#------------------------------------------------------------------------------ #$Date: 2016-02-14 04:40:26 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176432 $ #$URL: svn://www.crystallography.net/cod/cif/4/30/10/4301091.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_4301091 loop_ _publ_author_name 'Salah Ezzaher' 'Jean-Fran\,cois Capon' 'Fr\'ed\'eric Gloaguen' 'Fran\,cois Y. P\'etillon' 'Philippe Schollhammer' 'Jean Talarmin' 'Nelly Kervarec' _publ_contact_author_address ;Laboratoire de chimie, electrochimie moleculaire et chimie analytique (UMR 6521) Universite de Bretagne occidentale 6, avenue Victor Le Gorgeu CS 93837 F-29238 BREST cedex 3 FRANCE ; _publ_contact_author_email philippe.schollhammer@univ-brest.fr _publ_contact_author_name 'Schollhammer, Philippe' _publ_section_title ; Influence of a Pendant Amine in the Second Coordination Sphere on Proton Transfer at a Dissymmetrically Disubstituted Diiron System Related to the [2Fe]H Subsite of [FeFe]H2ase ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 2 _journal_page_last 4 _journal_paper_doi 10.1021/ic801369u _journal_volume 48 _journal_year 2009 _chemical_formula_moiety ; C34 H34 Fe2 N O4 P2 S2 1+, B F4 1-, 2(C3 H6 O) ; _chemical_formula_sum 'C40 H46 B F4 Fe2 N O6 P2 S2' _chemical_formula_weight 961.35 _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_creation_date 2008-04-22T12:31:50-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90 _cell_angle_beta 98.255(4) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 37.0169(15) _cell_length_b 11.4623(4) _cell_length_c 20.7172(10) _cell_measurement_reflns_used 6284 _cell_measurement_temperature 170(2) _cell_measurement_theta_max 23.12 _cell_measurement_theta_min 2.1 _cell_volume 8699.2(6) _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1980-2002)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 170(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.3622 _diffrn_measured_fraction_theta_full 0.88 _diffrn_measured_fraction_theta_max 0.88 _diffrn_measurement_device 'Kappa-geometry diffractometer' _diffrn_measurement_device_type 'Oxford Diffraction XCALIBUR2' _diffrn_measurement_method ; 1 stepped phi-scan over 360 deg with detector angle 30 deg. 1 stepped omega-scans over 106 deg. with kappa -79 deg. (chi -58.3 deg.) and detector angle 0 step 1 deg., exposure time 240 s detector distance 50 mm ; _diffrn_orient_matrix_UB_11 -0.0095545481 _diffrn_orient_matrix_UB_12 -0.0525503924 _diffrn_orient_matrix_UB_13 -0.008825649 _diffrn_orient_matrix_UB_21 0.0162148284 _diffrn_orient_matrix_UB_22 -0.0323172342 _diffrn_orient_matrix_UB_23 0.0096868112 _diffrn_orient_matrix_UB_31 -0.0045437303 _diffrn_orient_matrix_UB_32 -0.0047390625 _diffrn_orient_matrix_UB_33 0.0320065511 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_unetI/netI 