#------------------------------------------------------------------------------ #$Date: 2023-02-20 11:10:25 +0200 (Mon, 20 Feb 2023) $ #$Revision: 280970 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/62/7246239.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_7246239 loop_ _publ_author_name 'Tang, Wenlei' 'Shao, Zhen-Wu' 'Xiong, Li' 'Zhang, Zhiyuan' 'Tan, Kaiyuan' 'Feng, Xuan' 'Wu, Wenjing' 'Liu, Chong' _publ_section_title ; A siderophore-inspired two-dimensional Fe--hydroxamate metal--organic framework ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D3CE00022B _journal_year 2023 _chemical_formula_moiety 'C12 H12 Fe2 N6 O12' _chemical_formula_sum 'C12 H12 Fe2 N6 O12' _chemical_formula_weight 543.98 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2021-10-09 _audit_creation_method ; Olex2 1.5 (compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405) ; _audit_update_record ; 2022-12-01 deposited with the CCDC. 2023-02-10 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 111.89(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.635(18) _cell_length_b 21.87(2) _cell_length_c 17.252(18) _cell_measurement_reflns_used 711 _cell_measurement_temperature 193.00 _cell_measurement_theta_max 46.38 _cell_measurement_theta_min 8.73 _cell_volume 4774(9) _computing_cell_refinement 'SAINT V8.40B (Bruker, 2019)' _computing_data_collection 'Bruker BIS V6.2.14' _computing_data_reduction 'SAINT V8.40B (Bruker, 2019)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 193.00 _diffrn_detector CPAD _diffrn_detector_area_resol_mean 7.41 _diffrn_detector_type 'Bruker PHOTON III' _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.946 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 VENTURE Metaljet PHOTON III' _diffrn_measurement_method '\w and \f shutterless scans' _diffrn_measurement_specimen_support 'nylon loop' _diffrn_radiation_monochromator 'Helios Multi-layer Optic' _diffrn_radiation_probe x-ray _diffrn_radiation_type GaK\a _diffrn_radiation_wavelength 1.34139 _diffrn_reflns_av_R_equivalents 0.0877 _diffrn_reflns_av_unetI/netI 0.1073 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.946 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 15851 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.946 _diffrn_reflns_theta_full 53.594 _diffrn_reflns_theta_max 60.797 _diffrn_reflns_theta_min 3.511 _diffrn_source MetalJet _diffrn_source_current 2.86 _diffrn_source_power 0.19937059999999998 _diffrn_source_type 'Liquid Metal source' _diffrn_source_voltage 69.71 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.568 _exptl_absorpt_correction_T_max 0.7518 _exptl_absorpt_correction_T_min 0.4287 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1384 before and 0.0928 after correction. The Ratio of minimum to maximum transmission is 0.5702. The \l/2 correction factor is Not present. ; _exptl_crystal_density_diffrn 0.757 _exptl_crystal_description