#------------------------------------------------------------------------------ #$Date: 2019-11-17 09:20:43 +0200 (Sun, 17 Nov 2019) $ #$Revision: 229069 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/99/7229911.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_7229911 loop_ _publ_author_name 'Wei, Hai-Wen' 'Yang, Qing-Feng' 'Lai, Xiao-Yong' 'Wang, Xiao-Zhong' 'Yang, Tian-Lin' 'Hou, Qin' 'Liu, Xiang-Yu' _publ_section_title ; Field-induced slow relaxation of magnetization in a distorted octahedral mononuclear high-spin Co(ii) complex ; _journal_issue 7 _journal_name_full CrystEngComm _journal_page_first 962 _journal_paper_doi 10.1039/C7CE01981E _journal_volume 20 _journal_year 2018 _chemical_formula_moiety 'C28 H26 Fe N6 O8' _chemical_formula_sum 'C28 H26 Fe N6 O8' _chemical_formula_weight 630.40 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2017-07-03 _audit_creation_method ; Olex2 1.2 (compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335) ; _audit_update_record ; 2017-07-03 deposited with the CCDC. 2018-01-08 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 108.46(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.276(3) _cell_length_b 9.993(2) _cell_length_c 19.942(4) _cell_measurement_reflns_used 9936 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.072 _cell_measurement_theta_min 2.305 _cell_volume 2887.6(11) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _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 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1067 _diffrn_reflns_av_unetI/netI 0.0723 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 66619 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.497 _diffrn_reflns_theta_min 2.153 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.583 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6910 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.450 _exptl_crystal_description block _exptl_crystal_F_000 1304 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.755 _refine_diff_density_min -0.380 _refine_diff_density_rms 0.078 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 392 _refine_ls_number_reflns 6615 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.100 _refine_ls_R_factor_all 0.1177 _refine_ls_R_factor_gt 0.0680 _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^)+(0.0478P)^2^+2.9320P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1200 _refine_ls_wR_factor_ref 0.1337 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4456 _reflns_number_total 6615 