#------------------------------------------------------------------------------ #$Date: 2024-09-06 05:07:11 +0300 (Fri, 06 Sep 2024) $ #$Revision: 294644 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572157.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1572157 loop_ _publ_author_name 'Franc\'es-Poveda, Enrique' 'Mart\'inez de Sarasa Buchaca, Marc' 'Moya-L\'opez, Carmen' 'Vitorica-Yrezabal, I\~nigo J.' 'L\'opez-Solera, Isabel' 'Castro-Osma, Jos\'e A.' 'la Cruz-Mart\'inez, Felipe de' 'Lara-S\'anchez, Agust\'in' _publ_section_title ; Calcium-catalysed ring-opening copolymerisation of epoxides and cyclic anhydrides ; _journal_issue 32 _journal_name_full 'Polymer Chemistry' _journal_page_first 3238 _journal_page_last 3245 _journal_paper_doi 10.1039/D4PY00379A _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C44 H58 Ca2 I2 N8 O4, 2(C H2 Cl2), C3 H7' _chemical_formula_sum 'C49 H69 Ca2 Cl4 I2 N8 O4' _chemical_formula_weight 1309.88 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2024-02-13 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2024-02-13 deposited with the CCDC. 2024-07-08 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 95.473(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.835(2) _cell_length_b 17.351(3) _cell_length_c 26.132(5) _cell_measurement_reflns_used 9622 _cell_measurement_temperature 150.00 _cell_measurement_theta_max 28.40 _cell_measurement_theta_min 2.35 _cell_volume 5793.1(17) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 150.00 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0732 _diffrn_reflns_av_unetI/netI 0.0547 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 67749 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.350 _diffrn_reflns_theta_min 1.957 _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.495 _exptl_absorpt_correction_T_max 0.7458 _exptl_absorpt_correction_T_min 0.5105 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1420 before and 0.0923 after correction. The Ratio of minimum to maximum transmission is 0.6845. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.502 _exptl_crystal_description block _exptl_crystal_F_000 2660 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _refine_diff_density_max 1.502 _refine_diff_density_min -1.825 _refine_diff_density_rms 0.201 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 619 _refine_ls_number_reflns 10522 _refine_ls_number_restraints 44 _refine_ls_restrained_S_all 1.145 _refine_ls_R_factor_all 0.1283 _refine_ls_R_factor_gt 0.1078 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0131P)^2^+226.0766P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2780 _refine_ls_wR_factor_ref 0.2911 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8391 _reflns_number_total 10522 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4py00379a2.cif _cod_data_source_block mo_agu345_0m _cod_depositor_comments 'Adding full bibliography for 1572157--1572158.cif.' _cod_database_code 1572157 _shelx_shelxl_version_number 2019/1 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.796 _shelx_estimated_absorpt_t_min 0.735 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances Cl4-C48 = Cl3-C48 1.771 with sigma of 0.01 Cl4-Cl3 2.916 with sigma of 0.03 C46-C45 \\sim C47-C46 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Cl4 \\sim Cl3 \\sim C48: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A C47 \\sim C45 \\sim C46 \\sim C47 \\sim C46 \\sim C45: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A C48 \\sim Cl3 \\sim Cl4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A 4. Rigid body (RIGU) restrains Cl4, Cl3, C48 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C47, C45, C46, C47, C46, C45 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002 5.a Free rotating group: Cl4(Cl3,C48) 5.b Ternary CH refined with riding coordinates: C1(H1), C19(H19), C20(H20), C2(H2) 5.c Secondary CH2 refined with riding coordinates: C38(H38A,H38B), C44(H44A,H44B), C43(H43A,H43B), C46(H46A,H46B), C40(H40A, H40B), C47(H47A,H47B), C49(H49A,H49B), C42(H42A,H42B), C41(H41A,H41B), C39(H39A,H39B), C37(H37A,H37B), C48(H48A,H48B) 5.d Me refined with riding coordinates: C12(H12A,H12B,H12C), C45(H45A,H45B,H45C), C30(H30A,H30B,H30C), C11(H11A,H11B, H11C), C29(H29A,H29B,H29C), C7(H7A,H7B,H7C), C25(H25A,H25B,H25C), C24(H24A, H24B,H24C), C6(H6A,H6B,H6C) 5.e Aromatic/amide H refined with riding coordinates: C32(H32), C27(H27), C15(H15), C34(H34), C35(H35), C33(H33), C4(H4), C17(H17), C22(H22), C16(H16), C36(H36), C18(H18), C9(H9), C14(H14) ; _shelx_res_file ; TITL mo_AGU345_0m_a.res in P2(1)/c mo_agu345_0m.res created by SHELXL-2019/1 at 09:50:19 on 13-Feb-2024 CELL 0.71073 12.8355 17.3507 26.1316 90 95.473 90 ZERR 4 0.0022 0.003 0.0046 0 0.006 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Ca Cl I N O UNIT 196 276 8 16 8 32 16 DFIX 1.771 0.01 Cl4 C48 Cl3 C48 DFIX 2.916 0.03 Cl4 Cl3 SIMU Cl4 Cl3 C48 RIGU Cl4 Cl3 C48 SIMU 0.02 0.04 2 C47 C45 C46 C47 C46 C45 RIGU 0.002 0.002 C47 C45 C46 C47 C46 C45 SIMU 0.01 0.02 2 C48 Cl3 Cl4 SADI C46 C45 C47 C46 L.S. 25 PLAN 19 0 0 SIZE 0.22 0.18 0.16 TEMP -123.15 CONF MORE -1 BOND $H fmap 2 acta SHEL 999 0.83 OMIT 2 15 1 OMIT 12 1 4 OMIT 12 5 0 REM REM REM WGHT 0.013100 226.076599 FVAR 0.16263 I1 5 0.555646 0.380775 0.238526 11.00000 0.04114 0.03122 = 0.05622 -0.01088 0.00094 -0.00092 I2 5 1.095600 0.514766 0.365133 11.00000 0.03764 0.04228 = 0.07028 0.01179 -0.00427 0.00209 CA1 3 0.616750 0.517060 0.313888 11.00000 0.03244 0.02235 = 0.03289 0.00175 0.00138 -0.00111 CA2 3 0.880673 