#------------------------------------------------------------------------------ #$Date: 2021-06-03 06:57:50 +0300 (Thu, 03 Jun 2021) $ #$Revision: 265696 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/81/7158108.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_7158108 loop_ _publ_author_name 'Tsou, Yun-Jie' 'Guan, Ren-You' 'Han, Jeng-Liang' _publ_section_title ; Enantioselective organocatalytic vinylogous aldol−cyclization cascade reaction of 3-alkylidene oxindoles with o-quinones ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/D1OB00888A _journal_year 2021 _chemical_formula_moiety 'C32 H26 Br N O4.5' _chemical_formula_sum 'C32 H26 Br N O4.5' _chemical_formula_weight 576.45 _space_group_crystal_system monoclinic _space_group_IT_number 5 _space_group_name_Hall 'I 2y' _space_group_name_H-M_alt 'I 1 2 1' _atom_sites_solution_hydrogens mixed _audit_creation_date 2020-09-29 _audit_creation_method ; Olex2 1.2-ac3 (compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318) ; _audit_update_record ; 2020-09-29 deposited with the CCDC. 2021-06-01 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.737(16) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.179(2) _cell_length_b 15.131(6) _cell_length_c 26.209(11) _cell_measurement_reflns_used 3213 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 23.61 _cell_measurement_theta_min 2.91 _cell_volume 2843.7(18) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 150.15 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.1031 _diffrn_reflns_av_unetI/netI 0.0981 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 22836 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.243 _diffrn_reflns_theta_max 26.550 _diffrn_reflns_theta_min 2.909 _exptl_absorpt_coefficient_mu 1.484 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.346 _exptl_crystal_description BLOCK _exptl_crystal_F_000 1184 _exptl_transmission_factor_max 0.987 _exptl_transmission_factor_min 0.253 _platon_squeeze_details ; TITL g129_5br2_3_0m_a.res in P1 New:I2 CELL 7.1790 15.1310 26.2090 90.00 92.74 90.00 SPGR I2 # Solvent Accessible Volume = 233 # Electrons Found in S.A.V. = 71 # Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others Q101 0.438 0.220 0.222 ! 5.73 eA-3 Q102 0.090 0.597 0.243 ! 4.23 eA-3 Q103 0.603 0.809 0.436 ! 2.96 eA-3 Q104 0.691 0.256 0.127 ! 2.83 eA-3 Q105 0.755 0.514 0.089 ! 2.57 eA-3 Q106 0.810 0.580 0.114 ! 2.36 eA-3 Q107 0.101 0.485 0.243 ! 2.36 eA-3 Q108 0.413 0.698 0.393 ! 1.86 eA-3 Q109 0.059 0.336 0.296 ! 1.73 eA-3 Q110 0.902 0.378 0.042 ! 1.72 eA-3 C111 0.782 0.321 0.068 ! 1.67 eA-3 Q112 0.274 0.922 0.479 ! 1.66 eA-3 Q113 1.010 0.653 0.226 ! 1.62 eA-3 Q114 0.797 0.328 0.366 ! 1.57 eA-3 Q115 0.963 0.411 0.023 ! 1.49 eA-3 Q116 0.819 0.252 0.073 ! 1.46 eA-3 Q117 0.946 0.623 0.264 ! 1.44 eA-3 Q118 0.849 0.438 0.039 ! 1.43 eA-3 Q119 0.523 0.512 0.053 ! 1.33 eA-3 Q120 0.385 0.780 0.423 ! 1.29 eA-3 Q121 0.643 0.769 0.486 ! 1.28 eA-3 Q122 0.180 0.248 0.027 ! 1.26 eA-3 Q123 0.805 0.772 0.477 ! 1.25 eA-3 Q124 0.942 0.278 0.183 ! 1.24 eA-3 Q125 0.498 0.376-0.001 ! 1.19 eA-3 C126 1.001 0.359 0.003 ! 1.18 eA-3 Q127 0.055 0.707 0.201 ! 1.17 eA-3 Q128 0.370 0.470 0.038 ! 1.15 eA-3 Q129 0.065 0.529 0.032 ! 1.12 eA-3 Q130 0.123 0.206 0.179 ! 1.10 eA-3 Q131 0.952 0.564 0.005 ! 1.09 eA-3 C132 0.574 0.403 0.026 ! 1.08 eA-3 Q133 0.089 0.409 0.030 ! 1.08 eA-3 C134 0.604 0.465-0.001 ! 1.06 eA-3 Q135 0.095 0.007 0.478 ! 1.05 eA-3 Q136 0.994 0.762 0.250 ! 0.95 eA-3 Q137 0.095 0.477 0.042 ! 0.93 eA-3 Q138 0.527 0.985 0.453 ! 0.92 eA-3 Q139 0.756 0.480 0.017 ! 0.91 eA-3 Q140 0.245 0.190 0.143 ! 0.91 eA-3 Q141 0.339 0.578 0.312 ! 0.90 eA-3 Q142 0.379 0.339 0.495 ! 0.89 eA-3 Q143 0.689 0.348 0.097 ! 0.89 eA-3 Q144 0.685 0.373 0.270 ! 0.87 eA-3 Q145 0.335 0.229 0.266 ! 0.87 eA-3 Q146 0.308 0.387 0.364 ! 0.87 eA-3 Q147 0.711 0.609 0.173 ! 0.86 eA-3 Q148 0.600 0.332 0.410 ! 0.86 eA-3 Q149 0.344 0.468 0.358 ! 0.85 eA-3 Q150 0.939 0.302 0.100 ! 0.82 eA-3 Q151 0.971 0.327 0.034 ! 0.81 eA-3 Q152 1.000 0.656 0.003 ! 0.81 eA-3 Q153 0.982 0.599 0.211 ! 0.81 eA-3 Q154 0.929 0.237 0.102 ! 0.81 eA-3 Q155 0.146 0.378-0.001 ! 0.80 eA-3 Q156 0.024 0.831 0.421 ! 0.80 eA-3 Q157 0.594 0.045 0.423 ! 0.79 eA-3 Q158 0.050 0.373 0.392 ! 0.78 eA-3 Q159 0.871 0.022 0.476 ! 0.77 eA-3 Q160 0.160 0.264 0.211 ! 0.77 eA-3 Q161 0.475 0.517 0.089 ! 0.77 eA-3 Q162 0.282 0.910 0.244 ! 0.76 eA-3 Q163 0.099 0.797 0.082 ! 0.76 eA-3 Q164 0.476 0.438 0.054 ! 0.76 eA-3 Q165 0.222 0.343 0.151 ! 0.76 eA-3 Q166 0.722 0.843 0.651 ! 0.76 eA-3 Q167 0.193 0.283 0.310 ! 0.75 eA-3 Q168 0.627 0.312 0.308 ! 0.75 eA-3 Q169 0.777 0.346 0.854 ! 0.74 eA-3 Q170 0.906 0.043 0.295 ! 0.74 eA-3 Q171 0.457 0.798 0.140 ! 0.74 eA-3 Q172 0.841 0.452 0.442 ! 0.74 eA-3 Q173 0.718 0.187 0.052 ! 0.73 eA-3 Q174 0.759 0.919 0.195 ! 0.73 eA-3 Q175 0.907 0.523 0.373 ! 0.73 eA-3 Q176 0.280 0.345 0.445 ! 0.73 eA-3 Q177 0.720 0.343 0.554 ! 0.72 eA-3 Q178 0.685 0.391 0.340 ! 0.71 eA-3 Q179 0.781 0.925 0.465 ! 0.70 eA-3 Q180 0.690 0.545 0.150 ! 0.70 eA-3 Q181 0.092 0.798 0.821 ! 0.70 eA-3 Q182 0.655 0.786 0.287 ! 0.70 eA-3 Q183 0.155 0.286 0.787 ! 0.70 eA-3 Q184 0.991 0.365 0.079 ! 0.70 eA-3 Q185 0.154 0.042 0.257 ! 0.69 eA-3 Q186 1.009 0.955 0.427 ! 0.69 eA-3 Q187 0.131 0.994 0.172 ! 0.69 eA-3 Q188 0.453 0.228 0.276 ! 0.69 eA-3 Q189 0.660 0.319 0.362 ! 