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7ce01981e2.cif _cod_data_source_block zh-4fe _cod_depositor_comments 'Adding full bibliography for 7229910--7229911.cif.' _cod_database_code 7229911 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2.a Secondary CH2 refined with riding coordinates: C6(H6A,H6B), C14(H14A,H14B), C7(H7A,H7B), C15(H15A,H15B) 2.b Aromatic/amide H refined with riding coordinates: N6(H6), N4(H4), C26(H26), C25(H25), C24(H24), C22(H22), C21(H21), C18(H18), C19(H19), C17(H17) 2.c Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C16(H16A,H16B,H16C) 2.d Idealised tetrahedral OH refined as rotating group: O3(H3), O7(H7) ; _shelx_res_file ; TITL zh-4fe_a.res in P2(1)/n zh-4fe.res created by SHELXL-2016/6 at 20:01:58 on 03-Jul-2017 REM Old TITL ZH-4 Fe in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.161, Rweak 0.038, Alpha 0.073, Orientation as input REM Formula found by SHELXT: C29 N8 O5 Fe CELL 0.71073 15.2763 9.9927 19.9421 90 108.458 90 ZERR 4 0.0031 0.002 0.004 0 0.03 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Fe N O UNIT 112 104 4 24 32 EQIV $1 0.5-X,0.5+Y,0.5-Z EQIV $2 1-X,2-Y,1-Z L.S. 10 PLAN 20 HTAB N6 O6_$1 HTAB O3 O2 HTAB O7 O6 HTAB N4 O8_$2 BOND LIST 6 fmap 2 ACTA REM REM REM WGHT 0.047800 2.932000 FVAR 0.40097 FE1 3 0.484436 0.550344 0.260594 11.00000 0.02537 0.02317 = 0.02121 -0.00199 0.00577 0.00366 O5 5 0.411337 0.469950 0.323738 11.00000 0.03723 0.02572 = 0.03186 -0.01000 0.01292 -0.01046 O1 5 0.554238 0.639970 0.196308 11.00000 0.02386 0.04776 = 0.03608 0.00926 0.00748 0.00457 O2 5 0.534201 0.749398 0.094978 11.00000 0.03374 0.07283 = 0.03947 0.01454 0.01835 0.00209 N2 4 0.598074 0.412628 0.296960 11.00000 0.02456 0.02416 = 0.02225 -0.00248 0.00579 0.00098 N5 4 0.378947 0.685396 0.193876 11.00000 0.02415 0.02858 = 0.02586 0.00604 0.00815 0.00593 N3 4 0.518501 0.689778 0.350962 11.00000 0.03111 0.02373 = 0.02842 -0.00424 0.01398 -0.00384 O6 5 0.376581 0.490236 0.423925 11.00000 0.05704 0.04044 = 0.04369 -0.01646 0.03000 -0.02822 N6 4 0.269675 0.806562 0.121712 11.00000 0.02876 0.03176 = 0.02894 0.00825 0.00867 0.01141 AFIX 43 H6 2 0.217402 0.845763 0.103450 11.00000 -1.20000 AFIX 0 O3 5 0.410523 0.883244 0.010322 11.00000 0.05836 0.06099 = 0.03711 0.01803 0.02290 0.00967 AFIX 147 H3 2 0.448316 0.830820 0.035192 11.00000 -1.50000 AFIX 0 N1 4 0.446550 0.388465 0.181415 11.00000 0.02821 0.03334 = 0.02833 -0.00605 0.00221 0.00190 O4 5 0.268916 0.947447 -0.000446 11.00000 0.06071 0.09085 = 0.04518 0.03659 0.01594 0.03282 O7 5 0.383107 0.677836 0.512038 11.00000 0.11001 