0.547893 0.302973 11.00000 0.03172 0.02228 = 0.03911 0.00535 0.00262 0.00060 CL1 4 0.285762 0.522344 0.114477 11.00000 0.10290 0.09117 = 0.08253 0.01285 0.02765 0.03004 CL2 4 0.421131 0.429905 0.057524 11.00000 0.18026 0.11542 = 0.09631 -0.04340 0.04387 0.01188 O1 7 0.773583 0.484676 0.353319 11.00000 0.04261 0.02939 = 0.02950 0.00677 0.00188 0.00438 O2 7 0.722139 0.583287 0.263715 11.00000 0.02364 0.02546 = 0.03841 0.00490 -0.00094 0.00110 O3 7 0.451867 0.575685 0.294375 11.00000 0.04965 0.03299 = 0.03759 -0.00196 0.00424 0.00455 N7 6 0.874374 0.678190 0.207754 11.00000 0.02877 0.02141 = 0.04038 0.00363 0.00256 0.00019 N4 6 0.700073 0.580180 0.432662 11.00000 0.05601 0.01899 = 0.02966 0.00062 -0.00159 -0.00132 N5 6 0.930657 0.615202 0.226249 11.00000 0.04132 0.02331 = 0.04198 0.00243 0.01441 -0.00476 N2 6 0.644097 0.608359 0.389654 11.00000 0.04078 0.02305 = 0.03475 0.00106 0.00208 -0.00098 N1 6 0.555552 0.452106 0.390826 11.00000 0.03620 0.02622 = 0.03380 0.00109 -0.00006 0.00475 O4 7 0.899476 0.432654 0.255250 11.00000 0.05916 0.02624 = 0.04652 0.00214 0.00848 0.00502 N3 6 0.618813 0.457522 0.435949 11.00000 0.02639 0.02288 = 0.03988 0.00421 0.00290 -0.00314 N8 6 0.824900 0.736966 0.285490 11.00000 0.03407 0.02308 = 0.03667 0.00016 0.00240 0.00062 C3 1 0.732640 0.637569 0.466761 11.00000 0.03987 0.03143 = 0.03729 -0.00545 0.00272 -0.00259 C31 1 0.645769 0.640650 0.181998 11.00000 0.04550 0.02312 = 0.03391 0.00274 0.00022 -0.00467 C38 1 0.334731 0.655513 0.245944 11.00000 0.03181 0.03763 = 0.06739 0.00479 -0.00945 0.00392 AFIX 23 H38A 2 0.268036 0.652341 0.223651 11.00000 -1.20000 H38B 2 0.375934 0.699596 0.234732 11.00000 -1.20000 AFIX 0 C8 1 0.576512 0.417914 0.474111 11.00000 0.05087 0.02819 = 0.03692 0.00478 0.01388 0.00608 C1 1 0.797269 0.465596 0.404090 11.00000 0.03883 0.03046 = 0.02891 0.00469 -0.00130 -0.00160 AFIX 13 H1 2 0.867163 0.488415 0.415547 11.00000 -1.20000 AFIX 0 N6 6 0.874177 0.689872 0.322152 11.00000 0.07591 0.02767 = 0.03380 0.00181 0.00507 0.00441 C19 1 0.693929 0.651278 0.237288 11.00000 0.02106 0.02403 = 0.03627 0.00564 -0.00391 0.00172 AFIX 13 H19 2 0.640686 0.677892 0.256575 11.00000 -1.20000 AFIX 0 C10 1 0.474495 0.409301 0.401546 11.00000 0.02009 0.02568 = 0.04766 -0.00098 0.00147 0.00277 C26 1 0.909699 0.704421 0.163892 11.00000 0.04409 0.03147 = 0.02873 0.00933 0.00008 0.00802 C20 1 0.788132 0.707593 0.235156 11.00000 0.02604 0.02229 = 0.03482 0.00305 -0.00188 0.00287 AFIX 13 H20 2 0.759844 0.753217 0.214978 11.00000 -1.20000 AFIX 0 C32 1 0.569610 0.690051 0.161809 11.00000 0.03487 0.02893 = 0.04292 0.00382 0.00408 -0.00444 AFIX 43 H32 2 0.542436 0.727681 0.183357 11.00000 -1.20000 AFIX 0 C21 1 0.817970 0.810794 0.302066 11.00000 0.03005 0.02811 = 0.04866 -0.00440 0.00797 -0.00294 C13 1 0.804487 0.378892 0.413438 11.00000 0.04094 0.02784 = 0.03342 0.00718 0.00267 0.00167 C12 1 0.388099 0.393231 0.361962 11.00000 0.02839 0.03279 = 0.05429 0.00016 0.00879 -0.01115 AFIX 33 H12A 2 0.335659 0.361065 0.376619 11.00000 -1.50000 H12B 2 0.355843 0.441863 0.349726 11.00000 -1.50000 H12C 2 0.415167 0.366047 0.333139 11.00000 -1.50000 AFIX 0 C5 1 0.639055 0.684754 0.398000 11.00000 0.05249 0.02208 = 0.03740 -0.00426 0.00766 0.00153 C27 1 0.988080 0.658540 0.153139 11.00000 0.04232 0.04255 = 0.04287 0.00618 0.00941 -0.00238 AFIX 43 H27 2 1.027304 0.662015 0.124178 11.00000 -1.20000 AFIX 0 C44 1 0.937591 0.362091 0.279716 11.00000 0.05335 0.03330 = 0.06599 0.01058 -0.00114 0.00409 AFIX 23 H44A 2 0.924905 0.361698 0.316495 11.00000 -1.20000 H44B 2 1.013523 0.355823 0.276983 11.00000 -1.20000 AFIX 0 C43 1 0.876366 0.299290 0.250866 11.00000 0.09831 0.03201 = 0.07350 0.00174 0.00227 0.00113 AFIX 23 H43A 2 0.915151 0.249896 0.252830 11.00000 -1.20000 H43B 2 0.807245 0.291724 0.263993 11.00000 -1.20000 AFIX 0 C45 1 0.873876 0.640289 0.012169 11.00000 0.11524 0.11802 = 0.11149 0.02088 -0.00099 -0.00698 AFIX 33 H45A 2 0.814510 0.660729 0.028874 11.00000 -1.50000 H45B 2 0.937970 0.667300 0.025304 11.00000 -1.50000 H45C 2 0.861501 0.648032 -0.025063 11.00000 -1.50000 AFIX 0 C30 1 1.078650 0.540341 0.200179 11.00000 0.04843 0.03502 = 0.06556 0.01157 0.01698 0.01545 AFIX 33 H30A 2 1.124173 0.541001 0.172132 11.00000 -1.50000 H30B 2 1.121122 0.546995 0.233083 11.00000 -1.50000 H30C 2 1.041591 0.490955 0.200137 11.00000 -1.50000 AFIX 0 C15 1 0.865581 0.272211 0.467327 11.00000 0.09826 0.03402 = 0.04957 0.00818 -0.01787 0.01195 AFIX 43 H15 2 0.905115 0.253638 0.497392 11.00000 -1.20000 AFIX 0 C46 1 0.885849 0.553863 0.023743 11.00000 0.13239 0.12436 = 0.19419 0.03719 0.03465 0.00337 AFIX 23 H46A 2 0.824034 0.523710 0.009849 11.00000 -1.20000 H46B 2 0.901543 0.543241 0.060902 11.00000 -1.20000 AFIX 0 C40 1 0.376874 0.600504 0.329654 11.00000 0.05862 0.04148 = 0.05216 0.00739 0.01851 0.00199 AFIX 23 H40A 2 0.413613 0.619800 0.362172 11.00000 -1.20000 H40B 2 0.330688 0.557291 0.337592 11.00000 -1.20000 AFIX 0 C47 1 0.981462 0.540871 -0.006779 11.00000 0.13963 0.12252 = 0.21521 0.02734 0.04719 -0.00298 AFIX 23 H47A 2 0.961455 0.545718 -0.044175 11.00000 -1.20000 H47B 2 1.037214 0.578804 0.003435 11.00000 -1.20000 AFIX 0 C34 1 0.570173 0.632349 0.078700 11.00000 0.08800 0.06124 = 0.03528 -0.00297 -0.01162 0.00543 AFIX 43 H34 2 0.543878 0.629357 0.043521 11.00000 -1.20000 AFIX 0 C49 1 0.404584 0.475366 0.114603 11.00000 0.09565 0.07170 = 0.06652 -0.00695 0.00859 0.01334 AFIX 23 H49A 2 0.461697 0.513264 0.122000 11.00000 -1.20000 H49B 2 0.410289 0.436711 0.142597 11.00000 -1.20000 AFIX 0 C11 1 0.624870 0.414229 0.528012 11.00000 0.09557 