#------------------------------------------------------------------------------ #$Date: 2023-01-19 01:54:30 +0200 (Thu, 19 Jan 2023) $ #$Revision: 280424 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/71/21/7712155.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_7712155 loop_ _publ_author_name 'Tzani, Sofia' 'Pissas, Michael' 'Psycharis, Vassilis' 'Pantazis, Dimitrios A.' 'Sanakis, Yiannis' 'Raptopoulou, Catherine P.' _publ_section_title ; Synthesis and structural, magnetic and spectroscopic characterization of iron(iii) complexes with in situ formed ligands from methyl-2-pyridyl ketone transformations ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D2DT03944C _journal_year 2023 _chemical_formula_sum 'C24 H32.4 Cl4 Fe3 N3 O8.2' _chemical_formula_weight 803.48 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/6 _audit_update_record ; 2022-12-07 deposited with the CCDC. 2023-01-11 downloaded from the CCDC. ; _cell_angle_alpha 112.9060(10) _cell_angle_beta 101.9300(10) _cell_angle_gamma 105.5150(10) _cell_formula_units_Z 2 _cell_length_a 11.0768(2) _cell_length_b 12.9640(2) _cell_length_c 13.9148(3) _cell_measurement_reflns_used 17569 _cell_measurement_temperature 160(2) _cell_measurement_theta_max 71.88 _cell_measurement_theta_min 6.52 _cell_volume 1661.22(6) _computing_cell_refinement 'CrystalClear, Rigaku MSC, 2005' _computing_data_collection 'CrystalClear, Rigaku MSC, 2005' _computing_data_reduction 'CrystalClear, Rigaku MSC, 2005' _computing_molecular_graphics 'Diamond ver.3.1' _computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)' _computing_structure_solution 'SHELXL-2014/6 (Sheldrick, 2014)' _diffrn_ambient_temperature 160(2) _diffrn_measured_fraction_theta_full 0.834 _diffrn_measured_fraction_theta_max 0.948 _diffrn_measurement_device_type 'Rigaku R-AXIS SPIDER IPDS' _diffrn_measurement_method '\q scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0830 _diffrn_reflns_av_unetI/netI 0.0870 _diffrn_reflns_Laue_measured_fraction_full 0.834 _diffrn_reflns_Laue_measured_fraction_max 0.948 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 21930 _diffrn_reflns_point_group_measured_fraction_full 0.834 _diffrn_reflns_point_group_measured_fraction_max 0.948 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 62.491 _diffrn_reflns_theta_min 6.525 _exptl_absorpt_coefficient_mu 13.743 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.334 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'CrystalClear, Rigaku MSC, 2005' _exptl_crystal_colour orange-brown _exptl_crystal_density_diffrn 1.606 _exptl_crystal_description parallelepiped _exptl_crystal_F_000 818 _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _refine_diff_density_max 0.836 _refine_diff_density_min -0.981 _refine_diff_density_rms 0.147 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 384 _refine_ls_number_reflns 5011 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.123 _refine_ls_R_factor_all 0.0911 _refine_ls_R_factor_gt 0.0557 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+10.0246P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1115 _refine_ls_wR_factor_ref 0.1591 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3356 _reflns_number_total 5011 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d2dt03944c2.cif _cod_data_source_block shelxl_CCDC1 _cod_original_cell_volume 1661.21(6) _cod_original_formula_sum 'C24 H32.40 Cl4 Fe3 N3 O8.20' _cod_database_code 7712155 _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. ; _shelxl_version_number 2014/6 _shelx_res_file ; TITL *** KPST218 *** P-1 REM [Fe3Cl4(bicine)({pyC(CH3)O-CH2-C(OCH3)O-py}].Me2CO.0.2H2O REM LIGAND TRANSFORMED FROM pyCOCH3 CELL 1.54178 11.0768 12.9640 13.9148 112.906 101.930 105.515 ZERR 2.00 0.0002 0.0002 0.0003 0.001 0.001 0.001 LATT 1 SFAC C H N O FE CL UNIT 48 64.8 6 16.4 6 8 OMIT -2.00 125.00 OMIT -3 5 11 ! -2.69 731.65 7.58 0.121 0.9 OMIT -10 6 4 ! -2.28 718.27 7.49 0.120 1.0 OMIT -3 2 13 ! -2.86 458.17 5.98 0.096 0.9 OMIT -9 -1 5 ! -2.39 415.11 5.86 0.091 1.1 OMIT -8 6 4 ! -1.03 376.39 5.75 0.087 1.2 OMIT 4 -9 8 ! -1.24 375.81 5.64 0.087 1.2 OMIT -5 3 13 ! 0.00 333.07 5.48 0.082 0.8 OMIT 0 -2 1 ! 327.14 43.74 5.47 0.030 6.2 OMIT 5 -12 8 ! -6.90 373.35 5.25 0.086 1.0 OMIT -1 -10 4 ! 3.30 324.29 5.23 0.080 1.1 OMIT -10 7 8 ! -0.36 325.64 5.20 0.081 0.8 OMIT -8 5 2 ! 2.88 325.28 5.19 0.081 1.3 OMIT 6 -14 2 ! -0.28 306.49 5.18 0.078 0.8 OMIT -7 -2 1 ! 2.27 303.50 5.13 0.078 1.3 OMIT -9 5 6 ! -1.48 374.71 5.07 0.087 1.0 OMIT 9 -10 5 ! -15.64 361.64 4.99 0.085 0.9 OMIT 8 -5 7 ! -5.61 318.14 4.98 0.080 1.0 OMIT 4 -4 12 ! 1.08 288.74 4.90 0.076 0.9 OMIT 8 -10 5 ! 2.44 323.95 4.89 0.080 1.0 OMIT -11 5 0 ! -3.59 296.64 4.86 0.077 0.9 OMIT 5 -9 7 ! -7.32 311.09 4.81 0.079 1.2 OMIT -3 11 0 ! 0.52 268.08 4.78 0.073 1.0 OMIT 6 -13 6 ! 0.85 332.83 4.75 0.082 0.9 OMIT 0 11 1 ! -0.88 296.35 4.67 0.077 0.9 OMIT -10 0 11 ! 17.10 298.71 4.65 0.077 0.9 OMIT -10 0 3 ! -1.42 267.18 4.65 0.073 1.0 OMIT 9 -3 7 ! 2.39 272.39 4.64 0.074 0.8 OMIT -10 0 5 ! -2.80 252.41 4.63 0.071 1.0 OMIT -9 -1 7 ! 3.01 272.00 4.62 0.074 1.1 OMIT -10 3 4 ! 7.07 273.58 4.55 0.074 1.1 OMIT -7 -7 4 ! -11.53 288.37 4.54 0.076 1.0 OMIT 6 -9 8 ! -2.64 286.30 4.53 0.076 1.0 OMIT -8 0 4 ! -2.29 232.75 4.52 0.068 1.3 OMIT -10 2 4 ! -4.69 237.89 4.51 0.069 1.1 OMIT -7 -6 2 ! 5.30 258.20 4.85 0.072 1.0 OMIT -8 -8 11 ! 2.48 215.68 4.82 0.066 0.8 OMIT -9 3 7 ! 1.94 239.56 4.81 0.069 1.1 OMIT -9 -2 4 ! -10.17 255.93 4.74 0.072 1.1 OMIT 7 -9 1 ! -0.76 230.01 4.74 0.068 1.2 OMIT -12 5 2 ! 1.73 233.43 4.67 0.068 0.9 OMIT -9 0 7 ! -2.67 196.82 4.62 0.063 1.1 OMIT 9 1 4 ! -4.13 215.67 4.60 0.066 0.9 OMIT 12 -6 1 ! 50.56 356.28 4.56 0.084 0.8 OMIT 9 -7 4 ! 0.56 231.95 4.55 0.068 1.0 OMIT -8 -1 3 ! 3.72 215.00 4.46 0.066 1.2 OMIT 4 -5 12 ! 9.41 246.65 4.44 0.070 0.9 OMIT 5 -11 7 ! 1.08 222.63 4.77 0.067 1.0 OMIT 4 -10 6 ! -3.13 223.81 4.75 0.067 1.2 OMIT -11 5 1 ! -1.53 200.77 4.62 0.063 1.0 OMIT -7 -7 3 ! -2.79 186.46 4.60 0.061 0.9 OMIT -4 4 8 ! -0.11 175.02 4.57 0.059 1.2 OMIT 6 -11 8 ! -2.19 201.92 4.54 0.064 1.0 OMIT 7 -14 5 ! -0.40 178.71 4.50 0.060 0.8 FMAP 2 PLAN -20 ACTA BOND $H HTAB L.S. 4 TEMP -113.00 WGHT 0.032900 10.024600 FVAR 2.14136 FE1 5 0.174880 0.120832 0.864175 11.00000 0.02716 0.01606 = 0.01146 0.00703 0.00916 0.00632 FE2 5 0.252637 0.228342 0.708389 11.00000 0.02035 0.02041 = 0.00632 0.00680 0.00456 0.00735 FE3 5 0.121722 0.367309 0.607150 11.00000 0.03212 0.02819 = 0.01035 0.00907 0.00284 0.01127 CL1 6 -0.021470 -0.016286 0.826867 11.00000 0.04223 0.03157 = 0.02518 0.01166 0.01353 -0.00551 CL2 6 0.342711 0.087018 0.947911 