#\#CIF_1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-03-25 at 11:21:59 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : car01 apexiitemplate #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_global #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2011-03-25 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ? #------------------ AUTHOR DETAILS -------------------------------------------# # Name and address of author for correspondence _publ_contact_author_name 'Werner Kaminsky' _publ_contact_author_address ; Department of Chemistry University of Washington Seattle Washington, 98195, USA ; _publ_contact_author_email kaminsky@chem.washington.edu _publ_contact_author_fax '00(206)6858665' _publ_contact_author_phone '00(206)5437585' _publ_requested_journal 'Journal title here' _publ_section_title ; title here ; loop_ _publ_author_name _publ_author_address 'Caroline Saouma' ; Department of Chemistry Univ. of Washington Seattle, WA 98195 USA ; 'Werner Kaminsky' ; Department of Chemistry Univ. of Washington Seattle, WA 98195 USA ; 'James Mayer' ; Department of Chemistry Univ. of Washington Seattle, WA 98195 USA ; _publ_section_abstract ; Abstract here ; _publ_section_comment ; Details and comments here ; _publ_section_exptl_prep ; details of preparation here ; _publ_section_exptl_refinement ; All H atoms were initially located in a difference Fourier map and were refined with a riding model. H atoms were placed in geometrically idealised positions and constrained to ride on their parent atoms with C---H distances in the range 0.95-1.00 \%A. U~iso~ values were fixed such that they were 1.2U~eq~ of their parent atom U~eq~ for CH's and 1.5U~eq~ of their parent atom U~eq~ in case of methyl groups. ; # Insert blank lines between references _publ_section_references ; Bruker (2007) APEX2 (Version 2.1-4), SAINT (version 7.34A), SADABS (version 2007/4), BrukerAXS Inc, Madison, Wisconsin, USA. Flack H. D. & Bernardinelli, G. (71999). Acta Cryst. A55, 908-915. Flack H. D. & Bernardinelli, G. (2000). J. Appl. Cryst. 33, 1143-1148. Cambridge Structural Database: Allen, F. R. (2002). Acta Cryst. B58, 380-388. CrysAlis CCD, CrysAlis RED and associated programs: Oxford Diffraction (2006). Program name(s). Oxford Diffraction Ltd, Abingdon, England. COLLECT: Nonius [or Hooft, R. W. W.] (1998). COLLECT. Nonius BV, Delft, The Netherlands. DENZO/SCALEPACK: Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press. DIRDIF99: Beurskens, P.T., Beurskens, G., de Gelder, R., Garci\'ia-Granda, S., Gould, R.O., Israel, R. & Smits, J.M.M. (1999) The DIRDIF-99 program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. ORTEP-3: Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. PARST: Nardelli, M. (1995). J. Appl. Cryst. 28, 659. PLATON: Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. publCIF: Westrip, S. P. (2008). publCIF. In preparation. SADABS, TWINABS: Bruker (2001). Program name. Bruker AXS Inc., Madison, Wisconsin, USA. or Sheldrick, G. M. (1996). Program name. University of Göttingen, Germany. SHELX Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. SIR97: Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119. SIR2002: Burla, M. C., Camalli, M., Carrozzini, B., Cascarano, G. L., Giacovazzo, C., Polidori, G. & Spagna, R. (2003). J. Appl. Cryst. 36, 1103. WinGX: Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. ; # start Validation Reply Form _vrf_PLAT411_I ; PROBLEM: Short Inter H...H Contact H28B .. H20B .. 1.79 Ang. RESPONSE: Disordered pentane on symmetry center leads to additional bond messages of no physical consequence. ; _vrf_PLAT413_I ; PROBLEM: Short Inter XH3 .. XHn H27A .. H30G .. 1.53 Ang. RESPONSE: see above ; # end Validation Reply Form #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_car01 _audit_creation_date 2011-03-25T11:21:59-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; car01 ; _chemical_name_common car01 _chemical_formula_moiety 'C42 H44 Fe2 N8 S2, 0.25(C20 H48), 2(C8 H20 N)' _chemical_formula_sum 'C63 H96 Fe2 N10 S2' _chemical_formula_weight 1169.32 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 10.3343(5) _cell_length_b 19.1546(9) _cell_length_c 16.1851(8) _cell_angle_alpha 90 _cell_angle_beta 107.652(3) _cell_angle_gamma 90 _cell_volume 3053.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 350 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_special_details ; 20 seconds exposure at 0.5 degree steps per frame ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.591 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2007)' _exptl_absorpt_correction_T_min 0.9166 _exptl_absorpt_correction_T_max 0.9542 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_av_R_equivalents 0.0788 _diffrn_reflns_av_unetI/netI 0.0476 _diffrn_reflns_number 86220 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 28.66 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 0.982 _reflns_number_total 7698 _reflns_number_gt 5401 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0698P)^2^+4.9105P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7698 _refine_ls_number_parameters 362 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0912 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1558 _refine_ls_wR_factor_gt 0.1307 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.941 _refine_diff_density_min -1.213 _refine_diff_density_rms 0.094 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8124(4) 0.3124(2) 0.5073(2) 0.0362(8) Uani 1 1 d . . . H1A H 0.8556 0.2731 0.5443 0.054 Uiso 1 1 calc R . . H1B H 0.8229 0.3549 0.5425 0.054 Uiso 1 1 calc R . . H1C H 0.8555 0.3191 0.4617 0.054 Uiso 1 1 calc R . . C2 C 0.6628(3) 0.29703(17) 0.4665(2) 0.0286(7) Uani 1 1 d . . . H2A H 0.619 0.3369 0.4296 0.034 Uiso 1 1 calc R . . H2B H 0.6189 0.2913 0.5126 0.034 Uiso 1 1 calc R . . C3 C 0.6424(3) 0.23048(14) 0.41125(19) 0.0204(6) Uani 1 1 d . . . H3A H 0.6761 0.1903 0.4503 0.024 Uiso 1 1 calc R . . H3B H 0.6994 0.234 0.3721 0.024 Uiso 1 1 calc R . . C4 C 0.4937(3) 0.21465(14) 0.35529(18) 0.0180(6) Uani 1 1 d . . . C5 C 0.4425(3) 0.27428(14) 0.28886(18) 0.0206(6) Uani 1 1 d . . . H5A H 0.4412 0.3181 0.321 0.025 Uiso 1 1 calc R . . H5B H 0.5083 0.2805 0.256 0.025 Uiso 1 1 calc R . . C6 C 0.3022(3) 0.26312(15) 0.2246(2) 0.0244(6) Uani 1 1 d . . . H6A H 0.2365 0.2539 0.2569 0.029 Uiso 1 1 calc R . . H6B H 0.3043 0.2216 0.1887 0.029 Uiso 1 1 calc R . . C7 C 0.2546(4) 0.32601(17) 0.1658(2) 0.0340(8) Uani 1 1 d . . . H7A H 0.2531 0.3673 0.2012 0.051 Uiso 1 1 calc R . . H7B H 0.1631 0.3172 0.1267 0.051 Uiso 1 1 calc R . . H7C H 0.317 0.334 0.1316 0.051 Uiso 1 1 calc R . . C8 C 0.4069(3) 0.21040(14) 0.41534(17) 0.0170(5) Uani 1 1 d . . . C9 C 0.3245(3) 0.17450(14) 0.51727(18) 0.0194(6) Uani 1 1 d . . . C10 C 0.2821(3) 0.13958(16) 0.5799(2) 0.0264(7) Uani 1 1 d . . . H10 H 0.3091 0.0928 0.5959 0.032 Uiso 1 1 calc R . . C11 C 0.1987(4) 0.17581(18) 0.6180(2) 0.0298(7) Uani 1 1 d . . . H11 H 0.1695 0.1534 0.6615 0.036 Uiso 1 1 calc R . . C12 C 0.1565(3) 0.24419(18) 0.5943(2) 0.0289(7) Uani 1 1 d . . . H12 H 0.0999 0.2674 0.6221 0.035 Uiso 1 1 calc R . . C13 C 0.1964(3) 0.27846(17) 0.5306(2) 0.0259(6) Uani 1 1 d . . . H13 H 0.1672 0.3248 0.5137 0.031 Uiso 1 1 calc R . . C14 C 0.2808(3) 0.24294(15) 0.49198(18) 0.0203(6) Uani 1 1 d . . . C15 C 0.4993(3) 0.14749(14) 0.30603(17) 0.0165(5) Uani 1 1 d . . . C16 C 0.4979(3) 0.03778(15) 0.27097(19) 0.0224(6) Uani 1 1 d . . . C17 C 0.4898(5) -0.03454(17) 0.2627(2) 0.0390(9) Uani 1 1 d . . . H17 H 0.4677 -0.0628 0.3047 0.047 Uiso 1 1 calc R . . C18 C 0.5150(5) -0.06369(18) 0.1911(2) 0.0484(11) Uani 1 1 d . . . H18 H 0.5105 -0.113 0.184 0.058 Uiso 1 1 calc R . . C19 C 0.5471(4) -0.02224(17) 0.1285(2) 0.0335(8) Uani 1 1 d . . . H19 H 0.5644 -0.0438 0.0801 0.04 Uiso 1 1 calc R . . C20 C 0.5537(3) 0.04939(16) 0.13658(19) 0.0247(6) Uani 1 1 d . . . H20 H 0.5745 0.0776 0.094 0.03 Uiso 1 1 calc R . . C21 C 0.5293(3) 0.07933(15) 0.20886(18) 0.0201(6) Uani 1 1 d . . . C22 C 0.4857(3) -0.40768(17) 0.1045(2) 0.0284(7) Uani 1 1 d . . . H22A H 0.4175 -0.4452 0.0846 0.034 Uiso 1 1 calc R . . H22B H 0.4427 -0.3634 0.0784 0.034 Uiso 1 1 calc R . . C23 C 0.6035(4) -0.4227(2) 0.0709(2) 0.0379(8) Uani 1 1 d . . . H23A H 0.6764 -0.389 0.0955 0.057 Uiso 1 1 calc R . . H23B H 0.5738 -0.4189 0.0075 0.057 Uiso 1 1 calc R . . H23C H 0.637 -0.4701 0.0877 0.057 Uiso 1 1 calc R . . C24 C 0.6117(3) -0.33923(16) 0.2358(2) 0.0294(7) Uani 1 1 d . . . H24A H 0.6316 -0.3371 0.2996 0.035 Uiso 1 1 calc R . . H24B H 0.6989 -0.3468 0.2236 0.035 Uiso 1 1 calc R . . C25 C 0.5549(4) -0.26956(17) 0.1983(3) 0.0358(8) Uani 1 1 d . . . H25A H 0.5403 -0.2697 0.1356 0.054 Uiso 1 1 calc R . . H25B H 0.6193 -0.2325 0.2252 0.054 Uiso 1 1 calc R . . H25C H 0.4684 -0.2612 0.2098 0.054 Uiso 1 1 calc R . . C26 C 0.3877(3) -0.39479(17) 0.2218(2) 0.0305(7) Uani 1 1 d . . . H26A H 0.3312 -0.4361 0.198 0.037 Uiso 1 1 calc R . . H26B H 0.3397 -0.3532 0.1909 0.037 Uiso 1 1 calc R . . C27 C 0.3989(4) -0.3881(2) 0.3168(2) 0.0414(9) Uani 1 1 d . . . H27A H 0.4491 -0.4282 0.3487 0.062 Uiso 1 1 calc R . . H27B H 0.3078 -0.387 0.3235 0.062 Uiso 1 1 calc R . . H27C H 0.4471 -0.3449 0.34 0.062 Uiso 1 1 calc R . . C28 C 0.5995(3) -0.46512(17) 0.2467(2) 0.0283(7) Uani 1 1 d . . . H28A H 0.6848 -0.4683 0.2311 0.034 Uiso 1 1 calc R . . H28B H 0.6246 -0.4582 0.3103 0.034 Uiso 1 1 calc R . . C29 C 0.5243(4) -0.53350(17) 