# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2002 data_General #------------------------------------------------------------------------------ _journal_coden_Cambridge 188 #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name ' Kazunobu HARANO' _publ_contact_author_address ; Kumamoto University 5-1 Oe-hon-machi Kumamoto Kumamoto 862-0973 JAPAN ; _publ_contact_author_email ' harano@gpo.kumamoto-u.ac.jp ' _publ_contact_author_fax ' +81-96-371-4573 ' _publ_contact_author_phone ' +81-96-371-4573 ' _publ_requested_journal 'Perkin Transactions 2' #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST loop_ _publ_author_name 'Harano, Kazunobu' 'Abe, Masaki' 'Eto, Masashi' 'Kawaji, Tomohiro' 'Misaka, Junichi' 'Setoguchi, Koji' 'Yoshitake, Yasuyuki' _publ_section_title ; Non-hydroxylic Clathrate Hosts of [4+2]p Cycloadducts of Phencyclone and N-Arylmaleimides. Recognition of Aromatic Guests ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; #------------------------------------------------------------------------------ data_DA_PC_Nap_Butanone _database_code_CSD 180113 _audit_creation_date 'Tue May 14 10:26:11 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C47 H35 N O4 ' _chemical_formula_moiety '?' _chemical_formula_weight 677.80 _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 10.843(3) _cell_length_b 13.916(2) _cell_length_c 23.573(1) _cell_angle_alpha 90 _cell_angle_beta 91.144(10) _cell_angle_gamma 90 _cell_volume 3556(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 18.5 _cell_measurement_theta_max 20.0 _cell_measurement_temperature 293.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.266 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.000 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 8937 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9991 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.20 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 0.0 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^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 8153 _reflns_number_gt 4589 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.0992 _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 6795 _refine_ls_number_parameters 577 _refine_ls_goodness_of_fit_ref 1.225 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00230|Fo|^2^]' _refine_ls_shift/su_max 0.0033 _refine_diff_density_max 0.25 _refine_diff_density_min -0.22 _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) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; '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 O(8) O 1.0039(2) 0.2027(2) 1.02113(8) 0.0616(6) Uani 1.00 d . . . O(34) O 0.8788(2) 0.0361(2) 0.81409(9) 0.0616(6) Uani 1.00 d . . . O(36) O 1.1954(2) 0.2510(1) 0.80734(8) 0.0573(6) Uani 1.00 d . . . O(52) O 0.7678(4) -0.0015(2) 0.1623(1) 0.132(1) Uani 1.00 d . . . N(37) N 1.0347(2) 0.1446(2) 0.79779(8) 0.0404(6) Uani 1.00 d . . . C(1) C 0.8980(2) 0.1548(2) 0.9307(1) 0.0400(7) Uani 1.00 d . . . C(2) C 0.9964(2) 0.1054(2) 0.8933(1) 0.0378(6) Uani 1.00 d . . . C(3) C 1.1047(2) 0.1786(2) 0.8907(1) 0.0358(6) Uani 1.00 d . . . C(4) C 1.0623(2) 0.2665(2) 0.92647(10) 0.0355(6) Uani 1.00 d . . . C(5) C 0.9491(2) 0.3085(2) 0.8959(1) 0.0365(6) Uani 1.00 d . . . C(6) C 0.8531(2) 0.2443(2) 0.8986(1) 0.0394(6) Uani 1.00 d . . . C(7) C 0.9901(2) 0.2078(2) 0.9712(1) 0.0410(7) Uani 1.00 d . . . C(9) C 0.9379(2) 0.3979(2) 0.8656(1) 0.0405(7) Uani 1.00 d . . . C(10) C 1.0376(3) 0.4611(2) 0.8579(1) 0.0565(9) Uani 1.00 d . . . C(11) C 1.0211(4) 0.5457(2) 0.8281(2) 0.070(1) Uani 1.00 d . . . C(12) C 0.9071(4) 0.5694(2) 0.8051(2) 0.071(1) Uani 1.00 d . . . C(13) C 0.8089(3) 0.5093(2) 0.8114(1) 0.0610(10) Uani 1.00 d . . . C(14) C 0.8200(2) 0.4217(2) 0.8414(1) 0.0445(7) Uani 1.00 d . . . C(15) C 0.7350(2) 0.2633(2) 0.8720(1) 0.0434(7) Uani 1.00 d . . . C(16) C 0.6384(3) 0.1960(3) 0.8693(1) 0.0547(9) Uani 1.00 d . . . C(17) C 0.5267(3) 0.2199(3) 0.8448(1) 0.066(1) Uani 1.00 d . . . C(18) C 0.5067(3) 0.3106(3) 0.8227(1) 0.068(1) Uani 1.00 d . . . C(19) C 0.6001(3) 0.3762(3) 0.8229(1) 0.0593(9) Uani 1.00 d . . . C(20) C 0.7174(2) 0.3551(2) 0.8464(1) 0.0462(7) Uani 1.00 d . . . C(21) C 0.8083(2) 0.0931(2) 0.9621(1) 0.0477(8) Uani 1.00 d . . . C(22) C 0.8050(3) -0.0059(2) 0.9573(1) 0.0600(9) Uani 1.00 d . . . C(23) C 0.7241(4) -0.0595(3) 0.9897(2) 0.075(1) Uani 1.00 d . . . C(24) C 0.6460(3) -0.0144(3) 1.0262(2) 0.078(1) Uani 1.00 d . . . C(25) C 0.6479(3) 0.0836(4) 1.0310(2) 0.074(1) Uani 1.00 d . . . C(26) C 0.7282(3) 0.1379(3) 0.9998(1) 0.0619(10) Uani 1.00 d . . . C(27) C 1.1585(2) 0.3317(2) 0.9520(1) 0.0394(6) Uani 1.00 d . . . C(28) C 1.2803(2) 0.3292(2) 0.9364(1) 0.0458(7) Uani 1.00 d . . . C(29) C 1.3664(3) 0.3926(2) 0.9597(1) 0.0564(9) Uani 1.00 d . . . C(30) C 1.3288(3) 0.4591(2) 0.9992(1) 0.0635(10) Uani 1.00 d . . . C(31) C 1.2094(3) 0.4619(3) 1.0156(1) 0.066(1) Uani 1.00 d . . . C(32) C 1.1239(3) 0.3992(2) 0.9923(1) 0.0569(9) Uani 1.00 d . . . C(33) C 0.9588(2) 0.0880(2) 0.8320(1) 0.0422(7) Uani 1.00 d . . . C(35) C 1.1212(2) 0.1983(2) 0.8283(1) 0.0389(6) Uani 1.00 d . . . C(38) C 1.0342(2) 0.1385(2) 0.7363(1) 0.0422(7) Uani 1.00 d . . . C(39) C 1.1223(3) 0.0852(2) 0.7110(1) 0.0507(8) Uani 1.00 d . . . C(40) C 1.1238(3) 0.0774(3) 0.6516(1) 0.0613(10) Uani 1.00 d . . . C(41) C 1.0365(3) 0.1237(2) 0.6195(1) 0.0581(9) Uani 1.00 d . . . C(42) C 0.9444(3) 0.1798(2) 0.6445(1) 0.0504(8) Uani 1.00 d . . . C(43) C 0.8527(4) 0.2269(3) 0.6125(1) 0.071(1) Uani 1.00 d . . . C(44) C 0.7647(4) 0.2814(3) 0.6377(2) 0.082(1) Uani 1.00 d . . . C(45) C 0.7662(4) 0.2921(3) 0.6968(1) 0.069(1) Uani 1.00 d . . . C(46) C 0.8520(3) 0.2461(2) 0.7296(1) 0.0489(8) Uani 1.00 d . . . C(47) C 0.9425(2) 0.1882(2) 0.7049(1) 0.0439(7) Uani 1.00 d . . . C(48) C 0.5769(7) 0.0701(5) 0.1879(3) 0.160(3) Uani 1.00 d . . . C(49) C 0.7132(8) 0.0711(4) 0.1728(2) 0.150(2) Uani 1.00 d . . . C(50) C 0.765(1) 0.1638(6) 0.1734(3) 0.186(4) Uani 1.00 d . . . C(51) C 0.8946(8) 0.1627(5) 0.1591(3) 0.152(3) Uani 1.00 d . . . H(1) H 1.026(2) 0.047(2) 0.910(1) 0.038(6) Uiso 1.00 calc . . . H(2) H 1.181(2) 0.151(2) 0.9058(10) 0.032(6) Uiso 1.00 calc . . . H(3) H 1.117(3) 0.447(2) 0.877(1) 0.061(8) Uiso 1.00 calc . . . H(4) H 1.094(3) 0.585(3) 0.831(2) 0.09(1) Uiso 1.00 calc . . . H(5) H 0.899(3) 0.633(3) 0.781(2) 0.10(1) Uiso 1.00 calc . . . H(6) H 0.727(3) 0.525(2) 0.791(1) 0.063(8) Uiso 1.00 calc . . . H(7) H 0.653(2) 0.129(2) 0.885(1) 0.044(7) Uiso 1.00 calc . . . H(8) H 0.470(3) 0.175(2) 0.841(1) 0.047(8) Uiso 1.00 calc . . . H(9) H 0.424(3) 0.327(2) 0.807(1) 0.072(9) Uiso 1.00 calc . . . H(10) H 0.581(3) 0.440(2) 0.808(1) 0.070(9) Uiso 1.00 calc . . . H(11) H 0.865(3) -0.040(2) 0.930(2) 0.076(9) Uiso 1.00 calc . . . H(12) H 0.728(3) -0.129(3) 0.988(1) 0.08(1) Uiso 1.00 calc . . . H(13) H 0.588(3) -0.050(3) 1.047(2) 0.080(10) Uiso 1.00 calc . . . H(14) H 0.592(3) 0.117(3) 1.054(2) 0.08(1) Uiso 1.00 calc . . . H(15) H 0.737(3) 0.205(3) 1.004(2) 0.09(1) Uiso 1.00 calc . . . H(16) H 1.311(3) 0.286(2) 0.909(1) 0.055(8) Uiso 1.00 calc . . . H(17) H 1.449(3) 0.389(2) 0.944(1) 0.070(9) Uiso 1.00 calc . . . H(18) H 1.388(3) 0.496(2) 1.018(1) 0.071(9) Uiso 1.00 calc . . . H(19) H 1.184(3) 0.503(3) 1.043(2) 0.078(10) Uiso 1.00 calc . . . H(20) H 1.047(3) 0.396(2) 1.003(1) 0.058(9) Uiso 1.00 calc . . . H(21) H 1.178(3) 0.058(2) 0.736(1) 0.056(8) Uiso 1.00 calc . . . H(22) H 1.182(3) 0.047(2) 0.633(1) 0.062(9) Uiso 1.00 calc . . . H(23) H 1.047(3) 0.123(2) 0.580(1) 0.056(8) Uiso 1.00 calc . . . H(24) H 0.845(4) 0.224(3) 0.568(2) 0.10(1) Uiso 1.00 calc . . . H(25) H 0.701(4) 0.308(3) 0.617(2) 0.12(1) Uiso 1.00 calc . . . H(26) H 0.702(3) 0.331(2) 0.716(1) 0.075(9) Uiso 1.00 calc . . . H(27) H 0.849(3) 0.255(2) 0.770(1) 0.064(9) Uiso 1.00 calc . . . H(28) H 0.5292 0.1276 0.1953 0.1267 Uiso 1.00 calc . . . H(29) H 0.5188 0.0414 0.1537 0.1267 Uiso 1.00 calc . . . H(30) H 0.5481 0.0236 0.2175 0.1267 Uiso 1.00 calc . . . H(31) H 0.7192 0.2017 0.1468 0.1267 Uiso 1.00 calc . . . H(32) H 0.7547 0.1899 0.2105 0.1267 Uiso 1.00 calc . . . H(33) H 0.9431 0.1256 0.1858 0.1267 Uiso 1.00 calc . . . H(34) H 0.9076 0.1370 0.1221 0.1267 Uiso 1.00 calc . . . H(35) H 0.9273 0.2274 0.1597 0.1267 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 O(8) 0.069(1) 0.081(1) 0.0340(10) -0.009(1) -0.0011(9) 0.0010(10) O(34) 0.069(1) 0.063(1) 0.054(1) -0.030(1) -0.0010(10) -0.008(1) O(36) 0.064(1) 0.064(1) 0.045(1) -0.027(1) 0.0085(9) -0.0041(9) O(52) 0.212(4) 0.091(2) 0.093(2) 0.093(2) -0.016(2) -0.012(2) N(37) 0.045(1) 0.041(1) 0.035(1) -0.0072(9) 0.0009(9) -0.0035(9) C(1) 0.037(1) 0.044(1) 0.039(1) -0.001(1) 0.0003(10) 0.002(1) C(2) 0.043(1) 0.034(1) 0.037(1) 0.001(1) 0.000(1) 0.002(1) C(3) 0.035(1) 0.036(1) 0.036(1) 0.004(1) -0.0014(10) -0.0037(10) C(4) 0.036(1) 0.035(1) 0.035(1) 0.003(1) -0.0012(9) -0.0029(10) C(5) 0.034(1) 0.037(1) 0.039(1) 0.0036(10) -0.0026(9) -0.005(1) C(6) 0.039(1) 0.042(1) 0.037(1) 0.003(1) 0.0022(10) -0.003(1) C(7) 0.038(1) 0.042(1) 0.042(1) 0.007(1) 0.001(1) -0.001(1) C(9) 0.047(1) 0.033(1) 0.041(1) 0.006(1) -0.003(1) -0.005(1) C(10) 0.059(2) 0.039(1) 0.072(2) -0.001(1) -0.011(2) 0.004(1) C(11) 0.079(2) 0.043(2) 0.086(3) -0.004(2) -0.011(2) 0.010(2) C(12) 0.087(3) 0.041(2) 0.086(3) 0.010(2) -0.009(2) 0.016(2) C(13) 0.067(2) 0.051(2) 0.065(2) 0.019(2) -0.008(2) 0.005(1) C(14) 0.051(1) 0.042(1) 0.040(1) 0.015(1) 0.000(1) -0.008(1) C(15) 0.036(1) 0.056(2) 0.038(1) 0.004(1) 0.002(1) -0.005(1) C(16) 0.041(1) 0.070(2) 0.054(2) -0.005(1) 0.001(1) -0.001(2) C(17) 0.035(1) 0.097(3) 0.065(2) -0.010(2) 0.001(1) -0.008(2) C(18) 0.040(2) 0.098(3) 0.065(2) 0.017(2) -0.003(1) 0.004(2) C(19) 0.048(2) 0.072(2) 0.058(2) 0.019(2) 0.001(1) -0.003(2) C(20) 0.045(1) 0.054(2) 0.039(1) 0.013(1) 0.000(1) -0.007(1) C(21) 0.043(1) 0.059(2) 0.040(1) -0.009(1) 0.001(1) 0.006(1) C(22) 0.062(2) 0.058(2) 0.060(2) -0.013(2) 0.006(2) 0.008(2) C(23) 0.084(3) 0.072(2) 0.070(2) -0.025(2) 0.002(2) 0.017(2) C(24) 0.064(2) 0.110(3) 0.059(2) -0.033(2) 0.001(2) 0.030(2) C(25) 0.057(2) 0.110(3) 0.056(2) -0.006(2) 0.016(2) 0.007(2) C(26) 0.056(2) 0.077(2) 0.053(2) -0.006(2) 0.011(1) 0.005(2) C(27) 0.042(1) 0.038(1) 0.037(1) 0.003(1) -0.0040(10) -0.002(1) C(28) 0.045(1) 0.049(2) 0.043(1) -0.004(1) -0.003(1) -0.005(1) C(29) 0.051(2) 0.062(2) 0.056(2) -0.014(1) -0.004(1) -0.005(1) C(30) 0.062(2) 0.066(2) 0.061(2) -0.015(2) -0.018(2) -0.010(2) C(31) 0.072(2) 0.063(2) 0.062(2) -0.005(2) -0.005(2) -0.028(2) C(32) 0.050(2) 0.060(2) 0.061(2) 0.002(1) -0.002(1) -0.019(1) C(33) 0.047(1) 0.035(1) 0.045(1) -0.004(1) 0.001(1) -0.001(1) C(35) 0.039(1) 0.037(1) 0.040(1) 0.000(1) 0.002(1) -0.005(1) C(38) 0.048(1) 0.039(1) 0.040(1) -0.006(1) 0.000(1) -0.007(1) C(39) 0.052(2) 0.053(2) 0.046(2) 0.007(1) -0.001(1) -0.012(1) C(40) 0.061(2) 0.067(2) 0.056(2) 0.005(2) 0.009(1) -0.020(2) C(41) 0.067(2) 0.066(2) 0.041(2) 0.000(2) 0.002(1) -0.011(1) C(42) 0.062(2) 0.051(2) 0.038(1) -0.005(1) 0.002(1) -0.005(1) C(43) 0.089(3) 0.077(2) 0.047(2) 0.016(2) 0.002(2) 0.006(2) C(44) 0.091(3) 0.097(3) 0.059(2) 0.032(2) -0.005(2) 0.009(2) C(45) 0.078(2) 0.071(2) 0.059(2) 0.025(2) 0.004(2) 0.006(2) C(46) 0.057(2) 0.047(2) 0.043(1) 0.008(1) 0.007(1) -0.001(1) C(47) 0.050(1) 0.036(1) 0.046(1) -0.005(1) 0.003(1) -0.002(1) C(48) 0.202(6) 0.162(6) 0.117(4) 0.112(5) 0.071(4) 0.020(4) C(49) 0.302(9) 0.092(3) 0.055(2) 0.116(5) -0.019(4) -0.010(2) C(50) 0.32(1) 0.145(6) 0.094(4) 0.141(7) -0.036(5) -0.041(4) C(51) 0.209(7) 0.102(4) 0.144(6) 0.051(5) -0.004(5) -0.022(4) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SAPI91 _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 O(8) C(7) 1.185(3) . . yes O(34) C(33) 1.199(3) . . yes O(36) C(35) 1.201(3) . . yes O(52) C(49) 1.201(5) . . yes N(37) C(33) 1.405(3) . . yes N(37) C(35) 1.389(3) . . yes N(37) C(38) 1.451(3) . . yes C(1) C(2) 1.558(3) . . yes C(1) C(6) 1.533(4) . . yes C(1) C(7) 1.553(3) . . yes C(1) C(21) 1.503(4) . . yes C(2) C(3) 1.557(3) . . yes C(2) C(33) 1.514(4) . . yes C(3) C(4) 1.560(3) . . yes C(3) C(35) 1.511(3) . . yes C(4) C(5) 1.528(3) . . yes C(4) C(7) 1.558(3) . . yes C(4) C(27) 1.499(3) . . yes C(5) C(6) 1.373(3) . . yes C(5) C(9) 1.439(4) . . yes C(6) C(15) 1.439(3) . . yes C(9) C(10) 1.408(4) . . yes C(9) C(14) 1.428(4) . . yes C(10) C(11) 1.380(4) . . yes C(11) C(12) 1.380(5) . . yes C(12) C(13) 1.365(5) . . yes C(13) C(14) 1.414(4) . . yes C(14) C(20) 1.454(4) . . yes C(15) C(16) 1.406(4) . . yes C(15) C(20) 1.424(4) . . yes C(16) C(17) 1.372(4) . . yes C(17) C(18) 1.381(5) . . yes C(18) C(19) 1.363(5) . . yes C(19) C(20) 1.409(4) . . yes C(21) C(22) 1.383(4) . . yes C(21) C(26) 1.401(4) . . yes C(22) C(23) 1.392(4) . . yes C(23) C(24) 1.372(6) . . yes C(24) C(25) 1.369(6) . . yes C(25) C(26) 1.377(5) . . yes C(27) C(28) 1.378(4) . . yes C(27) C(32) 1.393(4) . . yes C(28) C(29) 1.390(4) . . yes C(29) C(30) 1.378(5) . . yes C(30) C(31) 1.360(5) . . yes C(31) C(32) 1.379(4) . . yes C(38) C(39) 1.358(4) . . yes C(38) C(47) 1.409(4) . . yes C(39) C(40) 1.406(4) . . yes C(40) C(41) 1.360(5) . . yes C(41) C(42) 1.406(4) . . yes C(42) C(43) 1.399(4) . . yes C(42) C(47) 1.430(4) . . yes C(43) C(44) 1.365(5) . . yes C(44) C(45) 1.401(5) . . yes C(45) C(46) 1.357(4) . . yes C(46) C(47) 1.405(4) . . yes C(48) C(49) 1.53(1) . . yes C(49) C(50) 1.41(1) . . yes C(50) C(51) 1.45(1) . . 