11.00000 0.04795 0.03640 = 0.02272 0.01436 0.00844 0.01992 CL3 6 -0.097656 0.321447 0.553185 11.00000 0.03612 0.02915 = 0.04133 0.00438 -0.00704 0.01163 CL4 6 0.201071 0.403235 0.484876 11.00000 0.09247 0.06715 = 0.03137 0.03696 0.03299 0.04178 N1 3 0.179239 0.257391 1.013345 11.00000 0.04355 0.01427 = 0.01190 0.00624 0.01188 0.00505 N2 3 0.164172 0.546023 0.723961 11.00000 0.03295 0.02964 = 0.01709 0.01380 0.00377 0.00761 N3 3 0.315008 0.114524 0.578234 11.00000 0.02068 0.03094 = 0.00676 0.00654 -0.00089 0.01219 O1 4 0.179061 0.256822 0.832237 11.00000 0.02464 0.01175 = 0.01155 0.00505 0.00671 0.00685 O2 4 0.261959 0.394984 0.735910 11.00000 0.02787 0.01391 = 0.01176 0.00901 0.00525 0.00494 O3 4 0.068944 0.389149 0.857746 11.00000 0.02705 0.02941 = 0.02814 0.01149 0.00918 0.00380 O4 4 0.120137 0.202261 0.572158 11.00000 0.02417 0.02572 = 0.00364 0.00277 0.00239 0.00931 O5 4 0.198177 0.073993 0.719557 11.00000 0.02779 0.01894 = 0.01271 0.00515 0.01060 0.01250 O6 4 0.441903 0.285674 0.793400 11.00000 0.02936 0.01701 = 0.02083 0.00869 0.00667 0.01177 O7 4 0.634867 0.265372 0.799973 11.00000 0.02133 0.05099 = 0.03431 0.01025 0.00530 0.01232 O8 4 0.496460 0.888711 0.613734 11.00000 0.07969 0.11001 = 0.05232 0.04884 0.03697 0.04596 C1 1 0.179709 0.245071 1.104538 11.00000 0.05530 0.02364 = 0.02660 0.02061 0.02188 0.01764 AFIX 43 H1 2 0.182916 0.172776 1.105040 11.00000 -1.40000 AFIX 0 C2 1 0.175691 0.333889 1.197690 11.00000 0.06819 0.04285 = 0.01799 0.01159 0.02576 0.01289 AFIX 43 H2 2 0.177562 0.323943 1.262042 11.00000 -1.40000 AFIX 0 C3 1 0.168893 0.437520 1.195327 11.00000 0.09687 0.02927 = 0.03603 0.00971 0.04793 0.01523 AFIX 43 H3 2 0.166573 0.500527 1.258519 11.00000 -1.40000 AFIX 0 C4 1 0.165494 0.448945 1.100632 11.00000 0.07560 0.02122 = 0.03752 0.01526 0.03620 0.02533 AFIX 43 H4 2 0.158280 0.518744 1.096799 11.00000 -1.40000 AFIX 0 C5 1 0.172769 0.356940 1.010960 11.00000 0.03168 0.01962 = 0.01888 0.00324 0.01967 0.01000 C6 1 0.178413 0.366401 0.906685 11.00000 0.02700 0.01350 = 0.01613 0.01020 0.00717 0.00783 C7 1 0.303921 0.472144 0.933847 11.00000 0.02619 0.02007 = 0.00403 0.00239 0.00011 0.00577 AFIX 23 H7A 2 0.382308 0.454104 0.959314 11.00000 -1.20000 H7B 2 0.308752 0.545067 0.997321 11.00000 -1.20000 AFIX 0 C8 1 0.317489 0.504364 0.839947 11.00000 0.02062 0.01836 = 0.00604 0.00445 -0.00462 0.00057 C9 1 0.243375 0.585743 0.828061 11.00000 0.02638 0.03077 = 0.01688 0.01122 0.00917 -0.00018 C10 1 0.266372 0.695866 0.914779 11.00000 0.03958 0.02902 = 0.01942 0.01223 -0.00264 0.00791 AFIX 43 H10 2 0.320559 0.720367 0.988465 11.00000 -1.40000 AFIX 0 C11 1 0.208742 0.769808 0.892010 11.00000 0.05902 0.01977 = 0.03883 0.00386 0.00032 0.00663 AFIX 43 H11 2 0.223707 0.846733 0.949958 11.00000 -1.40000 AFIX 0 C12 1 0.128867 0.730783 0.783849 11.00000 0.05230 0.02592 = 0.04602 0.01807 0.00781 0.02202 AFIX 43 H12 2 0.089700 0.781033 0.766384 11.00000 -1.40000 AFIX 0 C13 1 0.107538 0.619303 0.703157 11.00000 0.04771 0.04084 = 0.02519 0.01774 0.00273 0.01635 AFIX 43 H13 2 0.050827 0.591755 0.629451 11.00000 -1.40000 AFIX 0 C14 1 -0.059489 0.294399 0.821902 11.00000 0.02004 0.05578 = 0.07441 0.03407 0.01911 0.02078 AFIX 37 H14A 2 -0.129172 0.311050 0.781665 11.00000 -1.40000 H14B 2 -0.077561 0.291503 0.887037 11.00000 -1.40000 H14C 2 -0.059084 