0.2243(3) 0.0374(8) Uani 1 1 d . . . H29A H 0.4425 -0.5322 0.2429 0.056 Uiso 1 1 calc R . . H29B H 0.5831 -0.5718 0.254 0.056 Uiso 1 1 calc R . . H29C H 0.4984 -0.5409 0.1615 0.056 Uiso 1 1 calc R . . C200 C 0.3373(6) 0.5040(3) 0.5415(9) 0.0286(8) Uiso 0.25 1 d PRD A -1 H20A H 0.4322 0.5137 0.5745 0.043 Uiso 0.25 1 d PR B -1 H20B H 0.2925 0.4805 0.579 0.043 Uiso 0.25 1 d PR C -1 H20C H 0.2902 0.5481 0.5204 0.043 Uiso 0.25 1 d PR D -1 C201 C 0.3294(8) 0.4707(8) 0.4743(11) 0.0286(8) Uiso 0.25 1 d PD A -1 H20D H 0.2609 0.4958 0.4276 0.034 Uiso 0.25 1 calc PR A -1 H20E H 0.2869 0.4257 0.4815 0.034 Uiso 0.25 1 calc PR A -1 C202 C 0.4501(11) 0.4501(7) 0.4325(8) 0.0286(8) Uiso 0.25 1 d PD A -1 H20F H 0.4583 0.3987 0.4294 0.034 Uiso 0.25 1 calc PR A -1 H20G H 0.4296 0.4693 0.3731 0.034 Uiso 0.25 1 calc PR A -1 C203 C 0.5887(11) 0.4829(7) 0.4942(7) 0.0286(8) Uiso 0.25 1 d PD A -1 H20H H 0.5655 0.5257 0.521 0.034 Uiso 0.25 1 calc PR A -1 H20I H 0.6282 0.4493 0.5416 0.034 Uiso 0.25 1 calc PR A -1 C204 C 0.6774(13) 0.4981(7) 0.4607(10) 0.0286(8) Uiso 0.25 1 d PD A -1 H20J H 0.6867 0.4602 0.4223 0.043 Uiso 0.25 1 calc PR A -1 H20K H 0.764 0.505 0.5062 0.043 Uiso 0.25 1 calc PR A -1 H20L H 0.652 0.5413 0.4271 0.043 Uiso 0.25 1 calc PR A -1 C300 C 0.3561(12) 0.4499(7) 0.4258(7) 0.0286(8) Uiso 0.25 1 d PD E -2 H30A H 0.4076 0.4781 0.3962 0.043 Uiso 0.25 1 calc PR E -2 H30B H 0.2701 0.4353 0.384 0.043 Uiso 0.25 1 calc PR E -2 H30C H 0.4091 0.4086 0.4512 0.043 Uiso 0.25 1 calc PR E -2 C301 C 0.3325(9) 0.4851(7) 0.4841(11) 0.0286(8) Uiso 0.25 1 d PD E -2 H30D H 0.2771 0.4542 0.509 0.034 Uiso 0.25 1 calc PR E -2 H30E H 0.2705 0.5225 0.4533 0.034 Uiso 0.25 1 calc PR E -2 C302 C 0.4380(11) 0.5238(7) 0.5678(7) 0.0286(8) Uiso 0.25 1 d PD E -2 H30F H 0.3962 0.5667 0.5825 0.034 Uiso 0.25 1 calc PR E -2 H30G H 0.4611 0.4924 0.6188 0.034 Uiso 0.25 1 calc PR E -2 C303 C 0.5722(11) 0.5430(7) 0.5422(7) 0.0286(8) Uiso 0.25 1 d PD E -2 H30H H 0.6006 0.5009 0.5169 0.034 Uiso 0.25 1 calc PR E -2 H30I H 0.5475 0.579 0.4962 0.034 Uiso 0.25 1 calc PR E -2 C304 C 0.6711(11) 0.5645(7) 0.6006(8) 0.0286(8) Uiso 0.25 1 d PD E -2 H30J H 0.6979 0.6105 0.5848 0.043 Uiso 0.25 1 calc PR E -2 H30K H 0.7469 0.5318 0.6089 0.043 Uiso 0.25 1 calc PR E -2 H30L H 0.6472 0.5683 0.6546 0.043 Uiso 0.25 1 calc PR E -2 N1 N 0.4062(3) 0.15371(12) 0.46758(15) 0.0192(5) Uani 1 1 d . . . N2 N 0.3342(3) 0.26473(12) 0.42693(16) 0.0215(5) Uani 1 1 d . . . N3 N 0.4787(3) 0.08219(12) 0.33431(15) 0.0194(5) Uani 1 1 d . . . N4 N 0.5302(3) 0.14883(12) 0.23239(16) 0.0215(5) Uani 1 1 d . . . N5 N 0.5212(3) -0.40181(13) 0.20248(17) 0.0239(5) Uani 1 1 d . . . S1 S 0.33178(8) -0.02514(4) 0.45845(5) 0.02044(16) Uani 1 1 d . . . Fe1 Fe 0.47188(4) 0.059144(19) 0.45216(2) 0.01678(12) 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 C1 0.038(2) 0.0366(19) 0.0327(18) -0.0080(15) 0.0085(15) -0.0102(15) C2 0.0335(18) 0.0232(15) 0.0276(16) -0.0079(12) 0.0070(14) -0.0015(13) C3 0.0250(15) 0.0151(13) 0.0210(14) -0.0010(10) 0.0070(12) 0.0001(11) C4 0.0260(15) 0.0102(12) 0.0178(13) 0.0005(10) 0.0069(11) -0.0003(10) C5 0.0319(16) 0.0113(12) 0.0198(13) 0.0027(10) 0.0097(12) 0.0014(11) C6 0.0333(17) 0.0163(13) 0.0217(14) 0.0041(11) 0.0052(13) 0.0032(12) C7 0.047(2) 0.0230(16) 0.0261(16) 0.0060(13) 0.0026(15) 0.0073(15) C8 0.0212(14) 0.0121(12) 0.0165(13) 0.0014(10) 0.0039(11) 0.0016(10) C9 0.0255(15) 0.0166(13) 0.0177(13) -0.0013(10) 0.0088(11) -0.0013(11) C10 0.0382(18) 0.0203(14) 0.0236(15) -0.0005(12) 0.0135(13) -0.0032(13) C11 0.041(2) 0.0317(17) 0.0225(15) -0.0045(13) 0.0186(14) -0.0086(14) C12 0.0303(17) 0.0349(17) 0.0251(15) -0.0081(13) 0.0136(14) 0.0015(14) C13 0.0289(17) 0.0250(15) 0.0246(15) -0.0043(12) 0.0091(13) 0.0046(12) C14 0.0257(15) 0.0178(13) 0.0175(13) -0.0011(10) 0.0068(12) 0.0016(11) C15 0.0197(14) 0.0126(12) 0.0166(12) 0.0017(10) 0.0044(11) 0.0010(10) C16 0.0355(17) 0.0148(13) 0.0166(13) -0.0004(10) 0.0073(12) 0.0024(12) C17 0.083(3) 0.0139(14) 0.0245(16) -0.0013(12) 0.0227(18) -0.0031(16) C18 0.105(4) 0.0145(15) 0.0322(19) -0.0036(13) 0.031(2) 0.0037(18) C19 0.058(2) 0.0240(16) 0.0198(15) -0.0035(12) 0.0131(15) 0.0068(15) C20 0.0332(17) 0.0231(15) 0.0187(14) 0.0020(11) 0.0090(13) 0.0046(12) C21 0.0266(15) 0.0161(13) 0.0175(13) 0.0010(10) 0.0065(12) 0.0033(11) C22 0.0352(19) 0.0265(16) 0.0215(15) -0.0046(12) 0.0056(13) -0.0012(13) C23 0.048(2) 0.0378(19) 0.0343(19) -0.0031(15) 0.0213(17) -0.0052(16) C24 0.0295(18) 0.0250(16) 0.0302(17) -0.0044(13) 0.0040(14) -0.0043(13) C25 0.036(2) 0.0222(16) 0.048(2) -0.0020(15) 0.0113(17) -0.0038(14) C26 0.0326(18) 0.0246(15) 0.0378(18) -0.0039(13) 0.0160(15) 0.0014(13) C27 0.059(3) 0.0347(19) 0.038(2) 0.0034(15) 0.0250(19) 0.0122(17) C28 0.0306(18) 0.0246(15) 0.0289(16) 0.0005(13) 0.0077(14) 0.0045(13) C29 0.051(2) 0.0211(16) 0.044(2) -0.0014(14) 0.0200(18) -0.0002(15) N1 0.0299(14) 0.0127(10) 0.0168(11) 0.0009(8) 0.0098(10) 0.0015(9) N2 0.0292(14) 0.0152(11) 0.0215(12) 0.0003(9) 0.0097(11) 0.0028(10) N3 0.0317(14) 0.0116(10) 0.0154(11) 0.0018(9) 0.0077(10) 0.0008(9) N4 0.0303(14) 0.0165(11) 0.0196(12) 0.0007(9) 0.0104(10) 0.0015(10) N5 0.0257(14) 0.0213(12) 0.0238(13) -0.0043(10) 0.0059(11) -0.0012(10) S1 0.0270(4) 0.0133(3) 0.0198(3) 0.0028(3) 0.0053(3) -0.0013(3) Fe1 0.0266(2) 0.00980(18) 0.01413(19) 0.00138(14) 0.00642(15) 0.00017(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C2 1.514(5) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? C2 C3 1.535(4) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 C4 1.559(4) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 C8 1.512(4) . ? C4 C15 1.524(4) . ? C4 C5 1.548(4) . ? C5 C6 1.521(4) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 C7 1.522(4) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 N2 1.329(4) . ? C8 N1 1.378(3) . ? C9 N1 1.390(4) . ? C9 C10 1.391(4) . ? C9 C14 1.406(4) . ? C10 C11 1.388(5) . ? C10 H10 0.95 . ? C11 C12 1.397(5) . ? C11 H11 0.95 . ? C12 C13 1.387(5) . ? C12 H12 0.95 . ? C13 C14 1.394(4) . ? C13 H13 0.95 . ? C14 N2 1.393(4) . ? C15 N4 1.324(4) . ? C15 N3 1.371(3) . ? C16 C17 1.392(4) . ? C16 N3 1.392(4) . ? C16 C21 1.395(4) . ? C17 C18 1.380(5) . ? C17 H17 0.95 . ? C18 C19 1.403(5) . ? C18 H18 0.95 . ? C19 C20 1.378(4) . ? C19 H19 0.95 . ? C20 C21 1.393(4) . ? C20 H20 0.95 . ? C21 N4 1.384(4) . ? C22 C23 1.505(5) . ? C22 N5 1.520(4) . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 C25 1.509(5) . ? C24 N5 1.516(4) . ? C24 H24A 0.99 . ? C24 H24B 0.99 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 N5 1.509(4) . ? C26 C27 1.513(5) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C28 C29 1.510(5) . ? C28 N5 1.513(4) . ? C28 H28A 0.99 . ? C28 H28B 0.99 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C200 C201 1.243(16) . ? C200 H20A 0.9814 . ? C200 H20B 0.9784 . ? C200 H20C 0.9818 . ? C201 C202 1.638(14) . ? C201 H20D 0.99 . ? C201 H20E 0.99 . ? C202 C203 1.606(12) . ? C202 H20F 0.99 . ? C202 H20G 0.99 . ? C203 C204 1.233(13) . ? C203 H20H 0.99 . ? C203 H20I 0.99 . ? C204 H20J 0.98 . ? C204 H20K 0.98 . ? C204 H20L 0.98 . ? C300 C301 1.243(16) . ? C300 H30A 0.98 . ? C300 H30B 0.98 . ? C300 H30C 0.98 . ? C301 C302 1.637(14) . ? C301 H30D 0.99 . ? C301 H30E 0.99 . ? C302 C303 1.606(12) . ? C302 H20A 0.2378 . ? C302 H30F 0.99 . ? C302 H30G 0.99 . ? C303 C304 1.234(13) . ? C303 H30H 0.99 . ? C303 H30I 0.99 . ? C304 H30J 0.98 . ? C304 H30K 0.98 . ? C304 H30L 0.98 . ? N1 Fe1 1.976(2) . ? N3 Fe1 1.980(2) . ? S1 Fe1 2.1914(8) . ? S1 Fe1 2.2032(8) 3_656 ? Fe1 S1 2.2032(8) 3_656 ? Fe1 Fe1 2.7063(8) 3_656 ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 C3 110.9(3) . . ? C1 C2 H2A 109.5 . . ? C3 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 108 . . ? C2 C3 C4 115.9(2) . . ? C2 C3 H3A 108.3 . . ? C4 C3 H3A 108.3 . . ? C2 C3 H3B 108.3 . . ? C4 C3 H3B 108.3 . . ? H3A C3 H3B 107.4 . . ? C8 C4 C15 114.5(2) . . ? C8 C4 C5 110.0(2) . . ? C15 C4 C5 108.6(2) . . ? C8 C4 C3 108.0(2) . . ? C15 C4 C3 106.3(2) . . ? C5 C4 C3 109.2(2) . . ? C6 C5 C4 115.2(2) . . ? C6 C5 H5A 108.5 . . ? C4 C5 H5A 108.5 . . ? C6 C5 H5B 108.5 . . ? C4 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? C5 C6 C7 112.1(3) . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 N1 115.0(2) . . ? N2 C8 C4 121.3(2) . . ? N1 C8 C4 123.5(2) . . ? N1 C9 C10 131.7(3) . . ? N1 C9 C14 107.3(2) . . ? C10 C9 C14 121.1(3) . . ? C11 C10 C9 117.3(3) . . ? C11 C10 H10 121.4 . . ? C9 C10 H10 121.4 . . ? C10 C11 C12 122.1(3) . . ? C10 C11 H11 118.9 . . ? C12 C11 H11 118.9 . . ? C13 C12 C11 120.6(3) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 118.0(3) . . ? C12 C13 H13 121 . . ? C14 C13 H13 121 . . ? N2 C14 C13 129.6(3) . . ? N2 C14 C9 109.5(2) . . ? C13 C14 C9 120.9(3) . . ? N4 C15 N3 115.0(2) . . ? N4 C15 C4 120.8(2) . . ? N3 C15 C4 124.1(2) . . ? C17 C16 N3 131.4(3) . . ? C17 C16 C21 121.2(3) . . ? N3 C16 C21 107.4(2) . . ? C18 C17 C16 117.5(3) . . ? C18 C17 H17 121.2 . . ? C16 C17 H17 121.2 . . ? C17 C18 C19 121.5(3) . . ? C17 C18 H18 119.2 . . ? C19 C18 H18 119.2 . . ? C20 C19 C18 120.8(3) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 118.2(3) . . ? C19 C20 H20 120.9 . . ? C21 C20 H20 120.9 . . ? N4 C21 C20 129.7(3) . . ? N4 C21 C16 109.5(2) . . ? C20 C21 C16 120.7(3) . . ? C23 C22 N5 115.2(3) . . ? C23 C22 H22A 108.5 . . ? N5 C22 H22A 108.5 . . ? C23 C22 H22B 108.5 . . ? N5 C22 H22B 108.5 . . ? H22A C22 H22B 107.5 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 N5 115.7(3) . . ? C25 C24 H24A 108.4 . . ? N5 C24 H24A 108.4 . . ? C25 C24 H24B 108.4 . . ? N5 C24 H24B 108.4 . . ? H24A C24 H24B 107.4 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N5 C26 C27 115.2(3) . . ? N5 C26 H26A 108.5 . . ? C27 C26 H26A 108.5 . . ? N5 C26 H26B 108.5 . . ? C27 C26 H26B 108.5 . . ? H26A C26 H26B 107.5 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 N5 114.7(3) . . ? C29 C28 H28A 108.6 . . ? N5 C28 H28A 108.6 . . ? C29 C28 H28B 108.6 . . ? N5 C28 H28B 108.6 . . ? H28A C28 H28B 107.6 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C200 C201 C202 129.0(7) . . ? C200 C201 H20D 105 . . ? C202 C201 H20D 105 . . ? C200 C201 H20E 105 . . ? C202 C201 H20E 105 . . ? H20D C201 H20E 105.9 . . ? C203 C202 C201 107.2(7) . . ? C203 C202 H20F 110.3 . . ? C201 C202 H20F 110.3 . . ? C203 C202 H20G 110.3 . . ? C201 C202 H20G 110.3 . . ? H20F C202 H20G 108.5 . . ? C204 C203 C202 117.5(9) . . ? C204 C203 H20H 107.9 . . ? C202 C203 H20H 107.9 . . ? C204 C203 H20I 107.9 . . ? C202 C203 H20I 107.9 . . ? H20H C203 H20I 107.2 . . ? C301 C300 H30A 109.5 . . ? C301 C300 H30B 109.5 . . ? H30A C300 H30B 109.5 . . ? C301 C300 H30C 109.5 . . ? H30A C300 H30C 109.5 . . ? H30B C300 H30C 109.5 . . ? C300 C301 C302 129.8(7) . . ? C300 C301 H20C 154.4 . . ? C302 C301 H20C 60 . . ? C300 C301 H30D 104.8 . . ? C302 C301 H30D 104.8 . . ? H20C C301 H30D 92.8 . . ? C300 C301 H30E 104.8 . . ? C302 C301 H30E 104.8 . . ? H20C C301 H30E 51.6 . . ? H30D C301 H30E 105.8 . . ? C303 C302 C301 107.5(7) . . ? C303 C302 H20A 131.5 . . ? C301 C302 H20A 79.1 . . ? C303 C302 H20C 126.8 . . ? C301 C302 H20C 54.5 . . ? C303 C302 H30F 110.2 . . ? C301 C302 H30F 110.2 . . ? H20A C302 H30F 112 . . ? H20C C302 H30F 55.8 . . ? C303 C302 H30G 110.2 . . ? C301 C302 H30G 110.2 . . ? H20C C302 H30G 123 . . ? H30F C302 H30G 108.5 . . ? C304 C303 C302 117.3(9) . . ? C304 C303 H30H 108 . . ? C302 C303 H30H 108 . . ? C304 C303 H30I 108 . . ? C302 C303 H30I 108 . . ? H30H C303 H30I 107.2 . . ? C303 C304 H30J 109.5 . . ? C303 C304 H30K 109.5 . . ? H30J C304 H30K 109.5 . . ? C303 C304 H30L 109.5 . . ? H30J C304 H30L 109.5 . . ? H30K C304 H30L 109.5 . . ? C8 N1 C9 104.3(2) . . ? C8 N1 Fe1 125.38(19) . . ? C9 N1 Fe1 128.91(19) . . ? C8 N2 C14 104.0(2) . . ? C15 N3 C16 103.9(2) . . ? C15 N3 Fe1 125.43(19) . . ? C16 N3 Fe1 128.91(19) . . ? C15 N4 C21 104.2(2) . . ? C26 N5 C28 111.4(3) . . ? C26 N5 C24 111.1(2) . . ? C28 N5 C24 106.3(2) . . ? C26 N5 C22 106.0(2) . . ? C28 N5 C22 111.1(2) . . ? C24 N5 C22 111.0(2) . . ? Fe1 S1 Fe1 76.02(3) . 3_656 ? N1 Fe1 N3 91.79(10) . . ? N1 Fe1 S1 114.35(8) . . ? N3 Fe1 S1 115.21(8) . . ? N1 Fe1 S1 118.11(8) . 3_656 ? N3 Fe1 S1 113.83(8) . 3_656 ? S1 Fe1 S1 103.98(3) . 3_656 ? N1 Fe1 Fe1 135.84(7) . 3_656 ? N3 Fe1 Fe1 132.36(7) . 3_656 ? S1 Fe1 Fe1 52.19(2) . 3_656 ? S1 Fe1 Fe1 51.79(2) 3_656 3_656 ? # END of CIF 1 #\#CIF_2 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-05-27 at 11:47:48 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : car02b_0ma apexiitemplate #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_car02b_0ma _audit_creation_date 2011-05-27T11:47:48-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; car02b ; _chemical_name_common car02b _chemical_formula_moiety '8(C42 H44 Fe2 N8 S2), 24(C8 H20 N), 16(C2 H3 N), 8(C H4 O)' _chemical_formula_sum 'C568 H912 Fe16 N104 O8 S16' _chemical_formula_weight 10732.58 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.303(9) _cell_length_b 34.268(9) _cell_length_c 18.170(5) _cell_angle_alpha 90 _cell_angle_beta 98.320(15) _cell_angle_gamma 90 _cell_volume 16821(8) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 300 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.06 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5784 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.438 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2007)' _exptl_absorpt_correction_T_min 0.782 _exptl_absorpt_correction_T_max 0.9575 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_unetI/netI 0.027 _diffrn_reflns_number 126675 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.35 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 15248 _reflns_number_gt 10883 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.1015P)^2^+34.6727P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 15248 _refine_ls_number_parameters 951 _refine_ls_number_restraints 272 _refine_ls_R_factor_all 0.0944 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.2059 _refine_ls_wR_factor_gt 0.1607 _refine_ls_goodness_of_fit_ref 1.11 _refine_ls_restrained_S_all 1.125 _refine_ls_shift/su_max 0.104 _refine_ls_shift/su_mean 0.003 _refine_diff_density_max 0.711 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.071 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.02645(14) 0.22251(12) -0.01688(18) 0.0466(9) Uani 1 1 d . A 1 C2 C -0.08419(15) 0.17948(14) -0.0251(2) 0.0573(10) Uani 1 1 d . A 1 C3 C -0.12801(17) 0.15889(19) -0.0356(3) 0.0834(16) Uani 1 1 d . A 1 H3 H -0.1587 0.1718 -0.05 0.1 Uiso 1 1 calc R A 1 C4 C -0.12629(18) 0.1188(2) -0.0247(3) 0.0896(18) Uani 1 1 d . A 1 H4 H -0.1562 0.1042 -0.0316 0.107 Uiso 1 1 calc R A 1 C5 C -0.08161(16) 0.09981(16) -0.0037(3) 0.0693(13) Uani 1 1 d . A 1 H5 H -0.0814 0.0724 0.0042 0.083 Uiso 1 1 calc R A 1 C6 C -0.03694(14) 0.12033(13) 0.0058(2) 0.0527(9) Uani 1 1 d . A 1 H6 H -0.0063 0.1074 0.0201 0.063 Uiso 1 1 calc R A 1 C7 C -0.03897(13) 0.16026(12) -0.00634(18) 0.0452(8) Uani 1 1 d . A 1 C8 C 0.04191(16) 0.26585(12) 0.0423(2) 0.0561(10) Uani 1 1 d . A 1 C9 C 0.0923(2) 0.29155(15) 0.1306(3) 0.0751(14) Uani 1 1 d . A 1 C10 C 0.1188(3) 0.3156(2) 0.1845(4) 0.106(2) Uani 1 1 d . A 1 H10 H 0.1104 0.3424 0.1887 0.128 Uiso 1 1 calc R A 1 C11 C 0.1577(3) 0.2992(2) 0.2313(3) 0.112(2) Uani 1 1 d . A 1 H11 H 0.1764 0.3151 0.2681 0.135 Uiso 1 1 calc R A 1 C12 C 0.1702(2) 0.2606(2) 0.2261(3) 0.0854(16) Uani 1 1 d . A 1 H12 H 0.1969 0.2502 0.2598 0.103 Uiso 1 1 calc R A 1 C13 C 0.14484(17) 0.23633(16) 0.1726(2) 0.0663(12) Uani 1 1 d . A 1 H13 H 0.1535 0.2096 0.1691 0.08 Uiso 1 1 calc R A 1 C14 C 0.10601(16) 0.25275(14) 0.1243(2) 0.0574(11) Uani 1 1 d . A 1 C15 C 0.00006(16) 0.26094(12) -0.0213(2) 0.0569(10) Uani 1 1 d . A 1 C16 C -0.0371(2) 0.29526(15) -0.0203(3) 0.0788(14) Uani 1 1 d . A 1 H16A H -0.0631 0.2928 -0.0642 0.095 Uiso 1 1 d R A 1 H16B H -0.0194 0.3201 -0.0252 0.095 Uiso 1 1 d R A 1 C17 C -0.0628(3) 0.2973(3) 0.0510(7) 0.116(4) Uani 0.679(10) 1 d P A 1 H17A H -0.0787 0.2719 0.0585 0.139 Uiso 0.679(10) 1 calc PR A 1 H17B H -0.0377 0.3024 0.095 0.139 Uiso 0.679(10) 1 calc PR A 1 C18 C -0.1023(6) 0.3302(5) 0.0431(12) 0.206(9) Uani 0.679(10) 1 d P A 1 H18A H -0.0883 0.3539 0.0244 0.309 Uiso 0.679(10) 1 calc PR A 1 H18B H -0.1124 0.3355 0.0918 0.309 Uiso 0.679(10) 1 calc PR A 1 H18C H -0.1312 0.3219 0.0082 0.309 Uiso 0.679(10) 1 calc PR A 1 C19 C -0.0740(7) 0.3013(5) -0.0980(7) 0.085(6) Uani 0.321(10) 1 d P A 2 H19A H -0.0549 0.3103 -0.1371 0.102 Uiso 0.321(10) 1 d PR A 2 H19B H -0.0902 0.2762 -0.1143 0.102 Uiso 0.321(10) 1 d PR A 2 C20 C -0.1147(11) 0.3301(8) -0.0852(12) 0.145(12) Uani 0.321(10) 1 d P A 2 H20D H -0.1415 0.3296 -0.1274 0.217 Uiso 0.321(10) 1 d PR A 2 H20E H -0.0996 0.356 -0.081 0.217 Uiso 0.321(10) 1 d PR A 2 H20F H -0.1281 0.324 -0.0393 0.217 Uiso 0.321(10) 1 d PR A 2 C21 C 0.02202(16) 0.26060(12) -0.0971(2) 0.0529(9) Uani 1 1 d . A 1 H21A H 0.0431 0.2372 -0.098 0.064 Uiso 1 1 calc R A 1 H21B H -0.0058 0.258 -0.1383 0.064 Uiso 1 1 calc R A 1 C22 C 0.0524(2) 0.29615(14) -0.1123(3) 0.0732(13) Uani 1 1 d . A 1 H22A H 0.0309 0.3195 -0.1167 0.088 Uiso 1 1 calc R A 1 H22B H 0.079 0.3002 -0.0699 0.088 Uiso 1 1 calc R A 1 C23 C 0.0749(2) 0.29134(16) -0.1825(3) 0.0853(17) Uani 1 1 d . A 1 H23A H 0.0969 0.2686 -0.1778 0.128 Uiso 1 1 calc R A 1 H23B H 0.0939 0.3148 -0.191 0.128 Uiso 1 1 calc R A 1 H23C H 0.0486 0.2875 -0.2247 0.128 Uiso 1 1 calc R A 1 C24 C 0.18262(14) 0.06041(11) -0.0843(2) 0.0521(9) Uani 1 1 d . A 1 C25 C 0.12406(16) 0.01913(11) -0.1103(3) 0.0638(12) Uani 1 1 d . A 1 C26 C 0.0923(2) -0.01230(14) -0.1335(4) 0.0912(18) Uani 1 1 d . A 1 H26 H 0.1031 -0.0335 -0.1608 0.109 Uiso 1 1 calc R A 1 C27 C 0.04475(19) -0.01138(15) -0.1152(3) 0.0813(16) Uani 1 1 d . A 1 H27 H 0.023 -0.0325 -0.1301 0.098 Uiso 1 1 calc R A 1 C28 C 0.02790(16) 0.01916(13) -0.0762(2) 0.0605(11) Uani 1 1 d . A 1 H28 H -0.0051 0.0189 -0.0655 0.073 Uiso 1 1 calc R A 1 C29 C 0.05878(14) 0.05014(12) -0.0525(2) 0.0511(9) Uani 1 1 d . A 1 H29 H 0.0477 0.071 -0.0247 0.061 Uiso 1 1 calc R A 1 C30 C 0.10662(13) 0.04986(10) -0.0707(2) 0.0454(8) Uani 1 1 d . A 1 C31 C 0.24846(15) 0.09717(11) -0.0018(2) 0.0548(10) Uani 1 1 d . A 1 C32 C 0.29254(17) 0.11108(13) 0.1011(3) 0.0650(12) Uani 1 1 d . A 1 C33 C 0.3292(2) 0.11520(19) 0.1636(4) 0.0913(18) Uani 1 1 d . A 1 H33 H 0.3611 0.1038 0.1645 0.11 Uiso 1 1 calc R A 1 C34 C 0.3176(2) 0.13622(19) 0.2232(3) 0.0891(18) Uani 1 1 d . A 1 H34 H 0.3418 0.1391 0.266 0.107 Uiso 1 1 calc R A 1 C35 C 0.2718(2) 0.15321(15) 0.2224(2) 0.0725(14) Uani 1 1 d . A 1 H35 H 0.2653 0.1677 0.2645 0.087 Uiso 1 1 calc R A 1 C36 C 0.23468(17) 0.14965(12) 0.1611(2) 0.0563(10) Uani 1 1 d . A 1 H36 H 0.2029 0.161 0.1609 0.068 Uiso 1 1 calc R A 1 C37 C 0.24646(14) 0.12867(11) 0.1005(2) 0.0499(9) Uani 1 1 d . A 1 C38 C 0.23287(14) 0.08104(12) -0.0793(3) 0.0575(10) Uani 1 1 d . A 1 C39 C 0.27301(17) 0.05372(16) -0.1019(4) 0.0849(17) Uani 