data_global _audit_creation_date 2014-09-04 _audit_creation_method 'by CrystalStructure 4.1' _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 'ENTER NAME' _publ_contact_author_email 'ENTER EMAIL ADDRESS' _publ_contact_author_fax 'ENTER FAX NUMBER' _publ_contact_author_phone 'ENTER PHONE NUMBER' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal 'ENTER JOURNAL NAME HERE' _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 Rigaku (2014). CrystalStructure. Version 4.1. Rigaku Corporation, Tokyo, Japan. Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. SHELXS97 Rigaku (1998). REQAB. Rigaku Corporation, Tokyo, Japan. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #============================================================================== data_No111_ #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C46 H44 N2 O7' _chemical_formula_moiety 'C46 H44 N2 O7' _chemical_formula_weight 736.86 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' _space_group_IT_number 14 loop_ _symmetry_equiv_pos_site_id _space_group_symop_operation_xyz 1 '+X,+Y,+Z' 2 '1/2-X,1/2+Y,1/2-Z' 3 '-X,-Y,-Z' 4 '1/2+X,1/2-Y,1/2+Z' #------------------------------------------------------------------------------ _cell_length_a 14.623(3) _cell_length_b 14.418(3) _cell_length_c 19.212(4) _cell_angle_alpha 90.0000 _cell_angle_beta 110.272(3) _cell_angle_gamma 90.0000 _cell_volume 3799.7(14) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10472 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 27.50 _cell_measurement_temperature 110 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.280 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.288 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560.00 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.908 _exptl_absorpt_correction_T_max 0.991 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 110 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn724' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.111 _diffrn_reflns_number 59978 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_theta_max 27.470 _diffrn_reflns_theta_min 3.043 _diffrn_reflns_theta_full 27.470 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.000 _diffrn_reflns_Laue_measured_fraction_full 0.000 _diffrn_reflns_point_group_measured_fraction_max 0.000 _diffrn_reflns_point_group_measured_fraction_full 0.000 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # 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 8678 _reflns_number_gt 7380 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1449 _refine_ls_wR_factor_gt 0.1358 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 8678 _refine_ls_number_parameters 512 