0.0545 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 25334 _diffrn_reflns_theta_full 23.26 _diffrn_reflns_theta_max 23.26 _diffrn_reflns_theta_min 2.72 _diffrn_source 'sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.899 _exptl_absorpt_correction_type none _exptl_crystal_colour 'dark red' _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_description ; truncated lozenge, main faces {1 0 0}, diagonals [0 1 0] and [0 0 1] ; _exptl_crystal_F_000 3968 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.444 _refine_diff_density_min -0.256 _refine_diff_density_rms 0.06 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.97 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 523 _refine_ls_number_reflns 5501 _refine_ls_number_restraints 162 _refine_ls_restrained_S_all 0.962 _refine_ls_R_factor_all 0.06 _refine_ls_R_factor_gt 0.0335 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.0747 _reflns_number_gt 3931 _reflns_number_total 5501 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic801369u_si_002_2.cif _cod_data_source_block sez18-a-compound2 _cod_depositor_comments ; The following automatic conversions were performed: '_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_sg_symbol_Hall -C2yc _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 4301091 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.12358(10) 0.6495(3) 0.3663(2) 0.0278(9) Uani 1 1 d U A 1 C2 C 0.00929(10) 0.6559(3) 0.35863(17) 0.0311(9) Uani 1 1 d U A 1 C3 C 0.00840(11) 0.4221(3) 0.3583(2) 0.0456(11) Uani 1 1 d U A 1 C4 C 0.05182(10) 0.5523(3) 0.2902(2) 0.0353(10) Uani 1 1 d U A 1 C5A C 0.05107(10) 0.4444(3) 0.52566(19) 0.0370(10) Uani 0.8 1 d PU A 1 H5A H 0.05 0.4655 0.5717 0.044 Uiso 0.8 1 calc PR A 1 H5B H 0.0286 0.3998 0.5099 0.044 Uiso 0.8 1 calc PR A 1 C6A C 0.08244(12) 0.3671(4) 0.5241(2) 0.0349(12) Uiso 0.8 1 d PU A 1 H6A H 0.0796 0.2982 0.5518 0.042 Uiso 0.8 1 calc PR A 1 H6B H 0.1048 0.4087 0.5436 0.042 Uiso 0.8 1 calc PR A 1 C7A C 0.08756(12) 0.3255(3) 0.45710(19) 0.0460(11) Uani 0.8 1 d PU A 1 H7A H 0.0661 0.277 0.4402 0.055 Uiso 0.8 1 calc PR A 1 H7B H 0.1092 0.2737 0.4619 0.055 Uiso 0.8 1 calc PR A 1 C8 C 0.14141(8) 0.8864(3) 0.47522(17) 0.0237(8) Uani 1 1 d U A 1 H8A H 0.1521 0.8997 0.4347 0.028 Uiso 1 1 calc R A 1 H8B H 0.1358 0.9641 0.4922 0.028 Uiso 1 1 calc R A 1 C9 C 0.18445(8) 0.7181(3) 0.50182(16) 0.0218(8) Uani 1 1 d U A 1 H9A H 0.207 0.6964 0.5311 0.026 Uiso 1 1 calc R A 1 H9B H 0.1909 0.7284 0.4574 0.026 Uiso 1 1 calc R A 1 C10 C 0.08001(9) 0.9078(3) 0.38421(16) 0.0226(8) Uani 1 1 d U A 1 C11 C 0.07908(10) 1.0282(3) 0.39353(17) 0.0318(9) Uani 1 1 d U A 1 H11 H 0.0881 1.0603 0.435 0.038 Uiso 1 1 calc R A 1 C12 C 0.06518(11) 1.1008(3) 0.34301(18) 0.0388(10) Uani 1 1 d U A 1 H12 H 0.0655 1.1829 0.3494 0.047 Uiso 1 1 calc R A 1 