1 1 d U A 1 H39A H 0.283 0.0349 -0.0612 0.102 Uiso 1 1 d R A 1 H39B H 0.2585 0.0386 -0.1462 0.102 Uiso 1 1 d R A 1 C40 C 0.3163(6) 0.0736(6) -0.1196(15) 0.114(8) Uani 0.321(11) 1 d PU A 1 H40A H 0.328 0.0922 -0.0793 0.137 Uiso 0.321(11) 1 calc PR A 1 H40B H 0.3073 0.0887 -0.166 0.137 Uiso 0.321(11) 1 calc PR A 1 C41 C 0.3598(8) 0.0448(9) -0.130(2) 0.188(18) Uani 0.321(11) 1 d PU A 1 H41A H 0.3594 0.0226 -0.0962 0.283 Uiso 0.321(11) 1 calc PR A 1 H41B H 0.3915 0.0585 -0.1187 0.283 Uiso 0.321(11) 1 calc PR A 1 H41C H 0.3557 0.0354 -0.1815 0.283 Uiso 0.321(11) 1 calc PR A 1 C42 C 0.2837(3) 0.0142(2) -0.0529(7) 0.121(5) Uani 0.679(11) 1 d PU A 3 H42A H 0.2909 0.0207 0.0006 0.145 Uiso 0.679(11) 1 d PR A 3 H42B H 0.2539 -0.0027 -0.0606 0.145 Uiso 0.679(11) 1 d PR A 3 C43 C 0.3276(4) -0.0076(4) -0.0786(9) 0.178(8) Uani 0.679(11) 1 d PU A 3 H43A H 0.3258 -0.0061 -0.1328 0.266 Uiso 0.679(11) 1 d PR A 3 H43B H 0.3266 -0.035 -0.0634 0.266 Uiso 0.679(11) 1 d PR A 3 H43C H 0.3586 0.0043 -0.055 0.266 Uiso 0.679(11) 1 d PR A 3 C44 C 0.22636(15) 0.11643(12) -0.1331(2) 0.0552(10) Uani 1 1 d . A 1 H44A H 0.2027 0.1348 -0.1153 0.066 Uiso 1 1 calc R A 1 H44B H 0.2586 0.13 -0.13 0.066 Uiso 1 1 calc R A 1 C45 C 0.2084(2) 0.10740(16) -0.2140(3) 0.0788(15) Uani 1 1 d . A 1 H45A H 0.2335 0.0913 -0.2342 0.095 Uiso 1 1 calc R A 1 H45B H 0.1774 0.092 -0.2177 0.095 Uiso 1 1 calc R A 1 C46 C 0.1989(2) 0.14383(18) -0.2602(3) 0.0842(16) Uani 1 1 d . A 1 H46A H 0.1754 0.1605 -0.2388 0.126 Uiso 1 1 calc R A 1 H46B H 0.185 0.1367 -0.3112 0.126 Uiso 1 1 calc R A 1 H46C H 0.23 0.158 -0.2605 0.126 Uiso 1 1 calc R A 1 N9 N 0.19304(17) 0.01964(13) 0.1740(3) 0.123(2) Uani 1 1 d D B 4 C47 C 0.1976(3) 0.06230(18) 0.2036(6) 0.151(4) Uani 1 1 d D B 4 H47A H 0.2278 0.074 0.1886 0.181 Uiso 1 1 calc R B 4 H47B H 0.169 0.0774 0.1788 0.181 Uiso 1 1 calc R B 4 C48 C 0.2000(4) 0.0672(3) 0.2863(6) 0.187(5) Uani 1 1 d D B 4 H48A H 0.1667 0.0642 0.2998 0.28 Uiso 1 1 calc R B 4 H48B H 0.2128 0.0932 0.3009 0.28 Uiso 1 1 calc R B 4 H48C H 0.2219 0.0473 0.3119 0.28 Uiso 1 1 calc R B 4 C49 C 0.1456(3) 0.0015(2) 0.1949(5) 0.155(4) Uani 1 1 d D B 4 H49A H 0.144 -0.0263 0.1796 0.187 Uiso 1 1 calc R B 4 H49B H 0.147 0.0024 0.2496 0.187 Uiso 1 1 calc R B 4 C50 C 0.0991(3) 0.0219(3) 0.1593(6) 0.179(5) Uani 1 1 d D B 4 H50A H 0.0708 0.0124 0.1816 0.269 Uiso 1 1 calc R B 4 H50B H 0.0937 0.0165 0.1058 0.269 Uiso 1 1 calc R B 4 H50C H 0.1027 0.0501 0.1674 0.269 Uiso 1 1 calc R B 4 C51 C 0.2341(3) -0.0042(2) 0.2133(5) 0.143(4) Uani 1 1 d D B 4 H51A H 0.2297 -0.0317 0.1967 0.171 Uiso 1 1 calc R B 4 H51B H 0.2326 -0.0034 0.2674 0.171 Uiso 1 1 calc R B 4 C52 C 0.2855(3) 0.0101(3) 0.1993(6) 0.169(5) Uani 1 1 d D B 4 H52A H 0.2864 0.0113 0.1456 0.254 Uiso 1 1 calc R B 4 H52B H 0.3109 -0.008 0.2224 0.254 Uiso 1 1 calc R B 4 H52C H 0.2917 0.0362 0.2209 0.254 Uiso 1 1 calc R B 4 C53 C 0.1924(3) 0.0212(2) 0.0913(4) 0.149(4) Uani 1 1 d D B 4 H53A H 0.2238 0.0327 0.0806 0.179 Uiso 1 1 calc R B 4 H53B H 0.1651 0.0385 0.0693 0.179 Uiso 1 1 calc R B 4 C54 C 0.1857(4) -0.0184(3) 0.0548(5) 0.199(6) Uani 1 1 d D B 4 H54A H 0.2059 -0.0376 0.0854 0.299 Uiso 1 1 calc R B 4 H54B H 0.1962 -0.0172 0.0055 0.299 Uiso 1 1 calc R B 4 H54C H 0.1508 -0.026 0.0498 0.299 Uiso 1 1 calc R B 4 N11 N -0.0128(4) 0.1826(3) 0.2404(6) 0.103(4) Uani 0.5 1 d PDU . 5 C59 C -0.0041(6) 0.2182(5) 0.1890(7) 0.124(5) Uani 0.5 1 d PDU . 5 H59A H 0.032 0.2227 0.1926 0.149 Uiso 0.5 1 d PR . 5 H59B H -0.0167 0.2114 0.1367 0.149 Uiso 0.5 1 d PR . 5 C60 C -0.0286(9) 0.2549(6) 0.2097(15) 0.215(11) Uani 0.5 1 d PDU . 5 H60A H -0.0142 0.277 0.186 0.323 Uiso 0.5 1 d PR . 5 H60B H -0.0231 0.2584 0.2638 0.323 Uiso 0.5 1 d PR . 5 H60C H -0.0642 0.2535 0.1921 0.323 Uiso 0.5 1 d PR . 5 C61 C -0.0676(4) 0.1790(5) 0.2435(7) 0.115(4) Uani 0.5 1 d PDU . 5 H61A H -0.0797 0.2042 0.2605 0.138 Uiso 0.5 1 d PR . 5 H61B H -0.073 0.1588 0.2803 0.138 Uiso 0.5 1 d PR . 5 C62 C -0.0969(7) 0.1688(6) 0.1690(9) 0.152(6) Uani 0.5 1 d PDU . 5 H62A H -0.0913 0.1413 0.1581 0.228 Uiso 0.5 1 d PR . 5 H62B H -0.0857 0.1852 0.1304 0.228 Uiso 0.5 1 d PR . 5 H62C H -0.1323 0.1732 0.1699 0.228 Uiso 0.5 1 d PR . 5 C63 C 0.0099(5) 0.1867(5) 0.3182(6) 0.100(4) Uani 0.5 1 d PDU . 5 H63A H 0.0087 0.1614 0.3442 0.12 Uiso 0.5 1 d PR . 5 H63B H -0.0091 0.2061 0.343 0.12 Uiso 0.5 1 d PR . 5 C64 C 0.0661(6) 0.1952(8) 0.3245(12) 0.183(9) Uani 0.5 1 d PDU . 5 H64A H 0.0879 0.1724 0.3286 0.274 Uiso 0.5 1 d PR . 5 H64B H 0.0747 0.212 0.3681 0.274 Uiso 0.5 1 d PR . 5 H64C H 0.07 0.2098 0.2794 0.274 Uiso 0.5 1 d PR . 5 C65 C 0.0035(6) 0.1468(5) 0.2012(9) 0.138(5) Uani 0.5 1 d PDU . 5 H65A H -0.0152 0.1442 0.1505 0.165 Uiso 0.5 1 d PR . 5 H65B H 0.0392 0.1481 0.1971 0.165 Uiso 0.5 1 d PR . 5 C66 C -0.001(3) 0.1093(5) 0.241(2) 0.225(10) Uani 0.5 1 d PDU . 5 H66A H 0.0216 0.1096 0.2876 0.338 Uiso 0.5 1 d PR . 5 H66B H 0.0033 0.0852 0.2136 0.338 Uiso 0.5 1 d PR . 5 H66C H -0.0355 0.1106 0.2516 0.338 Uiso 0.5 1 d PR . 5 N10 N 0 0.13162(11) -0.25 0.0385(9) Uani 1 2 d S . . C55 C 0.04266(15) 0.10647(11) -0.21343(19) 0.0472(9) Uani 1 1 d . . . H55A H 0.0691 0.1238 -0.1889 0.057 Uiso 1 1 calc R . . H55B H 0.0308 0.0905 -0.1742 0.057 Uiso 1 1 calc R . . C56 C 0.06468(18) 0.07969(13) -0.2654(2) 0.0656(12) Uani 1 1 d . . . H56A H 0.0393 0.0614 -0.2883 0.098 Uiso 1 1 calc R . . H56B H 0.0921 0.065 -0.2375 0.098 Uiso 1 1 calc R . . H56C H 0.077 0.0951 -0.3043 0.098 Uiso 1 1 calc R . . C57 C 0.01590(14) 0.15663(11) -0.31100(17) 0.0430(8) Uani 1 1 d . . . H57A H 0.027 0.1393 -0.3489 0.052 Uiso 1 1 calc R . . H57B H -0.0132 0.1714 -0.3353 0.052 Uiso 1 1 calc R . . C58 C 0.05685(15) 0.18517(12) -0.2850(2) 0.0538(10) Uani 1 1 d . . . H58A H 0.0449 0.2045 -0.2521 0.081 Uiso 1 1 calc R . . H58B H 0.0671 0.1984 -0.3282 0.081 Uiso 1 1 calc R . . H58C H 0.0851 0.1711 -0.258 0.081 Uiso 1 1 calc R . . N12 N 0.2593(3) 0.2478(4) 0.0084(6) 0.039(2) Uani 0.5 1 d PD . 6 C67 C 0.2182(3) 0.2248(2) -0.0412(4) 0.056(2) Uani 0.5 1 d PD . 6 H67A H 0.2233 0.1966 -0.0317 0.067 Uiso 0.5 1 d PR . 6 H67B H 0.1858 0.2319 -0.0266 0.067 Uiso 0.5 1 d PR . 6 C68 C 0.2163(6) 0.2323(4) -0.1238(7) 0.067(4) Uani 0.5 1 d PD . 6 H68A H 0.206 0.2593 -0.1352 0.1 Uiso 0.5 1 d PR . 6 H68B H 0.1924 0.2144 -0.1516 0.1 Uiso 0.5 1 d PR . 6 H68C H 0.2491 0.2279 -0.138 0.1 Uiso 0.5 1 d PR . 6 C69 C 0.2504(3) 0.2908(2) -0.0004(4) 0.0487(17) Uani 0.5 1 d PD . 6 H69A H 0.277 0.3048 0.032 0.058 Uiso 0.5 1 d PR . 6 H69B H 0.2529 0.298 -0.0525 0.058 Uiso 0.5 1 d PR . 6 C70 C 0.2011(4) 0.3048(4) 0.0179(8) 0.066(3) Uani 0.5 1 d PD . 6 H70A H 0.1744 0.2904 -0.0124 0.099 Uiso 0.5 1 d PR . 6 H70B H 0.1973 0.3328 0.0071 0.099 Uiso 0.5 1 d PR . 6 H70C H 0.1995 0.3002 0.0707 0.099 Uiso 0.5 1 d PR . 6 C71 C 0.3090(3) 0.2390(2) -0.0129(4) 0.0491(18) Uani 0.5 1 d PD . 6 H71A H 0.3343 0.2545 0.0189 0.059 Uiso 0.5 1 d PR . 6 H71B H 0.3091 0.2475 -0.065 0.059 Uiso 0.5 1 d PR . 6 C72 C 0.3240(5) 0.1964(3) -0.0061(10) 0.079(4) Uani 0.5 1 d PD . 6 H72A H 0.3306 0.1891 0.0466 0.118 Uiso 0.5 1 d PR . 6 H72B H 0.3539 0.1921 -0.0292 0.118 Uiso 0.5 1 d PR . 6 H72C H 0.2969 0.1804 -0.0314 0.118 Uiso 0.5 1 d PR . 6 C73 C 0.2549(4) 0.2341(2) 0.0865(4) 0.061(2) Uani 0.5 1 d PD . 6 H73A H 0.2205 0.2381 0.0961 0.073 Uiso 0.5 1 d PR . 6 H73B H 0.2619 0.2057 0.0902 0.073 Uiso 0.5 1 d PR . 6 C74 C 0.2892(7) 0.2548(4) 0.1451(7) 0.070(4) Uani 0.5 1 d PD . 6 H74A H 0.3221 0.2565 0.1297 0.105 Uiso 0.5 1 d PR . 6 H74B H 0.2914 0.2405 0.192 0.105 Uiso 0.5 1 d PR . 6 H74C H 0.2767 0.2812 0.1518 0.105 Uiso 0.5 1 d PR . 6 N13 N -0.2280(8) 0.2515(7) -0.0752(12) 0.147(5) Uiso 0.25 1 d PD . 7 C75 C -0.2083(13) 0.2290(10) -0.1398(19) 0.147(5) Uiso 0.25 1 d PD . 7 H75A H -0.2058 0.2015 -0.1231 0.176 Uiso 0.25 1 d PR . 7 H75B H -0.2349 0.2306 -0.1829 0.176 Uiso 0.25 1 d PR . 7 C76 C -0.1609(11) 0.2463(13) -0.160(2) 0.147(5) Uiso 0.25 1 d PD C 7 H76A H -0.1588 0.2748 -0.1612 0.22 Uiso 0.25 1 d PR C 7 H76B H -0.1592 0.2357 -0.2094 0.22 Uiso 0.25 1 d PR C 7 H76C H -0.1332 0.236 -0.1246 0.22 Uiso 0.25 1 d PR C 7 C77 C -0.2032(13) 0.2415(10) -0.0007(15) 0.147(5) Uiso 0.25 1 d PD . 7 H77A H -0.1928 0.2142 -0.0072 0.176 Uiso 0.25 1 d PR . 7 H77B H -0.2306 0.2399 0.0295 0.176 Uiso 0.25 1 d PR . 7 C78 C -0.1672(14) 0.2612(13) 0.0570(18) 0.147(5) Uiso 0.25 1 d PD . 7 H78A H -0.1358 0.2549 0.0396 0.22 Uiso 0.25 1 d PR . 7 H78B H -0.1674 0.2502 0.1068 0.22 Uiso 0.25 1 d PR . 7 H78C H -0.171 0.2896 0.0589 0.22 Uiso 0.25 1 d PR . 7 C79 C -0.2817(9) 0.2471(12) -0.0757(16) 0.147(5) Uiso 0.25 1 d PD . 7 H79A H -0.2887 0.2209 -0.0974 0.176 Uiso 0.25 1 d PR . 7 H79B H -0.3008 0.2662 -0.1094 0.176 Uiso 0.25 1 d PR . 7 C80 C -0.3023(14) 0.2436(13) -0.0027(19) 0.147(5) Uiso 0.25 1 d PD . 7 H80A H -0.2971 0.2699 0.0184 0.22 Uiso 0.25 1 d PR . 7 H80B H -0.2841 0.2246 0.031 0.22 Uiso 0.25 1 d PR . 7 H80C H -0.3377 0.2374 -0.0093 0.22 Uiso 0.25 1 d PR . 