data_global _audit_creation_date 2016-06-27 _audit_creation_method 'by CrystalStructure 4.2.1' _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 (2016). CrystalStructure. Version 4.2.1. Rigaku Corporation, Tokyo, Japan. L. Palatinus, G. Chapuis (2007) J. Appl. Cryst. 40, 786-790 SuperFlip Sheldrick, G.M. (2008) SHELXL Version 2014/7, Acta Cryst. A64, 112-122. 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_160627_Sakamaki_4p_dcm_MeOH_a #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C53 H46 Cl2 N4 O4' _chemical_formula_moiety 'C53 H46 Cl2 N4 O4' _chemical_formula_weight 873.88 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' _space_group_IT_number 14 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 '+X,+Y,+Z' 2 '-X,1/2+Y,1/2-Z' 3 '-X,-Y,-Z' 4 '+X,-1/2-Y,-1/2+Z' #------------------------------------------------------------------------------ _cell_length_a 12.216(2) _cell_length_b 15.614(3) _cell_length_c 23.054(4) _cell_angle_alpha 90.0000 _cell_angle_beta 92.341(3) _cell_angle_gamma 90.0000 _cell_volume 4393.6(14) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9307 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 27.48 _cell_measurement_temperature 143 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832.00 _exptl_absorpt_coefficient_mu 0.200 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.690 _exptl_absorpt_correction_T_max 0.961 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 143 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_reflns_number 35570 _diffrn_reflns_av_R_equivalents 0.1443 _diffrn_reflns_theta_max 27.494 _diffrn_reflns_theta_min 3.097 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 29 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? _reflns_number_total 10009 _reflns_number_gt 3530 _reflns_threshold_expression F^2^>2.0\s(F^2^) _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . #============================================================================== # 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). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.1455 _refine_ls_R_factor_gt 0.0778 _refine_ls_wR_factor_ref 0.2234 _refine_ls_wR_factor_gt 0.1886 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 10009 _refine_ls_number_parameters 568 _refine_ls_goodness_of_fit_ref 0.850 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0876P)^2^] 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 0.004 _refine_diff_density_max 1.10 _refine_diff_density_min -0.83 _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) ; 'Cl' 'Cl' 0.1484 0.1585 ; 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_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl -0.38842(19) 1.15211(16) 0.38369(8) 0.1472(9) Uani 1 1 d . . . . . Cl2 Cl -0.58715(17) 1.10224(19) 0.32788(8) 0.1549(10) Uani 1 1 d . . . . . O1 O 0.2672(2) 0.50184(14) 0.46603(10) 0.0430(7) Uani 1 1 d . . . . . O2 O 0.5770(2) 1.25362(17) 0.70506(10) 0.0479(7) Uani 1 1 d . . . . . O3 O -0.1566(2) 1.65498(15) 0.33296(10) 0.0438(7) Uani 1 1 d . . . . . O4 O -0.4929(2) 0.91956(18) 0.13446(11) 0.0541(8) Uani 1 1 d . . . . . N1 N 0.2103(2) 0.84598(16) 0.40544(11) 0.0330(7) Uani 1 1 d . . . . . N2 N 0.2745(3) 1.15132(17) 0.53067(12) 0.0378(7) Uani 1 1 d . . . . . N3 N -0.0323(3) 1.31889(18) 0.38586(12) 0.0422(8) Uani 1 1 d . . . . . N4 N -0.1308(3) 1.00343(18) 0.27908(13) 0.0466(9) Uani 1 1 d . . . . . C1 C 0.2286(3) 0.9142(2) 0.44695(14) 0.0315(8) Uani 1 1 d . . . . . C2 C 0.3322(3) 0.9373(2) 0.46717(18) 0.0529(11) Uani 1 1 d . . . . . H2 H 0.3929 0.9016 0.4596 0.063 Uiso 1 1 calc R U . . . C3 C 0.3484(3) 1.0129(2) 0.49860(18) 0.0546(11) Uani 1 1 d . . . . . H3 H 0.4203 1.0282 0.5121 0.066 Uiso 1 1 calc R U . . . C4 C 0.2619(3) 1.0659(2) 0.51040(13) 0.0337(8) Uani 1 1 d . . . . . C5 C 0.1567(3) 1.0379(2) 0.49522(13) 0.0355(8) Uani 1 1 d . . . . . H5 H 0.0954 1.0703 0.5067 0.043 Uiso 1 1 calc R U . . . C6 C 0.1401(3) 0.9633(2) 0.46354(14) 0.0360(8) Uani 1 1 d . . . . . H6 H 0.0677 0.9454 0.4531 0.043 Uiso 1 1 calc R U . . . C7 C 0.2152(3) 1.2132(2) 0.49507(14) 0.0314(8) Uani 1 1 d . . . . . C8 C 0.1433(3) 1.2717(2) 0.51790(15) 0.0342(8) Uani 1 1 d . . . . . H8 H 0.1469 1.2831 0.5584 0.041 Uiso 1 1 calc R U . . . C9 C 0.0664(3) 1.3140(2) 0.48247(15) 0.0393(9) Uani 1 1 d . . . . . H9 H 0.0177 1.3542 0.4986 0.047 Uiso 1 1 calc R U . . . C10 C 0.0611(3) 1.2971(2) 0.42317(15) 0.0368(9) Uani 1 1 d . . . . . C11 C 0.1404(3) 1.2463(2) 0.39990(15) 0.0377(9) Uani 1 1 d . . . . . H11 H 0.1423 1.2402 0.3590 0.045 Uiso 1 1 calc R U . . . C12 C 0.2175(3) 