#------------------------------------------------------------------------------ #$Date: 2021-08-13 00:22:21 +0300 (Fri, 13 Aug 2021) $ #$Revision: 268048 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/43/1564343.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_1564343 loop_ _publ_author_name 'Taniguchi, Yoshimasa' 'Miwa, Mayuka' 'Kitada, Naoki' _publ_section_title ; Crystalline sponge X-ray analysis coupled with supercritical fluid chromatography: a novel analytical platform for the rapid separation, isolation, and characterization of analytes. ; _journal_name_full 'The Analyst' _journal_paper_doi 10.1039/d1an00948f _journal_year 2021 _chemical_formula_moiety ; (C48 H30 Br2 Cu2 N6 O12), 1.786(C12 H10 O), 0.216(C O), 0.216(C H3 O) ; _chemical_formula_sum 'C69.86 H48.51 Br2 Cu2 N6 O14.22' _chemical_formula_weight 1486.41 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2021-02-11 deposited with the CCDC. 2021-02-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 115.897(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 31.9635(7) _cell_length_b 7.78000(10) _cell_length_c 30.6494(6) _cell_measurement_reflns_used 20597 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 74.4580 _cell_measurement_theta_min 3.1910 _cell_volume 6856.4(3) _computing_cell_refinement 'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)' _computing_molecular_graphics 'shelXle (Hubschle et al., 2011)' _computing_publication_material 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 100.00(10) _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.951 _diffrn_measurement_device_type 'XtaLAB Synergy R, HyPix' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.058 _diffrn_reflns_av_unetI/netI 0.0141 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.951 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_number 56167 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.951 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 75.207 _diffrn_reflns_theta_min 2.887 _diffrn_source 'Rotating-anode X-ray tube' _exptl_absorpt_coefficient_mu 2.696 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.36587 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.75a (Rigaku Oxford Diffraction, 2020) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.440 _exptl_crystal_description block _exptl_crystal_F_000 3006 _exptl_crystal_size_max 0.589 _exptl_crystal_size_mid 0.252 _exptl_crystal_size_min 0.161 _refine_diff_density_max 0.910 _refine_diff_density_min -0.997 _refine_diff_density_rms 0.132 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1141 _refine_ls_number_reflns 19834 _refine_ls_number_restraints 1404 _refine_ls_restrained_S_all 1.108 _refine_ls_R_factor_all 0.0659 _refine_ls_R_factor_gt 0.0631 _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^)+(0.0759P)^2^+34.8898P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1904 _refine_ls_wR_factor_ref 0.1926 _reflns_Friedel_coverage 0.000 _reflns_number_gt 18669 _reflns_number_total 19834 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1an00948f1.cif _cod_data_source_block 5a@2 _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 1564343 _shelx_shelxl_version_number 2018/3 _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_min 0.300 _shelx_estimated_absorpt_t_max 0.671 _shelx_res_file ; TITL exp_1467_twin1_hklf4_a.res in P2(1)/c exp_1467_twin1_hklf5.res created by SHELXL-2018/3 at 18:14:06 on 02-Jan-2021 REM Old TITL exp_1467_twin1_hklf4 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.194, Rweak 0.019, Alpha 0.064 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C53 N9 O17 Cu2 Br2 CELL 1.54184 31.9635 7.7800 30.6494 90.000 115.897 90.000 ZERR 5.000 0.0007 0.0001 0.0006 0.000 0.003 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O CU BR UNIT 279.48 194.046 24 56.8658 8 8 L.S. 10 BOND LIST 4 FMAP 2 TEMP -173 ACTA SIZE 0.161 0.252 0.589 PLAN 200 WGHT 0.075900 34.889801 BASF 0.39225 FVAR 1.90816 0.76284 0.37193 0.41368 0.21593 BR1 6 0.732944 -0.046098 1.114431 11.00000 0.05791 0.01796 = 0.03242 -0.00097 0.00660 -0.00414 O1 4 0.654460 0.799403 0.921579 11.00000 0.08661 0.01834 = 0.02741 0.00078 0.01098 -0.00169 N1 3 0.723846 0.371133 1.057556 11.00000 0.02994 0.01837 = 0.02000 0.00072 0.00998 0.00044 CU1 5 0.753149 0.256424 1.122681 11.00000 0.02442 0.01967 = 0.02028 -0.00009 0.00686 0.00269 C1 1 0.678686 0.543220 0.969221 11.00000 0.03037 0.02163 = 0.02446 0.00145 0.00901 -0.00226 CU2 5 0.256720 0.718876 0.615029 11.00000 0.02238 0.01975 = 0.01998 -0.00020 0.00703 -0.00060 BR2 6 0.235392 1.021758 0.603091 11.00000 0.03156 0.01863 = 0.03222 0.00027 0.00746 0.00426 O2 4 0.636919 0.542109 0.884041 11.00000 0.02779 0.02059 = 0.01824 0.00065 0.00769 0.00048 N2 3 0.728993 1.114407 0.666984 11.00000 0.02735 0.02156 = 0.02563 -0.00010 0.01342 -0.00137 C2 1 0.682827 0.366942 0.970281 11.00000 0.03343 0.02528 = 0.01840 -0.00169 0.00865 0.00135 AFIX 43 H2 2 0.670582 0.302365 0.941038 11.00000 -1.20000 AFIX 0 C3 1 0.705280 0.284969 1.014970 11.00000 0.03330 0.01929 = 0.02055 0.00018 0.00942 0.00241 AFIX 43 H3 2 0.707659 0.163193 1.015565 11.00000 -1.20000 AFIX 0 N3 3 0.325453 0.711196 0.661381 11.00000 0.02373 0.01805 = 0.02150 0.00296 0.00781 0.00027 O3 4 0.640866 0.870035 0.751968 11.00000 0.03139 0.02299 = 0.02963 0.00296 0.02090 -0.00044 C4 1 0.719835 0.543181 1.055428 11.00000 0.06069 0.01917 = 0.02055 -0.00242 0.00624 -0.00371 AFIX 43 H4 2 0.733254 0.606349 1.084888 11.00000 -1.20000 AFIX 0 O4 4 0.677214 0.635252 0.742801 11.00000 0.06169 0.02475 = 0.06011 0.00852 0.04536 0.00632 N4 3 0.233540 0.604741 0.549118 11.00000 0.02820 0.02188 = 0.01893 0.00088 0.00920 0.00097 O5 4 0.496622 0.679563 0.743014 11.00000 0.01926 0.04088 = 0.02362 -0.00252 0.00923 -0.00124 N5 3 0.223714 -0.096885 0.151304 11.00000 0.03057 0.01889 = 0.02722 0.00127 0.01685 0.00281 C5 1 0.697189 0.632634 1.012569 11.00000 0.06029 0.01829 = 0.02808 0.00078 0.01093 -0.00220 AFIX 43 H5 2 0.694341 0.754132 1.012831 11.00000 -1.20000 AFIX 0 O6 4 0.483201 0.832320 0.797929 11.00000 0.02566 0.04956 = 0.03703 -0.01799 0.00410 0.00448 N6 3 -0.177273 0.265872 0.166120 11.00000 0.02091 0.01957 = 0.02153 -0.00264 0.00693 0.00261 C6 1 0.655953 0.645564 0.923470 11.00000 0.03999 0.02380 = 0.02347 0.00053 0.01237 -0.00177 C7 1 0.614827 0.625950 0.839082 11.00000 0.02577 0.02134 = 0.02055 0.00107 0.00767 0.00209 O7 4 0.173620 0.176095 0.413426 11.00000 0.06302 0.01972 = 0.02251 -0.00146 0.00684 -0.00087 C8 1 0.641244 0.703456 0.818907 11.00000 0.02097 0.02024 = 0.02245 -0.00246 0.01014 0.00001 AFIX 43 H8 2 0.674225 0.706891 0.835538 11.00000 -1.20000 AFIX 0 O8 4 0.137793 0.423751 0.378480 11.00000 0.02361 0.02524 = 0.01807 -0.00231 0.00531 -0.00131 C9 1 0.617281 0.776061 0.773172 11.00000 0.02423 0.02441 = 0.02421 -0.00342 0.01456 -0.00206 O9 4 0.136232 0.111657 0.241582 11.00000 0.02893 0.02460 = 0.02405 0.00028 0.01661 0.00168 C10 1 0.569264 0.771419 0.748040 11.00000 0.02631 0.02422 = 0.02324 -0.00042 0.01279 0.00106 AFIX 43 H10 2 0.553540 0.821095 0.716709 11.00000 -1.20000 AFIX 0 O10 4 0.157038 0.359888 0.219251 11.00000 0.07137 0.02443 = 0.05723 -0.00086 0.04770 0.00117 C11 1 0.545168 0.691697 0.770350 11.00000 0.02058 0.02684 = 0.02636 -0.00523 0.00903 -0.00079 O11 4 -0.005599 0.298363 0.240836 11.00000 0.01768 0.04225 = 0.02146 0.00057 0.00601 0.00134 C12 1 0.566504 0.618766 0.816236 11.00000 0.02492 0.02611 = 0.02696 -0.00208 0.01145 0.00033 AFIX 43 H12 2 0.549116 0.566981 0.831160 11.00000 -1.20000 AFIX 0 O12 4 -0.016914 0.142860 0.296597 11.00000 0.02972 0.06473 = 0.04397 0.02855 0.00396 -0.00574 C13 1 0.669567 0.785095 0.737357 11.00000 0.03109 0.02749 = 0.02753 -0.00022 0.01389 0.00026 C14 1 0.689623 0.904803 0.713285 11.00000 0.03234 0.02420 = 0.02349 -0.00063 0.01547 -0.00266 C16 1 0.741852 0.952363 0.678187 11.00000 0.02475 0.02975 = 0.02685 0.00235 0.01349 0.00410 AFIX 43 H16 2 0.765687 0.909107 0.670600 11.00000 -1.20000 AFIX 0 C15 1 0.722968 0.841457 0.700209 11.00000 0.03387 0.01937 = 0.02569 0.00618 0.01456 0.00489 AFIX 43 H15 2 0.732679 0.724900 0.706171 11.00000 -1.20000 AFIX 0 C18 1 0.676426 1.075996 0.703202 11.00000 0.04280 0.02703 = 0.04033 0.00338 0.02874 0.00427 AFIX 43 H18 2 0.653782 1.123562 0.711958 11.00000 -1.20000 AFIX 0 C17 1 0.696708 1.176913 0.680169 11.00000 0.04023 0.02442 = 0.04361 0.00161 0.02817 -0.00079 AFIX 43 H17 2 0.687561 1.293822 0.673466 11.00000 -1.20000 AFIX 0 C19 1 0.468953 0.756500 0.760618 11.00000 0.02288 0.02010 = 0.03448 0.00480 0.01114 0.00157 C20 1 0.419399 0.732199 0.726171 11.00000 0.02439 0.01816 = 0.02354 0.00250 0.00868 0.00027 C21 1 0.405143 0.637910 0.683333 11.00000 0.02387 0.01883 = 0.02731 0.00043 0.01164 0.00167 AFIX 43 H21 2 0.427209 0.580357 0.675531 11.00000 -1.20000 AFIX 0 C22 1 0.357717 0.630081 0.652204 11.00000 0.02668 0.01665 = 0.02046 -0.00024 0.00610 0.00144 AFIX 43 H22 2 0.347904 0.564422 0.623277 11.00000 -1.20000 