0.216205 0.772627 11.00000 -1.40000 AFIX 0 C15 1 0.464738 0.568132 0.859236 11.00000 10.01509 0.03918 = 0.02255 0.01779 0.00485 0.00321 AFIX 37 H15A 2 0.511597 0.513924 0.859658 11.00000 -1.40000 H15B 2 0.505701 0.642379 0.931004 11.00000 -1.40000 H15C 2 0.471236 0.588940 0.799400 11.00000 -1.40000 AFIX 0 C16 1 0.117655 0.118561 0.466741 11.00000 0.02994 0.03358 = 10.01299 0.01081 0.00003 10.02078 AFIX 23 H16A 2 0.084506 0.140803 0.408933 11.00000 -1.20000 H16B 2 0.056479 0.035452 0.444663 11.00000 -1.20000 AFIX 0 C17 1 0.259041 0.122219 0.476275 11.00000 0.02584 0.03458 = 0.01877 0.01288 0.00890 0.01871 AFIX 23 H17A 2 0.256112 0.053226 0.410090 11.00000 -1.20000 H17B 2 0.315522 0.198667 0.480875 11.00000 -1.20000 AFIX 0 C18 1 0.255215 -0.012640 0.559927 11.00000 0.01691 0.02344 = 0.02184 0.00735 0.00932 0.00776 AFIX 23 H18A 2 0.306825 -0.059754 0.527749 11.00000 -1.20000 H18B 2 0.161759 -0.052886 0.507324 11.00000 -1.20000 AFIX 0 C19 1 0.258701 -0.007719 0.670790 11.00000 0.03866 0.01537 = 0.01754 0.00643 0.01190 0.01342 AFIX 23 H19A 2 0.208805 -0.089490 0.659998 11.00000 -1.20000 H19B 2 0.352225 0.021370 0.719900 11.00000 -1.20000 AFIX 0 C20 1 0.462823 0.162754 0.621908 11.00000 0.03364 0.04361 = 0.02691 0.02164 0.01256 0.02249 AFIX 23 H20A 2 0.498189 0.210959 0.586287 11.00000 -1.20000 H20B 2 0.492796 0.094244 0.602372 11.00000 -1.20000 AFIX 0 C21 1 0.519030 0.241981 0.747433 11.00000 0.03654 0.02724 = 0.01937 0.00442 0.00608 0.00287 C22 1 0.615382 0.986288 0.803973 11.00000 0.06968 0.09106 = 0.05253 0.04076 0.00683 0.02676 AFIX 37 H22A 2 0.649616 1.055483 0.790591 11.00000 -1.40000 H22B 2 0.689906 0.966988 0.833206 11.00000 -1.40000 H22C 2 0.570287 1.006879 0.858196 11.00000 -1.40000 AFIX 0 C23 1 0.519828 0.880495 0.698798 11.00000 0.05366 0.08757 = 0.06128 0.04701 0.03108 0.03991 C24 1 0.462202 0.772468 0.700239 11.00000 0.15382 0.17363 = 0.24534 0.17428 -0.01670 -0.02001 AFIX 37 H24A 2 0.457456 0.704678 0.633307 11.00000 -1.40000 H24B 2 0.371806 0.761963 0.701856 11.00000 -1.40000 H24C 2 0.516568 0.774321 0.766574 11.00000 -1.40000 AFIX 0 O1W 4 0.455282 0.572948 0.447756 10.20000 0.10280 HKLF 4 REM *** KPST218 *** P-1 REM R1 = 0.0557 for 3356 Fo > 4sig(Fo) and 0.0911 for all 5011 data REM 384 parameters refined using 0 restraints END WGHT 0.0325 10.0315 REM Instructions for potential hydrogen bonds EQIV $1 -x, -y, -z+2 HTAB C1 Cl1_$1 EQIV $2 x, y, z+1 HTAB C2 Cl4_$2 EQIV $3 -x, -y+1, -z+1 HTAB C13 Cl4_$3 EQIV $4 x-1, y, z HTAB C14 O7_$4 HTAB C15 O6 EQIV $5 -x, -y, -z+1 HTAB C16 Cl1_$5 HTAB C16 Cl4 EQIV $6 x, y-1, z HTAB C18 O8_$6 HTAB C19 Cl3_$5 EQIV $7 -x+1, -y+1, -z+1 HTAB C20 O8_$7 HTAB C24 O1W REM Highest difference peak 0.836, deepest hole -0.981, 1-sigma level 0.147 Q1 1 0.1350 0.4659 0.6672 11.00000 0.05 0.84 Q2 1 0.1910 0.2240 0.6346 11.00000 0.05 0.73 Q3 1 0.2640 0.0553 0.8732 11.00000 0.05 0.71 Q4 1 0.1945 0.1553 0.7737 11.00000 0.05 0.70 Q5 1 0.2613 0.3191 0.7712 11.00000 0.05 0.69 Q6 1 0.1891 0.2210 0.9303 11.00000 0.05 0.66 Q7 1 0.3875 0.1998 0.7448 11.00000 0.05 0.66 Q8 1 0.2785 0.1593 0.9314 11.00000 0.05 0.65 Q9 1 0.5115 0.7765 0.6201 11.00000 0.05 0.65 Q10 1 0.2810 0.1920 0.7672 11.00000 0.05 0.62 Q11 1 0.0395 0.3433 0.5423 11.00000 0.05 0.61 Q12 1 0.0422 0.2624 0.7685 11.00000 0.05 0.61 Q13 1 0.4415 0.6527 0.5688 11.00000 