Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name _publ_author_address _publ_author_footnote 'C. E. Housecroft' ; ? # Address for author 1 ; ; ? # Footnote for author 1 ; 'Jonathon E. Beves' ; ? # Address 2 ; ; ? # Footnote 2 ; 'Edwin C. Constable' '' '' 'Cameron Kepert' '' '' 'Markus Neuburger' '' '' 'David J. Price' '' '' 'Silvia Schaffner' '' '' _publ_contact_author_name 'C. E. Housecroft' _publ_contact_author_address ; Departement Chemie University of Basel Spitalstrasse 51 Basel CH-4056 SWITZERLAND ; _publ_contact_author_email CATHERINE.HOUSECROFT@UNIBAS.CH _publ_requested_journal CrystEngComm _publ_section_title ; The conjugate acid of bis{4'-(4-pyridyl)-2,2':6',2"-terpyridine}iron(II) as a self-complementary hydrogen-bonded building block ; _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ? _journal_date_accepted ? _journal_date_from_coeditor ? _journal_date_printers_final ? _journal_date_printers_first ? _journal_date_proofs_in ? _journal_date_proofs_out ? # PROCESSING SUMMARY (IUCr Office Use Only): _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_issue ? _journal_name_full ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_volume ? _journal_year ? _publ_contact_author_fax '+44 1865 000000' _publ_contact_author_phone '+44 1865 000000' # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # The content below is held in the file 'script/refcif.dat'. This is a text # file which you may edit to reflect local conditions. # Items which need looking at are represented by a '?'. # Items for which there are choices are prefixed with 'choose from'. _publ_contact_letter ; Please consider this CIF submission for publication as a Short Format Paper in Acta Crystallographica E. The figures will be sent by e-mail. ; _publ_requested_category EO # choose from: FI FM FO CI CM CO AD _publ_requested_coeditor_name 'Prof William Clegg' data_jb34abs _database_code_depnum_ccdc_archive 'CCDC 653282' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Fe(tpypy)(tpypyH)](ClO4)3.EtOH' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H35 Cl3 Fe N8 O13' _chemical_formula_weight 1021.98 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.367(11) _cell_length_b 16.290(13) _cell_length_c 18.720(15) _cell_angle_alpha 90.00 _cell_angle_beta 105.060(14) _cell_angle_gamma 90.00 _cell_volume 4231(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 817 _cell_measurement_theta_min 2.577 _cell_measurement_theta_max 22.6135 _exptl_crystal_description plate _exptl_crystal_colour 'dark red/purple' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.008 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 0.625 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.859 _exptl_absorpt_correction_T_max 0.995 _exptl_absorpt_process_details 'SADABS, Bruker 1995' _exptl_special_details ; In a thin film of Paratone N oil on a mohair fibre ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 66 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 41745 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.1364 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 28.25 _reflns_number_total 10085 _reflns_number_gt 5425 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS, 1997)' _computing_cell_refinement 'SMART (BrukerAXS, 1997)' _computing_data_reduction 'SAINT+ (BrukerAXS, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10085 _refine_ls_number_parameters 612 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1488 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.1390 _refine_ls_wR_factor_gt 0.1120 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Fe1 Fe 0.33972(4) 0.11514(3) 0.21561(3) 0.01256(14) Uani 1 1 d . . . Cl1 Cl 0.21747(7) 0.60603(6) 0.19041(5) 0.0186(2) Uani 1 1 d . . . Cl2 Cl 0.20016(7) 0.62612(6) 0.48700(5) 0.0195(2) Uani 1 1 d . . . Cl3 Cl 0.34001(7) 0.18838(6) 0.49777(5) 0.0194(2) Uani 1 1 d . . . O1 O 0.1925(2) 0.54784(18) 0.23987(16) 0.0288(7) Uani 1 1 d . . . O2 O 0.2926(2) 0.57259(19) 0.16237(16) 0.0319(8) Uani 1 1 d . . . O3 O 0.2502(2) 0.68065(17) 0.22999(16) 0.0327(8) Uani 1 1 d . . . O4 O 0.13315(19) 0.62377(17) 0.13059(14) 0.0259(7) Uani 1 1 d . . . O5 O 0.1384(2) 0.6954(2) 0.46300(19) 0.0424(9) Uani 1 1 d . . . O6 O 0.29094(19) 0.65225(18) 0.53483(15) 0.0261(7) Uani 1 1 d . . . O7 O 0.15359(18) 0.57074(17) 0.52638(15) 0.0230(7) Uani 1 1 d . . . O8 O 0.2184(2) 0.5857(2) 0.42408(16) 0.0428(9) Uani 1 1 d . . . O9 O 0.3367(2) 0.24628(17) 0.43892(14) 0.0258(7) Uani 1 1 d . . . O10 O 0.40677(19) 0.21740(17) 0.56524(14) 0.0247(7) Uani 1 1 d . . . O11 O 0.3728(2) 0.10981(17) 0.47813(15) 0.0263(7) Uani 1 1 d . . . O12 O 0.24574(19) 0.17910(19) 0.50939(15) 0.0304(7) Uani 1 1 d . . . O13 O 0.0166(2) 0.4763(2) 0.10428(17) 0.0367(8) Uani 1 1 d D . . N1 N 0.3507(2) 0.23519(19) 0.22910(16) 0.0135(7) Uani 1 1 d . . . N2 N 0.4302(2) 0.11935(19) 0.30916(15) 0.0120(7) Uani 1 1 d . . . N3 N 0.3567(2) -0.0031(2) 0.23507(16) 0.0143(7) Uani 1 1 d . . . N4 N 0.8083(2) 0.1381(2) 0.63172(18) 0.0197(8) Uani 1 1 d D . . N5 N 0.4340(2) 0.10943(19) 0.15524(16) 0.0121(7) Uani 1 1 d . . . N6 N 0.2531(2) 0.11163(18) 0.12035(16) 0.0127(7) Uani 1 1 d . . . N7 N 0.2167(2) 0.11877(19) 0.24363(16) 0.0138(7) Uani 1 1 d . . . N8 N -0.0573(2) 0.1353(2) -0.23840(18) 0.0212(8) Uani 1 1 d . . . C1 C 0.2993(3) 0.2937(2) 0.1845(2) 0.0187(9) Uani 1 1 d . . . H1 H 0.2561 0.2777 0.1390 0.022 Uiso 1 1 calc R . . C2 C 0.3077(3) 0.3753(3) 0.2028(2) 0.0255(10) Uani 1 1 d . . . H2 H 0.2709 0.4149 0.1700 0.031 Uiso 1 1 calc R . . C3 C 0.3691(3) 0.4002(3) 0.2684(2) 0.0253(10) Uani 1 1 d . . . H3 H 0.3747 0.4567 0.2815 0.030 Uiso 1 1 calc R . . C4 C 0.4228(3) 0.3415(2) 0.3150(2) 0.0192(9) Uani 1 1 d . . . H4 H 0.4658 0.3572 0.3607 0.023 Uiso 1 1 calc R . . C5 C 0.4131(3) 0.2601(2) 0.2943(2) 0.0138(8) Uani 1 1 d . . . C6 C 0.4638(3) 0.1920(2) 0.3387(2) 0.0128(8) Uani 1 1 d . . . C7 C 0.5384(3) 0.1972(2) 0.40280(19) 0.0151(9) Uani 1 1 d . . . H7 H 0.5626 0.2491 0.4223 0.018 Uiso 1 1 calc R . . C8 C 0.5768(2) 0.1249(2) 0.43784(19) 0.0139(8) Uani 1 1 d . . . C9 C 0.6572(3) 0.1291(2) 0.5066(2) 0.0155(9) Uani 1 1 d . . . C10 C 0.6645(3) 0.1934(2) 0.5560(2) 0.0175(9) Uani 1 1 d . . . H10 H 0.6169 0.2353 0.5473 0.021 Uiso 1 1 calc R . . C11 C 0.7413(3) 0.1965(3) 0.6180(2) 0.0188(9) Uani 1 1 d . . . H11 H 0.7465 0.2411 0.6515 0.023 Uiso 1 1 calc R . . C12 C 0.8027(3) 0.0751(3) 0.5858(2) 0.0233(10) Uani 1 1 d . . . H12 H 0.8506 0.0334 0.5968 0.028 Uiso 1 1 calc