AFIX 0 C23 1 0.339405 0.802129 0.702162 11.00000 0.02304 0.01553 = 0.02605 0.00167 0.01063 0.00078 AFIX 43 H23 2 0.316510 0.861360 0.708268 11.00000 -1.20000 AFIX 0 C24 1 0.385570 0.815307 0.736309 11.00000 0.02582 0.02047 = 0.02169 -0.00081 0.00776 0.00162 AFIX 43 H24 2 0.393964 0.878309 0.765489 11.00000 -1.20000 AFIX 0 C25 1 0.189889 0.429816 0.461346 11.00000 0.02950 0.02433 = 0.01838 -0.00045 0.00785 -0.00185 C26 1 0.183817 0.605304 0.463738 11.00000 0.03368 0.02439 = 0.01819 0.00219 0.00813 0.00028 AFIX 43 H26 2 0.164924 0.668415 0.435385 11.00000 -1.20000 AFIX 0 C27 1 0.205676 0.686784 0.507996 11.00000 0.03259 0.02323 = 0.01984 0.00207 0.00979 0.00103 AFIX 43 H27 2 0.200815 0.806668 0.509506 11.00000 -1.20000 AFIX 0 C28 1 0.240241 0.436306 0.546256 11.00000 0.03850 0.02273 = 0.01943 -0.00046 0.00397 0.00280 AFIX 43 H28 2 0.260607 0.377549 0.574852 11.00000 -1.20000 AFIX 0 C29 1 0.218910 0.343319 0.503588 11.00000 0.04599 0.01775 = 0.02646 -0.00228 0.00727 -0.00112 AFIX 43 H29 2 0.223968 0.223136 0.503148 11.00000 -1.20000 AFIX 0 C30 1 0.167325 0.327148 0.416276 11.00000 0.03223 0.02385 = 0.02091 0.00165 0.00858 -0.00380 C31 1 0.114460 0.343739 0.333510 11.00000 0.02587 0.01849 = 0.01956 0.00185 0.00884 -0.00034 C32 1 0.139075 0.269497 0.310531 11.00000 0.02193 0.01871 = 0.02047 0.00097 0.00770 -0.00119 AFIX 43 H32 2 0.172103 0.266303 0.325500 11.00000 -1.20000 AFIX 0 C33 1 0.113338 0.200317 0.264820 11.00000 0.02567 0.02052 = 0.02490 0.00055 0.01622 0.00274 C34 1 0.065119 0.206254 0.241465 11.00000 0.02165 0.02452 = 0.01994 -0.00224 0.00758 -0.00131 AFIX 43 H34 2 0.048169 0.159486 0.209934 11.00000 -1.20000 AFIX 0 C35 1 0.043010 0.283050 0.266116 11.00000 0.01796 0.02730 = 0.02378 0.00064 0.00658 0.00219 C36 1 0.066259 0.352158 0.312532 11.00000 0.02503 0.02518 = 0.02101 0.00044 0.01094 -0.00052 AFIX 43 H36 2 0.050003 0.402298 0.328921 11.00000 -1.20000 AFIX 0 C37 1 0.156758 0.206671 0.219441 11.00000 0.03037 0.02569 = 0.02606 0.00069 0.01435 0.00004 C38 1 0.178829 0.094940 0.195614 11.00000 0.02915 0.02496 = 0.02314 -0.00200 0.01393 0.00054 C39 1 0.205107 0.175097 0.175511 11.00000 0.05560 0.01938 = 0.04182 -0.00441 0.03362 -0.00851 AFIX 43 H39 2 0.208110 0.296693 0.176553 11.00000 -1.20000 AFIX 0 C40 1 0.226639 0.077523 0.154190 11.00000 0.04757 0.02489 = 0.04387 -0.00280 0.03273 -0.00487 AFIX 43 H40 2 0.244565 0.134466 0.140698 11.00000 -1.20000 AFIX 0 C41 1 0.198311 -0.173193 0.171120 11.00000 0.03943 0.02204 = 0.03992 -0.00224 0.02337 -0.00372 AFIX 43 H41 2 0.195780 -0.294940 0.169814 11.00000 -1.20000 AFIX 0 C42 1 0.175548 -0.081490 0.193479 11.00000 0.03214 0.02816 = 0.03435 -0.00002 0.02305 -0.00128 AFIX 43 H42 2 0.157971 -0.140142 0.207087 11.00000 -1.20000 AFIX 0 C43 1 -0.032028 0.222178 0.259477 11.00000 0.02481 0.02378 = 0.02709 -0.00181 0.00803 -0.00282 C44 1 -0.082599 0.245451 0.226900 11.00000 0.02484 0.01715 = 0.02218 -0.00209 0.00899 0.00119 C45 1 -0.098403 0.338138 0.183901 11.00000 0.02531 0.02392 = 0.02532 -0.00063 0.01302 -0.00153 AFIX 43 H45 2 -0.077288 0.395785 0.174698 11.00000 -1.20000 AFIX 0 C46 1 -0.146255 0.343923 0.154653 11.00000 0.03059 0.01595 = 0.02268 0.00161 0.00933 0.00162 AFIX 43 H46 2 -0.157288 0.406543 0.125114 11.00000 -1.20000 AFIX 0 C48 1 -0.114668 0.165002 0.239408 11.00000 0.02645 0.02017 = 0.02311 0.00333 0.00837 0.00232 AFIX 43 H48 2 -0.104701 0.102852 0.268936 11.00000 -1.20000 AFIX 0 C47 1 -0.160965 0.177320 0.208214 11.00000 0.02597 0.02149 = 0.02642 -0.00285 0.01278 -0.00250 AFIX 43 H47 2 -0.182732 0.120593 0.216640 11.00000 -1.20000 AFIX 0 PART 1 21.0 SAME C201 > O213 SAME C301 > O313 SAME C401 > O413 SIMU C101 > O113 C101 1 0.046973 0.464240 0.450018 21.00000 0.05213 0.07119 = 0.05679 0.02266 0.03008 0.00143 C102 1 0.069892 0.550830 0.491556 21.00000 0.07667 0.06952 = 0.06822 0.01840 0.05082 0.00635 AFIX 43 H102 2 0.057740 0.659966 0.493978 21.00000 -1.20000 AFIX 0 C103 1 0.110202 0.495926 0.531945 21.00000 0.04699 0.07910 = 0.06581 0.02821 0.02528 -0.00869 AFIX 43 H103 2 0.125752 0.567116 0.559555 21.00000 -1.20000 AFIX 0 C104 1 0.126095 0.330325 0.529123 21.00000 0.03939 0.08850 = 0.05272 0.01751 0.00884 -0.00618 AFIX 43 H104 2 0.153311 0.288121 0.555449 21.00000 -1.20000 AFIX 0 C105 1 0.102693 0.224738 0.488173 21.00000 0.03618 0.06932 = 0.06396 0.02292 0.01660 -0.00294 C106 1 0.063243 0.298332 0.448735 21.00000 0.03819 0.07093 = 0.05202 0.03280 0.01987 0.00348 C107 1 0.039288 0.183039 0.407664 21.00000 0.03578 0.08098 = 0.05115 0.03185 0.02182 0.01022 AFIX 43 H107 2 0.012682 0.223743 0.380348 21.00000 -1.20000 AFIX 0 C108 1 0.054880 0.008801 0.407363 21.00000 0.04617 0.08602 = 0.05967 0.00998 0.03131 0.01622 AFIX 43 H108 2 0.038425 -0.065231 0.380651 21.00000 -1.20000 AFIX 0 C109 1 0.094086 -0.047366 0.446636 21.00000 0.04732 0.05057 = 0.07003 0.02427 0.01932 0.00504 AFIX 43 H109 2 0.105073 -0.160565 0.446271 21.00000 -1.20000 AFIX 0 C110 1 0.117061 0.051717 0.485050 21.00000 0.03997 0.05831 = 0.06489 0.01982 0.01490 0.00976 AFIX 43 H110 2 0.143875 0.006846 0.511341 21.00000 -1.20000 AFIX 0 C111 1 0.007936 0.539046 0.408551 21.00000 0.06881 0.09838 = 0.06403 0.03300 0.04440 0.03756 C112 1 -0.027629 0.652107 0.417050 21.00000 0.12952 0.22696 = 0.11371 0.09372 0.09155 0.10113 AFIX 33 H11A 2 -0.020450 0.650821 0.451575 21.00000 -1.50000 H11B 2 -0.025929 0.770311 0.406890 21.00000 -1.50000 H11C 2 -0.059040 0.606822 0.398069 21.00000 -1.50000 AFIX 0 O113 4 0.003473 0.527903 0.366987 21.00000 0.06794 0.07727 = 0.04896 0.02952 0.03377 0.03957 PART 0 PART 1 31.0 SUMP 1 0.001 1 3 1 4 1 5 SIMU 0.01 0.02 4 C201 > O213 SADI C211 C202 C211 C206 FLAT C201 C202 C206 C211 SADI C201 C206 C201 C202 C201 1 0.457690 0.475151 0.911206 31.00000 0.07312 0.12905 = 0.06602 0.03028 0.02121 0.00010 C202 1 0.438357 0.573823 0.932920 31.00000 0.07688 0.12827 = 0.07012 0.02835 0.01641 -0.00221 AFIX 43 H202 2 0.453849 0.676381 0.948448 31.00000 -1.20000 AFIX 0 C203 1 0.394526 0.530802 0.933794 31.00000 0.07138 0.12550 = 0.06466 0.03089 0.02045 0.00132 AFIX 43 H203 2 0.378646 0.611848 0.944325 31.00000 -1.20000 AFIX 0 C204 1 0.376614 0.367701 0.918768 31.00000 0.06603 0.12806 = 0.06123 0.02948 0.02212 0.00169 AFIX 43 H204 2 0.348971 0.334020 0.920844 31.00000 -1.20000 AFIX 0 C205 1 0.398617 0.251500 0.900542 31.00000 0.06806 0.12775 = 0.06129 0.02951 0.02232 0.00018 C206 1 0.440735 0.312143 0.901947 31.00000 0.07169 0.12804 = 0.06369 0.03086 0.02065 0.00075 C207 1 0.469707 0.188837 0.890575 31.00000 0.07267 0.13050 = 0.06407 0.02871 0.02181 -0.00017 AFIX 43 H207 2 0.500675 0.213835 0.895937 31.00000 -1.20000 AFIX 0 C208 1 0.446882 0.024688 0.870343 31.00000 0.07257 0.12785 = 0.05866 0.02767 0.02517 -0.00074 AFIX 43 H208 2 0.462162 -0.054440 0.858546 31.00000 -1.20000 AFIX 0 C209 1 0.405425 -0.017602 0.867896 31.00000 0.06912 0.12941 = 0.06183 0.02833 0.01810 -0.00173 AFIX 43 H209 2 0.390148 -0.118388 0.850897 31.00000 -1.20000 AFIX 0 C210 1 0.385948 0.076362 0.888254 31.00000 0.06896 0.12500 = 0.06079 0.02800 0.02035 0.00140 AFIX 43 H210 2 0.362365 0.027525 0.895332 31.00000 -1.20000 AFIX 0 C211 1 0.492570 0.527573 0.895488 31.00000 0.07102 0.12592 = 0.05988 0.03367 0.02474 -0.00865 C212 1 0.538588 0.598684 0.933789 31.00000 0.09684 0.13734 = 0.08440 0.03221 0.01289 -0.00877 AFIX 33 H21A 2 0.533813 0.646190 0.960886 31.00000 -1.50000 H21B 2 0.561624 0.506003 0.945638 31.00000 -1.50000 H21C 2 0.549812 0.689422 0.919382 31.00000 -1.50000 AFIX 0 O213 4 0.493416 0.463284 0.859056 31.00000 0.07451 0.11413 = 0.06602 0.03027 0.01951 -0.02596 PART 0 PART -1 -21.0 SIMU 0.01 0.02 4 C301 > O313 C301 1 -0.062176 0.027120 0.491191 -21.00000 0.04563 0.07190 = 0.04393 0.01599 0.02270 0.00518 C302 1 -0.099486 0.009809 0.501326 -21.00000 0.04687 0.07278 = 0.04589 0.01608 0.02244 0.00471 AFIX 43 H302 2 -0.130028 0.010863 0.475596 -21.00000 -1.20000 AFIX 0 C303 1 -0.093171 -0.010007 0.550447 -21.00000 0.04644 0.07280 = 0.04616 0.01560 0.02298 0.00569 AFIX 43 H303 2 -0.119220 -0.012215 0.557640 -21.00000 -1.20000 AFIX 0 C304 1 -0.048377 -0.025852 0.587173 -21.00000 0.04479 0.07213 = 0.04584 0.01552 0.02239 0.00548 AFIX 43 H304 2 -0.043995 -0.062230 0.618470 -21.00000 -1.20000 AFIX 0 C305 1 -0.009343 0.010905 0.578953 -21.00000 0.04630 0.07140 = 0.04504 0.01683 0.02276 0.00331 C306 1 -0.019124 0.014312 0.528440 -21.00000 0.04467 0.07169 = 0.04521 0.01582 0.02210 0.00536 C307 1 0.022023 -0.002958 0.519150 -21.00000 0.04017 0.07004 = 0.03965 0.01794 0.03066 0.00151 AFIX 43 H307 2 0.018993 -0.018483 0.487157 -21.00000 -1.20000 AFIX 0 C308 1 0.067423 0.004424 0.560331 -21.00000 0.04814 0.07024 = 0.04425 0.01602 0.02325 0.00042 AFIX 43 H308 2 0.094099 0.021215 0.554698 -21.00000 -1.20000 AFIX 0 C309 1 0.073003 -0.011737 0.606278 -21.00000 0.04478 0.06969 = 0.04334 0.01682 0.01928 0.00225 AFIX 43 H309 2 0.103002 -0.035075 0.631501 -21.00000 -1.20000 AFIX 0 C310 1 0.037651 0.004307 0.616545 -21.00000 0.04769 0.07179 = 0.04445 