#------------------------------------------------------------------------------ #$Date: 2021-06-03 00:16:17 +0300 (Thu, 03 Jun 2021) $ #$Revision: 265679 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/87/4518759.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_4518759 loop_ _publ_author_name 'Ma, Yun-Xiang' 'Gao, Bin' 'Li, Yongxin' 'Wei, Wei' 'Zhao, Yanli' 'Ma, Jian-Fang' _publ_section_title ; Macrocycle-Based Metal--Organic Frameworks with NO2-Driven On/Off Switch of Conductivity ; _journal_name_full 'ACS Applied Materials & Interfaces' _journal_paper_doi 10.1021/acsami.1c05481 _journal_year 2021 _chemical_formula_sum 'C81 H95 Co2 N3 O42' _chemical_formula_weight 1914.44 _space_group_crystal_system monoclinic _space_group_IT_number 11 _space_group_name_Hall '-P 2yb' _space_group_name_H-M_alt 'P 1 21/m 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2017/1 _cell_angle_alpha 90 _cell_angle_beta 94.305(7) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 12.5963(11) _cell_length_b 15.8309(12) _cell_length_c 21.3399(16) _cell_measurement_reflns_used 2152 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 21.3459 _cell_measurement_theta_min 3.5450 _cell_volume 4243.4(6) _computing_cell_refinement 'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)' _computing_data_collection 'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)' _computing_data_reduction 'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)' _computing_molecular_graphics XP(2017) _computing_publication_material WinGX _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_structure_solution 'SHELXT (2017)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 10.2375 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini ultra' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0929 _diffrn_reflns_av_unetI/netI 0.1308 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 23088 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 24.999 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 3.312 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.493 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.97918 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.38a (Rigaku Oxford Diffraction, 2017) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour Red _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Plate _exptl_crystal_F_000 1996 _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.120 _refine_diff_density_max 1.656 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.093 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 516 _refine_ls_number_reflns 7723 _refine_ls_number_restraints 20 _refine_ls_restrained_S_all 1.033 _refine_ls_R_factor_all 0.1448 _refine_ls_R_factor_gt 0.0814 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1249P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2101 _refine_ls_wR_factor_ref 0.2503 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4209 _reflns_number_total 7723 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file am1c05481_si_004.cif _cod_data_source_block A _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/ACS/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_sg_symbol_H-M 'P 21/m' _cod_database_code 4518759 _shelx_shelxl_version_number 2017/1 _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 0.891 _shelx_estimated_absorpt_t_max 0.943 _shelx_res_file ; TITL shelxt_a.res in P2(1)/m shelx.res created by SHELXL-2017/1 at 10:45:17 on 12-Oct-2020 CELL 0.71073 12.5963 15.8309 21.3399 90.000 94.305 90.000 ZERR 2.00 0.0011 0.0012 0.0016 0.000 0.007 0.000 LATT 1 SYMM - X, 1/2 + Y, - Z SFAC C H O CO N UNIT 162 186 86 4 6 MERG 2 OMIT -3.00 50.00 OMIT -2 1 4 OMIT 0 3 3 OMIT -1 2 4 OMIT -1 4 1 OMIT 1 3 2 OMIT 0 4 0 OMIT 0 0 4 OMIT 2 1 2 OMIT -2 1 1 OMIT 2 3 0 OMIT 1 2 1 OMIT 2 1 0 OMIT -1 2 6 OMIT 2 0 0 OMIT 2 0 2 OMIT -2 2 1 OMIT -1 2 2 OMIT -1 4 3 OMIT 0 6 2 OMIT 3 2 1 OMIT 1 8 1 ABIN DFIX 0.92 O19 H19A DFIX 0.92 O19 H19B ISOR 0.01 O1 O2 C1 FMAP 2 PLAN 10 SIZE 0.120 0.220 0.240 ACTA L.S. 20 WGHT 0.124900 FVAR 0.32730 C1 1 0.192811 1.131830 0.435862 11.00000 0.04757 0.05057 = 0.03839 -0.01185 -0.00161 0.00501 C2 1 0.245101 1.069392 0.396251 11.00000 0.04024 0.05162 = 0.03797 -0.01134 -0.00292 0.01041 C3 1 0.188311 1.030802 0.346007 11.00000 0.04606 0.06191 = 0.04097 -0.01374 -0.00197 0.00759 AFIX 43 H3 2 0.116508 1.042862 0.337078 11.00000 -1.20000 AFIX 0 C4 1 0.239405 0.974383 0.309439 11.00000 0.05181 0.05382 = 0.04156 -0.01279 -0.00313 0.01351 C5 1 0.343376 0.954624 0.323202 11.00000 0.04967 0.07073 = 0.04695 -0.02207 0.00127 0.02362 AFIX 43 H5 2 0.376737 0.916515 0.297952 11.00000 -1.20000 AFIX 0 C6 1 0.400069 0.990471 0.374238 11.00000 0.05273 0.06425 = 0.04768 -0.01353 -0.00265 0.01339 C7 1 0.350751 1.048600 0.409873 11.00000 0.05435 0.06906 = 0.04534 -0.02103 -0.00712 0.01021 AFIX 43 H7 2 0.388979 1.074329 0.443639 11.00000 -1.20000 AFIX 0 C8 1 0.512411 0.966772 0.389374 11.00000 0.04379 0.08983 = 0.06298 -0.02295 -0.02203 0.01443 C9 1 0.086854 0.957131 0.234812 11.00000 0.04724 0.05635 = 0.03505 -0.01777 -0.00271 0.01425 AFIX 23 