#------------------------------------------------------------------------------ #$Date: 2020-08-06 16:32:11 +0300 (Thu, 06 Aug 2020) $ #$Revision: 254937 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/77/1557764.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_1557764 loop_ _publ_author_name 'Dong, Zhaowen' 'Pezzato, Cristian' 'Sienkiewicz, Andrzej' 'Scopelliti, Rosario' 'Fadaei-Tirani, Farzaneh' 'Severin, Kay' _publ_section_title ; SET processes in Lewis acid--base reactions: the tritylation of N-heterocyclic carbenes ; _journal_issue 29 _journal_name_full 'Chemical Science' _journal_page_first 7615 _journal_paper_doi 10.1039/D0SC01278E _journal_volume 11 _journal_year 2020 _chemical_formula_moiety 'B C24 F20, C40 H39 N2, 0.5[C7H8]' _chemical_formula_sum 'C64 H39 B F20 N2' _chemical_formula_weight 1226.78 _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_date 2020-01-17 _audit_creation_method ; Olex2 1.3-alpha (compiled 2019.10.11 svn.r3662 for OlexSys, GUI svn.r5962) ; _audit_update_record ; 2020-01-28 deposited with the CCDC. 2020-04-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 18.0482(3) _cell_length_b 18.05071(19) _cell_length_c 34.8012(5) _cell_measurement_reflns_used 41391 _cell_measurement_temperature 140.00(10) _cell_measurement_theta_max 75.8550 _cell_measurement_theta_min 3.6070 _cell_volume 11337.6(3) _computing_cell_refinement 'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)' _computing_molecular_graphics 'Olex2 1.3-alpha (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-alpha (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 140.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2817 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -76.00 10.00 1.00 2.35 -- -40.91 101.00 -97.00 86 2 \w 9.00 36.00 1.00 2.35 -- 40.91-101.00 158.00 27 3 \w 81.00 107.00 1.00 9.37 -- 112.00-101.00 158.00 26 4 \w 119.00 145.00 1.00 9.37 -- 112.00 101.00 -97.00 26 5 \w -58.00 32.00 1.00 2.35 -- -40.91 38.00 -90.00 90 6 \w -112.00 -14.00 1.00 2.35 -- -40.91 -57.00 120.00 98 7 \w 42.00 96.00 1.00 2.35 -- 40.91-125.00 90.00 54 8 \w 62.00 115.00 1.00 2.35 -- 40.91 38.00 60.00 53 9 \w -6.00 64.00 1.00 2.35 -- 40.91 -38.00 -60.00 70 10 \w 137.00 177.00 1.00 9.37 -- 112.00 30.00 60.00 40 11 \w 37.00 63.00 1.00 9.37 -- 112.00-111.00 -60.00 26 12 \w 87.00 126.00 1.00 9.37 -- 112.00 -30.00 120.00 39 13 \w 36.00 109.00 1.00 9.37 -- 112.00-111.00-120.00 73 14 \w 45.00 72.00 1.00 9.37 -- 112.00 -61.00-150.00 27 15 \w 37.00 109.00 1.00 9.37 -- 112.00-111.00 30.00 72 16 \w 85.00 123.00 1.00 9.37 -- 112.00 30.00 60.00 38 17 \w 37.00 109.00 1.00 9.37 -- 112.00-111.00 -90.00 72 18 \w 36.00 62.00 1.00 9.37 -- 112.00-111.00 150.00 26 19 \w 98.00 140.00 1.00 9.37 -- 112.00 -30.00-150.00 42 20 \w 46.00 72.00 1.00 9.37 -- 112.00 -94.00-180.00 26 21 \w 124.00 150.00 1.00 9.37 -- 112.00 45.00-180.00 26 22 \w 152.00 177.00 1.00 9.37 -- 112.00 111.00 -60.00 25 23 \w 65.00 91.00 1.00 9.37 -- 112.00-111.00 0.00 26 24 \w 75.00 140.00 1.00 9.37 -- 112.00 -61.00-150.00 65 25 \w 85.00 136.00 1.00 9.37 -- 112.00 30.00 120.00 51 26 \w 141.00 168.00 1.00 9.37 -- 112.00 30.00 120.00 27 27 \w 36.00 109.00 1.00 9.37 -- 112.00-111.00 90.00 73 28 \w 36.00 109.00 1.00 9.37 -- 112.00-111.00 -30.00 73 29 \w 24.00 160.00 1.00 9.37 -- 112.00 0.00-120.00 136 30 \w 54.00 97.00 1.00 9.37 -- 112.00-111.00 120.00 43 31 \w 77.00 109.00 1.00 9.37 -- 112.00-111.00 150.00 32 32 \w 71.00 103.00 1.00 9.37 -- 112.00 178.00-180.00 32 33 \w 70.00 98.00 1.00 9.37 -- 112.00-111.00 60.00 28 34 \w 40.00 121.00 1.00 9.37 -- 112.00 -61.00 90.00 81 35 \w 38.00 81.00 1.00 9.37 -- 112.00 -30.00-150.00 43 36 \w 58.00 135.00 1.00 9.37 -- 112.00 -45.00 -60.00 77 37 \w 82.00 113.00 1.00 9.37 -- 112.00 178.00-120.00 31 38 \w 48.00 93.00 1.00 9.37 -- 112.00 -94.00 -90.00 45 39 \w 39.00 77.00 1.00 9.37 -- 112.00 -30.00 120.00 38 40 \w 98.00 123.00 1.00 9.37 -- 112.00 -61.00 -60.00 25 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0379433000 _diffrn_orient_matrix_UB_12 0.0324165000 _diffrn_orient_matrix_UB_13 0.0359227000 _diffrn_orient_matrix_UB_21 -0.0747451000 _diffrn_orient_matrix_UB_22 -0.0005879000 _diffrn_orient_matrix_UB_23 0.0213902000 _diffrn_orient_matrix_UB_31 0.0160676000 _diffrn_orient_matrix_UB_32 -0.0789229000 _diffrn_orient_matrix_UB_33 0.0145970000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_unetI/netI 0.0194 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_number 127435 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.243 _diffrn_reflns_theta_min 3.528 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 1.138 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.375 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020). Numerical absorption correction based on Gaussian integration over a multifaceted crystal model. Empirical absorption correction using spherical harmonics as implemented in SCALE3 ABSPACK scaling algorithm ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.437 _exptl_crystal_description prism _exptl_crystal_F_000 4976 _exptl_crystal_size_max 0.585 _exptl_crystal_size_mid 0.297 _exptl_crystal_size_min 0.094 _refine_diff_density_max 0.277 _refine_diff_density_min -0.202 _refine_diff_density_rms 0.042 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 790 _refine_ls_number_reflns 11828 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0402 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+3.6391P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1068 _refine_ls_wR_factor_ref 0.1109 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10432 _reflns_number_total 11828 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc01278e2.cif _cod_data_source_block dzw-129a _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Gaussian' was changed to 'gaussian' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas Adding full bibliography for 1557761--1557764.cif. ; _cod_database_code 1557764 _shelx_shelxl_version_number 2018/3 _audit_contact_author 'Farzaneh Fadaei Tirani' _chemical_oxdiff_formula 'C64 H39 B F20 N2' _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 0.901 _shelx_estimated_absorpt_t_min 0.556 _reflns_odcompleteness_completeness 99.93 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 74.33 _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.a Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C6(H6), C8(H8), C15(H15), C17(H17), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40) 2.b Idealised Me refined as rotating group: C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C19(H19A,H19B, H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL DZW-129a.res in Pbca dzw-129a.res created by SHELXL-2018/3 at 14:49:45 on 17-Jan-2020 CELL 1.54184 18.048196 18.050715 34.801159 90 90 90 ZERR 8 0.000267 0.000194 0.000486 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H B F N UNIT 512 312 8 160 16 L.S. 20 PLAN 5 SIZE 0.585 0.297 0.094 TEMP -133.15 CONF BOND $H fmap 2 acta MORE -1 ABIN REM REM REM WGHT 0.056800 3.639100 FVAR 0.18876 F1 4 0.541815 0.710424 0.585492 11.00000 0.03857 0.04916 = 0.05361 -0.00014 -0.00864 0.00601 F2 4 0.447954 0.809260 0.613317 11.00000 0.03856 0.05661 = 0.11489 -0.00710 -0.01516 0.01685 F3 4 0.471532 0.873025 0.683434 11.00000 0.04256 0.04046 = 0.11640 -0.01680 0.02299 0.00945 F4 4 0.589550 0.829401 0.726482 11.00000 0.06212 0.04149 = 0.05792 -0.01531 0.02320 -0.00330 F5 4 0.682480 0.726828 0.700312 11.00000 0.04318 0.04087 = 0.03679 -0.00345 0.00363 0.00283 F6 4 0.686616 0.778812 0.572360 11.00000 0.04271 0.04171 = 0.04219 0.01013 -0.00540 -0.00234 F7 4 0.775927 0.896421 0.571057 11.00000 0.06404 0.04002 = 0.06960 0.02063 -0.00358 -0.01003 F8 4 0.889414 0.908094 0.622459 11.00000 0.05209 0.04103 = 0.08092 0.00200 0.00230 -0.01768 F9 4 0.913513 0.796292 0.673637 11.00000 0.03859 