1.00 d . . . C(10) C 0.4615(3) 0.1278(5) 0.1693(3) 0.074(2) Uani 1.00 d . . . C(11) C 0.3947(4) 0.2052(4) 0.2000(3) 0.070(2) Uani 1.00 d . . . C(12) C 0.3092(3) 0.1698(4) 0.2324(3) 0.057(2) Uani 1.00 d . . . C(13) C 0.1031(3) -0.1249(4) 0.0634(2) 0.050(1) Uani 1.00 d . . . C(14) C 0.1844(3) -0.1424(4) 0.0133(2) 0.050(1) Uani 1.00 d . . . C(15) C 0.2160(3) -0.2540(4) -0.0006(3) 0.059(2) Uani 1.00 d . . . C(16) C 0.1646(3) -0.3447(4) 0.0315(3) 0.061(2) Uani 1.00 d . . . C(17) C 0.0780(3) -0.3239(4) 0.0726(3) 0.064(2) Uani 1.00 d . . . C(18) C 0.0471(3) -0.2150(4) 0.0903(3) 0.056(1) Uani 1.00 d . . . C(19) C 0.1620(3) 0.0502(4) 0.0310(2) 0.051(1) Uani 1.00 d . . . C(20) C 0.2211(3) -0.0311(4) -0.0090(2) 0.050(1) Uani 1.00 d . . . C(21) C 0.2964(3) 0.0076(4) -0.0592(3) 0.067(2) Uani 1.00 d . . . C(22) C 0.3112(3) 0.1222(5) -0.0697(3) 0.075(2) Uani 1.00 d . . . C(23) C 0.2513(4) 0.2009(4) -0.0292(3) 0.071(2) Uani 1.00 d . . . C(24) C 0.1762(3) 0.1659(4) 0.0208(3) 0.062(2) Uani 1.00 d . . . C(25) C 0.1223(3) 0.0450(4) 0.2894(2) 0.051(1) Uani 1.00 d . . . C(26) C 0.0690(3) 0.1088(4) 0.2150(3) 0.058(1) Uani 1.00 d . . . C(27) C 0.0253(3) 0.0446(4) 0.1364(3) 0.058(1) Uani 1.00 d . . . C(28) C 0.3067(3) -0.4599(4) 0.1783(3) 0.071(2) Uani 1.00 d . . . C(29) C 0.2051(4) -0.4643(5) 0.0309(3) 0.076(2) Uani 1.00 d . . . C(30) C 0.1585(3) -0.5626(4) 0.1617(3) 0.070(2) Uani 1.00 d . . . C(31) C 0.4853(4) 0.1160(4) 0.5041(4) 0.081(2) Uani 1.00 d . . . C(32) C 0.4482(3) 0.0542(6) 0.4335(3) 0.075(2) Uani 1.00 d . . . C(33) C 0.4626(4) -0.0608(6) 0.4290(3) 0.076(2) Uani 1.00 d . . . H(1) H 0.404(2) -0.261(3) 0.160(2) 0.0864 Uiso 1.00 calc . . . H(2) H 0.168(2) -0.392(3) 0.279(2) 0.0864 Uiso 1.00 calc . . . H(3) H 0.113(2) -0.200(3) 0.315(2) 0.0864 Uiso 1.00 calc . . . H(4) H 0.489(3) -0.048(3) 0.145(2) 0.0864 Uiso 1.00 calc . . . H(5) H 0.520(3) 0.161(3) 0.136(2) 0.0864 Uiso 1.00 calc . . . H(6) H 0.409(3) 0.292(3) 0.199(2) 0.0864 Uiso 1.00 calc . . . H(7) H 0.259(3) 0.223(3) 0.256(2) 0.0864 Uiso 1.00 calc . . . H(8) H 0.279(3) -0.269(3) -0.028(2) 0.0864 Uiso 1.00 calc . . . H(9) H 0.039(3) -0.390(3) 0.087(2) 0.0864 Uiso 1.00 calc . . . H(10) H -0.015(2) -0.198(3) 0.121(2) 0.0864 Uiso 1.00 calc . . . H(11) H 0.334(3) -0.047(3) -0.083(2) 0.0864 Uiso 1.00 calc . . . H(12) H 0.367(3) 0.159(3) -0.107(2) 0.0864 Uiso 1.00 calc . . . H(13) H 0.258(3) 0.280(3) -0.037(2) 0.0811 Uiso 1.00 calc . . . H(14) H 0.132(3) 0.224(3) 0.048(2) 0.0864 Uiso 1.00 calc . . . H(15) H 0.080(2) -0.022(3) 0.312(2) 0.0864 Uiso 1.00 calc . . . H(16) H 0.134(2) 0.104(3) 0.342(2) 0.0864 Uiso 1.00 calc . . . H(17) H 0.114(2) 0.178(3) 0.196(2) 0.0654 Uiso 1.00 calc . . . H(18) H 0.013(2) 0.153(3) 0.244(2) 0.0654 Uiso 1.00 calc . . . H(19) H -0.018(2) 0.100(3) 0.101(2) 0.0734 Uiso 1.00 calc . . . H(20) H -0.021(2) -0.020(3) 0.159(2) 0.0734 Uiso 1.00 calc . . . H(21) H 0.318(3) -0.517(3) 0.228(2) 0.0864 Uiso 1.00 calc . . . H(22) H 0.363(3) -0.461(3) 0.140(2) 0.0864 Uiso 1.00 calc . . . H(23) H 0.272(3) -0.466(3) -0.001(2) 0.0844 Uiso 1.00 calc . . . H(24) H 0.166(3) -0.522(3) 0.003(2) 0.0844 Uiso 1.00 calc . . . H(25) H 0.476(3) 0.199(3) 0.511(3) 0.0864 Uiso 1.00 calc . . . H(26) H 0.411(3) 0.095(3) 0.388(2) 0.0925 Uiso 1.00 calc . . . H(27) H 0.438(3) -0.107(4) 0.382(2) 0.0929 Uiso 1.00 calc . . . 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 N(1) 0.047(2) 0.056(2) 0.051(2) 0.009(2) -0.002(2) -0.003(2) N(2) 0.048(2) 0.068(3) 0.040(2) 0.010(2) 0.003(2) 0.000(2) N(3) 0.069(2) 0.050(2) 0.072(3) -0.001(2) 0.014(2) -0.002(2) N(4) 0.113(4) 0.062(3) 0.145(4) -0.008(3) 0.054(3) -0.002(3) C(1) 0.046(3) 0.052(3) 0.040(2) 0.007(2) -0.006(2) 0.001(2) C(2) 0.043(3) 0.051(3) 0.046(2) 0.007(2) -0.006(2) -0.003(2) C(3) 0.041(3) 0.057(3) 0.064(3) 0.005(3) -0.001(2) -0.003(2) C(4) 0.049(3) 0.050(3) 0.069(3) 0.010(2) -0.003(2) -0.007(2) C(5) 0.057(3) 0.055(3) 0.064(3) 0.000(2) 0.003(2) 0.004(2) C(6) 0.051(3) 0.057(3) 0.051(3) 0.003(3) 0.001(2) -0.003(2) C(7) 0.044(2) 0.059(3) 0.046(2) 0.004(3) -0.009(2) 0.000(2) C(8) 0.040(2) 0.057(3) 0.053(3) 0.004(2) -0.005(2) -0.005(2) C(9) 0.051(3) 0.060(4) 0.080(3) 0.005(3) 0.005(2) -0.001(3) C(10) 0.065(3) 0.072(4) 0.085(3) -0.012(3) 0.012(3) 0.005(3) C(11) 0.068(3) 0.063(3) 0.080(3) -0.007(3) -0.005(3) 0.003(3) C(12) 0.057(3) 0.051(3) 0.063(3) 0.004(2) -0.002(2) 0.001(2) C(13) 0.048(3) 0.060(3) 0.042(2) 0.012(3) -0.001(2) 0.000(2) C(14) 0.050(3) 0.062(3) 0.038(2) 0.006(3) 0.003(2) -0.001(2) C(15) 0.062(3) 0.074(4) 0.041(2) 0.006(3) 0.008(2) -0.001(2) C(16) 0.069(3) 0.069(3) 0.047(2) 0.008(3) 0.009(2) -0.002(2) C(17) 0.068(3) 0.067(4) 0.056(3) -0.006(3) 0.004(3) 0.003(3) C(18) 0.050(3) 0.073(3) 0.046(3) 0.002(3) 0.001(2) 0.005(3) C(19) 0.048(3) 0.066(4) 0.038(2) 0.004(3) -0.005(2) 0.000(2) C(20) 0.047(2) 0.064(3) 0.038(2) 0.008(3) 0.000(2) -0.002(2) C(21) 0.063(3) 0.078(4) 0.060(3) 0.005(3) 0.014(2) 0.003(3) C(22) 0.071(3) 0.078(4) 0.077(3) -0.004(3) 0.019(3) 0.011(3) C(23) 0.076(3) 0.064(3) 0.074(3) -0.002(3) 0.003(3) 0.006(3) C(24) 0.060(3) 0.070(4) 0.057(3) 0.006(3) 0.003(2) 0.000(3) C(25) 0.047(2) 0.061(3) 0.047(2) 0.013(2) 0.005(2) -0.006(2) C(26) 0.052(3) 0.064(3) 0.057(3) 