H9A 2 0.077947 1.017968 0.235737 11.00000 -1.20000 H9B 2 0.034559 0.931271 0.259893 11.00000 -1.20000 AFIX 0 C10 1 0.075480 0.924669 0.168361 11.00000 0.03962 0.04979 = 0.03028 -0.00813 -0.00363 0.00832 C11 1 0.009346 0.857582 0.151573 11.00000 0.03580 0.04045 = 0.03569 0.00087 0.00522 0.01000 C12 1 0.000804 0.826911 0.090518 11.00000 0.03101 0.04311 = 0.03009 -0.00129 0.00108 0.00893 C13 1 0.062621 0.863542 0.047712 11.00000 0.03734 0.03304 = 0.02845 -0.00084 -0.00512 0.00870 AFIX 43 H13 2 0.059226 0.842315 0.006975 11.00000 -1.20000 AFIX 0 C14 1 0.130002 0.931051 0.062895 11.00000 0.03113 0.03433 = 0.03955 -0.00020 -0.00273 0.01191 C15 1 0.134435 0.959315 0.123903 11.00000 0.02984 0.04046 = 0.04077 -0.00768 -0.00072 0.00515 C16 1 0.305289 1.017788 0.152478 11.00000 0.05142 0.05631 = 0.05084 -0.02282 -0.00663 -0.01005 AFIX 23 H16A 2 0.317942 0.959687 0.165404 11.00000 -1.20000 H16B 2 0.332226 1.054042 0.186708 11.00000 -1.20000 AFIX 0 C17 1 0.383686 0.964047 0.061740 11.00000 0.03536 0.03471 = 0.03421 0.00784 0.00077 -0.00173 C18 1 0.515601 1.070415 0.931844 11.00000 0.03041 0.03771 = 0.02722 0.00586 -0.00420 -0.01343 C19 1 0.494214 1.139978 0.967501 11.00000 0.02538 0.04090 = 0.02824 0.00834 0.00113 -0.00225 C20 1 0.569022 1.172655 1.011643 11.00000 0.03618 0.03574 = 0.02108 0.01291 -0.00068 -0.00545 C21 1 0.668194 1.135543 1.017282 11.00000 0.03421 0.03321 = 0.02779 0.00455 -0.00169 -0.00679 AFIX 43 H21 2 0.719336 1.157235 1.046643 11.00000 -1.20000 AFIX 0 C22 1 0.305224 0.932354 0.018748 11.00000 0.03420 0.03168 = 0.02588 0.00822 0.00176 -0.00243 C23 1 0.195898 0.972687 0.014307 11.00000 0.03613 0.03987 = 0.03542 0.00668 -0.00577 0.00563 C24 1 0.140359 0.971462 -0.051700 11.00000 0.04374 0.05311 = 0.04269 0.01750 -0.00459 0.01216 AFIX 33 H24A 2 0.071839 0.997882 -0.051133 11.00000 -1.50000 H24B 2 0.182713 1.001654 -0.079833 11.00000 -1.50000 H24C 2 0.131566 0.914078 -0.065682 11.00000 -1.50000 AFIX 0 C25 1 -0.068461 0.750000 0.074007 10.50000 0.03729 0.04620 = 0.03104 0.00000 -0.01023 0.00000 C26 1 -0.119940 0.750000 0.007780 10.50000 0.04703 0.05259 = 0.03447 0.00000 -0.01400 0.00000 AFIX 33 H26A 2 -0.162004 0.699796 0.001054 10.50000 -1.50000 H26B 2 -0.164791 0.798791 0.001708 10.50000 -1.50000 H26C 2 -0.065751 0.751413 -0.021526 10.50000 -1.50000 AFIX 0 C27 1 -0.022714 0.750000 0.226656 10.50000 0.06427 0.06903 = 0.02675 0.00000 0.01001 0.00000 AFIX 23 H27A 2 0.054411 0.750000 0.232380 10.50000 -1.20000 H27B 2 -0.049821 0.750001 0.268018 10.50000 -1.20000 AFIX 0 C28 1 0.539431 1.250000 1.050482 10.50000 0.03328 0.05325 = 0.02249 0.00000 -0.00141 0.00000 C29 1 0.591516 1.250000 1.116759 10.50000 0.06054 0.05786 = 0.03128 0.00000 -0.00259 0.00000 AFIX 33 H29A 2 0.570086 1.299539 1.138484 10.50000 -1.50000 H29B 2 0.569986 1.200512 1.138507 10.50000 -1.50000 H29C 2 0.667506 1.249949 1.115319 10.50000 -1.50000 AFIX 0 C30 1 0.384449 1.250000 0.923695 10.50000 0.03461 0.06019 = 0.02944 0.00000 -0.01319 0.00000 AFIX 23 H30A 2 0.316185 1.250000 0.899418 10.50000 -1.20000 H30B 2 0.439596 1.250000 0.894318 10.50000 -1.20000 AFIX 0 C31 1 0.428521 1.030501 0.891049 11.00000 0.04851 0.04335 = 0.03452 0.00669 -0.00381 -0.01365 AFIX 23 H31A 2 0.446799 0.972078 0.883379 11.00000 -1.20000 H31B 2 0.363498 1.031002 0.912687 11.00000 -1.20000 AFIX 0 C32 1 0.327580 1.043176 0.794519 11.00000 0.04445 0.04187 = 0.03174 0.00415 -0.00486 -0.00662 C33 1 0.270410 0.972038 0.804684 11.00000 0.05665 0.03564 = 0.03098 0.00212 -0.00576 -0.00330 AFIX 43 H33 2 0.289069 0.938336 0.839475 11.00000 -1.20000 AFIX 0 C34 1 0.184649 0.949532 0.763552 11.00000 0.04923 0.03136 = 0.04202 -0.00289 -0.00309 0.00040 C35 1 0.157760 0.997410 0.710803 11.00000 0.04060 0.03547 = 0.04280 -0.00229 -0.00866 -0.00010 AFIX 43 H35 2 0.100702 0.981804 0.683030 11.00000 -1.20000 AFIX 0 C36 1 0.217057 1.069573 0.699496 11.00000 0.03889 0.04389 = 0.03423 0.00266 -0.00322 0.00219 C37 1 0.300783 1.093041 0.741593 11.00000 0.05085 0.04251 = 0.04214 0.00748 0.00192 -0.01175 AFIX 43 H37 2 0.339180 1.141913 0.734693 11.00000 -1.20000 AFIX 0 C38 1 0.188231 1.121226 0.643122 11.00000 0.03416 0.04548 = 0.04480 0.00818 -0.00506 -0.00318 C39 1 0.121655 0.871718 0.774554 11.00000 0.06860 0.03924 = 0.04124 0.00089 -0.01142 -0.00646 O1 3 0.246235 1.156243 0.482749 11.00000 0.07587 0.11447 = 0.06416 -0.05236 -0.02041 0.03351 O2 3 0.102040 1.156382 0.420036 11.00000 0.06237 0.10043 = 0.07745 -0.04345 -0.01928 0.03249 O3 3 -0.071280 1.250000 0.363905 10.50000 0.05275 0.12006 = 0.05571 0.00000 -0.00947 0.00000 AFIX 3 H3A 2 -0.051181 1.212715 0.333265 10.50000 -1.50000 H3B 2 -0.127407 1.287285 0.354879 10.50000 -1.50000 AFIX 0 O4 3 -0.094645 1.161073 0.483374 11.00000 0.10153 0.13398 = 0.11856 0.02290 -0.00310 -0.06860 AFIX 3 H4A 2 -0.081658 1.103850 0.477689 11.00000 -1.50000 H4B 2 -0.154489 1.178250 0.502996 11.00000 -1.50000 AFIX 0 O5 3 0.081097 1.250000 0.544575 10.50000 0.03724 0.03854 = 0.02323 0.00000 -0.00148 0.00000 AFIX 3 H5A 2 0.057726 1.200492 0.566517 10.50000 -1.50000 H5B 2 0.057726 1.299508 0.566517 10.50000 -1.50000 AFIX 0 O6 3 0.417187 1.250000 0.548557 10.50000 