0.68 eA-3 C190 0.369 0.950 0.494 ! 0.68 eA-3 Q191 0.073 0.388 0.465 ! 0.68 eA-3 Q192 0.487 0.263 0.138 ! 0.67 eA-3 Q193 0.947 0.270 0.236 ! 0.67 eA-3 Q194 0.289 0.184 0.228 ! 0.67 eA-3 Q195 0.228 0.315 0.000 ! 0.67 eA-3 Q196 0.191 0.029 0.155 ! 0.66 eA-3 Q197 0.905 0.701 0.294 ! 0.66 eA-3 Q198 0.623 0.156 0.261 ! 0.66 eA-3 Q199 0.500 0.595 0.251 ! 0.66 eA-3 ; _refine_diff_density_max 3.305 _refine_diff_density_min -1.512 _refine_diff_density_rms 0.204 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.08(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.399 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 333 _refine_ls_number_reflns 5867 _refine_ls_number_restraints 19 _refine_ls_restrained_S_all 1.396 _refine_ls_R_factor_all 0.1774 _refine_ls_R_factor_gt 0.1340 _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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3476 _refine_ls_wR_factor_ref 0.3844 _reflns_Friedel_coverage 0.920 _reflns_Friedel_fraction_full 0.996 _reflns_Friedel_fraction_max 0.990 _reflns_number_gt 3954 _reflns_number_total 5867 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL g129_5br2_3_0m_a.res in P1 New:I2 g129_5br2_3.res created by SHELXL-2018/3 at 14:15:57 on 29-Sep-2020 CELL 0.71076 7.179 15.131 26.209 90 92.737 90 ZERR 4 0.002 0.006 0.011 0 0.016 0 LATT -2 SYMM -X,+Y,-Z SFAC C H Br N O UNIT 128 104 4 4 18 ISOR 0.001 0.002 C31 ISOR 0.001 0.002 C6 ISOR 0.001 0.002 O10 ISOR 0.001 0.002 C19 ISOR 0.001 0.002 C20 ISOR 0.001 0.002 O6 L.S. 50 0 20 PLAN -100 TEMP -123 CONF BOND $H ABIN fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 OMIT 1 -3 4 OMIT 1 3 4 OMIT -2 3 3 OMIT -2 -3 3 REM REM REM WGHT 0.200000 BASF 0.08034 FVAR 0.27802 BR02 3 -0.287452 0.036531 0.393307 11.00000 0.05100 0.07686 = 0.05359 -0.02837 0.01621 -0.00001 O004 5 -0.006802 -0.168377 0.165650 11.00000 0.02193 0.03719 = 0.03889 -0.02033 0.00555 0.00738 O006 5 0.164185 -0.003321 0.114905 11.00000 0.06930 0.02659 = 0.05085 -0.01459 0.00641 0.00120 O007 5 -0.230924 -0.113470 0.208350 11.00000 0.02115 0.05032 = 0.05829 -0.02121 0.01177 -0.00489 PART 1 O6 5 0.176007 0.195351 0.128831 10.75000 0.07210 0.07117 = 0.07188 -0.00056 0.00443 -0.00068 O10 5 0.023788 0.281027 0.182819 10.75000 0.14480 0.14332 = 0.14430 -0.00064 0.00752 -0.00024 PART 0 N00P 4 0.028857 0.128339 0.188302 11.00000 0.06933 0.02843 = 0.08119 -0.02727 0.03737 -0.00674 AFIX 3 H00P 2 0.089907 0.084359 0.174762 11.00000 -1.20000 AFIX 0 C009 1 0.235615 -0.213012 0.064723 11.00000 0.01626 0.02189 = 0.03429 -0.01405 -0.00568 -0.00070 C00A 1 0.222683 -0.237092 0.117193 11.00000 0.03634 0.02022 = 0.03126 -0.00494 0.00502 -0.00611 C00D 1 0.220486 -0.123108 0.056045 11.00000 0.02926 0.02301 = 0.03376 -0.00413 0.00687 -0.00447 C00E 1 0.188018 -0.079910 0.106686 11.00000 0.03734 0.01788 = 0.03301 -0.00869 0.00693 0.00901 C00J 1 0.276811 -0.148180 -0.032970 11.00000 0.02845 0.03658 = 0.03668 -0.00114 0.00054 0.00687 C00L 1 -0.065860 -0.108101 0.198942 11.00000 0.02329 0.03266 = 0.03922 -0.01210 0.00956 0.00272 C00N 1 -0.188001 0.066825 0.329375 11.00000 0.01802 0.07095 = 0.04856 -0.03723 0.01154 -0.00204 C00O 1 0.278147 -0.366251 0.038532 11.00000 0.02904 0.02513 = 0.07111 -0.01462 -0.00005 0.00835 AFIX 43 H00O 2 0.293240 -0.410304 0.013235 11.00000 -1.20000 AFIX 0 C00Q 1 0.272046 -0.389022 0.091890 11.00000 0.05824 0.02848 = 0.03253 -0.00269 -0.00029 -0.00868 AFIX 43 H00Q 2 0.289744 -0.449222 0.101203 11.00000 -1.20000 AFIX 0 C00S 1 0.260725 -0.275405 0.025222 11.00000 0.01798 0.02595 = 0.03742 -0.00917 0.00138 -0.00560 C00V 1 0.067732 -0.050859 0.226018 11.00000 0.03776 0.05739 = 0.03096 -0.03112 0.00825 -0.00089 C010 1 0.186630 -0.156263 0.147087 11.00000 0.02274 0.03332 = 0.03028 -0.00311 -0.00625 0.00408 C011 1 0.240994 -0.326624 0.131724 11.00000 0.03459 0.02864 = 0.03541 -0.01098 0.01006 0.00327 AFIX 43 H011 2 0.233105 -0.344653 0.166274 11.00000 -1.20000 AFIX 0 C013 1 0.320408 -0.138456 0.192612 11.00000 0.01547 0.03813 = 0.03425 -0.00871 0.00439 0.00584 AFIX 23 H01A 2 0.336818 -0.193158 0.213059 11.00000 -1.20000 H01B 2 0.443626 -0.121449 0.180299 11.00000 -1.20000 AFIX 0 C016 1 0.241742 -0.087520 0.008241 11.00000 0.01700 0.03156 = 0.04458 -0.01310 -0.00719 -0.00202 C019 1 -0.092171 0.000391 0.303421 11.00000 0.03862 0.04312 = 0.04082 -0.01425 -0.00234 0.00562 AFIX 43 H019 2 -0.078676 -0.057463 0.317186 11.00000 -1.20000 AFIX 0 C17 1 0.218922 0.347011 0.104624 11.00000 10.05000 AFIX 137 H17A 2 0.111147 0.338332 0.080775 11.00000 -1.50000 H17B 2 0.301489 0.391901 0.091000 11.00000 -1.50000 H17C 2 0.176062 0.366635 0.137712 11.00000 -1.50000 AFIX 0 C01B 1 0.236615 0.004628 -0.002445 11.00000 0.04485 0.04187 = 0.03720 -0.00038 -0.00376 -0.00131 AFIX 43 H01C 2 0.215043 0.045547 0.024123 11.00000 -1.20000 AFIX 0 C01D 1 -0.017681 0.022550 0.256737 11.00000 0.02301 0.04314 = 0.04516 -0.02688 0.00795 -0.00039 C19 1 0.047647 0.213781 0.164750 11.00000 0.09814 0.09797 = 0.09815 -0.00035 0.00499 -0.00010 C01E 1 0.280576 -0.242460 -0.022701 11.00000 0.04239 0.03798 = 0.03069 -0.00585 0.00307 0.00326 AFIX 43 H01E 2 0.297324 -0.282344 -0.050099 11.00000 -1.20000 AFIX 0 C20 1 0.366976 0.233121 0.059785 11.00000 10.05000 AFIX 137 H20A 2 0.463916 0.271232 0.046543 11.00000 -1.50000 H20B 2 0.255323 0.235641 0.036811 11.00000 -1.50000 H20C 2 0.412615 0.172130 0.061933 11.00000 -1.50000 AFIX 0 C01F 1 0.250523 -0.066943 0.225379 11.00000 0.03000 0.02561 = 0.03668 -0.01193 0.00598 -0.00695 C01J 1 0.298868 -0.022286 -0.089175 11.00000 0.04069 0.05656 = 0.03170 0.00283 -0.01014 -0.00903 AFIX 43 H01J 2 0.320380 0.002015 -0.121793 11.00000 -1.20000 AFIX 0 C01M 1 -0.206267 0.152816 0.309724 11.00000 0.03992 0.04134 = 0.05673 -0.01875 0.00941 -0.00781 AFIX 43 H01M 2 -0.269739 0.197152 0.327792 11.00000 -1.20000 AFIX 0 C01N 1 0.306336 -0.116398 -0.083200 11.00000 0.02216 0.05723 = 0.05692 0.01011 -0.01653 0.00684 AFIX 43 H01N 2 0.329367 -0.154975 -0.110794 11.00000 -1.20000 AFIX 0 C01P 1 -0.131895 0.171192 0.264688 11.00000 0.04186 0.04295 = 0.05746 -0.01910 0.02011 0.00038 AFIX 43 H01P 2 -0.142752 0.229711 0.251753 11.00000 -1.20000 AFIX 0 C01R 1 0.262290 0.034161 -0.050204 11.00000 0.04136 0.05641 = 0.06133 0.03486 -0.01414 0.00496 AFIX 43 H01R 2 0.254731 0.095795 -0.056893 11.00000 -1.20000 AFIX 0 C01X 1 -0.042683 0.110467 0.237050 11.00000 0.04718 0.03939 = 0.06927 -0.02890 0.02979 -0.01940 C31 1 0.320342 0.263819 0.111155 11.00000 10.05000 C6 1 0.519785 0.251559 0.150134 11.00000 10.05000 AFIX 137 H6A 2 0.522991 0.297346 0.176607 11.00000 -1.50000 H6B 2 0.629827 0.257268 0.129646 11.00000 -1.50000 H6C 2 0.519600 0.193114 0.166245 11.00000 -1.50000 AFIX 0 C3 1 0.399028 -0.016309 0.257291 11.00000 0.05177 0.05318 = 0.07154 -0.01767 -0.01532 0.00310 AFIX 137 H3A 2 0.471318 0.020763 0.234808 11.00000 -1.50000 H3B 2 0.482431 -0.058336 0.275373 11.00000 -1.50000 H3C 2 0.338515 0.021099 0.282143 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 -1 0 -1 -1 -2 REM g129_5br2_3_0m_a.res in P1 New:I2 REM wR2 = 0.3844, GooF = S = 1.399, Restrained GooF = 1.396 for all data REM R1 = 0.1340 for 3954 Fo > 4sig(Fo) and 0.1774 for all 5867 data REM 333 parameters refined using 19 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 3.305, deepest hole -1.512, 1-sigma level 0.204 Q1 1 0.4486 0.2316 0.2087 11.00000 0.05 3.30 Q2 1 0.6977 0.2468 0.1293 11.00000 0.05 2.88 Q3 1 0.0943 0.2067 0.1116 11.00000 0.05 2.04 Q4 1 0.3034 -0.1739 -0.1280 11.00000 0.05 1.56 Q5 1 0.1497 0.2624 0.2096 11.00000 0.05 1.51 Q6 1 0.4313 -0.1570 0.2032 11.00000 0.05 1.37 Q7 1 0.1753 0.2430 0.0300 11.00000 0.05 1.23 Q8 1 0.1129 0.2800 0.0780 11.00000 0.05 1.21 Q9 1 0.2313 0.1857 0.1404 11.00000 0.05 0.96 Q10 1 0.1410 0.1966 0.1850 11.00000 0.05 0.87 Q11 1 0.1198 -0.1561 0.0072 11.00000 0.05 0.87 Q12 1 0.1232 -0.1722 -0.0789 11.00000 0.05 0.70 Q13 1 0.2551 0.3302 0.1598 11.00000 0.05 0.70 Q14 1 0.1330 -0.2062 0.0741 11.00000 0.05 0.67 Q15 1 0.1520 -0.1780 0.2083 11.00000 0.05 0.65 Q16 1 0.0871 -0.1276 0.1115 11.00000 0.05 0.64 Q17 1 0.1256 -0.1182 0.1887 11.00000 0.05 0.58 Q18 1 0.2856 0.1832 -0.0373 11.00000 0.05 0.58 Q19 1 0.4714 0.3302 0.0812 11.00000 0.05 0.56 Q20 1 -0.5380 -0.0127 0.4257 11.00000 0.05 0.55 Q21 1 0.1662 0.0224 0.2586 11.00000 0.05 0.54 Q22 1 -0.0664 0.2857 0.1786 11.00000 0.05 0.53 Q23 1 0.0048 0.3402 0.0873 11.00000 0.05 0.53 Q24 1 -0.0921 0.2338 0.0984 11.00000 0.05 0.52 Q25 1 -0.1908 0.2906 0.2125 11.00000 0.05 0.52 Q26 1 0.0224 -0.1231 0.0582 11.00000 0.05 0.52 Q27 1 0.4849 0.1922 0.1095 11.00000 0.05 0.51 Q28 1 -0.5000 0.1665 0.5000 10.50000 0.05 0.50 Q29 1 0.5465 0.1689 0.1613 11.00000 0.05 0.50 Q30 1 0.2879 -0.3012 0.1298 11.00000 0.05 0.50 Q31 1 -0.3443 0.1280 0.2453 11.00000 0.05 0.50 Q32 1 0.2699 -0.3715 0.0718 11.00000 0.05 0.50 Q33 1 -0.2398 0.1045 0.3216 11.00000 0.05 0.49 Q34 1 0.3474 0.0251 0.0832 11.00000 0.05 0.49 Q35 1 0.2178 -0.1088 0.1418 11.00000 0.05 0.49 Q36 1 -0.0693 0.0373 0.2934 11.00000 0.05 0.49 Q37 1 0.2512 -0.0410 -0.0076 11.00000 0.05 0.49 Q38 1 0.4406 -0.2084 0.1365 11.00000 0.05 0.48 Q39 1 -0.0753 0.0286 0.3306 11.00000 0.05 0.48 Q40 1 0.2202 -0.1532 0.0504 11.00000 0.05 0.48 Q41 1 0.5904 0.1925 0.2084 11.00000 0.05 0.47 Q42 1 -0.1706 -0.1800 0.1394 11.00000 0.05 0.46 Q43 1 -0.0852 -0.2183 0.1705 11.00000 0.05 0.46 Q44 1 0.4048 -0.0514 0.1741 11.00000 0.05 0.45 Q45 1 0.1388 0.0405 0.1408 11.00000 0.05 0.45 Q46 1 0.3155 0.1267 -0.0937 11.00000 0.05 0.44 Q47 1 -0.2094 -0.1294 0.2813 11.00000 0.05 0.44 Q48 1 -0.1792 -0.1413 0.2740 11.00000 0.05 0.43 Q49 1 0.0696 0.2828 0.1252 11.00000 0.05 0.42 Q50 1 0.2473 0.2185 -0.0202 11.00000 0.05 0.42 Q51 1 -0.3562 0.0324 0.1801 11.00000 0.05 0.42 Q52 1 -0.2130 0.3614 0.1813 11.00000 0.05 0.42 Q53 1 -0.0506 0.0012 0.1430 11.00000 0.05 0.42 Q54 1 0.2297 0.0323 -0.0315 11.00000 0.05 0.41 Q55 1 0.3060 0.0377 -0.0535 11.00000 0.05 0.41 Q56 1 0.1528 -0.0273 0.1406 11.00000 0.05 0.41 Q57 1 0.2747 0.2268 -0.0114 11.00000 0.05 0.41 Q58 1 0.0622 0.4247 0.0536 11.00000 0.05 0.41 Q59 1 -0.3934 -0.1270 0.1912 11.00000 0.05 0.40 Q60 1 0.5370 -0.1258 -0.1113 11.00000 0.05 0.40 Q61 1 0.1276 -0.0442 -0.0076 11.00000 0.05 0.40 Q62 1 -0.2361 0.1362 0.1669 11.00000 0.05 0.40 Q63 1 0.1646 0.4029 0.1682 11.00000 0.05 0.40 Q64 1 -0.4821 0.0875 0.4809 11.00000 0.05 0.40 Q65 1 0.5000 0.3184 0.0000 10.50000 0.05 0.40 Q66 1 -0.0198 -0.0113 0.1785 11.00000 0.05 0.39 Q67 1 -0.2135 0.0303 0.2460 11.00000 0.05 0.39 Q68 1 0.5961 0.2698 0.0887 11.00000 0.05 0.39 Q69 1 0.4363 -0.4876 0.1308 11.00000 0.05 0.39 Q70 1 0.3828 0.3747 0.1409 11.00000 0.05 0.39 Q71 1 -0.1243 -0.0865 0.1516 11.00000 0.05 0.39 Q72 1 0.4409 0.2821 0.1294 11.00000 0.05 0.39 Q73 1 -0.0455 -0.0796 0.2072 11.00000 