0.05638 = 0.05895 -0.00273 -0.00859 -0.00990 F10 4 0.828716 0.676944 0.673912 11.00000 0.03599 0.04189 = 0.03932 0.00551 -0.00344 0.00002 F11 4 0.811996 0.561778 0.618463 11.00000 0.03563 0.04241 = 0.04990 0.00528 0.01468 0.00817 F12 4 0.844651 0.440358 0.658229 11.00000 0.04684 0.04646 = 0.07691 0.01039 0.00622 0.01951 F13 4 0.754655 0.395307 0.717025 11.00000 0.06089 0.04331 = 0.06754 0.02266 -0.00758 0.00512 F14 4 0.632357 0.476365 0.734704 11.00000 0.05172 0.05379 = 0.04445 0.01637 0.00662 -0.00699 F15 4 0.596885 0.595301 0.694531 11.00000 0.03690 0.03962 = 0.04426 0.00420 0.01462 0.00206 F16 4 0.558611 0.565861 0.610132 11.00000 0.03371 0.04233 = 0.04620 -0.00053 0.01062 -0.00556 F17 4 0.532191 0.483271 0.548279 11.00000 0.05152 0.04969 = 0.05706 -0.00420 -0.00232 -0.01945 F18 4 0.631910 0.480464 0.488781 11.00000 0.07506 0.04494 = 0.03932 -0.00898 -0.00201 -0.00902 F19 4 0.756002 0.564966 0.493170 11.00000 0.05270 0.04942 = 0.03240 -0.00059 0.01071 0.00435 F20 4 0.780620 0.652407 0.552516 11.00000 0.03223 0.04579 = 0.03798 -0.00113 0.00876 -0.00499 C41 1 0.617065 0.711016 0.641839 11.00000 0.02911 0.02852 = 0.04045 0.00155 0.00840 0.00050 C42 1 0.555831 0.735632 0.621354 11.00000 0.03228 0.03545 = 0.05050 -0.00029 0.00199 0.00021 C43 1 0.506418 0.788216 0.634888 11.00000 0.02916 0.03875 = 0.07898 0.00108 0.00024 0.00489 C44 1 0.517628 0.820204 0.670211 11.00000 0.03419 0.03051 = 0.08126 -0.00705 0.01898 0.00247 C45 1 0.577518 0.798262 0.691905 11.00000 0.04252 0.03103 = 0.05243 -0.00629 0.01863 -0.00370 C46 1 0.624761 0.744929 0.677613 11.00000 0.03396 0.03176 = 0.04178 0.00119 0.00976 -0.00049 C47 1 0.752298 0.720970 0.623155 11.00000 0.02886 0.03155 = 0.03244 -0.00095 0.00702 0.00098 C48 1 0.743570 0.780149 0.597726 11.00000 0.03324 0.03491 = 0.03632 0.00172 0.00218 0.00078 C49 1 0.788206 0.841701 0.596492 11.00000 0.04394 0.03288 = 0.04650 0.00621 0.00586 -0.00132 C50 1 0.845901 0.847726 0.622305 11.00000 0.03891 0.03282 = 0.05458 -0.00200 0.00803 -0.00712 C51 1 0.857776 0.791156 0.647983 11.00000 0.03087 0.04113 = 0.04389 -0.00519 0.00231 -0.00159 C52 1 0.812051 0.729480 0.647716 11.00000 0.03075 0.03354 = 0.03467 0.00132 0.00528 0.00263 C53 1 0.704132 0.587323 0.654761 11.00000 0.02942 0.03059 = 0.03260 0.00012 0.00240 -0.00106 C54 1 0.765645 0.543003 0.647329 11.00000 0.03230 0.03566 = 0.03789 0.00075 0.00412 0.00136 C55 1 0.783826 0.479779 0.667347 11.00000 0.03540 0.03465 = 0.05190 0.00109 -0.00074 0.00707 C56 1 0.738707 0.456833 0.697045 11.00000 0.04414 0.03266 = 0.04703 0.00881 -0.00756 -0.00053 C57 1 0.676633 0.497771 0.705663 11.00000 0.03933 0.03828 = 0.03523 0.00591 0.00051 -0.00796 C58 1 0.660366 0.560779 0.684515 11.00000 0.03130 0.03297 = 0.03472 -0.00114 0.00230 -0.00113 C59 1 0.669493 0.615918 0.584721 11.00000 0.02995 0.02920 = 0.03338 0.00220 0.00238 0.00271 C60 1 0.608100 0.569492 0.581007 11.00000 0.03162 0.03404 = 0.03620 0.00250 0.00425 0.00101 C61 1 0.593544 0.525429 0.549608 11.00000 0.03935 0.03344 = 0.04494 0.00249 -0.00178 -0.00416 C62 1 0.643186 0.524147 0.519598 11.00000 0.05168 0.03354 = 0.03305 -0.00223 -0.00390 -0.00033 C63 1 0.705723 0.567385 0.521821 11.00000 0.04295 0.03554 = 0.03008 0.00256 0.00556 0.00594 C64 1 0.717308 0.612223 0.553548 11.00000 0.03030 0.03203 = 0.03446 0.00340 0.00140 0.00052 B1 3 0.685778 0.657989 0.626040 11.00000 0.02620 0.03057 = 0.03167 0.00132 0.00476 0.00112 N1 5 0.785681 0.437302 0.382931 11.00000 0.03013 0.02722 = 0.03377 -0.00519 0.00182 0.00039 N2 5 0.871274 0.381142 0.416007 11.00000 0.03300 0.03250 = 0.03336 -0.00677 -0.00392 -0.00087 C1 1 0.829099 0.376297 0.383364 11.00000 0.02458 0.02629 = 0.03062 -0.00161 0.00142 -0.00374 C2 1 0.801353 0.480438 0.414670 11.00000 0.04885 0.03308 = 0.04479 -0.01422 -0.00273 0.00509 AFIX 43 H2 2 0.778658 0.526321 0.421016 11.00000 -1.20000 AFIX 0 C3 1 0.854293 0.446025 0.434924 11.00000 0.04923 0.03792 = 0.04262 -0.01543 -0.00843 0.00235 AFIX 43 H3 2 0.876140 0.463225 0.458102 11.00000 -1.20000 AFIX 0 C4 1 0.725284 0.460735 0.357732 11.00000 0.02815 0.02619 = 0.03301 -0.00255 0.00400 0.00395 C5 1 0.737688 0.519750 0.332537 11.00000 0.03205 0.02397 = 0.03946 -0.00313 0.00850 -0.00002 C6 1 0.677941 0.545524 0.311358 11.00000 0.04133 0.02653 = 0.03627 0.00300 0.00723 0.00246 AFIX 43 H6 2 0.685308 0.585260 0.293871 11.00000 -1.20000 AFIX 0 C7 1 0.607473 0.514914 0.314952 11.00000 0.03631 0.03282 = 0.03584 -0.00138 0.00142 0.00270 C8 1 0.597460 0.457353 0.340815 11.00000 0.02917 0.03377 = 0.03932 -0.00058 0.00534 0.00012 AFIX 43 H8 2 0.549685 0.435764 0.343244 11.00000 -1.20000 AFIX 0 C9 1 0.655100 0.430149 0.363340 11.00000 0.03063 0.02884 = 0.03245 -0.00083 0.00776 0.00112 C10 1 0.812438 0.555511 0.327867 11.00000 0.03515 0.02776 = 0.06254 0.00324 0.01109 -0.00238 AFIX 137 H10A 2 0.847529 0.519294 0.317431 11.00000 -1.50000 H10B 2 0.830107 0.572923 0.352917 11.00000 -1.50000 H10C 2 0.808373 0.597613 0.310213 11.00000 -1.50000 AFIX 0 C11 1 0.543012 0.546092 0.292809 11.00000 0.04768 0.04341 = 0.05242 0.00537 -0.01105 0.00337 AFIX 137 H11A 2 0.529428 0.594489 0.303450 11.00000 -1.50000 H11B 2 0.500698 0.512286 0.294805 11.00000 -1.50000 H11C 2 0.556926 0.551808 0.265752 11.00000 -1.50000 AFIX 0 C12 1 0.639663 0.371353 0.393053 11.00000 0.03419 0.04027 = 0.04407 0.01062 0.00949 0.00058 AFIX 137 H12A 2 0.650981 0.322470 0.382297 11.00000 -1.50000 H12B 2 0.587307 0.373283 0.400451 11.00000 -1.50000 H12C 2 0.670667 0.380089 0.415722 11.00000 -1.50000 AFIX 0 C13 1 0.916504 0.326805 0.436935 11.00000 0.03334 0.03400 = 0.03269 -0.00640 -0.00793 -0.00032 C14 1 0.992582 0.319723 0.429923 11.00000 0.03211 0.04175 = 0.04027 -0.00782 -0.00785 -0.00394 C15 1 1.031391 0.269742 0.452832 11.00000 0.03303 0.04537 = 0.04731 -0.00959 -0.00877 0.00296 AFIX 43 H15 2 1.082789 0.262894 0.448138 11.00000 -1.20000 AFIX 0 C16 1 0.998583 0.229657 0.482072 11.00000 0.04466 0.03931 = 0.04287 -0.00787 -0.01068 0.00439 C17 1 0.923703 0.241180 0.489480 11.00000 0.04570 0.04311 = 0.03529 -0.00229 -0.00523 0.00127 AFIX 43 H17 2 0.900716 0.214906 0.509909 11.00000 -1.20000 AFIX 0 C18 1 0.881554 0.290445 0.467599 11.00000 0.03722 0.04009 = 0.03214 -0.00651 -0.00517 0.00060 C19 1 1.034692 0.363305 0.400613 11.00000 0.02944 0.06838 = 0.05870 0.00824 -0.00767 -0.00813 AFIX 137 H19A 2 1.087302 0.364267 0.407564 11.00000 -1.50000 H19B 2 1.015509 0.414068 0.399745 11.00000 -1.50000 H19C 2 1.028856 0.340137 0.375327 11.00000 -1.50000 AFIX 0 C20 1 1.043722 0.176471 0.506052 11.00000 0.05921 0.05427 = 0.05905 0.00229 -0.00769 0.01779 AFIX 137 H20A 2 1.058391 0.200704 0.530076 11.00000 -1.50000 H20B 2 1.088122 0.161718 0.491761 11.00000 -1.50000 H20C 2 1.013938 0.132487 0.511876 11.00000 -1.50000 AFIX 0 C21 1 0.802049 0.304410 0.478919 11.00000 0.04056 0.05879 = 0.03362 -0.00228 0.00075 0.00425 AFIX 137 H21A 2 0.780665 0.258932 0.489577 11.00000 -1.50000 H21B 2 0.773674 0.319596 0.456239 11.00000 -1.50000 H21C 2 0.800183 0.343767 0.498292 11.00000 -1.50000 AFIX 0 C22 1 0.839908 0.318586 0.351324 11.00000 0.02522 0.02524 = 0.02787 -0.00254 0.00026 -0.00047 C23 1 0.773916 0.313439 0.322050 11.00000 0.02404 0.02679 = 0.02831 -0.00267 0.00107 0.00140 C24 1 0.724149 0.254680 0.321411 11.00000 0.03200 0.02976 = 0.03760 0.00482 -0.00461 -0.00288 AFIX 43 H24 2 0.726099 0.218262 0.341092 11.00000 -1.20000 AFIX 0 C25 1 0.671597 0.248416 0.292420 11.00000 0.03143 0.03339 = 0.04942 0.00388 -0.00892 -0.00548 AFIX 43 H25 2 0.637786 0.208084 0.292730 11.00000 -1.20000 AFIX 0 C26 1 0.667799 0.299780 0.263256 11.00000 0.02915 0.04005 = 0.03889 0.00150 -0.00682 0.00162 AFIX 43 H26 2 0.632299 0.294653 0.243277 11.00000 -1.20000 AFIX 0 C27 1 0.716487 0.359010 0.263483 11.00000 0.03103 0.03456 = 0.03319 0.00515 0.00045 0.00252 AFIX 43 H27 2 0.713786 0.395465 0.243844 11.00000 -1.20000 AFIX 0 C28 1 0.769087 0.365301 0.292225 11.00000 