0.04569 0.11838 = 0.07734 0.00000 -0.01417 0.00000 AFIX 3 H6A 2 0.451380 1.212690 0.523089 10.50000 -1.50000 H6B 2 0.456887 1.287310 0.574547 10.50000 -1.50000 AFIX 0 O7 3 0.570188 1.007821 0.424187 11.00000 0.06292 0.17855 = 0.15322 -0.08970 -0.04668 0.03886 O8 3 0.540971 0.898976 0.361915 11.00000 0.05281 0.08211 = 0.06515 -0.00978 -0.00186 0.02601 AFIX 3 H8 2 0.603900 0.889207 0.371937 11.00000 -1.50000 AFIX 0 O9 3 0.192279 0.933852 0.257661 11.00000 0.05473 0.07017 = 0.04726 -0.02906 -0.01525 0.02402 O10 3 0.196537 1.030660 0.141361 11.00000 0.04699 0.03640 = 0.06318 -0.01856 -0.00424 0.00028 O11 3 0.362542 1.034925 0.098261 11.00000 0.05040 0.03676 = 0.05931 -0.01433 -0.00104 -0.00328 O12 3 -0.056354 0.825004 0.194988 11.00000 0.04619 0.05598 = 0.03887 -0.00475 0.01095 0.00121 O13 3 0.393308 1.175342 0.959929 11.00000 0.02649 0.05574 = 0.03892 0.00304 -0.00077 -0.00625 O14 3 0.410807 1.072710 0.833294 11.00000 0.05485 0.05761 = 0.03299 0.01537 -0.01277 -0.02018 O15 3 0.153669 0.828046 0.822004 11.00000 0.11835 0.03620 = 0.05458 0.01251 -0.02770 -0.02534 AFIX 83 H15 2 0.115211 0.786561 0.824424 11.00000 -1.50000 AFIX 0 O16 3 0.045143 0.854034 0.738258 11.00000 0.09290 0.05852 = 0.05687 0.01136 -0.02460 -0.03258 O17 3 0.092979 1.125217 0.623621 11.00000 0.04246 0.07779 = 0.07842 0.04485 -0.00667 -0.01007 O18 3 0.262701 1.159939 0.618962 11.00000 0.03815 0.04889 = 0.03827 0.01205 -0.00377 0.00086 O19 3 -0.207355 1.025234 0.449928 10.50000 0.06916 0.07347 = 0.11211 0.01787 -0.03427 -0.00836 CO1 4 0.250401 1.250000 0.547389 10.50000 0.03245 0.04661 = 0.02307 0.00000 -0.00187 0.00000 CO2 4 0.008947 1.250000 0.452317 10.50000 0.03653 0.04753 = 0.03525 0.00000 -0.00289 0.00000 H19B 2 -0.229429 1.072232 0.471852 10.50000 0.10806 H19A 2 -0.272759 1.016238 0.427775 10.50000 0.04153 HKLF 4 REM shelxt_a.res in P2(1)/m REM R1 = 0.0814 for 4209 Fo > 4sig(Fo) and 0.1448 for all 7723 data REM 516 parameters refined using 20 restraints END WGHT 0.1337 0.0000 REM Highest difference peak 1.656, deepest hole -0.567, 1-sigma level 0.093 Q1 1 0.0011 1.0036 0.5078 11.00000 0.05 1.66 Q2 1 0.4619 1.2500 0.5039 10.50000 0.05 1.13 Q3 1 0.4481 1.2500 1.0498 10.50000 0.05 0.74 Q4 1 0.2110 1.0348 0.0299 11.00000 0.05 0.58 Q5 1 -0.1206 0.7500 0.1085 10.50000 0.05 0.46 Q6 1 0.4517 0.7500 0.2343 10.50000 0.05 0.43 Q7 1 -0.1490 0.7500 -0.1699 10.50000 0.05 0.41 Q8 1 0.3441 0.7500 0.2151 10.50000 0.05 0.39 Q9 1 0.1957 1.1247 0.4925 11.00000 0.05 0.39 Q10 1 -0.0463 1.2500 0.5004 10.50000 0.05 0.38 ; _shelx_res_checksum 18699 _shelx_hkl_file ; 0 0 -4 823.88 32.19 0 0 4 871.18 34.84 0 0 -5 830.94 36.21 0 0 5 890.11 39.35 0 0 -6 215.49 20.41 0 0 6 211.76 22.18 0 0 -7 73.99 13.15 0 0 7 71.63 14.62 0 0 -8 26.99 8.54 0 0 8 11.28 8.54 0 0 9 67.12 13.93 0 0 -9 77.13 15.01 0 0 10 1451.40 71.83 0 0 -10 1345.82 64.96 0 0 -11 827.71 54.36 0 0 11 857.44 58.09 0 0 12 332.06 39.15 0 0 13 484.06 47.79 0 0 -14 151.61 27.38 0 0 14 141.21 24.73 0 0 -15 37.19 14.92 0 0 15 65.45 20.51 0 0 -16 109.31 25.22 0 0 16 151.90 30.71 0 0 -17 26.79 12.76 0 0 -18 44.75 17.37 0 0 -19 24.83 15.60 0 0 -20 128.45 29.24 0 0 -21 163.77 34.64 0 0 -22 35.13 16.29 0 0 -23 102.74 34.34 0 0 -24 -7.65 9.71 0 0 -25 4.71 14.72 0 0 -26 11.97 14.62 0 0 -27 15.99 17.37 0 0 -28 37.78 19.04 0 1 4 452.17 25.91 0 1 4 444.13 25.81 0 1 -4 453.94 21.88 0 1 -5 6.57 5.50 0 1 5 7.36 6.77 0 -1 6 1389.68 53.38 0 1 6 1405.38 54.66 0 1 -6 1396.85 47.59 0 -1 -7 38.56 10.11 0 1 7 45.53 11.48 0 1 -7 44.84 10.89 0 -1 7 49.85 11.68 0 1 -8 61.92 11.97 0 1 8 67.32 14.03 0 -1 8 69.96 15.31 0 -1 -8 60.15 12.95 0 1 -9 13.05 7.07 0 1 9 3.34 5.40 0 -1 -9 12.85 7.16 0 -1 9 14.82 10.70 0 1 10 231.58 30.62 0 1 -10 182.12 23.75 0 -1 -10 197.83 26.40 0 -1 10 221.28 28.95 0 1 -11 8.34 5.89 0 1 11 14.52 6.38 0 -1 11 12.66 10.11 0 -1 12 11.09 9.62 0 1 12 6.38 5.40 0 -1 -13 196.94 29.34 0 1 13 211.37 31.99 0 -1 13 236.59 33.56 0 1 14 229.13 35.62 0 -1 14 219.32 35.03 0 -1 -14 197.33 30.62 0 -1 -15 110.30 24.43 0 1 -15 142.87 27.08 0 -1 15 139.83 28.06 0 1 15 138.36 30.03 0 -1 16 106.57 28.56 0 -1 -16 52.20 16.58 0 1 16 75.26 21.20 0 1 -16 71.73 19.72 0 -1 -17 28.56 13.64 0 1 -17 20.70 11.78 0 -1 17 19.04 9.22 0 -1 -18 19.92 12.27 0 1 -18 -4.42 10.60 0 -1 -19 58.19 18.64 0 1 -19 86.94 24.24 0 -1 -20 7.26 10.70 0 1 -20 -6.77 9.32 0 -1 -21 -0.20 12.27 0 1 -21 2.75 9.22 0 -1 -22 -9.03 18.64 0 1 -22 -8.83 11.78 0 1 -23 42.49 19.63 0 -1 -23 71.73 31.79 0 1 -24 -10.89 16.19 0 -1 -24 15.11 17.07 0 1 -25 2.55 12.76 0 -1 -25 -10.79 11.09 0 -1 -26 -44.65 27.48 0 1 -26 21.88 15.60 0 -1 -27 20.21 11.78 0 1 -27 -3.83 18.94 0 1 -28 -6.38 12.27 0 -1 -28 -12.95 22.57 0 2 3 870.98 34.34 0 -2 -3 884.33 32.48 0 2 3 916.31 33.66 0 2 4 3237.23 71.04 0 -2 -4 3166.67 70.16 0 2 -4 3202.88 50.83 0 2 4 3230.55 73.40 0 2 -5 0.29 3.73 0 2 5 -2.94 7.16 0 2 6 14.23 8.34 0 2 -6 8.93 4.71 0 2 7 -2.94 5.79 0 2 -7 1.96 4.61 0 2 -8 155.92 17.76 0 -2 8 172.21 21.49 0 -2 8 176.34 12.17 0 -2 -8 163.87 11.48 0 2 8 175.84 22.96 0 -2 9 547.26 21.00 0 2 -9 496.03 34.15 0 -2 -9 511.54 19.82 0 -2 9 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0.00 -8 6 