block _exptl_crystal_F_000 1096 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.543 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.092 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 191 _refine_ls_number_reflns 5217 _refine_ls_number_restraints 139 _refine_ls_restrained_S_all 0.956 _refine_ls_R_factor_all 0.1491 _refine_ls_R_factor_gt 0.0922 _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^)+(0.1817P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2820 _refine_ls_wR_factor_ref 0.3227 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2130 _reflns_number_total 5217 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ce00022b2.cif _cod_data_source_block SUM-31 _cod_depositor_comments ; The following automatic conversions were performed: data item '_diffrn_radiation_probe' value 'X-ray' was changed to 'x-ray' 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_cell_volume 4773(10) _cod_database_code 7246239 _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_max 0.717 _shelx_estimated_absorpt_t_min 0.674 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups 2. Restrained distances C6B-C6B_$1 \\sim C6A-C6A_$1 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints O2B \\sim O1B \\sim N3B \\sim C5B \\sim C6B \\sim C6A \\sim C5A \\sim O1A \\sim N3A \\sim O2A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A 4. Others Sof(O2B)=Sof(O1B)=Sof(N3B)=Sof(H3B)=Sof(C5B)=Sof(C6B)=Sof(H6B)=1-FVAR(1) Sof(C6A)=Sof(H6A)=Sof(C5A)=Sof(O1A)=Sof(N3A)=Sof(H3A)=Sof(O2A)=FVAR(1) 5.a Aromatic/amide H refined with riding coordinates: N2(H2), N3B(H3B), N1(H1), C3(H3), C2(H2A), C6B(H6B), C6A(H6A), N3A(H3A) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL a1_a.res in C2/c a1.res created by SHELXL-2018/3 at 09:36:29 on 09-Oct-2021 REM Old TITL A1 in C2/c REM SHELXT solution in C2/c: R1 0.335, Rweak 0.047, Alpha 0.088 REM 0.491 for 113 systematic absences, Orientation as input REM Formula found by SHELXT: C21 N6 O12 Fe2 CELL 1.34139 13.6352 21.8687 17.2523 90 111.891 90 ZERR 4 0.0177 0.0236 0.0181 0 0.051 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Fe N O DISP C 0.0137 0.0067 57.1 DISP Fe -0.2673 2.555 19450.3 DISP H 0 0 0.6 DISP N 0.0241 0.0134 109.9 DISP O 0.0389 0.0241 193.4 UNIT 48 48 8 24 48 EQIV $1 1.5-X,1.5-Y,-Z SIMU 0.01 0.02 2 O2B O1B N3B C5B C6B C6A C5A O1A N3A O2A SADI C6B C6B_$1 C6A C6A_$1 L.S. 20 PLAN 25 SIZE 0.1 0.12 0.1 TEMP -80.15 CONF BOND list 4 MORE -1 ABIN BOND $H fmap 2 acta SIZE 0.1 0.12 0.1 OMIT 1 5 2 OMIT 0 0 8 OMIT 0 2 4 REM REM REM WGHT 0.181700 FVAR 0.28258 0.45967 FE1 3 0.807207 0.547747 0.035620 11.00000 0.09448 0.10224 = 0.04683 0.00511 0.03300 0.02062 O4 5 0.831068 0.542365 0.156567 11.00000 0.08171 0.09660 = 0.04916 0.00250 0.03114 0.00520 O6 5 0.894709 0.523804 0.542341 11.00000 0.08483 0.08772 = 0.04273 -0.00764 0.02516 -0.01260 O5 5 0.765033 0.470747 0.413728 11.00000 0.10082 0.13596 = 0.04377 -0.02040 0.03081 -0.05807 PART 2 O2B 5 0.934121 0.591134 0.042321 -21.00000 0.08438 0.05087 = 0.05699 -0.00911 0.02753 0.00821 PART 0 N2 4 0.895171 0.538196 0.466493 11.00000 0.08555 0.07741 = 0.04845 0.00361 0.03147 -0.00054 AFIX 43 H2 2 0.939156 0.565662 0.460765 11.00000 -1.20000 AFIX 0 PART 2 O1B 5 0.734608 0.624646 0.004492 -21.00000 0.10155 0.06128 = 0.05698 0.00249 0.03426 0.01122 PART 0 O3 5 0.669726 0.514203 0.028977 11.00000 0.08494 0.20374 = 0.04033 0.00604 0.02122 0.01964 PART 2 N3B 4 0.901804 0.655580 0.025168 -21.00000 0.10526 0.05440 = 0.05529 -0.00640 0.02903 0.00329 AFIX 43 H3B 2 0.948283 0.682177 0.021446 -21.00000 -1.20000 AFIX 0 PART 0 N1 4 0.672652 0.502871 0.107153 11.00000 0.08833 0.22673 = 0.04326 -0.00431 0.03455 -0.00682 AFIX 43 H1 2 0.618392 0.485820 0.114642 11.00000 -1.20000 AFIX 0 C4 1 0.828692 0.510197 0.402546 11.00000 0.08596 0.09416 = 0.03638 -0.00771 0.01605 -0.00421 PART 2 C5B 1 0.816497 0.673135 0.016201 -21.00000 0.10608 0.05531 = 0.05460 -0.00537 0.03322 0.00796 PART 0 C3 1 0.831503 0.525274 0.320932 11.00000 0.08296 0.07767 = 0.04281 -0.00134 0.02471 -0.01602 AFIX 43 H3 2 0.887662 0.549062 0.316822 11.00000 -1.20000 AFIX 0 C1 1 0.754875 0.517265 0.169204 11.00000 0.08593 0.11645 = 0.03339 0.00430 0.01470 0.00134 C2 1 0.753023 0.504886 0.251304 11.00000 0.09173 0.13023 = 0.04924 0.01025 0.02565 -0.01429 AFIX 43 H2A 2 0.696130 0.482244 0.256165 11.00000 -1.20000 AFIX 0 PART 2 C6B 1 0.787215 0.729460 0.000224 -21.00000 0.11142 0.05619 = 0.05672 -0.01650 0.04444 0.01413 AFIX 43 H6B 2 0.836455 0.749586 -0.018089 -21.00000 -1.20000 AFIX 0 PART 1 C6A 1 0.804145 0.747336 0.019514 21.00000 0.11538 0.04826 = 0.05938 -0.01526 0.03809 0.01366 AFIX 43 H6A 2 0.848733 0.782286 0.033198 21.00000 -1.20000 AFIX 0 C5A 1 0.847104 0.685573 0.038826 21.00000 0.10872 0.05562 = 0.05936 -0.00670 0.03391 0.01008 O1A 5 0.770963 0.645236 0.020284 21.00000 0.10764 0.05703 = 0.05531 -0.00511 0.03369 0.01570 N3A 4 0.931519 0.662447 0.053491 21.00000 0.10040 0.05757 = 0.05440 -0.00303 0.03463 0.00201 AFIX 43 H3A 2 0.985643 0.686414 0.059276 21.00000 -1.20000 AFIX 0 O2A 5 0.947759 0.603769 0.061370 21.00000 0.09564 0.05871 = 0.05463 -0.01531 0.03552 0.01046 HKLF 4 REM a1_a.res in C2/c REM wR2 = 0.3227, GooF = S = 0.965, Restrained GooF = 0.956 for all data REM R1 = 0.0922 for 2130 Fo > 4sig(Fo) and 0.1491 for all 5217 data REM 191 parameters refined using 139 restraints END WGHT 0.1817 0.0000 REM Highest difference peak 0.543, deepest hole -0.715, 1-sigma level 0.092 Q1 1 0.5547 0.5169 0.0196 11.00000 0.05 0.54 Q2 1 0.8133 0.5027 0.0353 11.00000 0.05 0.42 Q3 1 0.8000 0.5894 0.0376 11.00000 0.05 0.39 Q4 1 0.8986 0.5492 0.0707 11.00000 0.05 0.38 Q5 1 0.6862 0.5717 -0.0148 11.00000 0.05 0.35 Q6 1 0.6474 0.5077 0.2212 11.00000 0.05 0.34 Q7 1 0.9136 0.4853 0.5416 11.00000 0.05 0.32 Q8 1 0.6859 0.4503 0.2103 11.00000 0.05 0.31 Q9 1 1.0357 0.5298 0.5530 11.00000 0.05 