# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address 'Wolfgang Bauer' ; Department Chemie und Biochemie Ludwig-Maximilians Universit\"at Butenandtstra\&se 5-13 (Haus D) D-81377 M\"unchen Bundesrepublik Deutschland ; M.M.Dirtu ; Institute of Condensed Matter and Nanosciences MOST- Inorganic Chemistry Universit\'e Catholique de Louvain Place L. Pasteur 1 1348 Louvain-la-Neuve Belgium ; 'Yann Garcia' ; Institute of Condensed Matter and Nanosciences MOST- Inorganic Chemistry Universit\'e Catholique de Louvain Place L. Pasteur 1 1348 Louvain-la-Neuve Belgium ; _publ_contact_author_address ; Inorganic Chemistry II Universit\"at Bayreuth Universit\"atsstra\&se 30 (NW I) D-95440 Bayreuth Bundesrepublik Deutschland ; _publ_contact_author_email weber@uni-bayreuth.de _publ_contact_author_fax +49-92155-2157 _publ_contact_author_phone +49-92155-2555 #TrackingRef 'allcif_poly.cif' _publ_contact_author_name 'Birgit Weber' _publ_section_title ; Iron(II) Spin transition Coordination Polymers with a Zigzag Structure ; data_mo231 _database_code_depnum_ccdc_archive 'CCDC 729769' _publ_section_abstract ? _publ_section_comment ? _audit_update_record 26-Aug-08 _chemical_name_common ; poly-(E,E)-((diethyl-2,2'-(1,2- phenylenebis(iminomethylidyne))bis(3-oxobutanato) (2-)- N,N',O$3,O!3')(bis(4-pyridylmethyl)sulfide)iron(ii) ; _chemical_compound_source ; The synthesis of (I) was carried out under argon using Schlenk tube techniques. [Fe(L1a)(MeOH)~2~] (0.43 g, 0.85 mmol) and Bis(4-pyridylmethyl)sulfide (0.92 g, 4.25 mmol) were dissolved in 50 ml ethanol and heated to reflux for four hours. After 24 hours at room temperature the product was filtered off and washed two times with ice-cold ethanol. (I) was obtained as dark purple solid with a yield of 75%. Crystals suitable for X-ray structure analysis were obtain after recrystallization from toluene. ; _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.49 #?# in millimeters _exptl_crystal_size_mid 0.44 #?# in millimeters _exptl_crystal_size_min 0.41 #?# in millimeters _exptl_crystal_density_method 'not measured' _exptl_crystal_density_meas 1.4446 _exptl_special_details ? #?# all that happened prior to measurement (crystal embedded in mother liquor) #:---------------------------------------------------------------------------- #:---------------------------DATA COLLECTION---------------------------------- #:---------------------------------------------------------------------------- _audit_author_name 'Weber, B.' _audit_creation_date ; 'Sat Aug 23 20:54:50 2008' ; _diffrn_ambient_temperature 225(2) #?# in K _diffrn_source_type 'Spellman generator' _diffrn_source_power 2.50 #?# in kW _diffrn_source_voltage 55 #?# in kV _diffrn_source_current 45 #?# in mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation '0.5 mm collimator' _diffrn_measurement_device 'CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Oxford XCalibur' _diffrn_measurement_method '\w scans' _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 phi -149.00 -89.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames -40.0000 -20.9181 0.0000 - 0.0000 0.0000 60 #__ type_ start__ end____ width___ exp.time_ 2 omega -2.00 50.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -20.9181 75.0000 120.0000 0.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 3 omega -47.00 3.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -20.9181 45.0000 240.0000 0.0000 0.0000 50 #__ type_ start__ end____ width___ exp.time_ 4 omega -52.00 0.