0.05413 = 0.07400 -0.03364 0.07317 -0.04571 AFIX 147 H7 2 0.380290 0.616400 0.484172 11.00000 -1.50000 AFIX 0 C2 1 0.410271 0.735472 0.141564 11.00000 0.02615 0.02350 = 0.02555 0.00220 0.00727 0.00147 C27 1 0.595911 0.311115 0.250881 11.00000 0.02878 0.02281 = 0.02405 0.00165 0.01385 0.00350 N4 4 0.529626 0.850423 0.427662 11.00000 0.07767 0.03266 = 0.05172 -0.02553 0.04224 -0.03021 AFIX 43 H4 2 0.545286 0.924968 0.449763 11.00000 -1.20000 AFIX 0 C23 1 0.669000 0.219598 0.262027 11.00000 0.03297 0.02962 = 0.03316 0.00566 0.01854 0.00343 C5 1 0.293231 0.730309 0.180141 11.00000 0.02882 0.02577 = 0.03237 0.00249 0.01252 0.00528 C10 1 0.468432 0.655436 0.394476 11.00000 0.03129 0.02525 = 0.02617 -0.00188 0.01343 -0.00611 C9 1 0.415526 0.528446 0.380142 11.00000 0.02781 0.02266 = 0.03277 -0.00250 0.00981 -0.00577 C28 1 0.516724 0.299861 0.189312 11.00000 0.02877 0.02603 = 0.02518 -0.00256 0.00874 -0.00278 C3 1 0.342962 0.811460 0.096030 11.00000 0.03470 0.02822 = 0.02480 0.00268 0.00878 0.00468 C13 1 0.555550 0.808903 0.372585 11.00000 0.04932 0.02891 = 0.03970 -0.00947 0.02226 -0.01478 C20 1 0.513352 0.199166 0.139809 11.00000 0.04685 0.03386 = 0.03052 -0.00811 0.01663 -0.00447 C26 1 0.670063 0.422833 0.354404 11.00000 0.03145 0.03024 = 0.02479 0.00030 0.00419 -0.00205 AFIX 43 H26 2 0.670792 0.490891 0.386386 11.00000 -1.20000 AFIX 0 C25 1 0.745387 0.335801 0.369361 11.00000 0.02774 0.04305 = 0.03144 0.01066 0.00430 0.00160 AFIX 43 H25 2 0.795219 0.346333 0.410358 11.00000 -1.20000 AFIX 0 C11 1 0.474349 0.755127 0.442934 11.00000 0.05494 0.02985 = 0.04371 -0.01448 0.03065 -0.01921 C24 1 0.744846 0.235894 0.323343 11.00000 0.02883 0.04059 = 0.04406 0.01300 0.01433 0.01339 AFIX 43 H24 2 0.794892 0.177949 0.332423 11.00000 -1.20000 AFIX 0 C4 1 0.337307 0.885897 0.030685 11.00000 0.04676 0.04231 = 0.02959 0.00744 0.01248 0.00328 C6 1 0.230815 0.700641 0.222216 11.00000 0.03469 0.03649 = 0.04765 0.01432 0.01937 0.01393 AFIX 23 H6A 2 0.185483 0.771693 0.214875 11.00000 -1.20000 H6B 2 0.266668 0.699948 0.271987 11.00000 -1.20000 AFIX 0 C1 1 0.506605 0.706956 0.144104 11.00000 0.03268 0.03460 = 0.03167 -0.00351 0.01196 -0.00335 C22 1 0.662759 0.116991 0.211141 11.00000 0.05119 0.03475 = 0.04779 -0.00065 0.02751 0.01461 AFIX 43 H22 2 0.710797 0.055902 0.218384 11.00000 -1.20000 AFIX 0 C21 1 0.588695 0.106730 0.152783 11.00000 0.06582 0.03377 = 0.04319 -0.01173 0.02981 0.00584 AFIX 43 H21 2 0.586345 0.038736 0.120416 11.00000 -1.20000 AFIX 0 C18 1 0.364386 0.280969 0.072870 11.00000 0.05718 0.05902 = 0.03277 -0.01381 -0.00948 -0.00152 AFIX 43 H18 2 0.311465 0.276892 0.033730 11.00000 -1.20000 AFIX 0 O8 5 0.444557 0.878304 0.532742 11.00000 0.19715 0.06064 = 0.11612 -0.06093 0.12765 -0.06623 C19 1 0.435020 0.192828 0.080141 11.00000 0.06578 0.04268 = 0.03828 -0.02120 0.01389 -0.00856 AFIX 43 H19 2 0.431008 0.128746 0.045475 11.00000 -1.20000 AFIX 0 C17 1 0.372919 0.376657 0.124847 11.00000 0.03578 0.05211 = 0.03980 -0.01054 -0.00358 0.00590 AFIX 43 H17 2 0.324206 0.435790 0.119661 11.00000 -1.20000 AFIX 0 C14 1 0.616449 0.884606 0.341614 11.00000 0.07577 0.04271 = 0.06207 -0.01214 0.04485 -0.02676 AFIX 23 H14A 2 0.603953 0.979368 0.343948 11.00000 -1.20000 H14B 2 0.601295 0.860660 0.292106 11.00000 -1.20000 AFIX 0 C12 1 0.433025 0.774365 0.499547 11.00000 0.10347 0.04885 = 0.06721 -0.03007 0.06627 -0.03174 C7 1 0.181221 0.568748 0.203504 11.00000 0.06494 0.05550 = 0.09728 -0.00194 0.04846 -0.00992 AFIX 23 H7A 2 0.226172 0.496837 0.213594 11.00000 -1.20000 H7B 2 0.147868 0.567097 0.153250 11.00000 -1.20000 AFIX 0 C15 1 0.718004 0.860801 0.377320 11.00000 0.08171 0.05707 = 0.13934 0.00062 0.06390 -0.00974 AFIX 23 H15A 2 0.728884 0.765088 0.381752 11.00000 -1.20000 H15B 2 0.751711 0.895762 0.347297 11.00000 -1.20000 AFIX 0 C8 1 0.114251 0.545407 0.244258 11.00000 0.08522 0.07064 = 0.13312 0.01318 0.06579 -0.00869 AFIX 137 H8A 2 0.063375 0.606440 0.227986 11.00000 -1.50000 H8B 2 0.145105 0.559853 0.293721 11.00000 -1.50000 H8C 2 0.091771 0.455114 0.236930 11.00000 -1.50000 AFIX 0 C16 1 0.754442 0.920819 0.446380 11.00000 0.10579 0.12101 = 0.10418 0.01573 -0.02065 -0.00962 AFIX 137 H16A 2 0.732523 1.011184 0.444728 11.00000 -1.50000 H16B 2 0.820642 0.920843 0.460556 11.00000 -1.50000 H16C 2 0.734410 0.870374 0.479818 11.00000 -1.50000 AFIX 0 HKLF 4 REM zh-4fe_a.res in P2(1)/n REM R1 = 0.0680 for 4456 Fo > 4sig(Fo) and 0.1177 for all 6615 data REM 392 parameters refined using 0 restraints END WGHT 0.0478 2.9385 REM Highest difference peak 0.755, deepest hole -0.380, 1-sigma level 0.078 Q1 1 0.8144 0.9206 0.4033 11.00000 0.05 0.76 Q2 1 0.4724 0.8622 0.5417 11.00000 0.05 0.37 Q3 1 0.1382 0.6179 0.1639 11.00000 0.05 0.36 Q4 1 0.4839 0.7819 0.0463 11.00000 0.05 0.32 Q5 1 0.2217 0.8852 -0.0016 11.00000 0.05 0.32 Q6 1 0.7446 0.8157 0.4224 11.00000 0.05 0.30 Q7 1 0.4782 0.8069 0.4223 11.00000 0.05 0.30 Q8 1 0.4036 0.9020 0.4881 11.00000 0.05 0.30 Q9 1 0.4163 0.8700 0.5568 11.00000 0.05 0.28 Q10 1 0.6147 0.6343 0.2296 11.00000 0.05 0.28 Q11 1 0.4788 0.6940 0.4342 11.00000 0.05 0.27 Q12 1 0.4407 0.7726 0.4525 11.00000 0.05 0.27 Q13 1 0.4813 0.4354 