0.05 0.38 Q74 1 0.0828 0.1653 -0.0517 11.00000 0.05 0.38 Q75 1 -0.3021 0.0912 0.3114 11.00000 0.05 0.38 Q76 1 0.0046 0.1655 0.0399 11.00000 0.05 0.38 Q77 1 0.3566 -0.0966 0.0695 11.00000 0.05 0.38 Q78 1 -0.2151 -0.0710 0.2126 11.00000 0.05 0.37 Q79 1 -0.3482 0.1890 0.3318 11.00000 0.05 0.37 Q80 1 0.3903 -0.0793 -0.1013 11.00000 0.05 0.37 Q81 1 -0.0712 0.0028 0.2326 11.00000 0.05 0.37 Q82 1 0.0416 -0.3888 0.1775 11.00000 0.05 0.37 Q83 1 0.3616 -0.0137 -0.0872 11.00000 0.05 0.36 Q84 1 -0.4892 0.0971 0.3124 11.00000 0.05 0.36 Q85 1 -0.1727 0.1805 0.3774 11.00000 0.05 0.36 Q86 1 0.1971 -0.0163 0.1097 11.00000 0.05 0.36 Q87 1 0.2416 0.3404 0.2109 11.00000 0.05 0.36 Q88 1 0.3188 -0.0569 -0.0524 11.00000 0.05 0.36 Q89 1 0.4066 -0.1862 0.0071 11.00000 0.05 0.36 Q90 1 -0.1662 -0.0881 0.2038 11.00000 0.05 0.36 Q91 1 0.4033 -0.2771 0.2218 11.00000 0.05 0.36 Q92 1 -0.2548 -0.0519 0.3192 11.00000 0.05 0.35 Q93 1 0.0773 0.0612 0.2899 11.00000 0.05 0.35 Q94 1 0.1467 0.1581 -0.0229 11.00000 0.05 0.35 Q95 1 0.2826 -0.1000 -0.0484 11.00000 0.05 0.35 Q96 1 -0.2103 0.0828 0.4700 11.00000 0.05 0.35 Q97 1 0.3431 0.1587 -0.0811 11.00000 0.05 0.35 Q98 1 0.1742 0.1968 0.0707 11.00000 0.05 0.35 Q99 1 -0.4931 0.0324 0.4120 11.00000 0.05 0.34 Q100 1 -0.1461 -0.0226 0.4334 11.00000 0.05 0.34 REM The information below was added by Olex2. REM REM R1 = 0.1340 for 3954 Fo > 4sig(Fo) and 0.1774 for all 22852 data REM n/a parameters refined using n/a restraints REM Highest difference peak 3.30, deepest hole -1.51 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1774 REM R1_gt = 0.1340 REM wR_ref = 0.3844 REM GOOF = 1.399 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 22852 REM Reflections_gt = 3954 REM Parameters = n/a REM Hole = -1.51 REM Peak = 3.30 REM Flack = n/a ; _cod_data_source_file d1ob00888a2.cif _cod_data_source_block g129_5br2_3 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'MULTI-SCAN' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_original_formula_sum 'C32 H26 Br N O4.50' _cod_database_code 7158108 _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. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.92(4) 0.08(4) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 3. Uiso/Uaniso restraints and constraints : with sigma of 0.001 and sigma for terminal atoms of 0.002 : with sigma of 0.001 and sigma for terminal atoms of 0.002 Uanis(O10) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 Uanis(C19) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 : with sigma of 0.001 and sigma for terminal atoms of 0.002 Uanis(O6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 4. Others Fixed Sof: O6(0.75) O10(0.75) Fixed Uiso: C17(0.05) C20(0.05) C31(0.05) C6(0.05) 5.a Riding coordinates: N00P(H00P) 5.b Secondary CH2 refined with riding coordinates: C013(H01A,H01B) 5.c Aromatic/amide H refined with riding coordinates: C00O(H00O), C00Q(H00Q), C011(H011), C019(H019), C01B(H01C), C01E(H01E), C01J(H01J), C01M(H01M), C01N(H01N), C01P(H01P), C01R(H01R) 5.d Idealised Me refined as rotating group: C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C6(H6A,H6B,H6C), C3(H3A,H3B,H3C) ; _shelx_fab_file ; -1 0 1 12.86 0.02 -2 0 2 -19.79 -0.25 -3 0 3 -15.26 -0.07 -4 0 4 -0.04 -0.08 -5 0 5 5.00 0.10 -6 0 6 2.07 0.14 -7 0 7 -0.63 0.04 -8 0 8 -1.48 -0.14 -8 1 7 0.26 1.38 -7 1 6 -0.56 -0.37 -6 1 5 0.81 -0.80 -5 1 4 1.69 1.55 -4 1 3 3.43 4.00 -3 1 2 4.17 1.75 -2 1 1 -9.19 -17.21 1 1 0 -19.39 -11.85 -1 1 2 12.85 14.12 -2 1 3 6.81 1.75 -3 1 4 0.80 -8.88 -4 1 5 -2.16 -3.44 -5 1 6 -3.06 2.85 -6 1 7 -1.12 3.65 -7 1 8 -0.16 1.90 -8 1 9 0.03 -1.93 -8 2 6 -2.40 0.32 -7 2 5 -3.65 -1.56 -6 2 4 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-1.44 1.62 9 4 1 -1.03 0.62 -8 9 1 0.07 0.98 8 9 1 -1.30 1.73 -7 12 1 -0.88 -0.81 7 12 1 0.20 0.52 -6 15 1 -0.76 0.08 6 15 1 0.03 1.10 -5 16 1 -1.09 -0.01 5 16 1 0.72 -0.55 -3 18 1 0.36 0.89 3 18 1 -0.02 1.64 -2 19 1 0.07 -1.20 2 19 1 -0.02 -0.22 0 0 2 17.81 0.20 -9 1 2 0.47 0.08 9 1 2 0.76 -1.08 0 2 2 11.29 -45.71 -9 3 2 3.31 0.66 9 3 2 1.48 0.34 -9 5 2 -0.99 -1.25 9 5 2 -0.34 -0.72 -8 10 2 1.01 0.45 8 10 2 0.52 -0.07 -7 13 2 0.46 0.09 7 13 2 -0.07 0.91 -1 19 2 0.18 1.44 1 19 2 -0.02 1.91 -9 0 3 0.58 -0.02 9 0 3 -1.66 0.02 0 1 3 -24.93 17.91 -9 2 3 -2.56 -1.11 9 2 3 -0.26 -0.20 -9 4 3 -1.14 0.99 9 4 3 -0.42 0.24 -8 9 3 -0.79 0.99 8 9 3 -0.16 0.96 -7 12 3 -0.68 1.09 7 12 3 -0.02 -0.69 -6 15 3 -0.94 0.53 6 15 3 -0.69 1.00 -5 16 3 0.85 -0.11 5 16 3 -0.08 0.16 4 17 3 -0.68 1.40 -3 18 3 0.24 0.81 3 18 3 0.77 1.24 -2 19 3 -0.62 -0.80 0 19 3 0.59 0.25 2 19 3 0.64 -0.62 0 0 4 50.26 0.15 -9 1 4 0.83 2.58 9 1 4 0.76 0.18 -9 3 4 1.60 -1.13 9 3 4 -0.39 -0.09 -9 5 4 0.91 -0.53 -8 10 4 0.27 -1.80 -7 13 4 0.18 -0.80 6 14 4 0.83 -1.48 -1 19 4 -0.41 -0.31 1 19 4 0.13 -0.27 -9 0 5 0.03 -0.19 9 0 5 -0.21 0.11 -9 2 5 -1.43 -0.77 9 2 5 0.17 0.54 -9 4 5 -1.56 0.99 9 4 5 -0.36 -0.35 -8 9 5 -0.14 0.83 8 9 5 -1.40 1.15 -7 12 5 -1.41 -0.57 7 12 5 0.57 0.33 -6 15 5 -0.81 -0.80 -5 16 5 -0.76 0.18 5 16 5 0.82 -0.07 -4 17 5 1.04 1.87 4 17 5 -1.03 0.40 -3 18 5 0.20 -0.28 3 18 5 0.17 0.73 -2 19 5 0.40 -0.51 0 19 5 1.15 0.38 2 19 5 0.59 0.98 -9 1 6 0.60 -0.28 9 1 6 -0.22 -0.57 -9 3 6 2.20 0.90 9 3 6 -0.06 0.20 8 8 6 0.98 -0.01 -6 14 6 0.23 1.76 6 14 6 0.36 -0.23 -1 19 6 -0.92 1.17 1 19 6 -0.50 0.71 -9 0 7 -0.95 -0.15 9 0 7 0.20 0.03 -9 2 7 -1.37 -0.95 9 2 7 0.17 -0.22 -9 4 7 -0.17 -0.17 -8 9 7 -0.26 0.91 8 9 7 0.18 -0.45 -7 12 7 -0.62 2.04 7 12 7 0.55 -0.24 -5 16 7 1.80 0.85 5 16 7 0.61 0.25 -4 17 7 0.75 0.33 4 17 7 -0.70 1.62 -3 18 7 0.36 0.32 3 18 7 1.60 0.34 0 19 7 0.32 -0.43 -9 1 8 0.96 1.17 -9 3 8 -0.01 -0.53 -8 8 8 0.22 -0.93 8 8 8 -0.65 1.28 7 11 8 -0.32 0.91 -6 14 8 1.16 0.71 6 14 8 -0.26 -1.02 5 15 8 -1.69 0.52 2 18 8 -0.60 -0.28 -1 19 8 -0.98 -0.10 1 19 8 -0.18 -1.11 -9 0 9 -0.16 -0.10 -9 2 9 -0.19 1.01 8 7 9 1.25 -0.17 -8 9 9 -0.28 0.91 -7 12 9 -0.91 -0.07 6 13 9 0.48 0.87 -5 16 9 0.26 0.67 -4 17 9 1.78 1.83 -3 18 9 -0.27 -0.22 0 19 9 0.09 0.38 -9 1 10 0.55 -1.47 8 6 10 -0.43 -0.57 -8 8 10 1.49 -0.43 -7 11 10 1.83 -0.59 7 11 10 -0.66 -1.31 -6 14 10 -0.83 0.37 -5 15 10 -0.06 -1.58 5 15 10 0.61 -1.15 4 16 10 -0.12 -1.08 3 17 10 -1.26 1.06 -2 18 10 -1.17 -0.54 2 18 10 -0.47 -0.88 -9 0 11 -2.32 -0.05 -8 7 11 -1.66 0.14 8 7 11 -0.27 0.33 7 10 11 -0.79 0.70 6 13 11 1.72 0.65 -1 18 11 1.27 -0.40 1 18 11 1.34 0.84 8 6 12 0.70 0.95 -8 8 12 -0.68 -1.19 -7 11 12 0.82 -0.02 -5 15 12 -0.22 -2.22 -4 16 12 0.21 -1.07 4 16 12 1.93 0.10 -3 17 12 0.12 0.75 3 17 12 -0.90 -0.01 -2 18 12 -0.12 -0.62 0 18 12 -0.18 0.85 8 3 13 0.50 1.06 8 5 13 -0.51 -0.90 -8 7 13 -0.19 1.21 -7 10 13 -0.61 -0.66 7 10 13 0.37 0.80 -6 13 13 -1.22 -0.08 5 14 13 0.42 -0.71 2 17 13 0.34 0.08 -1 18 13 -0.58 -1.13 1 18 13 0.67 0.08 8 0 14 0.50 0.09 8 2 14 1.70 -1.09 8 4 14 -0.87 0.82 -8 6 14 1.86 -0.94 7 9 14 0.35 -0.02 6 12 14 -0.66 -0.50 -4 16 14 0.47 -0.25 -3 17 14 0.49 1.47 0 18 14 0.86 0.04 8 1 15 -1.27 0.11 8 3 15 -0.44 0.13 -8 5 15 -1.09 -0.31 7 8 15 0.04 0.78 -7 10 15 1.59 -1.13 6 11 15 -0.53 0.45 -5 14 15 -0.57 -0.35 -4 15 15 0.86 -1.11 4 15 15 -0.58 0.35 -3 16 15 1.02 -1.99 3 16 15 -0.18 -1.59 -2 17 15 -1.63 1.41 0 17 15 -1.30 0.25 2 17 15 -0.59 0.15 8 0 16 1.67 0.08 8 2 16 0.11 0.20 -8 4 16 0.97 0.09 7 7 16 0.86 -0.21 -7 9 16 -1.72 0.87 -6 12 16 -0.77 -0.80 5 13 16 -0.01 1.15 2 16 16 1.08 -0.65 -1 17 16 -0.39 -0.25 1 17 16 0.19 -0.63 -8 1 17 -1.32 -1.14 -8 3 17 0.09 -0.06 -8 5 17 -0.61 -0.31 7 6 17 -0.78 1.22 -7 8 17 0.66 -0.69 -6 11 17 0.18 1.83 6 11 17 0.51 0.51 -4 15 17 -0.03 -0.05 -3 16 17 1.65 0.27 0 17 17 -0.94 0.34 -8 0 18 0.19 0.01 -8 2 18 1.06 -0.16 7 5 18 1.26 0.85 7 7 18 0.29 -0.82 6 10 18 0.81 -0.87 -5 13 18 1.09 -1.01 -4 14 18 -0.91 -1.26 4 14 18 0.81 1.68 -3 15 18 1.01 -0.73 3 15 18 0.95 0.70 -2 16 18 1.16 -1.86 0 16 18 0.75 -0.44 2 16 18 -0.12 -1.07 -8 1 19 -0.03 0.83 7 4 19 -0.63 -0.48 7 6 19 -0.84 -0.42 -7 8 19 -0.45 -1.87 6 9 19 -0.91 0.25 -6 11 19 -1.40 0.52 -5 12 19 -1.28 -0.81 5 12 19 -1.10 0.94 4 13 19 1.93 -1.01 3 14 19 -0.80 -1.81 2 15 19 -0.75 1.15 -1 16 19 0.92 -1.50 1 16 19 0.55 0.16 7 1 20 0.00 -1.97 7 3 20 -0.61 1.17 -7 7 20 0.02 2.22 6 8 20 1.91 0.59 -6 10 20 2.10 1.14 5 11 20 1.54 0.42 1 15 20 -0.95 0.20 0 16 20 1.84 1.58 7 0 21 -0.93 -0.07 7 2 21 1.06 0.18 -7 4 21 -0.80 0.26 -7 6 21 1.47 -1.07 6 7 21 0.52 -1.50 -6 9 21 -0.05 -2.53 5 10 21 -1.49 -0.63 -5 12 21 -1.89 0.38 -4 13 21 0.27 -0.26 -3 14 21 -1.60 -3.35 3 14 21 0.25 -0.67 -2 15 21 -1.64 -0.54 0 15 21 -0.88 -0.81 -7 1 22 -0.23 0.70 -7 3 22 0.07 -0.03 -7 5 22 0.22 1.11 6 6 22 -0.39 0.48 -6 8 22 -0.33 1.05 5 9 22 1.33 0.92 -5 11 22 -0.43 0.53 -4 12 22 -0.17 0.87 4 12 22 0.40 -1.47 -3 13 22 -0.89 1.92 3 13 22 -1.52 0.47 -2 14 22 -0.41 0.72 2 14 22 1.00 0.88 -1 15 22 0.41 -0.20 -7 0 23 0.63 0.23 -7 2 23 -0.79 -0.46 6 3 23 1.09 0.14 6 5 23 0.74 0.78 -6 7 23 0.68 0.37 5 8 23 -1.09 -0.77 -5 10 23 0.81 0.42 4 11 23 -1.27 0.27 3 12 23 0.54 0.89 2 13 23 0.35 -0.53 -1 14 23 0.53 1.18 1 14 23 -0.25 1.30 6 0 24 3.43 -0.42 6 2 24 -1.76 -1.14 6 4 24 -0.02 -0.38 -6 6 24 -0.43 0.93 5 7 24 0.40 2.46 -5 9 24 2.16 -1.42 4 10 24 1.32 1.05 -1 13 24 0.92 -0.22 1 13 24 2.20 -1.53 0 14 24 -1.23 0.13 6 1 25 -0.35 2.73 -6 5 25 1.76 1.09 5 6 25 1.22 -1.14 -5 8 25 -2.72 -0.20 4 9 25 0.18 -0.73 -4 11 25 -2.21 0.32 -3 12 25 -2.18 0.70 -2 13 25 1.43 1.77 0 13 25 2.97 -0.16 -6 0 26 0.95 -0.08 -6 2 26 0.18 0.24 -6 4 26 -0.93 -2.01 5 5 26 -1.23 0.05 -5 7 26 1.98 2.67 4 8 26 -0.71 0.76 -4 10 26 3.77 1.42 -3 11 26 1.48 1.02 -2 12 26 -0.47 -1.59 0 12 26 -2.62 -1.81 5 0 27 1.27 0.09 -6 1 27 -0.28 -1.21 5 2 27 0.34 0.85 5 4 27 0.33 0.04 -5 6 27 -1.58 -1.16 4 7 27 -0.36 -0.22 -4 9 27 -0.94 -1.98 -3 10 27 -0.74 -1.38 -2 11 27 0.34 2.61 0 11 27 0.99 2.96 2 11 27 -0.69 1.72 -1 12 27 2.33 -1.39 5 1 28 -0.92 -2.22 -5 3 28 -0.64 0.49 -5 5 28 1.16 2.00 4 6 28 -0.75 1.41 -4 8 28 -0.60 1.78 -3 9 28 2.15 0.24 -2 10 28 0.64 -2.59 2 10 28 1.41 -0.31 -1 11 28 -2.95 0.19 1 11 28 -1.21 -2.21 -5 0 29 -1.07 -0.85 4 1 29 0.92 -0.19 -5 2 29 -0.21 0.05 4 3 29 -0.39 1.03 -4 5 29 -1.38 -0.86 4 5 29 1.29 -0.53 3 6 29 0.06 1.43 -4 7 29 -0.27 0.23 -3 8 29 -1.51 -1.98 -2 9 29 -1.91 0.54 2 9 29 -2.32 0.17 -1 10 29 2.82 2.17 1 10 29 1.13 3.20 4 0 30 -2.71 0.03 4 2 30 1.54 -1.14 -4 4 30 0.26 1.30 3 5 30 0.65 0.25 -3 7 30 1.14 3.11 -2 8 30 0.84 -0.74 0 8 30 0.55 0.35 2 8 30 0.67 2.10 -1 9 30 -1.78 -2.73 1 9 30 0.40 -2.26 3 0 31 0.23 -0.15 -4 1 31 2.55 1.39 3 2 31 -0.22 0.59 -4 3 31 0.07 -1.66 -3 4 31 -0.25 -0.12 3 4 31 0.17 0.19 2 5 31 0.09 0.78 -3 6 31 0.79 -1.82 1 6 31 1.39 0.81 -2 7 31 -1.04 -0.45 0 7 31 -1.17 -0.86 -1 8 31 -0.77 3.03 2 0 32 3.61 -0.19 -3 1 32 -0.91 2.72 2 2 32 -1.42 0.78 -3 3 32 -0.17 1.00 -2 4 32 0.29 -0.19 2 4 32 1.18 -0.66 -1 5 32 -0.79 -0.87 1 