_publ_section_synopsis . #Added by publCIF _publ_section_related_literature ; ? ; #Added by publCIF #============================================================================== _audit_creation_date '2012-08-03' _audit_creation_method SHELXL-97 _audit_update_record ; ? ; #============================================================================== # SUBMISSION DETAILS _publ_requested_journal '' _publ_requested_category ? _publ_contact_author_name '' _publ_contact_author_address ; Department of Chemistry, The University of Texas, One UTSA Circle, San Antonio, Texas 78249-0698, U.S.A. ; _publ_contact_letter ; ; _publ_requested_coeditor_name ' ' _publ_contact_author_phone ' ' _publ_contact_author_fax ' ' _publ_contact_author_email ; hadi.arman@utsa.edu ; #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_paper_category ? _journal_coeditor_notes ; ; _journal_techeditor_code ? _iucr_compatibility_tag ACTA95 _journal_techeditor_notes ; ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; ; _publ_section_title_footnote ; Additional correspondence e-mail: ; loop_ _publ_author_name _publ_author_address 'Arman, Hadi D.' ; Department of Chemistry The University of Texas at San Antonio One UTSA Circle San Antonio, Texas 78249-0698, USA ; #============================================================================== # TEXT _publ_section_abstract ; (type here to add abstract) ; _publ_section_exptl_refinement ; All H-atoms on the title compound were placed on calculated positions and were refined with U~iso~(H) =1.2-1.5U~eq~(C). The four worst reflections omitted, 2 8 2, 0 7 2, -4 6 2, 1 6 2. ; #============================================================================== _publ_section_exptl_prep ; (type here to add preparation details) ; #============================================================================== _publ_section_comment ; (type here to add) ; _publ_section_references ; Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Rigaku Americas Corporation (2008). CrystalClear. Rigaku/MSC Inc., The Woodlands, Texas, USA. Rueping, M., Kuenkel, A., Tato, F. & Bats, J. W. (2009). Angew. Chem. Int. Ed. 48, 3699--3702. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany. Westrip, S. P. (2010). publCIF. J. Appl. Cryst. 43. Submitted. ; _publ_section_acknowledgements ; (type here to add acknowledgements) ; _publ_section_figure_captions ; (type here to add) ; _publ_section_table_legends ; ; data_[Fe(STIPS)(TPP)] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C53 H49 Fe N4 S Si, 0.5(C6 H6)' _chemical_formula_sum 'C56 H52 Fe N4 S Si' _chemical_formula_weight 897.02 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' '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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P-1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.113(3) _cell_length_b 12.600(3) _cell_length_c 16.927(4) _cell_angle_alpha 80.693(11) _cell_angle_beta 85.049(12) _cell_angle_gamma 77.332(11) _cell_volume 2278.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 98(2) _cell_measurement_reflns_used 9159 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 40.2 _exptl_crystal_description 'chip' _exptl_crystal_colour 'purple' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.307 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 0.446 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.777 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 98(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Saturn724 (2x2 bin mode) ; _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% '<1' _diffrn_reflns_number 13515 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0762 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _reflns_number_total 8871 _reflns_number_gt 7565 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010) ; _computing_cell_refinement ; CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010) ; _computing_data_reduction ; CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'publCIF (Westrip, 2010)' _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^)+(0.0400P)^2^+3.6000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8871 _refine_ls_number_parameters 568 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1358 _refine_ls_wR_factor_gt 0.1288 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.008 _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 0.92143(4) 0.53111(3) 0.29465(2) 0.01496(12) Uani 1 1 d . . . S1 S 1.02957(7) 0.54507(6) 0.17479(5) 0.02055(18) Uani 1 1 d . . . Si1 Si 1.02219(8) 0.70952(7) 0.11313(5) 0.01924(19) Uani 1 1 d . . . N1 N 0.7367(2) 0.60458(19) 0.27785(15) 0.0159(5) Uani 1 1 d . . . N3 N 1.0599(2) 0.43903(19) 0.36852(15) 0.0161(5) Uani 1 1 d . . . N2 N 0.8753(2) 0.38282(19) 0.28560(14) 0.0153(5) Uani 1 1 d . . . N4 N 0.9253(2) 0.66140(19) 0.35581(14) 0.0158(5) Uani 1 1 d . . . C35 C 1.0163(3) 0.7889(2) 0.39832(18) 0.0191(6) Uani 1 1 d . . . H35A H 1.0742 0.8197 0.4180 0.023 Uiso 1 1 calc R . . C16 C 1.0607(3) 0.2531(2) 0.33897(17) 0.0173(6) Uani 1 1 d . . . C26 C 1.1390(3) 0.4807(2) 0.40815(18) 0.0170(6) Uani 1 1 d . . . C6 C 0.5635(3) 0.4226(2) 0.19431(18) 0.0180(6) Uani 1 1 d . . . C28 C 1.2345(3) 0.6220(2) 0.44943(18) 0.0169(6) Uani 1 1 d . . . C4 C 0.6525(3) 0.5611(2) 0.24407(17) 0.0160(6) Uani 1 1 d . . . C1 C 0.6800(3) 0.7132(2) 0.28211(17) 0.0169(6) Uani 1 1 d . . . C14 C 0.8978(3) 0.2014(2) 0.26706(18) 0.0192(6) Uani 1 1 d . . . H14A H 0.9316 0.1269 0.2676 0.023 Uiso 1 1 calc R . . C5 C 0.6694(3) 0.4523(2) 0.22930(17) 0.0161(6) Uani 1 1 d . . . C12 C 0.7739(3) 0.3698(2) 0.24840(17) 0.0168(6) Uani 1 1 d . . . C15 C 0.9514(3) 0.2792(2) 0.29783(17) 0.0167(6) Uani 1 1 d . . . C33 C 1.2161(3) 0.6670(2) 0.52100(17) 0.0190(6) Uani 1 1 d . . . H33A H 1.1384 0.6773 0.5474 0.023 Uiso 1 1 calc R . . C27 C 1.1296(3) 0.5915(2) 0.41396(17) 0.0161(6) Uani 1 1 d . . . C23 C 1.1078(3) 0.3274(2) 0.37410(17) 0.0158(6) Uani 1 1 d . . . C34 C 1.0286(3) 0.6755(2) 0.39006(18) 0.0181(6) Uani 1 1 d . . . C37 C 0.8465(3) 0.7636(2) 0.34634(17) 0.0169(6) Uani 1 1 d . . . C17 C 1.1333(3) 0.1370(2) 0.34807(19) 0.0197(6) Uani 1 1 d . . . C2 C 0.5600(3) 0.7371(2) 0.24936(18) 0.0195(6) Uani 1 1 d . . . H2A H 0.5040 0.8042 0.2454 0.023 Uiso 1 1 calc R . . C39 C 0.6564(3) 0.9029(2) 0.31615(19) 0.0191(6) Uani 1 1 d . . . C11 C 0.4588(3) 0.4083(2) 0.24293(19) 0.0208(6) Uani 1 1 d . . . H11A H 0.4573 0.4128 0.2973 0.025 Uiso 1 1 calc R . . C13 C 0.7891(3) 0.2567(2) 0.23722(18) 0.0192(6) Uani 1 1 d . . . H13A H 0.7340 0.2271 0.2137 0.023 Uiso 1 1 calc R . . C38 C 0.7303(3) 0.7881(2) 0.31408(18) 0.0177(6) Uani 1 1 d . . . C36 C 0.9037(3) 0.8428(2) 0.37194(18) 0.0202(6) Uani 1 1 d . . . H36A H 0.8701 0.9174 0.3707 0.024 Uiso 1 1 calc R . . C32 C 1.3135(3) 0.6962(2) 0.55279(18) 0.0204(6) Uani 1 1 d . . . H32A H 1.3005 0.7271 0.5999 0.024 Uiso 1 1 calc R . . C3 C 0.5438(3) 0.6443(2) 0.22549(18) 0.0200(6) Uani 1 1 d . . . H3A H 0.4749 0.6359 0.2015 0.024 Uiso 1 1 calc R . . C24 C 1.2167(3) 0.2988(2) 0.42018(19) 0.0197(6) Uani 1 1 d . . . H24A H 1.2652 0.2287 0.4329 0.024 Uiso 1 1 calc R . . C25 C 1.2352(3) 0.3927(2) 0.44152(19) 0.0201(6) Uani 1 1 d . . . H25A H 1.2983 0.3992 0.4720 0.024 Uiso 1 1 calc R . . C29 C 1.3519(3) 0.6059(2) 0.41136(18) 0.0189(6) Uani 1 1 d . . . H29A H 1.3651 0.5763 0.3637 0.023 Uiso 1 1 calc R . . C51 C 1.1330(3) 0.6903(3) 0.02253(19) 0.0248(7) Uani 1 1 d . . . H51A H 1.2091 0.6417 0.0426 0.030 Uiso 1 1 calc R . . C30 C 1.4498(3) 0.6336(2) 0.44382(18) 0.0207(6) Uani 1 1 d . . . H30A H 1.5282 0.6215 0.4184 0.025 Uiso 1 1 calc R . . C10 C 0.3560(3) 0.3872(3) 0.2111(2) 0.0262(7) Uani 1 1 d . . . H10A H 0.2863 0.3783 0.2439 0.031 Uiso 1 1 calc R . . C48 C 0.8574(3) 0.7755(3) 0.0891(2) 0.0269(7) Uani 1 1 d . . . H48A H 0.8158 0.7984 0.1389 0.032 Uiso 1 1 calc R . . C40 C 0.6191(3) 0.9388(2) 0.3902(2) 0.0233(7) Uani 1 1 d . . . H40A H 0.6371 0.8903 0.4373 0.028 Uiso 1 1 calc R . . C31 C 1.4299(3) 0.6793(2) 0.51438(19) 0.0212(7) Uani 1 1 d . . . H31A H 1.4948 0.6987 0.5359 0.025 Uiso 1 1 calc R . . C45 C 1.0792(3) 0.7869(3) 0.18410(19) 0.0237(7) Uani 1 1 d . . . H45A H 1.0348 0.7700 0.2356 0.028 Uiso 1 1 calc R . . C44 C 0.6270(3) 0.9768(2) 0.2464(2) 0.0226(7) Uani 1 1 d . . . H44A H 0.6509 0.9544 0.1966 0.027 Uiso 1 1 calc R . . C7 C 0.5651(3) 0.4143(3) 0.1131(2) 0.0259(7) Uani 1 1 d . . . H7A H 0.6343 0.4233 0.0799 0.031 Uiso 1 1 calc R . . C18 C 1.2030(3) 0.0941(3) 0.2839(2) 0.0255(7) Uani 1 1 d . . . H18A H 1.1996 0.1356 0.2332 0.031 Uiso 1 1 calc R . . C43 C 0.5622(3) 1.0839(3) 0.2506(2) 0.0267(7) Uani 1 1 d . . . H43A H 0.5423 1.1325 0.2038 0.032 Uiso 1 1 calc R . . C22 C 1.1385(3) 0.0717(3) 0.4232(2) 0.0261(7) Uani 1 1 d . . . H22A H 1.0907 0.0983 0.4664 0.031 Uiso 1 1 calc R . . C9 C 0.3587(3) 0.3796(3) 0.1304(2) 0.0293(8) Uani 1 1 d . . . H9A H 0.2905 0.3658 0.1088 0.035 Uiso 1 1 calc R . . C42 C 0.5272(3) 1.1182(3) 0.3251(2) 0.0283(8) Uani 1 1 d . . . H42A H 0.4845 1.1899 0.3280 0.034 Uiso 1 1 calc R . . C8 C 0.4625(3) 0.3924(3) 0.0819(2) 0.0309(8) Uani 1 1 d . . . H8A H 0.4640 0.3865 0.0277 0.037 Uiso 1 1 calc R . . C41 C 0.5557(3) 1.0460(3) 0.3942(2) 0.0290(8) Uani 1 1 d . . . H41A H 0.5325 1.0690 0.4439 0.035 Uiso 1 1 calc R . . C46 C 1.2167(3) 0.7404(3) 0.1998(2) 0.0309(8) Uani 1 1 d . . . H46A H 1.2428 0.7809 0.2361 0.046 Uiso 1 1 calc R . . H46B H 1.2651 0.7470 0.1501 0.046 Uiso 1 1 calc R . . H46C H 1.2278 0.6643 0.2228 0.046 Uiso 1 1 calc R . . C21 C 1.2142(3) -0.0327(3) 0.4341(2) 0.0320(8) Uani 1 1 d . . . H21A H 1.2177 -0.0749 0.4846 0.038 Uiso 1 1 calc R . . C19 C 1.2776(3) -0.0103(3) 0.2953(2) 0.0340(9) Uani 1 1 d . . . H19A H 1.3241 -0.0380 0.2520 0.041 Uiso 1 1 calc R . . C52 C 1.1700(4) 0.7968(3) -0.0208(2) 0.0329(8) Uani 1 1 d . . . H52A H 1.2260 0.7804 -0.0658 0.049 Uiso 1 1 calc R . . H52B H 1.2095 0.8276 0.0156 0.049 Uiso 1 1 calc R . . H52C H 1.0975 0.8488 -0.0393 0.049 Uiso 1 1 calc R . . C49 C 0.7839(3) 0.6975(3) 0.0631(2) 0.0326(8) Uani 1 1 d . . . H49A H 0.7014 0.7368 0.0522 0.049 Uiso 1 1 calc R . . H49B H 0.7810 0.6371 0.1054 0.049 Uiso 1 1 calc R . . H49C H 0.8236 0.6699 0.0157 0.049 Uiso 1 1 calc R . . C47 C 1.0515(4) 0.9131(3) 0.1656(2) 0.0346(8) Uani 1 1 d . . . H47A H 1.0841 0.9424 0.2061 0.052 Uiso 1 1 calc R . . H47B H 0.9638 0.9403 0.1650 0.052 Uiso 1 1 calc R . . H47C H 1.0892 0.9354 0.1142 0.052 Uiso 1 1 calc R . . C20 C 1.2841(3) -0.0737(3) 0.3699(3) 0.0350(9) Uani 1 1 d . . . H20A H 1.3350 -0.1434 0.3770 0.042 Uiso 1 1 calc R . . C53 C 1.0855(4) 0.6302(3) -0.0368(2) 0.0350(9) Uani 1 1 d . . . H53A H 1.1438 0.6220 -0.0818 0.052 Uiso 1 1 calc R . . H53B H 1.0073 0.6722 -0.0551 0.052 Uiso 1 1 calc R . . H53C H 1.0757 0.5589 -0.0105 0.052 Uiso 1 1 calc R . . C50 C 0.8454(4) 0.8807(3) 0.0266(3) 0.0422(10) Uani 1 1 d . . . H50A H 0.7597 0.9104 0.0172 0.063 Uiso 1 1 calc R . . H50B H 0.8888 0.8631 -0.0227 0.063 Uiso 1 1 calc R . . H50C H 0.8800 0.9340 0.0465 0.063 Uiso 1 1 calc R . . C55 C 0.5097(6) 0.0992(4) 0.0160(5) 0.081(2) Uani 1 1 d D . . H55A H 0.5165 0.1674 0.0274 0.097 Uiso 1 1 calc R . . C54 C 0.4534(5) 0.0325(7) 0.0703(4) 0.089(2) Uani 1 1 d D . . H54A H 0.4209 0.0553 0.1187 0.107 Uiso 1 1 calc R . . C56 C 0.5561(5) 0.0671(6) -0.0546(4) 0.082(2) Uani 1 1 d D . . H56A H 0.5943 0.1131 -0.0923 0.098 Uiso 1 1 calc 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 0.0139(2) 0.0133(2) 0.0191(2) -0.00362(16) -0.00339(16) -0.00414(16) S1 0.0229(4) 0.0182(4) 0.0208(4) -0.0032(3) 0.0017(3) -0.0056(3) Si1 0.0200(4) 0.0177(4) 0.0211(4) -0.0025(3) -0.0018(3) -0.0061(3) N1 0.0137(12) 0.0154(12) 0.0194(13) -0.0028(10) -0.0027(10) -0.0041(9) N3 0.0157(12) 0.0130(11) 0.0204(13) -0.0024(10) -0.0006(10) -0.0049(9) N2 0.0141(12) 0.0141(12) 0.0189(13) -0.0048(10) -0.0023(10) -0.0032(9) N4 0.0152(12) 0.0143(12) 0.0189(13) -0.0047(10) -0.0029(10) -0.0028(9) C35 0.0191(15) 0.0173(14) 0.0233(16) -0.0064(12) -0.0030(12) -0.0059(12) C16 0.0160(15) 0.0173(14) 0.0183(15) -0.0011(12) -0.0008(12) -0.0042(11) C26 0.0154(15) 0.0187(14) 0.0191(15) -0.0059(12) -0.0005(11) -0.0064(11) C6 0.0195(15) 0.0129(13) 0.0227(16) -0.0019(12) -0.0057(12) -0.0040(11) C28 0.0176(15) 0.0138(13) 0.0199(15) -0.0013(12) -0.0051(12) -0.0039(11) C4 