0.02788 0.02681 = 0.03227 -0.00071 0.00352 -0.00025 AFIX 43 H28 2 0.802729 0.405766 0.291715 11.00000 -1.20000 AFIX 0 C29 1 0.906433 0.343296 0.326344 11.00000 0.02365 0.02919 = 0.03061 0.00013 -0.00008 0.00243 C30 1 0.940572 0.411675 0.330325 11.00000 0.02924 0.02865 = 0.04087 -0.00088 0.00446 0.00195 AFIX 43 H30 2 0.926763 0.443135 0.351004 11.00000 -1.20000 AFIX 0 C31 1 0.994863 0.435093 0.304488 11.00000 0.03316 0.03206 = 0.05496 0.00648 0.00898 0.00000 AFIX 43 H31 2 1.017709 0.482108 0.307671 11.00000 -1.20000 AFIX 0 C32 1 1.015281 0.390075 0.274411 11.00000 0.03112 0.04554 = 0.04712 0.00994 0.01182 0.00592 AFIX 43 H32 2 1.052432 0.405705 0.256855 11.00000 -1.20000 AFIX 0 C33 1 0.981296 0.321719 0.269872 11.00000 0.03190 0.04776 = 0.03554 -0.00289 0.00535 0.00701 AFIX 43 H33 2 0.995447 0.290519 0.249149 11.00000 -1.20000 AFIX 0 C34 1 0.927007 0.298518 0.295214 11.00000 0.02710 0.03546 = 0.03453 -0.00413 -0.00018 0.00254 AFIX 43 H34 2 0.903526 0.251963 0.291499 11.00000 -1.20000 AFIX 0 C35 1 0.852002 0.243741 0.371931 11.00000 0.03313 0.02400 = 0.02904 -0.00272 -0.00684 -0.00288 C36 1 0.915879 0.201577 0.368188 11.00000 0.03694 0.02868 = 0.04070 -0.00335 -0.00958 0.00050 AFIX 43 H36 2 0.954380 0.217458 0.351495 11.00000 -1.20000 AFIX 0 C37 1 0.923613 0.135814 0.388941 11.00000 0.05051 0.03137 = 0.05276 -0.00325 -0.02117 0.00502 AFIX 43 H37 2 0.967457 0.107213 0.386098 11.00000 -1.20000 AFIX 0 C38 1 0.868845 0.111733 0.413428 11.00000 0.07228 0.02754 = 0.04243 0.00411 -0.02151 -0.00639 AFIX 43 H38 2 0.874642 0.066825 0.427341 11.00000 -1.20000 AFIX 0 C39 1 0.805354 0.153640 0.417530 11.00000 0.06404 0.03216 = 0.03294 0.00253 -0.00557 -0.01185 AFIX 43 H39 2 0.767332 0.137785 0.434522 11.00000 -1.20000 AFIX 0 C40 1 0.796961 0.218782 0.396918 11.00000 0.04268 0.03095 = 0.02936 -0.00076 -0.00253 -0.00477 AFIX 43 H40 2 0.752882 0.246983 0.399859 11.00000 -1.20000 AFIX 0 HKLF 4 REM DZW-129a.res in Pbca REM wR2 = 0.1109, GooF = S = 1.046, Restrained GooF = 1.046 for all data REM R1 = 0.0402 for 10432 Fo > 4sig(Fo) and 0.0453 for all 11828 data REM 790 parameters refined using 0 restraints END WGHT 0.0568 3.6397 REM Highest difference peak 0.277, deepest hole -0.202, 1-sigma level 0.042 Q1 1 0.8450 0.2822 0.3622 11.00000 0.05 0.28 Q2 1 0.6957 0.6234 0.6421 11.00000 0.05 0.25 Q3 1 0.6426 0.6763 0.6364 11.00000 0.05 0.24 Q4 1 0.8599 0.8080 0.6264 11.00000 0.05 0.22 Q5 1 0.7239 0.6876 0.6230 11.00000 0.05 0.22 ; _shelx_res_checksum 61875 _shelx_fab_file ; 0 0 4 122.7825 0.1960 0 0 6 33.2582 0.1209 0 0 8 -25.5071 -0.0182 0 0 10 -46.5274 -0.1178 0 0 12 -43.4885 -0.1527 0 0 14 -33.0145 -0.1879 0 0 16 -23.0999 -0.2259 0 0 18 -13.9259 -0.1783 0 0 20 -4.6615 -0.0606 0 0 22 3.2762 -0.0135 0 0 24 7.7165 -0.0552 0 0 26 7.9022 -0.0401 0 0 28 5.2590 0.0792 0 0 30 2.2065 0.1712 0 0 32 -0.0319 0.1447 0 0 34 -1.7724 0.0622 0 0 36 -3.2440 0.0110 0 0 38 -3.9046 -0.0039 0 0 40 -3.3106 -0.0123 0 0 42 -1.8404 -0.0156 0 2 0 146.0194 -0.1468 0 2 1 -34.1080 0.0769 0 2 2 125.4686 -0.1722 0 2 3 -84.7243 -0.0091 0 2 4 76.2663 -0.2402 0 2 5 -96.1531 -0.1088 0 2 6 24.8706 -0.2251 0 2 7 -73.8426 -0.1439 0 2 8 -8.5532 -0.1466 0 2 9 -39.4323 -0.1315 0 2 10 -20.3850 -0.0706 0 2 11 -11.4980 -0.1018 0 2 12 -19.3274 -0.0253 0 2 13 3.8703 -0.0334 0 2 14 -15.5084 -0.0511 0 2 15 9.9834 0.0662 0 2 16 -12.7872 -0.1428 0 2 17 11.9774 0.1350 0 2 18 -9.7432 -0.1971 0 2 19 12.2212 0.1147 0 2 20 -5.1605 -0.1594 0 2 21 10.5513 0.0181 0 2 22 -0.2035 -0.1018 0 2 23 6.7836 -0.0440 0 2 24 3.1886 -0.0733 0 2 25 2.2614 0.0032 0 2 26 3.8999 -0.0233 0 2 27 -1.0182 0.0747 0 2 28 2.3720 0.0724 0 2 29 -2.3838 0.0867 0 2 30 0.3085 0.1373 0 2 31 -2.7492 0.0906 0 2 32 -0.9737 0.1056 0 2 33 -2.8970 0.1055 0 2 34 -1.5163 0.0308 0 2 35 -2.6219 0.0650 0 2 36 -1.8038 0.0091 0 2 37 -1.6602 -0.0010 0 2 38 -1.8470 0.0399 0 2 39 -0.3740 -0.0035 0 2 40 -1.4358 0.0532 0 2 41 0.6070 0.0298 0 2 42 -0.6702 0.0338 0 2 43 0.8655 0.0303 0 4 0 -4.4443 -0.1483 0 4 1 -28.3478 -0.0223 0 4 2 -1.1291 -0.2155 0 4 3 -68.5882 -0.0200 0 4 4 6.0457 -0.2782 0 4 5 -73.1647 0.0539 0 4 6 11.4223 -0.1918 0 4 7 -49.3888 0.1165 0 4 8 11.8106 -0.0579 0 4 9 -19.0995 0.0795 0 4 10 8.5485 0.0116 0 4 11 0.8223 -0.0148 0 4 12 4.3476 0.0514 0 4 13 7.2986 -0.0667 0 4 14 0.5724 0.0694 0 4 15 6.8167 -0.0511 0 4 16 -1.9641 0.0114 0 4 17 6.1399 -0.0007 0 4 18 -2.6607 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-0.2516 -0.1379 0 6 21 3.0388 -0.0022 0 6 22 1.8520 -0.1257 0 6 23 1.4397 0.0482 0 6 24 2.4356 -0.0089 0 6 25 -0.7268 0.0541 0 6 26 2.8428 0.0864 0 6 27 -2.3810 0.0395 0 6 28 2.9041 0.1057 0 6 29 -2.6956 0.0250 0 6 30 2.0725 0.1041 0 6 31 -1.9736 0.0263 0 6 32 0.8815 0.0949 0 6 33 -1.0010 0.0280 0 6 34 0.2506 0.0418 0 6 35 -0.0439 0.0040 0 6 36 0.3617 -0.0159 0 6 37 0.7897 -0.0204 0 6 38 0.7463 -0.0179 0 6 39 1.1885 -0.0090 0 6 40 0.8896 0.0061 0 6 41 1.0597 0.0150 0 6 42 0.6137 0.0079 0 8 0 -24.3796 -0.0825 0 8 1 0.1575 -0.1199 0 8 2 -18.1031 -0.0509 0 8 3 -0.3554 -0.2041 0 8 4 -5.1470 0.0459 0 8 5 -2.4239 -0.0653 0 8 6 2.9019 0.1586 0 8 7 -4.3194 0.0606 0 8 8 -0.0142 0.1895 0 8 9 -3.2090 0.0467 0 8 10 -9.9747 0.1505 0 8 11 1.1185 -0.0087 0 8 12 -18.4787 0.1107 0 8 13 6.2753 -0.0677 0 8 14 -20.2006 0.0673 0 8 15 10.5446 -0.1901 0 8 16 -15.6472 0.0228 0 8 17 13.1358 -0.3089 0 8 18 -8.6799 0.0169 0 8 19 12.9841 -0.2719 0 8 20 -2.9515 0.0312 0 8 21 10.0513 -0.0902 0 8 22 0.2296 0.0319 0 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5.0519 -0.1365 0 10 26 -2.7129 -0.0254 0 10 27 1.2939 -0.1517 0 10 28 -0.4802 -0.0005 0 10 29 -1.8608 -0.1128 0 10 30 1.5360 0.0343 0 10 31 -3.8898 -0.0587 0 10 32 2.5695 0.0560 0 10 33 -4.3861 -0.0590 0 10 34 2.6884 0.0571 0 10 35 -3.4094 -0.0935 0 10 36 2.1705 0.0444 0 10 37 -1.8242 -0.0941 0 10 38 1.2545 0.0253 0 10 39 -0.6887 -0.0595 0 12 1 0.8450 0.0413 0 12 2 -13.3102 -0.0302 0 12 3 0.7371 0.0977 0 12 4 -10.4156 -0.0132 0 12 5 -3.2844 0.0788 0 12 6 -5.6614 -0.0505 0 12 7 -9.2260 -0.0251 0 12 8 0.3293 -0.0912 0 12 9 -11.9800 -0.1325 0 12 10 5.3307 -0.0500 0 12 11 -8.7593 -0.1925 0 12 12 7.3582 0.0275 0 12 13 -1.8160 -0.2168 0 12 14 6.5300 0.0350 0 12 15 4.7434 -0.1909 0 12 16 3.7910 -0.0043 0 12 17 8.2918 -0.1302 0 12 18 -0.0246 -0.0076 0 12 19 8.3349 -0.1195 0 12 20 -3.5514 0.0013 0 12 21 6.3474 -0.1621 0 12 22 -5.6582 -0.0280 0 12 23 4.4640 -0.1679 0 12 24 -6.3322 -0.0498 0 12 25 3.4316 -0.1286 0 12 26 -5.7261 -0.0138 0 12 27 2.5891 -0.1065 0 12 28 -3.9163 0.0374 0 12 29 1.3769 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1.2933 0.0001 19 7 9 -0.7245 0.0221 19 7 10 0.6820 -0.0228 19 7 11 -0.2948 -0.0066 19 7 12 0.2009 -0.0258 19 7 13 0.1714 -0.0071 19 7 14 0.1395 -0.0077 19 7 15 0.3692 -0.0028 19 7 16 0.3217 -0.0009 19 7 17 0.3886 -0.0401 19 7 18 0.5451 -0.0064 19 7 19 0.3439 -0.0655 19 8 1 -0.5418 -0.0030 19 8 2 1.8063 -0.0098 19 8 3 -0.3590 0.0297 19 8 4 2.4065 0.0085 19 8 5 -0.2165 0.0350 19 8 6 2.0100 0.0203 19 8 7 -0.1851 0.0125 19 8 8 1.5161 0.0073 19 8 9 -0.1844 -0.0005 19 8 10 1.2646 -0.0028 19 8 11 -0.1151 0.0085 19 8 12 1.0598 0.0182 19 8 13 0.1753 0.0120 19 8 14 0.7007 0.0435 19 8 15 0.6289 -0.0049 19 8 16 0.1962 0.0336 19 8 17 0.8392 -0.0293 19 8 18 -0.2155 -0.0025 19 9 1 0.8625 0.0607 19 9 2 -0.6242 -0.0984 19 9 3 0.4234 0.0071 19 9 4 -0.6363 -0.0422 19 9 5 -0.2850 0.0035 19 9 6 -0.2394 0.0095 19 9 7 -0.8394 0.0124 19 9 8 0.0084 0.0108 19 9 9 -0.7856 -0.0061 19 9 10 0.0207 0.0002 19 9 11 -0.1480 -0.0058 19 9 12 0.0561 0.0091 19 9 13 0.5212 0.0278 19 9 14 0.1640 0.0103 19 9 15 0.7833 0.0302 19 9 16 0.2248 -0.0006 19 10 1 2.0893 -0.0417 19 10 2 0.8337 -0.0058 19 10 3 1.1504 -0.0048 19 10 4 0.9505 0.0222 19 10 5 0.0272 0.0082 19 10 6 0.5448 0.0265 19 10 7 -0.5642 -0.0202 19 10 8 0.1605 -0.0032 19 10 9 -0.6049 -0.0414 19 10 10 0.0076 -0.0297 19 10 11 -0.4867 -0.0297 19 10 12 0.0727 -0.0242 19 10 13 -0.3483 -0.0189 19 10 14 0.1755 -0.0065 19 11 1 -0.6940 -0.0052 19 11 2 -0.5286 -0.0186 19 11 3 -0.6919 0.0294 19 11 4 -0.4625 0.0219 19 11 5 -0.7758 0.0459 19 11 6 -0.0119 0.0294 19 11 7 -0.7960 0.0259 19 11 8 0.3468 0.0075 19 11 9 -0.4490 -0.0057 19 11 10 0.5141 0.0139 19 11 11 0.1808 -0.0077 19 12 1 1.2893 0.0092 19 12 2 -0.7752 -0.0373 19 12 3 0.6307 0.0344 19 12 4 -1.1370 0.0087 19 12 5 -0.1064 0.0104 19 12 6 -0.9548 0.0200 20 0 0 -0.5726 -0.0313 20 0 2 -0.5447 0.0155 20 0 4 -0.4934 0.0706 20 0 6 -0.3044 0.0352 20 0 8 0.1362 -0.0383 20 0 10 0.4581 -0.0439 20 0 12 0.2953 0.0087 20 0 14 -0.0547 0.0362 20 0 16 -0.1922 0.0169 20 0 18 -0.1623 -0.0072 20 0 20 -0.0603 -0.0130 20 1 0 0.1030 -0.0235 20 1 1 -0.2305 -0.0656 20 1 2 0.1966 0.0433 20 1 3 -0.4029 -0.0477 20 1 4 0.3515 0.0351 20 1 5 -0.0623 0.0069 20 1 6 0.3661 -0.0504 20 1 7 0.4828 0.0331 20 1 8 0.1772 -0.1064 20 1 9 0.7725 0.0141 20 1 10 -0.1428 -0.0603 20 1 11 0.4963 -0.0084 20 1 12 -0.4178 0.0245 20 1 13 -0.2399 -0.0173 20 1 14 -0.4582 0.0421 20 1 15 -0.9182 -0.0261 20 1 16 -0.2574 -0.0081 20 1 17 -1.1789 -0.0357 20 1 18 0.0201 -0.0388 20 1 19 -1.0628 -0.0341 20 1 20 0.2388 -0.0115 20 2 0 -2.0925 -0.0458 20 2 1 -0.0493 0.0664 20 2 2 -1.8601 -0.0304 20 2 3 -0.0544 0.1034 20 2 4 -1.3071 -0.0424 20 2 5 0.0684 0.0078 20 2 6 -0.5707 -0.0492 20 2 7 0.1368 -0.0670 20 2 8 0.2673 0.0022 20 2 9 0.0671 0.0148 20 2 10 0.8083 0.0469 20 2 11 0.0506 0.0897 20 2 12 0.7375 0.0362 20 2 13 0.2343 0.0226 20 2 14 0.3786 0.0143 20 2 15 0.4784 -0.0580 20 2 16 0.1469 0.0062 20 2 17 0.6144 -0.0466 20 2 18 0.0197 -0.0038 20 2 19 0.6190 -0.0149 20 2 20 -0.0640 -0.0085 20 3 0 -0.9238 -0.0430 20 3 1 -0.3697 0.0222 20 3 2 -0.5873 0.0338 20 3 3 -0.8932 -0.0170 20 3 4 -0.0015 0.0666 20 3 5 -0.9925 -0.0346 20 3 6 0.1875 0.0217 20 3 7 -0.8015 -0.0279 20 3 8 -0.1144 -0.0268 20 3 9 -0.5517 -0.0066 20 3 10 -0.5621 -0.0187 20 3 11 -0.3831 0.0133 20 3 12 -0.7459 0.0107 20 3 13 -0.2579 0.0136 20 3 14 -0.4617 0.0090 20 3 15 -0.0621 0.0048 20 3 16 0.0725 -0.0116 20 3 17 0.1266 0.0095 20 3 18 0.4962 -0.0134 20 3 19 0.1606 0.0155 20 4 0 -1.5948 0.0267 20 4 1 0.6464 -0.0546 20 4 2 -1.3980 0.0705 20 4 3 1.8103 -0.0065 20 4 4 -0.8983 0.0314 20 4 5 2.4795 -0.0243 20 4 6 -0.1397 0.0159 20 4 7 2.2960 -0.0142 20 4 8 0.8527 0.0527 20 4 9 1.4332 0.0400 20 4 10 1.6505 0.0347 20 4 11 0.6371 0.0386 20 4 12 1.7524 -0.0244 20 4 13 0.4121 -0.0212 20 4 14 1.2828 -0.0194 20 4 15 0.5523 -0.0373 20 4 16 0.7174 0.0266 20 4 17 0.7026 0.0029 20 4 18 0.2540 0.0325 20 4 19 0.7861 0.0285 20 5 0 -2.8252 -0.0991 20 5 1 -0.2150 -0.0077 20 5 2 -2.2299 -0.0537 20 5 3 -0.6781 -0.0013 20 5 4 -1.0435 -0.0100 20 5 5 -1.0664 0.0030 20 5 6 -0.1903 -0.0070 20 5 7 -1.0973 0.0045 20 5 8 0.1510 -0.0131 20 5 9 -0.7021 0.0027 20 5 10 0.3154 -0.0035 20 5 11 -0.1421 0.0045 20 5 12 0.5620 0.0024 20 5 13 0.2973 0.0156 20 5 14 0.8519 -0.0048 20 5 15 0.5115 0.0344 20 5 16 0.8787 -0.0120 20 5 17 0.5029 0.0470 20 5 18 0.5584 -0.0182 20 6 0 1.6993 0.0827 20 6 1 0.5721 0.0974 20 6 2 1.3559 0.0786 20 6 3 1.7631 0.0591 20 6 4 0.4911 0.0339 20 6 5 2.7302 0.0031 20 6 6 -0.3255 0.0400 20 6 7 2.8130 -0.0112 20 6 8 -0.4454 0.0603 20 6 9 1.8753 -0.0099 20 6 10 0.0968 0.0210 20 6 11 0.6836 -0.0182 20 6 12 0.6244 -0.0139 20 6 13 0.0159 -0.0123 20 6 14 0.7300 0.0107 20 6 15 -0.0917 0.0076 20 6 16 0.5874 0.0204 20 6 17 0.0476 0.0064 20 7 0 -3.1113 -0.0246 20 7 1 0.5803 -0.0564 20 7 2 -2.5479 0.0214 20 7 3 1.2200 -0.0299 20 7 4 -1.3229 0.0407 20 7 5 0.9966 -0.0054 20 7 6 -0.2217 0.0183 20 7 7 0.5409 0.0141 20 7 8 0.4093 -0.0063 20 7 9 0.3929 0.0203 20 7 10 0.6280 -0.0012 20 7 11 0.4457 0.0269 20 7 12 0.6861 0.0151 20 7 13 0.3705 0.0475 20 7 14 0.7885 0.0171 20 7 15 0.0893 0.0651 20 8 0 1.8924 0.0943 20 8 1 -0.2520 -0.0032 20 8 2 1.6679 0.0176 20 8 3 -0.3536 -0.0111 20 8 4 0.9529 -0.0299 20 8 5 0.1508 0.0091 20 8 6 -0.0414 -0.0139 20 8 7 0.6091 0.0223 20 8 8 -0.6706 -0.0095 20 8 9 0.5250 0.0038 20 8 10 -0.5459 -0.0345 20 8 11 0.1576 -0.0141 20 8 12 -0.0382 -0.0234 20 8 13 -0.0511 -0.0155 20 9 0 0.0710 -0.0270 20 9 1 0.8259 0.0004 20 9 2 -0.0645 0.0092 20 9 3 1.8311 0.0082 20 9 4 -0.3093 0.0430 20 9 5 1.6656 0.0242 20 9 6 -0.3522 0.0391 20 9 7 0.9374 0.0345 20 9 8 -0.1353 0.0068 20 9 9 0.3771 0.0274 20 9 10 0.0712 -0.0114 20 9 11 0.2139 0.0163 20 10 0 -0.2261 0.0210 20 10 1 -0.2975 -0.0697 20 10 2 -0.1460 -0.0044 20 10 3 -0.6052 -0.0487 20 10 4 -0.1158 0.0027 20 10 5 -0.4600 -0.0067 20 10 6 -0.3148 0.0206 20 10 7 -0.2124 -0.0016 21 0 2 -1.0266 -0.0142 21 0 4 -1.3315 0.0249 21 0 6 -0.9564 0.0546 21 0 8 -0.3932 0.0139 21 0 10 -0.0686 -0.0468 21 0 12 -0.1546 -0.0568 21 0 14 -0.4060 -0.0287 21 0 16 -0.4486 -0.0138 21 1 1 -0.3269 -0.0038 21 1 2 -0.4339 0.0970 21 1 3 -0.4169 0.0123 21 1 4 -0.6511 0.1020 21 1 5 -0.5031 -0.0083 21 1 6 -0.6118 -0.0135 21 1 7 -0.3690 -0.0261 21 1 8 -0.4113 -0.0661 21 1 9 -0.0266 -0.0121 21 1 10 -0.1648 -0.0064 21 1 11 0.2145 0.0059 21 1 12 0.0079 0.0127 21 1 13 0.2349 0.0131 21 1 14 0.0277 -0.0274 21 1 15 0.1676 0.0189 21 1 16 -0.0271 -0.0273 21 2 1 -1.0512 -0.0145 21 2 2 -0.6763 -0.0488 21 2 3 -0.4489 0.0384 21 2 4 -0.9021 -0.0259 21 2 5 0.2004 0.0034 21 2 6 -0.7328 0.0069 21 2 7 0.4669 -0.0683 21 2 8 -0.4579 0.0116 21 2 9 0.3475 -0.0701 21 2 10 -0.2692 -0.0045 21 2 11 0.0895 -0.0054 21 2 12 -0.2291 -0.0232 21 2 13 -0.0212 0.0327 21 2 14 -0.1986 -0.0392 21 2 15 0.0754 0.0099 21 2 16 -0.0237 -0.0408 21 3 1 -1.8952 0.0078 21 3 2 0.1162 -0.0313 21 3 3 -1.5475 -0.0276 21 3 4 0.2783 0.0025 21 3 5 -0.9001 -0.0826 21 3 6 0.3309 -0.0082 21 3 7 -0.0212 -0.0504 21 3 8 0.2183 0.0186 21 3 9 0.7518 0.0211 21 3 10 0.1902 0.0530 21 3 11 0.9535 0.0299 21 3 12 0.3950 0.0155 21 3 13 0.6373 0.0077 21 3 14 0.5982 -0.0359 21 3 15 0.3030 0.0113 21 4 1 -1.6870 -0.0463 21 4 2 -0.4318 -0.0136 21 4 3 -1.0218 0.0358 21 4 4 -0.7915 -0.0231 21 4 5 -0.3442 0.0396 21 4 6 -0.9897 -0.0240 21 4 7 -0.0311 -0.0065 21 4 8 -0.9121 -0.0201 21 4 9 0.0568 -0.0190 21 4 10 -0.5632 -0.0160 21 4 11 0.1545 0.0005 21 4 12 -0.1341 -0.0122 21 4 13 0.3675 0.0017 21 4 14 0.2014 -0.0026 21 5 1 -0.1995 0.0633 21 5 2 0.8741 -0.0600 21 5 3 -0.4288 0.0715 21 5 4 1.7322 -0.0408 21 5 5 -0.5956 0.0424 21 5 6 2.0558 -0.0132 21 5 7 -0.2762 0.0463 21 5 8 1.4917 0.0174 21 5 9 0.4745 0.0331 21 5 10 0.5563 0.0088 21 5 11 0.9952 -0.0161 21 5 12 0.0232 -0.0230 21 5 13 0.8947 -0.0199 21 6 1 -2.7618 -0.0507 21 6 2 -0.0465 0.0158 21 6 3 -1.8930 -0.0117 21 6 4 -0.3145 0.0207 21 6 5 -0.7943 -0.0173 21 6 6 -0.5691 0.0225 21 6 7 0.0309 -0.0400 21 6 8 -0.4552 0.0237 21 6 9 0.4492 -0.0283 21 6 10 -0.0282 0.0158 21 6 11 0.5220 0.0003 21 6 12 0.3218 0.0147 21 7 1 1.5155 0.0709 21 7 2 0.0029 0.0297 21 7 3 1.0101 0.0324 21 7 4 0.5528 0.0147 21 7 5 0.1207 0.0110 21 7 6 1.2031 0.0247 21 7 7 -0.5771 0.0115 21 7 8 1.1994 0.0233 21 7 9 -0.5481 -0.0122 21 8 1 -1.6151 0.0092 21 8 2 0.9573 -0.0319 21 8 3 -1.1774 0.0353 21 8 4 1.1617 -0.0189 21 8 5 -0.4885 0.0315 22 0 0 0.8713 -0.0274 22 0 2 0.6761 -0.0078 22 0 4 0.2145 0.0253 22 0 6 -0.1962 0.0339 22 0 8 -0.2945 0.0153 22 0 10 -0.1211 -0.0087 22 1 0 -1.0434 -0.0205 22 1 1 -0.5310 0.0005 22 1 2 -0.7947 0.0116 22 1 3 -1.2297 0.0093 22 1 4 -0.2686 0.0107 22 1 5 -1.2748 0.0382 22 1 6 0.1436 -0.0193 22 1 7 -0.9530 0.0328 22 1 8 0.2638 -0.0117 22 1 9 -0.5926 -0.0075 22 1 10 0.1763 0.0488 22 2 0 -0.3577 0.0218 22 2 1 -0.2413 -0.0361 22 2 2 -0.3666 0.0088 22 2 3 -0.5890 0.0367 22 2 4 -0.3601 -0.0531 22 2 5 -0.6850 0.0357 22 2 6 -0.2545 -0.0876 22 2 7 -0.5766 -0.0148 22 2 8 -0.0599 -0.0435 22 2 9 -0.2760 -0.0190 22 2 10 0.0400 0.0069 22 3 0 -1.2256 -0.0519 22 3 1 -0.1002 -0.0801 22 3 2 -0.9104 0.0079 22 3 3 -0.2829 -0.0489 22 3 4 -0.2799 0.0342 22 3 5 -0.4653 -0.0058 22 3 6 0.1775 0.0039 22 3 7 -0.6155 0.0081 22 3 8 0.3323 -0.0119 22 3 9 -0.5814 -0.0135 22 4 0 -0.6570 -0.0192 22 4 1 0.0225 -0.1151 22 4 2 -0.6936 0.0127 22 4 3 0.1585 -0.0731 22 4 