0.04359 = 0.03466 0.00578 0.01547 0.00584 AFIX 33 H11A 2 0.691449 0.442269 0.530868 11.00000 -1.50000 H11B 2 0.577598 0.437706 0.550882 11.00000 -1.50000 H11C 2 0.637466 0.360282 0.537846 11.00000 -1.50000 AFIX 0 C35 1 0.647581 0.582722 0.098321 11.00000 0.09880 0.04718 = 0.04384 -0.01410 -0.00878 0.00758 AFIX 43 H35 2 0.674916 0.545786 0.076330 11.00000 -1.20000 AFIX 0 C33 1 0.531273 0.686142 0.110287 11.00000 0.06902 0.04543 = 0.04590 0.01325 0.00246 0.00480 AFIX 43 H33 2 0.478099 0.720757 0.096958 11.00000 -1.20000 AFIX 0 C42 1 0.865374 0.330783 0.197058 11.00000 0.05776 0.03591 = 0.07020 -0.00917 0.00775 0.00137 AFIX 23 H42A 2 0.804240 0.307959 0.176527 11.00000 -1.20000 H42B 2 0.929123 0.320782 0.179560 11.00000 -1.20000 AFIX 0 C4 1 0.691880 0.704063 0.445513 11.00000 0.06423 0.02223 = 0.04157 -0.00169 0.00806 -0.00239 AFIX 43 H4 2 0.698192 0.754108 0.460230 11.00000 -1.20000 AFIX 0 C17 1 0.752455 0.248408 0.390899 11.00000 0.06412 0.02689 = 0.04324 -0.00188 0.00467 -0.00264 AFIX 43 H17 2 0.714306 0.213432 0.368269 11.00000 -1.20000 AFIX 0 C29 1 0.856710 0.770295 0.133678 11.00000 0.04946 0.05078 = 0.03615 0.01821 0.00479 0.00199 AFIX 33 H29A 2 0.801481 0.791874 0.152815 11.00000 -1.50000 H29B 2 0.908381 0.810381 0.128370 11.00000 -1.50000 H29C 2 0.825951 0.751292 0.100284 11.00000 -1.50000 AFIX 0 C22 1 0.862308 0.811349 0.351977 11.00000 0.04015 0.03039 = 0.04733 -0.00963 -0.00063 -0.00309 AFIX 43 H22 2 0.866165 0.854009 0.374868 11.00000 -1.20000 AFIX 0 C16 1 0.812079 0.221753 0.434959 11.00000 0.06023 0.02911 = 0.04911 0.00558 0.00468 0.00953 AFIX 43 H16 2 0.815138 0.168118 0.442257 11.00000 -1.20000 AFIX 0 C41 1 0.850081 0.415912 0.205099 11.00000 0.06542 0.03330 = 0.04621 -0.00149 0.00771 0.00090 AFIX 23 H41A 2 0.882742 0.446049 0.178703 11.00000 -1.20000 H41B 2 0.774615 0.428662 0.203012 11.00000 -1.20000 AFIX 0 C7 1 0.796684 0.621525 0.516253 11.00000 0.06825 0.04651 = 0.03600 -0.00366 -0.01682 -0.00475 AFIX 33 H7A 2 0.812124 0.566269 0.518826 11.00000 -1.50000 H7B 2 0.862348 0.650578 0.517466 11.00000 -1.50000 H7C 2 0.757674 0.637180 0.544996 11.00000 -1.50000 AFIX 0 C25 1 0.956666 0.706550 0.409739 11.00000 0.05150 0.05920 = 0.03961 -0.00251 -0.00254 -0.00134 AFIX 33 H25A 2 0.969341 0.748391 0.434751 11.00000 -1.50000 H25B 2 0.914411 0.666387 0.424143 11.00000 -1.50000 H25C 2 1.023707 0.684635 0.401917 11.00000 -1.50000 AFIX 0 C36 1 0.686322 0.585759 0.149663 11.00000 0.04913 0.03634 = 0.05322 -0.00692 -0.00616 0.01071 AFIX 43 H36 2 0.739643 0.551148 0.162830 11.00000 -1.20000 AFIX 0 C39 1 0.314842 0.663619 0.302125 11.00000 0.03095 0.04578 = 0.06260 0.00469 0.00418 0.01000 AFIX 23 H39A 2 0.338422 0.714669 0.315616 11.00000 -1.20000 H39B 2 0.239398 0.657749 0.306295 11.00000 -1.20000 AFIX 0 C2 1 0.717547 0.497710 0.439566 11.00000 0.05654 0.02403 = 0.02681 0.00416 -0.00005 0.00352 AFIX 13 H2 2 0.749692 0.490580 0.475640 11.00000 -1.20000 AFIX 0 C18 1 0.750161 0.327226 0.380888 11.00000 0.03977 0.03345 = 0.03611 0.00690 -0.00025 0.00192 AFIX 43 H18 2 0.710247 0.345829 0.350943 11.00000 -1.20000 AFIX 0 C24 1 0.766053 0.873535 0.270696 11.00000 0.04519 0.02320 = 0.05246 -0.00078 0.00350 0.00037 AFIX 33 H24A 2 0.770593 0.921638 0.290439 11.00000 -1.50000 H24B 2 0.800886 0.880149 0.239206 11.00000 -1.50000 H24C 2 0.692353 0.860303 0.261703 11.00000 -1.50000 AFIX 0 C6 1 0.585274 0.737074 0.359150 11.00000 0.03880 0.02553 = 0.04727 0.00567 0.00542 0.00324 AFIX 33 H6A 2 0.589704 0.790162 0.371976 11.00000 -1.50000 H6B 2 0.618951 0.733643 0.327111 11.00000 -1.50000 H6C 2 0.511612 0.722003 0.352681 11.00000 -1.50000 AFIX 0 C9 1 0.484627 0.387143 0.453088 11.00000 0.04732 0.02660 = 0.05228 0.00457 0.01587 -0.00241 AFIX 43 H9 2 0.436993 0.356700 0.470108 11.00000 -1.20000 AFIX 0 C37 1 0.395940 0.581015 0.244349 11.00000 0.03656 0.04077 = 0.04277 -0.00201 -0.00440 -0.00250 AFIX 23 H37A 2 0.348290 0.536514 0.237709 11.00000 -1.20000 H37B 2 0.444873 0.582934 0.217295 11.00000 -1.20000 AFIX 0 C14 1 0.863097 0.350594 0.456941 11.00000 0.04222 0.03232 = 0.05576 0.00264 -0.01204 0.00170 AFIX 43 H14 2 0.901662 0.385205 0.479676 11.00000 -1.20000 AFIX 0 C28 1 1.001262 0.604260 0.192865 11.00000 0.05348 0.02593 = 0.04576 0.00478 0.01079 -0.00002 C23 1 0.900938 0.736659 0.362738 11.00000 0.04054 0.03781 = 0.04085 -0.00333 0.00372 -0.00821 AFIX 6 CL4 4 0.789497 0.386089 0.064828 11.00000 0.28281 0.13684 = 0.14952 -0.02309 0.05515 0.00615 CL3 4 0.612379 0.284282 0.036995 11.00000 0.28638 0.13498 = 0.27329 -0.01975 0.11207 0.00457 C48 1 0.671185 0.347451 0.084208 11.00000 0.29350 0.15596 = 0.23071 -0.02323 0.08836 -0.01099 AFIX 23 H48A 2 0.686078 0.319283 0.117038 11.00000 -1.20000 H48B 2 0.622241 0.390003 0.089934 11.00000 -1.20000 AFIX 0 HKLF 4 REM mo_AGU345_0m_a.res in P2(1)/c REM wR2 = 0.2911, GooF = S = 1.145, Restrained GooF = 1.145 for all data REM R1 = 0.1078 for 8391 Fo > 4sig(Fo) and 0.1283 for all 10522 data REM 619 parameters refined using 44 restraints END WGHT 0.0144 225.9375 REM Highest difference peak 1.502, deepest hole -1.825, 1-sigma level 0.201 Q1 1 0.6225 0.3828 0.2440 11.00000 0.05 1.45 Q2 1 1.1570 0.5008 0.3729 11.00000 0.05 1.43 Q3 1 0.5038 0.5938 0.2306 11.00000 0.05 1.42 Q4 1 0.4858 0.3933 0.2313 11.00000 0.05 1.39 Q5 1 1.1437 0.7278 0.3725 11.00000 0.05 1.33 Q6 1 1.0213 0.5312 0.3591 11.00000 0.05 1.24 Q7 1 0.5551 0.3814 0.1981 11.00000 0.05 1.15 Q8 1 0.6062 0.5977 0.2428 11.00000 0.05 1.15 Q9 1 1.0170 0.5124 0.1117 11.00000 0.05 1.10 Q10 1 1.0873 0.5150 0.3303 11.00000 0.05 1.09 Q11 1 0.6833 0.2849 0.0737 11.00000 0.05 1.06 Q12 