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -20.9181 75.0000 0.0000 0.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 5 phi 89.00 149.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames -40.0000 -20.9181 0.0000 - 0.0000 0.0000 60 #__ type_ start__ end____ width___ exp.time_ 6 omega -52.00 0.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -20.9181 75.0000 120.0000 0.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 7 omega 40.00 92.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 21.0744 75.0000 120.0000 0.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 8 phi -61.00 1.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames 40.0000 21.0744 0.0000 - 0.0000 0.0000 62 #__ type_ start__ end____ width___ exp.time_ 9 phi 59.00 121.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames 40.0000 21.0744 0.0000 - 0.0000 0.0000 62 #__ type_ start__ end____ width___ exp.time_ 10 omega -10.00 42.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 21.0744 75.0000 0.0000 0.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 11 omega -10.00 42.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 21.0744 75.0000 240.0000 0.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 12 omega 1.00 52.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 21.0744 -75.0000 120.0000 0.0000 0.0000 51 #__ type_ start__ end____ width___ exp.time_ 13 omega 40.00 92.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 21.0744 75.0000 0.0000 0.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 14 omega 40.00 92.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 21.0744 75.0000 240.0000 0.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 15 omega -10.00 42.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 21.0744 75.0000 120.0000 0.0000 0.0000 52 #__ type_ start__ end____ width___ exp.time_ 16 omega -38.00 -5.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 21.0744 -75.0000 120.0000 0.0000 0.0000 33 #__ type_ start__ end____ width___ exp.time_ 17 omega -51.00 -1.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 21.0744 -45.0000 240.0000 0.0000 0.0000 50 #__ type_ start__ end____ width___ exp.time_ 18 omega -27.00 20.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 21.0744 -97.0000 345.0000 0.0000 0.0000 47 #__ type_ start__ end____ width___ exp.time_ 19 omega -5.00 23.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 21.0744 45.0000 120.0000 0.0000 0.0000 28 #__ type_ start__ end____ width___ exp.time_ 20 omega 12.00 53.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 21.0744 -76.0000 16.0000 0.0000 0.0000 41 #__ type_ start__ end____ width___ exp.time_ 21 omega 41.00 82.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 21.0744 -129.0000 327.0000 0.0000 0.0000 41 #__ type_ start__ end____ width___ exp.time_ 22 omega -3.00 47.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 21.0744 -45.0000 240.0000 0.0000 0.0000 50 #__ type_ start__ end____ width___ exp.time_ 23 phi -121.00 -93.00 1.0000 8.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames 40.0000 21.0744 0.0000 - 0.0000 0.0000 28 ; _diffrn_detector_area_resol_mean 15.9809 _diffrn_special_details ? _diffrn_orient_matrix_type ? _diffrn_orient_matrix_UB_11 0.0266964541 _diffrn_orient_matrix_UB_12 0.0076821107 _diffrn_orient_matrix_UB_13 0.0512497265 _diffrn_orient_matrix_UB_21 0.0516478689 _diffrn_orient_matrix_UB_22 0.0050084188 _diffrn_orient_matrix_UB_23 -0.0159386309 _diffrn_orient_matrix_UB_31 -0.0128955095 _diffrn_orient_matrix_UB_32 0.0360252046 _diffrn_orient_matrix_UB_33 -0.0087060680 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? ? _cell_length_a 12.164(7) _cell_length_b 19.0805(11) _cell_length_c 16.115(7) _cell_angle_alpha 90.00 _cell_angle_beta 125.95(3) _cell_angle_gamma 90.00 _cell_volume 3028(2) _cell_measurement_temperature 225(2) #?# in K _cell_measurement_reflns_used 6475 _cell_measurement_theta_min 3.7719 _cell_measurement_theta_max 26.2499 _cell_special_details ? #?# supposed (pseudo-)symmetries,subcells,deviation from standard setting loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? #?# same style as for the absorption correction routine, e.g.: #?# -1 0 -1 .0424 #:---------------------------------------------------------------------------- #:---------------------------ABSORPTION CORRECTION---------------------------- #:---------------------------------------------------------------------------- _exptl_absorpt_coefficient_mu 0.619 _exptl_absorpt_correction_type none #numerical (using crystal faces), refdelf (using DIFABS) _exptl_absorpt_correction_T_min . _exptl_absorpt_correction_T_max . _exptl_absorpt_process_details ? #?# 'XRed, rev. 1.09, Stoe (Darmstadt, Germany)' #:---------------------------------------------------------------------------- #:------------------------REFLECTION DATA ANALYSIS---------------------------- #:---------------------------------------------------------------------------- _diffrn_reflns_number 57671 #xl _diffrn_reflns_av_R_equivalents 0.0604 #xl _diffrn_reflns_av_sigmaI/netI 0.0292 #xl _diffrn_reflns_limit_h_min -15 #xl _diffrn_reflns_limit_h_max 15 #xl _diffrn_reflns_limit_k_min -23 #xl _diffrn_reflns_limit_k_max 23 #xl _diffrn_reflns_limit_l_min -20 #xl _diffrn_reflns_limit_l_max 20 #xl _diffrn_reflns_theta_min 3.78 #xl _diffrn_reflns_theta_max 26.31 #xl _diffrn_measured_fraction_theta_max 0.995 #xl _diffrn_reflns_theta_full 26.31 #xl _diffrn_measured_fraction_theta_full 0.995 #xl #:---------------------------------------------------------------------------- #:---------------------STRUCTURE SOLUTION AND REFINEMENT---------------------- #:---------------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _reflns_number_total 6157 #xl _reflns_number_gt 4539 #xl _reflns_threshold_expression >2sigma(I) #xl _reflns_special_details ? #?# "A description of reflection data not covered by the other data #?# names. It should include details of the Friedel pairs." _refine_ls_structure_factor_coef Fsqd #xl _refine_ls_matrix_type full #xl _refine_ls_weighting_scheme calc #xl _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+2.0115P] where P=(Fo^2^+2Fc^2^)/3' #xl _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refU _refine_ls_extinction_method none #xl _refine_ls_extinction_coef ? #xl _refine_ls_abs_structure_details ? #xl _refine_ls_abs_structure_Flack ? #xl _refine_ls_number_reflns 6157 #xl _refine_ls_number_parameters 401 #xl _refine_ls_number_restraints 0 #xl _refine_ls_R_factor_all 0.0571 #xl _refine_ls_R_factor_gt 0.0363 #xl _refine_ls_wR_factor_ref 0.1097 #xl _refine_ls_wR_factor_gt 0.0903 #xl _refine_ls_goodness_of_fit_ref 1.064 #xl _refine_ls_restrained_S_all 1.064 #xl _refine_ls_shift/su_max 0.000 #xl _refine_ls_shift/su_mean 0.000 #xl _refine_diff_density_max 0.458 #xl _refine_diff_density_min -0.435 #xl _refine_diff_density_rms 0.056 #xl _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. Anisotrop refinement of all none-hydrogen atoms. Details of H atom refinement: riding with U(H)=1.2*U(C) for CH2 and CH, 1.5*U(C) for CH3 C-bonded H: constr ; #:---------------------------------------------------------------------------- #:-----------------------------REFERENCES------------------------------------- #:---------------------------------------------------------------------------- _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_solution ; A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A. Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for crystal structure determination and refinement; J. Appl. Crystallogr. 1999, 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ; ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid Plot Program for Crystal Structure Illustrations, Oak Ridge National Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ. Glasgow) used --- SCHAKAL (E. Keller, University of Freiburg (Breisgau), Germany, 1995). ; _computing_publication_material ; PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version). #-- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses). ; #:---------------------------------------------------------------------------- #:---------------------TABLES AND GEOMETRICAL DATA---------------------------- #:---------------------------------------------------------------------------- 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 -0.17333(3) -0.207229(16) 0.04037(2) 0.03079(11) Uani 1 1 d . . . S1 S 0.28379(6) -0.52574(4) 0.17319(5) 0.04635(18) Uani 1 1 d . . . O1 O -0.11598(16) -0.18533(8) 0.18160(12) 0.0361(4) Uani 1 1 d . . . O2 O -0.31872(16) -0.28141(8) -0.01733(13) 0.0400(4) Uani 1 1 d . . . O3 O -0.6059(2) -0.34955(11) -0.31616(17) 0.0688(6) Uani 1 1 d . . . O4 O -0.55478(19) -0.25733(10) -0.37065(14) 0.0553(5) Uani 1 1 d . . . O5 O 0.1462(2) -0.03170(11) 0.39367(14) 0.0611(6) Uani 1 1 d . . . O6 O 0.22418(16) -0.01525(9) 0.30059(12) 0.0398(4) Uani 1 1 d . . . N1 N -0.03330(18) -0.13205(9) 0.06426(13) 0.0270(4) Uani 1 1 d . . . N2 N -0.20952(18) -0.20695(9) -0.10302(13) 0.0295(4) Uani 1 1 d . . . N3 N -0.01613(19) -0.29165(9) 0.09858(14) 0.0327(4) Uani 1 1 d . . . N4 N 0.6635(2) -0.37810(10) 0.48052(14) 0.0362(4) Uani 1 1 d . . . C1 C -0.0355(2) -0.14115(11) 0.24899(16) 0.0312(5) Uani 1 1 d . . . C2 C 0.0440(2) -0.09462(11) 0.23522(16) 0.0298(5) Uani 1 1 d . . . C3 C 0.0406(2) -0.09292(11) 0.14538(16) 0.0283(4) Uani 1 1 d . . . H3 H 0.0976 -0.0601 0.1446 0.034 Uiso 1 1 calc R . . C4 C -0.0216(2) -0.12669(11) -0.01837(15) 0.0277(4) Uani 1 1 d . . . C5 C 0.0749(2) -0.08608(12) -0.01668(17) 0.0343(5) Uani 1 1 d . . . H5 H 0.1365 -0.0589 0.0415 0.041 Uiso 1 1 calc R . . C6 C 0.0810(2) -0.08533(13) -0.09945(18) 0.0377(5) Uani 1 1 d . . . H6 H 0.1443 -0.0564 -0.0985 0.045 Uiso 1 1 calc R . . C7 C -0.0054(3) -0.12693(13) -0.18370(18) 0.0399(6) Uani 1 1 d . . . H7 H 0.0008 -0.1272 -0.2391 0.048 Uiso 1 1 calc R . . C8 C -0.1009(2) -0.16808(12) -0.18676(17) 0.0366(5) Uani 1 1 d . . . H8 H -0.1582 -0.1970 -0.2439 0.044 Uiso 1 1 calc R . . C9 C -0.1136(2) -0.16740(11) -0.10626(16) 0.0294(5) Uani 1 1 d . . . C10 C -0.3179(2) -0.23270(12) -0.18678(17) 0.0350(5) Uani 1 1 d . . . H10 H -0.3327 -0.2201 -0.2490 0.042 Uiso 1 1 calc R . . C11 C -0.4157(2) -0.27782(12) -0.19328(19) 0.0385(5) Uani 1 1 d . . . C12 C -0.4069(2) -0.30329(12) -0.1074(2) 0.0392(6) Uani 1 1 d . . . C13 