0.0156(15) 0.0177(14) 0.0166(14) -0.0036(12) -0.0001(11) -0.0071(11) C1 0.0161(15) 0.0148(14) 0.0194(15) -0.0016(12) -0.0009(12) -0.0032(11) C14 0.0208(16) 0.0138(14) 0.0244(16) -0.0051(12) -0.0018(12) -0.0049(12) C5 0.0179(15) 0.0188(14) 0.0137(14) -0.0048(11) 0.0002(11) -0.0066(12) C12 0.0169(15) 0.0201(15) 0.0157(14) -0.0036(12) -0.0023(11) -0.0074(12) C15 0.0184(15) 0.0157(14) 0.0165(14) -0.0017(12) 0.0007(12) -0.0056(11) C33 0.0173(15) 0.0248(16) 0.0170(15) -0.0053(12) -0.0016(12) -0.0072(12) C27 0.0147(14) 0.0175(14) 0.0178(15) -0.0049(12) 0.0010(11) -0.0059(11) C23 0.0136(14) 0.0172(14) 0.0178(15) -0.0031(12) -0.0017(11) -0.0053(11) C34 0.0166(15) 0.0204(15) 0.0196(15) -0.0060(12) -0.0025(12) -0.0056(12) C37 0.0184(15) 0.0152(14) 0.0164(14) -0.0013(11) -0.0015(11) -0.0030(11) C17 0.0167(15) 0.0155(14) 0.0297(17) -0.0069(13) -0.0069(13) -0.0046(12) C2 0.0160(15) 0.0168(14) 0.0258(16) -0.0026(12) -0.0024(12) -0.0033(12) C39 0.0139(15) 0.0163(14) 0.0291(17) -0.0047(13) -0.0037(12) -0.0056(11) C11 0.0195(16) 0.0211(15) 0.0241(16) -0.0061(13) -0.0038(13) -0.0058(12) C13 0.0200(15) 0.0195(15) 0.0201(15) -0.0053(12) -0.0022(12) -0.0060(12) C38 0.0172(15) 0.0150(14) 0.0202(15) -0.0018(12) -0.0012(12) -0.0026(11) C36 0.0196(16) 0.0169(14) 0.0251(16) -0.0058(12) -0.0023(13) -0.0031(12) C32 0.0246(17) 0.0205(15) 0.0190(15) -0.0057(12) -0.0059(12) -0.0071(12) C3 0.0161(15) 0.0218(15) 0.0232(16) -0.0043(13) -0.0044(12) -0.0045(12) C24 0.0174(15) 0.0162(14) 0.0254(16) -0.0005(12) -0.0063(12) -0.0030(12) C25 0.0183(15) 0.0191(15) 0.0246(16) -0.0036(12) -0.0071(12) -0.0052(12) C29 0.0196(16) 0.0179(14) 0.0206(15) -0.0046(12) -0.0013(12) -0.0055(12) C51 0.0283(18) 0.0246(16) 0.0233(17) -0.0047(13) 0.0019(13) -0.0098(13) C30 0.0157(15) 0.0233(15) 0.0228(16) -0.0021(13) -0.0003(12) -0.0042(12) C10 0.0180(16) 0.0248(16) 0.039(2) -0.0047(14) -0.0049(14) -0.0097(13) C48 0.0256(18) 0.0265(17) 0.0280(18) -0.0025(14) -0.0043(14) -0.0038(14) C40 0.0225(17) 0.0183(15) 0.0288(17) -0.0036(13) -0.0025(13) -0.0031(12) C31 0.0199(16) 0.0210(15) 0.0251(17) -0.0023(13) -0.0079(13) -0.0078(12) C45 0.0277(18) 0.0253(16) 0.0205(16) -0.0035(13) -0.0014(13) -0.0109(13) C44 0.0198(16) 0.0212(15) 0.0291(17) -0.0047(13) -0.0059(13) -0.0065(13) C7 0.0262(18) 0.0313(18) 0.0238(17) -0.0068(14) -0.0028(13) -0.0111(14) C18 0.0219(17) 0.0227(16) 0.0337(19) -0.0083(14) -0.0004(14) -0.0058(13) C43 0.0234(17) 0.0178(15) 0.039(2) 0.0009(14) -0.0091(15) -0.0057(13) C22 0.0315(19) 0.0198(16) 0.0295(18) -0.0040(14) -0.0076(14) -0.0081(14) C9 0.0265(18) 0.0282(17) 0.039(2) -0.0052(15) -0.0161(15) -0.0122(14) C42 0.0223(17) 0.0158(15) 0.048(2) -0.0084(15) -0.0015(15) -0.0044(13) C8 0.038(2) 0.0359(19) 0.0234(17) -0.0084(15) -0.0109(15) -0.0108(16) C41 0.0278(18) 0.0245(17) 0.037(2) -0.0126(15) 0.0020(15) -0.0050(14) C46 0.0303(19) 0.0307(18) 0.037(2) -0.0056(15) -0.0098(15) -0.0139(15) C21 0.038(2) 0.0192(16) 0.042(2) 0.0002(15) -0.0195(17) -0.0105(15) C19 0.0230(18) 0.0241(17) 0.056(2) -0.0169(17) 0.0014(16) -0.0016(14) C52 0.041(2) 0.038(2) 0.0242(18) -0.0038(15) 0.0017(15) -0.0202(17) C49 0.0254(18) 0.041(2) 0.0323(19) 0.0025(16) -0.0069(15) -0.0117(15) C47 0.041(2) 0.0282(18) 0.037(2) -0.0088(16) -0.0060(17) -0.0099(16) C20 0.0253(19) 0.0158(16) 0.067(3) -0.0098(17) -0.0153(18) -0.0027(14) C53 0.039(2) 0.043(2) 0.031(2) -0.0140(17) 0.0075(16) -0.0246(17) C50 0.042(2) 0.031(2) 0.052(3) 0.0086(18) -0.0210(19) -0.0094(17) C55 0.072(4) 0.040(3) 0.139(6) -0.020(3) -0.064(4) -0.005(3) C54 0.049(3) 0.161(7) 0.073(4) -0.055(5) -0.017(3) -0.022(4) C56 0.069(4) 0.109(5) 0.073(4) 0.043(4) -0.042(3) -0.056(4) _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 2.074(2) . ? Fe1 N1 2.082(2) . ? Fe1 N4 2.087(2) . ? Fe1 N3 2.088(2) . ? Fe1 S1 2.2688(10) . ? S1 Si1 2.1518(12) . ? Si1 C48 1.887(3) . ? Si1 C45 1.891(3) . ? Si1 C51 1.895(3) . ? N1 C1 1.386(4) . ? N1 C4 1.387(4) . ? N3 C23 1.382(4) . ? N3 C26 1.384(4) . ? N2 C15 1.386(4) . ? N2 C12 1.390(4) . ? N4 C37 1.383(4) . ? N4 C34 1.387(4) . ? C35 C36 1.361(4) . ? C35 C34 1.433(4) . ? C35 H35A 0.9300 . ? C16 C23 1.397(4) . ? C16 C15 1.401(4) . ? C16 C17 1.499(4) . ? C26 C27 1.396(4) . ? C26 C25 1.440(4) . ? C6 C7 1.393(4) . ? C6 C11 1.394(4) . ? C6 C5 1.504(4) . ? C28 C29 1.394(4) . ? C28 C33 1.399(4) . ? C28 C27 1.503(4) . ? C4 C5 1.401(4) . ? C4 C3 1.436(4) . ? C1 C38 1.394(4) . ? C1 C2 1.440(4) . ? C14 C13 1.350(4) . ? C14 C15 1.436(4) . ? C14 H14A 0.9300 . ? C5 C12 1.401(4) . ? C12 C13 1.438(4) . ? C33 C32 1.392(4) . ? C33 H33A 0.9300 . ? C27 C34 1.401(4) . ? C23 C24 1.444(4) . ? C37 C38 1.398(4) . ? C37 C36 1.433(4) . ? C17 C18 1.390(4) . ? C17 C22 1.397(4) . ? C2 C3 1.349(4) . ? C2 H2A 0.9300 . ? C39 C44 1.395(4) . ? C39 C40 1.400(4) . ? C39 C38 1.502(4) . ? C11 C10 1.397(4) . ? C11 H11A 0.9300 . ? C13 H13A 0.9300 . ? C36 H36A 0.9300 . ? C32 C31 1.385(4) . ? C32 H32A 0.9300 . ? C3 H3A 0.9300 . ? C24 C25 1.354(4) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C29 C30 1.392(4) . ? C29 H29A 0.9300 . ? C51 C53 1.541(5) . ? C51 C52 1.543(5) . ? C51 H51A 0.9800 . ? C30 C31 1.389(4) . ? C30 H30A 0.9300 . ? C10 C9 1.381(5) . ? C10 H10A 0.9300 . ? C48 C49 1.542(5) . ? C48 C50 1.545(5) . ? C48 H48A 0.9800 . ? C40 C41 1.389(4) . ? C40 H40A 0.9300 . ? C31 H31A 0.9300 . ? C45 C47 1.537(4) . ? C45 C46 1.541(5) . ? C45 H45A 0.9800 . ? C44 C43 1.393(4) . ? C44 H44A 0.9300 . ? C7 C8 1.394(5) . ? C7 H7A 0.9300 . ? C18 C19 1.386(4) . ? C18 H18A 0.9300 . ? C43 C42 1.394(5) . ? C43 H43A 0.9300 . ? C22 C21 1.391(4) . ? C22 H22A 0.9300 . ? C9 C8 1.382(5) . ? C9 H9A 0.9300 . ? C42 C41 1.376(5) . ? C42 H42A 0.9300 . ? C8 H8A 0.9300 . ? C41 H41A 0.9300 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C21 C20 1.382(5) . ? C21 H21A 0.9300 . ? C19 C20 1.379(5) . ? C19 H19A 0.9300 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C20 H20A 0.9300 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C55 C56 1.348(8) . ? C55 C54 1.350(8) . ? C55 H55A 0.9300 . ? C54 C56 1.351(9) 2_655 ? C54 H54A 0.9300 . ? C56 C54 1.351(9) 2_655 ? C56 H56A 0.9300 . ? 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 N1 87.28(9) . . ? N2 Fe1 N4 152.77(10) . . ? N1 Fe1 N4 86.03(9) . . ? N2 Fe1 N3 86.51(9) . . ? N1 Fe1 N3 150.24(10) . . ? N4 Fe1 N3 86.32(9) . . ? N2 Fe1 S1 95.65(7) . . ? N1 Fe1 S1 109.09(7) . . ? N4 Fe1 S1 111.48(7) . . ? N3 Fe1 S1 100.48(7) . . ? Si1 S1 Fe1 115.78(4) . . ? C48 Si1 C45 110.16(15) . . ? C48 Si1 C51 114.82(15) . . ? C45 Si1 C51 111.51(15) . . ? C48 Si1 S1 109.29(11) . . ? C45 Si1 S1 106.52(11) . . ? C51 Si1 S1 104.04(11) . . ? C1 N1 C4 105.5(2) . . ? C1 N1 Fe1 127.2(2) . . ? C4 N1 Fe1 126.01(19) . . ? C23 N3 C26 105.9(2) . . ? C23 N3 Fe1 126.78(19) . . ? C26 N3 Fe1 126.05(19) . . ? C15 N2 C12 105.5(2) . . ? C15 N2 Fe1 126.9(2) . . ? C12 N2 Fe1 126.10(19) . . ? C37 N4 C34 105.9(2) . . ? C37 N4 Fe1 126.08(19) . . ? C34 N4 Fe1 124.63(19) . . ? C36 C35 C34 107.0(3) . . ? C36 C35 H35A 126.5 . . ? C34 C35 H35A 126.5 . . ? C23 C16 C15 124.9(3) . . ? C23 C16 C17 116.3(3) . . ? C15 C16 C17 118.8(3) . . ? N3 C26 C27 125.6(3) . . ? N3 C26 C25 109.9(2) . . ? C27 C26 C25 124.4(3) . . ? C7 C6 C11 119.0(3) . . ? C7 C6 C5 121.3(3) . . ? C11 C6 C5 119.6(3) . . ? C29 C28 C33 118.9(3) . . ? C29 C28 C27 120.3(3) . . ? C33 C28 C27 120.8(3) . . ? N1 C4 C5 125.8(3) . . ? N1 C4 C3 110.0(2) . . ? C5 C4 C3 124.2(3) . . ? N1 C1 C38 125.5(3) . . ? N1 C1 C2 109.7(3) . . ? C38 C1 C2 124.8(3) . . ? C13 C14 C15 107.1(3) . . ? C13 C14 H14A 126.5 . . ? C15 C14 H14A 126.5 . . ? C12 C5 C4 124.8(3) . . ? C12 C5 C6 118.6(3) . . ? C4 C5 C6 116.5(3) . . ? N2 C12 C5 125.3(3) . . ? N2 C12 C13 109.5(2) . . ? C5 C12 C13 125.1(3) . . ? N2 C15 C16 124.7(3) . . ? N2 C15 C14 110.1(3) . . ? C16 C15 C14 125.0(3) . . ? C32 C33 C28 120.3(3) . . ? C32 C33 H33A 119.8 . . ? C28 C33 H33A 119.8 . . ? C26 C27 C34 124.5(3) . . ? C26 C27 C28 117.5(3) . . ? C34 C27 C28 118.0(3) . . ? N3 C23 C16 125.6(3) . . ? N3 C23 C24 109.7(2) . . ? C16 C23 C24 124.7(3) . . ? N4 C34 C27 125.2(3) . . ? N4 C34 C35 109.9(3) . . ? C27 C34 C35 124.9(3) . . ? N4 C37 C38 125.8(3) . . ? N4 C37 C36 109.7(3) . . ? C38 C37 C36 124.5(3) . . ? C18 C17 C22 118.4(3) . . ? C18 C17 C16 121.3(3) . . ? C22 C17 C16 120.1(3) . . ? C3 C2 C1 107.5(3) . . ? C3 C2 H2A 126.3 . . ? C1 C2 H2A 126.3 . . ? C44 C39 C40 118.5(3) . . ? C44 C39 C38 122.1(3) . . ? C40 C39 C38 119.4(3) . . ? C6 C11 C10 120.9(3) . . ? C6 C11 H11A 119.6 . . ? C10 C11 H11A 119.6 . . ? C14 C13 C12 107.7(3) . . ? C14 C13 H13A 126.1 . . ? C12 C13 H13A 126.1 . . ? C1 C38 C37 124.3(3) . . ? C1 C38 C39 119.4(3) . . ? C37 C38 C39 116.3(3) . . ? C35 C36 C37 107.5(3) . . ? C35 C36 H36A 126.2 . . ? C37 C36 H36A 126.2 . . ? C31 C32 C33 120.1(3) . . ? C31 C32 H32A 119.9 . . ? C33 C32 H32A 119.9 . . ? C2 C3 C4 107.3(3) . . ? C2 C3 H3A 126.4 . . ? C4 C3 H3A 126.4 . . ? C25 C24 C23 107.3(2) . . ? C25 C24 H24A 126.3 . . ? C23 C24 H24A 126.3 . . ? C24 C25 C26 107.1(3) . . ? C24 C25 H25A 126.5 . . ? C26 C25 H25A 126.5 . . ? C30 C29 C28 120.8(3) . . ? C30 C29 H29A 119.6 . . ? C28 C29 H29A 119.6 . . ? C53 C51 C52 111.0(3) . . ? C53 C51 Si1 111.9(2) . . ? C52 C51 Si1 114.5(2) . . ? C53 C51 H51A 106.3 . . ? C52 C51 H51A 106.3 . . ? Si1 C51 H51A 106.3 . . ? C31 C30 C29 119.7(3) . . ? C31 C30 H30A 120.2 . . ? C29 C30 H30A 120.2 . . ? C9 C10 C11 119.5(3) . . ? C9 C10 H10A 120.2 . . ? C11 C10 H10A 120.2 . . ? C49 C48 C50 109.2(3) . . ? C49 C48 Si1 114.5(2) . . ? C50 C48 Si1 113.5(3) . . ? C49 C48 H48A 106.3 . . ? C50 C48 H48A 106.3 . . ? Si1 C48 H48A 106.3 . . ? C41 C40 C39 120.8(3) . . ? C41 C40 H40A 119.6 . . ? C39 C40 H40A 119.6 . . ? C32 C31 C30 120.2(3) . . ? C32 C31 H31A 119.9 . . ? C30 C31 H31A 119.9 . . ? C47 C45 C46 111.4(3) . . ? C47 C45 Si1 117.6(2) . . ? C46 C45 Si1 111.4(2) . . ? C47 C45 H45A 105.1 . . ? C46 C45 H45A 105.1 . . ? Si1 C45 H45A 105.1 . . ? C43 C44 C39 120.6(3) . . ? C43 C44 H44A 119.7 . . ? C39 C44 H44A 119.7 . . ? C6 C7 C8 119.8(3) . . ? C6 C7 H7A 120.1 . . ? C8 C7 H7A 120.1 . . ? C19 C18 C17 120.3(3) . . ? C19 C18 H18A 119.8 . . ? C17 C18 H18A 119.8 . . ? C44 C43 C42 120.0(3) . . ? C44 C43 H43A 120.0 . . ? C42 C43 H43A 120.0 . . ? C21 C22 C17 120.8(3) . . ? C21 C22 H22A 119.6 . . ? C17 C22 H22A 119.6 . . ? C10 C9 C8 120.1(3) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C41 C42 C43 119.9(3) . . ? C41 C42 H42A 120.0 . . ? C43 C42 H42A 120.0 . . ? C9 C8 C7 120.7(3) . . ? C9 C8 H8A 119.6 . . ? C7 C8 H8A 119.6 . . ? C42 C41 C40 120.2(3) . . ? C42 C41 H41A 119.9 . . ? C40 C41 H41A 119.9 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C20 C21 C22 120.0(3) . . ? C20 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? C20 C19 C18 121.0(3) . . ? C20 C19 H19A 119.5 . . ? C18 C19 H19A 119.5 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C19 C20 C21 119.3(3) . . ? C19 C20 H20A 120.3 . . ? C21 C20 H20A 120.3 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C56 C55 C54 120.1(5) . . ? C56 C55 H55A 120.0 . . ? C54 C55 H55A 120.0 . . ? C55 C54 C56 120.4(6) . 2_655 ? C55 C54 H54A 119.8 . . ? C56 C54 H54A 119.8 2_655 . ? C55 C56 C54 119.5(5) . 2_655 ? C55 C56 H56A 120.3 . . ? C54 C56 H56A 120.3 2_655 . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.604 _refine_diff_density_min -0.627 _refine_diff_density_rms 0.079 #===END _publ_section_synopsis . #Added by publCIF _publ_section_related_literature ; ? ; #Added by publCIF #============================================================================== _audit_creation_date '2012-09-27' _audit_creation_method SHELXL-97 _audit_update_record ; ? ; #============================================================================== # SUBMISSION DETAILS _publ_requested_journal '' _publ_requested_category ? _publ_contact_author_name '' _publ_contact_author_address ; Department of Chemistry, The University of Texas, One UTSA Circle, San Antonio, Texas 78249-0698, U.S.A. ; _publ_contact_letter ; ; _publ_requested_coeditor_name ' ' _publ_contact_author_phone ' ' _publ_contact_author_fax ' ' _publ_contact_author_email ; hadi.arman@utsa.edu ; #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_paper_category ? _journal_coeditor_notes ; ; _journal_techeditor_code ? _iucr_compatibility_tag ACTA95 _journal_techeditor_notes ; ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; ; _publ_section_title_footnote ; Additional correspondence e-mail: ; loop_ _publ_author_name _publ_author_address 'Arman, Hadi D.' ; Department of Chemistry The University of Texas at San Antonio One UTSA Circle San Antonio, Texas 78249-0698, USA ; #============================================================================== # TEXT _publ_section_abstract ; (type here to add abstract) ; _publ_section_exptl_refinement ; All H-atoms on the title compound and solvent molecule were placed on calculated positions and were refined with U~iso~(H) =1.2-1.5 U~eq~(C). ; #============================================================================== _publ_section_exptl_prep ; (type here to add preparation details) ; #============================================================================== _publ_section_comment ; (type here to add) ; _publ_section_references ; Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Rigaku Americas Corporation (2008). CrystalClear. Rigaku/MSC Inc., The Woodlands, Texas, USA. Rueping, M., Kuenkel, A., Tato, F. & Bats, J. W. (2009). Angew. Chem. Int. Ed. 48, 3699--3702. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany. Westrip, S. P. (2010). publCIF. J. Appl. Cryst. 43. Submitted. ; _publ_section_acknowledgements ; (type here to add acknowledgements) ; _publ_section_figure_captions ; (type here to add) ; _publ_section_table_legends ; ; data_[Fe(STIPS)(TMP)] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C65 H73 Fe N4 S Si), C3 H5' _chemical_formula_sum 'C133 H151 Fe2 N8 S2 Si2' _chemical_formula_weight 2093.62 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' 'Si' 'Si' 0.0817 0.0704 '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' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P-1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.4086(5) _cell_length_b 14.4072(7) _cell_length_c 17.3566(12) _cell_angle_alpha 110.724(8) _cell_angle_beta 102.571(7) _cell_angle_gamma 95.034(7) _cell_volume 3010.6(3) _cell_formula_units_Z 1 _cell_measurement_temperature 98(2) _cell_measurement_reflns_used 18835 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.6 _exptl_crystal_description 'plaetlet' _exptl_crystal_colour 'purple' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1117 _exptl_absorpt_coefficient_mu 0.347 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.467 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 98(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Saturn724 (2x2 bin mode) ; _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% '<1' _diffrn_reflns_number 17753 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_reduction_process 'Lp corrections applied' _reflns_number_total 10578 _reflns_number_gt 9592 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010) ; _computing_cell_refinement ; CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010) ; _computing_data_reduction ; CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'publCIF (Westrip, 2010)' _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^)+(0.0300P)^2^+10.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10578 _refine_ls_number_parameters 676 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1471 _refine_ls_wR_factor_gt 0.1447 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _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 0.69888(3) 0.28769(3) 0.20394(2) 0.01316(12) Uani 1 1 d . . . S1 S 0.67562(6) 0.43016(6) 0.30435(5) 0.02502(19) Uani 1 1 d . . . Si1 Si 0.66910(6) 0.56843(6) 0.28576(5) 0.01974(19) Uani 1 1 d . . . N4 N 0.82690(17) 0.31392(18) 0.16000(15) 0.0156(5) Uani 1 1 d . . . N3 N 0.79779(17) 0.24071(17) 0.28738(15) 0.0150(5) Uani 1 1 d . . . N2 N 0.58114(17) 0.18650(17) 0.20763(15) 0.0144(5) Uani 1 1 d . . . N1 N 0.61065(18) 0.26156(18) 0.08150(15) 0.0154(5) Uani 1 1 d . . . C5 C 0.4418(2) 0.1870(2) 0.08902(18) 0.0158(6) Uani 1 1 d . . . C32 C 0.9043(2) 0.2705(2) 0.31686(18) 0.0168(6) Uani 1 1 d . . . C33 C 0.9667(2) 0.3137(2) 0.27962(18) 0.0168(6) Uani 1 1 d . . . C46 C 0.8288(2) 0.3328(2) 0.08809(18) 0.0173(6) Uani 1 1 d . . . C18 C 0.5822(2) 0.1487(2) 0.27003(18) 0.0160(6) Uani 1 1 d . . . C34 C 1.0828(2) 0.3323(2) 0.31398(18) 0.0172(6) Uani 1 1 d . . . C19 C 0.6697(2) 0.1544(2) 0.33346(18) 0.0167(6) Uani 1 1 d . . . C30 C 0.8605(2) 0.2015(2) 0.40425(19) 0.0206(6) Uani 1 1 d . . . H30A H 0.8622 0.1774 0.4476 0.025 Uiso 1 1 calc R . . C48 C 0.7621(2) 0.3311(2) -0.05747(19) 0.0192(6) Uani 1 1 d . . . C25 C 0.6458(2) 0.1697(2) 0.4765(2) 0.0232(7) Uani 1 1 d . . . C4 C 0.6408(2) 0.2879(2) 0.02002(18) 0.0175(6) Uani 1 1 d . . . C8 C 0.1618(2) 0.2175(2) 0.0418(2) 0.0250(7) Uani 1 1 d . . . H8A H 0.1231 0.2677 0.0598 0.030 Uiso 1 1 calc R . . C39 C 1.1372(2) 0.4256(2) 0.37627(19) 0.0204(6) Uani 1 1 d . . . C7 C 0.2680(2) 0.2385(2) 0.07760(18) 0.0184(6) Uani 1 1 d . . . C1 C 0.5043(2) 0.2301(2) 0.05149(18) 0.0161(6) Uani 1 1 d . . . C47 C 0.7424(2) 0.3197(2) 0.02103(18) 0.0174(6) Uani 1 1 d . . . C38 C 1.2451(2) 0.4424(2) 0.3976(2) 0.0256(7) Uani 1 1 d . . . H38A H 1.2815 0.5042 0.4390 0.031 Uiso 1 1 calc R . . C15 C 0.4794(2) 0.1641(2) 0.15995(18) 0.0155(6) Uani 1 1 d . . . C44 C 0.9951(2) 0.3662(2) 0.16291(19) 0.0183(6) Uani 1 1 d . . . H44A H 1.0670 0.3855 0.1819 0.022 Uiso 1 1 calc R . . C52 C 0.7802(2) 0.2551(3) -0.2003(2) 0.0246(7) Uani 1 1 d . . . H52A H 0.7778 0.1974 -0.2475 0.030 Uiso 1 1 calc R . . C6 C 0.3265(2) 0.1639(2) 0.04989(18) 0.0169(6) Uani 1 1 d . . . C3 C 0.5513(2) 0.2744(2) -0.04833(19) 0.0216(6) Uani 1 1 d . . . H3A H 0.5510 0.2869 -0.0974 0.026 Uiso 1 1 calc R . . C37 C 1.3004(2) 0.3709(3) 0.3598(2) 0.0277(7) Uani 1 1 d . . . C57 C 0.5336(3) 0.5652(3) 0.2228(2) 0.0281(7) Uani 1 1 d . . . H57A H 0.4864 0.5228 0.2378 0.034 Uiso 1 1 calc R . . C11 C 0.2778(2) 0.0693(2) -0.0129(2) 0.0263(7) Uani 1 1 d . . . C35 C 1.1371(2) 0.2566(2) 0.27855(19) 0.0222(6) Uani 1 1 d . . . C16 C 0.4161(2) 0.1106(2) 0.19324(19) 0.0185(6) Uani 1 1 d . . . H16A H 0.3448 0.0872 0.1722 0.022 Uiso 1 1 calc R . . C17 C 0.4792(2) 0.1008(2) 0.26072(19) 0.0199(6) Uani 1 1 d . . . H17A H 0.4599 0.0691 0.2948 0.024 Uiso 1 1 calc R . . C53 C 0.7584(2) 0.2446(2) -0.12869(19) 0.0207(6) Uani 1 1 d . . . C45 C 0.9337(2) 0.3652(2) 0.08980(19) 0.0195(6) Uani 1 1 d . . . H45A H 0.9553 0.3822 0.0484 0.023 Uiso 1 1 calc R . . C20 C 0.6562(2) 0.1087(2) 0.39667(19) 0.0196(6) Uani 1 1 d . . . C31 C 0.9427(2) 0.2462(2) 0.38960(19) 0.0212(6) Uani 1 1 d . . . H31A H 1.0117 0.2590 0.4209 0.025 Uiso 1 1 calc R . . C12 C 0.3184(2) 0.3419(2) 0.1440(2) 0.0261(7) Uani 1 1 d . . . H12A H 0.2662 0.3826 0.1548 0.039 Uiso 1 1 calc R . . H12B H 0.3674 0.3731 0.1236 0.039 Uiso 1 1 calc R . . H12C H 0.3539 0.3359 0.1960 0.039 Uiso 1 1 calc R . . C2 C 0.4677(2) 0.2402(2) -0.02829(19) 0.0201(6) Uani 1 1 d . . . H2A H 0.3989 0.2259 -0.0604 0.024 Uiso 1 1 calc R . . C43 C 0.9294(2) 0.3321(2) 0.20601(18) 0.0163(6) Uani 1 1 d . . . C29 C 0.7697(2) 0.1977(2) 0.34069(18) 0.0167(6) Uani 1 1 d . . . C21 C 0.6570(3) 0.0065(3) 0.3767(2) 0.0314(8) Uani 1 1 d . . . C58 C 0.5192(3) 0.5121(3) 0.1254(2) 0.0301(7) Uani 1 1 d . . . H58A H 0.4497 0.5114 0.0954 0.045 Uiso 1 1 calc R . . H58B H 0.5308 0.4441 0.1124 0.045 Uiso 1 1 calc R . . H58C H 0.5680 0.5479 0.1081 0.045 Uiso 1 1 calc R . . C60 C 0.7680(3) 0.5902(3) 0.2289(2) 0.0295(7) Uani 1 1 d . . . H60A H 0.7460 0.5367 0.1716 0.035 Uiso 1 1 calc R . . C49 C 0.7867(2) 0.4272(2) -0.0593(2) 0.0223(6) Uani 1 1 d . . . C50 C 0.8081(2) 0.4336(3) -0.1319(2) 0.0252(7) Uani 1 1 d . . . H50A H 0.8252 0.4970 -0.1329 0.030 Uiso 1 1 calc R . . C36 C 1.2448(2) 0.2773(3) 0.3020(2) 0.0275(7) Uani 1 1 d . . . H36A H 1.2808 0.2269 0.2782 0.033 Uiso 1 1 calc R . . C24 C 0.6381(3) 0.1266(3) 0.5357(2) 0.0315(8) Uani 1 1 d . . . H24A H 0.6312 0.1671 0.5888 0.038 Uiso 1 1 calc R . . C51 C 0.8051(2) 0.3489(3) -0.2034(2) 0.0260(7) Uani 1 1 d . . . C42 C 1.0817(3) 0.5075(2) 0.4189(2) 0.0279(7) Uani 1 1 d . . . H42A H 1.0080 0.4838 0.3976 0.042 Uiso 1 1 calc R . . H42B H 1.0995 0.5658 0.4068 0.042 Uiso 1 1 calc R . . H42C H 1.1021 0.5249 0.4796 0.042 Uiso 1 1 calc R . . C10 C 0.1707(3) 0.0514(3) -0.0464(2) 0.0351(8) Uani 1 1 d . . . H10A H 0.1380 -0.0115 -0.0881 0.042 Uiso 1 1 calc R . . C55 C 0.7311(3) 0.1401(2) -0.1298(2) 0.0260(7) Uani 1 1 d . . . H55A H 0.7323 0.0907 -0.1838 0.039 Uiso 1 1 calc R . . H55B H 0.6629 0.1312 -0.1216 0.039 Uiso 1 1 calc R . . H55C H 0.7807 0.1319 -0.0846 0.039 Uiso 1 1 calc R . . C63 C 0.6924(3) 0.6703(3) 0.3959(2) 0.0305(7) Uani 1 1 d . . . H63A H 0.6826 0.7333 0.3881 0.037 Uiso 1 1 calc R . . C9 C 0.1112(2) 0.1245(3) -0.0196(2) 0.0325(8) Uani 1 1 d . . . C54 C 0.7893(3) 0.5221(2) 0.0151(2) 0.0300(7) Uani 1 1 d . . . H54A H 0.8075 0.5797 0.0020 0.045 Uiso 1 1 calc R . . H54B H 0.8400 0.5252 0.0648 0.045 Uiso 1 1 calc R . . H54C H 0.7221 0.5221 0.0260 0.045 Uiso 1 1 calc R . . C59 C 0.4975(3) 0.6673(3) 0.2443(2) 0.0340(8) Uani 1 1 d . . . H59A H 0.4283 0.6584 0.2097 0.051 Uiso 1 1 calc R . . H59B H 0.5434 0.7131 0.2332 0.051 Uiso 1 1 calc R . . H59C H 0.4983 0.6945 0.3036 0.051 Uiso 1 1 calc R . . C61 C 0.7674(3) 0.6905(3) 0.2158(3) 0.0401(9) Uani 1 1 d . . . H61A H 0.8186 0.6985 0.1866 0.060 Uiso 1 1 calc R . . H61B H 0.7832 0.7455 0.2704 0.060 Uiso 1 1 calc R . . H61C H 0.7000 0.6899 0.1823 0.060 Uiso 1 1 calc R . . C40 C 1.0807(3) 0.1549(2) 0.2130(2) 0.0306(8) Uani 1 1 d . . . H40A H 1.1302 0.1131 0.1959 0.046 Uiso 1 1 calc R . . H40B H 1.0390 0.1630 0.1641 0.046 Uiso 1 1 calc R . . H40C H 1.0367 0.1236 0.2372 0.046 Uiso 1 1 calc R . . C22 C 0.6492(3) -0.0330(3) 0.4385(3) 0.0404(9) Uani 1 1 d . . . H22A H 0.6499 -0.1013 0.4255 0.048 Uiso 1 1 calc R . . C64 C 0.6117(3) 0.6483(3) 0.4402(2) 0.0369(8) Uani 1 1 d . . . H64A H 0.6249 0.7008 0.4958 0.055 Uiso 1 1 calc R . . H64B H 0.6161 0.5847 0.4458 0.055 Uiso 1 1 calc R . . H64C H 0.5435 0.6455 0.4067 0.055 Uiso 1 1 calc R . . C62 C 0.8776(3) 0.5815(3) 0.2681(3) 0.0362(8) Uani 1 1 d . . . H62A H 0.9225 0.5934 0.2351 0.054 Uiso 1 1 calc R . . H62B H 0.8781 0.5150 0.2683 0.054 Uiso 1 1 calc R . . H62C H 0.9017 0.6304 0.3257 0.054 Uiso 1 1 calc R . . C28 C 0.6446(3) 0.2800(3) 0.4986(2) 0.0342(8) Uani 1 1 d . . . H28A H 0.6375 0.3101 0.5556 0.051 Uiso 1 1 calc R . . H28B H 0.5871 0.2884 0.4591 0.051 Uiso 1 1 calc R . . H28C H 0.7083 0.3122 0.4951 0.051 Uiso 1 1 calc R . . C41 C 1.4175(3) 0.3937(3) 0.3784(2) 0.0390(9) Uani 1 1 d . . . H41A H 1.4431 0.4615 0.4195 0.058 Uiso 1 1 calc R . . H41B H 1.4363 0.3867 0.3266 0.058 Uiso 1 1 calc R . . H41C H 1.4473 0.3474 0.4010 0.058 Uiso 1 1 calc R . . C56 C 0.8285(3) 0.3595(3) -0.2810(2) 0.0362(9) Uani 1 1 d . . . H56A H 0.8227 0.2938 -0.3240 0.054 Uiso 1 1 calc R . . H56B H 0.8978 0.3963 -0.2658 0.054 Uiso 1 1 calc R . . H56C H 0.7799 0.3952 -0.3029 0.054 Uiso 1 1 calc R . . C14 C 0.3396(3) -0.0125(3) -0.0442(3) 0.0425(10) Uani 1 1 d . . . H14A H 0.2935 -0.0718 -0.0870 0.064 Uiso 1 1 calc R . . H14B H 0.3748 -0.0282 0.0028 0.064 Uiso 1 1 calc R . . H14C H 0.3898 0.0105 -0.0684 0.064 Uiso 1 1 calc R . . C23 C 0.6404(3) 0.0265(3) 0.5182(2) 0.0360(9) Uani 1 1 d . . . C27 C 0.6331(4) -0.0180(4) 0.5840(3) 0.0564(13) Uani 1 1 d . . . H27A H 0.6363 -0.0885 0.5609 0.085 Uiso 1 1 calc R . . H27B H 0.5686 -0.0098 0.5987 0.085 Uiso 1 1 calc R . . H27C H 0.6898 0.0160 0.6342 0.085 Uiso 1 1 calc R . . C65 C 0.8017(3) 0.6893(3) 0.4549(2) 0.0416(9) Uani 1 1 d . . . H65A H 0.8068 0.7419 0.5091 0.062 Uiso 1 1 calc R . . H65B H 0.8520 0.7094 0.4294 0.062 Uiso 1 1 calc R . . H65C H 0.8148 0.6286 0.4631 0.062 Uiso 1 1 calc R . . C13 C -0.0049(3) 0.1046(3) -0.0552(3) 0.0533(12) Uani 1 1 d . . . H13A H -0.0318 0.1642 -0.0291 0.080 Uiso 1 1 calc R . . H13B H -0.0355 0.0501 -0.0434 0.080 Uiso 1 1 calc R . . H13C H -0.0216 0.0869 -0.1159 0.080 Uiso 1 1 calc R . . C26 C 0.6655(4) -0.0601(3) 0.2904(3) 0.0516(11) Uani 1 1 d . . . H26A H 0.6693 -0.0208 0.2562 0.077 Uiso 1 1 calc R . . H26B H 0.6055 -0.1130 0.2628 0.077 Uiso 1 1 calc R . . H26C H 0.7270 -0.0892 0.2969 0.077 Uiso 1 1 calc R . . C67 C 1.0319(9) -0.0782(10) 0.3100(9) 0.080(3) Uani 0.50 1 d P . . H67A H 1.0883 -0.0525 0.2930 0.120 Uiso 0.50 1 calc PR . . H67B H 0.9679 -0.0663 0.2807 0.120 Uiso 0.50 1 calc PR . . H67C H 1.0285 -0.1494 0.2957 0.120 Uiso 0.50 1 calc PR . . C66 C 0.9967(9) -0.0208(10) 0.4584(8) 0.079(4) Uani 0.50 1 d P . . H66A H 0.9305 -0.0593 0.4313 0.095 Uiso 0.50 1 calc PR . . C68 C 1.0477(11) -0.0300(19) 0.3969(14) 0.152(9) Uani 0.50 1 d P . . H68A H 1.1142 0.0086 0.4214 0.182 Uiso 0.50 1 calc PR . . 