R . . C13 C 0.7281(3) 0.0694(3) 0.5219(2) 0.0210(9) Uani 1 1 d . . . H13 H 0.7256 0.0247 0.4888 0.025 Uiso 1 1 calc R . . C14 C 0.5402(3) 0.0499(2) 0.4079(2) 0.0152(9) Uani 1 1 d . . . H14 H 0.5649 0.0000 0.4317 0.018 Uiso 1 1 calc R . . C15 C 0.4668(3) 0.0489(2) 0.3427(2) 0.0134(8) Uani 1 1 d . . . C16 C 0.4227(3) -0.0231(2) 0.30037(19) 0.0126(8) Uani 1 1 d . . . C17 C 0.4451(3) -0.1035(2) 0.3214(2) 0.0167(9) Uani 1 1 d . . . H17 H 0.4903 -0.1158 0.3670 0.020 Uiso 1 1 calc R . . C18 C 0.4004(3) -0.1656(2) 0.2747(2) 0.0196(9) Uani 1 1 d . . . H18 H 0.4147 -0.2214 0.2879 0.024 Uiso 1 1 calc R . . C19 C 0.3347(3) -0.1461(3) 0.2086(2) 0.0213(9) Uani 1 1 d . . . H19 H 0.3039 -0.1883 0.1759 0.026 Uiso 1 1 calc R . . C20 C 0.3144(3) -0.0648(2) 0.1906(2) 0.0149(9) Uani 1 1 d . . . H20 H 0.2690 -0.0519 0.1453 0.018 Uiso 1 1 calc R . . C21 C 0.5305(3) 0.1101(2) 0.1783(2) 0.0154(8) Uani 1 1 d . . . H21 H 0.5598 0.1159 0.2298 0.018 Uiso 1 1 calc R . . C22 C 0.5896(3) 0.1026(2) 0.1310(2) 0.0167(9) Uani 1 1 d . . . H22 H 0.6577 0.1033 0.1494 0.020 Uiso 1 1 calc R . . C23 C 0.5468(3) 0.0939(2) 0.0558(2) 0.0178(9) Uani 1 1 d . . . H23 H 0.5856 0.0882 0.0220 0.021 Uiso 1 1 calc R . . C24 C 0.4484(3) 0.0937(2) 0.0307(2) 0.0168(9) Uani 1 1 d . . . H24 H 0.4184 0.0876 -0.0206 0.020 Uiso 1 1 calc R . . C25 C 0.3930(3) 0.1023(2) 0.08078(19) 0.0121(8) Uani 1 1 d . . . C26 C 0.2875(3) 0.1065(2) 0.0601(2) 0.0135(8) Uani 1 1 d . . . C27 C 0.2264(3) 0.1084(2) -0.01036(19) 0.0151(8) Uani 1 1 d . . . H27 H 0.2517 0.1043 -0.0523 0.018 Uiso 1 1 calc R . . C28 C 0.1275(3) 0.1163(2) -0.0194(2) 0.0162(8) Uani 1 1 d . . . C29 C 0.0622(3) 0.1214(2) -0.09510(19) 0.0153(8) Uani 1 1 d . . . C30 C 0.0811(3) 0.0773(3) -0.1538(2) 0.0211(9) Uani 1 1 d . . . H30 H 0.1350 0.0414 -0.1457 0.025 Uiso 1 1 calc R . . C31 C 0.0199(3) 0.0866(3) -0.2240(2) 0.0242(10) Uani 1 1 d . . . H31 H 0.0336 0.0569 -0.2637 0.029 Uiso 1 1 calc R . . C32 C -0.0758(3) 0.1780(3) -0.1821(2) 0.0214(9) Uani 1 1 d . . . H32 H -0.1303 0.2132 -0.1919 0.026 Uiso 1 1 calc R . . C33 C -0.0181(3) 0.1724(2) -0.1101(2) 0.0176(9) Uani 1 1 d . . . H33 H -0.0335 0.2031 -0.0715 0.021 Uiso 1 1 calc R . . C34 C 0.0926(3) 0.1207(2) 0.0433(2) 0.0171(9) Uani 1 1 d . . . H34 H 0.0254 0.1256 0.0385 0.020 Uiso 1 1 calc R . . C35 C 0.1572(3) 0.1177(2) 0.1130(2) 0.0160(8) Uani 1 1 d . . . C36 C 0.1353(3) 0.1226(2) 0.1853(2) 0.0152(8) Uani 1 1 d . . . C37 C 0.0450(3) 0.1310(2) 0.1962(2) 0.0216(10) Uani 1 1 d . . . H37 H -0.0099 0.1337 0.1550 0.026 Uiso 1 1 calc R . . C38 C 0.0344(3) 0.1357(3) 0.2675(2) 0.0249(10) Uani 1 1 d . . . H38 H -0.0277 0.1416 0.2759 0.030 Uiso 1 1 calc R . . C39 C 0.1156(3) 0.1317(3) 0.3262(2) 0.0244(10) Uani 1 1 d . . . H39 H 0.1101 0.1350 0.3756 0.029 Uiso 1 1 calc R . . C40 C 0.2046(3) 0.1227(2) 0.3123(2) 0.0199(9) Uani 1 1 d . . . H40 H 0.2599 0.1190 0.3531 0.024 Uiso 1 1 calc R . . C41 C 0.0652(4) 0.4233(3) 0.0673(3) 0.0479(14) Uani 1 1 d . . . H41A H 0.1346 0.4233 0.0935 0.057 Uiso 1 1 calc R . . H41B H 0.0589 0.4446 0.0167 0.057 Uiso 1 1 calc R . . C42 C 0.0300(4) 0.3404(4) 0.0623(4) 0.073(2) Uani 1 1 d . . . H42A H 0.0669 0.3066 0.0361 0.110 Uiso 1 1 calc R . . H42B H -0.0383 0.3397 0.0353 0.110 Uiso 1 1 calc R . . H42C H 0.0373 0.3184 0.1122 0.110 Uiso 1 1 calc R . . H13A H 0.044(3) 0.5253(17) 0.107(3) 0.051(17) Uiso 1 1 d D . . H4A H 0.855(3) 0.139(3) 0.6766(16) 0.050(15) Uiso 1 1 d D . . 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 0.0092(3) 0.0197(3) 0.0065(3) -0.0001(2) -0.0021(2) 0.0003(2) Cl1 0.0145(5) 0.0228(6) 0.0160(5) -0.0008(4) -0.0003(4) 0.0003(4) Cl2 0.0126(5) 0.0308(6) 0.0132(5) 0.0013(4) -0.0001(4) -0.0015(4) Cl3 0.0185(5) 0.0260(6) 0.0122(5) 0.0012(4) 0.0013(4) 0.0015(4) O1 0.0248(17) 0.0325(19) 0.0283(17) 0.0088(14) 0.0058(14) -0.0031(14) O2 0.0221(17) 0.044(2) 0.0317(18) 0.0020(15) 0.0115(14) 0.0077(14) O3 0.0326(19) 0.0210(17) 0.0325(18) -0.0048(14) -0.0132(15) 0.0001(14) O4 0.0173(15) 0.0368(19) 0.0161(15) 0.0036(13) -0.0091(12) 0.0008(14) O5 0.0209(18) 0.039(2) 0.065(2) 0.0291(18) 0.0070(16) 0.0105(15) O6 0.0149(15) 0.0420(19) 0.0165(15) -0.0002(13) -0.0047(12) -0.0061(13) O7 0.0172(16) 0.0283(17) 0.0234(16) 0.0063(13) 0.0050(13) -0.0021(13) O8 0.036(2) 0.073(3) 0.0239(17) -0.0224(17) 0.0158(15) -0.0192(18) O9 0.0364(18) 0.0261(17) 0.0144(15) 0.0068(13) 0.0055(13) 0.0078(14) O10 0.0251(17) 0.0300(18) 0.0121(14) 0.0004(13) -0.0073(12) -0.0025(13) O11 0.0345(18) 0.0197(16) 0.0234(16) -0.0021(13) 0.0049(13) 0.0052(14) O12 0.0210(17) 0.052(2) 0.0187(16) -0.0011(15) 0.0060(13) -0.0021(15) O13 0.035(2) 0.042(2) 0.0306(19) -0.0058(17) 0.0027(16) -0.0141(18) N1 0.0078(17) 0.0250(19) 0.0059(16) -0.0009(14) -0.0013(13) -0.0005(14) N2 0.0112(16) 0.0174(18) 0.0058(15) -0.0004(14) -0.0007(12) -0.0005(14) N3 0.0093(17) 0.0231(19) 0.0083(16) -0.0009(14) -0.0015(13) -0.0037(14) N4 0.0140(19) 0.030(2) 0.0100(17) 0.0008(15) -0.0065(14) -0.0008(16) N5 0.0084(16) 0.0151(18) 0.0108(16) -0.0018(14) -0.0008(12) -0.0006(13) N6 0.0112(16) 0.0152(18) 0.0100(15) 0.0004(14) -0.0003(13) -0.0004(14) N7 0.0121(16) 0.0191(18) 0.0072(15) 0.0008(14) -0.0028(13) 0.0021(14) N8 0.0179(19) 0.027(2) 0.0147(17) 0.0004(15) -0.0027(15) 0.0024(16) C1 0.015(2) 0.025(2) 0.012(2) 0.0008(17) -0.0047(17) 0.0034(18) C2 0.026(2) 0.020(2) 0.023(2) 0.0020(19) -0.0082(18) 0.0124(19) C3 0.031(3) 0.018(2) 0.024(2) -0.0014(18) 0.001(2) 0.0055(19) C4 0.021(2) 0.024(2) 0.009(2) -0.0007(17) -0.0011(17) 0.0020(19) C5 0.012(2) 0.019(2) 0.0097(19) -0.0021(16) 0.0011(16) -0.0020(17) C6 0.0088(19) 0.017(2) 0.0116(19) -0.0012(16) -0.0003(16) -0.0027(16) C7 0.015(2) 0.021(2) 0.0081(19) -0.0013(17) 0.0004(16) -0.0012(17) C8 0.0067(18) 0.024(2) 0.0088(18) 0.0018(17) -0.0018(15) 0.0034(17) C9 0.013(2) 0.024(2) 0.0097(19) 0.0014(17) 0.0020(16) -0.0023(18) C10 0.014(2) 0.025(2) 0.011(2) 0.0016(17) -0.0007(16) 0.0023(18) C11 0.019(2) 0.024(2) 0.012(2) -0.0023(17) -0.0003(17) -0.0028(19) C12 0.018(2) 0.026(3) 0.020(2) 0.0000(19) -0.0032(18) 0.0051(19) C13 0.017(2) 0.028(3) 0.013(2) -0.0038(18) -0.0059(17) 0.0015(19) C14 0.012(2) 0.023(2) 0.0087(19) 0.0009(17) 0.0003(16) 0.0037(17) C15 0.012(2) 0.016(2) 0.0107(19) 0.0011(16) 0.0009(16) 0.0003(17) C16 0.0082(19) 0.020(2) 0.0085(19) 0.0019(16) 0.0004(15) -0.0010(16) C17 0.017(2) 0.022(2) 0.0087(19) 0.0004(17) -0.0006(16) -0.0004(18) C18 0.022(2) 0.017(2) 0.019(2) 0.0033(18) 0.0039(18) 0.0007(18) C19 0.023(2) 0.023(2) 0.018(2) -0.0059(18) 0.0045(19) -0.0052(19) C20 0.014(2) 