7 C81 C -0.2212(11) 0.2938(7) -0.1043(19) 0.147(5) Uiso 0.25 1 d PD D 7 H81A H -0.1973 0.3101 -0.0717 0.176 Uiso 0.25 1 d PR D 7 H81B H -0.2094 0.2909 -0.1531 0.176 Uiso 0.25 1 d PR D 7 C82 C -0.2675(15) 0.3160(10) -0.094(4) 0.147(5) Uiso 0.25 1 d PD D 7 H82A H -0.2824 0.3145 -0.1462 0.22 Uiso 0.25 1 d PR D 7 H82B H -0.265 0.3434 -0.0782 0.22 Uiso 0.25 1 d PR D 7 H82C H -0.2883 0.3018 -0.0631 0.22 Uiso 0.25 1 d PR D 7 N14 N -0.1791(4) 0.2379(3) 0.0635(6) 0.092(3) Uiso 0.5 1 d PD E 8 C83 C -0.2065(6) 0.2109(5) 0.0769(9) 0.121(5) Uiso 0.5 1 d PD E 8 C84 C -0.2406(12) 0.1878(10) 0.082(3) 0.261(19) Uiso 0.5 1 d PD E 8 H84A H -0.2723 0.2016 0.0751 0.391 Uiso 0.5 1 d PR E 8 H84B H -0.2363 0.1741 0.1297 0.391 Uiso 0.5 1 d PR E 8 H84C H -0.2401 0.1688 0.0415 0.391 Uiso 0.5 1 d PR E 8 N15 N -0.2560(12) 0.1353(10) 0.0511(19) 0.275(13) Uiso 0.5 1 d PD F 9 C85 C -0.2758(11) 0.1180(9) -0.0046(19) 0.191(9) Uiso 0.5 1 d PD F 9 C86 C -0.287(3) 0.0937(19) -0.055(3) 0.47(4) Uiso 0.5 1 d PD F 9 H86A H -0.2769 0.1042 -0.1002 0.702 Uiso 0.5 1 d PR F 9 H86B H -0.3233 0.0895 -0.0633 0.702 Uiso 0.5 1 d PR F 9 H86C H -0.2707 0.0688 -0.0423 0.702 Uiso 0.5 1 d PR F 9 N16 N -0.2759(7) 0.1307(6) -0.0722(12) 0.171(6) Uiso 0.5 1 d PD G 10 C87 C -0.2962(8) 0.1100(7) -0.1239(12) 0.156(7) Uiso 0.5 1 d PD G 10 C88 C -0.3270(11) 0.0896(9) -0.1609(17) 0.241(13) Uiso 0.5 1 d PD G 10 H88A H -0.3474 0.0766 -0.128 0.362 Uiso 0.5 1 calc PR G 10 H88B H -0.3103 0.0699 -0.1874 0.362 Uiso 0.5 1 calc PR G 10 H88C H -0.3481 0.1058 -0.1969 0.362 Uiso 0.5 1 calc PR G 10 O1 O 0.4072(5) 0.1137(4) -0.0100(8) 0.161(4) Uiso 0.5 1 d PD H 11 H1 H 0.4121 0.1048 -0.0514 0.241 Uiso 0.5 1 d PR H 11 C89 C 0.4352(13) 0.0961(11) 0.0418(19) 0.293(18) Uiso 0.5 1 d PD H 11 H89A H 0.4338 0.1094 0.0892 0.439 Uiso 0.5 1 calc PR H 11 H89B H 0.4693 0.0964 0.0309 0.439 Uiso 0.5 1 calc PR H 11 H89C H 0.4241 0.0691 0.045 0.439 Uiso 0.5 1 calc PR H 11 N17 N -0.2336(5) 0.2174(4) -0.1315(7) 0.109(4) Uiso 0.5 1 d PD I 12 C91 C -0.2026(5) 0.2428(4) -0.1382(8) 0.098(4) Uiso 0.5 1 d PD I 12 C92 C -0.1655(6) 0.2593(5) -0.1560(10) 0.113(5) Uiso 0.5 1 d PD I 12 H92A H -0.1356 0.2487 -0.1264 0.169 Uiso 0.5 1 calc PR I 12 H92B H -0.1675 0.2874 -0.1468 0.169 Uiso 0.5 1 calc PR I 12 H92C H -0.1641 0.2548 -0.2089 0.169 Uiso 0.5 1 calc PR I 12 O2 O 0.4816(13) 0.1042(9) 0.262(2) 0.206(14) Uiso 0.25 1 d PD . 13 H2 H 0.5091 0.0944 0.2793 0.31 Uiso 0.25 1 d PR . 13 C93 C 0.455(2) 0.1072(18) 0.315(3) 0.23(2) Uiso 0.25 1 d PD J 13 H93A H 0.4758 0.1014 0.3625 0.339 Uiso 0.25 1 d PR J 13 H93B H 0.4279 0.0887 0.3061 0.339 Uiso 0.25 1 d PR J 13 H93C H 0.4425 0.1338 0.3156 0.339 Uiso 0.25 1 d PR J 13 N18 N -0.0533(11) 0.4550(8) 0.1519(17) 0.215(7) Uiso 0.25 1 d PD K 14 C94 C -0.0697(15) 0.4436(13) 0.2276(17) 0.215(7) Uiso 0.25 1 d PD K 14 H94A H -0.0442 0.4278 0.2586 0.258 Uiso 0.25 1 d PR K 14 H94B H -0.0749 0.4677 0.2556 0.258 Uiso 0.25 1 d PR K 14 C95 C -0.1188(17) 0.4218(16) 0.217(3) 0.215(7) Uiso 0.25 1 d PD K 14 H95A H -0.125 0.4103 0.2644 0.323 Uiso 0.25 1 d PR K 14 H95B H -0.1163 0.401 0.1809 0.323 Uiso 0.25 1 d PR K 14 H95C H -0.1462 0.4393 0.1983 0.323 Uiso 0.25 1 d PR K 14 C96 C -0.0912(14) 0.4794(11) 0.105(2) 0.215(7) Uiso 0.25 1 d PD K 14 H96A H -0.0852 0.4762 0.0527 0.258 Uiso 0.25 1 d PR K 14 H96B H -0.1239 0.4676 0.1086 0.258 Uiso 0.25 1 d PR K 14 C97 C -0.0930(16) 0.5216(11) 0.126(3) 0.215(7) Uiso 0.25 1 d PD K 14 H97A H -0.0953 0.5255 0.1787 0.323 Uiso 0.25 1 d PR K 14 H97B H -0.1223 0.5327 0.0956 0.323 Uiso 0.25 1 d PR K 14 H97C H -0.0632 0.5346 0.1137 0.323 Uiso 0.25 1 d PR K 14 C98 C -0.0450(17) 0.4193(10) 0.109(2) 0.215(7) Uiso 0.25 1 d PD K 14 H98A H -0.0252 0.4254 0.0694 0.258 Uiso 0.25 1 d PR K 14 H98B H -0.0771 0.4085 0.086 0.258 Uiso 0.25 1 d PR K 14 C99 C -0.013(2) 0.3885(12) 0.155(3) 0.215(7) Uiso 0.25 1 d PD K 14 H99A H 0.0187 0.3824 0.1389 0.323 Uiso 0.25 1 d PR K 14 H99B H -0.0332 0.3648 0.1539 0.323 Uiso 0.25 1 d PR K 14 H99C H -0.0073 0.3987 0.2062 0.323 Uiso 0.25 1 d PR K 14 C100 C -0.0051(13) 0.4776(12) 0.175(2) 0.215(7) Uiso 0.25 1 d PD K 14 H10A H -0.0118 0.4978 0.211 0.258 Uiso 0.25 1 d PR K 14 H10B H 0.0211 0.4602 0.1994 0.258 Uiso 0.25 1 d PR K 14 C101 C 0.0105(14) 0.4924(14) 0.104(3) 0.215(7) Uiso 0.25 1 d PD K 14 H10C H 0.0187 0.5198 0.1157 0.323 Uiso 0.25 1 d PR K 14 H10D H -0.0156 0.4913 0.0605 0.323 Uiso 0.25 1 d PR K 14 H10E H 0.04 0.4789 0.0917 0.323 Uiso 0.25 1 d PR K 14 O3 O -0.2865(9) 0.2313(7) -0.0693(13) 0.126(7) Uiso 0.25 1 d PD L 15 H3A H -0.2911 0.2295 -0.0247 0.189 Uiso 0.25 1 d PR L 15 C102 C -0.2570(13) 0.2045(10) -0.085(2) 0.135(11) Uiso 0.25 1 d PD L 15 H10F H -0.2233 0.2106 -0.0613 0.202 Uiso 0.25 1 calc PR L 15 H10G H -0.258 0.2028 -0.1387 0.202 Uiso 0.25 1 calc PR L 15 H10H H -0.2673 0.1794 -0.0657 0.202 Uiso 0.25 1 calc PR L 15 N1 N -0.00183(11) 0.18789(9) -0.00228(16) 0.0440(7) Uani 1 1 d . A 1 N2 N -0.07543(13) 0.21941(12) -0.03086(19) 0.0601(9) Uani 1 1 d D A 1 N3 N 0.07389(12) 0.23629(10) 0.06642(15) 0.0486(7) Uani 1 1 d . A 1 N4 N 0.05102(17) 0.29973(12) 0.0785(2) 0.0789(12) Uani 1 1 d . A 1 N5 N 0.14479(11) 0.07632(9) -0.05436(17) 0.0462(7) Uani 1 1 d . A 1 N6 N 0.17281(13) 0.02618(10) -0.1196(3) 0.0722(11) Uani 1 1 d . A 1 N7 N 0.21796(11) 0.11958(8) 0.03313(17) 0.0444(7) Uani 1 1 d . A 1 N8 N 0.29364(13) 0.09113(11) 0.0351(3) 0.0714(11) Uani 1 1 d . A 1 S1 S 0.09946(4) 0.13261(3) 0.09647(5) 0.0507(3) Uani 1 1 d . A 1 S2 S 0.11312(3) 0.17657(2) -0.07479(4) 0.0374(2) Uani 1 1 d . A 1 Fe1 Fe 0.072864(18) 0.181657(15) 0.02210(2) 0.03863(15) Uani 1 1 d . A 1 Fe2 Fe 0.142763(18) 0.128204(14) 0.00097(3) 0.03911(15) Uani 1 1 d . A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.048(2) 0.062(2) 0.0300(16) -0.0034(15) 0.0080(15) 0.0079(18) C2 0.046(2) 0.078(3) 0.048(2) 0.0109(19) 0.0065(17) 0.002(2) C3 0.042(2) 0.107(4) 0.099(4) 0.025(3) 0.000(2) 0.003(3) C4 0.047(3) 0.116(5) 0.102(4) 0.036(4) 0.001(3) -0.014(3) C5 0.050(3) 0.084(3) 0.071(3) 0.022(2) -0.001(2) -0.011(2) C6 0.041(2) 0.071(3) 0.047(2) 0.0074(18) 0.0095(16) -0.0053(18) C7 0.0397(19) 0.066(2) 0.0307(16) 0.0029(16) 0.0071(14) -0.0007(17) C8 0.068(3) 0.057(2) 0.045(2) -0.0133(18) 0.0130(18) 0.002(2) C9 0.088(4) 0.075(3) 0.060(3) -0.033(2) 0.006(2) 0.001(3) C10 0.115(5) 0.110(5) 0.090(4) -0.058(4) 0.000(4) -0.010(4) C11 0.112(5) 0.142(6) 0.078(4) -0.069(4) 0.002(4) -0.028(5) C12 0.081(3) 0.128(5) 0.044(2) -0.029(3) -0.001(2) -0.012(3) C13 0.066(3) 0.097(4) 0.036(2) -0.016(2) 0.0067(19) -0.006(2) C14 0.061(2) 0.077(3) 0.0358(19) -0.0199(19) 0.0125(17) -0.008(2) C15 0.063(3) 0.056(2) 0.052(2) -0.0067(18) 0.0089(19) 0.010(2) C16 0.077(3) 0.064(3) 0.093(4) -0.014(3) 0.003(3) 0.026(3) C17 0.081(6) 0.093(7) 0.174(10) -0.068(7) 0.020(6) 0.015(5) C18 0.168(14) 0.151(13) 0.32(2) -0.058(14) 0.095(15) 0.064(11) C19 0.111(13) 0.098(12) 0.046(7) 0.019(7) 0.012(8) 0.074(11) C20 0.20(3) 0.15(2) 0.087(14) 0.030(13) 0.027(15) 0.13(2) C21 0.066(3) 0.049(2) 0.0413(19) 0.0034(16) -0.0008(17) 0.0009(19) C22 0.099(4) 0.056(3) 0.063(3) 0.000(2) 0.005(2) -0.019(3) C23 0.113(4) 0.081(4) 0.060(3) 0.010(2) 0.005(3) -0.042(3) C24 0.041(2) 0.0348(19) 0.078(3) -0.0085(18) -0.0005(18) -0.0023(16) C25 0.051(2) 0.032(2) 0.106(4) -0.001(2) 0.004(2) -0.0073(17) C26 0.079(4) 0.042(3) 0.151(5) -0.012(3) 0.011(3) -0.021(2) C27 0.062(3) 0.052(3) 0.123(4) 0.013(3) -0.008(3) -0.026(2) C28 0.048(2) 0.064(3) 0.064(2) 0.027(2) -0.0096(19) -0.016(2) C29 0.044(2) 0.054(2) 0.051(2) 0.0151(17) -0.0053(16) -0.0054(17) C30 0.0407(19) 0.0349(18) 0.057(2) 0.0124(16) -0.0062(16) -0.0026(15) C31 0.043(2) 0.042(2) 0.077(3) -0.0008(19) -0.0021(19) -0.0081(17) C32 0.055(3) 0.053(2) 0.081(3) 0.012(2) -0.011(2) -0.010(2) C33 0.060(3) 0.095(4) 0.106(5) 0.019(4) -0.030(3) -0.009(3) C34 0.080(4) 0.103(4) 0.072(3) 0.020(3) -0.029(3) -0.030(3) C35 0.080(3) 0.079(3) 0.051(2) 0.019(2) -0.015(2) -0.034(3) C36 0.065(3) 0.052(2) 0.049(2) 0.0142(18) -0.0039(18) -0.020(2) C37 0.049(2) 0.040(2) 0.056(2) 0.0156(17) -0.0067(17) -0.0175(17) C38 0.038(2) 0.050(2) 0.085(3) -0.021(2) 0.0091(19) -0.0082(17) C39 0.049(3) 0.073(3) 0.130(5) -0.044(3) 0.002(3) 0.007(2) C40 0.054(9) 0.110(14) 0.18(2) -0.080(14) 0.027(10) -0.012(7) C41 0.069(11) 0.15(2) 0.36(5) -0.10(3) 0.068(19) 0.001(12) C42 0.075(5) 0.061(5) 0.208(12) -0.052(6) -0.040(6) 0.032(4) C43 0.104(8) 0.150(11) 0.252(16) -0.102(11) -0.065(8) 0.089(8) C44 0.049(2) 0.056(2) 0.063(2) -0.0239(19) 0.0182(18) -0.0185(18) C45 0.099(4) 0.076(3) 0.066(3) -0.032(3) 0.028(3) -0.032(3) C46 0.090(4) 0.109(4) 0.056(3) -0.029(3) 0.015(2) -0.033(3) N9 0.097(3) 0.089(3) 0.158(5) 0.089(3) -0.067(3) -0.058(3) C47 0.102(5) 0.089(5) 0.245(11) 0.094(6) -0.030(6) -0.050(4) C48 0.217(11) 0.139(8) 0.195(11) 0.044(8) -0.006(9) -0.101(8) C49 0.124(6) 0.132(6) 0.184(8) 0.107(6) -0.068(5) -0.088(5) C50 0.091(5) 0.174(8) 0.246(10) 0.139(8) -0.066(6) -0.073(5) C51 0.125(6) 0.096(5) 0.176(7) 0.078(5) -0.084(5) -0.052(4) C52 0.095(5) 0.130(7) 0.251(11) 0.080(7) -0.080(6) -0.028(5) C53 0.143(6) 0.122(6) 0.155(7) 0.085(5) -0.072(6) -0.066(5) C54 0.232(12) 0.166(9) 0.167(9) 0.056(7) -0.079(8) -0.103(9) N11 0.104(9) 0.164(7) 0.050(6) -0.003(5) 0.042(6) -0.008(5) C59 0.136(9) 0.168(10) 0.079(7) 0.011(7) 0.051(6) -0.028(8) C60 0.234(14) 0.212(14) 0.199(13) 0.021(9) 0.029(9) -0.011(9) C61 0.128(8) 0.148(9) 0.082(6) 0.019(6) 0.059(6) 0.008(7) C62 0.169(10) 0.170(10) 0.124(9) -0.013(8) 0.043(8) -0.002(8) C63 0.107(7) 0.141(9) 0.059(6) -0.006(6) 0.034(5) -0.027(7) C64 0.180(12) 0.212(12) 0.157(11) -0.007(9) 0.028(9) -0.010(9) C65 0.142(9) 0.158(10) 0.116(8) -0.048(7) 0.031(7) 0.014(8) C66 0.225(13) 0.220(12) 0.228(14) -0.002(10) 0.024(10) -0.003(10) N10 0.050(2) 0.037(2) 0.0274(18) 0 0.0045(16) 0 C55 0.060(2) 0.040(2) 0.0388(18) 0.0031(15) -0.0025(16) 0.0016(17) C56 0.078(3) 0.051(2) 0.064(3) -0.008(2) -0.005(2) 0.022(2) C57 0.057(2) 0.045(2) 0.0293(16) 0.0036(14) 0.0126(15) 0.0086(16) C58 0.054(2) 0.058(2) 0.051(2) 0.0149(18) 0.0129(18) -0.0038(19) N12 0.040(7) 0.042(4) 0.033(5) -0.002(3) -0.003(4) -0.021(5) C67 0.067(5) 0.050(5) 