#------------------------------------------------------------------------------ #$Date: 2019-11-17 07:26:06 +0200 (Sun, 17 Nov 2019) $ #$Revision: 228661 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/95/1549543.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_1549543 loop_ _publ_author_name 'Zhang, Hao' 'Wu, Yongzhen' 'Zhang, Weiwei' 'Li, Erpeng' 'Shen, Chao' 'Jiang, Huiyun' 'Tian, He' 'Zhu, Wei-Hong' _publ_section_title ; Low cost and stable quinoxaline-based hole-transporting materials with a D-A-D molecular configuration for efficient perovskite solar cells. ; _journal_issue 27 _journal_name_full 'Chemical science' _journal_page_first 5919 _journal_page_last 5928 _journal_paper_doi 10.1039/c8sc00731d _journal_volume 9 _journal_year 2018 _chemical_formula_moiety 'C60 H48 N4 O4' _chemical_formula_sum 'C60 H48 N4 O4' _chemical_formula_weight 889.02 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2017-06-27 _audit_creation_method ; Olex2 1.2 (compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337) ; _audit_update_record ; 2018-02-13 deposited with the CCDC. 2018-06-13 downloaded from the CCDC. ; _cell_angle_alpha 88.379(4) _cell_angle_beta 81.381(4) _cell_angle_gamma 74.642(4) _cell_formula_units_Z 2 _cell_length_a 12.0014(12) _cell_length_b 13.0411(12) _cell_length_c 17.0476(15) _cell_measurement_reflns_used 4207 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 26.281 _cell_measurement_theta_min 2.417 _cell_volume 2543.6(4) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 173.01 _diffrn_measured_fraction_theta_full 0.974 _diffrn_measured_fraction_theta_max 0.974 _diffrn_measurement_device_type 'Bruker D8Venture' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1287 _diffrn_reflns_av_unetI/netI 0.1232 _diffrn_reflns_Laue_measured_fraction_full 0.974 _diffrn_reflns_Laue_measured_fraction_max 0.974 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 33930 _diffrn_reflns_point_group_measured_fraction_full 0.974 _diffrn_reflns_point_group_measured_fraction_max 0.974 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.500 _diffrn_reflns_theta_min 2.514 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.5361 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1504 before and 0.0877 after correction. The Ratio of minimum to maximum transmission is 0.7190. The \l/2 correction factor is Not present.' _exptl_crystal_density_diffrn 1.161 _exptl_crystal_description block _exptl_crystal_F_000 936 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.267 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.054 _refine_ls_extinction_coef 0.024(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/8 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 647 _refine_ls_number_reflns 9238 _refine_ls_number_restraints 44 _refine_ls_restrained_S_all 1.032 _refine_ls_R_factor_all 0.1954 _refine_ls_R_factor_gt 0.0990 _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^)+(0.1219P)^2^+1.2160P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2315 _refine_ls_wR_factor_ref 0.2991 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4063 _reflns_number_total 9238 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8sc00731d2.cif _cod_data_source_block mo_d8v17152_0m _cod_depositor_comments 'Adding full bibliography for 1549543--1549544.cif.' _cod_database_code 1549543 _shelx_shelxl_version_number 2014/8 _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 0.999 _shelx_estimated_absorpt_t_min 0.989 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances O4-C57 1.48 with sigma of 0.02 O4'-C60' = O4-C60 1.48 with sigma of 0.02 O2-C46 = O2-C43 1.48 with sigma of 0.02 O2-C46' = O2-C46 = O2-C43 1.48 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints C21 \\sim C24 \\sim C25 \\sim C26: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 O2 \\sim C43 \\sim C46 \\sim C46': within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 4. Others Fixed Sof: C46(0.75) H46A(0.75) H46B(0.75) H46C(0.75) C46'(0.25) H46D(0.25) H46E(0.25) H46F(0.25) O4(0.5) C60(0.5) H60D(0.5) H60E(0.5) H60F(0.5) O4'(0.5) C60'(0.5) H60A(0.5) H60B(0.5) H60C(0.5) 5.a Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C25(H25), C26(H26), C28(H28), C29(H29), C31(H31), C32(H32), C34(H34), C35(H35), C37(H37), C38(H38), C41(H41), C42(H42), C44(H44), C45(H45), C48(H48), C49(H49), C51(H51), C52(H52), C55(H55), C56(H56), C58(H58), C59(H59) 5.b Idealised Me refined as rotating group: C39(H39A,H39B,H39C), C46(H46A,H46B,H46C), C46'(H46D,H46E,H46F), C53(H53A,H53B, H53C), C60(H60D,H60E,H60F), C60'(H60A,H60B,H60C) ; _shelx_res_file ; mo_d8v17152_0m.res created by SHELXL-2014/8 TITL mo_d8v17152_0m_a.res in P-1 REM Old TITL mo_d8v17152_0m in P-1 REM SHELXT solution in P-1 REM R1 0.380, Rweak 0.157, Alpha 0.178, Orientation as input REM Formula found by SHELXT: C62 N9 CELL 0.71073 12.0014 13.0411 17.0476 88.379 81.381 74.642 ZERR 2 0.0012 0.0012 0.0015 0.004 0.004 0.004 LATT 1 SFAC C H N O UNIT 120 96 8 8 DFIX 1.48 O4 C57 DFIX 1.48 O4' C60' O4 C60 DFIX 1.48 O2 C46 O2 C43 DFIX 1.48 O2 C46' O2 C46 O2 C43 SIMU 0.01 0.02 2 C21 C24 > C26 SIMU 0.01 0.02 2 O2 C43 C46 C46' L.S. 8 PLAN 20 SIZE 0.02 0.03 0.15 TEMP -100.14 BOND $H list 4 ABIN fmap 2 acta OMIT -3 51 OMIT 0 -1 1 OMIT 1 0 1 OMIT 1 1 0 OMIT -1 0 1 OMIT 1 -3 1 OMIT 0 3 3 OMIT 0 3 6 OMIT -3 -3 7 OMIT 1 1 1 OMIT -1 -3 4 OMIT -3 -3 2 OMIT 3 3 5 OMIT 5 -2 9 OMIT -2 3 5 OMIT 2 3 13 OMIT 10 1 7 OMIT 3 1 5 OMIT -1 -2 1 OMIT 1 -3 3 OMIT 1 -7 2 OMIT -4 4 12 OMIT -3 0 3 OMIT -1 -4 5 OMIT 10 2 10 OMIT -8 -1 9 OMIT 8 5 0 OMIT -1 4 5 OMIT 12 5 6 OMIT -4 1 0 OMIT 9 1 10 OMIT 0 -4 15 OMIT 10 2 11 OMIT 1 0 3 OMIT 3 -6 18 OMIT 3 -2 13 OMIT 1 1 4 OMIT -1 -12 6 OMIT 0 -3 8 OMIT 1 -1 8 OMIT -4 -2 6 OMIT -3 4 5 OMIT 9 -4 5 OMIT 4 6 6 OMIT 0 2 6 OMIT 5 -4 4 OMIT 4 0 4 OMIT -8 -2 8 OMIT 9 0 7 OMIT 4 -7 12 OMIT 1 2 5 OMIT 1 9 13 OMIT -11 4 3 OMIT 5 -2 6 OMIT -10 4 8 OMIT 7 0 3 OMIT 9 0 8 OMIT 10 0 11 OMIT -1 13 6 OMIT 3 2 4 OMIT 9 0 9 OMIT 11 1 5 OMIT -2 -1 1 OMIT -1 5 4 OMIT 6 11 12 OMIT 4 2 0 OMIT -8 -4 7 OMIT 8 9 1 OMIT -7 7 9 OMIT 3 4 5 OMIT 8 1 16 OMIT 7 -5 7 OMIT 