#------------------------------------------------------------------------------ #$Date: 2019-02-23 01:24:51 +0200 (Sat, 23 Feb 2019) $ #$Revision: 213799 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/06/1550636.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_1550636 loop_ _publ_author_name 'Valverde-Mu\~noz, Francisco Javier' 'Seredyuk, Maksym' 'Meneses-S\'anchez, Manuel' 'Mu\~noz, M. Carmen' 'Bartual-Murgui, Carlos' 'Real Cabezos, Jos\'e Antonio A' _publ_section_title ; Discrimination between two memory channels by molecular alloying in a doubly bistable spin crossover material ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/C8SC05256E _journal_year 2019 _chemical_formula_moiety '2(As F6), C30 H46 Fe N10' _chemical_formula_sum 'C30 H48 As2 F12 Fe N10' _chemical_formula_weight 982.47 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2018-06-06 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2018-11-19 deposited with the CCDC. 2019-02-22 downloaded from the CCDC. ; _cell_angle_alpha 91.428(7) _cell_angle_beta 100.894(7) _cell_angle_gamma 99.001(7) _cell_formula_units_Z 2 _cell_length_a 9.4189(8) _cell_length_b 10.3506(9) _cell_length_c 22.4440(18) _cell_measurement_reflns_used 3365 _cell_measurement_temperature 230(2) _cell_measurement_theta_max 29.9076 _cell_measurement_theta_min 2.9995 _cell_volume 2118.9(3) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SIR2004 (Burla et al., 2007)' _diffrn_ambient_temperature 230(2) _diffrn_detector_area_resol_mean 16.0267 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.888 _diffrn_measurement_device_type 'Supernova, Single source at offset, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_unetI/netI 0.0925 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.888 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 27229 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.888 _diffrn_reflns_theta_full 25.240 _diffrn_reflns_theta_max 29.962 _diffrn_reflns_theta_min 2.993 _exptl_absorpt_coefficient_mu 1.993 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.832 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Empirical absorption SCALE3 ABSPACK' _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.540 _exptl_crystal_description plate _exptl_crystal_F_000 996 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.854 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.088 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 497 _refine_ls_number_reflns 10931 _refine_ls_number_restraints 306 _refine_ls_restrained_S_all 1.013 _refine_ls_R_factor_all 0.1414 _refine_ls_R_factor_gt 0.0646 _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^)+(0.0728P)^2^+1.2108P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1470 _refine_ls_wR_factor_ref 0.1906 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5545 _reflns_number_total 10931 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8sc05256e2.cif _cod_data_source_block ja1197 _cod_original_cell_volume 2118.8(3) _cod_database_code 1550636 _shelx_shelxl_version_number 2016/6 _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 0.925 _shelx_estimated_absorpt_t_min 0.796 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, {H30A,H30B,H30C} of C30, {H10A,H10B,H10C} of C10, All C(H, H) groups At 1.5 times of: {H20A,H20B,H20C} of