0.052(4) -0.011(4) 0.014(4) -0.029(4) C68 0.066(7) 0.070(9) 0.061(8) -0.003(6) 0.000(6) -0.020(7) C69 0.057(5) 0.040(4) 0.049(4) 0.000(3) 0.006(4) -0.017(3) C70 0.064(8) 0.058(6) 0.075(7) -0.006(5) 0.009(7) -0.010(6) C71 0.059(5) 0.044(4) 0.046(4) 0.000(3) 0.012(3) -0.012(3) C72 0.092(10) 0.045(6) 0.097(9) -0.011(5) 0.004(9) -0.006(7) C73 0.099(7) 0.049(5) 0.037(4) 0.003(3) 0.019(4) -0.019(4) C74 0.110(10) 0.058(8) 0.042(6) 0.003(5) 0.011(6) -0.014(7) N1 0.0427(16) 0.0536(18) 0.0361(15) -0.0024(13) 0.0072(12) 0.0027(14) N2 0.052(2) 0.075(3) 0.0532(19) 0.0055(17) 0.0066(15) 0.0161(18) N3 0.0553(19) 0.059(2) 0.0313(14) -0.0115(13) 0.0075(13) -0.0014(16) N4 0.092(3) 0.067(3) 0.076(3) -0.034(2) 0.007(2) 0.005(2) N5 0.0390(16) 0.0386(16) 0.0584(18) -0.0012(13) -0.0018(13) -0.0034(13) N6 0.050(2) 0.0384(19) 0.127(3) -0.023(2) 0.009(2) -0.0037(15) N7 0.0414(16) 0.0356(15) 0.0540(17) 0.0008(13) -0.0008(13) -0.0075(13) N8 0.046(2) 0.059(2) 0.103(3) -0.006(2) -0.0111(19) -0.0011(17) S1 0.0478(5) 0.0683(6) 0.0357(4) 0.0154(4) 0.0051(4) -0.0062(4) S2 0.0432(5) 0.0415(5) 0.0277(4) 0.0005(3) 0.0060(3) -0.0037(4) Fe1 0.0396(3) 0.0482(3) 0.0284(2) -0.00063(19) 0.00606(19) -0.0025(2) Fe2 0.0398(3) 0.0395(3) 0.0372(3) 0.00406(19) 0.0029(2) -0.0042(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N2 1.329(5) . ? C1 N1 1.370(5) . ? C1 C15 1.510(6) . ? C2 C3 1.378(7) . ? C2 N2 1.396(6) . ? C2 C7 1.398(6) . ? C3 C4 1.388(8) . ? C3 H3 0.95 . ? C4 C5 1.386(7) . ? C4 H4 0.95 . ? C5 C6 1.397(6) . ? C5 H5 0.95 . ? C6 C7 1.386(6) . ? C6 H6 0.95 . ? C7 N1 1.381(5) . ? C8 N4 1.339(5) . ? C8 N3 1.367(5) . ? C8 C15 1.513(6) . ? C9 C14 1.391(7) . ? C9 N4 1.392(7) . ? C9 C10 1.399(7) . ? C10 C11 1.382(10) . ? C10 H10 0.95 . ? C11 C12 1.374(10) . ? C11 H11 0.95 . ? C12 C13 1.385(7) . ? C12 H12 0.95 . ? C13 C14 1.394(6) . ? C13 H13 0.95 . ? C14 N3 1.388(5) . ? C15 C16 1.555(6) . ? C15 C21 1.580(6) . ? C16 C17 1.562(12) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 C18 1.554(16) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 C20 1.53(2) . ? C19 H16A 0.7056 . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? C20 H20D 0.98 . ? C20 H20E 0.98 . ? C20 H20F 0.98 . ? C21 C22 1.521(6) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 C23 1.505(7) . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 N6 1.345(5) . ? C24 N5 1.350(5) . ? C24 C38 1.534(5) . ? C25 N6 1.387(6) . ? C25 C30 1.397(6) . ? C25 C26 1.409(6) . ? C26 C27 1.386(8) . ? C26 H26 0.95 . ? C27 C28 1.380(7) . ? C27 H27 0.95 . ? C28 C29 1.385(6) . ? C28 H28 0.95 . ? C29 C30 1.393(5) . ? C29 H29 0.95 . ? C30 N5 1.381(4) . ? C31 N8 1.332(5) . ? C31 N7 1.356(5) . ? C31 C38 1.515(6) . ? C32 N8 1.385(6) . ? C32 C37 1.394(6) . ? C32 C33 1.408(7) . ? C33 C34 1.376(9) . ? C33 H33 0.95 . ? C34 C35 1.377(8) . ? C34 H34 0.95 . ? C35 C36 1.399(6) . ? C35 H35 0.95 . ? C36 C37 1.392(6) . ? C36 H36 0.95 . ? C37 N7 1.387(5) . ? C38 C39 1.542(6) . ? C38 C44 1.551(6) . ? C39 C40 1.44(2) . ? C39 H39A 0.99 . ? C39 H39B 0.99 . ? C40 C41 1.58(3) . ? C40 H40A 0.99 . ? C40 H40B 0.99 . ? C41 H41A 0.98 . ? C41 H41B 0.98 . ? C41 H41C 0.98 . ? C42 C43 1.541(14) . ? C42 H39A 0.7263 . ? C42 H42A 0.99 . ? C42 H42B 0.99 . ? C43 H43A 0.98 . ? C43 H43B 0.98 . ? C43 H43C 0.98 . ? C44 C45 1.514(6) . ? C44 H44A 0.99 . ? C44 H44B 0.99 . ? C45 C46 1.505(8) . ? C45 H45A 0.99 . ? C45 H45B 0.99 . ? C46 H46A 0.98 . ? C46 H46B 0.98 . ? C46 H46C 0.98 . ? N9 C51 1.485(7) . ? N9 C53 1.501(9) . ? N9 C49 1.533(7) . ? N9 C47 1.557(9) . ? C47 C48 1.503(11) . ? C47 H47A 0.99 . ? C47 H47B 0.99 . ? C48 H48A 0.98 . ? C48 H48B 0.98 . ? C48 H48C 0.98 . ? C49 C50 1.512(9) . ? C49 H49A 0.99 . ? C49 H49B 0.99 . ? C50 H50A 0.98 . ? C50 H50B 0.98 . ? C50 H50C 0.98 . ? C51 C52 1.541(10) . ? C51 H51A 0.99 . ? C51 H51B 0.99 . ? C52 H52A 0.98 . ? C52 H52B 0.98 . ? C52 H52C 0.98 . ? C53 C54 1.507(11) . ? C53 H53A 0.99 . ? C53 H53B 0.99 . ? C54 H54A 0.98 . ? C54 H54B 0.98 . ? C54 H54C 0.98 . ? N11 N11 0.735(19) 2 ? N11 C63 1.089(17) 2 ? N11 C63 1.466(13) . ? N11 C65 1.516(13) . ? N11 C61 1.509(13) . ? N11 C59 1.576(13) . ? N11 C65 1.617(16) 2 ? N11 C64 1.79(2) 2 ? N11 C59 1.783(17) 2 ? C59 C63 1.096(18) 2 ? C59 C60 1.497(17) . ? C59 N11 1.783(17) 2 ? C59 H59A 0.9899 . ? C59 H59B 0.99 . ? C60 H60A 0.98 . ? C60 H60B 0.98 . ? C60 H60C 0.98 . ? C61 C64 1.36(2) 2 ? C61 C62 1.511(14) . ? C61 H61A 0.99 . ? C61 H61B 0.99 . ? C62 C64 1.23(3) 2 ? C62 H62A 0.98 . ? C62 H62B 0.98 . ? C62 H62C 0.98 . ? C63 N11 1.089(17) 2 ? C63 C59 1.096(18) 2 ? C63 C65 1.45(2) 2 ? C63 C64 1.548(16) . ? C63 H63A 0.99 . ? C63 H63B 0.99 . ? C64 C62 1.23(3) 2 ? C64 C61 1.36(2) 2 ? C64 N11 1.79(2) 2 ? C64 H64A 0.98 . ? C64 H64B 0.98 . ? C64 H64C 0.98 . ? C65 C63 1.45(2) 2 ? C65 C66 1.487(19) . ? C65 C66 1.67(4) 2 ? C65 H65A 0.99 . ? C65 H65B 0.99 . ? C66 C66 0.33(9) 2 ? C66 C65 1.67(4) 2 ? C66 H66A 0.98 . ? C66 H66B 0.98 . ? C66 H66C 0.98 . ? N10 C57 1.514(4) 2_554 ? N10 C57 1.514(4) . ? N10 C55 1.522(4) 2_554 ? N10 C55 1.522(4) . ? C55 C56 1.503(6) . ? C55 H55A 0.99 . ? C55 H55B 0.99 . ? C56 H56A 0.98 . ? C56 H56B 0.98 . ? C56 H56C 0.98 . ? C57 C58 1.509(5) . ? C57 H57A 0.99 . ? C57 H57B 0.99 . ? C58 H58A 0.98 . ? C58 H58B 0.98 . ? C58 H58C 0.98 . ? N12 N12 0.572(12) 7 ? N12 C67 1.229(14) 7 ? N12 C69 1.351(15) 7 ? N12 C69 1.497(12) . ? N12 C71 1.495(12) . ? N12 C73 1.517(12) . ? N12 C67 1.549(10) . ? C67 C69 1.185(11) 7 ? C67 N12 1.229(14) 7 ? C67 C68 1.515(13) . ? C67 H67A 0.99 . ? C67 H67B 0.99 . ? C68 C74 0.591(15) 7 ? C68 C73 1.501(16) 7 ? C68 H68A 0.98 . ? C68 H68B 0.98 . ? C68 H68C 0.98 . ? C69 C67 1.185(11) 7 ? C69 N12 1.351(15) 7 ? C69 C70 1.511(12) . ? C69 H69A 0.99 . ? C69 H69B 0.99 . ? C70 C71 1.527(15) 7 ? C70 H70A 0.98 . ? C70 H70B 0.98 . ? C70 H70C 0.98 . ? C71 C72 1.515(13) . ? C71 C70 1.527(15) 7 ? C71 H71A 0.99 . ? C71 H71B 0.99 . ? C72 C70 0.690(14) 7 ? C72 H72A 0.98 . ? C72 H72B 0.98 . ? C72 H72C 0.98 . ? C73 C74 1.492(14) . ? C73 C68 1.501(16) 7 ? C73 C69 1.770(10) 7 ? C73 H73A 0.99 . ? C73 H73B 0.99 . ? C74 C68 0.591(15) 7 ? C74 H74A 0.98 . ? C74 H74B 0.98 . ? C74 H74C 0.9799 . ? N13 C80 1.54(4) 7_455 ? N13 C77 1.464(16) . ? N13 C79 1.473(16) . ? N13 C81 1.563(16) . ? N13 C75 1.563(16) . ? C75 C76 1.515(19) . ? C75 H75A 0.99 . ? C75 H75B 0.99 . ? C76 H76A 0.98 . ? C76 H76B 0.98 . ? C76 H76C 0.98 . ? C77 C80 0.53(6) 7_455 ? C77 C79 1.55(5) 7_455 ? C77 C78 1.491(17) . ? C77 H77A 0.99 . ? C77 H77B 0.99 . ? C78 C79 1.51(5) 7_455 ? C78 H78A 0.98 . ? C78 H78B 0.98 . ? C78 H78C 0.98 . ? C79 C77 1.55(5) 7_455 ? C79 C80 1.518(18) . ? C79 C78 1.51(5) 7_455 ? C79 H79A 0.99 . ? C79 H79B 0.99 . ? C79 H3A 1.1658 . ? C80 C77 0.53(6) 7_455 ? C80 N13 1.54(4) 7_455 ? C80 H80A 0.98 . ? C80 H80B 0.98 . ? C80 H80C 0.98 . ? C80 H3A 0.7228 . ? C81 C82 1.51(2) . ? C81 H81A 0.99 . ? C81 H81B 0.99 . ? C82 H82A 0.98 . ? C82 H82B 0.98 . ? C82 H82C 0.98 . ? N14 C83 1.238(14) . ? C83 C84 1.23(2) . ? C84 H84A 0.98 . ? C84 H84B 0.98 . ? C84 H84C 0.98 . ? N15 C85 1.230(17) . ? N15 H84C 1.2481 . ? C85 C86 1.24(2) . ? C86 H86A 0.98 . ? C86 H86B 0.98 . ? C86 H86C 0.98 . ? N16 C87 1.241(16) . ? N16 H86A 1.038 . ? C87 C88 1.22(2) . ? C87 H86A 0.6622 . ? C88 H88A 0.98 . ? C88 H88B 0.98 . ? C88 H88C 0.98 . ? O1 C89 1.28(2) . ? O1 H1 0.84 . ? C89 H89A 0.98 . ? C89 H89B 0.98 . ? C89 H89C 0.98 . ? N17 C91 1.234(14) . ? N17 H75A 0.9299 . ? N17 H75B 1.033 . ? C91 C92 1.242(16) . ? C91 H75B 1.1868 . ? C92 H76A 0.5749 . ? C92 H76B 1.293 . ? C92 H76C 1.2611 . ? C92 H92A 0.98 . ? C92 H92B 0.98 . ? C92 H92C 0.98 . ? O2 O2 1.16(6) 2_655 ? O2 C93 1.27(3) . ? O2 H2 0.84 . ? C93 H93A 0.98 . ? C93 H93B 0.98 . ? C93 H93C 0.98 . ? N18 C98 1.483(17) . ? N18 C96 1.499(17) . ? N18 C100 1.530(17) . ? N18 C94 1.558(17) . ? C94 C95 1.523(19) . ? C94 H94A 0.99 . ? C94 H94B 0.99 . ? C95 H95A 0.98 . ? C95 H95B 0.98 . ? C95 H95C 0.98 . ? C96 C97 1.498(18) . ? C96 H96A 0.99 . ? C96 H96B 0.99 . ? C97 H97A 0.98 . ? C97 H97B 0.98 . ? C97 H97C 0.98 . ? C98 C99 1.535(18) . ? C98 H98A 0.99 . ? C98 H98B 0.99 . ? C99 H99A 0.98 . ? C99 H99B 0.98 . ? C99 H99C 0.98 . ? C100 C101 1.507(19) . ? C100 H10A 0.99 . ? C100 H10B 0.99 . ? C101 H10C 0.98 . ? C101 H10D 0.98 . ? C101 H10E 0.98 . ? O3 C102 1.28(2) . ? O3 H79A 0.6201 . ? O3 H3A 0.84 . ? C102 H10F 0.98 . ? C102 H10G 0.98 . ? C102 H10H 0.98 . ? N1 Fe1 2.035(3) . ? N3 Fe1 2.037(3) . ? N5 Fe2 2.047(3) . ? N7 Fe2 2.073(3) . ? S1 Fe1 2.2124(11) . ? S1 Fe2 2.2416(12) . ? S2 Fe1 2.2131(10) . ? S2 Fe2 2.2304(10) . ? Fe1 Fe2 2.7123(9) . ? 