Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_General #------------------------------------------------------------------------------ # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name ' Takanori Suzuki' _publ_contact_author_address ; Division of Chemistry Hokkaido University Graduate School of Science Sapporo 060-810 JAPAN ; _publ_contact_author_email TAK@SCI.HOKUDAI.AC.JP _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' Chemical Communications' _journal_coden_Cambridge 182 _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name 'Higuchi, Hiroki' 'Ohkita, Masakazu' 'Suzuki, Takanori' 'Tsuji, Takashi' _publ_section_synopsis ; ENTER SYNOPSIS ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _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_010501-2 _database_code_CSD 164961 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C48 H52 I6 N4 ' _chemical_formula_moiety '?' _chemical_formula_weight 1446.39 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 10.054(2) _cell_length_b 17.393(3) _cell_length_c 28.880(5) _cell_angle_alpha 90 _cell_angle_beta 92.970(9) _cell_angle_gamma 90 _cell_volume 5043(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9843 _cell_measurement_theta_min 0.7 _cell_measurement_theta_max 27.9 _cell_measurement_temperature 123.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'Platelet' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.905 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 3.733 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.830 _exptl_absorpt_correction_T_max 0.830 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number ? _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_theta_max 26.00 _diffrn_measured_fraction_theta_max 0.9713 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.9713 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 35 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 9651 _reflns_number_gt 4842 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.0812 _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 4842 _refine_ls_number_parameters 263 _refine_ls_goodness_of_fit_ref 1.501 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]' _refine_ls_shift/su_max 0.0025 _refine_diff_density_max 1.09 _refine_diff_density_min -1.24 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_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) ; 'I' 'I' -0.474 1.812 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I(1) I 0.47852(9) 0.11293(6) 0.49472(4) 0.0393(3) Uani 1.00 d . . . I(2) I 0.37912(9) 0.26470(6) 0.46826(4) 0.0378(3) Uani 1.00 d . . . I(3) I 0.2653(1) 0.41770(7) 0.44696(4) 0.0477(3) Uani 1.00 d . . . I(4) I -0.0315(1) 0.17552(6) 0.71566(4) 0.0422(3) Uani 1.00 d . . . I(5) I -0.05446(9) 0.27363(6) 0.63132(3) 0.0323(2) Uani 1.00 d . . . I(6) I -0.0680(1) 0.35997(7) 0.54609(4) 0.0452(3) Uani 1.00 d . . . N(1) N 1.017(1) -0.1008(6) 0.4643(4) 0.030(3) Uiso 1.00 d . . . N(2) N 0.621(1) 0.4024(6) 0.4038(4) 0.027(3) Uiso 1.00 d . . . N(3) N 0.196(1) 0.2189(6) 0.3444(4) 0.028(3) Uiso 1.00 d . . . N(4) N 0.560(1) -0.2960(6) 0.4079(4) 0.023(2) Uiso 1.00 d . . . C(1) C 0.757(1) 0.1116(7) 0.3418(4) 0.022(3) Uiso 1.00 d . . . C(2) C 0.733(1) 0.0901(7) 0.2898(4) 0.023(3) Uiso 1.00 d . . . C(3) C 0.687(1) 0.0072(7) 0.2840(4) 0.022(3) Uiso 1.00 d . . . C(4) C 0.571(1) -0.0134(7) 0.3143(4) 0.019(3) Uiso 1.00 d . . . C(5) C 0.828(1) 0.0590(7) 0.3731(4) 0.017(3) Uiso 1.00 d . . . C(6) C 0.770(1) 0.0350(7) 0.4148(4) 0.025(3) Uiso 1.00 d . . . C(7) C 0.831(1) -0.0212(7) 0.4434(4) 0.024(3) Uiso 1.00 d . . . C(8) C 0.956(1) -0.0511(8) 0.4351(5) 0.032(3) Uiso 1.00 d . . . C(9) C 1.017(1) -0.0278(8) 0.3933(5) 0.029(3) Uiso 1.00 d . . . C(10) C 0.952(1) 0.0245(8) 0.3635(5) 0.028(3) Uiso 1.00 d . . . C(11) C 0.949(1) -0.1369(8) 0.5023(5) 0.035(3) Uiso 1.00 d . . . C(12) C 1.154(1) -0.1187(8) 0.4619(5) 0.033(3) Uiso 1.00 d . . . C(13) C 0.713(1) 0.1831(7) 0.3580(4) 0.018(3) Uiso 1.00 d . . . C(14) C 0.624(1) 0.2334(7) 0.3306(5) 0.025(3) Uiso 1.00 d . . . C(15) C 0.596(1) 0.3034(8) 0.3466(5) 0.027(3) Uiso 1.00 d . . . C(16) C 0.644(1) 0.3320(8) 0.3904(5) 0.028(3) Uiso 1.00 d . . . C(17) C 0.722(1) 0.2803(7) 0.4195(4) 0.020(3) Uiso 1.00 d . . . C(18) C 0.756(1) 0.2069(7) 0.4028(4) 0.022(3) Uiso 1.00 d . . . C(19) C 0.557(1) 0.4595(9) 0.3694(5) 0.042(4) Uiso 1.00 d . . . C(20) C 0.666(1) 0.4347(9) 0.4487(5) 0.038(4) Uiso 1.00 d . . . C(21) C 0.856(1) 0.1098(7) 0.2624(5) 0.024(3) Uiso 1.00 d . . . C(22) C 0.948(1) 0.0524(8) 0.2481(5) 0.030(3) Uiso 1.00 d . . . C(23) C 1.055(1) 0.0757(9) 0.2218(5) 0.037(4) Uiso 1.00 d . . . C(24) C 1.071(1) 0.1530(9) 0.2093(5) 0.039(4) Uiso 1.00 d . . . C(25) C 0.980(1) 0.2061(9) 0.2235(5) 0.039(4) Uiso 1.00 d . . . C(26) C 0.876(1) 0.1855(8) 0.2497(5) 0.033(3) Uiso 1.00 d . . . C(27) C 0.652(1) -0.0161(7) 0.2347(4) 0.019(3) Uiso 1.00 d . . . C(28) C 0.652(1) -0.0945(8) 0.2256(5) 0.028(3) Uiso 1.00 d . . . C(29) C 0.615(1) -0.1225(8) 0.1788(5) 0.030(3) Uiso 1.00 d . . . C(30) C 0.581(1) -0.0700(7) 0.1437(5) 0.026(3) Uiso 1.00 d . . . C(31) C 0.584(1) 0.0096(8) 0.1534(5) 0.028(3) Uiso 1.00 d . . . C(32) C 0.621(1) 0.0343(7) 0.1980(4) 0.024(3) Uiso 1.00 d . . . C(33) C 0.463(1) 0.0401(7) 0.3180(4) 0.025(3) Uiso 1.00 d . . . C(34) C 0.421(1) 0.0937(8) 0.2846(5) 0.032(3) Uiso 1.00 d . . . C(35) C 0.334(1) 0.1505(8) 0.2922(5) 0.029(3) Uiso 1.00 d . . . C(36) C 0.275(1) 0.1578(7) 0.3357(4) 0.021(3) Uiso 1.00 d . . . C(37) C 0.308(1) 0.1006(7) 0.3708(4) 0.018(3) Uiso 1.00 d . . . C(38) C 0.399(1) 0.0450(8) 0.3622(5) 0.031(3) Uiso 1.00 d . . . C(39) C 0.192(2) 0.2903(9) 0.3158(5) 0.041(4) Uiso 1.00 d . . . C(40) C 0.097(1) 0.2180(8) 0.3807(5) 0.027(3) Uiso 1.00 d . . . C(41) C 0.571(1) -0.0858(7) 0.3384(4) 0.020(3) Uiso 1.00 d . . . C(42) C 0.446(1) -0.1190(7) 0.3508(4) 0.023(3) Uiso 1.00 d . . . C(43) C 0.443(1) -0.1885(7) 0.3727(5) 0.025(3) Uiso 1.00 d . . . C(44) C 0.560(1) -0.2289(7) 0.3866(4) 0.023(3) Uiso 1.00 d . . . C(45) C 0.686(1) -0.1954(8) 0.3726(5) 0.028(3) Uiso 1.00 d . . . C(46) C 0.686(1) -0.1285(7) 0.3494(5) 0.026(3) Uiso 1.00 d . . . C(47) C 0.436(1) -0.3310(8) 0.4225(5) 0.034(3) Uiso 1.00 d . . . C(48) C 0.685(1) -0.3403(8) 0.4157(5) 0.030(3) Uiso 1.00 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 I(1) 0.0265(5) 0.0577(6) 0.0334(5) 0.0046(5) -0.0004(4) -0.0004(5) I(2) 0.0287(5) 0.0501(6) 0.0343(5) -0.0041(5) -0.0009(4) -0.0058(5) I(3) 0.0493(6) 0.0464(6) 0.0464(6) 0.0007(5) -0.0056(5) -0.0031(5) I(4) 0.0512(6) 0.0455(6) 0.0298(5) 0.0095(5) 0.0011(5) -0.0027(5) I(5) 0.0245(4) 0.0385(5) 0.0333(5) 0.0008(4) -0.0053(4) -0.0047(4) I(6) 0.0408(6) 0.0539(6) 0.0393(6) -0.0029(5) -0.0125(5) 0.0054(5) #------------------------------------------------------------------------------ _computing_data_collection 'CRYSTALCLEAR' _computing_cell_refinement 'CRYSTALCLEAR' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution DirectMethod _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 I(1) I(2) 2.911(2) . . yes I(2) I(3) 2.949(2) . . yes I(4) I(5) 2.973(1) . . yes I(5) I(6) 2.881(2) . . yes N(1) C(8) 1.33(2) . . yes N(1) C(11) 1.46(2) . . yes N(1) C(12) 1.42(2) . . yes N(2) C(16) 1.31(2) . . yes N(2) C(19) 1.52(2) . . yes N(2) C(20) 1.46(2) . . yes N(3) C(36) 1.36(2) . . yes N(3) C(39) 1.49(2) . . yes N(3) C(40) 1.48(2) . . yes N(4) C(44) 1.32(2) . . yes N(4) C(47) 1.47(2) . . yes N(4) C(48) 1.48(2) . . yes C(1) C(2) 1.55(2) . . yes C(1) C(5) 1.45(2) . . yes C(1) C(13) 1.41(2) . . yes C(2) C(3) 1.52(2) . . yes C(2) C(21) 1.54(2) . . yes C(3) C(4) 1.53(2) . . yes C(3) C(27) 1.50(2) . . yes C(4) C(33) 1.44(2) . . yes C(4) C(41) 1.44(2) . . yes C(5) C(6) 1.43(2) . . yes C(5) C(10) 1.42(2) . . yes C(6) C(7) 1.40(2) . . yes C(7) C(8) 1.40(2) . . yes C(8) C(9) 1.44(2) . . yes C(9) C(10) 1.39(2) . . yes C(13) C(14) 1.45(2) . . yes C(13) C(18) 1.41(2) . . yes C(14) C(15) 1.34(2) . . yes C(15) C(16) 1.42(2) . . yes C(16) C(17) 1.44(2) . . yes C(17) C(18) 1.41(2) . . yes C(21) C(22) 1.44(2) . . yes C(21) C(26) 1.38(2) . . yes C(22) C(23) 1.40(2) . . yes C(23) C(24) 1.40(2) . . yes C(24) C(25) 1.38(2) . . yes C(25) C(26) 1.38(2) . . yes C(27) C(28) 1.39(2) . . yes C(27) C(32) 1.40(2) . . yes C(28) C(29) 1.47(2) . . yes C(29) C(30) 1.39(2) . . yes C(30) C(31) 1.41(2) . . yes C(31) C(32) 1.39(2) . . yes C(33) C(34) 1.39(2) . . yes C(33) C(38) 1.46(2) . . yes C(34) C(35) 1.35(2) . . yes C(35) C(36) 1.42(2) . . yes C(36) C(37) 1.45(2) . . yes C(37) C(38) 1.36(2) . . yes C(41) C(42) 1.45(2) . . yes C(41) C(46) 1.40(2) . . yes C(42) C(43) 1.37(2) . . yes C(43) C(44) 1.41(2) . . yes C(44) C(45) 1.47(2) . . yes C(45) C(46) 1.34(2) . . 