#------------------------------------------------------------------------------ #$Date: 2019-12-13 03:54:03 +0200 (Fri, 13 Dec 2019) $ #$Revision: 245034 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/65/1556534.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_1556534 loop_ _publ_author_name 'Khorloo, Michidmaa' 'Cheng, Yanhua' 'Zhang, Haoke' 'Chen, Ming' 'Sung, Herman H. Y.' 'Williams, Ian D.' 'Lam, Jacky W. Y.' 'Tang, Ben Zhong' _publ_section_title ; Polymorph selectivity of an AIE luminogen under nano-confinement to visualize polymer microstructures ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/C9SC04239C _journal_year 2020 _chemical_formula_moiety 'C H2 Cl2, 2(F6 P), 2(C34 H28 N)' _chemical_formula_sum 'C69 H58 Cl2 F12 N2 P2' _chemical_formula_weight 1276.01 _chemical_name_common TPE-Py _chemical_name_systematic TPE-EP-G _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2018-11-07 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2019-05-22 deposited with the CCDC. 2019-12-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.8053(14) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.2525(2) _cell_length_b 9.21940(13) _cell_length_c 59.1397(9) _cell_measurement_reflns_used 11185 _cell_measurement_temperature 100.03(11) _cell_measurement_theta_max 73.0670 _cell_measurement_theta_min 4.0480 _cell_volume 6121.70(17) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _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 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.03(11) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.3577 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.995 _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 29.00 105.50 0.75 25.00 -- 106.99 -77.00 -90.00 102 2 \w -117.00 -15.00 0.75 10.00 -- -40.57 -37.00 0.00 136 3 \w -69.00 32.25 0.75 10.00 -- -40.57 57.00 150.00 135 4 \w -92.00 -2.00 0.75 10.00 -- -40.57 125.00-150.00 120 5 \w 65.00 116.00 0.75 25.00 -- 106.99-125.00 -90.00 68 6 \w 38.00 115.25 0.75 25.00 -- 106.99-125.00 60.00 103 7 \w 46.00 164.50 0.75 25.00 -- 106.99 15.00 30.00 158 8 \w 33.00 134.25 0.75 25.00 -- 106.99 -45.00 0.00 135 9 \w 32.00 116.00 0.75 25.00 -- 106.99-125.00-180.00 112 10 \w 32.00 130.25 0.75 25.00 -- 106.99 -45.00 120.00 131 11 \w 109.00 178.00 0.75 25.00 -- 106.99 45.00 60.00 92 ; _diffrn_measurement_device 'kappa diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.1136970000 _diffrn_orient_matrix_UB_12 0.0206380000 _diffrn_orient_matrix_UB_13 -0.0156822000 _diffrn_orient_matrix_UB_21 0.0009888000 _diffrn_orient_matrix_UB_22 -0.1626067000 _diffrn_orient_matrix_UB_23 -0.0059458000 _diffrn_orient_matrix_UB_31 -0.0768846000 _diffrn_orient_matrix_UB_32 -0.0322975000 _diffrn_orient_matrix_UB_33 0.0200047000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_unetI/netI 0.0423 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 70 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_number 32777 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 66.500 _diffrn_reflns_theta_max 67.498 _diffrn_reflns_theta_min 3.959 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_current 0.80 _diffrn_source_power 0.040 _diffrn_source_target Cu _diffrn_source_type 'SuperNova (Cu) X-ray Source' _diffrn_source_voltage 50 _exptl_absorpt_coefficient_mu 2.143 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.72507 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.384 _exptl_crystal_description needle _exptl_crystal_F_000 2632 _exptl_crystal_preparation Luminescent _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.949 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.061 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 849 _refine_ls_number_reflns 10976 _refine_ls_number_restraints 86 _refine_ls_restrained_S_all 1.034 _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0623 _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^)+(0.0660P)^2^+8.2250P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1501 _refine_ls_wR_factor_ref 0.1577 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9143 _reflns_number_total 10976 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc04239c2.cif _cod_data_source_block khor3cult _cod_original_cell_volume 6121.68(17) _cod_database_code 1556534 _shelx_shelxl_version_number 2014/7 _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 0.958 _shelx_estimated_absorpt_t_min 0.674 _reflns_odcompleteness_completeness 99.81 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C3B-C2B \\sim C4B-C3B \\sim C5B-C4B \\sim C6B-C5B with sigma of 0.02 C3A-C2A \\sim C4A-C3A \\sim C5A-C4A \\sim C6A-C5A with sigma of 0.02 N1A-C2B \\sim N1A-C6B with sigma of 0.02 N1A-C6A \\sim N1A-C2A with sigma of 0.02 3. Rigid body (RIGU) restrains N1A, C2B, C3B, C4B, C5B, C6B with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 N1A, C2A, C3A, C4A, C5A, C6A with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 4. Others Fixed Sof: C2A(0.75) H2A(0.75) C2B(0.25) H2B(0.25) C3A(0.75) H3A(0.75) C3B(0.25) H3B(0.25) C4A(0.75) C4B(0.25) C5A(0.75) H5A(0.75) C5B(0.25) H5B(0.25) C6A(0.75) H6A(0.75) C6B(0.25) H6B(0.25) C7A(0.75) H7A(0.75) C7B(0.25) H7B(0.25) C8A(0.75) H8A(0.75) C8B(0.25) H8B(0.25) 5.a Secondary CH2 refined with riding coordinates: C1S(H1SA,H1SB) 5.