0.01495 0.02215 0.00424 AFIX 43 H310 2 0.043017 0.011799 0.649514 -21.00000 -1.20000 AFIX 0 C311 1 -0.069790 0.055004 0.441699 -21.00000 0.04645 0.07341 = 0.04560 0.01469 0.02429 0.00557 C312 1 -0.109984 -0.035081 0.400747 -21.00000 0.04892 0.07905 = 0.03977 0.00909 0.02259 0.01953 AFIX 33 H31A 2 -0.124421 -0.116892 0.414363 -21.00000 -1.50000 H31B 2 -0.133082 0.050277 0.381098 -21.00000 -1.50000 H31C 2 -0.098374 -0.096733 0.380367 -21.00000 -1.50000 AFIX 0 O313 4 -0.048156 0.161437 0.430553 -21.00000 0.04592 0.07874 = 0.05417 0.01696 0.01912 0.00943 PART 0 PART 2 41.0 SIMU 0.01 0.02 4 C401 > O413 ISOR 0.05 0.05 C401 > O413 SADI C411 C402 C411 C406 FLAT C401 C411 C412 O413 FLAT C401 C402 C406 C411 SADI C401 C402 C401 C406 FREE O413 H407 C401 1 0.458417 0.832919 1.088926 41.00000 0.12963 0.23833 = 0.08746 -0.02514 0.07536 -0.06926 C402 1 0.448784 0.992750 1.087333 41.00000 0.12924 0.23870 = 0.08684 -0.02558 0.07741 -0.06795 AFIX 43 H402 2 0.463611 1.061923 1.115510 41.00000 -1.20000 AFIX 0 C403 1 0.415357 1.068137 1.042689 41.00000 0.12899 0.24054 = 0.08959 -0.02647 0.07822 -0.06686 AFIX 43 H403 2 0.406884 1.185542 1.041896 41.00000 -1.20000 AFIX 0 C404 1 0.395839 0.970495 1.001458 41.00000 0.12668 0.23738 = 0.08782 -0.02447 0.07558 -0.07024 AFIX 43 H404 2 0.374629 1.022410 0.972020 41.00000 -1.20000 AFIX 0 C405 1 0.406378 0.797185 1.001740 41.00000 0.12769 0.23930 = 0.08846 -0.02346 0.07704 -0.07132 C406 1 0.438245 0.740772 1.047755 41.00000 0.12774 0.23880 = 0.08784 -0.02328 0.07720 -0.07206 C407 1 0.461538 0.571064 1.058293 41.00000 0.12873 0.23718 = 0.08756 -0.02530 0.07607 -0.07215 AFIX 43 H407 2 0.486268 0.540001 1.088538 41.00000 -1.20000 AFIX 0 C408 1 0.441605 0.457680 1.016224 41.00000 0.13066 0.23865 = 0.08911 -0.02387 0.07440 -0.07354 AFIX 43 H408 2 0.449114 0.338769 1.019827 41.00000 -1.20000 AFIX 0 C409 1 0.412476 0.520435 0.972054 41.00000 0.12992 0.23690 = 0.08538 -0.02506 0.07361 -0.07246 AFIX 43 H409 2 0.405974 0.450203 0.944482 41.00000 -1.20000 AFIX 0 C410 1 0.393049 0.669580 0.965159 41.00000 0.12647 0.23909 = 0.08708 -0.02437 0.07489 -0.07194 AFIX 43 H410 2 0.368695 0.695066 0.934144 41.00000 -1.20000 AFIX 0 C411 1 0.497286 0.743481 1.125108 41.00000 0.13336 0.24087 = 0.09294 -0.02360 0.07392 -0.07003 C412 1 0.542351 0.844754 1.135477 41.00000 0.14551 0.24325 = 0.10191 -0.02814 0.05963 -0.06321 AFIX 33 H41A 2 0.534303 0.960834 1.121955 41.00000 -1.50000 H41B 2 0.561478 0.852093 1.170588 41.00000 -1.50000 H41C 2 0.559799 0.785442 1.120451 41.00000 -1.50000 AFIX 0 O413 4 0.492266 0.591952 1.136152 41.00000 0.12253 0.22335 = 0.08944 -0.02000 0.08640 -0.08211 PART 0 PART 0 PART 3 51.0 DFIX 1.43 O601 C602 SIMU O601 C602 ISOR 0.1 0.1 O601 C602 O601 4 0.448227 1.023085 1.007800 51.00000 0.21441 0.13437 = 0.05236 0.03090 -0.00643 0.03582 C602 1 0.457996 1.146606 1.045363 51.00000 0.15569 0.10676 = 0.18123 -0.04186 -0.01711 0.02052 PART 0 PART 3 51.0 DFIX 1.43 O801 C802 SIMU 0.01 O801 C802 ISOR 0.01 0.01 O801 C802 O801 4 0.379257 0.167609 0.878254 51.00000 0.08039 0.08540 = 0.05982 0.00166 0.02965 -0.01035 C802 1 0.408955 0.050721 0.871686 51.00000 0.06161 0.04953 = 0.04507 0.01484 0.00631 -0.00777 AFIX 137 H80A 2 0.440725 0.068217 0.896848 51.00000 -1.50000 H80B 2 0.408166 0.068210 0.839670 51.00000 -1.50000 H80C 2 0.398893 -0.066601 0.873913 51.00000 -1.50000 PART 0 AFIX 0 HKLF 5 REM exp_1467_twin1_hklf4_a.res in P2(1)/c REM wR2 = 0.1926, GooF = S = 1.121, Restrained GooF = 1.108 for all data REM R1 = 0.0631 for 18669 Fo > 4sig(Fo) and 0.0659 for all 19834 data REM 1141 parameters refined using 1404 restraints END WGHT 0.0749 35.1309 REM Highest difference peak 0.910, deepest hole -0.997, 1-sigma level 0.132 Q1 1 0.7120 -0.0452 1.1177 11.00000 0.05 0.80 Q2 1 -0.0379 0.5298 0.3909 11.00000 0.05 0.80 Q3 1 0.4514 0.6107 0.8789 11.00000 0.05 0.80 Q4 1 0.4821 0.0178 0.9604 11.00000 0.05 0.76 Q5 1 0.0452 0.0595 0.5573 11.00000 0.05 0.73 Q6 1 0.0922 -0.0329 0.5994 11.00000 0.05 0.73 Q7 1 0.3952 0.5719 0.9675 11.00000 0.05 0.72 Q8 1 0.4800 0.5747 0.9181 11.00000 0.05 0.71 Q9 1 0.1008 0.6043 0.5426 11.00000 0.05 0.70 Q10 1 0.4683 0.5661 0.9287 11.00000 0.05 0.69 Q11 1 -0.0509 0.6787 0.3957 11.00000 0.05 0.68 Q12 1 0.3824 0.7772 0.9672 11.00000 0.05 0.66 Q13 1 0.3851 0.0311 0.9294 11.00000 0.05 0.66 Q14 1 0.2053 1.0306 0.6115 11.00000 0.05 0.65 Q15 1 -0.0264 0.7808 0.4408 11.00000 0.05 0.63 Q16 1 0.4908 1.0459 1.0022 11.00000 0.05 0.62 Q17 1 0.0244 0.6890 0.4816 11.00000 0.05 0.61 Q18 1 0.4293 0.9557 1.0650 11.00000 0.05 0.61 Q19 1 0.4499 0.6705 1.0495 11.00000 0.05 0.58 Q20 1 0.0864 0.6897 0.5472 11.00000 0.05 0.57 Q21 1 0.3770 -0.0724 0.9333 11.00000 0.05 0.55 Q22 1 0.4685 0.9073 1.0914 11.00000 0.05 0.55 Q23 1 0.4753 0.9951 0.9999 11.00000 0.05 0.54 Q24 1 0.0333 0.5672 0.4690 11.00000 0.05 0.54 Q25 1 0.4219 0.5902 0.9533 11.00000 0.05 0.54 Q26 1 -0.1197 0.1638 0.4186 11.00000 0.05 0.53 Q27 1 0.0149 0.5115 0.4394 11.00000 0.05 0.51 Q28 1 0.4560 0.5011 0.9566 11.00000 0.05 0.51 Q29 1 0.5220 0.6203 0.9684 11.00000 0.05 0.50 Q30 1 0.0512 0.7743 0.5270 11.00000 0.05 0.49 Q31 1 0.3962 1.0358 1.0257 11.00000 0.05 0.49 Q32 1 0.0421 0.7028 0.4990 11.00000 0.05 0.48 Q33 1 0.7599 0.1980 1.0820 11.00000 0.05 0.48 Q34 1 0.4251 0.0436 0.8657 11.00000 0.05 0.48 Q35 1 0.4493 1.0965 1.0093 11.00000 0.05 0.48 Q36 1 -0.0036 0.4395 0.4071 11.00000 0.05 0.47 Q37 1 0.4467 0.7946 1.0606 11.00000 0.05 0.46 Q38 1 0.0852 0.4713 0.5105 11.00000 0.05 0.46 Q39 1 -0.0777 0.2599 0.4205 11.00000 0.05 0.45 Q40 1 0.4534 1.0942 1.0890 11.00000 0.05 0.45 Q41 1 0.4746 0.5296 0.8503 11.00000 0.05 0.45 Q42 1 0.7892 0.2684 1.1203 11.00000 0.05 0.44 Q43 1 0.7256 0.0056 1.0306 11.00000 0.05 0.43 Q44 1 0.4442 1.0233 0.9683 11.00000 0.05 0.43 Q45 1 0.4763 0.6792 1.0987 11.00000 0.05 0.43 Q46 1 -0.1273 0.2787 0.3903 11.00000 0.05 0.42 Q47 1 0.5111 0.5975 0.9038 11.00000 0.05 0.41 Q48 1 0.7360 0.8739 1.0222 11.00000 0.05 0.41 Q49 1 0.2063 0.4040 0.3999 11.00000 0.05 0.41 Q50 1 0.1925 0.5183 0.3707 11.00000 0.05 0.41 Q51 1 0.2167 0.0150 0.1517 11.00000 0.05 0.41 Q52 1 0.4311 0.4551 0.9781 11.00000 0.05 0.41 Q53 1 0.4393 -0.1428 0.8727 11.00000 0.05 0.41 Q54 1 -0.1275 0.0738 0.4435 11.00000 0.05 0.40 Q55 1 0.4324 0.1794 0.9202 11.00000 0.05 0.40 Q56 1 -0.0976 -0.1333 0.4014 11.00000 0.05 0.40 Q57 1 0.4473 0.7393 0.9892 11.00000 0.05 0.39 Q58 1 0.2433 0.5887 0.6184 11.00000 0.05 0.39 Q59 1 0.4170 1.0007 0.9909 11.00000 0.05 0.39 Q60 1 0.4342 0.5220 1.0202 11.00000 0.05 0.39 Q61 1 0.7372 0.2820 0.9902 11.00000 0.05 0.39 Q62 1 0.7756 0.7778 0.7077 11.00000 0.05 0.39 Q63 1 0.1921 0.4049 0.2109 11.00000 0.05 0.39 Q64 1 0.1664 0.4538 0.1782 11.00000 0.05 0.39 Q65 1 0.2619 0.5943 0.6131 11.00000 0.05 0.38 Q66 1 0.4184 0.6147 0.8897 11.00000 0.05 0.38 Q67 1 0.2652 0.5889 0.5485 11.00000 0.05 0.38 Q68 1 0.2321 0.8826 0.5884 11.00000 0.05 0.38 Q69 1 0.7275 0.6022 1.0179 11.00000 0.05 0.38 Q70 1 0.2216 0.4110 0.1513 11.00000 0.05 0.38 Q71 1 0.2258 -0.1337 0.1874 11.00000 0.05 0.38 Q72 1 0.7687 1.1363 0.6704 11.00000 0.05 0.38 Q73 1 0.2313 0.4195 0.1967 11.00000 0.05 0.38 Q74 1 0.7199 0.5998 0.8211 11.00000 0.05 0.38 Q75 1 0.6391 0.9256 0.7104 11.00000 0.05 0.38 Q76 1 0.2548 0.9223 0.5801 11.00000 0.05 0.37 Q77 1 0.1230 0.4985 0.5862 11.00000 0.05 0.37 Q78 1 0.3766 0.2229 0.9298 11.00000 0.05 0.37 Q79 1 0.7433 -0.2079 1.1523 11.00000 0.05 0.37 Q80 1 0.4157 0.8055 1.0882 11.00000 0.05 0.37 Q81 1 0.4094 -0.0764 0.9328 11.00000 0.05 0.37 Q82 1 0.7511 1.0824 0.6887 11.00000 0.05 0.37 Q83 1 0.2188 0.4626 0.5558 11.00000 0.05 0.37 Q84 1 0.2656 0.2151 0.5911 11.00000 0.05 0.36 Q85 1 0.1970 0.3377 0.5137 11.00000 0.05 0.36 Q86 1 0.0067 -0.0772 0.5106 11.00000 0.05 0.36 Q87 1 0.2485 0.4048 0.2328 11.00000 0.05 0.36 Q88 1 0.2424 0.8782 0.5500 11.00000 0.05 0.36 Q89 1 0.7314 1.1481 0.6911 11.00000 0.05 0.36 Q90 1 0.7092 1.0546 0.6219 11.00000 0.05 0.36 Q91 1 0.2294 0.6935 0.6229 11.00000 0.05 0.36 Q92 1 0.4168 0.6727 1.0010 11.00000 0.05 0.36 Q93 1 0.7745 -0.0614 1.1084 11.00000 0.05 0.35 Q94 1 0.7525 0.3646 1.1215 11.00000 0.05 0.35 Q95 1 0.7007 0.6261 1.0802 11.00000 0.05 0.35 Q96 1 0.4622 0.1807 0.9504 11.00000 0.05 0.35 Q97 1 0.2498 1.0479 0.5591 11.00000 0.05 0.35 Q98 1 0.7039 -0.1823 1.1296 11.00000 0.05 0.35 Q99 1 0.2639 0.8138 0.7077 11.00000 0.05 0.35 Q100 1 0.7573 0.4202 1.0586 11.00000 0.05 0.35 Q101 1 0.7587 0.1571 1.1411 11.00000 0.05 0.34 Q102 1 0.4179 0.5179 0.8959 11.00000 0.05 0.34 Q103 1 0.1211 0.0767 0.5506 11.00000 0.05 0.34 Q104 1 0.3851 0.5371 0.9028 11.00000 0.05 0.34 Q105 1 0.2776 0.7451 0.6101 11.00000 0.05 0.34 Q106 1 0.4493 0.8332 0.9818 11.00000 0.05 0.34 Q107 1 0.7620 1.2799 0.7002 11.00000 0.05 0.34 Q108 1 0.7323 0.4990 0.7116 11.00000 0.05 0.34 Q109 1 0.0460 0.6085 0.4408 11.00000 0.05 0.34 Q110 1 0.7790 1.0168 0.6632 11.00000 0.05 0.34 Q111 1 0.1943 0.1322 0.4602 11.00000 0.05 0.34 Q112 1 0.4246 0.6942 0.8817 11.00000 0.05 0.34 Q113 1 0.1857 0.1213 0.1812 