0.30 Q10 1 0.6773 0.5278 0.0004 11.00000 0.05 0.28 Q11 1 0.8385 0.5848 0.3132 11.00000 0.05 0.27 Q12 1 0.8396 0.6812 0.0959 11.00000 0.05 0.26 Q13 1 0.8599 0.4824 0.1633 11.00000 0.05 0.25 Q14 1 1.0025 0.6640 0.0844 11.00000 0.05 0.23 Q15 1 0.8980 0.5112 0.4586 11.00000 0.05 0.23 Q16 1 0.6780 0.5584 0.0383 11.00000 0.05 0.22 Q17 1 0.7172 0.5147 0.3409 11.00000 0.05 0.21 Q18 1 0.9050 0.7022 0.0435 11.00000 0.05 0.21 Q19 1 1.0037 0.5959 0.0852 11.00000 0.05 0.21 Q20 1 0.8357 0.5689 0.3893 11.00000 0.05 0.20 Q21 1 0.8308 0.5361 0.4298 11.00000 0.05 0.17 Q22 1 0.9144 0.6007 0.4660 11.00000 0.05 0.17 Q23 1 0.8007 0.4505 0.2385 11.00000 0.05 0.17 Q24 1 1.0000 0.6979 0.2500 10.50000 0.05 0.17 Q25 1 0.9472 0.5321 0.3122 11.00000 0.05 0.17 ; _shelx_res_checksum 87149 _shelx_fab_file ; -17 1 3 3.0288 0.0058 -17 1 4 1.5885 -0.4935 -17 1 5 2.2373 0.1360 -17 1 6 -0.8089 -0.4578 -17 1 7 1.8644 0.0578 -17 1 8 -0.8013 -0.4166 -17 1 9 -3.7483 -0.0878 -17 1 10 2.6041 -0.1978 -17 3 3 -4.0814 -0.1147 -17 3 4 1.9587 -0.2134 -17 3 5 3.8445 0.0371 -17 3 6 1.1028 -0.1241 -17 3 7 -0.7608 -0.0149 -17 3 8 1.6615 -0.0386 -17 3 9 2.7810 -0.0563 -17 3 10 -0.4606 0.1038 -17 3 11 3.5283 -0.0742 -17 5 4 -4.3080 0.0499 -17 5 5 -0.2725 -0.1374 -17 5 6 -3.7658 0.1705 -17 5 7 1.6029 -0.0968 -17 5 8 -4.5371 0.2115 -17 5 9 -0.8020 -0.0441 -17 5 10 3.6413 0.2109 -17 5 11 5.1968 0.1376 -17 7 6 -2.8641 0.3805 -17 7 7 3.1053 -0.0297 -17 7 8 7.0932 0.3191 -17 7 9 -2.8062 0.0901 -16 0 2 -0.7751 -0.5165 -16 0 4 -1.1491 -0.1016 -16 0 6 4.1722 0.3458 -16 0 8 2.2285 0.6391 -16 0 10 4.6038 0.9115 -16 0 12 1.8116 1.0606 -16 0 14 -0.4037 0.8649 -16 2 1 -2.6181 -0.0322 -16 2 2 3.3216 0.1687 -16 2 3 2.2131 -0.0778 -16 2 4 0.9395 0.0866 -16 2 5 2.4910 -0.1503 -16 2 6 -1.3044 0.1651 -16 2 7 0.2757 -0.1702 -16 2 8 -4.9754 0.1322 -16 2 9 -1.2003 -0.1395 -16 2 10 -2.3566 0.1233 -16 2 11 1.7218 -0.0014 -16 2 12 2.5522 0.1702 -16 2 13 2.7535 0.0506 -16 2 14 5.0843 0.1429 -16 2 15 3.7429 -0.1036 -16 4 1 3.4094 -0.0470 -16 4 2 -4.4493 0.1840 -16 4 3 -2.4693 -0.1648 -16 4 4 3.3121 0.0381 -16 4 5 -0.7083 -0.1504 -16 4 6 -3.5959 0.0954 -16 4 7 4.6041 -0.0960 -16 4 8 4.2217 0.0022 -16 4 9 -0.5200 -0.0193 -16 4 10 1.6500 -0.0783 -16 4 11 6.1365 0.1116 -16 4 12 -0.3458 0.0110 -16 4 13 -3.4610 0.1457 -16 4 14 -5.2884 -0.0208 -16 4 15 1.7301 -0.1698 -16 6 1 -1.1505 0.0078 -16 6 2 -0.5042 0.2162 -16 6 3 1.2029 -0.0545 -16 6 4 2.7974 -0.0130 -16 6 5 -1.2350 -0.0140 -16 6 6 -3.1983 -0.0134 -16 6 7 -2.2760 0.0818 -16 6 8 -0.3756 -0.0309 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-15 1 9 -1.2263 0.3777 -15 1 10 0.2843 -0.1086 -15 1 11 -0.8636 0.4852 -15 1 12 2.3313 -0.3687 -15 1 13 3.6315 0.5616 -15 1 14 0.0617 -0.6414 -15 1 15 2.0724 0.2838 -15 1 16 -0.5359 -0.9222 -15 3 1 0.3853 -0.1341 -15 3 2 1.6905 0.2047 -15 3 3 -1.8122 -0.0455 -15 3 4 2.6747 0.0717 -15 3 5 1.0493 0.1898 -15 3 6 1.9592 -0.0875 -15 3 7 -3.2107 0.3834 -15 