10 3 10 OMIT 10 4 6 OMIT 12 4 3 OMIT -8 -11 4 OMIT -13 -5 3 OMIT 4 6 13 OMIT -8 5 1 OMIT 0 -4 3 OMIT -8 -4 10 OMIT 6 -2 6 OMIT 2 3 5 OMIT -1 4 2 OMIT 2 6 12 OMIT 7 -6 8 OMIT 0 -5 7 OMIT 3 -7 9 OMIT -8 1 13 OMIT 1 2 6 OMIT 1 -2 9 OMIT 8 -3 11 OMIT 5 -3 8 OMIT 0 2 8 OMIT -4 1 2 OMIT 4 -12 7 OMIT -5 3 14 OMIT -6 5 12 OMIT -2 0 4 OMIT 0 12 9 OMIT -6 7 6 OMIT -2 8 13 OMIT 3 5 8 OMIT 2 -7 17 OMIT 0 13 6 OMIT 6 1 5 OMIT 2 0 0 OMIT -2 4 7 OMIT -10 6 1 OMIT 5 0 0 OMIT 4 7 3 OMIT 10 0 7 OMIT 4 5 7 OMIT 11 1 2 OMIT 2 0 4 OMIT 6 -2 8 OMIT 2 6 0 OMIT -1 4 16 OMIT -9 -8 3 OMIT 9 3 9 OMIT -1 -10 4 OMIT 7 -6 6 OMIT 5 -5 8 OMIT 9 12 1 OMIT -1 3 15 OMIT -8 7 2 OMIT 8 8 10 OMIT 2 -5 9 OMIT 9 -6 4 OMIT 3 4 14 OMIT -3 -3 4 OMIT 5 8 3 OMIT 9 1 6 OMIT -3 5 5 OMIT -7 0 12 OMIT -4 2 2 OMIT -4 -4 7 OMIT 12 6 3 OMIT 3 2 13 OMIT 1 -7 15 OMIT 5 -11 1 OMIT 6 0 18 OMIT 5 8 10 OMIT 7 5 1 OMIT 9 3 8 OMIT -7 0 14 OMIT -2 -8 8 OMIT 6 -4 6 OMIT -4 5 4 OMIT 5 5 10 OMIT 2 3 0 OMIT 0 9 12 OMIT -2 -10 6 OMIT 7 -7 2 OMIT -4 6 15 OMIT 2 8 14 OMIT -7 -1 15 OMIT 11 4 15 OMIT -5 2 17 OMIT 4 6 1 OMIT -5 1 5 OMIT -3 3 1 OMIT 3 1 2 OMIT 1 7 12 OMIT 4 9 5 OMIT -8 3 3 OMIT -2 2 9 OMIT 8 -3 6 OMIT 7 -6 11 OMIT 9 -2 16 OMIT -10 4 3 OMIT -6 3 16 OMIT 0 3 2 OMIT 9 -4 8 OMIT -8 -9 4 OMIT 2 1 2 OMIT 2 0 1 OMIT 0 7 3 OMIT -1 0 19 OMIT 1 -4 3 OMIT 2 6 18 OMIT 8 -4 1 OMIT 1 12 9 OMIT 0 -8 15 OMIT -4 -3 6 OMIT 9 8 11 OMIT -3 -10 3 OMIT -1 12 9 OMIT 6 4 8 OMIT 3 13 10 OMIT 9 2 15 OMIT 11 -2 11 OMIT 5 2 2 OMIT 1 9 0 OMIT -1 -1 5 OMIT 3 1 18 OMIT -3 8 6 OMIT -6 2 13 OMIT 0 -4 2 OMIT 8 -3 4 OMIT -8 -12 5 OMIT 2 -6 16 OMIT 1 -4 8 OMIT 5 -1 11 OMIT -10 -4 9 OMIT -1 11 10 OMIT -9 4 1 OMIT 12 0 6 OMIT 1 -3 19 OMIT -1 4 4 OMIT 1 1 2 OMIT -3 0 2 OMIT 6 2 5 OMIT -1 0 2 OMIT 2 1 3 OMIT 2 2 4 OMIT -2 -5 2 OMIT 2 5 3 OMIT 0 4 6 OMIT 6 1 7 OMIT 2 1 1 OMIT 3 -3 8 OMIT -2 1 1 OMIT 4 -5 10 REM REM REM WGHT 0.121900 1.216000 EXTI 0.023644 FVAR 0.57747 O1 4 0.364014 0.971566 0.913684 11.00000 0.12225 0.09480 = 0.05483 -0.00309 -0.03202 0.01441 O2 4 -0.332883 0.898724 0.723129 11.00000 0.21881 0.11881 = 0.14790 -0.05548 0.10470 -0.07781 O3 4 1.175110 0.555209 -0.191487 11.00000 0.08831 0.08989 = 0.06107 -0.00011 -0.01483 -0.00689 N1 3 0.189696 0.775907 0.320717 11.00000 0.07272 0.05925 = 0.05630 -0.00588 -0.02365 0.00431 N2 3 0.278858 0.758381 0.161767 11.00000 0.06564 0.05783 = 0.05423 -0.01438 -0.01226 -0.00050 N3 3 0.134388 0.899691 0.669658 11.00000 0.14668 0.07819 = 0.05223 -0.00639 -0.05103 0.01169 N4 3 0.690437 0.633379 -0.125077 11.00000 0.06121 0.07810 = 0.07694 -0.01180 -0.00955 0.00191 C1 1 0.301003 0.782987 0.296844 11.00000 0.07102 0.05975 = 0.07033 -0.01691 -0.02536 0.01222 C2 1 0.367628 0.804514 0.352417 11.00000 0.07600 0.09169 = 0.07787 -0.03940 -0.03840 0.01988 C3 1 0.482744 0.797311 0.326889 11.00000 0.06494 0.13550 = 0.10531 -0.06680 -0.03290 0.02983 AFIX 43 H3 2 0.529047 0.812911 0.363159 11.00000 -1.20000 AFIX 0 C4 1 0.534391 0.767866 0.249483 11.00000 0.05738 0.10935 = 0.12021 -0.06500 -0.01992 0.01412 AFIX 43 H4 2 0.616162 0.758586 0.235705 11.00000 -1.20000 AFIX 0 C5 1 0.471191 0.751619 0.191909 11.00000 0.05934 0.07689 = 0.08916 -0.03660 -0.01325 0.00683 C6 1 0.349806 0.762782 0.215879 11.00000 0.06885 0.06133 = 0.06415 -0.01893 -0.02026 0.00115 C7 1 0.125831 0.760329 0.268073 11.00000 0.06949 0.05451 = 0.04836 0.00112 -0.01587 0.00122 C8 1 0.168694 0.759925 0.185823 11.00000 0.05390 0.05227 = 0.05388 -0.00738 -0.01021 0.00234 C9 1 0.010693 0.741910 0.302885 11.00000 0.07693 0.05423 = 0.04504 0.00382 -0.01902 -0.00605 C10 1 -0.054038 0.805074 0.367435 11.00000 0.08715 0.06413 = 0.04885 -0.00347 -0.00851 -0.00556 AFIX 43 H10 2 -0.026511 0.860345 0.386247 11.00000 -1.20000 AFIX 0 C11 1 -0.156300 0.787767 0.403458 11.00000 0.10205 0.06587 = 0.05626 0.00173 0.00788 -0.00909 AFIX 43 H11 2 -0.200296 0.831085 0.447230 11.00000 -1.20000 AFIX 0 C12 1 -0.196663 0.706287 0.376099 11.00000 0.09082 0.09229 = 0.06232 0.01452 -0.00660 -0.01974 AFIX 43 H12 2 -0.268154 0.694274 0.401332 11.00000 -1.20000 AFIX 0 C13 1 -0.133283 0.643359 0.312747 11.00000 0.10011 0.08045 = 0.06605 -0.00145 -0.01823 -0.02295 AFIX 43 H13 2 -0.161064 0.587979 0.294375 11.00000 -1.20000 AFIX 0 C14 1 -0.028663 0.660619 0.275543 11.00000 0.08774 0.07574 = 0.06403 -0.00742 -0.00846 -0.00965 AFIX 43 H14 2 0.015411 0.617188 0.231850 11.00000 -1.20000 AFIX 0 C15 1 0.097491 0.764325 0.119841 11.00000 0.06356 0.05755 = 0.04921 -0.00265 -0.01220 -0.00474 C16 1 0.152377 0.715313 0.047564 11.00000 0.06709 0.08117 = 0.05522 -0.00975 -0.01565 -0.01054 AFIX 43 H16 2 0.232960 0.678640 0.041434 11.00000 -1.20000 AFIX 0 C17 1 0.091424 0.719387 -0.014857 11.00000 0.06473 0.09606 = 0.05656 -0.01141 -0.00937 -0.00419 AFIX 43 H17 2 0.130056 0.685347 -0.063738 11.00000 -1.20000 AFIX 0 C18 1 -0.024678 0.772122 -0.007308 11.00000 0.08345 0.09620 = 0.05346 0.00383 -0.02211 -0.02063 AFIX 43 H18 2 -0.066438 0.774399 -0.050745 11.00000 -1.20000 AFIX 0 C19 1 -0.080541 0.821646 0.063098 11.00000 0.06683 0.07011 = 0.05737 -0.00325 -0.01347 -0.00402 AFIX 43 H19 2 -0.161017 0.858422 0.068018 11.00000 -1.20000 AFIX 0 C20 1 -0.020774 0.818705 0.127482 11.00000 0.06882 0.06555 = 0.05025 -0.00534 -0.01203 -0.00770 AFIX 43 H20 2 -0.060001 0.853295 0.176051 11.00000 -1.20000 AFIX 0 C21 1 0.311486 0.833018 0.436511 11.00000 0.08327 0.10364 = 0.07746 -0.04421 -0.04199 0.03211 C22 1 0.205711 0.909466 0.451681 11.00000 0.07583 0.05320 = 0.05780 -0.00571 -0.02013 -0.00029 AFIX 43 H22 2 0.170684 0.945393 0.408670 11.00000 -1.20000 AFIX 0 C23 1 0.150767 0.934060 0.527989 11.00000 0.08252 0.05036 = 0.05016 -0.00266 -0.02880 0.00494 AFIX 43 H23 2 0.079639 0.988544 0.536834 11.00000 -1.20000 AFIX 0 C24 1 0.196158 0.881797 0.591822 11.00000 0.12750 0.08082 = 0.06009 -0.02089 -0.04683 0.03316 C25 1 0.306561 0.808238 0.574889 11.00000 0.16670 0.14296 = 0.07589 -0.04078 -0.06990 0.08776 AFIX 43 H25 2 0.343433 0.772485 0.617263 11.00000 -1.20000 AFIX 0 C26 1 0.361216 0.787540 0.499014 11.00000 0.14154 0.15394 = 0.08381 -0.06382 -0.06878 0.08656 AFIX 43 H26 2 0.436838 0.739497 0.489834 11.00000 -1.20000 AFIX 0 C27 1 