4 -0.7064 -0.0132 22 4 5 0.2879 -0.0248 22 4 6 -0.4690 -0.0178 22 4 7 0.1412 0.0192 22 5 0 -1.6061 -0.0442 22 5 1 -0.0639 0.0397 22 5 2 -1.4088 0.0133 22 5 3 -0.2531 0.0404 22 5 4 -0.9784 0.0280 22 5 5 -0.4941 0.0250 0 0 0 0.0 0.0 ; _shelx_fab_checksum 58364 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - B-factor correction ; _oxdiff_exptl_absorpt_empirical_full_max 2.489 _oxdiff_exptl_absorpt_empirical_full_min 0.654 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, 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 F1 F 0.54181(5) 0.71042(6) 0.58549(3) 0.0471(2) Uani 1 1 d . . . . . F2 F 0.44795(6) 0.80926(7) 0.61332(5) 0.0700(4) Uani 1 1 d . . . . . F3 F 0.47153(6) 0.87303(6) 0.68343(4) 0.0665(4) Uani 1 1 d . . . . . F4 F 0.58955(7) 0.82940(6) 0.72648(3) 0.0538(3) Uani 1 1 d . . . . . F5 F 0.68248(5) 0.72683(5) 0.70031(3) 0.0403(2) Uani 1 1 d . . . . . F6 F 0.68662(5) 0.77881(5) 0.57236(3) 0.0422(2) Uani 1 1 d . . . . . F7 F 0.77593(7) 0.89642(6) 0.57106(4) 0.0579(3) Uani 1 1 d . . . . . F8 F 0.88941(6) 0.90809(6) 0.62246(4) 0.0580(3) Uani 1 1 d . . . . . F9 F 0.91351(6) 0.79629(6) 0.67364(3) 0.0513(2) Uani 1 1 d . . . . . F10 F 0.82872(5) 0.67694(5) 0.67391(3) 0.0391(2) Uani 1 1 d . . . . . F11 F 0.81200(5) 0.56178(5) 0.61846(3) 0.0426(2) Uani 1 1 d . . . . . F12 F 0.84465(6) 0.44036(6) 0.65823(4) 0.0567(3) Uani 1 1 d . . . . . F13 F 0.75466(7) 0.39531(6) 0.71702(3) 0.0572(3) Uani 1 1 d . . . . . F14 F 0.63236(6) 0.47637(6) 0.73470(3) 0.0500(2) Uani 1 1 d . . . . . F15 F 0.59689(5) 0.59530(5) 0.69453(3) 0.0403(2) Uani 1 1 d . . . . . F16 F 0.55861(5) 0.56586(5) 0.61013(3) 0.0407(2) Uani 1 1 d . . . . . F17 F 0.53219(6) 0.48327(6) 0.54828(3) 0.0528(3) Uani 1 1 d . . . . . F18 F 0.63191(7) 0.48046(6) 0.48878(3) 0.0531(3) Uani 1 1 d . . . . . F19 F 0.75600(6) 0.56497(5) 0.49317(3) 0.0448(2) Uani 1 1 d . . . . . F20 F 0.78062(5) 0.65241(5) 0.55252(3) 0.03867(19) Uani 1 1 d . . . . . C41 C 0.61707(8) 0.71102(8) 0.64184(4) 0.0327(3) Uani 1 1 d . . . . . C42 C 0.55583(9) 0.73563(9) 0.62135(5) 0.0394(3) Uani 1 1 d . . . . . C43 C 0.50642(9) 0.78822(10) 0.63489(6) 0.0490(4) Uani 1 1 d . . . . . C44 C 0.51763(9) 0.82020(9) 0.67021(6) 0.0487(4) Uani 1 1 d . . . . . C45 C 0.57752(10) 0.79826(8) 0.69191(5) 0.0420(4) Uani 1 1 d . . . . . C46 C 0.62476(8) 0.74493(8) 0.67761(5) 0.0358(3) Uani 1 1 d . . . . . C47 C 0.75230(8) 0.72097(8) 0.62315(4) 0.0310(3) Uani 1 1 d . . . . . C48 C 0.74357(8) 0.78015(8) 0.59773(4) 0.0348(3) Uani 1 1 d . . . . . C49 C 0.78821(10) 0.84170(9) 0.59649(5) 0.0411(3) Uani 1 1 d . . . . . C50 C 0.84590(9) 0.84773(9) 0.62230(5) 0.0421(4) Uani 1 1 d . . . . . C51 C 0.85778(9) 0.79116(9) 0.64798(5) 0.0386(3) Uani 1 1 d . . . . . C52 C 0.81205(8) 0.72948(8) 0.64772(4) 0.0330(3) Uani 1 1 d . . . . . C53 C 0.70413(8) 0.58732(8) 0.65476(4) 0.0309(3) Uani 1 1 d . . . . . C54 C 0.76565(8) 0.54300(8) 0.64733(4) 0.0353(3) Uani 1 1 d . . . . . C55 C 0.78383(9) 0.47978(9) 0.66735(5) 0.0407(3) Uani 1 1 d . . . . . C56 C 0.73871(10) 0.45683(9) 0.69705(5) 0.0413(3) Uani 1 1 d . . . . . C57 C 0.67663(9) 0.49777(9) 0.70566(4) 0.0376(3) Uani 1 1 d . . . . . C58 C 0.66037(8) 0.56078(8) 0.68451(4) 0.0330(3) Uani 1 1 d . . . . . C59 C 0.66949(8) 0.61592(8) 0.58472(4) 0.0308(3) Uani 1 1 d . . . . . C60 C 0.60810(8) 0.56949(8) 0.58101(4) 0.0340(3) Uani 1 1 d . . . . . C61 C 0.59354(9) 0.52543(8) 0.54961(5) 0.0392(3) Uani 1 1 d . . . . . C62 C 0.64319(10) 0.52415(8) 0.51960(4) 0.0394(3) Uani 1 1 d . . . . . C63 C 0.70572(9) 0.56739(8) 0.52182(4) 0.0362(3) Uani 1 1 d . . . . . C64 C 0.71731(8) 0.61222(8) 0.55355(4) 0.0323(3) Uani 1 1 d . . . . . B1 B 0.68578(9) 0.65799(9) 0.62604(5) 0.0295(3) Uani 1 1 d . . . . . N1 N 0.78568(7) 0.43730(6) 0.38293(3) 0.0304(2) Uani 1 1 d . . . . . N2 N 0.87127(7) 0.38114(7) 0.41601(3) 0.0330(3) Uani 1 1 d . . . . . C1 C 0.82910(7) 0.37630(7) 0.38336(4) 0.0272(3) Uani 1 1 d . . . . . C2 C 0.80135(10) 0.48044(9) 0.41467(5) 0.0422(4) Uani 1 1 d . . . . . H2 H 0.778658 0.526321 0.421016 0.051 Uiso 1 1 calc R U . . . C3 C 0.85429(10) 0.44603(9) 0.43492(5) 0.0433(4) Uani 1 1 d . . . . . H3 H 0.876140 0.463225 0.458102 0.052 Uiso 1 1 calc R U . . . C4 C 0.72528(8) 0.46073(7) 0.35773(4) 0.0291(3) Uani 1 1 d . . . . . C5 C 0.73769(8) 0.51975(7) 0.33254(4) 0.0318(3) Uani 1 1 d . . . . . C6 C 0.67794(9) 0.54552(8) 0.31136(4) 0.0347(3) Uani 1 1 d . . . . . H6 H 0.685308 0.585260 0.293871 0.042 Uiso 1 1 calc R U . . . C7 C 0.60747(9) 0.51491(8) 0.31495(4) 0.0350(3) Uani 1 1 d . . . . . C8 C 0.59746(8) 0.45735(8) 0.34081(4) 0.0341(3) Uani 1 1 d . . . . . H8 H 0.549685 0.435764 0.343244 0.041 Uiso 1 1 calc R U . . . C9 C 0.65510(8) 0.43015(8) 0.36334(4) 0.0306(3) Uani 1 1 d . . . . . C10 C 0.81244(9) 0.55551(8) 0.32787(5) 0.0418(4) Uani 1 1 d . . . . . H10A H 0.847529 0.519294 0.317431 0.063 Uiso 1 1 calc R U . . . H10B H 0.830107 0.572923 0.352917 0.063 Uiso 1 1 calc R U . . . H10C H 0.808373 0.597613 0.310213 0.063 Uiso 1 1 calc R U . . . C11 C 0.54301(10) 0.54609(10) 0.29281(5) 0.0478(4) Uani 1 1 d . . . . . H11A H 0.529428 0.594489 0.303450 0.072 Uiso 1 1 calc R U . . . H11B H 0.500698 0.512286 0.294805 0.072 Uiso 1 1 calc R U . . . H11C H 0.556926 0.551808 0.265752 0.072 Uiso 1 1 calc R U . . . C12 C 0.63966(9) 0.37135(9) 0.39305(5) 0.0395(3) Uani 1 1 d . . . . . H12A H 0.650981 0.322470 0.382297 0.059 Uiso 1 1 calc R U . . . H12B H 0.587307 0.373283 0.400451 0.059 Uiso 1 1 calc R U . . . H12C H 0.670667 0.380089 0.415722 0.059 Uiso 1 1 calc R U . . . C13 C 0.91650(8) 0.32680(8) 0.43693(4) 0.0333(3) Uani 1 1 d . . . . . C14 C 0.99258(9) 0.31972(9) 0.42992(5) 0.0380(3) Uani 1 1 d . . . . . C15 C 1.03139(9) 0.26974(9) 0.45283(5) 0.0419(4) Uani 1 1 d . . . . . H15 H 1.082789 0.262894 0.448138 0.050 Uiso 1 1 calc R U . . . C16 C 0.99858(10) 0.22966(9) 0.48207(5) 0.0423(4) Uani 1 1 d . . . . . C17 C 0.92370(10) 0.24118(9) 0.48948(5) 0.0414(3) Uani 1 1 d . . . . . H17 H 0.900716 0.214906 0.509909 0.050 Uiso 1 1 calc R U . . . C18 C 0.88155(9) 0.29045(9) 0.46760(4) 0.0365(3) Uani 1 1 d . . . . . C19 C 1.03469(10) 0.36331(12) 0.40061(6) 0.0522(4) Uani 1 1 d . . . . . H19A H 1.087302 0.364267 0.407564 0.078 Uiso 1 1 calc R U . . . H19B H 1.015509 0.414068 0.399745 0.078 Uiso 1 1 calc R U . . . H19C H 1.028856 0.340137 0.375327 0.078 Uiso 1 1 calc R U . . . C20 C 1.04372(12) 0.17647(11) 0.50605(6) 0.0575(5) Uani 1 1 d . . . . . H20A H 1.058391 0.200704 0.530076 0.086 Uiso 1 1 calc R U . . . H20B H 1.088122 0.161718 0.491761 0.086 Uiso 1 1 calc R U . . . H20C H 1.013938 0.132487 0.511876 0.086 Uiso 1 1 calc R U . . . C21 C 0.80205(10) 0.30441(10) 0.47892(5) 0.0443(4) Uani 1 1 d . . . . . H21A H 0.780665 0.258932 0.489577 0.066 Uiso 1 1 calc R U . . . H21B H 0.773674 0.319596 0.456239 0.066 Uiso 1 1 calc R U . . . H21C H 0.800183 0.343767 0.498292 0.066 Uiso 1 1 calc R U . . . C22 C 0.83991(7) 0.31859(7) 0.35132(4) 0.0261(3) Uani 1 1 d . . . . . C23 C 0.77392(7) 0.31344(7) 0.32205(4) 0.0264(3) Uani 1 1 d . . . . . C24 C 0.72415(8) 0.25468(8) 0.32141(4) 0.0331(3) Uani 1 1 d . . . . . H24 H 0.726099 0.218262 0.341092 0.040 Uiso 1 1 calc R U . . . C25 C 0.67160(8) 0.24842(8) 0.29242(5) 0.0381(3) Uani 1 1 d . . . . . H25 H 0.637786 0.208084 0.292730 0.046 Uiso 1 1 calc R U . . . C26 C 0.66780(8) 0.29978(9) 0.26326(4) 0.0360(3) Uani 1 1 d . . . . . H26 H 0.632299 0.294653 0.243277 0.043 Uiso 1 1 calc R U . . . C27 C 0.71649(8) 0.35901(8) 0.26348(4) 0.0329(3) Uani 1 1 d . . . . . H27 H 0.713786 0.395465 0.243844 0.040 Uiso 1 1 calc R U . . . C28 C 0.76909(8) 0.36530(7) 0.29223(4) 0.0290(3) Uani 1 1 d . . . . . H28 H 0.802729 0.405766 0.291715 0.035 Uiso 1 1 calc R U . . . C29 C 0.90643(7) 0.34330(7) 0.32634(4) 0.0278(3) Uani 1 1 d . . . . . C30 C 0.94057(8) 0.41168(8) 0.33033(4) 0.0329(3) Uani 1 1 d . . . . . H30 H 0.926763 0.443135 0.351004 0.040 Uiso 1 1 