1.2042(2) 0.43520(15) 0.0357(8) Uani 1 1 d . . . . . H12 H 0.2716 1.1693 0.4185 0.043 Uiso 1 1 calc R U . . . C13 C -0.0768(3) 1.2456(2) 0.35625(15) 0.0357(9) Uani 1 1 d . . . . . C14 C -0.0854(3) 1.2384(2) 0.29619(15) 0.0418(10) Uani 1 1 d . . . . . H14 H -0.0755 1.2875 0.2727 0.050 Uiso 1 1 calc R U . . . C15 C -0.1084(3) 1.1598(2) 0.27032(14) 0.0426(10) Uani 1 1 d . . . . . H15 H -0.1137 1.1555 0.2292 0.051 Uiso 1 1 calc R U . . . C16 C -0.1239(3) 1.0874(2) 0.30399(14) 0.0369(9) Uani 1 1 d . . . . . C17 C -0.1220(3) 1.0960(2) 0.36418(15) 0.0366(9) Uani 1 1 d . . . . . H17 H -0.1374 1.0478 0.3876 0.044 Uiso 1 1 calc R U . . . C18 C -0.0982(3) 1.1734(2) 0.38990(14) 0.0352(9) Uani 1 1 d . . . . . H18 H -0.0961 1.1780 0.4310 0.042 Uiso 1 1 calc R U . . . C19 C -0.0443(3) 0.9480(2) 0.29957(14) 0.0362(9) Uani 1 1 d . . . . . C20 C -0.0623(3) 0.8713(2) 0.32853(14) 0.0376(9) Uani 1 1 d . . . . . H20 H -0.1333 0.8463 0.3272 0.045 Uiso 1 1 calc R U . . . C21 C 0.0244(3) 0.8309(2) 0.35959(14) 0.0349(8) Uani 1 1 d . . . . . H21 H 0.0125 0.7779 0.3786 0.042 Uiso 1 1 calc R U . . . C22 C 0.1271(3) 0.8682(2) 0.36250(14) 0.0322(8) Uani 1 1 d . . . . . C23 C 0.1470(3) 0.9394(2) 0.32794(13) 0.0355(9) Uani 1 1 d . . . . . H23 H 0.2194 0.9612 0.3258 0.043 Uiso 1 1 calc R U . . . C24 C 0.0618(3) 0.9783(2) 0.29692(14) 0.0391(9) Uani 1 1 d . . . . . H24 H 0.0761 1.0267 0.2734 0.047 Uiso 1 1 calc R U . . . C25 C 0.2247(3) 0.7600(2) 0.42312(13) 0.0284(8) Uani 1 1 d . . . . . C26 C 0.2354(3) 0.7362(2) 0.48085(14) 0.0334(8) Uani 1 1 d . . . . . H26 H 0.2334 0.7790 0.5101 0.040 Uiso 1 1 calc R U . . . C27 C 0.2492(3) 0.6507(2) 0.49706(14) 0.0331(8) Uani 1 1 d . . . . . H27 H 0.2556 0.6357 0.5370 0.040 Uiso 1 1 calc R U . . . C28 C 0.2536(3) 0.5882(2) 0.45535(14) 0.0327(8) Uani 1 1 d . . . . . C29 C 0.2441(3) 0.6109(2) 0.39687(14) 0.0327(8) Uani 1 1 d . . . . . H29 H 0.2472 0.5679 0.3678 0.039 Uiso 1 1 calc R U . . . C30 C 0.2301(3) 0.6953(2) 0.38101(14) 0.0308(8) Uani 1 1 d . . . . . H30 H 0.2240 0.7100 0.3410 0.037 Uiso 1 1 calc R U . . . C31 C 0.3521(3) 1.1758(2) 0.57448(14) 0.0317(8) Uani 1 1 d . . . . . C32 C 0.3690(3) 1.1245(2) 0.62329(14) 0.0359(9) Uani 1 1 d . . . . . H32 H 0.3280 1.0732 0.6269 0.043 Uiso 1 1 calc R U . . . C33 C 0.4454(3) 1.1474(2) 0.66697(14) 0.0351(8) Uani 1 1 d . . . . . H33 H 0.4581 1.1109 0.6995 0.042 Uiso 1 1 calc R U . . . C34 C 0.5030(3) 1.2236(2) 0.66303(14) 0.0339(8) Uani 1 1 d . . . . . C35 C 0.4869(3) 1.2756(2) 0.61427(14) 0.0363(9) Uani 1 1 d . . . . . H35 H 0.5268 1.3275 0.6109 0.044 Uiso 1 1 calc R U . . . C36 C 0.4119(3) 1.2506(2) 0.57073(14) 0.0354(8) Uani 1 1 d . . . . . H36 H 0.4014 1.2858 0.5374 0.042 Uiso 1 1 calc R U . . . C37 C -0.0661(3) 1.4032(2) 0.37300(14) 0.0340(8) Uani 1 1 d . . . . . C38 C 0.0028(3) 1.4722(2) 0.38620(14) 0.0352(8) Uani 1 1 d . . . . . H38 H 0.0727 1.4626 0.4046 0.042 Uiso 1 1 calc R U . . . C39 C -0.0309(3) 1.5555(2) 0.37245(14) 0.0333(8) Uani 1 1 d . . . . . H39 H 0.0162 1.6025 0.3816 0.040 Uiso 1 1 calc R U . . . C40 C -0.1322(3) 1.5700(2) 0.34562(14) 0.0323(8) Uani 1 1 d . . . . . C41 C -0.2023(3) 1.5017(2) 0.33280(13) 0.0327(8) Uani 1 1 d . . . . . H41 H -0.2723 1.5113 0.3146 0.039 Uiso 1 1 calc R U . . . C42 C -0.1683(3) 1.4191(2) 0.34707(14) 0.0357(9) Uani 1 1 d . . . . . H42 H -0.2164 1.3724 0.3388 0.043 Uiso 1 1 calc R U . . . C43 C -0.2224(3) 0.9780(2) 0.24461(13) 0.0334(8) Uani 1 1 d . . . . . C44 C -0.2191(3) 0.9078(2) 0.20806(14) 0.0371(9) Uani 1 1 d . . . . . H44 H -0.1547 0.8737 0.2080 0.045 Uiso 1 1 calc R U . . . C45 C -0.3081(3) 0.8860(2) 0.17133(14) 0.0370(9) Uani 1 1 d . . . . . H45 H -0.3042 0.8371 0.1470 0.044 Uiso 1 1 calc R U . . . C46 C -0.4021(3) 0.9353(2) 0.17020(14) 0.0362(9) Uani 1 1 d . . . . . C47 C -0.4072(3) 1.0051(2) 0.20736(15) 0.0389(9) Uani 1 1 d . . . . . H47 H -0.4719 1.0388 0.2075 0.047 Uiso 1 1 calc R U . . . C48 C -0.3198(3) 1.0258(2) 0.24390(14) 0.0361(9) Uani 1 1 d . . . . . H48 H -0.3252 1.0734 0.2692 0.043 Uiso 1 1 calc R U . . . C49 C 0.2700(4) 0.4769(2) 0.52534(16) 0.0499(11) Uani 1 1 d . . . . . H49A H 0.2800 0.4147 0.5282 0.060 Uiso 1 1 calc R U . . . H49B H 0.3311 0.5057 0.5462 0.060 Uiso 1 1 calc R U . . . H49C H 0.2010 0.4930 0.5426 0.060 Uiso 1 1 calc R U . . . C50 C 0.6119(4) 1.1974(3) 0.74938(18) 0.0770(16) Uani 1 1 d . . . . . H50A H 0.6639 1.2269 0.7760 0.092 Uiso 1 1 calc R U . . . H50B H 0.5486 1.1783 0.7707 0.092 Uiso 1 1 calc R U . . . H50C H 0.6477 1.1477 0.7324 0.092 Uiso 1 1 calc R U . . . C51 C -0.2495(4) 1.6712(2) 0.29636(17) 0.0542(11) Uani 1 1 d . . . . . H51A H -0.2579 1.7331 0.2907 0.065 Uiso 1 1 calc R U . . . H51B H -0.2404 1.6435 0.2587 0.065 Uiso 1 1 calc R U . . . H51C H -0.3148 1.6482 0.3142 0.065 Uiso 1 1 calc R U . . . C52 C -0.4756(4) 0.8669(3) 0.0859(2) 0.0738(15) Uani 1 1 d . . . . . H52A H -0.5447 0.8596 0.0634 0.089 Uiso 1 1 calc R U . . . H52B H -0.4214 0.8937 0.0615 0.089 Uiso 1 1 calc R U . . . H52C H -0.4486 0.8108 0.0991 0.089 Uiso 1 1 calc R U . . . C53 C -0.5061(8) 1.0920(7) 0.3835(5) 0.236(7) Uani 1 1 d . . . . . H53A H -0.4853 1.0309 0.3871 0.283 Uiso 1 1 calc R U . . . H53B H -0.5467 1.1072 0.4184 0.283 Uiso 1 1 calc R U . . . 