data_General _audit_creation_date '2008-04-23' _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Mistuhiko Shionoya' _publ_contact_author_email 'shionoya@chem.s.u-tokyo.ac.jp ' shionoya@chem.s.u-tokyo.acjp' _publ_contact_author_fax ' +81-3-5841-8060 ' _publ_contact_author_phone ' +81-3-5841-8060 ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal _publ_requested_category 'CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; #============================================================================== # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Johnson, C.K. (1976). ORTEP-II. A FORTRAN Thermal-Ellipsoid Plot Program. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Rigaku (1998). PROCESS-AUTO. Automatic Data Acquisition and Processing Package for Imaging Plate Diffractometer. Rigaku Corporation, Tokyo 196-8666, Japan Rigaku & RAC (2007). CrystalStructure (Version 3.80). Single Crystal Structure Analysis Software. Rigaku, Tokyo 196-8666, Japan. Rigaku Americas, TX, USA 77381-5209. Sheldrick, G.M. (1997). SHELXS97. Program for the Solution of Crystal Structures. University of Gottingen, Germany. Sheldrick, G.M. (1997). SHELXL97. University of Gottingen, Germany. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; Hydrogen atoms of water were not located in d-Fourier maps. ; #============================================================================== data__080418 #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C57 H41 N3 O ' _chemical_formula_moiety 'C57 H39 N3, H2 O ' _chemical_formula_weight 783.97 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 '+X,+Y,+Z' 2 '-X,-Y,-Z' #------------------------------------------------------------------------------ _cell_length_a 8.9038(4) _cell_length_b 15.5360(5) _cell_length_c 16.0430(7) _cell_angle_alpha 76.0841(19) _cell_angle_beta 88.684(2) _cell_angle_gamma 75.237(2) _cell_volume 2081.24(15) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9631 _cell_measurement_theta_min 4.6 _cell_measurement_theta_max 68.3 _cell_measurement_temperature 93.1 #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824.00 _exptl_absorpt_coefficient_mu 0.574 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.873 _exptl_absorpt_correction_T_max 0.950 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54187 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 24042 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_theta_max 68.25 _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 68.25 _diffrn_measured_fraction_theta_full 0.973 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7415 _reflns_number_gt 