calc R U . . . C31 C 0.99486(9) 0.43509(9) 0.30449(5) 0.0401(3) Uani 1 1 d . . . . . H31 H 1.017709 0.482108 0.307671 0.048 Uiso 1 1 calc R U . . . C32 C 1.01528(9) 0.39008(9) 0.27441(5) 0.0413(3) Uani 1 1 d . . . . . H32 H 1.052432 0.405705 0.256855 0.050 Uiso 1 1 calc R U . . . C33 C 0.98130(9) 0.32172(9) 0.26987(4) 0.0384(3) Uani 1 1 d . . . . . H33 H 0.995447 0.290519 0.249149 0.046 Uiso 1 1 calc R U . . . C34 C 0.92701(8) 0.29852(8) 0.29521(4) 0.0324(3) Uani 1 1 d . . . . . H34 H 0.903526 0.251963 0.291499 0.039 Uiso 1 1 calc R U . . . C35 C 0.85200(8) 0.24374(7) 0.37193(4) 0.0287(3) Uani 1 1 d . . . . . C36 C 0.91588(9) 0.20158(8) 0.36819(5) 0.0354(3) Uani 1 1 d . . . . . H36 H 0.954380 0.217458 0.351495 0.043 Uiso 1 1 calc R U . . . C37 C 0.92361(10) 0.13581(9) 0.38894(5) 0.0449(4) Uani 1 1 d . . . . . H37 H 0.967457 0.107213 0.386098 0.054 Uiso 1 1 calc R U . . . C38 C 0.86885(12) 0.11173(9) 0.41343(5) 0.0474(4) Uani 1 1 d . . . . . H38 H 0.874642 0.066825 0.427341 0.057 Uiso 1 1 calc R U . . . C39 C 0.80535(11) 0.15364(9) 0.41753(4) 0.0430(4) Uani 1 1 d . . . . . H39 H 0.767332 0.137785 0.434522 0.052 Uiso 1 1 calc R U . . . C40 C 0.79696(9) 0.21878(8) 0.39692(4) 0.0343(3) Uani 1 1 d . . . . . H40 H 0.752882 0.246983 0.399859 0.041 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 F1 0.0386(5) 0.0492(5) 0.0536(6) -0.0001(4) -0.0086(4) 0.0060(4) F2 0.0386(6) 0.0566(7) 0.1149(11) -0.0071(7) -0.0152(6) 0.0168(5) F3 0.0426(6) 0.0405(5) 0.1164(11) -0.0168(6) 0.0230(6) 0.0095(4) F4 0.0621(7) 0.0415(5) 0.0579(6) -0.0153(4) 0.0232(5) -0.0033(5) F5 0.0432(5) 0.0409(5) 0.0368(4) -0.0034(4) 0.0036(4) 0.0028(4) F6 0.0427(5) 0.0417(5) 0.0422(5) 0.0101(4) -0.0054(4) -0.0023(4) F7 0.0640(7) 0.0400(5) 0.0696(7) 0.0206(5) -0.0036(6) -0.0100(5) F8 0.0521(6) 0.0410(5) 0.0809(8) 0.0020(5) 0.0023(5) -0.0177(5) F9 0.0386(5) 0.0564(6) 0.0589(6) -0.0027(5) -0.0086(4) -0.0099(4) F10 0.0360(5) 0.0419(5) 0.0393(5) 0.0055(4) -0.0034(4) 0.0000(4) F11 0.0356(5) 0.0424(5) 0.0499(5) 0.0053(4) 0.0147(4) 0.0082(4) F12 0.0468(6) 0.0465(6) 0.0769(7) 0.0104(5) 0.0062(5) 0.0195(5) F13 0.0609(7) 0.0433(5) 0.0675(7) 0.0227(5) -0.0076(5) 0.0051(5) F14 0.0517(6) 0.0538(6) 0.0444(5) 0.0164(4) 0.0066(4) -0.0070(5) F15 0.0369(5) 0.0396(5) 0.0443(5) 0.0042(4) 0.0146(4) 0.0021(4) F16 0.0337(4) 0.0423(5) 0.0462(5) -0.0005(4) 0.0106(4) -0.0056(4) F17 0.0515(6) 0.0497(6) 0.0571(6) -0.0042(5) -0.0023(5) -0.0195(5) F18 0.0751(7) 0.0449(5) 0.0393(5) -0.0090(4) -0.0020(5) -0.0090(5) F19 0.0527(6) 0.0494(5) 0.0324(4) -0.0006(4) 0.0107(4) 0.0043(4) F20 0.0322(4) 0.0458(5) 0.0380(4) -0.0011(4) 0.0088(3) -0.0050(4) C41 0.0291(7) 0.0285(6) 0.0405(7) 0.0015(5) 0.0084(6) 0.0005(5) C42 0.0323(7) 0.0355(7) 0.0505(9) -0.0003(6) 0.0020(6) 0.0002(6) C43 0.0292(8) 0.0387(8) 0.0790(13) 0.0011(8) 0.0002(8) 0.0049(6) C44 0.0342(8) 0.0305(7) 0.0813(13) -0.0070(8) 0.0190(8) 0.0025(6) C45 0.0425(9) 0.0310(7) 0.0524(9) -0.0063(6) 0.0186(7) -0.0037(6) C46 0.0340(7) 0.0318(7) 0.0418(8) 0.0012(6) 0.0098(6) -0.0005(6) C47 0.0289(7) 0.0316(7) 0.0324(7) -0.0010(5) 0.0070(5) 0.0010(5) C48 0.0332(7) 0.0349(7) 0.0363(7) 0.0017(6) 0.0022(6) 0.0008(6) C49 0.0439(9) 0.0329(7) 0.0465(8) 0.0062(6) 0.0059(7) -0.0013(6) C50 0.0389(8) 0.0328(7) 0.0546(9) -0.0020(7) 0.0080(7) -0.0071(6) C51 0.0309(7) 0.0411(8) 0.0439(8) -0.0052(6) 0.0023(6) -0.0016(6) C52 0.0307(7) 0.0335(7) 0.0347(7) 0.0013(5) 0.0053(5) 0.0026(5) C53 0.0294(7) 0.0306(7) 0.0326(7) 0.0001(5) 0.0024(5) -0.0011(5) C54 0.0323(7) 0.0357(7) 0.0379(7) 0.0007(6) 0.0041(6) 0.0014(6) C55 0.0354(8) 0.0346(7) 0.0519(9) 0.0011(6) -0.0007(7) 0.0071(6) C56 0.0441(9) 0.0327(7) 0.0470(8) 0.0088(6) -0.0076(7) -0.0005(6) C57 0.0393(8) 0.0383(8) 0.0352(7) 0.0059(6) 0.0005(6) -0.0080(6) C58 0.0313(7) 0.0330(7) 0.0347(7) -0.0011(5) 0.0023(6) -0.0011(5) C59 0.0300(7) 0.0292(6) 0.0334(7) 0.0022(5) 0.0024(5) 0.0027(5) C60 0.0316(7) 0.0340(7) 0.0362(7) 0.0025(5) 0.0043(6) 0.0010(6) C61 0.0393(8) 0.0334(7) 0.0449(8) 0.0025(6) -0.0018(7) -0.0042(6) C62 0.0517(9) 0.0335(7) 0.0331(7) -0.0022(6) -0.0039(6) -0.0003(6) C63 0.0429(8) 0.0355(7) 0.0301(7) 0.0026(5) 0.0056(6) 0.0059(6) C64 0.0303(7) 0.0320(7) 0.0345(7) 0.0034(5) 0.0014(5) 0.0005(5) B1 0.0262(7) 0.0306(7) 0.0317(7) 0.0013(6) 0.0048(6) 0.0011(6) N1 0.0301(6) 0.0272(5) 0.0338(6) -0.0052(4) 0.0018(5) 0.0004(4) N2 0.0330(6) 0.0325(6) 0.0334(6) -0.0068(5) -0.0039(5) -0.0009(5) C1 0.0246(6) 0.0263(6) 0.0306(6) -0.0016(5) 0.0014(5) -0.0037(5) C2 0.0488(9) 0.0331(7) 0.0448(8) -0.0142(6) -0.0027(7) 0.0051(6) C3 0.0492(9) 0.0379(8) 0.0426(8) -0.0154(6) -0.0084(7) 0.0024(7) C4 0.0281(6) 0.0262(6) 0.0330(6) -0.0026(5) 0.0040(5) 0.0039(5) C5 0.0321(7) 0.0240(6) 0.0395(7) -0.0031(5) 0.0085(6) 0.0000(5) C6 0.0413(8) 0.0265(6) 0.0363(7) 0.0030(5) 0.0072(6) 0.0025(6) C7 0.0363(7) 0.0328(7) 0.0358(7) -0.0014(6) 0.0014(6) 0.0027(6) C8 0.0292(7) 0.0338(7) 0.0393(7) -0.0006(6) 0.0053(6) 0.0001(5) C9 0.0306(7) 0.0288(6) 0.0325(7) -0.0008(5) 0.0078(5) 0.0011(5) C10 0.0352(8) 0.0278(7) 0.0625(10) 0.0032(6) 0.0111(7) -0.0024(6) C11 0.0477(10) 0.0434(9) 0.0524(10) 0.0054(7) -0.0111(8) 0.0034(7) C12 0.0342(8) 0.0403(8) 0.0441(8) 0.0106(6) 0.0095(6) 0.0006(6) C13 0.0333(7) 0.0340(7) 0.0327(7) -0.0064(5) -0.0079(6) -0.0003(6) C14 0.0321(7) 0.0418(8) 0.0403(8) -0.0078(6) -0.0079(6) -0.0039(6) C15 0.0330(8) 0.0454(8) 0.0473(9) -0.0096(7) -0.0088(6) 0.0030(6) C16 0.0447(9) 0.0393(8) 0.0429(8) -0.0079(6) -0.0107(7) 0.0044(7) C17 0.0457(9) 0.0431(8) 0.0353(7) -0.0023(6) -0.0052(6) 0.0013(7) C18 0.0372(8) 0.0401(8) 0.0321(7) -0.0065(6) -0.0052(6) 0.0006(6) C19 0.0294(8) 0.0684(12) 0.0587(11) 0.0082(9) -0.0077(7) -0.0081(8) C20 0.0592(12) 0.0543(10) 0.0590(11) 0.0023(9) -0.0077(9) 0.0178(9) C21 0.0406(9) 0.0588(10) 0.0336(8) -0.0023(7) 0.0007(6) 0.0042(7) C22 0.0252(6) 0.0252(6) 0.0279(6) -0.0025(5) 0.0003(5) -0.0005(5) C23 0.0240(6) 0.0268(6) 0.0283(6) -0.0027(5) 0.0011(5) 0.0014(5) C24 0.0320(7) 0.0298(7) 0.0376(7) 0.0048(5) -0.0046(6) -0.0029(5) C25 0.0314(7) 0.0334(7) 0.0494(9) 0.0039(6) -0.0089(6) -0.0055(6) C26 0.0291(7) 0.0400(8) 0.0389(8) 0.0015(6) -0.0068(6) 0.0016(6) C27 0.0310(7) 0.0346(7) 0.0332(7) 0.0051(5) 0.0005(5) 0.0025(5) C28 0.0279(6) 0.0268(6) 0.0323(6) -0.0007(5) 0.0035(5) -0.0003(5) C29 0.0237(6) 0.0292(6) 0.0306(6) 0.0001(5) -0.0001(5) 0.0024(5) C30 0.0292(7) 0.0286(6) 0.0409(7) -0.0009(5) 0.0045(6) 0.0019(5) C31 0.0332(7) 0.0321(7) 0.0550(9) 0.0065(6) 0.0090(7) 0.0000(6) C32 0.0311(7) 0.0455(8) 0.0471(8) 0.0099(7) 0.0118(6) 0.0059(6) C33 0.0319(7) 0.0478(8) 0.0355(7) -0.0029(6) 0.0054(6) 0.0070(6) C34 0.0271(7) 0.0355(7) 0.0345(7) -0.0041(6) -0.0002(5) 0.0025(5) C35 0.0331(7) 0.0240(6) 0.0290(6) -0.0027(5) -0.0068(5) -0.0029(5) C36 0.0369(8) 0.0287(7) 0.0407(8) -0.0034(6) -0.0096(6) 0.0005(6) C37 0.0505(9) 0.0314(7) 0.0528(9) -0.0033(7) -0.0212(8) 0.0050(7) C38 0.0723(12) 0.0275(7) 0.0424(8) 0.0041(6) -0.0215(8) -0.0064(7) C39 0.0640(11) 0.0322(7) 0.0329(7) 0.0025(6) -0.0056(7) -0.0118(7) C40 0.0427(8) 0.0310(7) 0.0294(7) -0.0008(5) -0.0025(6) -0.0048(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.0601 0 0 1 0.0343 -1 0 -1 0.1700 1 0 1 0.0499 -1 -2 1 0.2087 0 1 0 0.3558 0 -2 1 0.2162 1 -5 -5 0.2057 -3 5 -5 0.3320 1 2 -1 0.3075 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 C42 C41 C46 113.41(14) . . ? C42 C41 B1 127.53(14) . . ? C46 C41 B1 118.32(13) . . ? F1 C42 C41 121.01(14) . . ? F1 C42 C43 115.09(15) . . ? C43 C42 C41 123.87(16) . . ? F2 C43 C42 120.48(18) . . ? F2 C43 C44 119.66(16) . . ? C44 C43 C42 119.85(17) . . ? F3 C44 C43 120.84(18) . . ? F3 C44 C45 120.09(18) . . ? C43 C44 C45 119.06(15) . . ? F4 C45 C44 119.80(15) . . ? F4 C45 C46 120.96(17) . . ? C44 C45 C46 119.25(16) . . ? F5 C46 C41 119.60(13) . . ? F5 C46 C45 115.84(15) . . ? C45 C46 C41 124.54(16) . . ? C48 C47 B1 118.80(13) . . ? C52 C47 C48 113.22(13) . . ? C52 C47 B1 