0.0297 11.00000 0.05 0.27 Q14 1 0.5000 1.0000 0.5000 10.50000 0.05 0.26 Q15 1 0.4986 0.7629 0.3455 11.00000 0.05 0.26 Q16 1 0.4228 0.7172 0.4975 11.00000 0.05 0.26 Q17 1 0.5231 0.8432 0.3900 11.00000 0.05 0.25 Q18 1 0.3150 0.4559 0.4652 11.00000 0.05 0.25 Q19 1 0.8177 0.8916 0.4844 11.00000 0.05 0.25 Q20 1 0.3578 0.9520 0.4880 11.00000 0.05 0.25 ; _shelx_res_checksum 64069 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -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 Fe1 Fe 0.48444(3) 0.55034(4) 0.26059(2) 0.02363(14) Uani 1 1 d . O5 O 0.41134(15) 0.4700(2) 0.32374(11) 0.0311(5) Uani 1 1 d . O1 O 0.55424(15) 0.6400(2) 0.19631(12) 0.0364(6) Uani 1 1 d . O2 O 0.53420(16) 0.7494(3) 0.09498(13) 0.0471(7) Uani 1 1 d . N2 N 0.59807(17) 0.4126(2) 0.29696(13) 0.0240(6) Uani 1 1 d . N5 N 0.37895(17) 0.6854(3) 0.19388(13) 0.0261(6) Uani 1 1 d . N3 N 0.51850(17) 0.6898(3) 0.35096(13) 0.0267(6) Uani 1 1 d . O6 O 0.37658(17) 0.4902(2) 0.42392(13) 0.0438(7) Uani 1 1 d . N6 N 0.26968(18) 0.8066(3) 0.12171(13) 0.0299(6) Uani 1 1 d . H6 H 0.217402 0.845763 0.103450 0.036 Uiso 1 1 calc R O3 O 0.41052(19) 0.8832(3) 0.01032(13) 0.0503(7) Uani 1 1 d . H3 H 0.448316 0.830820 0.035192 0.075 Uiso 1 1 calc GR N1 N 0.44655(18) 0.3885(3) 0.18141(14) 0.0315(6) Uani 1 1 d . O4 O 0.2689(2) 0.9474(3) -0.00045(14) 0.0658(9) Uani 1 1 d . O7 O 0.3831(2) 0.6778(3) 0.51204(16) 0.0690(10) Uani 1 1 d . H7 H 0.380290 0.616400 0.484172 0.104 Uiso 1 1 calc GR C2 C 0.4103(2) 0.7355(3) 0.14156(16) 0.0253(7) Uani 1 1 d . C27 C 0.5959(2) 0.3111(3) 0.25088(15) 0.0239(7) Uani 1 1 d . N4 N 0.5296(2) 0.8504(3) 0.42766(16) 0.0489(9) Uani 1 1 d . H4 H 0.545286 0.924968 0.449763 0.059 Uiso 1 1 calc R C23 C 0.6690(2) 0.2196(3) 0.26203(17) 0.0300(7) Uani 1 1 d . C5 C 0.2932(2) 0.7303(3) 0.18014(17) 0.0283(7) Uani 1 1 d . C10 C 0.4684(2) 0.6554(3) 0.39448(16) 0.0266(7) Uani 1 1 d . C9 C 0.4155(2) 0.5284(3) 0.38014(17) 0.0277(7) Uani 1 1 d . C28 C 0.5167(2) 0.2999(3) 0.18931(16) 0.0266(7) Uani 1 1 d . C3 C 0.3430(2) 0.8115(3) 0.09603(16) 0.0294(7) Uani 1 1 d . C13 C 0.5556(3) 0.8089(3) 0.37259(18) 0.0374(8) Uani 1 1 d . C20 C 0.5134(2) 0.1992(3) 0.13981(17) 0.0360(8) Uani 1 1 d . C26 C 0.6701(2) 0.4228(3) 0.35440(16) 0.0299(7) Uani 1 1 d . H26 H 0.670792 0.490891 0.386386 0.036 Uiso 1 1 calc R C25 C 0.7454(2) 0.3358(4) 0.36936(18) 0.0353(8) Uani 1 1 d . H25 H 0.795219 0.346333 0.410358 0.042 Uiso 1 1 calc R C11 C 0.4743(3) 0.7551(3) 0.44293(19) 0.0393(9) Uani 1 1 d . C24 C 0.7448(2) 0.2359(4) 0.32334(19) 0.0372(8) Uani 1 1 d . H24 H 0.794892 0.177949 