#------------------------------------------------------------------------------ #$Date: 2016-05-12 06:02:26 +0300 (Thu, 12 May 2016) $ #$Revision: 182887 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/51/7225188.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_7225188 loop_ _publ_author_name 'Beldon, Patrick' 'Henke, Sebastian' 'Monserrat, Bartomeu' 'Tominaka, Satoshi' 'Stock, Norbert' 'Cheetham, Tony' _publ_section_title ; Transition metal coordination complexes of chrysazin ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/C5CE00792E _journal_year 2016 _chemical_formula_moiety 'C34 H28 Fe N2 O10' _chemical_formula_sum 'C34 H28 Fe N2 O10' _chemical_formula_weight 680.43 _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 mixed _audit_creation_date 2016-01-18 _audit_creation_method ; Olex2 1.2 (compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103) ; _audit_update_record ; 2016-04-20 deposited with the CCDC. 2016-05-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 100.448(4) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 10.0131(4) _cell_length_b 8.4169(4) _cell_length_c 18.1414(8) _cell_measurement_reflns_used 2527 _cell_measurement_temperature 269.95(10) _cell_measurement_theta_max 67.4910 _cell_measurement_theta_min 4.7180 _cell_volume 1503.59(12) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _diffrn_ambient_temperature 269.95(10) _diffrn_detector_area_resol_mean 16.1183 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_details ; 1 omega -25.00 2.00 1.0000 1.0900 omega____ theta____ kappa____ phi______ frames - -26.1037 -99.0000 -60.0000 27 2 omega -96.00 -68.00 1.0000 1.0900 omega____ theta____ kappa____ phi______ frames - -26.1037 -178.0000 60.0000 28 3 omega -13.00 27.00 1.0000 1.0900 omega____ theta____ kappa____ phi______ frames - -26.1037 -99.0000 -30.0000 40 4 omega -8.00 43.00 1.0000 1.0900 omega____ theta____ kappa____ phi______ frames - 26.1037 57.0000 150.0000 51 5 omega 47.00 93.00 1.0000 1.0900 omega____ theta____ kappa____ phi______ frames - 26.1037 57.0000 150.0000 46 6 omega -154.00 -127.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - -67.8019 -94.0000 30.0000 27 7 omega -95.00 -47.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - -67.8019 -61.0000 -60.0000 48 8 omega -143.00 -102.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - -67.8019 -61.0000 -60.0000 41 9 omega 88.00 133.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 67.8019 111.0000 -60.0000 45 10 omega 39.00 136.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 67.8019 61.0000 120.0000 97 11 omega 13.00 81.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 67.8019 -94.0000 -120.0000 68 12 omega -19.00 7.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 67.8019 -94.0000 -120.0000 26 13 omega -16.00 50.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 67.8019 -30.0000 -150.0000 66 14 omega 31.00 56.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 109.5000 21.0000 0.0000 25 15 omega 105.00 131.