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0819P)^2^+1.1183P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.55 _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' 0.0033 0.0016 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'H' 'H' 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; 'N' 'N' 0.0061 0.0033 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 'O' 'O' 0.0106 0.0060 ; International Tables for Crystallography (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_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C49A C 0.1614(2) 0.9794(2) 0.49016(18) 0.0284(8) Uani 0.572(5) 4 d . . . C50A C 0.0977(3) 1.0300(2) 0.4205(2) 0.0371(9) Uani 0.572(5) 4 d . . . C49B C 0.1512(4) 1.0173(3) 0.4413(2) 0.0251(10) Uiso 0.428(5) 4 d . . . C50B C 0.0908(4) 0.9796(3) 0.4853(3) 0.0387(13) Uiso 0.428(5) 4 d . . . C63A C 0.6004(4) 0.7553(4) 0.2611(3) 0.0557(18) Uani 0.527(9) 4 d . . . C63B C 0.5713(4) 0.7787(4) 0.2084(3) 0.0504(17) Uiso 0.473(9) 4 d . . . O1 O 0.76717(7) 0.57511(7) 0.50296(6) 0.0209(2) Uani 1 4 d . . . O2 O 0.66936(8) 0.47072(7) 0.31096(5) 0.0201(2) Uani 1 4 d . . . O3 O 0.61222(9) 0.42066(8) 0.19287(6) 0.0299(3) Uani 1 4 d . . . O11 O 0.51205(7) 0.78891(7) 0.45671(6) 0.0214(2) Uani 1 4 d . . . O12 O 0.37365(8) 0.72460(7) 0.27063(6) 0.0218(2) Uani 1 4 d . . . O13 O 0.29285(10) 0.71109(9) 0.14798(6) 0.0353(3) Uani 1 4 d . . . O61 O 0.73427(10) 0.72987(10) 0.22790(8) 0.0455(3) Uani 1 4 d . . . N1 N 1.03347(9) 0.36429(9) 0.58835(7) 0.0227(3) Uani 1 4 d . . . N11 N 0.25862(12) 0.97579(12) 0.48430(12) 0.0532(5) Uani 1 4 d . . . C1 C 0.75068(11) 0.42603(10) 0.43999(8) 0.0194(3) Uani 1 4 d . . . C2 C 0.79544(11) 0.34067(10) 0.43817(8) 0.0224(3) Uani 1 4 d . . . H2 H 0.76123 0.29563 0.40258 0.0269 Uiso 1 4 d . . . C3 C 0.88762(11) 0.32001(10) 0.48643(9) 0.0232(3) Uani 1 4 d . . . H3 H 0.91541 0.26126 0.48339 0.0278 Uiso 1 4 d . . . C4 C 0.94164(10) 0.38476(10) 0.54045(8) 0.0197(3) Uani 1 4 d . . . C5 C 0.89674(11) 0.47058(10) 0.54273(8) 0.0196(3) Uani 1 4 d . . . H5 H 0.93033 0.51609 0.57812 0.0235 Uiso 1 4 d . . . C6 C 0.80386(10) 0.48891(10) 0.49361(8) 0.0182(3) Uani 1 4 d . . . C7 C 0.67297(10) 0.59641(10) 0.46060(8) 0.0185(3) Uani 1 4 d . . . C8 C 0.63793(11) 0.68006(10) 0.47780(8) 0.0201(3) Uani 1 4 d . . . H8 H 0.67846 0.7189 0.51602 0.0241 Uiso 1 4 d . . . C9 C 0.51859(11) 0.56579(10) 0.36685(8) 0.0199(3) Uani 1 4 d . . . H9 H 0.47775 0.52652 0.32913 0.0238 Uiso 1 4 d . . . C10 C 0.61431(11) 0.53855(10) 0.40452(8) 0.0189(3) Uani 1 4 d . . . C11 C 0.65425(11) 0.45109(10) 0.38301(8) 0.0184(3) Uani 1 4 d . . . C12 C 0.58185(10) 0.37224(10) 0.36182(8) 0.0189(3) Uani 1 4 d . . . C13 C 0.53874(11) 0.32498(11) 0.40539(9) 0.0236(3) Uani 