23 -0.26 0.00 -7 6 23 -0.13 0.00 -6 6 23 2.69 0.00 4 6 23 0.72 0.00 5 6 23 -1.39 0.00 6 6 23 0.60 0.00 -8 7 23 1.73 0.00 -7 7 23 -1.07 0.00 -6 7 23 -0.47 0.00 -5 7 23 0.48 0.00 2 7 23 -2.91 0.00 3 7 23 -1.51 0.00 4 7 23 5.01 0.00 5 7 23 1.03 0.00 6 7 23 -0.72 0.00 -7 8 23 0.30 0.00 -6 8 23 -2.08 0.00 -5 8 23 5.26 0.00 -4 8 23 0.32 0.00 -3 8 23 -0.92 0.00 -2 8 23 -3.36 0.00 -1 8 23 1.82 0.00 0 8 23 0.78 0.00 1 8 23 1.63 0.00 2 8 23 -0.24 0.00 3 8 23 -2.41 0.00 4 8 23 -2.43 0.00 5 8 23 0.69 0.00 -6 9 23 -2.05 0.00 -5 9 23 1.75 0.00 -4 9 23 3.17 0.00 -3 9 23 -2.90 0.00 -2 9 23 1.73 0.00 -1 9 23 3.00 0.00 0 9 23 -1.68 0.00 1 9 23 -0.17 0.00 2 9 23 0.36 0.00 3 9 23 -0.25 0.00 4 9 23 -2.00 0.00 -5 10 23 -3.67 0.00 -4 10 23 -0.33 0.00 -3 10 23 0.94 0.00 -2 10 23 4.98 0.00 -1 10 23 -0.88 0.00 0 10 23 -3.23 0.00 1 10 23 -1.84 0.00 2 10 23 1.96 0.00 3 10 23 1.47 0.00 -4 11 23 -0.92 0.00 -3 11 23 1.17 0.00 -2 11 23 -1.20 0.00 -1 11 23 -1.26 0.00 0 11 23 3.06 0.00 1 11 23 -1.37 0.00 2 11 23 -0.22 0.00 -9 0 24 -1.22 0.00 -8 0 24 2.66 0.00 -7 0 24 0.67 0.00 -6 0 24 1.40 0.00 4 0 24 -0.11 0.00 5 0 24 1.57 0.00 6 0 24 0.73 0.00 7 0 24 -0.34 0.00 -9 1 24 2.03 0.00 -8 1 24 -4.04 0.00 -7 1 24 3.36 0.00 -6 1 24 2.67 0.00 4 1 24 -2.41 0.00 5 1 24 0.52 0.00 6 1 24 -0.04 0.00 7 1 24 -0.21 0.00 -9 2 24 1.71 0.00 -8 2 24 -2.56 0.00 -7 2 24 0.60 0.00 -6 2 24 -2.84 0.00 4 2 24 0.76 0.00 5 2 24 -1.73 0.00 6 2 24 1.23 0.00 7 2 24 -1.24 0.00 -9 3 24 -0.32 0.00 -8 3 24 1.41 0.00 -7 3 24 -1.88 0.00 -6 3 24 -1.81 0.00 4 3 24 1.93 0.00 5 3 24 -0.38 0.00 6 3 24 -0.84 0.00 -8 4 24 0.02 0.00 -7 4 24 1.28 0.00 -6 4 24 1.29 0.00 -5 4 24 -2.16 0.00 3 4 24 2.94 0.00 4 4 24 -2.10 0.00 5 4 24 0.39 0.00 6 4 24 0.32 0.00 -8 5 24 -1.81 0.00 -7 5 24 2.48 0.00 -6 5 24 0.85 0.00 -5 5 24 -0.41 0.00 -4 5 24 1.52 0.00 2 5 24 1.20 0.00 3 5 24 -1.73 0.00 4 5 24 0.66 0.00 5 5 24 -0.73 0.00 6 5 24 0.82 0.00 -7 6 24 -1.05 0.00 -6 6 24 -2.55 0.00 -5 6 24 0.58 0.00 -4 6 24 0.89 0.00 -3 6 24 1.97 0.00 0 6 24 -2.05 0.00 1 6 24 2.34 0.00 2 6 24 1.55 0.00 3 6 24 -2.22 0.00 4 6 24 -0.30 0.00 5 6 24 1.13 0.00 -7 7 24 -0.75 0.00 -6 7 24 -1.13 0.00 -5 7 24 0.33 0.00 -4 7 24 -1.60 0.00 -3 7 24 1.53 0.00 -2 7 24 0.97 0.00 -1 7 24 0.84 0.00 0 7 24 0.87 0.00 1 7 24 -0.18 0.00 2 7 24 0.25 0.00 3 7 24 4.48 0.00 4 7 24 -2.04 0.00 5 7 24 -2.33 0.00 -6 8 24 1.65 0.00 -5 8 24 -0.25 0.00 -4 8 24 -0.38 0.00 -3 8 24 -3.89 0.00 -2 8 24 2.02 0.00 -1 8 24 2.24 0.00 0 8 24 1.96 0.00 1 8 24 -2.00 0.00 2 8 24 -1.67 0.00 3 8 24 0.53 0.00 4 8 24 2.91 0.00 -5 9 24 -0.39 0.00 -4 9 24 -1.05 0.00 -3 9 24 -0.64 0.00 -2 9 24 1.56 0.00 -1 9 24 -1.53 0.00 0 9 24 -1.40 0.00 1 9 24 -0.41 0.00 2 9 24 1.06 0.00 3 9 24 -2.49 0.00 -3 10 24 1.96 0.00 -2 10 24 -1.57 0.00 -1 10 24 -2.08 0.00 0 10 24 0.39 0.00 1 10 24 0.10 0.00 -8 0 25 -0.10 0.00 -7 0 25 0.15 0.00 -6 0 25 1.59 0.00 -5 0 25 -2.50 0.00 -4 0 25 3.99 0.00 2 0 25 4.20 0.00 3 0 25 1.13 0.00 4 0 25 -0.66 0.00 5 0 25 -0.29 0.00 6 0 25 -0.85 0.00 -8 1 25 1.88 0.00 -7 1 25 1.90 0.00 -6 1 25 -3.55 0.00 -5 1 25 -0.58 0.00 -4 1 25 -3.35 0.00 2 1 25 0.62 0.00 3 1 25 2.34 0.00 4 1 25 -2.15 0.00 5 1 25 0.34 0.00 6 1 25 -0.17 0.00 -8 2 25 -1.65 0.00 -7 2 25 1.00 0.00 -6 2 25 -1.09 0.00 -5 2 25 1.66 0.00 -4 2 25 -2.69 0.00 1 2 25 -0.84 0.00 2 2 25 -4.71 0.00 3 2 25 -0.16 0.00 4 2 25 1.28 0.00 5 2 25 -0.80 0.00 6 2 25 -0.35 0.00 -7 3 25 -1.11 0.00 -6 3 25 2.30 0.00 -5 3 25 -0.55 0.00 -4 3 25 3.34 0.00 -3 3 25 -1.73 0.00 0 3 25 0.05 0.00 1 3 25 2.80 0.00 2 3 25 -1.04 0.00 3 3 25 -1.08 0.00 4 3 25 1.22 0.00 5 3 25 -0.25 0.00 -7 4 25 0.00 0.00 -6 4 25 0.41 0.00 -5 4 25 -1.34 0.00 -4 4 25 1.66 0.00 -3 4 25 0.72 0.00 -2 4 25 -1.61 0.00 -1 4 25 0.66 0.00 0 4 25 -1.86 0.00 1 4 25 -2.62 0.00 2 4 25 4.86 0.00 3 4 25 -1.15 0.00 4 4 25 -0.01 0.00 5 4 25 0.17 0.00 -7 5 25 -1.35 0.00 -6 5 25 0.14 0.00 -5 5 25 -0.60 0.00 -4 5 25 -1.65 0.00 -3 5 25 -1.13 0.00 -2 5 25 1.80 0.00 -1 5 25 0.23 0.00 0 5 25 0.68 0.00 1 5 25 -1.73 0.00 2 5 25 0.29 0.00 3 5 25 0.65 0.00 4 5 25 -0.30 0.00 5 5 25 1.73 0.00 -6 6 25 -0.47 0.00 -5 6 25 2.49 0.00 -4 6 25 -1.71 0.00 -3 6 25 -1.27 0.00 -2 6 25 -1.06 0.00 -1 6 25 0.35 0.00 0 6 25 0.60 0.00 1 6 25 1.59 0.00 2 6 25 -2.85 0.00 3 6 25 2.48 0.00 4 6 25 0.39 0.00 -5 7 25 0.17 0.00 -4 7 25 2.47 0.00 -3 7 25 -0.05 0.00 -2 7 25 -1.51 0.00 -1 7 25 0.16 0.00 0 7 25 1.93 0.00 1 7 25 -0.08 0.00 2 7 25 -0.98 0.00 3 7 25 -2.43 0.00 -4 8 25 -0.10 0.00 -3 8 25 2.51 0.00 -2 8 25 1.64 0.00 -1 8 25 -1.27 0.00 0 8 25 -1.22 0.00 1 8 25 0.39 0.00 2 8 25 1.74 0.00 -2 9 25 -0.26 0.00 -1 9 25 -0.11 0.00 0 9 25 -0.44 0.00 -7 0 26 -0.20 0.00 -6 0 26 -0.79 0.00 -5 0 26 -0.44 0.00 -4 0 26 -1.24 0.00 -3 0 26 -5.38 0.00 -2 0 26 3.57 0.00 -1 0 26 -0.68 0.00 0 0 26 2.90 0.00 1 0 26 3.76 0.00 2 0 26 -0.81 0.00 3 0 26 -3.25 0.00 4 0 26 0.40 0.00 -7 1 26 -2.90 0.00 -6 1 26 -0.04 0.00 -5 1 26 -1.36 0.00 -4 1 26 3.40 0.00 -3 1 26 -3.95 0.00 -2 1 26 2.25 0.00 -1 1 26 1.96 0.00 0 1 26 -2.01 0.00 1 1 26 -0.02 0.00 2 1 26 3.81 0.00 3 1 26 -3.08 0.00 4 1 26 -0.62 0.00 -6 2 26 1.59 0.00 -5 2 26 -1.73 0.00 -4 2 26 2.54 0.00 -3 2 26 3.27 0.00 -2 2 26 -2.28 0.00 -1 2 26 0.29 0.00 0 2 26 -2.01 