0.332423 0.045 Uiso 1 1 calc R C4 C 0.3373(3) 0.8859(4) 0.03068(18) 0.0395(9) Uani 1 1 d . C6 C 0.2308(2) 0.7006(3) 0.22222(19) 0.0381(9) Uani 1 1 d . H6A H 0.185483 0.771693 0.214875 0.046 Uiso 1 1 calc R H6B H 0.266668 0.699948 0.271987 0.046 Uiso 1 1 calc R C1 C 0.5066(2) 0.7070(3) 0.14410(17) 0.0326(8) Uani 1 1 d . C22 C 0.6628(3) 0.1170(4) 0.2111(2) 0.0418(9) Uani 1 1 d . H22 H 0.710797 0.055902 0.218384 0.050 Uiso 1 1 calc R C21 C 0.5887(3) 0.1067(4) 0.1528(2) 0.0446(10) Uani 1 1 d . H21 H 0.586345 0.038736 0.120416 0.054 Uiso 1 1 calc R C18 C 0.3644(3) 0.2810(4) 0.0729(2) 0.0552(11) Uani 1 1 d . H18 H 0.311465 0.276892 0.033730 0.066 Uiso 1 1 calc R O8 O 0.4446(3) 0.8783(3) 0.5327(2) 0.1063(16) Uani 1 1 d . C19 C 0.4350(3) 0.1928(4) 0.0801(2) 0.0495(10) Uani 1 1 d . H19 H 0.431008 0.128746 0.045475 0.059 Uiso 1 1 calc R C17 C 0.3729(3) 0.3767(4) 0.12485(19) 0.0462(10) Uani 1 1 d . H17 H 0.324206 0.435790 0.119661 0.055 Uiso 1 1 calc R C14 C 0.6164(3) 0.8846(4) 0.3416(2) 0.0548(12) Uani 1 1 d . H14A H 0.603953 0.979368 0.343948 0.066 Uiso 1 1 calc R H14B H 0.601295 0.860660 0.292106 0.066 Uiso 1 1 calc R C12 C 0.4330(3) 0.7744(4) 0.4995(2) 0.0640(14) Uani 1 1 d . C7 C 0.1812(3) 0.5687(4) 0.2035(3) 0.0672(13) Uani 1 1 d . H7A H 0.226172 0.496837 0.213594 0.081 Uiso 1 1 calc R H7B H 0.147868 0.567097 0.153250 0.081 Uiso 1 1 calc R C15 C 0.7180(4) 0.8608(5) 0.3773(3) 0.0859(18) Uani 1 1 d . H15A H 0.728884 0.765088 0.381752 0.103 Uiso 1 1 calc R H15B H 0.751711 0.895762 0.347297 0.103 Uiso 1 1 calc R C8 C 0.1143(4) 0.5454(5) 0.2443(3) 0.0890(17) Uani 1 1 d . H8A H 0.063375 0.606440 0.227986 0.134 Uiso 1 1 calc GR H8B H 0.145105 0.559853 0.293721 0.134 Uiso 1 1 calc GR H8C H 0.091771 0.455114 0.236930 0.134 Uiso 1 1 calc GR C16 C 0.7544(5) 0.9208(7) 0.4464(3) 0.123(3) Uani 1 1 d . H16A H 0.732523 1.011184 0.444728 0.184 Uiso 1 1 calc GR H16B H 0.820642 0.920843 0.460556 0.184 Uiso 1 1 calc GR H16C H 0.734410 0.870374 0.479818 0.184 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 Fe1 0.0254(2) 0.0232(2) 0.0212(2) -0.0020(2) 0.00577(17) 0.0037(2) O5 0.0372(13) 0.0257(12) 0.0319(12) -0.0100(10) 0.0129(10) -0.0105(10) O1 0.0239(12) 0.0478(15) 0.0361(13) 0.0093(12) 0.0075(10) 0.0046(11) O2 0.0337(14) 0.0728(19) 0.0395(14) 0.0145(14) 0.0183(12) 0.0021(13) N2 0.0246(14) 0.0242(14) 0.0223(13) -0.0025(11) 0.0058(11) 0.0010(11) N5 0.0242(14) 0.0286(14) 0.0259(14) 0.0060(12) 0.0081(11) 0.0059(11) N3 0.0311(15) 0.0237(14) 0.0284(14) -0.0042(12) 0.0140(12) -0.0038(12) O6 0.0570(16) 0.0404(14) 0.0437(14) -0.0165(12) 