C -0.0301(3) -0.14227(14) 0.3444(2) 0.0459(6) Uani 1 1 d . . . H13A H -0.0990 -0.1740 0.3349 0.069 Uiso 1 1 calc R . . H13B H -0.0466 -0.0955 0.3583 0.069 Uiso 1 1 calc R . . H13C H 0.0588 -0.1581 0.4017 0.069 Uiso 1 1 calc R . . C14 C -0.4982(3) -0.35989(15) -0.1149(2) 0.0585(8) Uani 1 1 d . . . H14A H -0.4803 -0.3668 -0.0483 0.088 Uiso 1 1 calc R . . H14B H -0.4810 -0.4032 -0.1370 0.088 Uiso 1 1 calc R . . H14C H -0.5922 -0.3462 -0.1642 0.088 Uiso 1 1 calc R . . C15 C 0.1392(2) -0.04608(12) 0.31764(17) 0.0352(5) Uani 1 1 d . . . C16 C 0.3182(3) 0.03528(14) 0.37566(19) 0.0429(6) Uani 1 1 d . . . H16A H 0.3758 0.0136 0.4436 0.051 Uiso 1 1 calc R . . H16B H 0.2691 0.0745 0.3791 0.051 Uiso 1 1 calc R . . C17 C 0.4029(3) 0.06041(14) 0.3415(2) 0.0495(7) Uani 1 1 d . . . H17A H 0.4516 0.0211 0.3391 0.074 Uiso 1 1 calc R . . H17B H 0.4674 0.0952 0.3895 0.074 Uiso 1 1 calc R . . H17C H 0.3444 0.0812 0.2738 0.074 Uiso 1 1 calc R . . C18 C -0.5317(3) -0.30019(13) -0.2955(2) 0.0448(6) Uani 1 1 d . . . C19 C -0.6758(3) -0.27482(18) -0.4718(2) 0.0611(8) Uani 1 1 d . . . H19A H -0.6678 -0.3222 -0.4912 0.073 Uiso 1 1 calc R . . H19B H -0.7562 -0.2732 -0.4716 0.073 Uiso 1 1 calc R . . C20 C -0.6884(4) -0.2240(2) -0.5437(3) 0.0811(11) Uani 1 1 d . . . H20A H -0.7007 -0.1776 -0.5257 0.122 Uiso 1 1 calc R . . H20B H -0.7661 -0.2357 -0.6125 0.122 Uiso 1 1 calc R . . H20C H -0.6067 -0.2246 -0.5412 0.122 Uiso 1 1 calc R . . C21 C 0.1155(3) -0.27546(13) 0.1538(2) 0.0480(7) Uani 1 1 d . . . H21 H 0.1418 -0.2301 0.1816 0.058 Uiso 1 1 calc R . . C22 C 0.2149(2) -0.32112(13) 0.1726(2) 0.0464(6) Uani 1 1 d . . . H22 H 0.3061 -0.3067 0.2123 0.056 Uiso 1 1 calc R . . C23 C 0.1809(2) -0.38835(12) 0.13322(16) 0.0334(5) Uani 1 1 d . . . C24 C 0.0456(2) -0.40666(13) 0.08149(18) 0.0396(6) Uani 1 1 d . . . H24 H 0.0177 -0.4527 0.0571 0.048 Uiso 1 1 calc R . . C25 C -0.0476(2) -0.35806(12) 0.06564(18) 0.0368(5) Uani 1 1 d . . . H25 H -0.1389 -0.3720 0.0296 0.044 Uiso 1 1 calc R . . C26 C 0.2848(2) -0.43573(14) 0.14071(19) 0.0419(6) Uani 1 1 d . . . H26A H 0.3750 -0.4163 0.1922 0.050 Uiso 1 1 calc R . . H26B H 0.2720 -0.4347 0.0747 0.050 Uiso 1 1 calc R . . C27 C 0.3231(3) -0.51704(14) 0.3000(2) 0.0471(6) Uani 1 1 d . . . H27A H 0.2445 -0.4971 0.2941 0.057 Uiso 1 1 calc R . . H27B H 0.3408 -0.5636 0.3312 0.057 Uiso 1 1 calc R . . C28 C 0.4445(2) -0.47099(12) 0.36802(17) 0.0379(5) Uani 1 1 d . . . C29 C 0.4339(3) -0.40964(14) 0.4085(2) 0.0458(6) Uani 1 1 d . . . H29 H 0.3516 -0.3981 0.3982 0.055 Uiso 1 1 calc R . . C30 C 0.5442(3) -0.36550(14) 0.4641(2) 0.0455(6) Uani 1 1 d . . . H30 H 0.5350 -0.3245 0.4917 0.055 Uiso 1 1 calc R . . C31 C 0.6739(2) -0.43844(13) 0.44329(19) 0.0417(6) Uani 1 1 d . . . H31 H 0.7576 -0.4491 0.4553 0.050 Uiso 1 1 calc R . . C32 C 0.5692(3) -0.48584(13) 0.3884(2) 0.0440(6) Uani 1 1 d . . . H32 H 0.5826 -0.5279 0.3650 0.053 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 0.03119(18) 0.02845(18) 0.02649(17) -0.00082(12) 0.01345(14) -0.00224(13) S1 0.0360(3) 0.0444(4) 0.0443(4) -0.0112(3) 0.0155(3) 0.0015(3) O1 0.0409(9) 0.0349(8) 0.0326(8) -0.0002(7) 0.0217(8) -0.0050(7) O2 0.0368(9) 0.0356(9) 0.0438(10) 0.0036(7) 0.0214(8) -0.0019(7) O3 0.0584(13) 0.0529(12) 0.0627(13) -0.0131(10) 0.0173(11) -0.0242(11) O4 0.0455(11) 0.0568(12) 0.0373(10) -0.0081(9) 0.0097(9) -0.0112(9) O5 0.0789(14) 0.0747(14) 0.0403(10) -0.0254(10) 0.0409(11) -0.0346(11) O6 0.0390(9) 0.0447(10) 0.0330(8) -0.0130(7) 