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 I(1) I(2) I(3) 175.88(5) . . . yes I(4) I(5) I(6) 175.93(5) . . . yes C(8) N(1) C(11) 122(1) . . . yes C(8) N(1) C(12) 121(1) . . . yes C(11) N(1) C(12) 115(1) . . . yes C(16) N(2) C(19) 119(1) . . . yes C(16) N(2) C(20) 124(1) . . . yes C(19) N(2) C(20) 115(1) . . . yes C(36) N(3) C(39) 123(1) . . . yes C(36) N(3) C(40) 122(1) . . . yes C(39) N(3) C(40) 113(1) . . . yes C(44) N(4) C(47) 121(1) . . . yes C(44) N(4) C(48) 120(1) . . . yes C(47) N(4) C(48) 117(1) . . . yes C(2) C(1) C(5) 119(1) . . . yes C(2) C(1) C(13) 120(1) . . . yes C(5) C(1) C(13) 120(1) . . . yes C(1) C(2) C(3) 111(1) . . . yes C(1) C(2) C(21) 110(1) . . . yes C(3) C(2) C(21) 113(1) . . . yes C(2) C(3) C(4) 113.3(10) . . . yes C(2) C(3) C(27) 114(1) . . . yes C(4) C(3) C(27) 109(1) . . . yes C(3) C(4) C(33) 119(1) . . . yes C(3) C(4) C(41) 120(1) . . . yes C(33) C(4) C(41) 120(1) . . . yes C(1) C(5) C(6) 120(1) . . . yes C(1) C(5) C(10) 123(1) . . . yes C(6) C(5) C(10) 116(1) . . . yes C(5) C(6) C(7) 121(1) . . . yes C(6) C(7) C(8) 121(1) . . . yes N(1) C(8) C(7) 121(1) . . . yes N(1) C(8) C(9) 120(1) . . . yes C(7) C(8) C(9) 117(1) . . . yes C(8) C(9) C(10) 119(1) . . . yes C(5) C(10) C(9) 122(1) . . . yes C(1) C(13) C(14) 123(1) . . . yes C(1) C(13) C(18) 118(1) . . . yes C(14) C(13) C(18) 118(1) . . . yes C(13) C(14) C(15) 119(1) . . . yes C(14) C(15) C(16) 123(1) . . . yes N(2) C(16) C(15) 122(1) . . . yes N(2) C(16) C(17) 120(1) . . . yes C(15) C(16) C(17) 116(1) . . . yes C(16) C(17) C(18) 119(1) . . . yes C(13) C(18) C(17) 120(1) . . . yes C(2) C(21) C(22) 122(1) . . . yes C(2) C(21) C(26) 118(1) . . . yes C(22) C(21) C(26) 119(1) . . . yes C(21) C(22) C(23) 118(1) . . . yes C(22) C(23) C(24) 121(1) . . . yes C(23) C(24) C(25) 118(1) . . . yes C(24) C(25) C(26) 121(1) . . . yes C(21) C(26) C(25) 120(1) . . . yes C(3) C(27) C(28) 116(1) . . . yes C(3) C(27) C(32) 125(1) . . . yes C(28) C(27) C(32) 118(1) . . . yes C(27) C(28) C(29) 119(1) . . . yes C(28) C(29) C(30) 119(1) . . . yes C(29) C(30) C(31) 119(1) . . . yes C(30) C(31) C(32) 119(1) . . . yes C(27) C(32) C(31) 123(1) . . . yes C(4) C(33) C(34) 125(1) . . . yes C(4) C(33) C(38) 118(1) . . . yes C(34) C(33) C(38) 115(1) . . . yes C(33) C(34) C(35) 123(1) . . . yes C(34) C(35) C(36) 120(1) . . . yes N(3) C(36) C(35) 120(1) . . . yes N(3) C(36) C(37) 121(1) . . . yes C(35) C(36) C(37) 117(1) . . . yes C(36) C(37) C(38) 119(1) . . . yes C(33) C(38) C(37) 121(1) . . . yes C(4) C(41) C(42) 119(1) . . . yes C(4) C(41) C(46) 123(1) . . . yes C(42) C(41) C(46) 117(1) . . . yes C(41) C(42) C(43) 120(1) . . . yes C(42) C(43) C(44) 122(1) . . . yes N(4) C(44) C(43) 123(1) . . . yes N(4) C(44) C(45) 119(1) . . . yes C(43) C(44) C(45) 116(1) . . . yes C(44) C(45) C(46) 120(1) . . . yes C(41) C(46) C(45) 123(1) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N(1) C(8) C(7) C(6) 175(1) . . . . yes N(1) C(8) C(9) C(10) -179(1) . . . . yes N(2) C(16) C(15) C(14) 175(1) . . . . yes N(2) C(16) C(17) C(18) -174(1) . . . . yes N(3) C(36) C(35) C(34) 174(1) . . . . yes N(3) C(36) C(37) C(38) -172(1) . . . . yes N(4) C(44) C(43) C(42) 179(1) . . . . yes N(4) C(44) C(45) C(46) 177(1) . . . . yes C(1) C(2) C(3) C(4) 48(1) . . . . yes C(1) C(2) C(3) C(27) 175.6(10) . . . . yes C(1) C(2) C(21) C(22) 103(1) . . . . yes C(1) C(2) C(21) C(26) -78(1) . . . . yes C(1) C(5) C(6) C(7) 173(1) . . . . yes C(1) C(5) C(10) C(9) -177(1) . . . . yes C(1) C(13) C(14) C(15) -174(1) . . . . yes C(1) C(13) C(18) C(17) 175(1) . . . . yes C(2) C(1) C(5) C(6) -126(1) . . . . yes C(2) C(1) C(5) C(10) 48(1) . . . . yes C(2) C(1) C(13) C(14) 11(1) . . . . yes C(2) C(1) C(13) C(18) -168(1) . . . . yes C(2) C(3) C(4) C(33) 43(1) . . . . yes C(2) C(3) C(4) C(41) -137(1) . . . . yes C(2) C(3) C(27) C(28) 159(1) . . . . yes C(2) C(3) C(27) C(32) -20(1) . . . . yes C(2) C(21) C(22) C(23) 177(1) . . . . yes C(2) C(21) C(26) C(25) -177(1) . . . . yes C(3) C(2) C(1) C(5) 45(1) . . . . yes C(3) C(2) C(1) C(13) -136(1) . . . . yes C(3) C(2) C(21) C(22) -23(1) . . . . yes C(3) C(2) C(21) C(26) 154(1) . . . . yes C(3) C(4) C(33) C(34) 27(1) . . . . yes C(3) C(4) C(33) C(38) -145(1) . . . . yes C(3) C(4) C(41) C(42) -154(1) . . . . yes C(3) C(4) C(41) C(46) 22(1) . . . . yes C(3) C(27) C(28) C(29) 177(1) . . . . yes C(3) C(27) C(32) C(31) -177(1) . . . . yes C(4) C(3) C(2) C(21) 175(1) . . . . yes C(4) C(3) C(27) C(28) -72(1) . . . . yes C(4) C(3) C(27) C(32) 108(1) . . . . yes C(4) C(33) C(34) C(35) -169(1) . . . . yes C(4) C(33) C(38) C(37) 171(1) . . . . yes C(4) C(41) C(42) C(43) 178(1) . . . . yes C(4) C(41) C(46) C(45) 178(1) . . . . yes C(5) C(1) C(2) C(21) -82(1) . . . . yes C(5) C(1) C(13) C(14) -170(1) . . . . yes C(5) C(1) C(13) C(18) 9(1) . . . . yes C(5) C(6) C(7) C(8) 6(1) . . . . yes C(5) C(10) C(9) C(8) 2(2) . . . . yes C(6) C(5) C(1) C(13) 55(1) . . . . yes C(6) C(5) C(10) C(9) -2(1) . . . . yes C(6) C(7) C(8) C(9) -5(1) . . . . yes C(7) C(6) C(5) C(10) -2(1) . . . . yes C(7) C(8) N(1) C(11) 10(2) . . . . yes C(7) C(8) N(1) C(12) -166(1) . . . . yes C(7) C(8) C(9) C(10) 1(2) . . . . yes C(9) C(8) N(1) C(11) -168(1) . . . . yes C(9) C(8) N(1) C(12) 15(2) . . . . yes C(10) C(5) C(1) C(13) -128(1) . . . . yes C(13) C(1) C(2) C(21) 95(1) . . . . yes C(13) C(14) C(15) C(16) -2(1) . . . . yes C(13) C(18) C(17) C(16) 0(1) . . . . yes C(14) C(13) C(18) C(17) -4(1) . . . . yes C(14) C(15) C(16) C(17) -2(1) . . . . yes C(15) C(14) C(13) C(18) 5(1) . . . . yes C(15) C(16) N(2) C(19) -8(1) . . . . yes C(15) C(16) N(2) C(20) 179(1) . . . . yes C(15) C(16) C(17) C(18) 4(1) . . . . yes C(17) C(16) N(2) C(19) 170(1) . . . . yes C(17) C(16) N(2) C(20) -2(1) . . . . yes C(21) C(2) C(3) C(27) -57(1) . . . . yes C(21) C(22) C(23) C(24) 0(2) . . . . yes C(21) C(26) C(25) C(24) 0(2) . . . . yes C(22) C(21) C(26) C(25) 0(2) . . . . yes C(22) C(23) C(24) C(25) 0(2) . . . . yes C(23) C(22) C(21) C(26) 0(2) . . . . yes C(23) C(24) C(25) C(26) 0(2) . . . . yes C(27) C(3) C(4) C(33) -85(1) . . . . yes C(27) C(3) C(4) C(41) 93(1) . . . . yes C(27) C(28) C(29) C(30) 0(1) . . . . yes C(27) C(32) C(31) C(30) -1(1) . . . . yes C(28) C(27) C(32) C(31) 3(1) . . . . yes C(28) C(29) C(30) C(31) 0(1) . . . . yes C(29) C(28) C(27) C(32) -2(1) . . . . yes C(29) C(30) C(31) C(32) 0(1) . . . . yes C(33) C(4) C(41) C(42) 24(1) . . . . yes C(33) C(4) C(41) C(46) -158(1) . . . . yes C(33) C(34) C(35) C(36) -1(2) . . . . yes C(33) C(38) C(37) C(36) -1(1) . . . . yes C(34) C(33) C(4) C(41) -151(1) . . . . yes C(34) C(33) C(38) C(37) -2(1) . . . . yes C(34) C(35) C(36) C(37) -2(1) . . . . yes C(35) C(34) C(33) C(38) 4(2) . . . . yes C(35) C(36) N(3) C(39) -16(1) . . . . yes C(35) C(36) N(3) C(40) 158(1) . . . . yes C(35) C(36) C(37) C(38) 4(1) . . . . yes C(37) C(36) N(3) C(39) 160(1) . . . . yes C(37) C(36) N(3) C(40) -24(1) . . . . yes C(38) C(33) C(4) C(41) 35(1) . . . . yes C(41) C(42) C(43) C(44) 3(1) . . . . yes C(41) C(46) C(45) C(44) 2(2) . . . . yes C(42) C(41) C(46) C(45) -3(1) . . . . yes C(42) C(43) C(44) C(45) -5(1) . . . . yes C(43) C(42) C(41) C(46) 0(1) . . . . yes C(43) C(44) N(4) C(47) -5(1) . . . . yes C(43) C(44) N(4) C(48) 171(1) . . . . yes C(43) C(44) C(45) C(46) 2(1) . . . . yes C(45) C(44) N(4) C(47) 179(1) . . . . yes C(45) C(44) N(4) C(48) -3(1) . . . . yes C(45) C(44) N(4) C(48) -3(1) . . . . 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 I(1) I(2) 2.911(2) . . ? I(2) I(3) 2.949(2) . . ? I(4) I(5) 2.973(1) . . ? I(5) I(6) 2.881(2) . . ? N(2) C(30) 3.40(2) . 2_655 ? C(15) C(29) 3.30(2) . 2_655 ? C(16) C(29) 3.32(2) . 2_655 ? C(16) C(30) 3.44(2) . 2_655 ? C(18) C(40) 3.53(2) . 1_655 ? C(19) C(23) 3.46(2) . 