0.526011 0.722378 0.109157 11.00000 0.05526 0.07205 = 0.09395 -0.03046 -0.01505 0.00378 C28 1 0.611099 0.767828 0.072024 11.00000 0.05826 0.08802 = 0.10450 -0.04296 -0.01319 0.00300 AFIX 43 H28 2 0.632606 0.820183 0.099646 11.00000 -1.20000 AFIX 0 C29 1 0.666311 0.738893 -0.004978 11.00000 0.06759 0.08832 = 0.10630 -0.02523 0.00057 -0.00712 AFIX 43 H29 2 0.725091 0.770918 -0.029290 11.00000 -1.20000 AFIX 0 C30 1 0.634407 0.661744 -0.046639 11.00000 0.07245 0.06458 = 0.08021 -0.03230 -0.00831 0.00536 C31 1 0.548720 0.617283 -0.009525 11.00000 0.06641 0.06025 = 0.08939 -0.01789 0.00088 -0.01031 AFIX 43 H31 2 0.525037 0.566349 -0.037199 11.00000 -1.20000 AFIX 0 C32 1 0.496784 0.645695 0.067310 11.00000 0.06684 0.06294 = 0.08156 -0.03145 -0.00116 0.00105 AFIX 43 H32 2 0.439724 0.612097 0.092219 11.00000 -1.20000 AFIX 0 C33 1 0.190889 0.913976 0.732943 11.00000 0.16025 0.05739 = 0.05743 -0.00491 -0.05048 0.01675 C34 1 0.173405 0.869021 0.805664 11.00000 0.27524 0.06105 = 0.07099 0.01342 -0.09365 -0.03150 AFIX 43 H34 2 0.121097 0.825010 0.813161 11.00000 -1.20000 AFIX 0 C35 1 0.226930 0.883849 0.868128 11.00000 0.25390 0.05795 = 0.07816 0.00923 -0.07059 -0.04361 AFIX 43 H35 2 0.211838 0.851671 0.917886 11.00000 -1.20000 AFIX 0 C36 1 0.302446 0.946102 0.856794 11.00000 0.13510 0.07293 = 0.04253 -0.00978 -0.04276 0.03826 C37 1 0.326674 0.993823 0.783348 11.00000 0.11820 0.08837 = 0.06322 -0.00979 -0.02459 0.02163 AFIX 43 H37 2 0.381077 1.035783 0.775578 11.00000 -1.20000 AFIX 0 C38 1 0.268190 0.977168 0.723123 11.00000 0.12202 0.09066 = 0.04271 -0.00674 -0.02316 0.03979 AFIX 43 H38 2 0.281339 1.010046 0.673398 11.00000 -1.20000 AFIX 0 C39 1 0.345027 0.927216 0.991561 11.00000 0.15998 0.08719 = 0.06158 -0.01002 -0.05364 0.00698 AFIX 137 H39A 2 0.368186 0.849409 0.987531 11.00000 -1.50000 H39B 2 0.262110 0.951626 1.013692 11.00000 -1.50000 H39C 2 0.391897 0.950512 1.026318 11.00000 -1.50000 AFIX 0 C40 1 0.013965 0.900599 0.682633 11.00000 0.14501 0.06149 = 0.05017 0.01422 -0.03061 0.01122 C41 1 -0.031472 0.841049 0.634211 11.00000 0.13879 0.05515 = 0.03955 0.01117 -0.01461 0.00800 AFIX 43 H41 2 0.019328 0.798781 0.592173 11.00000 -1.20000 AFIX 0 C42 1 -0.146724 0.842630 0.646248 11.00000 0.12883 0.06073 = 0.07889 0.01965 0.02873 -0.00943 AFIX 43 H42 2 -0.178042 0.804699 0.612222 11.00000 -1.20000 AFIX 0 C43 1 -0.215075 0.900946 0.709174 11.00000 0.19114 0.06530 = 0.12222 -0.01613 0.08188 -0.04303 C44 1 -0.176371 0.958536 0.756499 11.00000 0.24380 0.04739 = 0.08448 0.00229 0.06288 -0.00721 AFIX 43 H44 2 -0.228783 0.998906 0.798778 11.00000 -1.20000 AFIX 0 C45 1 -0.061144 0.960193 0.744799 11.00000 0.21870 0.06418 = 0.04132 0.00107 0.00101 -0.00772 AFIX 43 H45 2 -0.033305 1.001361 0.778618 11.00000 -1.20000 AFIX 0 PART 1 C46 1 -0.370213 0.920089 0.810895 10.75000 0.15502 0.11737 = 0.15390 -0.02187 0.02585 -0.01884 AFIX 137 H46A 2 -0.394499 0.997010 0.820934 10.75000 -1.50000 H46B 2 -0.304641 0.887502 0.839330 10.75000 -1.50000 H46C 2 -0.435759 0.889642 0.829465 10.75000 -1.50000 AFIX 0 PART 0 PART 2 C46' 1 -0.395586 0.874682 0.666170 10.25000 0.18867 0.17193 = 0.15448 -0.05398 0.08316 -0.06240 AFIX 137 H46D 2 -0.444734 0.940710 0.647654 10.25000 -1.50000 H46E 2 -0.444999 0.829574 0.689862 10.25000 -1.50000 H46F 2 -0.340821 0.836970 0.621212 10.25000 -1.50000 AFIX 0 PART 0 C47 1 0.815331 0.609304 -0.140684 11.00000 0.07533 0.05990 = 0.06119 -0.00066 -0.01384 -0.00850 C48 1 0.884700 0.540366 -0.093661 11.00000 0.07449 0.06550 = 0.05073 0.00758 0.00111 -0.00122 AFIX 43 H48 2 0.848681 0.507069 -0.050515 11.00000 -1.20000 AFIX 0 C49 1 1.004523 0.518644 -0.107637 11.00000 0.07857 0.06788 = 0.04014 0.00865 -0.01215 0.00429 AFIX 43 H49 2 1.050620 0.471122 -0.074454 11.00000 -1.20000 AFIX 0 C50 1 1.057615 0.567178 -0.171088 11.00000 0.06508 0.06225 = 0.05102 -0.00012 -0.00382 -0.00370 C51 1 0.989468 0.634432 -0.219148 11.00000 0.08958 0.06549 = 0.04779 0.00710 -0.00407 -0.00827 AFIX 43 H51 2 1.025433 0.665240 -0.263768 11.00000 -1.20000 AFIX 0 C52 1 0.871357 0.657132 -0.203367 11.00000 0.09146 0.05782 = 0.06039 0.00490 -0.02172 0.01223 AFIX 43 H52 2 0.825680 0.706634 -0.235626 11.00000 -1.20000 AFIX 0 C53 1 1.248851 0.474711 -0.151026 11.00000 0.11181 0.10284 = 0.07758 0.00551 -0.00822 0.00873 AFIX 137 H53A 2 1.329389 0.460719 -0.178300 11.00000 -1.50000 H53B 2 1.222800 0.409501 -0.150397 11.00000 -1.50000 H53C 2 1.245327 0.498283 -0.096419 11.00000 -1.50000 AFIX 0 C54 1 0.629391 0.607030 -0.183250 11.00000 0.08118 0.05672 = 0.08496 0.00565 -0.03471 0.00176 C55 1 0.679977 0.526082 -0.236981 11.00000 0.12748 0.06442 = 0.10594 -0.01328 -0.06146 0.01507 AFIX 43 H55 2 0.757616 0.484694 -0.235032 11.00000 -1.20000 AFIX 0 C56 1 0.618685 0.504097 -0.294211 11.00000 0.16008 0.06255 = 0.12072 -0.00261 -0.07589 -0.00201 AFIX 43 H56 2 0.654517 0.448815 -0.332185 11.00000 -1.20000 AFIX 0 C57 1 0.507097 0.562147 -0.295586 11.00000 0.12824 0.08780 = 0.13287 0.04980 -0.07894 -0.03089 C58 1 0.454123 0.640968 -0.243608 11.00000 0.10334 0.09696 = 0.13394 0.04626 -0.04637 -0.01386 AFIX 43 H58 2 0.375327 0.679885 -0.244656 11.00000 -1.20000 AFIX 0 C59 1 0.516104 0.663892 -0.189225 11.00000 0.07895 0.07433 = 0.10563 0.01676 -0.01985 -0.00165 AFIX 43 H59 2 0.479893 0.721814 -0.153535 11.00000 -1.20000 AFIX 0 PART 1 O4 4 0.423103 0.554390 -0.340596 10.50000 0.05183 0.10057 = 0.07669 0.00828 -0.01541 0.01587 C60 1 0.463690 0.472516 -0.398517 10.50000 0.11020 0.10192 = 0.07151 0.00486 -0.04539 -0.02808 AFIX 137 H60D 2 0.405983 0.479019 -0.434664 10.50000 -1.50000 H60E 2 0.475312 0.403303 -0.372480 10.50000 -1.50000 H60F 2 0.537954 0.478380 -0.428623 10.50000 -1.50000 AFIX 0 PART 0 PART 2 O4' 4 0.486511 0.517602 -0.377604 10.50000 0.08912 0.16383 = 0.09761 0.02348 -0.04824 -0.04570 C60' 1 0.362347 0.541699 -0.369173 10.50000 0.11568 0.13496 = 0.30415 0.08067 -0.04764 -0.03690 AFIX 137 H60A 2 0.339161 0.519844 -0.417466 10.50000 -1.50000 H60B 2 0.329134 0.618394 -0.360557 10.50000 -1.50000 H60C 2 0.333346 0.503434 -0.323698 10.50000 -1.50000 AFIX 0 HKLF 4 REM mo_d8v17152_0m_a.res in P-1 REM R1 = 0.0990 for 4063 Fo > 4sig(Fo) and 