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(33) N(37) C(35) 113.7(2) . . . yes C(33) N(37) C(38) 123.3(2) . . . yes C(35) N(37) C(38) 122.5(2) . . . yes C(2) C(1) C(6) 107.0(2) . . . yes C(2) C(1) C(7) 96.8(2) . . . yes C(2) C(1) C(21) 118.9(2) . . . yes C(6) C(1) C(7) 96.4(2) . . . yes C(6) C(1) C(21) 120.3(2) . . . yes C(7) C(1) C(21) 112.5(2) . . . yes C(1) C(2) C(3) 105.0(2) . . . yes C(1) C(2) C(33) 115.9(2) . . . yes C(3) C(2) C(33) 104.8(2) . . . yes C(2) C(3) C(4) 105.2(2) . . . yes C(2) C(3) C(35) 105.2(2) . . . yes C(4) C(3) C(35) 115.2(2) . . . yes C(3) C(4) C(5) 106.7(2) . . . yes C(3) C(4) C(7) 96.5(2) . . . yes C(3) C(4) C(27) 118.7(2) . . . yes C(5) C(4) C(7) 96.3(2) . . . yes C(5) C(4) C(27) 120.3(2) . . . yes C(7) C(4) C(27) 113.6(2) . . . yes C(4) C(5) C(6) 109.4(2) . . . yes C(4) C(5) C(9) 128.6(2) . . . yes C(6) C(5) C(9) 121.9(2) . . . yes C(1) C(6) C(5) 108.6(2) . . . yes C(1) C(6) C(15) 129.5(2) . . . yes C(5) C(6) C(15) 121.9(2) . . . yes O(8) C(7) C(1) 130.4(2) . . . yes O(8) C(7) C(4) 130.4(2) . . . yes C(1) C(7) C(4) 99.1(2) . . . yes C(5) C(9) C(10) 123.2(2) . . . yes C(5) C(9) C(14) 117.7(2) . . . yes C(10) C(9) C(14) 119.2(2) . . . yes C(9) C(10) C(11) 120.4(3) . . . yes C(10) C(11) C(12) 120.6(3) . . . yes C(11) C(12) C(13) 120.4(3) . . . yes C(12) C(13) C(14) 121.6(3) . . . yes C(9) C(14) C(13) 117.8(3) . . . yes C(9) C(14) C(20) 120.0(2) . . . yes C(13) C(14) C(20) 122.2(3) . . . yes C(6) C(15) C(16) 123.6(3) . . . yes C(6) C(15) C(20) 117.4(2) . . . yes C(16) C(15) C(20) 119.0(2) . . . yes C(15) C(16) C(17) 120.5(3) . . . yes C(16) C(17) C(18) 120.7(3) . . . yes C(17) C(18) C(19) 120.0(3) . . . yes C(18) C(19) C(20) 121.8(3) . . . yes C(14) C(20) C(15) 120.7(2) . . . yes C(14) C(20) C(19) 121.4(3) . . . yes C(15) C(20) C(19) 117.8(3) . . . yes C(1) C(21) C(22) 123.0(3) . . . yes C(1) C(21) C(26) 118.3(3) . . . yes C(22) C(21) C(26) 118.7(3) . . . yes C(21) C(22) C(23) 120.3(3) . . . yes C(22) C(23) C(24) 120.2(4) . . . yes C(23) C(24) C(25) 120.0(3) . . . yes C(24) C(25) C(26) 120.8(4) . . . yes C(21) C(26) C(25) 120.1(4) . . . yes C(4) C(27) C(28) 122.8(2) . . . yes C(4) C(27) C(32) 119.1(2) . . . yes C(28) C(27) C(32) 118.1(2) . . . yes C(27) C(28) C(29) 121.2(3) . . . yes C(28) C(29) C(30) 119.2(3) . . . yes C(29) C(30) C(31) 120.5(3) . . . yes C(30) C(31) C(32) 120.3(3) . . . yes C(27) C(32) C(31) 120.7(3) . . . yes O(34) C(33) N(37) 124.4(2) . . . yes O(34) C(33) C(2) 127.7(2) . . . yes N(37) C(33) C(2) 108.0(2) . . . yes O(36) C(35) N(37) 124.5(2) . . . yes O(36) C(35) C(3) 127.2(2) . . . yes N(37) C(35) C(3) 108.3(2) . . . yes N(37) C(38) C(39) 118.9(2) . . . yes N(37) C(38) C(47) 119.0(2) . . . yes C(39) C(38) C(47) 122.2(3) . . . yes C(38) C(39) C(40) 120.2(3) . . . yes C(39) C(40) C(41) 119.7(3) . . . yes C(40) C(41) C(42) 121.5(3) . . . yes C(41) C(42) C(43) 122.6(3) . . . yes C(41) C(42) C(47) 119.1(3) . . . yes C(43) C(42) C(47) 118.3(3) . . . yes C(42) C(43) C(44) 121.4(3) . . . yes C(43) C(44) C(45) 119.8(3) . . . yes C(44) C(45) C(46) 120.7(3) . . . yes C(45) C(46) C(47) 120.8(3) . . . yes C(38) C(47) C(42) 117.4(2) . . . yes C(38) C(47) C(46) 123.7(2) . . . yes C(42) C(47) C(46) 118.9(3) . . . yes O(52) C(49) C(48) 121.6(7) . . . yes O(52) C(49) C(50) 125.1(8) . . . yes C(48) C(49) C(50) 113.3(5) . . . yes C(49) C(50) C(51) 112.1(6) . . . 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 O(8) C(7) C(1) C(2) -120.6(3) . . . . yes O(8) C(7) C(1) C(6) 131.3(3) . . . . yes O(8) C(7) C(1) C(21) 4.6(4) . . . . yes O(8) C(7) C(4) C(3) 120.6(3) . . . . yes O(8) C(7) C(4) C(5) -131.8(3) . . . . yes O(8) C(7) C(4) C(27) -4.7(4) . . . . yes O(34) C(33) N(37) C(35) -179.6(3) . . . . yes O(34) C(33) N(37) C(38) -7.1(4) . . . . yes O(34) C(33) C(2) C(1) -65.1(4) . . . . yes O(34) C(33) C(2) C(3) 179.7(3) . . . . yes O(34) C(33) C(2) H(1) 63(1) . . . . no O(36) C(35) N(37) C(33) 179.6(3) . . . . yes O(36) C(35) N(37) C(38) 7.0(4) . . . . yes O(36) C(35) C(3) C(2) -179.9(3) . . . . yes O(36) C(35) C(3) C(4) 64.8(3) . . . . yes O(36) C(35) C(3) H(2) -60(1) . . . . no O(52) C(49) C(48) H(28) -177.6 . . . . no O(52) C(49) C(48) H(29) -61.1 . . . . no O(52) C(49) C(48) H(30) 49.0 . . . . no O(52) C(49) C(50) C(51) 0.4(8) . . . . yes O(52) C(49) C(50) H(31) 121.9 . . . . no O(52) C(49) C(50) H(32) -121.1 . . . . no N(37) C(33) C(2) C(1) 114.8(2) . . . . yes N(37) C(33) C(2) C(3) -0.4(3) . . . . yes N(37) C(33) C(2) H(1) -116(1) . . . . no N(37) C(35) C(3) C(2) 0.1(3) . . . . yes N(37) C(35) C(3) C(4) -115.2(2) . . . . yes N(37) C(35) C(3) H(2) 119(1) . . . . no N(37) C(38) C(39) C(40) 179.6(3) . . . . yes N(37) C(38) C(39) H(21) -2(2) . . . . no N(37) C(38) C(47) C(42) -179.5(2) . . . . yes N(37) C(38) C(47) C(46) 1.8(4) . . . . yes C(1) C(2) C(3) C(4) -0.3(2) . . . . yes C(1) C(2) C(3) C(35) -122.4(2) . . . . yes C(1) C(2) C(3) H(2) 120(1) . . . . no C(1) C(6) C(5) C(4) -0.7(3) . . . . yes C(1) C(6) C(5) C(9) 176.6(2) . . . . yes C(1) C(6) C(15) C(16) -3.2(4) . . . . yes C(1) C(6) C(15) C(20) 178.0(2) . . . . yes C(1) C(7) C(4) C(3) -57.3(2) . . . . yes C(1) C(7) C(4) C(5) 50.3(2) . . . . yes C(1) C(7) C(4) C(27) 177.4(2) . . . . yes C(1) C(21) C(22) C(23) 176.6(3) . . . . yes C(1) C(21) C(22) H(11) -2(2) . . . . no C(1) C(21) C(26) C(25) -177.5(3) . . . . yes C(1) C(21) C(26) H(15) -1(2) . . . . no C(2) C(1) C(6) C(5) -66.6(2) . . . . yes C(2) C(1) C(6) C(15) 110.8(3) . . . . yes C(2) C(1) C(7) C(4) 57.3(2) . . . . yes C(2) C(1) C(21) C(22) -3.1(4) . . . . yes C(2) C(1) C(21) C(26) 173.9(2) . . . . yes C(2) C(3) C(4) C(5) -64.0(2) . . . . yes C(2) C(3) C(4) C(7) 34.6(2) . . . . yes C(2) C(3) C(4) C(27) 156.1(2) . . . . yes C(2) C(33) N(37) C(35) 0.5(3) . . . . yes C(2) C(33) N(37) C(38) 173.0(2) . . . . yes C(3) C(2) C(1) C(6) 64.6(2) . . . . yes C(3) C(2) C(1) C(7) -34.2(2) . . . . yes C(3) C(2) C(1) C(21) -154.7(2) . . . . yes C(3) C(4) C(5) C(6) 67.3(2) . . . . yes C(3) C(4) C(5) C(9) -109.8(3) . . . . yes C(3) C(4) C(27) C(28) 13.2(4) . . . . yes C(3) C(4) C(27) C(32) -168.2(2) . . . . yes C(3) C(35) N(37) C(33) -0.4(3) . . . . yes C(3) C(35) N(37) C(38) -172.9(2) . . . . yes C(4) C(3) C(2) C(33) 122.2(2) . . . . yes C(4) C(3) C(2) H(1) -120(1) . . . . no C(4) C(5) C(6) C(15) -178.3(2) . . . . yes C(4) C(5) C(9) C(10) 2.6(4) . . . . yes C(4) C(5) C(9) C(14) -178.8(2) . . . . yes C(4) C(7) C(1) C(6) -50.8(2) . . . . yes C(4) C(7) C(1) C(21) -177.5(2) . . . . yes C(4) C(27) C(28) C(29) 178.1(3) . . . . yes C(4) C(27) C(28) H(16) 0(2) . . . . no C(4) C(27) C(32) C(31) -178.4(3) . . . . yes C(4) C(27) C(32) H(20) 5(2) . . . . no C(5) C(4) C(3) C(35) 51.3(3) . . . . yes C(5) C(4) C(3) H(2) 174(1) . . . . no C(5) C(4) C(27) C(28) -121.2(3) . . . . yes C(5) C(4) C(27) C(32) 57.4(3) . . . . yes C(5) C(6) C(1) C(7) 32.6(2) . . . . yes C(5) C(6) C(1) C(21) 153.4(2) . . . . yes C(5) C(6) C(15) C(16) 173.8(2) . . . . yes C(5) C(6) C(15) C(20) -5.0(4) . . . . yes C(5) C(9) C(10) C(11) 179.6(3) . . . . yes C(5) C(9) C(10) H(3) -6(2) . . . . no C(5) C(9) C(14) C(13) -179.6(2) . . . . yes C(5) C(9) C(14) C(20) -1.8(3) . . . . yes C(6) C(1) C(2) C(33) -50.5(3) . . . . yes C(6) C(1) C(2) H(1) -177(1) . . . . no C(6) C(1) C(21) C(22) 132.3(3) . . . . yes C(6) C(1) C(21) C(26) -50.7(4) . . . . yes C(6) C(5) C(4) C(7) -31.4(2) . . . . yes C(6) C(5) C(4) C(27) -153.5(2) . . . . yes C(6) C(5) C(9) C(10) -174.2(3) . . . . yes C(6) C(5) C(9) C(14) 4.4(3) . . . . yes C(6) C(15) C(16) C(17) 177.9(3) . . . . yes C(6) C(15) C(16) H(7) -2(1) . . . . no C(6) C(15) C(20) C(14) 7.4(4) . . . . yes C(6) C(15) C(20) C(19) -176.7(2) . . . . yes C(7) C(1) C(2) C(33) -149.3(2) . . . . yes C(7) C(1) C(2) H(1) 83(1) . . . . no C(7) C(1) C(6) C(15) -150.1(2) . . . . yes C(7) C(1) C(21) C(22) -115.2(3) . . . . yes C(7) C(1) C(21) C(26) 61.9(3) . . . . yes C(7) C(4) C(3) C(35) 149.9(2) . . . . yes C(7) C(4) C(3) H(2) -86(1) . . . . no C(7) C(4) C(5) C(9) 151.5(2) . . . . yes C(7) C(4) C(27) C(28) 125.5(3) . . . . yes C(7) C(4) C(27) C(32) -55.9(3) . . . . yes C(9) C(5) C(4) C(27) 29.4(4) . . . . yes C(9) C(5) C(6) C(15) -0.9(4) . . . . yes C(9) C(10) C(11) C(12) -0.4(5) . . . . yes C(9) C(10) C(11) H(4) 172(2) . . . . no C(9) C(14) C(13) C(12) 0.3(4) . . . . yes C(9) C(14) C(13) H(6) 174(2) . . . . no C(9) C(14) C(20) C(15) -4.1(4) . . . . yes C(9) C(14) C(20) C(19) -179.8(2) . . . . yes C(10) C(9) C(14) C(13) -1.0(4) . . . . yes C(10) C(9) C(14) C(20) 176.8(2) . . . . yes C(10) C(11) C(12) C(13) -0.3(6) . . . . yes C(10) C(11) C(12) H(5) -177(2) . . . . no C(11) C(10) C(9) C(14) 1.0(4) . . . . yes C(11) C(12) C(13) C(14) 0.4(6) . . . . yes C(11) C(12) C(13) H(6) -174(2) . . . . no C(12) C(11) C(10) H(3) -174(2) . . . . no C(12) C(13) C(14) C(20) -177.5(3) . . . . yes C(13) C(12) C(11) H(4) -171(2) . . . . no C(13) C(14) C(20) C(15) 173.6(3) . . . . yes C(13) C(14) C(20) C(19) -2.1(4) . . . . yes C(14) C(9) C(10) H(3) 175(2) . . . . no C(14) C(13) C(12) H(5) 177(2) . . . . no C(14) C(20) C(15) C(16) -171.4(2) . . . . yes C(14) C(20) C(19) C(18) 173.7(3) . . . . yes C(14) C(20) C(19) H(10) -9(2) . . . . no C(15) C(6) C(1) C(21) -29.2(4) . . . . yes C(15) C(16) C(17) C(18) -0.3(5) . . . . yes C(15) C(16) C(17) H(8) 175(2) . . . . no C(15) C(20) C(19) C(18) -2.1(4) . . . . yes C(15) C(20) C(19) H(10) 174(2) . . . . no C(16) C(15) C(20) C(19) 4.4(4) . . . . yes C(16) C(17) C(18) C(19) 2.8(5) . . . . yes C(16) C(17) C(18) H(9) -177(2) . . . . no C(17) C(16) C(15) C(20) -3.2(4) . . . . yes C(17) C(18) C(19) C(20) -1.5(5) . . . . yes C(17) C(18) C(19) H(10) -178(2) . . . . no C(18) C(17) C(16) H(7) -179(1) . . . . no C(19) C(18) C(17) H(8) -173(2) . . . . no C(20) C(14) C(13) H(6) -2(2) . . . . no C(20) C(15) C(16) H(7) 176(1) . . . . no C(20) C(19) C(18) H(9) 178(2) . . . . no C(21) C(1) C(2) C(33) 90.2(3) . . . . yes C(21) C(1) C(2) H(1) -36(1) . . . . no C(21) C(22) C(23) C(24) 0.8(5) . . . . yes C(21) C(22) C(23) H(12) -174(2) . . . . no C(21) C(26) C(25) C(24) 0.8(5) . . . . yes C(21) C(26) C(25) H(14) -175(2) . . . . no C(22) C(21) C(26) C(25) -0.3(5) . . . . yes C(22) C(21) C(26) H(15) 175(2) . . . . no C(22) C(23) C(24) C(25) -0.2(6) . . . . yes C(22) C(23) C(24) H(13) 177(2) . . . . no C(23) C(22) C(21) C(26) -0.5(5) . . . . yes C(23) C(24) C(25) C(26) -0.5(6) . . . . yes C(23) C(24) C(25) H(14) 175(2) . . . . no C(24) C(23) C(22) H(11) 179(2) . . . . no C(24) C(25) C(26) H(15) -174(2) . . . . no C(25) C(24) C(23) H(12) 175(2) . . . . no C(26) C(21) C(22) H(11) -179(2) . . . . no C(26) C(25) C(24) H(13) -177(2) . . . . no C(27) C(4) C(3) C(35) -88.6(3) . . . . yes C(27) C(4) C(3) H(2) 35(1) . . . . no C(27) C(28) C(29) C(30) 0.0(5) . . . . yes C(27) C(28) C(29) H(17) -175(2) . . . . no C(27) C(32) C(31) C(30) 0.5(5) . . . . yes C(27) C(32) C(31) H(19) -177(2) . . . . no C(28) C(27) C(32) C(31) 0.3(5) . . . . yes C(28) C(27) C(32) H(20) -175(2) . . . . no C(28) C(29) C(30) C(31) 0.8(5) . . . . yes C(28) C(29) C(30) H(18) 172(2) . . . . no C(29) C(28) C(27) C(32) -0.5(4) . . . . yes C(29) C(30) C(31) C(32) -1.1(6) . . . . yes C(29) C(30) C(31) H(19) 176(2) . . . . no C(30) C(29) C(28) H(16) 178(1) . . . . no C(30) C(31) C(32) H(20) 176(2) . . . . no C(31) C(30) C(29) H(17) 175(2) . . . . no C(32) C(27) C(28) H(16) -179(2) . . . . no C(32) C(31) C(30) H(18) -172(2) . . . . no C(33) N(37) C(38) C(39) -98.4(3) . . . . yes C(33) N(37) C(38) C(47) 