4494 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1926 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 7415 _refine_ls_number_parameters 551 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1003P)^2^+0.0674P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0050 _refine_diff_density_max 0.81 _refine_diff_density_min -0.43 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.018 0.009 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; 'N' 'N' 0.031 0.018 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'O' 'O' 0.049 0.032 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.2836(16) 0.5965(8) 0.4888(7) 0.507(8) Uani 1 1 d . . . N1 N -0.6258(3) 0.58538(17) 0.31311(16) 0.0583(7) Uani 1 1 d . . . N2 N 0.5698(3) 0.0433(2) 0.90514(15) 0.0672(8) Uani 1 1 d . . . N3 N 1.0892(3) 0.23265(16) -0.13694(14) 0.0501(6) Uani 1 1 d . . . C1 C 0.2733(3) 0.34167(16) 0.30286(15) 0.0368(6) Uani 1 1 d . . . C2 C 0.3303(3) 0.29486(17) 0.38736(15) 0.0378(6) Uani 1 1 d . . . C3 C 0.4785(3) 0.23332(17) 0.40152(15) 0.0379(6) Uani 1 1 d . . . C4 C 0.5682(3) 0.21542(16) 0.33134(15) 0.0361(6) Uani 1 1 d . . . C5 C 0.5133(3) 0.26527(16) 0.24700(15) 0.0376(6) Uani 1 1 d . . . C6 C 0.3685(3) 0.32946(16) 0.23341(15) 0.0364(6) Uani 1 1 d . . . C7 C 0.1093(3) 0.39917(16) 0.28821(14) 0.0360(6) Uani 1 1 d . . . C8 C -0.0119(3) 0.35828(17) 0.31341(15) 0.0405(6) Uani 1 1 d . . . H8 H 0.0114 0.2941 0.3382 0.049 Uiso 1 1 calc R . . C9 C -0.1655(3) 0.40880(17) 0.30316(15) 0.0391(6) Uani 1 1 d . . . H9 H -0.2454 0.3791 0.3222 0.047 Uiso 1 1 calc R . . C10 C -0.2046(3) 0.50287(17) 0.26517(14) 0.0368(6) Uani 1 1 d . . . C11 C -0.0842(3) 0.54359(17) 0.23808(15) 0.0392(6) Uani 1 1 d . . . H11 H -0.1080 0.6073 0.2112 0.047 Uiso 1 1 calc R . . C12 C 0.0707(3) 0.49305(17) 0.24953(15) 0.0384(6) Uani 1 1 d . . . H12 H 0.1508 0.5228 0.2308 0.046 Uiso 1 1 calc R . . C13 C -0.3683(3) 0.55779(17) 0.25593(16) 0.0397(6) Uani 1 1 d . . . C14 C -0.4751(3) 0.5391(2) 0.31759(17) 0.0497(7) Uani 1 1 d . . . H14 H -0.4390 0.4899 0.3666 0.060 Uiso 1 1 calc R . . C15 C -0.6724(4) 0.6543(2) 0.24358(19) 0.0526(8) Uani 1 1 d . . . H15 H -0.7787 0.6876 0.2384 0.063 Uiso 1 1 calc R . . C16 C -0.5773(3) 0.68039(19) 0.17922(17) 0.0465(7) Uani 1 1 d . . . H16 H -0.6162 0.7307 0.1316 0.056 Uiso 1 1 calc R . . C17 C -0.4232(3) 0.63121(18) 0.18575(16) 0.0450(7) Uani 1 1 d . . . H17 H -0.3546 0.6477 0.1421 0.054 Uiso 1 1 calc R . . C18 C 0.2322(3) 0.31088(17) 0.46154(15) 0.0391(6) Uani 1 1 d . . . C19 C 0.1647(3) 0.24381(19) 0.50888(16) 0.0471(7) Uani 1 1 d . . . H19 H 0.1817 0.1866 0.4939 0.056 Uiso 1 1 calc R . . C20 C 0.0737(4) 0.2591(2) 0.57715(17) 0.0566(8) Uani 1 1 d . . . H20 H 0.0253 0.2136 0.6075 0.068 Uiso 1 1 calc R . . C21 C 0.0530(4) 0.3410(2) 0.60154(18) 0.0591(9) Uani 1 1 d . . . H21 H -0.0078 0.3511 0.6494 0.071 Uiso 1 1 calc R . . C22 C 0.1200(4) 0.40736(19) 0.55666(17) 0.0502(8) Uani 1 1 d . . . H22 H 0.1066 0.4632 0.5737 0.060 Uiso 1 1 calc R . . C23 C 0.2077(3) 0.39295(18) 0.48611(16) 0.0436(7) Uani 1 1 d . . . H23 H 0.2514 0.4400 0.4543 0.052 Uiso 1 1 calc R . . C24 C 0.5338(3) 0.18371(17) 0.49201(15) 0.0391(6) Uani 1 1 d . . . C25 C 0.5665(3) 0.08895(17) 0.51784(15) 0.0408(6) Uani 1 1 d . . . H25 H 0.5659 0.0548 0.4761 0.049 Uiso 1 1 calc R . . C26 C 0.6000(3) 0.04275(19) 0.60344(15) 0.0434(7) Uani 1 1 d . . . H26 H 0.6188 -0.0222 0.6197 0.052 Uiso 1 1 calc R . . C27 C 0.6062(3) 0.09106(19) 0.66603(15) 0.0426(7) Uani 1 1 d . . . C28 C 0.5819(3) 0.18569(18) 0.63882(16) 0.0462(7) Uani 1 1 d . . . H28 H 0.5898 0.2197 0.6797 0.055 Uiso 1 1 calc R . . C29 C 0.5467(3) 0.23129(18) 0.55386(16) 0.0444(7) Uani 1 1 d . . . H29 H 0.5310 0.2960 0.5372 0.053 Uiso 1 1 calc R . . C30 C 0.6343(3) 0.04269(19) 0.75811(16) 0.0447(7) Uani 1 1 d . . . C31 C 0.7377(4) -0.0430(2) 0.78590(17) 0.0534(8) Uani 1 1 d . . . H31 H 0.7955 -0.0721 0.7453 0.064 Uiso 1 1 calc R . . C32 C 0.7570(4) -0.0862(2) 0.87270(18) 0.0596(9) Uani 1 1 d . . . H32 H 0.8269 -0.1449 0.8930 0.071 Uiso 1 1 calc R . . C33 C 0.6685(4) -0.0392(3) 0.92894(19) 0.0663(10) Uani 1 1 d . . . H33 H 0.6799 -0.0684 0.9885 0.080 Uiso 1 1 calc R . . C34 C 0.5549(4) 0.0811(2) 0.82130(17) 0.0534(8) Uani 1 1 d . . . H34 H 0.4835 0.1396 0.8029 0.064 Uiso 1 1 calc R . . C35 C 0.7165(3) 0.14215(17) 0.34475(15) 0.0385(6) Uani 1 1 d . . . C36 C 0.7259(3) 0.06428(17) 0.31398(16) 0.0434(7) Uani 1 1 d . . . H36 H 0.6400 0.0602 0.2824 0.052 Uiso 1 1 calc R . . C37 C 0.8597(4) -0.00723(19) 0.32916(16) 0.0492(7) Uani 1 1 d . . . H37 H 0.8646 -0.0603 0.3087 0.059 Uiso 1 1 calc R . . C38 C 0.9855(4) -0.00158(19) 0.37379(17) 0.0496(7) Uani 1 1 d . . . H38 H 1.0770 -0.0507 0.3840 0.059 Uiso 1 1 calc R . . C39 C 0.9790(3) 0.07545(19) 0.40374(17) 0.0472(7) Uani 1 1 d . . . H39 H 1.0666 0.0796 0.4338 0.057 Uiso 1 1 calc R . . C40 C 0.8438(3) 0.14726(18) 0.38995(15) 0.0414(6) Uani 1 1 d . . . H40 H 0.8389 0.1997 0.4115 0.050 Uiso 1 1 calc R . . C41 C 0.6116(3) 0.24703(16) 0.17278(15) 0.0366(6) Uani 1 1 d . . . C42 C 0.5697(3) 0.20153(17) 0.11589(15) 0.0412(6) Uani 1 1 d . . . H42 H 0.4747 0.1839 0.1228 0.049 Uiso 1 1 calc R . . C43 C 0.6630(3) 0.18133(18) 0.04966(15) 0.0423(7) Uani 1 1 d . . . H43 H 0.6319 0.1498 0.0119 0.051 Uiso 1 1 calc R . . C44 C 0.8026(3) 0.20700(16) 0.03777(15) 0.0366(6) Uani 1 1 d . . . C45 C 0.8438(3) 0.25322(17) 0.09436(15) 0.0415(6) Uani 1 1 d . . . H45 H 0.9375 0.2722 0.0868 0.050 Uiso 1 1 calc R . . C46 C 0.7510(3) 0.27187(17) 0.16112(16) 0.0409(6) Uani 1 1 d . . . H46 H 0.7830 0.3022 0.1997 0.049 Uiso 1 1 calc R . . C47 C 0.9050(3) 0.18688(17) -0.03353(15) 0.0379(6) Uani 1 1 d . . . C48 C 0.9198(3) 0.10853(18) -0.06331(16) 0.0440(7) Uani 1 1 d . . . H48 H 0.8617 0.0658 -0.0389 0.053 Uiso 1 1 calc R . . C49 C 1.0198(3) 0.09252(19) -0.12883(17) 0.0502(7) Uani 1 1 d . . . H49 H 1.0309 0.0391 -0.1498 0.060 Uiso 1 1 calc R . . C50 C 1.1022(3) 0.15561(19) -0.16258(17) 0.0484(7) Uani 1 1 d . . . H50 H 1.1722 0.1438 -0.2065 0.058 Uiso 1 1 calc R . . C51 C 0.9909(3) 0.24668(19) -0.07474(16) 0.0458(7) Uani 1 1 d . . . H51 H 0.9787 0.3022 -0.0571 0.055 Uiso 1 1 calc R . . C52 C 0.3178(3) 0.38682(16) 0.14431(15) 0.0367(6) Uani 1 1 d . . . C53 C 0.3682(3) 0.46524(17) 0.11361(16) 0.0428(7) Uani 1 1 d . . . H53 H 0.4352 0.4814 0.1490 0.051 Uiso 1 1 calc R . . C54 C 0.3229(3) 0.52071(18) 0.03223(16) 0.0463(7) Uani 1 1 d . . . H54 H 0.3579 0.5748 0.0125 0.056 Uiso 1 1 calc R . . C55 C 0.2275(3) 0.49764(19) -0.02005(16) 0.0472(7) Uani 1 1 d . . . H55 H 0.1967 0.5353 -0.0761 0.057 Uiso 1 1 calc R . . C56 C 0.1772(4) 0.41973(19) 0.00947(17) 0.0508(7) Uani 1 1 d . . . H56 H 0.1116 0.4034 -0.0266 0.061 Uiso 1 1 calc R . . C57 C 0.2208(3) 0.36451(18) 0.09121(16) 0.0453(7) Uani 1 1 d . . . H57 H 0.1840 0.3111 0.1109 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.69(2) 0.553(18) 0.383(14) -0.108(13) 0.129(14) -0.367(17) N1 0.0444(17) 0.0670(16) 0.0567(16) -0.0089(13) 0.0055(13) -0.0086(13) N2 0.073(2) 0.095(2) 0.0366(14) -0.0117(14) 0.0035(13) -0.0298(18) N3 0.0569(17) 0.0561(14) 0.0407(13) -0.0122(11) 0.0109(11) -0.0209(13) C1 0.0428(17) 0.0380(13) 0.0320(13) -0.0092(10) 0.0034(12) -0.0140(12) C2 0.0432(17) 0.0393(14) 0.0331(13) -0.0114(11) 0.0021(12) -0.0121(13) C3 0.0430(17) 0.0407(14) 0.0301(13) -0.0082(10) 0.0002(11) -0.0111(12) C4 0.0397(16) 0.0362(13) 0.0333(13) -0.0098(10) 0.0008(11) -0.0100(12) C5 0.0423(17) 0.0392(14) 0.0329(13) -0.0097(11) 0.0025(12) -0.0126(13) C6 0.0408(17) 0.0399(14) 0.0309(13) -0.0087(10) 0.0018(11) -0.0143(12) C7 0.0400(16) 0.0410(14) 0.0277(12) -0.0110(10) 0.0019(11) -0.0093(12) C8 0.0481(18) 0.0408(14) 0.0324(13) -0.0094(11) 0.0029(12) -0.0110(13) C9 0.0411(17) 0.0464(15) 0.0328(13) -0.0111(11) 0.0059(12) -0.0157(13) C10 0.0405(17) 0.0437(14) 0.0258(12) -0.0086(10) 0.0017(11) -0.0101(13) C11 0.0476(18) 0.0410(14) 0.0289(13) -0.0076(11) 0.0052(12) -0.0125(13) C12 