C13 C 0.05088(10) 1.0557(3) 0.28383(18) 0.0348(10) Uani 1 1 d U A 1 H13 H 0.0407 1.1062 0.2497 0.042 Uiso 1 1 calc R A 1 C14 C 0.05127(9) 0.9372(3) 0.27370(17) 0.0282(9) Uani 1 1 d U A 1 H14 H 0.0412 0.9055 0.2326 0.034 Uiso 1 1 calc R A 1 C15 C 0.06627(9) 0.8646(3) 0.32338(17) 0.0256(9) Uani 1 1 d U A 1 H15 H 0.0672 0.783 0.3156 0.031 Uiso 1 1 calc R A 1 C20 C 0.07012(9) 0.8587(3) 0.51315(17) 0.0222(8) Uani 1 1 d U A 1 C21 C 0.08515(10) 0.9007(3) 0.57352(19) 0.0382(10) Uani 1 1 d U A 1 H21 H 0.1109 0.9058 0.5843 0.046 Uiso 1 1 calc R A 1 C22 C 0.06311(11) 0.9355(4) 0.6184(2) 0.0514(12) Uani 1 1 d U A 1 H22 H 0.0739 0.9642 0.6597 0.062 Uiso 1 1 calc R A 1 C23 C 0.02580(11) 0.9290(3) 0.6040(2) 0.0436(11) Uani 1 1 d U A 1 H23 H 0.0108 0.9535 0.6351 0.052 Uiso 1 1 calc R A 1 C24 C 0.01038(10) 0.8871(3) 0.5445(2) 0.0344(10) Uani 1 1 d U A 1 H24 H -0.0154 0.8812 0.5345 0.041 Uiso 1 1 calc R A 1 C25 C 0.03210(9) 0.8534(3) 0.49925(18) 0.0277(9) Uani 1 1 d U A 1 H25 H 0.021 0.826 0.4578 0.033 Uiso 1 1 calc R A 1 C30 C 0.15066(9) 0.5811(3) 0.58788(16) 0.0221(8) Uani 1 1 d U A 1 C31 C 0.18116(10) 0.5423(3) 0.63046(19) 0.0316(9) Uani 1 1 d U A 1 H31 H 0.2028 0.5207 0.6139 0.038 Uiso 1 1 calc R A 1 C32 C 0.17963(11) 0.5356(3) 0.6966(2) 0.0396(10) Uani 1 1 d U A 1 H32 H 0.2003 0.509 0.7254 0.047 Uiso 1 1 calc R A 1 C33 C 0.14839(12) 0.5670(3) 0.72108(19) 0.0390(10) Uani 1 1 d U A 1 H33 H 0.1475 0.5608 0.7666 0.047 Uiso 1 1 calc R A 1 C34 C 0.11863(10) 0.6072(3) 0.6805(2) 0.0362(10) Uani 1 1 d U A 1 H34 H 0.0973 0.6306 0.6978 0.043 Uiso 1 1 calc R A 1 C35 C 0.11960(10) 0.6139(3) 0.6141(2) 0.0304(9) Uani 1 1 d U A 1 H35 H 0.0988 0.6412 0.5859 0.036 Uiso 1 1 calc R A 1 C40 C 0.18012(8) 0.4799(3) 0.47604(17) 0.0245(9) Uani 1 1 d U A 1 C41 C 0.18034(10) 0.3694(3) 0.50358(18) 0.0325(9) Uani 1 1 d U A 1 H41 H 0.1682 0.3565 0.5403 0.039 Uiso 1 1 calc R A 1 C42 C 0.19806(11) 0.2781(3) 0.4781(2) 0.0435(11) Uani 1 1 d U A 1 H42 H 0.1975 0.2028 0.4971 0.052 Uiso 1 1 calc R A 1 C43 C 0.21634(10) 0.2941(3) 0.4259(2) 0.0426(11) Uani 1 1 d U A 1 H43 H 0.2285 0.2307 0.4089 0.051 Uiso 1 1 calc R A 1 C44 C 0.21683(10) 0.4040(3) 0.39829(19) 0.0380(10) Uani 1 1 d U A 1 H44 H 0.2296 0.4162 0.3623 0.046 Uiso 1 1 calc R A 1 C45 C 0.19888(9) 0.4958(3) 0.42276(18) 0.0307(9) Uani 1 1 d U A 1 H45 H 0.1993 0.5707 0.4032 0.037 Uiso 1 1 calc R A 1 N50 N 0.17073(7) 0.8321(2) 0.52427(13) 0.0218(7) Uani 1 1 d U A 1 H50 H 0.1611 0.8192 0.5627 0.026 Uiso 1 1 calc R A 1 C51 C 0.20205(9) 0.9159(3) 0.53848(18) 0.0338(10) Uani 1 1 d U A 1 H51A H 0.1932 0.9897 0.5543 0.051 Uiso 1 1 calc R A 1 H51B H 0.2127 0.93 0.4985 0.051 Uiso 1 1 calc R A 1 H51C H 0.2206 0.8826 0.5719 0.051 Uiso 1 1 calc R A 1 O1 O 0.13790(7) 0.6646(2) 0.32098(14) 0.0408(7) Uani 1 1 d U A 1 O2 O -0.01168(7) 0.7296(2) 0.35179(13) 0.0448(7) Uani 