C20 2. Uiso/Uaniso restraints and constraints All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.2 Uanis(C20) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001 3.a Secondary CH2 refined with riding coordinates: C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C15(H15A, H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B) 3.b Me refined with riding coordinates: C10(H10A,H10B,H10C), C30(H30A,H30B,H30C) 3.c Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C4(H4), C11(H11), C12(H12), C14(H14), C21(H21), C22(H22), C24(H24) 3.d Idealised Me refined as rotating group: C20(H20A,H20B,H20C) ; _shelx_res_file ; TITL P-1 ja1197.res created by SHELXL-2016/6 at 13:10:29 on 06-Jun-2018 CELL 0.71069 9.4189 10.3506 22.444 91.428 100.894 99.001 ZERR 2 0.0008 0.0009 0.0018 0.007 0.007 0.007 LATT 1 SFAC C H N F Fe As UNIT 60 96 20 24 2 4 SIMU 0.04 0.08 1.7 ISOR 0.001 0.2 C8 C9 ISOR 0.001 0.001 C20 L.S. 4 PLAN 25 SIZE 0.04 0.06 0.12 LIST 1 fmap 2 acta MERG 2 OMIT -3 180 OMIT -3 8 0 OMIT 3 -1 17 OMIT -4 8 0 OMIT 9 -8 6 OMIT -6 8 2 OMIT -1 -4 3 OMIT -5 10 0 OMIT -5 11 4 OMIT -6 6 6 OMIT 3 -7 1 OMIT -7 7 7 OMIT -4 8 10 OMIT 0 -1 26 OMIT 0 -4 12 OMIT -4 9 3 OMIT -5 7 2 OMIT 6 -9 8 REM REM REM WGHT 0.072800 1.210800 FVAR 1.91700 AS1 6 1.099912 -0.152757 0.912499 11.00000 0.05958 0.04447 = 0.05182 0.00701 0.01104 0.00526 F1 4 1.017207 -0.141728 0.973253 11.00000 0.08793 0.07779 = 0.07468 0.00771 0.03291 0.02294 F2 4 1.010878 -0.308640 0.895664 11.00000 0.14257 0.05593 = 0.11981 -0.00882 0.06610 -0.01657 F3 4 1.242515 -0.208832 0.957891 11.00000 0.10701 0.12903 = 0.08026 0.04283 0.03061 0.06750 F4 4 1.184566 -0.163856 0.851938 11.00000 0.08288 0.09728 = 0.06195 -0.00135 0.02480 -0.00748 F5 4 1.192549 0.002516 0.928174 11.00000 0.07832 0.05726 = 0.09663 -0.00666 0.00645 -0.00695 F6 4 0.960035 -0.095276 0.867132 11.00000 0.05793 0.11965 = 0.10911 0.04979 -0.00469 0.00564 AS2 6 1.192438 -0.168121 0.638680 11.00000 0.05894 0.05896 = 0.04662 0.00251 0.00439 0.01733 F7 4 1.121894 -0.127059 0.700166 11.00000 0.13610 0.07799 = 0.06972 -0.00160 0.03972 0.02129 F8 4 1.096391 -0.320493 0.636960 11.00000 0.18544 0.07110 = 0.13938 -0.03079 0.06138 -0.01715 F9 4 1.335345 -0.212209 0.686440 11.00000 0.14006 0.16509 = 0.09619 0.01013 -0.02599 0.09956 F10 4 1.261760 -0.209042 0.577878 11.00000 0.11357 0.15319 = 0.07075 0.00973 0.03592 0.06473 F11 4 1.282396 -0.010846 0.643303 11.00000 0.12558 0.08195 = 0.12911 0.01800 0.02627 -0.01704 F12 4 1.050535 -0.116814 0.592705 11.00000 0.08812 0.17721 = 0.07486 -0.00218 -0.00593 0.06442 FE 5 0.879392 0.325076 0.778038 11.00000 0.04238 0.04058 = 0.03983 0.00563 0.01153 0.00645 N1 3 0.825265 0.304601 0.676895 11.00000 0.05090 0.05693 = 0.03885 0.00374 0.00394 0.01770 N2 3 1.023891 0.196245 0.752908 11.00000 0.04209 0.04139 = 0.04261 0.00438 0.00165 0.00858 N3 3 0.692908 0.172771 0.787252 11.00000 0.04309 0.04647 = 0.04014 0.00010 0.00585 0.00034 N4 3 0.901993 0.303669 0.876245 11.00000 0.04641 0.04579 = 0.04630 0.00146 0.01152 -0.00378 N5 3 0.732246 0.468755 0.767424 11.00000 0.03783 0.04976 = 0.05849 0.00373 0.01658 0.00884 N6 3 1.021002 0.511645 0.770481 11.00000 0.04077 0.04134 = 0.04661 0.00695 0.00798 0.01089 N7 3 1.184056 0.358223 0.851703 11.00000 0.04160 0.03772 = 0.05483 0.00539 0.00313 0.00642 N8 3 0.896388 0.240270 0.594593 11.00000 