3 8 5.1481 -0.1247 -15 3 9 2.8525 0.5084 -15 3 10 -6.0279 -0.2745 -15 3 11 3.1346 0.5991 -15 3 12 2.9320 -0.1795 -15 3 13 0.3925 0.4848 -15 3 14 -0.1159 -0.2758 -15 3 15 3.8540 0.0996 -15 3 16 -1.9059 -0.4362 -15 3 17 -0.7305 0.0782 -15 5 1 1.2678 0.0354 -15 5 2 -1.4435 0.1129 -15 5 3 -3.6614 0.1041 -15 5 4 0.8990 -0.0733 -15 5 5 0.5926 0.2125 -15 5 6 -1.7072 -0.2459 -15 5 7 1.8899 0.2993 -15 5 8 -4.4388 -0.1370 -15 5 9 -3.3666 0.3196 -15 5 10 3.1497 -0.1110 -15 5 11 1.5371 0.3268 -15 5 12 -2.2723 -0.0201 -15 5 13 0.4772 -0.0199 -15 5 14 2.6245 -0.0883 -15 5 15 -4.6868 -0.2772 -15 5 16 -1.6827 0.0294 -15 5 17 -2.4649 -0.1167 -15 7 1 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0.0516 12 2 6 5.8601 0.0370 12 2 7 3.6300 -0.0868 12 2 8 -3.5113 -0.2767 12 2 9 -0.9729 -0.1167 12 4 0 2.9826 0.0753 12 4 1 3.3962 0.1424 12 4 2 1.8229 0.3150 12 4 3 5.4927 0.1866 12 4 4 -2.8372 0.2831 12 4 5 -2.4432 0.3388 12 4 6 5.4394 0.1556 12 4 7 3.5795 0.1939 12 4 8 -1.0493 -0.0524 12 4 9 -10.5195 0.0352 12 6 0 1.3332 -0.1119 12 6 1 -7.3141 -0.0874 12 6 2 5.2698 0.1071 12 6 3 0.3427 0.1701 12 6 4 -6.3116 0.1550 12 6 5 1.8074 0.3745 12 6 6 -11.3725 0.1693 12 6 7 -3.8077 0.1731 12 6 8 6.6975 0.3697 12 8 0 -0.3479 -0.2808 12 8 1 4.3601 -0.3321 12 8 2 -7.3471 -0.1787 12 8 3 2.2700 -0.0299 12 8 4 0.6822 -0.0770 12 8 5 -4.0001 0.1141 12 8 6 4.0195 0.0147 12 8 7 -2.7268 -0.0215 12 8 8 -0.3715 0.4929 12 10 0 -4.1023 -0.2238 12 10 1 -3.1254 -0.3379 12 10 2 -0.4684 -0.2677 12 10 3 -4.2098 -0.1324 12 10 4 7.3769 -0.1436 12 10 5 -0.2424 -0.1336 12 10 6 -4.1262 0.0692 12 10 7 0.5790 -0.2373 12 12 0 5.0101 -0.1003 12 12 1 1.5187 -0.2104 12 12 2 3.9312 -0.1779 12 12 3 3.9543 -0.0509 12 12 4 -5.4270 -0.0819 12 12 5 0.6910 -0.0697 12 12 6 0.1348 0.0908 12 14 0 1.9265 0.0799 12 14 1 -11.2872 0.0457 12 14 2 -4.7832 0.0839 12 14 3 3.8079 0.1229 12 14 4 1.6029 0.0844 12 14 5 1.3830 0.0702 12 16 0 1.2400 0.1277 12 16 1 0.6944 0.3102 12 16 2 3.9059 0.1816 12 16 3 -4.7208 0.5434 12 18 0 0.2173 0.0803 13 1 0 2.2067 -0.6109 13 1 1 3.6888 -0.2594 13 1 2 1.8861 -0.6260 13 1 3 -7.3512 -0.4243 13 1 4 -3.1257 -0.4742 13 1 5 -0.8895 -0.3763 13 1 6 -1.3270 -0.3288 13 1 7 -4.4662 -0.3632 13 3 0 -2.5020 -0.1113 13 3 1 4.8672 0.0324 13 3 2 1.2677 -0.1840 13 3 3 4.1797 -0.2722 13 3 4 6.5276 -0.0889 13 3 5 2.1686 -0.3463 13 3 6 -3.9728 -0.1717 13 3 7 -6.9570 -0.1924 13 5 0 1.8640 0.2008 13 5 1 -1.4376 0.1225 13 5 2 4.2327 0.1762 13 5 3 -0.6213 0.0011 13 5 4 -2.7066 0.0609 13 5 5 -0.3010 -0.0153 13 5 6 -2.0697 -0.1429 13 5 7 8.8107 0.2376 13 7 0 0.3513 0.1514 13 7 1 -1.8431 0.1744 13 7 2 -1.7692 0.1558 13 7 3 0.9083 0.2138 13 7 4 0.4996 0.0661 13 7 5 2.4227 0.2080 13 7 6 1.2128 0.0247 13 9 0 -3.3505 -0.0011 13 9 1 -2.6367 0.0877 13 9 2 2.1340 0.0697 13 9 3 -5.8018 0.2191 13 9 4 1.5086 0.1723 13 9 5 1.4064 0.2770 13 9 6 -4.3888 0.2986 13 11 0 -1.0643 -0.1684 13 11 1 4.3878 -0.1361 13 11 2 -1.1449 -0.0857 13 11 3 3.8872 -0.0598 13 11 4 -3.4782 0.2367 13 11 5 -2.0489 -0.1491 13 13 0 0.6255 -0.2354 13 13 1 -5.6740 -0.2941 13 13 2 -3.2541 -0.2228 13 13 3 1.9048 -0.3460 13 13 4 4.7743 0.1439 13 15 0 -1.4692 -0.1602 13 15 1 -1.6615 -0.2604 13 15 2 2.4216 -0.1025 14 0 0 -6.8171 0.4312 14 0 2 3.8801 0.6324 14 0 4 3.8713 0.6062 14 2 0 -5.8069 -0.0669 14 2 1 -2.3446 -0.1232 14 2 2 7.4004 -0.0493 14 2 3 -0.0783 -0.0407 14 2 4 -1.3139 0.0182 14 2 5 -5.6235 0.1298 14 4 0 0.2072 -0.2836 14 4 1 -3.1503 -0.1747 14 4 2 0.5455 -0.2089 14 4 3 2.8406 -0.2211 14 4 4 -3.9505 -0.0961 14 4 5 -1.5466 -0.0485 14 6 0 5.0832 -0.1228 14 6 1 0.3956 -0.1326 14 6 2 -3.6870 -0.0947 14 6 3 -1.4254 -0.2272 14 6 4 5.4446 -0.2038 14 6 5 1.0662 -0.0173 14 8 0 2.2595 0.0603 14 8 1 -1.2220 0.0648 14 8 2 0.6132 -0.0366 14 8 3 -1.7801 0.0018 14 8 4 0.5375 -0.4242 14 10 0 -7.0508 0.1418 14 10 1 -2.2116 0.1597 14 10 2 -0.1083 -0.0012 14 10 3 1.6310 0.1679 14 12 0 2.6984 0.1713 14 12 1 1.6771 0.0600 14 12 2 -0.3065 0.0856 14 14 0 -1.7932 0.2184 15 1 0 -2.3602 0.4126 15 1 1 -0.1375 0.2292 15 1 2 4.8782 0.4558 15 1 3 4.0686 0.2826 15 3 0 -1.8122 0.1983 15 3 1 1.0900 0.2706 15 3 2 -6.9201 0.2921 15 3 3 -2.7163 0.1147 15 5 0 -0.0185 -0.0618 15 5 1 -0.5963 0.1428 15 5 2 -1.5436 -0.0077 15 5 3 -2.3516 -0.2706 15 7 0 8.3617 -0.2109 15 7 1 1.1089 -0.0967 15 7 2 1.7726 -0.2344 15 9 0 -6.5775 -0.2623 15 9 1 -0.7862 -0.0064 15 11 0 0.2724 -0.2493 16 0 0 5.1674 -0.7102 16 2 0 -1.3749 -0.0379 16 2 1 5.3293 -0.1575 16 4 0 -1.3611 0.2386 16 6 0 1.1442 0.4107 0 0 0 0.0 0.0 ; _shelx_fab_checksum 80581 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.80721(8) 0.54775(5) 0.03562(5) 0.0793(4) Uani 1 1 d . . . . . O4 O 0.8311(3) 0.54237(18) 0.1566(2) 0.0739(11) Uani 1 1 d . . . . . O6 O 0.8947(3) 0.52380(18) 0.5423(2) 0.0714(11) Uani 1 1 d . . . . . O5 O 0.7650(4) 0.4707(2) 0.4137(2) 0.0924(15) Uani 1 1 d . . . . . O2B O 0.9341(18) 0.5911(8) 0.0423(11) 0.064(3) Uani 0.540(19) 1 d . U P A 2 N2 N 0.8952(4) 0.5382(2) 0.4665(3) 0.0686(13) Uani 1 1 d . . . . . H2 H 0.939156 0.565662 0.460765 0.082 Uiso 1 1 calc R U . . . O1B O 0.7346(12) 0.6246(6) 0.0045(9) 0.072(3) Uani 0.540(19) 1 d . U P A 2 O3 O 0.6697(4) 0.5142(3) 0.0290(2) 0.1103(17) Uani 1 1 d . . . . . N3B N 0.9018(15) 0.6556(7) 0.0252(9) 0.072(3) Uani 0.540(19) 1 d . U P A 2 H3B H 0.948283 0.682177 0.021446 0.086 Uiso 0.540(19) 1 calc R U P A 2 N1 N 0.6727(5) 0.5029(4) 0.1072(3) 0.117(2) Uani 1 1 d . . . . . H1 H 0.618392 0.485820 0.114642 0.140 Uiso 1 1 calc R U . . . C4 C 0.8287(5) 0.5102(3) 0.4025(3) 0.0741(17) Uani 1 1 d . . . . . C5B C 0.8165(16) 0.6731(9) 0.0162(10) 0.071(3) Uani 0.540(19) 1 d . U P A 2 C3 C 0.8315(5) 0.5253(3) 0.3209(3) 0.0675(15) Uani 1 1 d . . . . . H3 H 0.887662 0.549062 0.316822 0.081 Uiso 1 1 calc R U . . . C1 C 0.7549(6) 0.5173(3) 0.1692(3) 0.0808(18) Uani 1 1 d . . . . . C2 C 0.7530(6) 0.5049(4) 0.2513(4) 0.091(2) Uani 1 1 d . . . . . H2A H 0.696130 