127.10(13) . . ? F6 C48 C47 119.00(13) . . ? F6 C48 C49 116.04(14) . . ? C49 C48 C47 124.94(15) . . ? F7 C49 C48 121.22(16) . . ? F7 C49 C50 119.68(14) . . ? C48 C49 C50 119.10(15) . . ? F8 C50 C49 120.52(15) . . ? F8 C50 C51 120.61(16) . . ? C51 C50 C49 118.86(14) . . ? F9 C51 C50 119.74(14) . . ? F9 C51 C52 120.27(15) . . ? C50 C51 C52 119.99(15) . . ? F10 C52 C47 120.84(13) . . ? F10 C52 C51 115.30(14) . . ? C47 C52 C51 123.85(14) . . ? C54 C53 B1 119.37(12) . . ? C58 C53 C54 113.20(13) . . ? C58 C53 B1 127.10(13) . . ? F11 C54 C53 119.20(13) . . ? F11 C54 C55 115.90(14) . . ? C55 C54 C53 124.90(14) . . ? F12 C55 C54 120.88(15) . . ? F12 C55 C56 119.95(14) . . ? C54 C55 C56 119.17(15) . . ? F13 C56 C55 120.68(16) . . ? F13 C56 C57 120.44(15) . . ? C57 C56 C55 118.88(14) . . ? F14 C57 C56 119.57(14) . . ? F14 C57 C58 120.58(15) . . ? C56 C57 C58 119.85(14) . . ? F15 C58 C53 121.09(13) . . ? F15 C58 C57 114.92(13) . . ? C57 C58 C53 123.98(14) . . ? C60 C59 B1 119.86(12) . . ? C64 C59 C60 113.11(13) . . ? C64 C59 B1 126.28(13) . . ? F16 C60 C59 118.95(13) . . ? F16 C60 C61 116.15(13) . . ? C61 C60 C59 124.89(14) . . ? F17 C61 C60 120.76(15) . . ? F17 C61 C62 120.04(15) . . ? C62 C61 C60 119.19(15) . . ? F18 C62 C61 121.05(15) . . ? F18 C62 C63 120.10(15) . . ? C63 C62 C61 118.84(14) . . ? F19 C63 C62 119.50(14) . . ? F19 C63 C64 120.44(14) . . ? C62 C63 C64 120.05(14) . . ? F20 C64 C59 121.32(13) . . ? F20 C64 C63 114.79(13) . . ? C63 C64 C59 123.88(14) . . ? C47 B1 C41 99.54(11) . . ? C53 B1 C41 113.21(11) . . ? C53 B1 C47 114.88(12) . . ? C59 B1 C41 114.85(12) . . ? C59 B1 C47 113.05(11) . . ? C59 B1 C53 101.95(11) . . ? C1 N1 C2 109.38(12) . . ? C1 N1 C4 132.44(11) . . ? C2 N1 C4 118.01(12) . . ? C1 N2 C3 109.07(12) . . ? C1 N2 C13 132.61(12) . . ? C3 N2 C13 117.01(12) . . ? N1 C1 N2 106.22(11) . . ? N1 C1 C22 128.11(12) . . ? N2 C1 C22 125.01(12) . . ? N1 C2 H2 126.1 . . ? C3 C2 N1 107.79(13) . . ? C3 C2 H2 126.1 . . ? N2 C3 H3 126.2 . . ? C2 C3 N2 107.53(14) . . ? C2 C3 H3 126.2 . . ? C5 C4 N1 118.52(13) . . ? C9 C4 N1 118.59(12) . . ? C9 C4 C5 122.32(13) . . ? C4 C5 C10 122.58(14) . . ? C6 C5 C4 117.69(13) . . ? C6 C5 C10 119.74(13) . . ? C5 C6 H6 119.0 . . ? C5 C6 C7 121.97(13) . . ? C7 C6 H6 119.0 . . ? C6 C7 C11 120.79(14) . . ? C8 C7 C6 118.34(14) . . ? C8 C7 C11 120.80(15) . . ? C7 C8 H8 118.9 . . ? C7 C8 C9 122.18(14) . . ? C9 C8 H8 118.9 . . ? C4 C9 C12 122.83(13) . . ? C8 C9 C4 117.39(13) . . ? C8 C9 C12 119.76(13) . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 N2 121.29(14) . . ? C14 C13 C18 122.06(14) . . ? C18 C13 N2 116.08(13) . . ? C13 C14 C19 124.68(15) . . ? C15 C14 C13 116.90(15) . . ? C15 C14 C19 118.39(15) . . ? C14 C15 H15 118.5 . . ? C16 C15 C14 123.04(16) . . ? C16 C15 H15 118.5 . . ? C15 C16 C17 118.32(15) . . ? C15 C16 C20 120.56(17) . . ? C17 C16 C20 121.09(17) . . ? C16 C17 H17 119.2 . . ? C16 C17 C18 121.56(16) . . ? C18 C17 H17 119.2 . . ? C13 C18 C21 123.23(14) . . ? C17 C18 C13 117.90(15) . . ? C17 C18 C21 118.82(15) . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C1 C22 C23 114.47(11) . . ? C1 C22 C29 108.08(10) . . ? C1 C22 C35 105.88(10) . . ? C29 C22 C23 103.95(10) . . ? C35 C22 C23 110.89(10) . . ? C35 C22 C29 113.77(11) . . ? C24 C23 C22 123.07(12) . . ? C24 C23 C28 117.26(12) . . ? C28 C23 C22 119.25(11) . . ? C23 C24 H24 119.5 . . ? C25 C24 C23 120.99(13) . . ? C25 C24 H24 119.5 . . ? C24 C25 H25 119.5 . . ? C26 C25 C24 120.97(14) . . ? C26 C25 H25 119.5 . . ? C25 C26 H26 120.5 . . ? C25 C26 C27 118.98(14) . . ? C27 C26 H26 120.5 . . ? C26 C27 H27 119.9 . . ? C28 C27 C26 120.21(13) . . ? C28 C27 H27 119.9 . . ? C23 C28 H28 119.2 . . ? C27 C28 C23 121.57(13) . . ? C27 C28 H28 119.2 . . ? C30 C29 C22 123.03(12) . . ? C30 C29 C34 118.22(13) . . ? C34 C29 C22 118.25(12) . . ? C29 C30 H30 119.4 . . ? C29 C30 C31 121.15(14) . . ? C31 C30 H30 119.4 . . ? C30 C31 H31 120.0 . . ? C32 C31 C30 119.97(15) . . ? C32 C31 H31 120.0 . . ? C31 C32 H32 120.2 . . ? C31 C32 C33 119.59(14) . . ? C33 C32 H32 120.2 . . ? C32 C33 H33 119.7 . . ? C34 C33 C32 120.66(14) . . ? C34 C33 H33 119.7 . . ? C29 C34 H34 119.8 . . ? C33 C34 C29 120.39(14) . . ? C33 C34 H34 119.8 . . ? C36 C35 C22 123.60(13) . . ? C36 C35 C40 118.23(13) . . ? C40 C35 C22 118.11(13) . . ? C35 C36 H36 120.0 . . ? C35 C36 C37 120.05(16) . . ? C37 C36 H36 120.0 . . ? C36 C37 H37 119.4 . . ? C38 C37 C36 121.14(16) . . ? C38 C37 H37 119.4 . . ? C37 C38 H38 120.4 . . ? C37 C38 C39 119.17(15) . . ? C39 C38 H38 120.4 . . ? C38 C39 H39 119.9 . . ? C38 C39 C40 120.14(16) . . ? C40 C39 H39 119.9 . . ? C35 C40 H40 119.4 . . ? C39 C40 C35 121.26(16) . . ? C39 C40 H40 119.4 . . ? 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 F1 C42 1.352(2) . ? F2 C43 1.350(2) . ? F3 C44 1.3465(18) . ? F4 C45 1.346(2) . ? F5 C46 1.3476(19) . ? F6 C48 1.3552(18) . ? F7 C49 1.3447(19) . ? F8 C50 1.3432(18) . ? F9 C51 1.3482(19) . ? F10 C52 1.3494(17) . ? F11 C54 1.3505(17) . ? F12 C55 1.3462(19) . ? F13 C56 1.3415(18) . ? F14 C57 1.3451(18) . ? F15 C58 1.3500(17) . ? F16 C60 1.3526(17) . ? F17 C61 1.3444(19) . ? F18 C62 1.3466(18) . ? F19 C63 1.3489(17) . ? F20 C64 1.3539(17) . ? C41 C42 1.388(2) . ? C41 C46 1.394(2) . ? C41 B1 1.660(2) . ? C42 C43 1.385(2) . ? C43 C44 1.373(3) . ? C44 C45 1.377(3) . ? C45 C46 1.379(2) . ? C47 C48 1.396(2) . ? C47 C52 1.385(2) . ? C47 B1 1.656(2) . ? C48 C49 1.373(2) . ? C49 C50 1.380(3) . ? C50 C51 1.374(2) . ? C51 C52 1.386(2) . ? C53 C54 1.393(2) . ? C53 C58 1.388(2) . ? C53 B1 1.654(2) . ? C54 C55 1.377(2) . ? C55 C56 1.379(2) . ? C56 C57 1.375(2) . ? C57 C58 1.386(2) . ? C59 C60 1.395(2) . ? C59 C64 1.388(2) . ? C59 B1 1.653(2) . ? C60 C61 1.377(2) . ? C61 C62 1.376(2) . ? C62 C63 1.374(2) . ? C63 C64 1.385(2) . ? N1 C1 1.3516(18) . ? N1 C2 1.3807(19) . ? N1 C4 1.4616(18) . ? N2 C1 1.3702(18) . ? N2 C3 1.3781(19) . ? N2 C13 1.4693(19) . ? C1 C22 1.5384(17) . ? C2 H2 0.9500 . ? C2 C3 1.340(2) . ? C3 H3 0.9500 . ? C4 C5 1.3978(19) . ? C4 C9 1.395(2) . ? C5 C6 1.387(2) . ? C5 C10 1.504(2) . ? C6 H6 0.9500 . ? C6 C7 1.392(2) . ? C7 C8 1.386(2) . ? C7 C11 1.505(2) . ? C8 H8 0.9500 . ? C8 C9 1.392(2) . ? C9 C12 1.5077(19) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.400(2) . ? C13 C18 1.403(2) . ? C14 C15 1.393(2) . ? C14 C19 1.496(2) . ? C15 H15 0.9500 . ? C15 C16 1.382(3) . ? C16 C17 1.391(2) . ? C16 C20 1.511(2) . ? C17 H17 0.9500 . ? C17 C18 1.396(2) . ? C18 C21 1.509(2) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.5701(18) . ? C22 C29 1.5480(18) . ? C22 C35 1.5450(18) . ? C23 C24 1.3900(19) . ? C23 C28 1.4004(19) . ? C24 H24 0.9500 . ? C24 C25 1.389(2) . ? C25 H25 0.9500 . ? C25 C26 1.376(2) . ? C26 H26 0.9500 . ? C26 C27 1.384(2) . ? C27 H27 0.9500 . ? C27 C28 1.384(2) . ? C28 H28 0.9500 . ? C29 C30 1.386(2) . ? C29 C34 1.4017(19) . ? C30 H30 0.9500 . ? C30 C31 1.395(2) . ? C31 H31 0.9500 . ? C31 C32 1.375(2) . ? C32 H32 0.9500 . ? C32 C33 1.387(2) . ? C33 H33 0.9500 . ? C33 C34 1.383(2) . ? C34 H34 0.9500 . ? C35 C36 1.388(2) . ? C35 C40 1.395(2) . ? C36 H36 0.9500 . ? C36 C37 1.397(2) . ? C37 H37 0.9500 . ? C37 C38 1.376(3) . ? C38 H38 0.9500 . ? C38 C39 1.380(3) . ? C39 H39 0.9500 . ? C39 C40 1.386(2) . ? C40 H40 0.9500 . ? 