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C15(H15), C16(H16), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C2A(H2A), C2B(H2B), C3A(H3A), C3B(H3B), C5A(H5A), C5B(H5B), C6A(H6A), C6B(H6B), C7A(H7A), C7B(H7B), C8A(H8A), C8B(H8B), C12A(H12A), C13A(H13A), C15A(H15A), C16A(H16A), C22A(H22A), C23A(H23A), C24A(H24A), C25A(H25A), C26A(H26A), C32A(H32A), C33A(H33A), C34A(H34A), C35A(H35A), C36A(H36A), C42A(H42A), C43A(H43A), C44A(H44A), C45A(H45A), C46A(H46A) 5.c Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C1A(H1AA,H1AB,H1AC) ; _shelx_res_file ; khor3cult.res created by SHELXL-2014/7 TITL khor3CuLT in P21/n #14 REM reset to P21/n #14 CELL 1.54184 11.252458 9.219397 59.13975 90 93.8053 90 ZERR 4 0.000203 0.000135 0.000913 0 0.0014 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Cl F N P UNIT 276 232 8 48 8 8 SADI C3B C2B C4B C3B C5B C4B C6B C5B SADI C3A C2A C4A C3A C5A C4A C6A C5A SADI N1A C2B N1A C6B SADI N1A C6A N1A C2A RIGU 0.001 0.001 N1A C2B C3B C4B C5B C6B RIGU 0.001 0.001 N1A C2A C3A C4A C5A C6A L.S. 10 PLAN 20 SIZE 0.02 0.02 0.2 TEMP -173 CONF BOND fmap 2 acta 133 OMIT 0 135 OMIT -2 0 8 OMIT -4 2 5 OMIT 1 0 21 OMIT 2 1 11 OMIT -7 2 61 OMIT 3 2 3 OMIT -5 1 2 OMIT -4 0 4 OMIT 1 8 5 OMIT 6 9 7 OMIT 2 0 28 OMIT -8 1 58 OMIT -2 2 2 OMIT 2 1 15 OMIT -8 2 56 OMIT 2 3 8 OMIT 2 3 16 OMIT -3 3 18 OMIT 0 0 30 OMIT -6 1 8 OMIT -6 1 11 OMIT 1 2 20 OMIT -3 2 2 OMIT 2 0 2 OMIT -4 1 3 OMIT 0 3 2 OMIT -5 0 7 OMIT 3 2 13 OMIT -1 4 22 REM REM REM WGHT 0.066000 8.225000 FVAR 2.67257 CL1 3 0.884124 0.426757 0.152366 11.00000 0.07165 0.04375 = 0.04889 0.00853 0.01739 0.00159 CL2 3 0.804609 0.135768 0.161695 11.00000 0.05605 0.06065 = 0.04859 0.01764 -0.00167 -0.01069 C1S 1 0.927087 0.255452 0.164017 11.00000 0.04086 0.04425 = 0.04175 0.00160 0.00550 0.00457 AFIX 23 H1SA 2 0.993471 0.215141 0.155805 11.00000 -1.20000 H1SB 2 0.954904 0.267056 0.180150 11.00000 -1.20000 AFIX 0 P1 6 0.186540 0.970032 0.194988 11.00000 0.02986 0.03226 = 0.02634 0.00353 0.00885 0.00252 F1 4 0.127254 0.948740 0.218627 11.00000 0.05604 0.05620 = 0.03936 0.00868 0.02667 0.00738 F2 4 0.247038 0.991545 0.171668 11.00000 0.05883 0.05816 = 0.03245 0.01541 0.01985 0.01390 F3 4 0.155914 1.137366 0.195546 11.00000 0.12315 0.04504 = 0.06518 0.00928 0.03188 0.02233 F4 4 0.307858 1.001676 0.208706 11.00000 0.04206 0.14890 = 0.05057 0.01332 -0.00024 -0.01109 F5 4 0.218463 0.804226 0.194685 11.00000 0.20045 0.04009 = 0.04108 0.00981 0.04573 0.02981 F6 4 0.064795 0.941926 0.181312 11.00000 0.05717 0.16431 = 0.06412 0.02846 -0.01021 -0.05058 P1A 6 0.907508 0.464778 0.227439 11.00000 0.04001 0.04365 = 0.03813 0.00572 0.01335 0.00770 F1A 4 0.846625 0.365172 0.245531 11.00000 0.06104 0.04364 = 0.04155 0.00462 0.01719 0.00176 F2A 4 0.970508 0.563693 0.209643 11.00000 0.06562 0.06901 = 0.07732 0.02776 0.04286 0.01783 F3A 4 0.833576 0.600757 0.235529 11.00000 0.09688 0.04732 = 0.09631 0.02188 0.06332 0.02501 F4A 4 1.011136 0.501918 0.246274 11.00000 0.07075 0.09257 = 0.06746 -0.01606 0.00215 -0.02125 F5A 4 0.984125 0.330961 0.219718 11.00000 0.05478 0.05517 = 0.05706 0.00148 0.01522 0.01857 F6A 4 0.805384 0.427241 0.208905 11.00000 0.04256 0.13281 = 0.04786 0.00913 0.00307 0.01046 N1 5 0.775518 0.943625 0.210732 11.00000 0.02577 0.03807 = 0.02541 -0.00338 0.00539 -0.00618 C1 1 0.854485 1.013905 0.228423 11.00000 0.03229 0.05717 = 0.03894 -0.01590 0.00067 -0.01300 AFIX 137 H1A 2 0.813266 1.096802 0.234711 11.00000 -1.50000 H1B 2 0.927083 1.047551 0.221782 11.00000 -1.50000 H1C 2 0.875514 0.944003 0.240517 11.00000 -1.50000 AFIX 0 C2 1 0.820617 0.838506 0.198036 11.00000 0.02486 0.03908 = 0.03014 -0.00003 0.00420 -0.00209 AFIX 43 H2 2 0.901540 0.810305 0.200696 11.00000 -1.20000 AFIX 0 C3 1 0.750221 0.771781 0.181251 11.00000 0.03167 0.03244 = 0.03167 -0.00352 0.00588 0.00132 AFIX 43 H3 2 0.782951 0.697685 0.172390 11.00000 -1.20000 AFIX 0 C4 1 0.630839 0.811761 0.177061 11.00000 0.02889 0.02650 = 0.02174 0.00082 0.00540 -0.00492 C5 1 0.587228 0.920873 0.190785 11.00000 0.02597 0.03252 = 0.02833 -0.00330 0.00324 -0.00190 AFIX 43 H5 2 0.506448 0.950672 0.188639 11.00000 -1.20000 AFIX 0 C6 1 0.660868 0.984686 0.207297 11.00000 0.03310 0.03689 = 0.02810 -0.00630 0.00705 -0.00259 AFIX 43 H6 2 0.630597 1.058961 0.216451 11.00000 -1.20000 AFIX 0 C7 1 0.557480 0.739124 0.159266 11.00000 0.03268 0.02736 = 0.02170 -0.00170 0.00544 -0.00017 AFIX 43 H7 2 0.597064 0.689358 0.147876 11.00000 -1.20000 AFIX 0 C8 1 0.439053 0.737523 0.157831 11.00000 0.03196 0.02291 = 0.02091 -0.00085 0.00397 -0.00150 AFIX 43 H8 2 0.400068 0.787172 0.169312 11.00000 -1.20000 AFIX 0 C10 1 0.136721 0.446198 0.089505 11.00000 0.02670 0.02662 = 0.02414 -0.00271 0.00400 0.00061 C11 1 0.215083 0.525814 0.106727 11.00000 0.02984 0.02401 = 0.02257 0.00055 0.00180 -0.00070 C12 1 0.171547 0.568710 0.127220 11.00000 0.02961 0.03419 = 0.02748 -0.00327 0.00487 -0.00502 AFIX 43 H12 2 0.091126 0.548627 0.130094 11.00000 -1.20000 AFIX 0 C13 1 0.244213 0.640311 0.143449 11.00000 0.03215 0.03325 = 0.02074 -0.00259 0.00706 -0.00304 AFIX 43 H13 2 0.212098 0.672369 0.157040 11.00000 -1.20000 AFIX 0 C14 1 0.363659 0.665806 0.140075 11.00000 0.03247 0.02204 = 0.01942 -0.00039 0.00288 -0.00008 C15 1 0.407832 0.621649 0.119538 11.00000 0.02967 0.02408 = 0.02418 0.00017 0.00420 -0.00101 AFIX 43 H15 2 0.489027 0.638478 0.116883 11.00000 -1.20000 AFIX 0 C16 1 0.334513 0.554105 0.103188 11.00000 0.03533 0.02714 = 0.01851 -0.00186 0.00453 0.00219 AFIX 43 H16 2 0.365594 0.526294 0.089283 11.00000 -1.20000 AFIX 0 C20 1 0.116567 0.494564 0.067959 11.00000 0.02745 0.02455 = 0.02632 -0.00036 0.00292 0.00237 C21 1 0.158882 0.640280 0.060607 11.00000 0.02979 0.02755 = 0.02623 0.00182 -0.00172 0.00104 C22 1 0.144473 0.764601 0.073410 11.00000 0.05235 0.02788 = 0.02867 0.00117 0.00633 0.00482 AFIX 43 H22 2 0.102620 0.759266 0.086818 11.00000 -1.20000 AFIX 0 C23 1 0.190571 0.896582 0.066827 11.00000 0.06762 0.02689 = 0.04029 -0.00478 0.00241 0.00156 AFIX 43 H23 2 0.181029 0.980462 0.075859 11.00000 -1.20000 AFIX 0 C24 1 0.250411 0.906575 0.047154 11.00000 0.05276 0.02913 = 0.04203 0.00514 -0.00031 -0.00576 AFIX 43 H24 2 0.283203 0.996528 0.042810 11.00000 -1.20000 AFIX 0 C25 1 0.262018 0.784263 0.033870 11.00000 0.03371 0.03376 = 0.03063 0.00519 -0.00008 -0.00097 AFIX 43 H25 2 0.301841 0.790478 0.020233 11.00000 -1.20000 AFIX 0 C26 1 0.215669 0.653171 0.040453 11.00000 0.02921 0.02801 = 0.02577 0.00118 -0.00349 0.00147 AFIX 43 H26 2 0.222639 0.570358 0.031074 11.00000 -1.20000 AFIX 0 C31 1 0.087491 0.307901 0.097968 11.00000 0.02944 0.02863 = 0.01814 -0.00200 0.00426 