0.05 0.60 Q14 1 0.4652 0.4419 0.4252 11.00000 0.05 0.60 Q15 1 0.5699 0.5329 0.8330 11.00000 0.05 0.59 Q16 1 0.5714 0.6606 0.6371 11.00000 0.05 0.59 Q17 1 0.1886 0.3799 0.6774 11.00000 0.05 0.58 Q18 1 0.2409 0.1367 0.6373 11.00000 0.05 0.56 Q19 1 0.4216 0.6006 0.4576 11.00000 0.05 0.55 Q20 1 0.2098 0.1508 0.4691 11.00000 0.05 0.55 ; _shelx_res_checksum 95677 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.17488(11) 0.12083(9) 0.86417(8) 0.0181(3) Uani 1 1 d . . . . . Fe2 Fe 0.25264(10) 0.22834(9) 0.70839(8) 0.0157(3) Uani 1 1 d . . . . . Fe3 Fe 0.12172(12) 0.36731(10) 0.60715(9) 0.0245(3) Uani 1 1 d . . . . . Cl1 Cl -0.0215(2) -0.01629(17) 0.82687(15) 0.0379(5) Uani 1 1 d . . . . . Cl2 Cl 0.3427(2) 0.08702(18) 0.94791(15) 0.0354(5) Uani 1 1 d . . . . . Cl3 Cl -0.0977(2) 0.32145(18) 0.55319(17) 0.0437(6) Uani 1 1 d . . . . . Cl4 Cl 0.2011(3) 0.4032(2) 0.48488(17) 0.0543(7) Uani 1 1 d . . . . . N1 N 0.1792(6) 0.2574(5) 1.0133(4) 0.0243(15) Uani 1 1 d . . . . . N2 N 0.1642(6) 0.5460(5) 0.7240(5) 0.0275(15) Uani 1 1 d . . . . . N3 N 0.3150(6) 0.1145(5) 0.5782(4) 0.0208(14) Uani 1 1 d . . . . . O1 O 0.1791(4) 0.2568(4) 0.8322(3) 0.0161(10) Uani 1 1 d . . . . . O2 O 0.2620(4) 0.3950(4) 0.7359(3) 0.0178(11) Uani 1 1 d . . . . . O3 O 0.0689(5) 0.3891(4) 0.8577(4) 0.0307(13) Uani 1 1 d . . . . . O4 O 0.1201(4) 0.2023(4) 0.5722(3) 0.0198(11) Uani 1 1 d . . . . . O5 O 0.1982(5) 0.0740(4) 0.7196(3) 0.0192(11) Uani 1 1 d . . . . . O6 O 0.4419(5) 0.2857(4) 0.7934(4) 0.0222(11) Uani 1 1 d . . . . . O7 O 0.6349(5) 0.2654(5) 0.8000(4) 0.0402(15) Uani 1 1 d . . . . . O8 O 0.4965(7) 0.8887(7) 0.6137(6) 0.072(2) Uani 1 1 d . . . . . C1 C 0.1797(8) 0.2451(7) 1.1045(6) 0.0302(19) Uani 1 1 d . . . . . H1 H 0.1829 0.1728 1.1050 0.042 Uiso 1 1 calc R U . . . C2 C 0.1757(9) 0.3339(8) 1.1977(6) 0.044(2) Uani 1 1 d . . . . . H2 H 0.1776 0.3239 1.2620 0.062 Uiso 1 1 calc R U . . . C3 C 0.1689(10) 0.4375(8) 1.1953(7) 0.054(3) Uani 1 1 d . . . . . H3 H 0.1666 0.5005 1.2585 0.075 Uiso 1 1 calc R U . . . C4 C 0.1655(9) 0.4489(7) 1.1006(7) 0.040(2) Uani 1 1 d . . . . . H4 H 0.1583 0.5187 1.0968 0.056 Uiso 1 1 calc R U . . . C5 C 0.1728(7) 0.3569(6) 1.0110(6) 0.0235(17) Uani 1 1 d . . . . . C6 C 0.1784(7) 0.3664(6) 0.9067(5) 0.0178(16) Uani 1 1 d . . . . . C7 C 0.3039(7) 0.4721(6) 0.9338(5) 0.0196(16) Uani 1 1 d . . . . . H7A H 0.3823 0.4541 0.9593 0.023 Uiso 1 1 calc R U . . . H7B H 0.3088 0.5451 0.9973 0.023 Uiso 1 1 calc R U . . . C8 C 0.3175(7) 0.5044(6) 0.8399(5) 0.0187(16) Uani 1 1 d . . . . . C9 C 0.2434(7) 0.5857(7) 0.8281(6) 0.0270(19) Uani 1 1 d . . . . . C10 C 0.2664(8) 0.6959(7) 0.9148(6) 0.033(2) Uani 1 1 d . . . . . H10 H 0.3206 0.7204 0.9885 0.046 Uiso 1 1 calc R U . . . C11 C 0.2087(9) 0.7698(7) 0.8920(7) 0.048(3) Uani 1 1 d . . . . . H11 H 0.2237 0.8467 0.9500 0.067 Uiso 1 1 calc R U . . . C12 C 0.1289(9) 0.7308(7) 0.7838(7) 0.041(2) Uani 1 1 d . . . . . H12 H 0.0897 0.7810 0.7664 0.058 Uiso 1 1 calc R U . . . C13 C 0.1075(9) 0.6193(8) 0.7032(7) 0.039(2) Uani 1 1 d . . . . . H13 H 0.0508 0.5918 0.6295 0.055 Uiso 1 1 calc R U . . . C14 C -0.0595(8) 0.2944(8) 0.8219(8) 0.047(2) Uani 1 1 d . . . . . H14A H -0.1292 0.3111 0.7817 0.066 Uiso 1 1 calc R U . . . H14B H -0.0776 0.2915 0.8870 0.066 Uiso 1 1 calc R U . . . H14C H -0.0591 0.2162 0.7726 0.066 Uiso 