1 4 d . . . H13 H 0.55234 0.34114 0.45592 0.0283 Uiso 1 4 d . . . C14 C 0.47504(12) 0.25327(12) 0.37249(9) 0.0283(3) Uani 1 4 d . . . H14 H 0.44406 0.22022 0.40094 0.0339 Uiso 1 4 d . . . C15 C 0.45570(12) 0.22886(12) 0.29875(9) 0.0295(4) Uani 1 4 d . . . H15 H 0.41349 0.17817 0.27812 0.0353 Uiso 1 4 d . . . C16 C 0.49726(12) 0.27759(11) 0.25484(9) 0.0263(3) Uani 1 4 d . . . H16 H 0.48324 0.26208 0.20414 0.0316 Uiso 1 4 d . . . C17 C 0.56007(11) 0.34983(10) 0.28789(8) 0.0200(3) Uani 1 4 d . . . C18 C 0.61362(11) 0.41377(10) 0.25592(8) 0.0210(3) Uani 1 4 d . . . C19 C 1.07126(11) 0.26971(10) 0.59785(9) 0.0233(3) Uani 1 4 d . . . H19A H 1.01586 0.22627 0.58857 0.0280 Uiso 1 4 d . . . H19B H 1.11435 0.26158 0.6501 0.0280 Uiso 1 4 d . . . C20 C 1.12777(14) 0.24328(12) 0.54774(11) 0.0361(4) Uani 1 4 d . . . H20A H 1.18373 0.28491 0.55709 0.0433 Uiso 1 4 d . . . H20B H 1.0852 0.24867 0.49575 0.0433 Uiso 1 4 d . . . H20C H 1.15083 0.1792 0.55804 0.0433 Uiso 1 4 d . . . C21 C 1.09605(11) 0.43539(11) 0.63522(9) 0.0237(3) Uani 1 4 d . . . H21A H 1.08245 0.4953 0.60839 0.0284 Uiso 1 4 d . . . H21B H 1.16491 0.41915 0.64392 0.0284 Uiso 1 4 d . . . C22 C 1.08287(14) 0.44749(13) 0.70960(9) 0.0343(4) Uani 1 4 d . . . H22A H 1.12633 0.49664 0.73775 0.0411 Uiso 1 4 d . . . H22B H 1.09868 0.38922 0.73748 0.0411 Uiso 1 4 d . . . H22C H 1.01508 0.46443 0.70164 0.0411 Uiso 1 4 d . . . C31 C 0.34477(11) 0.74656(10) 0.38606(8) 0.0206(3) Uani 1 4 d . . . C32 C 0.24686(12) 0.76426(12) 0.37488(10) 0.0307(4) Uani 1 4 d . . . H32 H 0.19855 0.72449 0.34306 0.0368 Uiso 1 4 d . . . C33 C 0.21811(13) 0.83702(13) 0.40825(11) 0.0368(4) Uani 1 4 d . . . H33 H 0.15077 0.84596 0.39988 0.0442 Uiso 1 4 d . . . C34 C 0.28736(12) 0.89912(12) 0.45505(10) 0.0307(4) Uani 1 4 d . . . C35 C 0.38620(11) 0.87910(10) 0.46999(8) 0.0218(3) Uani 1 4 d . . . H35 H 0.43509 0.91696 0.50336 0.0262 Uiso 1 4 d . . . C36 C 0.41236(11) 0.80399(10) 0.43596(8) 0.0193(3) Uani 1 4 d . . . C37 C 0.54273(11) 0.70526(10) 0.43794(8) 0.0186(3) Uani 1 4 d . . . C40 C 0.48059(11) 0.64823(10) 0.38236(8) 0.0190(3) Uani 1 4 d . . . C41 C 0.37681(11) 0.67697(10) 0.34143(8) 0.0194(3) Uani 1 4 d . . . C42 C 0.30819(11) 0.59651(10) 0.31228(8) 0.0205(3) Uani 1 4 d . . . C43 C 0.28257(12) 0.52573(11) 0.35103(9) 0.0268(3) Uani 1 4 d . . . H43 H 0.3076 0.52382 0.40371 0.0321 Uiso 1 4 d . . . C44 C 0.21893(13) 0.45760(12) 0.31009(11) 0.0334(4) Uani 1 4 d . . . H44 H 0.20073 0.40817 0.33529 0.0400 Uiso 1 4 d . . . C45 C 0.18152(14) 0.46072(12) 0.23280(11) 0.0376(4) Uani 1 4 d . . . H45 H 0.13844 0.41336 0.2061 0.0451 Uiso 1 4 d . . . C46 C 0.20642(13) 0.53204(12) 0.19451(10) 0.0328(4) Uani 1 4 d . . . H46 H 0.18046 0.53491 0.14187 0.0394 