0.00 1 2 26 -3.69 0.00 2 2 26 0.82 0.00 3 2 26 2.19 0.00 4 2 26 -0.81 0.00 -6 3 26 0.30 0.00 -5 3 26 1.61 0.00 -4 3 26 -3.56 0.00 -3 3 26 2.96 0.00 -2 3 26 -2.98 0.00 -1 3 26 1.14 0.00 0 3 26 2.16 0.00 1 3 26 -1.36 0.00 2 3 26 -2.22 0.00 3 3 26 1.52 0.00 4 3 26 -0.22 0.00 -6 4 26 -0.57 0.00 -5 4 26 2.20 0.00 -4 4 26 -1.92 0.00 -3 4 26 -0.35 0.00 -2 4 26 1.01 0.00 -1 4 26 -2.57 0.00 0 4 26 1.28 0.00 1 4 26 3.85 0.00 2 4 26 -1.08 0.00 3 4 26 -1.90 0.00 -5 5 26 -0.28 0.00 -4 5 26 0.63 0.00 -3 5 26 -0.33 0.00 -2 5 26 2.14 0.00 -1 5 26 -0.99 0.00 0 5 26 -3.57 0.00 1 5 26 2.29 0.00 2 5 26 1.32 0.00 3 5 26 0.36 0.00 -4 6 26 1.60 0.00 -3 6 26 -0.87 0.00 -2 6 26 -0.19 0.00 -1 6 26 1.90 0.00 0 6 26 1.11 0.00 1 6 26 -2.05 0.00 2 6 26 1.81 0.00 -3 7 26 0.20 0.00 -2 7 26 0.26 0.00 -1 7 26 -0.30 0.00 0 7 26 0.55 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 270519) # 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 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 0.524 0.250 0.434 527 130 ' ' 2 0.476 0.750 0.566 528 130 ' ' # Missing Reflections Below sin(th)/lambda = 0.25 loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta 1 0 0 1.621 1 1 0 2.070 2 1 0 3.490 0 2 0 2.573 1 2 0 3.042 2 3 0 5.046 0 4 0 5.152 -1 0 1 1.820 0 0 1 0.957 1 0 1 1.944 -2 1 1 3.554 -1 1 1 2.229 0 1 1 1.603 1 1 1 2.331 -1 2 1 3.152 0 2 1 2.746 1 2 1 3.225 -1 4 1 5.465 -1 0 2 2.414 0 0 2 1.914 1 0 2 2.600 -1 1 2 2.736 0 1 2 2.306 1 1 2 2.901 2 1 2 4.097 0 2 2 3.208 1 3 2 4.657 -1 0 3 3.190 0 0 3 2.872 0 1 3 3.147 0 3 3 4.815 0 0 4 3.830 -2 1 4 5.001 -1 2 4 4.797 -1 2 6 6.401 _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL shelxt_a.res in P2(1)/m CELL 12.5963 15.8309 21.3399 90.00 94.31 90.00 SPGR P21/m # Solvent Accessible Volume = 1056 # Electrons Found in S.A.V. = 257 # Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others C101 0.355 0.749 0.227 ! 5.00 eA-3 C102 0.537 0.253 0.766 ! 4.67 eA-3 C103 0.296 0.746 0.305 ! 4.33 eA-3 Q104 0.427 0.753 0.484 ! 3.91 eA-3 C105 0.157 0.217 0.231 ! 3.45 eA-3 C106 0.132 0.252 0.164 ! 3.06 eA-3 Q107 0.790 0.468 0.448 ! 3.04 eA-3 C108 0.684 0.249 0.852 ! 3.04 eA-3 C109 0.377 0.312 0.251 ! 3.01 eA-3 C110 0.223 0.749 0.305 ! 2.83 eA-3 C111 0.279 0.750 0.258 ! 2.77 eA-3 C112 0.183 0.217 0.282 ! 2.68 eA-3 C113 0.473 0.346 0.262 ! 2.51 eA-3 C114 0.540 0.228 0.297 ! 2.43 eA-3 C115 0.183 0.248 0.172 ! 2.34 eA-3 C116 0.123 0.681 0.390 ! 2.31 eA-3 C117 1.000 1.000 0.500 ! 1.92 eA-3 Q118 0.532 0.750 0.492 ! 1.79 eA-3 C119 0.152 0.743 0.391 ! 1.74 eA-3 C120 0.582 0.159 0.491 ! 1.42 eA-3 C121 0.136 0.244 0.313 ! 1.39 eA-3 C122 0.626 0.249 0.273 ! 1.33 eA-3 Q123 0.799 0.248 0.883 ! 1.27 eA-3 C124 0.332 0.750 0.453 ! 1.25 eA-3 Q125 0.371 0.751 0.422 ! 1.24 eA-3 C126 0.536 0.254 0.250 ! 1.23 eA-3 C127 0.442 0.185 0.285 ! 1.22 eA-3 C128 0.536 0.752 0.586 ! 1.21 eA-3 C129 0.658 0.169 0.479 ! 1.11 eA-3 C130 0.561 0.756 0.633 ! 1.08 eA-3 C131 0.396 0.629 0.481 ! 1.08 eA-3 C132 0.763 0.252 0.563 ! 1.07 eA-3 C133 0.417 0.253 0.227 ! 1.05 eA-3 C134 0.484 0.252 0.274 ! 1.04 eA-3 Q135 0.430 0.249 0.047 ! 1.04 eA-3 C136 0.649 0.182 0.322 ! 1.02 eA-3 C137 0.658 0.159 0.350 ! 1.01 eA-3 C138 0.679 0.218 0.289 ! 1.00 eA-3 Q139 0.233 0.190 0.331 ! 1.00 eA-3 C140 0.368 0.801 0.446 ! 1.00 eA-3 C141 0.596 0.879 0.724 ! 1.00 eA-3 C142 0.272 0.248 0.164 ! 0.98 eA-3 Q143 0.534 0.249 0.469 ! 0.97 eA-3 C144 0.669 0.221 0.314 ! 0.97 eA-3 C145 0.600 0.749 0.734 ! 0.96 eA-3 C146 0.472 0.253 0.320 ! 0.95 eA-3 C147 0.588 0.242 0.344 ! 0.95 eA-3 Q148 0.151 0.755 0.422 ! 0.95 eA-3 C149 0.583 0.328 0.331 ! 0.95 eA-3 C150 0.596 0.253 0.438 ! 0.94 eA-3 C151 0.359 0.785 0.494 ! 0.94 eA-3 C152 0.541 0.379 0.284 ! 0.93 eA-3 C153 0.719 0.295 0.567 ! 0.92 eA-3 C154 0.385 0.716 0.560 ! 0.92 eA-3 Q155 0.683 0.751 0.953 ! 0.91 eA-3 Q156 0.293 0.366 0.313 ! 0.91 eA-3 C157 0.627 0.128 0.305 ! 0.90 eA-3 C158 0.522 0.252 0.367 ! 0.88 eA-3 C159 0.395 0.667 0.720 ! 0.86 eA-3 Q160 0.250 0.747 0.070 ! 0.85 eA-3 C161 0.211 0.703 0.399 ! 0.85 eA-3 C162 0.283 0.806 0.177 ! 0.85 eA-3 C163 0.673 0.640 0.731 ! 0.85 eA-3 C164 0.247 0.261 0.258 ! 0.83 eA-3 Q165 0.119 0.249 0.891 ! 0.82 eA-3 Q166 0.528 0.112 0.329 ! 0.80 eA-3 Q167 0.534 0.893 0.701 ! 0.80 eA-3 C168 0.734 0.122 0.372 ! 0.80 eA-3 Q169 0.438 0.514 0.718 ! 0.79 eA-3 C170 0.439 0.813 0.540 ! 0.79 eA-3 C171 0.688 0.748 0.672 ! 0.79 eA-3 Q172 0.387 0.249 0.437 ! 0.78 eA-3 Q173 0.795 0.247 0.781 ! 0.77 eA-3 C174 0.575 0.138 0.263 ! 0.76 eA-3 Q175 0.067 0.752 0.312 ! 0.76 eA-3 Q176 0.482 0.843 0.269 ! 0.75 eA-3 Q177 0.199 0.033 0.032 ! 0.75 eA-3 Q178 0.264 0.249 0.359 ! 0.75 eA-3 C179 0.042 0.248 0.141 ! 0.75 eA-3 Q180 0.705 0.252 0.242 ! 0.75 eA-3 C181 0.677 0.249 0.453 ! 0.75 eA-3 C182 0.330 0.625 0.495 ! 0.74 eA-3 C183 0.518 0.748 0.281 ! 0.74 eA-3 Q184 0.860 0.248 0.445 ! 0.74 eA-3 Q185 0.667 0.108 0.325 ! 0.74 eA-3 Q186 0.630 0.252 0.961 ! 0.74 eA-3 Q187 0.148 0.828 0.310 ! 0.72 eA-3 Q188 0.609 0.077 0.292 ! 0.71 eA-3 C189 0.186 0.718 0.354 ! 0.71 eA-3 C190 0.330 0.756 0.641 ! 0.71 eA-3 Q191 0.019 0.799 0.343 ! 0.70 eA-3 Q192 0.835 0.250 0.922 ! 0.70 eA-3 C193 0.651 0.711 0.703 ! 