0.00074 C32 1 0.161210 0.217548 0.111860 11.00000 0.03239 0.03170 = 0.02767 -0.00035 -0.00054 -0.00290 AFIX 43 H32 2 0.240652 0.246566 0.116042 11.00000 -1.20000 AFIX 0 C33 1 0.119108 0.085691 0.119587 11.00000 0.04564 0.03307 = 0.03005 0.00602 -0.00070 0.00287 AFIX 43 H33 2 0.170445 0.024261 0.128682 11.00000 -1.20000 AFIX 0 C34 1 0.002037 0.043720 0.114018 11.00000 0.04057 0.03277 = 0.03313 0.00310 0.00761 -0.00821 AFIX 43 H34 2 -0.027002 -0.046013 0.119304 11.00000 -1.20000 AFIX 0 C35 1 -0.071605 0.133983 0.100707 11.00000 0.03055 0.03828 = 0.02869 0.00018 0.00792 -0.00476 AFIX 43 H35 2 -0.151841 0.106296 0.096978 11.00000 -1.20000 AFIX 0 C36 1 -0.029609 0.264302 0.092757 11.00000 0.02786 0.03138 = 0.02313 -0.00170 0.00523 0.00281 AFIX 43 H36 2 -0.081450 0.324854 0.083613 11.00000 -1.20000 AFIX 0 C41 1 0.055527 0.403566 0.049758 11.00000 0.02546 0.03022 = 0.02213 0.00251 0.00341 -0.00359 C42 1 0.087164 0.259486 0.046707 11.00000 0.02862 0.03324 = 0.02207 0.00067 0.00440 -0.00270 AFIX 43 H42 2 0.149717 0.218456 0.056220 11.00000 -1.20000 AFIX 0 C43 1 0.029418 0.174589 0.030098 11.00000 0.03144 0.03947 = 0.02785 -0.00845 0.00936 -0.00795 AFIX 43 H43 2 0.051014 0.075657 0.028535 11.00000 -1.20000 AFIX 0 C44 1 -0.059746 0.234029 0.015789 11.00000 0.03314 0.05301 = 0.02457 -0.00662 0.00581 -0.01480 AFIX 43 H44 2 -0.100376 0.176096 0.004460 11.00000 -1.20000 AFIX 0 C45 1 -0.089179 0.378227 0.018111 11.00000 0.02945 0.05739 = 0.02647 0.00923 -0.00139 -0.00768 AFIX 43 H45 2 -0.148749 0.420156 0.008009 11.00000 -1.20000 AFIX 0 C46 1 -0.032957 0.462718 0.034992 11.00000 0.03007 0.03885 = 0.03162 0.00741 -0.00039 -0.00271 AFIX 43 H46 2 -0.054944 0.561565 0.036493 11.00000 -1.20000 AFIX 0 N1A 5 0.341852 0.603733 0.228527 11.00000 0.03543 0.02657 = 0.02270 0.00144 0.00229 0.00075 C1A 1 0.291812 0.695263 0.246058 11.00000 0.06957 0.04252 = 0.02317 -0.00581 0.01021 0.01280 AFIX 137 H1AA 2 0.349766 0.703660 0.259111 11.00000 -1.50000 H1AB 2 0.218463 0.650942 0.250871 11.00000 -1.50000 H1AC 2 0.274006 0.791919 0.239822 11.00000 -1.50000 AFIX 0 PART 1 C2A 1 0.457583 0.616448 0.225503 10.75000 0.03454 0.02083 = 0.02227 0.00072 0.00097 0.00024 AFIX 43 H2A 2 0.505224 0.679486 0.235030 10.75000 -1.20000 AFIX 0 PART 0 PART 2 C2B 1 0.457952 0.591152 0.221290 10.25000 0.03646 0.03636 = 0.03302 -0.00841 0.00517 -0.00286 AFIX 43 H2B 2 0.520275 0.648252 0.228306 10.25000 -1.20000 AFIX 0 PART 0 PART 1 C3A 1 0.509133 0.539712 0.208802 10.75000 0.02966 0.02209 = 0.02367 -0.00019 0.00087 -0.00242 AFIX 43 H3A 2 0.592344 0.547854 0.207232 10.75000 -1.20000 AFIX 0 PART 0 PART 2 C3B 1 0.482070 0.497314 0.204212 10.25000 0.03643 0.03497 = 0.03292 -0.00798 0.00729 -0.00500 AFIX 43 H3B 2 0.560531 0.489294 0.199321 10.25000 -1.20000 AFIX 0 PART 0 PART 1 C4A 1 0.440277 0.449797 0.194102 10.75000 0.02724 0.02087 = 0.02164 0.00046 0.00304 -0.00215 PART 0 PART 2 C4B 1 0.391375 0.415174 0.194284 10.25000 0.03628 0.03148 = 0.02715 -0.00262 0.00597 -0.00403 PART 0 PART 1 C5A 1 0.319054 0.438553 0.197865 10.75000 0.02868 0.03392 = 0.02963 -0.00789 0.00535 -0.00425 AFIX 43 H5A 2 0.268839 0.377882 0.188416 10.75000 -1.20000 AFIX 0 PART 0 PART 2 C5B 1 0.281293 0.424929 0.202763 10.25000 0.03669 0.03440 = 0.03055 -0.00556 0.00754 -0.00512 AFIX 43 H5B 2 0.220262 0.362075 0.196721 10.25000 -1.20000 AFIX 0 PART 0 PART 1 C6A 1 0.272527 0.514674 0.215116 10.75000 0.03117 0.03205 = 0.02825 -0.00398 0.00646 -0.00191 AFIX 43 H6A 2 0.190482 0.504754 0.217690 10.75000 -1.20000 AFIX 0 PART 0 PART 2 C6B 1 0.254494 0.518678 0.219207 10.25000 0.03703 0.03805 = 0.03207 -0.00823 0.00649 -0.00393 AFIX 43 H6B 2 0.175881 0.524501 0.224085 10.25000 -1.20000 AFIX 0 PART 0 PART 1 C7A 1 0.493251 0.378682 0.174973 10.75000 0.02481 0.02367 = 0.02512 -0.00237 0.00384 -0.00210 AFIX 43 H7A 2 0.573049 0.402862 0.172196 10.75000 -1.20000 AFIX 0 PART 0 PART 2 C7B 1 0.409075 0.317754 0.174967 10.25000 0.03883 0.03194 = 0.04244 -0.00527 0.00416 -0.00550 AFIX 43 H7B 2 0.356490 0.237881 0.172477 10.25000 -1.20000 AFIX 0 PART 0 PART 1 C8A 1 0.437096 0.282398 0.161207 10.75000 0.02651 0.01967 = 0.02668 -0.00257 0.00283 0.00370 AFIX 43 H8A 2 0.359935 0.251617 0.164752 10.75000 -1.20000 AFIX 0 PART 0 PART 2 C8B 1 0.494996 0.336594 0.160929 10.25000 0.03227 0.03311 = 0.02754 -0.00234 -0.00110 -0.01958 AFIX 43 H8B 2 0.554065 0.410119 0.162628 10.25000 -1.20000 AFIX 0 PART 0 C10A 1 0.607639 -0.005802 0.082839 11.00000 0.02486 0.02850 = 0.02519 -0.00322 0.00449 -0.00459 C11A 1 0.562856 0.079758 0.101996 11.00000 0.02422 0.02299 = 0.02306 0.00079 -0.00026 0.00334 C12A 1 0.606792 0.216549 0.108106 11.00000 0.02718 0.02567 = 0.03034 0.00008 -0.00128 0.00182 AFIX 43 H12A 2 0.662191 0.262962 0.099055 11.00000 -1.20000 AFIX 0 C13A 1 0.570082 0.285722 0.127384 11.00000 0.04049 0.02657 = 0.04030 -0.01141 -0.00959 0.00882 AFIX 43 H13A 2 0.601743 0.378279 0.131488 11.00000 -1.20000 AFIX 0 C14A 1 0.486988 0.220441 0.140805 11.00000 0.04556 0.04325 = 0.02302 -0.00033 0.00139 0.02435 C15A 1 0.441769 0.086399 0.134252 11.00000 0.04582 0.03260 = 0.03024 0.00750 0.01448 0.01437 AFIX 43 H15A 2 0.383678 0.041733 0.142896 11.00000 -1.20000 AFIX 0 C16A 1 0.479410 0.016137 0.115380 11.00000 0.03411 0.02771 = 0.02862 0.00288 0.00809 0.00285 AFIX 43 H16A 2 0.448080 -0.076848 0.111443 11.00000 -1.20000 AFIX 0 C20A 1 0.612420 0.042937 0.061493 11.00000 0.02586 0.02393 = 0.02713 -0.00067 0.00424 -0.00306 C21A 1 0.564206 0.185677 0.053458 11.00000 0.02888 0.02450 = 0.02658 -0.00327 0.00292 -0.00103 C22A 1 0.452554 0.236352 0.058519 11.00000 0.02810 0.02666 = 0.01924 -0.00280 0.00419 -0.00109 AFIX 43 H22A 2 0.405351 0.181461 0.068146 11.00000 -1.20000 AFIX 0 C23A 1 0.410101 0.366512 0.049563 11.00000 0.02924 0.03218 = 0.02334 -0.00447 -0.00055 0.00411 AFIX 43 H23A 2 0.333417 0.399635 0.053003 11.00000 -1.20000 AFIX 0 C24A 1 0.477633 0.449218 0.035669 11.00000 0.03905 0.02896 = 0.02817 0.00282 -0.00060 0.00053 AFIX 43 H24A 2 0.447562 