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 C1 N1 114.8(4) . . ? N2 C1 C15 122.4(4) . . ? N1 C1 C15 122.7(3) . . ? C3 C2 N2 130.3(4) . . ? C3 C2 C7 120.7(5) . . ? N2 C2 C7 109.0(4) . . ? C2 C3 C4 118.4(5) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C3 C4 C5 121.0(5) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C4 C5 C6 121.0(5) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C7 C6 C5 117.6(4) . . ? C7 C6 H6 121.2 . . ? C5 C6 H6 121.2 . . ? N1 C7 C6 131.0(3) . . ? N1 C7 C2 107.8(4) . . ? C6 C7 C2 121.2(4) . . ? N4 C8 N3 114.9(4) . . ? N4 C8 C15 122.5(4) . . ? N3 C8 C15 122.6(3) . . ? C14 C9 N4 109.7(4) . . ? C14 C9 C10 120.2(5) . . ? N4 C9 C10 130.1(5) . . ? C11 C10 C9 117.7(6) . . ? C11 C10 H10 121.2 . . ? C9 C10 H10 121.2 . . ? C12 C11 C10 121.8(5) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C11 C12 C13 121.5(6) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C12 C13 C14 117.2(5) . . ? C12 C13 H13 121.4 . . ? C14 C13 H13 121.4 . . ? N3 C14 C9 107.6(4) . . ? N3 C14 C13 130.7(4) . . ? C9 C14 C13 121.6(4) . . ? C1 C15 C8 111.8(3) . . ? C1 C15 C16 109.9(4) . . ? C8 C15 C16 109.2(4) . . ? C1 C15 C21 106.6(3) . . ? C8 C15 C21 109.1(3) . . ? C16 C15 C21 110.3(4) . . ? C15 C16 C17 114.5(5) . . ? C15 C16 H16A 108.6 . . ? C17 C16 H16A 108.4 . . ? C15 C16 H16B 108.8 . . ? C17 C16 H16B 108.7 . . ? H16A C16 H16B 107.5 . . ? C18 C17 C16 110.2(11) . . ? C18 C17 H17A 109.6 . . ? C16 C17 H17A 109.6 . . ? C18 C17 H17B 109.6 . . ? C16 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? C17 C18 H20F 101.5 . . ? H18A C18 H20F 85.7 . . ? H18B C18 H20F 137.6 . . ? C20 C19 H16A 110.9 . . ? C20 C19 H19A 112.1 . . ? H16A C19 H19A 123.5 . . ? C20 C19 H19B 107.6 . . ? H16A C19 H19B 91.2 . . ? H19A C19 H19B 108.4 . . ? C19 C20 H20D 110.3 . . ? C19 C20 H20E 106.9 . . ? H20D C20 H20E 109.5 . . ? C19 C20 H20F 111.2 . . ? H20D C20 H20F 109.5 . . ? H20E C20 H20F 109.5 . . ? C22 C21 C15 115.9(3) . . ? C22 C21 H21A 108.3 . . ? C15 C21 H21A 108.3 . . ? C22 C21 H21B 108.3 . . ? C15 C21 H21B 108.3 . . ? H21A C21 H21B 107.4 . . ? C23 C22 C21 111.5(4) . . ? C23 C22 H22A 109.3 . . ? C21 C22 H22A 109.3 . . ? C23 C22 H22B 109.3 . . ? C21 C22 H22B 109.3 . . ? H22A C22 H22B 108 . . ? N6 C24 N5 115.7(3) . . ? N6 C24 C38 123.0(4) . . ? N5 C24 C38 121.3(3) . . ? N6 C25 C30 109.6(3) . . ? N6 C25 C26 131.1(5) . . ? C30 C25 C26 119.3(4) . . ? C27 C26 C25 117.9(5) . . ? C27 C26 H26 121 . . ? C25 C26 H26 121 . . ? C28 C27 C26 122.3(4) . . ? C28 C27 H27 118.9 . . ? C26 C27 H27 118.9 . . ? C27 C28 C29 120.5(4) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C28 C29 C30 118.1(4) . . ? C28 C29 H29 121 . . ? C30 C29 H29 121 . . ? N5 C30 C29 130.4(4) . . ? N5 C30 C25 107.6(3) . . ? C29 C30 C25 121.9(4) . . ? N8 C31 N7 116.0(4) . . ? N8 C31 C38 121.7(4) . . ? N7 C31 C38 122.2(3) . . ? N8 C32 C37 109.8(4) . . ? N8 C32 C33 130.2(5) . . ? C37 C32 C33 120.0(5) . . ? C34 C33 C32 117.9(6) . . ? C34 C33 H33 121 . . ? C32 C33 H33 121 . . ? C33 C34 C35 121.7(5) . . ? C33 C34 H34 119.1 . . ? C35 C34 H34 119.1 . . ? C34 C35 C36 121.6(5) . . ? C34 C35 H35 119.2 . . ? C36 C35 H35 119.2 . . ? C37 C36 C35 116.8(5) . . ? C37 C36 H36 121.6 . . ? C35 C36 H36 121.6 . . ? N7 C37 C36 130.5(4) . . ? N7 C37 C32 107.5(4) . . ? C36 C37 C32 121.9(4) . . ? C31 C38 C24 110.6(3) . . ? C31 C38 C39 110.7(4) . . ? C24 C38 C39 111.6(3) . . ? C31 C38 C44 106.9(3) . . ? C24 C38 C44 107.6(3) . . ? C39 C38 C44 109.2(4) . . ? C40 C39 C38 114.3(8) . . ? C40 C39 H39A 109.2 . . ? C38 C39 H39A 109 . . ? C40 C39 H39B 108.1 . . ? C38 C39 H39B 108.5 . . ? H39A C39 H39B 107.6 . . ? C39 C40 C41 112.9(19) . . ? C39 C40 H40A 109 . . ? C41 C40 H40A 109 . . ? C39 C40 H40B 109 . . ? C41 C40 H40B 109 . . ? H40A C40 H40B 107.8 . . ? C43 C42 H39A 114.1 . . ? C43 C42 H42A 110.6 . . ? H39A C42 H42A 88.7 . . ? C43 C42 H42B 109.6 . . ? H39A C42 H42B 123 . . ? H42A C42 H42B 108.2 . . ? C42 C43 H43A 110.5 . . ? C42 C43 H43B 108.9 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C38 116.3(4) . . ? C45 C44 H44A 108.2 . . ? C38 C44 H44A 108.2 . . ? C45 C44 H44B 108.2 . . ? C38 C44 H44B 108.2 . . ? H44A C44 H44B 107.4 . . ? C46 C45 C44 112.1(4) . . ? C46 C45 H45A 109.2 . . ? C44 C45 H45A 109.2 . . ? C46 C45 H45B 109.2 . . ? C44 C45 H45B 109.2 . . ? H45A C45 H45B 107.9 . . ? C51 N9 C53 113.6(7) . . ? C51 N9 C49 105.3(4) . . ? C53 N9 C49 112.0(5) . . ? C51 N9 C47 109.4(5) . . ? C53 N9 C47 107.6(5) . . ? C49 N9 C47 108.9(6) . . ? C48 C47 N9 116.1(6) . . ? C48 C47 H47A 108.3 . . ? N9 C47 H47A 108.3 . . ? C48 C47 H47B 108.3 . . ? N9 C47 H47B 108.3 . . ? H47A C47 H47B 107.4 . . ? C50 C49 N9 113.2(4) . . ? C50 C49 H49A 108.9 . . ? N9 C49 H49A 108.9 . . ? C50 C49 H49B 108.9 . . ? N9 C49 H49B 108.9 . . ? H49A C49 H49B 107.8 . . ? N9 C51 C52 112.8(5) . . ? N9 C51 H51A 109 . . ? C52 C51 H51A 109 . . ? N9 C51 H51B 109 . . ? C52 C51 H51B 109 . . ? H51A C51 H51B 107.8 . . ? N9 C53 C54 113.1(6) . . ? N9 C53 H53A 109 . . ? C54 C53 H53A 109 . . ? N9 C53 H53B 109 . . ? C54 C53 H53B 109 . . ? H53A C53 H53B 107.8 . . ? N11 N11 C63 105(2) 2 2 ? C63 N11 C63 148.2(11) 2 . ? N11 N11 C65 84.2(13) 2 . ? C63 N11 C65 65.0(11) 2 . ? C63 N11 C65 114.8(11) . . ? N11 N11 C61 150(2) 2 . ? C63 N11 C61 105.0(11) 2 . ? C63 N11 C61 104.8(10) . . ? C65 N11 C61 108.2(10) . . ? N11 N11 C59 93.9(14) 2 . ? C63 N11 C59 114.7(10) . . ? C65 N11 C59 105.6(11) . . ? C61 N11 C59 108.6(9) . . ? N11 N11 C65 68.9(12) 2 2 ? C63 N11 C65 135.6(13) 2 2 ? C65 N11 C65 70.5(14) . 2 ? C61 N11 C65 88.7(10) . 2 ? C59 N11 C65 162.5(11) . 2 ? N11 N11 C64 160.1(18) 2 2 ? C63 N11 C64 143.4(11) . 2 ? C65 N11 C64 98.7(12) . 2 ? C59 N11 C64 66.3(10) . 2 ? C65 N11 C64 130.7(11) 2 2 ? N11 N11 C59 61.9(12) 2 2 ? C63 N11 C59 124.5(13) 2 2 ? C65 N11 C59 145.9(10) . 2 ? C61 N11 C59 100.6(10) . 2 ? C59 N11 C59 81.4(11) . 2 ? C65 N11 C59 92.7(9) 2 2 ? C64 N11 C59 114.2(11) 2 2 ? C63 C59 C60 142.7(18) 2 . ? C60 C59 N11 113.0(13) . . ? C60 C59 N11 118.2(13) . 2 ? C63 C59 C64 56.7(11) 2 2 ? C60 C59 C64 87.7(15) . 2 ? N11 C59 C64 86.6(9) 2 2 ? C63 C59 H59A 106.6 2 . ? C60 C59 H59A 109.1 . . ? N11 C59 H59A 108.3 . . ? N11 C59 H59A 84.6 2 . ? C64 C59 H59A 163.2 2 . ? C60 C59 H59B 109.5 . . ? N11 C59 H59B 109.1 . . ? N11 C59 H59B 123.2 2 . ? H59A C59 H59B 107.6 . . ? C59 C60 C60 81.6(14) . 2 ? C59 C60 H60A 108.5 . . ? C60 C60 H60A 90.2 2 . ? C59 C60 H60B 110.4 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? C60 C60 H60C 151.7 2 . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C64 C61 C62 50.4(11) 2 . ? C64 C61 N11 76.9(10) 2 . ? C62 C61 N11 112.6(10) . . ? C64 C61 H61A 89.1 2 . ? C62 C61 H61A 108.9 . . ? N11 C61 H61A 108.7 . . ? C64 C61 H61B 157.9 2 . ? C62 C61 H61B 109.3 . . ? N11 C61 H61B 109.1 . . ? H61A C61 H61B 108.1 . . ? C64 C62 H62A 127 2 . ? C61 C62 H62A 109 . . ? C64 C62 H62B 50.8 2 . ? C61 C62 H62B 109.2 . . ? H62A C62 H62B 109.5 . . ? C64 C62 H62C 123.3 2 . ? C61 C62 H62C 110.2 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N11 C63 C59 92.4(13) 2 2 ? N11 C63 C65 71.9(10) 2 2 ? C59 C63 C65 151.1(16) 2 2 ? C59 C63 N11 87.0(12) 2 . ? C65 C63 N11 67.4(8) 2 . ? N11 C63 C64 83.4(11) 2 . ? C59 C63 C64 87.0(15) 2 . ? C65 C63 C64 114.1(16) 2 . ? N11 C63 C64 111.4(11) . . ? N11 C63 H63A 111.4 2 . ? C59 C63 H63A 154.8 2 . ? N11 C63 H63A 109.6 . . ? C64 C63 H63A 103.4 . . ? N11 C63 H63B 130.6 2 . ? C65 C63 H63B 127.9 2 . ? N11 C63 H63B 109.2 . . ? C64 C63 H63B 114.8 . . ? H63A C63 H63B 108.2 . . ? C62 C64 C61 71.2(15) 2 2 ? C62 C64 C63 122(2) 2 . ? C61 C64 C63 90.9(12) 2 . ? C62 C64 N11 111.5(19) 2 2 ? C62 C64 C59 158(2) 2 2 ? C61 C64 C59 101.6(13) 2 2 ? C63 C64 H64A 116.2 . . ? N11 C64 H64A 106.6 2 . ? C59 C64 H64A 152.3 2 . ? C62 C64 H64B 105.8 2 . ? C61 C64 H64B 159.7 2 . ? C63 C64 H64B 106.9 . . ? N11 C64 H64B 138.9 2 . ? C59 C64 H64B 88.1 2 . ? H64A C64 H64B 109.5 . . ? C62 C64 H64C 107.5 2 . ? C63 C64 H64C 105.2 . . ? N11 C64 H64C 75.5 2 . ? C59 C64 H64C 83.1 2 . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C63 C65 C66 154(3) 2 . ? C66 C65 N11 114.7(19) . . ? C66 C65 N11 110.7(17) . 2 ? C63 C65 C66 148(2) 2 2 ? N11 C65 C66 107(2) . 2 ? N11 C65 C66 100.7(16) 2 2 ? C63 C65 C65 100.4(8) 2 2 ? C66 C65 H65A 107.6 . . ? N11 C65 H65A 111.2 . . ? N11 C65 H65A 133.5 2 . ? C66 C65 H65A 117.3 2 . ? C65 C65 H65A 142.9 2 . ? C63 C65 H65B 98.9 2 . ? C66 C65 H65B 103.6 . . ? N11 C65 H65B 110.9 . . ? N11 C65 H65B 87.2 2 . ? C66 C65 H65B 102 2 . ? C65 C65 H65B 108.6 2 . ? H65A C65 H65B 108.3 . . ? C66 C66 C65 118(8) 2 . ? C65 C66 H66A 108.6 . . ? C66 C66 H66B 120.0 2 . ? C65 C66 H66B 117.2 . . ? C65 C66 H66B 170.6 2 . ? H66A C66 H66B 109.5 . . ? C66 C66 H66C 80.0 2 . ? C65 C66 H66C 102.3 . . ? C65 C66 H66C 73.7 2 . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C57 N10 C57 111.0(4) 2_554 . ? C57 N10 C55 111.0(2) 2_554 2_554 ? C57 N10 C55 106.5(2) . 2_554 ? C57 N10 C55 106.5(2) 2_554 . ? C57 N10 C55 111.0(2) . . ? C55 N10 C55 111.0(4) 2_554 . ? C56 C55 N10 114.9(3) . . ? C56 C55 H55A 108.5 . . ? N10 C55 H55A 108.5 . . ? C56 C55 H55B 108.5 . . ? N10 C55 H55B 108.5 . . ? H55A C55 H55B 107.5 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 N10 114.6(3) . . ? C58 C57 H57A 108.6 . . ? N10 C57 H57A 108.6 . . ? C58 C57 H57B 108.6 . . ? N10 C57 H57B 108.6 . . ? H57A C57 H57B 107.6 . . ? 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 . . ? N12 N12 C67 114(3) 7 7 ? N12 N12 C69 93(2) 7 7 ? C67 N12 C69 151.1(8) 7 7 ? C69 N12 C69 157.6(5) 7 . ? N12 N12 C71 133(3) 7 . ? C67 N12 C71 82.5(7) 7 . ? C69 N12 C71 86.9(8) 7 . ? C69 N12 C71 108.1(8) . . ? N12 N12 C73 113(3) 7 . ? C67 N12 C73 83.3(7) 7 . ? C69 N12 C73 75.9(7) 7 . ? C69 N12 C73 111.8(9) . . ? C71 N12 C73 112.1(7) . . ? C67 N12 C67 160.2(8) 7 . ? C69 N12 C67 110.2(6) . . ? C71 N12 C67 110.8(8) . . ? C73 N12 C67 103.8(8) . . ? C67 N12 C73 102.9(9) 7 7 ? C69 N12 C73 102.7(7) 7 7 ? C69 N12 C73 63.6(5) . 7 ? C71 N12 C73 84.3(7) . 7 ? C73 N12 C73 163.2(6) . 7 ? C67 N12 C73 65.5(5) . 7 ? C67 N12 C71 102.7(8) 7 7 ? C69 N12 C71 93.4(6) 7 7 ? C69 N12 C71 68.4(5) . 7 ? C71 N12 C71 167.5(6) . 7 ? C73 N12 C71 80.0(7) . 7 ? C67 N12 C71 61.4(5) . 7 ? C73 N12 C71 83.4(5) 7 7 ? C69 C67 N12 76.6(6) 7 7 ? C69 C67 C68 128.7(10) 7 . ? N12 C67 C68 107.2(9) 7 . ? C69 C67 N12 57.4(7) 7 . ? C68 C67 N12 114.1(8) . . ? C69 C67 C71 106.2(6) 7 7 ? C68 C67 C71 117.7(9) . 7 ? N12 C67 C71 69.8(6) . 7 ? C69 C67 C73 109.4(7) 7 7 ? C71 C67 C73 86.5(5) 7 7 ? C69 C67 C74 136.5(9) 7 7 ? N12 C67 C74 99.7(8) 7 7 ? N12 C67 C74 109.8(7) . 