0.0196(8) -0.0125(8) N1 0.0292(9) 0.0240(9) 0.0244(9) 0.0009(7) 0.0138(8) -0.0001(7) N2 0.0298(10) 0.0242(9) 0.0277(9) -0.0022(7) 0.0130(8) -0.0014(7) N3 0.0322(10) 0.0325(10) 0.0259(9) -0.0013(8) 0.0128(8) -0.0031(8) N4 0.0385(11) 0.0313(10) 0.0319(10) -0.0013(8) 0.0168(9) -0.0007(8) C1 0.0338(12) 0.0298(11) 0.0274(11) 0.0007(9) 0.0165(10) 0.0027(9) C2 0.0326(11) 0.0274(11) 0.0262(10) -0.0001(9) 0.0155(9) 0.0010(9) C3 0.0288(11) 0.0268(11) 0.0268(10) 0.0011(9) 0.0149(9) -0.0015(9) C4 0.0293(11) 0.0266(11) 0.0256(10) 0.0005(8) 0.0152(9) 0.0038(9) C5 0.0379(13) 0.0331(12) 0.0319(11) -0.0036(9) 0.0204(10) -0.0047(10) C6 0.0385(13) 0.0405(13) 0.0423(13) 0.0018(11) 0.0284(11) -0.0010(11) C7 0.0490(15) 0.0442(14) 0.0335(12) -0.0006(10) 0.0281(12) 0.0037(11) C8 0.0414(13) 0.0369(13) 0.0266(11) -0.0051(10) 0.0172(10) -0.0011(10) C9 0.0325(11) 0.0241(11) 0.0277(11) 0.0025(8) 0.0155(9) 0.0044(9) C10 0.0370(12) 0.0293(11) 0.0303(11) -0.0031(9) 0.0151(10) 0.0005(10) C11 0.0341(12) 0.0277(12) 0.0437(14) -0.0027(10) 0.0171(11) -0.0001(10) C12 0.0301(12) 0.0301(12) 0.0477(14) 0.0018(10) 0.0174(11) 0.0038(10) C13 0.0592(17) 0.0477(15) 0.0430(14) -0.0047(12) 0.0368(14) -0.0084(13) C14 0.0486(16) 0.0511(17) 0.0688(19) 0.0015(14) 0.0306(15) -0.0131(13) C15 0.0371(12) 0.0355(12) 0.0272(11) -0.0017(9) 0.0157(10) -0.0025(10) C16 0.0410(14) 0.0437(14) 0.0355(13) -0.0121(11) 0.0177(11) -0.0117(11) C17 0.0451(15) 0.0433(15) 0.0565(16) -0.0071(12) 0.0278(14) -0.0075(12) C18 0.0386(14) 0.0322(13) 0.0478(15) -0.0069(11) 0.0165(12) -0.0017(11) C19 0.0476(17) 0.071(2) 0.0411(15) -0.0181(14) 0.0127(14) -0.0100(15) C20 0.074(2) 0.088(3) 0.054(2) 0.0010(18) 0.0223(18) 0.003(2) C21 0.0383(14) 0.0307(13) 0.0475(15) 0.0044(11) 0.0097(12) -0.0043(11) C22 0.0273(12) 0.0393(14) 0.0491(15) 0.0096(12) 0.0092(11) -0.0031(11) C23 0.0310(12) 0.0429(13) 0.0239(10) 0.0065(9) 0.0147(10) 0.0025(10) C24 0.0350(13) 0.0416(14) 0.0366(13) -0.0124(10) 0.0178(11) -0.0059(11) C25 0.0308(12) 0.0395(13) 0.0372(12) -0.0074(10) 0.0183(10) -0.0054(10) C26 0.0335(13) 0.0576(16) 0.0336(12) 0.0051(11) 0.0191(11) 0.0048(11) C27 0.0429(14) 0.0456(15) 0.0427(14) 0.0027(12) 0.0194(12) -0.0091(12) C28 0.0419(13) 0.0369(13) 0.0289(11) 0.0071(10) 0.0175(11) -0.0042(11) C29 0.0421(14) 0.0509(16) 0.0519(15) -0.0015(12) 0.0318(13) -0.0033(12) C30 0.0515(16) 0.0415(14) 0.0521(15) -0.0085(12) 0.0354(14) -0.0038(12) C31 0.0312(12) 0.0337(13) 0.0453(14) 0.0005(11) 0.0142(11) 0.0046(10) C32 0.0396(14) 0.0315(13) 0.0466(14) -0.0030(11) 0.0173(12) 0.0002(11) 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 O1 1.9943(18) . ? Fe1 O2 2.0162(18) . ? Fe1 N1 2.0825(19) . ? Fe1 N2 2.083(2) . ? Fe1 N3 2.242(2) . ? Fe1 N4 2.296(2) 4_455 ? S1 C26 1.798(3) . ? S1 C27 1.812(3) . ? O1 C1 1.265(3) . ? O2 C12 1.267(3) . ? O3 C18 1.209(3) . ? O4 C18 1.347(3) . ? O4 C19 1.455(3) . ? O5 C15 1.209(3) . ? O6 C15 1.350(3) . ? O6 C16 1.441(3) . ? N1 C3 1.302(3) . ? N1 C4 1.423(3) . ? N2 C10 1.309(3) . ? N2 C9 1.416(3) . ? N3 C21 1.334(3) . ? N3 C25 1.340(3) . ? N4 C30 1.335(3) . ? N4 C31 1.338(3) . ? N4 Fe1 2.296(2) 4_656 ? C1 C2 1.423(3) . ? C1 C13 1.500(3) . ? C2 C3 1.424(3) . ? C2 C15 1.469(3) . ? C3 H3 0.9400 . ? C4 C5 1.393(3) . ? C4 C9 1.414(3) . ? C5 C6 1.379(3) . ? C5 H5 0.9400 . ? C6 C7 1.379(3) . ? C6 H6 0.9400 . ? C7 C8 1.379(3) . ? C7 H7 0.9400 . ? C8 C9 1.394(3) . ? C8 H8 0.9400 . ? C10 C11 1.421(3) . ? C10 H10 0.9400 . ? C11 C12 1.410(4) . ? C11 C18 1.469(4) . ? C12 C14 