0.020(2) 0.004(2) -0.004(2) C(27) 0.042(2) 0.084(4) 0.049(3) 0.017(2) 0.003(2) -0.007(3) C(28) 0.060(3) 0.056(3) 0.097(4) 0.005(3) 0.002(3) -0.003(3) C(29) 0.091(4) 0.074(4) 0.062(3) 0.002(3) 0.019(3) -0.011(3) C(30) 0.083(4) 0.040(3) 0.088(3) 0.001(3) 0.018(3) -0.004(3) C(31) 0.088(4) 0.087(4) 0.067(3) 0.016(4) -0.002(3) 0.000(4) C(32) 0.069(3) 0.100(5) 0.054(3) 0.017(3) -0.003(2) 0.008(3) C(33) 0.070(3) 0.100(5) 0.059(4) 0.002(3) -0.001(3) -0.014(3) #--------------------------------------------------------------------------- #-- _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00001|Fo|^2^]' _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0014(1) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1675 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0369 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0264 _refine_ls_wR_factor_gt 0.0264 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.360 _refine_ls_shift/su_max 0.0020 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.12 _refine_diff_density_max 0.14 #--------------------------------------------------------------------------- _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 N(1) C(1) 1.383(5) 1_555 1_555 yes N(1) C(7) 1.388(4) 1_555 1_555 yes N(1) C(25) 1.472(4) 1_555 1_555 yes N(2) C(13) 1.389(5) 1_555 1_555 yes N(2) C(19) 1.394(4) 1_555 1_555 yes N(2) C(27) 1.463(4) 1_555 1_555 yes N(3) C(28) 1.490(5) 1_555 1_555 yes N(3) C(29) 1.483(5) 1_555 1_555 yes N(3) C(30) 1.330(5) 1_555 1_555 yes N(4) C(30) 1.148(5) 1_555 1_555 yes C(1) C(2) 1.420(5) 1_555 1_555 yes C(1) C(6) 1.387(5) 1_555 1_555 yes C(2) C(3) 1.400(5) 1_555 1_555 yes C(2) C(8) 1.436(5) 1_555 1_555 yes C(3) C(4) 1.380(5) 1_555 1_555 yes C(4) C(5) 1.410(5) 1_555 1_555 yes C(4) C(28) 1.514(6) 1_555 1_555 yes C(5) C(6) 1.372(5) 1_555 1_555 yes C(7) C(8) 1.413(5) 1_555 1_555 yes C(7) C(12) 1.397(5) 1_555 1_555 yes C(8) C(9) 1.392(5) 1_555 1_555 yes C(9) C(10) 1.382(6) 1_555 1_555 yes C(10) C(11) 1.395(6) 1_555 1_555 yes C(11) C(12) 1.376(6) 1_555 1_555 yes C(13) C(14) 1.406(5) 1_555 1_555 yes C(13) C(18) 1.385(5) 1_555 1_555 yes C(14) C(15) 1.398(5) 1_555 1_555 yes C(14) C(20) 1.445(5) 1_555 1_555 yes C(15) C(16) 1.382(5) 1_555 1_555 yes C(16) C(17) 1.404(5) 1_555 1_555 yes C(16) C(29) 1.510(6) 1_555 1_555 yes C(17) C(18) 1.376(5) 1_555 1_555 yes C(19) C(20) 1.412(5) 1_555 1_555 yes C(19) C(24) 1.378(5) 1_555 1_555 yes C(20) C(21) 1.397(5) 1_555 1_555 yes C(21) C(22) 1.367(6) 1_555 1_555 yes C(22) C(23) 1.401(6) 1_555 1_555 yes C(23) C(24) 1.381(6) 1_555 1_555 yes C(25) C(26) 1.519(5) 1_555 1_555 yes C(26) C(27) 1.512(5) 1_555 1_555 yes C(31) C(32) 1.370(6) 1_555 1_555 yes C(31) C(33) 1.383(6) 1_555 3_656 yes C(32) C(33) 1.363(6) 1_555 1_555 yes #--------------------------------------------------------------------------- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(1) N(1) C(7) 109.2(3) 1_555 1_555 1_555 yes C(1) N(1) C(25) 124.6(3) 1_555 1_555 1_555 yes C(7) N(1) C(25) 125.6(3) 1_555 1_555 1_555 yes C(13) N(2) C(19) 109.3(3) 1_555 1_555 1_555 yes C(13) N(2) C(27) 125.4(3) 1_555 1_555 1_555 yes C(19) N(2) C(27) 125.0(4) 1_555 1_555 1_555 yes C(28) N(3) C(29) 121.3(4) 1_555 1_555 1_555 yes C(28) N(3) C(30) 117.0(4) 1_555 1_555 1_555 yes C(29) N(3) C(30) 116.3(4) 1_555 1_555 1_555 yes N(1) C(1) C(2) 108.6(4) 1_555 1_555 1_555 yes N(1) C(1) C(6) 130.2(4) 1_555 1_555 1_555 yes C(2) C(1) C(6) 121.3(4) 1_555 1_555 1_555 yes C(1) C(2) C(3) 118.8(4) 1_555 1_555 1_555 yes C(1) C(2) C(8) 106.6(3) 1_555 1_555 1_555 yes C(3) C(2) C(8) 134.4(4) 1_555 1_555 1_555 yes C(2) C(3) C(4) 119.6(4) 1_555 1_555 1_555 yes C(2) C(3) H(1) 118(2) 1_555 1_555 1_555 no C(4) C(3) H(1) 121(2) 1_555 1_555 1_555 no C(3) C(4) C(5) 120.1(4) 1_555 1_555 1_555 yes C(3) C(4) C(28) 121.0(4) 1_555 1_555 1_555 yes C(5) C(4) C(28) 118.9(4) 1_555 1_555 1_555 yes C(4) C(5) C(6) 121.3(4) 1_555 1_555 1_555 yes C(4) C(5) H(2) 116(2) 1_555 1_555 1_555 no C(6) C(5) H(2) 121(2) 1_555 1_555 1_555 no C(1) C(6) C(5) 118.5(4) 1_555 1_555 1_555 yes C(1) C(6) H(3) 119(2) 1_555 1_555 1_555 no C(5) C(6) H(3) 122(2) 1_555 1_555 1_555 no N(1) C(7) C(8) 108.5(4) 1_555 1_555 1_555 yes N(1) C(7) C(12) 129.8(4) 1_555 1_555 1_555 yes C(8) C(7) C(12) 121.7(4) 1_555 1_555 1_555 yes C(2) C(8) C(7) 107.1(3) 1_555 1_555 1_555 yes C(2) C(8) C(9) 134.1(4) 1_555 1_555 1_555 yes C(7) C(8) C(9) 118.8(4) 1_555 1_555 1_555 yes C(8) C(9) C(10) 119.7(4) 1_555 1_555 1_555 yes C(8) C(9) H(4) 117(2) 1_555 1_555 1_555 no C(10) C(9) H(4) 123(2) 1_555 1_555 1_555 no C(9) C(10) C(11) 120.3(4) 1_555 1_555 1_555 yes C(9) C(10) H(5) 121(2) 1_555 1_555 1_555 no C(11) C(10) H(5) 117(2) 1_555 1_555 1_555 no C(10) C(11) C(12) 121.9(4) 1_555 1_555 1_555 yes C(10) C(11) H(6) 119(2) 1_555 1_555 1_555 no C(12) C(11) H(6) 118(2) 1_555 1_555 1_555 no C(7) C(12) C(11) 117.5(4) 1_555 1_555 1_555 yes C(7) C(12) H(7) 118(2) 1_555 1_555 1_555 no C(11) C(12) H(7) 124(2) 1_555 1_555 1_555 no N(2) C(13) C(14) 108.3(4) 1_555 1_555 1_555 yes N(2) C(13) C(18) 129.9(4) 1_555 1_555 1_555 yes C(14) C(13) C(18) 121.8(4) 1_555 1_555 1_555 yes C(13) C(14) C(15) 119.0(4) 1_555 1_555 1_555 yes C(13) C(14) C(20) 107.3(4) 