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 109.5000 65.0000 0.0000 26 16 omega 31.00 71.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 109.5000 -43.0000 150.0000 40 17 omega 90.00 119.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 109.5000 65.0000 -30.0000 29 18 omega 110.00 178.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 109.5000 104.0000 -180.0000 68 19 omega 32.00 60.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 109.5000 -43.0000 30.0000 28 20 omega 74.00 122.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 109.5000 65.0000 -60.0000 48 21 omega 123.00 150.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 109.5000 -21.0000 90.0000 27 22 omega 30.00 73.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 109.5000 -43.0000 90.0000 43 23 omega 36.00 75.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 109.5000 -43.0000 -150.0000 39 24 omega 125.00 177.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 109.5000 -21.0000 150.0000 52 25 omega 58.00 152.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 109.5000 -77.0000 -180.0000 94 26 omega 126.00 167.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 109.5000 65.0000 -30.0000 41 27 omega 140.00 168.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 109.5000 -32.0000 -90.0000 28 28 omega 151.00 178.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 109.5000 65.0000 0.0000 27 29 omega 52.00 78.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 109.5000 -104.0000 150.0000 26 30 omega 121.00 154.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 109.5000 21.0000 0.0000 33 31 omega 48.00 73.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 109.5000 -65.0000 -150.0000 25 32 omega 144.00 172.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 109.5000 -32.0000 120.0000 28 33 omega 116.00 145.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 109.5000 -21.0000 -30.0000 29 34 omega 133.00 174.00 1.0000 4.3500 omega____ theta____ kappa____ phi______ frames - 109.5000 -32.0000 60.0000 41 ; _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.1300217000 _diffrn_orient_matrix_UB_12 0.0399622000 _diffrn_orient_matrix_UB_13 -0.0304284000 _diffrn_orient_matrix_UB_21 -0.0696005000 _diffrn_orient_matrix_UB_22 0.1488298000 _diffrn_orient_matrix_UB_23 -0.0387647000 _diffrn_orient_matrix_UB_31 0.0523363000 _diffrn_orient_matrix_UB_32 0.0985416000 _diffrn_orient_matrix_UB_33 0.0709530000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_unetI/netI 0.0308 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 5822 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 67.438 _diffrn_reflns_theta_max 67.438 _diffrn_reflns_theta_min 4.719 _diffrn_source 'Enhance Ultra (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 4.584 _exptl_absorpt_correction_T_max 0.488 _exptl_absorpt_correction_T_min 0.097 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour black _exptl_crystal_colour_primary black _exptl_crystal_density_diffrn 