1 1 d U A 1 O3 O -0.01302(8) 0.3496(3) 0.34791(17) 0.0769(10) Uani 1 1 d U A 1 O4 O 0.05896(7) 0.5629(2) 0.23796(16) 0.0517(8) Uani 1 1 d U A 1 S1A S 0.05018(2) 0.57961(7) 0.47819(5) 0.0287(2) Uani 0.8 1 d PU A 1 S2A S 0.09350(2) 0.43528(7) 0.39429(5) 0.0307(2) Uani 0.8 1 d PU A 1 Fe1 Fe 0.100790(12) 0.61979(4) 0.43278(2) 0.02116(15) Uani 1 1 d U A 1 Fe2 Fe 0.041176(13) 0.53842(4) 0.37022(3) 0.02948(16) Uani 1 1 d U A 1 P1 P 0.09710(2) 0.80874(7) 0.45207(4) 0.0205(2) Uani 1 1 d U A 1 P2 P 0.15122(2) 0.59703(7) 0.50025(4) 0.0219(2) Uani 1 1 d U A 1 C5B C 0.05107(10) 0.4444(3) 0.52566(19) 0.0370(10) Uani 0.2 1 d PDU B 2 H5C H 0.0708 0.4508 0.5633 0.044 Uiso 0.2 1 calc PR B 2 H5D H 0.0277 0.4378 0.5433 0.044 Uiso 0.2 1 calc PR B 2 C6B C 0.0570(5) 0.3316(14) 0.4888(9) 0.038(5) Uiso 0.2 1 d PDU B 2 H6C H 0.0582 0.2661 0.5202 0.046 Uiso 0.2 1 calc PR B 2 H6D H 0.0351 0.3187 0.4559 0.046 Uiso 0.2 1 calc PR B 2 C7B C 0.08756(12) 0.3255(3) 0.45710(19) 0.0460(11) Uani 0.2 1 d PDU B 2 H7C H 0.0876 0.2477 0.4364 0.055 Uiso 0.2 1 calc PR B 2 H7D H 0.1094 0.3291 0.4908 0.055 Uiso 0.2 1 calc PR B 2 S1B S 0.05018(2) 0.57961(7) 0.47819(5) 0.0287(2) Uani 0.2 1 d PU B 2 S2B S 0.09350(2) 0.43528(7) 0.39429(5) 0.0307(2) Uani 0.2 1 d PU B 2 B1 B 0.27852(12) 0.6087(4) 0.6394(2) 0.0362(12) Uani 1 1 d U . . F1 F 0.26206(6) 0.7045(2) 0.60953(12) 0.0662(7) Uani 1 1 d U . . F2 F 0.26891(7) 0.5105(2) 0.60211(12) 0.0792(8) Uani 1 1 d U . . F3 F 0.31572(6) 0.6206(2) 0.64763(11) 0.0573(7) Uani 1 1 d U . . F4 F 0.26678(6) 0.59211(18) 0.69967(11) 0.0470(6) Uiso 1 1 d U . . C70 C 0.17914(11) 0.8531(3) 0.7173(2) 0.0376(10) Uani 1 1 d U . . C71 C 0.21792(11) 0.8244(4) 0.7404(2) 0.0554(12) Uani 1 1 d U . . H71A H 0.2313 0.8196 0.7029 0.083 Uiso 1 1 calc R . . H71B H 0.2194 0.7493 0.7632 0.083 Uiso 1 1 calc R . . H71C H 0.2287 0.8855 0.7702 0.083 Uiso 1 1 calc R . . C72 C 0.15500(11) 0.8730(4) 0.7679(2) 0.0560(12) Uani 1 1 d U . . H72A H 0.1295 0.8747 0.7472 0.084 Uiso 1 1 calc R . . H72B H 0.1613 0.9475 0.7898 0.084 Uiso 1 1 calc R . . H72C H 0.1584 0.8096 0.8 0.084 Uiso 1 1 calc R . . O70 O 0.16761(8) 0.8617(2) 0.65954(14) 0.0496(8) Uani 1 1 d U . . C80 C 0.14974(12) 0.1752(3) 0.6337(2) 0.0474(11) Uani 1 1 d U . . C81 C 0.18752(13) 0.1980(4) 0.6655(2) 0.0782(15) Uani 1 1 d U . . H81A H 0.2045 0.1855 0.634 0.117 Uiso 1 1 calc R . . H81B H 0.1936 0.1447 0.7025 0.117 Uiso 1 1 calc R . . H81C H 0.1895 0.2788 0.6811 0.117 Uiso 1 1 calc R . . C82 C 0.12019(15) 0.2066(5) 0.6723(3) 0.0968(19) Uani 1 1 d U . . H82A H 0.0973 0.1698 0.6528 0.145 Uiso 1 1 calc R . . H82B H 0.1171 0.2915 0.6722 0.145 Uiso 1 1 calc R . . H82C H 0.1267 0.1792 0.7172 0.145 Uiso 1 1 calc R . . O80 O 0.14321(8) 0.1343(2) 0.57972(15) 0.0527(8) Uani 1 1 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 C1 0.027(2) 0.019(2) 