1_555 1_555 1_555 yes C(15) C(14) C(20) 133.6(4) 1_555 1_555 1_555 yes C(14) C(15) C(16) 119.6(4) 1_555 1_555 1_555 yes C(14) C(15) H(8) 120(2) 1_555 1_555 1_555 no C(16) C(15) H(8) 119(2) 1_555 1_555 1_555 no C(15) C(16) C(17) 119.5(4) 1_555 1_555 1_555 yes C(15) C(16) C(29) 120.6(4) 1_555 1_555 1_555 yes C(17) C(16) C(29) 119.7(4) 1_555 1_555 1_555 yes C(16) C(17) C(18) 122.0(4) 1_555 1_555 1_555 yes C(16) C(17) H(9) 117(2) 1_555 1_555 1_555 no C(18) C(17) H(9) 120(2) 1_555 1_555 1_555 no C(13) C(18) C(17) 117.5(4) 1_555 1_555 1_555 yes C(13) C(18) H(10) 119(2) 1_555 1_555 1_555 no C(17) C(18) H(10) 123(2) 1_555 1_555 1_555 no N(2) C(19) C(20) 108.2(4) 1_555 1_555 1_555 yes N(2) C(19) C(24) 130.1(4) 1_555 1_555 1_555 yes C(20) C(19) C(24) 121.7(4) 1_555 1_555 1_555 yes C(14) C(20) C(19) 106.7(4) 1_555 1_555 1_555 yes C(14) C(20) C(21) 134.6(4) 1_555 1_555 1_555 yes C(19) C(20) C(21) 118.7(4) 1_555 1_555 1_555 yes C(20) C(21) C(22) 120.1(4) 1_555 1_555 1_555 yes C(20) C(21) H(11) 116(2) 1_555 1_555 1_555 no C(22) C(21) H(11) 123(2) 1_555 1_555 1_555 no C(21) C(22) C(23) 119.9(5) 1_555 1_555 1_555 yes C(21) C(22) H(12) 125(2) 1_555 1_555 1_555 no C(23) C(22) H(12) 114(2) 1_555 1_555 1_555 no C(22) C(23) C(24) 121.6(5) 1_555 1_555 1_555 yes C(22) C(23) H(13) 121(2) 1_555 1_555 1_555 no C(24) C(23) H(13) 116(2) 1_555 1_555 1_555 no C(19) C(24) C(23) 117.9(4) 1_555 1_555 1_555 yes C(19) C(24) H(14) 121(2) 1_555 1_555 1_555 no C(23) C(24) H(14) 120(2) 1_555 1_555 1_555 no N(1) C(25) C(26) 115.0(3) 1_555 1_555 1_555 yes N(1) C(25) H(15) 106(1) 1_555 1_555 1_555 no N(1) C(25) H(16) 109(1) 1_555 1_555 1_555 no C(26) C(25) H(15) 109(2) 1_555 1_555 1_555 no C(26) C(25) H(16) 106(1) 1_555 1_555 1_555 no H(15) C(25) H(16) 109(2) 1_555 1_555 1_555 no C(25) C(26) C(27) 120.4(4) 1_555 1_555 1_555 yes C(25) C(26) H(17) 106(1) 1_555 1_555 1_555 no C(25) C(26) H(18) 106(1) 1_555 1_555 1_555 no C(27) C(26) H(17) 113(1) 1_555 1_555 1_555 no C(27) C(26) H(18) 106(1) 1_555 1_555 1_555 no H(17) C(26) H(18) 101(2) 1_555 1_555 1_555 no N(2) C(27) C(26) 116.0(3) 1_555 1_555 1_555 yes N(2) C(27) H(19) 109(1) 1_555 1_555 1_555 no N(2) C(27) H(20) 107(1) 1_555 1_555 1_555 no C(26) C(27) H(19) 107(1) 1_555 1_555 1_555 no C(26) C(27) H(20) 109(1) 1_555 1_555 1_555 no H(19) C(27) H(20) 105(2) 1_555 1_555 1_555 no N(3) C(28) C(4) 114.3(4) 1_555 1_555 1_555 yes N(3) C(28) H(21) 104(2) 1_555 1_555 1_555 no N(3) C(28) H(22) 103(2) 1_555 1_555 1_555 no C(4) C(28) H(21) 113(2) 1_555 1_555 1_555 no C(4) C(28) H(22) 111(2) 1_555 1_555 1_555 no H(21) C(28) H(22) 108(3) 1_555 1_555 1_555 no N(3) C(29) C(16) 113.9(4) 1_555 1_555 1_555 yes N(3) C(29) H(23) 103(2) 1_555 1_555 1_555 no N(3) C(29) H(24) 104(2) 1_555 1_555 1_555 no C(16) C(29) H(23) 110(2) 1_555 1_555 1_555 no C(16) C(29) H(24) 116(2) 1_555 1_555 1_555 no H(23) C(29) H(24) 107(3) 1_555 1_555 1_555 no N(3) C(30) N(4) 178.4(5) 1_555 1_555 1_555 yes C(32) C(31) C(33) 119.5(5) 1_555 1_555 3_656 yes C(32) C(31) H(25) 123(2) 1_555 1_555 1_555 no C(33) C(31) H(25) 116(2) 3_656 1_555 1_555 no C(31) C(32) C(33) 120.5(5) 1_555 1_555 1_555 yes C(31) C(32) H(26) 117(2) 1_555 1_555 1_555 no C(33) C(32) H(26) 121(2) 1_555 1_555 1_555 no C(31) C(33) C(32) 120.0(5) 3_656 1_555 1_555 yes C(31) C(33) H(27) 116(2) 3_656 1_555 1_555 no C(32) C(33) H(27) 123(2) 1_555 1_555 1_555 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N(1) C(1) C(2) C(3) -173.7(3) 1_555 1_555 1_555 1_555 yes N(1) C(1) C(2) C(8) 2.1(4) 1_555 1_555 1_555 1_555 yes N(1) C(1) C(6) C(5) 176.1(4) 1_555 1_555 1_555 1_555 yes N(1) C(7) C(8) C(2) -0.1(4) 1_555 1_555 1_555 1_555 yes N(1) C(7) C(8) C(9) -178.6(3) 1_555 1_555 1_555 1_555 yes N(1) C(7) C(12) C(11) 178.1(4) 1_555 1_555 1_555 1_555 yes N(1) C(25) C(26) C(27) 68.6(5) 1_555 1_555 1_555 1_555 yes N(2) C(13) C(14) C(15) 173.1(3) 1_555 1_555 1_555 1_555 yes N(2) C(13) C(14) C(20) -3.5(4) 1_555 1_555 1_555 1_555 yes N(2) C(13) C(18) C(17) -175.9(4) 1_555 1_555 1_555 1_555 yes N(2) C(19) C(20) C(14) 0.5(4) 1_555 1_555 1_555 1_555 yes N(2) C(19) C(20) C(21) 179.7(3) 1_555 1_555 1_555 1_555 yes N(2) C(19) C(24) C(23) -179.4(4) 1_555 1_555 1_555 1_555 yes N(2) C(27) C(26) C(25) -68.1(5) 1_555 1_555 1_555 1_555 yes N(3) C(28) C(4) C(3) -120.7(4) 1_555 1_555 1_555 1_555 yes N(3) C(28) C(4) C(5) 56.8(5) 1_555 1_555 1_555 1_555 yes N(3) C(29) C(16) C(15) 111.7(5) 1_555 1_555 1_555 1_555 yes N(3) C(29) C(16) C(17) -62.3(6) 1_555 1_555 1_555 1_555 yes N(4) C(30) N(3) C(28) -102(19) 1_555 1_555 1_555 1_555 yes N(4) C(30) N(3) C(29) 103(19) 1_555 1_555 1_555 1_555 yes C(1) N(1) C(7) C(8) 1.4(4) 1_555 1_555 1_555 1_555 yes C(1) N(1) C(7) C(12) -177.3(4) 1_555 1_555 1_555 1_555 yes C(1) N(1) C(25) C(26) -109.5(4) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) -2.6(6) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(8) C(7) -1.2(4) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(8) C(9) 176.9(4) 1_555 1_555 1_555 1_555 yes C(1) C(6) C(5) C(4) -1.7(6) 1_555 1_555 1_555 1_555 yes C(2) C(1) N(1) C(7) -2.2(4) 1_555 1_555 1_555 1_555 yes C(2) C(1) N(1) C(25) 