11.00000 0.05 0.33 Q114 1 0.6906 0.7502 0.8722 11.00000 0.05 0.33 Q115 1 0.6619 0.2798 1.0287 11.00000 0.05 0.33 Q116 1 0.2738 0.6690 0.6624 11.00000 0.05 0.33 Q117 1 0.3788 0.4875 0.9872 11.00000 0.05 0.33 Q118 1 0.4115 0.8174 0.9373 11.00000 0.05 0.33 Q119 1 0.7536 -0.0994 1.0603 11.00000 0.05 0.33 Q120 1 -0.1979 0.0555 0.1895 11.00000 0.05 0.33 Q121 1 0.1401 -0.2005 0.1581 11.00000 0.05 0.33 Q122 1 0.7733 0.5803 1.0990 11.00000 0.05 0.33 Q123 1 0.7546 0.2142 1.0205 11.00000 0.05 0.33 Q124 1 0.7438 0.0139 1.1195 11.00000 0.05 0.33 Q125 1 0.1811 0.1261 0.4297 11.00000 0.05 0.33 Q126 1 0.3262 0.0293 0.9016 11.00000 0.05 0.33 Q127 1 0.6871 0.5983 1.0386 11.00000 0.05 0.32 Q128 1 0.4386 0.7395 0.9088 11.00000 0.05 0.32 Q129 1 0.1626 -0.2936 0.1561 11.00000 0.05 0.32 Q130 1 0.7103 -0.0381 0.9807 11.00000 0.05 0.32 Q131 1 0.4300 -0.0243 0.9012 11.00000 0.05 0.32 Q132 1 0.2144 -0.1228 0.2692 11.00000 0.05 0.32 Q133 1 0.5020 1.0975 1.0397 11.00000 0.05 0.32 Q134 1 0.6907 0.2035 1.0520 11.00000 0.05 0.32 Q135 1 -0.1018 -0.0418 0.2875 11.00000 0.05 0.32 Q136 1 0.0519 0.4164 0.2671 11.00000 0.05 0.32 Q137 1 0.3719 1.0888 1.0401 11.00000 0.05 0.32 Q138 1 -0.0962 0.2776 0.3778 11.00000 0.05 0.32 Q139 1 0.7097 0.6299 0.7415 11.00000 0.05 0.32 Q140 1 0.2156 0.0237 0.2516 11.00000 0.05 0.32 Q141 1 0.2139 -0.3392 0.1670 11.00000 0.05 0.32 Q142 1 0.7522 0.6089 1.0652 11.00000 0.05 0.32 Q143 1 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86.0196 2 -31 -2 -4 225.469 76.9133 2 31 -2 5-4.50792 22.6831 2 -31 -2 -6-17.9942 18.5703 2 -31 3 30 369.162 92.3678 2 -31 3 29 243.160 102.516 2 -31 3 28 189.176 104.646 2 31 -3 -26 1490.29 87.3580 2 -31 3 20 536.084 159.168 2 -31 3 19 298.427 46.8051 2 -31 3 18 186.977 32.7300 2 -31 3 17 1706.57 52.7839 2 -31 3 16 135.044 34.9246 2 -31 3 15 117.191 61.7724 2 -31 -3 8 568.147 50.0760 2 -31 3 7 3539.11 93.1343 2 -31 3 6 372.562 46.5552 2 -31 3 5 196.978 44.1621 2 -31 3 4-38.1233 47.8822 2 -31 -3 -2 842.508 88.4777 2 -31 -3 -3 2524.61 122.865 2 -31 -3 -4 41.1614 55.3521 2 -31 -3 -5 36.0223 43.4155 2 -31 4 29 391.271 81.9798 2 -31 4 28 232.437 91.3981 2 -31 4 20 87.5704 112.717 2 -31 4 19 615.360 140.934 2 -31 4 18 176.316 36.7777 2 -31 4 17 310.886 42.4065 2 -31 4 16 18.8624 28.0299 2 -31 4 15 1252.14 63.6390 2 -31 -4 8 1609.61 62.2184 2 -31 4 7 1175.71 58.1566 2 -31 4 6 1360.01 60.0272 2 -31 4 5 893.993 64.3362 2 -31 -4 4 370.528 69.5305 2 -31 -4 -3 262.727 53.5293 2 -31 5 21 1500.66 132.901 2 31 -5 -18 2851.65 104.774 2 -31 5 17 1408.75 54.2141 2 -31 5 16 102.147 51.0803 2 -31 5 15 623.539 69.3166 2 -31 5 8 659.427 80.3896 2 -31 5 7 436.620 34.5649 2 -31 -5 6 1291.23 54.7999 2 -31 -5 5 535.955 38.7297 2 -31 -5 4 4893.45 139.143 2 -31 -5 3 3201.02 113.809 2 -31 6 9 106.607 44.1198 2 -32 0 30 3470.24 203.556 2 -32 0 28 787.764 79.1710 2 -32 0 20 373.163 186.216 2 -32 0 18 703.142 67.5992 2 -32 0 16 463.519 82.2448 2 -32 0 8 59.7614 76.4666 2 -32 0 6 1077.92 118.213 2 -32 0 4 1328.26 120.363 2 -32 0 -4 620.982 83.7724 2 -32 0 -6 1632.57 95.2567 2 -32 1 30 1740.97 158.806 2 -32 -1 29 3723.95 89.7283 2 -32 -1 28 1703.60 72.6093 2 -32 -1 27-116.247 39.6145 2 -32 1 26 1641.23 127.567 2 -32 1 20 228.348 169.558 2 -32 -1 19 712.943 54.7774 2 -32 -1 18 3028.35 85.6249 2 -32 -1 17 1965.45 66.5041 2 -32 -1 16 74.2226 50.0720 2 -32 -1 15 2424.73 132.194 2 -32 1 8 201.166 54.7739 2 -32 1 7 702.421 67.4020 2 -32 1 6 618.961 61.1724 2 -32 1 5 1760.90 81.1411 2 -32 -1 4 3.58054 55.6070 2 -32 -1 -2 271.246 55.6807 2 -32 -1 -3 162.682 52.7619 2 -32 -1 -4 17.6164 41.4030 2 32 -1 5-32.6554 21.7862 2 -32 -1 -6-2.94289 17.9952 2 -32 2 30 431.176 112.298 2 -32 2 29 847.014 130.950 2 -32 2 28 1837.31 173.107 2 -32 2 27 430.618 123.244 2 -32 2 20 5669.87 309.060 2 -32 2 19 5339.03 108.642 2 -32 2 18 4800.97 90.0795 2 -32 2 17 2963.92 75.2393 2 -32 -2 16 1146.09 59.2859 2 -32 2 15 746.946 82.9192 2 -32 2 8 2696.86 89.7739 2 -32 2 7 503.503 57.4833 2 -32 2 6 11762.5 167.863 2 -32 2 5 1459.46 72.1812 2 -32 2 4 5799.19 121.877 2 -32 -2 -2 1890.83 123.223 2 -32 -2 -3 2061.51 121.693 2 -32 -2 -4 3108.46 56.3947 2 -32 -2 -5 7.82457 51.5666 2 -32 3 31 112.905 66.6618 2 -32 3 30 346.452 88.4078 2 -32 3 29 717.892 108.527 2 -32 3 28 127.249 93.8928 2 -32 3 27 254.776 108.210 2 32 -3 -26 539.139 56.4701 2 -32 3 20 10.2785 127.349 2 -32 3 19 200.085 43.0717 2 -32 3 18 157.146 29.4740 2 -32 -3 17 205.955 37.7875 2 -32 3 16-0.69394 27.5945 2 -32 3 15 222.878 62.1547 2 -32 3 8 30.4749 50.5975 2 -32 3 7 5.04549 33.7121 2 -32 3 6 471.664 46.2353 2 -32 3 5 745.107 51.3602 2 -32 3 4 50.9313 36.0273 2 -32 -3 3 521.263 76.7011 2 -32 -3 -2 276.611 64.2818 2 -32 -3 -3 30.3654 44.9648 2 -32 4 28 559.423 89.2655 2 -32 4 27 339.116 85.3614 2 -32 4 20 134.119 108.202 2 32 -4 -18 266.369 53.2121 2 -32 4 17 75.1158 32.4888 2 -32 4 16 704.425 49.7590 2 -32 4 15 4080.68 95.4281 2 32 -4 -14 500.772 63.9470 2 -32 4 8 85.9738 64.8829 2 -32 4 7 4517.87 166.802 2 -32 4 6 658.053 53.9909 2 -32 4 5 533.363 52.2730 2 -32 -4 4 53.8302 49.4202 2 -32 -4 3 4027.05 134.664 2 32 -5 -18 2701.39 94.6911 2 32 -5 -17 58.8144 38.3565 2 -32 5 16 101.675 41.8114 2 -32 5 15 1659.29 82.2290 2 -32 5 8 650.890 76.3654 2 -32 5 7 647.202 41.5033 2 -32 5 6 1678.46 95.0078 2 -32 5 3 306.331 54.0943 2 -33 0 30 901.252 135.907 2 -33 0 28 248.704 121.457 2 -33 0 20 417.227 168.425 2 -33 0 18 1224.63 74.5971 2 -33 0 16 879.481 105.360 2 -33 0 8 98.3523 74.2390 2 -33 0 6 330.460 88.2689 2 -33 0 4 39.5024 76.5832 2 -33 0 -2 1461.99 104.289 2 -33 0 -4 396.295 67.5930 2 -33 -1 30 356.480 78.9060 2 -33 -1 29 665.900 91.5297 2 -33 -1 28 769.429 101.274 2 -33 -1 27 465.217 96.1860 2 -33 -1 20 1636.62 155.634 2 -33 -1 19 57.1127 35.3348 2 -33 -1 18 1107.15 52.8876 2 -33 -1 17 6942.26 104.679 2 -33 -1 16 2.82429 39.0844 2 -33 1 8 281.404 52.1501 2 -33 -1 7 5469.20 148.551 2 -33 -1 6 2566.32 111.452 2 -33 -1 5 74.5839 56.4212 2 -33 -1 4 2668.51 109.616 2 -33 -1 -2 4346.11 110.288 2 -33 -1 -3 433.432 50.1995 2 -33 -1 -4 1076.28 37.8248 2 33 1 5 379.437 26.2406 2 -33 2 31 297.394 85.3961 2 -33 2 30 900.966 115.121 2 -33 2 29 3738.59 195.608 2 -33 2 28 1265.58 143.959 2 -33 2 27 60.6688 111.066 2 -33 2 20 891.828 173.343 2 -33 2 19 127.422 34.2138 2 -33 2 18 6252.70 95.2352 2 -33 -2 17 201.717 41.0643 2 -33 -2 16 226.334 42.7669 2 -33 -2 15-124.820 47.0498 2 -33 2 8 1355.58 70.7763 2 -33 2 7 56.7946 44.9152 2 -33 2 6 1336.47 69.3287 2 -33 2 5 139.512 43.5809 2 -33 2 4 1243.67 64.1471 2 -33 -2 -2 134.717 59.4463 2 33 -2 3 134.399 21.3193 2 -33 3 30 238.587 348.840 2 -33 3 29 213.438 81.5693 2 -33 3 28 122.535 88.2349 2 -33 3 27 195.741 92.8577 2 -33 3 20-70.9947 117.503 2 -33 3 19 75.1621 40.6114 2 -33 3 18 61.9806 30.1503 2 -33 -3 17 15.6640 26.5157 2 -33 -3 16 743.444 47.9429 2 -33 3 15 176.753 56.3831 2 -33 3 8 829.356 66.4846 2 -33 3 7 649.588 64.1932 2 -33 3 6 897.284 69.4441 2 -33 3 5 385.405 57.1799 2 -33 3 4 43.3231 46.0154 2 -33 3 3 273.487 44.3417 2 33 -4 -18 334.655 52.1293 2 33 -4 -17 718.103 64.2189 2 33 -4 -16 994.574 74.2899 2 -33 4 15 1768.15 62.9370 2 33 -4 -14 124.914 45.2552 2 -33 4 8 795.055 83.1368 2 -33 4 7 1522.21 101.987 2 -33 4 6 1154.85 94.0079 2 -33 4 5 555.570 75.4492 2 -33 4 4 344.407 67.2704 2 33 -5 -18 1091.04 58.7620 2 33 -5 -17 496.784 47.0961 2 -33 5 15 996.363 59.0469 2 -33 5 9 1104.68 76.0369 2 -33 5 8 1550.42 82.0519 2 -33 5 7 186.390 50.5770 2 -33 5 6 3005.00 100.459 2 -34 0 30 317.105 100.654 2 -34 0 28 44.8465 106.344 2 -34 0 20 787.150 174.302 2 -34 0 18 105.286 45.8209 2 -34 0 16 564.100 63.3912 2 -34 0 8 176.184 81.8274 2 -34 0 6-18.8452 70.8566 2 -34 0 4 695.113 94.3572 2 -34 0 -2 1465.19 94.5145 2 -34 1 31 979.989 107.437 2 -34 1 30 749.642 108.986 2 -34 1 29 2421.57 165.999 2 -34 -1 28 855.138 97.0218 2 -34 -1 27 302.547 84.1323 2 -34 -1 20 414.921 112.427 2 -34 -1 19 1071.35 49.3979 2 -34 -1 18 3488.66 80.8253 2 -34 -1 17 2069.73 68.1388 2 -34 -1 16 261.358 41.9937 2 -34 1 15 2149.94 137.973 2 -34 -1 8 251.875 60.4425 2 -34 -1 7-55.9640 49.9499 2 -34 -1 6 438.024 64.6729 2 -34 -1 5 950.627 74.6007 2 -34 -1 4 176.185 52.0071 2 -34 1 3 212.318 77.7111 2 -34 1 -1 279.093 65.2436 2 -34 -1 -2-16.2851 50.2192 2 34 -1 3 21.7931 20.0294 2 -34 2 31 213.433 69.1894 2 -34 2 30 337.482 91.8776 2 -34 2 29 1787.18 135.618 2 -34 2 28 609.094 112.078 2 -34 2 27 190.655 112.429 2 -34 2 20 2476.33 201.120 2 -34 -2 19 1295.21 52.3154 2 -34 -2 18 1462.71 54.9516 2 -34 -2 17 1468.83 55.1366 2 -34 -2 16 150.980 35.4016 2 -34 -2 15 72.2469 47.0714 2 -34 -2 9 343.634 87.7701 2 -34 2 8 323.958 44.2685 2 -34 2 7 62.5428 39.6392 2 -34 -2 6 5491.98 193.051 2 -34 -2 5-11.3416 63.8957 2 -34 -2 4 2506.70 137.794 2 -34 3 28-5.03307 67.6536 2 -34 3 27 213.771 81.2344 2 -34 3 21 320.516 109.863 2 -34 3 19 77.0073 34.6713 2 -34 3 18-0.52387 25.6198 2 -34 3 17 216.698 31.7406 2 -34 3 16-49.2396 35.7888 2 -34 -3 15 144.349 60.6099 2 -34 3 9 129.268 63.7474 2 -34 3 8 10.8432 33.7010 2 -34 3 7 106.551 