0.538401 0.029618 11.00000 -1.20000 AFIX 0 C25A 1 0.588951 0.400987 0.030690 11.00000 0.04259 0.03279 = 0.03300 0.00409 0.01149 -0.00526 AFIX 43 H25A 2 0.636430 0.457885 0.021384 11.00000 -1.20000 AFIX 0 C26A 1 0.631465 0.270184 0.039207 11.00000 0.02869 0.03212 = 0.03728 -0.00351 0.01325 -0.00162 AFIX 43 H26A 2 0.707414 0.236742 0.035375 11.00000 -1.20000 AFIX 0 C31A 1 0.654067 -0.153862 0.089674 11.00000 0.03099 0.02287 = 0.02524 -0.00072 0.00947 -0.00489 C32A 1 0.622416 -0.279012 0.077338 11.00000 0.04056 0.02684 = 0.02654 -0.00314 0.00634 -0.00400 AFIX 43 H32A 2 0.566696 -0.273141 0.064580 11.00000 -1.20000 AFIX 0 C33A 1 0.672151 -0.411471 0.083685 11.00000 0.05001 0.02820 = 0.03278 -0.00569 0.00878 -0.00062 AFIX 43 H33A 2 0.649764 -0.496074 0.075277 11.00000 -1.20000 AFIX 0 C34A 1 0.753323 -0.422035 0.101960 11.00000 0.04266 0.02112 = 0.04370 0.00228 0.01338 0.00708 AFIX 43 H34A 2 0.789407 -0.512669 0.105804 11.00000 -1.20000 AFIX 0 C35A 1 0.782869 -0.297884 0.114987 11.00000 0.03151 0.03002 = 0.03512 0.00354 0.00505 0.00013 AFIX 43 H35A 2 0.837805 -0.304615 0.127853 11.00000 -1.20000 AFIX 0 C36A 1 0.731630 -0.166426 0.108971 11.00000 0.03005 0.02143 = 0.02902 -0.00130 0.00880 -0.00271 AFIX 43 H36A 2 0.749375 -0.083357 0.118082 11.00000 -1.20000 AFIX 0 C41A 1 0.668130 -0.044806 0.043553 11.00000 0.03646 0.02630 = 0.02439 0.00014 0.01006 -0.00121 C42A 1 0.787990 -0.082575 0.045120 11.00000 0.03376 0.03107 = 0.03208 0.00151 0.00923 0.00019 AFIX 43 H42A 2 0.837548 -0.053965 0.057979 11.00000 -1.20000 AFIX 0 C43A 1 0.835281 -0.161862 0.027963 11.00000 0.03928 0.02937 = 0.05357 0.00040 0.02372 0.00286 AFIX 43 H43A 2 0.917742 -0.184940 0.028880 11.00000 -1.20000 AFIX 0 C44A 1 0.763461 -0.207310 0.009616 11.00000 0.06146 0.03077 = 0.03750 -0.00595 0.02912 -0.00216 AFIX 43 H44A 2 0.795777 -0.264910 -0.001799 11.00000 -1.20000 AFIX 0 C45A 1 0.645028 -0.169655 0.007737 11.00000 0.06577 0.03196 = 0.02359 -0.00247 0.00763 -0.00277 AFIX 43 H45A 2 0.595824 -0.200912 -0.005010 11.00000 -1.20000 AFIX 0 C46A 1 0.597179 -0.086263 0.024374 11.00000 0.04033 0.03402 = 0.03031 -0.00102 0.00562 0.00338 AFIX 43 H46A 2 0.516050 -0.057270 0.022733 11.00000 -1.20000 AFIX 0 HKLF 4 REM khor3CuLT in P21/n #14 REM R1 = 0.0623 for 9143 Fo > 4sig(Fo) and 0.0744 for all 10976 data REM 849 parameters refined using 86 restraints END WGHT 0.0654 7.9201 REM Highest difference peak 0.949, deepest hole -0.711, 1-sigma level 0.061 Q1 1 0.3045 0.8862 0.2026 11.00000 0.05 0.95 Q2 1 0.8050 0.2458 0.1615 11.00000 0.05 0.92 Q3 1 0.9682 0.4535 0.1632 11.00000 0.05 0.90 Q4 1 0.2456 1.1152 0.2018 11.00000 0.05 0.76 Q5 1 0.0794 1.0603 0.1906 11.00000 0.05 0.63 Q6 1 0.1155 0.8288 0.1897 11.00000 0.05 0.63 Q7 1 0.9374 0.5337 0.2403 11.00000 0.05 0.49 Q8 1 0.2356 0.7760 0.1916 11.00000 0.05 0.37 Q9 1 0.9989 0.6307 0.2237 11.00000 0.05 0.36 Q10 1 0.6926 -0.3229 0.0814 11.00000 0.05 0.34 Q11 1 1.0242 0.7198 0.2701 11.00000 0.05 0.34 Q12 1 0.6412 -0.0633 0.0722 11.00000 0.05 0.31 Q13 1 0.5942 0.0807 0.0792 11.00000 0.05 0.31 Q14 1 0.4997 0.1363 0.1397 11.00000 0.05 0.30 Q15 1 0.5461 0.2751 0.1413 11.00000 0.05 0.30 Q16 1 0.7604 0.5579 0.2250 11.00000 0.05 0.27 Q17 1 0.8309 0.4954 0.2180 11.00000 0.05 0.27 Q18 1 0.3572 0.7559 0.2453 11.00000 0.05 0.26 Q19 1 0.7992 0.4622 0.1984 11.00000 0.05 0.24 Q20 1 0.7240 -0.1579 0.0961 11.00000 0.05 0.24 ; _shelx_res_checksum 38288 _olex2_date_sample_data_collection 2018-11-06 _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 ; _oxdiff_exptl_absorpt_empirical_full_max 1.558 _oxdiff_exptl_absorpt_empirical_full_min 0.671 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.88412(10) 0.42676(10) 0.15237(2) 0.0542(2) Uani 1 1 d . . . . . Cl2 Cl 0.80461(9) 0.13577(11) 0.16170(2) 0.0553(3) Uani 1 1 d . . . . . C1S C 0.9271(3) 0.2555(4) 0.16402(6) 0.0422(8) Uani 1 1 d . . . . . H1SA H 0.9935 0.2151 0.1558 0.051 Uiso 1 1 calc R . . . . H1SB H 0.9549 0.2671 0.1801 0.051 Uiso 1 1 calc R . . . . P1 P 0.18654(7) 0.97003(9) 0.19499(2) 0.02918(18) Uani 1 1 d . . . . . F1 F 0.12725(19) 0.9487(2) 0.21863(3) 0.0495(5) Uani 1 1 d . . . . . F2 F 0.24704(19) 0.9915(2) 0.17167(3) 0.0491(5) Uani 1 1 d . . . . . F3 F 0.1559(3) 1.1374(3) 0.19555(4) 0.0766(8) Uani 1 1 d . . . . . F4 F 0.3079(2) 1.0017(4) 0.20871(4) 0.0807(9) Uani 1 1 d . . . . . F5 F 0.2185(4) 0.8042(3) 0.19468(4) 0.0922(11) Uani 1 1 d . . . . . F6 F 0.0648(2) 0.9419(4) 0.18131(5) 0.0958(12) Uani 1 1 d . . . . . P1A P 0.90751(8) 0.46478(10) 0.22744(2) 0.0401(2) Uani 1 1 d . . . . . F1A F 0.8466(2) 0.3652(2) 0.24553(3) 0.0481(5) Uani 1 1 d . . . . . F2A F 0.9705(2) 0.5637(3) 0.20964(4) 0.0690(7) Uani 1 1 d . . . . . F3A F 0.8336(3) 0.6008(3) 0.23553(5) 0.0776(9) Uani 1 1 d . . . . . F4A F 1.0111(3) 0.5019(3) 0.24627(5) 0.0770(8) Uani 1 1 d . . . . . F5A F 0.9841(2) 0.3310(3) 0.21972(4) 0.0552(6) Uani 1 1 d . . . . . F6A F 0.8054(2) 0.4272(4) 0.20890(4) 0.0744(8) Uani 1 1 d . . . . . N1 N 0.7755(2) 0.9436(3) 0.21073(4) 0.0296(5) Uani 1 1 d . . . . . C1 C 0.8545(3) 1.0139(4) 0.22842(6) 0.0429(8) Uani 1 1 d . . . . . H1A H 0.8133 1.0968 0.2347 0.064 Uiso 1 1 calc GR . . . . H1B H 0.9271 1.0476 0.2218 0.064 Uiso 1 1 calc GR . . . . H1C H 0.8755 0.9440 0.2405 0.064 Uiso 1 1 calc GR . . . . C2 C 0.8206(3) 0.8385(3) 0.19804(5) 0.0313(6) Uani 1 1 d . . . . . H2 H 0.9015 0.8103 0.2007 0.038 Uiso 1 1 calc R . . . . C3 C 0.7502(3) 0.7718(3) 0.18125(5) 0.0318(6) Uani 1 1 d . . . . . H3 H 0.7830 0.6977 0.1724 0.038 Uiso 1 1 calc R . . . . C4 C 0.6308(3) 0.8118(3) 0.17706(5) 0.0255(6) Uani 1 1 d . . . . . C5 C 0.5872(3) 0.9209(3) 0.19079(5) 0.0289(6) Uani 1 1 d . . . . . H5 H 0.5064 0.9507 0.1886 0.035 Uiso 1 1 calc R . . . . C6 C 0.6609(3) 0.9847(4) 0.20730(5) 0.0325(7) Uani 1 1 d . . . . . H6 H 0.6306 1.0590 0.2165 0.039 Uiso 1 1 calc R . . . . C7 C 0.5575(3) 0.7391(3) 0.15927(5) 0.0271(6) Uani 1 1 d . . . . . H7 H 0.5971 0.6894 0.1479 0.032 Uiso 1 1 calc R . . . . C8 C 0.4391(3) 0.7375(3) 