0.035(3) -0.0070(18) -0.0024(19) 0.0016(16) C2 0.025(2) 0.035(2) 0.032(3) 0.0035(18) -0.0022(18) -0.0073(18) C3 0.037(2) 0.031(2) 0.062(3) 0.009(2) -0.017(2) -0.0015(19) C4 0.031(2) 0.029(2) 0.041(3) -0.007(2) -0.011(2) 0.0050(18) C5A 0.033(2) 0.032(2) 0.043(3) 0.0116(18) -0.0015(19) -0.0088(18) C7A 0.067(3) 0.0140(19) 0.051(3) 0.0015(18) -0.014(2) 0.0004(19) C8 0.0252(19) 0.0180(18) 0.028(2) 0.0015(16) 0.0040(16) 0.0004(16) C9 0.0206(19) 0.0243(18) 0.020(2) 0.0001(15) 0.0002(15) 0.0003(15) C10 0.0256(19) 0.0231(19) 0.020(2) -0.0039(15) 0.0051(17) -0.0010(16) C11 0.047(2) 0.027(2) 0.020(2) -0.0029(17) 0.0000(18) 0.0026(19) C12 0.061(3) 0.022(2) 0.031(3) 0.0032(18) 0.001(2) 0.004(2) C13 0.048(3) 0.034(2) 0.022(3) 0.0114(18) 0.0037(19) 0.0010(19) C14 0.034(2) 0.031(2) 0.020(2) 0.0009(17) 0.0024(17) -0.0038(17) C15 0.032(2) 0.0219(19) 0.024(2) 0.0011(16) 0.0057(18) -0.0010(17) C20 0.024(2) 0.0183(19) 0.025(2) 0.0008(16) 0.0056(17) 0.0033(15) C21 0.033(2) 0.054(3) 0.029(3) -0.009(2) 0.007(2) 0.005(2) C22 0.046(3) 0.083(3) 0.025(3) -0.015(2) 0.005(2) 0.008(2) C23 0.049(3) 0.055(3) 0.031(3) -0.001(2) 0.022(2) 0.010(2) C24 0.028(2) 0.035(2) 0.042(3) 0.007(2) 0.012(2) 0.0061(18) C25 0.032(2) 0.027(2) 0.024(2) -0.0017(17) 0.0047(18) 0.0060(17) C30 0.026(2) 0.0205(18) 0.020(2) 0.0007(15) 0.0034(17) -0.0078(16) C31 0.033(2) 0.029(2) 0.032(3) -0.0010(18) 0.0008(18) -0.0073(18) C32 0.045(3) 0.042(2) 0.028(3) 0.0048(19) -0.007(2) -0.005(2) C33 0.061(3) 0.041(2) 0.017(3) 0.0047(19) 0.011(2) -0.016(2) C34 0.040(2) 0.040(2) 0.031(3) -0.0037(19) 0.016(2) -0.007(2) C35 0.032(2) 0.026(2) 0.033(3) -0.0009(18) 0.0055(19) -0.0059(17) C40 0.0172(19) 0.028(2) 0.025(2) -0.0036(17) -0.0088(17) 0.0011(16) C41 0.035(2) 0.026(2) 0.035(3) 0.0023(18) 0.0011(18) 0.0047(18) C42 0.055(3) 0.028(2) 0.046(3) 0.000(2) 0.003(2) 0.011(2) C43 0.042(3) 0.041(2) 0.044(3) -0.013(2) 0.002(2) 0.016(2) C44 0.034(2) 0.048(3) 0.032(3) -0.006(2) 0.0051(19) 0.009(2) C45 0.030(2) 0.028(2) 0.034(3) -0.0001(18) 0.0055(19) 0.0017(17) N50 0.0235(16) 0.0215(15) 0.0216(18) -0.0012(13) 0.0071(13) -0.0031(13) C51 0.029(2) 0.028(2) 0.042(3) -0.0076(18) -0.0006(19) -0.0111(17) O1 0.0449(17) 0.0462(17) 0.033(2) -0.0030(14) 0.0133(14) 0.0013(13) O2 0.0385(17) 0.0380(16) 0.0529(19) -0.0019(14) -0.0105(14) 0.0094(14) O3 0.056(2) 0.0432(19) 0.119(3) 0.0158(18) -0.0298(19) -0.0239(16) O4 0.0540(19) 0.061(2) 0.037(2) -0.0052(16) -0.0066(16) 0.0120(15) S1A 0.0215(5) 0.0273(5) 0.0363(6) 0.0048(4) 0.0007(4) -0.0028(4) S2A 0.0320(5) 0.0195(5) 0.0378(7) -0.0043(4) -0.0051(5) 0.0003(4) Fe1 0.0201(3) 0.0173(3) 0.0252(3) -0.0011(2) 0.0004(2) -0.0009(2) Fe2 0.0251(3) 0.0244(3) 0.0359(4) 0.0014(2) -0.0059(2) -0.0031(2) P1 0.0223(5) 0.0185(5) 0.0202(6) -0.0013(4) 0.0020(4) 0.0002(4) P2 0.0196(5) 0.0190(5) 0.0264(7) -0.0004(4) 0.0009(4) -0.0016(4) C5B 