0.482244 0.256165 0.109 Uiso 1 1 calc R U . . . C6B C 0.7872(11) 0.7295(7) 0.0002(10) 0.071(3) Uani 0.540(19) 1 d D U P A 2 H6B H 0.836455 0.749586 -0.018089 0.085 Uiso 0.540(19) 1 calc R U P A 2 C6A C 0.8041(8) 0.7473(9) 0.0195(11) 0.073(3) Uani 0.460(19) 1 d D U P A 1 H6A H 0.848733 0.782286 0.033198 0.087 Uiso 0.460(19) 1 calc R U P A 1 C5A C 0.8471(19) 0.6856(9) 0.0388(13) 0.074(3) Uani 0.460(19) 1 d . U P A 1 O1A O 0.7710(14) 0.6452(8) 0.0203(9) 0.072(3) Uani 0.460(19) 1 d . U P A 1 N3A N 0.9315(15) 0.6624(8) 0.0535(10) 0.069(3) Uani 0.460(19) 1 d . U P A 1 H3A H 0.985643 0.686414 0.059276 0.083 Uiso 0.460(19) 1 calc R U P A 1 O2A O 0.948(2) 0.6038(11) 0.0614(12) 0.067(3) Uani 0.460(19) 1 d . U P A 1 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 Fe1 0.0945(8) 0.1022(8) 0.0468(5) 0.0051(4) 0.0330(5) 0.0206(5) O4 0.082(3) 0.097(3) 0.049(2) 0.0025(19) 0.031(2) 0.005(2) O6 0.085(3) 0.088(3) 0.043(2) -0.0076(18) 0.025(2) -0.013(2) O5 0.101(3) 0.136(4) 0.044(2) -0.020(2) 0.031(2) -0.058(3) O2B 0.084(6) 0.051(6) 0.057(7) -0.009(4) 0.028(5) 0.008(5) N2 0.086(4) 0.077(3) 0.048(3) 0.004(2) 0.031(3) -0.001(3) O1B 0.102(6) 0.061(6) 0.057(5) 0.002(4) 0.034(5) 0.011(5) O3 0.085(3) 0.204(5) 0.040(2) 0.006(3) 0.021(2) 0.020(3) N3B 0.105(6) 0.054(5) 0.055(6) -0.006(4) 0.029(5) 0.003(4) N1 0.088(4) 0.227(8) 0.043(3) -0.004(4) 0.035(3) -0.007(5) C4 0.086(4) 0.094(5) 0.036(3) -0.008(3) 0.016(3) -0.004(4) C5B 0.106(6) 0.055(5) 0.055(5) -0.005(4) 0.033(5) 0.008(5) C3 0.083(4) 0.078(4) 0.043(3) -0.001(3) 0.025(3) -0.016(3) C1 0.086(5) 0.116(5) 0.033(3) 0.004(3) 0.015(3) 0.001(4) C2 0.092(5) 0.130(6) 0.049(4) 0.010(3) 0.026(4) -0.014(4) C6B 0.111(6) 0.056(6) 0.057(6) -0.017(5) 0.044(5) 0.014(5) C6A 0.115(6) 0.048(7) 0.059(7) -0.015(5) 0.038(5) 0.014(6) C5A 0.109(6) 0.056(5) 0.059(5) -0.007(4) 0.034(5) 0.010(4) O1A 0.108(6) 0.057(6) 0.055(5) -0.005(4) 0.034(5) 0.016(5) N3A 0.100(6) 0.058(5) 0.054(6) -0.003(5) 0.035(5) 0.002(5) O2A 0.096(6) 0.059(7) 0.055(7) -0.015(5) 0.036(5) 0.010(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0137 0.0067 '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' Fe Fe -0.2673 2.5550 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0389 0.0241 '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 O4 Fe1 O5 163.4(2) . 6_565 ? O4 Fe1 O1A 97.2(4) . . ? O4 Fe1 O2A 91.8(6) . . ? O6 Fe1 O4 91.89(15) 6_565 . ? O6 Fe1 O5 80.20(16) 6_565 6_565 ? O6 Fe1 O3 104.6(2) 6_565 . ? O6 Fe1 O1A 154.1(5) 6_565 . ? O6 Fe1 O2A 88.1(7) 6_565 . ? O5 Fe1 O1A 96.1(4) 6_565 . ? O5 Fe1 O2A 102.4(5) 6_565 . ? O2B Fe1 O4 100.0(5) . . ? O2B Fe1 O5 93.5(5) . 6_565 ? O2B Fe1 O3 172.5(6) . . ? O1B Fe1 O4 102.1(4) . . ? O1B Fe1 O5 88.1(4) . 6_565 ? O1B Fe1 O2B 86.8(7) . . ? O1B Fe1 O3 86.0(5) . . ? O3 Fe1 O4 79.61(18) . . ? O3 Fe1 O5 88.2(2) . 6_565 ? O3 Fe1 O1A 100.9(6) . . ? O3 Fe1 O2A 164.8(6) . . ? O2A Fe1 O1A 67.5(9) . . ? C1 O4 Fe1 112.5(4) . . ? N2 O6 Fe1 110.8(3) . 