0.15783(5) 0.0252(6) Uani 1 1 d . . . . . H8 H 0.4001 0.7872 0.1693 0.030 Uiso 1 1 calc R . . . . C10 C 0.1367(3) 0.4462(3) 0.08951(5) 0.0257(6) Uani 1 1 d . . . . . C11 C 0.2151(3) 0.5258(3) 0.10673(5) 0.0255(6) Uani 1 1 d . . . . . C12 C 0.1715(3) 0.5687(3) 0.12722(5) 0.0303(6) Uani 1 1 d . . . . . H12 H 0.0911 0.5486 0.1301 0.036 Uiso 1 1 calc R . . . . C13 C 0.2442(3) 0.6403(3) 0.14345(5) 0.0285(6) Uani 1 1 d . . . . . H13 H 0.2121 0.6724 0.1570 0.034 Uiso 1 1 calc R . . . . C14 C 0.3637(3) 0.6658(3) 0.14007(4) 0.0246(6) Uani 1 1 d . . . . . C15 C 0.4078(3) 0.6216(3) 0.11954(5) 0.0259(6) Uani 1 1 d . . . . . H15 H 0.4890 0.6385 0.1169 0.031 Uiso 1 1 calc R . . . . C16 C 0.3345(3) 0.5541(3) 0.10319(5) 0.0269(6) Uani 1 1 d . . . . . H16 H 0.3656 0.5263 0.0893 0.032 Uiso 1 1 calc R . . . . C20 C 0.1166(3) 0.4946(3) 0.06796(5) 0.0261(6) Uani 1 1 d . . . . . C21 C 0.1589(3) 0.6403(3) 0.06061(5) 0.0280(6) Uani 1 1 d . . . . . C22 C 0.1445(3) 0.7646(3) 0.07341(5) 0.0361(7) Uani 1 1 d . . . . . H22 H 0.1026 0.7593 0.0868 0.043 Uiso 1 1 calc R . . . . C23 C 0.1906(4) 0.8966(4) 0.06683(6) 0.0450(8) Uani 1 1 d . . . . . H23 H 0.1810 0.9805 0.0759 0.054 Uiso 1 1 calc R . . . . C24 C 0.2504(3) 0.9066(4) 0.04715(6) 0.0415(8) Uani 1 1 d . . . . . H24 H 0.2832 0.9965 0.0428 0.050 Uiso 1 1 calc R . . . . C25 C 0.2620(3) 0.7843(3) 0.03387(5) 0.0328(7) Uani 1 1 d . . . . . H25 H 0.3018 0.7905 0.0202 0.039 Uiso 1 1 calc R . . . . C26 C 0.2157(3) 0.6532(3) 0.04045(5) 0.0279(6) Uani 1 1 d . . . . . H26 H 0.2226 0.5704 0.0311 0.033 Uiso 1 1 calc R . . . . C31 C 0.0875(3) 0.3079(3) 0.09797(4) 0.0253(6) Uani 1 1 d . . . . . C32 C 0.1612(3) 0.2175(3) 0.11186(5) 0.0307(6) Uani 1 1 d . . . . . H32 H 0.2407 0.2466 0.1160 0.037 Uiso 1 1 calc R . . . . C33 C 0.1191(3) 0.0857(4) 0.11959(5) 0.0364(7) Uani 1 1 d . . . . . H33 H 0.1704 0.0243 0.1287 0.044 Uiso 1 1 calc R . . . . C34 C 0.0020(3) 0.0437(4) 0.11402(5) 0.0353(7) Uani 1 1 d . . . . . H34 H -0.0270 -0.0460 0.1193 0.042 Uiso 1 1 calc R . . . . C35 C -0.0716(3) 0.1340(3) 0.10071(5) 0.0322(7) Uani 1 1 d . . . . . H35 H -0.1518 0.1063 0.0970 0.039 Uiso 1 1 calc R . . . . C36 C -0.0296(3) 0.2643(3) 0.09276(5) 0.0273(6) Uani 1 1 d . . . . . H36 H -0.0815 0.3249 0.0836 0.033 Uiso 1 1 calc R . . . . C41 C 0.0555(3) 0.4036(3) 0.04976(5) 0.0259(6) Uani 1 1 d . . . . . C42 C 0.0872(3) 0.2595(3) 0.04671(5) 0.0279(6) Uani 1 1 d . . . . . H42 H 0.1497 0.2185 0.0562 0.033 Uiso 1 1 calc R . . . . C43 C 0.0294(3) 0.1746(4) 0.03010(5) 0.0326(7) Uani 1 1 d . . . . . H43 H 0.0510 0.0757 0.0285 0.039 Uiso 1 1 calc R . . . . C44 C -0.0597(3) 0.2340(4) 0.01579(5) 0.0367(7) Uani 1 1 d . . . . . H44 H -0.1004 0.1761 0.0045 0.044 Uiso 1 1 calc R . . . . C45 C -0.0892(3) 0.3782(4) 0.01811(5) 0.0379(8) Uani 1 1 d . . . . . H45 H -0.1487 0.4202 0.0080 0.046 Uiso 1 1 calc R . . . . C46 C -0.0330(3) 0.4627(4) 0.03499(5) 0.0336(7) Uani 1 1 d . . . . . H46 H -0.0549 0.5616 0.0365 0.040 Uiso 1 1 calc R . . . . N1A N 0.3419(2) 0.6037(3) 0.22853(4) 0.0282(5) Uani 1 1 d D U . . . C1A C 0.2918(4) 0.6953(4) 0.24606(5) 0.0448(9) Uani 1 1 d . . . . . H1AA H 0.3498 0.7037 0.2591 0.067 Uiso 1 1 calc GR . . . . H1AB H 0.2185 0.6509 0.2509 0.067 Uiso 1 1 calc GR . . . . H1AC H 0.2740 0.7919 0.2398 0.067 Uiso 1 1 calc GR . . . . C2A C 0.4576(5) 0.6164(6) 0.22550(10) 0.0259(11) Uani 0.75 1 d D U P A 1 H2A H 0.5052 0.6795 0.2350 0.031 Uiso 0.75 1 calc R . P A 1 C2B C 0.4580(16) 0.591(3) 0.2213(4) 0.035(4) Uani 0.25 1 d D U P A 2 H2B H 0.5203 0.6483 0.2283 0.042 Uiso 0.25 1 calc R . P A 2 C3A C 0.5091(4) 0.5397(5) 0.20880(8) 0.0252(9) Uani 0.75 1 d D U P A 1 H3A H 0.5923 0.5479 0.2072 0.030 Uiso 0.75 1 calc R . P A 1 C3B C 0.4821(15) 0.4973(17) 0.2042(3) 0.035(3) Uani 0.25 1 d D U P A 2 H3B H 0.5605 0.4893 0.1993 0.041 Uiso 0.25 1 calc R . P A 2 C4A C 0.4403(4) 0.4498(5) 0.19410(7) 0.0232(8) Uani 0.75 1 d D U P A 1 C4B C 0.3914(15) 0.4152(17) 0.1943(2) 0.031(3) Uani 0.25 1 d D U P A 2 C5A C 0.3191(5) 0.4386(5) 0.19787(9) 0.0306(10) Uani 0.75 1 d D U P A 1 H5A H 0.2688 0.3779 0.1884 0.037 Uiso 0.75 1 calc R . P A 1 C5B C 0.2813(14) 0.4249(18) 0.2028(3) 0.034(3) Uani 0.25 1 d D U P A 2 H5B H 0.2203 0.3621 0.1967 0.040 Uiso 0.25 1 calc R . P A 2 C6A C 0.2725(5) 0.5147(8) 0.21512(12) 0.0303(13) Uani 0.75 1 d D U P A 1 H6A H 0.1905 0.5048 0.2177 0.036 Uiso 0.75 1 calc R . P A 1 C6B C 0.2545(18) 0.519(3) 0.2192(4) 0.036(4) Uani 0.25 1 d D U P A 2 H6B H 0.1759 0.5245 0.2241 0.043 Uiso 0.25 1 calc R . P A 2 C7A C 0.4933(3) 0.3787(4) 0.17497(8) 0.0244(8) Uani 0.75 1 d . . P A 1 H7A H 0.5730 0.4029 0.1722 0.029 Uiso 0.75 1 calc R . P A 1 C7B C 0.4091(13) 0.3178(15) 0.1750(3) 0.038(3) Uani 0.25 1 d . . P A 2 H7B H 0.3565 0.2379 0.1725 0.045 Uiso 0.25 1 calc R . P A 2 C8A C 0.4371(5) 0.2824(5) 0.16121(8) 0.0242(8) Uani 0.75 1 d . . P A 1 H8A H 0.3599 0.2516 0.1648 0.029 Uiso 0.75 1 calc R . P A 1 C8B C 0.4950(14) 0.3366(17) 0.1609(2) 0.031(3) Uani 0.25 1 d . . P A 2 H8B H 0.5541 0.4101 0.1626 0.037 Uiso 0.25 1 calc R . P A 2 C10A C 0.6076(3) -0.0058(3) 0.08284(5) 0.0261(6) Uani 1 1 d . . . . . C11A C 0.5629(2) 0.0798(3) 0.10200(5) 0.0235(6) Uani 1 1 d . . . . . C12A C 0.6068(3) 0.2165(3) 0.10811(5) 0.0279(6) Uani 1 1 d . . . . . H12A H 0.6622 0.2630 0.0991 0.033 Uiso 1 1 calc R . . . . C13A C 0.5701(3) 0.2857(3) 0.12738(6) 0.0363(7) Uani 1 1 d . . . . . H13A H 0.6017 0.3783 0.1315 0.044 Uiso 1 1 calc R . . . . C14A C 0.4870(3) 0.2204(4) 0.14081(5) 0.0373(8) Uani 1 1 d . . . . . C15A C 0.4418(3) 0.0864(3) 0.13425(5) 0.0357(7) Uani 1 1 d . . . . . H15A H 0.3837 0.0417 0.1429 0.043 Uiso 1 1 calc R . . . . C16A C 0.4794(3) 0.0161(3) 0.11538(5) 0.0299(6) Uani 1 1 d . . . . . H16A H 0.4481 -0.0768 0.1114 0.036 Uiso 1 1 calc R . . . . C20A C 0.6124(2) 0.0429(3) 0.06149(5) 0.0255(6) Uani 1 1 d . . . . . C21A C 0.5642(3) 0.1857(3) 0.05346(5) 0.0266(6) Uani 1 1 d . . . . . C22A C 0.4526(3) 0.2364(3) 0.05852(4) 0.0246(6) Uani 1 1 d . . . . . H22A H 0.4054 