2_655 ? C(24) C(35) 3.47(2) . 1_655 ? C(25) C(44) 3.38(2) . 2_655 ? C(25) C(43) 3.45(2) . 2_655 ? C(29) C(39) 3.45(2) . 2_545 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_Compound_3 _database_code_CSD 164962 _audit_creation_date 'Sat Feb 10 15:04:52 2001' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C48 H50 N4 ' _chemical_formula_moiety 'C48 H50 N4 ' _chemical_formula_weight 682.95 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 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 _cell_length_a 14.612(3) _cell_length_b 16.076(2) _cell_length_c 17.1807(7) _cell_angle_alpha 90 _cell_angle_beta 91.792(1) _cell_angle_gamma 90 _cell_volume 4034.0(10) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 110.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'cube' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.124 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.066 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_reflns_number 24462 _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_theta_max 26.00 _diffrn_measured_fraction_theta_max 0.9754 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.9754 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 1.5 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7741 _reflns_number_gt 3614 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.0656 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4074 _refine_ls_number_parameters 469 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]' _refine_ls_shift/su_max 0.0001 _refine_diff_density_max 0.31 _refine_diff_density_min -0.25 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_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) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N(1) N 0.0559(2) -0.2097(2) 0.4713(2) 0.047(1) Uani 1.00 d . . . N(2) N 0.6868(2) -0.1071(2) 0.3901(2) 0.038(1) Uani 1.00 d . . . N(3) N 0.3194(2) -0.3144(2) 0.1096(2) 0.042(1) Uani 1.00 d . . . N(4) N -0.2420(2) 0.0146(2) 0.1463(2) 0.049(1) Uani 1.00 d . . . C(1) C 0.3179(2) -0.0194(2) 0.3062(2) 0.026(1) Uani 1.00 d . . . C(2) C 0.2949(2) 0.0408(2) 0.2533(2) 0.025(1) Uani 1.00 d . . . C(3) C 0.1978(2) 0.0548(2) 0.2270(2) 0.026(1) Uani 1.00 d . . . C(4) C 0.1478(2) -0.0069(2) 0.1921(2) 0.028(1) Uani 1.00 d . . . C(5) C 0.2484(2) -0.0680(2) 0.3482(2) 0.026(1) Uani 1.00 d . . . C(6) C 0.1741(2) -0.0310(2) 0.3839(2) 0.028(1) Uani 1.00 d . . . C(7) C 0.1107(2) -0.0770(2) 0.4241(2) 0.031(1) Uani 1.00 d . . . C(8) C 0.1187(2) -0.1635(3) 0.4311(2) 0.033(1) Uani 1.00 d . . . C(9) C 0.1932(3) -0.2009(2) 0.3955(2) 0.036(1) Uani 1.00 d . . . C(10) C 0.2558(2) -0.1543(2) 0.3554(2) 0.030(1) Uani 1.00 d . . . C(11) C -0.0092(3) -0.1681(3) 0.5192(3) 0.064(2) Uani 1.00 d . . . C(12) C 0.0675(3) -0.2985(3) 0.4783(3) 0.051(1) Uani 1.00 d . . . C(13) C 0.4143(2) -0.0436(2) 0.3259(2) 0.027(1) Uani 1.00 d . . . C(14) C 0.4789(2) -0.0595(2) 0.2697(2) 0.031(1) Uani 1.00 d . . . C(15) C 0.5678(2) -0.0821(2) 0.2903(2) 0.035(1) Uani 1.00 d . . . C(16) C 0.5970(2) -0.0880(2) 0.3686(2) 0.031(1) Uani 1.00 d . . . C(17) C 0.5318(2) -0.0735(2) 0.4253(2) 0.031(1) Uani 1.00 d . . . C(18) C 0.4424(2) -0.0530(2) 0.4032(2) 0.029(1) Uani 1.00 d . . . C(19) C 0.7478(3) -0.1393(3) 0.3323(3) 0.049(1) Uani 1.00 d . . . C(20) C 0.7106(3) -0.1233(3) 0.4707(3) 0.049(1) Uani 1.00 d . . . C(21) C 0.3625(2) 0.1000(2) 0.2197(2) 0.029(1) Uani 1.00 d . . . C(22) C 0.3515(2) 0.1262(2) 0.1430(2) 0.035(1) Uani 1.00 d . . . C(23) C 0.4132(3) 0.1809(3) 0.1099(2) 0.043(1) Uani 1.00 d . . . C(24) C 0.4865(3) 0.2116(3) 0.1549(3) 0.044(1) Uani 1.00 d . . . C(25) C 0.4968(3) 0.1885(3) 0.2308(3) 0.040(1) Uani 1.00 d . . . C(26) C 0.4360(2) 0.1330(2) 0.2637(2) 0.034(1) Uani 1.00 d . . . C(27) C 0.1612(2) 0.1386(2) 0.2446(2) 0.026(1) Uani 1.00 d . . . C(28) C 0.0973(2) 0.1789(2) 0.1953(2) 0.028(1) Uani 1.00 d . . . C(29) C 0.0624(2) 0.2563(2) 0.2142(2) 0.033(1) Uani 1.00 d . . . C(30) C 0.0924(2) 0.2960(2) 0.2817(2) 0.034(1) Uani 1.00 d . . . C(31) C 0.1584(2) 0.2589(2) 0.3293(2) 0.032(1) Uani 1.00 d . . . C(32) C 0.1922(2) 0.1815(2) 0.3110(2) 0.028(1) Uani 1.00 d . . . C(33) C 0.1902(2) -0.0864(2) 0.1672(2) 0.026(1) Uani 1.00 d . . . C(34) C 0.1516(2) -0.1638(2) 0.1833(2) 0.030(1) Uani 1.00 d . . . C(35) C 0.1918(3) -0.2380(2) 0.1635(2) 0.034(1) Uani 1.00 d . . . C(36) C 0.2749(2) -0.2395(2) 0.1250(2) 0.032(1) Uani 1.00 d . . . C(37) C 0.3130(2) -0.1630(3) 0.1061(2) 0.034(1) Uani 1.00 d . . . C(38) C 0.2723(2) -0.0887(2) 0.1273(2) 0.034(1) Uani 1.00 d . . . C(39) C 0.2668(3) -0.3882(3) 0.0921(3) 0.049(1) Uani 1.00 d . . . C(40) C 0.4045(3) -0.3110(3) 0.0673(3) 0.055(2) Uani 1.00 d . . . C(41) C 0.0460(2) -0.0026(2) 0.1805(2) 0.026(1) Uani 1.00 d . . . C(42) C 0.0033(2) -0.0230(2) 0.1096(2) 0.030(1) Uani 1.00 d . . . C(43) C -0.0904(2) -0.0170(2) 0.0968(2) 0.033(1) Uani 1.00 d . . . C(44) C -0.1467(2) 0.0099(2) 0.1566(2) 0.034(1) Uani 1.00 d . . . C(45) C -0.1046(2) 0.0291(2) 0.2283(2) 0.031(1) Uani 1.00 d . . . C(46) C -0.0111(2) 0.0229(2) 0.2398(2) 0.029(1) Uani 1.00 d . . . C(47) C -0.2923(3) 0.0733(3) 0.1929(3) 0.057(2) Uani 1.00 d . . . C(48) C -0.2817(3) -0.0032(5) 0.0706(3) 0.104(2) Uani 1.00 d . . . H(1) H 0.1662 0.0286 0.3799 0.0342 Uiso 1.00 calc . . . H(2) H 0.0594 -0.0484 0.4480 0.0411 Uiso 1.00 calc . . . H(3) H 0.2013 -0.2605 0.3988 0.0449 Uiso 1.00 calc . . . H(4) H 0.3067 -0.1826 0.3313 0.0385 Uiso 1.00 calc . . . H(5) H 0.0220 -0.1372 0.5597 0.0774 Uiso 1.00 calc . . . H(6) H -0.0459 -0.1297 0.4889 0.0774 Uiso 1.00 calc . . . H(7) H -0.0492 -0.2070 0.5428 0.0774 Uiso 1.00 calc . . . H(8) H 0.0185 -0.3232 0.5066 0.0612 Uiso 1.00 calc . . . H(9) H 0.0673 -0.3247 0.4277 0.0612 Uiso 1.00 calc . . . H(10) H 0.1239 -0.3120 0.5047 0.0612 Uiso 1.00 calc . . . H(11) H 0.4600 -0.0540 0.2146 0.0391 Uiso 1.00 calc . . . H(12) H 0.6110 -0.0938 0.2503 0.0407 Uiso 1.00 calc . . . H(13) H 0.5496 -0.0784 0.4800 0.0400 Uiso 1.00 calc . . . H(14) H 0.3983 -0.0451 0.4429 0.0360 Uiso 1.00 calc . . . H(15) H 0.7238 -0.1906 0.3108 0.0573 Uiso 1.00 calc . . . H(16) H 0.7526 -0.1006 0.2899 0.0573 Uiso 1.00 calc . . . H(17) H 0.8074 -0.1497 0.3536 0.0573 Uiso 1.00 calc . . . H(18) H 0.6764 -0.1698 0.4901 0.0588 Uiso 1.00 calc . . . H(19) H 0.7743 -0.1355 0.4788 0.0588 Uiso 1.00 calc . . . H(20) H 0.6966 -0.0759 0.5029 0.0588 Uiso 1.00 calc . . . H(21) H 0.2992 0.1059 0.1125 0.0430 Uiso 1.00 calc . . . H(22) H 0.4051 0.1976 0.0559 0.0543 Uiso 1.00 calc . . . H(23) H 0.5300 0.2493 0.1324 0.0528 Uiso 1.00 calc . . . H(24) H 0.5477 0.2101 0.2622 0.0501 Uiso 1.00 calc . . . H(25) H 0.4437 0.1178 0.3187 0.0423 Uiso 1.00 calc . . . H(26) H 0.0769 0.1515 0.1479 0.0368 Uiso 1.00 calc . . . H(27) H 0.0172 0.2825 0.1802 0.0403 Uiso 1.00 calc . . . H(28) H 0.0674 0.3495 0.2952 0.0394 Uiso 1.00 calc . . . H(29) H 0.1804 0.2875 0.3762 0.0401 Uiso 1.00 calc . . . H(30) H 0.2395 0.1561 0.3441 0.0357 Uiso 1.00 calc . . . H(31) H 0.0939 -0.1649 0.2096 0.0376 Uiso 1.00 calc . . . H(32) H 0.1626 -0.2897 0.1767 0.0422 Uiso 1.00 calc . . . H(33) H 0.3689 -0.1616 0.0778 0.0395 Uiso 1.00 calc . . . H(34) H 0.3018 -0.0361 0.1148 0.0429 Uiso 1.00 calc . . . H(35) H 0.2111 -0.3882 0.1203 0.0568 Uiso 1.00 calc . . . H(36) H 0.2508 -0.3905 0.0376 0.0568 Uiso 1.00 calc . . . H(37) H 0.3005 -0.4371 0.1057 0.0568 Uiso 1.00 calc . . . H(38) H 0.4429 -0.3580 0.0804 0.0653 Uiso 1.00 calc . . . H(39) H 0.3926 -0.3116 0.0125 0.0653 Uiso 1.00 calc . . . H(40) H 0.4384 -0.2616 0.0803 0.0653 Uiso 1.00 calc . . . H(41) H 0.0416 -0.0416 0.0676 0.0359 Uiso 1.00 calc . . . H(42) H -0.1179 -0.0321 0.0467 0.0411 Uiso 1.00 calc . . . H(43) H -0.1424 0.0462 0.2705 0.0396 Uiso 1.00 calc . . . H(44) H 0.0167 0.0379 0.2898 0.0379 Uiso 1.00 calc . . . H(45) H -0.2814 0.0622 0.2473 0.0699 Uiso 1.00 calc . . . H(46) H -0.2724 0.1287 0.1825 0.0699 Uiso 1.00 calc . . . H(47) H -0.3563 0.0695 0.1816 0.0699 Uiso 1.00 calc . . . H(48) H -0.3468 0.0005 0.0695 0.1218 Uiso 1.00 calc . . . H(49) H -0.2590 0.0342 0.0322 0.1218 Uiso 1.00 calc . . . H(50) H -0.2658 -0.0591 0.0542 0.1218 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) 0.044(2) 0.050(2) -0.013(2) 0.011(2) 0.011(2) N(2) 0.022(2) 