Uiso 1 4 d . . . C47 C 0.27072(11) 0.59935(11) 0.23566(9) 0.0236(3) Uani 1 4 d . . . C48 C 0.31024(12) 0.68163(11) 0.21021(8) 0.0247(3) Uani 1 4 d . . . C51 C 0.32738(13) 1.04535(12) 0.52563(10) 0.0305(4) Uani 1 4 d . . . H51A H 0.29404 1.1062 0.51847 0.0366 Uiso 1 4 d . . . H51B H 0.3808 1.04994 0.50524 0.0366 Uiso 1 4 d . . . C52 C 0.37056(19) 1.02541(16) 0.60739(12) 0.0537(6) Uani 1 4 d . . . H52A H 0.40531 0.96605 0.61513 0.0644 Uiso 1 4 d . . . H52B H 0.31834 1.02221 0.62835 0.0644 Uiso 1 4 d . . . H52C H 0.41617 1.07498 0.63198 0.0644 Uiso 1 4 d . . . C61 C 0.66988(16) 0.65639(14) 0.19073(12) 0.0454(5) Uani 1 4 d . . . C62 C 0.57075(19) 0.67786(19) 0.1949(2) 0.0761(9) Uani 1 4 d . . . C64 C 0.67932(19) 0.7987(2) 0.24924(19) 0.0820(10) Uani 1 4 d . . . H49A H 0.16315 1.0135 0.53531 0.0341 Uiso 0.572(5) 4 calc R . . H49B H 0.13629 0.91601 0.49215 0.0341 Uiso 0.572(5) 4 calc R . . H50A H 0.12451 1.09194 0.41896 0.0556 Uiso 0.572(5) 4 calc R . . H50B H 0.03129 1.03564 0.42125 0.0556 Uiso 0.572(5) 4 calc R . . H50C H 0.09643 0.99489 0.37646 0.0556 Uiso 0.572(5) 4 calc R . . H49C H 0.15204 1.08595 0.44179 0.0302 Uiso 0.428(5) 4 calc R . . H49D H 0.12564 0.99548 0.38924 0.0302 Uiso 0.428(5) 4 calc R . . H50D H 0.09655 0.91188 0.48822 0.0581 Uiso 0.428(5) 4 calc R . . H50E H 0.02236 0.99688 0.46063 0.0581 Uiso 0.428(5) 4 calc R . . H50F H 0.11463 1.00577 0.5355 0.0581 Uiso 0.428(5) 4 calc R . . H61A H 0.69404 0.59631 0.21512 0.0545 Uiso 1 4 calc R . . H61B H 0.66588 0.65249 0.1383 0.0545 Uiso 1 4 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C49A 0.0246(16) 0.0245(14) 0.0400(18) 0.0020(11) 0.0161(13) -0.0065(12) C50A 0.0238(19) 0.0375(18) 0.045(2) 0.0040(13) 0.0061(15) 0.0005(14) C63A 0.050(3) 0.070(3) 0.053(3) -0.021(2) 0.026(2) -0.011(2) O1 0.0184(5) 0.0171(5) 0.0239(5) 0.0015(4) 0.0030(4) -0.0032(4) O2 0.0242(5) 0.0188(5) 0.0183(5) -0.0027(4) 0.0085(4) -0.0018(4) O3 0.0428(7) 0.0272(6) 0.0210(6) -0.0061(5) 0.0128(5) -0.0024(4) O11 0.0190(5) 0.0165(5) 0.0265(6) 0.0009(4) 0.0052(4) -0.0036(4) O12 0.0240(6) 0.0220(5) 0.0191(5) 0.0019(4) 0.0069(4) 0.0013(4) O13 0.0449(8) 0.0365(7) 0.0214(6) 0.0099(6) 0.0074(5) 0.0038(5) O61 0.0355(8) 0.0433(8) 0.0542(9) 0.0007(6) 0.0110(7) -0.0040(7) N1 0.0211(6) 0.0197(6) 0.0240(7) 0.0022(5) 0.0036(5) -0.0016(5) N11 0.0254(8) 0.0474(10) 0.0915(14) -0.0100(7) 0.0263(9) -0.0473(10) C1 0.0199(7) 0.0192(7) 0.0187(7) -0.0007(6) 0.0063(6) -0.0006(5) C2 0.0230(8) 0.0193(7) 0.0233(8) 0.0002(6) 0.0059(6) -0.0039(6) C3 0.0239(8) 0.0183(7) 0.0261(8) 0.0031(6) 0.0070(6) -0.0013(6) C4 0.0191(7) 0.0214(7) 0.0188(7) 0.0003(6) 0.0067(6) 0.0015(6) C5 0.0204(7) 0.0186(7) 0.0189(7) -0.0006(6) 0.0057(6) -0.0016(5) C6 0.0197(7) 0.0155(7) 0.0198(7) 0.0008(5) 0.0075(6) 0.0001(5) C7 0.0176(7) 0.0192(7) 0.0183(7) 0.0001(5) 0.0056(6) 0.0012(5) C8 0.0210(7) 0.0175(7) 0.0205(7) -0.0014(6) 0.0057(6) -0.0014(5) C9 0.0210(7) 0.0196(7) 0.0178(7) -0.0008(6) 0.0053(6) -0.0023(5) C10 0.0205(7) 0.0177(7) 0.0186(7) 0.0000(5) 0.0070(6) -0.0006(5) C11 0.0204(7) 0.0184(7) 0.0169(7) -0.0001(6) 0.0070(6) -0.0011(5) C12 0.0175(7) 0.0181(7) 0.0198(7) 0.0024(5) 0.0050(6) 0.0001(5) C13 0.0252(8) 0.0263(8) 0.0201(7) -0.0005(6) 0.0089(6) -0.0005(6) C14 0.0263(8) 0.0311(9) 0.0284(8) -0.0067(7) 0.0107(7) 0.0021(7) C15 0.0263(8) 0.0307(9) 0.0288(9) -0.0115(7) 0.0063(7) -0.0034(7) C16 0.0269(8) 0.0295(8) 0.0205(8) -0.0057(7) 0.0056(6) -0.0036(6) C17 0.0193(7) 0.0193(7) 0.0202(7) 0.0013(6) 0.0055(6) -0.0007(6) C18 0.0236(7) 0.0189(7) 0.0195(7) 0.0010(6) 0.0063(6) -0.0018(5) C19 0.0229(8) 0.0206(7) 0.0256(8) 0.0023(6) 0.0072(6) 0.0029(6) C20 0.0385(10) 0.0284(9) 0.0497(11) 0.0030(8) 0.0256(9) -0.0030(8) C21 0.0207(7) 0.0214(7) 0.0262(8) -0.0002(6) 0.0047(6) -0.0005(6) C22 0.0427(10) 0.0308(9) 0.0260(9) -0.0012(8) 0.0076(8) -0.0054(7) C31 0.0211(7) 0.0197(7) 0.0214(7) -0.0004(6) 0.0078(6) -0.0031(6) C32 0.0209(8) 0.0291(9) 0.0412(10) -0.0044(6) 0.0098(7) -0.0151(7) C33 0.0219(8) 0.0346(10) 0.0569(12) -0.0048(7) 0.0174(8) -0.0215(9) C34 0.0263(8) 0.0275(8) 0.0432(10) -0.0037(7) 0.0181(8) -0.0137(7) C35 0.0234(7) 0.0189(7) 0.0232(7) -0.0028(6) 0.0081(6) -0.0038(6) C36 0.0194(7) 0.0181(7) 0.0208(7) 0.0010(5) 0.0073(6) 0.0011(5) C37 0.0212(7) 0.0154(7) 0.0198(7) 0.0011(5) 0.0079(6) -0.0005(5) C40 0.0191(7) 0.0194(7) 0.0180(7) 0.0003(5) 0.0059(6) 0.0001(5) C41 0.0208(7) 0.0187(7) 0.0183(7) 0.0005(6) 0.0064(6) -0.0003(5) C42 0.0188(7) 0.0194(7) 0.0228(7) 0.0019(6) 0.0064(6) -0.0050(6) C43 0.0272(8) 0.0248(8) 0.0291(8) -0.0022(6) 0.0109(7) -0.0032(6) C44 0.0339(9) 0.0226(8) 0.0462(11) -0.0047(7) 0.0172(8) -0.0046(7) C45 0.0332(10) 0.0256(9) 0.0471(11) -0.0058(7) 0.0051(8) -0.0152(8) C46 0.0322(9) 0.0305(9) 0.0284(9) 0.0024(7) 0.0013(7) -0.0109(7) C47 0.0230(8) 0.0220(7) 0.0232(8) 0.0060(6) 0.0047(6) -0.0043(6) C48 0.0251(8) 0.0250(8) 0.0215(8) 0.0079(6) 0.0051(6) -0.0030(6) C51 0.0301(9) 0.0235(8) 0.0389(10) -0.0021(7) 0.0131(7) -0.0111(7) C52 0.0739(16) 0.0501(13) 0.0420(12) 0.0103(11) 0.0264(11) -0.0014(10) C61 0.0544(13) 0.0333(10) 0.0456(12) -0.0076(9) 0.0137(10) 0.0085(8) C62 0.0432(14) 0.0529(15) 0.128(3) -0.0073(11) 0.0252(15) 0.0023(16) C64 0.0383(13) 0.094(2) 0.106(2) 0.0075(13) 0.0147(14) -0.0523(19) #============================================================================== _computing_data_collection 'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r16' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r16' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.1 (Rigaku, 2014)' _computing_molecular_graphics 'CrystalStructure 4.1' #============================================================================== # 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_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 C49A C50A 1.526(4) yes . . C49A N11 1.465(4) yes . . C49B C50B 1.519(8) yes . . C49B N11 1.615(5) yes . . C63A C62 1.634(6) yes . . C63A C64 1.399(7) yes . . C63B C62 1.477(6) yes . . C63B C64 1.529(6) yes . . O1 C6 1.3898(18) yes . . O1 C7 1.3701(16) yes . . O2 C11 1.502(2) yes . . O2 C18 1.3636(16) yes . . O3 C18 1.208(2) yes . . O11 C36 1.3887(19) yes . . O11 C37 1.3777(19) yes . . O12 C41 1.510(2) yes . . O12 C48 1.3584(17) yes . . O13 C48 1.2099(19) yes . . O61 C61 1.433(2) yes . . O61 C64 1.423(4) yes . . N1 C4 1.3714(17) yes . . N1 C19 1.459(2) yes . . N1 C21 1.4588(19) yes . . N11 C34 1.370(3) yes . . N11 C51 1.447(2) yes . . C1 C2 1.400(2) yes . . C1 C6 1.3902(19) yes . . C1 C11 1.4992(19) yes . . C2 C3 1.3782(19) yes . . C3 C4 1.416(2) yes . . C4 C5 1.409(2) yes . . C5 C6 1.3845(18) yes . . C7 C8 1.394(2) yes . . C7 C10 1.3972(19) yes . . C8 C37 1.385(2) yes . . C9 C10 1.391(2) yes . . C9 C40 1.387(2) yes . . C10 C11 1.506(2) yes . . C11 C12 1.510(2) yes . . C12 C13 1.389(3) yes . . C12 C17 1.382(2) yes . . C13 C14 1.389(2) yes . . C14 C15 1.390(2) yes . . C15 C16 1.389(3) yes . . C16 C17 1.388(2) yes . . C17 C18 1.474(2) yes . . C19 C20 1.519(3) yes . . C21 C22 1.517(3) yes . . C31 C32 1.396(2) yes . . C31 C36 1.3874(19) yes . . C31 C41 1.497(2) yes . . C32 C33 1.369(3) yes . . C33 C34 1.416(2) yes . . C34 C35 1.403(2) yes . . C35 C36 1.386(2) yes . . C37 C40 1.4034(19) yes . . C40 C41 1.505(2) yes . . C41 C42 1.509(2) yes . . C42 C43 1.389(2) yes . . C42 C47 1.382(2) yes . . C43 C44 1.394(2) yes . . C44 C45 1.394(3) yes . . C45 C46 1.384(3) yes . . C46 C47 1.391(2) yes . . C47 C48 1.475(2) yes . . C51 C52 1.504(3) yes . . C61 C62 1.511(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_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C50A C49A N11 105.2(3) yes . . . C50B C49B N11 103.5(3) yes . . . C62 C63A C64 101.0(4) yes . . . C62 C63B C64 102.5(3) yes . . . C6 O1 C7 118.51(10) yes . . . C11 O2 C18 111.21(12) yes . . . C36 O11 C37 117.81(11) yes . . . C41 O12 C48 111.17(12) yes . . . C61 O61 C64 108.65(18) yes . . . C4 N1 C19 121.70(12) yes . . . C4 N1 C21 121.46(13) yes . . . C19 N1 C21 116.76(11) yes . . . C49A N11 C34 120.22(18) yes . . . C49A N11 C51 116.2(2) yes . . . C49B N11 C34 118.1(2) yes . . . C49B N11 C51 113.05(19) yes . . . C34 N11 C51 122.04(17) yes . . . C2 C1 C6 116.45(12) yes . . . C2 C1 C11 121.55(12) yes . . . C6 C1 C11 121.80(13) yes . . . C1 C2 C3 122.00(13) yes . . . C2 C3 C4 121.19(14) yes . . . N1 C4 C3 121.19(13) yes . . . N1 C4 C5 121.79(12) yes . . . C3 C4 C5 117.02(12) yes . . . C4 C5 C6 120.28(13) yes . . . O1 C6 C1 122.48(12) yes . . . O1 C6 C5 114.46(12) yes . . . C1 C6 C5 123.05(14) yes . . . O1 C7 C8 115.44(12) yes . . . O1 C7 C10 123.13(13) yes . . . C8 C7 C10 121.43(12) yes . . . C7 C8 C37 118.52(12) yes . . . C10 C9 C40 122.40(13) yes . . . C7 C10 C9 118.09(14) yes . . . C7 C10 C11 121.24(13) yes . . . C9 C10 C11 120.63(12) yes . . . O2 C11 C1 108.47(14) yes . . . O2 C11 C10 106.85(11) yes . . . O2 C11 C12 101.92(11) yes . . . C1 C11 C10 110.94(12) yes . . . C1 C11 C12 114.18(12) yes . . . C10 C11 C12 113.70(14) yes . . . C11 C12 C13 128.99(14) yes . . . C11 C12 C17 110.09(14) yes . . . C13 C12 C17 120.91(13) yes . . . C12 C13 C14 117.65(15) yes . . . C13 C14 C15 121.32(18) yes . . . C14 C15 C16 120.89(15) yes . . . C15 C16 C17 117.45(15) yes . . . C12 C17 C16 121.72(16) yes . . . C12 C17 C18 108.39(12) yes . . . C16 C17 C18 129.89(15) yes . . . O2 C18 O3 121.72(15) yes . . . O2 C18 C17 108.33(13) yes . . . O3 C18 C17 129.94(13) yes . . . N1 C19 C20 114.90(14) yes . . . N1 C21 C22 113.90(15) yes . . . C32 C31 C36 116.38(15) yes . . . C32 C31 C41 122.85(13) yes . . . C36 C31 C41 120.43(15) yes . . . C31 C32 C33 122.21(15) yes . . . C32 C33 C34 120.91(17) yes . . . N11 C34 C33 121.13(16) yes . . . N11 C34 C35 121.52(14) yes . . . C33 C34 C35 117.35(17) yes . . . C34 C35 C36 119.85(13) yes . . . O11 C36 C31 122.04(14) yes . . . O11 C36 C35 114.89(12) yes . . . C31 C36 C35 123.05(15) yes . . . O11 C37 C8 116.17(12) yes . . . O11 C37 C40 121.89(13) yes . . . C8 C37 C40 121.93(14) yes . . . C9 C40 C37 117.61(13) yes . . . C9 C40 C41 122.00(12) yes . . . C37 C40 C41 120.39(14) yes . . . O12 C41 C31 107.05(11) yes . . . O12 C41 C40 107.84(14) yes . . . O12 C41 C42 101.91(11) yes . . . C31 C41 C40 110.14(11) yes . . . C31 C41 C42 115.35(15) yes . . . C40 C41 C42 113.74(12) yes . . . C41 C42 C43 129.35(13) yes . . . C41 C42 C47 109.86(14) yes . . . C43 C42 C47 120.77(13) yes . . . C42 C43 C44 117.82(15) yes . . . C43 C44 C45 121.15(18) yes . . . C44 C45 C46 120.77(16) yes . . . C45 C46 C47 117.81(16) yes . . . C42 C47 C46 121.67(16) yes . . . C42 C47 C48 108.70(13) yes . . . C46 C47 C48 129.63(15) yes . . . O12 C48 O13 122.13(15) yes . . . O12 C48 C47 108.26(13) yes . . . O13 C48 C47 129.61(14) yes . . . N11 C51 C52 113.65(18) yes . . . O61 C61 C62 107.39(19) yes . . . C63A C62 C61 100.4(2) yes . . . C63B C62 C61 105.3(3) yes . . . C63A C64 O61 108.4(3) yes . . . C63B C64 O61 107.9(3) yes . . . #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================