0.1815 0.0681 0.029 Uiso 1 1 calc R . . . . C23A C 0.4101(3) 0.3665(3) 0.04956(5) 0.0284(6) Uani 1 1 d . . . . . H23A H 0.3334 0.3996 0.0530 0.034 Uiso 1 1 calc R . . . . C24A C 0.4776(3) 0.4492(3) 0.03567(5) 0.0322(7) Uani 1 1 d . . . . . H24A H 0.4476 0.5384 0.0296 0.039 Uiso 1 1 calc R . . . . C25A C 0.5890(3) 0.4010(4) 0.03069(5) 0.0357(7) Uani 1 1 d . . . . . H25A H 0.6364 0.4579 0.0214 0.043 Uiso 1 1 calc R . . . . C26A C 0.6315(3) 0.2702(3) 0.03921(5) 0.0322(7) Uani 1 1 d . . . . . H26A H 0.7074 0.2367 0.0354 0.039 Uiso 1 1 calc R . . . . C31A C 0.6541(3) -0.1539(3) 0.08967(5) 0.0260(6) Uani 1 1 d . . . . . C32A C 0.6224(3) -0.2790(3) 0.07734(5) 0.0311(6) Uani 1 1 d . . . . . H32A H 0.5667 -0.2731 0.0646 0.037 Uiso 1 1 calc R . . . . C33A C 0.6722(3) -0.4115(3) 0.08369(5) 0.0367(7) Uani 1 1 d . . . . . H33A H 0.6498 -0.4961 0.0753 0.044 Uiso 1 1 calc R . . . . C34A C 0.7533(3) -0.4220(3) 0.10196(6) 0.0354(7) Uani 1 1 d . . . . . H34A H 0.7894 -0.5127 0.1058 0.042 Uiso 1 1 calc R . . . . C35A C 0.7829(3) -0.2979(3) 0.11499(5) 0.0321(7) Uani 1 1 d . . . . . H35A H 0.8378 -0.3046 0.1279 0.039 Uiso 1 1 calc R . . . . C36A C 0.7316(3) -0.1664(3) 0.10897(5) 0.0265(6) Uani 1 1 d . . . . . H36A H 0.7494 -0.0834 0.1181 0.032 Uiso 1 1 calc R . . . . C41A C 0.6681(3) -0.0448(3) 0.04355(5) 0.0287(6) Uani 1 1 d . . . . . C42A C 0.7880(3) -0.0826(3) 0.04512(5) 0.0320(7) Uani 1 1 d . . . . . H42A H 0.8375 -0.0540 0.0580 0.038 Uiso 1 1 calc R . . . . C43A C 0.8353(3) -0.1619(4) 0.02796(6) 0.0398(8) Uani 1 1 d . . . . . H43A H 0.9177 -0.1849 0.0289 0.048 Uiso 1 1 calc R . . . . C44A C 0.7635(3) -0.2073(4) 0.00962(6) 0.0421(8) Uani 1 1 d . . . . . H44A H 0.7958 -0.2649 -0.0018 0.051 Uiso 1 1 calc R . . . . C45A C 0.6450(4) -0.1697(4) 0.00774(5) 0.0402(8) Uani 1 1 d . . . . . H45A H 0.5958 -0.2009 -0.0050 0.048 Uiso 1 1 calc R . . . . C46A C 0.5972(3) -0.0863(4) 0.02437(5) 0.0347(7) Uani 1 1 d . . . . . H46A H 0.5160 -0.0573 0.0227 0.042 Uiso 1 1 calc R . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0716(6) 0.0438(5) 0.0489(5) 0.0085(4) 0.0174(4) 0.0016(4) Cl2 0.0561(6) 0.0607(6) 0.0486(5) 0.0176(4) -0.0017(4) -0.0107(5) C1S 0.0409(19) 0.044(2) 0.0417(19) 0.0016(15) 0.0055(15) 0.0046(15) P1 0.0299(4) 0.0323(4) 0.0263(4) 0.0035(3) 0.0089(3) 0.0025(3) F1 0.0560(13) 0.0562(13) 0.0394(11) 0.0087(9) 0.0267(9) 0.0074(10) F2 0.0588(13) 0.0582(13) 0.0325(10) 0.0154(9) 0.0199(9) 0.0139(10) F3 0.123(2) 0.0450(14) 0.0652(16) 0.0093(11) 0.0319(16) 0.0223(14) F4 0.0421(13) 0.149(3) 0.0506(14) 0.0133(16) -0.0002(11) -0.0111(15) F5 0.200(4) 0.0401(13) 0.0411(13) 0.0098(10) 0.0457(17) 0.0298(17) F6 0.0572(16) 0.164(3) 0.0641(16) 0.0285(19) -0.0102(13) -0.0506(19) P1A 0.0400(5) 0.0437(5) 0.0381(5) 0.0057(4) 0.0134(4) 0.0077(4) F1A 0.0610(13) 0.0436(11) 0.0416(11) 0.0046(9) 0.0172(9) 0.0018(10) F2A 0.0656(15) 0.0690(16) 0.0773(17) 0.0278(13) 0.0429(13) 0.0178(13) F3A 0.097(2) 0.0473(13) 0.096(2) 0.0219(13) 0.0633(17) 0.0250(13) F4A 0.0708(17) 0.093(2) 0.0675(16) -0.0161(15) 0.0022(13) -0.0212(15) F5A 0.0548(13) 0.0552(13) 0.0571(13) 0.0015(10) 0.0152(10) 0.0186(11) F6A 0.0426(13) 0.133(3) 0.0479(13) 0.0091(14) 0.0031(10) 0.0105(15) N1 0.0258(13) 0.0381(14) 0.0254(12) -0.0034(10) 0.0054(10) -0.0062(11) C1 0.0323(17) 0.057(2) 0.0389(18) -0.0159(16) 0.0007(14) -0.0130(16) C2 0.0249(15) 0.0391(17) 0.0301(15) 0.0000(13) 0.0042(12) -0.0021(13) C3 0.0317(16) 0.0324(16) 0.0317(15) -0.0035(12) 0.0059(12) 0.0013(13) C4 0.0289(15) 0.0265(14) 0.0217(13) 0.0008(11) 0.0054(11) -0.0049(12) C5 0.0260(14) 0.0325(16) 0.0283(15) -0.0033(12) 0.0032(11) -0.0019(12) C6 0.0331(16) 0.0369(17) 0.0281(15) -0.0063(12) 0.0071(12) -0.0026(13) C7 0.0327(16) 0.0274(15) 0.0217(13) -0.0017(11) 0.0054(11) -0.0002(12) C8 0.0320(15) 0.0229(14) 0.0209(13) -0.0008(10) 0.0040(11) -0.0015(11) C10 0.0267(14) 0.0266(14) 0.0241(14) -0.0027(11) 0.0040(11) 0.0006(11) C11 0.0298(15) 0.0240(14) 0.0226(13) 0.0005(11) 0.0018(11) -0.0007(11) C12 0.0296(15) 0.0342(16) 0.0275(15) -0.0033(12) 0.0049(12) -0.0050(12) C13 0.0321(15) 0.0332(16) 0.0207(13) -0.0026(11) 0.0071(11) -0.0030(12) C14 0.0325(15) 0.0220(13) 0.0194(13) -0.0004(10) 0.0029(11) -0.0001(11) C15 0.0297(15) 0.0241(14) 0.0242(14) 0.0002(11) 0.0042(11) -0.0010(11) C16 0.0353(16) 0.0271(14) 0.0185(13) -0.0019(11) 0.0045(11) 0.0022(12) C20 0.0275(14) 0.0246(14) 0.0263(14) -0.0004(11) 0.0029(11) 0.0024(11) C21 0.0298(15) 0.0276(15) 0.0262(14) 0.0018(11) -0.0017(11) 0.0010(12) C22 0.052(2) 0.0279(16) 0.0287(16) 0.0012(12) 0.0063(14) 0.0048(14) C23 0.068(2) 0.0269(17) 0.0403(19) -0.0048(14) 0.0024(17) 0.0016(16) C24 0.053(2) 0.0291(17) 0.0420(19) 0.0051(14) -0.0003(15) -0.0058(15) C25 0.0337(16) 0.0338(16) 0.0306(15) 0.0052(12) -0.0001(12) -0.0010(13) C26 0.0292(15) 0.0280(15) 0.0258(14) 0.0012(11) -0.0035(11) 0.0015(12) C31 0.0294(15) 0.0286(15) 0.0181(13) -0.0020(11) 0.0043(11) 0.0007(12) C32 0.0324(16) 0.0317(16) 0.0277(15) -0.0004(12) -0.0005(12) -0.0029(13) C33 0.0456(19) 0.0331(17) 0.0301(16) 0.0060(13) -0.0007(13) 0.0029(14) C34 0.0406(18) 0.0328(17) 0.0331(16) 0.0031(13) 0.0076(13) -0.0082(14) C35 0.0306(16) 0.0383(17) 0.0287(15) 0.0002(12) 0.0079(12) -0.0048(13) C36 0.0279(15) 0.0314(15) 0.0231(14) -0.0017(11) 0.0052(11) 0.0028(12) C41 0.0255(14) 0.0302(15) 0.0221(13) 0.0025(11) 0.0034(11) -0.0036(12) C42 0.0286(15) 0.0332(16) 0.0221(13) 0.0007(11) 0.0044(11) -0.0027(12) C43 0.0314(16) 0.0395(17) 0.0278(15) -0.0084(13) 0.0094(12) -0.0080(13) C44 0.0331(17) 0.053(2) 0.0246(15) -0.0066(13) 0.0058(12) -0.0148(15) C45 0.0295(16) 0.057(2) 0.0265(15) 0.0092(14) -0.0014(12) -0.0077(15) C46 0.0301(16) 0.0388(17) 0.0316(16) 0.0074(13) -0.0004(12) -0.0027(13) N1A 0.0354(10) 0.0266(11) 0.0227(10) 0.0014(8) 0.0023(8) 0.0007(8) C1A 0.070(2) 0.0425(19) 0.0232(15) -0.0058(13) 0.0102(15) 0.0128(18) C2A 0.0345(13) 0.021(2) 0.022(2) 0.0007(17) 0.0010(12) 0.0002(12) C2B 0.036(2) 0.036(7) 0.033(7) -0.008(6) 0.005(3) -0.003(2) C3A 0.0297(16) 