1 1 calc R U . . . C15 C 0.4647(6) 0.5681(7) 0.8592(6) 0.0265(18) Uani 1 1 d . . . . . H15A H 0.5116 0.5139 0.8597 0.037 Uiso 1 1 calc R U . . . H15B H 0.5057 0.6424 0.9310 0.037 Uiso 1 1 calc R U . . . H15C H 0.4712 0.5889 0.7994 0.037 Uiso 1 1 calc R U . . . C16 C 0.1177(7) 0.1186(7) 0.4667(5) 0.0249(16) Uani 1 1 d . . . . . H16A H 0.0845 0.1408 0.4089 0.030 Uiso 1 1 calc R U . . . H16B H 0.0565 0.0355 0.4447 0.030 Uiso 1 1 calc R U . . . C17 C 0.2590(7) 0.1222(7) 0.4763(6) 0.0245(17) Uani 1 1 d . . . . . H17A H 0.2561 0.0532 0.4101 0.029 Uiso 1 1 calc R U . . . H17B H 0.3155 0.1987 0.4809 0.029 Uiso 1 1 calc R U . . . C18 C 0.2552(7) -0.0126(6) 0.5599(6) 0.0215(16) Uani 1 1 d . . . . . H18A H 0.3068 -0.0598 0.5277 0.026 Uiso 1 1 calc R U . . . H18B H 0.1618 -0.0529 0.5073 0.026 Uiso 1 1 calc R U . . . C19 C 0.2587(8) -0.0077(6) 0.6708(5) 0.0233(17) Uani 1 1 d . . . . . H19A H 0.2088 -0.0895 0.6600 0.028 Uiso 1 1 calc R U . . . H19B H 0.3522 0.0214 0.7199 0.028 Uiso 1 1 calc R U . . . C20 C 0.4628(7) 0.1628(7) 0.6219(6) 0.0308(19) Uani 1 1 d . . . . . H20A H 0.4982 0.2110 0.5863 0.037 Uiso 1 1 calc R U . . . H20B H 0.4928 0.0942 0.6024 0.037 Uiso 1 1 calc R U . . . C21 C 0.5190(8) 0.2420(7) 0.7474(6) 0.033(2) Uani 1 1 d . . . . . C22 C 0.6154(11) 0.9863(10) 0.8040(8) 0.072(3) Uani 1 1 d . . . . . H22A H 0.6496 1.0555 0.7906 0.101 Uiso 1 1 calc R U . . . H22B H 0.6899 0.9670 0.8332 0.101 Uiso 1 1 calc R U . . . H22C H 0.5703 1.0069 0.8582 0.101 Uiso 1 1 calc R U . . . C23 C 0.5198(10) 0.8805(11) 0.6988(9) 0.058(3) Uani 1 1 d . . . . . C24 C 0.4622(18) 0.7725(16) 0.7002(17) 0.199(11) Uani 1 1 d . . . . . H24A H 0.4575 0.7047 0.6333 0.278 Uiso 1 1 calc R U . . . H24B H 0.3718 0.7620 0.7019 0.278 Uiso 1 1 calc R U . . . H24C H 0.5166 0.7743 0.7666 0.278 Uiso 1 1 calc R U . . . O1W O 0.455(4) 0.573(4) 0.448(4) 0.103(14) Uiso 0.2 1 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 Fe1 0.0272(6) 0.0161(6) 0.0115(6) 0.0070(5) 0.0092(5) 0.0063(5) Fe2 0.0203(6) 0.0204(6) 0.0063(5) 0.0068(5) 0.0046(4) 0.0074(5) Fe3 0.0321(7) 0.0282(7) 0.0103(6) 0.0091(5) 0.0028(5) 0.0113(6) Cl1 0.0422(12) 0.0316(11) 0.0252(10) 0.0117(9) 0.0135(9) -0.0055(9) Cl2 0.0480(13) 0.0364(11) 0.0227(10) 0.0144(9) 0.0084(9) 0.0199(10) Cl3 0.0361(12) 0.0292(11) 0.0413(12) 0.0044(9) -0.0070(10) 0.0116(10) Cl4 0.0925(19) 0.0672(16) 0.0314(12) 0.0370(12) 0.0330(12) 0.0418(15) N1 0.044(4) 0.014(3) 0.012(3) 0.006(3) 0.012(3) 0.005(3) N2 0.033(4) 0.030(4) 0.017(3) 0.014(3) 0.004(3) 0.008(3) N3 0.021(3) 0.031(4) 0.007(3) 0.007(3) -0.001(2) 0.012(3) O1 0.025(3) 0.012(2) 0.012(2) 0.0050(19) 0.007(2) 0.007(2) O2 0.028(3) 0.014(2) 0.012(2) 0.009(2) 0.005(2) 0.005(2) O3 0.027(3) 0.029(3) 0.028(3) 0.011(2) 0.009(2) 0.004(2) O4 0.024(3) 0.026(3) 0.004(2) 0.003(2) 0.002(2) 0.009(2) O5 0.028(3) 0.019(3) 0.013(2) 0.005(2) 0.011(2) 0.013(2) O6 0.029(3) 0.017(3) 0.021(3) 0.009(2) 0.007(2) 0.012(2) O7 0.021(3) 0.051(4) 0.034(3) 0.010(3) 0.005(3) 0.012(3) O8 0.080(5) 0.110(6) 0.052(5) 0.049(5) 0.037(4) 0.046(5) C1 0.055(5) 0.024(4) 0.027(4) 0.021(4) 0.022(4) 0.018(4) C2 0.068(6) 0.043(5) 0.018(4) 0.012(4) 0.026(4) 0.013(5) C3 0.097(8) 0.029(5) 0.036(5) 0.010(4) 0.048(6) 0.015(5) C4 0.076(7) 0.021(4) 0.038(5) 0.015(4) 0.036(5) 0.025(5) C5 0.032(4) 0.020(4) 0.019(4) 0.003(3) 0.020(3) 0.010(3) C6 