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 Cl1 0.1217(18) 0.185(2) 0.1345(15) -0.0623(14) 0.0062(13) -0.0205(16) Cl2 0.0808(13) 0.292(3) 0.0921(12) -0.0410(14) 0.0022(10) 0.0256(17) O1 0.0575(19) 0.0247(13) 0.0465(15) 0.0005(11) -0.0030(13) 0.0039(12) O2 0.0490(18) 0.0510(17) 0.0419(15) 0.0044(12) -0.0192(12) -0.0112(14) O3 0.0464(17) 0.0272(13) 0.0564(16) 0.0031(11) -0.0173(13) 0.0085(12) O4 0.0342(16) 0.0653(19) 0.0615(17) -0.0089(15) -0.0148(13) -0.0033(14) N1 0.0384(18) 0.0224(14) 0.0371(16) -0.0019(12) -0.0130(13) 0.0021(13) N2 0.0419(19) 0.0225(15) 0.0471(17) -0.0052(13) -0.0193(14) 0.0057(14) N3 0.051(2) 0.0207(15) 0.0521(18) -0.0053(13) -0.0292(15) 0.0071(14) N4 0.057(2) 0.0261(16) 0.0541(19) -0.0085(14) -0.0312(16) 0.0106(15) C1 0.038(2) 0.0222(17) 0.0338(19) -0.0005(14) -0.0066(15) 0.0007(16) C2 0.037(2) 0.028(2) 0.091(3) -0.018(2) -0.026(2) 0.0130(18) C3 0.033(2) 0.036(2) 0.093(3) -0.016(2) -0.030(2) 0.0045(18) C4 0.046(2) 0.0214(17) 0.0323(19) 0.0019(14) -0.0131(16) 0.0028(16) C5 0.038(2) 0.036(2) 0.0327(19) -0.0061(16) 0.0032(16) 0.0000(17) C6 0.029(2) 0.039(2) 0.040(2) -0.0056(16) 0.0029(16) -0.0112(17) C7 0.030(2) 0.0236(18) 0.040(2) 0.0023(15) -0.0095(15) -0.0010(15) C8 0.037(2) 0.0259(18) 0.039(2) -0.0027(15) -0.0112(16) 0.0038(16) C9 0.041(2) 0.0279(19) 0.048(2) -0.0073(16) -0.0117(17) 0.0074(17) C10 0.040(2) 0.0254(18) 0.043(2) -0.0003(16) -0.0151(17) 0.0033(17) C11 0.043(2) 0.036(2) 0.033(2) 0.0074(16) -0.0034(16) 0.0029(18) C12 0.032(2) 0.0319(19) 0.043(2) 0.0024(16) 0.0011(16) 0.0047(17) C13 0.038(2) 0.0290(19) 0.039(2) -0.0061(16) -0.0137(16) 0.0034(17) C14 0.056(3) 0.0263(19) 0.042(2) 0.0060(16) -0.0161(18) 0.0067(18) C15 0.065(3) 0.033(2) 0.0287(19) 0.0002(16) -0.0145(18) 0.0089(19) C16 0.045(2) 0.0287(19) 0.036(2) -0.0050(16) -0.0141(16) 0.0055(17) C17 0.038(2) 0.0287(19) 0.042(2) 0.0006(16) -0.0054(16) -0.0016(16) C18 0.042(2) 0.035(2) 0.0284(18) -0.0037(15) -0.0079(15) 0.0016(17) C19 0.052(3) 0.0273(19) 0.0279(18) -0.0051(15) -0.0143(16) 0.0070(18) C20 0.037(2) 0.0268(19) 0.047(2) -0.0035(16) -0.0138(17) 0.0000(16) C21 0.037(2) 0.0261(18) 0.041(2) 0.0010(15) -0.0106(16) -0.0007(16) C22 0.038(2) 0.0276(18) 0.0307(18) -0.0042(15) -0.0057(15) 0.0061(16) C23 0.042(2) 0.033(2) 0.0322(19) -0.0001(15) 0.0017(16) 0.0005(17) C24 0.058(3) 0.030(2) 0.0286(19) 0.0024(15) 0.0019(17) 0.0030(19) C25 0.0259(18) 0.0239(17) 0.0349(19) 0.0006(14) -0.0040(14) 0.0002(14) C26 0.036(2) 0.0284(19) 0.036(2) -0.0039(15) 0.0003(15) 0.0060(16) C27 0.037(2) 0.0297(19) 0.0321(19) 0.0008(15) -0.0038(15) 0.0025(16) C28 0.032(2) 0.0254(18) 0.040(2) 0.0027(15) -0.0037(15) 0.0027(15) C29 0.030(2) 0.0296(19) 0.039(2) -0.0078(15) 0.0048(15) 0.0020(15) C30 0.031(2) 0.0317(19) 0.0295(18) -0.0042(15) -0.0029(14) 0.0019(16) C31 0.032(2) 0.0276(18) 0.0351(19) -0.0021(15) -0.0092(15) 0.0041(15) C32 0.038(2) 0.0282(19) 0.041(2) 0.0024(16) -0.0025(17) -0.0037(16) C33 0.037(2) 0.036(2) 0.0311(19) 0.0013(15) -0.0051(15) 0.0021(17) C34 0.0254(19) 0.041(2) 0.035(2) -0.0029(16) -0.0047(15) -0.0026(16) C35 0.034(2) 0.033(2) 0.042(2) 0.0026(16) -0.0075(16) -0.0065(16) C36 0.039(2) 0.0318(19) 0.0343(19) 0.0076(15) -0.0089(16) -0.0004(17) C37 0.040(2) 0.0284(18) 0.0321(18) -0.0022(15) -0.0119(15) 0.0054(17) C38 0.034(2) 0.0317(19) 0.039(2) -0.0017(16) -0.0078(16) 0.0049(16) C39 0.033(2) 0.0266(18) 0.040(2) -0.0008(15) -0.0034(16) -0.0006(16) C40 0.037(2) 0.0250(18) 0.0344(19) 0.0000(14) -0.0014(15) 0.0040(16) C41 0.034(2) 0.0310(19) 0.0326(18) -0.0005(14) -0.0106(15) 0.0069(16) C42 0.044(2) 0.0274(19) 0.0348(19) -0.0041(15) -0.0095(16) 0.0016(17) C43 0.043(2) 0.0276(18) 0.0286(18) 0.0002(14) -0.0105(15) -0.0010(16) C44 0.041(2) 0.0236(18) 0.045(2) -0.0014(16) -0.0098(17) 0.0070(16) C45 0.041(2) 0.036(2) 0.0332(19) -0.0038(16) -0.0060(16) -0.0037(18) C46 0.030(2) 0.041(2) 0.037(2) 0.0018(17) -0.0063(15) -0.0091(17) C47 0.035(2) 0.041(2) 0.040(2) 0.0061(17) -0.0007(16) 0.0049(18) C48 0.043(2) 