7 ? C71 C67 C74 106.4(7) 7 7 ? N12 C67 H67A 127.8 7 . ? C68 C67 H67A 108.8 . . ? N12 C67 H67A 108.8 . . ? C71 C67 H67A 129.4 7 . ? C73 C67 H67A 140.6 7 . ? C74 C67 H67A 120 7 . ? C69 C67 H67B 122.2 7 . ? N12 C67 H67B 95 7 . ? C68 C67 H67B 108.7 . . ? N12 C67 H67B 108.6 . . ? C73 C67 H67B 111.2 7 . ? C74 C67 H67B 101.3 7 . ? H67A C67 H67B 107.6 . . ? C74 C68 C73 78(2) 7 7 ? C74 C68 C67 138(3) 7 . ? C73 C68 C67 75.1(7) 7 . ? C67 C68 H68A 109.6 . . ? C74 C68 H68B 92.4 7 . ? C73 C68 H68B 168.2 7 . ? C67 C68 H68B 109.3 . . ? H68A C68 H68B 109.5 . . ? C74 C68 H68C 95.6 7 . ? C73 C68 H68C 78.3 7 . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67 C69 N12 75.0(6) 7 7 ? C67 C69 C70 126.1(9) 7 . ? N12 C69 C70 99.7(8) 7 . ? N12 C69 C70 115.2(8) . . ? C67 C69 C73 107.9(7) 7 7 ? C70 C69 C73 112.7(8) . 7 ? C67 C69 C71 102.9(6) 7 7 ? C73 C69 C71 84.0(4) 7 7 ? N12 C69 H69A 130.8 7 . ? N12 C69 H69A 108.7 . . ? C70 C69 H69A 108.4 . . ? C73 C69 H69A 135.9 7 . ? C71 C69 H69A 136.7 7 . ? C67 C69 H69B 125.4 7 . ? N12 C69 H69B 100.4 7 . ? N12 C69 H69B 108.4 . . ? C70 C69 H69B 108.4 . . ? C71 C69 H69B 114.8 7 . ? H69A C69 H69B 107.6 . . ? C72 C70 C69 142(3) 7 . ? C72 C70 C71 76.0(18) 7 7 ? C69 C70 C71 80.3(7) . 7 ? C69 C70 H70A 109.3 . . ? C72 C70 H70B 85.9 7 . ? C69 C70 H70B 109.8 . . ? C71 C70 H70B 159.5 7 . ? H70A C70 H70B 109.5 . . ? C72 C70 H70C 96.3 7 . ? C69 C70 H70C 109.3 . . ? C71 C70 H70C 82.3 7 . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? N12 C71 C72 114.8(9) . . ? N12 C71 C70 92.9(8) . 7 ? C72 C71 C67 138.0(9) . 7 ? C70 C71 C67 128.5(7) 7 7 ? C72 C71 N12 118.3(8) . 7 ? C70 C71 N12 93.8(6) 7 7 ? C72 C71 C69 73.1(7) . 7 ? C67 C71 C69 83.0(4) 7 7 ? N12 C71 H71A 108.9 . . ? C72 C71 H71A 108.1 . . ? C70 C71 H71A 131.9 7 . ? N12 C71 H71A 116.5 7 . ? C69 C71 H71A 136.7 7 . ? N12 C71 H71B 108.4 . . ? C72 C71 H71B 108.8 . . ? C70 C71 H71B 104.9 7 . ? C67 C71 H71B 112.1 7 . ? N12 C71 H71B 96.2 7 . ? C69 C71 H71B 112.7 7 . ? H71A C71 H71B 107.6 . . ? C70 C72 C71 77.8(19) 7 . ? C70 C72 H72A 108.7 7 . ? C71 C72 H72A 109.6 . . ? C70 C72 H72B 135.1 7 . ? C71 C72 H72B 110 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 108.8 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C74 C73 N12 113.2(8) . . ? C68 C73 N12 94.4(7) 7 . ? C74 C73 C69 145.4(10) . 7 ? C68 C73 C69 137.7(8) 7 7 ? C74 C73 N12 122.5(7) . 7 ? C68 C73 N12 101.0(7) 7 7 ? C69 C73 C67 87.7(4) 7 7 ? C74 C73 H73A 108.8 . . ? C68 C73 H73A 105.2 7 . ? N12 C73 H73A 109 . . ? C69 C73 H73A 105.3 7 . ? N12 C73 H73A 92.3 7 . ? C67 C73 H73A 114.9 7 . ? C74 C73 H73B 109 . . ? C68 C73 H73B 129.8 7 . ? N12 C73 H73B 109.1 . . ? N12 C73 H73B 114.3 7 . ? C67 C73 H73B 134.1 7 . ? H73A C73 H73B 107.7 . . ? C68 C74 C73 79(2) 7 . ? C68 C74 H74A 85.9 7 . ? C73 C74 H74A 109.4 . . ? C67 C74 H74A 71.5 7 . ? C68 C74 H74B 157.2 7 . ? C73 C74 H74B 109.5 . . ? C67 C74 H74B 170.1 7 . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? C67 C74 H74C 78.8 7 . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C80 N13 C79 115(2) 7_455 . ? C77 N13 C79 107.9(17) . . ? C80 N13 C81 98(2) 7_455 . ? C77 N13 C81 117.9(19) . . ? C79 N13 C81 105.0(17) . . ? C80 N13 C75 123(3) 7_455 . ? C77 N13 C75 114.6(19) . . ? C79 N13 C75 113.3(18) . . ? C81 N13 C75 97.6(16) . . ? C76 C75 N13 113(2) . . ? C76 C75 C80 97(2) . 7_455 ? C76 C75 H75A 115 . . ? N13 C75 H75A 104.8 . . ? C80 C75 H75A 92.5 7_455 . ? C76 C75 H75B 110.2 . . ? N13 C75 H75B 106 . . ? C80 C75 H75B 134.2 7_455 . ? H75A C75 H75B 107.7 . . ? C75 C76 H76A 116.8 . . ? C75 C76 H76B 103.4 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 107.9 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C80 C77 C79 76(5) 7_455 7_455 ? C80 C77 N13 88(6) 7_455 . ? C79 C77 N13 128(3) 7_455 . ? C78 C77 N13 136(2) . . ? C80 C77 H77A 146.7 7_455 . ? C79 C77 H77A 117.5 7_455 . ? C78 C77 H77A 109.9 . . ? N13 C77 H77A 102.3 . . ? C80 C77 H77B 102.4 7_455 . ? C78 C77 H77B 96.3 . . ? N13 C77 H77B 104 . . ? H77A C77 H77B 105.3 . . ? C77 C78 C79 62(2) . 7_455 ? C77 C78 H78A 101.1 . . ? C79 C78 H78A 155.7 7_455 . ? C77 C78 H78B 112.6 . . ? C79 C78 H78B 65.9 7_455 . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 114.3 . . ? C79 C78 H78C 94.1 7_455 . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C77 C79 N13 111(2) 7_455 . ? N13 C79 C80 120(2) . . ? N13 C79 C78 166(3) . 7_455 ? C77 C79 H79A 121.6 7_455 . ? N13 C79 H79A 103.1 . . ? C80 C79 H79A 101.7 . . ? C78 C79 H79A 77.8 7_455 . ? C77 C79 H79B 101.7 7_455 . ? N13 C79 H79B 111.8 . . ? C80 C79 H79B 111.3 . . ? C78 C79 H79B 81 7_455 . ? H79A C79 H79B 107.5 . . ? N13 C79 H3A 112.4 . . ? C78 C79 H3A 53.6 7_455 . ? H79A C79 H3A 78.1 . . ? H79B C79 H3A 132.6 . . ? C77 C80 N13 71(5) 7_455 7_455 ? C77 C80 C79 84(5) 7_455 . ? N13 C80 C79 125(3) 7_455 . ? C77 C80 C75 65(5) 7_455 7_455 ? C79 C80 C75 143(3) . 7_455 ? C79 C80 H80A 102.6 . . ? C77 C80 H80B 116.9 7_455 . ? C79 C80 H80B 112.4 . . ? C75 C80 H80B 70.1 7_455 . ? H80A C80 H80B 109.5 . . ? C77 C80 H80C 118.9 7_455 . ? N13 C80 H80C 121.7 7_455 . ? C79 C80 H80C 113.2 . . ? C75 C80 H80C 99.1 7_455 . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C77 C80 H3A 124.7 7_455 . ? N13 C80 H3A 111.5 7_455 . ? C75 C80 H3A 139.4 7_455 . ? H80A C80 H3A 141.5 . . ? H80B C80 H3A 71.5 . . ? H80C C80 H3A 105.9 . . ? N13 C81 C82 106.3(19) . . ? N13 C81 H81A 115 . . ? C82 C81 H81A 97.5 . . ? N13 C81 H81B 106.2 . . ? C82 C81 H81B 123.3 . . ? H81A C81 H81B 108.8 . . ? C81 C82 H82A 95 . . ? C81 C82 H82B 119.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 112.8 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C83 N14 H77A 71.6 . . ? C83 N14 H78B 108.8 . . ? H77A N14 H78B 172.5 . . ? H77B N14 H78B 123.1 . . ? C84 C83 N14 168(3) . . ? C84 C83 H77B 101.9 . . ? C83 C84 H84A 110 . . ? C83 C84 H84B 112.1 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 106.3 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C85 N15 H84C 116.8 . . ? N15 C85 C86 165(5) . . ? C85 C86 H86A 107.2 . . ? C85 C86 H86B 110.7 . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 110.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C88 C87 N16 160(3) . . ? C88 C87 H86A 127.4 . . ? C88 C87 H86B 76.8 . . ? N16 C87 H86B 85.8 . . ? H86A C87 H86B 79.9 . . ? C89 O1 H1 109.4 . . ? C91 N17 H75A 82.8 . . ? C91 N17 H75B 62.4 . . ? H75A N17 H75B 109 . . ? N17 C91 C92 160.6(16) . . ? C92 C91 H75A 124.5 . . ? N17 C91 H75B 50.5 . . ? C92 C91 H75B 122.4 . . ? H75A C91 H75B 74 . . ? C91 C92 H76A 138.8 . . ? C91 C92 H76B 96.6 . . ? H76A C92 H76B 112.1 . . ? C91 C92 H76C 97.9 . . ? H76A C92 H76C 116.2 . . ? H76B C92 H76C 77.6 . . ? O2 O2 C93 154(7) 2_655 . ? O2 O2 H2 50.3 2_655 . ? C93 O2 H2 109.1 . . ? O2 C93 H93A 109.9 . . ? O2 C93 H93B 109.3 . . ? H93A C93 H93B 109.5 . . ? O2 C93 H93C 109.3 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 111.00 . . ? C98 N18 C96 108.0(19) . . ? C98 N18 C100 112(2) . . ? C96 N18 C100 111.6(19) . . ? C98 N18 C94 109.7(19) . . ? C96 N18 C94 112(2) . . ? C100 N18 C94 103.5(18) . . ? C95 C94 N18 112(2) . . ? C95 C94 H94A 109.8 . . ? N18 C94 H94A 111.8 . . ? C95 C94 H94B 106.4 . . ? N18 C94 H94B 108.9 . . ? H94A C94 H94B 107.7 . . ? C94 C95 H95A 110.3 . . ? C94 C95 H95B 107.1 . . ? H95A C95 H95B 109.5 . . ? C94 C95 H95C 111 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? C97 C96 N18 116(2) . . ? C97 C96 H96A 111.5 . . ? N18 C96 H96A 106.6 . . ? C97 C96 H96B 108.3 . . ? N18 C96 H96B 106.7 . . ? H96A C96 H96B 107.3 . . ? C96 C97 H97A 112.9 . . ? C96 C97 H97B 106.5 . . ? H97A C97 H97B 109.5 . . ? C96 C97 H97C 108.9 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? N18 C98 C99 114(2) . . ? N18 C98 H98A 110.3 . . ? C99 C98 H98A 102.6 . . ? N18 C98 H98B 109.9 . . ? C99 C98 H98B 112.1 . . ? H98A C98 H98B 109.0 . . ? C98 C99 H99A 116.1 . . ? C98 C99 H99B 106.5 . . ? H99A C99 H99B 109.5 . . ? C98 C99 H99C 105.6 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? N18 C100 C101 106(2) . . ? N18 C100 H10A 107.4 . . ? C101 C100 H10A 116.1 . . ? N18 C100 H10B 110.8 . . ? C101 C100 H10B 108.4 . . ? H10A C100 H10B 108 . . ? C100 C101 H10C 102.3 . . ? C100 C101 H10D 114 . . ? H10C C101 H10D 109.5 . . ? C100 C101 H10E 111.9 . . ? H10C C101 H10E 109.5 . . ? H10D C101 H10E 109.5 . . ? C102 O3 H79B 128.8 . . ? H79A O3 H79B 94.5 . . ? C102 O3 H3A 110.1 . . ? H79A O3 H3A 137.9 . . ? H79B O3 H3A 119.2 . . ? O3 C102 H75A 137.1 . . ? H75A C102 H79A 132.2 . . ? C1 N1 C7 104.3(3) . . ? C1 N1 Fe1 125.5(3) . . ? C7 N1 Fe1 130.1(3) . . ? C1 N2 C2 104.0(3) . . ? C8 N3 C14 104.2(3) . . ? C8 N3 Fe1 125.7(2) . . ? C14 N3 Fe1 130.1(3) . . ? C8 N4 C9 103.5(4) . . ? C24 N5 C30 104.2(3) . . ? C24 N5 Fe2 128.7(2) . . ? C30 N5 Fe2 127.1(3) . . ? C24 N6 C25 102.9(3) . . ? C31 N7 C37 103.7(3) . . ? C31 N7 Fe2 126.8(2) . . ? C37 N7 Fe2 128.5(3) . . ? C31 N8 C32 103.0(4) . . ? Fe1 S1 Fe2 75.03(3) . . ? Fe1 S2 Fe2 75.24(3) . . ? N1 Fe1 N3 86.88(13) . . ? N1 Fe1 S1 116.29(9) . . ? N3 Fe1 S1 118.19(9) . . ? N1 Fe1 S2 115.63(9) . . ? N3 Fe1 S2 114.02(9) . . ? S1 Fe1 S2 105.61(4) . . ? N1 Fe1 Fe2 138.05(9) . . ? N3 Fe1 Fe2 135.00(9) . . ? S1 Fe1 Fe2 52.98(3) . . ? S2 Fe1 Fe2 52.67(3) . . ? N5 Fe2 N7 85.33(12) . . ? N5 Fe2 S2 112.05(9) . . ? N7 Fe2 S2 122.42(9) . . ? N5 Fe2 S1 119.56(9) . . ? N7 Fe2 S1 113.78(9) . . ? S2 Fe2 S1 104.05(4) . . ? N5 Fe2 Fe1 136.52(8) . . ? N7 Fe2 Fe1 138.15(9) . . ? S2 Fe2 Fe1 52.09(3) . . ? S1 Fe2 Fe1 52.00(3) . . ? # END of CIF 2