0.027(4) 0.013(4) 0.016(4) 0.010(3) 0.007(3) 0.008(3) C7 0.026(4) 0.020(4) 0.004(3) 0.002(3) 0.000(3) 0.006(3) C8 0.021(4) 0.018(4) 0.006(3) 0.004(3) -0.005(3) 0.001(3) C9 0.026(4) 0.031(5) 0.017(4) 0.011(3) 0.009(3) 0.000(4) C10 0.040(5) 0.029(5) 0.019(4) 0.012(4) -0.003(4) 0.008(4) C11 0.059(6) 0.020(5) 0.039(5) 0.004(4) 0.000(5) 0.007(4) C12 0.052(6) 0.026(5) 0.046(6) 0.018(4) 0.008(5) 0.022(4) C13 0.048(5) 0.041(5) 0.025(5) 0.018(4) 0.003(4) 0.016(5) C14 0.020(4) 0.056(6) 0.074(7) 0.034(5) 0.019(5) 0.021(4) C15 0.015 0.039(5) 0.023(4) 0.018(4) 0.005(3) 0.003(3) C16 0.030(4) 0.034(4) 0.013 0.011(3) 0.000(3) 0.021 C17 0.026(4) 0.035(5) 0.019(4) 0.013(3) 0.009(3) 0.019(4) C18 0.017(4) 0.023(4) 0.022(4) 0.007(3) 0.009(3) 0.008(3) C19 0.039(5) 0.015(4) 0.018(4) 0.006(3) 0.012(3) 0.013(4) C20 0.034(5) 0.044(5) 0.027(4) 0.022(4) 0.013(4) 0.022(4) C21 0.037(5) 0.027(5) 0.019(4) 0.004(4) 0.006(4) 0.003(4) C22 0.070(8) 0.091(9) 0.053(7) 0.041(7) 0.007(6) 0.027(7) C23 0.054(7) 0.088(9) 0.061(7) 0.047(7) 0.031(6) 0.040(6) C24 0.154(17) 0.174(18) 0.25(2) 0.174(19) -0.017(16) -0.020(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 '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 O5 Fe1 O1 74.35(18) . . ? O5 Fe1 N1 149.2(2) . . ? O1 Fe1 N1 75.8(2) . . ? O5 Fe1 Cl1 104.15(14) . . ? O1 Fe1 Cl1 118.80(15) . . ? N1 Fe1 Cl1 96.66(17) . . ? O5 Fe1 Cl2 98.23(15) . . ? O1 Fe1 Cl2 129.58(15) . . ? N1 Fe1 Cl2 94.87(18) . . ? Cl1 Fe1 Cl2 111.43(9) . . ? O6 Fe2 O4 145.80(19) . . ? O6 Fe2 O1 99.67(19) . . ? O4 Fe2 O1 110.92(19) . . ? O6 Fe2 O5 95.42(19) . . ? O4 Fe2 O5 107.79(19) . . ? O1 Fe2 O5 72.57(18) . . ? O6 Fe2 O2 93.71(19) . . ? O4 Fe2 O2 74.76(18) . . ? O1 Fe2 O2 84.91(18) . . ? O5 Fe2 O2 156.81(19) . . ? O6 Fe2 N3 80.4(2) . . ? O4 Fe2 N3 79.60(19) . . ? O1 Fe2 N3 151.9(2) . . ? O5 Fe2 N3 79.4(2) . . ? O2 Fe2 N3 123.2(2) . . ? O2 Fe3 O4 75.92(18) . . ? O2 Fe3 N2 76.9(2) . . ? O4 Fe3 N2 150.2(2) . . ? O2 Fe3 Cl4 112.62(15) . . ? O4 Fe3 Cl4 102.09(15) . . ? N2 Fe3 Cl4 99.50(18) . . ? O2 Fe3 Cl3 137.40(15) . . ? O4 Fe3 Cl3 99.06(15) . . ? N2 Fe3 Cl3 92.67(19) . . ? Cl4 Fe3 Cl3 109.81(10) . . ? C5 N1 C1 119.6(6) . . ? C5 N1 Fe1 116.2(4) . . ? C1 N1 Fe1 124.1(5) . . ? C9 N2 C13 118.1(7) . . ? C9 N2 Fe3 117.3(5) . . ? C13 N2 Fe3 124.3(5) . . ? C20 N3 C17 113.6(5) . . ? C20 N3 C18 111.6(6) . . ? C17 N3 C18 110.5(5) . . ? C20 N3 Fe2 106.9(4) . . ? C17 N3 Fe2 107.0(4) . . ? C18 N3 Fe2 106.8(4) . . ? C6 O1 Fe1 124.3(4) . . ? C6 O1 Fe2 127.4(4) . . ? Fe1 O1 Fe2 104.4(2) . . ? C8 O2 Fe3 123.1(4) . . ? C8 O2 Fe2 128.1(4) . . ? Fe3 O2 Fe2 104.9(2) . . ? C6 O3 C14 113.6(6) . . ? C16 O4 Fe2 117.4(4) . . ? C16 O4 Fe3 123.5(4) . . ? Fe2 O4 Fe3 104.12(19) . . ? C19 O5 Fe1 127.2(4) . . ? C19 O5 Fe2 115.3(4) . . ? Fe1 O5 Fe2 104.8(2) . . ? C21 O6 Fe2 120.5(5) . . ? N1 C1 C2 122.1(7) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C1 C2 C3 118.4(7) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C4 C3 C2 119.4(8) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 118.9(8) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 121.6(7) . . ? N1 C5 C6 116.4(6) . . ? C4 C5 C6 122.0(7) . . ? O1 C6 O3 110.6(5) . . ? O1 C6 C5 106.9(5) . . ? O3 C6 C5 112.6(6) . . ? O1 C6 C7 110.5(6) . . ? O3 C6 C7 105.9(5) . . ? C5 C6 C7 110.5(5) . . ? C6 C7 C8 117.3(5) . . ? C6 C7 H7A 