0.022(2) 0.0237(18) -0.0002(14) 0.0009(12) -0.0024(13) C3B 0.036(4) 0.035(6) 0.033(6) -0.008(4) 0.007(4) -0.005(3) C4A 0.0272(18) 0.0209(19) 0.0216(16) 0.0005(14) 0.0030(14) -0.0021(14) C4B 0.036(4) 0.031(5) 0.027(4) -0.003(4) 0.006(4) -0.004(4) C5A 0.0287(19) 0.034(2) 0.030(2) -0.0079(16) 0.0053(14) -0.0043(15) C5B 0.037(4) 0.034(5) 0.031(5) -0.006(4) 0.008(3) -0.005(4) C6A 0.0312(18) 0.032(2) 0.028(2) -0.0040(18) 0.0065(14) -0.0019(15) C6B 0.037(2) 0.038(6) 0.032(7) -0.008(6) 0.006(3) -0.004(3) C7A 0.025(2) 0.0237(19) 0.025(2) -0.0024(17) 0.0038(16) -0.0021(17) C7B 0.039(8) 0.032(7) 0.042(8) -0.005(6) 0.004(6) -0.005(6) C8A 0.027(2) 0.020(2) 0.027(2) -0.0026(17) 0.0028(18) 0.004(2) C8B 0.032(8) 0.033(7) 0.028(8) -0.002(6) -0.001(6) -0.020(6) C10A 0.0249(14) 0.0285(15) 0.0252(14) -0.0032(11) 0.0045(11) -0.0046(11) C11A 0.0242(14) 0.0230(14) 0.0231(13) 0.0008(10) -0.0003(10) 0.0033(11) C12A 0.0272(15) 0.0257(15) 0.0303(15) 0.0001(11) -0.0013(11) 0.0018(12) C13A 0.0405(18) 0.0266(15) 0.0403(17) -0.0114(13) -0.0096(14) 0.0088(13) C14A 0.0456(19) 0.0432(19) 0.0230(15) -0.0003(13) 0.0014(13) 0.0244(15) C15A 0.0458(19) 0.0326(17) 0.0302(16) 0.0075(13) 0.0145(14) 0.0144(14) C16A 0.0341(16) 0.0277(15) 0.0286(15) 0.0029(12) 0.0081(12) 0.0029(12) C20A 0.0259(14) 0.0239(14) 0.0271(14) -0.0007(11) 0.0042(11) -0.0031(11) C21A 0.0289(15) 0.0245(14) 0.0266(14) -0.0033(11) 0.0029(11) -0.0010(12) C22A 0.0281(14) 0.0267(14) 0.0192(13) -0.0028(10) 0.0042(11) -0.0011(11) C23A 0.0292(15) 0.0322(16) 0.0233(14) -0.0045(11) -0.0005(11) 0.0041(12) C24A 0.0390(17) 0.0290(15) 0.0282(15) 0.0028(12) -0.0006(12) 0.0005(13) C25A 0.0426(18) 0.0328(17) 0.0330(16) 0.0041(13) 0.0115(13) -0.0053(14) C26A 0.0287(15) 0.0321(16) 0.0373(16) -0.0035(13) 0.0133(13) -0.0016(13) C31A 0.0310(15) 0.0229(14) 0.0252(14) -0.0007(11) 0.0095(11) -0.0049(11) C32A 0.0406(17) 0.0268(15) 0.0265(14) -0.0031(12) 0.0063(12) -0.0040(13) C33A 0.050(2) 0.0282(16) 0.0328(16) -0.0057(12) 0.0088(14) -0.0006(14) C34A 0.0427(18) 0.0211(15) 0.0437(18) 0.0023(12) 0.0134(14) 0.0071(13) C35A 0.0315(16) 0.0300(16) 0.0351(16) 0.0035(12) 0.0050(12) 0.0001(13) C36A 0.0300(15) 0.0214(14) 0.0290(14) -0.0013(11) 0.0088(11) -0.0027(11) C41A 0.0365(16) 0.0263(15) 0.0244(14) 0.0001(11) 0.0101(12) -0.0012(12) C42A 0.0338(16) 0.0311(16) 0.0321(16) 0.0015(12) 0.0092(12) 0.0002(13) C43A 0.0393(18) 0.0294(16) 0.054(2) 0.0004(14) 0.0237(16) 0.0029(14) C44A 0.061(2) 0.0308(17) 0.0375(18) -0.0059(14) 0.0291(16) -0.0022(16) C45A 0.066(2) 0.0320(17) 0.0236(15) -0.0025(12) 0.0076(15) -0.0028(16) C46A 0.0403(18) 0.0340(17) 0.0303(16) -0.0010(13) 0.0056(13) 0.0034(14) 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' Cl Cl 0.3639 0.7018 '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' P P 0.2955 0.4335 '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 Cl2 C1S Cl1 109.6(2) F2 P1 F1 179.27(13) F3 P1 F1 89.85(13) F3 P1 F2 90.16(13) F4 P1 F1 88.28(13) F4 P1 F2 91.00(13) F4 P1 F3 89.49(19) F4 P1 F5 89.7(2) F5 P1 F1 89.97(12) F5 P1 F2 90.01(12) F5 P1 F3 179.2(2) F6 P1 F1 91.71(14) F6 P1 F2 89.02(14) F6 P1 F3 89.3(2) F6 P1 F4 178.8(2) F6 P1 F5 91.5(2) F2A P1A F1A 178.96(15) F2A P1A F3A 90.69(13) F2A P1A F4A 90.10(16) F3A P1A F1A 89.74(12) F4A P1A F1A 88.96(14) F4A P1A F3A 89.63(18) F5A P1A F1A 90.64(12) F5A P1A F2A 88.91(13) F5A P1A F3A 178.53(18) F5A P1A F4A 88.96(15) F6A P1A F1A 90.82(14) F6A P1A F2A 90.12(16) F6A P1A F3A 90.60(17) F6A P1A F4A 179.7(2) F6A P1A F5A 90.81(15) C2 N1 C1 118.7(3) C2 N1 C6 120.7(3) C6 N1 C1 120.6(3) N1 C2 C3 120.3(3) C2 C3 C4 120.7(3) C3 C4 C5 117.1(3) C3 C4 C7 119.9(3) C5 C4 C7 123.0(3) C6 C5 C4 120.1(3) N1 C6 C5 121.0(3) C8 C7 C4 124.7(3) C7 C8 C14 125.6(3) C20 C10 C11 122.2(3) C20 C10 C31 123.7(3) C31 C10 C11 114.0(2) C12 C11 C10 120.4(3) C12 C11 C16 118.3(3) C16 C11 C10 121.3(2) C13 C12 C11 120.8(3) C12 C13 C14 120.8(3) C13 C14 C8 119.5(2) C13 C14 C15 118.4(3) C15 C14 C8 122.0(3) C16 C15 C14 120.6(3) C15 C16 C11 121.1(3) C10 C20 C21 122.1(3) C10 C20 C41 122.2(3) C41 C20 C21 115.7(2) C22 C21 C20 122.0(3) C22 C21 C26 118.2(3) C26 C21 C20 119.8(3) C23 C22 C21 120.7(3) C24 C23 C22 120.3(3) C25 C24 C23 119.4(3) C26 C25 C24 120.0(3) C25 C26 C21 121.2(3) C32 C31 C10 119.1(3) C36 C31 C10 122.7(3) C36 C31 C32 118.2(3) C33 C32 C31 120.7(3) C34 C33 C32 120.2(3) C35 C34 C33 119.3(3) C34 C35 C36 120.7(3) C35 C36 C31 121.0(3) C42 C41 C20 121.3(3) C42 C41 C46 118.2(3) C46 C41 C20 120.5(3) C43 C42 C41 121.4(3) C44 C43 C42 119.9(3) C45 C44 C43 119.4(3) C44 C45 C46 120.8(3) C45 C46 C41 120.4(3) C2A N1A C1A 117.8(3) C2A N1A C6A 120.4(4) C2B N1A C1A 131.8(7) C6A N1A C1A 121.8(3) C6B N1A C1A 108.5(8) C6B N1A C2B 119.7(11) N1A C2A C3A 121.0(4) C3B C2B N1A 120.6(14) C2A C3A C4A 120.6(4) C2B C3B C4B 119.1(14) C3A C4A C5A 116.8(4) C3A C4A C7A 120.5(4) C5A C4A C7A 122.6(4) C3B C4B C7B 122.2(14) C5B C4B C3B 118.2(12) C5B C4B C7B 119.6(13) C6A C5A C4A 120.3(4) C6B C5B C4B 123.8(15) N1A C6A C5A 120.9(5) N1A C6B C5B 118.4(15) C8A C7A C4A 124.5(4) C8B C7B C4B 123.1(15) C7A C8A C14A 124.4(5) C7B C8B C14A 111.8(15) C11A C10A C31A 113.8(2) C20A C10A C11A 124.9(3) C20A C10A C31A 121.3(3) C12A C11A C10A 122.8(3) C12A C11A C16A 118.3(3) C16A C11A C10A 118.7(3) C13A C12A C11A 120.5(3) C12A C13A C14A 120.8(3) C13A C14A C8A 126.8(4) C13A C14A C8B 97.3(6) C15A C14A C8A 114.9(4) C15A C14A C8B 144.0(6) C15A C14A C13A 118.2(3) C16A C15A C14A 121.3(3) C15A C16A C11A 121.0(3) C10A C20A C21A 124.0(3) C10A C20A C41A 121.8(3) C21A C20A C41A 114.2(2) C22A C21A C20A 122.9(3) C22A C21A C26A 118.2(3) C26A C21A C20A 118.8(3) C23A C22A C21A 120.2(3) C22A C23A C24A 121.0(3) C25A C24A C23A 119.4(3) C24A C25A C26A 120.1(3) C25A C26A C21A 121.1(3) C32A C31A C10A 122.4(3) C36A C31A C10A 118.8(2) C36A C31A C32A 118.8(3) C33A C32A C31A 120.1(3) C34A C33A C32A 120.8(3) C33A C34A C35A 119.6(3) C36A C35A C34A 119.6(3) C35A C36A C31A 120.8(3) C42A C41A C20A 122.4(3) C42A C41A C46A 119.0(3) C46A C41A C20A 118.5(3) C43A C42A