169.1(3) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(6) C(5) -5.2(6) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) -4.1(6) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(28) 173.4(4) 1_555 1_555 1_555 1_555 yes C(2) C(8) C(7) C(12) 178.7(3) 1_555 1_555 1_555 1_555 yes C(2) C(8) C(9) C(10) -177.7(4) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(6) 7.3(5) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(8) C(7) 173.5(4) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(8) C(9) -8.3(8) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) 6.4(6) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(2) C(8) -176.8(4) 1_555 1_555 1_555 1_555 yes C(4) C(28) N(3) C(29) 68.3(5) 1_555 1_555 1_555 1_555 yes C(4) C(28) N(3) C(30) -84.8(5) 1_555 1_555 1_555 1_555 yes C(6) C(1) N(1) C(7) 176.7(4) 1_555 1_555 1_555 1_555 yes C(6) C(1) N(1) C(25) -12.0(6) 1_555 1_555 1_555 1_555 yes C(6) C(1) C(2) C(8) -176.9(3) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(4) C(28) -171.1(4) 1_555 1_555 1_555 1_555 yes C(7) N(1) C(25) C(26) 60.3(5) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) 0.3(6) 1_555 1_555 1_555 1_555 yes C(7) C(12) C(11) C(10) 0.2(7) 1_555 1_555 1_555 1_555 yes C(8) C(7) N(1) C(25) -169.7(3) 1_555 1_555 1_555 1_555 yes C(8) C(7) C(12) C(11) -0.5(6) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(11) -0.6(7) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(7) C(12) 0.2(6) 1_555 1_555 1_555 1_555 yes C(9) C(10) C(11) C(12) 0.4(7) 1_555 1_555 1_555 1_555 yes C(12) C(7) N(1) C(25) 11.6(6) 1_555 1_555 1_555 1_555 yes C(13) N(2) C(19) C(20) -2.7(4) 1_555 1_555 1_555 1_555 yes C(13) N(2) C(19) C(24) 176.0(4) 1_555 1_555 1_555 1_555 yes C(13) N(2) C(27) C(26) 114.6(4) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) 2.9(6) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(20) C(19) 1.8(4) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(20) C(21) -177.1(4) 1_555 1_555 1_555 1_555 yes C(13) C(18) C(17) C(16) 2.1(6) 1_555 1_555 1_555 1_555 yes C(14) C(13) N(2) C(19) 3.9(4) 1_555 1_555 1_555 1_555 yes C(14) C(13) N(2) C(27) -170.4(3) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(18) C(17) 5.2(6) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) 4.1(6) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(29) -169.9(4) 1_555 1_555 1_555 1_555 yes C(14) C(20) C(19) C(24) -178.4(4) 1_555 1_555 1_555 1_555 yes C(14) C(20) C(21) C(22) 178.2(4) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(18) -7.8(6) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(20) C(19) -174.1(4) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(20) C(21) 7.0(8) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(18) -6.7(6) 1_555 1_555 1_555 1_555 yes C(16) C(15) C(14) C(20) 178.4(4) 1_555 1_555 1_555 1_555 yes C(16) C(29) N(3) C(28) -66.3(5) 1_555 1_555 1_555 1_555 yes C(16) C(29) N(3) C(30) 86.9(5) 1_555 1_555 1_555 1_555 yes C(18) C(13) N(2) C(19) -175.1(4) 1_555 1_555 1_555 1_555 yes C(18) C(13) N(2) C(27) 10.6(6) 1_555 1_555 1_555 1_555 yes C(18) C(13) C(14) C(20) 175.6(3) 1_555 1_555 1_555 1_555 yes C(18) C(17) C(16) C(29) 167.3(4) 1_555 1_555 1_555 1_555 yes C(19) N(2) C(27) C(26) -58.8(5) 1_555 1_555 1_555 1_555 yes C(19) C(20) C(21) C(22) -0.7(6) 1_555 1_555 1_555 1_555 yes C(19) C(24) C(23) C(22) 0.8(7) 1_555 1_555 1_555 1_555 yes C(20) C(19) N(2) C(27) 171.6(3) 1_555 1_555 1_555 1_555 yes C(20) C(19) C(24) C(23) -0.8(6) 1_555 1_555 1_555 1_555 yes C(20) C(21) C(22) C(23) 0.6(7) 1_555 1_555 1_555 1_555 yes C(21) C(20) C(19) C(24) 0.8(6) 1_555 1_555 1_555 1_555 yes C(21) C(22) C(23) C(24) -0.7(7) 1_555 1_555 1_555 1_555 yes C(24) C(19) N(2) C(27) -9.7(6) 1_555 1_555 1_555 1_555 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 N(2) N(2) 3.412(6) 1_555 3_555 ? N(2) C(27) 3.576(5) 1_555 3_555 ? N(4) C(26) 3.332(6) 1_555 1_545 ? N(4) C(27) 3.599(6) 1_555 2_545 ? C(6) C(15) 3.330(5) 1_555 4_545 ? C(13) C(27) 3.571(5) 1_555 3_555 ? C(18) C(24) 3.543(6) 1_555 3_555 ? #--------------------------------------------------------------------------- #==END data_anti-[3.3](3,9)carbazolophane _database_code_CSD 151873 #--------------------------------------------------------------------------- _audit_creation_date 'Tue Sep 6 10:42:59 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #--------------------------------------------------------------------------- _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SAPI91 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #--------------------------------------------------------------------------- _chemical_compound_source ? _chemical_name_common 'anti-[3.3](3,9)carbazolophane' _chemical_formula_weight 440.55 _chemical_formula_analytical ? _chemical_formula_sum 'C30 H24 N4 ' _chemical_formula_moiety 'C30 H24 N4 ' _chemical_formula_structural ? _chemical_melting_point 242-243 C #--------------------------------------------------------------------------- _cell_length_a 7.888(8) _cell_length_b 19.486(10) _cell_length_c 14.567(7) _cell_angle_alpha 90 _cell_angle_beta 91.09(6) _cell_angle_gamma 90 _cell_volume 2238(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.0 _cell_measurement_theta_max 12.5 #--------------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,-z -x,-y,-z 1/2+x,1/2-y,z #--------------------------------------------------------------------------- _exptl_crystal_description 'column' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.180 _exptl_crystal_density_diffrn 1.307 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928.00 _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #--------------------------------------------------------------------------- _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.63 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 2 -1 -1 3 -2 0 2 -2 _diffrn_reflns_number 5516 _reflns_number_total 5145 _reflns_number_gt 2325 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_av_sigmaI/netI 0.128 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.02553 _diffrn_orient_matrix_UB_12 0.05009 _diffrn_orient_matrix_UB_13 -0.00594 _diffrn_orient_matrix_UB_21 -0.00658 _diffrn_orient_matrix_UB_22 0.00378 _diffrn_orient_matrix_UB_23 0.06830 _diffrn_orient_matrix_UB_31 0.12403 _diffrn_orient_matrix_UB_32 0.01051 _diffrn_orient_matrix_UB_33 0.00374 #--------------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #--------------------------------------------------------------------------- loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N(1) N 1.2557(2) 0.0565(1) 0.1815(1) 0.0450(7) Uani 1.00 d . . . N(2) N 0.9490(3) -0.0671(1) 0.1804(1) 0.0447(7) Uani 1.00 d . . . N(3) N 0.6717(3) 0.1544(1) 0.4416(2) 0.0504(7) Uani 1.00 d . . . N(4) N 0.6889(4) 0.0902(1) 0.5881(2) 0.087(1) Uani 1.00 d . . . C(1) C 1.1664(3) 0.0879(1) 0.2514(2) 0.0412(8) Uani 1.00 d . . . C(2) C 1.1097(3) 0.1531(1) 0.2218(2) 0.0430(8) Uani 1.00 d . . . C(3) C 0.9985(3) 0.1904(1) 0.2759(2) 0.0467(9) Uani 1.00 d . . . C(4) C 0.9509(3) 0.1640(1) 0.3599(2) 0.0449(9) Uani 1.00 d . . . C(5) C 1.0214(3) 0.1017(1) 0.3915(2) 0.0461(9) Uani 1.00 d . . . C(6) C 1.1270(3) 0.0626(1) 0.3380(2) 0.0441(8) Uani 1.00 d . . . C(7) C 1.2639(3) 0.1021(2) 0.1085(2) 0.0489(9) Uani 1.00 d . . . C(8) C 1.1739(3) 0.1624(1) 0.1302(2) 0.0477(9) Uani 1.00 d . . . C(9) C 1.1607(4) 0.2153(2) 0.0660(2) 0.060(1) Uani 1.00 d . . . C(10) C 1.2386(4) 0.2076(2) -0.0180(2) 0.071(1) Uani 1.00 d . . . C(11) C 1.3301(4) 0.1486(2) -0.0374(2) 0.071(1) Uani 1.00 d . . . C(12) C 1.3439(4) 0.0950(2) 0.0244(2) 0.061(1) Uani 1.00 d . . . C(13) C 0.8404(3) -0.0169(1) 0.2117(2) 0.0397(8) Uani 1.00 d . . . C(14) C 0.7716(3) -0.0384(1) 0.2959(2) 0.0377(8) Uani 1.00 d . . . C(15) C 0.6706(3) 0.0066(1) 0.3455(2) 0.0442(8) Uani 1.00 d . . . C(16) C 0.6383(3) 0.0717(1) 0.3109(2) 0.0466(9) Uani 1.00 d . . . C(17) C 0.6959(4) 0.0894(1) 0.2236(2) 0.0500(9) Uani 1.00 d . . . C(18) C 0.7961(3) 0.0462(1) 0.1730(2) 0.0476(9) Uani 1.00 d . . . C(19) C 0.9446(3) -0.1229(1) 0.2396(2) 0.0435(8) Uani 1.00 d . . . C(20) C 0.8378(3) -0.1063(1) 0.3128(2) 0.0409(8) Uani 1.00 d . . . C(21) C 0.8154(4) -0.1542(2) 0.3831(2) 0.0535(10) Uani 1.00 d . . . C(22) C 0.8930(4) -0.2170(2) 0.3762(2) 0.065(1) Uani 1.00 d . . . C(23) C 0.9924(4) -0.2331(2) 0.3011(3) 0.067(1) Uani 1.00 d . . . C(24) C 1.0217(4) -0.1865(2) 0.2319(2) 0.058(1) Uani 1.00 d . . . C(25) C 1.3204(4) -0.0139(2) 0.1856(2) 0.0503(9) Uani 1.00 d . . . C(26) C 1.2441(4) -0.0637(2) 0.1150(2) 0.0563(10) Uani 1.00 d . . . C(27) C 1.0522(4) -0.0614(2) 0.0986(2) 0.0540(10) Uani 1.00 d . . . C(28) C 0.8158(4) 0.1993(2) 0.4153(2) 0.0523(10) Uani 1.00 d . . . C(29) C 0.5566(4) 0.1256(2) 0.3696(2) 0.059(1) Uani 1.00 d . . . C(30) C 0.6846(4) 0.1192(2) 0.5200(2) 0.056(1) Uani 1.00 d . . . H(1) H 0.943(3) 0.235(1) 0.248(2) 0.0793 Uiso 1.00 calc . . . H(2) H 0.985(3) 0.080(1) 0.455(2) 0.0793 Uiso 1.00 calc . . . H(3) H 1.169(3) 0.016(1) 0.359(2) 0.0793 Uiso 1.00 calc . . . H(4) H 1.095(3) 0.258(1) 0.082(2) 0.0793 Uiso 1.00 calc . . . H(5) H 1.232(3) 0.247(1) -0.063(2) 0.0793 Uiso 1.00 calc . . . H(6) H 1.387(3) 0.145(1) -0.096(2) 0.0793 Uiso 1.00 calc . . . H(7) H 1.412(3) 0.051(1) 0.013(2) 0.0793 Uiso 1.00 calc . . . H(8) H 0.625(3) -0.009(1) 0.411(2) 0.0793 Uiso 1.00 calc . . . H(9) H 0.666(3) 0.138(1) 0.201(2) 0.0793 Uiso 1.00 calc . . . H(10) H 0.841(3) 0.062(1) 0.114(2) 0.0793 Uiso 1.00 calc . . . H(11) H 0.732(3) -0.140(1) 0.436(2) 0.0793 Uiso 1.00 calc . . . H(12) H 0.879(3) -0.253(1) 0.423(2) 0.0793 Uiso 1.00 calc . . . H(13) H 1.044(3) -0.280(1) 0.295(2) 0.0793 Uiso 1.00 calc . . . H(14) H 1.097(3) -0.197(1) 0.179(2) 0.0793 Uiso 1.00 calc . . . H(15) H 1.296(3) -0.033(1) 0.250(2) 0.0793 Uiso 1.00 calc . . . H(16) H 1.446(3) -0.012(1) 0.177(2) 0.0793 Uiso 1.00 calc . . . H(17) H 1.288(3) -0.114(1) 0.140(2) 0.0793 Uiso 1.00 calc . . . H(18) H 1.298(3) -0.058(1) 0.051(2) 0.0793 Uiso 1.00 calc . . . H(19) H 1.019(3) -0.015(1) 0.069(2) 0.0793 Uiso 1.00 calc . . . H(20) H 1.022(3) -0.101(1) 0.057(2) 0.0793 Uiso 1.00 calc . . . H(21) H 0.765(3) 0.240(1) 0.377(2) 0.0793 Uiso 1.00 calc . . . H(22) H 0.864(3) 0.217(1) 0.472(2) 0.0793 Uiso 1.00 calc . . . H(23) H 0.517(3) 0.167(1) 0.329(2) 0.0793 Uiso 1.00 calc . . . H(24) H 0.457(3) 0.106(1) 0.405(2) 0.0793 Uiso 1.00 calc . . . 