1.503 _exptl_crystal_description block _exptl_crystal_F_000 704 _exptl_crystal_size_max 0.4481 _exptl_crystal_size_mid 0.2249 _exptl_crystal_size_min 0.1057 _refine_diff_density_max 0.290 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.053 _refine_ls_extinction_coef 0.0012(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 220 _refine_ls_number_reflns 2679 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.039 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0385 _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^)+(0.0725P)^2^+0.1511P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1055 _refine_ls_wR_factor_ref 0.1113 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2349 _reflns_number_total 2679 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c5ce00792e2.cif _cod_data_source_block FeChrys-1 _cod_original_cell_volume 1503.60(12) _cod_database_code 7225188 _chemical_oxdiff_formula 'Fe2 C34 N2 O10 H26' _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. ; _reflns_odcompleteness_completeness 93.99 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 69.95 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2.a Aromatic/amide H refined with riding coordinates: C1(H1), C7(H7), C8(H8), C9(H9), C13(H13), C14(H14), C15(H15) 2.b Idealised Me refined as rotating group: C16(H16A,H16B,H16C), C17(H17A,H17B,H17C) ; _shelx_shelxl_version_number 2014/7 _shelx_res_file ; TITL pjb131221-02-FeAcO2-Chrys-Xal1-ABS in P21/n #14 REM reset to P21/n #14 CELL 1.54184 10.013107 8.416919 18.141409 90 100.4478 90 ZERR 2 0.000386 0.000393 0.000825 0 0.0042 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O Fe UNIT 68 56 4 20 2 L.S. 4 0 0 PLAN 10 BOND MORE -1 BOND $H CONF fmap 2 acta REM REM REM WGHT 0.072500 0.151100 EXTI 0.001162 FVAR 6.22219 FE1 5 0.500000 0.500000 0.500000 10.50000 0.03530 0.04091 = 0.04837 0.00293 0.00993 -0.00473 O1 4 0.459785 0.582763 0.596126 11.00000 0.04169 0.04932 = 0.05091 -0.00361 0.00888 -0.01156 O2 4 0.300108 0.433699 0.477676 11.00000 0.03765 0.04988 = 0.04147 0.00069 0.00856 -0.00396 O3 4 0.163369 0.272890 0.371709 11.00000 0.05914 0.07041 = 0.04916 -0.01298 0.01518 -0.01291 H3 2 0.231648 0.338146 0.397135 11.00000 -1.50000 O4 4 -0.073636 0.325270 0.651520 11.00000 0.04956 0.08589 = 0.05769 0.00168 0.02095 -0.01594 O5 4 0.467450 0.734201 0.448063 11.00000 0.05695 0.04514 = 0.05657 0.00710 0.00218 -0.00283 N1 3 0.376940 0.901140 0.355033 11.00000 0.04983 0.04379 = 0.04691 0.00420 0.00831 -0.00359 C1 1 0.365907 0.614120 0.703441 11.00000 0.05105 0.04501 = 0.04336 0.00059 -0.00065 -0.00508 AFIX 43 H1 2 0.442637 0.670544 0.725546 11.00000 -1.20000 AFIX 0 C2 1 0.359170 0.553981 0.629440 11.00000 0.04101 0.03637 = 0.04242 0.00353 0.00416 -0.00028 C3 1 0.239130 0.466108 0.597401 11.00000 0.03647 0.03376 = 0.03904 0.00475 0.00333 0.00151 C4 1 0.217661 0.406396 0.521868 11.00000 0.03283 0.03326 = 0.04120 0.00727 0.00535 0.00282 C5 1 0.096773 0.312320 0.492277 11.00000 0.03585 0.03202 = 0.04340 