108.0 . . ? C8 C7 H7A 108.0 . . ? C6 C7 H7B 108.0 . . ? C8 C7 H7B 108.0 . . ? H7A C7 H7B 107.2 . . ? O2 C8 C15 107.9(6) . . ? O2 C8 C9 107.3(5) . . ? C15 C8 C9 108.5(6) . . ? O2 C8 C7 109.2(5) . . ? C15 C8 C7 110.7(5) . . ? C9 C8 C7 113.1(6) . . ? N2 C9 C10 122.7(8) . . ? N2 C9 C8 114.1(6) . . ? C10 C9 C8 122.9(7) . . ? C9 C10 C11 118.4(7) . . ? C9 C10 H10 120.8 . . ? C11 C10 H10 120.8 . . ? C10 C11 C12 119.4(8) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C13 C12 C11 118.8(8) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? N2 C13 C12 122.5(8) . . ? N2 C13 H13 118.8 . . ? C12 C13 H13 118.8 . . ? O3 C14 H14A 109.5 . . ? O3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C8 C15 H15A 109.5 . . ? C8 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C8 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O4 C16 C17 109.3(5) . . ? O4 C16 H16A 109.8 . . ? C17 C16 H16A 109.8 . . ? O4 C16 H16B 109.8 . . ? C17 C16 H16B 109.8 . . ? H16A C16 H16B 108.3 . . ? N3 C17 C16 107.8(6) . . ? N3 C17 H17A 110.2 . . ? C16 C17 H17A 110.2 . . ? N3 C17 H17B 110.2 . . ? C16 C17 H17B 110.2 . . ? H17A C17 H17B 108.5 . . ? N3 C18 C19 108.4(5) . . ? N3 C18 H18A 110.0 . . ? C19 C18 H18A 110.0 . . ? N3 C18 H18B 110.0 . . ? C19 C18 H18B 110.0 . . ? H18A C18 H18B 108.4 . . ? O5 C19 C18 107.4(6) . . ? O5 C19 H19A 110.2 . . ? C18 C19 H19A 110.2 . . ? O5 C19 H19B 110.2 . . ? C18 C19 H19B 110.2 . . ? H19A C19 H19B 108.5 . . ? N3 C20 C21 111.7(6) . . ? N3 C20 H20A 109.3 . . ? C21 C20 H20A 109.3 . . ? N3 C20 H20B 109.3 . . ? C21 C20 H20B 109.3 . . ? H20A C20 H20B 107.9 . . ? O7 C21 O6 122.9(7) . . ? O7 C21 C20 119.9(8) . . ? O6 C21 C20 117.1(7) . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C23 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O8 C23 C24 122.0(13) . . ? O8 C23 C22 119.9(11) . . ? C24 C23 C22 118.1(12) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O5 1.958(4) . ? Fe1 O1 1.970(4) . ? Fe1 N1 2.121(6) . ? Fe1 Cl1 2.215(2) . ? Fe1 Cl2 2.223(2) . ? Fe2 O6 1.950(5) . ? Fe2 O4 1.987(4) . ? Fe2 O1 2.004(4) . ? Fe2 O5 2.007(5) . ? Fe2 O2 2.011(4) . ? Fe2 N3 2.217(6) . ? Fe3 O2 1.950(4) . ? Fe3 O4 1.995(5) . ? Fe3 N2 2.098(6) . ? Fe3 Cl4 2.214(2) . ? Fe3 Cl3 2.224(2) . ? N1 C5 1.324(9) . ? N1 C1 1.338(8) . ? N2 C9 1.336(9) . ? N2 C13 1.356(10) . ? N3 C20 1.479(9) . ? N3 C17 1.479(8) . ? N3 C18 1.497(9) . ? O1 C6 1.398(8) . ? O2 C8 1.433(7) . ? O3 C6 1.424(8) . ? O3 C14 1.441(9) . ? O4 C16 1.435(8) . ? O5 C19 1.428(8) . ? O6 C21 1.289(9) . ? O7 C21 1.226(9) . ? O8 C23 1.211(11) . ? C1 C2 1.377(10) . ? C1 H1 0.9500 . ? C2 C3 1.378(12) . ? C2 H2 0.9500 . ? C3 C4 1.376(11) . ? C3 H3 0.9500 . ? C4 C5 1.386(10) . ? C4 H4 0.9500 . ? C5 C6 1.515(9) . ? C6 C7 1.521(9) . ? C7 C8 1.542(9) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C15 1.530(9) . ? C8 C9 1.535(10) . ? C9 C10 1.377(10) . ? C10 C11 1.381(11) . ? C10 H10 0.9500 . ? C11 C12 1.386(11) . ? C11 H11 0.9500 . ? C12 C13 1.360(11) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.530(9) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.511(9) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.518(10) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C22 C23 1.471(14) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.385(16) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ?