#------------------------------------------------------------------------------ #$Date: 2020-06-05 12:31:55 +0300 (Fri, 05 Jun 2020) $ #$Revision: 252672 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/76/1557659.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_1557659 loop_ _publ_author_name 'Karim, Suhana' 'Chakraborty, Aratrika' 'Samanta, Debabrata' 'Zangrando, Ennio' 'Ghosh, Totan' 'Das, Debasis' _publ_section_title ; A dinuclear iron complex as an efficient electrocatalyst for homogeneous water oxidation reaction ; _journal_issue 9 _journal_name_full 'Catalysis Science & Technology' _journal_page_first 2830 _journal_paper_doi 10.1039/D0CY00011F _journal_volume 10 _journal_year 2020 _chemical_formula_moiety 'C32 H34 Cl2 Fe2 N6 O7, 2(Cl), 3(H2 O)' _chemical_formula_sum 'C32 H40 Cl4 Fe2 N6 O10' _chemical_formula_weight 922.20 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-03-09 deposited with the CCDC. 2020-03-25 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 102.136(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 11.8719(6) _cell_length_b 16.9617(8) _cell_length_c 9.4064(5) _cell_measurement_reflns_used 4146 _cell_measurement_temperature 125(2) _cell_measurement_theta_max 25.71 _cell_measurement_theta_min 2.65 _cell_volume 1851.81(16) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 125(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'BRUKER SMART APEX CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA-PHI SCAN' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0804 _diffrn_reflns_av_unetI/netI 0.0569 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 20605 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.388 _diffrn_reflns_theta_min 2.519 _exptl_absorpt_coefficient_mu 1.137 _exptl_absorpt_correction_T_max 0.883 _exptl_absorpt_correction_T_min 0.804 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.654 _exptl_crystal_description block _exptl_crystal_F_000 948 _exptl_crystal_size_max 0.363 _exptl_crystal_size_mid 0.260 _exptl_crystal_size_min 0.250 _refine_diff_density_max 0.838 _refine_diff_density_min -0.713 _refine_diff_density_rms 0.092 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 259 _refine_ls_number_reflns 3781 _refine_ls_number_restraints 10 _refine_ls_restrained_S_all 1.056 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0487 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+5.1614P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1100 _refine_ls_wR_factor_ref 0.1185 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3083 _reflns_number_total 3781 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0cy00011f2.cif _cod_data_source_block shelx_CCDC1 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'MULTI-SCAN' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas Adding full bibliography for 1557658--1557659.cif. ; _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 1557659 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_res_file ; TITL TEST_a.res in P2(1)/c shelx.res created by SHELXL-2018/3 at 11:26:07 on 29-Feb-2020 CELL 0.71073 11.8719 16.9617 9.4064 90.000 102.136 90.000 ZERR 2.00 0.0006 0.0008 0.0005 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O CL FE UNIT 64 80 12 20 8 4 MERG 2 OMIT 0 2 0 dfix 0.85 o1w h11a o1w h12a O2w H20 dfix 1.35 h11a h12a FMAP 2 PLAN 10 ACTA HTAB 2.00000 BOND $H CONF L.S. 10 TEMP -147.81 WGHT 0.033200 5.161400 FVAR 0.39444 FE 6 0.406968 0.419061 0.513150 11.00000 0.01760 0.01622 = 0.01422 -0.00012 0.00346 -0.00075 CL1 5 0.378269 0.367453 0.284521 11.00000 0.03181 0.02552 = 0.01406 -0.00262 0.00504 -0.00235 N1 3 0.553148 0.355863 0.631838 11.00000 0.02003 0.01797 = 0.01592 0.00062 0.00342 -0.00015 N2 3 0.259361 0.494122 0.498915 11.00000 0.01980 0.02289 = 0.02006 0.00259 0.00459 0.00111 N3 3 0.398161 0.441419 0.742439 11.00000 0.01778 0.01860 = 0.01257 -0.00155 0.00258 -0.00236 O1 4 0.494597 0.391416 0.966456 11.00000 0.02364 0.02773 = 0.01281 0.00135 0.00372 -0.00264 O2 4 0.304189 0.519441 0.881662 11.00000 0.02507 0.03089 = 0.01978 -0.00577 0.00843 -0.00040 O3 4 0.301093 0.325412 0.568888 11.00000 0.02538 0.02228 = 0.01458 -0.00429 0.00528 -0.00787 H3A 2 0.261171 0.306064 0.511366 11.00000 -1.20000 O4 4 0.500000 0.500000 0.500000 10.50000 0.02060 0.01848 = 0.02380 0.00089 0.00318 -0.00273 C1 1 0.620011 0.307840 0.571547 11.00000 0.02411 0.02097 = 0.02152 -0.00408 0.00871 -0.00179 AFIX 43 H1 2 0.592734 0.291016 0.474049 11.00000 -1.20000 AFIX 0 C2 1 0.726002 0.282008 0.644594 11.00000 0.02699 0.02481 = 0.02484 -0.00334 0.00773 0.00242 AFIX 43 H2 2 0.770741 0.247645 0.598906 11.00000 -1.20000 AFIX 0 C3 1 0.766648 0.307234 0.787206 11.00000 0.02168 0.02745 = 0.02176 0.00300 0.00069 0.00281 AFIX 43 H3 2 0.839780 0.290547 0.840546 11.00000 -1.20000 AFIX 0 C4 1 0.698323 0.357097 0.849595 11.00000 0.02358 0.02499 = 0.01738 -0.00089 0.00403 -0.00058 AFIX 43 H4 2 0.724237 0.375574 0.946290 11.00000 -1.20000 AFIX 0 C5 1 0.591732 0.379670 0.769184 11.00000 0.02211 0.01813 = 0.01604 0.00151 0.00657 -0.00090 C6 1 0.177233 0.505891 0.378373 11.00000 0.02356 0.03186 = 0.02074 0.00463 0.00390 -0.00021 AFIX 43 H6 2 0.180758 0.477147 0.292737 11.00000 -1.20000 AFIX 0 C7 1 0.088416 0.558246 0.375449 11.00000 0.01960 0.03749 = 0.03365 0.00685 0.00051 0.00312 AFIX 43 H7 2 0.031978 0.565900 0.288642 11.00000 -1.20000 AFIX 0 C8 1 0.082034 0.599636 0.500033 11.00000 0.02158 0.03427 = 0.04260 0.00463 0.00572 0.00659 AFIX 43 H8 2 0.021199 0.636070 0.499674 11.00000 -1.20000 AFIX 0 C9 1 0.165195 0.587503 0.625491 11.00000 0.02416 0.02639 = 0.03422 -0.00281 0.00925 0.00204 AFIX 43 H9 2 0.161834 0.614667 0.712824 11.00000 -1.20000 AFIX 0 C10 1 0.253684 0.534579 0.620369 11.00000 0.02009 0.01995 = 0.02332 0.00014 0.00512 -0.00222 C11 1 0.348776 0.520594 0.753497 11.00000 0.02352 0.01985 = 0.01976 -0.00341 0.00647 0.00184 AFIX 13 H11 2 0.409827 0.561888 0.760595 11.00000 -1.20000 AFIX 0 C12 1 0.513969 0.430941 0.840255 11.00000 0.01922 0.01911 = 0.01551 -0.00041 0.00265 -0.00247 AFIX 13 H12 2 0.550787 0.483388 0.867177 11.00000 -1.20000 AFIX 0 C13 1 0.241078 0.340672 0.682770 11.00000 0.02639 0.03593 = 0.01394 -0.00423 0.00676 -0.01246 AFIX 23 H13A 2 0.218026 0.290276 0.721484 11.00000 -1.20000 H13B 2 0.170510 0.371584 0.644347 11.00000 -1.20000 AFIX 0 C14 1 0.319293 0.386463 0.803443 11.00000 0.02489 0.02234 = 0.01387 -0.00150 0.00822 -0.00618 C15 1 0.404382 0.336888 0.909212 11.00000 0.02449 0.02504 = 0.01714 0.00138 0.00450 -0.00299 AFIX 23 H15A 2 0.368715 0.315567 0.987282 11.00000 -1.20000 H15B 2 0.433710 0.292591 0.858795 11.00000 -1.20000 AFIX 0 C16 1 0.251458 0.443194 0.884520 11.00000 0.02580 0.03172 = 0.01997 -0.00208 0.00878 -0.00324 AFIX 23 H16A 2 0.169230 0.445137 0.834946 11.00000 -1.20000 H16B 2 0.256750 0.425483 0.985996 11.00000 -1.20000 AFIX 0 CL2 5 -0.009613 0.175887 0.620693 11.00000 0.04359 0.06869 = 0.06289 0.00845 0.01756 0.00163 O1W 4 0.124079 0.249722 0.406935 11.00000 0.06206 0.06687 = 0.02688 -0.02128 0.02383 -0.02477 H12A 2 0.080859 0.229668 0.454765 11.00000 -1.50000 H11A 2 0.086108 0.277226 0.342133 11.00000 -1.50000 isor 0.01 o2w O2W 4 0.000000 0.500000 0.000000 10.50000 0.28285 0.10167 = 0.20440 0.04108 0.18942 0.07091 H20 2 0.065215 0.504299 0.057389 11.00000 -1.50000 HKLF 4 REM TEST_a.res in P2(1)/c REM wR2 = 0.1185, GooF = S = 1.040, Restrained GooF = 1.056 for all data REM R1 = 0.0487 for 3083 Fo > 4sig(Fo) and 0.0639 for all 3781 data REM 259 parameters refined using 10 restraints END WGHT 0.0295 5.0226 REM Instructions for potential hydrogen bonds HTAB O3 O1W EQIV $3 x+1, y, z HTAB C2 Cl2_$3 EQIV $4 -x+1, -y+1, -z+2 HTAB C4 O2_$4 EQIV $5 -x, y+1/2, -z+3/2 HTAB C9 Cl2_$5 EQIV $1 -x+1, -y+1, -z+1 HTAB C11 Cl1_$1 HTAB C12 O2_$4 EQIV $6 x, -y+1/2, z+1/2 HTAB C13 O1W_$6 EQIV $7 x, y, z+1 HTAB C15 Cl1_$7 HTAB C15 Cl1_$6 HTAB O1W Cl2 EQIV $8 x, -y+1/2, z-1/2 HTAB O1W Cl2_$8 REM Highest difference peak 0.838, deepest hole -0.713, 1-sigma level 0.092 Q1 1 0.0591 0.2512 0.3796 11.00000 0.05 0.83 Q2 1 0.3370 0.4228 0.5008 11.00000 0.05 0.50 Q3 1 0.4611 0.3462 0.3023 11.00000 0.05 0.48 Q4 1 0.1428 0.2895 0.3921 11.00000 0.05 0.46 Q5 1 0.1422 0.2275 0.4345 11.00000 0.05 0.43 Q6 1 0.3992 0.4289 0.4353 11.00000 0.05 0.42 Q7 1 0.3142 0.4716 0.4840 11.00000 0.05 0.38 Q8 1 0.4832 0.4223 0.5323 11.00000 0.05 0.35 Q9 1 0.0070 0.1244 0.5456 11.00000 0.05 0.33 Q10 1 0.4307 0.5005 0.4995 11.00000 0.05 0.31 ; _shelx_res_checksum 40879 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.40697(4) 0.41906(3) 0.51315(5) 0.01599(14) Uani 1 1 d . . . . . Cl1 Cl 0.37827(8) 0.36745(5) 0.28452(9) 0.0238(2) Uani 1 1 d . . . . . N1 N 0.5531(2) 0.35586(17) 0.6318(3) 0.0180(6) Uani 1 1 d . . . . . N2 N 0.2594(2) 0.49412(18) 0.4989(3) 0.0209(6) Uani 1 1 d . . . . . N3 N 0.3982(2) 0.44142(17) 0.7424(3) 0.0164(6) Uani 1 1 d . . . . . O1 O 0.4946(2) 0.39142(15) 0.9665(2) 0.0214(5) Uani 1 1 d . . . . . O2 O 0.3042(2) 0.51944(16) 0.8817(3) 0.0247(6) Uani 1 1 d . . . . . O3 O 0.3011(2) 0.32541(15) 0.5689(3) 0.0206(6) Uani 1 1 d . . . . . H3A H 0.261(4) 0.306(3) 0.511(5) 0.025 Uiso 1 1 d . U . . . O4 O 0.500000 0.500000 0.500000 0.0212(8) Uani 1 2 d S . P . . C1 C 0.6200(3) 0.3078(2) 0.5715(4) 0.0216(8) Uani 1 1 d . . . . . H1 H 0.592734 0.291016 0.474049 0.026 Uiso 1 1 calc R U . . . C2 C 0.7260(3) 0.2820(2) 0.6446(4) 0.0252(8) Uani 1 1 d . . . . . H2 H 0.770741 0.247645 0.598906 0.030 Uiso 1 1 calc R U . . . C3 C 0.7666(3) 0.3072(2) 0.7872(4) 0.0242(8) Uani 1 1 d . . . . . H3 H 0.839780 0.290547 0.840546 0.029 Uiso 1 1 calc R U . . . C4 C 0.6983(3) 0.3571(2) 0.8496(4) 0.0220(8) Uani 1 1 d . . . . . H4 H 0.724237 0.375574 0.946290 0.026 Uiso 1 1 calc R U . . . C5 C 0.5917(3) 0.3797(2) 0.7692(4) 0.0184(7) Uani 1 1 d . . . . . C6 C 0.1772(3) 0.5059(2) 0.3784(4) 0.0255(8) Uani 1 1 d . . . . . H6 H 0.180758 0.477147 0.292737 0.031 Uiso 1 1 calc R U . . . C7 C 0.0884(3) 0.5582(2) 0.3754(5) 0.0310(9) Uani 1 1 d . . . . . H7 H 0.031978 0.565900 0.288642 0.037 Uiso 1 1 calc R U . . . C8 C 0.0820(3) 0.5996(3) 0.5000(5) 0.0330(10) Uani 1 1 d . . . . . H8 H 0.021199 0.636070 0.499674 0.040 Uiso 1 1 calc R U . . . C9 C 0.1652(3) 0.5875(2) 0.6255(5) 0.0278(8) Uani 1 1 d . . . . . H9 H 0.161834 0.614667 0.712824 0.033 Uiso 1 1 calc R U . . . C10 C 0.2537(3) 0.5346(2) 0.6204(4) 0.0210(8) Uani 1 1 d . . . . . C11 C 0.3488(3) 0.5206(2) 0.7535(4) 0.0208(7) Uani 1 1 d . . . . . H11 H 0.409827 0.561888 0.760595 0.025 Uiso 1 1 calc R U . . . C12 C 0.5140(3) 0.4309(2) 0.8403(4) 0.0181(7) Uani 1 1 d . . . . . H12 H 0.550787 0.483388 0.867177 0.022 Uiso 1 1 calc R U . . . C13 C 0.2411(3) 0.3407(2) 0.6828(4) 0.0251(8) Uani 1 1 d . . . . . H13A H 0.218026 0.290276 0.721484 0.030 Uiso 1 1 calc R U . . . H13B H 0.170510 0.371584 0.644347 0.030 Uiso 1 1 calc R U . . . C14 C 0.3193(3) 0.3865(2) 0.8034(4) 0.0198(7) Uani 1 1 d . . . . . C15 C 0.4044(3) 0.3369(2) 0.9092(4) 0.0222(8) Uani 1 1 d . . . . . H15A H 0.368715 0.315567 0.987282 0.027 Uiso 1 1 calc R U . . . H15B H 0.433710 0.292591 0.858795 0.027 Uiso 1 1 calc R U . . . C16 C 0.2515(3) 0.4432(2) 0.8845(4) 0.0252(8) Uani 1 1 d . . . . . H16A H 0.169230 0.445137 0.834946 0.030 Uiso 1 1 calc R U . . . H16B H 0.256750 0.425483 0.985996 0.030 Uiso 1 1 calc R U . . . Cl2 Cl -0.00961(11) 0.17589(9) 0.62069(16) 0.0575(4) Uani 1 1 d . . . . . O1W O 0.1241(3) 0.2497(2) 0.4069(3) 0.0498(9) Uani 1 1 d D . . . . H12A H 0.081(4) 0.230(3) 0.455(5) 0.075 Uiso 1 1 d D U . . . H11A H 0.086(4) 0.277(3) 0.342(5) 0.075 Uiso 1 1 d D U . . . O2W O 0.000000 0.500000 0.000000 0.176(5) Uani 1 2 d DS U P . . H20 H 0.065(7) 0.504(11) 0.057(16) 0.264 Uiso 1 1 d D U . . . 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 Fe 0.0176(3) 0.0162(2) 0.0142(3) -0.0001(2) 0.00346(18) -0.00075(19) Cl1 0.0318(5) 0.0255(5) 0.0141(4) -0.0026(3) 0.0050(3) -0.0024(4) N1 0.0200(15) 0.0180(14) 0.0159(14) 0.0006(12) 0.0034(12) -0.0002(12) N2 0.0198(15) 0.0229(15) 0.0201(15) 0.0026(13) 0.0046(12) 0.0011(12) N3 0.0178(14) 0.0186(14) 0.0126(14) -0.0016(12) 0.0026(11) -0.0024(11) O1 0.0236(13) 0.0277(13) 0.0128(12) 0.0013(10) 0.0037(10) -0.0026(10) O2 0.0251(14) 0.0309(14) 0.0198(13) -0.0058(11) 0.0084(11) -0.0004(11) O3 0.0254(14) 0.0223(13) 0.0146(13) -0.0043(10) 0.0053(10) -0.0079(10) O4 0.0206(18) 0.0185(17) 0.0238(19) 0.0009(15) 0.0032(14) -0.0027(14) C1 0.0241(19) 0.0210(18) 0.0215(18) -0.0041(15) 0.0087(15) -0.0018(15) C2 0.027(2) 0.0248(19) 0.025(2) -0.0033(16) 0.0077(16) 0.0024(15) C3 0.0217(18) 0.0275(19) 0.0218(19) 0.0030(16) 0.0007(15) 0.0028(15) C4 0.0236(19) 0.0250(19) 0.0174(18) -0.0009(15) 0.0040(14) -0.0006(15) C5 0.0221(18) 0.0181(17) 0.0160(17) 0.0015(14) 0.0066(14) -0.0009(14) C6 0.0236(19) 0.032(2) 0.0207(19) 0.0046(16) 0.0039(15) -0.0002(16) C7 0.0196(19) 0.037(2) 0.034(2) 0.0069(19) 0.0005(17) 0.0031(17) C8 0.022(2) 0.034(2) 0.043(3) 0.0046(19) 0.0057(18) 0.0066(17) C9 0.0242(19) 0.026(2) 0.034(2) -0.0028(17) 0.0093(16) 0.0020(16) C10 0.0201(18) 0.0200(18) 0.0233(19) 0.0001(15) 0.0051(14) -0.0022(14) C11 0.0235(18) 0.0198(17) 0.0198(18) -0.0034(15) 0.0065(14) 0.0018(14) C12 0.0192(17) 0.0191(17) 0.0155(17) -0.0004(14) 0.0027(13) -0.0025(14) C13 0.0264(19) 0.036(2) 0.0139(17) -0.0042(16) 0.0068(15) -0.0125(17) C14 0.0249(18) 0.0223(17) 0.0139(17) -0.0015(14) 0.0082(14) -0.0062(15) C15 0.0245(19) 0.0250(18) 0.0171(18) 0.0014(15) 0.0045(15) -0.0030(15) C16 0.026(2) 0.032(2) 0.0200(19) -0.0021(16) 0.0088(15) -0.0032(16) Cl2 0.0436(7) 0.0687(9) 0.0629(9) 0.0085(7) 0.0176(6) 0.0016(6) O1W 0.062(2) 0.067(3) 0.0269(17) -0.0213(16) 0.0238(16) -0.0248(19) O2W 0.283(12) 0.102(7) 0.204(11) 0.041(8) 0.189(10) 0.071(9) 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Fe N1 88.61(8) . . ? O4 Fe N2 92.78(8) . . ? N1 Fe N2 152.86(11) . . ? O4 Fe O3 170.07(7) . . ? N1 Fe O3 87.39(11) . . ? N2 Fe O3 86.69(11) . . ? O4 Fe N3 95.31(8) . . ? N1 Fe N3 77.12(11) . . ? N2 Fe N3 