0.00403 0.00196 0.00124 C6 1 0.076307 0.247560 0.419191 11.00000 0.04321 0.03910 = 0.04784 -0.00020 0.00510 0.00085 C7 1 -0.037551 0.155618 0.392979 11.00000 0.05022 0.05059 = 0.05526 -0.00947 -0.00131 -0.00361 AFIX 43 H7 2 -0.049679 0.113030 0.344922 11.00000 -1.20000 AFIX 0 C8 1 -0.132077 0.127095 0.437204 11.00000 0.04109 0.05025 = 0.07273 -0.00700 0.00053 -0.00949 AFIX 43 H8 2 -0.207883 0.065385 0.418885 11.00000 -1.20000 AFIX 0 C9 1 -0.116007 0.189139 0.508895 11.00000 0.03862 0.04675 = 0.06386 0.00185 0.00870 -0.00637 AFIX 43 H9 2 -0.180842 0.169477 0.538548 11.00000 -1.20000 AFIX 0 C10 1 -0.002656 0.280886 0.536373 11.00000 0.03542 0.03677 = 0.04708 0.00594 0.00563 0.00284 C11 1 0.012670 0.348522 0.612895 11.00000 0.03809 0.04676 = 0.04746 0.00908 0.00881 0.00053 C12 1 0.136402 0.442352 0.641538 11.00000 0.04074 0.03812 = 0.03934 0.00630 0.00547 0.00111 C13 1 0.148242 0.505558 0.712422 11.00000 0.05139 0.05252 = 0.04268 0.00586 0.01202 0.00092 AFIX 43 H13 2 0.079283 0.490724 0.739865 11.00000 -1.20000 AFIX 0 C14 1 0.264064 0.591965 0.742964 11.00000 0.06248 0.05404 = 0.03712 -0.00286 0.00540 -0.00212 AFIX 43 H14 2 0.271760 0.634845 0.790795 11.00000 -1.20000 AFIX 0 C15 1 0.394298 0.759643 0.386609 11.00000 0.04557 0.04200 = 0.05638 -0.00075 0.01186 -0.00381 AFIX 43 H15 2 0.348817 0.673946 0.361135 11.00000 -1.20000 AFIX 0 C16 1 0.446361 1.037505 0.392416 11.00000 0.08512 0.04931 = 0.07628 0.00482 -0.00340 -0.01222 AFIX 137 H16A 2 0.395582 1.078227 0.428365 11.00000 -1.50000 H16B 2 0.454335 1.118296 0.356113 11.00000 -1.50000 H16C 2 0.535270 1.006555 0.417596 11.00000 -1.50000 AFIX 0 C17 1 0.279119 0.927439 0.286270 11.00000 0.06251 0.06974 = 0.05181 0.00875 0.00634 -0.00054 AFIX 137 H17A 2 0.323326 0.978879 0.250014 11.00000 -1.50000 H17B 2 0.206673 0.993503 0.296752 11.00000 -1.50000 H17C 2 0.242884 0.827269 0.266722 11.00000 -1.50000 AFIX 0 HKLF 4 REM pjb131221-02-FeAcO2-Chrys-Xal1-ABS in P21/n #14 REM R1 = 0.0385 for 2349 Fo > 4sig(Fo) and 0.0444 for all 2679 data REM 220 parameters refined using 0 restraints END WGHT 0.0725 0.1511 REM Highest difference peak 0.290, deepest hole -0.406, 1-sigma level 0.053 Q1 1 0.5711 0.6276 0.4779 11.00000 0.05 0.29 Q2 1 0.5856 0.3725 0.4834 11.00000 0.05 0.29 Q3 1 0.4049 0.6197 0.4903 11.00000 0.05 0.27 Q4 1 0.0361 0.2963 0.5120 11.00000 0.05 0.23 Q5 1 0.0001 0.3011 0.5675 11.00000 0.05 0.21 Q6 1 -0.0455 0.2274 0.6366 11.00000 0.05 0.20 Q7 1 -0.0582 0.1187 0.4220 11.00000 0.05 0.18 Q8 1 0.1855 0.4650 0.6180 11.00000 0.05 0.18 Q9 1 0.1018 0.2689 0.4656 11.00000 0.05 0.17 Q10 1 0.3589 0.5923 0.6604 11.00000 0.05 0.16 REM The information below was added by Olex2. REM REM R1 = 0.0385 for 2349 Fo > 4sig(Fo) and 0.0444 for all 6109 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.29, deepest hole -0.41 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0444 REM R1_gt = 0.0385 REM wR_ref = 0.1113 REM GOOF = 1.039 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 6109 REM Reflections_gt = 2349 