0.1954 for all 9238 data REM 647 parameters refined using 44 restraints END WGHT 0.1219 1.2192 REM Highest difference peak 0.267, deepest hole -0.303, 1-sigma level 0.054 Q1 1 -0.2923 0.8784 0.7424 11.00000 0.05 0.27 Q2 1 0.3268 0.7386 0.5135 11.00000 0.05 0.26 Q3 1 -0.1420 0.9452 0.7741 11.00000 0.05 0.26 Q4 1 0.8009 0.5816 -0.2766 11.00000 0.05 0.25 Q5 1 -0.3769 0.9314 0.6962 11.00000 0.05 0.24 Q6 1 0.4728 0.9168 0.8888 11.00000 0.05 0.20 Q7 1 0.7049 0.5569 -0.2736 11.00000 0.05 0.20 Q8 1 0.3098 0.7564 0.1030 11.00000 0.05 0.20 Q9 1 0.7365 0.5421 -0.2757 11.00000 0.05 0.19 Q10 1 0.4541 0.7993 0.1622 11.00000 0.05 0.19 Q11 1 0.0194 0.9420 0.5414 11.00000 0.05 0.18 Q12 1 0.3974 0.8169 0.4844 11.00000 0.05 0.18 Q13 1 0.2121 0.7865 0.0944 11.00000 0.05 0.18 Q14 1 1.2741 0.5245 -0.2223 11.00000 0.05 0.18 Q15 1 0.1244 0.8429 0.9310 11.00000 0.05 0.18 Q16 1 0.6282 0.8206 0.2041 11.00000 0.05 0.18 Q17 1 -0.0535 0.7170 -0.1358 11.00000 0.05 0.17 Q18 1 0.1250 0.8282 0.3883 11.00000 0.05 0.17 Q19 1 0.4941 0.9208 0.4140 11.00000 0.05 0.17 Q20 1 0.4964 0.7981 0.2124 11.00000 0.05 0.17 ; _shelx_res_checksum 12613 _shelx_fab_file ; -14 -6 1 1.6929 -0.0001 -14 -5 1 -2.0684 -0.0007 -14 -5 2 3.7437 0.0004 -14 -4 1 2.7994 0.0002 -14 -4 2 -1.3239 0.0001 -14 -3 1 -0.5347 0.0005 -14 -3 2 -0.3766 -0.0009 -14 -2 1 0.9844 -0.0007 -13 -9 1 -2.1165 -0.0000 -13 -9 2 2.5769 0.0000 -13 -9 3 -1.8396 0.0001 -13 -8 1 3.9314 -0.0005 -13 -8 2 -2.5128 0.0006 -13 -8 3 2.0648 -0.0004 -13 -8 4 -0.2877 0.0002 -13 -7 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11 10 6 -2.1878 0.0003 11 10 7 0.3128 -0.0003 11 10 8 -2.5922 0.0004 11 10 9 0.5888 -0.0003 11 10 10 -1.2827 0.0002 11 10 11 -1.2049 -0.0003 11 11 0 3.4267 -0.0005 11 11 1 -1.3047 0.0002 11 11 2 0.1393 0.0001 11 11 3 0.8079 -0.0005 11 11 4 -0.7582 0.0006 11 11 5 -1.3456 -0.0002 11 11 6 0.4761 -0.0002 11 11 7 -2.7076 0.0004 11 11 8 0.3106 -0.0002 11 11 9 -1.3171 -0.0002 11 11 10 -1.0881 0.0003 11 12 0 2.4722 0.0002 11 12 1 -3.3621 -0.0005 11 12 2 3.4642 0.0003 11 12 3 -1.8732 0.0000 11 12 4 0.0767 -0.0002 11 12 5 -0.4393 0.0001 11 12 6 -1.1508 -0.0000 11 12 7 -0.4151 0.0002 11 12 8 -1.5850 -0.0005 11 13 1 -0.7597 0.0007 11 13 2 0.6553 0.0001 11 13 3 0.4055 -0.0006 11 13 4 -2.0861 0.0005 12 -5 1 0.0923 -0.0006 12 -5 2 -1.4762 -0.0001 12 -5 3 1.2893 0.0001 12 -5 4 -2.0235 -0.0005 12 -4 0 -3.0514 -0.0009 12 -4 1 1.9475 0.0007 12 -4 2 -0.8868 -0.0010 12 -4 3 -1.7920 0.0005 12 -4 4 1.3820 -0.0002 12 -4 5 -1.6510 -0.0000 12 -4 6 -0.0276 0.0002 12 -4 7 -0.8568 0.0003 12 -4 8 0.1612 -0.0003 12 -3 0 -3.2407 0.0011 12 -3 1 4.4501 -0.0014 12 -3 2 -5.6368 0.0009 12 -3 3 3.1149 -0.0004 12 -3 4 -1.8870 -0.0000 12 -3 5 -1.0370 -0.0001 12 -3 6 0.7556 0.0005 12 -3 7 -1.7231 -0.0005 12 -3 8 -0.2858 0.0005 12 -3 9 -0.6422 0.0001 12 -3 10 -1.0513 -0.0003 12 -2 0 0.4862 -0.0009 12 -2 1 -0.6496 0.0004 12 -2 2 -0.5493 0.0003 12 -2 3 -0.7260 -0.0008 12 -2 4 0.1527 0.0006 12 -2 5 -2.0567 -0.0001 12 -2 6 1.5538 -0.0002 12 -2 7 -2.8601 0.0004 12 -2 8 1.5150 0.0000 12 -2 9 -2.7433 0.0000 12 -2 10 1.1717 0.0000 12 -2 11 -2.1176 0.0003 12 -1 0 0.0181 0.0010 12 -1 1 -0.0893 -0.0002 12 -1 2 -0.9972 -0.0005 12 -1 3 -0.2731 0.0008 12 -1 4 -0.4470 -0.0007 12 -1 5 -1.2967 0.0003 12 -1 6 0.8233 0.0002 12 -1 7 -1.6651 -0.0002 12 -1 8 0.1622 0.0002 12 -1 9 -0.6790 0.0003 12 -1 10 -1.0274 -0.0002 12 -1 11 0.3673 0.0002 12 -1 12 -0.4503 0.0001 12 0 0 -2.2344 -0.0003 12 0 1 1.9690 0.0004 12 0 2 -1.9308 -0.0002 12 0 3 -0.3137 -0.0001 12 0 4 -0.0910 -0.0001 12 0 5 -1.0085 0.0005 12 0 6 0.2756 -0.0008 12 0 7 -0.5662 0.0007 12 0 8 -0.5466 -0.0001 12 0 9 0.2640 -0.0002 12 0 10 -1.5070 0.0003 12 0 11 0.7363 0.0001 12 0 12 -0.3734 -0.0004 12 0 13 -0.3080 0.0002 12 1 0 -0.5321 0.0001 12 1 1 2.0721 -0.0001 12 1 2 -4.0923 -0.0002 12 1 3 2.7816 0.0005 12 1 4 -1.9864 -0.0006 12 1 5 -0.6338 0.0001 12 1 6 1.6859 0.0003 12 1 7 -2.3742 -0.0004 12 1 8 1.9608 0.0002 12 1 9 -1.8792 0.0002 12 1 10 0.4624 -0.0001 12 1 11 -0.0819 -0.0001 12 1 12 -0.7801 0.0003 12 1 13 0.7976 -0.0002 12 2 0 -0.3343 -0.0003 12 2 1 -0.3384 0.0004 12 2 2 0.0061 -0.0001 12 2 3 -0.5989 -0.0004 12 2 4 -0.2393 0.0002 12 2 5 -0.2479 -0.0000 12 2 6 0.7139 -0.0003 12 2 7 -0.7918 -0.0000 12 2 8 0.3783 0.0005 12 2 9 0.3730 -0.0007 12 2 10 -1.5263 0.0004 12 2 11 1.2324 0.0003 12 2 12 -1.0879 -0.0006 12 2 13 0.6545 0.0004 12 3 0 0.8681 0.0013 12 3 1 -0.3518 -0.0009 12 3 2 -0.1045 -0.0000 12 3 3 -0.6898 0.0004 12 3 4 0.4630 -0.0005 12 3 5 0.0106 -0.0000 12 3 6 -0.4009 0.0002 12 3 7 0.5454 -0.0001 12 3 8 0.6997 -0.0002 12 3 9 -1.7363 0.0004 12 3 10 1.4265 -0.0003 12 3 11 -0.7954 0.0002 12 3 12 -0.5612 -0.0001 12 3 13 0.6315 0.0001 12 3 14 0.2203 -0.0001 12 4 0 -0.7944 -0.0007 12 4 1 1.7322 0.0001 12 4 2 -2.1223 -0.0000 12 4 3 1.4958 0.0001 12 4 4 -0.3603 -0.0008 12 4 5 -0.5963 0.0010 12 4 6 0.9093 -0.0008 12 4 7 0.4691 0.0002 12 4 8 -1.5803 0.0004 12 4 9 1.9519 -0.0005 12 4 10 -1.8932 0.0003 12 4 11 1.0660 -0.0000 12 4 12 -1.4724 -0.0002 12 4 13 1.3245 0.0001 12 4 14 -0.8007 0.0003 12 5 0 -1.2641 -0.0008 12 5 1 2.1507 0.0009 12 5 2 -1.3804 -0.0009 12 5 3 0.4467 0.0003 12 5 4 0.4483 -0.0002 12 5 5 -0.2890 0.0002 12 5 6 -0.0757 -0.0004 12 5 7 0.5356 0.0006 12 5 8 -0.5716 -0.0005 12 5 9 -0.2562 0.0003 12 5 10 0.4423 -0.0001 12 5 11 -1.1634 0.0000 12 5 12 0.2266 -0.0002 12 5 13 0.5080 0.0003 12 6 0 2.2136 0.0016 12 6 1 -0.2883 -0.0013 12 6 2 -0.2835 0.0005 12 6 3 0.6358 0.0000 12 6 4 0.5742 -0.0003 12 6 5 -1.4931 0.0002 12 6 6 1.1680 0.0001 12 6 7 -0.2905 -0.0002 12 6 8 -1.5958 0.0003 12 6 9 1.3500 -0.0003 12 6 10 -1.3149 0.0002 12 6 11 -0.2222 -0.0002 12 6 12 0.0836 -0.0001 12 6 13 -0.0188 0.0002 12 7 0 3.4984 -0.0009 12 7 1 -1.2254 0.0006 12 7 2 1.1261 -0.0004 12 7 3 -0.8464 0.0000 12 7 4 1.8157 0.0001 12 7 5 -2.5954 -0.0000 12 7 6 1.5475 -0.0000 12 7 7 -0.9699 0.0002 12 7 8 -2.0343 -0.0000 12 7 9 2.3730 -0.0001 12 7 10 -3.1468 0.0002 12 7 11 1.0231 -0.0003 12 7 12 -0.0312 -0.0000 12 7 13 -0.3728 0.0002 12 8 0 -0.4816 0.0002 12 8 1 1.3652 0.0000 12 8 2 -1.0929 -0.0005 12 8 3 2.1119 0.0007 12 8 4 -1.8754 -0.0005 12 8 5 0.2707 0.0003 12 8 6 -0.1450 0.0002 12 8 7 -2.0494 -0.0003 12 8 8 0.4188 0.0004 12 8 9 -0.9479 -0.0002 12 8 10 -1.1938 -0.0000 12 8 11 0.9835 0.0000 12 8 12 -1.0766 -0.0001 12 9 0 -0.7647 -0.0006 12 9 1 2.4121 0.0004 12 9 2 -1.5421 -0.0002 12 9 3 1.2625 0.0000 12 9 4 -0.5097 0.0002 12 9 5 -1.1672 0.0001 12 9 6 0.0267 -0.0002 12 9 7 -1.9112 0.0005 12 9 8 -0.3551 -0.0004 12 9 9 -0.5901 0.0002 12 9 10 -1.2310 -0.0002 12 9 11 0.5210 0.0002 12 10 0 -0.6019 -0.0002 12 10 1 1.1604 0.0001 12 10 2 -0.4287 -0.0001 12 10 3 1.0792 0.0002 12 10 4 -1.8858 0.0001 12 10 5 1.0254 -0.0002 12 10 6 -2.9959 0.0004 12 10 7 0.7317 -0.0003 12 10 8 -2.2304 -0.0001 12 10 9 -0.0384 0.0003 12 11 0 -0.9138 -0.0004 12 11 1 1.2752 0.0004 12 11 2 -0.1387 -0.0002 12 11 3 -0.0964 0.0000 12 11 4 -0.2020 0.0002 12 11 5 -1.3903 -0.0001 12 11 6 -0.1208 0.0000 12 11 7 -2.2247 0.0000 12 12 2 0.0024 -0.0007 12 12 3 -1.7051 0.0006 13 -3 2 -0.0553 -0.0008 13 -3 3 1.6765 0.0007 13 -3 4 -4.5508 -0.0005 13 -2 0 0.9871 0.0001 13 -2 1 -3.7118 -0.0004 13 -2 2 4.4365 0.0003 13 -2 3 -5.6507 -0.0005 13 -2 4 2.6449 0.0004 13 -2 5 -1.0957 0.0000 13 -2 6 -2.2836 -0.0003 13 -2 7 2.2060 0.0005 13 -1 0 0.1187 0.0006 13 -1 1 -0.2800 -0.0008 13 -1 2 -1.1964 0.0003 13 -1 3 -0.2762 0.0000 13 -1 4 -0.2054 -0.0001 13 -1 5 -1.6158 -0.0002 13 -1 6 1.2555 0.0005 13 -1 7 -2.6423 -0.0002 13 -1 8 1.4512 -0.0001 13 -1 9 -2.2237 0.0004 13 0 0 0.2029 -0.0010 13 0 1 -1.3683 0.0004 13 0 2 -0.0509 0.0001 13 0 3 -0.0538 -0.0004 13 0 4 -2.4534 -0.0000 13 0 5 3.0520 0.0004 13 0 6 -4.5116 -0.0005 13 0 7 3.8825 0.0003 13 0 8 -3.6972 0.0003 13 0 9 1.2562 -0.0004 13 0 10 -0.4401 0.0002 13 1 0 3.2568 -0.0012 13 1 1 -4.7362 0.0014 13 1 2 3.3999 -0.0012 13 1 3 -3.0469 0.0006 13 1 4 1.0029 -0.0002 13 1 5 -0.8097 -0.0001 13 1 6 0.6822 -0.0000 13 1 7 -0.9825 0.0004 13 1 8 0.7807 -0.0004 13 1 9 -1.1521 0.0003 13 1 10 0.5082 0.0001 13 1 11 -0.9781 -0.0006 13 2 0 -3.7487 0.0018 13 2 1 2.4552 -0.0017 13 2 2 -1.4308 0.0011 13 2 3 -0.2080 -0.0008 13 2 4 -0.5127 0.0004 13 2 5 1.6288 -0.0004 13 2 6 -2.0711 0.0003 13 2 7 2.4739 -0.0001 13 2 8 -1.9752 0.0001 13 2 9 1.7003 0.0000 13 2 10 -2.0861 -0.0000 13 2 11 1.7349 0.0000 13 3 0 2.6854 -0.0006 13 3 1 -2.2983 0.0001 13 3 2 1.3117 0.0001 13 3 3 -1.2662 -0.0003 13 3 4 1.3822 0.0001 13 3 5 -0.8562 -0.0000 13 3 6 1.1714 -0.0002 13 3 7 -0.2101 0.0004 13 3 8 0.9829 -0.0004 13 3 9 -1.7652 0.0004 13 3 10 2.5361 -0.0001 13 3 11 -3.1429 -0.0003 13 4 0 2.1790 0.0001 13 4 1 -2.4852 0.0002 13 4 2 1.8708 -0.0006 13 4 3 0.1993 0.0006 13 4 4 -1.6010 -0.0007 13 4 5 2.9414 0.0004 13 4 6 -1.3994 -0.0002 13 4 7 1.2909 0.0000 13 4 8 -0.7139 0.0000 13 4 9 1.6499 0.0001 13 4 10 -2.3989 -0.0003 13 4 11 1.8079 0.0001 13 5 0 -0.8234 -0.0001 13 5 1 1.0756 -0.0002 13 5 2 0.0513 0.0003 13 5 3 0.0602 -0.0005 13 5 4 0.5369 0.0004 13 5 5 0.8425 -0.0003 13 5 6 -0.3831 0.0001 13 5 7 0.5206 0.0000 13 5 8 0.8636 0.0001 13 5 9 -1.4101 -0.0003 13 5 10 0.9402 0.0004 13 5 11 -0.7712 -0.0005 13 6 0 0.9150 0.0003 13 6 1 -2.2483 -0.0005 13 6 2 3.4947 0.0003 13 6 3 -1.2435 -0.0001 13 6 4 0.3082 -0.0000 13 6 5 0.9705 -0.0001 13 6 6 0.2488 0.0004 13 6 7 -1.3609 -0.0005 13 6 8 2.5609 0.0002 13 6 9 -3.2245 0.0001 13 6 10 2.4139 -0.0004 13 6 11 -1.7179 0.0004 13 7 0 -1.6537 0.0001 13 7 1 2.2001 -0.0003 13 7 2 0.1209 0.0005 13 7 3 0.2575 -0.0005 13 7 4 -0.2238 0.0002 13 7 5 1.8182 0.0004 13 7 6 -2.6546 -0.0006 13 7 7 2.3750 0.0006 13 7 8 -2.3650 -0.0003 13 7 9 1.6696 -0.0000 13 7 10 -2.4890 0.0001 13 8 0 -2.3852 -0.0006 13 8 1 2.8410 0.0005 13 8 2 -0.8758 -0.0004 13 8 3 1.5781 0.0004 13 8 4 -1.5197 -0.0002 13 8 5 1.7444 0.0003 13 8 6 -1.9592 -0.0004 13 8 7 -0.1743 0.0005 13 8 8 1.3287 -0.0006 13 8 9 -4.0900 0.0005 13 9 0 3.8028 -0.0001 13 9 1 -2.6881 0.0002 13 9 2 3.7362 -0.0002 13 9 3 -2.6483 0.0004 13 9 4 2.0170 -0.0002 13 9 5 -1.6891 0.0003 13 9 6 -0.2481 -0.0001 13 9 7 -0.3862 0.0001 13 9 8 -1.1957 -0.0001 13 10 0 -0.5349 0.0000 13 10 1 1.2336 -0.0000 13 10 2 0.5812 0.0001 13 10 3 -0.7356 0.0001 13 10 4 0.5349 0.0001 13 10 5 -1.1072 -0.0001 13 10 6 -0.9824 0.0003 14 0 2 0.5452 -0.0003 14 0 3 -2.7171 0.0005 14 0 4 1.8170 -0.0005 14 1 0 0.5089 -0.0002 14 1 1 0.1400 -0.0002 14 1 2 -1.7765 0.0000 14 1 3 0.4771 -0.0001 14 1 4 0.4591 0.0000 14 1 5 -1.9486 -0.0002 14 1 6 2.7097 0.0003 14 2 0 -1.9686 -0.0004 14 2 1 2.6215 -0.0000 14 2 2 -4.1639 0.0000 14 2 3 3.7514 -0.0000 14 2 4 -3.1010 -0.0002 14 2 5 2.6712 0.0001 14 2 6 -1.5455 0.0001 14 2 7 1.6686 -0.0003 14 3 0 2.1430 0.0001 14 3 1 -3.3698 -0.0002 14 3 2 3.3236 0.0004 14 3 3 -3.4136 -0.0009 14 3 4 4.4021 0.0007 14 3 5 -4.2937 -0.0004 14 3 6 5.3917 0.0001 14 3 7 -3.6907 -0.0000 14 3 8 3.0680 0.0003 14 4 0 -2.7576 0.0002 14 4 1 2.2933 -0.0001 14 4 2 -1.1715 -0.0001 14 4 3 1.3753 0.0000 14 4 4 -1.1392 0.0002 14 4 5 3.2097 -0.0005 14 4 6 -2.4936 0.0005 14 4 7 3.5295 -0.0003 14 4 8 -2.5344 -0.0000 14 5 0 0.5010 -0.0007 14 5 1 2.2826 0.0005 14 5 2 -2.0728 -0.0003 14 5 3 1.1526 0.0001 14 5 4 2.9262 -0.0002 14 5 5 -3.8118 0.0003 14 5 6 5.2006 -0.0004 14 5 7 -2.6939 0.0004 14 5 8 1.7506 -0.0003 14 6 0 -0.2090 -0.0001 14 6 1 0.9072 0.0002 14 6 2 0.0237 -0.0002 14 6 3 1.7371 0.0000 14 6 4 -1.1613 0.0002 14 6 5 2.3797 -0.0003 14 6 6 -0.8491 0.0002 14 6 7 1.1111 -0.0001 14 7 0 1.9786 0.0001 14 7 1 1.2285 -0.0001 14 7 2 -0.6006 0.0003 14 7 3 0.6951 -0.0003 14 7 4 2.2258 0.0005 14 7 5 -2.3600 -0.0005 14 7 6 2.4330 0.0005 14 8 2 1.6181 0.0001 14 8 3 0.4326 -0.0001 14 8 4 0.3687 0.0004 0 0 0 0.0 0.0 ; _shelx_fab_checksum 41408 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 O1 O 0.3640(3) 0.9716(3) 0.9137(2) 0.0968(13) Uani 1 1 d . . . . . O2 O -0.3329(6) 0.8987(4) 0.7231(4) 0.168(2) Uani 1 1 d D U . . . O3 O 1.1751(3) 0.5552(3) -0.19149(19) 0.0825(10) Uani 1 1 d . . . . . N1 N 0.1897(4) 0.7759(3) 0.3207(2) 0.0653(11) Uani 1 1 d . . . . . N2 N 0.2789(4) 0.7584(3) 0.1618(2) 0.0616(10) Uani 1 1 d . . . . . N3 N 0.1344(6) 0.8997(4) 0.6697(3) 0.0963(16) Uani 1 1 d . . . . . N4 N 0.6904(4) 0.6334(3) -0.1251(3) 0.0758(12) Uani 1 1 d . . . . . C1 C 0.3010(5) 0.7830(4) 0.2968(3) 0.0708(14) Uani 1 1 d . . . . . C2 C 0.3676(5) 0.8045(4) 0.3524(3) 0.0863(18) Uani 