43.4581 2 -34 3 6 175.608 46.7919 2 -34 3 5 36.5541 42.2982 2 -34 -3 4 13.1994 55.4647 2 34 -4 -18 298.218 46.2799 2 34 -4 -17 4600.24 123.099 2 34 -4 -16 1287.87 71.7952 2 34 -4 -15 179.137 42.6852 2 -34 4 14 135.086 31.3731 2 -34 4 9 2657.59 112.085 2 -34 4 8 103.311 55.3741 2 -34 4 7 3507.87 123.473 2 -34 4 6 1212.62 83.5025 2 -34 4 5 911.671 77.0909 2 -35 0 30 406.339 94.8267 2 -35 0 28 69.9075 95.9481 2 -35 0 20 239.200 137.775 2 -35 0 18 484.775 61.7503 2 -35 0 16 127.816 51.0644 2 -35 0 8 743.179 95.7896 2 -35 0 6 101.392 65.1251 2 -35 0 4 82.8745 66.4885 2 -35 1 31 93.8311 66.2020 2 -35 1 30 337.699 89.5663 2 -35 1 29 226.325 94.4453 2 -35 1 28 626.919 115.099 2 -35 1 27 934.867 132.845 2 -35 1 21 1693.37 178.969 2 -35 1 20 383.531 132.952 2 -35 -1 19 113.458 27.5555 2 -35 -1 18 2077.90 62.3930 2 -35 -1 17 1927.87 62.9315 2 -35 -1 16 257.760 40.0466 2 -35 -1 15 423.409 44.4096 2 -35 -1 8-46.7721 43.6511 2 -35 -1 7 2849.08 101.311 2 -35 -1 6 1718.84 82.1126 2 -35 -1 5 121.557 48.8600 2 -35 -1 4 1150.13 71.3485 2 -35 -1 3 2389.08 89.0110 2 -35 2 29 154.238 75.8637 2 -35 2 28 960.987 111.781 2 -35 2 27 96.0072 90.6694 2 -35 2 21 1658.20 166.239 2 -35 2 20 657.896 85.0198 2 -35 -2 19 9.79822 27.4663 2 -35 -2 18 5949.12 76.8507 2 -35 -2 17 42.3891 30.7191 2 -35 -2 16 536.223 40.4288 2 -35 -2 15-79.4187 41.7881 2 -35 -2 8 292.433 79.3963 2 -35 -2 7 151.961 70.9135 2 -35 -2 6 507.847 81.7301 2 -35 -2 5 529.800 82.1530 2 -35 -2 4 988.787 93.1693 2 -35 -2 3 111.910 65.0173 2 -35 -3 19 67.1226 48.1203 2 35 -3 -18 537.466 41.3758 2 -35 3 17 44.1772 27.9365 2 -35 3 16 117.633 27.1445 2 -35 3 15-53.7709 35.0429 2 -35 -3 9 237.967 63.5761 2 -35 3 8 88.4636 40.4023 2 -35 -3 7 268.515 61.7918 2 -35 -3 6 2264.93 108.413 2 -35 -3 5-29.9463 49.3646 2 35 -4 -20 355.881 38.5694 2 35 -4 -18 2.42169 30.7931 2 35 -4 -17 531.783 48.8243 2 35 -4 -16 426.558 44.5271 2 35 -4 -15 747.468 54.4820 2 35 -4 -14 18.2967 31.9956 2 -35 4 9 89.7098 44.4209 2 -35 4 8 590.810 60.1870 2 -36 0 28 172.010 88.5360 2 -36 0 20 288.719 70.4995 2 -36 0 18 287.846 48.2071 2 -36 0 16 111.362 45.8907 2 -36 0 8 194.440 68.9892 2 -36 0 6 1938.90 113.890 2 -36 0 4 1516.30 97.8950 2 -36 1 29 1004.40 103.982 2 -36 1 28 557.945 98.3251 2 -36 1 27 450.214 100.673 2 -36 1 20 189.450 68.2131 2 -36 -1 19 619.774 40.4920 2 -36 -1 18 2866.02 58.6490 2 -36 -1 17 664.772 42.7003 2 -36 -1 16 69.8344 34.0197 2 -36 -1 15 1519.14 55.9680 2 -36 -1 9 260.998 50.6727 2 -36 -1 8 515.467 58.7646 2 -36 -1 7 31.6852 44.5252 2 -36 -1 6 1211.68 70.1204 2 -36 -1 5 477.343 51.9255 2 -36 -1 4 118.833 41.5146 2 -36 -1 3 52.9713 56.7039 2 -36 -2 20 1229.94 67.2682 2 -36 -2 19-15.3517 20.5675 2 -36 -2 18 4359.45 61.1812 2 -36 -2 17 1350.67 39.7553 2 -36 -2 16 21.4461 35.3931 2 -36 -2 15 333.050 42.6625 2 -36 -2 9 1069.02 91.3125 2 -36 -2 8 247.736 65.9943 2 -36 -2 7 1001.38 89.8427 2 -36 -2 6 2899.95 124.728 2 -36 -2 5 32.7529 53.5595 2 -36 -2 4 578.573 71.7868 2 -36 -2 3 143.129 52.2164 2 36 -3 -19 51.9827 24.5157 2 36 -3 -18 108.899 28.5250 2 36 -3 -17 377.057 35.7240 2 36 -3 -16-12.7603 25.3701 2 36 -3 -15 154.741 31.3641 2 36 -3 -14 130.220 38.2565 2 -36 -3 9 222.100 55.5369 2 -36 -3 8 36.7979 47.9145 2 -37 0 20 663.278 74.0057 2 -37 0 18 672.355 55.3515 2 -37 0 16 156.346 45.1744 2 -37 0 8 2374.84 115.214 2 -37 0 6 43.3493 50.7210 2 -37 1 26 86.1966 77.0550 2 -37 -1 20 395.336 52.0129 2 -37 -1 19 6.59450 25.8091 2 -37 -1 18 1165.03 44.2002 2 -37 -1 17 393.867 27.7274 2 -37 -1 16-33.2601 27.5285 2 -37 -1 15 141.398 31.8612 2 -37 -1 9 176.665 45.2350 2 -37 -1 8-64.2597 37.5506 2 -37 -1 7 1395.17 64.2137 2 -37 -1 6 888.371 77.6187 2 -37 -1 5-22.4814 46.4878 2 -37 -1 4 120.961 49.7584 2 -37 -2 20 115.648 36.2557 2 -37 -2 19 48.9105 22.1897 2 -37 -2 18 1725.70 48.8797 2 -37 -2 17 162.300 24.7595 2 -37 -2 16 46.5157 22.4132 2 -37 -2 15-43.5396 27.8843 2 -37 -2 9-2.44630 28.7184 2 -37 -2 8 310.575 62.5015 2 -37 -2 7 32.4991 50.7409 2 -37 -2 6 55.0128 45.0086 2 37 -3 -17 611.853 43.9704 2 37 -3 -16 13.0984 26.2142 2 37 -3 -15 798.952 50.2728 2 37 -3 -14 487.225 43.0193 2 -38 0 20 433.083 42.7341 2 -38 0 18 33.7556 34.4226 2 -38 0 16 444.696 45.1265 2 -38 0 8 3076.59 110.565 2 -38 -1 20 455.587 35.1490 2 -38 -1 19 201.790 32.0422 2 -38 -1 18 945.162 37.4051 2 -38 -1 17-49.8534 23.7540 2 -38 -1 16-38.5321 24.8085 2 -38 -1 15 1071.85 41.1436 2 -38 1 14 1749.09 92.5831 2 -38 -1 9 398.733 36.7913 2 -38 -1 8 84.4151 28.9488 2 -38 -2 21 258.862 43.6050 2 -38 -2 20 403.932 51.2388 2 -38 -2 19 34.1635 41.3600 2 -38 -2 18 2507.21 98.3748 2 -38 -2 17 573.024 59.0599 2 -38 -2 16-12.6182 42.0264 2 -38 -2 15 154.077 48.3863 2 38 -2 -14 5419.50 108.633 2 -39 0 22 687.043 57.2827 2 -39 0 20 402.626 34.9558 2 -39 0 18 943.258 48.0682 2 -39 0 16 353.078 39.6755 2 -39 0 14 829.984 66.0174 2 -39 -1 20 253.833 45.5701 2 -39 -1 19-41.6364 21.3512 2 -39 -1 18 1741.01 47.4279 2 -39 -1 17-36.6722 22.7661 2 -39 -1 16-12.4109 25.5848 2 -39 -1 15 759.524 38.8191 2 -39 -1 14 606.496 60.6231 2 0 0 0 0.00000 0.00000 0 TITL exp_1467_twin1_hklf4 in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 31.963547 7.779980 30.649420 90.0000 115.8975 90.0000 ZERR 5.00 0.000698 0.000114 0.000627 0.0000 0.0026 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O Cu Br UNIT 240.00 150.00 30.00 60.00 10.00 10.00 TREF HKLF 5 BASF 0.40933 END ; _shelx_hkl_checksum 76931 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.73294(3) -0.04610(9) 1.11443(3) 0.0408(2) Uani 1 1 d . . . . . O1 O 0.6545(2) 0.7994(6) 0.92158(18) 0.0491(15) Uani 1 1 d . . . . . N1 N 0.72385(17) 0.3711(6) 1.05756(17) 0.0231(10) Uani 1 1 d . . . . . Cu1 Cu 0.75315(3) 0.25642(11) 1.12268(3) 0.0225(2) Uani 1 1 d . . . . . C1 C 0.6787(2) 0.5432(8) 0.9692(2) 0.0266(13) Uani 1 1 d . . . . . Cu2 Cu 0.25672(3) 0.71888(11) 0.61503(3) 0.02150(19) Uani 1 1 d . . . . . Br2 Br 0.23539(2) 1.02176(8) 0.60309(2) 0.02980(16) Uani 1 1 d . . . . . O2 O 0.63692(13) 0.5421(5) 0.88404(14) 0.0231(8) Uani 1 1 d . . . . . N2 N 0.72899(17) 1.1144(6) 0.66698(18) 0.0242(10) Uani 1 1 d . . . . . C2 C 0.6828(2) 0.3669(8) 0.9703(2) 0.0267(13) Uani 1 1 d . . . . . H2 H 0.670582 0.302365 0.941038 0.032 Uiso 1 1 calc R U . . . C3 C 0.7053(2) 0.2850(8) 1.0150(2) 0.0252(12) Uani 1 1 d . . . . . H3 H 0.707659 0.163193 1.015565 0.030 Uiso 1 1 calc R U . . . N3 N 0.32545(16) 0.7112(6) 0.66138(17) 0.0218(10) Uani 1 1 d . . . . . O3 O 0.64087(14) 0.8700(5) 0.75197(15) 0.0253(9) Uani 1 1 d . . . . . C4 C 0.7198(3) 0.5432(8) 1.0554(2) 0.0376(17) Uani 1 1 d . . . . . H4 H 0.733254 0.606349 1.084888 0.045 Uiso 1 1 calc R U . . . O4 O 0.67721(19) 0.6353(6) 0.7428(2) 0.0421(12) Uani 1 1 d . . . . . N4 N 0.23354(17) 0.6047(6) 0.54912(17) 0.0234(10) Uani 1 1 d . . . . . O5 O 0.49662(13) 0.6796(6) 0.74301(15) 0.0280(9) Uani 1 1 d . . . . . N5 N 0.22371(17) -0.0969(6) 0.15130(18) 0.0240(10) Uani 1 1 d . . . . . C5 C 0.6972(3) 0.6326(9) 1.0126(2) 0.0386(17) Uani 1 1 d . . . . . H5 H 0.694341 0.754132 1.012831 0.046 Uiso 1 1 calc R U . . . O6 O 0.48320(15) 0.8323(7) 0.79793(18) 0.0409(12) Uani 1 1 d . . . . . N6 N -0.17727(15) 0.2659(6) 0.16612(17) 0.0215(10) Uani 1 1 d . . . . . C6 C 0.6560(2) 0.6456(9) 0.9235(2) 0.0296(14) Uani 1 1 d . . . . . C7 C 0.61483(19) 0.6259(8) 0.8391(2) 0.0234(12) Uani 1 1 d . . . . . O7 O 0.17362(18) 0.1761(6) 0.41343(16) 0.0393(12) Uani 1 1 d . . . . . C8 C 0.64124(19) 0.7035(7) 0.8189(2) 0.0210(11) Uani 1 1 d . . . . . H8 H 0.674225 0.706891 0.835538 0.025 Uiso 1 1 calc R U . . . O8 O 0.13779(13) 0.4238(6) 0.37848(14) 0.0237(9) Uani 1 1 d . . . . . C9 C 0.61728(19) 0.7761(8) 0.7732(2) 0.0228(12) Uani 1 1 d . . . . . O9 O 0.13623(14) 0.1117(5) 0.24158(15) 0.0240(9) Uani 1 1 d . . . . . C10 C 0.5693(2) 0.7714(8) 0.7480(2) 0.0239(12) Uani 1 1 d . . . . . H10 H 0.553540 0.821095 0.716709 0.029 Uiso 1 1 calc R U . . . O10 O 0.1570(2) 0.3599(7) 0.2193(2) 0.0440(13) Uani 1 1 d . . . . . C11 C 0.54517(19) 0.6917(8) 0.7703(2) 0.0250(12) Uani 1 1 d . . . . . O11 O -0.00560(13) 0.2984(6) 0.24084(14) 0.0280(10) Uani 1 1 d . . . . . C12 C 0.5665(2) 0.6188(8) 0.8162(2) 0.0260(12) Uani 1 1 d . . . . . H12 H 0.549116 0.566981 0.831160 0.031 Uiso 1 1 calc R U . . . O12 O -0.01691(16) 0.1429(8) 0.29660(19) 0.0505(15) Uani 1 1 d . . . . . C13 C 0.6696(2) 0.7851(9) 0.7374(2) 0.0283(13) Uani 1 1 d . . . . . C14 C 0.6896(2) 0.9048(8) 0.7133(2) 0.0255(12) Uani 1 1 d . . . . . C16 C 0.7419(2) 0.9524(8) 0.6782(2) 0.0263(13) Uani 1 1 d . . . . . H16 H 0.765687 0.909107 0.670600 0.032 Uiso 1 1 calc R U . . . C15 C 0.7230(2) 0.8415(8) 0.7002(2) 0.0258(12) Uani 1 1 d . . . . . H15 H 0.732679 0.724900 0.706171 0.031 Uiso 1 1 calc R U . . . C18 C 0.6764(2) 1.0760(9) 0.7032(3) 0.0329(14) Uani 1 1 d . . . . . H18 H 0.653782 1.123562 0.711958 0.039 Uiso 1 1 calc R U . . . C17 C 0.6967(2) 1.1769(9) 0.6802(3) 0.0325(14) Uani 1 1 d . . . . . H17 H 0.687561 1.293822 0.673466 0.039 Uiso 1 1 calc R U . . . C19 C 0.46895(19) 