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 0.0099(2) 0.0158(2) 0.0166(2) 0.00972(16) 0.00369(15) 0.00084(15) S1 0.0344(4) 0.0208(4) 0.0245(4) 0.0111(3) 0.0118(3) 0.0080(3) Si1 0.0191(4) 0.0186(4) 0.0205(4) 0.0078(3) 0.0029(3) 0.0030(3) N4 0.0113(11) 0.0206(12) 0.0180(12) 0.0117(10) 0.0035(9) 0.0014(9) N3 0.0122(11) 0.0175(12) 0.0187(12) 0.0113(10) 0.0040(9) 0.0015(9) N2 0.0111(11) 0.0158(11) 0.0176(12) 0.0084(10) 0.0039(9) 0.0011(9) N1 0.0117(11) 0.0190(12) 0.0199(12) 0.0121(10) 0.0051(9) 0.0023(9) C5 0.0117(13) 0.0156(13) 0.0186(14) 0.0050(11) 0.0040(11) 0.0015(11) C32 0.0133(14) 0.0188(14) 0.0187(14) 0.0088(12) 0.0030(11) 0.0016(11) C33 0.0120(14) 0.0191(14) 0.0188(14) 0.0071(12) 0.0035(11) 0.0019(11) C46 0.0161(14) 0.0196(14) 0.0199(15) 0.0112(12) 0.0063(11) 0.0023(11) C18 0.0160(14) 0.0153(13) 0.0189(14) 0.0081(11) 0.0071(11) 0.0005(11) C34 0.0121(14) 0.0251(15) 0.0171(14) 0.0122(12) 0.0035(11) 0.0009(11) C19 0.0183(14) 0.0141(13) 0.0195(14) 0.0079(11) 0.0065(11) 0.0020(11) C30 0.0200(15) 0.0264(16) 0.0215(15) 0.0166(13) 0.0051(12) 0.0045(12) C48 0.0119(13) 0.0289(16) 0.0207(15) 0.0150(13) 0.0035(11) 0.0016(12) C25 0.0153(14) 0.0329(17) 0.0225(16) 0.0151(14) 0.0026(12) -0.0020(12) C4 0.0176(14) 0.0196(14) 0.0185(14) 0.0114(12) 0.0046(11) 0.0027(11) C8 0.0154(15) 0.0274(17) 0.0287(17) 0.0071(14) 0.0046(12) 0.0057(12) C39 0.0185(15) 0.0245(15) 0.0198(15) 0.0113(13) 0.0050(12) 0.0010(12) C7 0.0162(14) 0.0216(15) 0.0191(14) 0.0095(12) 0.0059(11) 0.0019(11) C1 0.0123(13) 0.0171(14) 0.0194(14) 0.0083(12) 0.0032(11) 0.0019(11) C47 0.0172(14) 0.0200(14) 0.0194(15) 0.0120(12) 0.0066(11) 0.0020(11) C38 0.0211(16) 0.0275(17) 0.0213(16) 0.0060(13) 0.0008(12) -0.0043(13) C15 0.0120(13) 0.0146(13) 0.0203(14) 0.0061(11) 0.0063(11) 0.0015(11) C44 0.0110(13) 0.0221(15) 0.0224(15) 0.0092(12) 0.0057(11) -0.0006(11) C52 0.0185(15) 0.0326(17) 0.0204(15) 0.0091(13) 0.0044(12) -0.0006(13) C6 0.0118(14) 0.0216(15) 0.0189(14) 0.0107(12) 0.0033(11) 0.0007(11) C3 0.0191(15) 0.0286(16) 0.0205(15) 0.0149(13) 0.0032(12) 0.0039(12) C37 0.0165(15) 0.0381(19) 0.0258(17) 0.0119(15) 0.0027(13) 0.0000(13) C57 0.0248(17) 0.0291(17) 0.0303(18) 0.0139(14) 0.0040(14) 0.0019(13) C11 0.0178(15) 0.0234(16) 0.0310(18) 0.0040(14) 0.0044(13) 0.0025(13) C35 0.0157(15) 0.0263(16) 0.0227(16) 0.0085(13) 0.0038(12) 0.0014(12) C16 0.0109(13) 0.0198(14) 0.0247(15) 0.0084(12) 0.0065(11) -0.0019(11) C17 0.0188(15) 0.0206(15) 0.0237(15) 0.0115(12) 0.0089(12) -0.0012(12) C53 0.0127(14) 0.0279(16) 0.0232(15) 0.0143(13) 0.0026(11) -0.0011(12) C45 0.0174(14) 0.0239(15) 0.0205(15) 0.0111(12) 0.0087(12) 0.0002(12) C20 0.0159(14) 0.0223(15) 0.0232(15) 0.0147(13) 0.0027(12) -0.0019(11) C31 0.0150(14) 0.0292(16) 0.0217(15) 0.0145(13) 0.0017(12) 0.0028(12) C12 0.0194(15) 0.0245(16) 0.0280(17) 0.0043(14) 0.0039(13) 0.0030(13) C2 0.0138(14) 0.0270(16) 0.0208(15) 0.0129(13) 0.0007(11) 0.0034(12) C43 0.0119(13) 0.0175(14) 0.0200(14) 0.0078(12) 0.0046(11) 0.0015(11) C29 0.0171(14) 0.0174(14) 0.0188(14) 0.0105(12) 0.0052(11) 0.0035(11) C21 0.0368(19) 0.0245(17) 0.0350(19) 0.0161(15) 0.0076(15) 0.0010(14) C58 0.0294(18) 0.0312(18) 0.0258(17) 0.0130(14) -0.0022(14) 0.0013(14) C60 0.0303(18) 0.0250(17) 0.0332(18) 0.0110(14) 0.0098(14) 0.0025(14) C49 0.0183(15) 0.0271(16) 0.0248(16) 0.0156(13) 0.0043(12) 0.0001(12) C50 0.0215(16) 0.0310(17) 0.0284(17) 0.0199(14) 0.0052(13) -0.0020(13) C36 0.0183(16) 0.0319(18) 0.0294(17) 0.0082(14) 0.0063(13) 0.0058(13) C24 0.0237(17) 0.049(2) 0.0220(16) 0.0199(16) 0.0017(13) -0.0058(15) C51 0.0176(15) 0.0402(19) 0.0232(16) 0.0188(15) 0.0030(12) -0.0021(13) C42 0.0263(17) 0.0259(17) 0.0286(17) 0.0070(14) 0.0085(14) 0.0024(13) C10 0.0187(16) 0.0261(17) 0.040(2) -0.0044(15) -0.0005(14) -0.0024(13) C55 0.0246(16) 0.0266(17) 0.0271(17) 0.0116(14) 0.0071(13) 0.0001(13) C63 0.0336(19) 0.0247(17) 0.0271(17) 0.0070(14) 0.0015(14) 0.0035(14) C9 0.0148(16) 0.0332(19) 0.038(2) 0.0045(15) 0.0007(14) 0.0015(13) C54 0.039(2) 0.0258(17) 0.0301(18) 0.0164(14) 0.0113(15) 0.0023(14) C59 0.0298(18) 0.041(2) 0.0341(19) 0.0185(16) 0.0050(15) 0.0127(15) C61 0.044(2) 0.033(2) 0.050(2) 0.0200(18) 0.0211(18) 0.0049(17) C40 0.0221(16) 0.0257(17) 0.0366(19) 0.0048(15) 0.0057(14) 0.0032(13) C22 0.045(2) 0.0298(19) 0.051(2) 0.0287(18) 0.0047(18) -0.0029(16) C64 0.038(2) 0.042(2) 0.0262(18) 0.0076(16) 0.0063(15) 0.0096(16) C62 0.0261(18) 0.0325(19) 0.049(2) 0.0132(17) 0.0111(16) 0.0046(15) C28 0.043(2) 0.0354(19) 0.0252(17) 0.0107(15) 0.0115(15) 0.0093(16) C41 0.0191(17) 0.054(2) 0.035(2) 0.0116(18) 0.0022(14) -0.0023(16) C56 0.0346(19) 0.051(2) 0.0252(18) 0.0208(17) 0.0079(15) -0.0052(17) C14 0.0213(18) 0.0274(18) 0.055(2) -0.0065(17) 0.0014(16) 0.0031(14) C23 0.0281(18) 0.047(2) 0.038(2) 0.0324(18) -0.0020(15) -0.0103(16) C27 0.052(3) 0.073(3) 0.052(3) 0.051(2) -0.005(2) -0.019(2) C65 0.033(2) 0.042(2) 0.033(2) 0.0038(17) -0.0039(16) -0.0024(17) C13 0.0175(18) 0.045(2) 0.066(3) -0.006(2) -0.0046(18) 0.0036(16) C26 0.087(3) 0.0217(19) 0.053(3) 0.0155(18) 0.028(2) 0.016(2) C67 0.062(7) 0.105(10) 0.092(9) 0.047(8) 0.039(7) 0.027(7) C66 0.056(6) 0.089(9) 0.120(10) 0.063(9) 0.028(8) 0.037(6) C68 0.045(8) 0.29(3) 0.19(2) 0.15(2) 0.038(10) 0.062(12) _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 N1 2.078(2) . ? Fe1 N2 2.080(2) . ? Fe1 N3 2.081(2) . ? Fe1 N4 2.081(2) . ? Fe1 S1 2.2726(9) . ? S1 Si1 2.1339(11) . ? Si1 C60 1.883(4) . ? Si1 C63 1.892(3) . ? Si1 C57 1.893(3) . ? N4 C46 1.373(4) . ? N4 C43 1.381(4) . ? N3 C29 1.378(4) . ? N3 C32 1.380(4) . ? N2 C18 1.372(4) . ? N2 C15 1.375(4) . ? N1 C4 1.377(4) . ? N1 C1 1.381(4) . ? C5 C15 1.388(4) . ? C5 C1 1.394(4) . ? C5 C6 1.501(4) . ? C32 C33 1.391(4) . ? C32 C31 1.429(4) . ? C33 C43 1.392(4) . ? C33 C34 1.503(4) . ? C46 C47 1.396(4) . ? C46 C45 1.433(4) . ? C18 C19 1.397(4) . ? C18 C17 1.436(4) . ? C34 C35 1.399(4) . ? C34 C39 1.402(4) . ? C19 C29 1.389(4) . ? C19 C20 1.499(4) . ? C30 C31 1.345(4) . ? C30 C29 1.436(4) . ? C30 H30A 0.9300 . ? C48 C53 1.398(4) . ? C48 C49 1.408(4) . ? C48 C47 1.504(4) . ? C25 C24 1.392(4) . ? C25 C20 1.399(4) . ? C25 C28 1.499(5) . ? C4 C47 1.393(4) . ? C4 C3 1.436(4) . ? C8 C9 1.382(5) . ? C8 C7 1.383(4) . ? C8 H8A 0.9300 . ? C39 C38 1.389(4) . ? C39 C42 1.506(4) . ? C7 C6 1.396(4) . ? C7 C12 1.508(4) . ? C1 C2 1.428(4) . ? C38 C37 1.382(5) . ? C38 H38A 0.9300 . ? C15 C16 1.436(4) . ? C44 C45 1.348(4) . ? C44 C43 1.431(4) . ? C44 H44A 0.9300 . ? C52 C51 1.386(5) . ? C52 C53 1.391(4) . ? C52 H52A 0.9300 . ? C6 C11 1.398(4) . ? C3 C2 1.347(4) . ? C3 H3A 0.9300 . ? C37 C36 1.386(5) . ? C37 C41 1.513(4) . ? C57 C59 1.533(5) . ? C57 C58 1.548(5) . ? C57 H57A 0.9800 . ? C11 C10 1.390(5) . ? C11 C14 1.512(5) . ? C35 C36 1.387(4) . ? C35 C40 1.505(4) . ? C16 C17 1.347(4) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C53 C55 1.511(4) . ? C45 H45A 0.9300 . ? C20 C21 1.390(4) . ? C31 H31A 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C2 H2A 0.9300 . ? C21 C22 1.397(5) . ? C21 C26 1.502(5) . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C60 C62 1.516(5) . ? C60 C61 1.541(5) . ? C60 H60A 0.9800 . ? C49 C50 1.383(4) . ? C49 C54 1.504(5) . ? C50 C51 1.388(5) . ? C50 H50A 0.9300 . ? C36 H36A 0.9300 . ? C24 C23 1.370(5) . ? C24 H24A 0.9300 . ? C51 C56 1.503(4) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C10 C9 1.387(5) . ? C10 H10A 0.9300 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C63 C64 1.528(5) . ? C63 C65 1.532(5) . ? C63 H63A 0.9800 . ? C9 C13 1.506(5) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C22 C23 1.382(6) . ? C22 H22A 0.9300 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C23 C27 1.511(5) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C67 C68 1.38(2) . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C66 C66 1.33(3) 2_756 ? C66 C68 1.36(2) . ? C66 H66A 0.9300 . ? C68 H68A 0.9300 . ? 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 N1 Fe1 N2 86.35(9) . . ? N1 Fe1 N3 150.09(9) . . ? N2 Fe1 N3 85.99(9) . . ? N1 Fe1 N4 85.71(9) . . ? N2 Fe1 N4 149.38(9) . . ? N3 Fe1 N4 86.33(9) . . ? N1 Fe1 S1 112.72(7) . . ? N2 Fe1 S1 98.37(7) . . ? N3 Fe1 S1 96.99(7) . . ? N4 Fe1 S1 111.97(7) . . ? Si1 S1 Fe1 123.00(4) . . ? C60 Si1 C63 112.71(16) . . ? C60 Si1 C57 110.69(16) . . ? C63 Si1 C57 107.23(15) . . ? C60 Si1 S1 110.45(11) . . ? C63 Si1 S1 106.01(12) . . ? C57 Si1 S1 109.59(11) . . ? C46 N4 C43 105.8(2) . . ? C46 N4 Fe1 128.20(18) . . ? C43 N4 Fe1 125.24(19) . . ? C29 N3 C32 105.6(2) . . ? C29 N3 Fe1 126.41(19) . . ? C32 N3 Fe1 125.91(18) . . ? C18 N2 C15 105.9(2) . . ? C18 N2 Fe1 126.83(18) . . ? C15 N2 Fe1 125.64(18) . . ? C4 N1 C1 105.8(2) . . ? C4 N1 Fe1 127.83(19) . . ? C1 N1 Fe1 125.49(19) . . ? C15 C5 C1 124.2(3) . . ? C15 C5 C6 118.1(2) . . ? C1 C5 C6 117.7(2) . . ? N3 C32 C33 125.5(3) . . ? N3 C32 C31 110.1(2) . . ? C33 C32 C31 124.3(3) . . ? C32 C33 C43 124.1(3) . . ? C32 C33 C34 119.2(3) . . ? C43 C33 C34 116.4(2) . . ? N4 C46 C47 125.7(3) . . ? N4 C46 C45 110.1(2) . . ? C47 C46 C45 124.1(3) . . ? N2 C18 C19 125.8(2) . . ? N2 C18 C17 110.0(2) . . ? C19 C18 C17 124.2(3) . . ? C35 C34 C39 120.0(3) . . ? C35 C34 C33 118.6(3) . . ? C39 C34 C33 121.3(3) . . ? C29 C19 C18 124.2(3) . . ? C29 C19 C20 117.3(3) . . ? C18 C19 C20 118.5(2) . . ? C31 C30 C29 107.4(3) . . ? C31 C30 H30A 126.3 . . ? C29 C30 H30A 126.3 . . ? C53 C48 C49 119.8(3) . . ? C53 C48 C47 119.1(3) . . ? C49 C48 C47 121.0(3) . . ? C24 C25 C20 118.8(3) . . ? C24 C25 C28 120.5(3) . . ? C20 C25 C28 120.7(3) . . ? N1 C4 C47 126.1(3) . . ? N1 C4 C3 109.6(2) . . ? C47 C4 C3 124.2(3) . . ? C9 C8 C7 122.1(3) . . ? C9 C8 H8A 118.9 . . ? C7 C8 H8A 118.9 . . ? C38 C39 C34 118.4(3) . . ? C38 C39 C42 119.9(3) . . ? C34 C39 C42 121.7(3) . . ? C8 C7 C6 119.1(3) . . ? C8 C7 C12 119.5(3) . . ? C6 C7 C12 121.4(3) . . ? N1 C1 C5 125.7(3) . . ? N1 C1 C2 109.9(2) . . ? C5 C1 C2 124.2(3) . . ? C4 C47 C46 123.6(3) . . ? C4 C47 C48 118.6(3) . . ? C46 C47 C48 117.5(2) . . ? C37 C38 C39 122.6(3) . . ? C37 C38 H38A 118.7 . . ? C39 C38 H38A 118.7 . . ? N2 C15 C5 126.1(3) . . ? N2 C15 C16 109.9(2) . . ? C5 C15 C16 124.0(3) . . ? C45 C44 C43 107.5(2) . . ? C45 C44 H44A 126.3 . . ? C43 C44 H44A 126.3 . . ? C51 C52 C53 121.9(3) . . ? C51 C52 H52A 119.0 . . ? C53 C52 H52A 119.0 . . ? C7 C6 C11 120.1(3) . . ? C7 C6 C5 118.9(3) . . ? C11 C6 C5 121.0(3) . . ? C2 C3 C4 107.4(3) . . ? C2 C3 H3A 126.3 . . ? C4 C3 H3A 126.3 . . ? C38 C37 C36 117.7(3) . . ? C38 C37 C41 121.7(3) . . ? C36 C37 C41 120.5(3) . . ? C59 C57 C58 111.1(3) . . ? C59 C57 Si1 115.4(2) . . ? C58 C57 Si1 111.5(2) . . ? C59 C57 H57A 106.1 . . ? C58 C57 H57A 106.1 . . ? Si1 C57 H57A 106.1 . . ? C10 C11 C6 118.7(3) . . ? C10 C11 C14 120.2(3) . . ? C6 C11 C14 121.1(3) . . ? C36 C35 C34 119.2(3) . . ? C36 C35 C40 119.6(3) . . ? C34 C35 C40 121.2(3) . . ? C17 C16 C15 107.1(2) . . ? C17 C16 H16A 126.4 . . ? C15 C16 H16A 126.4 . . ? C16 C17 C18 107.0(3) . . ? C16 C17 H17A 126.5 . . ? C18 C17 H17A 126.5 . . ? C52 C53 C48 119.2(3) . . ? C52 C53 C55 119.2(3) . . ? C48 C53 C55 121.5(3) . . ? C44 C45 C46 107.0(3) . . ? C44 C45 H45A 126.5 . . ? C46 C45 H45A 126.5 . . ? C21 C20 C25 120.2(3) . . ? C21 C20 C19 120.0(3) . . ? C25 C20 C19 119.8(3) . . ? C30 C31 C32 107.2(3) . . ? C30 C31 H31A 126.4 . . ? C32 C31 H31A 126.4 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C2 C1 107.2(3) . . ? C3 C2 H2A 126.4 . . ? C1 C2 H2A 126.4 . . ? N4 C43 C33 126.6(3) . . ? N4 C43 C44 109.6(2) . . ? C33 C43 C44 123.6(3) . . ? N3 C29 C19 125.7(3) . . ? N3 C29 C30 109.7(2) . . ? C19 C29 C30 124.6(3) . . ? C20 C21 C22 118.6(3) . . ? C20 C21 C26 120.6(3) . . ? C22 C21 C26 120.8(3) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C62 C60 C61 110.5(3) . . ? C62 C60 Si1 115.2(3) . . ? C61 C60 Si1 112.1(2) . . ? C62 C60 H60A 106.1 . . ? C61 C60 H60A 106.1 . . ? Si1 C60 H60A 106.1 . . ? C50 C49 C48 118.7(3) . . ? C50 C49 C54 119.7(3) . . ? C48 C49 C54 121.6(3) . . ? C49 C50 C51 122.6(3) . . ? C49 C50 H50A 118.7 . . ? C51 C50 H50A 118.7 . . ? C37 C36 C35 121.9(3) . . ? C37 C36 H36A 119.0 . . ? C35 C36 H36A 119.0 . . ? C23 C24 C25 122.1(3) . . ? C23 C24 H24A 118.9 . . ? C25 C24 H24A 118.9 . . ? C52 C51 C50 117.7(3) . . ? C52 C51 C56 121.6(3) . . ? C50 C51 C56 120.7(3) . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C9 C10 C11 122.0(3) . . ? C9 C10 H10A 119.0 . . ? C11 C10 H10A 119.0 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C64 C63 C65 109.6(3) . . ? C64 C63 Si1 110.8(2) . . ? C65 C63 Si1 115.0(3) . . ? C64 C63 H63A 107.0 . . ? C65 C63 H63A 107.0 . . ? Si1 C63 H63A 107.0 . . ? C8 C9 C10 117.9(3) . . ? C8 C9 C13 120.1(3) . . ? C10 C9 C13 121.9(3) . . ? C49 C54 H54A 109.5 . . ? C49 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C49 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C35 C40 H40A 109.5 . . ? C35 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C35 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C23 C22 C21 122.0(3) . . ? C23 C22 H22A 119.0 . . ? C21 C22 H22A 119.0 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C37 C41 H41A 109.5 . . ? C37 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C37 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C51 C56 H56A 109.5 . . ? C51 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C51 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C24 C23 C22 118.2(3) . . ? C24 C23 C27 120.9(4) . . ? C22 C23 C27 120.8(4) . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C63 C65 H65A 109.5 . . ? C63 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C63 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C68 C67 H67A 109.5 . . ? C68 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C68 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C66 C66 C68 145.5(19) 2_756 . ? C66 C66 H66A 107.3 2_756 . ? C68 C66 H66A 107.3 . . ? C66 C68 C67 140.1(17) . . ? C66 C68 H68A 110.0 . . ? C67 C68 H68A 110.0 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.998 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.079 #===END _publ_section_synopsis . #Added by publCIF _publ_section_related_literature ; ? ; #Added by publCIF #============================================================================== _audit_creation_date '2013-02-07' _audit_creation_method SHELXL-97 _audit_update_record ; ? ; #============================================================================== # SUBMISSION DETAILS _publ_requested_journal '' _publ_requested_category ? _publ_contact_author_name '' _publ_contact_author_address ; Department of Chemistry, The University of Texas, One UTSA Circle, San Antonio, Texas 78249-0698, U.S.A. ; _publ_contact_letter ; ; _publ_requested_coeditor_name ' ' _publ_contact_author_phone ' ' _publ_contact_author_fax ' ' _publ_contact_author_email ; hadi.arman@utsa.edu ; #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_paper_category ? _journal_coeditor_notes ; ; _journal_techeditor_code ? _iucr_compatibility_tag ACTA95 _journal_techeditor_notes ; ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; ; _publ_section_title_footnote ; Additional correspondence e-mail: ; loop_ _publ_author_name _publ_author_address '' ; Department of Chemistry The University of Texas at San Antonio One UTSA Circle San Antonio, Texas 78249-0698, USA ; #============================================================================== # TEXT _publ_section_abstract ; (type here to add abstract) ; _publ_section_exptl_refinement ; All H-atoms were placed on calculated positions.Carbon-bound H-atoms were refined with U~iso~(H) = 1.2-1.5U~eq~(C). ; #============================================================================== _publ_section_exptl_prep ; (type here to add preparation details) ; #============================================================================== _publ_section_comment ; (type here to add) ; _publ_section_references ; Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Rigaku Americas Corporation (2008). CrystalClear. Rigaku/MSC Inc., The Woodlands, Texas, USA. Rueping, M., Kuenkel, A., Tato, F. & Bats, J. W. (2009). Angew. Chem. Int. Ed. 48, 3699--3702. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany. Westrip, S. P. (2010). publCIF. J. Appl. Cryst. 43. Submitted. ; _publ_section_acknowledgements ; (type here to add acknowledgements) ; _publ_section_figure_captions ; (type here to add) ; _publ_section_table_legends ; ; data_[Fe(SSiPh3)(TMP)] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C74 H67 Fe N4 S Si, 0.8(C H2 Cl2)' _chemical_formula_sum 'C74.80 H68.60 Cl1.60 Fe N4 S Si' _chemical_formula_weight 1196.26 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' 'Si' 'Si' 0.0817 0.0704 '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' 'S' 'S' 0.1246 0.1234 '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' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 2(1)/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.4254(13) _cell_length_b 18.9508(14) _cell_length_c 22.8901(19) _cell_angle_alpha 90.00 _cell_angle_beta 108.668(8) _cell_angle_gamma 90.00 _cell_volume 6750.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 98(2) _cell_measurement_reflns_used 20068 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description 'needle' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2514 _exptl_absorpt_coefficient_mu 0.379 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.362 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 98(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Saturn724 (2x2 bin mode) ; _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% '<1' _diffrn_reflns_number 9440 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1255 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 23.10 _diffrn_reflns_reduction_process 'Lp corrections applied' _reflns_number_total 9440 _reflns_number_gt 5585 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010) ; _computing_cell_refinement ; CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010) ; _computing_data_reduction ; CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'publCIF (Westrip, 2010)' _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^)+(0.0100P)^2^+40.0000P] 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 const _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9440 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1424 _refine_ls_R_factor_gt 0.0900 _refine_ls_wR_factor_ref 0.1982 _refine_ls_wR_factor_gt 0.1813 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.006 _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 0.12488(6) 0.71944(5) 0.76541(4) 0.0243(3) Uani 1 1 d . . . Si1 Si 0.02821(16) 0.54406(12) 0.69149(10) 0.0456(6) Uani 1 1 d . . . S1 S 0.04811(17) 0.61999(13) 0.75775(12) 0.0651(7) Uani 1 1 d . . . N3 N 0.0456(3) 0.7818(3) 0.7998(2) 0.0250(13) Uani 1 1 d . . . N2 N 0.0803(3) 0.7787(3) 0.6853(2) 0.0224(12) Uani 1 1 d . . . N1 N 0.2354(3) 0.7059(3) 0.7424(2) 0.0233(13) Uani 1 1 d . . . N4 N 0.2016(3) 0.7081(3) 0.8569(2) 0.0258(13) Uani 1 1 d . . . C15 C 0.1109(4) 0.7765(3) 0.6357(3) 0.0248(16) Uani 1 1 d . . . C1 C 0.2456(4) 0.7130(3) 0.6852(3) 0.0248(16) Uani 1 1 d . . . C16 C 0.0495(4) 0.8126(3) 0.5838(3) 0.0256(16) Uani 1 1 d . . . H16A H 0.0537 0.8182 0.5445 0.031 Uiso 1 1 calc R . . C20 C -0.1204(4) 0.8837(3) 0.6762(3) 0.0236(16) Uani 1 1 d . . . C19 C -0.0442(4) 0.8377(3) 0.7036(3) 0.0226(16) Uani 1 1 d . . . C43 C 0.1757(4) 0.7159(4) 0.9078(3) 0.0254(16) Uani 1 1 d . . . C18 C 0.0051(4) 0.8173(3) 0.6664(3) 0.0228(16) Uani 1 1 d . . . C44 C 0.2394(4) 0.6862(4) 0.9611(3) 0.0276(17) Uani 1 1 d . . . H44A H 0.2366 0.6838 1.0010 0.033 Uiso 1 1 calc R . . C4 C 0.3114(4) 0.6727(3) 0.7777(3) 0.0249(16) Uani 1 1 d . . . C45 C 0.3030(4) 0.6631(3) 0.9417(3) 0.0293(17) Uani 1 1 d . . . H45A H 0.3535 0.6418 0.9661 0.035 Uiso 1 1 calc R . . C3 C 0.3660(4) 0.6592(4) 0.7425(3) 0.0312(18) Uani 1 1 d . . . H3A H 0.4196 0.6377 0.7561 0.037 Uiso 1 1 calc R . . C11 C 0.1828(4) 0.7019(4) 0.5296(3) 0.0259(16) Uani 1 1 d . . . C10 C 0.2133(4) 0.7075(4) 0.4788(3) 0.0298(17) Uani 1 1 d . . . H10A H 0.1954 0.6741 0.4474 0.036 Uiso 1 1 calc R . . C29 C -0.0237(4) 0.8214(3) 0.7661(3) 0.0264(17) Uani 1 1 d . . . C17 C -0.0142(4) 0.8362(3) 0.6035(3) 0.0240(16) Uani 1 1 d . . . H17A H -0.0626 0.8607 0.5799 0.029 Uiso 1 1 calc R . . C7 C 0.2700(4) 0.8050(3) 0.5731(3) 0.0270(16) Uani 1 1 d . . . C33 C 0.1011(4) 0.7477(4) 0.9107(3) 0.0285(17) Uani 1 1 d . . . C52 C 0.5666(4) 0.6335(4) 0.9322(3) 0.0302(17) Uani 1 1 d . . . H52A H 0.6164 0.6602 0.9471 0.036 Uiso 1 1 calc R . . C6 C 0.2128(4) 0.7514(3) 0.5770(3) 0.0261(16) Uani 1 1 d . . . C34 C 0.0822(4) 0.7515(4) 0.9697(3) 0.0339(19) Uani 1 1 d . . . C47 C 0.3311(4) 0.6588(3) 0.8411(3) 0.0247(16) Uani 1 1 d . . . C32 C 0.0407(4) 0.7802(4) 0.8585(3) 0.0300(17) Uani 1 1 d . . . C25 C -0.1998(4) 0.8530(3) 0.6431(3) 0.0284(17) Uani 1 1 d . . . C46 C 0.2805(4) 0.6764(3) 0.8770(3) 0.0239(16) Uani 1 1 d . . . C49 C 0.4199(4) 0.5523(4) 0.8835(3) 0.0305(18) Uani 1 1 d . . . C2 C 0.3251(4) 0.6839(3) 0.6848(3) 0.0283(17) Uani 1 1 d . . . H2A H 0.3454 0.6821 0.6513 0.034 Uiso 1 1 calc R . . C50 C 0.4961(4) 0.5231(4) 0.9199(3) 0.0338(19) Uani 1 1 d . . . H50A H 0.4978 0.4750 0.9281 0.041 Uiso 1 1 calc R . . C28 C -0.2106(5) 0.7749(4) 0.6368(3) 0.0395(19) Uani 1 1 d . . . H28A H -0.2687 0.7641 0.6124 0.059 Uiso 1 1 calc R . . H28B H -0.1984 0.7541 0.6769 0.059 Uiso 1 1 calc R . . H28C H -0.1718 0.7564 0.6169 0.059 Uiso 1 1 calc R . . C31 C -0.0331(4) 0.8181(4) 0.8614(3) 0.0339(18) Uani 1 1 d . . . H31A H -0.0505 0.8240 0.8959 0.041 Uiso 1 1 calc R . . C53 C 0.4896(4) 0.6665(4) 0.8974(3) 0.0281(17) Uani 1 1 d . . . C9 C 0.2686(4) 0.7602(4) 0.4735(3) 0.0318(18) Uani 1 1 d . . . C56 C 0.4868(5) 0.7448(4) 0.8874(4) 0.046(2) Uani 1 1 d . . . H56A H 0.4297 0.7585 0.8631 0.070 Uiso 1 1 calc R . . H56B H 0.5264 0.7576 0.8661 0.070 Uiso 1 1 calc R . . H56C H 0.5024 0.7685 0.9265 0.070 Uiso 1 1 calc R . . C48 C 0.4166(4) 0.6248(3) 0.8735(3) 0.0273(17) Uani 1 1 d . . . C38 C 0.0246(5) 0.6996(5) 1.0448(4) 0.047(2) Uani 1 1 d . . . H38A H -0.0012 0.6618 1.0579 0.056 Uiso 1 1 calc R . . C5 C 0.1863(4) 0.7452(3) 0.6339(3) 0.0249(16) Uani 1 1 d . . . C63 C -0.0301(5) 0.5777(4) 0.6121(3) 0.0327(18) Uani 1 1 d . . . C51 C 0.5693(4) 0.5621(4) 0.9447(3) 0.0303(17) Uani 1 1 d . . . C24 C -0.2687(4) 0.8973(4) 0.6152(3) 0.0358(19) Uani 1 1 d . . . H24A H -0.3207 0.8775 0.5919 0.043 Uiso 1 1 calc R . . C8 C 0.2962(4) 0.8079(4) 0.5215(3) 0.0325(18) Uani 1 1 d . . . H8A H 0.3339 0.8435 0.5190 0.039 Uiso 1 1 calc R . . C14 C 0.1236(5) 0.6439(4) 0.5330(3) 0.0374(19) Uani 1 1 d . . . H14A H 0.1102 0.6158 0.4962 0.056 Uiso 1 1 calc R . . H14B H 0.0717 0.6635 0.5368 0.056 Uiso 1 1 calc R . . H14C H 0.1507 0.6148 0.5682 0.056 Uiso 1 1 calc R . . C30 C -0.0723(4) 0.8434(4) 0.8045(3) 0.0328(18) Uani 1 1 d . . . H30A H -0.1222 0.8704 0.7924 0.039 Uiso 1 1 calc R . . C21 C -0.1125(4) 0.9564(4) 0.6835(3) 0.0289(17) Uani 1 1 d . . . C61 C 0.2661(5) 0.4883(4) 0.6754(3) 0.041(2) Uani 1 1 d . . . H61A H 0.3110 0.5116 0.6671 0.049 Uiso 1 1 calc R . . C65 C -0.1061(5) 0.6665(4) 0.5405(3) 0.045(2) Uani 1 1 d . . . H65A H -0.1256 0.7127 0.5335 0.054 Uiso 1 1 calc R . . C64 C -0.0605(4) 0.6448(4) 0.6002(3) 0.0348(19) Uani 1 1 d . . . H64A H -0.0506 0.6769 0.6325 0.042 Uiso 1 1 calc R . . C23 C -0.2624(5) 0.9700(4) 0.6210(3) 0.039(2) Uani 1 1 d . . . C66 C -0.1223(5) 0.6211(4) 0.4930(3) 0.042(2) Uani 1 1 d . . . H66A H -0.1532 0.6363 0.4535 0.050 Uiso 1 1 calc R . . C54 C 0.3414(5) 0.5054(4) 0.8552(4) 0.040(2) Uani 1 1 d . . . H54A H 0.3558 0.4573 0.8671 0.061 Uiso 1 1 calc R . . H54B H 0.3237 0.5091 0.8110 0.061 Uiso 1 1 calc R . . H54C H 0.2953 0.5204 0.8696 0.061 Uiso 1 1 calc R . . C62 C 0.1952(5) 0.5254(4) 0.6794(3) 0.0360(19) Uani 1 1 d . . . H62A H 0.1942 0.5741 0.6743 0.043 Uiso 1 1 calc R . . C39 C 0.0446(4) 0.6940(4) 0.9895(3) 0.039(2) Uani 1 1 d . . . C57 C 0.1256(5) 0.4930(4) 0.6908(3) 0.039(2) Uani 1 1 d . . . C35 C 0.1024(5) 0.8131(4) 1.0061(3) 0.0383(19) Uani 1 1 d . . . C60 C 0.2683(5) 0.4167(4) 0.6839(3) 0.044(2) Uani 1 1 d . . . H60A H 0.3159 0.3912 0.6823 0.053 Uiso 1 1 calc R . . C67 C -0.0941(5) 