81.6(3) . . . . yes C(33) C(2) C(3) C(35) 0.2(2) . . . . yes C(33) C(2) C(3) H(2) -116(1) . . . . no C(35) N(37) C(38) C(39) 73.5(3) . . . . yes C(35) N(37) C(38) C(47) -106.5(3) . . . . yes C(35) C(3) C(2) H(1) 117(1) . . . . no C(38) C(39) C(40) C(41) 0.0(5) . . . . yes C(38) C(39) C(40) H(22) 175(2) . . . . no C(38) C(47) C(42) C(41) -0.3(4) . . . . yes C(38) C(47) C(42) C(43) 178.8(3) . . . . yes C(38) C(47) C(46) C(45) 180.0(3) . . . . yes C(38) C(47) C(46) H(27) 0(2) . . . . no C(39) C(38) C(47) C(42) 0.5(4) . . . . yes C(39) C(38) C(47) C(46) -178.2(3) . . . . yes C(39) C(40) C(41) C(42) 0.2(5) . . . . yes C(39) C(40) C(41) H(23) 172(1) . . . . no C(40) C(39) C(38) C(47) -0.4(4) . . . . yes C(40) C(41) C(42) C(43) -179.1(3) . . . . yes C(40) C(41) C(42) C(47) -0.1(5) . . . . yes C(41) C(40) C(39) H(21) -178(2) . . . . no C(41) C(42) C(43) C(44) -179.6(4) . . . . yes C(41) C(42) C(43) H(24) 0(2) . . . . no C(41) C(42) C(47) C(46) 178.5(3) . . . . yes C(42) C(41) C(40) H(22) -175(2) . . . . no C(42) C(43) C(44) C(45) 1.0(7) . . . . yes C(42) C(43) C(44) H(25) -174(3) . . . . no C(42) C(47) C(46) C(45) 1.3(4) . . . . yes C(42) C(47) C(46) H(27) -178(2) . . . . no C(43) C(42) C(41) H(23) 8(2) . . . . no C(43) C(42) C(47) C(46) -2.5(4) . . . . yes C(43) C(44) C(45) C(46) -2.2(7) . . . . yes C(43) C(44) C(45) H(26) -179(2) . . . . no C(44) C(43) C(42) C(47) 1.4(5) . . . . yes C(44) C(45) C(46) C(47) 1.1(6) . . . . yes C(44) C(45) C(46) H(27) -179(2) . . . . no C(45) C(44) C(43) H(24) -179(2) . . . . no C(46) C(45) C(44) H(25) 173(3) . . . . no C(47) C(38) C(39) H(21) 177(2) . . . . no C(47) C(42) C(41) H(23) -172(2) . . . . no C(47) C(42) C(43) H(24) -178(2) . . . . no C(47) C(46) C(45) H(26) 177(2) . . . . no C(48) C(49) C(50) C(51) 179.8(5) . . . . yes C(48) C(49) C(50) H(31) -58.7 . . . . no C(48) C(49) C(50) H(32) 58.3 . . . . no C(49) C(50) C(51) H(33) -61.3 . . . . no C(49) C(50) C(51) H(34) 60.1 . . . . no C(49) C(50) C(51) H(35) 179.8 . . . . no C(50) C(49) C(48) H(28) 3.0 . . . . no C(50) C(49) C(48) H(29) 119.5 . . . . no C(50) C(49) C(48) H(30) -130.5 . . . . no H(1) C(2) C(3) H(2) 0(2) . . . . no H(3) C(10) C(11) H(4) -1(3) . . . . no H(4) C(11) C(12) H(5) 11(3) . . . . no H(5) C(12) C(13) H(6) 2(3) . . . . no H(7) C(16) C(17) H(8) -3(2) . . . . no H(8) C(17) C(18) H(9) 6(3) . . . . no H(9) C(18) C(19) H(10) 1(3) . . . . no H(11) C(22) C(23) H(12) 4(3) . . . . no H(12) C(23) C(24) H(13) -7(3) . . . . no H(13) C(24) C(25) H(14) -1(3) . . . . no H(14) C(25) C(26) H(15) 9(3) . . . . no H(16) C(28) C(29) H(17) 3(2) . . . . no H(17) C(29) C(30) H(18) -12(3) . . . . no H(18) C(30) C(31) H(19) 5(3) . . . . no H(19) C(31) C(32) H(20) -1(3) . . . . no H(21) C(39) C(40) H(22) -2(3) . . . . no H(22) C(40) C(41) H(23) -3(3) . . . . no H(24) C(43) C(44) H(25) 5(4) . . . . no H(25) C(44) C(45) H(26) -3(4) . . . . no H(26) C(45) C(46) H(27) -2(3) . . . . no H(31) C(50) C(51) H(33) 178.9 . . . . no H(31) C(50) C(51) H(34) -59.6 . . . . no H(31) C(50) C(51) H(35) 60.1 . . . . no H(32) C(50) C(51) H(33) 58.6 . . . . no H(32) C(50) C(51) H(34) -180.0 . . . . no H(32) C(50) C(51) H(35) -60.3 . . . . no H(32) C(50) C(51) H(35) -60.3 . . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(8) C(22) 3.466(4) . 3_757 ? O(8) C(51) 3.527(8) . 1_556 ? O(8) C(23) 3.573(5) . 3_757 ? O(34) C(13) 3.576(4) . 2_646 ? O(36) C(50) 3.470(6) . 4_555 ? O(36) C(18) 3.488(4) . 1_655 ? O(36) O(52) 3.565(4) . 3_756 ? O(52) C(35) 2.998(4) . 3_756 ? O(52) N(37) 3.059(4) . 3_756 ? O(52) C(3) 3.100(4) . 3_756 ? O(52) C(33) 3.200(4) . 3_756 ? O(52) C(2) 3.236(4) . 3_756 ? O(52) C(39) 3.400(4) . 3_756 ? O(52) C(24) 3.448(5) . 1_554 ? O(52) C(25) 3.537(5) . 1_554 ? C(24) C(24) 3.399(8) . 3_657 ? C(24) C(25) 3.567(5) . 3_657 ? C(25) C(49) 3.408(6) . 1_556 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data_phencyclone_m-MeNPMA_host_ _database_code_CSD 180114 _audit_creation_date 'Sat Jun 8 11:43:49 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C40 H27 N O3 ' _chemical_formula_moiety 'C40 H27 N O3 ' _chemical_formula_weight 569.66 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 11.667(3) _cell_length_b 14.264(3) _cell_length_c 9.053(2) _cell_angle_alpha 90.09(2) _cell_angle_beta 100.01(2) _cell_angle_gamma 77.15(2) _cell_volume 1445.5(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 16.2 _cell_measurement_theta_max 19.4 _cell_measurement_temperature 293.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.309 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 6963 _diffrn_reflns_av_R_equivalents 0.012 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 1.0001 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.0001 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.23 #------------------------------------------------------------------------------ # 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 6630 _reflns_number_gt 3632 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.0750 _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 3632 _refine_ls_number_parameters 477 _refine_ls_goodness_of_fit_ref 1.282 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00181|Fo|^2^]' _refine_ls_shift/su_max 0.1960 _refine_diff_density_max 0.20 _refine_diff_density_min -0.23 _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) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; '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 O8 O 0.5978(2) 0.0043(1) 1.3204(2) 0.0508(6) Uani 1.00 d . . . O34 O 0.1671(2) 0.2642(2) 1.3376(3) 0.0644(7) Uani 1.00 d . . . O37 O 0.4835(2) 0.4023(1) 1.3476(3) 0.0634(7) Uani 1.00 d . . . N35 N 0.3090(2) 0.3510(2) 1.3283(3) 0.0459(7) Uani 1.00 d . . . C1 C 0.3905(2) 0.1067(2) 1.2742(3) 0.0337(6) Uani 1.00 d . . . C2 C 0.3717(2) 0.1604(2) 1.1211(3) 0.0336(6) Uani 1.00 d . . . C3 C 0.4630(2) 0.2055(2) 1.1196(3) 0.0349(6) Uani 1.00 d . . . C4 C 0.5522(2) 0.1819(2) 1.2680(3) 0.0357(6) Uani 1.00 d . . . C5 C 0.4867(2) 0.2331(2) 1.3942(3) 0.0382(7) Uani 1.00 d . . . C6 C 0.3795(2) 0.1862(2) 1.3941(3) 0.0369(7) Uani 1.00 d . . . C7 C 0.5290(2) 0.0801(2) 1.2945(3) 0.0366(7) Uani 1.00 d . . . C9 C 0.3328(2) 0.0238(2) 1.2888(3) 0.0370(7) Uani 1.00 d . . . C10 C 0.3675(3) -0.0595(2) 1.2118(3) 0.0454(8) Uani 1.00 d . . . C11 C 0.3127(3) -0.1358(2) 1.2180(4) 0.0552(9) Uani 1.00 d . . . C12 C 0.2227(3) -0.1298(2) 1.3010(4) 0.0551(9) Uani 1.00 d . . . C13 C 0.1890(3) -0.0488(2) 1.3801(4) 0.0550(10) Uani 1.00 d . . . C14 C 0.2437(3) 0.0280(2) 1.3738(3) 0.0444(8) Uani 1.00 d . . . C15 C 0.6806(2) 0.1852(2) 1.2730(3) 0.0410(7) Uani 1.00 d . . . C16 C 0.7356(3) 0.2483(2) 1.3596(3) 0.0504(9) Uani 1.00 d . . . C17 C 0.8542(3) 0.2481(3) 1.3578(4) 0.063(1) Uani 1.00 d . . . C18 C 0.9183(3) 0.1857(3) 1.2716(5) 0.074(1) Uani 1.00 d . . . C19 C 0.8652(3) 0.1231(3) 1.1845(5) 0.075(1) Uani 1.00 d . . . C20 C 0.7470(3) 0.1225(2) 1.1860(4) 0.0552(9) Uani 1.00 d . . . C21 C 0.2758(2) 0.1669(2) 0.9946(3) 0.0349(6) Uani 1.00 d . . . C22 C 0.1765(3) 0.1255(2) 0.9950(3) 0.0467(8) Uani 1.00 d . . . C23 C 0.0923(3) 0.1284(2) 0.8679(4) 0.0538(9) Uani 1.00 d . . . C24 C 0.1040(3) 0.1723(2) 0.7360(4) 0.0538(9) Uani 1.00 d . . . C25 C 0.1958(3) 0.2171(2) 0.7342(3) 0.0472(8) Uani 1.00 d . . . C26 C 0.2828(2) 0.2185(2) 0.8638(3) 0.0372(7) Uani 1.00 d . . . C27 C 0.3748(3) 0.2733(2) 0.8674(3) 0.0402(7) Uani 1.00 d . . . C28 C 0.3738(3) 0.3366(2) 0.7467(3) 0.0541(9) Uani 1.00 d . . . C29 C 0.4544(3) 0.3939(2) 0.7547(4) 0.060(1) Uani 1.00 d . . . C30 C 0.5394(3) 0.3915(2) 0.8829(4) 0.0566(10) Uani 1.00 d . . . C31 C 0.5440(3) 0.3305(2) 1.0023(3) 0.0463(8) Uani 1.00 d . . . C32 C 0.4638(2) 0.2694(2) 0.9967(3) 0.0371(7) Uani 1.00 d . . . C33 C 0.2700(3) 0.2678(2) 1.3514(3) 0.0434(8) Uani 1.00 d . . . C36 C 0.4322(3) 0.3387(2) 1.3563(3) 0.0434(8) Uani 1.00 d . . . C38 C 0.2296(3) 0.4404(2) 1.2665(4) 0.0614(9) Uani 1.00 d . . . C39 C 0.1741(7) 0.5032(4) 1.3566(6) 0.191(3) Uani 1.00 d . . . C40 C 0.0981(10) 0.5868(5) 1.2893(9) 0.272(4) Uani 1.00 d . . . C41 C 0.0816(6) 0.6061(3) 1.1419(9) 0.160(2) Uani 1.00 d . . . C42 C 0.1377(4) 0.5431(3) 1.0494(6) 0.088(1) Uani 1.00 d . . . C43 C 0.2118(3) 0.4587(2) 1.1172(4) 0.066(1) Uani 1.00 d . . . C44 C 0.1185(6) 0.5630(6) 0.8858(8) 0.174(3) Uani 1.00 d . . . H1 H 0.542(3) 0.224(2) 1.489(3) 0.054(8) Uiso 1.00 calc . . . H2 H 0.376(2) 0.162(2) 1.492(3) 0.040(7) Uiso 1.00 calc . . . H3 H 0.442(3) -0.063(2) 1.152(4) 0.073(9) Uiso 1.00 calc . . . H4 H 0.336(3) -0.195(3) 1.158(4) 0.09(1) Uiso 1.00 calc . . . H5 H 0.182(3) -0.182(2) 1.307(4) 0.069(9) Uiso 1.00 calc . . . H6 H 0.133(3) -0.044(3) 1.441(4) 0.070(10) Uiso 1.00 calc . . . H7 H 0.214(2) 0.083(2) 1.428(3) 0.038(7) Uiso 1.00 calc . . . H8 H 0.691(3) 0.292(2) 1.420(3) 0.048(8) Uiso 1.00 calc . . . H9 H 0.885(3) 0.300(3) 1.411(4) 0.08(1) Uiso 1.00 calc . . . H10 H 1.003(4) 0.184(3) 1.271(5) 0.11(1) Uiso 1.00 calc . . . H11 H 0.907(4) 0.083(3) 1.111(5) 0.11(1) Uiso 1.00 calc . . . H12 H 0.707(3) 0.082(2) 1.124(4) 0.061(9) Uiso 1.00 calc . . . H13 H 0.164(2) 0.092(2) 1.093(3) 0.050(8) Uiso 1.00 calc . . . H14 H 0.026(3) 0.099(3) 0.874(4) 0.074(10) Uiso 1.00 calc . . . H15 H 0.042(3) 0.174(3) 0.648(4) 0.08(1) Uiso 1.00 calc . . . H16 H 0.199(3) 0.252(2) 0.642(4) 0.057(8) Uiso 1.00 calc . . . H17 H 0.314(3) 0.342(3) 0.660(4) 0.071(10) Uiso 1.00 calc . . . H18 H 0.455(3) 0.437(3) 0.667(4) 0.08(1) Uiso 1.00 calc . . . H19 H 0.594(3) 0.432(2) 0.895(3) 0.053(8) Uiso 1.00 calc . . . H20 H 0.604(3) 0.327(2) 1.090(4) 0.054(8) Uiso 1.00 calc . . . H21 H 0.1870 0.4906 1.4644 0.1267 Uiso 1.00 calc . . . H22 H 0.0600 0.6343 1.3524 0.1267 Uiso 1.00 calc . . . H23 H 0.0285 0.6649 1.1029 0.1267 Uiso 1.00 calc . . . H24 H 0.2515 0.4123 1.0555 0.0780 Uiso 1.00 calc . . . H25 H 0.1434 0.6194 0.8562 0.1267 Uiso 1.00 calc . . . H26 H 0.1655 0.5093 0.8345 0.1267 Uiso 1.00 calc . . . H27 H 0.0371 0.5690 0.8350 0.1267 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 O8 0.045(1) 0.037(1) 0.064(1) -0.0022(8) -0.0015(9) 0.0075(9) O34 0.043(1) 0.054(1) 0.092(2) -0.006(1) 0.009(1) -0.001(1) O37 0.075(2) 0.037(1) 0.083(2) -0.021(1) 0.016(1) -0.003(1) N35 0.054(1) 0.031(1) 0.048(1) -0.003(1) 0.005(1) 0.0021(10) C1 0.036(1) 0.030(1) 0.033(1) -0.0066(10) 0.002(1) 0.0052(9) C2 0.037(1) 0.029(1) 0.033(1) -0.005(1) 0.005(1) 0.0040(9) C3 0.037(1) 0.033(1) 0.033(1) -0.006(1) 0.004(1) 0.0001(10) C4 0.036(1) 0.034(1) 0.035(1) -0.009(1) 0.002(1) 0.003(1) C5 0.045(1) 0.034(1) 0.033(1) -0.009(1) 0.001(1) 0.002(1) C6 0.043(1) 0.034(1) 0.032(1) -0.007(1) 0.005(1) 0.004(1) C7 0.038(1) 0.036(1) 0.035(1) -0.009(1) 0.001(1) 0.004(1) C9 0.038(1) 0.036(1) 0.035(1) -0.008(1) 0.000(1) 0.008(1) C10 0.051(2) 0.040(1) 0.048(2) -0.014(1) 0.011(1) -0.002(1) C11 0.066(2) 0.041(2) 0.060(2) -0.019(1) 0.006(2) 0.001(1) C12 0.061(2) 0.047(2) 0.060(2) -0.026(2) -0.001(2) 0.014(1) C13 0.052(2) 0.064(2) 0.054(2) -0.023(2) 0.010(2) 0.010(2) C14 0.046(2) 0.043(2) 0.045(2) -0.012(1) 0.008(1) 0.005(1) C15 0.037(1) 0.041(1) 0.043(1) -0.011(1) -0.001(1) 0.009(1) C16 0.051(2) 0.052(2) 0.047(2) -0.018(1) -0.002(1) 0.004(1) C17 0.057(2) 0.066(2) 0.067(2) -0.033(2) -0.012(2) 0.013(2) C18 0.039(2) 0.071(2) 0.113(3) -0.018(2) 0.004(2) 0.019(2) C19 0.046(2) 0.070(2) 0.113(3) -0.012(2) 0.025(2) -0.002(2) C20 0.045(2) 0.056(2) 0.067(2) -0.015(1) 0.011(2) -0.008(2) C21 0.037(1) 0.030(1) 0.035(1) -0.004(1) 0.004(1) 0.0005(10) C22 0.046(2) 0.044(2) 0.046(2) -0.010(1) -0.003(1) 0.008(1) C23 0.045(2) 0.053(2) 0.059(2) -0.016(1) -0.009(1) 0.005(1) C24 0.047(2) 0.059(2) 0.047(2) -0.007(1) -0.008(1) -0.003(1) C25 0.051(2) 0.052(2) 0.032(1) -0.002(1) 0.002(1) 0.002(1) C26 0.041(1) 0.034(1) 0.033(1) -0.002(1) 0.004(1) -0.001(1) C27 0.052(2) 0.033(1) 0.033(1) -0.004(1) 0.010(1) 0.001(1) C28 0.074(2) 0.051(2) 0.037(2) -0.015(2) 0.007(1) 0.007(1) C29 0.090(3) 0.048(2) 0.047(2) -0.024(2) 0.019(2) 0.011(1) C30 0.076(2) 0.046(2) 0.055(2) -0.026(2) 0.015(2) 0.006(1) C31 0.055(2) 0.041(1) 0.045(2) -0.017(1) 0.009(1) 0.003(1) C32 0.042(1) 0.034(1) 0.035(1) -0.006(1) 0.011(1) 0.002(1) C33 0.047(2) 0.040(1) 0.042(2) -0.006(1) 0.008(1) -0.003(1) C36 0.058(2) 0.037(1) 0.036(1) -0.012(1) 0.008(1) -0.002(1) C38 0.068(2) 0.033(1) 0.068(2) 0.004(1) -0.011(2) -0.005(1) C39 0.263(8) 0.120(4) 0.083(3) 0.119(5) -0.047(4) -0.046(3) C40 0.38(1) 0.126(5) 0.148(6) 0.173(7) -0.107(7) -0.078(5) C41 0.185(6) 0.047(2) 0.175(6) 0.043(3) -0.081(5) -0.012(3) C42 0.071(2) 0.065(2) 0.120(4) -0.016(2) -0.010(2) 0.045(2) C43 0.059(2) 0.056(2) 0.081(2) -0.006(2) 0.012(2) 0.025(2) C44 0.121(5) 0.209(7) 0.163(6) 0.024(5) 0.022(4) 0.144(6) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SAPI91 _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 O8 C7 1.190(3) . . yes O34 C33 1.198(3) . . yes O37 C36 1.203(3) . . yes N35 C33 1.390(4) . . yes N35 C36 1.386(4) . . yes N35 C38 1.448(3) . . yes C1 C2 1.543(3) . . yes C1 C6 1.568(4) . . yes C1 C7 1.553(3) . . yes C1 C9 1.502(3) . . yes C2 C3 1.363(3) . . yes C2 C21 1.443(3) . . yes C3 C4 1.536(3) . . yes C3 C32 1.441(3) . . yes C4 C5 1.574(4) . . yes C4 C7 1.562(3) . . yes C4 C15 1.502(4) . . yes C5 C6 1.544(4) . . yes C5 C36 1.513(4) . . yes C6 C33 1.518(4) . . yes C9 C10 1.395(4) . . yes C9 C14 1.388(4) . . yes C10 C11 1.386(4) . . yes C11 C12 1.382(5) . . yes C12 C13 1.377(5) . . yes C13 C14 1.391(4) . . yes C15 C16 1.384(4) . . yes C15 C20 1.386(4) . . yes C16 C17 1.386(5) . . yes C17 C18 1.366(6) . . yes C18 C19 1.369(6) . . yes C19 C20 1.384(5) . . yes C21 C22 1.413(4) . . yes C21 C26 1.419(3) . . yes C22 C23 1.371(4) . . yes C23 C24 1.390(4) . . yes C24 C25 1.367(4) . . yes C25 C26 1.415(4) . . yes C26 C27 1.457(4) . . yes C27 C28 1.416(4) . . yes C27 C32 1.415(4) . . yes C28 C29 1.370(5) . . yes C29 C30 1.383(5) . . yes C30 C31 1.375(4) . . yes C31 C32 1.409(4) . . yes C38 C39 1.345(6) . . yes C38 C43 1.348(5) . . yes C39 C40 1.388(7) . . yes C40 C41 1.335(10) . . yes C41 C42 1.365(8) . . yes C42 C43 1.390(4) . . yes C42 C44 1.477(8) . . 