0.07261 0.08092 = 0.03899 -0.00218 0.01000 0.02112 N9 3 0.579509 0.055990 0.850484 11.00000 0.04433 0.05816 = 0.06184 0.00449 0.01441 -0.00583 N10 3 0.700637 0.665456 0.736325 11.00000 0.05517 0.05317 = 0.06016 0.00660 0.01034 0.02744 C1 1 0.745349 0.350806 0.627674 11.00000 0.06694 0.09024 = 0.05274 0.01167 0.00282 0.03105 AFIX 43 H1 2 0.672717 0.401626 0.628967 11.00000 -1.20000 AFIX 0 C2 1 0.787099 0.311832 0.576013 11.00000 0.08337 0.10148 = 0.04437 0.01594 -0.00255 0.03280 AFIX 43 H2 2 0.749155 0.330101 0.536359 11.00000 -1.20000 AFIX 0 C3 1 0.916499 0.238091 0.655453 11.00000 0.05617 0.04930 = 0.03971 0.00168 0.00992 0.01070 C4 1 1.020065 0.176993 0.696450 11.00000 0.05539 0.03905 = 0.05318 0.00110 0.01512 0.01382 AFIX 43 H4 2 1.081024 0.126029 0.682259 11.00000 -1.20000 AFIX 0 C5 1 1.131399 0.144086 0.796612 11.00000 0.05872 0.04185 = 0.05746 0.00358 0.00263 0.01768 AFIX 23 H5A 2 1.174766 0.080777 0.776405 11.00000 -1.20000 H5B 2 1.084907 0.100450 0.827389 11.00000 -1.20000 AFIX 0 C6 1 1.249521 0.257669 0.825974 11.00000 0.04780 0.04845 = 0.06968 0.01037 -0.00239 0.01584 AFIX 23 H6A 2 1.318430 0.225826 0.857701 11.00000 -1.20000 H6B 2 1.302889 0.294573 0.795737 11.00000 -1.20000 AFIX 0 C7 1 0.987456 0.188778 0.554775 11.00000 0.12819 0.06933 = 0.05381 -0.01161 0.03020 0.02705 AFIX 23 H7A 2 0.924523 0.148054 0.517652 11.00000 -1.20000 H7B 2 1.037442 0.122509 0.575398 11.00000 -1.20000 AFIX 0 C8 1 1.103032 0.301407 0.538746 11.00000 0.13337 0.13496 = 0.13303 0.00631 0.02742 0.02191 AFIX 23 H8A 2 1.147279 0.267474 0.507268 11.00000 -1.20000 H8B 2 1.051713 0.370365 0.521717 11.00000 -1.20000 AFIX 0 C9 1 1.210652 0.354857 0.584535 11.00000 0.15595 0.15693 = 0.15620 0.00747 0.03144 0.02532 AFIX 23 H9A 2 1.255663 0.285037 0.604379 11.00000 -1.20000 H9B 2 1.167584 0.397441 0.614059 11.00000 -1.20000 AFIX 0 C10 1 1.329751 0.453790 0.566733 11.00000 0.15310 0.08483 = 0.18626 0.02615 0.04939 0.01255 AFIX 33 H10A 2 1.401640 0.486594 0.602312 11.00000 -1.20000 H10B 2 1.375664 0.412393 0.538455 11.00000 -1.20000 H10C 2 1.287387 0.525049 0.548156 11.00000 -1.20000 AFIX 0 C11 1 0.570939 0.094626 0.754855 11.00000 0.05089 0.04897 = 0.04752 -0.00520 0.00326 0.01205 AFIX 43 H11 2 0.540517 0.091983 0.712873 11.00000 -1.20000 AFIX 0 C12 1 0.501061 0.021591 0.793168 11.00000 0.04421 0.05604 = 0.06433 -0.00739 0.00630 0.00236 AFIX 43 H12 2 0.416103 -0.040043 0.782491 11.00000 -1.20000 AFIX 0 C13 1 0.695085 0.146789 0.844827 11.00000 0.03473 0.05120 = 0.05249 0.00156 0.00879 -0.00657 C14 1 0.806744 0.217545 0.892748 11.00000 0.05442 0.05747 = 0.03742 0.00403 0.01142 -0.00831 AFIX 43 H14 2 0.809016 0.201149 0.933442 11.00000 -1.20000 AFIX 0 C15 1 1.020149 0.375328 0.923144 11.00000 0.07040 0.05155 = 0.03719 0.00016 0.00450 -0.01465 AFIX 23 H15A 2 1.002771 0.353489 0.963214 11.00000 -1.20000 H15B 2 1.023583 0.468962 0.919757 11.00000 -1.20000 AFIX 0 C16 1 1.163481 0.337155 0.914221 11.00000 0.05420 0.05107 = 0.05064 0.00943 -0.00531 -0.00428 AFIX 23 H16A 2 1.243887 0.389153 0.942551 11.00000 -1.20000 H16B 2 1.163755 0.245635 0.922465 11.00000 -1.20000 AFIX 0 C17 1 0.542070 0.006019 0.907300 11.00000 0.07881 0.08761 = 0.07867 0.01128 0.02534 -0.01931 AFIX 23 H17A 2 0.567561 0.076465 0.938675 11.00000 -1.20000 H17B 2 0.437192 -0.023770 0.901118 11.00000 -1.20000 AFIX 0 C18 1 0.618985 -0.102127 0.927575 11.00000 0.08423 0.10884 = 0.09605 0.00427 0.04034 -0.00990 AFIX 23 H18A 2 0.723445 -0.069356 0.936228 11.00000 -1.20000 H18B 2 0.591789 -0.130119 0.965386 11.00000 -1.20000 AFIX 0 C19 1 0.591834 -0.215160 0.885628 11.00000 0.07508 0.06163 = 0.06904 -0.00583 -0.00600 0.01818 C21 1 0.585618 0.476826 0.756427 11.00000 0.04211 0.07165 = 0.07463 0.00437 0.01988 0.01449 AFIX 43 H21 2 0.511342 0.409740 0.761354 11.00000 -1.20000 AFIX 0 C22 1 0.565472 0.593757 0.737834 11.00000 0.04668 0.08226 = 0.08016 0.00582 0.01560 0.02849 AFIX 43 H22 2 0.475775 0.622613 0.727564 11.00000 -1.20000 AFIX 0 C23 1 0.798841 0.585128 0.754723 11.00000 0.04573 0.04317 = 0.04751 0.00441 0.00689 0.01866 C24 1 0.955599 0.608857 0.759085 11.00000 0.04624 0.03613 = 0.04732 0.00381 0.00616 0.00358 AFIX 43 H24 2 1.005984 0.691172 0.753810 11.00000 -1.20000 AFIX 0 C25 1 1.182232 0.530734 0.778798 11.00000 0.03929 0.04414 = 0.06159 0.01411 0.01376 0.00970 AFIX 23 H25A 2 1.219999 0.621744 0.773922 11.00000 -1.20000 H25B 2 1.210710 0.477163 0.748425 11.00000 -1.20000 AFIX 0 C26 1 1.245246 0.492537 0.841693 11.00000 0.03579 0.04618 = 0.06360 0.00576 0.00557 0.00141 AFIX 23 H26A 2 1.350886 0.500783 0.846626 11.00000 -1.20000 H26B 2 1.223980 0.551681 0.871816 11.00000 -1.20000 AFIX 0 C27 1 0.727875 0.795785 0.713446 11.00000 0.08328 0.06597 = 0.09579 0.01528 0.01572 0.03841 AFIX 23 H27A 2 0.830659 0.833076 0.726181 11.00000 -1.20000 H27B 2 0.670373 0.852531 0.729991 11.00000 -1.20000 AFIX 0 C28 1 0.684577 0.786349 0.641267 11.00000 0.06595 0.06963 = 0.11166 0.02304 0.01980 0.01147 AFIX 23 H28A 2 0.748338 0.736174 0.624706 11.00000 -1.20000 H28B 2 0.584523 0.741333 0.628570 11.00000 -1.20000 AFIX 0 C29 1 0.698158 0.918592 0.617630 11.00000 0.09504 0.09301 = 0.13333 0.02906 0.03003 0.03126 AFIX 23 H29A 2 0.799700 0.961125 0.627482 11.00000 -1.20000 H29B 2 0.640266 0.971089 0.636517 11.00000 -1.20000 AFIX 0 C30 1 0.645218 0.908768 0.549319 11.00000 0.12834 0.18549 = 0.08831 0.03839 0.01865 0.05515 AFIX 33 H30A 2 0.654266 0.994987 0.534168 11.00000 -1.20000 H30B 2 0.703455 0.857576 0.530753 11.00000 -1.20000 H30C 2 0.544401 0.867517 0.539767 11.00000 -1.20000 AFIX 0 C20 1 0.647329 -0.343990 0.916459 11.00000 0.09970 0.10114 = 0.10029 0.00600 0.01799 0.01530 AFIX 137 H20A 2 0.620507 -0.417160 0.887188 11.00000 -1.50000 H20B 2 0.602233 -0.363797 0.950819 11.00000 -1.50000 H20C 2 0.751928 -0.326878 0.929525 11.00000 -1.50000 AFIX 0 HKLF 4 REM P-1 REM R1 = 0.0646 for 5545 Fo > 4sig(Fo) and 0.1414 for all 10931 data REM 497 parameters refined using 306 restraints END WGHT 0.0728 1.2108 REM Highest difference peak 0.854, deepest hole -0.618, 1-sigma level 0.088 Q1 1 1.1435 0.2362 0.5681 11.00000 0.05 0.85 Q2 1 1.1747 0.4047 0.5488 11.00000 0.05 0.81 Q3 1 0.5994 -0.2664 0.9404 11.00000 0.05 0.77 Q4 1 1.2426 -0.3232 0.6643 11.00000 0.05 0.57 Q5 1 0.6953 0.8735 0.6711 11.00000 0.05 0.52 Q6 1 0.4178 0.3555 0.7753 11.00000 0.05 0.51 Q7 1 1.2054 -0.3356 0.9499 11.00000 0.05 0.46 Q8 1 1.2235 -0.0769 0.9546 11.00000 0.05 0.45 Q9 1 0.6915 0.7936 0.5973 11.00000 0.05 0.42 Q10 1 1.3508 -0.2203 0.7006 11.00000 0.05 0.42 Q11 1 0.8566 0.3257 0.7202 11.00000 0.05 0.40 Q12 1 0.6461 -0.4428 0.9223 11.00000 0.05 0.40 Q13 1 1.2008 -0.0514 0.6056 11.00000 0.05 0.38 Q14 1 0.5927 -0.0665 0.8894 11.00000 0.05 0.38 