1 0.9022 0.4753 0.0599 11.00000 0.05 1.05 Q13 1 0.8190 0.5515 0.2982 11.00000 0.05 1.02 Q14 1 0.5586 0.3800 0.2780 11.00000 0.05 1.02 Q15 1 0.6028 0.8423 0.2397 11.00000 0.05 1.02 Q16 1 0.9752 0.4834 -0.0612 11.00000 0.05 0.99 Q17 1 0.4135 0.4801 0.0396 11.00000 0.05 0.99 Q18 1 1.0445 0.7392 0.3580 11.00000 0.05 0.92 Q19 1 0.6887 0.3840 0.5271 11.00000 0.05 0.79 ; _shelx_res_checksum 29728 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 I1 I 0.55565(8) 0.38078(5) 0.23853(4) 0.0431(3) Uani 1 1 d . . . . . I2 I 1.09560(8) 0.51477(6) 0.36513(4) 0.0507(3) Uani 1 1 d . . . . . Ca1 Ca 0.6167(2) 0.51706(14) 0.31389(9) 0.0293(5) Uani 1 1 d . . . . . Ca2 Ca 0.8807(2) 0.54789(14) 0.30297(10) 0.0311(6) Uani 1 1 d . . . . . Cl1 Cl 0.2858(5) 0.5223(4) 0.1145(2) 0.0910(18) Uani 1 1 d . . . . . Cl2 Cl 0.4211(8) 0.4299(5) 0.0575(3) 0.129(3) Uani 1 1 d . . . . . O1 O 0.7736(7) 0.4847(5) 0.3533(3) 0.034(2) Uani 1 1 d . . . . . O2 O 0.7221(7) 0.5833(5) 0.2637(3) 0.0294(18) Uani 1 1 d . . . . . O3 O 0.4519(8) 0.5757(5) 0.2944(3) 0.040(2) Uani 1 1 d . . . . . N7 N 0.8744(8) 0.6782(6) 0.2078(4) 0.030(2) Uani 1 1 d . . . . . N4 N 0.7001(10) 0.5802(6) 0.4327(4) 0.035(3) Uani 1 1 d . . . . . N5 N 0.9307(9) 0.6152(6) 0.2262(4) 0.035(2) Uani 1 1 d . . . . . N2 N 0.6441(9) 0.6084(6) 0.3897(4) 0.033(2) Uani 1 1 d . . . . . N1 N 0.5556(9) 0.4521(6) 0.3908(4) 0.032(2) Uani 1 1 d . . . . . O4 O 0.8995(9) 0.4327(5) 0.2553(4) 0.044(2) Uani 1 1 d . . . . . N3 N 0.6188(8) 0.4575(6) 0.4359(4) 0.030(2) Uani 1 1 d . . . . . N8 N 0.8249(9) 0.7370(6) 0.2855(4) 0.031(2) Uani 1 1 d . . . . . C3 C 0.7326(11) 0.6376(8) 0.4668(5) 0.036(3) Uani 1 1 d . . . . . C31 C 0.6458(11) 0.6407(7) 0.1820(5) 0.034(3) Uani 1 1 d . . . . . C38 C 0.3347(12) 0.6555(8) 0.2459(6) 0.047(4) Uani 1 1 d . . . . . H38A H 0.268036 0.652341 0.223651 0.056 Uiso 1 1 calc R U . . . H38B H 0.375934 0.699596 0.234732 0.056 Uiso 1 1 calc R U . . . C8 C 0.5765(12) 0.4179(7) 0.4741(5) 0.038(3) Uani 1 1 d . . . . . C1 C 0.7973(11) 0.4656(7) 0.4041(5) 0.033(3) Uani 1 1 d . . . . . H1 H 0.867163 0.488415 0.415547 0.040 Uiso 1 1 calc R U . . . N6 N 0.8742(11) 0.6899(6) 0.3222(4) 0.046(3) Uani 1 1 d . . . . . C19 C 0.6939(9) 0.6513(7) 0.2373(5) 0.028(3) Uani 1 1 d . . . . . H19 H 0.640686 0.677892 0.256575 0.033 Uiso 1 1 calc R U . . . C10 C 0.4745(10) 0.4093(7) 0.4015(5) 0.031(3) Uani 1 1 d . . . . . C26 C 0.9097(11) 0.7044(7) 0.1639(5) 0.035(3) Uani 1 1 d . . . . . C20 C 0.7881(10) 0.7076(7) 0.2352(5) 0.028(3) Uani 1 1 d . . . . . H20 H 0.759844 0.753217 0.214978 0.034 Uiso 1 1 calc R U . . . C32 C 0.5696(11) 0.6901(7) 0.1618(5) 0.036(3) Uani 1 1 d . . . . . H32 H 0.542436 0.727681 0.183357 0.043 Uiso 1 1 calc R U . . . C21 C 0.8180(11) 0.8108(7) 0.3021(5) 0.035(3) Uani 1 1 d . . . . . C13 C 0.8045(11) 0.3789(7) 0.4134(5) 0.034(3) Uani 1 1 d . . . . . C12 C 0.3881(10) 0.3932(8) 0.3620(5) 0.038(3) Uani 1 1 d . . . . . H12A H 0.335659 0.361065 0.376619 0.057 Uiso 1 1 calc R U . . . H12B H 0.355843 0.441863 0.349726 0.057 Uiso 1 1 calc R U . . . H12C H 0.415167 0.366047 0.333139 0.057 Uiso 1 1 calc R U . . . C5 C 0.6391(12) 0.6848(7) 0.3980(5) 0.037(3) Uani 1 1 d . . . . . C27 C 0.9881(12) 0.6585(8) 0.1531(6) 0.042(3) Uani 1 1 d . . . . . H27 H 1.027304 0.662015 0.124178 0.051 Uiso 1 1 calc R U . . . C44 C 0.9376(14) 0.3621(8) 0.2797(7) 0.051(4) Uani 1 1 d . . . . . H44A H 0.924905 0.361698 0.316495 0.062 Uiso 1 1 calc R U . . . H44B H 1.013523 0.355823 0.276983 0.062 Uiso 1 1 calc R U . . . C43 C 0.8764(18) 0.2993(9) 0.2509(7) 0.068(5) Uani 1 1 d . . . . . H43A H 0.915151 0.249896 0.252830 0.082 Uiso 1 1 calc R U . . . H43B H 0.807245 0.291724 0.263993 0.082 Uiso 1 1 calc R U . . . C45 C 0.874(2) 0.6403(15) 0.0122(11) 0.116(8) Uani 1 1 d D U . . . H45A H 0.814510 0.660729 0.028874 0.174 Uiso 1 1 calc R U . . . H45B H 0.937970 0.667300 0.025304 0.174 Uiso 1 1 calc R U . . . H45C H 0.861501 0.648032 -0.025063 0.174 Uiso 1 1 calc R U . . . C30 C 1.0787(13) 0.5403(8) 0.2002(6) 0.049(4) Uani 1 1 d . . . . . H30A H 1.124173 0.541001 0.172132 0.073 Uiso 1 1 calc R U . . . H30B H 1.121122 0.546995 0.233083 0.073 Uiso 1 1 calc R U . . . H30C H 1.041591 0.490955 0.200137 0.073 Uiso 1 1 calc R U . . . C15 C 0.8656(16) 0.2722(9) 0.4673(6) 0.062(5) Uani 1 1 d . . . . . H15 H 0.905115 0.253638 0.497392 0.075 Uiso 1 1 calc R U . . . C46 C 0.886(3) 0.5539(17) 0.0237(15) 0.149(9) Uani 1 1 d D U . . . H46A H 0.824034 0.523710 0.009849 0.179 Uiso 1 1 calc R U . . . H46B H 0.901543 0.543241 0.060902 0.179 Uiso 1 1 calc R U . . . C40 C 0.3769(13) 0.6005(9) 0.3297(6) 0.050(4) Uani 1 1 d . . . . . H40A H 0.413613 0.619800 0.362172 0.060 Uiso 1 1 calc R U . . . H40B H 0.330688 0.557291 0.337592 0.060 Uiso 1 1 calc R U . . . C47 C 0.981(3) 0.5409(18) -0.0068(16) 0.157(10) Uani 1 1 d D U . . . H47A H 0.961455 0.545718 -0.044175 0.189 Uiso 1 1 calc R U . . . H47B H 1.037214 0.578804 0.003435 0.189 Uiso 1 1 calc R U . . . C34 C 0.5702(16) 0.6323(10) 0.0787(6) 0.063(5) Uani 1 1 d . . . . . H34 H 0.543878 0.629357 0.043521 0.075 Uiso 1 1 calc R U . . . C49 C 0.4046(18) 0.4754(12) 0.1146(8) 0.078(6) Uani 1 1 d . . . . . H49A H 0.461697 0.513264 0.122000 0.093 Uiso 1 1 calc R U . . . H49B H 0.410289 0.436711 0.142597 0.093 Uiso 1 1 calc R U . . . C11 C 0.6249(16) 0.4142(9) 0.5280(5) 0.057(5) Uani 1 1 d . . . . . H11A H 0.691449 0.442269 0.530868 0.086 Uiso 1 1 calc R U . . . H11B H 0.577598 0.437706 0.550882 0.086 Uiso 1 1 calc R U . . . H11C H 0.637466 0.360282 0.537846 0.086 Uiso 1 1 calc R U . . . C35 C 0.6476(17) 0.5827(10) 0.0983(6) 0.064(5) Uani 