5 32 -1.02 -2.17 -2 6 32 0.71 0.52 0 6 32 0.33 1.03 -1 0 33 2.25 -0.04 1 0 33 1.10 -0.06 -2 1 33 -0.99 -1.83 0 1 33 -0.65 -1.91 2 1 33 -0.91 0.69 -1 2 33 -0.67 1.44 1 2 33 -1.05 0.49 -2 3 33 1.20 0.66 0 3 33 0.72 0.52 -1 4 33 0.61 -0.48 1 4 33 -0.18 1.03 0 5 33 -0.52 -1.24 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 190619) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material ; _platon_squeeze_void_probe_radius 1.20 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-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 Br02 Br -0.2875(3) 0.03653(16) 0.39331(8) 0.0600(8) Uani 1 1 d . . . . . O004 O -0.0068(14) -0.1684(8) 0.1656(4) 0.033(3) Uani 1 1 d . . . . . O006 O 0.164(2) -0.0033(8) 0.1149(5) 0.049(3) Uani 1 1 d . . . . . O007 O -0.2309(15) -0.1135(9) 0.2083(5) 0.043(3) Uani 1 1 d . . . . . O6 O 0.176(4) 0.1954(17) 0.1288(10) 0.072(6) Uani 0.75 1 d . U P A 1 O10 O 0.024(7) 0.281(3) 0.1828(18) 0.144(14) Uani 0.75 1 d . U P A 1 N00P N 0.029(3) 0.1283(11) 0.1883(8) 0.059(5) Uani 1 1 d . . . . . H00P H 0.089907 0.084359 0.174762 0.070 Uiso 1 1 d R . . . . C009 C 0.2356(19) -0.2130(9) 0.0647(6) 0.024(3) Uani 1 1 d . . . . . C00A C 0.223(2) -0.2371(10) 0.1172(6) 0.029(3) Uani 1 1 d . . . . . C00D C 0.220(2) -0.1231(10) 0.0560(6) 0.029(3) Uani 1 1 d . . . . . C00E C 0.188(2) -0.0799(10) 0.1067(6) 0.029(3) Uani 1 1 d . . . . . C00J C 0.277(2) -0.1482(12) -0.0330(6) 0.034(4) Uani 1 1 d . . . . . C00L C -0.066(2) -0.1081(11) 0.1989(6) 0.031(3) Uani 1 1 d . . . . . C00N C -0.188(2) 0.0668(14) 0.3294(7) 0.046(5) Uani 1 1 d . . . . . C00O C 0.278(2) -0.3663(12) 0.0385(8) 0.042(4) Uani 1 1 d . . . . . H00O H 0.293240 -0.410304 0.013235 0.050 Uiso 1 1 calc R . . . . C00Q C 0.272(3) -0.3890(12) 0.0919(7) 0.040(4) Uani 1 1 d . . . . . H00Q H 0.289744 -0.449222 0.101203 0.048 Uiso 1 1 calc R . . . . C00S C 0.2607(19) -0.2754(10) 0.0252(6) 0.027(3) Uani 1 1 d . . . . . C00V C 0.068(2) -0.0509(13) 0.2260(6) 0.042(4) Uani 1 1 d . . . . . C010 C 0.187(2) -0.1563(11) 0.1471(6) 0.029(3) Uani 1 1 d . . . . . C011 C 0.241(2) -0.3266(11) 0.1317(6) 0.033(3) Uani 1 1 d . . . . . H011 H 0.233105 -0.344653 0.166274 0.039 Uiso 1 1 calc R . . . . C013 C 0.3204(19) -0.1385(11) 0.1926(6) 0.029(3) Uani 1 1 d . . . . . H01A H 0.336818 -0.193158 0.213059 0.035 Uiso 1 1 calc R . . . . H01B H 0.443626 -0.121449 0.180299 0.035 Uiso 1 1 calc R . . . . C016 C 0.242(2) -0.0875(11) 0.0082(7) 0.031(3) Uani 1 1 d . . . . . C019 C -0.092(2) 0.0004(13) 0.3034(7) 0.041(4) Uani 1 1 d . . . . . H019 H -0.078676 -0.057463 0.317186 0.049 Uiso 1 1 calc R . . . . C17 C 0.219(3) 0.3470(14) 0.1046(8) 0.050 Uiso 1 1 d . . . . . H17A H 0.111147 0.338332 0.080775 0.075 Uiso 1 1 calc GR . . . . H17B H 0.301489 0.391901 0.091000 0.075 Uiso 1 1 calc GR . . . . H17C H 0.176062 0.366635 0.137712 0.075 Uiso 1 1 calc GR . . . . C01B C 0.237(2) 0.0046(12) -0.0024(7) 0.041(4) Uani 1 1 d . . . . . H01C H 0.215043 0.045547 0.024123 0.050 Uiso 1 1 calc R . . . . C01D C -0.0177(19) 0.0226(12) 0.2567(6) 0.037(4) Uani 1 1 d . . . . . C19 C 0.048(6) 0.214(3) 0.1647(14) 0.098(10) Uani 1 1 d . U . . . C01E C 0.281(2) -0.2425(12) -0.0227(7) 0.037(4) Uani 1 1 d . . . . . H01E H 0.297324 -0.282344 -0.050099 0.044 Uiso 1 1 calc R . . . . C20 C 0.367(3) 0.2331(15) 0.0598(8) 0.050 Uiso 1 1 d . U . . . H20A H 0.463916 0.271232 0.046543 0.075 Uiso 1 1 calc GR . . . . H20B H 0.255323 0.235641 0.036811 0.075 Uiso 1 1 calc GR . . . . H20C H 0.412615 0.172130 0.061933 0.075 Uiso 1 1 calc GR . . . . C01F C 0.251(2) -0.0669(10) 0.2254(6) 0.031(3) Uani 1 1 d . . . . . C01J C 0.299(2) -0.0223(13) -0.0892(7) 0.043(4) Uani 1 1 d . . . . . H01J H 0.320380 0.002015 -0.121793 0.052 Uiso 1 1 calc R . . . . C01M C -0.206(3) 0.1528(13) 0.3097(8) 0.046(5) Uani 1 1 d . . . . . H01M H -0.269739 0.197152 0.327792 0.055 Uiso 1 1 calc R . . . . C01N C 0.306(2) -0.1164(14) -0.0832(8) 0.046(5) Uani 1 1 d . . . . . H01N H 0.329367 -0.154975 -0.110794 0.055 Uiso 1 1 calc R . . . . C01P C -0.132(3) 0.1712(14) 0.2647(8) 0.047(5) Uani 1 1 d . . . . . H01P H -0.142752 0.229711 0.251753 0.056 Uiso 1 1 calc R . . . . C01R C 0.262(2) 0.0342(17) -0.0502(8) 0.054(5) Uani 1 1 d . . . . . H01R H 0.254731 0.095795 -0.056893 0.064 Uiso 1 1 calc R . . . . C01X C -0.043(3) 0.1105(13) 0.2371(9) 0.051(5) Uani 1 1 d . . . . . C31 C 0.320(3) 0.2638(15) 0.1112(8) 0.050 Uiso 1 1 d . U . . . C6 C 0.520(3) 0.2516(14) 0.1501(8) 0.050 Uiso 1 1 d . U . . . H6A H 0.522991 0.297346 0.176607 0.075 Uiso 1 1 calc GR . . . . H6B H 0.629827 0.257268 0.129646 0.075 Uiso 1 1 calc GR . . . . H6C H 0.519600 0.193114 0.166245 0.075 Uiso 1 1 calc GR . . . . C3 C 0.399(3) -0.0163(16) 0.2573(10) 0.059(6) Uani 1 1 d . . . . . H3A H 0.471318 0.020763 0.234808 0.089 Uiso 1 1 calc GR . . . . H3B H 0.482431 -0.058336 0.275373 0.089 Uiso 1 1 calc GR . . . . H3C H 0.338515 0.021099 0.282143 0.089 Uiso 1 1 calc GR . . . . 