0.0410(17) 0.0443(15) 0.0316(13) -0.0103(11) 0.0050(12) -0.0131(13) C13 0.0411(17) 0.0466(15) 0.0331(13) -0.0114(11) 0.0020(12) -0.0126(13) C14 0.0445(19) 0.0605(18) 0.0389(15) -0.0060(13) 0.0013(13) -0.0099(15) C15 0.0418(19) 0.0620(18) 0.0522(18) -0.0179(15) -0.0049(14) -0.0054(15) C16 0.0437(18) 0.0531(16) 0.0390(15) -0.0104(12) -0.0035(13) -0.0063(14) C17 0.0483(19) 0.0510(16) 0.0357(14) -0.0099(12) 0.0032(13) -0.0135(14) C18 0.0439(17) 0.0430(14) 0.0273(13) -0.0079(11) 0.0008(12) -0.0062(13) C19 0.056(2) 0.0493(16) 0.0332(14) -0.0109(12) 0.0064(13) -0.0086(14) C20 0.072(2) 0.0544(18) 0.0402(16) -0.0075(13) 0.0163(15) -0.0155(16) C21 0.077(2) 0.0561(18) 0.0363(15) -0.0102(13) 0.0178(15) -0.0062(17) C22 0.062(2) 0.0476(16) 0.0379(15) -0.0145(13) 0.0027(14) -0.0048(15) C23 0.0499(19) 0.0461(15) 0.0337(14) -0.0110(11) 0.0026(12) -0.0094(13) C24 0.0405(17) 0.0452(15) 0.0304(13) -0.0094(11) 0.0002(11) -0.0086(12) C25 0.0485(18) 0.0446(15) 0.0299(13) -0.0085(11) 0.0016(12) -0.0135(13) C26 0.0461(18) 0.0491(15) 0.0328(13) -0.0069(11) 0.0026(12) -0.0110(13) C27 0.0399(17) 0.0582(17) 0.0271(13) -0.0117(12) -0.0001(11) -0.0068(13) C28 0.0507(19) 0.0513(16) 0.0354(14) -0.0143(12) -0.0003(13) -0.0072(14) C29 0.0502(19) 0.0471(15) 0.0343(14) -0.0119(12) -0.0030(12) -0.0075(13) C30 0.0429(18) 0.0600(17) 0.0306(13) -0.0074(12) -0.0010(12) -0.0152(14) C31 0.052(2) 0.0687(19) 0.0362(15) -0.0060(13) 0.0020(13) -0.0167(16) C32 0.055(2) 0.077(2) 0.0400(16) 0.0089(15) -0.0089(15) -0.0247(17) C33 0.075(3) 0.099(3) 0.0298(15) -0.0002(17) -0.0037(16) -0.045(2) C34 0.053(2) 0.077(2) 0.0348(15) -0.0145(14) 0.0050(14) -0.0226(17) C35 0.0464(17) 0.0417(14) 0.0264(12) -0.0055(10) 0.0057(12) -0.0129(13) C36 0.0530(19) 0.0437(15) 0.0324(13) -0.0078(11) 0.0042(12) -0.0119(14) C37 0.059(2) 0.0446(15) 0.0386(15) -0.0107(12) 0.0079(14) -0.0040(14) C38 0.0455(19) 0.0492(16) 0.0427(16) -0.0018(13) 0.0042(14) -0.0011(14) C39 0.0438(18) 0.0547(17) 0.0400(15) -0.0045(13) 0.0022(13) -0.0135(14) C40 0.0447(18) 0.0416(14) 0.0354(14) -0.0047(11) 0.0020(12) -0.0108(13) C41 0.0387(16) 0.0421(14) 0.0282(13) -0.0076(10) 0.0027(11) -0.0100(12) C42 0.0416(17) 0.0518(16) 0.0332(13) -0.0108(11) 0.0044(12) -0.0169(13) C43 0.0474(18) 0.0522(16) 0.0317(13) -0.0140(12) 0.0031(12) -0.0171(14) C44 0.0382(16) 0.0397(14) 0.0305(13) -0.0068(10) 0.0018(11) -0.0092(12) C45 0.0449(17) 0.0469(15) 0.0358(14) -0.0108(11) 0.0016(12) -0.0168(13) C46 0.0433(17) 0.0485(15) 0.0338(13) -0.0154(11) 0.0025(12) -0.0121(13) C47 0.0407(17) 0.0412(14) 0.0307(13) -0.0068(11) 0.0016(11) -0.0104(12) C48 0.0464(18) 0.0480(15) 0.0398(14) -0.0118(12) 