1 1 d . . . . . H35 H 0.674916 0.545786 0.076330 0.077 Uiso 1 1 calc R U . . . C33 C 0.5313(14) 0.6861(9) 0.1103(6) 0.054(4) Uani 1 1 d . . . . . H33 H 0.478099 0.720757 0.096958 0.064 Uiso 1 1 calc R U . . . C42 C 0.8654(14) 0.3308(9) 0.1971(7) 0.055(4) Uani 1 1 d . . . . . H42A H 0.804240 0.307959 0.176527 0.065 Uiso 1 1 calc R U . . . H42B H 0.929123 0.320782 0.179560 0.065 Uiso 1 1 calc R U . . . C4 C 0.6919(13) 0.7041(8) 0.4455(5) 0.042(3) Uani 1 1 d . . . . . H4 H 0.698192 0.754108 0.460230 0.051 Uiso 1 1 calc R U . . . C17 C 0.7525(13) 0.2484(8) 0.3909(6) 0.045(4) Uani 1 1 d . . . . . H17 H 0.714306 0.213432 0.368269 0.054 Uiso 1 1 calc R U . . . C29 C 0.8567(12) 0.7703(9) 0.1337(5) 0.045(4) Uani 1 1 d . . . . . H29A H 0.801481 0.791874 0.152815 0.068 Uiso 1 1 calc R U . . . H29B H 0.908381 0.810381 0.128370 0.068 Uiso 1 1 calc R U . . . H29C H 0.825951 0.751292 0.100284 0.068 Uiso 1 1 calc R U . . . C22 C 0.8623(11) 0.8113(8) 0.3520(5) 0.040(3) Uani 1 1 d . . . . . H22 H 0.866165 0.854009 0.374868 0.048 Uiso 1 1 calc R U . . . C16 C 0.8121(13) 0.2218(8) 0.4350(6) 0.046(4) Uani 1 1 d . . . . . H16 H 0.815138 0.168118 0.442257 0.055 Uiso 1 1 calc R U . . . C41 C 0.8501(14) 0.4159(8) 0.2051(6) 0.048(4) Uani 1 1 d . . . . . H41A H 0.882742 0.446049 0.178703 0.058 Uiso 1 1 calc R U . . . H41B H 0.774615 0.428662 0.203012 0.058 Uiso 1 1 calc R U . . . C7 C 0.7967(14) 0.6215(9) 0.5163(5) 0.052(4) Uani 1 1 d . . . . . H7A H 0.812124 0.566269 0.518826 0.077 Uiso 1 1 calc R U . . . H7B H 0.862348 0.650578 0.517466 0.077 Uiso 1 1 calc R U . . . H7C H 0.757674 0.637180 0.544996 0.077 Uiso 1 1 calc R U . . . C25 C 0.9567(13) 0.7066(10) 0.4097(6) 0.051(4) Uani 1 1 d . . . . . H25A H 0.969341 0.748391 0.434751 0.076 Uiso 1 1 calc R U . . . H25B H 0.914411 0.666387 0.424143 0.076 Uiso 1 1 calc R U . . . H25C H 1.023707 0.684635 0.401917 0.076 Uiso 1 1 calc R U . . . C36 C 0.6863(13) 0.5858(8) 0.1497(6) 0.047(4) Uani 1 1 d . . . . . H36 H 0.739643 0.551148 0.162830 0.056 Uiso 1 1 calc R U . . . C39 C 0.3148(12) 0.6636(9) 0.3021(6) 0.046(4) Uani 1 1 d . . . . . H39A H 0.338422 0.714669 0.315616 0.056 Uiso 1 1 calc R U . . . H39B H 0.239398 0.657749 0.306295 0.056 Uiso 1 1 calc R U . . . C2 C 0.7175(12) 0.4977(7) 0.4396(5) 0.036(3) Uani 1 1 d . . . . . H2 H 0.749692 0.490580 0.475640 0.043 Uiso 1 1 calc R U . . . C18 C 0.7502(11) 0.3272(8) 0.3809(5) 0.037(3) Uani 1 1 d . . . . . H18 H 0.710247 0.345829 0.350943 0.044 Uiso 1 1 calc R U . . . C24 C 0.7661(12) 0.8735(7) 0.2707(6) 0.040(3) Uani 1 1 d . . . . . H24A H 0.770593 0.921638 0.290439 0.061 Uiso 1 1 calc R U . . . H24B H 0.800886 0.880149 0.239206 0.061 Uiso 1 1 calc R U . . . H24C H 0.692353 0.860303 0.261703 0.061 Uiso 1 1 calc R U . . . C6 C 0.5853(11) 0.7371(7) 0.3592(5) 0.037(3) Uani 1 1 d . . . . . H6A H 0.589704 0.790162 0.371976 0.056 Uiso 1 1 calc R U . . . H6B H 0.618951 0.733643 0.327111 0.056 Uiso 1 1 calc R U . . . H6C H 0.511612 0.722003 0.352681 0.056 Uiso 1 1 calc R U . . . C9 C 0.4846(12) 0.3871(8) 0.4531(6) 0.041(3) Uani 1 1 d . . . . . H9 H 0.436993 0.356700 0.470108 0.050 Uiso 1 1 calc R U . . . C37 C 0.3959(11) 0.5810(8) 0.2443(5) 0.041(3) Uani 1 1 d . . . . . H37A H 0.348290 0.536514 0.237709 0.049 Uiso 1 1 calc R U . . . H37B H 0.444873 0.582934 0.217295 0.049 Uiso 1 1 calc R U . . . C14 C 0.8631(12) 0.3506(8) 0.4569(6) 0.045(4) Uani 1 1 d . . . . . H14 H 0.901662 0.385205 0.479676 0.053 Uiso 1 1 calc R U . . . C28 C 1.0013(12) 0.6043(8) 0.1929(5) 0.041(3) Uani 1 1 d . . . . . C23 C 0.9009(12) 0.7367(8) 0.3627(5) 0.040(3) Uani 1 1 d . . . . . Cl4 Cl 0.7895(10) 0.3861(6) 0.0648(4) 0.188(5) Uani 1 1 d DG U . . . Cl3 Cl 0.6124(10) 0.2843(7) 0.0370(6) 0.226(6) Uani 1 1 d DG U . . . C48 C 0.671(2) 0.347(2) 0.0842(9) 0.223(9) Uani 1 1 d DG U . . . H48A H 0.686078 0.319283 0.117038 0.267 Uiso 1 1 calc R U . . . H48B H 0.622241 0.390003 0.089934 0.267 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 I1 0.0411(6) 0.0312(5) 0.0562(6) -0.0109(4) 0.0009(4) -0.0009(4) I2 0.0376(6) 0.0423(5) 0.0703(7) 0.0118(5) -0.0043(5) 0.0021(4) Ca1 0.0324(14) 0.0224(12) 0.0329(13) 0.0018(10) 0.0014(10) -0.0011(10) Ca2 0.0317(15) 0.0223(12) 0.0391(14) 0.0054(10) 0.0026(11) 0.0006(10) Cl1 0.103(5) 0.091(4) 0.083(4) 0.013(3) 0.028(3) 0.030(3) Cl2 0.180(8) 0.115(6) 0.096(5) -0.043(4) 0.044(5) 0.012(5) O1 0.043(5) 0.029(4) 0.030(4) 0.007(4) 0.002(4) 0.004(4) O2 0.024(5) 0.025(4) 0.038(5) 0.005(4) -0.001(4) 0.001(3) O3 0.050(6) 0.033(5) 0.038(5) -0.002(4) 0.004(4) 0.005(4) N7 0.029(6) 0.021(5) 0.040(6) 0.004(4) 0.003(4) 0.000(4) N4 0.056(8) 0.019(5) 0.030(5) 0.001(4) -0.002(5) -0.001(5) N5 0.041(7) 0.023(5) 0.042(6) 0.002(4) 0.014(5) -0.005(5) N2 0.041(7) 0.023(5) 0.035(6) 0.001(4) 0.002(5) -0.001(5) N1 0.036(6) 0.026(5) 0.034(6) 0.001(4) 0.000(5) 0.005(5) O4 0.059(7) 0.026(5) 0.047(6) 0.002(4) 0.008(5) 0.005(4) N3 0.026(6) 0.023(5) 0.040(6) 0.004(4) 0.003(4) -0.003(4) N8 0.034(6) 0.023(5) 0.037(6) 0.000(4) 0.002(5) 0.001(4) C3 0.040(8) 0.031(7) 0.037(7) -0.005(5) 0.003(6) -0.003(6) C31 0.046(8) 0.023(6) 0.034(7) 0.003(5) 0.000(6) -0.005(6) C38 0.032(8) 0.038(8) 0.067(10) 0.005(7) -0.009(7) 0.004(6) C8 0.051(9) 0.028(7) 0.037(7) 0.005(5) 0.014(6) 0.006(6) C1 0.039(8) 0.030(7) 0.029(6) 0.005(5) -0.001(5) -0.002(6) N6 0.076(10) 0.028(6) 0.034(6) 0.002(5) 0.005(6) 0.004(6) C19 0.021(6) 0.024(6) 0.036(6) 0.006(5) -0.004(5) 0.002(5) C10 0.020(6) 0.026(6) 0.048(7) -0.001(5) 0.001(5) 0.003(5) C26 0.044(8) 0.031(7) 0.029(6) 0.009(5) 0.000(6) 0.008(6) C20 0.026(7) 0.022(6) 0.035(6) 0.003(5) -0.002(5) 0.003(5) C32 