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 N(1) 0.038(1) 0.053(1) 0.044(1) -0.001(1) 0.003(1) 0.003(1) N(2) 0.042(1) 0.052(1) 0.040(1) 0.000(1) 0.003(1) 0.003(1) N(3) 0.048(1) 0.048(1) 0.055(2) -0.003(1) 0.002(1) -0.008(1) N(4) 0.102(2) 0.076(2) 0.083(2) 0.001(2) 0.009(2) 0.022(2) C(1) 0.030(1) 0.050(2) 0.043(2) -0.005(1) -0.001(1) -0.004(1) C(2) 0.041(2) 0.043(2) 0.045(2) -0.012(1) -0.004(1) -0.001(1) C(3) 0.052(2) 0.038(2) 0.050(2) -0.013(1) -0.002(1) 0.000(1) C(4) 0.045(2) 0.041(2) 0.049(2) -0.007(1) -0.002(1) -0.009(1) C(5) 0.044(2) 0.053(2) 0.041(2) -0.007(1) 0.000(1) -0.001(1) C(6) 0.039(2) 0.049(2) 0.044(2) -0.004(1) -0.005(1) 0.003(1) C(7) 0.038(2) 0.064(2) 0.045(2) -0.010(1) -0.001(1) 0.006(2) C(8) 0.045(2) 0.052(2) 0.045(2) -0.015(1) -0.002(1) 0.006(1) C(9) 0.062(2) 0.059(2) 0.059(2) -0.018(2) 0.000(2) 0.012(2) C(10) 0.071(2) 0.083(3) 0.059(2) -0.023(2) 0.002(2) 0.021(2) C(11) 0.057(2) 0.105(3) 0.051(2) -0.022(2) 0.011(2) 0.012(2) C(12) 0.044(2) 0.085(3) 0.055(2) -0.005(2) 0.010(2) 0.006(2) C(13) 0.035(1) 0.043(2) 0.041(2) -0.006(1) -0.006(1) -0.001(1) C(14) 0.037(1) 0.039(2) 0.037(2) -0.010(1) -0.002(1) 0.003(1) C(15) 0.040(2) 0.048(2) 0.044(2) -0.009(1) 0.000(1) -0.004(1) C(16) 0.041(2) 0.043(2) 0.055(2) -0.002(1) -0.008(1) -0.005(1) C(17) 0.050(2) 0.041(2) 0.059(2) -0.007(1) -0.016(1) 0.004(2) C(18) 0.051(2) 0.048(2) 0.044(2) -0.010(1) -0.008(1) 0.008(1) C(19) 0.044(2) 0.044(2) 0.043(2) -0.004(1) -0.004(1) 0.003(1) C(20) 0.041(2) 0.042(2) 0.040(2) -0.008(1) -0.004(1) 0.004(1) C(21) 0.055(2) 0.050(2) 0.055(2) -0.013(2) -0.001(1) 0.010(2) C(22) 0.069(2) 0.053(2) 0.073(2) -0.009(2) -0.010(2) 0.024(2) C(23) 0.062(2) 0.045(2) 0.094(3) 0.006(2) -0.015(2) 0.006(2) C(24) 0.055(2) 0.055(2) 0.064(2) 0.006(2) 0.000(2) -0.004(2) C(25) 0.038(2) 0.058(2) 0.054(2) 0.001(2) -0.001(1) -0.003(2) C(26) 0.045(2) 0.073(2) 0.051(2) -0.002(2) 0.006(1) -0.010(2) C(27) 0.051(2) 0.071(2) 0.040(2) -0.008(2) 0.006(1) -0.006(2) C(28) 0.054(2) 0.048(2) 0.055(2) -0.008(2) 0.003(2) -0.009(2) C(29) 0.050(2) 0.051(2) 0.074(2) 0.003(2) -0.007(2) -0.008(2) C(30) 0.055(2) 0.046(2) 0.068(2) 0.004(2) 0.008(2) -0.005(2) #--------------------------------------------------------------------------- _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00001|Fo|^2^]' _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0080(4) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2325 _refine_ls_number_parameters 380 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0312 _refine_ls_wR_factor_gt 0.0312 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.570 _refine_ls_shift/su_max 1.0740 _refine_ls_shift/su_mean 0.0450 _refine_diff_density_min -0.19 _refine_diff_density_max 0.14 #--------------------------------------------------------------------------- _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 N(1) C(1) 1.392(3) 1_555 1_555 yes N(1) C(7) 1.389(3) 1_555 1_555 yes N(1) C(25) 1.463(3) 1_555 1_555 yes N(2) C(13) 1.383(3) 1_555 1_555 yes N(2) C(19) 1.389(3) 1_555 1_555 yes N(2) C(27) 1.459(3) 1_555 1_555 yes N(3) C(28) 1.491(4) 1_555 1_555 yes N(3) C(29) 1.484(4) 1_555 1_555 yes N(3) C(30) 1.334(4) 1_555 1_555 yes N(4) C(30) 1.141(4) 1_555 1_555 yes C(1) C(2) 1.411(3) 1_555 1_555 yes C(1) C(6) 1.394(3) 1_555 1_555 yes C(2) C(3) 1.395(4) 1_555 1_555 yes C(2) C(8) 1.447(3) 1_555 1_555 yes C(3) C(4) 1.386(4) 1_555 1_555 yes C(4) C(5) 1.410(4) 1_555 1_555 yes C(4) C(28) 1.514(4) 1_555 1_555 yes C(5) C(6) 1.380(4) 1_555 1_555 yes C(7) C(8) 1.411(4) 1_555 1_555 yes C(7) C(12) 1.396(4) 1_555 1_555 yes C(8) C(9) 1.395(4) 1_555 1_555 yes C(9) C(10) 1.387(4) 1_555 1_555 yes C(10) C(11) 1.390(5) 1_555 1_555 yes C(11) C(12) 1.381(4) 1_555 1_555 yes C(13) C(14) 1.413(3) 1_555 1_555 yes C(13) C(18) 1.394(3) 1_555 1_555 yes C(14) C(15) 1.395(3) 1_555 1_555 yes C(14) C(20) 1.442(3) 1_555 1_555 yes C(15) C(16) 1.387(3) 1_555 1_555 yes C(16) C(17) 1.401(4) 1_555 1_555 yes C(16) C(29) 1.507(4) 1_555 1_555 yes C(17) C(18) 1.379(4) 1_555 1_555 yes C(19) C(20) 1.409(3) 1_555 1_555 yes C(19) C(24) 1.386(4) 1_555 1_555 yes C(20) C(21) 1.400(3) 1_555 1_555 yes C(21) C(22) 1.372(4) 1_555 1_555 yes C(22) C(23) 1.394(4) 1_555 1_555 yes C(23) C(24) 1.379(4) 1_555 1_555 yes C(25) C(26) 1.529(4) 1_555 1_555 yes C(26) C(27) 1.529(4) 1_555 1_555 yes #--------------------------------------------------------------------------- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(1) N(1) C(7) 108.0(2) 1_555 1_555 1_555 yes C(1) N(1) C(25) 124.3(2) 1_555 1_555 1_555 yes C(7) N(1) C(25) 127.6(2) 1_555 1_555 1_555 yes C(13) N(2) C(19) 109.0(2) 1_555 1_555 1_555 yes C(13) N(2) C(27) 125.0(2) 1_555 1_555 1_555 yes C(19) N(2) C(27) 126.0(2) 1_555 1_555 1_555 yes C(28) N(3) C(29) 119.9(2) 1_555 1_555 1_555 yes C(28) N(3) C(30) 118.4(2) 1_555 1_555 1_555 yes C(29) N(3) C(30) 116.5(2) 1_555 1_555 1_555 yes N(1) C(1) C(2) 109.5(2) 1_555 1_555 1_555 yes N(1) C(1) C(6) 129.1(2) 1_555 1_555 1_555 yes C(2) C(1) C(6) 121.3(2) 1_555 1_555 1_555 yes C(1) C(2) C(3) 119.7(2) 1_555 1_555 1_555 yes C(1) C(2) C(8) 106.2(2) 1_555 1_555 1_555 yes C(3) C(2) C(8) 133.7(3) 1_555 1_555 1_555 yes C(2) C(3) C(4) 119.3(3) 1_555 1_555 1_555 yes C(2) C(3) H(1) 118(1) 1_555 1_555 1_555 no C(4) C(3) H(1) 122(1) 1_555 1_555 1_555 no