0.7565(8) 0.7606(2) 0.0263(13) Uani 1 1 d . . . . . C20 C 0.41940(19) 0.7322(8) 0.7262(2) 0.0227(12) Uani 1 1 d . . . . . C21 C 0.40514(19) 0.6379(7) 0.6833(2) 0.0232(11) Uani 1 1 d . . . . . H21 H 0.427209 0.580357 0.675531 0.028 Uiso 1 1 calc R U . . . C22 C 0.35772(19) 0.6301(7) 0.6522(2) 0.0228(12) Uani 1 1 d . . . . . H22 H 0.347904 0.564422 0.623277 0.027 Uiso 1 1 calc R U . . . C23 C 0.33940(19) 0.8021(7) 0.7022(2) 0.0216(11) Uani 1 1 d . . . . . H23 H 0.316510 0.861360 0.708268 0.026 Uiso 1 1 calc R U . . . C24 C 0.38557(19) 0.8153(8) 0.7363(2) 0.0236(12) Uani 1 1 d . . . . . H24 H 0.393964 0.878309 0.765489 0.028 Uiso 1 1 calc R U . . . C25 C 0.1899(2) 0.4298(8) 0.4613(2) 0.0250(13) Uani 1 1 d . . . . . C26 C 0.1838(2) 0.6053(8) 0.4637(2) 0.0266(13) Uani 1 1 d . . . . . H26 H 0.164924 0.668415 0.435385 0.032 Uiso 1 1 calc R U . . . C27 C 0.2057(2) 0.6868(8) 0.5080(2) 0.0258(13) Uani 1 1 d . . . . . H27 H 0.200815 0.806668 0.509506 0.031 Uiso 1 1 calc R U . . . C28 C 0.2402(2) 0.4363(8) 0.5463(2) 0.0300(14) Uani 1 1 d . . . . . H28 H 0.260607 0.377549 0.574852 0.036 Uiso 1 1 calc R U . . . C29 C 0.2189(2) 0.3433(9) 0.5036(2) 0.0331(15) Uani 1 1 d . . . . . H29 H 0.223968 0.223136 0.503148 0.040 Uiso 1 1 calc R U . . . C30 C 0.1673(2) 0.3271(8) 0.4163(2) 0.0268(13) Uani 1 1 d . . . . . C31 C 0.11446(19) 0.3437(8) 0.3335(2) 0.0217(11) Uani 1 1 d . . . . . C32 C 0.13908(19) 0.2695(8) 0.3105(2) 0.0209(11) Uani 1 1 d . . . . . H32 H 0.172103 0.266303 0.325500 0.025 Uiso 1 1 calc R U . . . C33 C 0.11334(19) 0.2003(8) 0.2648(2) 0.0218(12) Uani 1 1 d . . . . . C34 C 0.06512(19) 0.2063(8) 0.2415(2) 0.0226(12) Uani 1 1 d . . . . . H34 H 0.048169 0.159486 0.209934 0.027 Uiso 1 1 calc R U . . . C35 C 0.04301(18) 0.2831(8) 0.2661(2) 0.0239(12) Uani 1 1 d . . . . . C36 C 0.06626(19) 0.3522(8) 0.3125(2) 0.0234(12) Uani 1 1 d . . . . . H36 H 0.050003 0.402298 0.328921 0.028 Uiso 1 1 calc R U . . . C37 C 0.1568(2) 0.2067(8) 0.2194(2) 0.0266(13) Uani 1 1 d . . . . . C38 C 0.1788(2) 0.0949(8) 0.1956(2) 0.0248(12) Uani 1 1 d . . . . . C39 C 0.2051(3) 0.1751(9) 0.1755(3) 0.0345(15) Uani 1 1 d . . . . . H39 H 0.208110 0.296693 0.176553 0.041 Uiso 1 1 calc R U . . . C40 C 0.2266(2) 0.0775(9) 0.1542(3) 0.0342(15) Uani 1 1 d . . . . . H40 H 0.244565 0.134466 0.140698 0.041 Uiso 1 1 calc R U . . . C41 C 0.1983(2) -0.1732(9) 0.1711(2) 0.0316(14) Uani 1 1 d . . . . . H41 H 0.195780 -0.294940 0.169814 0.038 Uiso 1 1 calc R U . . . C42 C 0.1755(2) -0.0815(9) 0.1935(2) 0.0285(13) Uani 1 1 d . . . . . H42 H 0.157971 -0.140142 0.207087 0.034 Uiso 1 1 calc R U . . . C43 C -0.0320(2) 0.2222(8) 0.2595(2) 0.0264(13) Uani 1 1 d . . . . . C44 C -0.08260(19) 0.2455(8) 0.2269(2) 0.0219(11) Uani 1 1 d . . . . . C45 C -0.0984(2) 0.3381(8) 0.1839(2) 0.0241(12) Uani 1 1 d . . . . . H45 H -0.077288 0.395785 0.174698 0.029 Uiso 1 1 calc R U . . . C46 C -0.1463(2) 0.3439(8) 0.1547(2) 0.0239(12) Uani 1 1 d . . . . . H46 H -0.157288 0.406543 0.125114 0.029 Uiso 1 1 calc R U . . . C48 C -0.11467(19) 0.1650(8) 0.2394(2) 0.0241(12) Uani 1 1 d . . . . . H48 H -0.104701 0.102852 0.268936 0.029 Uiso 1 1 calc R U . . . C47 C -0.1610(2) 0.1773(8) 0.2082(2) 0.0241(12) Uani 1 1 d . . . . . H47 H -0.182732 0.120593 0.216640 0.029 Uiso 1 1 calc R U . . . C101 C 0.0470(4) 0.4642(15) 0.4500(4) 0.058(3) Uani 0.763(4) 1 d D U P A 1 C102 C 0.0699(4) 0.5508(17) 0.4916(4) 0.065(3) Uani 0.763(4) 1 d D U P A 1 H102 H 0.057740 0.659966 0.493978 0.077 Uiso 0.763(4) 1 calc R U P A 1 C103 C 0.1102(4) 0.4959(18) 0.5319(5) 0.064(4) Uani 0.763(4) 1 d D U P A 1 H103 H 0.125752 0.567116 0.559555 0.076 Uiso 0.763(4) 1 calc R U P A 1 C104 C 0.1261(4) 0.3303(18) 0.5291(4) 0.064(4) Uani 0.763(4) 1 d D U P A 1 H104 H 0.153311 0.288121 0.555449 0.077 Uiso 0.763(4) 1 calc R U P A 1 C105 C 0.1027(3) 0.2247(16) 0.4882(4) 0.058(3) Uani 0.763(4) 1 d D U P A 1 C106 C 0.0632(3) 0.2983(15) 0.4487(4) 0.054(3) Uani 0.763(4) 1 d D U P A 1 C107 C 0.0393(3) 0.1830(16) 0.4077(4) 0.055(3) Uani 0.763(4) 1 d D U P A 1 H107 H 0.012682 0.223743 0.380348 0.066 Uiso 0.763(4) 1 calc R U P A 1 C108 C 0.0549(5) 0.009(3) 0.4074(5) 0.061(4) Uani 0.763(4) 1 d D U P A 1 H108 H 0.038425 -0.065231 0.380651 0.073 Uiso 0.763(4) 1 calc R U P A 1 C109 C 0.0941(4) -0.0474(16) 0.4466(5) 0.058(4) Uani 0.763(4) 1 d D U P A 1 H109 H 0.105073 -0.160565 0.446271 0.070 Uiso 0.763(4) 1 calc R U P A 1 C110 C 0.1171(4) 0.0517(16) 0.4851(5) 0.057(3) Uani 0.763(4) 1 d D U P A 1 H110 H 0.143875 0.006846 0.511341 0.069 Uiso 0.763(4) 1 calc R U P A 1 C111 C 0.0079(4) 0.539(2) 0.4086(5) 0.072(4) Uani 0.763(4) 1 d D U P A 1 C112 C -0.0276(7) 0.652(3) 0.4170(7) 0.143(10) Uani 0.763(4) 1 d D U P A 1 H11A H -0.020450 0.650821 0.451575 0.214 Uiso 0.763(4) 1 calc R U P A 1 H11B H -0.025929 0.770311 0.406890 0.214 Uiso 0.763(4) 1 calc R U P A 1 H11C H -0.059040 0.606822 0.398069 0.214 Uiso 0.763(4) 1 calc R U P A 1 O113 O 0.0035(3) 0.5279(12) 0.3670(3) 0.062(2) Uani 0.763(4) 1 d D U P A 1 C201 C 0.4577(7) 0.475(3) 0.9112(8) 0.093(4) Uani 0.372(7) 1 d D U P B 1 C202 C 0.4384(8) 0.574(4) 0.9329(10) 0.097(5) Uani 0.372(7) 1 d D U P B 1 H202 H 0.453849 0.676381 0.948448 0.117 Uiso 0.372(7) 1 calc R U P B 1 C203 C 0.3945(9) 0.531(4) 0.9338(11) 0.091(5) Uani 0.372(7) 1 d D U P B 1 H203 H 0.378646 0.611848 0.944325 0.109 Uiso 0.372(7) 1 calc R U P B 1 C204 C 0.3766(9) 0.368(4) 0.9188(10) 0.087(5) Uani 0.372(7) 1 d D U P B 1 H204 H 0.348971 0.334020 0.920844 0.105 Uiso 0.372(7) 1 calc R U P B 1 C205 C 0.3986(8) 0.252(3) 0.9005(11) 0.088(4) Uani 0.372(7) 1 d D U P B 1 C206 C 0.4407(8) 0.312(3) 0.9019(10) 0.091(4) Uani 0.372(7) 1 d D U P B 1 C207 C 0.4697(9) 0.189(4) 0.8906(11) 0.092(4) Uani 0.372(7) 1 d D U P B 1 H207 H 0.500675 0.213835 0.895937 0.110 Uiso 0.372(7) 1 calc R U P B 1 C208 C 0.4469(9) 0.025(4) 0.8703(11) 0.088(5) Uani 0.372(7) 1 d D U P B 1 H208 H 0.462162 -0.054440 0.858546 0.105 Uiso 0.372(7) 1 calc R U P B 1 C209 C 0.4054(10) -0.018(4) 0.8679(13) 0.091(5) Uani 0.372(7) 1 d D U P B 1 H209 H 0.390148 -0.118388 0.850897 0.109 Uiso 0.372(7) 1 calc R U P B 1 C210 C 0.3859(10) 0.076(4) 0.8883(11) 0.088(5) Uani 0.372(7) 1 d D U P B 1 H210 H 0.362365 0.027525 0.895332 0.105 Uiso 0.372(7) 1 calc R U P B 1 C211 C 0.4926(8) 0.528(4) 0.8955(9) 0.087(5) Uani 0.372(7) 1 d D U P B 1 C212 C 0.5386(10) 0.599(5) 0.9338(11) 0.116(7) Uani 0.372(7) 1 d D U P B 1 H21A H 0.533813 0.646190 0.960886 0.174 Uiso 0.372(7) 1 calc R U P B 1 H21B H 0.561624 0.506003 0.945638 0.174 Uiso 0.372(7) 1 calc R U P B 1 H21C H 0.549812 0.689422 0.919382 0.174 Uiso 0.372(7) 1 calc R U P B 1 O213 O 0.4934(8) 0.463(4) 0.8591(8) 0.089(6) Uani 0.372(7) 1 d D U P B 1 C301 C -0.0622(7) 0.027(5) 0.4912(8) 0.053(4) Uani 0.237(4) 1 d D U P A -1 C302 C -0.0995(9) 0.010(6) 0.5013(10) 0.054(4) Uani 0.237(4) 1 d D U P A -1 H302 H -0.130028 0.010863 0.475596 0.065 Uiso 0.237(4) 1 calc R U P A -1 C303 C -0.0932(11) -0.010(8) 0.5504(12) 0.054(5) Uani 0.237(4) 1 d D U P A -1 H303 H -0.119220 -0.012215 0.557640 0.065 Uiso 0.237(4) 1 calc R U P A -1 C304 C -0.0484(11) -0.026(10) 0.5872(13) 0.053(5) Uani 0.237(4) 1 d D U P A -1 H304 H -0.043995 -0.062230 0.618470 0.064 Uiso 0.237(4) 1 calc R U P A -1 C305 C -0.0093(8) 0.011(5) 0.5790(8) 0.053(4) Uani 0.237(4) 1 d D U P A -1 C306 C -0.0191(7) 0.014(5) 0.5284(7) 0.053(4) Uani 0.237(4) 1 d D U P A -1 C307 C 0.0220(8) -0.003(5) 0.5191(9) 0.045(4) Uani 0.237(4) 1 d D U P A -1 H307 H 0.018993 -0.018483 0.487157 0.054 Uiso 0.237(4) 1 calc R U P A -1 C308 C 0.0674(10) 0.004(6) 0.5603(10) 0.053(5) Uani 0.237(4) 1 d D U P A -1 H308 H 0.094099 0.021215 0.554698 0.064 Uiso 0.237(4) 1 calc R U P A -1 C309 C 0.0730(9) -0.012(5) 0.6063(9) 0.053(5) Uani 0.237(4) 1 d D U P A -1 H309 H 0.103002 -0.035075 0.631501 0.063 Uiso 0.237(4) 1 calc R U P A -1 C310 C 0.0377(8) 0.004(5) 0.6165(9) 0.054(4) Uani 0.237(4) 1 d D U P A -1 H310 H 0.043017 0.011799 0.649514 0.065 Uiso 0.237(4) 1 calc R U P A -1 C311 C -0.0698(11) 0.055(5) 0.4417(8) 0.054(5) Uani 0.237(4) 1 d D U P A -1 C312 C -0.1100(10) -0.035(5) 0.4007(10) 0.055(6) Uani 0.237(4) 1 d D U P A -1 H31A H -0.124421 -0.116892 0.414363 0.082 Uiso 0.237(4) 1 calc R U P A -1 H31B H -0.133082 0.050277 0.381098 0.082 Uiso 0.237(4) 1 calc R U P A -1 H31C H -0.098374 -0.096733 0.380367 0.082 Uiso 0.237(4) 1 calc R U P A -1 O313 O -0.0482(8) 0.161(3) 0.4306(9) 0.061(5) Uani 0.237(4) 1 d D U P A -1 C401 C 0.4584(8) 0.833(3) 1.0889(8) 0.142(6) Uani 0.414(6) 1 d D U P C 2 C402 C 0.4488(10) 0.993(4) 1.0873(10) 0.141(6) Uani 0.414(6) 1 d D U P C 2 H402 H 0.463611 1.061923 1.115510 0.169 Uiso 0.414(6) 1 calc R U P C 2 C403 C 0.4154(11) 1.068(4) 1.0427(10) 0.142(6) Uani 0.414(6) 1 d D U P C 2 H403 H 0.406884 1.185542 1.041896 0.170 Uiso 0.414(6) 1 calc R U P C 2 C404 C 0.3958(11) 0.970(4) 1.0015(10) 0.140(6) Uani 0.414(6) 1 d D U P C 2 H404 H 0.374629 1.022410 0.972020 0.168 Uiso 0.414(6) 1 calc R U P C 2 C405 C 0.4064(11) 0.797(4) 1.0017(9) 0.141(6) Uani 