0.5532(4) 0.5018(4) 0.047(2) Uani 1 1 d . . . H67A H -0.1053 0.5219 0.4689 0.057 Uiso 1 1 calc R . . C37 C 0.0430(5) 0.7613(5) 1.0801(3) 0.044(2) Uani 1 1 d . . . C55 C 0.6514(5) 0.5289(4) 0.9849(3) 0.043(2) Uani 1 1 d . . . H55A H 0.6954 0.5643 0.9976 0.065 Uiso 1 1 calc R . . H55B H 0.6691 0.4928 0.9621 0.065 Uiso 1 1 calc R . . H55C H 0.6422 0.5084 1.0206 0.065 Uiso 1 1 calc R . . C26 C -0.0291(5) 0.9905(4) 0.7200(3) 0.0379(19) Uani 1 1 d . . . H26A H -0.0363 1.0408 0.7195 0.057 Uiso 1 1 calc R . . H26B H 0.0145 0.9787 0.7019 0.057 Uiso 1 1 calc R . . H26C H -0.0121 0.9738 0.7618 0.057 Uiso 1 1 calc R . . C13 C 0.2964(5) 0.7661(5) 0.4177(3) 0.049(2) Uani 1 1 d . . . H13A H 0.2704 0.7290 0.3893 0.073 Uiso 1 1 calc R . . H13B H 0.3578 0.7621 0.4296 0.073 Uiso 1 1 calc R . . H13C H 0.2789 0.8110 0.3984 0.073 Uiso 1 1 calc R . . C36 C 0.0804(5) 0.8160(5) 1.0595(3) 0.045(2) Uani 1 1 d . . . H36A H 0.0916 0.8574 1.0825 0.054 Uiso 1 1 calc R . . C22 C -0.1839(5) 0.9991(4) 0.6550(3) 0.039(2) Uani 1 1 d . . . H22A H -0.1785 1.0479 0.6589 0.047 Uiso 1 1 calc R . . C12 C 0.3035(5) 0.8576(4) 0.6243(3) 0.0367(19) Uani 1 1 d . . . H12A H 0.3411 0.8902 0.6136 0.055 Uiso 1 1 calc R . . H12B H 0.3346 0.8333 0.6616 0.055 Uiso 1 1 calc R . . H12C H 0.2563 0.8828 0.6305 0.055 Uiso 1 1 calc R . . C40 C 0.1458(6) 0.8749(4) 0.9872(4) 0.061(3) Uani 1 1 d . . . H40A H 0.1558 0.8642 0.9491 0.091 Uiso 1 1 calc R . . H40B H 0.1997 0.8840 1.0186 0.091 Uiso 1 1 calc R . . H40C H 0.1097 0.9158 0.9820 0.091 Uiso 1 1 calc R . . C69 C -0.0505(6) 0.4782(5) 0.7114(4) 0.060(3) Uani 1 1 d . . . C68 C -0.0478(5) 0.5318(4) 0.5617(4) 0.045(2) Uani 1 1 d . . . H68A H -0.0281 0.4855 0.5683 0.054 Uiso 1 1 calc R . . C59 C 0.2014(6) 0.3823(4) 0.6947(4) 0.052(2) Uani 1 1 d . . . H59A H 0.2031 0.3336 0.6999 0.063 Uiso 1 1 calc R . . C41 C 0.0217(6) 0.7648(6) 1.1402(4) 0.072(3) Uani 1 1 d . . . H41A H -0.0044 0.7212 1.1462 0.108 Uiso 1 1 calc R . . H41B H -0.0175 0.8030 1.1382 0.108 Uiso 1 1 calc R . . H41C H 0.0734 0.7724 1.1740 0.108 Uiso 1 1 calc R . . C71 C -0.0886(7) 0.4107(5) 0.7900(5) 0.066(3) Uani 1 1 d . . . H71A H -0.0772 0.3968 0.8308 0.079 Uiso 1 1 calc R . . C58 C 0.1312(5) 0.4204(4) 0.6978(4) 0.049(2) Uani 1 1 d . . . H58A H 0.0859 0.3963 0.7049 0.059 Uiso 1 1 calc R . . C42 C 0.0257(5) 0.6269(4) 0.9527(4) 0.050(2) Uani 1 1 d . . . H42A H -0.0002 0.5934 0.9728 0.075 Uiso 1 1 calc R . . H42B H 0.0783 0.6077 0.9496 0.075 Uiso 1 1 calc R . . H42C H -0.0129 0.6367 0.9121 0.075 Uiso 1 1 calc R . . C74 C -0.1234(7) 0.4522(5) 0.6698(5) 0.073(3) Uani 1 1 d . . . H74A H -0.1367 0.4647 0.6285 0.087 Uiso 1 1 calc R . . C72 C -0.1588(8) 0.3867(6) 0.7462(6) 0.087(3) Uani 1 1 d . . . H72A H -0.1942 0.3549 0.7575 0.105 Uiso 1 1 calc R . . C27 C -0.3380(5) 1.0167(5) 0.5897(4) 0.063(3) Uani 1 1 d . . . H27A H -0.3218 1.0652 0.5984 0.094 Uiso 1 1 calc R . . H27B H -0.3847 1.0057 0.6049 0.094 Uiso 1 1 calc R . . H27C H -0.3556 1.0089 0.5460 0.094 Uiso 1 1 calc R . . C70 C -0.0310(7) 0.4579(6) 0.7733(6) 0.096(4) Uani 1 1 d . . . H70A H 0.0182 0.4747 0.8030 0.115 Uiso 1 1 calc R . . C73 C -0.1800(9) 0.4063(6) 0.6879(6) 0.097(4) Uani 1 1 d . . . H73A H -0.2307 0.3905 0.6592 0.117 Uiso 1 1 calc R . . Cl1 Cl 0.0520(2) 1.0443(2) 0.89832(17) 0.0886(11) Uani 0.80 1 d P . . Cl2 Cl 0.1185(3) 1.0650(2) 1.0316(2) 0.1184(16) Uani 0.80 1 d P . . C75 C 0.1248(7) 1.0793(7) 0.9533(5) 0.085(5) Uani 0.80 1 d P . . H75A H 0.1239 1.1297 0.9460 0.102 Uiso 0.80 1 calc PR . . H75B H 0.1798 1.0616 0.9524 0.102 Uiso 0.80 1 calc PR . . 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 0.0242(5) 0.0287(5) 0.0176(5) 0.0021(4) 0.0033(4) -0.0002(4) Si1 0.0569(16) 0.0507(15) 0.0318(13) 0.0083(11) 0.0180(11) 0.0197(12) S1 0.0733(18) 0.0534(15) 0.0553(16) -0.0098(12) 0.0018(13) -0.0003(12) N3 0.019(3) 0.038(3) 0.015(3) 0.005(3) 0.001(2) -0.001(3) N2 0.023(3) 0.027(3) 0.016(3) 0.000(2) 0.003(2) 0.007(2) N1 0.032(3) 0.023(3) 0.016(3) 0.000(2) 0.008(2) 0.002(2) N4 0.023(3) 0.032(3) 0.023(3) 0.003(3) 0.009(3) 0.000(3) C15 0.032(4) 0.022(4) 0.017(4) -0.004(3) 0.004(3) 0.000(3) C1 0.031(4) 0.024(4) 0.020(4) 0.002(3) 0.008(3) 0.001(3) C16 0.028(4) 0.029(4) 0.018(4) 0.005(3) 0.006(3) -0.001(3) C20 0.024(4) 0.029(4) 0.015(4) 0.000(3) 0.002(3) 0.002(3) C19 0.025(4) 0.025(4) 0.014(4) 0.004(3) 0.001(3) -0.003(3) C43 0.024(4) 0.032(4) 0.021(4) 0.009(3) 0.007(3) 0.002(3) C18 0.021(4) 0.027(4) 0.017(4) 0.000(3) 0.001(3) -0.007(3) C44 0.026(4) 0.041(4) 0.014(4) -0.002(3) 0.004(3) 0.000(3) C4 0.027(4) 0.024(4) 0.022(4) 0.001(3) 0.005(3) -0.001(3) C45 0.030(4) 0.031(4) 0.021(4) 0.001(3) 0.001(3) 0.001(3) C3 0.028(4) 0.035(4) 0.028(4) 0.001(3) 0.005(3) 0.004(3) C11 0.023(4) 0.040(4) 0.015(4) -0.002(3) 0.006(3) 0.005(3) C10 0.032(4) 0.040(5) 0.015(4) -0.002(3) 0.004(3) 0.008(3) C29 0.017(4) 0.029(4) 0.031(4) -0.005(3) 0.005(3) 0.002(3) C17 0.024(4) 0.024(4) 0.021(4) 0.002(3) 0.005(3) 0.001(3) C7 0.027(4) 0.034(4) 0.020(4) -0.003(3) 0.006(3) 0.005(3) C33 0.029(4) 0.040(4) 0.017(4) 0.010(3) 0.009(3) -0.002(3) C52 0.025(4) 0.041(5) 0.024(4) -0.004(3) 0.007(3) -0.002(3) C6 0.024(4) 0.033(4) 0.019(4) 0.003(3) 0.003(3) 0.005(3) C34 0.027(4) 0.056(5) 0.017(4) 0.006(4) 0.003(3) 0.008(3) C47 0.028(4) 0.023(4) 0.018(4) 0.002(3) 0.000(3) -0.003(3) C32 0.025(4) 0.046(4) 0.020(4) 0.000(3) 0.009(3) -0.003(3) C25 0.036(4) 0.030(4) 0.019(4) 0.001(3) 0.008(3) 0.005(3) C46 0.025(4) 0.029(4) 0.016(4) -0.003(3) 0.004(3) -0.003(3) C49 0.028(4) 0.033(4) 0.026(4) -0.004(3) 0.001(3) 0.006(3) C2 0.030(4) 0.034(4) 0.019(4) -0.001(3) 0.006(3) 0.001(3) C50 0.041(5) 0.029(4) 0.024(4) -0.004(3) -0.001(3) 0.006(3) C28 0.037(5) 0.041(5) 0.034(5) -0.003(4) 0.001(4) -0.003(4) C31 0.027(4) 0.053(5) 0.021(4) 0.008(4) 0.006(3) 0.005(4) C53 0.028(4) 0.039(4) 0.018(4) 0.002(3) 0.009(3) 0.002(3) C9 0.028(4) 0.042(5) 0.027(4) 0.005(3) 0.012(3) 0.010(3) C56 0.042(5) 0.037(5) 0.050(5) -0.005(4) -0.001(4) -0.001(4) C48 0.030(4) 0.027(4) 0.023(4) -0.003(3) 0.006(3) 0.002(3) C38 0.023(4) 0.080(7) 0.037(5) 0.027(5) 0.010(4) 0.012(4) C5 0.025(4) 0.030(4) 0.020(4) -0.001(3) 0.009(3) -0.003(3) C63 0.035(4) 0.032(4) 0.030(4) -0.007(3) 0.010(3) -0.005(3) C51 0.027(4) 0.040(5) 0.022(4) 0.000(3) 0.005(3) 0.008(3) C24 0.023(4) 0.051(5) 0.026(4) -0.009(4) -0.003(3) 0.004(3) C8 0.026(4) 0.039(4) 0.035(5) 0.007(4) 0.013(3) 0.001(3) C14 0.055(5) 0.031(4) 0.025(4) -0.003(3) 0.011(4) -0.004(4) C30 0.021(4) 0.045(5) 0.030(4) -0.001(4) 0.006(3) 0.006(3) C21 0.029(4) 0.039(5) 0.018(4) -0.002(3) 0.007(3) 0.001(3) C61 0.034(5) 0.046(5) 0.041(5) -0.001(4) 0.011(4) 0.002(4) C65 0.040(5) 0.052(5) 0.034(5) 0.006(4) -0.001(4) 0.007(4) C64 0.035(5) 0.028(4) 0.037(5) -0.006(3) 0.006(4) 0.000(3) C23 0.039(5) 0.040(5) 0.033(5) 0.002(4) 0.006(4) 0.010(4) C66 0.036(5) 0.060(6) 0.022(4) 0.000(4) -0.001(3) -0.004(4) C54 0.042(5) 0.025(4) 0.043(5) 0.009(4) -0.002(4) 0.011(3) C62 0.047(5) 0.033(4) 0.030(4) -0.002(3) 0.015(4) 0.009(4) C39 0.023(4) 0.065(6) 0.026(4) 0.015(4) 0.005(3) 0.007(4) C57 0.061(6) 0.035(5) 0.020(4) 0.005(3) 0.011(4) 0.014(4) C35 0.030(4) 0.060(5) 0.026(4) 0.008(4) 0.010(3) 0.013(4) C60 0.046(5) 0.043(5) 0.032(5) -0.004(4) -0.005(4) 0.014(4) C67 0.063(6) 0.046(5) 0.029(5) -0.012(4) 0.009(4) -0.002(4) C37 0.033(5) 0.077(7) 0.024(5) 0.009(4) 0.012(4) 0.011(4) C55 0.037(5) 0.056(5) 0.030(5) 0.005(4) 0.001(4) 0.013(4) C26 0.052(5) 0.037(5) 0.022(4) -0.001(3) 0.009(4) -0.004(4) C13 0.044(5) 0.074(6) 0.033(5) -0.003(4) 0.020(4) -0.003(4) C36 0.041(5) 0.062(6) 0.029(5) 0.001(4) 0.009(4) 0.022(4) C22 0.045(5) 0.034(4) 0.038(5) 0.005(4) 0.012(4) 0.014(4) C12 0.034(5) 0.033(4) 0.039(5) 0.005(3) 0.006(4) -0.005(3) C40 0.081(7) 0.058(6) 0.045(6) -0.011(5) 0.024(5) -0.003(5) C69 0.079(7) 0.076(7) 0.037(5) 0.032(5) 0.033(5) 0.053(6) C68 0.049(5) 0.035(5) 0.046(5) 0.001(4) 0.009(4) -0.004(4) C59 0.068(7) 0.028(5) 0.064(6) 0.009(4) 0.027(5) 0.007(4) C41 0.068(7) 0.120(9) 0.036(6) 0.019(6) 0.028(5) 0.027(6) C71 0.078(8) 0.058(6) 0.065(7) 0.018(5) 0.029(6) -0.009(5) C58 0.047(5) 0.041(5) 0.064(6) 0.011(4) 0.024(5) 0.011(4) C42 0.037(5) 0.067(6) 0.046(5) 0.012(5) 0.012(4) -0.014(4) C74 0.072(7) 0.081(8) 0.068(7) -0.017(6) 0.027(6) -0.026(6) C72 0.095(10) 0.104(9) 0.067(8) 0.010(7) 0.032(7) -0.003(7) C27 0.049(6) 0.060(6) 0.060(6) 0.001(5) -0.009(5) 0.022(5) C70 0.056(7) 0.124(10) 0.108(10) 0.041(8) 0.027(7) 0.036(7) C73 0.124(11) 0.096(9) 0.090(10) 0.000(7) 0.060(8) -0.036(8) Cl1 0.093(3) 0.095(3) 0.072(2) -0.012(2) 0.018(2) 0.008(2) Cl2 0.196(5) 0.079(3) 0.106(3) -0.022(2) 0.085(3) -0.008(3) C75 0.057(8) 0.106(10) 0.065(9) 0.057(8) -0.017(7) -0.037(7) _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 N1 2.062(5) . ? Fe1 N2 2.073(5) . ? Fe1 N4 2.080(5) . ? Fe1 N3 2.090(6) . ? Fe1 S1 2.243(3) . ? Si1 C63 1.873(7) . ? Si1 C57 1.874(8) . ? Si1 C69 1.953(11) . ? Si1 S1 2.040(3) . ? N3 C32 1.372(8) . ? N3 C29 1.376(8) . ? N2 C18 1.380(8) . ? N2 C15 1.382(8) . ? N1 C1 1.379(8) . ? N1 C4 1.399(8) . ? N4 C46 1.368(8) . ? N4 C43 1.372(8) . ? C15 C5 1.385(9) . ? C15 C16 1.458(9) . ? C1 C5 1.403(9) . ? C1 C2 1.420(9) . ? C16 C17 1.341(9) . ? C16 H16A 0.9300 . ? C20 C21 1.388(9) . ? C20 C25 1.407(9) . ? C20 C19 1.488(9) . ? C19 C29 1.394(9) . ? C19 C18 1.407(9) . ? C43 C33 1.387(9) . ? C43 C44 1.442(9) . ? C18 C17 1.417(9) . ? C44 C45 1.335(9) . ? C44 H44A 0.9300 . ? C4 C3 1.407(9) . ? C4 C47 1.408(9) . ? C45 C46 1.429(9) . ? C45 H45A 0.9300 . ? C3 C2 1.359(9) . ? C3 H3A 0.9300 . ? C11 C6 1.401(9) . ? C11 C10 1.409(9) . ? C11 C14 1.487(9) . ? C10 C9 1.382(10) . ? C10 H10A 0.9300 . ? C29 C30 1.426(10) . ? C17 H17A 0.9300 . ? C7 C8 1.381(9) . ? C7 C6 1.405(9) . ? C7 C12 1.502(9) . ? C33 C32 1.424(9) . ? C33 C34 1.483(10) . ? C52 C51 1.381(9) . ? C52 C53 1.406(9) . ? C52 H52A 0.9300 . ? C6 C5 1.504(10) . ? C34 C39 1.397(10) . ? C34 C35 1.411(10) . ? C47 C46 1.384(9) . ? C47 C48 1.506(9) . ? C32 C31 1.428(10) . ? C25 C24 1.390(9) . ? C25 C28 1.492(9) . ? C49 C50 1.378(9) . ? C49 C48 1.392(9) . ? C49 C54 1.528(9) . ? C2 H2A 0.9300 . ? C50 C51 1.370(9) . ? C50 H50A 0.9300 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C31 C30 1.342(9) . ? C31 H31A 0.9300 . ? C53 C48 1.394(9) . ? C53 C56 1.501(10) . ? C9 C8 1.384(10) . ? C9 C13 1.491(10) . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C38 C37 1.399(11) . ? C38 C39 1.409(11) . ? C38 H38A 0.9300 . ? C63 C64 1.362(9) . ? C63 C68 1.400(10) . ? C51 C55 1.506(9) . ? C24 C23 1.384(10) . ? C24 H24A 0.9300 . ? C8 H8A 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C30 H30A 0.9300 . ? C21 C22 1.402(9) . ? C21 C26 1.504(9) . ? C61 C60 1.371(10) . ? C61 C62 1.387(10) . ? C61 H61A 0.9300 . ? C65 C66 1.345(10) . ? C65 C64 1.392(10) . ? C65 H65A 0.9300 . ? C64 H64A 0.9300 . ? C23 C22 1.390(10) . ? C23 C27 1.506(10) . ? C66 C67 1.360(10) . ? C66 H66A 0.9300 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C62 C57 1.394(11) . ? C62 H62A 0.9300 . ? C39 C42 1.504(11) . ? C57 C58 1.385(10) . ? C35 C36 1.381(10) . ? C35 C40 1.505(11) . ? C60 C59 1.367(11) . ? C60 H60A 0.9300 . ? C67 C68 1.399(10) . ? C67 H67A 0.9300 . ? C37 C36 1.364(11) . ? C37 C41 1.524(11) . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C36 H36A 0.9300 . ? C22 H22A 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C69 C74 1.362(13) . ? C69 C70 1.402(13) . ? C68 H68A 0.9300 . ? C59 C58 1.381(11) . ? C59 H59A 0.9300 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C71 C72 1.341(13) . ? C71 C70 1.440(14) . ? C71 H71A 0.9300 . ? C58 H58A 0.9300 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C74 C73 1.428(13) . ? C74 H74A 0.9300 . ? C72 C73 1.320(14) . ? C72 H72A 0.9300 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C70 H70A 0.9300 . ? C73 H73A 0.9300 . ? Cl1 C75 1.578(11) . ? Cl2 C75 1.846(13) . ? C75 H75A 0.9700 . ? C75 H75B 0.9700 . ? 