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(33) N(35) C(36) 114.1(2) . . . yes C(33) N(35) C(38) 123.3(3) . . . yes C(36) N(35) C(38) 122.3(2) . . . yes C(2) C(1) C(6) 106.2(2) . . . yes C(2) C(1) C(7) 95.1(2) . . . yes C(2) C(1) C(9) 120.0(2) . . . yes C(6) C(1) C(7) 97.6(2) . . . yes C(6) C(1) C(9) 118.2(2) . . . yes C(7) C(1) C(9) 115.3(2) . . . yes C(1) C(2) C(3) 109.0(2) . . . yes C(1) C(2) C(21) 128.9(2) . . . yes C(3) C(2) C(21) 122.1(2) . . . yes C(2) C(3) C(4) 109.4(2) . . . yes C(2) C(3) C(32) 121.7(2) . . . yes C(4) C(3) C(32) 128.8(2) . . . yes C(3) C(4) C(5) 106.6(2) . . . yes C(3) C(4) C(7) 95.7(2) . . . yes C(3) C(4) C(15) 119.7(2) . . . yes C(5) C(4) C(7) 96.7(2) . . . yes C(5) C(4) C(15) 118.2(2) . . . yes C(7) C(4) C(15) 115.5(2) . . . yes C(4) C(5) C(6) 104.9(2) . . . yes C(4) C(5) C(36) 112.5(2) . . . yes C(4) C(5) H(1) 108(1) . . . no C(6) C(5) C(36) 105.2(2) . . . yes C(6) C(5) H(1) 113(1) . . . no C(36) C(5) H(1) 111(1) . . . no C(1) C(6) C(5) 105.8(2) . . . yes C(1) C(6) C(33) 113.2(2) . . . yes C(1) C(6) H(2) 113(1) . . . no C(5) C(6) C(33) 104.8(2) . . . yes C(5) C(6) H(2) 112(1) . . . no C(33) C(6) H(2) 106(1) . . . no O(8) C(7) C(1) 130.6(2) . . . yes O(8) C(7) C(4) 129.9(2) . . . yes C(1) C(7) C(4) 99.5(2) . . . yes C(1) C(9) C(10) 119.1(2) . . . yes C(1) C(9) C(14) 122.2(2) . . . yes C(10) C(9) C(14) 118.6(3) . . . yes C(9) C(10) C(11) 120.6(3) . . . yes C(9) C(10) H(3) 116(1) . . . no C(11) C(10) H(3) 122(1) . . . no C(10) C(11) C(12) 120.0(3) . . . yes C(10) C(11) H(4) 119(2) . . . no C(12) C(11) H(4) 120(2) . . . no C(11) C(12) C(13) 120.0(3) . . . yes C(11) C(12) H(5) 121(2) . . . no C(13) C(12) H(5) 118(2) . . . no C(12) C(13) C(14) 120.0(3) . . . yes C(12) C(13) H(6) 122(2) . . . no C(14) C(13) H(6) 117(2) . . . no C(9) C(14) C(13) 120.6(3) . . . yes C(9) C(14) H(7) 123(1) . . . no C(13) C(14) H(7) 115(1) . . . no C(4) C(15) C(16) 123.1(3) . . . yes C(4) C(15) C(20) 118.5(3) . . . yes C(16) C(15) C(20) 118.4(3) . . . yes C(15) C(16) C(17) 120.1(3) . . . yes C(15) C(16) H(8) 118(1) . . . no C(17) C(16) H(8) 120(1) . . . no C(16) C(17) C(18) 120.6(3) . . . yes C(16) C(17) H(9) 115(2) . . . no C(18) C(17) H(9) 123(2) . . . no C(17) C(18) C(19) 120.1(3) . . . yes C(17) C(18) H(10) 120(2) . . . no C(19) C(18) H(10) 118(2) . . . no C(18) C(19) C(20) 119.6(4) . . . yes C(18) C(19) H(11) 121(2) . . . no C(20) C(19) H(11) 118(2) . . . no C(15) C(20) C(19) 121.1(3) . . . yes C(15) C(20) H(12) 117(2) . . . no C(19) C(20) H(12) 121(2) . . . no C(2) C(21) C(22) 123.7(2) . . . yes C(2) C(21) C(26) 117.3(2) . . . yes C(22) C(21) C(26) 119.1(2) . . . yes C(21) C(22) C(23) 120.9(3) . . . yes C(21) C(22) H(13) 121(1) . . . no C(23) C(22) H(13) 117(1) . . . no C(22) C(23) C(24) 120.0(3) . . . yes C(22) C(23) H(14) 117(2) . . . no C(24) C(23) H(14) 122(2) . . . no C(23) C(24) C(25) 120.3(3) . . . yes C(23) C(24) H(15) 118(2) . . . no C(25) C(24) H(15) 121(2) . . . no C(24) C(25) C(26) 121.6(3) . . . yes C(24) C(25) H(16) 118(1) . . . no C(26) C(25) H(16) 119(1) . . . no C(21) C(26) C(25) 117.7(3) . . . yes C(21) C(26) C(27) 120.1(2) . . . yes C(25) C(26) C(27) 122.2(2) . . . yes C(26) C(27) C(28) 121.4(3) . . . yes C(26) C(27) C(32) 120.6(2) . . . yes C(28) C(27) C(32) 117.8(3) . . . yes C(27) C(28) C(29) 121.6(3) . . . yes C(27) C(28) H(17) 119(2) . . . no C(29) C(28) H(17) 118(2) . . . no C(28) C(29) C(30) 120.4(3) . . . yes C(28) C(29) H(18) 121(2) . . . no C(30) C(29) H(18) 118(2) . . . no C(29) C(30) C(31) 119.9(3) . . . yes C(29) C(30) H(19) 122(1) . . . no C(31) C(30) H(19) 117(1) . . . no C(30) C(31) C(32) 121.1(3) . . . yes C(30) C(31) H(20) 120(1) . . . no C(32) C(31) H(20) 118(1) . . . no C(3) C(32) C(27) 117.3(2) . . . yes C(3) C(32) C(31) 123.4(2) . . . yes C(27) C(32) C(31) 119.1(2) . . . yes O(34) C(33) N(35) 124.2(3) . . . yes O(34) C(33) C(6) 127.9(3) . . . yes N(35) C(33) C(6) 107.9(2) . . . yes O(37) C(36) N(35) 124.4(3) . . . yes O(37) C(36) C(5) 127.7(3) . . . yes N(35) C(36) C(5) 107.9(2) . . . yes N(35) C(38) C(39) 120.4(3) . . . yes N(35) C(38) C(43) 118.6(3) . . . yes C(39) C(38) C(43) 121.1(3) . . . yes C(38) C(39) C(40) 117.2(5) . . . yes C(38) C(39) H(21) 121.4 . . . no C(40) C(39) H(21) 121.4 . . . no C(39) C(40) C(41) 122.1(6) . . . yes C(39) C(40) H(22) 118.6 . . . no C(41) C(40) H(22) 119.2 . . . no C(40) C(41) C(42) 121.2(4) . . . yes C(40) C(41) H(23) 117.9 . . . no C(42) C(41) H(23) 120.9 . . . no C(41) C(42) C(43) 116.3(4) . . . yes C(41) C(42) C(44) 121.7(5) . . . yes C(43) C(42) C(44) 122.0(5) . . . yes C(38) C(43) C(42) 122.0(4) . . . yes C(38) C(43) H(24) 119.4 . . . no C(42) C(43) H(24) 118.6 . . . no C(42) C(44) H(25) 115.1 . . . no C(42) C(44) H(26) 111.4 . . . no C(42) C(44) H(27) 114.5 . . . no H(25) C(44) H(26) 104.0 . . . no H(25) C(44) H(27) 106.8 . . . no H(26) C(44) H(27) 104.0 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O8 C14 3.024(3) . 2_658 ? O8 C9 3.493(3) . 2_658 ? O8 C13 3.506(4) . 2_658 ? O34 C18 3.299(4) . 1_455 ? O34 C25 3.598(4) . 1_556 ? O37 C29 3.318(4) . 2_667 ? O37 C30 3.543(4) . 2_667 ? C11 C20 3.600(5) . 2_657 ? C12 C16 3.415(4) . 2_658 ? C13 C16 3.552(4) . 2_658 ? C17 C44 3.587(6) . 2_667 ? C19 C23 3.553(5) . 2_657 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ data_yy_pcmx_pc-m-Me_p-xylene _database_code_CSD 180115 _audit_creation_date 'Sat May 11 19:35:11 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C48 H37 N O3 ' _chemical_formula_moiety '?' _chemical_formula_weight 675.83 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 11.385(4) _cell_length_b 16.895(5) _cell_length_c 10.483(4) _cell_angle_alpha 101.11(3) _cell_angle_beta 114.33(2) _cell_angle_gamma 95.93(3) _cell_volume 1764(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 18.5 _cell_measurement_theta_max 19.6 _cell_measurement_temperature 293.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 8513 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 1.0011 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.0011 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.70 #------------------------------------------------------------------------------ # 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 8103 _reflns_number_gt 4962 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.0779 _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 4962 _refine_ls_number_parameters 565 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00490|Fo|^2^]' _refine_ls_shift/su_max 0.0259 _refine_diff_density_max 0.17 _refine_diff_density_min -0.24 _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) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; '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 O(8) O 0.5291(1) 0.45038(9) 0.1497(2) 0.0528(4) Uani 1.00 d . . . O(34) O 0.5551(2) 0.1578(1) -0.1720(2) 0.0643(5) Uani 1.00 d . . . O(37) O 0.1627(2) 0.23723(10) -0.3682(2) 0.0601(5) Uani 1.00 d . . . N(35) N 0.3446(2) 0.1789(1) -0.2852(2) 0.0446(4) Uani 1.00 d . . . C(1) C 0.3333(2) 0.3550(1) -0.0584(2) 0.0372(5) Uani 1.00 d . . . C(2) C 0.2947(2) 0.2796(1) -0.0117(2) 0.0360(4) Uani 1.00 d . . . C(3) C 0.4046(2) 0.2475(1) 0.0489(2) 0.0361(4) Uani 1.00 d . . . C(4) C 0.5239(2) 0.3023(1) 0.0553(2) 0.0363(5) Uani 1.00 d . . . C(5) C 0.5032(2) 0.2914(1) -0.1057(2) 0.0379(5) Uani 1.00 d . . . C(6) C 0.3734(2) 0.3211(1) -0.1811(2) 0.0388(5) Uani 1.00 d . . . C(7) C 0.4743(2) 0.3845(1) 0.0685(2) 0.0376(5) Uani 1.00 d . . . C(9) C 0.2516(2) 0.4205(1) -0.0768(2) 0.0422(5) Uani 1.00 d . . . C(10) C 0.2391(2) 0.4633(1) 0.0420(3) 0.0558(6) Uani 1.00 d . . . C(11) C 0.1635(3) 0.5237(2) 0.0286(4) 0.0680(8) Uani 1.00 d . . . C(12) C 0.1014(3) 0.5415(2) -0.1021(4) 0.0716(9) Uani 1.00 d . . . C(13) C 0.1136(3) 0.4995(2) -0.2207(4) 0.0708(9) Uani 1.00 d . . . C(14) C 0.1885(2) 0.4391(1) -0.2089(3) 0.0536(6) Uani 1.00 d . . . C(15) C 0.6589(2) 0.3050(1) 0.1709(2) 0.0412(5) Uani 1.00 d . . . C(16) C 0.7587(2) 0.2805(1) 0.1393(3) 0.0499(6) Uani 1.00 d . . . C(17) C 0.8804(2) 0.2821(2) 0.2514(3) 0.0618(7) Uani 1.00 d . . . C(18) C 0.9039(2) 0.3093(2) 0.3930(3) 0.0683(7) Uani 1.00 d . . . C(19) C 0.8059(3) 0.3352(2) 0.4253(3) 0.0674(8) Uani 1.00 d . . . C(20) C 0.6833(2) 0.3327(2) 0.3148(2) 0.0538(6) Uani 1.00 d . . . C(21) C 0.1676(2) 0.2412(1) -0.0320(2) 0.0396(5) Uani 1.00 d . . . C(22) C 0.0513(2) 0.2706(1) -0.0985(3) 0.0519(6) Uani 1.00 d . . . C(23) C -0.0655(2) 0.2333(2) -0.1081(3) 0.0629(7) Uani 1.00 d . . . C(24) C -0.0732(2) 0.1657(2) -0.0537(3) 0.0646(8) Uani 1.00 d . . . C(25) C 0.0366(2) 0.1341(1) 0.0082(3) 0.0558(7) Uani 1.00 d . . . C(26) C 0.1599(2) 0.1696(1) 0.0196(2) 0.0418(5) Uani 1.00 d . . . C(27) C 0.2747(2) 0.1331(1) 0.0759(2) 0.0430(5) Uani 1.00 d . . . C(28) C 0.2682(2) 0.0584(1) 0.1172(3) 0.0571(7) Uani 1.00 d . . . C(29) C 0.3748(3) 0.0220(2) 0.1628(3) 0.0654(8) Uani 1.00 d . . . C(30) C 0.4930(3) 0.0572(1) 0.1686(3) 0.0595(7) Uani 1.00 d . . . C(31) C 0.5047(2) 0.1308(1) 0.1334(2) 0.0493(6) Uani 1.00 d . . . C(32) C 0.3973(2) 0.1704(1) 0.0881(2) 0.0390(5) Uani 1.00 d . . . C(33) C 0.4770(2) 0.2026(1) -0.1877(2) 0.0434(5) Uani 1.00 d . . . C(36) C 0.2775(2) 0.2439(1) -0.2908(2) 0.0432(5) Uani 1.00 d . . . C(38) C 0.2804(2) 0.0935(1) -0.3596(2) 0.0480(5) Uani 1.00 d . . . C(39) C 0.3032(3) 0.0523(2) -0.4707(3) 0.0700(8) Uani 1.00 d . . . C(40) C 0.2415(4) -0.0301(2) -0.5349(4) 0.085(1) Uani 1.00 d . . . C(41) C 0.1616(3) -0.0690(2) -0.4876(3) 0.0763(8) Uani 1.00 d . . . C(42) C 0.1414(2) -0.0283(1) -0.3744(3) 0.0598(6) Uani 1.00 d . . . C(43) C 0.0586(3) -0.0706(2) -0.3180(4) 0.090(1) Uani 1.00 d . . . C(44) C 0.2015(2) 0.0549(1) -0.3110(3) 0.0534(6) Uani 1.00 d . . . H(1) H 0.577(2) 0.321(1) -0.108(2) 0.038(5) Uiso 1.00 calc . . . H(2) H 0.382(2) 0.364(1) -0.229(2) 0.042(5) Uiso 1.00 calc . . . H(3) H 0.285(3) 0.451(2) 0.140(3) 0.070(7) Uiso 1.00 calc . . . H(4) H 0.157(4) 0.552(2) 0.118(4) 0.110(9) Uiso 1.00 calc . . . H(5) H 0.046(3) 0.582(2) -0.108(4) 0.099(8) Uiso 1.00 calc . . . H(6) H 0.075(3) 0.512(2) -0.313(3) 0.082(8) Uiso 1.00 calc . . . H(7) H 0.199(3) 0.410(2) -0.295(3) 0.078(8) Uiso 1.00 calc . . . H(8) H 0.744(2) 0.261(2) 0.038(3) 0.061(7) Uiso 1.00 calc . . . H(9) H 0.949(3) 0.265(2) 0.229(3) 0.078(8) Uiso 1.00 calc . . . H(10) H 0.990(3) 0.305(2) 0.470(3) 0.084(8) Uiso 1.00 calc . . . H(11) H 0.822(3) 0.354(2) 0.530(4) 0.082(8) Uiso 1.00 calc . . . H(12) H 0.618(3) 0.351(2) 0.338(3) 0.059(7) Uiso 1.00 calc . . . H(13) H 0.055(3) 0.317(2) -0.137(3) 0.065(7) Uiso 1.00 calc . . . H(14) H -0.143(3) 0.253(2) -0.148(3) 0.073(7) Uiso 1.00 calc . . . H(15) H -0.148(3) 0.140(2) -0.056(3) 0.067(7) Uiso 1.00 calc . . . H(16) H 0.032(2) 0.086(2) 0.047(3) 0.056(6) Uiso 1.00 calc . . . H(17) H 0.185(3) 0.035(2) 0.120(3) 0.072(7) Uiso 1.00 calc . . . H(18) H 0.365(3) -0.029(2) 0.190(4) 0.099(8) Uiso 1.00 calc . . . H(19) H 0.572(3) 0.032(2) 0.201(3) 0.063(7) Uiso 1.00 calc . . . H(20) H 0.578(3) 0.155(2) 0.132(3) 0.065(7) Uiso 1.00 calc . . . H(21) H 0.360(3) 0.084(2) -0.496(3) 0.081(8) Uiso 1.00 calc . . . H(22) H 0.261(3) -0.058(2) -0.617(4) 0.109(9) Uiso 1.00 calc . . . H(23) H 0.115(3) -0.127(2) -0.537(4) 0.102(9) Uiso 1.00 calc . . . H(24) H 0.192(2) 0.085(2) -0.224(3) 0.063(7) Uiso 1.00 calc . . . H(25) H -0.0145 -0.0447 -0.3210 0.0994 Uiso 1.00 calc . . . H(26) H 0.0219 -0.1277 -0.3683 0.0994 Uiso 1.00 calc . . . H(27) H 0.1091 -0.0697 -0.2151 0.0624 Uiso 1.00 calc . . . C(45) C 0.5932(4) 0.2159(3) 0.5404(4) 0.105(1) Uani 1.00 d . . . C(46) C 0.5035(3) 0.2755(2) 0.5187(3) 0.0721(9) Uani 1.00 d . . . C(47) C 0.5459(3) 0.3583(2) 0.5924(3) 0.0807(9) Uani 1.00 d . . . C(48) C 0.4626(3) 0.4131(2) 0.5681(3) 0.0792(9) Uani 1.00 d . . . C(49) C 0.3322(3) 0.3879(2) 0.4672(3) 0.0715(9) Uani 1.00 d . . . C(50) C 0.2414(4) 0.4466(2) 0.4391(5) 0.102(1) Uani 1.00 d . . . C(51) C 0.2902(3) 0.3050(2) 0.3930(3) 0.0819(9) Uani 1.00 d . . . C(52) C 0.3731(4) 0.2510(2) 0.4201(3) 0.0797(9) Uani 1.00 d . . . H(28) H 0.6391 0.3789 0.6666 0.0995 Uiso 1.00 calc . . . H(29) H 0.4958 0.4710 0.6235 0.0925 Uiso 1.00 calc . . . H(30) H 0.1966 0.2858 0.3224 0.0995 Uiso 1.00 calc . . . H(31) H 0.3404 0.1919 0.3634 0.0624 Uiso 1.00 calc . . . H(32) H 0.5685 0.1721 0.5762 0.1228 Uiso 1.00 calc . . . H(33) H 0.6044 0.1930 0.4572 0.1228 Uiso 1.00 calc . . . H(34) H 0.6847 0.2440 0.6172 0.0925 Uiso 1.00 calc . . . H(35) H 0.2845 0.5030 0.4970 0.1194 Uiso 1.00 calc . . . H(36) H 0.2042 0.4502 0.3383 0.1194 Uiso 1.00 calc . . . H(37) H 0.1672 0.4326 0.4584 0.0947 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 O(8) 0.0450(8) 0.0413(8) 0.0575(9) 0.0034(6) 0.0154(7) 0.0015(7) O(34) 0.0582(10) 0.0595(10) 0.065(1) 0.0299(8) 0.0166(8) 0.0087(8) O(37) 0.0460(9) 0.0564(9) 0.0538(9) 0.0146(7) 0.0018(7) 0.0074(7) N(35) 0.0468(10) 0.0403(9) 0.0405(9) 0.0111(7) 0.0138(7) 0.0091(7) C(1) 0.0319(9) 0.0334(9) 0.0447(10) 0.0074(7) 0.0148(8) 0.0125(7) C(2) 0.0329(9) 0.0352(9) 0.0376(9) 0.0056(7) 0.0136(7) 0.0107(7) C(3) 0.0314(9) 0.0380(9) 0.0364(9) 0.0057(7) 0.0128(7) 0.0110(7) C(4) 0.0312(9) 0.0361(9) 0.0399(9) 0.0059(7) 0.0139(7) 0.0118(7) C(5) 0.0331(9) 0.0408(10) 0.044(1) 0.0093(8) 0.0186(8) 0.0172(8) C(6) 0.0378(10) 0.0381(9) 0.0419(10) 0.0089(8) 0.0163(8) 0.0168(8) C(7) 0.0338(9) 0.0377(10) 0.0411(10) 0.0040(7) 0.0169(8) 0.0111(8) C(9) 0.0348(9) 0.0322(9) 0.057(1) 0.0057(7) 0.0171(8) 0.0137(8) C(10) 0.045(1) 0.054(1) 0.063(1) 0.0146(10) 0.021(1) 0.009(1) C(11) 0.051(1) 0.053(1) 0.094(2) 0.016(1) 0.032(1) 0.004(1) C(12) 0.058(2) 0.046(1) 0.117(2) 0.024(1) 0.039(2) 0.029(1) C(13) 0.066(2) 0.067(2) 0.096(2) 0.033(1) 0.035(2) 0.048(2) C(14) 0.051(1) 0.050(1) 0.067(1) 0.0189(10) 0.026(1) 0.028(1) C(15) 0.0308(9) 0.0403(10) 0.046(1) 0.0042(7) 0.0107(8) 0.0147(8) C(16) 0.035(1) 0.048(1) 0.060(1) 0.0077(8) 0.0154(9) 0.014(1) C(17) 0.034(1) 0.060(1) 0.081(2) 0.0127(10) 0.013(1) 0.022(1) C(18) 0.042(1) 0.067(2) 0.070(2) 0.008(1) -0.001(1) 0.023(1) C(19) 0.054(1) 0.079(2) 0.052(1) 0.010(1) 0.006(1) 0.020(1) C(20) 0.043(1) 0.064(1) 0.048(1) 0.010(1) 0.0132(10) 0.018(1) C(21) 0.0348(9) 0.0387(10) 0.0414(10) 0.0038(7) 0.0159(8) 0.0069(8) C(22) 0.033(1) 0.049(1) 0.069(1) 0.0082(9) 0.0173(10) 0.019(1) C(23) 0.035(1) 0.059(1) 0.090(2) 0.009(1) 0.024(1) 0.018(1) C(24) 0.042(1) 0.053(1) 0.099(2) -0.002(1) 0.038(1) 0.012(1) C(25) 0.052(1) 0.042(1) 0.078(2) 0.0003(9) 0.037(1) 0.013(1) C(26) 0.041(1) 0.0354(9) 0.047(1) 0.0021(8) 0.0215(9) 0.0072(8) C(27) 0.044(1) 0.0380(10) 0.045(1) 0.0049(8) 0.0181(9) 0.0114(8) C(28) 0.058(1) 0.043(1) 0.074(2) 0.006(1) 0.030(1) 0.024(1) C(29) 0.068(2) 0.045(1) 0.085(2) 0.012(1) 0.028(1) 0.034(1) C(30) 0.057(1) 0.048(1) 0.072(2) 0.018(1) 0.021(1) 0.026(1) C(31) 0.043(1) 0.046(1) 0.058(1) 0.0099(9) 0.0177(10) 0.0227(10) C(32) 0.0394(10) 0.0370(9) 0.0377(9) 0.0057(8) 0.0146(8) 0.0111(8) C(33) 0.046(1) 0.046(1) 0.0416(10) 0.0156(9) 0.0199(9) 0.0149(8) C(36) 0.044(1) 0.045(1) 0.0384(10) 0.0133(8) 0.0137(9) 0.0142(8) C(38) 0.052(1) 0.039(1) 0.043(1) 0.0119(9) 0.0121(9) 0.0085(8) C(39) 0.090(2) 0.055(1) 0.065(2) 0.016(1) 0.037(2) 0.008(1) C(40) 0.116(3) 0.058(2) 0.074(2) 0.020(2) 0.043(2) -0.003(1) C(41) 0.084(2) 0.046(1) 0.072(2) 0.011(1) 0.015(1) 0.002(1) C(42) 0.053(1) 0.044(1) 0.060(1) 0.0072(10) 0.006(1) 0.011(1) C(43) 0.086(2) 0.066(2) 0.094(2) -0.009(2) 0.024(2) 0.022(2) C(44) 0.055(1) 0.048(1) 0.046(1) 0.0073(10) 0.014(1) 0.0095(10) C(45) 0.112(3) 0.130(3) 0.098(3) 0.033(2) 0.061(2) 0.047(2) C(46) 0.087(2) 0.084(2) 0.056(1) 0.015(2) 0.042(1) 0.021(1) C(47) 0.065(2) 0.102(2) 0.059(2) -0.008(2) 0.024(1) 0.007(2) C(48) 0.087(2) 0.071(2) 0.070(2) -0.009(2) 0.043(2) -0.007(1) C(49) 0.079(2) 0.075(2) 0.066(2) 0.004(1) 0.041(1) 0.017(1) C(50) 0.110(3) 0.101(3) 0.122(3) 0.032(2) 0.070(3) 0.045(2) C(51) 0.077(2) 0.078(2) 0.066(2) -0.006(2) 0.015(1) 0.013(1) C(52) 0.100(2) 0.064(2) 0.059(2) 0.001(2) 0.029(2) 0.006(1) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SAPI91 _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 O(8) C(7) 1.187(2) . . yes O(34) C(33) 1.206(2) . . yes O(37) C(36) 1.200(2) . . yes N(35) C(33) 1.388(3) . . yes N(35) C(36) 1.397(3) . . yes N(35) C(38) 1.451(3) . . yes C(1) C(2) 1.536(3) . . yes C(1) C(6) 1.563(3) . . yes C(1) C(7) 1.554(3) . . yes C(1) C(9) 1.508(3) . . yes C(2) C(3) 1.371(3) . . yes C(2) C(21) 1.435(3) . . yes C(3) C(4) 1.533(3) . . yes C(3) C(32) 1.444(3) . . yes C(4) C(5) 1.574(3) . . yes C(4) C(7) 1.554(3) . . yes C(4) C(15) 1.504(3) . . yes C(5) C(6) 1.550(3) . . yes C(5) C(33) 1.510(3) . . yes C(6) C(36) 1.520(3) . . yes C(9) C(10) 1.384(3) . . yes C(9) C(14) 1.388(3) . . yes C(10) C(11) 1.393(3) . . yes C(11) C(12) 1.368(4) . . yes C(12) C(13) 1.375(4) . . yes C(13) C(14) 1.388(3) . . yes C(15) C(16) 1.389(3) . . yes C(15) C(20) 1.388(3) . . yes C(16) C(17) 1.392(3) . . yes C(17) C(18) 1.367(4) . . yes C(18) C(19) 1.381(4) . . yes C(19) C(20) 1.389(3) . . yes C(21) C(22) 1.412(3) . . yes C(21) C(26) 1.426(3) . . yes C(22) C(23) 1.367(3) . . yes C(23) C(24) 1.380(4) . . yes C(24) C(25) 1.369(4) . . yes C(25) C(26) 1.417(3) . . yes C(26) C(27) 1.452(3) . . yes C(27) C(28) 1.415(3) . . yes C(27) C(32) 1.415(3) . . yes C(28) C(29) 1.367(3) . . yes C(29) C(30) 1.386(4) . . yes C(30) C(31) 1.372(3) . . yes C(31) C(32) 1.408(3) . . yes C(38) C(39) 1.371(4) . . yes C(38) C(44) 1.371(3) . . yes C(39) C(40) 1.390(4) . . yes C(40) C(41) 1.372(5) . . yes C(41) C(42) 1.369(4) . . yes C(42) C(43) 1.494(4) . . yes C(42) C(44) 1.397(3) . . yes C(45) C(46) 1.489(5) . . yes C(46) C(47) 1.386(4) . . yes C(46) C(52) 1.374(4) . . yes C(47) C(48) 1.376(5) . . yes C(48) C(49) 1.380(4) . . yes C(49) C(50) 1.487(5) . . yes C(49) C(51) 1.390(4) . . yes C(51) C(52) 1.364(4) . . 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(33) N(35) C(36) 113.3(2) . . . yes C(33) N(35) C(38) 122.6(2) . . . yes C(36) N(35) C(38) 123.7(2) . . . yes C(2) C(1) C(6) 105.8(1) . . . yes C(2) C(1) C(7) 96.2(1) . . . yes C(2) C(1) C(9) 120.3(2) . . . yes C(6) C(1) C(7) 97.6(1) . . . yes C(6) C(1) C(9) 118.4(2) . . . yes C(7) C(1) C(9) 114.2(2) . . . yes C(1) C(2) C(3) 108.3(2) . . . yes C(1) C(2) C(21) 129.4(2) . . . yes C(3) C(2) C(21) 122.1(2) . . . yes C(2) C(3) C(4) 109.5(2) . . . yes C(2) C(3) C(32) 121.7(2) . . . yes C(4) C(3) C(32) 128.7(2) . . . yes C(3) C(4) C(5) 106.8(1) . . . yes C(3) C(4) C(7) 96.8(1) . . . yes C(3) C(4) C(15) 119.1(2) . . . yes C(5) C(4) C(7) 96.0(1) . . . yes C(5) C(4) C(15) 118.8(2) . . . yes C(7) C(4) C(15) 114.9(2) . . . yes C(4) C(5) C(6) 104.4(1) . . . yes C(4) C(5) C(33) 113.5(1) . . . yes C(6) C(5) C(33) 105.2(2) . . . yes C(1) C(6) C(5) 105.7(1) . . . yes C(1) C(6) C(36) 112.6(2) . . . yes C(5) C(6) C(36) 104.3(2) . . . yes O(8) C(7) C(1) 130.6(2) . . . yes O(8) C(7) C(4) 130.3(2) . . . yes C(1) C(7) C(4) 99.1(1) . . . yes C(1) C(9) C(10) 118.8(2) . . . yes C(1) C(9) C(14) 122.2(2) . . . yes C(10) C(9) C(14) 119.0(2) . . . yes C(9) C(10) C(11) 120.3(2) . . . yes C(10) C(11) C(12) 120.2(3) . . . yes C(11) C(12) C(13) 119.9(2) . . . yes C(12) C(13) C(14) 120.4(3) . . . yes C(9) C(14) C(13) 120.1(3) . . . yes C(4) C(15) C(16) 122.7(2) . . . yes C(4) C(15) C(20) 118.1(2) . . . yes C(16) C(15) C(20) 119.1(2) . . . yes C(15) C(16) C(17) 119.9(2) . . . yes C(16) C(17) C(18) 120.8(3) . . . yes C(17) C(18) C(19) 119.7(2) . . . yes C(18) C(19) C(20) 120.3(3) . . . yes C(15) C(20) C(19) 120.2(2) . . . yes C(2) C(21) C(22) 123.9(2) . . . yes C(2) C(21) C(26) 117.4(2) . . . yes C(22) C(21) C(26) 118.7(2) . . . yes C(21) C(22) C(23) 120.8(2) . . . yes C(22) C(23) C(24) 121.0(2) . . . yes C(23) C(24) C(25) 120.0(2) . . . yes C(24) C(25) C(26) 121.4(2) . . . yes C(21) C(26) C(25) 118.0(2) . . . yes C(21) C(26) C(27) 120.2(2) . . . yes C(25) C(26) C(27) 121.8(2) . . . yes C(26) C(27) C(28) 121.8(2) . . . yes C(26) C(27) C(32) 120.7(2) . . . yes C(28) C(27) C(32) 117.5(2) . . . yes C(27) C(28) C(29) 121.5(2) . . . yes C(28) C(29) C(30) 120.6(2) . . . yes C(29) C(30) C(31) 119.7(2) . . . yes C(30) C(31) C(32) 121.0(2) . . . yes C(3) C(32) C(27) 117.4(2) . . . yes C(3) C(32) C(31) 123.0(2) . . . yes C(27) C(32) C(31) 119.5(2) . . . yes O(34) C(33) N(35) 124.4(2) . . . yes O(34) C(33) C(5) 127.2(2) . . . yes N(35) C(33) C(5) 108.3(2) . . . yes O(37) C(36) N(35) 124.3(2) . . . yes O(37) C(36) C(6) 127.3(2) . . . yes N(35) C(36) C(6) 108.4(2) . . . yes N(35) C(38) C(39) 120.7(2) . . . yes N(35) C(38) C(44) 117.7(2) . . . yes C(39) C(38) C(44) 121.5(2) . . . yes C(38) C(39) C(40) 117.9(3) . . . yes C(39) C(40) C(41) 120.9(3) . . . yes C(40) C(41) C(42) 121.2(3) . . . yes C(41) C(42) C(43) 121.8(3) . . . yes C(41) C(42) C(44) 118.1(3) . . . yes C(43) C(42) C(44) 120.1(3) . . . yes C(38) C(44) C(42) 120.4(2) . . . yes C(45) C(46) C(47) 122.8(3) . . . yes C(45) C(46) C(52) 120.9(3) . . . yes C(47) C(46) C(52) 116.2(3) . . . yes C(46) C(47) C(48) 122.1(3) . . . yes C(47) C(48) C(49) 121.2(3) . . . yes C(48) C(49) C(50) 121.7(3) . . . yes C(48) C(49) C(51) 116.6(3) . . . yes C(50) C(49) C(51) 121.7(3) . . . yes C(49) C(51) C(52) 121.7(3) . . . yes C(46) C(52) C(51) 122.2(3) . . . 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 O(8) C(7) C(1) C(2) -129.9(2) . . . . yes O(8) C(7) C(1) C(6) 123.2(2) . . . . yes O(8) C(7) C(1) C(9) -2.7(3) . . . . yes O(8) C(7) C(4) C(3) 131.9(2) . . . . yes O(8) C(7) C(4) C(5) -120.3(2) . . . . yes O(8) C(7) C(4) C(15) 5.4(3) . . . . yes O(34) C(33) N(35) C(36) -175.2(2) . . . . yes O(34) C(33) N(35) C(38) 11.9(3) . . . . yes O(34) C(33) C(5) C(4) -72.6(3) . . . . yes O(34) C(33) C(5) C(6) 173.9(2) . . . . yes O(34) C(33) C(5) H(1) 51(1) . . . . no O(37) C(36) N(35) C(33) 179.5(2) . . . . yes O(37) C(36) N(35) C(38) -7.6(3) . . . . yes O(37) C(36) C(6) C(1) 61.6(3) . . . . yes O(37) C(36) C(6) C(5) 175.7(2) . . . . yes O(37) C(36) C(6) H(2) -61(1) . . . . no N(35) C(33) C(5) C(4) 106.1(2) . . . . yes N(35) C(33) C(5) C(6) -7.4(2) . . . . yes N(35) C(33) C(5) H(1) -129(1) . . . . no N(35) C(36) C(6) C(1) -116.8(2) . . . . yes N(35) C(36) C(6) C(5) -2.8(2) . . . . yes N(35) C(36) C(6) H(2) 119(1) . . . . no N(35) C(38) C(39) C(40) 178.3(3) . . . . yes N(35) C(38) C(39) H(21) -2(2) . . . . no N(35) C(38) C(44) C(42) -177.3(2) . . . . yes N(35) C(38) C(44) H(24) -2(1) . . . . no C(1) C(2) C(3) C(4) 3.6(2) . . . . yes C(1) C(2) C(3) C(32) -172.5(2) . . . . yes C(1) C(2) C(21) C(22) -2.3(3) . . . . yes C(1) C(2) C(21) C(26) 178.2(2) . . . . yes C(1) C(6) C(5) C(4) 5.1(2) . . . . yes C(1) C(6) C(5) C(33) 124.8(2) . . . . yes C(1) C(6) C(5) H(1) -115(1) . . . . no C(1) C(7) C(4) C(3) -49.4(2) . . . . yes C(1) C(7) C(4) C(5) 58.4(1) . . . . yes C(1) C(7) C(4) C(15) -175.9(2) . . . . yes C(1) C(9) C(10) C(11) -179.4(2) . . . . yes C(1) C(9) C(10) H(3) 0(1) . . . . no C(1) C(9) C(14) C(13) 179.5(2) . . . . yes C(1) C(9) C(14) H(7) -1(1) . . . . no C(2) C(1) C(6) C(5) -68.4(2) . . . . yes C(2) C(1) C(6) C(36) 44.8(2) . . . . yes C(2) C(1) C(6) H(2) 168(1) . . . . no C(2) C(1) C(7) C(4) 51.4(2) . . . . yes C(2) C(1) C(9) C(10) 61.3(2) . . . . yes C(2) C(1) C(9) C(14) -118.6(2) . . . . yes C(2) C(3) C(4) C(5) -69.3(2) . . . . yes C(2) C(3) C(4) C(7) 29.1(2) . . . . yes C(2) C(3) C(4) C(15) 152.6(2) . . . . yes