0.023(2) 0.0068(18) -0.0006(17) -0.0002(16) -0.0022(17) C21 0.013(2) 0.018(2) 0.0109(19) 0.0046(17) -0.0026(15) -0.0005(17) C22 0.012(2) 0.019(2) 0.018(2) 0.0009(17) 0.0007(16) 0.0002(17) C23 0.016(2) 0.020(2) 0.019(2) -0.0017(17) 0.0072(17) 0.0034(17) C24 0.014(2) 0.024(2) 0.0094(19) -0.0013(16) -0.0024(16) 0.0000(17) C25 0.0110(19) 0.013(2) 0.0098(18) -0.0005(15) -0.0015(15) -0.0012(16) C26 0.013(2) 0.014(2) 0.0129(19) -0.0017(16) 0.0023(16) -0.0014(16) C27 0.017(2) 0.020(2) 0.0073(18) -0.0021(16) 0.0005(15) 0.0004(18) C28 0.016(2) 0.018(2) 0.0124(19) 0.0005(17) 0.0000(16) -0.0041(18) C29 0.012(2) 0.023(2) 0.0085(18) 0.0016(17) -0.0016(15) -0.0013(18) C30 0.015(2) 0.024(2) 0.019(2) 0.0010(18) -0.0054(18) 0.0040(18) C31 0.025(2) 0.030(3) 0.014(2) -0.0059(18) -0.0002(19) 0.002(2) C32 0.013(2) 0.028(3) 0.019(2) 0.0057(19) -0.0033(17) 0.0001(18) C33 0.016(2) 0.025(2) 0.011(2) -0.0016(17) 0.0007(17) -0.0006(18) C34 0.0109(19) 0.022(2) 0.016(2) 0.0006(18) 0.0003(16) 0.0018(17) C35 0.0122(19) 0.023(2) 0.0118(19) -0.0004(18) 0.0010(15) 0.0001(18) C36 0.013(2) 0.019(2) 0.0110(19) 0.0023(17) -0.0021(15) 0.0014(17) C37 0.014(2) 0.033(3) 0.016(2) 0.0025(19) -0.0005(17) 0.0022(19) C38 0.013(2) 0.041(3) 0.022(2) 0.000(2) 0.0064(18) 0.0001(19) C39 0.021(2) 0.041(3) 0.012(2) -0.0002(19) 0.0051(18) 0.000(2) C40 0.020(2) 0.030(2) 0.0070(18) 0.0006(18) -0.0010(16) -0.0043(19) C41 0.039(3) 0.049(4) 0.053(4) 0.007(3) 0.005(3) 0.014(3) C42 0.057(4) 0.057(4) 0.118(6) -0.040(4) 0.044(4) -0.025(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N2 1.892(3) . ? Fe1 N6 1.892(3) . ? Fe1 N3 1.964(4) . ? Fe1 N7 1.971(3) . ? Fe1 N1 1.973(4) . ? Fe1 N5 1.979(3) . ? Cl1 O2 1.425(3) . ? Cl1 O1 1.434(3) . ? Cl1 O3 1.437(3) . ? Cl1 O4 1.449(3) . ? Cl2 O8 1.432(3) . ? Cl2 O5 1.433(3) . ? Cl2 O7 1.436(3) . ? Cl2 O6 1.441(3) . ? Cl3 O12 1.435(3) . ? Cl3 O9 1.442(3) . ? Cl3 O11 1.444(3) . ? Cl3 O10 1.452(3) . ? O13 C41 1.402(6) . ? O13 H13A 0.884(19) . ? N1 C1 1.353(5) . ? N1 C5 1.374(5) . ? N2 C6 1.342(5) . ? N2 C15 1.348(5) . ? N3 C20 1.345(5) . ? N3 C16 1.377(5) . ? N4 C12 1.328(5) . ? N4 C11 1.330(5) . ? N4 H4A 0.927(19) . ? N5 C21 1.341(4) . ? N5 C25 1.370(4) . ? N6 C26 1.346(4) . ? N6 C35 1.351(5) . ? N7 C40 1.343(4) . ? N7 C36 1.379(5) . ? N8 C31 1.333(5) . ? N8 C32 1.345(5) . ? C1 C2 1.371(6) . ? C1 H1 0.9500 . ? C2 C3 1.373(6) . ? C2 H2 0.9500 . ? C3 C4 1.387(5) . ? C3 H3 0.9500 . ? C4 C5 1.378(5) . ? C4 H4 0.9500 . ? C5 C6 1.463(5) . ? C6 C7 1.388(5) . ? C7 C8 1.390(5) . ? C7 H7 0.9500 . ? C8 C14 1.390(5) . ? C8 C9 1.490(5) . ? C9 C10 1.383(5) . ? C9 C13 1.384(5) . ? C10 C11 1.379(5) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.387(5) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.390(5) . ? C14 H14 0.9500 . ? C15 C16 1.465(5) . ? C16 C17 1.381(5) . ? C17 C18 1.380(5) . ? C17 H17 0.9500 . ? C18 C19 1.385(5) . ? C18 H18 0.9500 . ? C19 C20 1.378(5) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.383(5) . ? C21 H21 0.9500 . ? C22 C23 1.388(5) . ? C22 H22 0.9500 . ? C23 C24 1.370(5) . ? C23 H23 0.9500 . ? C24 C25 1.385(5) . ? C24 H24 0.9500 . ? C25 C26 1.466(5) . ? C26 C27 1.382(5) . ? C27 C28 1.393(5) . ? C27 H27 0.9500 . ? C28 C34 1.392(5) . ? C28 C29 1.485(5) . ? C29 C33 1.390(5) . ? C29 C30 1.397(5) . ? C30 C31 1.387(5) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.390(5) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.392(5) . ? C34 H34 0.9500 . ? C35 C36 1.470(5) . ? C36 C37 1.371(5) . ? C37 C38 1.385(5) . ? C37 H37 0.9500 . ? C38 C39 1.381(6) . ? C38 H38 0.9500 . ? C39 C40 1.378(5) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.437(7) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? 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 N2 Fe1 N6 177.82(13) . . ? N2 Fe1 N3 80.88(13) . . ? N6 Fe1 N3 99.49(13) . . ? N2 Fe1 N7 101.58(13) . . ? N6 Fe1 N7 80.56(13) . . ? N3 Fe1 N7 93.26(12) . . ? N2 Fe1 N1 80.37(13) . . ? N6 Fe1 N1 99.31(13) . . ? N3 Fe1 N1 161.19(12) . . ? N7 Fe1 N1 89.07(12) . . ? N2 Fe1 N5 97.03(14) . . ? N6 Fe1 N5 80.84(14) . . ? N3 Fe1 N5 89.38(12) . . ? N7 Fe1 N5 161.39(12) . . ? N1 Fe1 N5 94.34(12) . . ? O2 Cl1 O1 108.98(18) . . ? O2 Cl1 O3 109.61(19) . . ? O1 Cl1 O3 109.21(19) . . ? O2 Cl1 O4 110.65(18) . . ? O1 Cl1 O4 109.37(17) . . ? O3 Cl1 O4 109.00(17) . . ? O8 Cl2 O5 109.5(2) . . ? O8 Cl2 O7 110.06(19) . . ? O5 Cl2 O7 108.81(18) . . ? O8 Cl2 O6 108.51(18) . . ? O5 Cl2 O6 110.4(2) . . ? O7 Cl2 O6 109.50(17) . . ? O12 Cl3 O9 109.87(17) . . ? O12 Cl3 O11 109.15(18) . . ? O9 Cl3 O11 109.50(17) . . ? O12 Cl3 O10 109.79(17) . . ? O9 Cl3 O10 109.57(18) . . ? O11 Cl3 O10 108.94(17) . . ? C41 O13 H13A 108(3) . . ? C1 N1 C5 117.7(3) . . ? C1 N1 Fe1 127.3(3) . . ? C5 N1 Fe1 114.8(2) . . ? C6 N2 C15 120.3(3) . . ? C6 N2 Fe1 120.0(3) . . ? C15 N2 Fe1 119.5(3) . . ? C20 N3 C16 117.9(3) . . ? C20 N3 Fe1 127.2(3) . . ? C16 N3 Fe1 114.9(2) . . ? C12 N4 C11 120.6(3) . . ? C12 N4 H4A 120(3) . . ? C11 N4 H4A 119(3) . . ? C21 N5 C25 117.7(3) . . ? C21 N5 Fe1 128.3(2) . . ? C25 N5 Fe1 114.1(2) . . ? C26 N6 C35 120.3(3) . . ? C26 N6 Fe1 119.8(2) . . ? C35 N6 Fe1 119.8(2) . . ? C40 N7 C36 117.5(3) . . ? C40 N7 Fe1 127.2(2) . . ? C36 N7 Fe1 115.2(2) . . ? C31 N8 C32 118.2(3) . . ? N1 C1 C2 122.0(4) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C1 C2 C3 120.3(4) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C2 C3 C4 118.9(4) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 119.1(4) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? N1 C5 C4 122.0(3) . . ? N1 C5 C6 113.2(3) . . ? C4 C5 C6 124.8(3) . . ? N2 C6 C7 121.6(3) . . ? N2 C6 C5 111.3(3) . . ? C7 C6 C5 127.1(4) . . ? C6 C7 C8 118.6(4) . . ? C6 C7 H7 120.7 . . ? C8 C7 H7 120.7 . . ? C14 C8 C7 119.5(3) . . ? C14 C8 C9 121.0(3) . . ? C7 C8 C9 119.5(4) . . ? C10 C9 C13 118.0(3) . . ? C10 C9 C8 121.3(3) . . ? C13 C9 C8 120.7(3) . . ? C11 C10 C9 119.8(4) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? N4 C11 C10 121.1(4) . . ? N4 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? N4 C12 C13 120.9(4) . . ? N4 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C9 C13 C12 119.6(4) . . ? C9 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C15 C14 C8 119.0(4) . . ? C15 C14 H14 120.5 . . ? C8 C14 H14 120.5 . . ? N2 C15 C14 121.0(3) . . ? N2 C15 C16 111.6(3) . . ? C14 C15 C16 127.4(4) . . ? N3 C16 C17 122.2(3) . . ? N3 C16 C15 113.1(3) . . ? C17 C16 C15 124.7(3) . . ? C18 C17 C16 118.6(4) . . ? C18 C17 H17 120.7 . . ? C16 C17 H17 120.7 . . ? C17 C18 C19 119.6(4) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C20 C19 C18 119.4(4) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? N3 C20 C19 122.3(4) . . ? N3 C20 H20 118.9 . . ? C19 C20 H20 118.9 . . ? N5 C21 C22 123.2(3) . . ? N5 C21 H21 118.4 . . ? C22 C21 H21 118.4 . . ? C21 C22 C23 118.4(4) . . ? C21 C22 H22 120.8 . . ? C23 C22 H22 120.8 . . ? C24 C23 C22 119.6(4) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C25 119.4(3) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? N5 C25 C24 121.8(3) . . ? N5 C25 C26 114.0(3) . . ? C24 C25 C26 124.3(3) . . ? N6 C26 C27 121.2(3) . . ? N6 C26 C25 111.2(3) . . ? C27 C26 C25 127.5(3) . . ? C26 C27 C28 119.5(3) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C34 C28 C27 118.8(3) . . ? C34 C28 C29 121.6(3) . . ? C27 C28 C29 119.6(3) . . ? C33 C29 C30 118.0(3) . . ? C33 C29 C28 120.8(3) . . ? C30 C29 C28 121.2(3) . . ? C31 C30 C29 118.9(4) . . ? C31 C30 H30 120.5 . . ? C29 C30 H30 120.5 . . ? N8 C31 C30 123.2(4) . . ? N8 C31 H31 118.4 . . ? C30 C31 H31 118.4 . . ? N8 C32 C33 122.5(4) . . ? N8 C32 H32 118.8 . . ? C33 C32 H32 118.8 . . ? C32 C33 C29 119.3(4) . . ? C32 C33 H33 120.4 . . ? C29 C33 H33 120.4 . . ? C35 C34 C28 119.3(3) . . ? C35 C34 H34 120.3 . . ? C28 C34 H34 120.3 . . ? N6 C35 C34 120.8(3) . . ? N6 C35 C36 111.5(3) . . ? C34 C35 C36 127.7(3) . . ? C37 C36 N7 121.9(3) . . ? C37 C36 C35 125.4(3) . . ? N7 C36 C35 112.7(3) . . ? C36 C37 C38 119.6(4) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C39 C38 C37 118.9(4) . . ? C39 C38 H38 120.6 . . ? C37 C38 H38 120.6 . . ? C40 C39 C38 119.3(4) . . ? C40 C39 H39 120.4 . . ? C38 C39 H39 120.4 . . ? N7 C40 C39 122.9(4) . . ? N7 C40 H40 118.6 . . ? C39 C40 H40 118.6 . . ? O13 C41 C42 113.4(5) . . ? O13 C41 H41A 108.9 . . ? C42 C41 H41A 108.9 . . ? O13 C41 H41B 108.9 . . ? C42 C41 H41B 108.9 . . ? H41A C41 H41B 107.7 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? 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 O13 H13A O4 0.884(19) 2.03(2) 2.896(5) 166(5) . N4 H4A N8 0.927(19) 1.76(2) 2.684(5) 177(4) 1_656 _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.563 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.106 # Attachment 'Fe_4_pyH__4_py__thiocyanate_H2O.cif' data_jb1023_2 _database_code_depnum_ccdc_archive 'CCDC 653283' _audit_creation_date 07-07-03 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title '7031256 jb1023_2_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 13.15620(10) _cell_length_b 20.3741(2) _cell_length_c 18.8557(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5054.19(8) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c n ' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,z x+1/2,-y+1/2,-z x,-y,z+1/2 -x,y,-z+1/2 -x+1/2,-y+1/2,z+1/2 x+1/2,y+1/2,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C40 H34 Fe2 N10 O1 S4 # Dc = 1.20 Fooo = 2284.00 Mu = 7.77 M = 455.37 # Found Formula = C46 H33 Fe2 N14 O2 S6 # Dc = 1.47 FOOO = 2284.00 Mu = 8.75 M = 558.98 _chemical_formula_sum 'C46 H33 Fe2 N14 O2 S6' _chemical_formula_moiety 'C40 H29 Fe N8, C6 Fe N6 S6, 2(H2 O)' _chemical_compound_source ? _chemical_formula_weight 1117.95 _cell_measurement_reflns_used 22215 _cell_measurement_theta_min 1 _cell_measurement_theta_max 28 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_max 0.28 _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2284 _exptl_absorpt_coefficient_mu 0.875 # Sheldrick geometric approximatio 0.80 0.90 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 0.90 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 173 _diffrn_reflns_number 43208 _reflns_number_total 6034 _diffrn_reflns_av_R_equivalents 0.043 # Number of reflections with Friedels Law is 6034 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 6022 _diffrn_reflns_theta_min 1.843 _diffrn_reflns_theta_max 27.869 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.869 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min 0 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 26 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.33 _refine_diff_density_max 0.46 _refine_ls_number_reflns 3836 _refine_ls_number_restraints 11 _refine_ls_number_parameters 333 #_refine_ls_R_factor_ref 0.0279 _refine_ls_wR_factor_ref 0.0319 _refine_ls_goodness_of_fit_ref 1.0827 #_reflns_number_all 5995 _refine_ls_R_factor_all 0.0445 _refine_ls_wR_factor_all 0.0463 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 3836 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_gt 0.0319 _refine_ls_shift/su_max 0.000602 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.422 0.297 0.196 ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fih. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Fe1 Fe 0.5000 0.173580(14) 0.7500 0.0187 1.0000 Uani S T . . . . Fe2 Fe 0.5000 0.5000 0.5000 0.0325 1.0000 Uani S . . . . . N1 N 0.40634(10) 0.15849(6) 0.66974(8) 0.0219 1.0000 Uani . . . . . . N2 N 0.5000 0.08136(9) 0.7500 0.0204 1.0000 Uani S T . . . . N3 N 0.5000 -0.26241(10) 0.7500 0.0342 1.0000 Uani S T . . . . N4 N 0.38127(10) 0.18888(6) 0.81244(8) 0.0227 1.0000 Uani . . . . . . N5 N 0.5000 0.26578(8) 0.7500 0.0201 1.0000 Uani S T . . . . N6 N 0.500000(7) 0.60874(10) 0.750000(7) 0.0378 1.0000 Uani S T . . . . N7 N 0.40517(14) 0.46226(10) 0.57558(10) 0.0450 1.0000 Uani . . . . . . N8 N 0.51380(15) 0.40544(10) 0.46199(12) 0.0479 1.0000 Uani . . . . . . N9 N 0.62586(14) 0.48473(9) 0.56335(10) 0.0422 1.0000 Uani . . . . . . C1 C 0.35940(14) 0.20408(8) 0.63010(10) 0.0273 1.0000 Uani . . . . . . C2 C 0.29101(15) 0.18806(9) 0.57712(11) 0.0341 1.0000 Uani . . . . . . C3 C 0.27053(15) 0.12255(9) 0.56358(11) 0.0349 1.0000 Uani . . . . . . C4 C 0.31918(14) 0.07484(9) 0.60343(10) 0.0302 1.0000 Uani . . . . . . C5 C 0.38594(12) 0.09381(7) 0.65616(10) 0.0237 1.0000 Uani . . . . . . C6 C 0.44226(12) 0.04886(7) 0.70255(9) 0.0216 1.0000 Uani . . . . . . C7 C 0.44088(12) -0.01934(8) 0.70111(10) 0.0232 1.0000 Uani . . . . . . C8 C 0.5000 -0.05381(10) 0.7500 0.0232 1.0000 Uani S T . . . . C9 C 0.5000 -0.12657(11) 0.7500 0.0239 1.0000 Uani S T . . . . C10 C 0.48181(14) -0.16172(8) 0.68806(11) 0.0299 1.0000 Uani . . . . . . C11 C 0.48149(15) -0.22954(8) 0.69024(11) 0.0342 1.0000 Uani . . . . . . C12 C 0.32204(14) 0.14368(8) 0.84357(11) 0.0315 1.0000 Uani . . . . . . C13 C 0.23795(15) 0.15986(10) 0.88393(12) 0.0373 1.0000 Uani . . . . . . C14 C 0.21295(14) 0.22510(10) 0.89263(11) 0.0343 1.0000 Uani . . . . . . C15 C 0.27276(13) 0.27258(9) 0.86073(10) 0.0289 1.0000 Uani . . . . . . C16 C 0.35656(13) 0.25326(8) 0.82142(9) 0.0230 1.0000 Uani . . . . . . C17 C 0.42729(12) 0.29836(8) 0.78604(9) 0.0217 1.0000 Uani . . . . . . C18 C 0.42485(14) 0.36630(8) 0.78639(10) 0.0262 1.0000 Uani . . . . . . C19 C 0.5000 0.40065(10) 0.7500 0.0255 1.0000 Uani S T . . . . C20 C 0.5000 0.47358(11) 0.7500 0.0271 1.0000 Uani S T . . . . C21 C 0.59055(16) 0.50829(8) 0.75418(11) 0.0340 1.0000 Uani . . . . . . C22 C 0.58729(17) 0.57604(9) 0.75462(12) 0.0384 1.0000 Uani . . . . . . C23 C 0.34766(16) 0.42486(10) 0.59918(12) 0.0381 1.0000 Uani . . . . . . C24 C 0.52094(14) 0.35064(11) 0.47836(12) 0.0376 1.0000 Uani . . . . . . C25 C 0.70175(14) 0.47469(9) 0.59175(10) 0.0297 1.0000 Uani . . . . . . S1 S 0.26702(4) 0.37449(3) 0.63455(4) 0.0533 1.0000 Uani . . . . . . S2 S 0.53260(5) 0.27407(3) 0.50037(3) 0.0448 1.0000 Uani . . . . . . S3 S 0.80730(4) 0.45929(2) 0.63357(3) 0.0383 1.0000 Uani . . . . . . O1 O 0.5296(3) 0.0576(3) 0.4558(2) 0.0854 0.5000 Uani . U . . . . O2 O 0.5645(5) 0.0970(2) 0.5067(2) 0.0866 0.5000 Uani . U . . . . H1 H 0.5000 0.6520 0.7500 0.0463 1.0000 Uiso RS . . . . . H2 H 0.5386 0.0429 0.4970 0.1011 0.5000 Uiso . . . . . . H3 H 0.5016 0.0937 0.4601 0.1011 0.5000 Uiso . . . . . . H6 H 0.6268 0.1018 0.5023 0.1005 0.5000 Uiso . . . . . . H7 H 0.5522 0.0571 0.5033 0.1005 0.5000 Uiso . . . . . . H11 H 0.3739 0.2489 0.6398 0.0307 1.0000 Uiso R . . . . . H31 H 0.2242 0.1106 0.5291 0.0412 1.0000 Uiso R . . . . . H41 H 0.3073 0.0300 0.5951 0.0348 1.0000 Uiso R . . . . . H71 H 0.3995 -0.0411 0.6684 0.0268 1.0000 Uiso R . . . . . H101 H 0.4700 -0.1402 0.6459 0.0338 1.0000 Uiso R . . . . . H111 H 0.4681 -0.2532 0.6487 0.0402 1.0000 Uiso R . . . . . H121 H 0.3409 0.0984 0.8364 0.0364 1.0000 Uiso R . . . . . H131 H 0.1985 0.1271 0.9051 0.0445 1.0000 Uiso R . . . . . H141 H 0.1565 0.2374 0.9203 0.0398 1.0000 Uiso R . . . . . H151 H 0.2566 0.3175 0.8669 0.0338 1.0000 Uiso R . . . . . H181 H 0.3736 0.3891 0.8108 0.0290 1.0000 Uiso R . . . . . H211 H 0.6513 0.4864 0.7568 0.0393 1.0000 Uiso R . . . . . H221 H 0.6470 0.6010 0.7583 0.0442 1.0000 Uiso R . . . . . H222 H 0.2586 0.2212 0.5523 0.0401 1.0000 Uiso R . . . . . 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 0.01909(15) 0.01029(13) 0.02680(17) 0.0000 -0.00025(14) 0.0000 Fe2 0.02808(18) 0.0350(2) 0.0343(2) -0.00058(15) -0.00582(17) 0.00292(16) N1 0.0214(6) 0.0146(6) 0.0299(8) -0.0001(5) 0.0005(6) 0.0006(5) N2 0.0203(8) 0.0120(8) 0.0291(10) 0.0000 0.0017(9) 0.0000 N3 0.0455(13) 0.0131(9) 0.0440(13) 0.0000 0.0019(12) 0.0000 N4 0.0220(7) 0.0159(6) 0.0301(7) 0.0001(5) 0.0011(6) -0.0005(5) N5 0.0201(8) 0.0130(8) 0.0270(10) 0.0000 0.0004(8) 0.0000 N6 0.0617(15) 0.0120(9) 0.0398(13) 0.0000 0.0063(13) 0.0000 N7 0.0413(10) 0.0501(11) 0.0436(10) 0.0023(9) 0.0013(8) -0.0005(9) N8 0.0414(11) 0.0431(10) 0.0592(13) -0.0091(9) -0.0046(9) 0.0041(8) N9 0.0370(9) 0.0464(10) 0.0433(10) 0.0025(8) -0.0111(8) 0.0028(8) C1 0.0302(9) 0.0183(7) 0.0333(9) 0.0027(7) -0.0027(7) 0.0018(6) C2 0.0361(10) 0.0286(9) 0.0374(10) 0.0040(8) -0.0089(9) 0.0049(7) C3 0.0349(10) 0.0329(9) 0.0369(11) -0.0040(8) -0.0114(8) 0.0001(8) C4 0.0311(9) 0.0223(8) 0.0373(10) -0.0050(7) -0.0050(8) -0.0014(7) C5 0.0227(8) 0.0157(7) 0.0327(9) -0.0013(7) -0.0005(7) 0.0000(6) C6 0.0211(7) 0.0155(7) 0.0283(9) -0.0017(7) 0.0018(6) -0.0006(6) C7 0.0233(8) 0.0158(7) 0.0307(9) -0.0027(7) 0.0007(7) -0.0019(6) C8 0.0254(11) 0.0131(9) 0.0311(12) 0.0000 0.0063(10) 0.0000 C9 0.0232(10) 0.0137(9) 0.0347(13) 0.0000 0.0036(11) 0.0000 C10 0.0384(10) 0.0172(7) 0.0340(10) 0.0006(7) 0.0004(8) 0.0010(7) C11 0.0458(12) 0.0181(8) 0.0388(11) -0.0050(7) 0.0006(9) 0.0002(7) C12 0.0312(9) 0.0186(8) 0.0447(11) 0.0017(8) 0.0074(8) -0.0035(7) C13 0.0331(10) 0.0301(9) 0.0487(12) 0.0036(9) 0.0112(9) -0.0094(8) C14 0.0261(9) 0.0347(9) 0.0420(11) -0.0035(9) 0.0097(8) -0.0008(8) C15 0.0258(8) 0.0233(8) 0.0375(10) -0.0023(8) 0.0048(7) 0.0012(7) C16 0.0238(8) 0.0159(7) 0.0292(9) -0.0010(6) -0.0011(7) -0.0013(6) C17 0.0224(7) 0.0164(7) 0.0264(9) -0.0005(6) 0.0007(7) 0.0009(6) C18 0.0288(9) 0.0159(7) 0.0338(10) -0.0026(7) 0.0045(8) 0.0035(6) C19 0.0354(12) 0.0116(9) 0.0295(12) 0.0000 0.0016(11) 0.0000 C20 0.0389(13) 0.0131(10) 0.0293(12) 0.0000 0.0055(12) 0.0000 C21 0.0409(10) 0.0175(7) 0.0436(11) 0.0005(8) 0.0056(9) -0.0013(7) C22 0.0494(11) 0.0173(8) 0.0487(12) -0.0004(9) 0.0040(10) -0.0081(8) C23 0.0332(10) 0.0360(10) 0.0451(12) -0.0035(9) -0.0046(9) 0.0109(9) C24 0.0261(10) 0.0483(12) 0.0384(11) -0.0123(10) -0.0034(8) 0.0001(8) C25 0.0325(9) 0.0241(8) 0.0327(9) 0.0015(7) 0.0000(8) -0.0044(7) S1 0.0363(3) 0.0330(3) 0.0908(5) 0.0050(3) 0.0064(3) 0.0044(2) S2 0.0421(3) 0.0473(3) 0.0449(3) 0.0040(3) -0.0055(2) -0.0013(2) S3 0.0288(2) 0.0326(2) 0.0536(3) 0.0045(2) -0.0098(2) -0.00253(19) O1 0.074(3) 0.137(4) 0.045(2) -0.032(2) -0.0120(19) 0.022(3) O2 0.125(4) 0.080(3) 0.055(2) -0.005(2) 0.011(3) 0.010(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1910(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . N4 6_656 1.9807(14) yes Fe1 . N1 6_656 1.9755(14) yes Fe1 . N1 . 1.9755(14) yes Fe1 . N2 . 1.8788(18) yes Fe1 . N4 . 1.9807(14) yes Fe1 . N5 . 1.8785(17) yes Fe2 . N9 2_666 2.0652(17) yes Fe2 . N8 2_666 2.064(2) yes Fe2 . N7 2_666 2.0442(19) yes Fe2 . N7 . 2.0442(19) yes Fe2 . N8 . 2.064(2) yes Fe2 . N9 . 2.0652(17) yes N1 . C1 . 1.343(2) yes N1 . C5 . 1.369(2) yes N2 . C6 6_656 1.3476(18) yes N2 . C6 . 1.3476(18) yes N3 . C11 6_656 1.333(2) yes N3 . C11 . 1.333(2) yes N4 . C12 . 1.342(2) yes N4 . C16 . 1.362(2) yes N5 . C17 6_656 1.3481(18) yes N5 . C17 . 1.3481(18) yes N6 . C22 6_656 1.331(2) yes N6 . C22 . 1.331(2) yes N6 . H1 . 0.881 no N7 . C23 . 1.162(3) yes N8 . C24 . 1.162(3) yes N9 . C25 . 1.151(3) yes C1 . C2 . 1.383(3) yes C1 . H11 . 0.950 no C2 . C3 . 1.385(3) yes C2 . H222 . 0.925 no C3 . C4 . 1.385(3) yes C3 . H31 . 0.923 no C4 . C5 . 1.382(3) yes C4 . H41 . 0.939 no C5 . C6 . 1.467(2) yes C6 . C7 . 1.390(2) yes C7 . C8 . 1.396(2) yes C7 . H71 . 0.935 no C8 . C9 . 1.483(3) yes C9 . C10 6_656 1.391(2) yes C9 . C10 . 1.391(2) yes C10 . C11 . 1.383(2) yes C10 . H101 . 0.921 no C11 . H111 . 0.936 no C12 . C13 . 1.383(3) yes C12 . H121 . 0.964 no C13 . C14 . 1.379(3) yes C13 . H131 . 0.935 no C14 . C15 . 1.384(3) yes C14 . H141 . 0.941 no C15 . C16 . 1.386(2) yes C15 . H151 . 0.947 no C16 . C17 . 1.468(2) yes C17 . C18 . 1.385(2) yes C18 . C19 . 1.392(2) yes C18 . H181 . 