1 1 d . . . . . C3 C 0.4827(5) 0.7973(5) 0.3269(4) 0.109(2) Uani 1 1 d . . . . . H3 H 0.5290 0.8129 0.3632 0.131 Uiso 1 1 calc R . . . . C4 C 0.5344(5) 0.7679(5) 0.2495(4) 0.101(2) Uani 1 1 d . . . . . H4 H 0.6162 0.7586 0.2357 0.121 Uiso 1 1 calc R . . . . C5 C 0.4712(4) 0.7516(4) 0.1919(3) 0.0789(16) Uani 1 1 d . . . . . C6 C 0.3498(4) 0.7628(4) 0.2159(3) 0.0668(13) Uani 1 1 d . . . . . C7 C 0.1258(4) 0.7603(3) 0.2681(3) 0.0601(12) Uani 1 1 d . . . . . C8 C 0.1687(4) 0.7599(3) 0.1858(3) 0.0561(12) Uani 1 1 d . . . . . C9 C 0.0107(4) 0.7419(4) 0.3029(3) 0.0599(12) Uani 1 1 d . . . . . C10 C -0.0540(5) 0.8051(4) 0.3674(3) 0.0696(14) Uani 1 1 d . . . . . H10 H -0.0265 0.8603 0.3862 0.083 Uiso 1 1 calc R . . . . C11 C -0.1563(5) 0.7878(4) 0.4035(3) 0.0793(16) Uani 1 1 d . . . . . H11 H -0.2003 0.8311 0.4472 0.095 Uiso 1 1 calc R . . . . C12 C -0.1967(5) 0.7063(5) 0.3761(3) 0.0834(16) Uani 1 1 d . . . . . H12 H -0.2682 0.6943 0.4013 0.100 Uiso 1 1 calc R . . . . C13 C -0.1333(5) 0.6434(4) 0.3127(3) 0.0817(15) Uani 1 1 d . . . . . H13 H -0.1611 0.5880 0.2944 0.098 Uiso 1 1 calc R . . . . C14 C -0.0287(5) 0.6606(4) 0.2755(3) 0.0782(15) Uani 1 1 d . . . . . H14 H 0.0154 0.6172 0.2318 0.094 Uiso 1 1 calc R . . . . C15 C 0.0975(4) 0.7643(3) 0.1198(3) 0.0585(12) Uani 1 1 d . . . . . C16 C 0.1524(4) 0.7153(4) 0.0476(3) 0.0686(13) Uani 1 1 d . . . . . H16 H 0.2330 0.6786 0.0414 0.082 Uiso 1 1 calc R . . . . C17 C 0.0914(4) 0.7194(4) -0.0149(3) 0.0754(15) Uani 1 1 d . . . . . H17 H 0.1301 0.6853 -0.0637 0.091 Uiso 1 1 calc R . . . . C18 C -0.0247(5) 0.7721(4) -0.0073(3) 0.0771(15) Uani 1 1 d . . . . . H18 H -0.0664 0.7744 -0.0507 0.092 Uiso 1 1 calc R . . . . C19 C -0.0805(4) 0.8216(4) 0.0631(3) 0.0669(13) Uani 1 1 d . . . . . H19 H -0.1610 0.8584 0.0680 0.080 Uiso 1 1 calc R . . . . C20 C -0.0208(4) 0.8187(4) 0.1275(3) 0.0630(12) Uani 1 1 d . . . . . H20 H -0.0600 0.8533 0.1761 0.076 Uiso 1 1 calc R . . . . C21 C 0.3115(5) 0.8330(5) 0.4365(3) 0.0949(19) Uani 1 1 d . U . . . C22 C 0.2057(4) 0.9095(3) 0.4517(3) 0.0643(13) Uani 1 1 d . . . . . H22 H 0.1707 0.9454 0.4087 0.077 Uiso 1 1 calc R . . . . C23 C 0.1508(4) 0.9341(3) 0.5280(3) 0.0632(13) Uani 1 1 d . . . . . H23 H 0.0796 0.9885 0.5368 0.076 Uiso 1 1 calc R . . . . C24 C 0.1962(5) 0.8818(4) 0.5918(3) 0.097(2) Uani 1 1 d . U . . . C25 C 0.3066(6) 0.8082(6) 0.5749(4) 0.147(3) Uani 1 1 d . U . . . H25 H 0.3434 0.7725 0.6173 0.176 Uiso 1 1 calc R . . . . C26 C 0.3612(6) 0.7875(6) 0.4990(4) 0.144(3) Uani 1 1 d . U . . . H26 H 0.4368 0.7395 0.4898 0.172 Uiso 1 1 calc R . . . . C27 C 0.5260(5) 0.7224(4) 0.1092(3) 0.0766(15) Uani 1 1 d . . . . . C28 C 0.6111(5) 0.7678(5) 0.0720(4) 0.0869(18) Uani 1 1 d . . . . . H28 H 0.6326 0.8202 0.0996 0.104 Uiso 1 1 calc R . . . . C29 C 0.6663(5) 0.7389(5) -0.0050(4) 0.0909(17) Uani 1 1 d . . . . . H29 H 0.7251 0.7709 -0.0293 0.109 Uiso 1 1 calc R . . . . C30 C 0.6344(5) 0.6617(4) -0.0466(3) 0.0766(15) Uani 1 1 d . . . . . C31 C 0.5487(4) 0.6173(4) -0.0095(3) 0.0742(14) Uani 1 1 d . . . . . H31 H 0.5250 0.5663 -0.0372 0.089 Uiso 1 1 calc R . . . . C32 C 0.4968(4) 0.6457(4) 0.0673(3) 0.0743(15) Uani 1 1 d . . . . . H32 H 0.4397 0.6121 0.0922 0.089 Uiso 1 1 calc R . . . . C33 C 0.1909(7) 0.9140(5) 0.7329(3) 0.097(2) Uani 1 1 d . . . . . C34 C 0.1734(8) 0.8690(4) 0.8057(3) 0.131(3) Uani 1 1 d . . . . . H34 H 0.1211 0.8250 0.8132 0.158 Uiso 1 1 calc R . . . . C35 C 0.2269(8) 0.8838(5) 0.8681(4) 0.125(3) Uani 1 1 d . . . . . H35 H 0.2118 0.8517 0.9179 0.150 Uiso 1 1 calc R . . . . C36 C 0.3024(6) 0.9461(5) 0.8568(3) 0.093(2) Uani 1 1 d . . . . . C37 C 0.3267(5) 0.9938(5) 0.7833(3) 0.098(2) Uani 1 1 d . . . . . H37 H 0.3811 1.0358 0.7756 0.118 Uiso 1 1 calc R . . . . C38 C 0.2682(6) 0.9772(6) 0.7231(3) 0.097(2) Uani 1 1 d . . . . . H38 H 0.2813 1.0100 0.6734 0.116 Uiso 1 1 calc R . . . . C39 C 0.3450(6) 0.9272(5) 0.9916(3) 0.106(2) Uani 1 1 d . . . . . H39A H 0.3682 0.8494 0.9875 0.160 Uiso 1 1 calc GR . . . . H39B H 0.2621 0.9516 1.0137 0.160 Uiso 1 1 calc GR . . . . H39C H 0.3919 0.9505 1.0263 0.160 Uiso 1 1 calc GR . . . . C40 C 0.0140(7) 0.9006(4) 0.6826(3) 0.0915(19) Uani 1 1 d . . . . . C41 C -0.0315(7) 0.8410(4) 0.6342(3) 0.0843(18) Uani 1 1 d . . . . . H41 H 0.0193 0.7988 0.5922 0.101 Uiso 1 1 calc R . . . . C42 C -0.1467(7) 0.8426(4) 0.6462(3) 0.098(2) Uani 1 1 d . . . . . H42 H -0.1780 0.8047 0.6122 0.117 Uiso 1 1 calc R . . . . C43 C -0.2151(8) 0.9009(5) 0.7092(5) 0.135(3) Uani 1 1 d D U . . . C44 C -0.1764(11) 0.9585(5) 0.7565(4) 0.140(4) Uani 1 1 d . . . . . H44 H -0.2288 0.9989 0.7988 0.169 Uiso 1 1 calc R . . . . C45 C -0.0611(9) 0.9602(5) 0.7448(3) 0.116(3) Uani 1 1 d . . . . . H45 H -0.0333 1.0014 0.7786 0.139 Uiso 1 1 calc R . . . . C46 C -0.3702(10) 0.9201(9) 0.8109(6) 0.150(4) Uani 0.75 1 d D U P A 1 H46A H -0.3945 0.9970 0.8209 0.225 Uiso 0.75 1 calc GR . P A 1 H46B H -0.3046 0.8875 0.8393 0.225 Uiso 0.75 1 calc GR . P A 1 H46C H -0.4358 0.8896 0.8295 0.225 Uiso 0.75 1 calc GR . P A 1 C46' C -0.396(3) 0.875(3) 0.6662(17) 0.179(10) Uani 0.25 1 d D U P A 2 H46D H -0.4447 0.9407 0.6477 0.269 Uiso 0.25 1 calc GR . P A 2 H46E H -0.4450 0.8296 0.6899 0.269 Uiso 0.25 1 calc GR . P A 2 H46F H -0.3408 0.8370 0.6212 0.269 Uiso 0.25 1 calc GR . P A 2 C47 C 0.8153(5) 0.6093(4) -0.1407(3) 0.0668(13) Uani 1 1 d . . . . . C48 C 0.8847(4) 0.5404(4) -0.0937(3) 0.0681(13) Uani 1 1 d . . . . . H48 H 0.8487 0.5071 -0.0505 0.082 Uiso 1 1 calc R . . . . C49 C 1.0045(4) 0.5186(4) -0.1076(2) 0.0665(13) Uani 1 1 d . . . . . H49 H 1.0506 0.4711 -0.0745 0.080 Uiso 1 1 calc R . . . . C50 C 1.0576(4) 0.5672(4) -0.1711(3) 0.0625(12) Uani 1 1 d . . . . . C51 C 0.9895(5) 0.6344(4) -0.2191(3) 0.0707(14) Uani 1 1 d . . . . . H51 H 1.0254 0.6652 -0.2638 0.085 Uiso 1 1 calc R . . . . C52 C 0.8714(5) 0.6571(4) -0.2034(3) 0.0750(15) Uani 1 1 d . . . . . H52 H 0.8257 0.7066 -0.2356 0.090 Uiso 1 1 calc R . . . . C53 C 1.2489(5) 0.4747(5) -0.1510(3) 0.105(2) Uani 1 1 d . . . . . H53A H 1.3294 0.4607 -0.1783 0.158 Uiso 1 1 calc GR . . . . H53B H 1.2228 0.4095 -0.1504 0.158 Uiso 1 1 calc GR . . . . H53C H 1.2453 0.4983 -0.0964 