0.042(2) 0.048(2) 0.007(2) -0.001(2) -0.008(2) N(3) 0.039(2) 0.033(2) 0.055(2) 0.012(2) -0.001(2) -0.013(2) N(4) 0.025(2) 0.076(3) 0.048(2) 0.011(2) -0.005(2) -0.009(2) C(1) 0.024(2) 0.024(2) 0.030(2) 0.002(2) 0.003(2) -0.006(2) C(2) 0.021(2) 0.025(2) 0.028(2) -0.001(2) 0.004(2) -0.001(2) C(3) 0.024(2) 0.023(2) 0.032(2) -0.001(2) 0.004(2) 0.001(2) C(4) 0.026(2) 0.028(2) 0.030(2) 0.001(2) 0.007(2) -0.001(2) C(5) 0.023(2) 0.030(2) 0.025(2) 0.001(2) 0.000(2) 0.004(2) C(6) 0.025(2) 0.027(2) 0.032(2) 0.000(2) -0.001(2) 0.003(2) C(7) 0.026(2) 0.036(2) 0.031(2) 0.000(2) 0.002(2) 0.005(2) C(8) 0.031(2) 0.037(3) 0.030(2) -0.008(2) 0.000(2) 0.004(2) C(9) 0.041(2) 0.031(2) 0.036(2) -0.005(2) -0.002(2) 0.001(2) C(10) 0.030(2) 0.028(2) 0.033(2) 0.002(2) 0.000(2) 0.002(2) C(11) 0.044(3) 0.077(4) 0.071(4) -0.008(3) 0.021(2) 0.027(3) C(12) 0.045(3) 0.050(3) 0.058(3) -0.020(2) -0.010(2) 0.022(2) C(13) 0.024(2) 0.024(2) 0.033(2) -0.001(2) 0.003(2) 0.001(2) C(14) 0.030(2) 0.029(2) 0.033(2) 0.003(2) 0.005(2) -0.001(2) C(15) 0.030(2) 0.030(2) 0.048(3) 0.003(2) 0.015(2) 0.001(2) C(16) 0.023(2) 0.023(2) 0.046(3) 0.002(2) 0.003(2) 0.000(2) C(17) 0.026(2) 0.028(2) 0.039(2) 0.000(2) -0.001(2) -0.004(2) C(18) 0.029(2) 0.024(2) 0.036(2) 0.001(2) 0.005(2) -0.004(2) C(19) 0.028(2) 0.049(3) 0.071(3) 0.012(2) 0.013(2) -0.002(2) C(20) 0.025(2) 0.051(3) 0.071(3) 0.013(2) -0.008(2) -0.006(2) C(21) 0.023(2) 0.023(2) 0.040(2) 0.002(2) 0.002(2) 0.000(2) C(22) 0.028(2) 0.034(2) 0.044(3) -0.001(2) 0.005(2) 0.002(2) C(23) 0.038(2) 0.039(3) 0.052(3) 0.002(2) 0.007(2) 0.014(2) C(24) 0.032(2) 0.031(3) 0.071(3) -0.001(2) 0.015(2) 0.016(2) C(25) 0.027(2) 0.033(3) 0.061(3) -0.001(2) 0.004(2) 0.001(2) C(26) 0.028(2) 0.027(2) 0.046(3) 0.000(2) 0.007(2) 0.003(2) C(27) 0.018(2) 0.027(2) 0.032(2) 0.000(2) 0.006(2) 0.003(2) C(28) 0.025(2) 0.027(2) 0.033(2) -0.002(2) 0.002(2) 0.001(2) C(29) 0.024(2) 0.028(2) 0.046(3) 0.001(2) 0.003(2) 0.004(2) C(30) 0.028(2) 0.024(2) 0.051(3) 0.003(2) 0.013(2) -0.001(2) C(31) 0.032(2) 0.029(2) 0.035(2) -0.005(2) 0.009(2) -0.005(2) C(32) 0.028(2) 0.028(2) 0.028(2) 0.001(2) 0.001(2) 0.001(2) C(33) 0.022(2) 0.026(2) 0.029(2) 0.001(2) 0.001(2) -0.002(2) C(34) 0.027(2) 0.029(2) 0.035(2) 0.000(2) 0.000(2) 0.000(2) C(35) 0.034(2) 0.027(2) 0.039(2) 0.004(2) -0.005(2) -0.002(2) C(36) 0.029(2) 0.031(2) 0.036(2) 0.007(2) -0.005(2) -0.006(2) C(37) 0.024(2) 0.041(3) 0.037(2) 0.006(2) 0.004(2) -0.010(2) C(38) 0.028(2) 0.034(2) 0.040(2) -0.004(2) 0.005(2) -0.004(2) C(39) 0.064(3) 0.030(3) 0.054(3) 0.015(2) 0.006(2) -0.004(2) C(40) 0.042(3) 0.052(3) 0.071(3) 0.017(2) -0.002(2) -0.023(3) C(41) 0.026(2) 0.021(2) 0.031(2) 0.001(2) 0.002(2) 0.002(2) C(42) 0.029(2) 0.025(2) 0.036(2) 0.000(2) 0.006(2) -0.001(2) C(43) 0.033(2) 0.038(2) 0.028(2) -0.001(2) -0.004(2) 0.001(2) C(44) 0.024(2) 0.034(2) 0.043(3) 0.003(2) 0.001(2) 0.004(2) C(45) 0.025(2) 0.037(2) 0.032(2) 0.005(2) 0.004(2) -0.004(2) C(46) 0.028(2) 0.026(2) 0.034(2) 0.002(2) 0.002(2) -0.003(2) C(47) 0.026(2) 0.056(3) 0.089(4) 0.009(2) 0.009(2) 0.003(3) C(48) 0.039(3) 0.207(8) 0.066(4) 0.026(4) -0.015(3) -0.013(4) #------------------------------------------------------------------------------ _computing_data_collection '.' _computing_cell_refinement '.' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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(8) 1.382(5) . . yes N(1) C(11) 1.441(6) . . yes N(1) C(12) 1.442(5) . . yes N(2) C(16) 1.387(4) . . yes N(2) C(19) 1.450(5) . . yes N(2) C(20) 1.441(5) . . yes N(3) C(36) 1.398(5) . . yes N(3) C(39) 1.441(5) . . yes N(3) C(40) 1.460(5) . . yes N(4) C(44) 1.400(4) . . yes N(4) C(47) 1.451(5) . . yes N(4) C(48) 1.436(6) . . yes C(1) C(2) 1.362(5) . . yes C(1) C(5) 1.486(5) . . yes C(1) C(13) 1.490(4) . . yes C(2) C(3) 1.493(5) . . yes C(2) C(21) 1.500(5) . . yes C(3) C(4) 1.361(5) . . yes C(3) C(27) 1.484(5) . . yes C(4) C(33) 1.490(5) . . yes C(4) C(41) 1.496(5) . . yes C(5) C(6) 1.397(5) . . yes C(5) C(10) 1.397(5) . . yes C(6) C(7) 1.387(5) . . yes C(7) C(8) 1.401(5) . . yes C(8) C(9) 1.401(5) . . yes C(9) C(10) 1.383(5) . . yes C(13) C(14) 1.395(5) . . yes C(13) C(18) 1.385(5) . . yes C(14) C(15) 1.383(5) . . yes C(15) C(16) 1.403(5) . . yes C(16) C(17) 1.402(5) . . yes C(17) C(18) 1.389(5) . . yes C(21) C(22) 1.388(5) . . yes C(21) C(26) 1.397(5) . . yes C(22) C(23) 1.393(5) . . yes C(23) C(24) 1.392(6) . . yes C(24) C(25) 1.361(6) . . yes C(25) C(26) 1.391(5) . . yes C(27) C(28) 1.399(5) . . yes C(27) C(32) 1.397(5) . . yes C(28) C(29) 1.388(5) . . yes C(29) C(30) 1.383(5) . . yes C(30) C(31) 1.379(5) . . yes C(31) C(32) 1.378(5) . . yes C(33) C(34) 1.396(5) . . yes C(33) C(38) 1.400(5) . . yes C(34) C(35) 1.378(5) . . yes C(35) C(36) 1.400(5) . . yes C(36) C(37) 1.394(5) . . yes C(37) C(38) 1.388(5) . . yes C(41) C(42) 1.391(5) . . yes C(41) C(46) 1.398(5) . . yes C(42) C(43) 1.382(5) . . yes C(43) C(44) 1.405(5) . . yes C(44) C(45) 1.394(5) . . yes C(45) C(46) 1.378(5) . . 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(8) N(1) C(11) 119.8(4) . 1_555 1_555 yes C(8) N(1) C(12) 119.6(4) . 1_555 1_555 yes C(11) N(1) C(12) 119.3(4) . 1_555 1_555 yes C(16) N(2) C(19) 119.6(3) . 1_555 1_555 yes C(16) N(2) C(20) 119.6(3) . 1_555 1_555 yes C(19) N(2) C(20) 117.3(3) . 1_555 1_555 yes C(36) N(3) C(39) 120.0(3) . 1_555 1_555 yes C(36) N(3) C(40) 118.1(3) . 1_555 1_555 yes C(39) N(3) C(40) 112.6(3) . 1_555 1_555 yes C(44) N(4) C(47) 119.0(3) . 1_555 1_555 yes C(44) N(4) C(48) 118.4(4) . 1_555 1_555 yes C(47) N(4) C(48) 115.6(4) . 1_555 1_555 yes C(2) C(1) C(5) 122.7(3) . 1_555 1_555 yes C(2) C(1) C(13) 123.3(3) . 1_555 1_555 yes C(5) C(1) C(13) 114.1(3) . 1_555 1_555 yes C(1) C(2) C(3) 121.4(3) . 1_555 1_555 yes C(1) C(2) C(21) 123.8(3) . 1_555 1_555 yes C(3) C(2) C(21) 114.8(3) . 1_555 1_555 yes C(2) C(3) C(4) 121.1(3) . 1_555 1_555 yes C(2) C(3) C(27) 114.9(3) . 1_555 1_555 yes C(4) C(3) C(27) 124.0(3) . 1_555 1_555 yes C(3) C(4) C(33) 122.0(3) . 1_555 1_555 yes C(3) C(4) C(41) 123.0(3) . 1_555 1_555 yes C(33) C(4) C(41) 114.9(3) . 1_555 1_555 yes C(1) C(5) C(6) 122.8(3) . 1_555 1_555 yes C(1) C(5) C(10) 120.9(3) . 1_555 1_555 yes C(6) C(5) C(10) 116.3(3) . 1_555 1_555 yes C(5) C(6) C(7) 122.2(3) . 1_555 1_555 yes C(6) C(7) C(8) 121.1(4) . 1_555 1_555 yes N(1) C(8) C(7) 121.4(4) . 1_555 1_555 yes N(1) C(8) C(9) 121.7(4) . 1_555 1_555 yes C(7) C(8) C(9) 117.0(3) . 1_555 1_555 yes C(8) C(9) C(10) 121.3(4) . 1_555 1_555 yes C(5) C(10) C(9) 122.2(4) . 1_555 1_555 yes C(1) C(13) C(14) 123.1(3) . 1_555 1_555 yes C(1) C(13) C(18) 119.7(3) . 1_555 1_555 yes C(14) C(13) C(18) 117.2(3) . 1_555 1_555 yes C(13) C(14) C(15) 121.4(3) . 1_555 1_555 yes C(14) C(15) C(16) 121.2(3) . 1_555 1_555 yes N(2) C(16) C(15) 121.8(3) . 1_555 1_555 yes N(2) C(16) C(17) 120.7(4) . 1_555 1_555 yes C(15) C(16) C(17) 117.5(3) . 1_555 1_555 yes C(16) C(17) C(18) 120.2(3) . 1_555 1_555 yes C(13) C(18) C(17) 122.4(3) . 1_555 1_555 yes C(2) C(21) C(22) 119.9(3) . 1_555 1_555 yes C(2) C(21) C(26) 122.4(3) . 1_555 1_555 yes C(22) C(21) C(26) 117.6(3) . 1_555 1_555 yes C(21) C(22) C(23) 121.4(3) . 1_555 1_555 yes C(22) C(23) C(24) 119.6(4) . 1_555 1_555 yes C(23) C(24) C(25) 119.6(4) . 1_555 1_555 yes C(24) C(25) C(26) 120.8(4) . 1_555 1_555 yes C(21) C(26) C(25) 120.8(4) . 1_555 1_555 yes C(3) C(27) C(28) 122.3(3) . 1_555 1_555 yes C(3) C(27) C(32) 120.3(3) . 1_555 1_555 yes C(28) C(27) C(32) 117.3(3) . 1_555 1_555 yes C(27) C(28) C(29) 121.1(3) . 1_555 1_555 yes C(28) C(29) C(30) 120.1(3) . 1_555 1_555 yes C(29) C(30) C(31) 119.6(3) . 1_555 1_555 yes C(30) C(31) C(32) 120.3(3) . 1_555 1_555 yes C(27) C(32) C(31) 121.5(3) . 1_555 1_555 yes C(4) C(33) C(34) 122.2(3) . 1_555 1_555 yes C(4) C(33) C(38) 122.3(3) . 1_555 1_555 yes C(34) C(33) C(38) 115.6(3) . 1_555 1_555 yes C(33) C(34) C(35) 122.9(3) . 1_555 1_555 yes C(34) C(35) C(36) 121.0(4) . 1_555 1_555 yes N(3) C(36) C(35) 121.4(4) . 1_555 1_555 yes N(3) C(36) C(37) 121.6(4) . 1_555 1_555 yes C(35) C(36) C(37) 117.0(3) . 1_555 1_555 yes C(36) C(37) C(38) 121.4(3) . 1_555 1_555 yes C(33) C(38) C(37) 122.1(4) . 1_555 1_555 yes C(4) C(41) C(42) 121.6(3) . 1_555 1_555 yes C(4) C(41) C(46) 122.0(3) . 