C(2) C(3) C(32) C(27) -6.5(3) . . . . yes C(2) C(3) C(32) C(31) 171.8(2) . . . . yes C(2) C(21) C(22) C(23) -176.8(2) . . . . yes C(2) C(21) C(22) H(13) 3(1) . . . . no C(2) C(21) C(26) C(25) 176.2(2) . . . . yes C(2) C(21) C(26) C(27) -6.4(3) . . . . yes C(3) C(2) C(1) C(6) 65.0(2) . . . . yes C(3) C(2) C(1) C(7) -34.7(2) . . . . yes C(3) C(2) C(1) C(9) -157.5(2) . . . . yes C(3) C(2) C(21) C(22) -177.7(2) . . . . yes C(3) C(2) C(21) C(26) 2.8(3) . . . . yes C(3) C(4) C(5) C(6) 60.7(2) . . . . yes C(3) C(4) C(5) C(33) -53.3(2) . . . . yes C(3) C(4) C(5) H(1) -176(1) . . . . no C(3) C(4) C(15) C(16) 118.6(2) . . . . yes C(3) C(4) C(15) C(20) -61.0(2) . . . . yes C(3) C(32) C(27) C(26) 2.8(3) . . . . yes C(3) C(32) C(27) C(28) -178.7(2) . . . . yes C(3) C(32) C(31) C(30) -179.5(2) . . . . yes C(3) C(32) C(31) H(20) -3(1) . . . . no C(4) C(3) C(2) C(21) 179.9(2) . . . . yes C(4) C(3) C(32) C(27) 178.2(2) . . . . yes C(4) C(3) C(32) C(31) -3.5(3) . . . . yes C(4) C(5) C(6) C(36) -113.7(2) . . . . yes C(4) C(5) C(6) H(2) 125(1) . . . . no C(4) C(7) C(1) C(6) -55.5(2) . . . . yes C(4) C(7) C(1) C(9) 178.6(2) . . . . yes C(4) C(15) C(16) C(17) -178.1(2) . . . . yes C(4) C(15) C(16) H(8) 1(1) . . . . no C(4) C(15) C(20) C(19) 179.1(2) . . . . yes C(4) C(15) C(20) H(12) -1(1) . . . . no C(5) C(4) C(3) C(32) 106.5(2) . . . . yes C(5) C(4) C(15) C(16) -14.6(3) . . . . yes C(5) C(4) C(15) C(20) 165.9(2) . . . . yes C(5) C(6) C(1) C(7) 30.2(2) . . . . yes C(5) C(6) C(1) C(9) 153.1(2) . . . . yes C(5) C(33) N(35) C(36) 6.0(2) . . . . yes C(5) C(33) N(35) C(38) -166.9(2) . . . . yes C(6) C(1) C(2) C(21) -110.9(2) . . . . yes C(6) C(1) C(9) C(10) -166.4(2) . . . . yes C(6) C(1) C(9) C(14) 13.8(3) . . . . yes C(6) C(5) C(4) C(7) -38.2(2) . . . . yes C(6) C(5) C(4) C(15) -161.1(2) . . . . yes C(6) C(36) N(35) C(33) -2.0(2) . . . . yes C(6) C(36) N(35) C(38) 170.9(2) . . . . yes C(7) C(1) C(2) C(21) 149.4(2) . . . . yes C(7) C(1) C(6) C(36) 143.5(2) . . . . yes C(7) C(1) C(6) H(2) -92(1) . . . . no C(7) C(1) C(9) C(10) -52.3(2) . . . . yes C(7) C(1) C(9) C(14) 127.8(2) . . . . yes C(7) C(4) C(3) C(32) -155.1(2) . . . . yes C(7) C(4) C(5) C(33) -152.2(2) . . . . yes C(7) C(4) C(5) H(1) 84(1) . . . . no C(7) C(4) C(15) C(16) -127.4(2) . . . . yes C(7) C(4) C(15) C(20) 53.0(2) . . . . yes C(9) C(1) C(2) C(21) 26.6(3) . . . . yes C(9) C(1) C(6) C(36) -93.7(2) . . . . yes C(9) C(1) C(6) H(2) 30(1) . . . . no C(9) C(10) C(11) C(12) -0.3(4) . . . . yes C(9) C(10) C(11) H(4) 179(2) . . . . no C(9) C(14) C(13) C(12) 0.1(4) . . . . yes C(9) C(14) C(13) H(6) 177(2) . . . . no C(10) C(9) C(14) C(13) -0.3(3) . . . . yes C(10) C(9) C(14) H(7) 178(1) . . . . no C(10) C(11) C(12) C(13) 0.0(4) . . . . yes C(10) C(11) C(12) H(5) 176(2) . . . . no C(11) C(10) C(9) C(14) 0.4(3) . . . . yes C(11) C(12) C(13) C(14) 0.1(4) . . . . yes C(11) C(12) C(13) H(6) -176(2) . . . . no C(12) C(11) C(10) H(3) 179(1) . . . . no C(12) C(13) C(14) H(7) -178(1) . . . . no C(13) C(12) C(11) H(4) -179(2) . . . . no C(14) C(9) C(10) H(3) -179(1) . . . . no C(14) C(13) C(12) H(5) -176(2) . . . . no C(15) C(4) C(3) C(32) -31.7(3) . . . . yes C(15) C(4) C(5) C(33) 85.0(2) . . . . yes C(15) C(4) C(5) H(1) -38(1) . . . . no C(15) C(16) C(17) C(18) -1.3(4) . . . . yes C(15) C(16) C(17) H(9) -179(1) . . . . no C(15) C(20) C(19) C(18) -0.8(4) . . . . yes C(15) C(20) C(19) H(11) -178(1) . . . . no C(16) C(15) C(20) C(19) -0.5(3) . . . . yes C(16) C(15) C(20) H(12) 178(1) . . . . no C(16) C(17) C(18) C(19) 0.1(4) . . . . yes C(16) C(17) C(18) H(10) 174(1) . . . . no C(17) C(16) C(15) C(20) 1.5(3) . . . . yes C(17) C(18) C(19) C(20) 0.9(4) . . . . yes C(17) C(18) C(19) H(11) 178(1) . . . . no C(18) C(17) C(16) H(8) 179(1) . . . . no C(18) C(19) C(20) H(12) -179(1) . . . . no C(19) C(18) C(17) H(9) 178(1) . . . . no C(20) C(15) C(16) H(8) -179(1) . . . . no C(20) C(19) C(18) H(10) -173(2) . . . . no C(21) C(2) C(3) C(32) 3.7(3) . . . . yes C(21) C(22) C(23) C(24) -0.3(4) . . . . yes C(21) C(22) C(23) H(14) 177(2) . . . . no C(21) C(26) C(25) C(24) 1.7(3) . . . . yes C(21) C(26) C(25) H(16) -177(1) . . . . no C(21) C(26) C(27) C(28) -174.8(2) . . . . yes C(21) C(26) C(27) C(32) 3.6(3) . . . . yes C(22) C(21) C(26) C(25) -3.3(3) . . . . yes C(22) C(21) C(26) C(27) 174.1(2) . . . . yes C(22) C(23) C(24) C(25) -1.4(4) . . . . yes C(22) C(23) C(24) H(15) 178(2) . . . . no C(23) C(22) C(21) C(26) 2.7(3) . . . . yes C(23) C(24) C(25) C(26) 0.6(4) . . . . yes C(23) C(24) C(25) H(16) -179(1) . . . . no C(24) C(23) C(22) H(13) 179(1) . . . . no C(24) C(25) C(26) C(27) -175.7(2) . . . . yes C(25) C(24) C(23) H(14) -179(1) . . . . no C(25) C(26) C(27) C(28) 2.5(3) . . . . yes C(25) C(26) C(27) C(32) -179.1(2) . . . . yes C(26) C(21) C(22) H(13) -177(1) . . . . no C(26) C(25) C(24) H(15) -179(1) . . . . no C(26) C(27) C(28) C(29) 176.4(2) . . . . yes C(26) C(27) C(28) H(17) -8(1) . . . . no C(26) C(27) C(32) C(31) -175.6(2) . . . . yes C(27) C(26) C(25) H(16) 4(1) . . . . no C(27) C(28) C(29) C(30) -0.6(4) . . . . yes C(27) C(28) C(29) H(18) 179(2) . . . . no C(27) C(32) C(31) C(30) -1.2(3) . . . . yes C(27) C(32) C(31) H(20) 174(1) . . . . no C(28) C(27) C(32) C(31) 2.9(3) . . . . yes C(28) C(29) C(30) C(31) 2.4(4) . . . . yes C(28) C(29) C(30) H(19) -179(1) . . . . no C(29) C(28) C(27) C(32) -2.1(4) . . . . yes C(29) C(30) C(31) C(32) -1.5(4) . . . . yes C(29) C(30) C(31) H(20) -177(2) . . . . no C(30) C(29) C(28) H(17) -175(1) . . . . no C(31) C(30) C(29) H(18) -178(2) . . . . no C(32) C(27) C(28) H(17) 173(1) . . . . no C(32) C(31) C(30) H(19) -179(1) . . . . no C(33) N(35) C(38) C(39) -73.8(3) . . . . yes C(33) N(35) C(38) C(44) 103.4(2) . . . . yes C(33) C(5) C(6) C(36) 6.0(2) . . . . yes C(33) C(5) C(6) H(2) -114(1) . . . . no C(36) N(35) C(38) C(39) 114.0(3) . . . . yes C(36) N(35) C(38) C(44) -68.8(3) . . . . yes C(36) C(6) C(5) H(1) 125(1) . . . . no C(38) C(39) C(40) C(41) -0.7(5) . . . . yes C(38) C(39) C(40) H(22) -179(2) . . . . no C(38) C(44) C(42) C(41) -1.4(4) . . . . yes C(38) C(44) C(42) C(43) 178.3(2) . . . . yes C(39) C(38) C(44) C(42) -0.2(4) . . . . yes C(39) C(38) C(44) H(24) 174(1) . . . . no C(39) C(40) C(41) C(42) -0.9(5) . . . . yes C(39) C(40) C(41) H(23) 177(2) . . . . no C(40) C(39) C(38) C(44) 1.2(4) . . . . yes C(40) C(41) C(42) C(43) -177.7(3) . . . . yes C(40) C(41) C(42) C(44) 1.9(4) . . . . yes C(41) C(40) C(39) H(21) -179(2) . . . . no C(41) C(42) C(43) H(25) -122.3 . . . . no C(41) C(42) C(43) H(26) -0.1 . . . . no C(41) C(42) C(43) H(27) 119.6 . . . . no C(41) C(42) C(44) H(24) -176(1) . . . . no C(42) C(41) C(40) H(22) 178(2) . . . . no C(43) C(42) C(41) H(23) 3(2) . . . . no C(43) C(42) C(44) H(24) 3(1) . . . . no C(44) C(38) C(39) H(21) -179(2) . . . . no C(44) C(42) C(41) H(23) -176(2) . . . . no C(44) C(42) C(43) H(25) 58.0 . . . . no C(44) C(42) C(43) H(26) -179.7 . . . . no C(44) C(42) C(43) H(27) -60.1 . . . . no H(1) C(5) C(6) H(2) 4(1) . . . . no H(3) C(10) C(11) H(4) 0(2) . . . . no H(4) C(11) C(12) H(5) -2(3) . . . . no H(5) C(12) C(13) H(6) 6(3) . . . . no H(6) C(13) C(14) H(7) -1(2) . . . . no H(8) C(16) C(17) H(9) 1(2) . . . . no H(9) C(17) C(18) H(10) -7(2) . . . . no H(10) C(18) C(19) H(11) 4(2) . . . . no H(11) C(19) C(20) H(12) 2(2) . . . . no H(13) C(22) C(23) H(14) -2(2) . . . . no H(14) C(23) C(24) H(15) 0(2) . . . . no H(15) C(24) C(25) H(16) 0(2) . . . . no H(17) C(28) C(29) H(18) 4(2) . . . . no H(18) C(29) C(30) H(19) 0(2) . . . . no H(19) C(30) C(31) H(20) 4(2) . . . . no H(21) C(39) C(40) H(22) 0(3) . . . . no H(22) C(40) C(41) H(23) -3(3) . . . . no C(45) C(46) C(47) C(48) 178.1(3) . . . . yes C(45) C(46) C(47) H(28) -2.9 . . . . no C(45) C(46) C(52) C(51) -176.9(3) . . . . yes C(45) C(46) C(52) H(31) 0.0 . . . . no C(46) C(47) C(48) C(49) -0.6(5) . . . . yes C(46) C(47) C(48) H(29) 179.0 . . . . no C(46) C(52) C(51) C(49) -2.0(5) . . . . yes C(46) C(52) C(51) H(30) -179.3 . . . . no C(47) C(46) C(45) H(32) 118.8 . . . . no C(47) C(46) C(45) H(33) -115.6 . . . . no C(47) C(46) C(45) H(34) 2.3 . . . . no C(47) C(46) C(52) C(51) 1.6(4) . . . . yes C(47) C(46) C(52) H(31) 178.4 . . . . no C(47) C(48) C(49) C(50) -179.5(3) . . . . yes C(47) C(48) C(49) C(51) 0.3(4) . . . . yes C(48) C(47) C(46) C(52) -0.3(4) . . . . yes C(48) C(49) C(50) H(35) 1.3 . . . . no C(48) C(49) C(50) H(36) 120.0 . . . . no C(48) C(49) C(50) H(37) -119.6 . . . . no C(48) C(49) C(51) C(52) 1.0(4) . . . . yes C(48) C(49) C(51) H(30) 178.4 . . . . no C(49) C(48) C(47) H(28) -179.6 . . . . no C(49) C(51) C(52) H(31) -178.8 . . . . no C(50) C(49) C(48) H(29) 0.9 . . . . no C(50) C(49) C(51) C(52) -179.2(3) . . . . yes C(50) C(49) C(51) H(30) -1.8 . . . . no C(51) C(49) C(48) H(29) -179.3 . . . . no C(51) C(49) C(50) H(35) -178.5 . . . . no C(51) C(49) C(50) H(36) -59.8 . . . . no C(51) C(49) C(50) H(37) 60.6 . . . . no C(52) C(46) C(45) H(32) -62.9 . . . . no C(52) C(46) C(45) H(33) 62.7 . . . . no C(52) C(46) C(45) H(34) -179.4 . . . . no C(52) C(46) C(47) H(28) 178.7 . . . . no H(28) C(47) C(48) H(29) 0.0 . . . . no H(30) C(51) C(52) H(31) 3.9 . . . . no H(30) C(51) C(52) H(31) 3.9 . . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(8) C(14) 3.299(3) . 2_665 ? O(8) C(48) 3.343(3) . 2_666 ? O(8) C(9) 3.559(3) . 2_665 ? O(34) C(29) 3.228(3) . 2_655 ? O(34) C(45) 3.518(4) . 1_554 ? O(37) C(18) 3.502(3) . 1_454 ? C(11) C(11) 3.496(5) . 2_565 ? C(11) C(12) 3.529(4) . 2_565 ? C(12) C(16) 3.422(4) . 2_665 ? C(27) C(52) 3.417(4) . . ? C(42) C(42) 3.584(5) . 2_554 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END #------------------------------------------------------------------------------ data_DA_PC_p-MePM_m-Xylene _database_code_CSD 180116 _audit_creation_date 'Sat May 11 20:05:58 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C48 H37 N O3 ' _chemical_formula_moiety '?' _chemical_formula_weight 675.83 _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 14.802(2) _cell_length_b 14.302(2) _cell_length_c 16.739(2) _cell_angle_alpha 90 _cell_angle_beta 94.052(8) _cell_angle_gamma 90 _cell_volume 3534.9(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.8 _cell_measurement_theta_max 20.0 _cell_measurement_temperature 293.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 8768 _diffrn_reflns_av_R_equivalents 0.016 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9991 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.01 #------------------------------------------------------------------------------ # 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 8117 _reflns_number_gt 5390 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.0805 _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 5390 _refine_ls_number_parameters 565 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00422|Fo|^2^]' _refine_ls_shift/su_max 0.0192 _refine_diff_density_max 0.23 _refine_diff_density_min -0.33 _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) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; '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 O(8) O 0.5893(1) -0.06796(9) 0.88974(9) 0.0527(4) Uani 1.00 d . . . O(34) O 0.70395(9) 0.2999(1) 0.9056(1) 0.0607(5) Uani 1.00 d . . . O(36) O 0.40031(9) 0.2622(1) 0.9219(1) 0.0645(5) Uani 1.00 d . . . N(37) N 0.54854(10) 0.3026(1) 0.90718(9) 0.0412(4) Uani 1.00 d . . . C(1) C 0.6511(1) 0.0913(1) 0.8649(1) 0.0393(4) Uani 1.00 d . . . C(2) C 0.6217(1) 0.1577(1) 0.9330(1) 0.0412(5) Uani 1.00 d . . . C(3) C 0.5184(1) 0.1444(1) 0.9343(1) 0.0403(5) Uani 1.00 d . . . C(4) C 0.4921(1) 0.0730(1) 0.8650(1) 0.0376(4) Uani 1.00 d . . . C(5) C 0.5146(1) 0.1199(1) 0.7863(1) 0.0362(4) Uani 1.00 d . . . C(6) C 0.6066(1) 0.1308(1) 0.78672(10) 0.0364(4) Uani 1.00 d . . . C(7) C 0.5797(1) 0.0136(1) 0.8756(1) 0.0395(5) Uani 1.00 d . . . C(9) C 0.4550(1) 0.1507(1) 0.7200(1) 0.0402(4) Uani 1.00 d . . . C(10) C 0.3600(1) 0.1464(1) 0.7194(1) 0.0521(6) Uani 1.00 d . . . C(11) C 0.3063(2) 0.1693(2) 0.6522(2) 0.0653(7) Uani 1.00 d . . . C(12) C 0.3459(2) 0.1975(2) 0.5829(2) 0.0681(7) Uani 1.00 d . . . C(13) C 0.4375(2) 0.2067(2) 0.5828(1) 0.0584(6) Uani 1.00 d . . . C(14) C 0.4951(1) 0.1855(1) 0.6516(1) 0.0436(5) Uani 1.00 d . . . C(15) C 0.6486(1) 0.1765(1) 0.7224(1) 0.0408(5) Uani 1.00 d . . . C(16) C 0.7411(1) 0.2000(2) 0.7259(1) 0.0538(6) Uani 1.00 d . . . C(17) C 0.7778(2) 0.2427(2) 0.6623(2) 0.0663(7) Uani 