REM Parameters = n/a REM Hole = -0.41 REM Peak = 0.29 REM Flack = n/a ; 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 _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy Fe1 Fe 0.5000 0.5000 0.5000 0.04123(18) Uani 1 2 d S T P O1 O 0.45978(14) 0.58276(18) 0.59613(8) 0.0472(4) Uani 1 1 d . . . O2 O 0.30011(13) 0.43370(19) 0.47768(7) 0.0428(3) Uani 1 1 d . . . O3 O 0.16337(18) 0.2729(2) 0.37171(9) 0.0589(4) Uani 1 1 d . . . H3 H 0.232(3) 0.338(4) 0.3971(18) 0.088 Uiso 1 1 d R . . O4 O -0.07364(17) 0.3253(2) 0.65152(9) 0.0630(5) Uani 1 1 d . . . O5 O 0.46745(17) 0.73420(19) 0.44806(9) 0.0539(4) Uani 1 1 d . . . N1 N 0.37694(18) 0.9011(2) 0.35503(10) 0.0469(4) Uani 1 1 d . . . C1 C 0.3659(2) 0.6141(3) 0.70344(11) 0.0476(5) Uani 1 1 d . . . H1 H 0.4426 0.6705 0.7255 0.057 Uiso 1 1 calc R . . C2 C 0.3592(2) 0.5540(3) 0.62944(11) 0.0404(4) Uani 1 1 d . . . C3 C 0.2391(2) 0.4661(2) 0.59740(11) 0.0369(4) Uani 1 1 d . . . C4 C 0.21766(18) 0.4064(2) 0.52187(10) 0.0359(4) Uani 1 1 d . . . C5 C 0.09677(19) 0.3123(2) 0.49228(11) 0.0377(4) Uani 1 1 d . . . C6 C 0.0763(2) 0.2476(3) 0.41919(12) 0.0438(5) Uani 1 1 d . . . C7 C -0.0376(2) 0.1556(3) 0.39298(13) 0.0534(5) Uani 1 1 d . . . H7 H -0.0497 0.1130 0.3449 0.064 Uiso 1 1 calc R . . C8 C -0.1321(2) 0.1271(3) 0.43720(14) 0.0559(6) Uani 1 1 d . . . H8 H -0.2079 0.0654 0.4189 0.067 Uiso 1 1 calc R . . C9 C -0.1160(2) 0.1891(3) 0.50889(13) 0.0498(5) Uani 1 1 d . . . H9 H -0.1808 0.1695 0.5385 0.060 Uiso 1 1 calc R . . C10 C -0.00266(19) 0.2809(2) 0.53637(11) 0.0400(4) Uani 1 1 d . . . C11 C 0.0127(2) 0.3485(3) 0.61290(11) 0.0440(5) Uani 1 1 d . . . C12 C 0.1364(2) 0.4424(3) 0.64154(11) 0.0396(4) Uani 1 1 d . . . C13 C 0.1482(3) 0.5056(3) 0.71242(13) 0.0484(5) Uani 1 1 d . . . H13 H 0.0793 0.4907 0.7399 0.058 Uiso 1 1 calc R . . C14 C 0.2641(2) 0.5920(3) 0.74296(12) 0.0517(5) Uani 1 1 d . . . H14 H 0.2718 0.6348 0.7908 0.062 Uiso 1 1 calc R . . C15 C 0.3943(2) 0.7596(3) 0.38661(12) 0.0477(5) Uani 1 1 d . . . H15 H 0.3488 0.6739 0.3611 0.057 Uiso 1 1 calc R . . C16 C 0.4464(3) 1.0375(3) 0.39242(18) 0.0725(8) Uani 1 1 d . . . H16A H 0.3956 1.0782 0.4284 0.109 Uiso 1 1 calc GR . . H16B H 0.4543 1.1183 0.3561 0.109 Uiso 1 1 calc GR . . H16C H 0.5353 1.0066 0.4176 0.109 Uiso 1 1 calc GR . . C17 C 0.2791(3) 0.9274(4) 0.28627(13) 0.0619(6) Uani 1 1 d . . . H17A H 0.3233 0.9789 0.2500 0.093 Uiso 1 1 calc GR . . H17B H 0.2067 0.9935 0.2968 0.093 Uiso 1 1 calc GR . . H17C H 0.2429 0.8273 0.2667 0.093 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 0.0353(3) 0.0409(3) 0.0484(3) 0.00293(19) 0.00993(18) -0.00473(18) O1 0.0417(7) 0.0493(9) 0.0509(8) -0.0036(7) 0.0089(6) -0.0116(6) O2 0.0377(7) 0.0499(8) 0.0415(7) 0.0007(6) 0.0086(6) -0.0040(6) O3 0.0591(9) 0.0704(11) 0.0492(9) -0.0130(8) 0.0152(7) -0.0129(8) O4 0.0496(9) 0.0859(13) 0.0577(10) 0.0017(9) 0.0209(7) -0.0159(9) O5 0.0570(9) 0.0451(9) 0.0566(9) 0.0071(7) 0.0022(7) -0.0028(7) N1 0.0498(10) 0.0438(10) 0.0469(10) 0.0042(8) 0.0083(8) -0.0036(8) C1 