C(3) C(4) C(5) 119.8(3) 1_555 1_555 1_555 yes C(3) C(4) C(28) 120.5(3) 1_555 1_555 1_555 yes C(5) C(4) C(28) 119.6(3) 1_555 1_555 1_555 yes C(4) C(5) C(6) 121.9(3) 1_555 1_555 1_555 yes C(4) C(5) H(2) 121(1) 1_555 1_555 1_555 no C(6) C(5) H(2) 116(1) 1_555 1_555 1_555 no C(1) C(6) C(5) 117.6(3) 1_555 1_555 1_555 yes C(1) C(6) H(3) 121(1) 1_555 1_555 1_555 no C(5) C(6) H(3) 121(1) 1_555 1_555 1_555 no N(1) C(7) C(8) 109.3(2) 1_555 1_555 1_555 yes N(1) C(7) C(12) 129.6(3) 1_555 1_555 1_555 yes C(8) C(7) C(12) 121.1(3) 1_555 1_555 1_555 yes C(2) C(8) C(7) 106.8(2) 1_555 1_555 1_555 yes C(2) C(8) C(9) 133.4(3) 1_555 1_555 1_555 yes C(7) C(8) C(9) 119.8(3) 1_555 1_555 1_555 yes C(8) C(9) C(10) 118.9(3) 1_555 1_555 1_555 yes C(8) C(9) H(4) 119(1) 1_555 1_555 1_555 no C(10) C(9) H(4) 121(1) 1_555 1_555 1_555 no C(9) C(10) C(11) 120.6(3) 1_555 1_555 1_555 yes C(9) C(10) H(5) 118(1) 1_555 1_555 1_555 no C(11) C(10) H(5) 121(1) 1_555 1_555 1_555 no C(10) C(11) C(12) 121.8(3) 1_555 1_555 1_555 yes C(10) C(11) H(6) 119(1) 1_555 1_555 1_555 no C(12) C(11) H(6) 118(1) 1_555 1_555 1_555 no C(7) C(12) C(11) 117.8(3) 1_555 1_555 1_555 yes C(7) C(12) H(7) 118(1) 1_555 1_555 1_555 no C(11) C(12) H(7) 123(1) 1_555 1_555 1_555 no N(2) C(13) C(14) 109.1(2) 1_555 1_555 1_555 yes N(2) C(13) C(18) 129.9(3) 1_555 1_555 1_555 yes C(14) C(13) C(18) 121.0(3) 1_555 1_555 1_555 yes C(13) C(14) C(15) 119.7(2) 1_555 1_555 1_555 yes C(13) C(14) C(20) 106.0(2) 1_555 1_555 1_555 yes C(15) C(14) C(20) 134.1(2) 1_555 1_555 1_555 yes C(14) C(15) C(16) 119.3(3) 1_555 1_555 1_555 yes C(14) C(15) H(8) 119(1) 1_555 1_555 1_555 no C(16) C(15) H(8) 121(1) 1_555 1_555 1_555 no C(15) C(16) C(17) 119.7(3) 1_555 1_555 1_555 yes C(15) C(16) C(29) 120.6(3) 1_555 1_555 1_555 yes C(17) C(16) C(29) 119.4(3) 1_555 1_555 1_555 yes C(16) C(17) C(18) 122.2(3) 1_555 1_555 1_555 yes C(16) C(17) H(9) 116(1) 1_555 1_555 1_555 no C(18) C(17) H(9) 121(1) 1_555 1_555 1_555 no C(13) C(18) C(17) 117.7(3) 1_555 1_555 1_555 yes C(13) C(18) H(10) 122(1) 1_555 1_555 1_555 no C(17) C(18) H(10) 119(1) 1_555 1_555 1_555 no N(2) C(19) C(20) 108.3(2) 1_555 1_555 1_555 yes N(2) C(19) C(24) 129.3(3) 1_555 1_555 1_555 yes C(20) C(19) C(24) 122.4(3) 1_555 1_555 1_555 yes C(14) C(20) C(19) 107.5(2) 1_555 1_555 1_555 yes C(14) C(20) C(21) 133.4(3) 1_555 1_555 1_555 yes C(19) C(20) C(21) 119.1(3) 1_555 1_555 1_555 yes C(20) C(21) C(22) 118.6(3) 1_555 1_555 1_555 yes C(20) C(21) H(11) 116(1) 1_555 1_555 1_555 no C(22) C(21) H(11) 124(1) 1_555 1_555 1_555 no C(21) C(22) C(23) 121.1(3) 1_555 1_555 1_555 yes C(21) C(22) H(12) 122(1) 1_555 1_555 1_555 no C(23) C(22) H(12) 116(1) 1_555 1_555 1_555 no C(22) C(23) C(24) 122.0(3) 1_555 1_555 1_555 yes C(22) C(23) H(13) 120(1) 1_555 1_555 1_555 no C(24) C(23) H(13) 117(1) 1_555 1_555 1_555 no C(19) C(24) C(23) 116.8(3) 1_555 1_555 1_555 yes C(19) C(24) H(14) 121(1) 1_555 1_555 1_555 no C(23) C(24) H(14) 122(1) 1_555 1_555 1_555 no N(1) C(25) C(26) 115.8(2) 1_555 1_555 1_555 yes N(1) C(25) H(15) 108(1) 1_555 1_555 1_555 no N(1) C(25) H(16) 107(1) 1_555 1_555 1_555 no C(26) C(25) H(15) 107(1) 1_555 1_555 1_555 no C(26) C(25) H(16) 108(1) 1_555 1_555 1_555 no H(15) C(25) H(16) 108(2) 1_555 1_555 1_555 no C(25) C(26) C(27) 117.5(3) 1_555 1_555 1_555 yes C(25) C(26) H(17) 102(1) 1_555 1_555 1_555 no C(25) C(26) H(18) 111(1) 1_555 1_555 1_555 no C(27) C(26) H(17) 112(1) 1_555 1_555 1_555 no C(27) C(26) H(18) 106(1) 1_555 1_555 1_555 no H(17) C(26) H(18) 105(1) 1_555 1_555 1_555 no N(2) C(27) C(26) 115.9(2) 1_555 1_555 1_555 yes N(2) C(27) H(19) 105(1) 1_555 1_555 1_555 no N(2) C(27) H(20) 107(1) 1_555 1_555 1_555 no C(26) C(27) H(19) 109(1) 1_555 1_555 1_555 no C(26) C(27) H(20) 107(1) 1_555 1_555 1_555 no H(19) C(27) H(20) 111(2) 1_555 1_555 1_555 no N(3) C(28) C(4) 114.8(2) 1_555 1_555 1_555 yes N(3) C(28) H(21) 107(1) 1_555 1_555 1_555 no N(3) C(28) H(22) 105(1) 1_555 1_555 1_555 no C(4) C(28) H(21) 108(1) 1_555 1_555 1_555 no C(4) C(28) H(22) 110(1) 1_555 1_555 1_555 no H(21) C(28) H(22) 109(2) 1_555 1_555 1_555 no N(3) C(29) C(16) 113.7(2) 1_555 1_555 1_555 yes N(3) C(29) H(23) 106(1) 1_555 1_555 1_555 no N(3) C(29) H(24) 104(1) 1_555 1_555 1_555 no C(16) C(29) H(23) 110(1) 1_555 1_555 1_555 no C(16) C(29) H(24) 111(1) 1_555 1_555 1_555 no H(23) C(29) H(24) 110(2) 1_555 1_555 1_555 no N(3) C(30) N(4) 177.0(3) 1_555 1_555 1_555 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 N(1) C(1) C(2) C(3) 171.6(2) 1_555 1_555 1_555 1_555 yes N(1) C(1) C(2) C(8) -2.2(3) 1_555 1_555 1_555 1_555 yes N(1) C(1) C(6) C(5) -173.5(2) 1_555 1_555 1_555 1_555 yes N(1) C(7) C(8) C(2) 0.8(3) 1_555 1_555 1_555 1_555 yes N(1) C(7) C(8) C(9) -178.4(2) 1_555 1_555 1_555 1_555 yes N(1) C(7) C(12) C(11) 179.1(3) 1_555 1_555 1_555 1_555 yes N(1) C(25) C(26) C(27) -43.6(4) 1_555 1_555 1_555 1_555 yes N(2) C(13) C(14) C(15) 173.9(2) 1_555 1_555 1_555 1_555 yes N(2) C(13) C(14) C(20) -2.6(3) 1_555 1_555 1_555 1_555 yes N(2) C(13) C(18) C(17) -174.1(2) 1_555 1_555 1_555 1_555 yes N(2) C(19) C(20) C(14) 1.5(3) 1_555 1_555 1_555 1_555 yes N(2) C(19) C(20) C(21) -178.7(2) 1_555 1_555 1_555 1_555 yes N(2) C(19) C(24) C(23) -178.8(3) 