0.939 no C19 . C20 . 1.486(3) yes C20 . C21 6_656 1.388(2) yes C20 . C21 . 1.388(2) yes C21 . C22 . 1.381(2) yes C21 . H211 . 0.917 no C22 . H221 . 0.938 no C23 . S1 . 1.620(2) yes C24 . S2 . 1.621(2) yes C25 . S3 . 1.628(2) yes O1 . O2 . 1.333(6) yes O1 . H2 . 0.840 no O1 . H3 . 0.828 no O2 . H6 . 0.829 no O2 . H7 . 0.832 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N4 6_656 Fe1 . N1 6_656 89.31(6) yes N4 6_656 Fe1 . N1 . 93.50(6) yes N1 6_656 Fe1 . N1 . 162.09(8) yes N4 6_656 Fe1 . N2 . 99.05(4) yes N1 6_656 Fe1 . N2 . 81.05(4) yes N1 . Fe1 . N2 . 81.05(4) yes N4 6_656 Fe1 . N4 . 161.89(8) yes N1 6_656 Fe1 . N4 . 93.50(6) yes N1 . Fe1 . N4 . 89.31(6) yes N2 . Fe1 . N4 . 99.05(4) yes N4 6_656 Fe1 . N5 . 80.95(4) yes N1 6_656 Fe1 . N5 . 98.95(4) yes N1 . Fe1 . N5 . 98.95(4) yes N2 . Fe1 . N5 . 179.994 yes N4 . Fe1 . N5 . 80.95(4) yes N9 2_666 Fe2 . N8 2_666 89.41(8) yes N9 2_666 Fe2 . N7 2_666 91.69(8) yes N8 2_666 Fe2 . N7 2_666 86.83(8) yes N9 2_666 Fe2 . N7 . 88.31(8) yes N8 2_666 Fe2 . N7 . 93.17(8) yes N7 2_666 Fe2 . N7 . 179.994 yes N9 2_666 Fe2 . N8 . 90.59(8) yes N8 2_666 Fe2 . N8 . 179.994 yes N7 2_666 Fe2 . N8 . 93.17(8) yes N7 . Fe2 . N8 . 86.83(8) yes N9 2_666 Fe2 . N9 . 179.994 yes N8 2_666 Fe2 . N9 . 90.59(8) yes N7 2_666 Fe2 . N9 . 88.31(8) yes N7 . Fe2 . N9 . 91.69(8) yes N8 . Fe2 . N9 . 89.41(8) yes Fe1 . N1 . C1 . 127.28(11) yes Fe1 . N1 . C5 . 114.55(11) yes C1 . N1 . C5 . 118.13(15) yes C6 6_656 N2 . Fe1 . 119.44(9) yes C6 6_656 N2 . C6 . 121.13(19) yes Fe1 . N2 . C6 . 119.44(9) yes C11 6_656 N3 . C11 . 119.7(2) yes Fe1 . N4 . C12 . 127.60(12) yes Fe1 . N4 . C16 . 114.44(11) yes C12 . N4 . C16 . 117.90(15) yes C17 6_656 N5 . Fe1 . 119.49(9) yes C17 6_656 N5 . C17 . 121.02(18) yes Fe1 . N5 . C17 . 119.49(9) yes C22 6_656 N6 . C22 . 119.9(2) yes C22 6_656 N6 . H1 . 120.1 no C22 . N6 . H1 . 120.1 no Fe2 . N7 . C23 . 155.61(18) yes Fe2 . N8 . C24 . 144.3(2) yes Fe2 . N9 . C25 . 172.34(18) yes N1 . C1 . C2 . 122.54(16) yes N1 . C1 . H11 . 117.7 no C2 . C1 . H11 . 119.8 no C1 . C2 . C3 . 119.14(17) yes C1 . C2 . H222 . 119.5 no C3 . C2 . H222 . 121.3 no C2 . C3 . C4 . 119.09(18) yes C2 . C3 . H31 . 120.8 no C4 . C3 . H31 . 120.1 no C3 . C4 . C5 . 119.19(16) yes C3 . C4 . H41 . 121.0 no C5 . C4 . H41 . 119.8 no C4 . C5 . N1 . 121.91(15) yes C4 . C5 . C6 . 125.13(15) yes N1 . C5 . C6 . 112.97(14) yes C5 . C6 . N2 . 111.95(14) yes C5 . C6 . C7 . 127.28(16) yes N2 . C6 . C7 . 120.77(16) yes C6 . C7 . C8 . 118.87(16) yes C6 . C7 . H71 . 119.6 no C8 . C7 . H71 . 121.5 no C7 . C8 . C7 6_656 119.6(2) yes C7 . C8 . C9 . 120.21(10) yes C7 6_656 C8 . C9 . 120.21(10) yes C8 . C9 . C10 6_656 120.99(11) yes C8 . C9 . C10 . 120.99(11) yes C10 6_656 C9 . C10 . 118.0(2) yes C9 . C10 . C11 . 119.35(18) yes C9 . C10 . H101 . 120.7 no C11 . C10 . H101 . 120.0 no C10 . C11 . N3 . 121.78(19) yes C10 . C11 . H111 . 119.3 no N3 . C11 . H111 . 118.9 no N4 . C12 . C13 . 122.82(16) yes N4 . C12 . H121 . 116.5 no C13 . C12 . H121 . 120.7 no C12 . C13 . C14 . 119.08(17) yes C12 . C13 . H131 . 120.6 no C14 . C13 . H131 . 120.3 no C13 . C14 . C15 . 119.09(17) yes C13 . C14 . H141 . 120.6 no C15 . C14 . H141 . 120.3 no C14 . C15 . C16 . 119.09(16) yes C14 . C15 . H151 . 119.6 no C16 . C15 . H151 . 121.3 no C15 . C16 . N4 . 122.01(15) yes C15 . C16 . C17 . 124.72(15) yes N4 . C16 . C17 . 113.26(14) yes C16 . C17 . N5 . 111.76(14) yes C16 . C17 . C18 . 127.50(16) yes N5 . C17 . C18 . 120.73(16) yes C17 . C18 . C19 . 118.94(16) yes C17 . C18 . H181 . 120.9 no C19 . C18 . H181 . 120.2 no C18 6_656 C19 . C18 . 119.6(2) yes C18 6_656 C19 . C20 . 120.18(10) yes C18 . C19 . C20 . 120.18(10) yes C19 . C20 . C21 6_656 120.64(11) yes C19 . C20 . C21 . 120.64(11) yes C21 6_656 C20 . C21 . 118.7(2) yes C20 . C21 . C22 . 118.89(19) yes C20 . C21 . H211 . 120.2 no C22 . C21 . H211 . 120.9 no C21 . C22 . N6 . 121.80(19) yes C21 . C22 . H221 . 121.0 no N6 . C22 . H221 . 117.2 no N7 . C23 . S1 . 177.9(2) yes N8 . C24 . S2 . 179.0(2) yes N9 . C25 . S3 . 178.38(18) yes H2 . O1 . H3 . 106.8 no H6 . O2 . H7 . 107.4 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag N6 . H1 . N3 1_565 180 0.88 1.74 2.625(2) yes # Attachment 'Fe_4_pyH__4_py__thiocyanate_MeCN.cif' data_jb842 _database_code_depnum_ccdc_archive 'CCDC 653284' _audit_creation_date 07-07-05 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title '3271209 jb842_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 13.30570(10) _cell_length_b 20.3495(2) _cell_length_c 18.4014(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4982.44(8) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c n ' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,z x+1/2,-y+1/2,-z x,-y,z+1/2 -x,y,-z+1/2 -x+1/2,-y+1/2,z+1/2 x+1/2,y+1/2,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C40 H28 Fe2 N8 O2 S4 # Dc = 1.19 Fooo = 2292.00 Mu = 7.87 M = 446.34 # Found Formula = C48 H32 Fe2 N15 S6 # Dc = 1.50 FOOO = 2292.00 Mu = 8.86 M = 561.49 _chemical_formula_sum 'C48 H32 Fe2 N15 S6' _chemical_formula_moiety 'C40 H29 Fe N8, C6 Fe N6 S6, C2 H3 N' _chemical_compound_source ? _chemical_formula_weight 1122.97 _cell_measurement_reflns_used 19798 _cell_measurement_theta_min 1 _cell_measurement_theta_max 28 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_min 0.22 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.48 _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2292 _exptl_absorpt_coefficient_mu 0.886 # Sheldrick geometric approximatio 0.77 0.82 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 0.82 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 173 _diffrn_reflns_number 39664 _reflns_number_total 5914 _diffrn_reflns_av_R_equivalents 0.036 # Number of reflections with Friedels Law is 5914 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 5911 _diffrn_reflns_theta_min 1.829 _diffrn_reflns_theta_max 27.829 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.829 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min 0 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 26 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.82 _refine_diff_density_max 0.74 _refine_ls_number_reflns 4094 _refine_ls_number_restraints 454 _refine_ls_number_parameters 340 #_refine_ls_R_factor_ref 0.0701 _refine_ls_wR_factor_ref 0.0414 _refine_ls_goodness_of_fit_ref 0.9055 #_reflns_number_all 5856 _refine_ls_R_factor_all 0.0910 _refine_ls_wR_factor_all 0.0432 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 4094 _refine_ls_R_factor_gt 0.0701 _refine_ls_wR_factor_gt 0.0414 _refine_ls_shift/su_max 0.036550 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.04 -0.188 0.914 -0.483E-01 0.224 ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fih. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Fe1 Fe 0.5000 0.17465(2) 0.7500 0.0170 1.0000 Uani S T . . . . Fe2 Fe 0.5000 0.5000 0.5000 0.0390 1.0000 Uani S . . . . . N1 N 0.40275(16) 0.15980(10) 0.67111(12) 0.0188 1.0000 Uani . . . . . . N2 N 0.5000 0.08268(13) 0.7500 0.0166 1.0000 Uani S T . . . . N3 N 0.5000 -0.26182(16) 0.7500 0.0465 1.0000 Uani S T . . . . N4 N 0.38637(16) 0.18986(11) 0.81707(13) 0.0196 1.0000 Uani . . . . . . N5 N 0.5000 0.26648(14) 0.7500 0.0188 1.0000 Uani S T . . . . N6 N 0.500000(7) 0.60898(17) 0.750000(7) 0.0481 1.0000 Uani S T . . . . N7 N 0.4072(2) 0.46367(18) 0.57911(17) 0.0477 1.0000 Uani . . . . . . N8 N 0.5093(3) 0.40446(18) 0.46158(19) 0.0549 1.0000 Uani . . . . . . N9 N 0.6263(2) 0.48383(16) 0.56239(16) 0.0440 1.0000 Uani . . . . . . N10 N 0.4634(11) -0.0526(5) 0.5057(10) 0.0924 0.5000 Uani D U . . . . C1 C 0.3531(2) 0.20560(13) 0.63245(16) 0.0246 1.0000 Uani . . . . . . C2 C 0.2813(2) 0.18933(15) 0.58119(17) 0.0294 1.0000 Uani . . . . . . C3 C 0.2601(2) 0.12376(16) 0.56790(17) 0.0331 1.0000 Uani . . . . . . C4 C 0.3108(2) 0.07639(15) 0.60687(16) 0.0280 1.0000 Uani . . . . . . C5 C 0.38130(19) 0.09511(12) 0.65780(15) 0.0201 1.0000 Uani . . . . . . C6 C 0.43987(19) 0.04988(12) 0.70319(14) 0.0176 1.0000 Uani . . . . . . C7 C 0.4387(2) -0.01799(12) 0.70213(16) 0.0214 1.0000 Uani . . . . . . C8 C 0.5000 -0.05284(17) 0.7500 0.0226 1.0000 Uani S T . . . . C9 C 0.5000 -0.12512(17) 0.7500 0.0273 1.0000 Uani S T . . . . C10 C 0.4826(2) -0.16075(13) 0.6865(2) 0.0358 1.0000 Uani . . . . . . C11 C 0.4825(3) -0.22853(15) 0.6894(2) 0.0442 1.0000 Uani . . . . . . C12 C 0.3317(2) 0.14471(14) 0.85199(16) 0.0269 1.0000 Uani . . . . . . C13 C 0.2484(2) 0.16041(15) 0.89375(18) 0.0334 1.0000 Uani . . . . . . C14 C 0.2189(2) 0.22567(15) 0.89798(18) 0.0314 1.0000 Uani . . . . . . C15 C 0.2749(2) 0.27311(15) 0.86347(17) 0.0281 1.0000 Uani . . . . . . C16 C 0.3588(2) 0.25431(12) 0.82414(15) 0.0200 1.0000 Uani . . . . . . C17 C 0.42834(19) 0.29932(12) 0.78691(14) 0.0186 1.0000 Uani . . . . . . C18 C 0.4253(2) 0.36730(13) 0.78698(15) 0.0231 1.0000 Uani . . . . . . C19 C 0.5000 0.40212(16) 0.7500 0.0235 1.0000 Uani S T . . . . C20 C 0.5000 0.47450(17) 0.7500 0.0274 1.0000 Uani S T . . . . C21 C 0.5900(3) 0.50944(12) 0.7496(2) 0.0377 1.0000 Uani . . . . . . C22 C 0.5872(3) 0.57714(14) 0.7502(3) 0.0454 1.0000 Uani . . . . . . C23 C 0.3471(2) 0.42653(18) 0.59917(19) 0.0384 1.0000 Uani . . . . . . C24 C 0.5151(2) 0.3499(2) 0.4798(2) 0.0473 1.0000 Uani . . . . . . C25 C 0.7025(2) 0.47471(15) 0.59072(16) 0.0292 1.0000 Uani . . . . . . C26 C 0.5243(14) 0.0710(5) 0.4977(14) 0.1070 0.5000 Uani D U . . . . C27 C 0.5000 0.0000 0.5000 0.1141 1.0000 Uani DS U . . . . S1 S 0.26265(7) 0.37671(4) 0.62984(7) 0.0564 1.0000 Uani . . . . . . S2 S 0.52618(7) 0.27331(6) 0.50357(6) 0.0552 1.0000 Uani . . . . . . S3 S 0.80735(6) 0.45981(4) 0.63203(5) 0.0372 1.0000 Uani . . . . . . H1 H 0.5000 0.6512 0.7500 0.0571 1.0000 Uiso RS . . . . . H11 H 0.3684 0.2500 0.6407 0.0289 1.0000 Uiso R . . . . . H31 H 0.2120 0.1122 0.5341 0.0392 1.0000 Uiso R . . . . . H41 H 0.2975 0.0325 0.5990 0.0326 1.0000 Uiso R . . . . . H71 H 0.3959 -0.0401 0.6701 0.0258 1.0000 Uiso R . . . . . H101 H 0.4714 -0.1390 0.6429 0.0430 1.0000 Uiso R . . . . . H111 H 0.4700 -0.2523 0.6471 0.0518 1.0000 Uiso R . . . . . H121 H 0.3504 0.1008 0.8479 0.0319 1.0000 Uiso R . . . . . H131 H 0.2131 0.1271 0.9173 0.0403 1.0000 Uiso R . . . . . H141 H 0.1621 0.2367 0.9254 0.0372 1.0000 Uiso R . . . . . H151 H 0.2573 0.3179 0.8658 0.0338 1.0000 Uiso R . . . . . H181 H 0.3743 0.3890 0.8116 0.0273 1.0000 Uiso R . . . . . H211 H 0.6511 0.4873 0.7481 0.0449 1.0000 Uiso R . . . . . H221 H 0.6470 0.6010 0.7514 0.0539 1.0000 Uiso R . . . . . H222 H 0.2486 0.2223 0.5556 0.0360 1.0000 Uiso R . . . . . H261 H 0.5881 0.0774 0.4756 0.1264 0.5000 Uiso R . . . . . H262 H 0.5262 0.0869 0.5463 0.1264 0.5000 Uiso R . . . . . H263 H 0.4745 0.0941 0.4711 0.1264 0.5000 Uiso R . . . . . 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 0.0168(2) 0.0108(2) 0.0233(3) 0.0000 -0.0012(3) 0.0000 Fe2 0.0272(3) 0.0585(4) 0.0312(3) 0.0069(3) -0.0067(3) -0.0050(4) N1 0.0211(10) 0.0129(10) 0.0226(12) 0.0011(9) -0.0010(9) 0.0003(8) N2 0.0159(12) 0.0110(12) 0.0227(14) 0.0000 0.0003(14) 0.0000 N3 0.056(2) 0.0120(15) 0.071(3) 0.0000 0.018(3) 0.0000 N4 0.0205(10) 0.0125(10) 0.0258(12) 0.0000(9) -0.0006(9) -0.0021(8) N5 0.0199(13) 0.0149(14) 0.0216(14) 0.0000 -0.0045(15) 0.0000 N6 0.067(3) 0.0105(15) 0.067(3) 0.0000 0.019(3) 0.0000 N7 0.0373(15) 0.070(2) 0.0357(16) 0.0124(16) -0.0021(13) -0.0033(16) N8 0.0351(16) 0.069(2) 0.060(2) -0.0002(17) -0.0031(16) -0.0043(18) N9 0.0335(14) 0.061(2) 0.0371(16) 0.0106(15) -0.0089(13) -0.0050(14) N10 0.073(4) 0.148(6) 0.057(5) -0.023(6) -0.009(4) 0.039(5) C1 0.0257(13) 0.0182(12) 0.0299(15) 0.0056(12) -0.0031(12) 0.0023(10) C2 0.0300(14) 0.0289(15) 0.0293(15) 0.0057(13) -0.0062(12) 0.0053(12) C3 0.0292(14) 0.0387(17) 0.0313(15) -0.0058(14) -0.0109(13) 0.0014(13) C4 0.0267(13) 0.0264(14) 0.0307(15) -0.0031(12) -0.0042(12) -0.0001(12) C5 0.0195(12) 0.0164(12) 0.0244(14) 0.0002(10) -0.0004(11) -0.0006(10) C6 0.0196(11) 0.0119(11) 0.0212(13) -0.0017(10) 0.0005(10) -0.0015(9) C7 0.0214(12) 0.0126(12) 0.0302(14) -0.0041(11) 0.0007(11) -0.0017(10) C8 0.0233(16) 0.0139(16) 0.0307(19) 0.0000 0.0036(18) 0.0000 C9 0.0271(17) 0.0127(16) 0.042(2) 0.0000 0.007(2) 0.0000 C10 0.0417(18) 0.0170(13) 0.0485(19) -0.0056(12) 0.0061(15) 0.0017(12) C11 0.047(2) 0.0199(14) 0.065(2) -0.0126(15) 0.0080(18) 0.0008(14) C12 0.0295(14) 0.0181(13) 0.0330(16) 0.0043(12) 0.0064(13) -0.0039(11) C13 0.0314(15) 0.0302(16) 0.0386(18) -0.0014(14) 0.0086(14) -0.0093(13) C14 0.0232(13) 0.0315(15) 0.0395(17) -0.0062(14) 0.0099(13) 0.0011(12) C15 0.0271(14) 0.0258(14) 0.0314(16) -0.0039(13) 0.0058(12) 0.0019(12) C16 0.0237(13) 0.0147(12) 0.0215(13) -0.0009(10) -0.0018(11) 0.0000(10) C17 0.0232(12) 0.0145(12) 0.0182(13) 0.0001(10) -0.0001(11) -0.0003(10) C18 0.0303(14) 0.0141(12) 0.0250(14) -0.0025(11) 0.0066(12) 0.0046(11) C19 0.0355(19) 0.0125(16) 0.0224(17) 0.0000 0.001(2) 0.0000 C20 0.044(2) 0.0096(15) 0.0280(19) 0.0000 0.017(2) 0.0000 C21 0.0508(17) 0.0170(12) 0.0454(17) -0.0017(17) 0.0199(19) -0.0031(12) C22 0.0570(19) 0.0173(12) 0.062(2) -0.0005(19) 0.014(2) -0.0052(13) C23 0.0316(16) 0.0427(18) 0.0409(19) 0.0040(16) -0.0015(15) 0.0135(15) C24 0.0252(17) 0.080(3) 0.0362(18) -0.0044(18) -0.0048(14) -0.0088(18) C25 0.0326(15) 0.0291(15) 0.0258(15) 0.0023(12) 0.0009(13) -0.0044(12) C26 0.070(5) 0.189(6) 0.062(5) -0.004(7) -0.001(5) 0.017(6) C27 0.083(4) 0.190(6) 0.069(4) -0.017(5) -0.010(4) 0.033(5) S1 0.0444(5) 0.0302(4) 0.0946(8) 0.0067(5) 0.0190(6) 0.0075(4) S2 0.0377(5) 0.0822(8) 0.0455(5) 0.0215(5) -0.0081(4) -0.0067(5) S3 0.0278(4) 0.0333(4) 0.0504(5) 0.0040(4) -0.0089(4) -0.0038(3) _refine_ls_extinction_coef 300(40) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.1905(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . N4 6_656 1.976(2) yes Fe1 . N1 6_656 1.968(2) yes Fe1 . N1 . 