Q15 1 0.6173 -0.2337 0.8409 11.00000 0.05 0.37 Q16 1 0.6508 -0.4004 0.9504 11.00000 0.05 0.37 Q17 1 0.5867 -0.2150 0.8322 11.00000 0.05 0.36 Q18 1 1.3691 -0.0970 0.6478 11.00000 0.05 0.35 Q19 1 0.6597 -0.3349 0.9026 11.00000 0.05 0.35 Q20 1 1.1556 -0.0739 0.5914 11.00000 0.05 0.35 Q21 1 1.0751 -0.0222 0.8979 11.00000 0.05 0.35 Q22 1 0.4619 -0.2299 0.8698 11.00000 0.05 0.34 Q23 1 0.8676 0.3082 0.8314 11.00000 0.05 0.34 Q24 1 0.9770 0.3086 0.5055 11.00000 0.05 0.34 Q25 1 0.4823 -0.2709 0.8675 11.00000 0.05 0.34 ; _shelx_res_checksum 98802 _olex2_submission_special_instructions 'No special instructions were received' _publcif_funding_html ; ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 As1 As 1.09991(6) -0.15276(5) 0.91250(3) 0.05222(18) Uani 1 1 d . U F1 F 1.0172(4) -0.1417(3) 0.97325(16) 0.0768(10) Uani 1 1 d . U F2 F 1.0109(5) -0.3086(4) 0.8957(2) 0.1046(15) Uani 1 1 d . U F3 F 1.2425(5) -0.2088(4) 0.95789(18) 0.0979(13) Uani 1 1 d . U F4 F 1.1846(4) -0.1639(4) 0.85194(16) 0.0818(11) Uani 1 1 d . U F5 F 1.1925(4) 0.0025(3) 0.92817(17) 0.0810(11) Uani 1 1 d . U F6 F 0.9600(4) -0.0953(4) 0.86713(19) 0.0986(13) Uani 1 1 d . U As2 As 1.19244(6) -0.16812(6) 0.63868(3) 0.05480(19) Uani 1 1 d . U F7 F 1.1219(5) -0.1271(4) 0.70017(17) 0.0917(12) Uani 1 1 d . U F8 F 1.0964(6) -0.3205(4) 0.6370(2) 0.1328(19) Uani 1 1 d . U F9 F 1.3353(6) -0.2122(5) 0.6864(2) 0.1321(19) Uani 1 1 d . U F10 F 1.2618(5) -0.2090(5) 0.57788(18) 0.1054(14) Uani 1 1 d . U F11 F 1.2824(5) -0.0108(4) 0.6433(2) 0.1155(15) Uani 1 1 d . U F12 F 1.0505(4) -0.1168(5) 0.59270(19) 0.1118(15) Uani 1 1 d . U Fe Fe 0.87939(7) 0.32508(7) 0.77804(3) 0.04045(19) Uani 1 1 d . U N1 N 0.8253(5) 0.3046(4) 0.67690(18) 0.0486(10) Uani 1 1 d . U N2 N 1.0239(4) 0.1962(4) 0.75291(19) 0.0427(9) Uani 1 1 d . U N3 N 0.6929(4) 0.1728(4) 0.78725(18) 0.0443(10) Uani 1 1 d . U N4 N 0.9020(4) 0.3037(4) 0.87624(18) 0.0471(10) Uani 1 1 d . U N5 N 0.7322(4) 0.4688(4) 0.7674(2) 0.0475(10) Uani 1 1 d . U N6 N 1.0210(4) 0.5116(4) 0.77048(18) 0.0425(10) Uani 1 1 d . U N7 N 1.1841(4) 0.3582(4) 0.85170(19) 0.0455(10) Uani 1 1 d . U N8 N 0.8964(5) 0.2403(5) 0.5946(2) 0.0635(13) Uani 1 1 d . U N9 N 0.5795(5) 0.0560(4) 0.8505(2) 0.0558(12) Uani 1 1 d . U N10 N 0.7006(5) 0.6655(4) 0.7363(2) 0.0542(11) Uani 1 1 d . U C1 C 0.7453(7) 0.3508(6) 0.6277(3) 0.0690(17) Uani 1 1 d . U H1 H 0.672717 0.401626 0.628967 0.083 Uiso 1 1 calc R . C2 C 0.7871(7) 0.3118(7) 0.5760(3) 0.0763(19) Uani 1 1 d . U H2 H 0.749155 0.330101 0.536359 0.092 Uiso 1 1 calc R . C3 C 0.9165(6) 0.2381(5) 0.6555(2) 0.0481(12) Uani 1 1 d . U C4 C 1.0201(6) 0.1770(5) 0.6964(2) 0.0480(12) Uani 1 1 d . U H4 H 1.081024 0.126029 0.682259 0.058 Uiso 1 1 calc R . C5 C 1.1314(6) 0.1441(5) 0.7966(3) 0.0528(13) Uani 1 1 d . U H5A H 1.174766 0.080777 0.776405 0.063 Uiso 1 1 calc R . H5B H 1.084907 0.100450 0.827389 0.063 Uiso 1 1 calc R . C6 C 1.2495(6) 0.2577(5) 0.8260(3) 0.0562(14) Uani 1 1 d . U H6A H 1.318430 0.225826 0.857701 0.067 Uiso 1 1 calc R . H6B H 1.302889 0.294573 0.795737 0.067 Uiso 1 1 calc R . C7 C 0.9875(8) 0.1888(6) 0.5548(3) 0.081(2) Uani 1 1 d . U H7A H 0.924523 0.148054 0.517652 0.097 Uiso 1 1 calc R . H7B H 1.037442 0.122509 0.575398 0.097 Uiso 1 1 calc R . C8 C 1.1030(11) 0.3014(10) 0.5387(5) 0.134(3) Uani 1 1 d . U H8A H 1.147279 0.267474 0.507268 0.160 Uiso 