75.77(11) . . ? O3 Fe N3 74.94(10) . . ? O4 Fe Cl1 101.66(3) . . ? N1 Fe Cl1 104.09(8) . . ? N2 Fe Cl1 102.16(9) . . ? O3 Fe Cl1 88.13(7) . . ? N3 Fe Cl1 163.00(8) . . ? C5 N1 C1 118.5(3) . . ? C5 N1 Fe 115.3(2) . . ? C1 N1 Fe 124.7(2) . . ? C6 N2 C10 118.9(3) . . ? C6 N2 Fe 125.3(3) . . ? C10 N2 Fe 115.8(2) . . ? C11 N3 C12 113.1(3) . . ? C11 N3 C14 104.3(3) . . ? C12 N3 C14 104.8(3) . . ? C11 N3 Fe 109.0(2) . . ? C12 N3 Fe 110.7(2) . . ? C14 N3 Fe 115.0(2) . . ? C12 O1 C15 103.3(2) . . ? C11 O2 C16 105.7(3) . . ? C13 O3 Fe 117.2(2) . . ? C13 O3 H3A 107(4) . . ? Fe O3 H3A 119(4) . . ? Fe O4 Fe 180.0 3_666 . ? N1 C1 C2 122.9(3) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C1 C2 C3 118.6(3) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C4 C3 C2 118.7(3) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C3 C4 C5 119.1(3) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 122.1(3) . . ? N1 C5 C12 118.7(3) . . ? C4 C5 C12 119.2(3) . . ? N2 C6 C7 122.0(4) . . ? N2 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C6 C7 C8 119.3(4) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C7 C8 C9 119.4(4) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C8 C9 C10 118.3(4) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? N2 C10 C9 122.1(3) . . ? N2 C10 C11 117.3(3) . . ? C9 C10 C11 120.6(3) . . ? O2 C11 N3 105.8(3) . . ? O2 C11 C10 111.0(3) . . ? N3 C11 C10 108.7(3) . . ? O2 C11 H11 110.4 . . ? N3 C11 H11 110.4 . . ? C10 C11 H11 110.4 . . ? O1 C12 N3 106.3(3) . . ? O1 C12 C5 108.5(3) . . ? N3 C12 C5 111.2(3) . . ? O1 C12 H12 110.3 . . ? N3 C12 H12 110.3 . . ? C5 C12 H12 110.3 . . ? O3 C13 C14 109.2(3) . . ? O3 C13 H13A 109.8 . . ? C14 C13 H13A 109.8 . . ? O3 C13 H13B 109.8 . . ? C14 C13 H13B 109.8 . . ? H13A C13 H13B 108.3 . . ? C15 C14 N3 102.1(3) . . ? C15 C14 C13 115.2(3) . . ? N3 C14 C13 111.1(3) . . ? C15 C14 C16 111.4(3) . . ? N3 C14 C16 103.3(3) . . ? C13 C14 C16 112.6(3) . . ? O1 C15 C14 103.4(3) . . ? O1 C15 H15A 111.1 . . ? C14 C15 H15A 111.1 . . ? O1 C15 H15B 111.1 . . ? C14 C15 H15B 111.1 . . ? H15A C15 H15B 109.1 . . ? O2 C16 C14 106.0(3) . . ? O2 C16 H16A 110.5 . . ? C14 C16 H16A 110.5 . . ? O2 C16 H16B 110.5 . . ? C14 C16 H16B 110.5 . . ? H16A C16 H16B 108.7 . . ? H12A O1W H11A 109(3) . . ? H20 O2W H20 180.00(2) . 3_565 ? 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 Fe O4 1.7825(5) . ? Fe N1 2.143(3) . ? Fe N2 2.147(3) . ? Fe O3 2.158(3) . ? Fe N3 2.214(3) . ? Fe Cl1 2.2802(10) . ? N1 C5 1.339(4) . ? N1 C1 1.343(4) . ? N2 C6 1.346(5) . ? N2 C10 1.346(5) . ? N3 C11 1.478(4) . ? N3 C12 1.496(4) . ? N3 C14 1.517(4) . ? O1 C12 1.423(4) . ? O1 C15 1.432(4) . ? O2 C11 1.415(4) . ? O2 C16 1.440(5) . ? O3 C13 1.429(4) . ? O3 H3A 0.72(4) . ? C1 C2 1.373(5) . ? C1 H1 0.9500 . ? C2 C3 