0.69 eA-3 Q194 0.427 0.922 0.079 ! 0.69 eA-3 Q195 0.768 0.253 0.289 ! 0.69 eA-3 C196 0.298 0.206 0.278 ! 0.69 eA-3 C197 0.322 0.202 0.164 ! 0.69 eA-3 C198 0.605 0.252 0.391 ! 0.69 eA-3 Q199 0.494 0.999 0.783 ! 0.68 eA-3 ) ; _shelx_fab_checksum 18560 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1928(6) 1.1318(4) 0.4359(3) 0.0458(16) Uani 1 1 d . U . . . C2 C 0.2451(5) 1.0694(4) 0.3963(3) 0.0436(15) Uani 1 1 d . . . . . C3 C 0.1883(6) 1.0308(4) 0.3460(3) 0.0499(17) Uani 1 1 d . . . . . H3 H 0.116508 1.042862 0.337078 0.060 Uiso 1 1 calc R U . . . C4 C 0.2394(6) 0.9744(4) 0.3094(3) 0.0494(17) Uani 1 1 d . . . . . C5 C 0.3434(6) 0.9546(4) 0.3232(3) 0.0559(19) Uani 1 1 d . . . . . H5 H 0.376737 0.916515 0.297952 0.067 Uiso 1 1 calc R U . . . C6 C 0.4001(6) 0.9905(4) 0.3742(3) 0.0552(18) Uani 1 1 d . . . . . C7 C 0.3508(6) 1.0486(4) 0.4099(3) 0.0568(19) Uani 1 1 d . . . . . H7 H 0.388979 1.074329 0.443639 0.068 Uiso 1 1 calc R U . . . C8 C 0.5124(6) 0.9668(5) 0.3894(4) 0.067(2) Uani 1 1 d . . . . . C9 C 0.0869(5) 0.9571(4) 0.2348(3) 0.0465(16) Uani 1 1 d . . . . . H9A H 0.077947 1.017968 0.235737 0.056 Uiso 1 1 calc R U . . . H9B H 0.034559 0.931271 0.259893 0.056 Uiso 1 1 calc R U . . . C10 C 0.0755(5) 0.9247(4) 0.1684(3) 0.0402(15) Uani 1 1 d . . . . . C11 C 0.0093(5) 0.8576(3) 0.1516(3) 0.0372(14) Uani 1 1 d . . . . . C12 C 0.0008(5) 0.8269(3) 0.0905(3) 0.0348(14) Uani 1 1 d . . . . . C13 C 0.0626(5) 0.8635(3) 0.0477(3) 0.0333(13) Uani 1 1 d . . . . . H13 H 0.059226 0.842315 0.006975 0.040 Uiso 1 1 calc R U . . . C14 C 0.1300(5) 0.9311(3) 0.0629(3) 0.0353(14) Uani 1 1 d . . . . . C15 C 0.1344(5) 0.9593(3) 0.1239(3) 0.0372(14) Uani 1 1 d . . . . . C16 C 0.3053(6) 1.0178(4) 0.1525(3) 0.0534(18) Uani 1 1 d . . . . . H16A H 0.317942 0.959687 0.165404 0.064 Uiso 1 1 calc R U . . . H16B H 0.332226 1.054042 0.186708 0.064 Uiso 1 1 calc R U . . . C17 C 0.3837(5) 0.9640(3) 0.0617(3) 0.0349(14) Uani 1 1 d . . . . . C18 C 0.5156(5) 1.0704(3) 0.9318(2) 0.0321(13) Uani 1 1 d . . . . . C19 C 0.4942(4) 1.1400(3) 0.9675(2) 0.0315(13) Uani 1 1 d . . . . . C20 C 0.5690(5) 1.1727(3) 1.0116(2) 0.0311(13) Uani 1 1 d . . . . . C21 C 0.6682(5) 1.1355(3) 1.0173(2) 0.0319(13) Uani 1 1 d . . . . . H21 H 0.719336 1.157235 1.046643 0.038 Uiso 1 1 calc R U . . . C22 C 0.3052(4) 0.9324(3) 0.0187(2) 0.0306(13) Uani 1 1 d . . . . . C23 C 0.1959(5) 0.9727(3) 0.0143(3) 0.0376(14) Uani 1 1 d . . . . . C24 C 0.1404(5) 0.9715(4) -0.0517(3) 0.0469(16) Uani 1 1 d . . . . . H24A H 0.071839 0.997882 -0.051133 0.070 Uiso 1 1 calc R U . . . H24B H 0.182713 1.001654 -0.079833 0.070 Uiso 1 1 calc R U . . . H24C H 0.131566 0.914078 -0.065682 0.070 Uiso 1 1 calc R U . . . C25 C -0.0685(7) 0.750000 0.0740(4) 0.039(2) Uani 1 2 d S T P . . C26 C -0.1199(7) 0.750000 0.0078(4) 0.046(2) Uani 1 2 d S T P . . H26A H -0.162004 0.699796 0.001054 0.068 Uiso 0.5 1 calc R U P . . H26B H -0.164791 0.798791 0.001708 0.068 Uiso 0.5 1 calc R U P . . H26C H -0.065751 0.751413 -0.021526 0.068 Uiso 1 2 calc R U P . . C27 C -0.0227(9) 0.750000 0.2267(4) 0.053(2) Uani 1 2 d S T P . . H27A H 0.054411 0.750000 0.232380 0.064 Uiso 1 2 calc R U P . . H27B H -0.049821 0.750001 0.268018 0.064 Uiso 1 2 calc R U P . . C28 C 0.5394(7) 1.250000 1.0505(4) 0.0365(19) Uani 1 2 d S T P . . C29 C 0.5915(8) 1.250000 1.1168(4) 0.050(2) Uani 1 2 d S T P . . H29A H 0.570086 1.299539 1.138484 0.075 Uiso 0.5 1 calc R U P . . H29B H 0.569986 1.200512 1.138507 0.075 Uiso 0.5 1 calc R U P . . H29C H 0.667506 1.249949 1.115319 0.075 Uiso 1 2 calc R U P . . C30 C 0.3844(7) 1.250000 0.9237(4) 0.042(2) Uani 1 2 d S T P . . H30A H 0.316185 1.250000 0.899418 0.051 Uiso 1 2 calc R U P . . H30B H 0.439596 1.250000 0.894318 0.051 Uiso 1 2 calc R U P . . C31 C 0.4285(5) 1.0305(3) 0.8910(3) 0.0425(15) Uani 1 1 d . . . . . H31A H 0.446799 0.972078 0.883379 0.051 Uiso 1 1 calc R U . . . H31B H 0.363498 1.031002 0.912687 0.051 Uiso 1 1 calc R U . . . C32 C 0.3276(5) 1.0432(3) 0.7945(3) 0.0397(15) Uani 1 1 d . . . . . C33 C 0.2704(5) 0.9720(3) 0.8047(3) 0.0415(15) Uani 1 1 d . . . . . H33 H 0.289069 0.938336 0.839475 0.050 Uiso 1 1 calc R U . . . C34 C 0.1846(5) 0.9495(3) 0.7636(3) 0.0412(15) Uani 1 1 d . . . . . C35 C 0.1578(5) 0.9974(3) 0.7108(3) 0.0402(15) Uani 1 1 d . . . . . H35 H 0.100702 0.981804 0.683030 0.048 Uiso 1 1 calc R U . . . C36 C 0.2171(5) 1.0696(3) 0.6995(3) 0.0393(14) Uani 1 1 d . . . . . C37 C 0.3008(5) 1.0930(4) 0.7416(3) 0.0452(16) Uani 1 1 d . . . . . H37 H 0.339180 1.141913 0.734693 0.054 Uiso 1 1 calc R U . . . C38 C 0.1882(5) 1.1212(3) 0.6431(3) 0.0419(15) Uani 1 1 d . . . . . C39 C 0.1217(6) 0.8717(4) 0.7746(3) 0.0505(18) Uani 1 1 d . . . . . O1 O 0.2462(4) 1.1562(4) 0.4827(2) 0.0861(18) Uani 1 1 d . U . . . O2 O 0.1020(4) 1.1564(3) 0.4200(3) 0.0813(17) Uani 1 1 d . U . . . O3 O -0.0713(6) 1.250000 0.3639(3) 0.077(2) Uani 1 2 d S T P . . H3A H -0.051181 1.212715 0.333265 0.115 Uiso 0.5 1 d R U P . . H3B H -0.127407 1.287285 0.354879 0.115 Uiso 0.5 1 d R U P . . O4 O -0.0946(6) 1.1611(4) 0.4834(3) 0.119(2) Uani 1 1 d . . . . . H4A H -0.081658 1.103850 0.477689 0.178 Uiso 1 1 d R U . . . H4B H -0.154489 1.178250 0.502996 0.178 Uiso 1 1 d R U . . . O5 O 0.0811(4) 1.250000 0.5446(2) 0.0332(12) Uani 1 2 d S T P . . H5A H 0.057726 1.200492 0.566517 0.050 Uiso 0.5 1 d R U P . . H5B H 0.057726 1.299508 0.566517 0.050 Uiso 0.5 1 d R U P . . O6 O 0.4172(6) 1.250000 0.5486(4) 0.081(2) Uani 1 2 d S T P . . H6A H 0.451380 1.212690 0.523089 0.122 Uiso 0.5 1 d R U P . . H6B H 0.456887 1.287310 0.574547 0.122 Uiso 0.5 1 d R U P . . O7 O 0.5702(5) 1.0078(5) 0.4242(4) 0.134(3) Uani 1 1 d . . . . . O8 O 0.5410(4) 0.8990(3) 0.3619(2) 0.0670(14) Uani 1 1 d . . . . . H8 H 0.603900 0.889207 0.371937 0.101 Uiso 1 1 d R U . . . O9 O 0.1923(4) 0.9339(3) 0.2577(2) 0.0583(13) Uani 1 1 d . . . . . O10 O 0.1965(4) 1.0307(2) 0.1414(2) 0.0493(11) Uani 1 1 d . . . . . O11 O 0.3625(4) 1.0349(2) 0.0983(2) 0.0491(11) Uani 1 1 d . . . . . O12 O -0.0564(3) 0.8250(2) 0.19499(19) 0.0466(11) Uani 1 1 d . . . . . O13 O 0.3933(3) 1.1753(2) 0.95993(18) 0.0405(10) Uani 1 1 d . . . . . O14 O 0.4108(3) 1.0727(2) 0.83329(18) 0.0493(11) Uani 1 1 d . . . . . O15 O 0.1537(4) 0.8280(2) 0.8220(2) 0.0714(16) Uani 1 1 d . . . . . H15 H 0.115211 0.786561 0.824424 0.107 Uiso 1 1 calc R U . . . O16 O 0.0451(4) 0.8540(3) 0.7383(2) 0.0710(15) Uani 1 1 d . . . . . O17 O 0.0930(4) 1.1252(3) 0.6236(2) 0.0668(15) Uani 1 1 d . . . . . O18 O 0.2627(3) 1.1599(2) 0.61896(18) 0.0421(10) Uani 1 1 d . . . . . O19 O -0.2074(10) 1.0252(7) 0.4499(7) 0.087(4) Uani 0.5 1 d D . P . . Co1 Co 0.25040(9) 1.250000 0.54739(5) 0.0342(3) Uani 1 2 d S T P . . Co2 Co 0.00895(9) 1.250000 0.45232(5) 0.0401(3) Uani 1 2 d S T P . . H19B H -0.229(14) 1.072(7) 0.472(7) 0.11(7) Uiso 0.5 1 d D . P . . H19A H -0.273(5) 1.016(7) 0.428(5) 0.04(3) Uiso 0.5 1 d D . P . . 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 C1 0.048(4) 0.051(3) 0.038(4) -0.012(3) -0.002(3) 0.005(3) C2 0.040(4) 0.052(3) 0.038(4) -0.011(3) -0.003(3) 0.010(3) C3 0.046(4) 0.062(4) 0.041(4) -0.014(3) -0.002(3) 0.008(3) C4 0.052(5) 0.054(4) 0.042(4) -0.013(3) -0.003(3) 0.014(3) C5 0.050(5) 0.071(4) 0.047(4) -0.022(3) 0.001(3) 0.024(4) C6 0.053(5) 0.064(4) 0.048(4) -0.014(3) -0.003(3) 0.013(4) C7 0.054(5) 0.069(4) 0.045(4) -0.021(3) -0.007(4) 0.010(4) C8 0.044(5) 0.090(5) 0.063(5) -0.023(4) -0.022(4) 0.014(4) C9 0.047(4) 0.056(4) 0.035(4) -0.018(3) -0.003(3) 0.014(3) C10 0.040(4) 0.050(3) 0.030(3) -0.008(3) -0.004(3) 0.008(3) C11 0.036(4) 0.040(3) 0.036(3) 0.001(3) 0.005(3) 0.010(3) C12 0.031(3) 0.043(3) 0.030(3) -0.001(2) 0.001(3) 0.009(3) C13 0.037(4) 0.033(3) 0.028(3) -0.001(2) -0.005(3) 0.009(3) C14 0.031(3) 0.034(3) 0.040(4) 0.000(2) -0.003(3) 0.012(3) C15 0.030(3) 0.040(3) 0.041(4) -0.008(3) -0.001(3) 0.005(3) C16 0.051(5) 0.056(4) 0.051(4) -0.023(3) -0.007(4) -0.010(3) C17 0.035(4) 0.035(3) 0.034(3) 0.008(2) 0.001(3) -0.002(3) C18 0.030(3) 0.038(3) 0.027(3) 0.006(2) -0.004(3) -0.013(3) C19 0.025(3) 0.041(3) 0.028(3) 0.008(2) 0.001(3) -0.002(3) C20 0.036(4) 0.036(3) 0.021(3) 0.013(2) -0.001(3) -0.005(3) C21 0.034(4) 0.033(3) 0.028(3) 0.005(2) -0.002(3) -0.007(3) C22 0.034(3) 0.032(3) 0.026(3) 0.008(2) 0.002(3) -0.002(2) C23 0.036(4) 0.040(3) 0.035(3) 0.007(3) -0.006(3) 0.006(3) C24 0.044(4) 0.053(4) 0.043(4) 0.017(3) -0.005(3) 0.012(3) C25 0.037(5) 0.046(4) 0.031(5) 0.000 -0.010(4) 0.000 C26 0.047(6) 0.053(5) 0.034(5) 0.000 -0.014(4) 0.000 C27 0.064(7) 0.069(6) 0.027(5) 0.000 0.010(5) 0.000 C28 0.033(5) 0.053(5) 0.022(4) 0.000 -0.001(4) 0.000 C29 0.061(7) 0.058(5) 0.031(5) 0.000 -0.003(4) 0.000 C30 0.035(5) 0.060(5) 0.029(5) 0.000 -0.013(4) 0.000 C31 0.049(4) 0.043(3) 0.035(3) 0.007(3) -0.004(3) -0.014(3) C32 0.044(4) 0.042(3) 0.032(3) 0.004(3) -0.005(3) -0.007(3) C33 0.057(4) 0.036(3) 0.031(3) 0.002(2) -0.006(3) -0.003(3) C34 0.049(4) 0.031(3) 0.042(4) -0.003(3) -0.003(3) 0.000(3) C35 0.041(4) 0.035(3) 0.043(4) -0.002(3) -0.009(3) 0.000(3) C36 0.039(4) 0.044(3) 0.034(3) 0.003(3) -0.003(3) 0.002(3) C37 0.051(4) 0.043(3) 0.042(4) 0.007(3) 0.002(3) -0.012(3) C38 0.034(4) 0.045(3) 0.045(4) 0.008(3) -0.005(3) -0.003(3) C39 0.069(5) 0.039(3) 0.041(4) 0.001(3) -0.011(4) -0.006(3) O1 0.076(4) 0.114(4) 0.064(3) -0.052(3) -0.020(3) 0.034(3) O2 0.062(3) 0.100(4) 0.077(4) -0.043(3) -0.019(3) 0.032(3) O3 0.053(5) 0.120(6) 0.056(5) 0.000 -0.009(4) 0.000 O4 0.102(5) 0.134(5) 0.119(5) 0.023(4) -0.003(4) -0.069(4) O5 0.037(3) 0.039(3) 0.023(3) 0.000 -0.001(2) 0.000 O6 0.046(5) 0.118(6) 0.077(6) 0.000 -0.014(4) 0.000 O7 0.063(4) 0.179(7) 0.153(7) -0.090(6) -0.047(4) 0.039(4) O8 0.053(3) 0.082(3) 0.065(3) -0.010(3) -0.002(3) 0.026(3) O9 0.055(3) 0.070(3) 0.047(3) -0.029(2) -0.015(2) 0.024(2) O10 0.047(3) 0.036(2) 0.063(3) -0.019(2) -0.004(2) 0.000(2) O11 0.050(3) 0.037(2) 0.059(3) -0.014(2) -0.001(2) -0.0033(19) O12 0.046(3) 0.056(2) 0.039(3) -0.005(2) 0.011(2) 0.001(2) O13 0.026(2) 0.056(2) 0.039(2) 0.0030(19) -0.0008(18) -0.0062(19) O14 0.055(3) 0.058(2) 0.033(2) 0.0154(19) -0.013(2) -0.020(2) O15 0.118(5) 0.036(2) 0.055(3) 0.013(2) -0.028(3) -0.025(3) O16 0.093(4) 0.059(3) 0.057(3) 0.011(2) -0.025(3) -0.033(3) O17 0.042(3) 0.078(3) 0.078(4) 0.045(3) -0.007(3) -0.010(2) O18 0.038(3) 0.049(2) 0.038(2) 0.0121(19) -0.004(2) 