0.035(8) 0.029(7) 0.043(7) 0.004(5) 0.004(6) -0.004(6) C21 0.030(7) 0.028(6) 0.049(8) -0.004(6) 0.008(6) -0.003(5) C13 0.041(8) 0.028(6) 0.033(7) 0.007(5) 0.003(6) 0.002(6) C12 0.028(7) 0.033(7) 0.054(8) 0.000(6) 0.009(6) -0.011(6) C5 0.052(9) 0.022(6) 0.037(7) -0.004(5) 0.008(6) 0.002(6) C27 0.042(9) 0.043(8) 0.043(8) 0.006(6) 0.009(6) -0.002(7) C44 0.053(10) 0.033(8) 0.066(10) 0.011(7) -0.001(8) 0.004(7) C43 0.098(16) 0.032(8) 0.074(12) 0.002(8) 0.002(11) 0.001(9) C45 0.115(18) 0.118(15) 0.111(18) 0.021(14) -0.001(14) -0.007(14) C30 0.048(10) 0.035(8) 0.066(10) 0.012(7) 0.017(8) 0.015(7) C15 0.098(15) 0.034(8) 0.050(9) 0.008(7) -0.018(9) 0.012(9) C46 0.132(19) 0.124(15) 0.19(2) 0.037(14) 0.035(16) 0.003(14) C40 0.059(11) 0.041(8) 0.052(9) 0.007(7) 0.019(8) 0.002(7) C47 0.140(19) 0.123(16) 0.22(2) 0.027(16) 0.047(16) -0.003(15) C34 0.088(14) 0.061(11) 0.035(8) -0.003(7) -0.012(8) 0.005(10) C49 0.096(17) 0.072(13) 0.067(12) -0.007(10) 0.009(11) 0.013(12) C11 0.096(14) 0.044(9) 0.035(8) 0.006(6) 0.015(8) 0.006(9) C35 0.099(15) 0.047(9) 0.044(9) -0.014(7) -0.009(9) 0.008(10) C33 0.069(12) 0.045(9) 0.046(9) 0.013(7) 0.002(8) 0.005(8) C42 0.058(11) 0.036(8) 0.070(11) -0.009(7) 0.008(8) 0.001(7) C4 0.064(10) 0.022(6) 0.042(8) -0.002(5) 0.008(7) -0.002(6) C17 0.064(11) 0.027(7) 0.043(8) -0.002(6) 0.005(7) -0.003(7) C29 0.049(9) 0.051(9) 0.036(7) 0.018(6) 0.005(6) 0.002(7) C22 0.040(8) 0.030(7) 0.047(8) -0.010(6) -0.001(6) -0.003(6) C16 0.060(10) 0.029(7) 0.049(8) 0.006(6) 0.005(7) 0.010(7) C41 0.065(11) 0.033(8) 0.046(8) -0.001(6) 0.008(7) 0.001(7) C7 0.068(11) 0.047(9) 0.036(8) -0.004(6) -0.017(7) -0.005(8) C25 0.052(10) 0.059(10) 0.040(8) -0.003(7) -0.003(7) -0.001(8) C36 0.049(9) 0.036(8) 0.053(9) -0.007(6) -0.006(7) 0.011(7) C39 0.031(8) 0.046(9) 0.063(10) 0.005(7) 0.004(7) 0.010(7) C2 0.057(9) 0.024(6) 0.027(6) 0.004(5) 0.000(6) 0.004(6) C18 0.040(8) 0.033(7) 0.036(7) 0.007(5) 0.000(6) 0.002(6) C24 0.045(9) 0.023(6) 0.052(8) -0.001(6) 0.003(6) 0.000(6) C6 0.039(8) 0.026(6) 0.047(8) 0.006(6) 0.005(6) 0.003(6) C9 0.047(9) 0.027(7) 0.052(8) 0.005(6) 0.016(7) -0.002(6) C37 0.037(8) 0.041(8) 0.043(8) -0.002(6) -0.004(6) -0.003(6) C14 0.042(9) 0.032(7) 0.056(9) 0.003(6) -0.012(7) 0.002(6) C28 0.053(9) 0.026(7) 0.046(8) 0.005(6) 0.011(7) 0.000(6) C23 0.041(8) 0.038(8) 0.041(7) -0.003(6) 0.004(6) -0.008(6) Cl4 0.283(14) 0.137(8) 0.150(8) -0.023(6) 0.055(8) 0.006(8) Cl3 0.286(14) 0.135(8) 0.273(13) -0.020(9) 0.112(11) 0.005(9) C48 0.293(17) 0.156(14) 0.231(15) -0.023(13) 0.088(13) -0.011(13) 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 Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 I1 Ca1 Ca2 104.65(8) . . ? O1 Ca1 I1 105.1(2) . . ? O1 Ca1 Ca2 40.2(2) . . ? O1 Ca1 O2 80.5(3) . . ? O1 Ca1 O3 162.6(3) . . ? O1 Ca1 N2 75.3(3) . . ? O1 Ca1 N1 81.6(3) . . ? O2 Ca1 I1 98.4(2) . . ? O2 Ca1 Ca2 40.3(2) . . ? O2 Ca1 O3 103.1(3) . . ? O2 Ca1 N2 95.1(3) . . ? O2 Ca1 N1 160.0(3) . . ? O3 Ca1 I1 91.4(2) . . ? O3 Ca1 Ca2 141.1(3) . . ? O3 Ca1 N2 87.4(3) . . ? O3 Ca1 N1 91.4(3) . . ? N2 Ca1 I1 166.4(3) . . ? N2 Ca1 Ca2 84.5(3) . . ? N1 Ca1 I1 95.0(3) . . ? N1 Ca1 Ca2 121.4(3) . . ? N1 Ca1 N2 71.6(3) . . ? I2 Ca2 Ca1 138.70(9) . . ? O1 Ca2 I2 99.4(2) . . ? O1 Ca2 Ca1 39.5(2) . . ? O1 Ca2 O2 80.0(3) . . ? O1 Ca2 N5 157.0(4) . . ? O1 Ca2 O4 89.7(3) . . ? O1 Ca2 N6 108.9(4) . . ? O2 Ca2 I2 173.6(2) . . ? O2 Ca2 Ca1 40.5(2) . . ? O2 Ca2 N5 78.2(4) . . ? O2 Ca2 O4 97.0(3) . . ? O2 Ca2 N6 77.3(4) . . ? N5 Ca2 I2 103.0(3) . . ? N5 Ca2 Ca1 118.3(3) . . ? N5 Ca2 N6 73.4(4) . . ? O4 Ca2 I2 89.4(3) . . ? O4 Ca2 Ca1 93.6(3) . . ? O4 Ca2 N5 85.7(3) . . ? O4 Ca2 N6 158.9(4) . . ? N6 Ca2 I2 97.0(3) . . ? N6 Ca2 Ca1 94.8(3) . . ? Ca1 O1 Ca2 100.3(3) . . ? C1 O1 Ca1 127.6(8) . . ? C1 O1 Ca2 125.8(8) . . ? Ca2 O2 Ca1 99.1(3) . . ? C19 O2 Ca1 124.7(7) . . ? C19 O2 Ca2 129.0(7) . . ? C40 O3 Ca1 128.5(9) . . ? C37 O3 Ca1 125.9(8) . . ? C37 O3 C40 104.7(11) . . ? N5 N7 C20 120.1(10) . . ? C26 N7 N5 111.0(10) . . ? C26 N7 C20 128.8(10) . . ? N2 N4 C3 112.2(10) . . ? N2 N4 C2 121.1(10) . . ? C3 N4 C2 126.7(11) . . ? N7 N5 Ca2 119.7(8) . . ? C28 N5 Ca2 135.6(9) . . ? C28 N5 N7 104.6(10) . . ? N4 N2 Ca1 116.2(7) . . ? C5 N2 Ca1 137.5(9) . . ? C5 N2 N4 104.4(10) . . ? N3 N1 Ca1 117.1(8) . . ? C10 N1 Ca1 137.3(9) . . ? C10 N1 N3 105.6(10) . . ? C44 O4 Ca2 121.8(9) . . ? C41 O4 Ca2 126.3(8) . . ? C41 O4 C44 109.6(11) . . ? N1 N3 C2 122.3(10) . . ? C8 N3 N1 110.5(11) . . ? C8 N3 C2 127.1(11) . . ? N6 N8 C20 121.0(10) . . ? C21 N8 N6 112.3(11) . . ? C21 N8 C20 126.6(11) . . ? N4 C3 C7 122.4(12) . . ? C4 C3 N4 105.5(12) . . ? C4 C3 C7 132.1(13) . . ? C32 C31 C19 119.9(12) . . ? C32 C31 C36 119.0(12) . . ? C36 C31 C19 120.7(12) . . ? H38A C38 H38B 109.0 . . ? C39 C38 H38A 111.0 . . ? C39 C38 H38B 111.0 . . ? C37 C38 H38A 111.0 . . ? C37 C38 H38B 111.0 . . ? C37 C38 C39 103.9(12) . . ? N3 C8 C11 123.7(14) . . ? C9 C8 N3 107.0(12) . . ? C9 C8 C11 129.3(13) . . ? O1 C1 H1 107.7 . . ? O1 C1 C13 113.4(10) . . ? O1 C1 C2 113.2(11) . . ? C13 C1 H1 107.7 . . ? C13 C1 C2 107.0(10) . . ? C2 C1 H1 107.7 . . ? N8 N6 Ca2 117.9(8) . . ? C23 N6 Ca2 137.1(9) . . ? C23 N6 N8 104.9(11) . . ? O2 C19 C31 115.3(10) . . ? O2 C19 H19 107.3 . . ? O2 C19 C20 112.4(9) . . ? C31 C19 H19 107.3 . . ? C31 C19 C20 106.7(10) . . ? C20 C19 H19 107.3 . . ? N1 C10 C12 120.7(12) . . ? N1 C10 C9 110.8(12) . . ? C9 C10 C12 128.5(12) . . ? N7 C26 C29 121.8(12) . . ? C27 C26 N7 107.4(11) . . ? C27 C26 C29 130.7(13) . . ? N7 C20 C19 115.1(10) . . ? N7 C20 H20 105.7 . . ? N8 C20 N7 111.7(10) . . ? N8 C20 C19 112.0(10) . . ? N8 C20 H20 105.7 . . ? C19 C20 H20 105.7 . . ? C31 C32 H32 119.4 . . ? C31 C32 C33 121.1(14) . . ? C33 C32 H32 119.4 . . ? N8 C21 C22 106.0(12) . . ? N8 C21 C24 123.8(12) . . ? C22 C21 C24 130.1(12) . . ? C18 C13 C1 121.5(12) . . ? C18 C13 C14 118.5(12) . . ? C14 C13 C1 119.9(12) . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C5 C4 110.7(12) . . ? N2 C5 C6 121.2(12) . . ? C4 C5 C6 128.1(12) . . ? C26 C27 H27 126.7 . . ? C26 C27 C28 106.6(13) . . ? C28 C27 H27 126.7 . . ? O4 C44 H44A 110.8 . . ? O4 C44 H44B 110.8 . . ? O4 C44 C43 104.7(13) . . ? H44A C44 H44B 108.9 . . ? C43 C44 H44A 110.8 . . ? C43 C44 H44B 110.8 . . ? C44 C43 H43A 111.4 . . ? C44 C43 H43B 111.4 . . ? H43A C43 H43B 109.3 . . ? C42 C43 C44 101.7(14) . . ? C42 C43 H43A 111.4 . . ? C42 C43 H43B 111.4 . . ? H45A C45 H45B 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C46 C45 H45A 109.5 . . ? C46 C45 H45B 109.5 . . ? C46 C45 H45C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? C16 C15 H15 119.7 . . ? C16 C15 C14 120.7(15) . . ? C14 C15 H15 119.7 . . ? C45 C46 H46A 112.5 . . ? C45 C46 H46B 112.5 . . ? C45 C46 C47 96(3) . . ? H46A C46 H46B 110.0 . . ? C47 C46 H46A 112.5 . . ? C47 C46 H46B 112.5 . . ? O3 C40 H40A 110.7 . . ? O3 C40 H40B 110.7 . . ? O3 C40 C39 105.4(12) . . ? H40A C40 H40B 108.8 . . ? C39 C40 H40A 110.7 . . ? C39 C40 H40B 110.7 . . ? C46 C47 H47A 110.7 . . ? C46 C47 H47B 110.7 . . ? C47 C47 C46 105(3) 3_765 . ? C47 C47 H47A 110.7 3_765 . ? C47 C47 H47B 110.7 3_765 . ? H47A C47 H47B 108.8 . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C33 C34 C35 119.5(15) . . ? Cl1 C49 H49A 108.9 . . ? Cl1 C49 H49B 108.9 . . ? Cl2 C49 Cl1 113.4(13) . . ? Cl2 C49 H49A 108.9 . . ? Cl2 C49 H49B 108.9 . . ? H49A C49 H49B 107.7 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C34 C35 H35 119.5 . . ? C34 C35 C36 121.1(16) . . ? C36 C35 H35 119.5 . . ? C32 C33 H33 120.0 . . ? C34 C33 C32 120.0(15) . . ? C34 C33 H33 120.0 . . ? C43 C42 H42A 111.1 . . ? C43 C42 H42B 111.1 . . ? C43 C42 C41 103.2(13) . . ? H42A C42 H42B 109.1 . . ? C41 C42 H42A 111.1 . . ? C41 C42 H42B 111.1 . . ? C3 C4 C5 107.1(12) . . ? C3 C4 H4 126.5 . . ? C5 C4 H4 126.5 . . ? C16 C17 H17 120.7 . . ? C18 C17 H17 120.7 . . ? C18 C17 C16 118.7(14) . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C21 C22 H22 126.6 . . ? C21 C22 C23 106.9(12) . . ? C23 C22 H22 126.6 . . ? C15 C16 C17 120.3(13) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? O4 C41 C42 105.9(13) . . ? O4 C41 H41A 110.5 . . ? O4 C41 H41B 110.5 . . ? C42 C41 H41A 110.5 . . ? C42 C41 H41B 110.5 . . ? H41A C41 H41B 108.7 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? C31 C36 H36 120.4 . . ? C35 C36 C31 119.2(14) . . ? C35 C36 H36 120.4 . . ? C38 C39 H39A 110.7 . . ? C38 C39 H39B 110.7 . . ? C40 C39 C38 105.4(12) . . ? C40 C39 H39A 110.7 . . ? C40 C39 H39B 110.7 . . ? H39A C39 H39B 108.8 . . ? N4 C2 C1 112.5(11) . . ? N4 C2 H2 106.4 . . ? N3 C2 N4 110.1(11) . . ? N3 C2 C1 114.4(10) . . ? N3 C2 H2 106.4 . . ? C1 C2 H2 106.4 . . ? C13 C18 C17 121.5(13) . . ? C13 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C9 C10 106.2(12) . . ? C8 C9 H9 126.9 . . ? C10 C9 H9 126.9 . . ? O3 C37 C38 104.2(11) . . ? O3 C37 H37A 110.9 . . ? O3 C37 H37B 110.9 . . ? C38 C37 H37A 110.9 . . ? C38 C37 H37B 110.9 . . ? H37A C37 H37B 108.9 . . ? C13 C14 H14 119.8 . . ? C15 C14 C13 120.4(14) . . ? C15 C14 H14 119.8 . . ? N5 C28 C27 110.4(13) . . ? N5 C28 C30 120.7(12) . . ? C27 C28 C30 128.9(14) . . ? N6 C23 C22 109.7(12) . . ? N6 C23 C25 120.8(13) . . ? C22 C23 C25 129.3(13) . . ? Cl4 C48 H48A 109.5 . . ? Cl4 C48 H48B 109.5 . . ? Cl3 C48 Cl4 110.8 . . ? Cl3 C48 H48A 109.5 . . ? Cl3 C48 H48B 109.5 . . ? H48A C48 H48B 108.1 . . ? 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 I1 Ca1 3.129(3) . ? I2 Ca2 3.118(3) . ? Ca1 Ca2 3.468(4) . ? Ca1 O1 2.244(9) . ? Ca1 O2 2.282(9) . ? Ca1 O3 2.360(10) . ? Ca1 N2 2.534(11) . ? Ca1 N1 2.496(11) . ? Ca2 O1 2.273(9) . ? Ca2 O2 2.274(9) . ? Ca2 N5 2.458(10) . ? Ca2 O4 2.381(10) . ? Ca2 N6 2.517(12) . ? Cl1 C49 1.73(2) . ? Cl2 C49 1.72(2) . ? O1 C1 1.373(14) . ? O2 C19 1.397(14) . ? O3 C40 1.460(17) . ? O3 C37 1.433(16) . ? N7 N5 1.372(15) . ? N7 C26 1.351(16) . ? N7 C20 1.466(16) . ? N4 N2 1.365(15) . ? N4 C3 1.374(16) . ? N4 C2 1.457(15) . ? N5 C28 1.330(18) . ? N2 C5 1.346(16) . ? N1 N3 1.370(14) . ? N1 C10 1.330(16) . ? O4 C44 1.445(16) . ? O4 C41 1.430(18) . ? N3 C8 1.366(16) . ? N3 C2 1.442(17) . ? N8 N6 1.367(15) . ? N8 C20 1.447(16) . ? N8 C21 1.358(16) . ? C3 C4 1.363(19) . ? C3 C7 1.491(19) . ? C31 C19 1.527(17) . ? C31 C32 1.368(19) . ? C31 C36 1.406(19) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C38 C39 1.52(2) . ? C38 C37 1.52(2) . ? C8 C11 1.49(2) . ? C8 C9 1.36(2) . ? C1 H1 1.0000 . ? C1 C13 1.525(17) . ? C1 C2 1.549(19) . ? N6 C23 1.354(18) . ? C19 H19 1.0000 . ? C19 C20 1.560(17) . ? C10 C12 1.469(18) . ? C10 C9 1.395(19) . ? C26 C27 1.33(2) . ? C26 C29 1.513(18) . ? C20 H20 1.0000 . ? C32 H32 0.9500 . ? C32 C33 1.39(2) . ? C21 C22 1.372(19) . ? C21 C24 1.482(19) . ? C13 C18 1.378(19) . ? C13 C14 1.391(19) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C5 C4 1.40(2) . ? C5 C6 1.482(18) . ? C27 H27 0.9500 . ? C27 C28 1.400(19) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C44 C43 1.50(2) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C43 C42 1.50(2) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C45 C46 1.53(3) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C30 C28 1.489(19) . ? C15 H15 0.9500 . ? C15 C16 1.36(2) . ? C15 C14 