C41A 120.1(3) C44A C43A C42A 120.3(3) C43A C44A C45A 120.2(3) C44A C45A C46A 120.2(3) C45A C46A C41A 120.0(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Cl1 C1S 1.777(4) Cl2 C1S 1.764(4) P1 F1 1.6006(19) P1 F2 1.5904(19) P1 F3 1.582(3) P1 F4 1.568(3) P1 F5 1.571(2) P1 F6 1.566(3) P1A F1A 1.598(2) P1A F2A 1.594(2) P1A F3A 1.595(2) P1A F4A 1.595(3) P1A F5A 1.589(2) P1A F6A 1.573(3) N1 C1 1.477(4) N1 C2 1.346(4) N1 C6 1.347(4) C2 C3 1.374(4) C3 C4 1.399(4) C4 C5 1.402(4) C4 C7 1.457(4) C5 C6 1.371(4) C7 C8 1.330(4) C8 C14 1.463(4) C10 C11 1.495(4) C10 C20 1.355(4) C10 C31 1.490(4) C11 C12 1.394(4) C11 C16 1.398(4) C12 C13 1.386(4) C13 C14 1.392(4) C14 C15 1.403(4) C15 C16 1.377(4) C20 C21 1.499(4) C20 C41 1.495(4) C21 C22 1.389(4) C21 C26 1.394(4) C22 C23 1.389(5) C23 C24 1.385(5) C24 C25 1.385(5) C25 C26 1.382(4) C31 C32 1.402(4) C31 C36 1.392(4) C32 C33 1.393(4) C33 C34 1.391(5) C34 C35 1.383(5) C35 C36 1.385(4) C41 C42 1.390(4) C41 C46 1.391(4) C42 C43 1.384(4) C43 C44 1.382(5) C44 C45 1.379(5) C45 C46 1.386(5) N1A C1A 1.477(4) N1A C2A 1.331(6) N1A C2B 1.406(18) N1A C6A 1.353(6) N1A C6B 1.347(17) C2A C3A 1.374(6) C2B C3B 1.371(14) C3A C4A 1.398(6) C3B C4B 1.371(14) C4A C5A 1.400(6) C4A C7A 1.468(6) C4B C5B 1.370(14) C4B C7B 1.48(2) C5A C6A 1.371(6) C5B C6B 1.350(14) C7A C8A 1.335(6) C7B C8B 1.33(2) C8A C14A 1.479(5) C8B C14A 1.599(17) C10A C11A 1.495(4) C10A C20A 1.344(4) C10A C31A 1.507(4) C11A C12A 1.393(4) C11A C16A 1.397(4) C12A C13A 1.393(4) C13A C14A 1.402(5) C14A C15A 1.382(5) C15A C16A 1.381(4) C20A C21A 1.489(4) C20A C41A 1.504(4) C21A C22A 1.391(4) C21A C26A 1.405(4) C22A C23A 1.384(4) C23A C24A 1.385(4) C24A C25A 1.379(5) C25A C26A 1.380(5) C31A C32A 1.399(4) C31A C36A 1.395(4) C32A C33A 1.385(5) C33A C34A 1.371(5) C34A C35A 1.407(5) C35A C36A 1.379(4) C41A C42A 1.390(4) C41A C46A 1.396(4) C42A C43A 1.385(4) C43A C44A 1.375(5) C44A C45A 1.374(5) C45A C46A 1.385(5) 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 N1 C2 C3 C4 0.0(5) C1 N1 C2 C3 -179.3(3) C1 N1 C6 C5 179.4(3) C2 N1 C6 C5 -0.1(5) C2 C3 C4 C5 -0.5(4) C2 C3 C4 C7 -179.7(3) C3 C4 C5 C6 0.7(4) C3 C4 C7 C8 160.3(3) C4 C5 C6 N1 -0.4(5) C4 C7 C8 C14 179.8(3) C5 C4 C7 C8 -18.8(5) C6 N1 C2 C3 0.3(5) C7 C4 C5 C6 179.8(3) C7 C8 C14 C13 163.7(3) C7 C8 C14 C15 -16.5(4) C8 C14 C15 C16 179.9(3) C10 C11 C12 C13 178.8(3) C10 C11 C16 C15 -177.0(3) C10 C20 C21 C22 -45.4(4) C10 C20 C21 C26 134.0(3) C10 C20 C41 C42 -46.5(4) C10 C20 C41 C46 135.2(3) C10 C31 C32 C33 -178.3(3) C10 C31 C36 C35 179.1(3) C11 C10 C20 C21 -7.8(4) C11 C10 C20 C41 169.5(3) C11 C10 C31 C32 -40.7(4) C11 C10 C31 C36 138.9(3) C11 C12 C13 C14 -2.7(5) C12 C11 C16 C15 0.5(4) C12 C13 C14 C8 -178.0(3) C12 C13 C14 C15 2.1(4) C13 C14 C15 C16 -0.3(4) C14 C15 C16 C11 -1.0(4) C16 C11 C12 C13 1.4(4) C20 C10 C11 C12 124.0(3) C20 C10 C11 C16 -58.6(4) C20 C10 C31 C32 137.1(3) C20 C10 C31 C36 -43.3(4) C20 C21 C22 C23 176.3(3) C20 C21 C26 C25 -176.1(3) C20 C41 C42 C43 179.0(3) C20 C41 C46 C45 179.9(3) C21 C20 C41 C42 130.9(3) C21 C20 C41 C46 -47.4(4) C21 C22 C23 C24 0.9(6) C22 C21 C26 C25 3.3(4) C22 C23 C24 C25 1.2(6) C23 C24 C25 C26 -1.0(5) C24 C25 C26 C21 -1.3(5) C26 C21 C22 C23 -3.1(5) C31 C10 C11 C12 -58.2(4) C31 C10 C11 C16 119.2(3) C31 C10 C20 C21 174.6(3) C31 C10 C20 C41 -8.1(4) C31 C32 C33 C34 -1.6(5) C32 C31 C36 C35 -1.2(4) C32 C33 C34 C35 0.2(5) C33 C34 C35 C36 0.6(5) C34 C35 C36 C31 -0.1(4) C36 C31 C32 C33 2.0(4) C41 C20 C21 C22 137.2(3) C41 C20 C21 C26 -43.4(4) C41 C42 C43 C44 1.6(4) C42 C41 C46 C45 1.4(4) C42 C43 C44 C45 0.7(4) C43 C44 C45 C46 -1.9(5) C44 C45 C46 C41 0.8(5) C46 C41 C42 C43 -2.6(4) N1A C2A C3A C4A 2.0(7) N1A C2B C3B C4B 0(3) C1A N1A C2A C3A -177.0(4) C1A N1A C2B C3B -179.4(12) C1A N1A C6A C5A 175.2(5) C1A N1A C6B C5B -179.5(17) C2A N1A C6A C5A -1.5(10) C2A C3A C4A C5A -2.3(6) C2A C3A C4A C7A 174.2(4) C2B N1A C6B C5B -1(3) C2B C3B C4B C5B -3(2) C2B C3B C4B C7B 176.6(17) C3A C4A C5A C6A 0.7(7) C3A C4A C7A C8A 174.4(4) C3B C4B C5B C6B 5(3) C3B C4B C7B C8B -24(2) C4A C5A C6A N1A 1.2(10) C4A C7A C8A C14A 174.5(4) C4B C5B C6B N1A -3(3) C4B C7B C8B C14A -176.4(12) C5A C4A C7A C8A -9.3(6) C5B C4B C7B C8B 155.9(15) C6A N1A C2A C3A -0.1(9) C6B N1A C2B C3B 3(3) C7A C4A C5A C6A -175.7(5) C7A C8A C14A C13A -27.6(6) C7A C8A C14A C15A 155.0(4) C7B C4B C5B C6B -174.9(18) C7B C8B C14A C13A 169.0(10) C7B C8B C14A C15A -20.5(17) C8A C14A C15A C16A 179.4(3) C8B C14A C15A C16A -167.5(9) C10A C11A C12A C13A -173.9(3) C10A C11A C16A C15A 175.3(3) C10A C20A C21A C22A -45.7(4) C10A C20A C21A C26A 137.5(3) C10A C20A C41A C42A -62.6(4) C10A C20A C41A C46A 119.1(3) C10A C31A C32A C33A 176.8(3) C10A C31A C36A C35A -175.4(3) C11A C10A C20A C21A -5.3(5) C11A C10A C20A C41A 174.8(3) C11A C10A C31A C32A 133.1(3) C11A C10A C31A C36A -47.1(3) C11A C12A C13A C14A -1.0(4) C12A C11A C16A C15A -0.3(4) C12A C13A C14A C8A -177.9(3) C12A C13A C14A C8B 173.0(6) C12A C13A C14A C15A -0.6(5) C13A C14A C15A C16A 1.8(5) C14A C15A C16A C11A -1.3(5) C16A C11A C12A C13A 1.5(4) C20A C10A C11A C12A -54.1(4) C20A C10A C11A C16A 130.6(3) C20A C10A C31A C32A -49.6(4) C20A C10A C31A C36A 130.3(3) C20A C21A C22A C23A -176.6(3) C20A C21A C26A C25A 177.8(3) C20A C41A C42A C43A -179.1(3) C20A C41A C46A C45A -178.7(3) C21A C20A C41A C42A 117.4(3) C21A C20A C41A C46A -60.9(4) C21A C22A C23A C24A -0.6(4) C22A C21A C26A C25A 0.9(4) C22A C23A C24A C25A 0.0(4) C23A C24A C25A C26A 1.1(5) C24A C25A C26A C21A -1.6(5) C26A C21A C22A C23A 0.2(4) C31A C10A C11A C12A 123.2(3) C31A C10A C11A C16A -52.2(3) C31A C10A C20A C21A 177.7(3) C31A C10A C20A C41A -2.3(4) C31A C32A C33A C34A -0.4(5) C32A C31A C36A C35A 4.4(4) C32A C33A C34A C35A 2.6(5) C33A C34A C35A C36A -1.3(5) C34A C35A C36A C31A -2.3(4) C36A C31A C32A C33A -3.1(4) C41A C20A C21A C22A 134.2(3) C41A C20A C21A C26A -42.5(4) C41A C42A C43A C44A -1.9(5) C42A C41A C46A C45A 3.0(5) C42A C43A C44A C45A 2.5(5) C43A C44A C45A C46A -0.3(5) C44A C45A C46A C41A -2.4(5) C46A C41A C42A C43A -0.8(5)