1_555 1_555 1_555 1_555 yes N(2) C(27) C(26) C(25) -52.7(4) 1_555 1_555 1_555 1_555 yes N(3) C(28) C(4) C(3) 125.4(3) 1_555 1_555 1_555 1_555 yes N(3) C(28) C(4) C(5) -50.8(3) 1_555 1_555 1_555 1_555 yes N(3) C(29) C(16) C(15) 73.6(3) 1_555 1_555 1_555 1_555 yes N(3) C(29) C(16) C(17) -100.5(3) 1_555 1_555 1_555 1_555 yes N(4) C(30) N(3) C(28) 127(6) 1_555 1_555 1_555 1_555 yes N(4) C(30) N(3) C(29) -77(6) 1_555 1_555 1_555 1_555 yes C(1) N(1) C(7) C(8) -2.1(3) 1_555 1_555 1_555 1_555 yes C(1) N(1) C(7) C(12) 177.9(3) 1_555 1_555 1_555 1_555 yes C(1) N(1) C(25) C(26) 116.2(3) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) 2.7(4) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(8) C(7) 0.8(3) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(8) C(9) 179.9(3) 1_555 1_555 1_555 1_555 yes C(1) C(6) C(5) C(4) 1.8(4) 1_555 1_555 1_555 1_555 yes C(2) C(1) N(1) C(7) 2.7(3) 1_555 1_555 1_555 1_555 yes C(2) C(1) N(1) C(25) -174.6(2) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(6) C(5) 4.1(4) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 3.0(4) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(28) -173.2(2) 1_555 1_555 1_555 1_555 yes C(2) C(8) C(7) C(12) -179.2(2) 1_555 1_555 1_555 1_555 yes C(2) C(8) C(9) C(10) -179.6(3) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(6) -6.4(4) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(8) C(7) -171.7(3) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(8) C(9) 7.3(5) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) -5.4(4) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(2) C(8) 174.5(3) 1_555 1_555 1_555 1_555 yes C(4) C(28) N(3) C(29) -65.2(3) 1_555 1_555 1_555 1_555 yes C(4) C(28) N(3) C(30) 88.6(3) 1_555 1_555 1_555 1_555 yes C(6) C(1) N(1) C(7) -179.5(3) 1_555 1_555 1_555 1_555 yes C(6) C(1) N(1) C(25) 3.2(4) 1_555 1_555 1_555 1_555 yes C(6) C(1) C(2) C(8) 179.8(2) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(4) C(28) 170.9(2) 1_555 1_555 1_555 1_555 yes C(7) N(1) C(25) C(26) -60.6(4) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) -0.7(4) 1_555 1_555 1_555 1_555 yes C(7) C(12) C(11) C(10) -0.7(5) 1_555 1_555 1_555 1_555 yes C(8) C(7) N(1) C(25) 175.1(2) 1_555 1_555 1_555 1_555 yes C(8) C(7) C(12) C(11) -0.9(4) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(11) -0.8(5) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(7) C(12) 1.6(4) 1_555 1_555 1_555 1_555 yes C(9) C(10) C(11) C(12) 1.6(5) 1_555 1_555 1_555 1_555 yes C(12) C(7) N(1) C(25) -4.9(5) 1_555 1_555 1_555 1_555 yes C(13) N(2) C(19) C(20) -3.2(3) 1_555 1_555 1_555 1_555 yes C(13) N(2) C(19) C(24) 174.4(3) 1_555 1_555 1_555 1_555 yes C(13) N(2) C(27) C(26) 117.2(3) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) 0.4(4) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(20) C(19) 0.7(3) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(20) C(21) -179.0(3) 1_555 1_555 1_555 1_555 yes C(13) C(18) C(17) C(16) -0.3(4) 1_555 1_555 1_555 1_555 yes C(14) C(13) N(2) C(19) 3.7(3) 1_555 1_555 1_555 1_555 yes C(14) C(13) N(2) C(27) -175.8(2) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(18) C(17) 5.9(4) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) 5.0(4) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(29) -169.1(2) 1_555 1_555 1_555 1_555 yes C(14) C(20) C(19) C(24) -176.3(2) 1_555 1_555 1_555 1_555 yes C(14) C(20) C(21) C(22) 177.1(3) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(18) -6.1(4) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(20) C(19) -175.2(3) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(20) C(21) 5.1(5) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(18) -5.2(4) 1_555 1_555 1_555 1_555 yes C(16) C(15) C(14) C(20) 175.8(2) 1_555 1_555 1_555 1_555 yes C(16) C(29) N(3) C(28) 69.8(3) 1_555 1_555 1_555 1_555 yes C(16) C(29) N(3) C(30) -84.4(3) 1_555 1_555 1_555 1_555 yes C(18) C(13) N(2) C(19) -176.3(2) 1_555 1_555 1_555 1_555 yes C(18) C(13) N(2) C(27) 4.2(4) 1_555 1_555 1_555 1_555 yes C(18) C(13) C(14) C(20) 177.4(2) 1_555 1_555 1_555 1_555 yes C(18) C(17) C(16) C(29) 169.0(2) 1_555 1_555 1_555 1_555 yes C(19) N(2) C(27) C(26) -62.2(4) 1_555 1_555 1_555 1_555 yes C(19) C(20) C(21) C(22) -2.6(4) 1_555 1_555 1_555 1_555 yes C(19) C(24) C(23) C(22) -1.3(5) 1_555 1_555 1_555 1_555 yes C(20) C(19) N(2) C(27) 176.3(2) 1_555 1_555 1_555 1_555 yes C(20) C(19) C(24) C(23) -1.4(4) 1_555 1_555 1_555 1_555 yes C(20) C(21) C(22) C(23) 0.0(5) 1_555 1_555 1_555 1_555 yes C(21) C(20) C(19) C(24) 3.4(4) 1_555 1_555 1_555 1_555 yes C(21) C(22) C(23) C(24) 2.0(5) 1_555 1_555 1_555 1_555 yes C(24) C(19) N(2) C(27) -6.1(4) 1_555 1_555 1_555 1_555 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 N(1) C(16) 3.539(4) 1_555 1_655 ? N(1) C(17) 3.573(5) 1_555 1_655 ? N(2) C(11) 3.396(4) 1_555 3_755 ? N(4) C(6) 3.477(4) 1_555 3_756 ? N(4) C(15) 3.555(4) 1_555 3_656 ? C(1) C(29) 3.574(5) 1_555 1_655 ? C(11) C(27) 3.560(5) 1_555 3_755 ? C(16) C(25) 3.496(4) 1_555 1_455 ? C(21) C(23) 3.553(4) 1_555 4_445 ? C(22) C(23) 3.464(5) 1_555 4_445 ? C(22) C(30) 3.591(4) 1_555 2_646 ? #---------------------------------------------------------------------------