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 N1 Fe1 N2 86.1(2) . . ? N1 Fe1 N4 86.8(2) . . ? N2 Fe1 N4 151.0(2) . . ? N1 Fe1 N3 150.7(2) . . ? N2 Fe1 N3 86.6(2) . . ? N4 Fe1 N3 86.0(2) . . ? N1 Fe1 S1 113.21(16) . . ? N2 Fe1 S1 110.79(16) . . ? N4 Fe1 S1 97.85(16) . . ? N3 Fe1 S1 95.86(17) . . ? C63 Si1 C57 109.9(3) . . ? C63 Si1 C69 105.8(4) . . ? C57 Si1 C69 107.6(4) . . ? C63 Si1 S1 113.0(2) . . ? C57 Si1 S1 115.9(3) . . ? C69 Si1 S1 103.8(3) . . ? Si1 S1 Fe1 127.09(16) . . ? C32 N3 C29 105.3(6) . . ? C32 N3 Fe1 126.5(4) . . ? C29 N3 Fe1 127.0(4) . . ? C18 N2 C15 106.4(5) . . ? C18 N2 Fe1 126.3(4) . . ? C15 N2 Fe1 126.3(4) . . ? C1 N1 C4 103.6(5) . . ? C1 N1 Fe1 127.9(4) . . ? C4 N1 Fe1 127.2(4) . . ? C46 N4 C43 106.2(5) . . ? C46 N4 Fe1 126.0(4) . . ? C43 N4 Fe1 126.3(4) . . ? N2 C15 C5 126.9(6) . . ? N2 C15 C16 108.5(6) . . ? C5 C15 C16 124.7(6) . . ? N1 C1 C5 125.0(6) . . ? N1 C1 C2 111.1(6) . . ? C5 C1 C2 123.9(6) . . ? C17 C16 C15 107.1(6) . . ? C17 C16 H16A 126.5 . . ? C15 C16 H16A 126.5 . . ? C21 C20 C25 120.6(6) . . ? C21 C20 C19 119.7(6) . . ? C25 C20 C19 119.6(6) . . ? C29 C19 C18 124.3(6) . . ? C29 C19 C20 117.2(6) . . ? C18 C19 C20 118.4(6) . . ? N4 C43 C33 127.3(6) . . ? N4 C43 C44 109.9(6) . . ? C33 C43 C44 122.9(6) . . ? N2 C18 C19 125.9(6) . . ? N2 C18 C17 109.9(6) . . ? C19 C18 C17 124.2(6) . . ? C45 C44 C43 106.2(6) . . ? C45 C44 H44A 126.9 . . ? C43 C44 H44A 126.9 . . ? N1 C4 C3 111.4(6) . . ? N1 C4 C47 123.2(6) . . ? C3 C4 C47 125.3(6) . . ? C44 C45 C46 108.4(6) . . ? C44 C45 H45A 125.8 . . ? C46 C45 H45A 125.8 . . ? C2 C3 C4 106.7(6) . . ? C2 C3 H3A 126.7 . . ? C4 C3 H3A 126.7 . . ? C6 C11 C10 117.4(6) . . ? C6 C11 C14 121.9(6) . . ? C10 C11 C14 120.7(6) . . ? C9 C10 C11 123.0(7) . . ? C9 C10 H10A 118.5 . . ? C11 C10 H10A 118.5 . . ? N3 C29 C19 125.5(6) . . ? N3 C29 C30 109.9(6) . . ? C19 C29 C30 124.7(6) . . ? C16 C17 C18 108.1(6) . . ? C16 C17 H17A 125.9 . . ? C18 C17 H17A 125.9 . . ? C8 C7 C6 118.8(6) . . ? C8 C7 C12 120.2(7) . . ? C6 C7 C12 121.0(6) . . ? C43 C33 C32 122.5(6) . . ? C43 C33 C34 120.6(6) . . ? C32 C33 C34 116.8(6) . . ? C51 C52 C53 121.1(6) . . ? C51 C52 H52A 119.4 . . ? C53 C52 H52A 119.4 . . ? C11 C6 C7 120.7(6) . . ? C11 C6 C5 119.5(6) . . ? C7 C6 C5 119.8(6) . . ? C39 C34 C35 119.9(7) . . ? C39 C34 C33 120.1(7) . . ? C35 C34 C33 120.0(7) . . ? C46 C47 C4 125.7(6) . . ? C46 C47 C48 117.0(6) . . ? C4 C47 C48 117.3(6) . . ? N3 C32 C33 126.0(6) . . ? N3 C32 C31 110.5(6) . . ? C33 C32 C31 123.5(6) . . ? C24 C25 C20 118.4(6) . . ? C24 C25 C28 120.0(6) . . ? C20 C25 C28 121.6(6) . . ? N4 C46 C47 126.2(6) . . ? N4 C46 C45 109.3(6) . . ? C47 C46 C45 124.5(6) . . ? C50 C49 C48 118.4(6) . . ? C50 C49 C54 120.2(6) . . ? C48 C49 C54 121.4(6) . . ? C3 C2 C1 107.2(6) . . ? C3 C2 H2A 126.4 . . ? C1 C2 H2A 126.4 . . ? C51 C50 C49 122.8(7) . . ? C51 C50 H50A 118.6 . . ? C49 C50 H50A 118.6 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C31 C32 106.6(7) . . ? C30 C31 H31A 126.7 . . ? C32 C31 H31A 126.7 . . ? C48 C53 C52 118.4(6) . . ? C48 C53 C56 121.3(6) . . ? C52 C53 C56 120.3(6) . . ? C10 C9 C8 117.3(7) . . ? C10 C9 C13 121.3(7) . . ? C8 C9 C13 121.3(7) . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C49 C48 C53 120.8(6) . . ? C49 C48 C47 119.0(6) . . ? C53 C48 C47 120.1(6) . . ? C37 C38 C39 120.9(8) . . ? C37 C38 H38A 119.6 . . ? C39 C38 H38A 119.6 . . ? C15 C5 C1 123.4(6) . . ? C15 C5 C6 120.1(6) . . ? C1 C5 C6 116.2(6) . . ? C64 C63 C68 116.7(7) . . ? C64 C63 Si1 123.6(5) . . ? C68 C63 Si1 119.6(6) . . ? C50 C51 C52 118.4(6) . . ? C50 C51 C55 121.6(7) . . ? C52 C51 C55 120.0(7) . . ? C23 C24 C25 122.2(7) . . ? C23 C24 H24A 118.9 . . ? C25 C24 H24A 118.9 . . ? C7 C8 C9 122.8(7) . . ? C7 C8 H8A 118.6 . . ? C9 C8 H8A 118.6 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C31 C30 C29 107.7(6) . . ? C31 C30 H30A 126.1 . . ? C29 C30 H30A 126.1 . . ? C20 C21 C22 119.0(6) . . ? C20 C21 C26 121.8(6) . . ? C22 C21 C26 119.2(6) . . ? C60 C61 C62 118.5(8) . . ? C60 C61 H61A 120.7 . . ? C62 C61 H61A 120.7 . . ? C66 C65 C64 120.7(8) . . ? C66 C65 H65A 119.7 . . ? C64 C65 H65A 119.7 . . ? C63 C64 C65 121.3(7) . . ? C63 C64 H64A 119.3 . . ? C65 C64 H64A 119.3 . . ? C24 C23 C22 118.4(7) . . ? C24 C23 C27 120.9(7) . . ? C22 C23 C27 120.6(7) . . ? C65 C66 C67 121.0(7) . . ? C65 C66 H66A 119.5 . . ? C67 C66 H66A 119.5 . . ? C49 C54 H54A 109.5 . . ? C49 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C49 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C61 C62 C57 123.0(7) . . ? C61 C62 H62A 118.5 . . ? C57 C62 H62A 118.5 . . ? C34 C39 C38 119.2(8) . . ? C34 C39 C42 120.7(7) . . ? C38 C39 C42 120.1(7) . . ? C58 C57 C62 115.5(7) . . ? C58 C57 Si1 122.5(7) . . ? C62 C57 Si1 121.9(6) . . ? C36 C35 C34 118.5(8) . . ? C36 C35 C40 120.4(8) . . ? C34 C35 C40 121.1(7) . . ? C59 C60 C61 120.7(8) . . ? C59 C60 H60A 119.6 . . ? C61 C60 H60A 119.6 . . ? C66 C67 C68 118.2(7) . . ? C66 C67 H67A 120.9 . . ? C68 C67 H67A 120.9 . . ? C36 C37 C38 118.2(7) . . ? C36 C37 C41 122.6(8) . . ? C38 C37 C41 119.2(8) . . ? C51 C55 H55A 109.5 . . ? C51 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C51 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C37 C36 C35 123.4(8) . . ? C37 C36 H36A 118.3 . . ? C35 C36 H36A 118.3 . . ? C23 C22 C21 121.3(7) . . ? C23 C22 H22A 119.4 . . ? C21 C22 H22A 119.4 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C35 C40 H40A 109.5 . . ? C35 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C35 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C74 C69 C70 118.2(10) . . ? C74 C69 Si1 124.6(7) . . ? C70 C69 Si1 117.2(9) . . ? C67 C68 C63 122.1(7) . . ? C67 C68 H68A 118.9 . . ? C63 C68 H68A 118.9 . . ? C60 C59 C58 119.5(8) . . ? C60 C59 H59A 120.2 . . ? C58 C59 H59A 120.2 . . ? C37 C41 H41A 109.5 . . ? C37 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C37 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C72 C71 C70 119.5(11) . . ? C72 C71 H71A 120.2 . . ? C70 C71 H71A 120.2 . . ? C59 C58 C57 122.6(8) . . ? C59 C58 H58A 118.7 . . ? C57 C58 H58A 118.7 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C69 C74 C73 121.8(11) . . ? C69 C74 H74A 119.1 . . ? C73 C74 H74A 119.1 . . ? C73 C72 C71 123.1(12) . . ? C73 C72 H72A 118.5 . . ? C71 C72 H72A 118.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C69 C70 C71 118.8(11) . . ? C69 C70 H70A 120.6 . . ? C71 C70 H70A 120.6 . . ? C72 C73 C74 118.6(12) . . ? C72 C73 H73A 120.7 . . ? C74 C73 H73A 120.7 . . ? Cl1 C75 Cl2 116.7(7) . . ? Cl1 C75 H75A 108.1 . . ? Cl2 C75 H75A 108.1 . . ? Cl1 C75 H75B 108.1 . . ? Cl2 C75 H75B 108.1 . . ? H75A C75 H75B 107.3 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 23.10 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.167 _refine_diff_density_min -0.818 _refine_diff_density_rms 0.094 #===END _publ_section_synopsis . #Added by publCIF _publ_section_related_literature ; ? ; #Added by publCIF #============================================================================== _audit_creation_date '2013-04-23' _audit_creation_method SHELXL-97 _audit_update_record ; ? ; #============================================================================== # SUBMISSION DETAILS _publ_requested_journal '' _publ_requested_category ? _publ_contact_author_name '' _publ_contact_author_address ; Department of Chemistry, The University of Texas, One UTSA Circle, San Antonio, Texas 78249-0698, U.S.A. ; _publ_contact_letter ; ; _publ_requested_coeditor_name ' ' _publ_contact_author_phone ' ' _publ_contact_author_fax ' ' _publ_contact_author_email ; hadi.arman@utsa.edu ; #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_paper_category ? _journal_coeditor_notes ; ; _journal_techeditor_code ? _iucr_compatibility_tag ACTA95 _journal_techeditor_notes ; ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; ; _publ_section_title_footnote ; Additional correspondence e-mail: ; loop_ _publ_author_name _publ_author_address '' ; Department of Chemistry The University of Texas at San Antonio One UTSA Circle San Antonio, Texas 78249-0698, USA ; #============================================================================== # TEXT _publ_section_abstract ; (type here to add abstract) ; _publ_section_exptl_refinement ; All H-atoms were placed on calculated positions. Carbon-bound H-atoms were refined with U~iso~(H) =1.2-1.5U~eq~(C). The reflections with Delta(F^2)/esd > 10.0, were omitted. ; #============================================================================== _publ_section_exptl_prep ; (type here to add preparation details) ; #============================================================================== _publ_section_comment ; (type here to add) ; _publ_section_references ; Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Rigaku Americas Corporation (2008). CrystalClear. Rigaku/MSC Inc., The Woodlands, Texas, USA. Rueping, M., Kuenkel, A., Tato, F. & Bats, J. W. (2009). Angew. Chem. Int. Ed. 48, 3699--3702. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany. Westrip, S. P. (2010). publCIF. J. Appl. Cryst. 43. Submitted. ; _publ_section_acknowledgements ; (type here to add acknowledgements) ; _publ_section_figure_captions ; (type here to add) ; _publ_section_table_legends ; ; data_[Fe(NMI)2(TMP)] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H64 Fe N8, 2(C6 H6), C6' _chemical_formula_sum 'C82 H76 Fe N8' _chemical_formula_weight 1229.36 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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'Pcca' _symmetry_space_group_name_Hall '-P 2a 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 23.0929(16) _cell_length_b 14.8314(10) _cell_length_c 19.2077(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6578.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 98(2) _cell_measurement_reflns_used 25629 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.6 _exptl_crystal_description 'platelet' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2600 _exptl_absorpt_coefficient_mu 0.282 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.751 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 98(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Saturn724 (2x2 bin mode) ; _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% '<1' _diffrn_reflns_number 33972 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_reduction_process 'Lp corrections applied' _reflns_number_total 5821 _reflns_number_gt 4510 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010) ; _computing_cell_refinement ; CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010) ; _computing_data_reduction ; CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010) ; _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^)+(0.0500P)^2^+12.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5821 _refine_ls_number_parameters 412 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1349 _refine_ls_wR_factor_gt 0.1251 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 0.5000 0.0000 0.0000 0.01452(14) Uani 1 2 d S . . N1 N 0.57393(8) -0.02527(15) 0.04956(11) 0.0158(5) Uani 1 1 d . . . N3 N 0.45820(9) -0.03764(15) 0.08595(11) 0.0183(5) Uani 1 1 d . . . N2 N 0.50538(9) 0.12753(15) 0.03172(11) 0.0173(5) Uani 1 1 d . . . C20 C 0.39320(11) 0.27599(18) -0.05297(14) 0.0190(6) Uani 1 1 d . . . C7 C 0.69107(11) 0.21316(18) 0.10400(14) 0.0189(6) Uani 1 1 d . . . C17 C 0.48947(11) 0.28075(19) 0.04088(15) 0.0228(6) Uani 1 1 d . . . H17A H 0.4721 0.3369 0.0356 0.027 Uiso 1 1 calc R . . C8 C 0.73080(11) 0.26330(18) 0.14244(14) 0.0193(6) Uani 1 1 d . . . H8A H 0.7643 0.2840 0.1208 0.023 Uiso 1 1 calc R . . C9 C 0.72186(11) 0.28309(18) 0.21193(14) 0.0201(6) Uani 1 1 d . . . C15 C 0.54882(11) 0.16802(18) 0.07021(13) 0.0177(6) Uani 1 1 d . . . C18 C 0.46927(11) 0.19665(18) 0.01220(13) 0.0185(6) Uani 1 1 d . . . C12 C 0.70145(13) 0.1982(2) 0.02758(15) 0.0324(7) Uani 1 1 d . . . H12A H 0.7376 0.2252 0.0145 0.049 Uiso 1 1 calc R . . H12B H 0.6706 0.2252 0.0013 0.049 Uiso 1 1 calc R . . H12C H 0.7027 0.1346 0.0182 0.049 Uiso 1 1 calc R . . C25 C 0.40911(11) 0.31456(19) -0.11657(14) 0.0224(6) Uani 1 1 d . . . C2 C 0.65066(11) -0.10116(19) 0.09990(14) 0.0199(6) Uani 1 1 d . . . H2A H 0.6751 -0.1481 0.1130 0.024 Uiso 1 1 calc R . . N4 N 0.40151(11) -0.11543(19) 0.15541(13) 0.0333(6) Uani 1 1 d . . . C5 C 0.59785(10) 0.12498(18) 0.09632(13) 0.0168(5) Uani 1 1 d . . . C22 C 0.33377(12) 0.40557(19) -0.02888(15) 0.0249(6) Uani 1 1 d . . . H22A H 0.3081 0.4357 0.0003 0.030 Uiso 1 1 calc R . . C16 C 0.53809(11) 0.26269(19) 0.07658(15) 0.0228(6) Uani 1 1 d . . . H16A H 0.5606 0.3040 0.1009 0.027 Uiso 1 1 calc R . . C11 C 0.63122(11) 0.2007(2) 