0.033(2) 0.032(2) 0.043(3) 0.0116(18) -0.0015(19) -0.0088(18) C7B 0.067(3) 0.0140(19) 0.051(3) 0.0015(18) -0.014(2) 0.0004(19) S1B 0.0215(5) 0.0273(5) 0.0363(6) 0.0048(4) 0.0007(4) -0.0028(4) S2B 0.0320(5) 0.0195(5) 0.0378(7) -0.0043(4) -0.0051(5) 0.0003(4) B1 0.040(3) 0.050(3) 0.022(3) 0.002(2) 0.017(2) -0.003(2) F1 0.0631(17) 0.0730(17) 0.0639(18) 0.0350(14) 0.0134(14) 0.0199(14) F2 0.095(2) 0.0793(19) 0.0670(19) -0.0307(16) 0.0262(16) -0.0264(16) F3 0.0338(14) 0.0791(18) 0.0602(17) 0.0099(13) 0.0113(12) -0.0028(12) C70 0.055(3) 0.029(2) 0.028(3) -0.0096(19) 0.002(2) -0.0040(19) C71 0.054(3) 0.053(3) 0.054(3) -0.011(2) -0.011(2) 0.006(2) C72 0.062(3) 0.064(3) 0.043(3) -0.012(2) 0.013(2) 0.001(2) O70 0.063(2) 0.0550(19) 0.029(2) -0.0003(14) -0.0007(16) -0.0091(15) C80 0.062(3) 0.032(2) 0.049(3) 0.004(2) 0.011(3) 0.000(2) C81 0.082(3) 0.069(4) 0.075(4) 0.005(3) -0.017(3) 0.006(3) C82 0.103(4) 0.130(5) 0.065(4) -0.021(4) 0.038(3) 0.006(4) O80 0.068(2) 0.0458(18) 0.046(2) -0.0081(16) 0.0132(17) -0.0019(15) 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' P P 0.1023 0.0942 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.01 -4 0 -1 0.03 7 0 1 0.02 0 1 -1 0.05 0 -1 1 0.055 0 -1 -1 0.055 0 1 1 0.055 -1 0 0 0.01 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 O1 C1 Fe1 176.8(3) . . ? O2 C2 Fe2 178.5(3) . . ? O3 C3 Fe2 176.9(4) . . ? O4 C4 Fe2 179.1(4) . . ? C6A C5A S1A 116.9(3) . . ? C6A C5A H5A 108.1 . . ? S1A C5A H5A 108.1 . . ? C6A C5A H5B 108.1 . . ? S1A C5A H5B 108.1 . . ? H5A C5A H5B 107.3 . . ? C5A C6A C7A 114.6(4) . . ? C5A C6A H6A 108.6 . . ? C7A C6A H6A 108.6 . . ? C5A C6A H6B 108.6 . . ? C7A C6A H6B 108.6 . . ? H6A C6A H6B 107.6 . . ? C6A C7A S2A 118.5(3) . . ? C6A C7A H7A 107.7 . . ? S2A C7A H7A 107.7 . . ? C6A C7A H7B 107.7 . . ? S2A C7A H7B 107.7 . . ? H7A C7A H7B 107.1 . . ? N50 C8 P1 119.8(2) . . ? N50 C8 H8A 107.4 . . ? P1 C8 H8A 107.4 . . ? N50 C8 H8B 107.4 . . ? P1 C8 H8B 107.4 . . ? H8A C8 H8B 106.9 . . ? N50 C9 P2 113.9(2) . . ? N50 C9 H9A 108.8 . . ? P2 C9 H9A 108.8 . . ? N50 C9 H9B 108.8 . . ? P2 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C15 C10 C11 117.9(3) . . ? C15 C10 P1 121.0(2) . . ? C11 C10 P1 121.0(3) . . ? C12 C11 C10 120.5(3) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C13 C12 C11 120.5(3) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 120.0(3) . . ? C12 C13 H13 120 . . ? C14 C13 H13 120 . . ? C13 C14 C15 119.7(3) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C14 C15 C10 121.5(3) . . ? C14 C15 H15 119.3 . . ? C10 C15 H15 119.3 . . ? C21 C20 C25 117.7(3) . . ? C21 C20 P1 123.5(3) . . ? C25 C20 P1 118.8(3) . . ? C22 C21 C20 120.7(4) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C23 C22 C21 120.8(4) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C24 C23 C22 