0.414(6) 1 d D U P C 2 C406 C 0.4382(10) 0.741(4) 1.0478(8) 0.141(6) Uani 0.414(6) 1 d D U P C 2 C407 C 0.4615(11) 0.571(4) 1.0583(10) 0.141(6) Uani 0.414(6) 1 d D U P C 2 H407 H 0.486268 0.540001 1.088538 0.169 Uiso 0.414(6) 1 calc R U P C 2 C408 C 0.4416(12) 0.458(4) 1.0162(11) 0.143(6) Uani 0.414(6) 1 d D U P C 2 H408 H 0.449114 0.338769 1.019827 0.172 Uiso 0.414(6) 1 calc R U P C 2 C409 C 0.4125(12) 0.520(5) 0.9721(10) 0.141(6) Uani 0.414(6) 1 d D U P C 2 H409 H 0.405974 0.450203 0.944482 0.169 Uiso 0.414(6) 1 calc R U P C 2 C410 C 0.3930(11) 0.670(5) 0.9652(10) 0.141(6) Uani 0.414(6) 1 d D U P C 2 H410 H 0.368695 0.695066 0.934144 0.169 Uiso 0.414(6) 1 calc R U P C 2 C411 C 0.4973(9) 0.743(4) 1.1251(8) 0.147(6) Uani 0.414(6) 1 d D U P C 2 C412 C 0.5424(12) 0.845(6) 1.1355(15) 0.162(8) Uani 0.414(6) 1 d D U P C 2 H41A H 0.534303 0.960834 1.121955 0.242 Uiso 0.414(6) 1 calc R U P C 2 H41B H 0.561478 0.852093 1.170588 0.242 Uiso 0.414(6) 1 calc R U P C 2 H41C H 0.559799 0.785442 1.120451 0.242 Uiso 0.414(6) 1 calc R U P C 2 O413 O 0.4923(10) 0.592(4) 1.1362(9) 0.131(7) Uani 0.414(6) 1 d D U P C 2 O601 O 0.448(2) 1.023(7) 1.0078(15) 0.16(2) Uani 0.216(7) 1 d D U P D 3 C602 C 0.458(4) 1.147(11) 1.045(3) 0.18(4) Uani 0.216(7) 1 d D U P D 3 O801 O 0.3793(12) 0.168(5) 0.8783(13) 0.076(9) Uani 0.216(7) 1 d D U P D 3 C802 C 0.4090(15) 0.051(5) 0.8717(19) 0.058(10) Uani 0.216(7) 1 d D U P D 3 H80A H 0.440725 0.068217 0.896848 0.087 Uiso 0.216(7) 1 calc R U P D 3 H80B H 0.408166 0.068210 0.839670 0.087 Uiso 0.216(7) 1 calc R U P D 3 H80C H 0.398893 -0.066601 0.873913 0.087 Uiso 0.216(7) 1 calc R U P D 3 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 Br1 0.0579(5) 0.0180(3) 0.0324(4) -0.0010(3) 0.0066(3) -0.0041(3) O1 0.087(4) 0.018(3) 0.027(3) 0.001(2) 0.011(3) -0.002(3) N1 0.030(2) 0.018(2) 0.020(2) 0.0007(19) 0.010(2) 0.000(2) Cu1 0.0244(4) 0.0197(4) 0.0203(4) -0.0001(3) 0.0069(3) 0.0027(3) C1 0.030(3) 0.022(3) 0.024(3) 0.001(2) 0.009(2) -0.002(2) Cu2 0.0224(4) 0.0198(4) 0.0200(4) -0.0002(3) 0.0070(3) -0.0006(3) Br2 0.0316(3) 0.0186(3) 0.0322(3) 0.0003(3) 0.0075(3) 0.0043(2) O2 0.0278(19) 0.021(2) 0.0182(19) 0.0006(16) 0.0077(16) 0.0005(16) N2 0.027(2) 0.022(3) 0.026(2) 0.000(2) 0.013(2) -0.001(2) C2 0.033(3) 0.025(3) 0.018(3) -0.002(2) 0.009(2) 0.001(3) C3 0.033(3) 0.019(3) 0.021(3) 0.000(2) 0.009(2) 0.002(2) N3 0.024(2) 0.018(2) 0.022(2) 0.003(2) 0.0078(19) 0.0003(18) O3 0.031(2) 0.023(2) 0.030(2) 0.0030(18) 0.0209(18) -0.0004(17) C4 0.061(4) 0.019(3) 0.021(3) -0.002(3) 0.006(3) -0.004(3) O4 0.062(3) 0.025(3) 0.060(3) 0.009(2) 0.045(3) 0.006(2) N4 0.028(2) 0.022(3) 0.019(2) 0.001(2) 0.0092(19) 0.001(2) O5 0.0193(18) 0.041(3) 0.024(2) -0.0025(19) 0.0092(16) -0.0012(18) N5 0.031(2) 0.019(2) 0.027(3) 0.001(2) 0.017(2) 0.003(2) C5 0.060(4) 0.018(3) 0.028(3) 0.001(3) 0.011(3) -0.002(3) O6 0.026(2) 0.050(3) 0.037(3) -0.018(2) 0.0041(19) 0.004(2) N6 0.021(2) 0.020(2) 0.022(2) -0.0026(19) 0.0069(18) 0.0026(19) C6 0.040(3) 0.024(3) 0.023(3) 0.001(3) 0.012(3) -0.002(3) C7 0.026(3) 0.021(3) 0.021(3) 0.001(2) 0.008(2) 0.002(2) O7 0.063(3) 0.020(2) 0.023(2) -0.0015(19) 0.007(2) -0.001(2) C8 0.021(2) 0.020(3) 0.022(3) -0.002(2) 0.010(2) 0.000(2) O8 0.0236(19) 0.025(2) 0.0181(19) -0.0023(17) 0.0053(16) -0.0013(16) C9 0.024(3) 0.024(3) 0.024(3) -0.003(2) 0.015(2) -0.002(2) O9 0.029(2) 0.025(2) 0.024(2) 0.0003(17) 0.0166(17) 0.0017(17) C10 0.026(3) 0.024(3) 0.023(3) 0.000(2) 0.013(2) 0.001(2) O10 0.071(4) 0.024(3) 0.057(3) -0.001(2) 0.048(3) 0.001(2) C11 0.021(3) 0.027(3) 0.026(3) -0.005(2) 0.009(2) -0.001(2) O11 0.0177(18) 0.042(3) 0.021(2) 0.0006(19) 0.0060(16) 0.0013(17) C12 0.025(3) 0.026(3) 0.027(3) -0.002(3) 0.011(2) 0.000(2) O12 0.030(2) 0.065(4) 0.044(3) 0.029(3) 0.004(2) -0.006(2) C13 0.031(3) 0.027(4) 0.028(3) 0.000(3) 0.014(3) 0.000(3) C14 0.032(3) 0.024(3) 0.023(3) -0.001(2) 0.015(2) -0.003(2) C16 0.025(3) 0.030(3) 0.027(3) 0.002(3) 0.013(2) 0.004(2) C15 0.034(3) 0.019(3) 0.026(3) 0.006(2) 0.015(2) 0.005(2) C18 0.043(4) 0.027(3) 0.040(4) 0.003(3) 0.029(3) 0.004(3) C17 0.040(3) 0.024(3) 0.044(4) 0.002(3) 0.028(3) -0.001(3) C19 0.023(3) 0.020(3) 0.034(3) 0.005(3) 0.011(3) 0.002(2) C20 0.024(3) 0.018(3) 0.024(3) 0.002(2) 0.009(2) 0.000(2) C21 0.024(3) 0.019(3) 0.027(3) 0.000(2) 0.012(2) 0.002(2) C22 0.027(3) 0.017(3) 0.020(3) 0.000(2) 0.006(2) 0.001(2) C23 0.023(3) 0.016(3) 0.026(3) 0.002(2) 0.011(2) 0.001(2) C24 0.026(3) 0.020(3) 0.022(3) -0.001(2) 0.008(2) 0.002(2) C25 0.029(3) 0.024(3) 0.018(3) 0.000(2) 0.008(2) -0.002(2) C26 0.034(3) 0.024(3) 0.018(3) 0.002(2) 0.008(2) 0.000(3) C27 0.033(3) 0.023(3) 0.020(3) 0.002(2) 0.010(2) 0.001(2) C28 0.039(3) 0.023(3) 0.019(3) 0.000(2) 0.004(2) 0.003(3) C29 0.046(4) 0.018(3) 0.026(3) -0.002(3) 0.007(3) -0.001(3) C30 0.032(3) 0.024(3) 0.021(3) 0.002(2) 0.009(2) -0.004(2) C31 0.026(3) 0.018(3) 0.020(3) 0.002(2) 0.009(2) 0.000(2) C32 0.022(2) 0.019(3) 0.020(3) 0.001(2) 0.008(2) -0.001(2) C33 0.026(3) 0.021(3) 0.025(3) 0.001(2) 0.016(2) 0.003(2) C34 0.022(3) 0.025(3) 0.020(3) -0.002(2) 0.008(2) -0.001(2) C35 0.018(2) 0.027(3) 0.024(3) 0.001(2) 0.007(2) 0.002(2) C36 0.025(3) 0.025(3) 0.021(3) 0.000(2) 0.011(2) -0.001(2) C37 0.030(3) 0.026(3) 0.026(3) 0.001(3) 0.014(2) 0.000(2) C38 0.029(3) 0.025(3) 0.023(3) -0.002(2) 0.014(2) 0.001(2) C39 0.056(4) 0.019(3) 0.042(4) -0.004(3) 0.034(3) -0.009(3) C40 0.048(4) 0.025(3) 0.044(4) -0.003(3) 0.033(3) -0.005(3) C41 0.039(3) 0.022(3) 0.040(4) -0.002(3) 0.023(3) -0.004(3) C42 0.032(3) 0.028(3) 0.034(3) 0.000(3) 0.023(3) -0.001(3) C43 0.025(3) 0.024(3) 0.027(3) -0.002(3) 0.008(2) -0.003(2) C44 0.025(3) 0.017(3) 0.022(3) -0.002(2) 0.009(2) 0.001(2) C45 0.025(3) 0.024(3) 0.025(3) -0.001(2) 0.013(2) -0.002(2) C46 0.031(3) 0.016(3) 0.023(3) 0.002(2) 0.009(2) 0.002(2) C48 0.026(3) 0.020(3) 0.023(3) 0.003(2) 0.008(2) 0.002(2) C47 0.026(3) 0.021(3) 0.026(3) -0.003(2) 0.013(2) -0.003(2) C101 0.052(6) 0.071(8) 0.057(7) 0.023(6) 0.030(5) 0.001(6) C102 0.077(8) 0.070(8) 0.068(8) 0.018(7) 0.051(7) 0.006(7) C103 0.047(6) 0.079(9) 0.066(8) 0.028(7) 0.025(6) -0.009(6) C104 0.039(5) 0.088(10) 0.053(7) 0.018(7) 0.009(5) -0.006(6) C105 0.036(5) 0.069(8) 0.064(7) 0.023(6) 0.017(5) -0.003(5) C106 0.038(5) 0.071(8) 0.052(6) 0.033(6) 0.020(5) 0.003(5) C107 0.036(5) 0.081(9) 0.051(6) 0.032(6) 0.022(5) 0.010(5) C108 0.046(6) 0.086(11) 0.060(8) 0.010(7) 0.031(6) 0.016(7) C109 0.047(6) 0.051(9) 0.070(8) 0.024(7) 0.019(6) 0.005(6) C110 0.040(5) 0.058(8) 0.065(8) 0.020(6) 0.015(5) 0.010(5) C111 0.069(8) 0.098(11) 0.064(8) 0.033(8) 0.044(7) 0.038(8) C112 0.130(15) 0.23(3) 0.114(15) 0.094(17) 0.092(13) 0.101(17) O113 0.068(5) 0.077(6) 0.049(4) 0.030(4) 0.034(4) 0.040(4) C201 0.073(7) 0.129(10) 0.066(7) 0.030(7) 0.021(6) 0.000(7) C202 0.077(7) 0.128(10) 0.070(7) 0.028(7) 0.016(6) -0.002(7) C203 0.071(7) 0.125(10) 0.065(7) 0.031(7) 0.020(6) 0.001(7) C204 0.066(7) 0.128(10) 0.061(7) 0.029(7) 0.022(6) 0.002(7) C205 0.068(7) 0.128(10) 0.061(7) 0.030(7) 0.022(6) 0.000(7) C206 0.072(7) 0.128(10) 0.064(6) 0.031(7) 0.021(6) 0.001(7) C207 0.073(7) 0.131(10) 0.064(7) 0.029(7) 0.022(6) 0.000(7) C208 0.073(7) 0.128(10) 0.059(7) 0.028(7) 0.025(6) -0.001(7) C209 0.069(7) 0.129(11) 0.062(7) 0.028(8) 0.018(6) -0.002(7) C210 0.069(7) 0.125(10) 0.061(7) 0.028(7) 0.020(6) 0.001(7) C211 0.071(7) 0.126(10) 0.060(7) 0.034(7) 0.025(6) -0.009(7) C212 0.097(11) 0.137(13) 0.084(11) 0.032(11) 0.013(10) -0.009(11) O213 0.075(9) 0.114(12) 0.066(9) 0.030(9) 0.020(8) -0.026(8) C301 0.046(6) 0.072(9) 0.044(7) 0.016(7) 0.023(6) 0.005(6) C302 0.047(6) 0.073(9) 0.046(7) 0.016(7) 0.022(6) 0.005(7) C303 0.046(7) 0.073(10) 0.046(7) 0.016(7) 0.023(6) 0.006(7) C304 0.045(7) 0.072(9) 0.046(7) 0.016(7) 0.022(6) 0.005(7) C305 0.046(6) 0.071(9) 0.045(7) 0.017(7) 0.023(6) 0.003(6) C306 0.045(6) 0.072(9) 0.045(6) 0.016(6) 0.022(6) 0.005(6) C307 0.040(6) 0.070(9) 0.040(6) 0.018(6) 0.031(5) 0.002(6) C308 0.048(7) 0.070(10) 0.044(7) 0.016(7) 0.023(6) 0.000(7) C309 0.045(7) 0.070(10) 0.043(7) 0.017(7) 0.019(6) 0.002(7) C310 0.048(6) 0.072(9) 0.044(7) 0.015(7) 0.022(6) 0.004(7) C311 0.046(7) 0.073(10) 0.046(7) 0.015(7) 0.024(6) 0.006(7) C312 0.049(10) 0.079(13) 0.040(10) 0.009(10) 0.023(9) 0.020(10) O313 0.046(8) 0.079(11) 0.054(9) 0.017(9) 0.019(8) 0.009(8) C401 0.130(9) 0.238(14) 0.087(7) -0.025(9) 0.075(7) -0.069(9) C402 0.129(9) 0.239(14) 0.087(7) -0.026(9) 0.077(7) -0.068(10) C403 0.129(9) 0.241(14) 0.090(7) -0.026(9) 0.078(7) -0.067(10) C404 0.127(9) 0.237(14) 0.088(7) -0.024(9) 0.076(7) -0.070(10) C405 0.128(9) 0.239(14) 0.088(7) -0.023(9) 0.077(7) -0.071(9) C406 0.128(9) 0.239(14) 0.088(7) -0.023(9) 0.077(7) -0.072(9) C407 0.129(9) 0.237(14) 0.088(7) -0.025(9) 0.076(7) -0.072(9) C408 0.131(9) 0.239(14) 0.089(7) -0.024(9) 0.074(7) -0.074(10) C409 0.130(10) 0.237(14) 0.085(7) -0.025(9) 0.074(8) -0.072(10) C410 0.126(9) 0.239(14) 0.087(7) -0.024(9) 0.075(7) -0.072(10) C411 0.133(9) 0.241(14) 0.093(7) -0.024(9) 0.074(7) -0.070(10) C412 0.146(12) 0.243(16) 0.102(11) -0.028(12) 0.060(11) -0.063(13) O413 0.123(11) 0.223(15) 0.089(9) -0.020(10) 0.086(8) -0.082(11) O601 0.21(5) 0.13(4) 0.05(2) 0.03(3) -0.01(3) 0.04(4) C602 0.16(6) 0.11(5) 0.18(6) -0.04(5) -0.02(5) 0.02(5) O801 0.080(12) 0.085(13) 0.060(12) 0.002(10) 0.030(9) -0.010(10) C802 0.062(13) 0.050(13) 0.045(13) 0.015(10) 0.006(9) -0.008(10) 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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 N1 C3 117.0(5) . . ? C4 N1 Cu1 119.0(4) . . ? C3 N1 Cu1 123.9(4) . . ? N1 Cu1 N6 122.5(2) . 