1_555 1_555 yes C(42) C(41) C(46) 116.5(3) . 1_555 1_555 yes C(41) C(42) C(43) 122.6(4) . 1_555 1_555 yes C(42) C(43) C(44) 120.3(3) . 1_555 1_555 yes N(4) C(44) C(43) 121.8(4) . 1_555 1_555 yes N(4) C(44) C(45) 120.6(4) . 1_555 1_555 yes C(43) C(44) C(45) 117.5(3) . 1_555 1_555 yes C(44) C(45) C(46) 121.3(3) . 1_555 1_555 yes C(41) C(46) C(45) 121.9(3) . 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(8) C(7) C(6) 179.8(3) 1_555 1_555 1_555 1_555 yes N(1) C(8) C(9) C(10) -180.0(4) 1_555 1_555 1_555 1_555 yes N(2) C(16) C(15) C(14) -177.2(3) 1_555 1_555 1_555 1_555 yes N(2) C(16) C(17) C(18) 178.9(3) 1_555 1_555 1_555 1_555 yes N(3) C(36) C(35) C(34) 175.4(3) 1_555 1_555 1_555 1_555 yes N(3) C(36) C(37) C(38) -174.6(3) 1_555 1_555 1_555 1_555 yes N(4) C(44) C(43) C(42) -178.3(4) 1_555 1_555 1_555 1_555 yes N(4) C(44) C(45) C(46) 178.5(4) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) -59.1(5) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(27) 118.7(4) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(21) C(22) 145.0(4) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(21) C(26) -37.2(5) 1_555 1_555 1_555 1_555 yes C(1) C(5) C(6) C(7) -178.8(3) 1_555 1_555 1_555 1_555 yes C(1) C(5) C(10) C(9) 178.7(3) 1_555 1_555 1_555 1_555 yes C(1) C(13) C(14) C(15) -179.8(4) 1_555 1_555 1_555 1_555 yes C(1) C(13) C(18) C(17) -178.4(3) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(5) C(6) -47.2(5) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(5) C(10) 134.3(4) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(13) C(14) -47.5(5) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(13) C(18) 134.1(4) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(33) -9.8(5) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(41) 166.3(3) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(27) C(28) 146.3(3) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(27) C(32) -31.6(5) 1_555 1_555 1_555 1_555 yes C(2) C(21) C(22) C(23) -179.8(4) 1_555 1_555 1_555 1_555 yes C(2) C(21) C(26) C(25) -179.3(4) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(5) -7.5(5) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(13) 171.2(3) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(21) C(22) -37.6(5) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(21) C(26) 140.1(3) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(33) C(34) 133.6(4) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(33) C(38) -45.2(5) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(41) C(42) 133.6(4) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(41) C(46) -45.6(5) 1_555 1_555 1_555 1_555 yes C(3) C(27) C(28) C(29) 178.3(3) 1_555 1_555 1_555 1_555 yes C(3) C(27) C(32) C(31) -179.1(3) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(2) C(21) 123.5(4) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(27) C(28) -36.0(5) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(27) C(32) 146.1(4) 1_555 1_555 1_555 1_555 yes C(4) C(33) C(34) C(35) -177.2(3) 1_555 1_555 1_555 1_555 yes C(4) C(33) C(38) C(37) 178.1(3) 1_555 1_555 1_555 1_555 yes C(4) C(41) C(42) C(43) -177.9(4) 1_555 1_555 1_555 1_555 yes C(4) C(41) C(46) C(45) 178.1(4) 1_555 1_555 1_555 1_555 yes C(5) C(1) C(2) C(21) 169.7(3) 1_555 1_555 1_555 1_555 yes C(5) C(1) C(13) C(14) 131.3(4) 1_555 1_555 1_555 1_555 yes C(5) C(1) C(13) C(18) -47.2(5) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) 0.3(6) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(8) 0.0(6) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(1) C(13) 134.0(3) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(9) 0.1(5) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) -0.2(5) 1_555 1_555 1_555 1_555 yes C(7) C(6) C(5) C(10) -0.2(5) 1_555 1_555 1_555 1_555 yes C(7) C(8) N(1) C(11) -11.8(6) 1_555 1_555 1_555 1_555 yes C(7) C(8) N(1) C(12) -178.9(4) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) 0.1(5) 1_555 1_555 1_555 1_555 yes C(9) C(8) N(1) C(11) 168.2(4) 1_555 1_555 1_555 1_555 yes C(9) C(8) N(1) C(12) 1.2(6) 1_555 1_555 1_555 1_555 yes C(10) C(5) C(1) C(13) -44.5(5) 1_555 1_555 1_555 1_555 yes C(13) C(1) C(2) C(21) -11.6(5) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) -1.6(6) 1_555 1_555 1_555 1_555 yes C(13) C(18) C(17) C(16) -2.0(6) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(18) C(17) 3.1(5) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) 2.7(6) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(18) -1.3(5) 1_555 1_555 1_555 1_555 yes C(15) C(16) N(2) C(19) -13.5(6) 1_555 1_555 1_555 1_555 yes C(15) C(16) N(2) C(20) -171.7(4) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(18) -1.0(5) 1_555 1_555 1_555 1_555 yes C(17) C(16) N(2) C(19) 166.6(4) 1_555 1_555 1_555 1_555 yes C(17) C(16) N(2) C(20) 8.4(5) 1_555 1_555 1_555 1_555 yes C(21) C(2) C(3) C(27) -58.7(4) 1_555 1_555 1_555 1_555 yes C(21) C(22) C(23) C(24) -1.3(6) 1_555 1_555 1_555 1_555 yes C(21) C(26) C(25) C(24) -0.4(6) 1_555 1_555 1_555 1_555 yes C(22) C(21) C(26) C(25) -1.5(5) 1_555 1_555 1_555 1_555 yes C(22) C(23) C(24) C(25) -0.7(6) 1_555 1_555 1_555 1_555 yes C(23) C(22) C(21) C(26) 2.3(6) 1_555 1_555 1_555 1_555 yes C(23) C(24) C(25) C(26) 1.5(6) 1_555 1_555 1_555 1_555 yes C(27) C(3) C(4) C(33) 172.6(3) 1_555 1_555 1_555 1_555 yes C(27) C(3) C(4) C(41) -11.3(6) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(30) 1.8(5) 1_555 1_555 1_555 1_555 yes C(27) C(32) C(31) C(30) -0.1(5) 1_555 1_555 1_555 1_555 yes C(28) C(27) C(32) C(31) 2.9(5) 1_555 1_555 1_555 1_555 yes C(28) C(29) C(30) C(31) 1.1(5) 1_555 1_555 1_555 1_555 yes C(29) C(28) C(27) C(32) -3.7(5) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(31) C(32) -2.0(5) 1_555 1_555 1_555 1_555 yes C(33) C(4) C(41) C(42) -50.1(5) 1_555 1_555 1_555 1_555 yes C(33) C(4) C(41) C(46) 130.7(4) 1_555 1_555 1_555 1_555 yes C(33) C(34) C(35) C(36) -0.4(5) 1_555 1_555 1_555 1_555 yes C(33) C(38) C(37) C(36) -1.4(6) 1_555 1_555 1_555 1_555 yes C(34) C(33) C(4) C(41) -42.8(5) 1_555 1_555 1_555 1_555 yes C(34) C(33) C(38) C(37) -0.7(5) 1_555 1_555 1_555 1_555 yes C(34) C(35) C(36) C(37) -1.7(5) 1_555 1_555 1_555 1_555 yes C(35) C(34) C(33) C(38) 1.6(5) 1_555 1_555 1_555 1_555 yes C(35) C(36) N(3) C(39) 34.1(5) 1_555 1_555 1_555 1_555 yes C(35) C(36) N(3) C(40) 178.3(3) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(38) 2.6(5) 1_555 1_555 1_555 1_555 yes C(37) C(36) N(3) C(39) -148.8(4) 1_555 1_555 1_555 1_555 yes C(37) C(36) N(3) C(40) -4.6(5) 1_555 1_555 1_555 1_555 yes C(38) C(33) C(4) C(41) 138.5(3) 1_555 1_555 1_555 1_555 yes C(41) C(42) C(43) C(44) -0.4(6) 1_555 1_555 1_555 1_555 yes C(41) C(46) C(45) C(44) 0.1(6) 1_555 1_555 1_555 1_555 yes C(42) C(41) C(46) C(45) -1.2(6) 1_555 1_555 1_555 1_555 yes C(42) C(43) C(44) C(45) -0.7(6) 1_555 1_555 1_555 1_555 yes C(43) C(42) C(41) C(46) 1.3(6) 1_555 1_555 1_555 1_555 yes C(43) C(44) N(4) C(47) -153.7(4) 1_555 1_555 1_555 1_555 yes C(43) C(44) N(4) C(48) -4.4(7) 1_555 1_555 1_555 1_555 yes C(43) C(44) C(45) C(46) 0.9(6) 1_555 1_555 1_555 1_555 yes C(45) C(44) N(4) C(47) 28.8(6) 1_555 1_555 1_555 1_555 yes C(45) C(44) N(4) C(48) 178.1(5) 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) C(39) 3.595(5) . 2_655 ? C(8) C(39) 3.557(6) . 4_545 ? C(15) C(24) 3.544(6) . 2_645 ? C(16) C(24) 3.465(5) . 2_645 ? C(17) C(18) 3.592(5) . 3_656 ? C(19) C(30) 3.265(5) . 2_645 ? C(19) C(29) 3.360(5) . 2_645 ? C(19) C(31) 3.536(6) . 2_645 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_Dication_4(2+)_triiodide_salt _database_code_CSD 164963 _audit_creation_date 'Thu Mar 15 17:16:11 2001' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C48 H50 I6 N4 ' _chemical_formula_moiety '?' _chemical_formula_weight 1444.38 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 9.6884(8) _cell_length_b 23.432(1) _cell_length_c 22.8948(4) _cell_angle_alpha 90 _cell_angle_beta 107.5794(4) _cell_angle_gamma 90 _cell_volume 4954.9(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 97.