0.158 Uiso 1 1 calc GR . . . . C54 C 0.6294(5) 0.6070(4) -0.1833(3) 0.0758(15) Uani 1 1 d . . . . . C55 C 0.6800(6) 0.5261(4) -0.2370(4) 0.102(2) Uani 1 1 d . . . . . H55 H 0.7576 0.4847 -0.2350 0.122 Uiso 1 1 calc R . . . . C56 C 0.6187(7) 0.5041(5) -0.2942(4) 0.114(2) Uani 1 1 d . . . . . H56 H 0.6545 0.4488 -0.3322 0.137 Uiso 1 1 calc R . . . . C57 C 0.5071(7) 0.5621(6) -0.2956(5) 0.110(2) Uani 1 1 d D . . . . C58 C 0.4541(7) 0.6410(7) -0.2436(5) 0.112(2) Uani 1 1 d . . . . . H58 H 0.3753 0.6799 -0.2447 0.134 Uiso 1 1 calc R . . . . C59 C 0.5161(5) 0.6639(5) -0.1892(4) 0.0895(17) Uani 1 1 d . . . . . H59 H 0.4799 0.7218 -0.1535 0.107 Uiso 1 1 calc R . . . . O4 O 0.4231(10) 0.5544(8) -0.3406(6) 0.083(3) Uani 0.5 1 d D . P B 1 C60 C 0.4637(18) 0.4725(13) -0.3985(10) 0.091(6) Uani 0.5 1 d D . P B 1 H60D H 0.4060 0.4790 -0.4347 0.137 Uiso 0.5 1 calc GR . P B 1 H60E H 0.4753 0.4033 -0.3725 0.137 Uiso 0.5 1 calc GR . P B 1 H60F H 0.5380 0.4784 -0.4286 0.137 Uiso 0.5 1 calc GR . P B 1 O4' O 0.4865(12) 0.5176(15) -0.3776(9) 0.111(5) Uani 0.5 1 d D . P B 2 C60' C 0.3623(14) 0.5417(19) -0.3692(19) 0.184(11) Uani 0.5 1 d D . P B 2 H60A H 0.3392 0.5198 -0.4175 0.276 Uiso 0.5 1 calc GR . P B 2 H60B H 0.3291 0.6184 -0.3606 0.276 Uiso 0.5 1 calc GR . P B 2 H60C H 0.3333 0.5034 -0.3237 0.276 Uiso 0.5 1 calc GR . P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.122(3) 0.095(3) 0.055(2) -0.0031(19) -0.032(2) 0.014(2) O2 0.219(6) 0.119(3) 0.148(4) -0.055(3) 0.105(4) -0.078(4) O3 0.088(3) 0.090(3) 0.061(2) -0.0001(18) -0.0148(19) -0.007(2) N1 0.073(3) 0.059(2) 0.056(2) -0.0059(18) -0.024(2) 0.004(2) N2 0.066(3) 0.058(2) 0.054(2) -0.0144(18) -0.012(2) -0.0005(19) N3 0.147(5) 0.078(3) 0.052(3) -0.006(2) -0.051(3) 0.012(3) N4 0.061(3) 0.078(3) 0.077(3) -0.012(2) -0.010(2) 0.002(2) C1 0.071(4) 0.060(3) 0.070(3) -0.017(2) -0.025(3) 0.012(2) C2 0.076(4) 0.092(4) 0.078(4) -0.039(3) -0.038(3) 0.020(3) C3 0.065(4) 0.136(5) 0.105(5) -0.067(4) -0.033(3) 0.030(3) C4 0.057(3) 0.109(5) 0.120(5) -0.065(4) -0.020(3) 0.014(3) C5 0.059(3) 0.077(3) 0.089(4) -0.037(3) -0.013(3) 0.007(3) C6 0.069(3) 0.061(3) 0.064(3) -0.019(2) -0.020(3) 0.001(2) C7 0.069(3) 0.055(3) 0.048(3) 0.001(2) -0.016(3) 0.001(2) C8 0.054(3) 0.052(3) 0.054(3) -0.007(2) -0.010(2) 0.002(2) C9 0.077(3) 0.054(3) 0.045(3) 0.004(2) -0.019(2) -0.006(2) C10 0.087(4) 0.064(3) 0.049(3) -0.003(2) -0.009(3) -0.006(3) C11 0.102(4) 0.066(3) 0.056(3) 0.002(3) 0.008(3) -0.009(3) C12 0.091(4) 0.092(4) 0.062(3) 0.015(3) -0.007(3) -0.020(3) C13 0.100(4) 0.080(4) 0.066(3) -0.001(3) -0.018(3) -0.023(3) C14 0.088(4) 0.076(4) 0.064(3) -0.007(3) -0.008(3) -0.010(3) C15 0.064(3) 0.058(3) 0.049(3) -0.003(2) -0.012(2) -0.005(2) C16 0.067(3) 0.081(3) 0.055(3) -0.010(2) -0.016(2) -0.011(3) C17 0.065(3) 0.096(4) 0.057(3) -0.011(3) -0.009(3) -0.004(3) C18 0.083(4) 0.096(4) 0.053(3) 0.004(3) -0.022(3) -0.021(3) C19 0.067(3) 0.070(3) 0.057(3) -0.003(2) -0.013(2) -0.004(2) C20 0.069(3) 0.066(3) 0.050(3) -0.005(2) -0.012(2) -0.008(2) C21 0.083(4) 0.104(4) 0.077(3) -0.044(3) -0.042(3) 0.032(3) C22 0.076(3) 0.053(3) 0.058(3) -0.006(2) -0.020(2) 0.000(2) C23 0.083(3) 0.050(3) 0.050(3) -0.003(2) -0.029(2) 0.005(2) C24 0.128(4) 0.081(4) 0.060(3) -0.021(3) -0.047(3) 0.033(3) C25 0.167(5) 0.143(5) 0.076(3) -0.041(3) -0.070(4) 0.088(4) C26 0.142(5) 0.154(5) 0.084(4) -0.064(3) -0.069(3) 0.087(4) C27 0.055(3) 0.072(3) 0.094(4) -0.030(3) -0.015(3) 0.004(3) C28 0.058(3) 0.088(4) 0.104(5) -0.043(3) -0.013(3) 0.003(3) C29 0.068(3) 0.088(4) 0.106(5) -0.025(4) 0.001(3) -0.007(3) C30 0.072(3) 0.065(3) 0.080(4) -0.032(3) -0.008(3) 0.005(3) C31 0.066(3) 0.060(3) 0.089(4) -0.018(3) 0.001(3) -0.010(3) C32 0.067(3) 0.063(3) 0.082(4) -0.031(3) -0.001(3) 0.001(2) C33 0.160(6) 0.057(3) 0.057(4) -0.005(3) -0.050(4) 0.017(4) C34 0.275(9) 0.061(3) 0.071(4) 0.013(3) -0.094(5) -0.032(5) C35 0.254(9) 0.058(4) 0.078(4) 0.009(3) -0.071(5) -0.044(5) C36 0.135(5) 0.073(4) 0.043(3) -0.010(3) -0.043(3) 0.038(4) C37 0.118(5) 0.088(4) 0.063(4) -0.010(3) -0.025(3) 0.022(3) C38 0.122(5) 0.091(5) 0.043(3) -0.007(3) -0.023(3) 0.040(4) C39 0.160(6) 0.087(4) 0.062(3) -0.010(3) -0.054(4) 0.007(4) C40 0.145(6) 0.061(3) 0.050(3) 0.014(3) -0.031(4) 0.011(4) C41 0.139(6) 0.055(3) 0.040(3) 0.011(2) -0.015(3) 0.008(3) C42 0.129(6) 0.061(3) 0.079(4) 0.020(3) 0.029(4) -0.009(3) C43 0.191(7) 0.065(4) 0.122(5) -0.016(4) 0.082(5) -0.043(4) C44 0.244(10) 0.047(4) 0.084(5) 0.002(3) 0.063(6) -0.007(5) C45 0.219(9) 0.064(4) 0.041(3) 0.001(3) 0.001(5) -0.008(5) C46 0.155(8) 0.117(7) 0.154(9) -0.022(7) 0.026(7) -0.019(6) C46' 0.189(18) 0.172(18) 0.154(18) -0.054(16) 0.083(16) -0.062(16) C47 0.075(4) 0.060(3) 0.061(3) -0.001(2) -0.014(3) -0.008(3) C48 0.074(3) 0.066(3) 0.051(3) 0.008(2) 0.001(2) -0.001(3) C49 0.079(4) 0.068(3) 0.040(3) 0.009(2) -0.012(2) 0.004(3) C50 0.065(3) 0.062(3) 0.051(3) 0.000(2) -0.004(2) -0.004(2) C51 0.090(4) 0.065(3) 0.048(3) 0.007(2) -0.004(3) -0.008(3) C52 0.091(4) 0.058(3) 0.060(3) 0.005(2) -0.022(3) 0.012(3) C53 0.112(5) 0.103(5) 0.078(4) 0.006(3) -0.008(3) 0.009(4) C54 0.081(4) 0.057(3) 0.085(4) 0.006(3) -0.035(3) 0.002(3) C55 0.127(5) 0.064(4) 0.106(5) -0.013(3) -0.061(4) 0.015(3) C56 0.160(6) 0.063(4) 0.121(5) -0.003(3) -0.076(5) -0.002(4) C57 0.128(6) 0.088(5) 0.133(7) 0.050(5) -0.079(5) -0.031(5) C58 0.103(5) 0.097(5) 0.134(6) 0.046(5) -0.046(5) -0.014(4) C59 0.079(4) 0.074(4) 0.106(5) 0.017(3) -0.020(4) -0.002(3) O4 0.052(6) 0.101(7) 0.077(6) 0.008(5) -0.015(5) 0.016(5) C60 0.110(15) 0.102(12) 0.072(9) 0.005(8) -0.045(9) -0.028(10) O4' 0.089(9) 0.164(15) 0.098(11) 0.023(9) -0.048(8) -0.046(10) C60' 0.116(17) 0.135(17) 0.30(3) 0.081(19) -0.05(2) -0.037(16) 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' 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 C36 O1 C39 116.6(5) C43 O2 C46 105.0(7) C46' O2 C43 125.4(14) C50 O3 C53 116.0(4) C7 N1 C1 120.1(4) C8 N2 C6 119.8(4) C24 N3 C40 118.7(5) C33 N3 C24 120.6(6) C33 N3 C40 120.7(6) C30 N4 C47 118.4(4) C30 N4 C54 121.3(4) C54 N4 C47 119.0(4) N1 C1 C2 120.3(5) N1 C1 C6 118.7(5) C2 C1 C6 120.9(5) C1 C2 C21 119.8(5) C3 C2 C1 117.5(5) C3 C2 C21 