0.20650(14) 0.0218(6) Uani 1 1 d . . . C19 C 0.42129(11) 0.18968(18) -0.03094(13) 0.0173(6) Uani 1 1 d . . . C21 C 0.35488(11) 0.32143(18) -0.00880(14) 0.0199(6) Uani 1 1 d . . . C1 C 0.59929(11) -0.10878(18) 0.05794(13) 0.0171(5) Uani 1 1 d . . . C6 C 0.64104(10) 0.18041(17) 0.13637(14) 0.0169(5) Uani 1 1 d . . . C4 C 0.60859(10) 0.03382(18) 0.08652(13) 0.0163(5) Uani 1 1 d . . . C26 C 0.33858(12) 0.2826(2) 0.06072(14) 0.0263(6) Uani 1 1 d . . . H26A H 0.3122 0.3226 0.0839 0.039 Uiso 1 1 calc R . . H26B H 0.3728 0.2752 0.0886 0.039 Uiso 1 1 calc R . . H26C H 0.3204 0.2250 0.0541 0.039 Uiso 1 1 calc R . . C3 C 0.65689(11) -0.01372(18) 0.11672(14) 0.0193(6) Uani 1 1 d . . . H3A H 0.6867 0.0113 0.1429 0.023 Uiso 1 1 calc R . . C29 C 0.41660(12) -0.0983(2) 0.08957(15) 0.0304(7) Uani 1 1 d . . . H29A H 0.3998 -0.1258 0.0510 0.037 Uiso 1 1 calc R . . C24 C 0.38707(12) 0.3987(2) -0.13433(15) 0.0264(7) Uani 1 1 d . . . H24A H 0.3977 0.4242 -0.1767 0.032 Uiso 1 1 calc R . . C23 C 0.34989(12) 0.44548(19) -0.09108(16) 0.0264(7) Uani 1 1 d . . . C31 C 0.46958(12) -0.0156(2) 0.15299(14) 0.0289(7) Uani 1 1 d . . . H31A H 0.4971 0.0265 0.1670 0.035 Uiso 1 1 calc R . . C10 C 0.67193(12) 0.2518(2) 0.24269(14) 0.0237(6) Uani 1 1 d . . . H10A H 0.6651 0.2652 0.2893 0.028 Uiso 1 1 calc R . . C27 C 0.32881(14) 0.5381(2) -0.1101(2) 0.0400(8) Uani 1 1 d . . . H27A H 0.3035 0.5600 -0.0743 0.060 Uiso 1 1 calc R . . H27B H 0.3082 0.5354 -0.1534 0.060 Uiso 1 1 calc R . . H27C H 0.3613 0.5780 -0.1147 0.060 Uiso 1 1 calc R . . C14 C 0.57698(14) 0.1708(3) 0.24231(16) 0.0407(9) Uani 1 1 d . . . H14A H 0.5536 0.1368 0.2104 0.061 Uiso 1 1 calc R . . H14B H 0.5558 0.2226 0.2579 0.061 Uiso 1 1 calc R . . H14C H 0.5868 0.1337 0.2816 0.061 Uiso 1 1 calc R . . C30 C 0.43546(14) -0.0630(2) 0.19662(16) 0.0351(8) Uani 1 1 d . . . H30A H 0.4352 -0.0604 0.2450 0.042 Uiso 1 1 calc R . . C13 C 0.76401(12) 0.3410(2) 0.25147(16) 0.0281(6) Uani 1 1 d . . . H13A H 0.7958 0.3567 0.2217 0.042 Uiso 1 1 calc R . . H13B H 0.7782 0.3083 0.2911 0.042 Uiso 1 1 calc R . . H13C H 0.7449 0.3949 0.2669 0.042 Uiso 1 1 calc R . . C28 C 0.45161(14) 0.2685(2) -0.16419(16) 0.0335(7) Uani 1 1 d . . . H28A H 0.4572 0.3045 -0.2052 0.050 Uiso 1 1 calc R . . H28B H 0.4368 0.2104 -0.1772 0.050 Uiso 1 1 calc R . . H28C H 0.4879 0.2611 -0.1405 0.050 Uiso 1 1 calc R . . C32 C 0.35699(17) -0.1790(3) 0.17815(19) 0.0553(11) Uani 1 1 d . . . H32A H 0.3397 -0.2070 0.1382 0.083 Uiso 1 1 calc R . . H32B H 0.3278 -0.1474 0.2041 0.083 Uiso 1 1 calc R . . H32C H 0.3743 -0.2244 0.2071 0.083 Uiso 1 1 calc R . . C37 C 0.3612(2) 0.5635(4) 0.1126(3) 0.093(2) Uani 1 1 d . . . H37A H 0.3262 0.5909 0.1013 0.111 Uiso 1 1 calc R . . C35 C 0.4612(2) 0.5459(4) 0.0960(3) 0.0788(16) Uani 1 1 d . . . H35A H 0.4945 0.5620 0.0718 0.095 Uiso 1 1 calc R . . C36 C 0.4094(2) 0.5858(4) 0.0785(3) 0.0829(16) Uani 1 1 d . . . H36A H 0.4081 0.6283 0.0429 0.099 Uiso 1 1 calc R . . C33 C 0.4167(3) 0.4593(4) 0.1828(3) 0.098(2) Uani 1 1 d . . . H33A H 0.4185 0.4167 0.2182 0.118 Uiso 1 1 calc R . . C34 C 0.4653(3) 0.4827(4) 0.1485(3) 0.0854(17) Uani 1 1 d . . . H34A H 0.5007 0.4569 0.1600 0.103 Uiso 1 1 calc R . . C38 C 0.3637(3) 0.4984(5) 0.1655(3) 0.099(2) Uani 1 1 d . . . H38A H 0.3302 0.4815 0.1889 0.118 Uiso 1 1 calc R . . C39 C 0.77660(14) 0.0223(2) -0.07289(17) 0.0376(8) Uani 1 1 d . . . C40 C 0.80281(17) 0.0453(3) -0.1347(2) 0.0531(10) Uani 1 1 d . . . C41 C 0.7758(3) 0.0236(4) -0.1966(2) 0.093(2) Uani 1 1 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 0.0143(2) 0.0118(3) 0.0175(3) 0.0002(2) -0.0014(2) 0.0012(2) N1 0.0160(10) 0.0135(12) 0.0179(11) 0.0004(9) -0.0001(8) 0.0007(8) N3 0.0168(11) 0.0158(12) 0.0223(11) 0.0009(10) -0.0016(9) 0.0007(9) N2 0.0164(10) 0.0154(11) 0.0202(11) -0.0003(9) -0.0020(9) 0.0020(9) C20 0.0204(13) 0.0133(14) 0.0234(14) -0.0011(11) -0.0080(11) 0.0009(11) C7 0.0181(13) 0.0131(14) 0.0255(14) -0.0024(11) 0.0014(10) 0.0037(11) C17 0.0238(14) 0.0124(14) 0.0322(15) -0.0012(12) -0.0056(12) 0.0046(11) C8 0.0145(12) 0.0135(14) 0.0298(14) -0.0002(12) 0.0011(10) 0.0027(10) C9 0.0194(13) 0.0143(14) 0.0265(14) 0.0009(12) -0.0053(11) 0.0029(11) C15 0.0189(13) 0.0141(14) 0.0202(13) -0.0020(11) -0.0009(10) -0.0016(10) C18 0.0193(13) 0.0140(14) 0.0223(13) 0.0026(11) -0.0012(10) 0.0017(10) C12 0.0280(15) 0.039(2) 0.0299(16) -0.0120(15) 0.0084(12) -0.0107(14) C25 0.0230(14) 0.0190(15) 0.0251(14) 0.0003(12) -0.0045(11) 0.0010(11) C2 0.0190(13) 0.0181(15) 0.0227(14) 0.0013(12) -0.0032(10) 0.0045(11) N4 0.0351(14) 0.0391(17) 0.0258(13) 0.0019(12) 0.0004(11) -0.0168(12) C5 0.0157(12) 0.0164(14) 0.0184(13) -0.0001(11) 0.0015(10) -0.0008(10) C22 0.0228(14) 0.0174(15) 0.0345(16) -0.0036(13) -0.0059(12) 0.0048(11) C16 0.0224(14) 0.0163(15) 0.0299(15) -0.0042(12) -0.0050(11) -0.0023(11) C11 0.0212(13) 0.0203(15) 0.0238(14) 0.0014(12) 0.0001(11) -0.0012(11) C19 0.0189(13) 0.0139(14) 0.0193(13) -0.0008(11) 0.0004(10) 0.0027(10) C21 0.0188(12) 0.0160(14) 0.0249(14) -0.0018(12) -0.0071(11) 0.0003(11) C1 0.0176(12) 0.0150(14) 0.0187(13) 0.0010(11) 0.0010(10) 0.0031(11) C6 0.0166(12) 0.0108(13) 0.0233(13) 0.0006(11) -0.0030(10) 0.0020(10) C4 0.0164(12) 0.0163(14) 0.0163(12) -0.0001(11) 0.0002(10) -0.0015(10) C26 0.0273(15) 0.0272(17) 0.0244(14) -0.0017(13) -0.0008(12) 0.0041(12) C3 0.0160(12) 0.0193(16) 0.0225(13) -0.0011(12) -0.0034(10) 0.0009(11) C29 0.0294(15) 0.038(2) 0.0240(15) -0.0006(14) -0.0008(12) -0.0127(14) C24 0.0284(15) 0.0228(16) 0.0281(15) 0.0093(13) -0.0076(12) -0.0036(12) C23 0.0236(14) 0.0150(15) 0.0405(17) 0.0046(13) -0.0116(12) 0.0004(12) C31 0.0296(15) 0.0348(19) 0.0222(14) -0.0033(14) -0.0011(12) -0.0109(13) C10 0.0269(14) 0.0246(16) 0.0198(13) -0.0012(12) -0.0018(11) -0.0027(12) C27 0.0354(17) 0.0224(17) 0.062(2) 0.0118(17) -0.0092(16) 0.0058(14) C14 0.0363(18) 0.061(2) 0.0250(16) -0.0040(17) 0.0064(13) -0.0216(17) C30 0.0438(18) 0.041(2) 0.0210(15) 0.0003(14) -0.0005(13) -0.0137(15) C13 0.0259(15) 0.0257(16) 0.0327(15) -0.0027(14) -0.0064(12) -0.0031(12) C28 0.0444(18) 0.0281(18) 0.0279(16) 0.0025(14) 0.0077(14) 0.0036(15) C32 0.061(2) 0.070(3) 0.0351(19) 0.005(2) 0.0076(17) -0.042(2) C37 0.083(4) 0.088(4) 0.108(5) -0.054(4) 0.033(3) -0.018(3) C35 0.069(3) 0.081(4) 0.087(4) -0.026(3) 0.014(3) -0.029(3) C36 0.081(4) 0.088(4) 0.080(3) -0.027(3) 0.015(3) -0.034(3) C33 0.115(5) 0.079(4) 0.101(4) -0.046(3) 0.043(4) -0.030(4) C34 0.091(4) 0.062(4) 0.103(4) -0.033(3) 0.025(3) -0.022(3) C38 0.103(4) 0.089(4) 0.104(5) -0.051(4) 0.064(4) -0.048(4) C39 0.0447(18) 0.0287(19) 0.0393(18) -0.0068(15) -0.0055(15) 0.0094(14) C40 0.054(2) 0.047(2) 0.059(2) -0.019(2) 0.0220(19) -0.0137(19) C41 0.157(5) 0.086(4) 0.036(2) -0.015(2) 0.028(3) -0.067(4) _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 N1 1.990(2) 5_655 ? Fe1 N1 1.990(2) . ? Fe1 N2 1.991(2) 5_655 ? Fe1 N2 1.991(2) . ? Fe1 N3 1.992(2) . ? Fe1 N3 1.992(2) 5_655 ? N1 C1 1.380(3) . ? N1 C4 1.383(3) . ? N3 C29 1.318(4) . ? N3 C31 1.354(3) . ? N2 C18 1.374(3) . ? N2 C15 1.383(3) . ? C20 C25 1.398(4) . ? C20 C21 1.399(4) . ? C20 C19 1.496(4) . ? C7 C8 1.393(4) . ? C7 C6 1.399(4) . ? C7 C12 1.504(4) . ? C17 C16 1.343(4) . ? C17 C18 1.441(4) . ? C17 H17A 0.9300 . ? C8 C9 1.382(4) . ? C8 H8A 0.9300 . ? C9 C10 1.376(4) . ? C9 C13 1.503(4) . ? C15 C5 1.393(4) . ? C15 C16 1.431(4) . ? C18 C19 1.387(4) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C25 C24 1.390(4) . ? C25 C28 1.506(4) . ? C2 C3 1.344(4) . ? C2 C1 1.439(4) . ? C2 H2A 0.9300 . ? N4 C29 1.336(4) . ? N4 C30 1.358(4) . ? N4 C32 1.462(4) . ? C5 C4 1.387(4) . ? C5 C6 1.504(4) . ? C22 C23 1.384(4) . ? C22 C21 1.394(4) . ? C22 H22A 0.9300 . ? C16 H16A 0.9300 . ? C11 C10 1.393(4) . ? C11 C6 1.399(4) . ? C11 C14 1.496(4) . ? C19 C1 1.391(4) 5_655 ? C21 C26 1.502(4) . ? C1 C19 1.391(4) 5_655 ? C4 C3 1.441(4) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C3 H3A 0.9300 . ? C29 H29A 0.9300 . ? C24 C23 1.382(4) . ? C24 H24A 0.9300 . ? C23 C27 1.502(4) . ? C31 C30 1.348(4) . ? C31 H31A 0.9300 . ? C10 H10A 0.9300 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C30 H30A 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C37 C36 1.334(7) . ? C37 C38 1.403(9) . ? C37 H37A 0.9300 . ? C35 C36 1.376(8) . ? C35 C34 1.379(8) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? C33 C34 1.347(7) . ? C33 C38 1.395(9) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C38 H38A 0.9300 . ? C39 C40 1.377(5) . ? C39 C39 1.395(7) 2_655 ? C40 C41 1.379(6) . ? C41 C41 1.383(10) 2_655 ? 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 N1 Fe1 N1 180.00(17) 5_655 . ? N1 Fe1 N2 88.80(9) 5_655 5_655 ? N1 Fe1 N2 91.20(9) . 5_655 ? N1 Fe1 N2 91.20(9) 5_655 . ? N1 Fe1 N2 88.80(9) . . ? N2 Fe1 N2 180.0 5_655 . ? N1 Fe1 N3 91.92(8) 5_655 . ? N1 Fe1 N3 88.08(8) . . ? N2 Fe1 N3 87.55(9) 5_655 . ? N2 Fe1 N3 92.45(9) . . ? N1 Fe1 N3 88.08(8) 5_655 5_655 ? N1 Fe1 N3 91.92(8) . 5_655 ? N2 Fe1 N3 92.45(9) 5_655 5_655 ? N2 Fe1 N3 87.55(9) . 5_655 ? N3 Fe1 N3 180.00(18) . 5_655 ? C1 N1 C4 105.3(2) . . ? C1 N1 Fe1 126.09(17) . . ? C4 N1 Fe1 128.51(17) . . ? C29 N3 C31 104.8(2) . . ? C29 N3 Fe1 126.02(19) . . ? C31 N3 Fe1 128.77(19) . . ? C18 N2 C15 105.2(2) . . ? C18 N2 Fe1 125.99(17) . . ? C15 N2 Fe1 128.40(17) . . ? C25 C20 C21 119.9(2) . . ? C25 C20 C19 118.9(2) . . ? C21 C20 C19 121.0(2) . . ? C8 C7 C6 119.6(2) . . ? C8 C7 C12 119.4(2) . . ? C6 C7 C12 120.9(2) . . ? C16 C17 C18 107.1(2) . . ? C16 C17 H17A 126.5 . . ? C18 C17 H17A 126.5 . . ? C9 C8 C7 121.8(2) . . ? C9 C8 H8A 119.1 . . ? C7 C8 H8A 119.1 . . ? C10 C9 C8 117.9(2) . . ? C10 C9 C13 121.2(3) . . ? C8 C9 C13 120.8(2) . . ? N2 C15 C5 125.7(2) . . ? N2 C15 C16 110.2(2) . . ? C5 C15 C16 124.0(2) . . ? N2 C18 C19 126.3(2) . . ? N2 C18 C17 110.2(2) . . ? C19 C18 C17 123.5(2) . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C24 C25 C20 119.0(3) . . ? C24 C25 C28 119.8(3) . . ? C20 C25 C28 121.1(3) . . ? C3 C2 C1 107.4(2) . . ? C3 C2 H2A 126.3 . . ? C1 C2 H2A 126.3 . . ? C29 N4 C30 107.0(2) . . ? C29 N4 C32 126.1(3) . . ? C30 N4 C32 126.9(3) . . ? C4 C5 C15 122.9(2) . . ? C4 C5 C6 118.9(2) . . ? C15 C5 C6 118.2(2) . . ? C23 C22 C21 121.8(3) . . ? C23 C22 H22A 119.1 . . ? C21 C22 H22A 119.1 . . ? C17 C16 C15 107.3(2) . . ? C17 C16 H16A 126.4 . . ? C15 C16 H16A 126.4 . . ? C10 C11 C6 119.2(2) . . ? C10 C11 C14 119.8(3) . . ? C6 C11 C14 121.0(2) . . ? C18 C19 C1 124.0(2) . 5_655 ? C18 C19 C20 116.8(2) . . ? C1 C19 C20 119.0(2) 5_655 . ? C22 C21 C20 119.0(3) . . ? C22 C21 C26 120.1(3) . . ? C20 C21 C26 120.8(2) . . ? N1 C1 C19 125.9(2) . 5_655 ? N1 C1 C2 110.2(2) . . ? C19 C1 C2 124.0(2) 5_655 . ? C11 C6 C7 119.2(2) . . ? C11 C6 C5 120.2(2) . . ? C7 C6 C5 120.7(2) . . ? N1 C4 C5 125.7(2) . . ? N1 C4 C3 110.1(2) . . ? C5 C4 C3 124.1(2) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C2 C3 C4 107.0(2) . . ? C2 C3 H3A 126.5 . . ? C4 C3 H3A 126.5 . . ? N3 C29 N4 111.7(3) . . ? N3 C29 H29A 124.2 . . ? N4 C29 H29A 124.2 . . ? C23 C24 C25 122.1(3) . . ? C23 C24 H24A 119.0 . . ? C25 C24 H24A 119.0 . . ? C24 C23 C22 118.1(3) . . ? C24 C23 C27 121.0(3) . . ? C22 C23 C27 120.9(3) . . ? C30 C31 N3 110.6(3) . . ? C30 C31 H31A 124.7 . . ? N3 C31 H31A 124.7 . . ? C9 C10 C11 122.3(3) . . ? C9 C10 H10A 118.8 . . ? C11 C10 H10A 118.8 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C31 C30 N4 105.9(3) . . ? C31 C30 H30A 127.1 . . ? N4 C30 H30A 127.1 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N4 C32 H32A 109.5 . . ? N4 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N4 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C36 C37 C38 119.4(6) . . ? C36 C37 H37A 120.3 . . ? C38 C37 H37A 120.3 . . ? C36 C35 C34 122.0(5) . . ? C36 C35 H35A 119.0 . . ? C34 C35 H35A 119.0 . . ? C37 C36 C35 119.9(6) . . ? C37 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? C34 C33 C38 120.4(7) . . ? C34 C33 H33A 119.8 . . ? C38 C33 H33A 119.8 . . ? C33 C34 C35 118.4(6) . . ? C33 C34 H34A 120.8 . . ? C35 C34 H34A 120.8 . . ? C33 C38 C37 119.7(5) . . ? C33 C38 H38A 120.1 . . ? C37 C38 H38A 120.1 . . ? C40 C39 C39 120.3(2) . 2_655 ? C39 C40 C41 119.1(4) . . ? C40 C41 C41 120.5(2) . 2_655 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.534 _refine_diff_density_min -0.422 _refine_diff_density_rms 0.064