0.034(2) 0.0320(19) 0.0005(15) -0.0014(16) 0.0022(17) C49 0.060(3) 0.033(2) 0.056(3) 0.0063(18) -0.011(2) -0.001(2) C50 0.089(4) 0.081(4) 0.057(3) 0.026(3) -0.039(3) -0.028(3) C51 0.058(3) 0.035(2) 0.068(3) 0.0052(19) -0.016(2) 0.015(2) C52 0.061(3) 0.077(3) 0.080(3) -0.028(3) -0.035(3) -0.001(3) C53 0.102(8) 0.256(13) 0.355(16) 0.188(12) 0.070(9) 0.065(8) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2006)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'Superflip (Palatinus, et al., 2007)' _computing_structure_refinement 'SHELXL Version 2014/7 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.2.1 (Rigaku, 2016)' _computing_molecular_graphics 'CrystalStructure 4.2.1' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Cl1 C53 1.717(11) . ? Cl2 C53 1.596(11) . ? O1 C28 1.380(4) . ? O1 C49 1.421(4) . ? O2 C34 1.380(4) . ? O2 C50 1.400(5) . ? O3 C40 1.388(4) . ? O3 C51 1.409(4) . ? O4 C46 1.376(4) . ? O4 C52 1.412(5) . ? N1 C25 1.413(4) . ? N1 C22 1.432(4) . ? N1 C1 1.443(4) . ? N2 C31 1.409(4) . ? N2 C4 1.420(4) . ? N2 C7 1.444(4) . ? N3 C37 1.408(4) . ? N3 C13 1.428(4) . ? N3 C10 1.441(4) . ? N4 C43 1.403(4) . ? N4 C19 1.431(4) . ? N4 C16 1.433(4) . ? C1 C2 1.380(5) . ? C1 C6 1.391(5) . ? C2 C3 1.395(5) . ? C2 H2 0.9500 . ? C3 C4 1.378(5) . ? C3 H3 0.9500 . ? C4 C5 1.388(5) . ? C5 C6 1.386(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.386(5) . ? C7 C12 1.389(5) . ? C8 C9 1.387(5) . ? C8 H8 0.9500 . ? C9 C10 1.392(5) . ? C9 H9 0.9500 . ? C10 C11 1.377(5) . ? C11 C12 1.385(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.389(5) . ? C13 C18 1.399(5) . ? C14 C15 1.388(5) . ? C14 H14 0.9500 . ? C15 C16 1.388(5) . ? C15 H15 0.9500 . ? C16 C17 1.393(5) . ? C17 C18 1.372(5) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.383(5) . ? C19 C20 1.394(5) . ? C20 C21 1.403(5) . ? C20 H20 0.9500 . ? C21 C22 1.384(5) . ? C21 H21 0.9500 . ? C22 C23 1.395(5) . ? C23 C24 1.380(5) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.383(4) . ? C25 C30 1.404(4) . ? C26 C27 1.395(4) . ? C26 H26 0.9500 . ? C27 C28 1.372(4) . ? C27 H27 0.9500 . ? C28 C29 1.394(5) . ? C29 C30 1.376(5) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.382(5) . ? C31 C32 1.390(4) . ? C32 C33 1.391(5) . ? C32 H32 0.9500 . ? C33 C34 1.387(5) . ? C33 H33 0.9500 . ? C34 C35 1.394(5) . ? C35 C36 1.387(5) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.385(5) . ? C37 C38 1.392(5) . ? C38 C39 1.397(4) . ? C38 H38 0.9500 . ? C39 C40 1.380(5) . ? C39 H39 0.9500 . ? C40 C41 1.392(5) . ? C41 C42 1.390(4) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.384(5) . ? C43 C48 1.403(5) . ? C44 C45 1.393(5) . ? C44 H44 0.9500 . ? C45 C46 1.382(5) . ? C45 H45 0.9500 . ? C46 C47 1.388(5) . ? C47 C48 1.372(5) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? 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 C28 O1 C49 116.0(3) . . ? C34 O2 C50 118.1(3) . . ? C40 O3 C51 117.2(3) . . ? C46 O4 C52 115.8(3) . . ? C25 N1 C22 120.5(3) . . ? C25 N1 C1 119.7(3) . . ? C22 N1 C1 111.4(3) . . ? C31 N2 C4 123.5(3) . . ? C31 N2 C7 122.3(3) . . ? C4 N2 C7 113.3(3) . . ? C37 N3 C13 123.1(3) . . ? C37 N3 C10 124.4(3) . . ? C13 N3 C10 111.9(3) . . ? C43 N4 C19 125.2(3) . . ? C43 N4 C16 121.2(3) . . ? C19 N4 C16 113.0(3) . . ? C2 C1 C6 118.4(3) . . ? C2 C1 N1 122.2(3) . . ? C6 C1 N1 119.2(3) . . ? C1 C2 C3 120.4(4) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C4 C3 C2 121.1(4) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 118.1(3) . . ? C3 C4 N2 123.7(3) . . ? C5 C4 N2 117.7(3) . . ? C6 C5 C4 120.7(3) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C1 120.7(3) . . ? C5 C6 H6 119.7 . . ? C1 C6 H6 119.7 . . ? C8 C7 C12 118.9(3) . . ? C8 C7 N2 122.5(3) . . ? C12 C7 N2 117.9(3) . . ? C7 C8 C9 121.0(3) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C8 C9 C10 119.4(3) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C11 C10 C9 119.1(3) . . ? C11 C10 N3 117.1(3) . . ? C9 C10 N3 123.0(3) . . ? C10 C11 C12 121.1(3) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C11 C12 C7 119.7(3) . . ? C11 C12 H12 120.2 . . ? C7 C12 H12 120.2 . . ? C14 C13 C18 118.6(3) . . ? C14 C13 N3 123.6(3) . . ? C18 C13 N3 117.2(3) . . ? C15 C14 C13 120.4(3) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C16 C15 C14 120.6(3) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 118.8(3) . . ? C15 C16 N4 121.9(3) . . ? C17 C16 N4 119.0(3) . . ? C18 C17 C16 120.6(3) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C13 120.8(3) . . ? C17 C18 H18 119.6 . . ? C13 C18 H18 119.6 . . ? C24 C19 C20 118.8(3) . . ? C24 