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'cube' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.936 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 3.799 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_reflns_number 26529 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_theta_max 26.00 _diffrn_measured_fraction_theta_max 0.9568 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.9568 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 9318 _reflns_number_gt 7707 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0430 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 7707 _refine_ls_number_parameters 526 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.90 _refine_diff_density_min -0.91 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_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) ; 'I' 'I' -0.474 1.812 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I(1) I 1.0000 0.0000 0.0000 0.0324(1) Uani 1.00 d S . . I(2) I 1.22172(4) 0.06696(2) 0.08878(2) 0.0428(1) Uani 1.00 d . . . I(3) I 0.5000 0.5000 0.0000 0.0258(1) Uani 1.00 d S . . I(4) I 0.59769(4) 0.43268(1) -0.08771(1) 0.03335(9) Uani 1.00 d . . . I(5) I 0.34330(3) 0.17257(1) 0.22988(1) 0.02654(8) Uani 1.00 d . . . I(6) I 0.37141(3) 0.28641(1) 0.28355(1) 0.02120(7) Uani 1.00 d . . . I(7) I 0.42308(3) 0.39933(1) 0.33944(1) 0.02775(8) Uani 1.00 d . . . N(1) N 0.2081(4) 0.2676(1) -0.0340(1) 0.0158(8) Uani 1.00 d . . . N(2) N 1.0371(4) 0.5093(2) 0.1818(2) 0.0189(9) Uani 1.00 d . . . N(3) N 1.1508(4) 0.3873(2) 0.0591(2) 0.0203(9) Uani 1.00 d . . . N(4) N 0.4559(4) 0.0617(2) -0.0925(2) 0.0233(9) Uani 1.00 d . . . C(1) C 0.7349(4) 0.3019(2) 0.1513(2) 0.0132(9) Uani 1.00 d . . . C(2) C 0.7966(4) 0.2494(2) 0.1866(2) 0.0131(9) Uani 1.00 d . . . C(3) C 0.8055(4) 0.1998(2) 0.1553(2) 0.0139(9) Uani 1.00 d . . . C(4) C 0.8004(4) 0.2031(2) 0.0897(2) 0.0143(9) Uani 1.00 d . . . C(5) C 0.6009(4) 0.2948(2) 0.1044(2) 0.0137(9) Uani 1.00 d . . . C(6) C 0.5016(4) 0.2515(2) 0.1089(2) 0.0132(9) Uani 1.00 d . . . C(7) C 0.3739(4) 0.2420(2) 0.0641(2) 0.0146(9) Uani 1.00 d . . . C(8) C 0.3323(4) 0.2766(2) 0.0106(2) 0.0142(9) Uani 1.00 d . . . C(9) C 0.4300(4) 0.3208(2) 0.0052(2) 0.0143(9) Uani 1.00 d . . . C(10) C 0.5573(4) 0.3292(2) 0.0502(2) 0.0146(9) Uani 1.00 d . . . C(11) C 0.1205(4) 0.2165(2) -0.0326(2) 0.021(1) Uani 1.00 d . . . C(12) C 0.1529(4) 0.3085(2) -0.0830(2) 0.021(1) Uani 1.00 d . . . C(13) C 0.8075(4) 0.3553(2) 0.1650(2) 0.0140(9) Uani 1.00 d . . . C(14) C 0.9571(4) 0.3593(2) 0.1996(2) 0.0141(9) Uani 1.00 d . . . C(15) C 1.0306(4) 0.4096(2) 0.2072(2) 0.0156(10) Uani 1.00 d . . . C(16) C 0.9621(4) 0.4609(2) 0.1799(2) 0.0159(10) Uani 1.00 d . . . C(17) C 0.8096(5) 0.4587(2) 0.1502(2) 0.0181(10) Uani 1.00 d . . . C(18) C 0.7358(4) 0.4078(2) 0.1439(2) 0.0149(9) Uani 1.00 d . . . C(19) C 1.1894(5) 0.5146(2) 0.2192(2) 0.021(1) Uani 1.00 d . . . C(20) C 0.9738(5) 0.5596(2) 0.1455(2) 0.026(1) Uani 1.00 d . . . C(21) C 0.8422(4) 0.2544(2) 0.2548(2) 0.0142(9) Uani 1.00 d . . . C(22) C 0.9677(4) 0.2277(2) 0.2912(2) 0.018(1) Uani 1.00 d . . . C(23) C 1.0143(5) 0.2361(2) 0.3538(2) 0.023(1) Uani 1.00 d . . . C(24) C 0.9347(5) 0.2711(2) 0.3815(2) 0.026(1) Uani 1.00 d . . . C(25) C 0.8094(5) 0.2968(2) 0.3455(2) 0.024(1) Uani 1.00 d . . . C(26) C 0.7643(4) 0.2893(2) 0.2827(2) 0.018(1) Uani 1.00 d . . . C(27) C 0.8315(4) 0.1432(2) 0.1842(2) 0.0148(9) Uani 1.00 d . . . C(28) C 0.9318(4) 0.1064(2) 0.1707(2) 0.0181(10) Uani 1.00 d . . . C(29) C 0.9564(5) 0.0526(2) 0.1963(2) 0.024(1) Uani 1.00 d . . . C(30) C 0.8783(5) 0.0336(2) 0.2347(2) 0.027(1) Uani 1.00 d . . . C(31) C 0.7780(5) 0.0695(2) 0.2474(2) 0.028(1) Uani 1.00 d . . . C(32) C 0.7543(5) 0.1237(2) 0.2231(2) 0.020(1) Uani 1.00 d . . . C(33) C 0.8943(4) 0.2464(2) 0.0763(2) 0.0146(9) Uani 1.00 d . . . C(34) C 1.0321(4) 0.2565(2) 0.1180(2) 0.0139(9) Uani 1.00 d . . . C(35) C 1.1197(4) 0.2998(2) 0.1102(2) 0.0150(9) Uani 1.00 d . . . C(36) C 1.0700(4) 0.3397(2) 0.0626(2) 0.0173(10) Uani 1.00 d . . . C(37) C 0.9326(4) 0.3293(2) 0.0195(2) 0.0157(10) Uani 1.00 d . . . C(38) C 0.8496(4) 0.2831(2) 0.0253(2) 0.0154(10) Uani 1.00 d . . . C(39) C 1.2869(5) 0.3975(2) 0.1079(2) 0.021(1) Uani 1.00 d . . . C(40) C 1.0809(5) 0.4377(2) 0.0274(2) 0.029(1) Uani 1.00 d . . . C(41) C 0.7187(4) 0.1659(2) 0.0455(2) 0.0140(9) Uani 1.00 d . . . C(42) C 0.7485(4) 0.1562(2) -0.0114(2) 0.018(1) Uani 1.00 d . . . C(43) C 0.6665(5) 0.1218(2) -0.0553(2) 0.021(1) Uani 1.00 d . . . C(44) C 0.5417(4) 0.0933(2) -0.0482(2) 0.0186(10) Uani 1.00 d . . . C(45) C 0.5148(4) 0.0995(2) 0.0097(2) 0.0174(10) Uani 1.00 d . . . C(46) C 0.6004(4) 0.1336(2) 0.0545(2) 0.0161(10) Uani 1.00 d . . . C(47) C 0.4767(6) 0.0581(2) -0.1529(2) 0.034(1) Uani 1.00 d . . . C(48) C 0.3302(5) 0.0314(2) -0.0849(2) 0.033(1) Uani 1.00 d . . . H(1) H 0.5269 0.2280 0.1444 0.0149 Uiso 1.00 calc . . . H(2) H 0.3108 0.2123 0.0696 0.0172 Uiso 1.00 calc . . . H(3) H 0.4042 0.3448 -0.0301 0.0150 Uiso 1.00 calc . . . H(4) H 0.6209 0.3588 0.0456 0.0163 Uiso 1.00 calc . . . H(5) H 0.0917 0.2163 0.0035 0.0251 Uiso 1.00 calc . . . H(6) H 0.0360 0.2163 -0.0675 0.0251 Uiso 1.00 calc . . . H(7) H 0.1755 0.1830 -0.0336 0.0251 Uiso 1.00 calc . . . H(8) H 0.1369 0.3444 -0.0664 0.0244 Uiso 1.00 calc . . . H(9) H 0.2209 0.3135 -0.1051 0.0244 Uiso 1.00 calc . . . H(10) H 0.0637 0.2953 -0.1104 0.0244 Uiso 1.00 calc . . . H(11) H 1.0056 0.3251 0.2183 0.0157 Uiso 1.00 calc . . . H(12) H 1.1299 0.4107 0.2316 0.0183 Uiso 1.00 calc . . . H(13) H 0.7574 0.4929 0.1345 0.0207 Uiso 1.00 calc . . . H(14) H 0.6334 0.4078 0.1252 0.0175 Uiso 1.00 calc . . . H(15) H 1.1989 0.5080 0.2609 0.0255 Uiso 1.00 calc . . . H(16) H 1.2471 0.4869 0.2059 0.0255 Uiso 1.00 calc . . . H(17) H 1.2253 0.5516 0.2144 0.0255 Uiso 1.00 calc . . . H(18) H 1.0438 0.5895 0.1527 0.0316 Uiso 1.00 calc . . . H(19) H 0.9455 0.5501 0.1027 0.0316 Uiso 1.00 calc . . . H(20) H 0.8918 0.5721 0.1560 0.0316 Uiso 1.00 calc . . . H(21) H 1.0223 0.2038 0.2724 0.0218 Uiso 1.00 calc . . . H(22) H 1.1001 0.2177 0.3784 0.0253 Uiso 1.00 calc . . . H(23) H 0.9669 0.2770 0.4248 0.0298 Uiso 1.00 calc . . . H(24) H 0.7540 0.3204 0.3645 0.0275 Uiso 1.00 calc . . . H(25) H 0.6788 0.3083 0.2580 0.0201 Uiso 1.00 calc . . . H(26) H 0.9830 0.1189 0.1430 0.0228 Uiso 1.00 calc . . . H(27) H 1.0271 0.0281 0.1882 0.0277 Uiso 1.00 calc . . . H(28) H 0.8950 -0.0036 0.2523 0.0325 Uiso 1.00 calc . . . H(29) H 0.7225 0.0563 0.2733 0.0324 Uiso 1.00 calc . . . H(30) H 0.6844 0.1483 0.2323 0.0229 Uiso 1.00 calc . . . H(31) H 1.0654 0.2322 0.1530 0.0161 Uiso 1.00 calc . . . H(32) H 1.2164 0.3030 0.1372 0.0170 Uiso 1.00 calc . . . H(33) H 0.8961 0.3551 -0.0141 0.0186 Uiso 1.00 calc . . . H(34) H 0.7606 0.2755 -0.0059 0.0178 Uiso 1.00 calc . . . H(35) H 1.3511 0.3659 0.1106 0.0251 Uiso 1.00 calc . . . H(36) H 1.3321 0.4312 0.0999 0.0251 Uiso 1.00 calc . . . H(37) H 1.2677 0.4012 0.1463 0.0251 Uiso 1.00 calc . . . H(38) H 1.1519 0.4664 0.0286 0.0333 Uiso 1.00 calc . . . H(39) H 1.0320 0.4288 -0.0144 0.0333 Uiso 1.00 calc . . . H(40) H 1.0134 0.4519 0.0463 0.0333 Uiso 1.00 calc . . . H(41) H 0.8298 0.1754 -0.0183 0.0216 Uiso 1.00 calc . . . H(42) H 0.6923 0.1160 -0.0928 0.0235 Uiso 1.00 calc . . . H(43) H 0.4348 0.0800 0.0170 0.0215 Uiso 1.00 calc . . . H(44) H 0.5822 0.1363 0.0933 0.0185 Uiso 1.00 calc . . . H(45) H 0.5702 0.0431 -0.1495 0.0406 Uiso 1.00 calc . . . H(46) H 0.4050 0.0345 -0.1792 0.0406 Uiso 1.00 calc . . . H(47) H 0.4698 0.0955 -0.1708 0.0406 Uiso 1.00 calc . . . H(48) H 0.2641 0.0577 -0.0764 0.0385 Uiso 1.00 calc . . . H(49) H 0.2823 0.0111 -0.1216 0.0385 Uiso 1.00 calc . . . H(50) H 0.3607 0.0048 -0.0520 0.0385 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 I(1) 0.0428(3) 0.0299(2) 0.0336(2) 0.0111(2) 0.0254(2) 0.0109(2) I(2) 0.0504(2) 0.0483(2) 0.0409(2) -0.0021(2) 0.0304(2) 0.0019(2) I(3) 0.0256(2) 0.0232(2) 0.0215(2) -0.0068(2) -0.0036(2) 0.0098(2) I(4) 0.0430(2) 0.0266(2) 0.0278(2) -0.0082(1) 0.0067(1) 0.0050(1) I(5) 0.0229(2) 0.0231(2) 0.0311(2) 0.0031(1) 0.0043(1) 0.0078(1) I(6) 0.0142(1) 0.0269(2) 0.0198(1) -0.0005(1) 0.0011(1) 0.0082(1) I(7) 0.0232(2) 0.0235(2) 0.0317(2) -0.0016(1) 0.0010(1) 0.0046(1) N(1) 0.014(2) 0.015(2) 0.017(2) -0.002(1) 0.002(1) 0.000(1) N(2) 0.020(2) 0.018(2) 0.015(2) -0.002(1) -0.001(1) -0.001(1) N(3) 0.021(2) 0.014(2) 0.026(2) 0.000(1) 0.007(1) 0.001(1) N(4) 