0.0300(13) -0.0282(13) N6 0.0288(15) 0.0318(15) 0.0289(15) 0.0082(12) 0.0087(12) 0.0114(12) O3 0.0584(18) 0.0610(18) 0.0371(15) 0.0180(13) 0.0229(14) 0.0097(14) N1 0.0282(15) 0.0333(16) 0.0283(15) -0.0060(13) 0.0022(12) 0.0019(13) O4 0.0607(19) 0.091(2) 0.0452(16) 0.0366(17) 0.0159(14) 0.0328(18) O7 0.110(3) 0.0541(18) 0.074(2) -0.0336(16) 0.073(2) -0.0457(18) C2 0.0261(17) 0.0235(16) 0.0256(16) 0.0022(14) 0.0073(13) 0.0015(14) C27 0.0288(17) 0.0228(16) 0.0240(16) 0.0017(13) 0.0138(13) 0.0035(13) N4 0.078(2) 0.0327(17) 0.052(2) -0.0255(15) 0.0422(18) -0.0302(16) C23 0.0330(18) 0.0296(18) 0.0332(18) 0.0057(15) 0.0185(15) 0.0034(15) C5 0.0288(18) 0.0258(17) 0.0324(18) 0.0025(14) 0.0125(14) 0.0053(14) C10 0.0313(17) 0.0253(17) 0.0262(16) -0.0019(14) 0.0134(14) -0.0061(14) C9 0.0278(17) 0.0227(17) 0.0328(18) -0.0025(14) 0.0098(14) -0.0058(14) C28 0.0288(17) 0.0260(17) 0.0252(16) -0.0026(14) 0.0087(14) -0.0028(14) C3 0.0347(19) 0.0282(17) 0.0248(16) 0.0027(14) 0.0088(14) 0.0047(15) C13 0.049(2) 0.0289(18) 0.040(2) -0.0095(16) 0.0223(17) -0.0148(17) C20 0.047(2) 0.0339(19) 0.0305(19) -0.0081(16) 0.0166(17) -0.0045(17) C26 0.0315(18) 0.0302(18) 0.0248(16) 0.0003(14) 0.0042(14) -0.0021(15) C25 0.0277(18) 0.043(2) 0.0314(18) 0.0107(17) 0.0043(15) 0.0016(16) C11 0.055(2) 0.0299(18) 0.044(2) -0.0145(16) 0.0306(18) -0.0192(17) C24 0.0288(18) 0.041(2) 0.044(2) 0.0130(18) 0.0143(16) 0.0134(16) C4 0.047(2) 0.042(2) 0.0296(19) 0.0074(17) 0.0125(17) 0.0033(19) C6 0.0347(19) 0.036(2) 0.048(2) 0.0143(17) 0.0194(17) 0.0139(16) C1 0.0327(19) 0.0346(19) 0.0317(19) -0.0035(16) 0.0120(16) -0.0033(16) C22 0.051(2) 0.035(2) 0.048(2) -0.0007(18) 0.028(2) 0.0146(18) C21 0.066(3) 0.034(2) 0.043(2) -0.0117(18) 0.030(2) 0.0058(19) C18 0.057(3) 0.059(3) 0.033(2) -0.014(2) -0.0095(19) -0.002(2) O8 0.197(4) 0.061(2) 0.116(3) -0.061(2) 0.128(3) -0.066(3) C19 0.066(3) 0.043(2) 0.038(2) -0.0212(18) 0.014(2) -0.009(2) C17 0.036(2) 0.052(2) 0.040(2) -0.0105(19) -0.0036(17) 0.0059(18) C14 0.076(3) 0.043(2) 0.062(3) -0.012(2) 0.045(2) -0.027(2) C12 0.103(4) 0.049(3) 0.067(3) -0.030(2) 0.066(3) -0.032(3) C7 0.065(3) 0.056(3) 0.097(4) -0.002(3) 0.048(3) -0.010(2) C15 0.082(4) 0.057(3) 0.139(6) 0.001(3) 0.064(4) -0.010(3) C8 0.085(4) 0.071(3) 0.133(5) 0.013(3) 0.066(4) -0.009(3) C16 0.106(5) 0.121(6) 0.104(5) 0.016(5) -0.021(4) -0.010(4) 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O5 Fe1 O1 177.21(9) O5 Fe1 N2 94.53(9) O5 Fe1 N5 99.88(9) O5 Fe1 N3 77.49(9) O5 Fe1 N1 94.60(9) O1 Fe1 N2 88.12(9) O1 Fe1 N5 77.65(9) O1 Fe1 N3 101.21(9) O1 Fe1 N1 