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 Br02 0.0510(11) 0.0769(15) 0.0536(11) -0.0284(11) 0.0162(8) 0.0000(11) O004 0.022(5) 0.037(6) 0.039(6) -0.020(5) 0.006(4) 0.007(5) O006 0.069(9) 0.027(6) 0.051(8) -0.015(5) 0.006(7) 0.001(6) O007 0.021(5) 0.050(8) 0.058(8) -0.021(6) 0.012(5) -0.005(5) O6 0.072(6) 0.071(6) 0.072(6) -0.0006(15) 0.0044(15) -0.0007(15) O10 0.145(14) 0.143(14) 0.144(14) -0.001(3) 0.008(3) 0.000(3) N00P 0.069(11) 0.028(8) 0.081(13) -0.027(8) 0.037(10) -0.007(8) C009 0.016(6) 0.022(7) 0.034(8) -0.014(6) -0.006(5) -0.001(5) C00A 0.036(8) 0.020(7) 0.031(8) -0.005(6) 0.005(6) -0.006(6) C00D 0.029(7) 0.023(8) 0.034(8) -0.004(6) 0.007(6) -0.004(6) C00E 0.037(8) 0.018(7) 0.033(8) -0.009(6) 0.007(7) 0.009(6) C00J 0.028(8) 0.037(9) 0.037(8) -0.001(7) 0.001(7) 0.007(7) C00L 0.023(7) 0.033(9) 0.039(9) -0.012(7) 0.010(6) 0.003(6) C00N 0.018(7) 0.071(14) 0.049(10) -0.037(9) 0.012(7) -0.002(7) C00O 0.029(8) 0.025(8) 0.071(12) -0.015(8) 0.000(8) 0.008(6) C00Q 0.058(11) 0.028(9) 0.033(8) -0.003(7) 0.000(8) -0.009(8) C00S 0.018(6) 0.026(8) 0.037(8) -0.009(6) 0.001(6) -0.006(6) C00V 0.038(9) 0.057(12) 0.031(8) -0.031(8) 0.008(7) -0.001(8) C010 0.023(7) 0.033(9) 0.030(7) -0.003(6) -0.006(6) 0.004(6) C011 0.035(8) 0.029(8) 0.035(8) -0.011(6) 0.010(7) 0.003(7) C013 0.015(6) 0.038(9) 0.034(8) -0.009(7) 0.004(6) 0.006(6) C016 0.017(6) 0.032(8) 0.045(9) -0.013(7) -0.007(6) -0.002(6) C019 0.039(9) 0.043(10) 0.041(9) -0.014(7) -0.002(8) 0.006(7) C01B 0.045(9) 0.042(10) 0.037(9) 0.000(7) -0.004(8) -0.001(8) C01D 0.023(6) 0.043(11) 0.045(9) -0.027(8) 0.008(6) 0.000(7) C19 0.098(10) 0.098(10) 0.098(10) -0.0003(15) 0.0050(15) -0.0001(15) C01E 0.042(9) 0.038(10) 0.031(8) -0.006(7) 0.003(7) 0.003(7) C01F 0.030(8) 0.026(8) 0.037(8) -0.012(6) 0.006(7) -0.007(6) C01J 0.041(10) 0.057(12) 0.032(9) 0.003(8) -0.010(8) -0.009(9) C01M 0.040(9) 0.041(11) 0.057(11) -0.019(9) 0.009(8) -0.008(8) C01N 0.022(8) 0.057(12) 0.057(11) 0.010(9) -0.017(8) 0.007(8) C01P 0.042(9) 0.043(11) 0.057(11) -0.019(9) 0.020(8) 0.000(8) C01R 0.041(9) 0.056(12) 0.061(11) 0.035(12) -0.014(8) 0.005(11) C01X 0.047(10) 0.039(11) 0.069(13) -0.029(10) 0.030(10) -0.019(9) C3 0.052(11) 0.053(13) 0.072(14) -0.018(11) -0.015(11) 0.003(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C00L O004 C010 116.9(12) . . ? C19 O6 C31 123(3) . . ? C19 N00P H00P 116.5 . . ? C01X N00P H00P 115.2 . . ? C01X N00P C19 127(2) . . ? C00D C009 C00A 113.6(13) . . ? C00D C009 C00S 123.1(15) . . ? C00S C009 C00A 123.3(14) . . ? C009 C00A C010 108.6(13) . . ? C011 C00A C009 119.6(14) . . ? C011 C00A C010 131.7(15) . . ? C009 C00D C00E 107.2(14) . . ? C016 C00D C009 121.5(15) . . ? C016 C00D C00E 131.2(14) . . ? O006 C00E C00D 127.6(16) . . ? O006 C00E C010 126.1(15) . . ? C00D C00E C010 106.3(12) . . ? C016 C00J C01E 119.1(15) . . ? C01N C00J C016 120.9(17) . . ? C01N C00J C01E 120.0(16) . . ? O004 C00L C00V 120.0(13) . . ? O007 C00L O004 115.1(14) . . ? O007 C00L C00V 124.3(14) . . ? C019 C00N Br02 117.6(17) . . ? C01M C00N Br02 120.8(12) . . ? C01M C00N C019 121.5(18) . . ? C00Q C00O H00O 121.2 . . ? C00S C00O H00O 121.2 . . ? C00S C00O C00Q 117.5(16) . . ? C00O C00Q H00Q 117.9 . . ? C011 C00Q C00O 124.2(17) . . ? C011 C00Q H00Q 117.9 . . ? C009 C00S C00O 118.5(16) . . ? C01E C00S C009 116.8(15) . . ? C01E C00S C00O 124.5(16) . . ? C00L C00V C01D 114.9(14) . . ? C01F C00V C00L 120.8(14) . . ? C01F C00V C01D 124.2(14) . . ? O004 C010 C00E 110.1(12) . . ? O004 C010 C013 109.0(12) . . ? C00A C010 O004 104.9(12) . . ? C00A C010 C00E 104.1(13) . . ? C00A C010 C013 116.2(13) . . ? C013 C010 C00E 112.1(13) . . ? C00A C011 C00Q 116.8(15) . . ? C00A C011 H011 121.6 . . ? C00Q C011 H011 121.6 . . ? C010 C013 H01A 109.3 . . ? C010 C013 H01B 109.3 . . ? H01A C013 H01B 108.0 . . ? C01F C013 C010 111.4(12) . . ? C01F C013 H01A 109.3 . . ? C01F C013 H01B 109.3 . . ? C00D C016 C00J 117.4(15) . . ? C00D C016 C01B 124.0(15) . . ? C01B C016 C00J 118.6(17) . . ? C00N C019 H019 121.1 . . ? C01D C019 C00N 117.8(19) . . ? C01D C019 H019 121.1 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C31 C17 H17A 109.5 . . ? C31 C17 H17B 109.5 . . ? C31 C17 H17C 109.5 . . ? C016 C01B H01C 119.9 . . ? C01R C01B C016 120.2(19) . . ? C01R C01B H01C 119.9 . . ? C019 C01D C00V 118.0(17) . . ? C019 C01D C01X 119.3(15) . . ? C01X C01D C00V 122.3(16) . . ? O6 C19 N00P 101(3) . . ? O10 C19 O6 126(4) . . ? O10 C19 N00P 127(4) . . ? C00J C01E H01E 119.1 . . ? C00S C01E C00J 121.8(15) . . ? C00S C01E H01E 119.1 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C31 C20 H20A 109.5 . . ? C31 C20 H20B 109.5 . . ? C31 C20 H20C 109.5 . . ? C00V C01F C013 120.0(13) . . ? C00V C01F C3 124.2(15) . . ? C013 C01F C3 115.8(14) . . ? C01N C01J H01J 118.4 . . ? C01R C01J H01J 118.4 . . ? C01R C01J C01N 123.1(19) . . ? C00N C01M H01M 120.7 . . ? C01P C01M C00N 118.6(18) . . ? C01P C01M H01M 120.7 . . ? C00J C01N C01J 115.4(19) . . ? C00J C01N H01N 122.3 . . ? C01J C01N H01N 122.3 . . ? C01M C01P H01P 118.4 . . ? C01M C01P C01X 123(2) . . ? C01X C01P H01P 118.4 . . ? C01B C01R C01J 122(2) . . ? C01B C01R H01R 119.1 . . ? C01J C01R H01R 119.1 . . ? N00P C01X C01D 117.0(15) . . ? C01P C01X N00P 124(2) . . ? C01P C01X C01D 119.5(19) . . ? O6 C31 C6 107.3(17) . . ? C17 C31 O6 105.9(18) . . ? C17 C31 C20 107.3(18) . . ? C17 C31 C6 123.8(18) . . ? C20 C31 O6 104.2(18) . . ? C20 C31 C6 106.7(17) . . ? C31 C6 H6A 109.5 . . ? C31 C6 H6B 109.5 . . ? C31 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C01F C3 H3A 109.5 . . ? C01F C3 H3B 109.5 . . ? C01F C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? 