0.001(2) O19 0.069(8) 0.073(7) 0.112(10) 0.018(7) -0.034(8) -0.008(7) Co1 0.0324(7) 0.0466(6) 0.0231(6) 0.000 -0.0019(5) 0.000 Co2 0.0365(7) 0.0475(6) 0.0353(7) 0.000 -0.0029(5) 0.000 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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' 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 O1 C1 O2 124.5(6) . . ? O1 C1 C2 115.7(6) . . ? O2 C1 C2 119.8(6) . . ? C7 C2 C3 119.4(6) . . ? C7 C2 C1 120.0(5) . . ? C3 C2 C1 120.6(6) . . ? C4 C3 C2 119.2(6) . . ? C5 C4 O9 114.7(5) . . ? C5 C4 C3 120.8(6) . . ? O9 C4 C3 124.5(6) . . ? C4 C5 C6 120.7(6) . . ? C7 C6 C5 119.0(6) . . ? C7 C6 C8 121.0(6) . . ? C5 C6 C8 120.0(6) . . ? C6 C7 C2 120.8(6) . . ? O7 C8 O8 124.0(7) . . ? O7 C8 C6 121.9(7) . . ? O8 C8 C6 114.1(6) . . ? O9 C9 C10 104.7(5) . . ? C15 C10 C11 118.6(5) . . ? C15 C10 C9 120.0(6) . . ? C11 C10 C9 121.3(6) . . ? C10 C11 C12 121.1(5) . . ? C10 C11 O12 119.4(5) . . ? C12 C11 O12 119.3(5) . . ? C13 C12 C11 118.0(5) . . ? C13 C12 C25 121.8(5) . . ? C11 C12 C25 120.0(6) . . ? C12 C13 C14 122.5(5) . . ? C15 C14 C13 116.9(5) . . ? C15 C14 C23 121.2(5) . . ? C13 C14 C23 121.9(5) . . ? C10 C15 C14 122.9(5) . . ? C10 C15 O10 117.4(5) . . ? C14 C15 O10 119.6(5) . . ? O10 C16 O11 112.6(5) . . ? C18 C17 C22 121.7(5) 3_676 . ? C18 C17 O11 118.2(5) 3_676 . ? C22 C17 O11 120.0(5) . . ? C19 C18 C17 118.6(5) . 3_676 ? C19 C18 C31 119.8(5) . . ? C17 C18 C31 121.5(5) 3_676 . ? C18 C19 C20 121.6(5) . . ? C18 C19 O13 118.3(5) . . ? C20 C19 O13 120.0(5) . . ? C21 C20 C19 117.9(5) . . ? C21 C20 C28 123.1(5) . . ? C19 C20 C28 119.0(6) . . ? C20 C21 C22 122.7(5) . 3_676 ? C21 C22 C17 117.3(5) 3_676 . ? C21 C22 C23 123.5(5) 3_676 . ? C17 C22 C23 119.1(5) . . ? C22 C23 C24 113.9(5) . . ? C22 C23 C14 108.3(4) . . ? C24 C23 C14 112.8(5) . . ? C26 C25 C12 114.5(4) . . ? C26 C25 C12 114.5(4) . 4_575 ? C12 C25 C12 106.1(6) . 4_575 ? O12 C27 O12 114.1(7) 4_575 . ? C29 C28 C20 113.4(4) . . ? C29 C28 C20 113.4(4) . 4_585 ? C20 C28 C20 105.3(6) . 4_585 ? O13 C30 O13 113.6(6) . 4_585 ? O14 C31 C18 111.9(5) . . ? C33 C32 O14 125.2(5) . . ? C33 C32 C37 119.8(5) . . ? O14 C32 C37 115.0(5) . . ? C32 C33 C34 120.5(5) . . ? C35 C34 C33 120.5(5) . . ? C35 C34 C39 118.8(5) . . ? C33 C34 C39 120.7(5) . . ? C34 C35 C36 119.3(5) . . ? C37 C36 C35 119.9(5) . . ? C37 C36 C38 120.6(5) . . ? C35 C36 C38 119.5(5) . . ? C36 C37 C32 119.9(5) . . ? O17 C38 O18 124.6(6) . . ? O17 C38 C36 118.3(6) . . ? O18 C38 C36 117.2(5) . . ? O16 C39 O15 124.7(6) . . ? O16 C39 C34 119.5(6) . . ? O15 C39 C34 115.8(6) . . ? C1 O1 Co1 140.5(5) . . ? C1 O2 Co2 133.0(4) . . ? Co2 O5 Co1 112.8(2) . . ? C4 O9 C9 119.3(5) . . ? C16 O10 C15 116.7(4) . . ? C17 O11 C16 115.1(4) . . ? C11 O12 C27 117.3(6) . . ? C19 O13 C30 115.8(5) . . ? C32 O14 C31 115.6(4) . . ? C38 O18 Co1 127.9(4) . . ? O1 Co1 O1 94.3(4) 4_585 . ? O1 Co1 O18 175.20(19) 4_585 . ? O1 Co1 O18 89.7(2) . . ? O1 Co1 O18 89.7(2) 4_585 4_585 ? O1 Co1 O18 175.20(19) . 4_585 ? O18 Co1 O18 86.2(2) . 4_585 ? O1 Co1 O6 89.0(2) 4_585 . ? O1 Co1 O6 89.0(2) . . ? O18 Co1 O6 88.4(2) . . ? O18 Co1 O6 88.4(2) 4_585 . ? O1 Co1 O5 90.35(19) 4_585 . ? O1 Co1 O5 90.35(19) . . ? O18 Co1 O5 92.28(15) . . ? O18 Co1 O5 92.28(15) 4_585 . ? O6 Co1 O5 179.1(3) . . ? O2 Co2 O2 93.1(4) . 4_585 ? O2 Co2 O4 175.8(3) . 4_585 ? O2 Co2 O4 90.4(3) 4_585 4_585 ? O2 Co2 O4 90.4(3) . . ? O2 Co2 O4 175.8(3) 4_585 . ? O4 Co2 O4 86.1(5) 4_585 . ? O2 Co2 O3 86.9(2) . . ? O2 Co2 O3 86.9(2) 4_585 . ? O4 Co2 O3 90.9(2) 4_585 . ? O4 Co2 O3 90.9(2) . . ? O2 Co2 O5 95.56(18) . . ? O2 Co2 O5 95.57(18) 4_585 . ? O4 Co2 O5 86.5(2) 4_585 . ? O4 Co2 O5 86.5(2) . . ? O3 Co2 O5 176.4(3) . . ? 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 C1 O1 1.226(7) . ? C1 O2 1.231(8) . ? C1 C2 1.486(8) . ? C2 C7 1.381(9) . ? C2 C3 1.385(8) . ? C3 C4 1.377(9) . ? C4 C5 1.357(9) . ? C4 O9 1.373(7) . ? C5 C6 1.379(9) . ? C6 C7 1.372(9) . ? C6 C8 1.476(10) . ? C8 O7 1.193(8) . ? C8 O8 1.287(8) . ? C9 O9 1.428(7) . ? C9 C10 1.505(8) . ? C10 C15 1.363(8) . ? C10 C11 1.380(8) . ? C11 C12 1.387(8) . ? C11 O12 1.387(7) . ? C12 C13 1.373(8) . ? C12 C25 1.524(7) . ? C13 C14 1.388(8) . ? C14 C15 1.374(8) . ? C14 C23 1.526(8) . ? C15 O10 1.408(7) . ? C16 O10 1.388(8) . ? C16 O11 1.434(8) . ? C17 C18 1.378(8) 3_676 ? C17 C22 1.391(8) . ? C17 O11 1.403(7) . ? C18 C19 1.377(8) . ? C18 C31 1.489(8) . ? C19 C20 1.382(7) . ? C19 O13 1.387(6) . ? C20 C21 1.378(8) . ? C20 C28 1.540(7) . ? C21 C22 1.377(7) 3_676 ? C22 C23 1.514(8) . ? C23 C24 1.525(8) . ? C25 C26 1.510(11) . ? C27 O12 1.415(6) 4_575 ? C27 O12 1.415(6) . ? C28 C29 1.514(11) . ? C30 O13 1.412(6) . ? C30 O13 1.412(6) 4_585 ? C31 O14 1.405(6) . ? C32 C33 1.363(8) . ? C32 O14 1.368(7) . ? C32 C37 1.398(8) . ? C33 C34 1.386(8) . ? C34 C35 1.378(8) . ? C34 C39 1.493(9) . ? C35 C36 1.396(8) . ? C36 C37 1.384(8) . ? C36 C38 1.477(8) . ? C38 O17 1.242(7) . ? C38 O18 1.263(7) . ? C39 O16 1.223(7) . ? C39 O15 1.267(7) . ? O1 Co1 2.024(5) . ? O2 Co2 2.041(5) . ? O3 Co2 2.072(7) . ? O4 Co2 2.062(6) . ? O5 Co2 2.106(5) . ? O5 Co1 2.129(5) . ? O6 Co1 2.099(7) . ? O18 Co1 2.087(4) . ?