86.84(10) N2 Fe1 N5 162.70(9) N2 Fe1 N3 99.91(10) N2 Fe1 N1 76.89(10) N5 Fe1 N3 92.57(10) N5 Fe1 N1 92.35(10) N1 Fe1 N3 171.31(10) C9 O5 Fe1 118.49(19) C1 O1 Fe1 117.2(2) C27 N2 Fe1 113.83(19) C26 N2 Fe1 127.3(2) C26 N2 C27 118.7(3) C2 N5 Fe1 108.59(19) C5 N5 Fe1 144.9(2) C5 N5 C2 106.2(3) C10 N3 Fe1 108.95(19) C13 N3 Fe1 142.8(2) C13 N3 C10 106.5(3) C5 N6 C3 108.6(3) C28 N1 Fe1 112.07(19) C17 N1 Fe1 129.5(2) C17 N1 C28 117.8(3) N5 C2 C1 119.0(3) C3 C2 N5 109.7(3) C3 C2 C1 131.2(3) N2 C27 C23 122.0(3) N2 C27 C28 118.1(3) C23 C27 C28 119.9(3) C13 N4 C11 109.2(3) C27 C23 C22 119.0(3) C24 C23 C27 117.3(3) C24 C23 C22 123.7(3) N5 C5 N6 110.3(3) N5 C5 C6 125.7(3) N6 C5 C6 124.0(3) N3 C10 C9 118.2(3) N3 C10 C11 109.8(3) C11 C10 C9 131.9(3) O5 C9 O6 125.4(3) O5 C9 C10 116.3(3) O6 C9 C10 118.3(3) N1 C28 C27 118.0(3) N1 C28 C20 122.3(3) C20 C28 C27 119.7(3) N6 C3 C4 121.3(3) C2 C3 N6 105.3(3) C2 C3 C4 133.4(3) N3 C13 N4 109.6(3) N3 C13 C14 125.6(3) N4 C13 C14 124.8(3) C28 C20 C21 119.2(3) C19 C20 C28 117.6(3) C19 C20 C21 123.1(3) N2 C26 C25 122.8(3) C24 C25 C26 119.1(3) N4 C11 C10 104.8(3) N4 C11 C12 121.7(3) C10 C11 C12 133.5(3) C25 C24 C23 120.2(3) O3 C4 C3 116.6(3) O4 C4 O3 122.7(3) O4 C4 C3 120.7(3) C5 C6 C7 113.4(3) O1 C1 C2 116.0(3) O2 C1 O1 125.2(3) O2 C1 C2 118.8(3) C21 C22 C23 121.3(3) C22 C21 C20 120.9(3) C19 C18 C17 118.8(3) C18 C19 C20 119.8(3) N1 C17 C18 123.6(4) C13 C14 C15 114.3(4) O7 C12 C11 118.0(3) O8 C12 O7 121.5(4) O8 C12 C11 120.5(4) C6 C7 C8 112.0(4) C16 C15 C14 114.4(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Fe1 O5 2.090(2) Fe1 O1 2.109(2) Fe1 N2 2.153(2) Fe1 N5 2.198(3) Fe1 N3 2.206(3) Fe1 N1 2.206(3) O5 C9 1.251(4) O1 C1 1.258(4) O2 C1 1.257(4) N2 C27 1.362(4) N2 C26 1.317(4) N5 C2 1.373(4) N5 C5 1.328(4) N3 C10 1.370(4) N3 C13 1.330(4) O6 C9 1.261(4) N6 C5 1.342(4) N6 C3 1.372(4) O3 C4 1.305(4) N1 C28 1.361(4) N1 C17 1.322(4) O4 C4 1.202(4) O7 C12 1.302(5) C2 C3 1.366(4) C2 C1 1.484(4) C27 C23 1.405(4) C27 C28 1.429(4) N4 C13 1.346(4) N4 C11 1.369(4) C23 C24 1.403(5) C23 C22 1.424(5) C5 C6 1.486(4) C10 C9 1.483(4) C10 C11 1.371(4) C28 C20 1.399(4) C3 C4 1.479(5) C13 C14 1.478(5) C20 C21 1.434(5) C20 C19 1.396(5) C26 C25 1.397(5) C25 C24 1.354(5) C11 C12 1.470(5) C6 C7 1.507(5) C22 C21 1.346(5) C18 C19 1.365(6) C18 C17 1.386(5) O8 C12 1.214(5) C14 C15 1.507(7) C7 C8 1.513(6) C15 C16 1.443(8) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N6 H6 O6 0.86 1.99 2.811(3) 160.2 2 O3 H3 O2 0.82 1.68 2.488(4) 169.2 . O7 H7 O6 0.82 1.73 2.550(3) 178.0 . N4 H4 O8 0.86 1.99 2.816(4) 159.6 3_676