0.022(2) 0.023(2) 0.022(2) -0.005(2) 0.003(1) -0.005(1) C(1) 0.016(2) 0.014(2) 0.013(2) -0.001(1) 0.008(1) 0.000(1) C(2) 0.010(2) 0.018(2) 0.012(2) 0.000(1) 0.004(1) 0.003(1) C(3) 0.009(2) 0.018(2) 0.015(2) -0.002(1) 0.005(1) 0.001(1) C(4) 0.013(2) 0.018(2) 0.012(2) 0.001(2) 0.005(1) -0.001(1) C(5) 0.016(2) 0.014(2) 0.012(2) 0.002(1) 0.006(1) 0.000(1) C(6) 0.013(2) 0.013(2) 0.014(2) 0.002(1) 0.005(1) 0.001(1) C(7) 0.012(2) 0.014(2) 0.018(2) -0.001(1) 0.005(2) 0.002(1) C(8) 0.014(2) 0.014(2) 0.016(2) 0.001(1) 0.006(1) -0.005(1) C(9) 0.018(2) 0.013(2) 0.012(2) 0.002(2) 0.006(1) 0.003(1) C(10) 0.016(2) 0.010(2) 0.018(2) -0.001(1) 0.006(2) 0.000(1) C(11) 0.017(2) 0.019(2) 0.024(2) -0.006(2) 0.004(2) -0.004(2) C(12) 0.019(2) 0.026(2) 0.014(2) 0.004(2) 0.000(2) 0.001(2) C(13) 0.013(2) 0.016(2) 0.013(2) 0.001(1) 0.003(1) -0.001(1) C(14) 0.014(2) 0.018(2) 0.011(2) 0.000(2) 0.004(1) -0.001(1) C(15) 0.015(2) 0.017(2) 0.015(2) 0.000(2) 0.003(1) 0.000(2) C(16) 0.022(2) 0.016(2) 0.010(2) 0.002(2) 0.006(1) 0.000(1) C(17) 0.023(2) 0.015(2) 0.013(2) 0.001(2) 0.001(2) 0.002(2) C(18) 0.018(2) 0.012(2) 0.012(2) 0.000(2) 0.002(1) -0.002(1) C(19) 0.021(2) 0.019(2) 0.023(2) -0.004(2) 0.005(2) -0.001(2) C(20) 0.031(2) 0.018(2) 0.024(2) -0.002(2) 0.003(2) 0.004(2) C(21) 0.021(2) 0.012(2) 0.009(2) -0.006(2) 0.004(1) 0.002(1) C(22) 0.019(2) 0.016(2) 0.018(2) -0.002(2) 0.004(2) 0.002(2) C(23) 0.022(2) 0.027(2) 0.015(2) -0.003(2) -0.002(2) 0.005(2) C(24) 0.034(3) 0.028(3) 0.014(2) -0.015(2) 0.005(2) 0.000(2) C(25) 0.028(2) 0.030(2) 0.018(2) -0.006(2) 0.014(2) -0.005(2) C(26) 0.019(2) 0.019(2) 0.017(2) -0.003(2) 0.009(2) 0.003(2) C(27) 0.013(2) 0.017(2) 0.011(2) 0.000(2) -0.002(1) -0.001(1) C(28) 0.016(2) 0.015(2) 0.021(2) 0.001(2) 0.002(2) 0.001(2) C(29) 0.017(2) 0.013(2) 0.034(2) 0.003(2) -0.004(2) -0.002(2) C(30) 0.035(3) 0.017(2) 0.022(2) -0.005(2) -0.004(2) 0.005(2) C(31) 0.037(3) 0.026(2) 0.021(2) -0.005(2) 0.011(2) 0.007(2) C(32) 0.019(2) 0.023(2) 0.018(2) 0.000(2) 0.006(2) 0.001(2) C(33) 0.014(2) 0.014(2) 0.017(2) 0.000(1) 0.006(2) -0.003(1) C(34) 0.015(2) 0.016(2) 0.012(2) 0.003(2) 0.007(1) -0.001(1) C(35) 0.014(2) 0.016(2) 0.014(2) 0.000(2) 0.003(1) -0.004(1) C(36) 0.017(2) 0.019(2) 0.020(2) -0.001(2) 0.012(2) -0.001(2) C(37) 0.017(2) 0.021(2) 0.012(2) 0.004(2) 0.009(1) 0.002(2) C(38) 0.013(2) 0.021(2) 0.013(2) 0.001(2) 0.004(1) -0.002(2) C(39) 0.021(2) 0.018(2) 0.025(2) -0.005(2) 0.009(2) -0.002(2) C(40) 0.033(3) 0.023(2) 0.033(3) -0.001(2) 0.013(2) 0.002(2) C(41) 0.015(2) 0.012(2) 0.016(2) 0.002(1) 0.006(1) 0.002(1) C(42) 0.016(2) 0.023(2) 0.017(2) 0.002(2) 0.006(2) -0.002(2) C(43) 0.021(2) 0.025(2) 0.018(2) -0.002(2) 0.006(2) -0.002(2) C(44) 0.018(2) 0.017(2) 0.017(2) 0.004(2) -0.001(2) -0.001(2) C(45) 0.015(2) 0.018(2) 0.019(2) 0.001(2) 0.005(2) 0.002(2) C(46) 0.014(2) 0.017(2) 0.016(2) 0.002(2) 0.002(1) 0.000(2) C(47) 0.038(3) 0.038(3) 0.025(2) -0.004(2) 0.009(2) -0.011(2) C(48) 0.028(2) 0.026(3) 0.037(3) -0.007(2) -0.002(2) -0.004(2) #------------------------------------------------------------------------------ _computing_data_collection '.' _computing_cell_refinement '.' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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 I(1) I(2) 2.9275(4) . . yes I(1) I(2) 2.9275(4) . 3_755 yes I(3) I(4) 2.9264(4) . . yes I(3) I(4) 2.9264(4) . 3_665 yes I(5) I(6) 2.9152(4) . . yes I(6) I(7) 2.9158(4) . . yes N(1) C(8) 1.340(5) . . yes N(1) C(11) 1.474(5) . . yes N(1) C(12) 1.450(5) . . yes N(2) C(16) 1.340(5) . . yes N(2) C(19) 1.471(5) . . yes N(2) C(20) 1.465(5) . . yes N(3) C(36) 1.380(5) . . yes N(3) C(39) 1.467(5) . . yes N(3) C(40) 1.442(6) . . yes N(4) C(44) 1.324(5) . . yes N(4) C(47) 1.459(6) . . yes N(4) C(48) 1.465(6) . . yes C(1) C(2) 1.495(5) . . yes C(1) C(5) 1.423(5) . . yes C(1) C(13) 1.423(6) . . yes C(2) C(3) 1.383(6) . . yes C(2) C(21) 1.494(5) . . yes C(3) C(4) 1.488(5) . . yes C(3) C(27) 1.469(5) . . yes C(4) C(33) 1.457(5) . . yes C(4) C(41) 1.387(5) . . yes C(5) C(6) 1.423(5) . . yes C(5) C(10) 1.433(5) . . yes C(6) C(7) 1.366(5) . . yes C(7) C(8) 1.422(5) . . yes C(8) C(9) 1.433(6) . . yes C(9) C(10) 1.361(5) . . yes C(13) C(14) 1.429(5) . . yes C(13) C(18) 1.422(5) . . yes C(14) C(15) 1.361(6) . . yes C(15) C(16) 1.423(6) . . yes C(16) C(17) 1.429(6) . . yes C(17) C(18) 1.376(6) . . yes C(21) C(22) 1.396(6) . . yes C(21) C(26) 1.392(6) . . yes C(22) C(23) 1.381(6) . . yes C(23) C(24) 1.402(7) . . yes C(24) C(25) 1.383(7) . . yes C(25) C(26) 1.381(6) . . yes C(27) C(28) 1.401(6) . . yes C(27) C(32) 1.402(6) . . yes C(28) C(29) 1.381(6) . . yes C(29) C(30) 1.395(7) . . yes C(30) C(31) 1.381(7) . . yes C(31) C(32) 1.378(6) . . yes C(33) C(34) 1.408(5) . . yes C(33) C(38) 1.409(5) . . yes C(34) C(35) 1.368(6) . . yes C(35) C(36) 1.406(6) . . yes C(36) C(37) 1.418(6) . . yes C(37) C(38) 1.378(6) . . yes C(41) C(42) 1.437(5) . . yes C(41) C(46) 1.439(6) . . yes C(42) C(43) 1.344(6) . . yes C(43) C(44) 1.433(6) . . yes C(44) C(45) 1.435(6) . . yes C(45) C(46) 1.365(6) . . 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 I(2) I(1) I(2) 180.0 . 1_555 3_755 yes I(4) I(3) I(4) 180.0 . 1_555 3_665 yes I(5) I(6) I(7) 175.69(1) . 1_555 1_555 yes C(8) N(1) C(11) 120.2(3) . 1_555 1_555 yes C(8) N(1) C(12) 121.5(3) . 1_555 1_555 yes C(11) N(1) C(12) 118.3(3) . 1_555 1_555 yes C(16) N(2) C(19) 122.0(3) . 1_555 1_555 yes C(16) N(2) C(20) 122.1(3) . 1_555 1_555 yes C(19) N(2) C(20) 115.9(3) . 1_555 1_555 yes C(36) N(3) C(39) 118.9(3) . 1_555 1_555 yes C(36) N(3) C(40) 120.1(4) . 1_555 1_555 yes C(39) N(3) C(40) 115.3(4) . 1_555 1_555 yes C(44) N(4) C(47) 121.5(4) . 1_555 1_555 yes C(44) N(4) C(48) 122.2(4) . 1_555 1_555 yes C(47) N(4) C(48) 116.2(4) . 1_555 1_555 yes C(2) C(1) C(5) 115.8(3) . 1_555 1_555 yes C(2) C(1) C(13) 121.0(3) . 1_555 1_555 yes C(5) C(1) C(13) 123.2(4) . 1_555 1_555 yes C(1) C(2) C(3) 119.3(3) . 1_555 1_555 yes C(1) C(2) C(21) 116.4(3) . 1_555 1_555 yes C(3) C(2) C(21) 124.3(3) . 1_555 1_555 yes C(2) C(3) C(4) 119.4(4) . 1_555 1_555 yes C(2) C(3) C(27) 123.7(3) . 1_555 1_555 yes C(4) C(3) C(27) 116.7(3) . 1_555 1_555 yes C(3) C(4) C(33) 114.7(3) . 1_555 1_555 yes C(3) C(4) C(41) 122.7(3) . 1_555 1_555 yes C(33) C(4) C(41) 122.6(3) . 1_555 1_555 yes C(1) C(5) C(6) 120.8(3) . 1_555 1_555 yes C(1) C(5) C(10) 123.4(4) . 1_555 1_555 yes C(6) C(5) C(10) 115.8(3) . 1_555 1_555 yes C(5) C(6) C(7) 122.7(4) . 1_555 1_555 yes C(6) C(7) C(8) 120.7(4) . 1_555 1_555 yes N(1) C(8) C(7) 121.5(4) . 1_555 1_555 yes N(1) C(8) C(9) 120.9(4) . 1_555 1_555 yes C(7) C(8) C(9) 117.6(3) . 1_555 1_555 yes C(8) C(9) C(10) 120.7(3) . 1_555 1_555 yes C(5) C(10) C(9) 122.4(4) . 1_555 1_555 yes C(1) C(13) C(14) 122.0(4) . 1_555 1_555 yes C(1) C(13) C(18) 121.8(3) . 1_555 1_555 yes C(14) C(13) C(18) 116.2(4) . 1_555 1_555 yes C(13) C(14) C(15) 122.1(4) . 1_555 1_555 yes C(14) C(15) C(16) 121.2(4) . 1_555 1_555 yes N(2) C(16) C(15) 121.6(4) . 1_555 1_555 yes N(2) C(16) C(17) 121.3(4) . 1_555 1_555 yes C(15) C(16) C(17) 117.2(4) . 1_555 1_555 yes C(16) C(17) C(18) 120.8(4) . 1_555 1_555 yes C(13) C(18) C(17) 121.9(4) . 1_555 1_555 yes C(2) C(21) C(22) 121.2(4) . 1_555 1_555 yes C(2) C(21) C(26) 119.7(3) . 1_555 1_555 yes C(22) C(21) C(26) 119.0(3) . 1_555 1_555 yes C(21) C(22) C(23) 120.5(4) . 1_555 1_555 yes C(22) C(23) C(24) 120.1(4) . 1_555 1_555 yes C(23) C(24) C(25) 119.3(4) . 1_555 1_555 yes C(24) C(25) C(26) 120.6(4) . 1_555 1_555 yes C(21) C(26) C(25) 120.5(4) . 1_555 1_555 yes C(3) C(27) C(28) 119.5(4) . 1_555 1_555 yes C(3) C(27) C(32) 121.9(4) . 1_555 1_555 yes C(28) C(27) C(32) 118.6(4) . 1_555 1_555 yes C(27) C(28) C(29) 120.8(4) . 1_555 1_555 yes C(28) C(29) C(30) 120.0(4) . 1_555 1_555 yes C(29) C(30) C(31) 119.3(4) . 1_555 1_555 yes C(30) C(31) C(32) 121.2(4) . 1_555 1_555 yes C(27) C(32) C(31) 120.1(4) . 1_555 1_555 yes C(4) C(33) C(34) 119.9(3) . 1_555 1_555 yes C(4) C(33) C(38) 123.0(4) . 1_555 1_555 yes C(34) C(33) C(38) 116.8(4) . 1_555 1_555 yes C(33) C(34) C(35) 122.3(4) . 1_555 1_555 yes C(34) C(35) C(36) 120.9(4) . 1_555 1_555 yes N(3) C(36) C(35) 121.0(4) . 1_555 1_555 yes N(3) C(36) C(37) 122.0(4) . 1_555 1_555 yes C(35) C(36) C(37) 117.0(4) . 