0.0510(12) 0.0450(12) 0.0434(11) 0.0006(9) -0.0006(9) -0.0051(9) C2 0.0410(10) 0.0364(10) 0.0424(10) 0.0035(8) 0.0042(8) -0.0003(8) C3 0.0365(10) 0.0338(10) 0.0390(10) 0.0048(8) 0.0033(8) 0.0015(8) C4 0.0328(9) 0.0333(10) 0.0412(10) 0.0073(8) 0.0054(7) 0.0028(7) C5 0.0359(9) 0.0320(10) 0.0434(10) 0.0040(8) 0.0020(8) 0.0012(7) C6 0.0432(10) 0.0391(11) 0.0478(11) -0.0002(9) 0.0051(8) 0.0009(9) C7 0.0502(12) 0.0506(13) 0.0553(13) -0.0095(10) -0.0013(10) -0.0036(10) C8 0.0411(11) 0.0502(14) 0.0727(15) -0.0070(11) 0.0005(10) -0.0095(10) C9 0.0386(10) 0.0468(12) 0.0639(14) 0.0019(10) 0.0087(9) -0.0064(9) C10 0.0354(9) 0.0368(11) 0.0471(11) 0.0059(8) 0.0056(8) 0.0028(8) C11 0.0381(10) 0.0468(12) 0.0475(11) 0.0091(9) 0.0088(8) 0.0005(9) C12 0.0407(10) 0.0381(10) 0.0393(10) 0.0063(8) 0.0055(8) 0.0011(8) C13 0.0514(13) 0.0525(14) 0.0427(12) 0.0059(9) 0.0120(9) 0.0009(9) C14 0.0625(13) 0.0540(14) 0.0371(10) -0.0029(9) 0.0054(9) -0.0021(11) C15 0.0456(11) 0.0420(12) 0.0564(13) -0.0007(9) 0.0119(10) -0.0038(9) C16 0.085(2) 0.0493(14) 0.0763(19) 0.0048(13) -0.0034(15) -0.0122(14) C17 0.0625(14) 0.0697(17) 0.0518(13) 0.0087(12) 0.0063(11) -0.0005(13) 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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 6 0 -5 0.0639 5.9968 -0.0030 -4.9794 0.9311 -0.2248 -0.0398 -6 0 5 0.0639 -5.9968 0.0030 4.9794 -0.9311 0.2248 0.0398 -6 0 6 0.0529 -5.9974 0.0026 5.9790 -0.9616 0.1860 0.1106 6 0 -6 0.0529 5.9974 -0.0026 -5.9790 0.9616 -0.1860 -0.1106 -1 5 -5 0.1824 -0.9979 5.0015 -5.0042 0.2224 1.0078 0.0856 1 -5 5 0.1824 0.9979 -5.0015 5.0042 -0.2224 -1.0078 -0.0856 2 0 11 0.0928 1.9909 -0.0060 11.0019 -0.0762 -0.5659 0.8842 0 5 5 0.2135 -0.0054 4.9967 4.9950 0.0470 0.5504 0.8465 0 -5 -5 0.2084 0.0054 -4.9967 -4.9950 -0.0470 -0.5504 -0.8465 -2 0 -10 0.1355 -1.9915 0.0056 -10.0023 0.0456 0.5272 -0.8134 6 1 -2 0.0716 5.9944 0.9955 -1.9812 0.8795 -0.1923 0.2713 -5 0 -5 0.0865 -4.9915 0.0061 -5.0136 -0.4962 0.5427 -0.6164 5 0 6 0.0662 4.9909 -0.0065 6.0132 0.4657 -0.5814 0.6872 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 O1 Fe1 O1 180.0 . 3_666 O1 Fe1 O2 85.56(6) 3_666 3_666 O1 Fe1 O2 85.56(6) . . O1 Fe1 O2 94.44(6) 3_666 . O1 Fe1 O2 94.44(6) . 3_666 O1 Fe1 O5 88.62(6) 3_666 . O1 Fe1 O5 88.62(6) . 3_666 O1 Fe1 O5 91.38(6) . . O1 Fe1 O5 91.38(6) 3_666 3_666 O2 Fe1 O2 180.0 . 3_666 O2 Fe1 O5 95.55(6) . . O2 Fe1 O5 84.45(6) . 3_666 O2 Fe1 O5 84.45(6) 3_666 . O2 Fe1 O5 95.55(6) 3_666 3_666 O5 Fe1 O5 180.0 . 3_666 C2 O1 Fe1 130.27(14) . . C4 O2 Fe1 130.39(12) . . C6 O3 H3 106(2) . . C15 O5 Fe1 124.26(15) . . C15 N1 C16 119.9(2) . . C15 N1 C17 121.6(2) . . C16 N1 C17 118.2(2) . . C2 C1 H1 118.8 . . C14 C1 H1 118.8 . . C14 C1 C2 122.4(2) . . O1 C2 C1 117.89(19) . . O1 C2 C3 124.99(19) . . C1 C2 C3 117.12(18) . . C4 C3 C2 122.22(18) . . C12 C3 C2 118.61(18) . . C12 C3 C4 119.14(18) . . O2 C4 C3 122.37(18) . . O2 C4 C5 117.04(17) . . C3 C4 C5 120.59(17) . . C6 C5 C4 121.46(18) . . C10 C5 C4 120.99(18) . . C10 C5 C6 117.54(18) . . O3 