1 1 calc R . H8B H 1.051713 0.370365 0.521717 0.160 Uiso 1 1 calc R . C9 C 1.2107(13) 0.3549(12) 0.5845(5) 0.156(4) Uani 1 1 d . U H9A H 1.255663 0.285037 0.604379 0.188 Uiso 1 1 calc R . H9B H 1.167584 0.397441 0.614059 0.188 Uiso 1 1 calc R . C10 C 1.3298(11) 0.4538(8) 0.5667(5) 0.140(4) Uani 1 1 d . U H10A H 1.401640 0.486594 0.602312 0.168 Uiso 1 1 calc R . H10B H 1.375664 0.412393 0.538455 0.168 Uiso 1 1 calc R . H10C H 1.287387 0.525049 0.548156 0.168 Uiso 1 1 calc R . C11 C 0.5709(6) 0.0946(5) 0.7549(2) 0.0497(13) Uani 1 1 d . U H11 H 0.540517 0.091983 0.712873 0.060 Uiso 1 1 calc R . C12 C 0.5011(6) 0.0216(6) 0.7932(3) 0.0563(14) Uani 1 1 d . U H12 H 0.416103 -0.040043 0.782491 0.068 Uiso 1 1 calc R . C13 C 0.6951(5) 0.1468(5) 0.8448(2) 0.0476(13) Uani 1 1 d . U C14 C 0.8067(6) 0.2175(5) 0.8927(2) 0.0513(13) Uani 1 1 d . U H14 H 0.809016 0.201149 0.933442 0.062 Uiso 1 1 calc R . C15 C 1.0201(6) 0.3753(5) 0.9231(2) 0.0566(15) Uani 1 1 d . U H15A H 1.002771 0.353489 0.963214 0.068 Uiso 1 1 calc R . H15B H 1.023583 0.468962 0.919757 0.068 Uiso 1 1 calc R . C16 C 1.1635(6) 0.3372(5) 0.9142(2) 0.0553(14) Uani 1 1 d . U H16A H 1.243887 0.389153 0.942551 0.066 Uiso 1 1 calc R . H16B H 1.163755 0.245635 0.922465 0.066 Uiso 1 1 calc R . C17 C 0.5421(8) 0.0060(7) 0.9073(3) 0.084(2) Uani 1 1 d . U H17A H 0.567561 0.076465 0.938675 0.101 Uiso 1 1 calc R . H17B H 0.437192 -0.023770 0.901118 0.101 Uiso 1 1 calc R . C18 C 0.6190(8) -0.1021(8) 0.9276(4) 0.096(2) Uani 1 1 d . U H18A H 0.723445 -0.069356 0.936228 0.115 Uiso 1 1 calc R . H18B H 0.591789 -0.130119 0.965386 0.115 Uiso 1 1 calc R . C19 C 0.5918(7) -0.2152(6) 0.8856(3) 0.0707(17) Uani 1 1 d . U C21 C 0.5856(6) 0.4768(6) 0.7564(3) 0.0611(16) Uani 1 1 d . U H21 H 0.511342 0.409740 0.761354 0.073 Uiso 1 1 calc R . C22 C 0.5655(6) 0.5938(7) 0.7378(3) 0.0673(17) Uani 1 1 d . U H22 H 0.475775 0.622613 0.727564 0.081 Uiso 1 1 calc R . C23 C 0.7988(5) 0.5851(5) 0.7547(2) 0.0445(12) Uani 1 1 d . U C24 C 0.9556(5) 0.6089(5) 0.7591(2) 0.0439(12) Uani 1 1 d . U H24 H 1.005984 0.691172 0.753810 0.053 Uiso 1 1 calc R . C25 C 1.1822(5) 0.5307(5) 0.7788(2) 0.0473(12) Uani 1 1 d . U H25A H 1.219999 0.621744 0.773922 0.057 Uiso 1 1 calc R . H25B H 1.210710 0.477163 0.748425 0.057 Uiso 1 1 calc R . C26 C 1.2452(5) 0.4925(5) 0.8417(2) 0.0496(13) Uani 1 1 d . U H26A H 1.350886 0.500783 0.846626 0.060 Uiso 1 1 calc R . H26B H 1.223980 0.551681 0.871816 0.060 Uiso 1 1 calc R . C27 C 0.7279(8) 0.7958(6) 0.7134(3) 0.0789(19) Uani 1 1 d . U H27A H 0.830659 0.833076 0.726181 0.095 Uiso 1 1 calc R . H27B H 0.670373 0.852531 0.729991 0.095 Uiso 1 1 calc R . C28 C 0.6846(7) 0.7863(7) 0.6413(3) 0.082(2) Uani 1 1 d . U H28A H 0.748338 0.736174 0.624706 0.098 Uiso 1 1 calc R . H28B H 0.584523 0.741333 0.628570 0.098 Uiso 1 1 calc R . C29 C 0.6982(9) 0.9186(8) 0.6176(4) 0.104(3) Uani 1 1 d . U H29A H 0.799700 0.961125 0.627482 0.125 Uiso 1 1 calc R . H29B H 0.640266 0.971089 0.636517 0.125 Uiso 1 1 calc R . C30 C 0.6452(10) 0.9088(10) 0.5493(4) 0.131(3) Uani 1 1 d . U H30A H 0.654266 0.994987 0.534168 0.157 Uiso 1 1 calc R . H30B H 0.703455 0.857576 0.530753 0.157 Uiso 1 1 calc R . H30C H 0.544401 0.867517 0.539767 0.157 Uiso 1 1 calc R . C20 C 0.6473(9) -0.3440(7) 0.9165(4) 0.101(2) Uani 1 1 d . U H20A H 0.620507 -0.417160 0.887188 0.151 Uiso 1 1 calc GR . H20B H 0.602233 -0.363797 0.950819 0.151 Uiso 1 1 calc GR . H20C H 0.751928 -0.326878 0.929525 0.151 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 As1 0.0596(4) 0.0445(3) 0.0518(4) 0.0070(2) 0.0110(3) 0.0053(3) F1 0.088(3) 0.078(2) 0.075(2) 0.0077(19) 0.033(2) 0.023(2) F2 0.143(4) 0.056(2) 0.120(3) -0.009(2) 0.066(3) -0.017(2) F3 0.107(3) 0.129(4) 0.080(3) 0.043(2) 0.031(2) 0.068(3) F4 0.083(3) 0.097(3) 0.062(2) -0.0013(19) 0.025(2) -0.007(2) F5 0.078(2) 0.057(2) 0.097(3) -0.0067(19) 0.006(2) -0.0069(18) F6 0.058(2) 0.120(3) 0.109(3) 0.050(3) -0.005(2) 0.006(2) As2 0.0589(4) 0.0590(4) 0.0466(3) 0.0025(3) 0.0044(3) 0.0173(3) F7 0.136(4) 0.078(3) 0.070(3) -0.002(2) 0.040(2) 0.021(2) F8 0.185(5) 0.071(3) 0.139(4) -0.031(3) 0.061(4) -0.017(3) F9 0.140(4) 0.165(5) 0.096(3) 0.010(3) -0.026(3) 0.100(4) F10 0.114(3) 0.153(4) 0.071(3) 0.010(3) 0.036(2) 0.065(3) F11 0.126(4) 0.082(3) 0.129(4) 0.018(3) 0.026(3) -0.017(3) F12 0.088(3) 0.177(5) 0.075(3) -0.002(3) -0.006(2) 0.064(3) Fe 0.0424(4) 0.0406(4) 0.0398(4) 0.0056(3) 0.0115(3) 0.0065(3) N1 0.051(3) 0.057(3) 0.039(2) 0.004(2) 0.004(2) 0.018(2) N2 0.042(2) 0.041(2) 0.043(2) 0.0044(18) 0.0016(19) 0.0086(18) N3 0.043(2) 0.046(2) 0.040(2) 0.0001(19) 0.0058(19) 0.0003(19) N4 0.046(2) 0.046(2) 0.046(3) 0.0015(19) 0.012(2) -0.004(2) N5 0.038(2) 0.050(3) 0.058(3) 0.004(2) 0.017(2) 0.0088(19) N6 0.041(2) 0.041(2) 0.047(2) 0.0070(18) 0.0080(19) 0.0109(19) N7 0.042(2) 0.038(2) 0.055(3) 0.0054(19) 0.003(2) 0.0064(18) N8 0.073(3) 0.081(4) 0.039(3) -0.002(2) 0.010(2) 0.021(3) N9 0.044(3) 0.058(3) 0.062(3) 0.004(2) 0.014(2) -0.006(2) N10 0.055(3) 0.053(3) 0.060(3) 0.007(2) 0.010(2) 0.027(2) C1 0.067(4) 0.090(5) 0.053(4) 0.012(3) 0.003(3) 0.031(3) C2 0.083(5) 0.101(5) 0.044(4) 0.016(3) -0.003(3) 0.033(4) C3 0.056(3) 0.049(3) 0.040(3) 0.002(2) 0.010(2) 0.011(3) C4 0.055(3) 0.039(3) 0.053(3) 0.001(2) 0.015(3) 0.014(2) C5 0.059(3) 0.042(3) 0.057(3) 0.004(2) 0.003(3) 0.018(3) C6 0.048(3) 0.048(3) 0.070(4) 0.010(3) -0.002(3) 0.016(3) C7 0.128(6) 0.069(4) 0.054(4) -0.012(3) 0.030(4) 0.027(4) C8 0.133(3) 0.135(3) 0.133(3) 0.0063(10) 0.0274(12) 0.0219(11) C9 0.156(4) 0.157(4) 0.156(4) 0.0075(10) 0.0314(13) 0.0253(12) C10 0.153(9) 0.085(6) 0.186(11) 0.026(6) 0.049(8) 0.013(6) C11 0.051(3) 0.049(3) 0.048(3) -0.005(2) 0.003(3) 0.012(3) C12 0.044(3) 0.056(3) 0.064(4) -0.007(3) 0.006(3) 0.002(3) C13 0.035(3) 0.051(3) 0.052(3) 0.002(2) 0.009(2) -0.007(2) C14 0.054(3) 0.057(3) 0.037(3) 0.004(2) 0.011(2) -0.008(3) C15 0.070(4) 0.052(3) 0.037(3) 0.000(2) 0.005(3) -0.015(3) C16 0.054(3) 0.051(3) 0.051(3) 0.009(3) -0.005(3) -0.004(3) C17 0.079(5) 0.088(5) 0.079(5) 0.011(4) 0.025(4) -0.019(4) C18 0.084(5) 0.109(6) 0.096(6) 0.004(5) 0.040(5) -0.010(5) C19 0.075(4) 0.062(4) 0.069(4) -0.006(3) -0.006(3) 0.018(3) C21 0.042(3) 0.072(4) 0.075(4) 0.004(3) 0.020(3) 0.014(3) C22 0.047(3) 0.082(5) 0.080(4) 0.006(3) 0.016(3) 0.028(3) C23 0.046(3) 0.043(3) 0.048(3) 0.004(2) 0.007(2) 0.019(2) C24 0.046(3) 0.036(3) 0.047(3) 0.004(2) 0.006(2) 0.004(2) C25 0.039(3) 0.044(3) 0.062(3) 0.014(2) 0.014(2) 0.010(2) C26 0.036(3) 0.046(3) 0.064(4) 0.006(3) 0.006(2) 0.001(2) C27 0.083(5) 0.066(4) 0.096(5) 0.015(4) 0.016(4) 0.038(4) C28 0.066(4) 0.070(5) 0.112(6) 0.023(4) 0.020(4) 0.011(3) C29 0.095(6) 0.093(6) 0.133(8) 0.029(5) 0.030(5) 0.031(5) C30 0.128(8) 