6_566 ? C4 O5 Fe1 110.3(3) . 6_566 ? N3B O2B Fe1 105.2(12) . . ? O6 N2 H2 121.2 . . ? C4 N2 O6 117.6(5) . . ? C4 N2 H2 121.2 . . ? C5B O1B Fe1 107.5(9) . . ? N1 O3 Fe1 109.5(4) . . ? O2B N3B H3B 118.5 . . ? C5B N3B O2B 123.0(15) . . ? C5B N3B H3B 118.5 . . ? O3 N1 H1 120.6 . . ? C1 N1 O3 118.9(6) . . ? C1 N1 H1 120.6 . . ? O5 C4 N2 119.1(5) . . ? O5 C4 C3 123.8(5) . . ? N2 C4 C3 117.0(6) . . ? N3B C5B O1B 115.9(15) . . ? N3B C5B C6B 123.3(17) . . ? C6B C5B O1B 119.4(14) . . ? C4 C3 H3 120.5 . . ? C2 C3 C4 119.0(6) . . ? C2 C3 H3 120.5 . . ? O4 C1 N1 119.2(5) . . ? O4 C1 C2 124.3(6) . . ? N1 C1 C2 116.5(6) . . ? C3 C2 C1 120.6(6) . . ? C3 C2 H2A 119.7 . . ? C1 C2 H2A 119.7 . . ? C5B C6B H6B 108.2 . . ? C6B C6B H6B 108.2 7_665 . ? C6A C6A H6A 121.5 7_665 . ? C6A C6A C5A 117(2) 7_665 . ? C5A C6A H6A 121.5 . . ? O1A C5A C6A 110.7(16) . . ? N3A C5A C6A 135.4(18) . . ? N3A C5A O1A 112.4(15) . . ? C5A O1A Fe1 120.4(11) . . ? C5A N3A H3A 118.2 . . ? C5A N3A O2A 123.6(17) . . ? O2A N3A H3A 118.2 . . ? N3A O2A Fe1 115.6(16) . . ? 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 Fe1 O4 1.992(4) . ? Fe1 O6 1.945(4) 6_565 ? Fe1 O5 2.004(4) 6_565 ? Fe1 O2B 1.94(2) . ? Fe1 O1B 1.924(11) . ? Fe1 O3 1.976(6) . ? Fe1 O1A 2.182(16) . ? Fe1 O2A 2.18(3) . ? O4 C1 1.264(7) . ? O6 N2 1.348(5) . ? O5 C4 1.288(7) . ? O2B N3B 1.47(2) . ? N2 H2 0.8800 . ? N2 C4 1.292(7) . ? O1B C5B 1.498(18) . ? O3 N1 1.357(6) . ? N3B H3B 0.8800 . ? N3B C5B 1.18(2) . ? N1 H1 0.8800 . ? N1 C1 1.268(8) . ? C4 C3 1.460(7) . ? C5B C6B 1.29(2) . ? C3 H3 0.9500 . ? C3 C2 1.352(8) . ? C1 C2 1.451(7) . ? C2 H2A 0.9500 . ? C6B C6B 1.353(16) 7_665 ? C6B H6B 0.9500 . ? C6A C6A 1.381(18) 7_665 ? C6A H6A 0.9500 . ? C6A C5A 1.46(2) . ? C5A O1A 1.31(2) . ? C5A N3A 1.19(2) . ? N3A H3A 0.8800 . ? N3A O2A 1.30(2) . ? 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 Fe1 O4 C1 N1 -4.7(9) . . . . ? Fe1 O4 C1 C2 177.1(6) . . . . ? Fe1 O6 N2 C4 10.1(6) 6_566 . . . ? Fe1 O5 C4 N2 -10.7(7) 6_566 . . . ? Fe1 O5 C4 C3 168.7(5) 6_566 . . . ? Fe1 O2B N3B C5B 4.9(15) . . . . ? Fe1 O1B C5B N3B 14.0(15) . . . . ? Fe1 O1B C5B C6B -179.2(11) . . . . ? Fe1 O3 N1 C1 3.5(9) . . . . ? O4 C1 C2 C3 6.2(11) . . . . ? O6 N2 C4 O5 0.7(9) . . . . ? O6 N2 C4 C3 -178.8(5) . . . . ? O5 C4 C3 C2 11.2(10) . . . . ? O2B N3B C5B O1B -12.9(18) . . . . ? O2B N3B C5B C6B -179.2(11) . . . . ? N2 C4 C3 C2 -169.4(6) . . . . ? O1B C5B C6B C6B 30(4) . . . 7_665 ? O3 N1 C1 O4 0.8(11) . . . . ? O3 N1 C1 C2 179.2(6) . . . . ? N3B C5B C6B C6B -164(3) . . . 7_665 ? N1 C1 C2 C3 -172.0(7) . . . . ? C4 C3 C2 C1 -178.0(6) . . . . ? C6A C6A C5A O1A -5(2) 7_665 . . . ? C6A C6A C5A N3A 160(3) 7_665 . . . ? C6A C5A O1A Fe1 177.0(10) . . . . ? C6A C5A N3A O2A -173.2(16) . . . . ? C5A N3A O2A Fe1 5(2) . . . . ? O1A C5A N3A O2A -9(2) . . . . ? N3A C5A O1A Fe1 8.7(19) . . . . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.849 -0.178 -0.929 3263.1 796.5 '20 DMF'