0.0067(13) -0.0157(14) C49 0.057(2) 0.0527(17) 0.0454(16) -0.0194(13) 0.0108(14) -0.0153(15) C50 0.0501(19) 0.0599(18) 0.0376(15) -0.0141(13) 0.0082(13) -0.0165(15) C51 0.0529(19) 0.0483(15) 0.0375(15) -0.0127(12) 0.0081(13) -0.0138(14) C52 0.0398(16) 0.0394(14) 0.0305(13) -0.0098(11) 0.0053(11) -0.0085(12) C53 0.0464(18) 0.0491(15) 0.0332(14) -0.0090(11) 0.0034(12) -0.0141(13) C54 0.0537(19) 0.0475(15) 0.0367(14) -0.0053(12) 0.0053(13) -0.0158(14) C55 0.054(2) 0.0537(17) 0.0308(14) -0.0054(12) -0.0002(13) -0.0120(15) C56 0.056(2) 0.0564(17) 0.0402(15) -0.0105(13) -0.0104(14) -0.0146(15) C57 0.0544(19) 0.0445(15) 0.0375(14) -0.0055(12) -0.0040(13) -0.0168(14) #============================================================================== _computing_data_collection 'PROCESS-AUTO (Rigaku, 1998)' _computing_cell_refinement 'PROCESS-AUTO (Rigaku, 1998)' _computing_data_reduction 'CrystalStructure (Rigaku & RAC 2007)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_publication_material 'CrystalStructure (Rigaku & RAC 2007)' _computing_molecular_graphics 'ORTEP (Johnson, 1976)' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C15 1.336(3) . ? N1 C14 1.346(3) . ? N2 C34 1.327(3) . ? N2 C33 1.330(4) . ? N3 C51 1.333(3) . ? N3 C50 1.334(3) . ? C1 C6 1.404(3) . ? C1 C2 1.412(3) . ? C1 C7 1.495(3) . ? C2 C3 1.405(4) . ? C2 C18 1.492(3) . ? C3 C4 1.406(3) . ? C3 C24 1.498(3) . ? C4 C5 1.415(3) . ? C4 C35 1.488(3) . ? C5 C6 1.399(3) . ? C5 C41 1.501(3) . ? C6 C52 1.501(3) . ? C7 C8 1.392(4) . ? C7 C12 1.396(3) . ? C8 C9 1.383(3) . ? C9 C10 1.397(3) . ? C10 C11 1.390(4) . ? C10 C13 1.480(4) . ? C11 C12 1.394(4) . ? C13 C14 1.387(4) . ? C13 C17 1.390(3) . ? C15 C16 1.371(4) . ? C16 C17 1.383(4) . ? C18 C23 1.387(3) . ? C18 C19 1.393(4) . ? C19 C20 1.378(4) . ? C20 C21 1.387(4) . ? C21 C22 1.368(4) . ? C22 C23 1.390(4) . ? C24 C25 1.385(3) . ? C24 C29 1.395(3) . ? C25 C26 1.388(3) . ? C26 C27 1.400(3) . ? C27 C28 1.390(4) . ? C27 C30 1.482(3) . ? C28 C29 1.378(3) . ? C30 C34 1.388(4) . ? C30 C31 1.388(4) . ? C31 C32 1.386(4) . ? C32 C33 1.399(4) . ? C35 C40 1.389(4) . ? C35 C36 1.396(3) . ? C36 C37 1.386(4) . ? C37 C38 1.376(4) . ? C38 C39 1.381(4) . ? C39 C40 1.397(4) . ? C41 C46 1.386(3) . ? C41 C42 1.390(3) . ? C42 C43 1.380(3) . ? C43 C44 1.395(4) . ? C44 C45 1.392(3) . ? C44 C47 1.488(3) . ? C45 C46 1.379(3) . ? C47 C48 1.386(3) . ? C47 C51 1.389(4) . ? C48 C49 1.389(4) . ? C49 C50 1.373(4) . ? C52 C53 1.382(3) . ? C52 C57 1.386(3) . ? C53 C54 1.384(3) . ? C54 C55 1.373(4) . ? C55 C56 1.371(4) . ? C56 C57 1.385(3) . ? 