1.00 d . . . C(18) C 0.7240(2) 0.2602(2) 0.5925(2) 0.0722(8) Uani 1.00 d . . . C(19) C 0.6337(2) 0.2402(2) 0.5881(1) 0.0619(7) Uani 1.00 d . . . C(20) C 0.5924(1) 0.1998(1) 0.6532(1) 0.0435(5) Uani 1.00 d . . . C(21) C 0.7480(1) 0.0579(1) 0.8673(1) 0.0459(5) Uani 1.00 d . . . C(22) C 0.8154(1) 0.0918(2) 0.9212(1) 0.0543(6) Uani 1.00 d . . . C(23) C 0.9034(2) 0.0576(2) 0.9206(2) 0.0690(8) Uani 1.00 d . . . C(24) C 0.9250(2) -0.0090(2) 0.8657(2) 0.0752(8) Uani 1.00 d . . . C(25) C 0.8586(2) -0.0428(2) 0.8118(2) 0.0723(8) Uani 1.00 d . . . C(26) C 0.7705(2) -0.0106(2) 0.8126(1) 0.0575(6) Uani 1.00 d . . . C(27) C 0.4041(1) 0.0207(1) 0.8678(1) 0.0415(5) Uani 1.00 d . . . C(28) C 0.3356(1) 0.0508(2) 0.9147(1) 0.0493(5) Uani 1.00 d . . . C(29) C 0.2523(2) 0.0057(2) 0.9099(2) 0.0608(7) Uani 1.00 d . . . C(30) C 0.2370(2) -0.0700(2) 0.8597(2) 0.0633(7) Uani 1.00 d . . . C(31) C 0.3053(2) -0.1019(2) 0.8149(2) 0.0627(7) Uani 1.00 d . . . C(32) C 0.3884(1) -0.0568(1) 0.8185(1) 0.0514(6) Uani 1.00 d . . . C(33) C 0.6340(1) 0.2599(1) 0.9141(1) 0.0432(5) Uani 1.00 d . . . C(35) C 0.4789(1) 0.2405(1) 0.9208(1) 0.0433(5) Uani 1.00 d . . . C(38) C 0.5339(1) 0.4004(1) 0.8921(1) 0.0421(5) Uani 1.00 d . . . C(39) C 0.5863(1) 0.4667(1) 0.9337(1) 0.0496(5) Uani 1.00 d . . . C(40) C 0.5668(1) 0.5606(2) 0.9222(1) 0.0550(6) Uani 1.00 d . . . C(41) C 0.4953(1) 0.5903(1) 0.8705(1) 0.0525(6) Uani 1.00 d . . . C(42) C 0.4458(2) 0.5225(2) 0.8275(1) 0.0565(6) Uani 1.00 d . . . C(43) C 0.4643(1) 0.4285(2) 0.8373(1) 0.0522(6) Uani 1.00 d . . . C(44) C 0.4708(2) 0.6923(2) 0.8641(2) 0.0713(8) Uani 1.00 d . . . C(45) C 0.4778(2) 0.1187(3) 0.3792(2) 0.091(1) Uani 1.00 d . . . C(46) C 0.5602(2) 0.0769(2) 0.3999(2) 0.0769(9) Uani 1.00 d . . . C(47) C 0.6420(2) 0.1242(2) 0.3983(2) 0.0788(9) Uani 1.00 d . . . C(48) C 0.6421(3) 0.2168(3) 0.3768(2) 0.101(1) Uani 1.00 d . . . C(49) C 0.5615(5) 0.2603(3) 0.3572(2) 0.131(2) Uani 1.00 d . . . C(50) C 0.4804(4) 0.2134(4) 0.3564(2) 0.124(2) Uani 1.00 d . . . C(51) C 0.3918(3) 0.0653(4) 0.3821(3) 0.147(2) Uani 1.00 d . . . C(52) C 0.7287(2) 0.0749(3) 0.4225(3) 0.114(1) Uani 1.00 d . . . H(1) H 0.651(2) 0.139(2) 0.985(2) 0.064(6) Uiso 1.00 calc . . . H(2) H 0.502(1) 0.118(1) 0.985(1) 0.042(5) Uiso 1.00 calc . . . H(3) H 0.333(1) 0.128(2) 0.767(1) 0.052(6) Uiso 1.00 calc . . . H(4) H 0.240(2) 0.168(2) 0.655(2) 0.074(7) Uiso 1.00 calc . . . H(5) H 0.312(2) 0.213(2) 0.540(2) 0.083(8) Uiso 1.00 calc . . . H(6) H 0.465(1) 0.231(2) 0.534(1) 0.057(6) Uiso 1.00 calc . . . H(7) H 0.778(2) 0.190(2) 0.776(2) 0.071(7) Uiso 1.00 calc . . . H(8) H 0.841(2) 0.261(2) 0.669(2) 0.096(9) Uiso 1.00 calc . . . H(9) H 0.747(2) 0.294(2) 0.545(2) 0.097(9) Uiso 1.00 calc . . . H(10) H 0.598(2) 0.255(2) 0.540(2) 0.075(7) Uiso 1.00 calc . . . H(11) H 0.801(2) 0.139(2) 0.959(1) 0.059(6) Uiso 1.00 calc . . . H(12) H 0.950(2) 0.079(2) 0.960(2) 0.094(9) Uiso 1.00 calc . . . H(13) H 0.989(2) -0.030(2) 0.856(2) 0.077(8) Uiso 1.00 calc . . . H(14) H 0.870(2) -0.095(2) 0.779(2) 0.082(8) Uiso 1.00 calc . . . H(15) H 0.726(2) -0.033(2) 0.775(2) 0.070(7) Uiso 1.00 calc . . . H(16) H 0.350(2) 0.105(2) 0.952(2) 0.076(7) Uiso 1.00 calc . . . H(17) H 0.204(2) 0.023(2) 0.942(2) 0.071(7) Uiso 1.00 calc . . . H(18) H 0.182(2) -0.103(2) 0.853(2) 0.078(8) Uiso 1.00 calc . . . H(19) H 0.295(2) -0.158(2) 0.775(2) 0.063(6) Uiso 1.00 calc . . . H(20) H 0.437(2) -0.079(2) 0.783(2) 0.065(7) Uiso 1.00 calc . . . H(21) H 0.637(2) 0.445(2) 0.974(2) 0.072(7) Uiso 1.00 calc . . . H(22) H 0.601(2) 0.608(2) 0.952(1) 0.059(6) Uiso 1.00 calc . . . H(23) H 0.397(2) 0.537(2) 0.789(2) 0.091(8) Uiso 1.00 calc . . . H(24) H 0.432(1) 0.381(2) 0.808(1) 0.054(6) Uiso 1.00 calc . . . H(25) H 0.5208 0.7296 0.8487 0.0858 Uiso 1.00 calc . . . H(26) H 0.4205 0.7032 0.8264 0.0858 Uiso 1.00 calc . . . H(27) H 0.4544 0.7163 0.9155 0.0858 Uiso 1.00 calc . . . H(28) H 0.5623 0.0099 0.4164 0.0931 Uiso 1.00 calc . . . H(29) H 0.6974 0.2528 0.3755 0.1220 Uiso 1.00 calc . . . H(30) H 0.5560 0.3266 0.3390 0.1646 Uiso 1.00 calc . . . H(31) H 0.4173 0.2427 0.3419 0.1502 Uiso 1.00 calc . . . H(32) H 0.3377 0.0984 0.3696 0.1536 Uiso 1.00 calc . . . H(33) H 0.3909 0.0091 0.3490 0.1536 Uiso 1.00 calc . . . H(34) H 0.3852 0.0389 0.4377 0.1536 Uiso 1.00 calc . . . H(35) H 0.7301 0.0526 0.4784 0.1275 Uiso 1.00 calc . . . H(36) H 0.7391 0.0216 0.3906 0.1275 Uiso 1.00 calc . . . H(37) H 0.7815 0.1153 0.4211 0.1275 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 O(8) 0.0544(8) 0.0415(7) 0.0627(9) 0.0043(6) 0.0064(6) 0.0067(6) O(34) 0.0356(7) 0.0561(9) 0.090(1) -0.0064(6) -0.0005(7) -0.0052(8) O(36) 0.0400(8) 0.0490(8) 0.107(1) 0.0010(6) 0.0198(8) -0.0048(8) N(37) 0.0360(7) 0.0426(8) 0.0451(8) -0.0017(6) 0.0037(6) -0.0036(6) C(1) 0.0390(9) 0.0414(9) 0.0376(9) 0.0028(7) 0.0023(7) 0.0007(7) C(2) 0.0392(9) 0.0489(10) 0.0351(8) 0.0017(7) -0.0015(7) -0.0009(7) C(3) 0.0427(9) 0.0434(9) 0.0356(9) -0.0012(7) 0.0083(7) -0.0014(7) C(4) 0.0400(9) 0.0364(8) 0.0370(9) 0.0004(7) 0.0081(7) 0.0002(7) C(5) 0.0377(8) 0.0365(8) 0.0346(8) -0.0009(6) 0.0046(6) 0.0002(6) C(6) 0.0361(8) 0.0389(9) 0.0344(8) 0.0001(7) 0.0034(6) -0.0014(7) C(7) 0.0427(9) 0.0430(10) 0.0330(8) 0.0013(7) 0.0049(7) 0.0000(7) C(9) 0.0413(9) 0.0367(8) 0.0419(9) 0.0005(7) -0.0010(7) -0.0011(7) C(10) 0.043(1) 0.050(1) 0.063(1) 0.0009(8) -0.0018(9) 0.0083(9) C(11) 0.046(1) 0.062(1) 0.085(2) 0.0028(10) -0.016(1) 0.013(1) C(12) 0.068(1) 0.066(1) 0.067(2) 0.003(1) -0.025(1) 0.013(1) C(13) 0.073(1) 0.056(1) 0.045(1) 0.001(1) -0.005(1) 0.0086(9) C(14) 0.053(1) 0.0387(9) 0.0389(9) 0.0019(8) 0.0001(8) -0.0022(7) C(15) 0.0431(9) 0.0402(9) 0.0401(9) 0.0009(7) 0.0097(7) -0.0002(7) C(16) 0.043(1) 0.058(1) 0.061(1) -0.0041(9) 0.0115(9) 0.0076(10) C(17) 0.053(1) 0.070(1) 0.079(2) -0.004(1) 0.026(1) 0.011(1) C(18) 0.078(2) 0.080(2) 0.062(1) -0.004(1) 0.032(1) 0.018(1) C(19) 0.073(2) 0.071(1) 0.043(1) 0.000(1) 0.015(1) 0.011(1) C(20) 0.053(1) 0.0405(9) 0.0377(9) 0.0012(8) 0.0096(8) 0.0002(7) C(21) 0.0403(9) 0.050(1) 0.047(1) 0.0053(8) 0.0054(8) 0.0091(8) C(22) 0.041(1) 0.063(1) 0.058(1) 0.0010(9) -0.0001(9) 0.004(1) C(23) 0.040(1) 0.087(2) 0.079(2) 0.002(1) -0.002(1) 0.015(1) C(24) 0.044(1) 0.082(2) 0.101(2) 0.017(1) 0.013(1) 0.016(2) C(25) 0.058(1) 0.072(2) 0.088(2) 0.017(1) 0.021(1) 0.001(1) C(26) 0.050(1) 0.061(1) 0.062(1) 0.009(1) 0.0090(10) -0.003(1) C(27) 0.0399(9) 0.0413(9) 0.0436(9) -0.0021(7) 0.0062(7) 0.0059(7) C(28) 0.045(1) 0.051(1) 0.054(1) -0.0030(8) 0.0145(8) 0.0026(9) C(29) 0.047(1) 0.063(1) 0.074(1) -0.0030(10) 0.019(1) 0.013(1) C(30) 0.045(1) 0.067(1) 0.077(2) -0.015(1) 0.006(1) 0.011(1) C(31) 0.061(1) 0.052(1) 0.074(2) -0.016(1) 0.002(1) -0.003(1) C(32) 0.049(1) 0.049(1) 0.057(1) -0.0051(9) 0.0066(9) -0.0020(9) C(33) 0.0377(9) 0.0482(10) 0.0429(10) -0.0023(8) -0.0018(7) -0.0056(8) C(35) 0.0395(9) 0.0432(9) 0.0479(10) -0.0019(7) 0.0090(7) -0.0065(8) C(38) 0.0400(9) 0.0424(9) 0.0441(10) -0.0014(7) 0.0052(7) -0.0021(7) C(39) 0.045(1) 0.048(1) 0.055(1) -0.0030(8) -0.0015(9) -0.0029(9) C(40) 0.051(1) 0.047(1) 0.066(1) -0.0076(9) 0.0026(10) -0.0055(10) C(41) 0.051(1) 0.048(1) 0.060(1) -0.0004(9) 0.0139(9) 0.0070(9) C(42) 0.049(1) 0.059(1) 0.061(1) 0.0026(9) -0.0006(10) 0.007(1) C(43) 0.049(1) 0.053(1) 0.054(1) -0.0036(9) -0.0043(9) -0.0008(9) C(44) 0.071(2) 0.052(1) 0.091(2) 0.004(1) 0.008(1) 0.009(1) C(45) 0.085(2) 0.117(3) 0.067(2) 0.042(2) -0.021(1) -0.043(2) C(46) 0.071(2) 0.079(2) 0.078(2) 0.021(1) -0.018(1) -0.028(1) C(47) 0.085(2) 0.079(2) 0.072(2) 0.004(1) 0.005(1) -0.019(1) C(48) 0.156(3) 0.082(2) 0.069(2) 0.009(2) 0.032(2) -0.006(2) C(49) 0.224(6) 0.109(3) 0.060(2) 0.049(4) 0.009(3) 0.009(2) C(50) 0.160(4) 0.140(4) 0.066(2) 0.091(3) -0.027(2) -0.024(2) C(51) 0.074(2) 0.187(4) 0.173(4) 0.043(3) -0.038(2) -0.103(4) C(52) 0.066(2) 0.100(2) 0.176(4) -0.004(2) -0.001(2) -0.025(2) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SAPI91 _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 O(8) C(7) 1.197(2) . . yes O(34) C(33) 1.200(2) . . yes O(36) C(35) 1.205(2) . . yes N(37) C(33) 1.403(2) . . yes N(37) C(35) 1.393(2) . . yes N(37) C(38) 1.435(2) . . yes C(1) C(2) 1.569(3) . . yes C(1) C(6) 1.531(2) . . yes C(1) C(7) 1.553(3) . . yes C(1) C(21) 1.510(2) . . yes C(2) C(3) 1.542(3) . . yes C(2) C(33) 1.508(3) . . yes C(3) C(4) 1.573(2) . . yes C(3) C(35) 1.505(3) . . yes C(4) C(5) 1.536(2) . . yes C(4) C(7) 1.549(2) . . yes C(4) C(27) 1.506(2) . . yes C(5) C(6) 1.370(2) . . yes C(5) C(9) 1.438(2) . . yes C(6) C(15) 1.438(2) . . yes C(9) C(10) 1.407(3) . . yes C(9) C(14) 1.416(3) . . yes C(10) C(11) 1.371(3) . . yes C(11) C(12) 1.396(4) . . yes C(12) C(13) 1.361(4) . . yes C(13) C(14) 1.417(3) . . yes C(14) C(20) 1.454(3) . . yes C(15) C(16) 1.408(3) . . yes C(15) C(20) 1.416(3) . . yes C(16) C(17) 1.372(3) . . yes C(17) C(18) 1.390(4) . . yes C(18) C(19) 1.364(4) . . yes C(19) C(20) 1.411(3) . . yes C(21) C(22) 1.384(3) . . yes C(21) C(26) 1.397(3) . . yes C(22) C(23) 1.391(3) . . yes C(23) C(24) 1.378(4) . . yes C(24) C(25) 1.375(4) . . yes C(25) C(26) 1.384(3) . . yes C(27) C(28) 1.394(3) . . yes C(27) C(32) 1.391(3) . . yes C(28) C(29) 1.389(3) . . yes C(29) C(30) 1.378(4) . . yes C(30) C(31) 1.378(4) . . yes C(31) C(32) 1.387(3) . . yes C(38) C(39) 1.381(3) . . yes C(38) C(43) 1.390(3) . . yes C(39) C(40) 1.385(3) . . yes C(40) C(41) 1.386(3) . . yes C(41) C(42) 1.385(3) . . yes C(41) C(44) 1.505(3) . . yes C(42) C(43) 1.380(3) . . yes C(45) C(46) 1.381(4) . . yes C(45) C(50) 1.408(7) . . yes C(45) C(51) 1.488(6) . . yes C(46) C(47) 1.389(4) . . yes C(47) C(48) 1.372(5) . . yes C(47) C(52) 1.495(4) . . yes C(48) C(49) 1.364(6) . . yes C(49) C(50) 1.375(7) . . 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(33) N(37) C(35) 112.5(2) . . . yes C(33) N(37) C(38) 124.3(1) . . . yes C(35) N(37) C(38) 123.1(1) . . . yes C(2) C(1) C(6) 105.8(1) . . . yes C(2) C(1) C(7) 97.1(1) . . . yes C(2) C(1) C(21) 119.0(2) . . . yes C(6) C(1) C(7) 96.2(1) . . . yes C(6) C(1) C(21) 119.3(1) . . . yes C(7) C(1) C(21) 115.1(1) . . . yes C(1) C(2) C(3) 105.2(1) . . . yes C(1) C(2) C(33) 113.0(1) . . . yes C(3) C(2) C(33) 104.9(1) . . . yes C(2) C(3) C(4) 105.3(1) . . . yes C(2) C(3) C(35) 105.1(1) . . . yes C(4) C(3) C(35) 114.1(1) . . . yes C(3) C(4) C(5) 106.9(1) . . . yes C(3) C(4) C(7) 96.3(1) . . . yes C(3) C(4) C(27) 118.0(1) . . . yes C(5) C(4) C(7) 96.1(1) . . . yes C(5) C(4) C(27) 118.9(1) . . . yes C(7) C(4) C(27) 116.3(1) . . . yes C(4) C(5) C(6) 108.8(1) . . . yes C(4) C(5) C(9) 129.6(2) . . . yes C(6) C(5) C(9) 121.6(2) . . . yes C(1) C(6) C(5) 109.2(1) . . . yes C(1) C(6) C(15) 128.7(2) . . . yes C(5) C(6) C(15) 122.0(2) . . . yes O(8) C(7) C(1) 130.4(2) . . . yes O(8) C(7) C(4) 130.0(2) . . . yes C(1) C(7) C(4) 99.6(1) . . . yes C(5) C(9) C(10) 123.4(2) . . . yes C(5) C(9) C(14) 117.6(2) . . . yes C(10) C(9) C(14) 119.0(2) . . . yes C(9) C(10) C(11) 121.1(2) . . . yes C(10) C(11) C(12) 119.9(2) . . . yes C(11) C(12) C(13) 120.4(2) . . . yes C(12) C(13) C(14) 121.4(2) . . . yes C(9) C(14) C(13) 118.1(2) . . . yes C(9) C(14) C(20) 120.4(2) . . . yes C(13) C(14) C(20) 121.6(2) . . . yes C(6) C(15) C(16) 123.2(2) . . . yes C(6) C(15) C(20) 117.4(2) . . . yes C(16) C(15) C(20) 119.4(2) . . . yes C(15) C(16) C(17) 120.7(2) . . . yes C(16) C(17) C(18) 119.9(2) . . . yes C(17) C(18) C(19) 120.6(2) . . . yes C(18) C(19) C(20) 121.4(2) . . . yes C(14) C(20) C(15) 120.4(2) . . . yes C(14) C(20) C(19) 121.8(2) . . . yes C(15) C(20) C(19) 117.8(2) . . . yes C(1) C(21) C(22) 123.1(2) . . . yes C(1) C(21) C(26) 118.3(2) . . . yes C(22) C(21) C(26) 118.6(2) . . . yes C(21) C(22) C(23) 120.3(2) . . . yes C(22) C(23) C(24) 120.6(2) . . . yes C(23) C(24) C(25) 119.4(2) . . . yes C(24) C(25) C(26) 120.5(3) . . . yes C(21) C(26) C(25) 120.5(2) . . . yes C(4) C(27) C(28) 122.0(2) . . . yes C(4) C(27) C(32) 119.1(2) . . . yes C(28) C(27) C(32) 118.8(2) . . . yes C(27) C(28) C(29) 120.2(2) . . . yes C(28) C(29) C(30) 120.4(2) . . . yes C(29) C(30) C(31) 119.8(2) . . . yes C(30) C(31) C(32) 120.3(2) . . . yes C(27) C(32) C(31) 120.5(2) . . . yes O(34) C(33) N(37) 124.3(2) . . . yes O(34) C(33) C(2) 127.2(2) . . . yes N(37) C(33) C(2) 108.6(1) . . . yes O(36) C(35) N(37) 124.4(2) . . . yes O(36) C(35) C(3) 126.8(2) . . . yes N(37) C(35) C(3) 108.8(1) . . . yes N(37) C(38) C(39) 120.5(2) . . . yes N(37) C(38) C(43) 119.5(2) . . . yes C(39) C(38) C(43) 119.9(2) . . . yes C(38) C(39) C(40) 119.4(2) . . . yes C(39) C(40) C(41) 121.7(2) . . . yes C(40) C(41) C(42) 117.6(2) . . . yes C(40) C(41) C(44) 120.7(2) . . . yes C(42) C(41) C(44) 121.7(2) . . . yes C(41) C(42) C(43) 121.8(2) . . . yes C(38) C(43) C(42) 119.4(2) . . . yes C(46) C(45) C(50) 116.4(4) . . . yes C(46) C(45) C(51) 120.8(4) . . . yes C(50) C(45) C(51) 122.9(4) . . . yes C(45) C(46) C(47) 122.6(3) . . . yes C(46) C(47) C(48) 119.5(3) . . . yes C(46) C(47) C(52) 119.9(3) . . . yes C(48) C(47) C(52) 120.6(3) . . . yes C(47) C(48) C(49) 119.1(4) . . . yes C(48) C(49) C(50) 121.9(4) . . . yes C(45) C(50) C(49) 120.5(4) . . . 