1.39(2) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C46 C47 1.54(3) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C40 C39 1.50(2) . ? C47 C47 1.53(6) 3_765 ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C34 H34 0.9500 . ? C34 C35 1.38(2) . ? C34 C33 1.37(2) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C35 H35 0.9500 . ? C35 C36 1.39(2) . ? C33 H33 0.9500 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C42 C41 1.51(2) . ? C4 H4 0.9500 . ? C17 H17 0.9500 . ? C17 C16 1.40(2) . ? C17 C18 1.392(19) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C22 H22 0.9500 . ? C22 C23 1.41(2) . ? C16 H16 0.9500 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C25 C23 1.46(2) . ? C36 H36 0.9500 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C2 H2 1.0000 . ? C18 H18 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C9 H9 0.9500 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C14 H14 0.9500 . ? Cl4 C48 1.7773 . ? Cl3 C48 1.7651 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? 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 Ca1 O1 C1 C13 99.2(12) . . . . ? Ca1 O1 C1 C2 -22.9(15) . . . . ? Ca1 O2 C19 C31 -92.3(12) . . . . ? Ca1 O2 C19 C20 145.0(8) . . . . ? Ca1 O3 C40 C39 154.2(10) . . . . ? Ca1 O3 C37 C38 -149.2(9) . . . . ? Ca1 N2 C5 C4 -162.5(10) . . . . ? Ca1 N2 C5 C6 16(2) . . . . ? Ca1 N1 N3 C8 -178.6(8) . . . . ? Ca1 N1 N3 C2 -0.9(14) . . . . ? Ca1 N1 C10 C12 -3.5(19) . . . . ? Ca1 N1 C10 C9 178.5(9) . . . . ? Ca2 O1 C1 C13 -114.2(11) . . . . ? Ca2 O1 C1 C2 123.6(10) . . . . ? Ca2 O2 C19 C31 123.6(10) . . . . ? Ca2 O2 C19 C20 1.0(14) . . . . ? Ca2 N5 C28 C27 174.7(10) . . . . ? Ca2 N5 C28 C30 -4(2) . . . . ? Ca2 O4 C44 C43 143.8(12) . . . . ? Ca2 O4 C41 C42 -166.8(10) . . . . ? Ca2 N6 C23 C22 -170.7(11) . . . . ? Ca2 N6 C23 C25 6(2) . . . . ? O1 C1 C13 C18 -26.6(19) . . . . ? O1 C1 C13 C14 156.4(13) . . . . ? O1 C1 C2 N4 -51.9(15) . . . . ? O1 C1 C2 N3 74.6(13) . . . . ? O2 C19 C20 N7 62.6(13) . . . . ? O2 C19 C20 N8 -66.5(13) . . . . ? O3 C40 C39 C38 17.0(16) . . . . ? N7 N5 C28 C27 -1.4(16) . . . . ? N7 N5 C28 C30 179.6(13) . . . . ? N7 C26 C27 C28 -1.5(17) . . . . ? N4 N2 C5 C4 0.4(16) . . . . ? N4 N2 C5 C6 179.0(12) . . . . ? N4 C3 C4 C5 -2.3(17) . . . . ? N5 N7 C26 C27 0.7(16) . . . . ? N5 N7 C26 C29 176.0(12) . . . . ? N5 N7 C20 N8 64.9(14) . . . . ? N5 N7 C20 C19 -64.3(14) . . . . ? N2 N4 C3 C4 2.7(16) . . . . ? N2 N4 C3 C7 -178.9(13) . . . . ? N2 N4 C2 N3 -56.2(16) . . . . ? N2 N4 C2 C1 72.7(16) . . . . ? N2 C5 C4 C3 1.2(18) . . . . ? N1 N3 C8 C11 -178.4(12) . . . . ? N1 N3 C8 C9 -0.3(14) . . . . ? N1 N3 C2 N4 68.2(14) . . . . ? N1 N3 C2 C1 -59.5(15) . . . . ? N1 C10 C9 C8 -0.3(15) . . . . ? O4 C44 C43 C42 35.4(18) . . . . ? N3 N1 C10 C12 178.1(11) . . . . ? N3 N1 C10 C9 0.1(14) . . . . ? N3 C8 C9 C10 0.4(15) . . . . ? N8 N6 C23 C22 3.6(16) . . . . ? N8 N6 C23 C25 -179.4(13) . . . . ? N8 C21 C22 C23 3.6(16) . . . . ? C3 N4 N2 Ca1 165.3(9) . . . . ? C3 N4 N2 C5 -1.9(15) . . . . ? C3 N4 C2 N3 122.0(14) . . . . ? C3 N4 C2 C1 -109.1(15) . . . . ? C31 C19 C20 N7 -64.8(13) . . . . ? C31 C19 C20 N8 166.1(10) . . . . ? C31 C32 C33 C34 0(2) . . . . ? C8 N3 C2 N4 -114.5(13) . . . . ? C8 N3 C2 C1 117.7(13) . . . . ? C1 C13 C18 C17 -176.6(13) . . . . ? C1 C13 C14 C15 176.4(16) . . . . ? N6 N8 C20 N7 -61.7(15) . . . . ? N6 N8 C20 C19 69.0(15) . . . . ? N6 N8 C21 C22 -1.5(16) . . . . ? N6 N8 C21 C24 -178.4(13) . . . . ? C19 C31 C32 C33 174.0(13) . . . . ? C19 C31 C36 C35 -173.7(15) . . . . ? C10 N1 N3 C8 0.1(13) . . . . ? C10 N1 N3 C2 177.8(11) . . . . ? C26 N7 N5 Ca2 -176.4(9) . . . . ? C26 N7 N5 C28 0.5(15) . . . . ? C26 N7 C20 N8 -115.7(14) . . . . ? C26 N7 C20 C19 115.1(14) . . . . ? C26 C27 C28 N5 1.9(18) . . . . ? C26 C27 C28 C30 -179.2(16) . . . . ? C20 N7 N5 Ca2 3.1(14) . . . . ? C20 N7 N5 C28 180.0(11) . . . . ? C20 N7 C26 C27 -178.8(12) . . . . ? C20 N7 C26 C29 -3(2) . . . . ? C20 N8 N6 Ca2 -6.8(16) . . . . ? C20 N8 N6 C23 177.6(12) . . . . ? C20 N8 C21 C22 179.7(12) . . . . ? C20 N8 C21 C24 3(2) . . . . ? C32 C31 C19 O2 145.9(12) . . . . ? C32 C31 C19 C20 -88.5(14) . . . . ? C32 C31 C36 C35 0(2) . . . . ? C21 N8 N6 Ca2 174.3(9) . . . . ? C21 N8 N6 C23 -1.3(16) . . . . ? C21 N8 C20 N7 117.0(13) . . . . ? C21 N8 C20 C19 -112.2(13) . . . . ? C21 C22 C23 N6 -4.6(17) . . . . ? C21 C22 C23 C25 178.8(15) . . . . ? C13 C1 C2 N4 -177.5(11) . . . . ? C13 C1 C2 N3 -51.0(14) . . . . ? C12 C10 C9 C8 -178.2(13) . . . . ? C44 O4 C41 C42 -4.0(17) . . . . ? C44 C43 C42 C41 -37.4(19) . . . . ? C43 C42 C41 O4 26.2(18) . . . . ? C45 C46 C47 C47 171(4) . . . 3_765 ? C40 O3 C37 C38 41.1(14) . . . . ? C34 C35 C36 C31 0(3) . . . . ? C11 C8 C9 C10 178.3(14) . . . . ? C35 C34 C33 C32 0(3) . . . . ? C33 C34 C35 C36 1(3) . . . . ? C29 C26 C27 C28 -176.2(15) . . . . ? C16 C15 C14 C13 1(3) . . . . ? C16 C17 C18 C13 0(2) . . . . ? C41 O4 C44 C43 -20.0(18) . . . . ? C7 C3 C4 C5 179.5(16) . . . . ? C36 C31 C19 O2 -40.9(17) . . . . ? C36 C31 C19 C20 84.7(14) . . . . ? C36 C31 C32 C33 1(2) . . . . ? C39 C38 C37 O3 -29.6(15) . . . . ? C2 N4 N2 Ca1 -16.3(16) . . . . ? C2 N4 N2 C5 176.5(12) . . . . ? C2 N4 C3 C4 -175.6(14) . . . . ? C2 N4 C3 C7 3(2) . . . . ? C2 N3 C8 C11 4(2) . . . . ? C2 N3 C8 C9 -177.9(12) . . . . ? C2 C1 C13 C18 98.9(14) . . . . ? C2 C1 C13 C14 -78.1(16) . . . . ? C18 C13 C14 C15 -1(2) . . . . ? C18 C17 C16 C15 1(3) . . . . ? C24 C21 C22 C23 -179.7(14) . . . . ? C6 C5 C4 C3 -177.2(14) . . . . ? C37 O3 C40 C39 -36.5(15) . . . . ? C37 C38 C39 C40 7.3(16) . . . . ? C14 C13 C18 C17 0(2) . . . . ? C14 C15 C16 C17 -1(3) . . . . ?