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 Br02 C00N 1.91(2) . ? O004 C00L 1.345(18) . ? O004 C010 1.504(19) . ? O006 C00E 1.193(19) . ? O007 C00L 1.225(19) . ? O6 C19 1.38(4) . ? O6 C31 1.55(3) . ? O10 C19 1.14(6) . ? N00P H00P 0.8807 . ? N00P C19 1.44(4) . ? N00P C01X 1.43(3) . ? C009 C00A 1.43(2) . ? C009 C00D 1.38(2) . ? C009 C00S 1.42(2) . ? C00A C010 1.48(2) . ? C00A C011 1.41(2) . ? C00D C00E 1.51(2) . ? C00D C016 1.38(2) . ? C00E C010 1.57(2) . ? C00J C016 1.45(2) . ? C00J C01E 1.45(3) . ? C00J C01N 1.43(3) . ? C00L C00V 1.45(2) . ? C00N C019 1.41(2) . ? C00N C01M 1.40(3) . ? C00O H00O 0.9500 . ? C00O C00Q 1.44(3) . ? C00O C00S 1.42(3) . ? C00Q H00Q 0.9500 . ? C00Q C011 1.43(2) . ? C00S C01E 1.37(2) . ? C00V C01D 1.52(2) . ? C00V C01F 1.34(2) . ? C010 C013 1.52(2) . ? C011 H011 0.9500 . ? C013 H01A 0.9900 . ? C013 H01B 0.9900 . ? C013 C01F 1.48(2) . ? C016 C01B 1.42(2) . ? C019 H019 0.9500 . ? C019 C01D 1.40(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C17 C31 1.46(3) . ? C01B H01C 0.9500 . ? C01B C01R 1.35(3) . ? C01D C01X 1.43(3) . ? C01E H01E 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C20 C31 1.48(3) . ? C01F C3 1.53(3) . ? C01J H01J 0.9500 . ? C01J C01N 1.43(3) . ? C01J C01R 1.37(3) . ? C01M H01M 0.9500 . ? C01M C01P 1.35(3) . ? C01N H01N 0.9500 . ? C01P H01P 0.9500 . ? C01P C01X 1.35(2) . ? C01R H01R 0.9500 . ? C31 C6 1.73(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Br02 C00N C019 C01D -179.5(11) . . . . ? Br02 C00N C01M C01P 179.3(14) . . . . ? O004 C00L C00V C01D 171.8(16) . . . . ? O004 C00L C00V C01F -12(3) . . . . ? O004 C010 C013 C01F -50.4(18) . . . . ? O006 C00E C010 O004 68(2) . . . . ? O006 C00E C010 C00A 180.0(17) . . . . ? O006 C00E C010 C013 -54(2) . . . . ? O007 C00L C00V C01D -17(3) . . . . ? O007 C00L C00V C01F 159.1(19) . . . . ? C009 C00A C010 O004 113.4(13) . . . . ? C009 C00A C010 C00E -2.4(15) . . . . ? C009 C00A C010 C013 -126.1(15) . . . . ? C009 C00A C011 C00Q 0(2) . . . . ? C009 C00D C00E O006 -178.4(17) . . . . ? C009 C00D C00E C010 0.3(17) . . . . ? C009 C00D C016 C00J 1(2) . . . . ? C009 C00D C016 C01B -176.9(15) . . . . ? C009 C00S C01E C00J 0(2) . . . . ? C00A C009 C00D C00E -1.9(18) . . . . ? C00A C009 C00D C016 175.8(14) . . . . ? C00A C009 C00S C00O -1(2) . . . . ? C00A C009 C00S C01E -176.6(14) . . . . ? C00A C010 C013 C01F -168.7(14) . . . . ? C00D C009 C00A C010 2.8(17) . . . . ? C00D C009 C00A C011 -178.3(15) . . . . ? C00D C009 C00S C00O 178.8(14) . . . . ? C00D C009 C00S C01E 4(2) . . . . ? C00D C00E C010 O004 -110.7(14) . . . . ? C00D C00E C010 C00A 1.3(16) . . . . ? C00D C00E C010 C013 127.7(13) . . . . ? C00D C016 C01B C01R 178.7(15) . . . . ? C00E C00D C016 C00J 178.3(15) . . . . ? C00E C00D C016 C01B 0(3) . . . . ? C00E C010 C013 C01F 71.7(17) . . . . ? C00J C016 C01B C01R 1(2) . . . . ? C00L O004 C010 C00A 172.6(13) . . . . ? C00L O004 C010 C00E -75.9(16) . . . . ? C00L O004 C010 C013 47.5(18) . . . . ? C00L C00V C01D C019 77(2) . . . . ? C00L C00V C01D C01X -96(2) . . . . ? C00L C00V C01F C013 6(3) . . . . ? C00L C00V C01F C3 -173.2(19) . . . . ? C00N C019 C01D C00V -173.7(14) . . . . ? C00N C019 C01D C01X -1(2) . . . . ? C00N C01M C01P C01X 1(3) . . . . ? C00O C00Q C011 C00A -3(3) . . . . ? C00O C00S C01E C00J -174.7(15) . . . . ? C00Q C00O C00S C009 -1(2) . . . . ? C00Q C00O C00S C01E 173.8(16) . . . . ? C00S C009 C00A C010 -176.9(13) . . . . ? C00S C009 C00A C011 2(2) . . . . ? C00S C009 C00D C00E 177.9(13) . . . . ? C00S C009 C00D C016 -4(2) . . . . ? C00S C00O C00Q C011 3(3) . . . . ? C00V C01D C01X N00P -4(3) . . . . ? C00V C01D C01X C01P 175.2(17) . . . . ? C010 O004 C00L O007 171.3(15) . . . . ? C010 O004 C00L C00V -17(2) . . . . ? C010 C00A C011 C00Q 178.6(16) . . . . ? C010 C013 C01F C00V 26(2) . . . . ? C010 C013 C01F C3 -154.6(17) . . . . ? C011 C00A C010 O004 -65(2) . . . . ? C011 C00A C010 C00E 178.9(17) . . . . ? C011 C00A C010 C013 55(2) . . . . ? C016 C00D C00E O006 4(3) . . . . ? C016 C00D C00E C010 -177.1(15) . . . . ? C016 C00J C01E C00S -3(2) . . . . ? C016 C00J C01N C01J 0(2) . . . . ? C016 C01B C01R C01J -2(3) . . . . ? C019 C00N C01M C01P 1(3) . . . . ? C019 C01D C01X N00P -177.3(17) . . . . ? C019 C01D C01X C01P 2(3) . . . . ? C01D C00V C01F C013 -177.9(17) . . . . ? C01D C00V C01F C3 3(3) . . . . ? C19 O6 C31 C17 -43(3) . . . . ? C19 O6 C31 C20 -156(3) . . . . ? C19 O6 C31 C6 91(3) . . . . ? C19 N00P C01X C01D -169(2) . . . . ? C19 N00P C01X C01P 11(4) . . . . ? C01E C00J C016 C00D 2(2) . . . . ? C01E C00J C016 C01B -179.4(15) . . . . ? C01E C00J C01N C01J 179.7(15) . . . . ? C01F C00V C01D C019 -99(2) . . . . ? C01F C00V C01D C01X 88(2) . . . . ? C01M C00N C019 C01D -1(2) . . . . ? C01M C01P C01X N00P 177(2) . . . . ? C01M C01P C01X C01D -3(3) . . . . ? C01N C00J C016 C00D -178.0(14) . . . . ? C01N C00J C016 C01B 0(2) . . . . ? C01N C00J C01E C00S 177.2(15) . . . . ? C01N C01J C01R C01B 2(3) . . . . ? C01R C01J C01N C00J -1(2) . . . . ? C01X N00P C19 O6 161(2) . . . . ? C01X N00P C19 O10 7(6) . . . . ? C31 O6 C19 O10 5(6) . . . . ? C31 O6 C19 N00P -148(2) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.052 0.400 0.000 89 22 ' ' 2 -0.057 0.900 0.500 89 22 ' ' 3 0.086 0.660 0.248 16 7 ' ' 4 0.413 0.160 0.252 16 7 ' ' 5 0.586 0.160 0.748 16 7 ' ' 6 0.913 0.660 0.752 16 7 ' ' loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.92(4) 2 0.08(4) loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta 0 2 0 2.692 0 1 1 1.554 0 0 2 1.556 0 2 2 3.110 0 1 3 2.695 0 0 4 3.113