C6 C5 122.51(19) . . O3 C6 C7 117.1(2) . . C7 C6 C5 120.4(2) . . C6 C7 H7 119.7 . . C8 C7 C6 120.6(2) . . C8 C7 H7 119.7 . . C7 C8 H8 119.7 . . C7 C8 C9 120.7(2) . . C9 C8 H8 119.7 . . C8 C9 H9 120.1 . . C8 C9 C10 119.7(2) . . C10 C9 H9 120.1 . . C5 C10 C11 119.68(18) . . C9 C10 C5 121.0(2) . . C9 C10 C11 119.27(19) . . O4 C11 C10 120.7(2) . . O4 C11 C12 121.1(2) . . C12 C11 C10 118.11(17) . . C3 C12 C11 121.31(18) . . C13 C12 C3 121.40(19) . . C13 C12 C11 117.29(19) . . C12 C13 H13 120.1 . . C12 C13 C14 119.8(2) . . C14 C13 H13 120.1 . . C1 C14 C13 120.7(2) . . C1 C14 H14 119.7 . . C13 C14 H14 119.7 . . O5 C15 N1 123.9(2) . . O5 C15 H15 118.1 . . N1 C15 H15 118.1 . . N1 C16 H16A 109.5 . . N1 C16 H16B 109.5 . . N1 C16 H16C 109.5 . . H16A C16 H16B 109.5 . . H16A C16 H16C 109.5 . . H16B C16 H16C 109.5 . . N1 C17 H17A 109.5 . . N1 C17 H17B 109.5 . . N1 C17 H17C 109.5 . . H17A C17 H17B 109.5 . . H17A C17 H17C 109.5 . . H17B C17 H17C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Fe1 O1 1.9857(14) . Fe1 O1 1.9858(15) 3_666 Fe1 O2 2.0464(13) . Fe1 O2 2.0464(13) 3_666 Fe1 O5 2.1837(16) . Fe1 O5 2.1837(16) 3_666 O1 C2 1.288(2) . O2 C4 1.272(2) . O3 H3 0.93(3) . O3 C6 1.349(3) . O4 C11 1.223(2) . O5 C15 1.237(3) . N1 C15 1.319(3) . N1 C16 1.446(3) . N1 C17 1.457(3) . C1 H1 0.9300 . C1 C2 1.425(3) . C1 C14 1.362(3) . C2 C3 1.441(3) . C3 C4 1.439(3) . C3 C12 1.428(3) . C4 C5 1.464(3) . C5 C6 1.414(3) . C5 C10 1.411(3) . C6 C7 1.389(3) . C7 H7 0.9300 . C7 C8 1.368(3) . C8 H8 0.9300 . C8 C9 1.384(3) . C9 H9 0.9300 . C9 C10 1.388(3) . C10 C11 1.482(3) . C11 C12 1.482(3) . C12 C13 1.377(3) . C13 H13 0.9300 . C13 C14 1.396(3) . C14 H14 0.9300 . C15 H15 0.9300 . C16 H16A 0.9600 . C16 H16B 0.9600 . C16 H16C 0.9600 . C17 H17A 0.9600 . C17 H17B 0.9600 . C17 H17C 0.9600 . 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 Fe1 O1 C2 C1 171.63(14) Fe1 O1 C2 C3 -8.8(3) Fe1 O2 C4 C3 20.5(3) Fe1 O2 C4 C5 -160.43(13) Fe1 O5 C15 N1 -178.82(15) O1 C2 C3 C4 -2.7(3) O1 C2 C3 C12 179.37(19) O2 C4 C5 C6 3.3(3) O2 C4 C5 C10 -177.74(17) O3 C6 C7 C8 -178.7(2) O4 C11 C12 C3 178.3(2) O4 C11 C12 C13 -1.7(3) C1 C2 C3 C4 176.85(18) C1 C2 C3 C12 -1.1(3) C2 C1 C14 C13 1.2(4) C2 C3 C4 O2 -3.3(3) C2 C3 C4 C5 177.63(18) C2 C3 C12 C11 -177.93(18) C2 C3 C12 C13 2.0(3) C3 C4 C5 C6 -177.60(18) C3 C4 C5 C10 1.4(3) C3 C12 C13 C14 -1.4(3) C4 C3 C12 C11 4.1(3) C4 C3 C12 C13 -175.94(18) C4 C5 C6 O3 -2.4(3) C4 C5 C6 C7 178.48(19) C4 C5 C10 C9 -178.74(19) C4 C5 C10 C11 2.1(3) C5 C6 C7 C8 0.4(3) C5 C10 C11 O4 178.6(2) C5 C10 C11 C12 -2.5(3) C6 C5 C10 C9 0.3(3) C6 C5 C10 C11 -178.86(17) C6 C7 C8 C9 -0.1(4) C7 C8 C9 C10 -0.2(4) C8 C9 C10 C5 0.1(3) C8 C9 C10 C11 179.2(2) C9 C10 C11 O4 -0.5(3) C9 C10 C11 C12 178.40(19) C10 C5 C6 O3 178.57(19) C10 C5 C6 C7 -0.5(3) C10 C11 C12 C3 -0.7(3) C10 C11 C12 C13 179.37(18) C11 C12 C13 C14 178.5(2) C12 C3 C4 O2 174.58(18) C12 C3 C4 C5 -4.5(3) C12 C13 C14 C1 -0.2(3) C14 C1 C2 O1 179.1(2) C14 C1 C2 C3 -0.5(3) C16 N1 C15 O5 0.4(3) C17 N1 C15 O5 -173.7(2)