C19 N4 117.3(3) . . ? C20 C19 N4 123.3(4) . . ? C19 C20 C21 120.0(4) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 120.0(3) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 119.1(3) . . ? C21 C22 N1 123.2(3) . . ? C23 C22 N1 117.0(3) . . ? C24 C23 C22 120.1(4) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C19 121.0(3) . . ? C23 C24 H24 119.5 . . ? C19 C24 H24 119.5 . . ? C26 C25 C30 117.9(3) . . ? C26 C25 N1 122.6(3) . . ? C30 C25 N1 119.5(3) . . ? C25 C26 C27 121.3(3) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C28 C27 C26 120.0(3) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 O1 125.3(3) . . ? C27 C28 C29 119.5(3) . . ? O1 C28 C29 115.2(3) . . ? C30 C29 C28 120.3(3) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C25 120.9(3) . . ? C29 C30 H30 119.5 . . ? C25 C30 H30 119.5 . . ? C36 C31 C32 118.4(3) . . ? C36 C31 N2 121.7(3) . . ? C32 C31 N2 119.9(3) . . ? C31 C32 C33 120.7(3) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C34 C33 C32 120.0(3) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? O2 C34 C33 124.4(3) . . ? O2 C34 C35 115.7(3) . . ? C33 C34 C35 119.8(3) . . ? C36 C35 C34 119.1(3) . . ? C36 C35 H35 120.5 . . ? C34 C35 H35 120.5 . . ? C31 C36 C35 121.9(3) . . ? C31 C36 H36 119.0 . . ? C35 C36 H36 119.0 . . ? C42 C37 C38 118.9(3) . . ? C42 C37 N3 120.6(3) . . ? C38 C37 N3 120.6(3) . . ? C37 C38 C39 120.1(3) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C40 C39 C38 120.3(3) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C39 C40 O3 115.6(3) . . ? C39 C40 C41 120.1(3) . . ? O3 C40 C41 124.3(3) . . ? C42 C41 C40 119.1(3) . . ? C42 C41 H41 120.4 . . ? C40 C41 H41 120.4 . . ? C37 C42 C41 121.5(3) . . ? C37 C42 H42 119.2 . . ? C41 C42 H42 119.2 . . ? C44 C43 C48 117.4(3) . . ? C44 C43 N4 121.8(3) . . ? C48 C43 N4 120.8(3) . . ? C43 C44 C45 121.4(4) . . ? C43 C44 H44 119.3 . . ? C45 C44 H44 119.3 . . ? C46 C45 C44 120.2(3) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? O4 C46 C45 124.1(3) . . ? O4 C46 C47 117.0(3) . . ? C45 C46 C47 118.9(3) . . ? C48 C47 C46 120.7(4) . . ? C48 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? C47 C48 C43 121.3(3) . . ? C47 C48 H48 119.3 . . ? C43 C48 H48 119.3 . . ? O1 C49 H49A 109.5 . . ? O1 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? O1 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? O2 C50 H50A 109.5 . . ? O2 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? O2 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O3 C51 H51A 109.5 . . ? O3 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O3 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O4 C52 H52A 109.5 . . ? O4 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? O4 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? Cl2 C53 Cl1 116.0(5) . . ? Cl2 C53 H53A 108.3 . . ? Cl1 C53 H53A 108.3 . . ? Cl2 C53 H53B 108.3 . . ? Cl1 C53 H53B 108.3 . . ? H53A C53 H53B 107.4 . . ? 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 C25 N1 C1 C2 73.0(4) . . . . ? C22 N1 C1 C2 -138.6(4) . . . . ? C25 N1 C1 C6 -112.6(4) . . . . ? C22 N1 C1 C6 35.8(4) . . . . ? C6 C1 C2 C3 -6.3(6) . . . . ? N1 C1 C2 C3 168.1(4) . . . . ? C1 C2 C3 C4 0.3(6) . . . . ? C2 C3 C4 C5 6.3(6) . . . . ? C2 C3 C4 N2 -165.8(4) . . . . ? C31 N2 C4 C3 -43.8(5) . . . . ? C7 N2 C4 C3 125.3(4) . . . . ? C31 N2 C4 C5 144.0(3) . . . . ? C7 N2 C4 C5 -46.9(4) . . . . ? C3 C4 C5 C6 -6.8(5) . . . . ? N2 C4 C5 C6 165.7(3) . . . . ? C4 C5 C6 C1 0.8(5) . . . . ? C2 C1 C6 C5 5.8(5) . . . . ? N1 C1 C6 C5 -168.8(3) . . . . ? C31 N2 C7 C8 -63.4(5) . . . . ? C4 N2 C7 C8 127.4(4) . . . . ? C31 N2 C7 C12 127.0(4) . . . . ? C4 N2 C7 C12 -42.2(4) . . . . ? C12 C7 C8 C9 7.1(5) . . . . ? N2 C7 C8 C9 -162.4(3) . . . . ? C7 C8 C9 C10 0.2(6) . . . . ? C8 C9 C10 C11 -7.5(5) . . . . ? C8 C9 C10 N3 162.7(3) . . . . ? C37 N3 C10 C11 -123.3(4) . . . . ? C13 N3 C10 C11 47.6(5) . . . . ? C37 N3 C10 C9 66.4(5) . . . . ? C13 N3 C10 C9 -122.7(4) . . . . ? C9 C10 C11 C12 7.5(5) . . . . ? N3 C10 C11 C12 -163.2(3) . . . . ? C10 C11 C12 C7 -0.1(6) . . . . ? C8 C7 C12 C11 -7.1(5) . . . . ? N2 C7 C12 C11 162.9(3) . . . . ? C37 N3 C13 C14 50.3(5) . . . . ? C10 N3 C13 C14 -120.8(4) . . . . ? C37 N3 C13 C18 -138.9(4) . . . . ? C10 N3 C13 C18 50.0(5) . . . . ? C18 C13 C14 C15 -3.8(6) . . . . ? N3 C13 C14 C15 166.9(4) . . . . ? C13 C14 C15 C16 0.4(6) . . . . ? C14 C15 C16 C17 3.6(6) . . . . ? C14 C15 C16 N4 -170.1(4) . . . . ? C43 N4 C16 C15 -71.0(5) . . . . ? C19 N4 C16 C15 117.0(4) . . . . ? C43 N4 C16 C17 115.3(4) . . . . ? C19 N4 C16 C17 -56.7(5) . . . . ? C15 C16 C17 C18 -4.3(6) . . . . ? N4 C16 C17 C18 169.6(4) . . . . ? C16 C17 C18 C13 0.9(6) . . . . ? C14 C13 C18 C17 3.1(6) . . . . ? N3 C13 C18 C17 -168.2(3) . . . . ? C43 N4 C19 C24 137.4(4) . . . . ? C16 N4 C19 C24 -51.0(4) . . . . ? C43 N4 C19 C20 -51.3(5) . . . . ? C16 N4 C19 C20 120.3(4) . . . . ? C24 C19 C20 C21 6.8(5) . . . . ? N4 C19 C20 C21 -164.4(3) . . . . ? C19 C20 C21 C22 1.4(5) . . . . ? C20 C21 C22 C23 -8.8(5) . . . . ? C20 C21 C22 N1 161.5(3) . . . . ? C25 N1 C22 C21 38.8(5) . . . . ? C1 N1 C22 C21 -109.4(4) . . . . ? C25 N1 C22 C23 -150.8(3) . . . . ? C1 N1 C22 C23 61.1(4) . . . . ? C21 C22 C23 C24 8.0(5) . . . . ? N1 C22 C23 C24 -162.9(3) . . . . ? C22 C23 C24 C19 0.2(5) . . . . ? C20 C19 C24 C23 -7.6(5) . . . . ? N4 C19 C24 C23 164.1(3) . . . . ? C22 N1 C25 C26 -132.9(3) . . . . ? C1 N1 C25 C26 12.6(5) . . . . ? C22 N1 C25 C30 48.1(5) . . . . ? C1 N1 C25 C30 -166.4(3) . . . . ? C30 C25 C26 C27 -1.1(5) . . . . ? N1 C25 C26 C27 179.8(3) . . . . ? C25 C26 C27 C28 0.7(6) . . . . ? C26 C27 C28 O1 179.8(3) . . . . ? C26 C27 C28 C29 0.0(5) . . . . ? C49 O1 C28 C27 4.0(5) . . . . ? C49 O1 C28 C29 -176.1(3) . . . . ? C27 C28 C29 C30 -0.2(5) . . . . ? O1 C28 C29 C30 180.0(3) . . . . ? C28 C29 C30 C25 -0.3(5) . . . . ? C26 C25 C30 C29 0.9(5) . . . . ? N1 C25 C30 C29 -180.0(3) . . . . ? C4 N2 C31 C36 138.8(4) . . . . ? C7 N2 C31 C36 -29.4(5) . . . . ? C4 N2 C31 C32 -41.9(5) . . . . ? C7 N2 C31 C32 149.9(3) . . . . ? C36 C31 C32 C33 -0.8(5) . . . . ? N2 C31 C32 C33 179.9(3) . . . . ? C31 C32 C33 C34 2.2(5) . . . . ? C50 O2 C34 C33 12.4(6) . . . . ? C50 O2 C34 C35 -168.1(4) . . . . ? C32 C33 C34 O2 177.3(3) . . . . ? C32 C33 C34 C35 -2.2(5) . . . . ? O2 C34 C35 C36 -178.6(3) . . . . ? C33 C34 C35 C36 0.9(5) . . . . ? C32 C31 C36 C35 -0.5(5) . . . . ? N2 C31 C36 C35 178.8(3) . . . . ? C34 C35 C36 C31 0.5(6) . . . . ? C13 N3 C37 C42 23.7(5) . . . . ? C10 N3 C37 C42 -166.4(3) . . . . ? C13 N3 C37 C38 -156.4(3) . . . . ? C10 N3 C37 C38 13.5(5) . . . . ? C42 C37 C38 C39 -1.0(5) . . . . ? N3 C37 C38 C39 179.0(3) . . . . ? C37 C38 C39 C40 -0.2(5) . . . . ? C38 C39 C40 O3 -178.9(3) . . . . ? C38 C39 C40 C41 0.9(5) . . . . ? C51 O3 C40 C39 168.6(3) . . . . ? C51 O3 C40 C41 -11.1(5) . . . . ? C39 C40 C41 C42 -0.4(5) . . . . ? O3 C40 C41 C42 179.3(3) . . . . ? C38 C37 C42 C41 1.6(5) . . . . ? N3 C37 C42 C41 -178.5(3) . . . . ? C40 C41 C42 C37 -0.8(5) . . . . ? C19 N4 C43 C44 -26.6(5) . . . . ? C16 N4 C43 C44 162.4(3) . . . . ? C19 N4 C43 C48 156.6(3) . . . . ? C16 N4 C43 C48 -14.4(5) . . . . ? C48 C43 C44 C45 0.9(5) . . . . ? N4 C43 C44 C45 -176.0(3) . . . . ? C43 C44 C45 C46 0.8(5) . . . . ? C52 O4 C46 C45 -19.0(5) . . . . ? C52 O4 C46 C47 161.4(4) . . . . ? C44 C45 C46 O4 178.6(3) . . . . ? C44 C45 C46 C47 -1.8(5) . . . . ? O4 C46 C47 C48 -179.2(3) . . . . ? C45 C46 C47 C48 1.2(5) . . . . ? C46 C47 C48 C43 0.6(5) . . . . ? C44 C43 C48 C47 -1.6(5) . . . . ? N4 C43 C48 C47 175.3(3) . . . . ? #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. _shelx_res_file ; shelxl.res created by SHELXL-2014/7 TITL 160627_Sakamaki_4p_dcm_MeOH_a CELL 0.71075 12.21620 15.61370 23.05380 90.000 92.341 90.000 ZERR 4 0.00220 0.00280 0.00410 0.000 0.003 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O CL UNIT 212 184 16 16 8 L.S. 5 FMAP 2 PLAN -25 WPDB -2 BOND $H CONF LIST 4 TEMP -129.8 ACTA SIZE 0.200 0.200 0.200 REM HTAB HTAB WGHT 0.087600 FVAR 1.02829 CL1 5 -0.388420 1.152110 0.383693 11.00000 0.12171 0.18546 = 0.13449 -0.06235 0.00617 -0.02047 CL2 5 -0.587152 1.102244 0.327880 11.00000 0.08079 0.29162 = 0.09215 -0.04100 0.00220 0.02562 O1 4 0.267218 0.501842 0.466030 11.00000 0.05746 0.02469 = 0.04651 0.00047 -0.00295 0.00387 O2 4 0.576982 1.253619 0.705061 11.00000 0.04905 0.05097 = 0.04186 0.00441 -0.01919 -0.01123 O3 4 -0.156592 1.654981 0.332959 11.00000 0.04636 0.02716 = 0.05636 0.00311 -0.01730 0.00853 O4 4 -0.492882 0.919563 0.134464 11.00000 0.03419 0.06527 = 0.06148 -0.00892 -0.01483 -0.00328 N1 3 0.210283 0.845983 0.405437 11.00000 0.03841 0.02235 = 0.03714 -0.00191 -0.01300 0.00211 N2 3 0.274537 1.151318 0.530670 11.00000 0.04195 0.02252 = 0.04707 -0.00520 -0.01927 0.00570 N3 3 -0.032293 1.318885 0.385863 11.00000 0.05117 0.02071 = 0.05211 -0.00534 -0.02917 0.00713 N4 3 -0.130809 1.003430 0.279077 11.00000 0.05684 0.02605 = 0.05414 -0.00854 -0.03119 0.01056 C1 1 0.228558 0.914186 0.446951 11.00000 0.03793 0.02219 = 0.03382 -0.00054 -0.00655 0.00067 C2 1 0.332220 0.937346 0.467173 11.00000 0.03710 0.02826 = 0.09100 -0.01787 -0.02646 0.01296 AFIX 43 H2 2 0.392937 0.901588 0.459644 11.00000 -1.20000 AFIX 0 C3 1 0.348417 1.012923 0.498597 11.00000 0.03295 0.03564 = 0.09266 -0.01633 -0.02958 0.00452 AFIX 43 H3 2 0.420315 1.028159 0.512091 11.00000 -1.20000 AFIX 0 C4 1 0.261891 1.065859 0.510396 11.00000 0.04626 0.02136 = 0.03230 0.00193 -0.01314 0.00277 C5 1 0.156722 1.037906 0.495215 11.00000 0.03760 0.03629 = 0.03273 -0.00608 0.00324 -0.00002 AFIX 43 H5 2 0.095425 1.070309 0.506666 11.00000 -1.20000 AFIX 0 C6 1 0.140147 0.963260 0.463543 11.00000 0.02930 0.03863 = 0.04026 -0.00563 0.00291 -0.01122 AFIX 43 H6 2 0.067659 0.945436 0.453061 11.00000 -1.20000 AFIX 0 C7 1 0.215167 1.213183 0.495070 11.00000 0.02980 0.02355 = 0.03986 0.00229 -0.00948 -0.00097 C8 1 0.143347 1.271744 0.517897 11.00000 0.03654 0.02591 = 0.03898 -0.00274 -0.01123 0.00382 AFIX 43 H8 2 0.146885 1.283112 0.558413 11.00000 -1.20000 AFIX 0 C9 1 0.066381 1.314005 0.482474 11.00000 0.04117 0.02792 = 0.04771 -0.00727 -0.01174 0.00737 AFIX 43 H9 2 0.017700 1.354170 0.498560 11.00000 -1.20000 AFIX 0 C10 1 0.061089 1.297058 0.423165 11.00000 0.04036 0.02544 = 0.04320 -0.00032 -0.01513 0.00330 C11 1 0.140384 1.246342 0.399904 11.00000 0.04321 0.03613 = 0.03326 0.00740 -0.00343 0.00291 AFIX 43 H11 2 0.142284 1.240151 0.358963 11.00000 -1.20000 AFIX 0 C12 1 0.217452 1.204185 0.435203 11.00000 0.03233 0.03193 = 0.04286 0.00242 0.00110 0.00467 AFIX 43 H12 2 0.271591 1.169297 0.418538 11.00000 -1.20000 AFIX 0 C13 1 -0.076795 1.245615 0.356254 11.00000 0.03799 0.02902 = 0.03877 -0.00613 -0.01375 0.00336 C14 1 -0.085437 1.238391 0.296189 11.00000 0.05556 0.02631 = 0.04201 0.00599 -0.01612 0.00670 AFIX 43 H14 2 -0.075545 1.287528 0.272672 11.00000 -1.20000 AFIX 0 C15 1 -0.108448 1.159778 0.270320 11.00000 0.06514 0.03275 = 0.02866 0.00016 -0.01447 0.00895 AFIX 43 H15 2 -0.113669 1.155476 0.229195 11.00000 -1.20000 AFIX 0 C16 1 -0.123896 1.087408 0.303988 11.00000 0.04485 0.02866 = 0.03583 -0.00495 -0.01411 0.00550 C17 1 -0.122019 1.095973 0.364184 11.00000 0.03831 0.02865 = 0.04223 0.00057 -0.00539 -0.00155 AFIX 43 H17 2 -0.137404 1.047772 0.387642 11.00000 -1.20000 AFIX 0 C18 1 -0.098159 1.173371 0.389895 11.00000 0.04150 0.03487 = 0.02836 -0.00372 -0.00790 0.00156 AFIX 43 H18 2 -0.096118 1.177972 0.431015 11.00000 -1.20000 AFIX 0 C19 1 -0.044267 0.948018 0.299574 11.00000 0.05212 0.02726 = 0.02789 -0.00507 -0.01434 0.00700 C20 1 -0.062306 0.871252 0.328534 11.00000 0.03723 0.02679 = 0.04745 -0.00350 -0.01376 0.00004 AFIX 43 H20 2 -0.133267 0.846261 0.327244 11.00000 -1.20000 AFIX 0 C21 1 0.024358 0.830901 0.359588 11.00000 0.03657 0.02607 = 0.04119 0.00101 -0.01059 -0.00074 AFIX 43 H21 2 0.012461 0.777941 0.378615 11.00000 -1.20000 AFIX 0 C22 1 0.127147 0.868239 0.362503 11.00000 0.03768 0.02763 = 0.03073 -0.00416 -0.00569 0.00607 C23 1 0.147018 0.939449 0.327943 11.00000 0.04171 0.03258 = 0.03223 -0.00009 0.00173 0.00046 AFIX 43 H23 2 0.219358 0.961205 0.325761 11.00000 -1.20000 AFIX 0 C24 1 0.061769 0.978342 0.296920 11.00000 0.05843 0.03037 = 0.02862 0.00241 0.00188 0.00299 AFIX 43 H24 2 0.076136 1.026675 0.273384 11.00000 -1.20000 AFIX 0 C25 1 0.224684 0.759964 0.423124 11.00000 0.02589 0.02390 = 0.03489 0.00062 -0.00395 0.00021 C26 1 0.235432 0.736225 0.480852 11.00000 0.03596 0.02843 = 0.03584 -0.00389 0.00027 0.00602 AFIX 43 H26 2 0.233382 0.779026 0.510075 11.00000 -1.20000 AFIX 0 C27 1 0.249230 0.650674 0.497064 11.00000 0.03694 0.02974 = 0.03214 0.00084 -0.00379 0.00250 AFIX 43 H27 2 0.255614 0.635669 0.536994 11.00000 -1.20000 AFIX 0 C28 1 0.253580 0.588214 0.455346 11.00000 0.03237 0.02543 = 0.03997 0.00267 -0.00369 0.00270 C29 1 0.244062 0.610902 0.396870 11.00000 0.02977 0.02957 = 0.03902 -0.00783 0.00478 0.00203 AFIX 43 H29 2 0.247232 0.567901 0.367833 11.00000 -1.20000 AFIX 0 C30 1 0.230096 0.695290 0.381006 11.00000 0.03084 0.03169 = 0.02953 -0.00420 -0.00294 0.00193 AFIX 43 H30 2 0.224034 0.709994 0.341018 11.00000 -1.20000 AFIX 0 C31 1 0.352087 1.175774 0.574476 11.00000 0.03154 0.02763 = 0.03506 -0.00212 -0.00922 0.00410 C32 1 0.369004 1.124503 0.623294 11.00000 0.03815 0.02823 = 0.04094 0.00236 -0.00250 -0.00374 AFIX 43 H32 2 0.327966 1.073228 0.626883 11.00000 -1.20000 AFIX 0 C33 1 0.445376 1.147429 0.666974 11.00000 0.03721 0.03639 = 0.03113 0.00133 -0.00507 0.00207 AFIX 43 H33 2 0.458056 1.110898 0.699510 11.00000 -1.20000 AFIX 0 C34 1 0.502985 1.223582 0.663027 11.00000 0.02542 0.04088 = 0.03489 -0.00288 -0.00466 -0.00263 C35 1 0.486929 1.275643 0.614272 11.00000 0.03353 0.03309 = 0.04156 0.00255 -0.00753 -0.00654 AFIX 43 H35 2 0.526778 1.327534 0.610916 11.00000 -1.20000 AFIX 0 C36 1 0.411922 1.250575 0.570734 11.00000 0.03913 0.03183 = 0.03429 0.00759 -0.00889 -0.00042 AFIX 43 H36 2 0.401381 1.285834 0.537390 11.00000 -1.20000 AFIX 0 C37 1 -0.066059 1.403245 0.373004 11.00000 0.04042 0.02837 = 0.03210 -0.00223 -0.01192 0.00542 C38 1 0.002753 1.472197 0.386204 11.00000 0.03429 0.03172 = 0.03893 -0.00169 -0.00777 0.00486 AFIX 43 H38 2 0.072690 1.462581 0.404587 11.00000 -1.20000 AFIX 0 C39 1 -0.030910 1.555544 0.372450 11.00000 0.03267 0.02655 = 0.04019 -0.00079 -0.00339 -0.00063 AFIX 43 H39 2 0.016200 1.602460 0.381613 11.00000 -1.20000 AFIX 0 C40 1 -0.132246 1.570019 0.345624 11.00000 0.03713 0.02503 = 0.03439 0.00002 -0.00137 0.00402 C41 1 -0.202277 1.501654 0.332805 11.00000 0.03360 0.03105 = 0.03255 -0.00050 -0.01062 0.00686 AFIX 43 H41 2 -0.272319 1.511321 0.314555 11.00000 -1.20000 AFIX 0 C42 1 -0.168338 1.419058 0.347067 11.00000 0.04407 0.02736 = 0.03478 -0.00409 -0.00954 0.00157 AFIX 43 H42 2 -0.216387 1.372385 0.338839 11.00000 -1.20000 AFIX 0 C43 1 -0.222445 0.977982 0.244609 11.00000 0.04298 0.02764 = 0.02863 0.00025 -0.01045 -0.00097 C44 1 -0.219108 0.907792 0.208055 11.00000 0.04143 0.02358 = 0.04534 -0.00136 -0.00979 0.00697 AFIX 43 H44 2 -0.154684 0.873719 0.208015 11.00000 -1.20000 AFIX 0 C45 1 -0.308123 0.886018 0.171331 11.00000 0.04109 0.03602 = 0.03315 -0.00384 -0.00595 -0.00375 AFIX 43 H45 2 -0.304210 0.837118 0.146983 11.00000 -1.20000 AFIX 0 C46 1 -0.402105 0.935321 0.170204 11.00000 0.03044 0.04075 = 0.03665 0.00184 -0.00634 -0.00914 C47 1 -0.407203 1.005062 0.207362 11.00000 0.03540 0.04082 = 0.04036 0.00613 -0.00066 0.00495 AFIX 43 H47 2 -0.471920 1.038787 0.207481 11.00000 -1.20000 AFIX 0 C48 1 -0.319776 1.025773 0.243900 11.00000 0.04250 0.03366 = 0.03195 0.00049 -0.00137 0.00220 AFIX 43 H48 2 -0.325222 1.073431 0.269236 11.00000 -1.20000 AFIX 0 C49 1 0.270036 0.476890 0.525342 11.00000 0.05977 0.03298 = 0.05590 0.00629 -0.01108 -0.00132 AFIX 33 H49A 2 0.279950 0.414723 0.528154 11.00000 -1.20000 H49B 2 0.331094 0.505740 0.546161 11.00000 -1.20000 H49C 2 0.201009 0.492996 0.542618 11.00000 -1.20000 AFIX 0 C50 1 0.611928 1.197391 0.749375 11.00000 0.08857 0.08142 = 0.05745 0.02572 -0.03914 -0.02837 AFIX 33 H50A 2 0.663929 1.226853 0.776012 11.00000 -1.20000 H50B 2 0.548590 1.178293 0.770702 11.00000 -1.20000 H50C 2 0.647720 1.147676 0.732423 11.00000 -1.20000 AFIX 0 C51 1 -0.249529 1.671171 0.296360 11.00000 0.05826 0.03536 = 0.06756 0.00524 -0.01608 0.01457 AFIX 33 H51A 2 -0.257926 1.733075 0.290748 11.00000 -1.20000 H51B 2 -0.240435 1.643476 0.258714 11.00000 -1.20000 H51C 2 -0.314844 1.648219 0.314168 11.00000 -1.20000 AFIX 0 C52 1 -0.475558 0.866891 0.085898 11.00000 0.06061 0.07749 = 0.08019 -0.02836 -0.03505 -0.00108 AFIX 33 H52A 2 -0.544729 0.859630 0.063387 11.00000 -1.20000 H52B 2 -0.421369 0.893685 0.061487 11.00000 -1.20000 H52C 2 -0.448552 0.810803 0.099117 11.00000 -1.20000 AFIX 0 C53 1 -0.506135 1.091989 0.383522 11.00000 0.10196 0.25556 = 0.35454 0.18753 0.07020 0.06538 AFIX 23 H53A 2 -0.485254 1.030899 0.387142 11.00000 -1.20000 H53B 2 -0.546697 1.107226 0.418371 11.00000 -1.20000 AFIX 0 HKLF 4 REM 160627_Sakamaki_4p_dcm_MeOH_a REM R1 = 0.0778 for 3530 Fo > 4sig(Fo) and 0.1455 for all 10009 data REM 568 parameters refined using 0 restraints END WGHT 0.0880 0.0000 REM Instructions for potential hydrogen bonds EQIV $1 x+1, y, z HTAB C12 Cl2_$1 EQIV $2 -x-1, y+1/2, -z+1/2 HTAB C51 Cl2_$2 EQIV $3 -x, y+1/2, -z+1/2 HTAB C52 O1_$3 REM Highest difference peak 1.095, deepest hole -0.832, 1-sigma level 0.074 Q1 1 -0.5109 1.1683 0.3229 11.00000 0.05 1.10 Q2 1 -0.4502 1.1651 0.4178 11.00000 0.05 0.55 Q3 1 -0.3719 1.1998 0.3593 11.00000 0.05 0.34 Q4 1 -0.6047 1.1203 0.3257 11.00000 0.05 0.32 Q5 1 -0.0060 1.1216 0.2696 11.00000 0.05 0.27 Q6 1 -0.5681 1.0644 0.3362 11.00000 0.05 0.26 Q7 1 0.0518 0.9385 0.4243 11.00000 0.05 0.26 Q8 1 -0.0844 1.7005 0.3356 11.00000 0.05 0.26 Q9 1 -0.0822 1.4058 0.3853 11.00000 0.05 0.24 Q10 1 0.4113 1.2660 0.5543 11.00000 0.05 0.23 Q11 1 -0.0195 0.9429 0.2826 11.00000 0.05 0.22 Q12 1 -0.0591 1.3785 0.5144 11.00000 0.05 0.22 Q13 1 -0.6185 0.8239 0.3756 11.00000 0.05 0.22 Q14 1 -0.2088 1.1191 0.3001 11.00000 0.05 0.22 Q15 1 -0.6850 1.0777 0.2830 11.00000 0.05 0.21 Q16 1 -0.5777 0.9753 0.3296 11.00000 0.05 0.21 Q17 1 -0.3338 0.8847 0.1833 11.00000 0.05 0.20 Q18 1 0.3091 1.2996 0.4395 11.00000 0.05 0.20 Q19 1 0.3457 0.6104 0.4857 11.00000 0.05 0.20 Q20 1 -0.5527 0.9003 0.4006 11.00000 0.05 0.20 Q21 1 -0.0464 1.1177 0.3095 11.00000 0.05 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