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_3 _geom_angle_publ_flag C15 N1 C14 116.0(3) . . ? C34 N2 C33 115.8(3) . . ? C51 N3 C50 116.7(2) . . ? C6 C1 C2 119.6(2) . . ? C6 C1 C7 120.9(2) . . ? C2 C1 C7 119.5(2) . . ? C3 C2 C1 120.2(2) . . ? C3 C2 C18 120.1(2) . . ? C1 C2 C18 119.7(2) . . ? C2 C3 C4 120.0(2) . . ? C2 C3 C24 118.6(2) . . ? C4 C3 C24 121.2(2) . . ? C3 C4 C5 119.5(2) . . ? C3 C4 C35 120.6(2) . . ? C5 C4 C35 119.8(2) . . ? C6 C5 C4 120.2(2) . . ? C6 C5 C41 120.8(2) . . ? C4 C5 C41 119.0(2) . . ? C5 C6 C1 120.2(2) . . ? C5 C6 C52 119.4(2) . . ? C1 C6 C52 120.4(2) . . ? C8 C7 C12 117.7(2) . . ? C8 C7 C1 119.3(2) . . ? C12 C7 C1 123.0(2) . . ? C9 C8 C7 121.6(2) . . ? C8 C9 C10 120.9(3) . . ? C11 C10 C9 117.7(2) . . ? C11 C10 C13 121.1(2) . . ? C9 C10 C13 121.2(2) . . ? C10 C11 C12 121.5(2) . . ? C11 C12 C7 120.6(3) . . ? C14 C13 C17 116.4(3) . . ? C14 C13 C10 121.6(2) . . ? C17 C13 C10 122.0(2) . . ? N1 C14 C13 124.9(3) . . ? N1 C15 C16 124.4(3) . . ? C15 C16 C17 118.0(3) . . ? C16 C17 C13 120.2(3) . . ? C23 C18 C19 118.1(2) . . ? C23 C18 C2 120.6(2) . . ? C19 C18 C2 121.3(2) . . ? C20 C19 C18 121.0(3) . . ? C19 C20 C21 119.9(3) . . ? C22 C21 C20 120.0(3) . . ? C21 C22 C23 120.0(3) . . ? C18 C23 C22 120.9(3) . . ? C25 C24 C29 117.8(2) . . ? C25 C24 C3 120.8(2) . . ? C29 C24 C3 121.3(2) . . ? C24 C25 C26 121.4(2) . . ? C25 C26 C27 120.5(2) . . ? C28 C27 C26 117.6(2) . . ? C28 C27 C30 121.5(2) . . ? C26 C27 C30 120.8(2) . . ? C29 C28 C27 121.5(2) . . ? C28 C29 C24 120.9(2) . . ? C34 C30 C31 116.5(3) . . ? C34 C30 C27 120.9(3) . . ? C31 C30 C27 122.6(2) . . ? C32 C31 C30 120.2(3) . . ? C31 C32 C33 116.8(3) . . ? N2 C33 C32 124.8(3) . . ? N2 C34 C30 125.8(3) . . ? C40 C35 C36 119.0(2) . . ? C40 C35 C4 121.9(2) . . ? C36 C35 C4 119.0(2) . . ? C37 C36 C35 120.5(3) . . ? C38 C37 C36 120.3(3) . . ? C37 C38 C39 120.1(3) . . ? C38 C39 C40 120.1(3) . . ? C35 C40 C39 120.2(3) . . ? C46 C41 C42 117.9(2) . . ? C46 C41 C5 120.6(2) . . ? C42 C41 C5 121.4(2) . . ? C43 C42 C41 121.6(3) . . ? C42 C43 C44 120.4(2) . . ? C45 C44 C43 118.0(2) . . ? C45 C44 C47 120.4(2) . . ? C43 C44 C47 121.6(2) . . ? C46 C45 C44 121.2(3) . . ? C45 C46 C41 120.9(2) . . ? C48 C47 C51 116.0(2) . . ? C48 C47 C44 122.6(2) . . ? C51 C47 C44 121.4(2) . . ? C47 C48 C49 120.0(3) . . ? C50 C49 C48 118.5(3) . . ? N3 C50 C49 123.5(3) . . ? N3 C51 C47 125.4(3) . . ? C53 C52 C57 118.2(2) . . ? C53 C52 C6 119.3(2) . . ? C57 C52 C6 122.5(2) . . ? C52 C53 C54 121.2(3) . . ? C55 C54 C53 120.0(3) . . ? C56 C55 C54 119.3(2) . . ? C55 C56 C57 120.9(3) . . ? C56 C57 C52 120.3(3) . . ? #==============================================================================