122.6(5) C2 C3 H3 119.0 C2 C3 C4 122.0(5) C4 C3 H3 119.0 C3 C4 H4 118.8 C5 C4 C3 122.4(5) C5 C4 H4 118.8 C4 C5 C6 116.9(5) C4 C5 C27 122.2(5) C6 C5 C27 120.9(5) N2 C6 C1 119.3(5) N2 C6 C5 120.8(4) C1 C6 C5 119.8(5) N1 C7 C8 120.2(5) N1 C7 C9 114.5(4) C8 C7 C9 125.3(4) N2 C8 C7 120.2(4) N2 C8 C15 114.3(4) C7 C8 C15 125.5(4) C10 C9 C7 118.1(5) C14 C9 C7 121.6(4) C14 C9 C10 120.1(5) C9 C10 H10 119.9 C11 C10 C9 120.2(5) C11 C10 H10 119.9 C10 C11 H11 120.0 C10 C11 C12 120.0(5) C12 C11 H11 120.0 C11 C12 H12 119.9 C13 C12 C11 120.2(5) C13 C12 H12 119.9 C12 C13 H13 119.9 C12 C13 C14 120.1(6) C14 C13 H13 119.9 C9 C14 C13 119.3(5) C9 C14 H14 120.3 C13 C14 H14 120.3 C16 C15 C8 118.7(4) C16 C15 C20 118.8(4) C20 C15 C8 122.4(4) C15 C16 H16 119.6 C17 C16 C15 120.7(4) C17 C16 H16 119.6 C16 C17 H17 119.7 C18 C17 C16 120.5(5) C18 C17 H17 119.7 C17 C18 H18 120.1 C17 C18 C19 119.8(5) C19 C18 H18 120.1 C18 C19 H19 119.6 C18 C19 C20 120.8(4) C20 C19 H19 119.6 C15 C20 H20 120.4 C19 C20 C15 119.3(4) C19 C20 H20 120.4 C22 C21 C2 119.9(5) C26 C21 C2 122.2(5) C26 C21 C22 117.8(5) C21 C22 H22 119.5 C23 C22 C21 120.9(4) C23 C22 H22 119.5 C22 C23 H23 119.2 C24 C23 C22 121.6(4) C24 C23 H23 119.2 C23 C24 N3 121.6(5) C23 C24 C25 116.1(5) C25 C24 N3 122.2(5) C24 C25 H25 119.4 C26 C25 C24 121.2(5) C26 C25 H25 119.4 C21 C26 C25 122.0(5) C21 C26 H26 119.0 C25 C26 H26 119.0 C28 C27 C5 120.8(5) C28 C27 C32 117.8(5) C32 C27 C5 121.3(6) C27 C28 H28 119.2 C27 C28 C29 121.6(5) C29 C28 H28 119.2 C28 C29 H29 120.2 C28 C29 C30 119.6(6) C30 C29 H29 120.2 C29 C30 N4 119.2(6) C31 C30 N4 122.3(5) C31 C30 C29 118.5(5) C30 C31 H31 119.6 C30 C31 C32 120.9(5) C32 C31 H31 119.6 C27 C32 H32 119.2 C31 C32 C27 121.5(5) C31 C32 H32 119.2 C34 C33 N3 123.3(8) C34 C33 C38 117.2(6) C38 C33 N3 119.5(6) C33 C34 H34 118.2 C35 C34 C33 123.7(8) C35 C34 H34 118.2 C34 C35 H35 121.1 C36 C35 C34 117.9(7) C36 C35 H35 121.1 O1 C36 C37 111.9(7) C35 C36 O1 126.1(6) C35 C36 C37 121.9(6) C36 C37 H37 121.4 C38 C37 C36 117.3(7) C38 C37 H37 121.4 C33 C38 H38 119.0 C37 C38 C33 122.0(6) C37 C38 H38 119.0 O1 C39 H39A 109.5 O1 C39 H39B 109.5 O1 C39 H39C 109.5 H39A C39 H39B 109.5 H39A C39 H39C 109.5 H39B C39 H39C 109.5 C41 C40 N3 121.5(6) C45 C40 N3 120.1(7) C45 C40 C41 118.4(8) C40 C41 H41 119.3 C42 C41 C40 121.5(6) C42 C41 H41 119.3 C41 C42 H42 121.5 C43 C42 C41 117.1(8) C43 C42 H42 121.5 C42 C43 O2 116.8(8) C44 C43 O2 119.6(8) C44 C43 C42 123.7(9) C43 C44 H44 119.8 C43 C44 C45 120.5(7) C45 C44 H44 119.8 C40 C45 H45 120.6 C44 C45 C40 118.8(8) C44 C45 H45 120.6 O2 C46 H46A 109.5 O2 C46 H46B 109.5 O2 C46 H46C 109.5 H46A C46 H46B 109.5 H46A C46 H46C 109.5 H46B C46 H46C 109.5 O2 C46' H46D 109.5 O2 C46' H46E 109.5 O2 C46' H46F 109.5 H46D C46' H46E 109.5 H46D C46' H46F 109.5 H46E C46' H46F 109.5 C48 C47 N4 121.6(5) C48 C47 C52 117.5(5) C52 C47 N4 120.8(5) C47 C48 H48 119.1 C49 C48 C47 121.7(5) C49 C48 H48 119.1 C48 C49 H49 120.4 C48 C49 C50 119.2(4) C50 C49 H49 120.4 O3 C50 C49 126.0(4) O3 C50 C51 114.5(4) C51 C50 C49 119.5(5) C50 C51 H51 119.7 C52 C51 C50 120.5(5) C52 C51 H51 119.7 C47 C52 H52 119.3 C51 C52 C47 121.4(5) C51 C52 H52 119.3 O3 C53 H53A 109.5 O3 C53 H53B 109.5 O3 C53 H53C 109.5 H53A C53 H53B 109.5 H53A C53 H53C 109.5 H53B C53 H53C 109.5 C55 C54 N4 121.9(5) C55 C54 C59 116.9(6) C59 C54 N4 121.2(5) C54 C55 H55 119.8 C54 C55 C56 120.4(6) C56 C55 H55 119.8 C55 C56 H56 120.3 C57 C56 C55 119.4(7) C57 C56 H56 120.3 C56 C57 O4 132.6(9) C56 C57 O4' 98.8(9) C58 C57 C56 122.0(7) C58 C57 O4 105.3(8) C58 C57 O4' 138.4(9) C57 C58 H58 121.0 C57 C58 C59 118.1(7) C59 C58 H58 121.0 C54 C59 H59 118.4 C58 C59 C54 123.2(6) C58 C59 H59 118.4 C57 O4 C60 113.1(13) O4 C60 H60D 109.5 O4 C60 H60E 109.5 O4 C60 H60F 109.5 H60D C60 H60E 109.5 H60D C60 H60F 109.5 H60E C60 H60F 109.5 C60' O4' C57 102(2) O4' C60' H60A 109.5 O4' C60' H60B 109.5 O4' C60' H60C 109.5 H60A C60' H60B 109.5 H60A C60' H60C 109.5 H60B C60' H60C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C36 1.400(7) O1 C39 1.444(6) O2 C43 1.406(8) O2 C46 1.508(9) O2 C46' 1.403(19) O3 C50 1.369(5) O3 C53 1.418(6) N1 C1 1.363(6) N1 C7 1.316(5) N2 C6 1.358(5) N2 C8 1.319(5) N3 C24 1.413(7) N3 C33 1.399(7) N3 C40 1.426(8) N4 C30 1.416(6) N4 C47 1.432(6) N4 C54 1.417(6) C1 C2 1.406(6) C1 C6 1.419(6) C2 C3 1.364(8) C2 C21 1.502(7) C3 H3 0.9500 C3 C4 1.389(8) C4 H4 0.9500 C4 C5 1.380(7) C5 C6 1.422(7) C5 C27 1.479(7) C7 C8 1.419(6) C7 C9 1.497(7) C8 C15 1.502(6) C9 C10 1.396(6) C9 C14 1.387(7) C10 H10 0.9500 C10 C11 1.359(7) C11 H11 0.9500 C11 C12 1.396(8) C12 H12 0.9500 C12 C13 1.375(7) C13 H13 0.9500 C13 C14 1.390(7) C14 H14 0.9500 C15 C16 1.392(6) C15 C20 1.397(6) C16 H16 0.9500 C16 C17 1.371(6) C17 H17 0.9500 C17 C18 1.369(6) C18 H18 0.9500 C18 C19 1.371(6) C19 H19 0.9500 C19 C20 1.393(6) C20 H20 0.9500 C21 C22 1.385(6) C21 C26 1.346(7) C22 H22 0.9500 C22 C23 1.373(6) C23 H23 0.9500 C23 C24 1.373(6) C24 C25 1.410(8) C25 H25 0.9500 C25 C26 1.359(8) C26 H26 0.9500 C27 C28 1.379(8) C27 C32 1.390(7) C28 H28 0.9500 C28 C29 1.393(7) C29 H29 0.9500 C29 C30 1.410(7) C30 C31 1.376(7) C31 H31 0.9500 C31 C32 1.379(7) C32 H32 0.9500 C33 C34 1.368(8) C33 C38 1.385(9) C34 H34 0.9500 C34 C35 1.366(8) C35 H35 0.9500 C35 C36 1.359(10) C36 C37 1.408(8) C37 H37 0.9500 C37 C38 1.380(8) C38 H38 0.9500 C39 H39A 0.9800 C39 H39B 0.9800 C39 H39C 0.9800 C40 C41 1.406(8) C40 C45 1.389(9) C41 H41 0.9500 C41 C42 1.362(8) C42 H42 0.9500 C42 C43 1.362(9) C43 C44 1.327(11) C44 H44 0.9500 C44 C45 1.373(11) C45 H45 0.9500 C46 H46A 0.9800 C46 H46B 0.9800 C46 H46C 0.9800 C46' H46D 0.9800 C46' H46E 0.9800 C46' H46F 0.9800 C47 C48 1.381(6) C47 C52 1.397(7) C48 H48 0.9500 C48 C49 1.375(6) C49 H49 0.9500 C49 C50 1.395(6) C50 C51 1.375(6) C51 H51 0.9500 C51 C52 1.355(7) C52 H52 0.9500 C53 H53A 0.9800 C53 H53B 0.9800 C53 H53C 0.9800 C54 C55 1.368(7) C54 C59 1.383(7) C55 H55 0.9500 C55 C56 1.385(8) C56 H56 0.9500 C56 C57 1.356(9) C57 C58 1.335(10) C57 O4 1.380(10) C57 O4' 1.606(18) C58 H58 0.9500 C58 C59 1.357(9) C59 H59 0.9500 O4 C60 1.411(14) C60 H60D 0.9800 C60 H60E 0.9800 C60 H60F 0.9800 O4' C60' 1.425(15) C60' H60A 0.9800 C60' H60B 0.9800 C60' H60C 0.9800