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 F1 C42 C43 F2 2.1(2) . . . . ? F1 C42 C43 C44 -176.77(15) . . . . ? F2 C43 C44 F3 -0.8(3) . . . . ? F2 C43 C44 C45 -179.95(16) . . . . ? F3 C44 C45 F4 0.5(2) . . . . ? F3 C44 C45 C46 -178.98(15) . . . . ? F4 C45 C46 F5 0.0(2) . . . . ? F4 C45 C46 C41 -178.72(14) . . . . ? F6 C48 C49 F7 -0.9(2) . . . . ? F6 C48 C49 C50 178.06(14) . . . . ? F7 C49 C50 F8 0.6(3) . . . . ? F7 C49 C50 C51 -179.76(15) . . . . ? F8 C50 C51 F9 0.1(2) . . . . ? F8 C50 C51 C52 179.45(15) . . . . ? F9 C51 C52 F10 -1.1(2) . . . . ? F9 C51 C52 C47 177.92(14) . . . . ? F11 C54 C55 F12 0.4(2) . . . . ? F11 C54 C55 C56 -179.50(14) . . . . ? F12 C55 C56 F13 -0.1(3) . . . . ? F12 C55 C56 C57 -179.60(15) . . . . ? F13 C56 C57 F14 1.0(2) . . . . ? F13 C56 C57 C58 -179.29(14) . . . . ? F14 C57 C58 F15 -2.4(2) . . . . ? F14 C57 C58 C53 178.49(14) . . . . ? F16 C60 C61 F17 1.7(2) . . . . ? F16 C60 C61 C62 -177.40(14) . . . . ? F17 C61 C62 F18 -0.8(2) . . . . ? F17 C61 C62 C63 -179.54(14) . . . . ? F18 C62 C63 F19 -0.8(2) . . . . ? F18 C62 C63 C64 -179.92(14) . . . . ? F19 C63 C64 F20 1.1(2) . . . . ? F19 C63 C64 C59 -177.80(13) . . . . ? C41 C42 C43 F2 -179.83(15) . . . . ? C41 C42 C43 C44 1.3(3) . . . . ? C42 C41 C46 F5 -179.16(13) . . . . ? C42 C41 C46 C45 -0.5(2) . . . . ? C42 C41 B1 C47 106.74(16) . . . . ? C42 C41 B1 C53 -130.83(15) . . . . ? C42 C41 B1 C59 -14.3(2) . . . . ? C42 C43 C44 F3 178.01(16) . . . . ? C42 C43 C44 C45 -1.1(3) . . . . ? C43 C44 C45 F4 179.59(15) . . . . ? C43 C44 C45 C46 0.1(2) . . . . ? C44 C45 C46 F5 179.40(14) . . . . ? C44 C45 C46 C41 0.7(2) . . . . ? C46 C41 C42 F1 177.49(13) . . . . ? C46 C41 C42 C43 -0.5(2) . . . . ? C46 C41 B1 C47 -62.71(15) . . . . ? C46 C41 B1 C53 59.72(17) . . . . ? C46 C41 B1 C59 176.27(12) . . . . ? C47 C48 C49 F7 -179.94(15) . . . . ? C47 C48 C49 C50 -1.0(3) . . . . ? C48 C47 C52 F10 -179.43(12) . . . . ? C48 C47 C52 C51 1.6(2) . . . . ? C48 C47 B1 C41 -62.77(15) . . . . ? C48 C47 B1 C53 176.00(12) . . . . ? C48 C47 B1 C59 59.55(16) . . . . ? C48 C49 C50 F8 -178.34(15) . . . . ? C48 C49 C50 C51 1.3(2) . . . . ? C49 C50 C51 F9 -179.47(15) . . . . ? C49 C50 C51 C52 -0.2(2) . . . . ? C50 C51 C52 F10 179.61(14) . . . . ? C50 C51 C52 C47 -1.4(2) . . . . ? C52 C47 C48 F6 -179.45(13) . . . . ? C52 C47 C48 C49 -0.4(2) . . . . ? C52 C47 B1 C41 105.74(15) . . . . ? C52 C47 B1 C53 -15.5(2) . . . . ? C52 C47 B1 C59 -131.94(14) . . . . ? C53 C54 C55 F12 -179.80(15) . . . . ? C53 C54 C55 C56 0.4(3) . . . . ? C54 C53 C58 F15 -177.31(13) . . . . ? C54 C53 C58 C57 1.7(2) . . . . ? C54 C53 B1 C41 -172.94(13) . . . . ? C54 C53 B1 C47 -59.51(18) . . . . ? C54 C53 B1 C59 63.13(16) . . . . ? C54 C55 C56 F13 179.71(15) . . . . ? C54 C55 C56 C57 0.3(3) . . . . ? C55 C56 C57 F14 -179.57(15) . . . . ? C55 C56 C57 C58 0.2(2) . . . . ? C56 C57 C58 F15 177.83(14) . . . . ? C56 C57 C58 C53 -1.3(2) . . . . ? C58 C53 C54 F11 178.57(13) . . . . ? C58 C53 C54 C55 -1.3(2) . . . . ? C58 C53 B1 C41 14.1(2) . . . . ? C58 C53 B1 C47 127.55(15) . . . . ? C58 C53 B1 C59 -109.81(15) . . . . ? C59 C60 C61 F17 -178.89(14) . . . . ? C59 C60 C61 C62 2.0(2) . . . . ? C60 C59 C64 F20 -178.68(12) . . . . ? C60 C59 C64 C63 0.1(2) . . . . ? C60 C59 B1 C41 -57.27(17) . . . . ? C60 C59 B1 C47 -170.58(12) . . . . ? C60 C59 B1 C53 65.55(15) . . . . ? C60 C61 C62 F18 178.39(14) . . . . ? C60 C61 C62 C63 -0.4(2) . . . . ? C61 C62 C63 F19 177.96(14) . . . . ? C61 C62 C63 C64 -1.1(2) . . . . ? C62 C63 C64 F20 -179.83(13) . . . . ? C62 C63 C64 C59 1.3(2) . . . . ? C64 C59 C60 F16 177.56(12) . . . . ? C64 C59 C60 C61 -1.8(2) . . . . ? C64 C59 B1 C41 133.37(14) . . . . ? C64 C59 B1 C47 20.1(2) . . . . ? C64 C59 B1 C53 -103.81(15) . . . . ? B1 C41 C42 F1 7.6(2) . . . . ? B1 C41 C42 C43 -170.39(15) . . . . ? B1 C41 C46 F5 -8.3(2) . . . . ? B1 C41 C46 C45 170.37(14) . . . . ? B1 C47 C48 F6 -9.4(2) . . . . ? B1 C47 C48 C49 169.61(15) . . . . ? B1 C47 C52 F10 11.5(2) . . . . ? B1 C47 C52 C51 -167.43(14) . . . . ? B1 C53 C54 F11 4.7(2) . . . . ? B1 C53 C54 C55 -175.15(15) . . . . ? B1 C53 C58 F15 -4.0(2) . . . . ? B1 C53 C58 C57 175.02(14) . . . . ? B1 C59 C60 F16 6.9(2) . . . . ? B1 C59 C60 C61 -172.47(14) . . . . ? B1 C59 C64 F20 -8.7(2) . . . . ? B1 C59 C64 C63 170.11(14) . . . . ? N1 C1 C22 C23 -23.97(19) . . . . ? N1 C1 C22 C29 91.32(16) . . . . ? N1 C1 C22 C35 -146.43(13) . . . . ? N1 C2 C3 N2 -0.5(2) . . . . ? N1 C4 C5 C6 -174.33(12) . . . . ? N1 C4 C5 C10 5.6(2) . . . . ? N1 C4 C9 C8 175.44(12) . . . . ? N1 C4 C9 C12 -2.9(2) . . . . ? N2 C1 C22 C23 166.70(12) . . . . ? N2 C1 C22 C29 -78.02(16) . . . . ? N2 C1 C22 C35 44.24(17) . . . . ? N2 C13 C14 C15 176.29(13) . . . . ? N2 C13 C14 C19 -1.9(2) . . . . ? N2 C13 C18 C17 -176.77(13) . . . . ? N2 C13 C18 C21 0.6(2) . . . . ? C1 N1 C2 C3 -0.29(19) . . . . ? C1 N1 C4 C5 -109.16(17) . . . . ? C1 N1 C4 C9 79.27(19) . . . . ? C1 N2 C3 C2 1.04(19) . . . . ? C1 N2 C13 C14 93.90(19) . . . . ? C1 N2 C13 C18 -94.64(19) . . . . ? C1 C22 C23 C24 -106.79(15) . . . . ? C1 C22 C23 C28 80.89(15) . . . . ? C1 C22 C29 C30 -8.60(18) . . . . ? C1 C22 C29 C34 179.66(12) . . . . ? C1 C22 C35 C36 -119.41(14) . . . . ? C1 C22 C35 C40 57.78(15) . . . . ? C2 N1 C1 N2 0.91(16) . . . . ? C2 N1 C1 C22 -170.00(14) . . . . ? C2 N1 C4 C5 76.20(17) . . . . ? C2 N1 C4 C9 -95.36(16) . . . . ? C3 N2 C1 N1 -1.20(16) . . . . ? C3 N2 C1 C22 170.08(13) . . . . ? C3 N2 C13 C14 -100.83(17) . . . . ? C3 N2 C13 C18 70.63(18) . . . . ? C4 N1 C1 N2 -174.07(14) . . . . ? C4 N1 C1 C22 15.0(2) . . . . ? C4 N1 C2 C3 175.52(14) . . . . ? C4 C5 C6 C7 0.6(2) . . . . ? C5 C4 C9 C8 4.2(2) . . . . ? C5 C4 C9 C12 -174.17(13) . . . . ? C5 C6 C7 C8 0.5(2) . . . . ? C5 C6 C7 C11 177.44(15) . . . . ? C6 C7 C8 C9 0.7(2) . . . . ? C7 C8 C9 C4 -3.0(2) . . . . ? C7 C8 C9 C12 175.46(14) . . . . ? C9 C4 C5 C6 -3.1(2) . . . . ? C9 C4 C5 C10 176.79(14) . . . . ? C10 C5 C6 C7 -179.24(14) . . . . ? C11 C7 C8 C9 -176.23(14) . . . . ? C13 N2 C1 N1 164.93(15) . . . . ? C13 N2 C1 C22 -23.8(2) . . . . ? C13 N2 C3 C2 -167.54(15) . . . . ? C13 C14 C15 C16 -1.8(2) . . . . ? C14 C13 C18 C17 -5.4(2) . . . . ? C14 C13 C18 C21 172.02(14) . . . . ? C14 C15 C16 C17 -1.6(2) . . . . ? C14 C15 C16 C20 -179.75(16) . . . . ? C15 C16 C17 C18 1.5(2) . . . . ? C16 C17 C18 C13 1.8(2) . . . . ? C16 C17 C18 C21 -175.71(15) . . . . ? C18 C13 C14 C15 5.3(2) . . . . ? C18 C13 C14 C19 -172.83(15) . . . . ? C19 C14 C15 C16 176.50(16) . . . . ? C20 C16 C17 C18 179.72(16) . . . . ? C22 C23 C24 C25 -172.93(13) . . . . ? C22 C23 C28 C27 173.48(12) . . . . ? C22 C29 C30 C31 -172.78(13) . . . . ? C22 C29 C34 C33 173.72(13) . . . . ? C22 C35 C36 C37 177.60(13) . . . . ? C22 C35 C40 C39 -177.42(13) . . . . ? C23 C22 C29 C30 113.41(14) . . . . ? C23 C22 C29 C34 -58.34(15) . . . . ? C23 C22 C35 C36 115.87(14) . . . . ? C23 C22 C35 C40 -66.93(15) . . . . ? C23 C24 C25 C26 0.7(2) . . . . ? C24 C23 C28 C27 0.7(2) . . . . ? C24 C25 C26 C27 -1.1(2) . . . . ? C25 C26 C27 C28 1.4(2) . . . . ? C26 C27 C28 C23 -1.2(2) . . . . ? C28 C23 C24 C25 -0.5(2) . . . . ? C29 C22 C23 C24 135.55(13) . . . . ? C29 C22 C23 C28 -36.77(15) . . . . ? C29 C22 C35 C36 -0.87(18) . . . . ? C29 C22 C35 C40 176.32(12) . . . . ? C29 C30 C31 C32 0.1(2) . . . . ? C30 C29 C34 C33 1.6(2) . . . . ? C30 C31 C32 C33 0.4(2) . . . . ? C31 C32 C33 C34 0.2(2) . . . . ? C32 C33 C34 C29 -1.2(2) . . . . ? C34 C29 C30 C31 -1.0(2) . . . . ? C35 C22 C23 C24 12.91(18) . . . . ? C35 C22 C23 C28 -159.41(12) . . . . ? C35 C22 C29 C30 -125.87(14) . . . . ? C35 C22 C29 C34 62.39(16) . . . . ? C35 C36 C37 C38 -0.3(2) . . . . ? C36 C35 C40 C39 -0.1(2) . . . . ? C36 C37 C38 C39 -0.2(2) . . . . ? C37 C38 C39 C40 0.5(2) . . . . ? C38 C39 C40 C35 -0.4(2) . . . . ? C40 C35 C36 C37 0.4(2) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -0.0009 -0.0092 -0.9996 -0.0362 -0.0213 -0.0139 0.0009 0.0092 0.9996 0.0362 0.0213 0.0139 -0.9991 -0.0325 -0.9943 -0.0747 0.0534 -0.0280 0.9991 0.0325 0.9943 0.0747 -0.0534 0.0280 -0.9463 -2.0236 1.0788 -0.0628 0.0950 0.1603 -0.0254 1.0048 -0.0370 0.0303 0.0005 -0.0802 0.0518 -2.0003 1.0736 -0.0243 0.0203 0.1744 1.1207 -5.0466 -4.8178 -0.2941 -0.1839 0.3460 -3.1264 4.9077 -5.1673 -0.1452 0.1203 -0.5130 0.9463 2.0236 -1.0788 0.0628 -0.0950 -0.1603 loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 0.000 0.000 263.4 67.1 '1 toluene' 2 0.000 0.500 0.500 263.4 67.1 '1 toluene' 3 0.500 0.500 0.000 263.4 67.1 '1 toluene' 4 0.500 1.000 0.500 263.4 67.1 '1 toluene'