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 O(8) C(7) C(1) C(2) -122.1(2) . . . . yes O(8) C(7) C(1) C(6) 131.1(2) . . . . yes O(8) C(7) C(1) C(21) 4.6(3) . . . . yes O(8) C(7) C(4) C(3) 121.4(2) . . . . yes O(8) C(7) C(4) C(5) -130.8(2) . . . . yes O(8) C(7) C(4) C(27) -4.2(3) . . . . yes O(34) C(33) N(37) C(35) -179.3(2) . . . . yes O(34) C(33) N(37) C(38) -2.5(3) . . . . yes O(34) C(33) C(2) C(1) -64.2(2) . . . . yes O(34) C(33) C(2) C(3) -178.2(2) . . . . yes O(34) C(33) C(2) H(1) 62(1) . . . . no O(36) C(35) N(37) C(33) 176.2(2) . . . . yes O(36) C(35) N(37) C(38) -0.6(3) . . . . yes O(36) C(35) C(3) C(2) -175.5(2) . . . . yes O(36) C(35) C(3) C(4) 69.6(3) . . . . yes O(36) C(35) C(3) H(2) -54(1) . . . . no N(37) C(33) C(2) C(1) 115.4(2) . . . . yes N(37) C(33) C(2) C(3) 1.4(2) . . . . yes N(37) C(33) C(2) H(1) -117(1) . . . . no N(37) C(35) C(3) C(2) 3.8(2) . . . . yes N(37) C(35) C(3) C(4) -111.0(2) . . . . yes N(37) C(35) C(3) H(2) 124(1) . . . . no N(37) C(38) C(39) C(40) -175.6(2) . . . . yes N(37) C(38) C(39) H(21) 2(1) . . . . no N(37) C(38) C(43) C(42) 175.0(2) . . . . yes N(37) C(38) C(43) H(24) -5(1) . . . . no C(1) C(2) C(3) C(4) -1.7(2) . . . . yes C(1) C(2) C(3) C(35) -122.5(1) . . . . yes C(1) C(2) C(3) H(2) 116(1) . . . . no C(1) C(6) C(5) C(4) 0.6(2) . . . . yes C(1) C(6) C(5) C(9) 180.0 . . . . yes C(1) C(6) C(15) C(16) -6.3(3) . . . . yes C(1) C(6) C(15) C(20) 174.9(2) . . . . yes C(1) C(7) C(4) C(3) -57.0(1) . . . . yes C(1) C(7) C(4) C(5) 50.8(1) . . . . yes C(1) C(7) C(4) C(27) 177.4(1) . . . . yes C(1) C(21) C(22) C(23) 179.5(2) . . . . yes C(1) C(21) C(22) H(11) 0(1) . . . . no C(1) C(21) C(26) C(25) 179.3(2) . . . . yes C(1) C(21) C(26) H(15) 1(1) . . . . no C(2) C(1) C(6) C(5) -67.8(2) . . . . yes C(2) C(1) C(6) C(15) 109.9(2) . . . . yes C(2) C(1) C(7) C(4) 56.3(1) . . . . yes C(2) C(1) C(21) C(22) -8.1(3) . . . . yes C(2) C(1) C(21) C(26) 171.7(2) . . . . yes C(2) C(3) C(4) C(5) -63.0(2) . . . . yes C(2) C(3) C(4) C(7) 35.3(2) . . . . yes C(2) C(3) C(4) C(27) 159.7(2) . . . . yes C(2) C(33) N(37) C(35) 1.0(2) . . . . yes C(2) C(33) N(37) C(38) 177.8(2) . . . . yes C(3) C(2) C(1) C(6) 65.8(2) . . . . yes C(3) C(2) C(1) C(7) -32.7(2) . . . . yes C(3) C(2) C(1) C(21) -156.5(2) . . . . yes C(3) C(4) C(5) C(6) 66.2(2) . . . . yes C(3) C(4) C(5) C(9) -113.2(2) . . . . yes C(3) C(4) C(27) C(28) 18.1(3) . . . . yes C(3) C(4) C(27) C(32) -165.9(2) . . . . yes C(3) C(35) N(37) C(33) -3.1(2) . . . . yes C(3) C(35) N(37) C(38) -180.0(2) . . . . yes C(4) C(3) C(2) C(33) 117.7(2) . . . . yes C(4) C(3) C(2) H(1) -120(1) . . . . no C(4) C(5) C(6) C(15) -177.3(2) . . . . yes C(4) C(5) C(9) C(10) 3.6(3) . . . . yes C(4) C(5) C(9) C(14) -175.1(2) . . . . yes C(4) C(7) C(1) C(6) -50.5(1) . . . . yes C(4) C(7) C(1) C(21) -177.0(1) . . . . yes C(4) C(27) C(28) C(29) 174.0(2) . . . . yes C(4) C(27) C(28) H(16) -7(1) . . . . no C(4) C(27) C(32) C(31) -174.8(2) . . . . yes C(4) C(27) C(32) H(20) 2(1) . . . . no C(5) C(4) C(3) C(35) 51.7(2) . . . . yes C(5) C(4) C(3) H(2) 176(1) . . . . no C(5) C(4) C(27) C(28) -114.1(2) . . . . yes C(5) C(4) C(27) C(32) 62.0(2) . . . . yes C(5) C(6) C(1) C(7) 31.4(2) . . . . yes C(5) C(6) C(1) C(21) 154.8(2) . . . . yes C(5) C(6) C(15) C(16) 171.1(2) . . . . yes C(5) C(6) C(15) C(20) -7.7(3) . . . . yes C(5) C(9) C(10) C(11) -174.4(2) . . . . yes C(5) C(9) C(10) H(3) 6(1) . . . . no C(5) C(9) C(14) C(13) 173.4(2) . . . . yes C(5) C(9) C(14) C(20) -7.5(3) . . . . yes C(6) C(1) C(2) C(33) -48.0(2) . . . . yes C(6) C(1) C(2) H(1) -176(1) . . . . no C(6) C(1) C(21) C(22) 123.9(2) . . . . yes C(6) C(1) C(21) C(26) -56.3(2) . . . . yes C(6) C(5) C(4) C(7) -32.4(2) . . . . yes C(6) C(5) C(4) C(27) -157.0(2) . . . . yes C(6) C(5) C(9) C(10) -175.7(2) . . . . yes C(6) C(5) C(9) C(14) 5.5(3) . . . . yes C(6) C(15) C(16) C(17) 179.3(2) . . . . yes C(6) C(15) C(16) H(7) -5(1) . . . . no C(6) C(15) C(20) C(14) 5.5(3) . . . . yes C(6) C(15) C(20) C(19) -176.8(2) . . . . yes C(7) C(1) C(2) C(33) -146.5(1) . . . . yes C(7) C(1) C(2) H(1) 85(1) . . . . no C(7) C(1) C(6) C(15) -150.9(2) . . . . yes C(7) C(1) C(21) C(22) -122.6(2) . . . . yes C(7) C(1) C(21) C(26) 57.2(2) . . . . yes C(7) C(4) C(3) C(35) 150.1(1) . . . . yes C(7) C(4) C(3) H(2) -84(1) . . . . no C(7) C(4) C(5) C(9) 148.3(2) . . . . yes C(7) C(4) C(27) C(28) 131.8(2) . . . . yes C(7) C(4) C(27) C(32) -52.1(2) . . . . yes C(9) C(5) C(4) C(27) 23.6(3) . . . . yes C(9) C(5) C(6) C(15) 2.1(3) . . . . yes C(9) C(10) C(11) C(12) 0.0(4) . . . . yes C(9) C(10) C(11) H(4) -177(1) . . . . no C(9) C(14) C(13) C(12) 2.4(3) . . . . yes C(9) C(14) C(13) H(6) -179(1) . . . . no C(9) C(14) C(20) C(15) 2.0(3) . . . . yes C(9) C(14) C(20) C(19) -175.6(2) . . . . yes C(10) C(9) C(14) C(13) -5.5(3) . . . . yes C(10) C(9) C(14) C(20) 173.7(2) . . . . yes C(10) C(11) C(12) C(13) -3.1(4) . . . . yes C(10) C(11) C(12) H(5) -179(2) . . . . no C(11) C(10) C(9) C(14) 4.4(3) . . . . yes C(11) C(12) C(13) C(14) 1.9(4) . . . . yes C(11) C(12) C(13) H(6) -175(1) . . . . no C(12) C(11) C(10) H(3) 178(1) . . . . no C(12) C(13) C(14) C(20) -176.7(2) . . . . yes C(13) C(12) C(11) H(4) 174(1) . . . . no C(13) C(14) C(20) C(15) -178.9(2) . . . . yes C(13) C(14) C(20) C(19) 3.5(3) . . . . yes C(14) C(9) C(10) H(3) -174(1) . . . . no C(14) C(13) C(12) H(5) 178(2) . . . . no C(14) C(20) C(15) C(16) -173.3(2) . . . . yes C(14) C(20) C(19) C(18) 174.8(2) . . . . yes C(14) C(20) C(19) H(10) -4(1) . . . . no C(15) C(6) C(1) C(21) -27.5(3) . . . . yes C(15) C(16) C(17) C(18) -2.1(4) . . . . yes C(15) C(16) C(17) H(8) 176(2) . . . . no C(15) C(20) C(19) C(18) -2.9(3) . . . . yes C(15) C(20) C(19) H(10) 178(1) . . . . no C(16) C(15) C(20) C(19) 4.4(3) . . . . yes C(16) C(17) C(18) C(19) 3.7(4) . . . . yes C(16) C(17) C(18) H(9) 176(2) . . . . no C(17) C(16) C(15) C(20) -2.0(3) . . . . yes C(17) C(18) C(19) C(20) -1.2(4) . . . . yes C(17) C(18) C(19) H(10) 177(1) . . . . no C(18) C(17) C(16) H(7) -177(1) . . . . no C(19) C(18) C(17) H(8) -175(2) . . . . no C(20) C(14) C(13) H(6) 1(1) . . . . no C(20) C(15) C(16) H(7) 173(1) . . . . no C(20) C(19) C(18) H(9) -174(2) . . . . no C(21) C(1) C(2) C(33) 89.6(2) . . . . yes C(21) C(1) C(2) H(1) -38(1) . . . . no C(21) C(22) C(23) C(24) 1.2(4) . . . . yes C(21) C(22) C(23) H(12) -176(2) . . . . no C(21) C(26) C(25) C(24) 1.1(4) . . . . yes C(21) C(26) C(25) H(14) 171(2) . . . . no C(22) C(21) C(26) C(25) -0.9(3) . . . . yes C(22) C(21) C(26) H(15) -178(1) . . . . no C(22) C(23) C(24) C(25) -1.0(4) . . . . yes C(22) C(23) C(24) H(13) 170(1) . . . . no C(23) C(22) C(21) C(26) -0.3(3) . . . . yes C(23) C(24) C(25) C(26) -0.2(4) . . . . yes C(23) C(24) C(25) H(14) -170(2) . . . . no C(24) C(23) C(22) H(11) -178(1) . . . . no C(24) C(25) C(26) H(15) 178(1) . . . . no C(25) C(24) C(23) H(12) 177(2) . . . . no C(26) C(21) C(22) H(11) 179(1) . . . . no C(26) C(25) C(24) H(13) -172(1) . . . . no C(27) C(4) C(3) C(35) -85.6(2) . . . . yes C(27) C(4) C(3) H(2) 39(1) . . . . no C(27) C(28) C(29) C(30) 1.0(3) . . . . yes C(27) C(28) C(29) H(17) 178(1) . . . . no C(27) C(32) C(31) C(30) 0.5(4) . . . . yes C(27) C(32) C(31) H(19) 177(1) . . . . no C(28) C(27) C(32) C(31) 1.3(3) . . . . yes C(28) C(27) C(32) H(20) 178(1) . . . . no C(28) C(29) C(30) C(31) 0.9(4) . . . . yes C(28) C(29) C(30) H(18) -179(2) . . . . no C(29) C(28) C(27) C(32) -2.1(3) . . . . yes C(29) C(30) C(31) C(32) -1.7(4) . . . . yes C(29) C(30) C(31) H(19) -178(1) . . . . no C(30) C(29) C(28) H(16) -177(1) . . . . no C(30) C(31) C(32) H(20) -176(1) . . . . no C(31) C(30) C(29) H(17) -177(1) . . . . no C(32) C(27) C(28) H(16) 176(1) . . . . no C(32) C(31) C(30) H(18) 178(1) . . . . no C(33) N(37) C(38) C(39) -45.4(3) . . . . yes C(33) N(37) C(38) C(43) 136.9(2) . . . . yes C(33) C(2) C(3) C(35) -3.1(2) . . . . yes C(33) C(2) C(3) H(2) -123(1) . . . . no C(35) N(37) C(38) C(39) 131.1(2) . . . . yes C(35) N(37) C(38) C(43) -46.6(3) . . . . yes C(35) C(3) C(2) H(1) 118(1) . . . . no C(38) C(39) C(40) C(41) 0.7(3) . . . . yes C(38) C(39) C(40) H(22) 177(1) . . . . no C(38) C(43) C(42) C(41) 0.5(4) . . . . yes C(38) C(43) C(42) H(23) -179(2) . . . . no C(39) C(38) C(43) C(42) -2.8(3) . . . . yes C(39) C(38) C(43) H(24) 176(1) . . . . no C(39) C(40) C(41) C(42) -2.9(3) . . . . yes C(39) C(40) C(41) C(44) 175.0(2) . . . . yes C(40) C(39) C(38) C(43) 2.2(3) . . . . yes C(40) C(41) C(42) C(43) 2.3(3) . . . . yes C(40) C(41) C(42) H(23) -177(2) . . . . no C(40) C(41) C(44) H(25) 58.2 . . . . no C(40) C(41) C(44) H(26) 179.9 . . . . no C(40) C(41) C(44) H(27) -60.4 . . . . no C(41) C(40) C(39) H(21) -177(1) . . . . no C(41) C(42) C(43) H(24) -178(1) . . . . no C(42) C(41) C(40) H(22) -179(1) . . . . no C(42) C(41) C(44) H(25) -124.1 . . . . no C(42) C(41) C(44) H(26) -2.4 . . . . no C(42) C(41) C(44) H(27) 117.3 . . . . no C(43) C(38) C(39) H(21) 180.0 . . . . no C(43) C(42) C(41) C(44) -175.5(2) . . . . yes C(44) C(41) C(40) H(22) -1(1) . . . . no C(44) C(41) C(42) H(23) 4(2) . . . . no C(45) C(46) C(47) C(48) 1.3(4) . . . . yes C(45) C(46) C(47) C(52) 179.2(3) . . . . yes C(45) C(50) C(49) C(48) 2.5(6) . . . . yes C(45) C(50) C(49) H(30) 179.0 . . . . no C(46) C(45) C(50) C(49) -1.5(5) . . . . yes C(46) C(45) C(50) H(31) -179.4 . . . . no C(46) C(45) C(51) H(32) 177.3 . . . . no C(46) C(45) C(51) H(33) -56.8 . . . . no C(46) C(45) C(51) H(34) 57.2 . . . . no C(46) C(47) C(48) C(49) -0.4(5) . . . . yes C(46) C(47) C(48) H(29) 179.3 . . . . no C(46) C(47) C(52) H(35) -60.3 . . . . no C(46) C(47) C(52) H(36) 59.8 . . . . no C(46) C(47) C(52) H(37) -177.6 . . . . no C(47) C(46) C(45) C(50) -0.3(4) . . . . yes C(47) C(46) C(45) C(51) -179.9(3) . . . . yes C(47) C(48) C(49) C(50) -1.5(6) . . . . yes C(47) C(48) C(49) H(30) -177.6 . . . . no C(48) C(47) C(46) H(28) -179.2 . . . . no C(48) C(47) C(52) H(35) 117.6 . . . . no C(48) C(47) C(52) H(36) -122.4 . . . . no C(48) C(47) C(52) H(37) 0.3 . . . . no C(48) C(49) C(50) H(31) -179.9 . . . . no C(49) C(48) C(47) C(52) -178.2(3) . . . . yes C(49) C(50) C(45) C(51) 178.0(3) . . . . yes C(50) C(45) C(46) H(28) -179.8 . . . . no C(50) C(45) C(51) H(32) -2.2 . . . . no C(50) C(45) C(51) H(33) 123.7 . . . . no C(50) C(45) C(51) H(34) -122.3 . . . . no C(50) C(49) C(48) H(29) 178.9 . . . . no C(51) C(45) C(46) H(28) 0.7 . . . . no C(51) C(45) C(50) H(31) 0.1 . . . . no C(52) C(47) C(46) H(28) -1.3 . . . . no C(52) C(47) C(48) H(29) 1.4 . . . . no H(1) C(2) C(3) H(2) -2(1) . . . . no H(3) C(10) C(11) H(4) 1(2) . . . . no H(4) C(11) C(12) H(5) -2(2) . . . . no H(5) C(12) C(13) H(6) 0(2) . . . . no H(7) C(16) C(17) H(8) 1(2) . . . . no H(8) C(17) C(18) H(9) -2(3) . . . . no H(9) C(18) C(19) H(10) 4(2) . . . . no H(11) C(22) C(23) H(12) 3(2) . . . . no H(12) C(23) C(24) H(13) -11(2) . . . . no H(13) C(24) C(25) H(14) 17(2) . . . . no H(14) C(25) C(26) H(15) -10(2) . . . . no H(16) C(28) C(29) H(17) 0(2) . . . . no H(17) C(29) C(30) H(18) 3(2) . . . . no H(18) C(30) C(31) H(19) 1(2) . . . . no H(19) C(31) C(32) H(20) 0(2) . . . . no H(21) C(39) C(40) H(22) 0(2) . . . . no H(23) C(42) C(43) H(24) 1(2) . . . . no H(29) C(48) C(49) H(30) 2.7 . . . . no H(30) C(49) C(50) H(31) -3.4 . . . . no H(30) C(49) C(50) H(31) -3.4 . . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(8) C(28) 3.391(3) . 3_657 ? O(8) C(17) 3.494(3) . 2_646 ? O(34) C(51) 3.429(4) . 4_555 ? O(34) C(12) 3.513(3) . 4_555 ? O(36) C(52) 3.447(4) . 4_455 ? C(18) C(25) 3.504(4) . 2_656 ? C(19) C(25) 3.525(4) . 2_656 ? C(19) C(48) 3.563(4) . . ? C(19) C(47) 3.595(4) . . ? C(22) C(29) 3.368(3) . 3_657 ? C(38) C(40) 3.584(3) . 3_667 ? C(39) C(40) 3.446(3) . 3_667 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------