0.185(10) 0.088(7) 0.038(6) 0.019(6) 0.055(7) C20 0.100(3) 0.101(3) 0.100(3) 0.0060(10) 0.0180(11) 0.0153(11) 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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 F1 As1 F3 89.95(18) F1 As1 F4 179.45(18) F2 As1 F1 90.23(18) F2 As1 F3 90.4(2) F2 As1 F4 89.96(18) F2 As1 F5 178.40(18) F2 As1 F6 90.3(2) F4 As1 F3 89.53(18) F5 As1 F1 91.29(18) F5 As1 F3 89.1(2) F5 As1 F4 88.53(18) F5 As1 F6 90.21(19) F6 As1 F1 90.51(19) F6 As1 F3 179.2(2) F6 As1 F4 90.0(2) F8 As2 F7 88.8(2) F8 As2 F10 91.0(2) F8 As2 F11 176.3(2) F8 As2 F12 91.4(3) F9 As2 F7 89.2(2) F9 As2 F8 90.7(3) F9 As2 F10 90.9(2) F9 As2 F11 90.3(3) F9 As2 F12 177.2(2) F10 As2 F7 179.8(2) F10 As2 F11 92.5(2) F11 As2 F7 87.6(2) F12 As2 F7 89.1(2) F12 As2 F10 90.9(2) F12 As2 F11 87.5(2) N2 Fe N1 75.00(15) N2 Fe N3 98.22(15) N2 Fe N4 102.54(16) N2 Fe N6 97.06(15) N3 Fe N1 92.85(16) N4 Fe N1 167.54(16) N4 Fe N3 75.28(15) N4 Fe N6 104.30(15) N5 Fe N1 84.43(16) N5 Fe N2 158.39(16) N5 Fe N3 89.22(16) N5 Fe N4 98.96(16) N5 Fe N6 75.39(15) N6 Fe N1 88.15(15) N6 Fe N3 164.42(15) C1 N1 Fe 142.4(4) C3 N1 Fe 110.9(3) C3 N1 C1 105.8(5) C4 N2 Fe 116.6(3) C4 N2 C5 119.5(4) C5 N2 Fe 123.6(3) C11 N3 Fe 143.0(4) C13 N3 Fe 111.4(3) C13 N3 C11 105.6(4) C14 N4 Fe 116.1(3) C14 N4 C15 118.5(4) C15 N4 Fe 125.4(3) C21 N5 Fe 141.0(4) C23 N5 Fe 111.8(3) C23 N5 C21 105.2(4) C24 N6 Fe 115.6(3) C24 N6 C25 119.2(4) C25 N6 Fe 125.2(3) C6 N7 C16 113.9(4) C6 N7 C26 115.1(4) C26 N7 C16 114.2(4) C2 N8 C7 125.5(5) C3 N8 C2 107.4(5) C3 N8 C7 126.7(5) C12 N9 C17 126.3(5) C13 N9 C12 106.7(5) C13 N9 C17 127.0(5) C22 N10 C27 126.1(5) C23 N10 C22 105.7(5) C23 N10 C27 127.9(5) N1 C1 C2 110.1(5) C1 C2 N8 105.8(5) N1 C3 N8 110.9(5) N1 C3 C4 120.3(5) N8 C3 C4 128.8(5) N2 C4 C3 116.7(4) N2 C5 C6 108.3(4) N7 C6 C5 110.4(4) N8 C7 C8 110.9(6) C9 C8 C7 116.4(10) C8 C9 C10 115.4(11) C12 C11 N3 109.7(5) C11 C12 N9 106.7(5) N3 C13 N9 111.3(4) N3 C13 C14 120.8(4) N9 C13 C14 127.9(5) N4 C14 C13 116.5(5) N4 C15 C16 108.3(4) N7 C16 C15 110.4(4) C18 C17 N9 111.8(6) C19 C18 C17 115.9(7) C18 C19 C20 113.4(6) C22 C21 N5 110.0(5) C21 C22 N10 107.9(5) N5 C23 N10 111.1(4) N5 C23 C24 119.9(4) N10 C23 C24 128.9(5) N6 C24 C23 116.5(5) N6 C25 C26 109.1(4) N7 C26 C25 111.2(4) N10 C27 C28 109.6(5) C29 C28 C27 110.3(6) C28 C29 C30 109.8(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance As1 F1 1.703(3) As1 F2 1.696(4) As1 F3 1.713(4) As1 F4 1.711(3) As1 F5 1.699(3) As1 F6 1.701(4) As2 F7 1.712(3) As2 F8 1.687(4) As2 F9 1.685(4) As2 F10 1.692(4) As2 F11 1.705(4) As2 F12 1.692(4) Fe N1 2.228(4) Fe N2 2.184(4) Fe N3 2.214(4) Fe N4 2.194(4) Fe N5 2.174(4) Fe N6 2.198(4) N1 C1 1.357(7) N1 C3 1.330(6) N2 C4 1.271(6) N2 C5 1.449(6) N3 C11 1.366(6) N3 C13 1.323(6) N4 C14 1.276(6) N4 C15 1.469(6) N5 C21 1.372(6) N5 C23 1.332(6) N6 C24 1.267(6) N6 C25 1.476(6) N7 C6 1.450(6) N7 C16 1.469(6) N7 C26 1.459(6) N8 C2 1.369(7) N8 C3 1.344(6) N8 C7 1.492(7) N9 C12 1.365(7) N9 C13 1.350(6) N9 C17 1.471(7) N10 C22 1.376(7) N10 C23 1.353(6) N10 C27 1.458(7) C1 C2 1.364(8) C3 C4 1.443(7) C5 C6 1.526(7) C7 C8 1.564(11) C8 C9 1.339(12) C9 C10 1.516(13) C11 C12 1.355(7) C13 C14 1.446(7) C15 C16 1.511(8) C17 C18 1.463(10) C18 C19 1.443(9) C19 C20 1.630(9) C21 C22 1.320(8) C23 C24 1.442(7) C25 C26 1.512(7) C27 C28 1.591(9) C28 C29 1.476(9) C29 C30 1.516(10)