1_656 ? N1 Cu1 N2 106.8(2) . 4_576 ? N6 Cu1 N2 99.5(2) 1_656 4_576 ? N1 Cu1 Br1 109.92(15) . . ? N6 Cu1 Br1 105.58(15) 1_656 . ? N2 Cu1 Br1 112.18(15) 4_576 . ? C2 C1 C5 118.8(6) . . ? C2 C1 C6 123.7(6) . . ? C5 C1 C6 117.5(6) . . ? N4 Cu2 N3 119.8(2) . . ? N4 Cu2 N5 106.5(2) . 4_566 ? N3 Cu2 N5 105.1(2) . 4_566 ? N4 Cu2 Br2 108.51(15) . . ? N3 Cu2 Br2 106.25(14) . . ? N5 Cu2 Br2 110.47(14) 4_566 . ? C6 O2 C7 115.9(5) . . ? C16 N2 C17 117.1(5) . . ? C16 N2 Cu1 117.7(4) . 4_575 ? C17 N2 Cu1 124.6(4) . 4_575 ? C1 C2 C3 118.8(6) . . ? N1 C3 C2 122.9(6) . . ? C23 N3 C22 118.3(5) . . ? C23 N3 Cu2 117.2(4) . . ? C22 N3 Cu2 124.3(4) . . ? C13 O3 C9 118.6(5) . . ? N1 C4 C5 123.2(6) . . ? C28 N4 C27 117.6(5) . . ? C28 N4 Cu2 119.7(4) . . ? C27 N4 Cu2 122.0(4) . . ? C19 O5 C11 118.2(5) . . ? C41 N5 C40 116.6(5) . . ? C41 N5 Cu2 126.2(4) . 4_565 ? C40 N5 Cu2 117.1(4) . 4_565 ? C4 C5 C1 119.2(6) . . ? C46 N6 C47 117.6(5) . . ? C46 N6 Cu1 124.7(4) . 1_454 ? C47 N6 Cu1 117.5(4) . 1_454 ? O1 C6 O2 123.9(6) . . ? O1 C6 C1 124.7(6) . . ? O2 C6 C1 111.4(5) . . ? C8 C7 C12 123.6(5) . . ? C8 C7 O2 119.8(5) . . ? C12 C7 O2 116.6(5) . . ? C7 C8 C9 116.9(5) . . ? C30 O8 C31 117.9(5) . . ? C10 C9 C8 122.6(5) . . ? C10 C9 O3 116.5(5) . . ? C8 C9 O3 120.7(5) . . ? C37 O9 C33 117.4(5) . . ? C11 C10 C9 117.3(5) . . ? C10 C11 C12 123.5(5) . . ? C10 C11 O5 116.3(5) . . ? C12 C11 O5 120.1(5) . . ? C43 O11 C35 118.4(5) . . ? C11 C12 C7 116.1(6) . . ? O4 C13 O3 124.0(6) . . ? O4 C13 C14 125.1(6) . . ? O3 C13 C14 110.9(5) . . ? C15 C14 C18 118.3(6) . . ? C15 C14 C13 118.2(6) . . ? C18 C14 C13 123.5(6) . . ? N2 C16 C15 124.6(6) . . ? C14 C15 C16 118.3(6) . . ? C14 C18 C17 119.3(6) . . ? N2 C17 C18 122.3(6) . . ? O6 C19 O5 124.0(5) . . ? O6 C19 C20 126.2(6) . . ? O5 C19 C20 109.8(5) . . ? C21 C20 C24 118.9(5) . . ? C21 C20 C19 123.0(5) . . ? C24 C20 C19 118.0(5) . . ? C20 C21 C22 118.5(5) . . ? N3 C22 C21 122.8(5) . . ? N3 C23 C24 123.7(5) . . ? C23 C24 C20 117.7(5) . . ? C26 C25 C29 118.6(6) . . ? C26 C25 C30 123.9(6) . . ? C29 C25 C30 117.5(6) . . ? C27 C26 C25 118.8(6) . . ? N4 C27 C26 123.2(6) . . ? N4 C28 C29 123.2(6) . . ? C28 C29 C25 118.6(6) . . ? O7 C30 O8 123.7(6) . . ? O7 C30 C25 124.5(6) . . ? O8 C30 C25 111.8(5) . . ? C36 C31 C32 123.0(5) . . ? C36 C31 O8 116.3(5) . . ? C32 C31 O8 120.6(5) . . ? C33 C32 C31 117.1(5) . . ? C32 C33 C34 122.9(5) . . ? C32 C33 O9 119.5(5) . . ? C34 C33 O9 117.5(5) . . ? C35 C34 C33 116.9(5) . . ? C34 C35 C36 123.7(5) . . ? C34 C35 O11 116.3(5) . . ? C36 C35 O11 119.9(5) . . ? C31 C36 C35 116.4(5) . . ? O10 C37 O9 123.8(6) . . ? O10 C37 C38 124.9(6) . . ? O9 C37 C38 111.3(5) . . ? C42 C38 C39 118.4(6) . . ? C42 C38 C37 124.1(6) . . ? C39 C38 C37 117.5(6) . . ? C40 C39 C38 119.4(6) . . ? N5 C40 C39 123.4(6) . . ? N5 C41 C42 122.9(6) . . ? C38 C42 C41 119.2(6) . . ? O12 C43 O11 124.3(5) . . ? O12 C43 C44 124.6(6) . . ? O11 C43 C44 111.1(5) . . ? C45 C44 C48 119.3(5) . . ? C45 C44 C43 122.4(5) . . ? C48 C44 C43 118.3(5) . . ? C44 C45 C46 117.9(5) . . ? N6 C46 C45 123.2(5) . . ? C47 C48 C44 118.5(6) . . ? N6 C47 C48 123.4(6) . . ? C102 C101 C106 115.8(11) . . ? C102 C101 C111 122.1(12) . . ? C106 C101 C111 122.1(11) . . ? C101 C102 C103 126.4(13) . . ? C104 C103 C102 116.2(13) . . ? C103 C104 C105 121.6(11) . . ? C104 C105 C106 116.6(11) . . ? C104 C105 C110 122.9(10) . . ? C106 C105 C110 120.5(11) . . ? C101 C106 C105 123.2(11) . . ? C101 C106 C107 122.0(9) . . ? C105 C106 C107 114.8(10) . . ? C108 C107 C106 121.9(10) . . ? C109 C108 C107 118.5(14) . . ? C110 C109 C108 122.1(13) . . ? C109 C110 C105 122.2(11) . . ? O113 C111 C101 123.1(10) . . ? O113 C111 C112 117.2(11) . . ? C101 C111 C112 119.5(12) . . ? C202 C201 C206 114(2) . . ? C202 C201 C211 126.5(17) . . ? C206 C201 C211 119.1(15) . . ? C201 C202 C203 123(2) . . ? C204 C203 C202 118(2) . . ? C203 C204 C205 121(2) . . ? C204 C205 C206 114(2) . . ? C204 C205 C210 126(2) . . ? C206 C205 C210 119(2) . . ? C201 C206 C205 127(2) . . ? C201 C206 C207 114.9(18) . . ? C205 C206 C207 117.7(18) . . ? C208 C207 C206 114.7(19) . . ? C209 C208 C207 122(2) . . ? C210 C209 C208 121(3) . . ? C209 C210 C205 122(2) . . ? O213 C211 C201 121(2) . . ? O213 C211 C212 117(2) . . ? C201 C211 C212 118(2) . . ? C306 C301 C302 117.9(19) . . ? C306 C301 C311 122.7(19) . . ? C302 C301 C311 119.4(18) . . ? C301 C302 C303 121(2) . . ? C304 C303 C302 119(3) . . ? C303 C304 C305 121(3) . . ? C304 C305 C306 114(2) . . ? C304 C305 C310 123(2) . . ? C306 C305 C310 121.4(19) . . ? C301 C306 C305 124.8(19) . . ? C301 C306 C307 120.6(19) . . ? C305 C306 C307 114.5(17) . . ? C308 C307 C306 118(2) . . ? C309 C308 C307 122(2) . . ? C310 C309 C308 121(2) . . ? C309 C310 C305 121(2) . . ? O313 C311 C301 123(2) . . ? O313 C311 C312 117(2) . . ? C301 C311 C312 119(2) . . ? C402 C401 C406 118(2) . . ? C402 C401 C411 128.0(18) . . ? C406 C401 C411 111.4(15) . . ? C401 C402 C403 120(2) . . ? C404 C403 C402 120(3) . . ? C403 C404 C405 121(2) . . ? C404 C405 C406 112(2) . . ? C404 C405 C410 133(2) . . ? C406 C405 C410 114(2) . . ? C401 C406 C405 128(2) . . ? C401 C406 C407 106.3(18) . . ? C405 C406 C407 125(2) . . ? C408 C407 C406 111(2) . . ? C409 C408 C407 121(3) . . ? C410 C409 C408 124(3) . . ? C409 C410 C405 123(3) . . ? O413 C411 C401 120(2) . . ? O413 C411 C412 130(3) . . ? C401 C411 C412 109(2) . . ? 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 Br1 Cu1 2.4244(11) . ? O1 C6 1.198(8) . ? N1 C4 1.344(8) . ? N1 C3 1.352(8) . ? N1 Cu1 2.006(5) . ? Cu1 N6 2.034(5) 1_656 ? Cu1 N2 2.089(5) 4_576 ? C1 C2 1.377(9) . ? C1 C5 1.383(9) . ? C1 C6 1.496(9) . ? Cu2 N4 2.028(5) . ? Cu2 N3 2.030(5) . ? Cu2 N5 2.067(5) 4_566 ? Cu2 Br2 2.4359(10) . ? O2 C6 1.355(8) . ? O2 C7 1.405(7) . ? N2 C16 1.324(8) . ? N2 C17 1.352(8) . ? C2 C3 1.393(8) . ? N3 C23 1.332(8) . ? N3 C22 1.339(8) . ? O3 C13 1.356(7) . ? O3 C9 1.398(7) . ? C4 C5 1.380(9) . ? O4 C13 1.188(8) . ? N4 C28 1.337(8) . ? N4 C27 1.345(7) . ? O5 C19 1.360(7) . ? O5 C11 1.408(7) . ? N5 C41 1.346(8) . ? N5 C40 1.360(8) . ? O6 C19 1.187(8) . ? N6 C46 1.334(8) . ? N6 C47 1.350(8) . ? C7 C8 1.384(8) . ? C7 C12 1.391(8) . ? O7 C30 1.202(8) . ? C8 C9 1.390(8) . ? O8 C30 1.357(7) . ? O8 C31 1.395(7) . ? C9 C10 1.385(8) . ? O9 C37 1.351(7) . ? O9 C33 1.405(7) . ? C10 C11 1.380(9) . ? O10 C37 1.192(8) . ? C11 C12 1.388(9) . ? O11 C43 1.346(7) . ? O11 C35 1.406(6) . ? O12 C43 1.195(8) . ? C13 C14 1.495(9) . ? C14 C15 1.383(9) . ? C14 C18 1.390(9) . ? C16 C15 1.386(9) . ? C18 C17 1.391(9) . ? C19 C20 1.483(8) . ? C20 C21 1.395(8) . ? C20 C24 1.406(8) . ? C21 C22 1.396(8) . ? C23 C24 1.391(8) . ? C25 C26 1.385(9) . ? C25 C29 1.393(9) . ? C25 C30 1.482(8) . ? C26 C27 1.379(8) . ? C28 C29 1.386(9) . ? C31 C36 1.388(8) . ? C31 C32 1.390(8) . ? C32 C33 1.387(8) . ? C33 C34 1.388(8) . ? C34 C35 1.376(8) . ? C35 C36 1.393(8) . ? C37 C38 1.496(9) . ? C38 C42 1.376(9) . ? C38 C39 1.388(9) . ? C39 C40 1.367(9) . ? C41 C42 1.394(9) . ? C43 C44 1.494(8) . ? C44 C45 1.389(8) . ? C44 C48 1.390(8) . ? C45 C46 1.395(8) . ? C48 C47 1.370(8) . ? C101 C102 1.340(14) . ? C101 C106 1.399(13) . ? C101 C111 1.458(15) . ? C102 C103 1.408(15) . ? C103 C104 1.401(18) . ? C104 C105 1.410(17) . ? C105 C106 1.431(13) . ? C105 C110 1.439(16) . ? C106 C107 1.461(16) . ? C107 C108 1.45(2) . ? C108 C109 1.376(16) . ? C109 C110 1.328(17) . ? C111 O113 1.221(13) . ? C111 C112 1.547(18) . ? C201 C202 1.332(18) . ? C201 C206 1.360(18) . ? C201 C211 1.45(2) . ? C202 C203 1.45(2) . ? C203 C204 1.39(2) . ? C204 C205 1.40(2) . ? C205 C206 1.41(2) . ? C205 C210 1.42(2) . ? C206 C207 1.48(2) . ? C207 C208 1.47(3) . ? C208 C209 1.34(2) . ? C209 C210 1.28(2) . ? C211 O213 1.23(2) . ? C211 C212 1.53(2) . ? C301 C306 1.354(18) . ? C301 C302 1.364(19) . ? C301 C311 1.44(2) . ? C302 C303 1.44(2) . ? C303 C304 1.39(3) . ? C304 C305 1.41(2) . ? C305 C306 1.44(2) . ? C305 C310 1.44(2) . ? C306 C307 1.47(2) . ? C307 C308 1.45(3) . ? C308 C309 1.35(2) . ? C309 C310 1.30(2) . ? C311 O313 1.22(2) . ? C311 C312 1.52(2) . ? C401 C402 1.277(19) . ? C401 C406 1.346(19) . ? C401 C411 1.43(2) . ? C402 C403 1.44(2) . ? C403 C404 1.37(2) . ? C404 C405 1.39(2) . ? C405 C406 1.40(2) . ? C405 C410 1.42(2) . ? C406 C407 1.48(2) . ? C407 C408 1.46(3) . ? C408 C409 1.36(2) . ? C409 C410 1.29(2) . ? C411 O413 1.26(2) . ? C411 C412 1.55(2) . ? O601 C602 1.43(2) . ? O801 C802 1.39(2) . ?