1_555 1_555 yes C(36) C(37) C(38) 121.4(4) . 1_555 1_555 yes C(33) C(38) C(37) 121.1(4) . 1_555 1_555 yes C(4) C(41) C(42) 122.4(4) . 1_555 1_555 yes C(4) C(41) C(46) 122.0(3) . 1_555 1_555 yes C(42) C(41) C(46) 115.6(3) . 1_555 1_555 yes C(41) C(42) C(43) 122.6(4) . 1_555 1_555 yes C(42) C(43) C(44) 121.6(4) . 1_555 1_555 yes N(4) C(44) C(43) 122.0(4) . 1_555 1_555 yes N(4) C(44) C(45) 121.1(4) . 1_555 1_555 yes C(43) C(44) C(45) 116.9(4) . 1_555 1_555 yes C(44) C(45) C(46) 121.0(4) . 1_555 1_555 yes C(41) C(46) C(45) 122.0(4) . 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(8) C(7) C(6) 179.3(4) 1_555 1_555 1_555 1_555 yes N(1) C(8) C(9) C(10) -178.8(4) 1_555 1_555 1_555 1_555 yes N(2) C(16) C(15) C(14) -172.9(4) 1_555 1_555 1_555 1_555 yes N(2) C(16) C(17) C(18) 174.3(4) 1_555 1_555 1_555 1_555 yes N(3) C(36) C(35) C(34) 171.9(4) 1_555 1_555 1_555 1_555 yes N(3) C(36) C(37) C(38) -176.7(4) 1_555 1_555 1_555 1_555 yes N(4) C(44) C(43) C(42) 176.3(4) 1_555 1_555 1_555 1_555 yes N(4) C(44) C(45) C(46) -177.7(4) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) 19.8(5) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(27) -165.2(3) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(21) C(22) -140.9(4) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(21) C(26) 34.7(5) 1_555 1_555 1_555 1_555 yes C(1) C(5) C(6) C(7) -178.0(4) 1_555 1_555 1_555 1_555 yes C(1) C(5) C(10) C(9) 178.5(4) 1_555 1_555 1_555 1_555 yes C(1) C(13) C(14) C(15) 172.9(4) 1_555 1_555 1_555 1_555 yes C(1) C(13) C(18) C(17) -171.5(4) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(5) C(6) 28.3(5) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(5) C(10) -151.0(4) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(13) C(14) 17.9(6) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(13) C(18) -163.4(4) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(33) 47.0(5) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(41) -136.3(4) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(27) C(28) -135.3(4) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(27) C(32) 47.5(6) 1_555 1_555 1_555 1_555 yes C(2) C(21) C(22) C(23) 175.2(4) 1_555 1_555 1_555 1_555 yes C(2) C(21) C(26) C(25) -176.5(4) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(5) 48.7(5) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(13) -131.7(4) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(21) C(22) 40.4(6) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(21) C(26) -144.0(4) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(33) C(34) 38.2(5) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(33) C(38) -136.0(4) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(41) C(42) -158.9(4) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(41) C(46) 19.7(6) 1_555 1_555 1_555 1_555 yes C(3) C(27) C(28) C(29) -178.7(4) 1_555 1_555 1_555 1_555 yes C(3) C(27) C(32) C(31) 177.5(4) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(2) C(21) -161.5(3) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(27) C(28) 39.8(5) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(27) C(32) -137.4(4) 1_555 1_555 1_555 1_555 yes C(4) C(33) C(34) C(35) -174.3(4) 1_555 1_555 1_555 1_555 yes C(4) C(33) C(38) C(37) 169.3(4) 1_555 1_555 1_555 1_555 yes C(4) C(41) C(42) C(43) -177.5(4) 1_555 1_555 1_555 1_555 yes C(4) C(41) C(46) C(45) 176.2(4) 1_555 1_555 1_555 1_555 yes C(5) C(1) C(2) C(21) -130.1(4) 1_555 1_555 1_555 1_555 yes C(5) C(1) C(13) C(14) -162.5(4) 1_555 1_555 1_555 1_555 yes C(5) C(1) C(13) C(18) 16.1(6) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) -1.5(6) 1_555 1_555 1_555 1_555 yes C(5) C(10) C(9) C(8) 0.4(6) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(1) C(13) -151.3(4) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(10) C(9) -0.8(6) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) 1.0(6) 1_555 1_555 1_555 1_555 yes C(7) C(6) C(5) C(10) 1.4(6) 1_555 1_555 1_555 1_555 yes C(7) C(8) N(1) C(11) -8.3(6) 1_555 1_555 1_555 1_555 yes C(7) C(8) N(1) C(12) 168.8(4) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) -0.5(6) 1_555 1_555 1_555 1_555 yes C(9) C(8) N(1) C(11) 169.9(4) 1_555 1_555 1_555 1_555 yes C(9) C(8) N(1) C(12) -12.9(6) 1_555 1_555 1_555 1_555 yes C(10) C(5) C(1) C(13) 29.4(6) 1_555 1_555 1_555 1_555 yes C(13) C(1) C(2) C(21) 49.5(5) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) -1.3(6) 1_555 1_555 1_555 1_555 yes C(13) C(18) C(17) C(16) -1.5(6) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(18) C(17) 7.2(6) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) 7.1(6) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(18) -5.8(5) 1_555 1_555 1_555 1_555 yes C(15) C(16) N(2) C(19) -8.8(6) 1_555 1_555 1_555 1_555 yes C(15) C(16) N(2) C(20) 169.6(4) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(18) -5.7(6) 1_555 1_555 1_555 1_555 yes C(17) C(16) N(2) C(19) 171.3(4) 1_555 1_555 1_555 1_555 yes C(17) C(16) N(2) C(20) -10.3(6) 1_555 1_555 1_555 1_555 yes C(21) C(2) C(3) C(27) 13.4(6) 1_555 1_555 1_555 1_555 yes C(21) C(22) C(23) C(24) 0.8(6) 1_555 1_555 1_555 1_555 yes C(21) C(26) C(25) C(24) 1.7(6) 1_555 1_555 1_555 1_555 yes C(22) C(21) C(26) C(25) -0.8(6) 1_555 1_555 1_555 1_555 yes C(22) C(23) C(24) C(25) 0.1(7) 1_555 1_555 1_555 1_555 yes C(23) C(22) C(21) C(26) -0.5(6) 1_555 1_555 1_555 1_555 yes C(23) C(24) C(25) C(26) -1.3(7) 1_555 1_555 1_555 1_555 yes C(27) C(3) C(4) C(33) -128.3(4) 1_555 1_555 1_555 1_555 yes C(27) C(3) C(4) C(41) 48.4(5) 1_555 1_555 1_555 1_555 yes C(27) C(28) C(29) C(30) 1.7(6) 1_555 1_555 1_555 1_555 yes C(27) C(32) C(31) C(30) 0.6(7) 1_555 1_555 1_555 1_555 yes C(28) C(27) C(32) C(31) 0.3(6) 1_555 1_555 1_555 1_555 yes C(28) C(29) C(30) C(31) -0.9(6) 1_555 1_555 1_555 1_555 yes C(29) C(28) C(27) C(32) -1.4(6) 1_555 1_555 1_555 1_555 yes C(29) C(30) C(31) C(32) -0.3(7) 1_555 1_555 1_555 1_555 yes C(33) C(4) C(41) C(42) 17.5(6) 1_555 1_555 1_555 1_555 yes C(33) C(4) C(41) C(46) -163.9(4) 1_555 1_555 1_555 1_555 yes C(33) C(34) C(35) C(36) 5.8(6) 1_555 1_555 1_555 1_555 yes C(33) C(38) C(37) C(36) 4.0(6) 1_555 1_555 1_555 1_555 yes C(34) C(33) C(4) C(41) -138.5(4) 1_555 1_555 1_555 1_555 yes C(34) C(33) C(38) C(37) -5.1(6) 1_555 1_555 1_555 1_555 yes C(34) C(35) C(36) C(37) -6.8(6) 1_555 1_555 1_555 1_555 yes C(35) C(34) C(33) C(38) 0.2(6) 1_555 1_555 1_555 1_555 yes C(35) C(36) N(3) C(39) -3.2(6) 1_555 1_555 1_555 1_555 yes C(35) C(36) N(3) C(40) -155.4(4) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(38) 2.0(6) 1_555 1_555 1_555 1_555 yes C(37) C(36) N(3) C(39) 175.4(4) 1_555 1_555 1_555 1_555 yes C(37) C(36) N(3) C(40) 23.2(6) 1_555 1_555 1_555 1_555 yes C(38) C(33) C(4) C(41) 47.3(6) 1_555 1_555 1_555 1_555 yes C(41) C(42) C(43) C(44) 1.0(7) 1_555 1_555 1_555 1_555 yes C(41) C(46) C(45) C(44) 1.6(6) 1_555 1_555 1_555 1_555 yes C(42) C(41) C(46) C(45) -5.1(6) 1_555 1_555 1_555 1_555 yes C(42) C(43) C(44) C(45) -4.7(6) 1_555 1_555 1_555 1_555 yes C(43) C(42) C(41) C(46) 3.8(6) 1_555 1_555 1_555 1_555 yes C(43) C(44) N(4) C(47) -5.1(7) 1_555 1_555 1_555 1_555 yes C(43) C(44) N(4) C(48) 178.5(4) 1_555 1_555 1_555 1_555 yes C(43) C(44) C(45) C(46) 3.4(6) 1_555 1_555 1_555 1_555 yes C(45) C(44) N(4) C(47) 175.9(4) 1_555 1_555 1_555 1_555 yes C(45) C(44) N(4) C(48) -0.4(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 I(1) I(2) 2.9275(4) . . ? I(1) I(2) 2.9275(4) . 3_755 ? I(3) I(4) 2.9264(4) . . ? I(3) I(4) 2.9264(4) . 3_665 ? I(5) I(6) 2.9152(4) . . ? I(6) I(7) 2.9158(4) . . ? N(1) C(36) 3.365(5) . 1_455 ? N(1) C(24) 3.456(6) . 4_454 ? N(1) C(25) 3.533(5) . 4_454 ? N(1) C(37) 3.563(5) . 1_455 ? N(3) C(8) 3.497(5) . 1_655 ? C(7) C(35) 3.253(5) . 1_455 ? C(8) C(36) 3.447(5) . 1_455 ? C(8) C(35) 3.545(5) . 1_455 ? C(8) C(24) 3.570(6) . 4_454 ? C(9) C(39) 3.556(6) . 1_455 ? C(9) C(24) 3.569(6) . 4_454 ? C(12) C(20) 3.471(6) . 3_665 ? C(12) C(25) 3.544(6) . 4_454 ? C(12) C(24) 3.595(6) . 4_454 ? C(15) C(47) 3.481(6) . 4_555 ? C(19) C(29) 3.507(6) . 2_755 ? C(24) C(43) 3.387(6) . 4_555 ? C(24) C(44) 3.572(6) . 4_555 ? C(40) C(40) 3.373(10) . 3_765 ? #------------------------------------------------------------------------------