1.394(5) . ? C2 H2 0.9500 . ? C3 C4 1.385(5) . ? C3 H3 0.9500 . ? C4 C5 1.385(5) . ? C4 H4 0.9500 . ? C5 C12 1.522(5) . ? C6 C7 1.374(5) . ? C6 H6 0.9500 . ? C7 C8 1.382(6) . ? C7 H7 0.9500 . ? C8 C9 1.386(6) . ? C8 H8 0.9500 . ? C9 C10 1.390(5) . ? C9 H9 0.9500 . ? C10 C11 1.518(5) . ? C11 H11 1.0000 . ? C12 H12 1.0000 . ? C13 C14 1.520(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.515(5) . ? C14 C16 1.554(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? O1W H12A 0.824(19) . ? O1W H11A 0.823(19) . ? O2W H20 0.85(2) . ? O2W H20 0.85(2) 3_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 C1 C2 0.1(5) . . . . ? Fe N1 C1 C2 165.4(3) . . . . ? N1 C1 C2 C3 -0.6(6) . . . . ? C1 C2 C3 C4 0.2(6) . . . . ? C2 C3 C4 C5 0.6(5) . . . . ? C1 N1 C5 C4 0.8(5) . . . . ? Fe N1 C5 C4 -165.9(3) . . . . ? C1 N1 C5 C12 -177.2(3) . . . . ? Fe N1 C5 C12 16.2(4) . . . . ? C3 C4 C5 N1 -1.1(5) . . . . ? C3 C4 C5 C12 176.8(3) . . . . ? C10 N2 C6 C7 0.4(6) . . . . ? Fe N2 C6 C7 -176.4(3) . . . . ? N2 C6 C7 C8 -0.7(6) . . . . ? C6 C7 C8 C9 -0.1(6) . . . . ? C7 C8 C9 C10 1.0(6) . . . . ? C6 N2 C10 C9 0.6(5) . . . . ? Fe N2 C10 C9 177.7(3) . . . . ? C6 N2 C10 C11 -179.1(3) . . . . ? Fe N2 C10 C11 -2.1(4) . . . . ? C8 C9 C10 N2 -1.3(6) . . . . ? C8 C9 C10 C11 178.4(3) . . . . ? C16 O2 C11 N3 -40.1(3) . . . . ? C16 O2 C11 C10 77.7(3) . . . . ? C12 N3 C11 O2 -78.8(3) . . . . ? C14 N3 C11 O2 34.4(3) . . . . ? Fe N3 C11 O2 157.7(2) . . . . ? C12 N3 C11 C10 161.9(3) . . . . ? C14 N3 C11 C10 -84.9(3) . . . . ? Fe N3 C11 C10 38.4(3) . . . . ? N2 C10 C11 O2 -141.1(3) . . . . ? C9 C10 C11 O2 39.1(5) . . . . ? N2 C10 C11 N3 -25.1(4) . . . . ? C9 C10 C11 N3 155.1(3) . . . . ? C15 O1 C12 N3 37.9(3) . . . . ? C15 O1 C12 C5 -81.8(3) . . . . ? C11 N3 C12 O1 98.0(3) . . . . ? C14 N3 C12 O1 -14.9(3) . . . . ? Fe N3 C12 O1 -139.4(2) . . . . ? C11 N3 C12 C5 -144.1(3) . . . . ? C14 N3 C12 C5 103.0(3) . . . . ? Fe N3 C12 C5 -21.5(3) . . . . ? N1 C5 C12 O1 121.0(3) . . . . ? C4 C5 C12 O1 -57.0(4) . . . . ? N1 C5 C12 N3 4.4(4) . . . . ? C4 C5 C12 N3 -173.6(3) . . . . ? Fe O3 C13 C14 -40.3(4) . . . . ? C11 N3 C14 C15 -131.4(3) . . . . ? C12 N3 C14 C15 -12.3(3) . . . . ? Fe N3 C14 C15 109.4(2) . . . . ? C11 N3 C14 C13 105.3(3) . . . . ? C12 N3 C14 C13 -135.7(3) . . . . ? Fe N3 C14 C13 -13.9(4) . . . . ? C11 N3 C14 C16 -15.7(3) . . . . ? C12 N3 C14 C16 103.4(3) . . . . ? Fe N3 C14 C16 -134.9(2) . . . . ? O3 C13 C14 C15 -82.1(4) . . . . ? O3 C13 C14 N3 33.4(4) . . . . ? O3 C13 C14 C16 148.7(3) . . . . ? C12 O1 C15 C14 -45.8(3) . . . . ? N3 C14 C15 O1 35.4(3) . . . . ? C13 C14 C15 O1 155.9(3) . . . . ? C16 C14 C15 O1 -74.3(3) . . . . ? C11 O2 C16 C14 29.0(3) . . . . ? C15 C14 C16 O2 101.5(3) . . . . ? N3 C14 C16 O2 -7.4(3) . . . . ? C13 C14 C16 O2 -127.4(3) . . . . ?