119.4(4) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C25 120.2(4) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C24 C25 C20 121.2(3) . . ? C24 C25 H25 119.4 . . ? C20 C25 H25 119.4 . . ? C35 C30 C31 118.4(3) . . ? C35 C30 P2 119.2(3) . . ? C31 C30 P2 122.3(3) . . ? C32 C31 C30 119.9(3) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C33 C32 C31 120.5(4) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C34 C33 C32 120.5(4) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 119.8(4) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C34 C35 C30 120.9(4) . . ? C34 C35 H35 119.5 . . ? C30 C35 H35 119.5 . . ? C41 C40 C45 118.0(3) . . ? C41 C40 P2 121.7(3) . . ? C45 C40 P2 119.8(3) . . ? C42 C41 C40 120.6(4) . . ? C42 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? C43 C42 C41 121.1(4) . . ? C43 C42 H42 119.4 . . ? C41 C42 H42 119.4 . . ? C42 C43 C44 119.1(4) . . ? C42 C43 H43 120.4 . . ? C44 C43 H43 120.4 . . ? C45 C44 C43 120.4(4) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C44 C45 C40 120.7(3) . . ? C44 C45 H45 119.7 . . ? C40 C45 H45 119.7 . . ? C9 N50 C51 109.4(2) . . ? C9 N50 C8 113.1(2) . . ? C51 N50 C8 109.2(2) . . ? C9 N50 H50 108.4 . . ? C51 N50 H50 108.4 . . ? C8 N50 H50 108.4 . . ? C5A S1A Fe1 116.31(12) . . ? C5A S1A Fe2 110.04(13) . . ? Fe1 S1A Fe2 69.18(3) . . ? C7A S2A Fe1 114.14(12) . . ? C7A S2A Fe2 109.07(14) . . ? Fe1 S2A Fe2 69.16(3) . . ? C1 Fe1 P2 93.59(12) . . ? C1 Fe1 P1 90.03(11) . . ? P2 Fe1 P1 94.05(4) . . ? C1 Fe1 S1A 152.83(12) . . ? P2 Fe1 S1A 113.14(4) . . ? P1 Fe1 S1A 92.75(4) . . ? C1 Fe1 S2A 87.22(11) . . ? P2 Fe1 S2A 99.31(4) . . ? P1 Fe1 S2A 166.49(4) . . ? S1A Fe1 S2A 83.81(4) . . ? C1 Fe1 Fe2 98.64(11) . . ? P2 Fe1 Fe2 150.94(3) . . ? P1 Fe1 Fe2 112.10(3) . . ? S1A Fe1 Fe2 55.45(3) . . ? S2A Fe1 Fe2 55.42(3) . . ? C4 Fe2 C2 92.19(16) . . ? C4 Fe2 C3 100.11(18) . . ? C2 Fe2 C3 96.95(16) . . ? C4 Fe2 S2A 87.40(12) . . ? C2 Fe2 S2A 162.34(11) . . ? C3 Fe2 S2A 100.50(12) . . ? C4 Fe2 S1A 152.64(12) . . ? C2 Fe2 S1A 88.64(12) . . ? C3 Fe2 S1A 106.93(14) . . ? S2A Fe2 S1A 83.75(4) . . ? C4 Fe2 Fe1 98.61(12) . . ? C2 Fe2 Fe1 107.32(11) . . ? C3 Fe2 Fe1 148.58(12) . . ? S2A Fe2 Fe1 55.41(3) . . ? S1A Fe2 Fe1 55.37(3) . . ? C20 P1 C10 100.04(15) . . ? C20 P1 C8 102.81(15) . . ? C10 P1 C8 95.45(14) . . ? C20 P1 Fe1 119.34(11) . . ? C10 P1 Fe1 119.21(11) . . ? C8 P1 Fe1 116.02(11) . . ? C30 P2 C40 106.82(16) . . ? C30 P2 C9 99.18(15) . . ? C40 P2 C9 98.14(14) . . ? C30 P2 Fe1 121.18(11) . . ? C40 P2 Fe1 113.09(11) . . ? C9 P2 Fe1 115.27(11) . . ? H6C C6B H6D 107.2 . . ? F1 B1 F3 110.7(4) . . ? F1 B1 F2 109.9(4) . . ? F3 B1 F2 108.9(4) . . ? F1 B1 F4 109.9(3) . . ? F3 B1 F4 109.8(4) . . ? F2 B1 F4 107.5(3) . . ? O70 C70 C71 121.5(4) . . ? O70 C70 C72 121.3(4) . . ? C71 C70 C72 117.2(4) . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C70 C72 H72A 109.5 . . ? C70 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C70 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? O80 C80 C81 122.2(4) . . ? O80 C80 C82 121.8(4) . . ? C81 C80 C82 116.0(4) . . ? C80 C81 H81A 109.5 . . ? C80 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C80 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C80 C82 H82A 109.5 . . ? C80 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C80 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 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 C1 O1 1.156(4) . ? C1 Fe1 1.748(5) . ? C2 O2 1.143(4) . ? C2 Fe2 1.784(4) . ? C3 O3 1.148(4) . ? C3 Fe2 1.796(4) . ? C4 O4 1.157(4) . ? C4 Fe2 1.765(5) . ? C5A C6A 1.465(5) . ? C5A S1A 1.833(3) . ? C5A H5A 0.99 . ? C5A H5B 0.99 . ? C6A C7A 1.506(6) . ? C6A H6A 0.99 . ? C6A H6B 0.99 . ? C7A S2A 1.846(4) . ? C7A H7A 0.99 . ? C7A H7B 0.99 . ? C8 N50 1.510(4) . ? C8 P1 1.867(3) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 N50 1.500(4) . ? C9 P2 1.852(3) . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? C10 C15 1.381(4) . ? C10 C11 1.395(4) . ? C10 P1 1.847(3) . ? C11 C12 1.378(5) . ? C11 H11 0.95 . ? C12 C13 1.366(5) . ? C12 H12 0.95 . ? C13 C14 1.375(4) . ? C13 H13 0.95 . ? C14 C15 1.377(4) . ? C14 H14 0.95 . ? C15 H15 0.95 . ? C20 C21 1.381(5) . ? C20 C25 1.397(4) . ? C20 P1 1.814(3) . ? C21 C22 1.380(5) . ? C21 H21 0.95 . ? C22 C23 1.372(5) . ? C22 H22 0.95 . ? C23 C24 1.369(5) . ? C23 H23 0.95 . ? C24 C25 1.376(5) . ? C24 H24 0.95 . ? C25 H25 0.95 . ? C30 C35 1.391(5) . ? C30 C31 1.402(5) . ? C30 P2 1.828(4) . ? C31 C32 1.381(5) . ? C31 H31 0.95 . ? C32 C33 1.376(5) . ? C32 H32 0.95 . ? C33 C34 1.367(5) . ? C33 H33 0.95 . ? C34 C35 1.383(5) . ? C34 H34 0.95 . ? C35 H35 0.95 . ? C40 C41 1.389(5) . ? C40 C45 1.398(5) . ? C40 P2 1.831(3) . ? C41 C42 1.380(5) . ? C41 H41 0.95 . ? C42 C43 1.367(5) . ? C42 H42 0.95 . ? C43 C44 1.385(5) . ? C43 H43 0.95 . ? C44 C45 1.380(5) . ? C44 H44 0.95 . ? C45 H45 0.95 . ? N50 C51 1.502(4) . ? N50 H50 0.93 . ? C51 H51A 0.98 . ? C51 H51B 0.98 . ? C51 H51C 0.98 . ? S1A Fe1 2.2611(10) . ? S1A Fe2 2.2634(11) . ? S2A Fe1 2.2627(10) . ? S2A Fe2 2.2629(10) . ? Fe1 P2 2.1812(10) . ? Fe1 P1 2.2101(9) . ? Fe1 Fe2 2.5687(7) . ? C6B H6C 0.99 . ? C6B H6D 0.99 . ? B1 F1 1.360(5) . ? B1 F3 1.370(5) . ? B1 F2 1.383(5) . ? B1 F4 1.393(5) . ? C70 O70 1.215(4) . ? C70 C71 1.484(5) . ? C70 C72 1.490(5) . ? C71 H71A 0.98 . ? C71 H71B 0.98 . ? C71 H71C 0.98 . ? C72 H72A 0.98 . ? C72 H72B 0.98 . ? C72 H72C 0.98 . ? C80 O80 1.205(5) . ? C80 C81 1.481(6) . ? C80 C82 1.489(6) . ? C81 H81A 0.98 . ? C81 H81B 0.98 . ? C81 H81C 0.98 . ? C82 H82A 0.98 . ? C82 H82B 0.98 . ? C82 H82C 0.98 . ? 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 N50 H50 O70 0.93 2.04 2.842(4) 142.7 .