1.968(2) yes Fe1 . N2 . 1.872(3) yes Fe1 . N4 . 1.976(2) yes Fe1 . N5 . 1.869(3) yes Fe2 . N8 2_666 2.072(4) yes Fe2 . N9 2_666 2.061(3) yes Fe2 . N7 2_666 2.047(3) yes Fe2 . N7 . 2.047(3) yes Fe2 . N8 . 2.072(4) yes Fe2 . N9 . 2.061(3) yes N1 . C1 . 1.346(3) yes N1 . C5 . 1.369(3) yes N2 . C6 6_656 1.352(3) yes N2 . C6 . 1.352(3) yes N3 . C11 6_656 1.325(4) yes N3 . C11 . 1.325(4) yes N4 . C12 . 1.337(3) yes N4 . C16 . 1.368(3) yes N5 . C17 6_656 1.348(3) yes N5 . C17 . 1.348(3) yes N6 . C22 6_656 1.329(4) yes N6 . C22 . 1.329(4) yes N6 . H1 . 0.859 no N7 . C23 . 1.161(4) yes N8 . C24 . 1.163(5) yes N9 . C25 . 1.155(4) yes N10 . C27 . 1.180(12) yes C1 . C2 . 1.383(4) yes C1 . H11 . 0.938 no C2 . C3 . 1.385(4) yes C2 . H222 . 0.928 no C3 . C4 . 1.378(4) yes C3 . H31 . 0.924 no C4 . C5 . 1.380(4) yes C4 . H41 . 0.922 no C5 . C6 . 1.467(4) yes C6 . C7 . 1.381(3) yes C7 . C8 . 1.395(3) yes C7 . H71 . 0.934 no C8 . C9 . 1.471(5) yes C9 . C10 6_656 1.394(4) yes C9 . C10 . 1.394(4) yes C10 . C11 . 1.380(4) yes C10 . H101 . 0.929 no C11 . H111 . 0.933 no C12 . C13 . 1.385(4) yes C12 . H121 . 0.930 no C13 . C14 . 1.387(4) yes C13 . H131 . 0.932 no C14 . C15 . 1.375(4) yes C14 . H141 . 0.937 no C15 . C16 . 1.384(4) yes C15 . H151 . 0.943 no C16 . C17 . 1.471(4) yes C17 . C18 . 1.384(4) yes C18 . C19 . 1.397(3) yes C18 . H181 . 0.928 no C19 . C20 . 1.473(5) yes C20 . C21 6_656 1.392(4) yes C20 . C21 . 1.392(4) yes C21 . C22 . 1.378(4) yes C21 . H211 . 0.930 no C22 . H221 . 0.932 no C23 . S1 . 1.615(4) yes C24 . S2 . 1.625(5) yes C25 . S3 . 1.618(3) yes C26 . C27 . 1.481(9) yes C26 . H261 . 0.950 no C26 . H262 . 0.950 no C26 . H263 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N4 6_656 Fe1 . N1 6_656 88.95(9) yes N4 6_656 Fe1 . N1 . 93.81(9) yes N1 6_656 Fe1 . N1 . 162.34(13) yes N4 6_656 Fe1 . N2 . 99.01(6) yes N1 6_656 Fe1 . N2 . 81.17(6) yes N1 . Fe1 . N2 . 81.17(6) yes N4 6_656 Fe1 . N4 . 161.97(13) yes N1 6_656 Fe1 . N4 . 93.81(9) yes N1 . Fe1 . N4 . 88.95(9) yes N2 . Fe1 . N4 . 99.01(6) yes N4 6_656 Fe1 . N5 . 80.99(6) yes N1 6_656 Fe1 . N5 . 98.83(6) yes N1 . Fe1 . N5 . 98.83(6) yes N2 . Fe1 . N5 . 179.994 yes N4 . Fe1 . N5 . 80.99(6) yes N8 2_666 Fe2 . N9 2_666 89.53(13) yes N8 2_666 Fe2 . N7 2_666 86.54(14) yes N9 2_666 Fe2 . N7 2_666 92.18(12) yes N8 2_666 Fe2 . N7 . 93.46(14) yes N9 2_666 Fe2 . N7 . 87.82(12) yes N7 2_666 Fe2 . N7 . 179.994 yes N8 2_666 Fe2 . N8 . 179.994 yes N9 2_666 Fe2 . N8 . 90.47(13) yes N7 2_666 Fe2 . N8 . 93.46(14) yes N7 . Fe2 . N8 . 86.54(14) yes N8 2_666 Fe2 . N9 . 90.47(13) yes N9 2_666 Fe2 . N9 . 179.994 yes N7 2_666 Fe2 . N9 . 87.82(12) yes N7 . Fe2 . N9 . 92.18(12) yes N8 . Fe2 . N9 . 89.53(13) yes Fe1 . N1 . C1 . 127.34(19) yes Fe1 . N1 . C5 . 114.62(17) yes C1 . N1 . C5 . 118.0(2) yes C6 6_656 N2 . Fe1 . 119.59(14) yes C6 6_656 N2 . C6 . 120.8(3) yes Fe1 . N2 . C6 . 119.59(14) yes C11 6_656 N3 . C11 . 118.5(4) yes Fe1 . N4 . C12 . 127.53(19) yes Fe1 . N4 . C16 . 114.49(17) yes C12 . N4 . C16 . 117.9(2) yes C17 6_656 N5 . Fe1 . 119.72(15) yes C17 6_656 N5 . C17 . 120.6(3) yes Fe1 . N5 . C17 . 119.72(15) yes C22 6_656 N6 . C22 . 121.6(4) yes C22 6_656 N6 . H1 . 119.2 no C22 . N6 . H1 . 119.2 no Fe2 . N7 . C23 . 151.3(3) yes Fe2 . N8 . C24 . 143.3(3) yes Fe2 . N9 . C25 . 173.0(3) yes N1 . C1 . C2 . 122.3(3) yes N1 . C1 . H11 . 118.3 no C2 . C1 . H11 . 119.4 no C1 . C2 . C3 . 119.4(3) yes C1 . C2 . H222 . 119.8 no C3 . C2 . H222 . 120.8 no C2 . C3 . C4 . 118.9(3) yes C2 . C3 . H31 . 120.3 no C4 . C3 . H31 . 120.8 no C3 . C4 . C5 . 119.6(3) yes C3 . C4 . H41 . 120.1 no C5 . C4 . H41 . 120.3 no C4 . C5 . N1 . 121.9(2) yes C4 . C5 . C6 . 125.1(2) yes N1 . C5 . C6 . 113.0(2) yes C5 . C6 . N2 . 111.6(2) yes C5 . C6 . C7 . 127.8(2) yes N2 . C6 . C7 . 120.6(2) yes C6 . C7 . C8 . 119.5(3) yes C6 . C7 . H71 . 119.9 no C8 . C7 . H71 . 120.6 no C7 . C8 . C7 6_656 118.9(3) yes C7 . C8 . C9 . 120.56(16) yes C7 6_656 C8 . C9 . 120.56(16) yes C8 . C9 . C10 6_656 121.35(18) yes C8 . C9 . C10 . 121.35(18) yes C10 6_656 C9 . C10 . 117.3(4) yes C9 . C10 . C11 . 119.2(3) yes C9 . C10 . H101 . 120.2 no C11 . C10 . H101 . 120.6 no C10 . C11 . N3 . 122.9(4) yes C10 . C11 . H111 . 119.2 no N3 . C11 . H111 . 117.9 no N4 . C12 . C13 . 122.9(3) yes N4 . C12 . H121 . 118.4 no C13 . C12 . H121 . 118.7 no C12 . C13 . C14 . 118.6(3) yes C12 . C13 . H131 . 119.6 no C14 . C13 . H131 . 121.9 no C13 . C14 . C15 . 119.5(3) yes C13 . C14 . H141 . 119.2 no C15 . C14 . H141 . 121.3 no C14 . C15 . C16 . 119.0(3) yes C14 . C15 . H151 . 121.5 no C16 . C15 . H151 . 119.5 no C15 . C16 . N4 . 122.1(2) yes C15 . C16 . C17 . 125.4(2) yes N4 . C16 . C17 . 112.6(2) yes C16 . C17 . N5 . 111.8(2) yes C16 . C17 . C18 . 127.1(2) yes N5 . C17 . C18 . 121.1(2) yes C17 . C18 . C19 . 119.1(3) yes C17 . C18 . H181 . 119.8 no C19 . C18 . H181 . 121.1 no C18 . C19 . C18 6_656 119.0(3) yes C18 . C19 . C20 . 120.48(16) yes C18 6_656 C19 . C20 . 120.48(16) yes C19 . C20 . C21 6_656 120.71(17) yes C19 . C20 . C21 . 120.71(17) yes C21 6_656 C20 . C21 . 118.6(3) yes C20 . C21 . C22 . 119.2(3) yes C20 . C21 . H211 . 120.3 no C22 . C21 . H211 . 120.5 no C21 . C22 . N6 . 120.7(3) yes C21 . C22 . H221 . 119.8 no N6 . C22 . H221 . 119.4 no N7 . C23 . S1 . 177.7(4) yes N8 . C24 . S2 . 178.2(4) yes N9 . C25 . S3 . 177.9(3) yes C27 . C26 . H261 . 110.0 no C27 . C26 . H262 . 108.2 no H261 . C26 . H262 . 109.5 no C27 . C26 . H263 . 110.2 no H261 . C26 . H263 . 109.5 no H262 . C26 . H263 . 109.5 no C26 . C27 . N10 . 167.7(13) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag N6 . H1 . N3 1_565 180 0.86 1.77 2.629(2) yes