1.502(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C16 C17 1.504(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C19 C20 1.450(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 C22 1.372(4) . ? C21 H21 0.9400 . ? C22 C23 1.383(4) . ? C22 H22 0.9400 . ? C23 C24 1.383(3) . ? C23 C26 1.501(3) . ? C24 C25 1.368(3) . ? C24 H24 0.9400 . ? C25 H25 0.9400 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C28 1.502(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C32 1.380(4) . ? C28 C29 1.383(4) . ? C29 C30 1.379(4) . ? C29 H29 0.9400 . ? C30 H30 0.9400 . ? C31 C32 1.378(3) . ? C31 H31 0.9400 . ? C32 H32 0.9400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O2 107.32(7) . . ? O1 Fe1 N1 86.82(7) . . ? O2 Fe1 N1 165.84(7) . . ? O1 Fe1 N2 165.93(7) . . ? O2 Fe1 N2 86.18(7) . . ? N1 Fe1 N2 79.66(7) . . ? O1 Fe1 N3 91.84(7) . . ? O2 Fe1 N3 89.45(8) . . ? N1 Fe1 N3 90.77(8) . . ? N2 Fe1 N3 92.23(7) . . ? O1 Fe1 N4 88.15(7) . 4_455 ? O2 Fe1 N4 89.79(8) . 4_455 ? N1 Fe1 N4 90.04(8) . 4_455 ? N2 Fe1 N4 87.97(7) . 4_455 ? N3 Fe1 N4 179.19(7) . 4_455 ? C26 S1 C27 101.45(12) . . ? C1 O1 Fe1 134.03(15) . . ? C12 O2 Fe1 133.08(16) . . ? C18 O4 C19 114.0(2) . . ? C15 O6 C16 116.46(18) . . ? C3 N1 C4 120.59(18) . . ? C3 N1 Fe1 126.03(15) . . ? C4 N1 Fe1 113.37(13) . . ? C10 N2 C9 121.0(2) . . ? C10 N2 Fe1 124.89(16) . . ? C9 N2 Fe1 113.59(13) . . ? C21 N3 C25 115.8(2) . . ? C21 N3 Fe1 120.53(16) . . ? C25 N3 Fe1 122.59(16) . . ? C30 N4 C31 116.3(2) . . ? C30 N4 Fe1 121.76(16) . 4_656 ? C31 N4 Fe1 120.84(16) . 4_656 ? O1 C1 C2 122.5(2) . . ? O1 C1 C13 114.6(2) . . ? C2 C1 C13 123.0(2) . . ? C1 C2 C3 123.76(19) . . ? C1 C2 C15 120.00(19) . . ? C3 C2 C15 116.2(2) . . ? N1 C3 C2 126.8(2) . . ? N1 C3 H3 116.6 . . ? C2 C3 H3 116.6 . . ? C5 C4 C9 119.17(19) . . ? C5 C4 N1 124.57(19) . . ? C9 C4 N1 116.24(19) . . ? C6 C5 C4 120.7(2) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C7 120.2(2) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C8 C7 C6 120.1(2) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C7 C8 C9 120.9(2) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C8 C9 C4 118.8(2) . . ? C8 C9 N2 125.0(2) . . ? C4 C9 N2 116.15(19) . . ? N2 C10 C11 126.6(2) . . ? N2 C10 H10 116.7 . . ? C11 C10 H10 116.7 . . ? C12 C11 C10 123.9(2) . . ? C12 C11 C18 118.1(2) . . ? C10 C11 C18 118.0(2) . . ? O2 C12 C11 122.5(2) . . ? O2 C12 C14 114.7(2) . . ? C11 C12 C14 122.8(2) . . ? C1 C13 H13A 109.5 . . ? C1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O5 C15 O6 120.1(2) . . ? O5 C15 C2 127.4(2) . . ? O6 C15 C2 112.48(19) . . ? O6 C16 C17 106.4(2) . . ? O6 C16 H16A 110.4 . . ? C17 C16 H16A 110.4 . . ? O6 C16 H16B 110.4 . . ? C17 C16 H16B 110.4 . . ? H16A C16 H16B 108.6 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O3 C18 O4 119.8(2) . . ? O3 C18 C11 127.3(3) . . ? O4 C18 C11 112.8(2) . . ? C20 C19 O4 107.7(3) . . ? C20 C19 H19A 110.2 . . ? O4 C19 H19A 110.2 . . ? C20 C19 H19B 110.2 . . ? O4 C19 H19B 110.2 . . ? H19A C19 H19B 108.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 C22 123.9(2) . . ? N3 C21 H21 118.1 . . ? C22 C21 H21 118.1 . . ? C21 C22 C23 120.1(2) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C24 116.1(2) . . ? C22 C23 C26 120.8(2) . . ? C24 C23 C26 123.0(2) . . ? C25 C24 C23 120.2(2) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? N3 C25 C24 123.7(2) . . ? N3 C25 H25 118.2 . . ? C24 C25 H25 118.2 . . ? C23 C26 S1 116.69(17) . . ? C23 C26 H26A 108.1 . . ? S1 C26 H26A 108.1 . . ? C23 C26 H26B 108.1 . . ? S1 C26 H26B 108.1 . . ? H26A C26 H26B 107.3 . . ? C28 C27 S1 111.85(18) . . ? C28 C27 H27A 109.2 . . ? S1 C27 H27A 109.2 . . ? C28 C27 H27B 109.2 . . ? S1 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? C32 C28 C29 117.1(2) . . ? C32 C28 C27 121.7(2) . . ? C29 C28 C27 121.0(2) . . ? C30 C29 C28 119.9(2) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? N4 C30 C29 123.3(2) . . ? N4 C30 H30 118.3 . . ? C29 C30 H30 118.3 . . ? N4 C31 C32 123.9(2) . . ? N4 C31 H31 118.0 . . ? C32 C31 H31 118.0 . . ? C31 C32 C28 119.3(2) . . ? C31 C32 H32 120.3 . . ? C28 C32 H32 120.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Fe1 O1 C1 -175.5(2) . . . . ? N1 Fe1 O1 C1 3.9(2) . . . . ? N2 Fe1 O1 C1 -12.2(4) . . . . ? N3 Fe1 O1 C1 94.5(2) . . . . ? N4 Fe1 O1 C1 -86.3(2) 4_455 . . . ? O1 Fe1 O2 C12 163.2(2) . . . . ? N1 Fe1 O2 C12 -14.1(4) . . . . ? N2 Fe1 O2 C12 -12.8(2) . . . . ? N3 Fe1 O2 C12 -105.0(2) . . . . ? N4 Fe1 O2 C12 75.2(2) 4_455 . . . ? O1 Fe1 N1 C3 -2.99(18) . . . . ? O2 Fe1 N1 C3 174.4(2) . . . . ? N2 Fe1 N1 C3 173.08(18) . . . . ? N3 Fe1 N1 C3 -94.79(18) . . . . ? N4 Fe1 N1 C3 85.15(18) 4_455 . . . ? O1 Fe1 N1 C4 176.09(14) . . . . ? O2 Fe1 N1 C4 -6.5(4) . . . . ? N2 Fe1 N1 C4 -7.84(13) . . . . ? N3 Fe1 N1 C4 84.29(14) . . . . ? N4 Fe1 N1 C4 -95.77(14) 4_455 . . . ? O1 Fe1 N2 C10 -146.6(3) . . . . ? O2 Fe1 N2 C10 17.38(18) . . . . ? N1 Fe1 N2 C10 -162.95(19) . . . . ? N3 Fe1 N2 C10 106.67(18) . . . . ? N4 Fe1 N2 C10 -72.54(18) 4_455 . . . ? O1 Fe1 N2 C9 25.2(4) . . . . ? O2 Fe1 N2 C9 -170.76(14) . . . . ? N1 Fe1 N2 C9 8.91(13) . . . . ? N3 Fe1 N2 C9 -81.47(15) . . . . ? N4 Fe1 N2 C9 99.32(15) 4_455 . . . ? O1 Fe1 N3 C21 -69.2(2) . . . . ? O2 Fe1 N3 C21 -176.5(2) . . . . ? N1 Fe1 N3 C21 17.6(2) . . . . ? N2 Fe1 N3 C21 97.3(2) . . . . ? O1 Fe1 N3 C25 123.12(18) . . . . ? O2 Fe1 N3 C25 15.81(18) . . . . ? N1 Fe1 N3 C25 -150.03(18) . . . . ? N2 Fe1 N3 C25 -70.35(18) . . . . ? Fe1 O1 C1 C2 -3.2(3) . . . . ? Fe1 O1 C1 C13 177.24(16) . . . . ? O1 C1 C2 C3 0.2(3) . . . . ? C13 C1 C2 C3 179.8(2) . . . . ? O1 C1 C2 C15 -177.9(2) . . . . ? C13 C1 C2 C15 1.7(3) . . . . ? C4 N1 C3 C2 -177.1(2) . . . . ? Fe1 N1 C3 C2 1.9(3) . . . . ? C1 C2 C3 N1 0.2(4) . . . . ? C15 C2 C3 N1 178.4(2) . . . . ? C3 N1 C4 C5 6.4(3) . . . . ? Fe1 N1 C4 C5 -172.71(17) . . . . ? C3 N1 C4 C9 -175.21(19) . . . . ? Fe1 N1 C4 C9 5.7(2) . . . . ? C9 C4 C5 C6 0.1(3) . . . . ? N1 C4 C5 C6 178.4(2) . . . . ? C4 C5 C6 C7 -2.4(4) . . . . ? C5 C6 C7 C8 1.8(4) . . . . ? C6 C7 C8 C9 1.2(4) . . . . ? C7 C8 C9 C4 -3.5(3) . . . . ? C7 C8 C9 N2 179.1(2) . . . . ? C5 C4 C9 C8 2.9(3) . . . . ? N1 C4 C9 C8 -175.58(19) . . . . ? C5 C4 C9 N2 -179.55(18) . . . . ? N1 C4 C9 N2 2.0(3) . . . . ? C10 N2 C9 C8 -19.0(3) . . . . ? Fe1 N2 C9 C8 168.74(18) . . . . ? C10 N2 C9 C4 163.5(2) . . . . ? Fe1 N2 C9 C4 -8.7(2) . . . . ? C9 N2 C10 C11 174.4(2) . . . . ? Fe1 N2 C10 C11 -14.3(3) . . . . ? N2 C10 C11 C12 -1.9(4) . . . . ? N2 C10 C11 C18 179.2(2) . . . . ? Fe1 O2 C12 C11 2.8(4) . . . . ? Fe1 O2 C12 C14 -178.89(17) . . . . ? C10 C11 C12 O2 8.5(4) . . . . ? C18 C11 C12 O2 -172.6(2) . . . . ? C10 C11 C12 C14 -169.6(2) . . . . ? C18 C11 C12 C14 9.3(4) . . . . ? C16 O6 C15 O5 -1.3(3) . . . . ? C16 O6 C15 C2 177.80(19) . . . . ? C1 C2 C15 O5 -12.6(4) . . . . ? C3 C2 C15 O5 169.1(2) . . . . ? C1 C2 C15 O6 168.40(19) . . . . ? C3 C2 C15 O6 -9.9(3) . . . . ? C15 O6 C16 C17 178.6(2) . . . . ? C19 O4 C18 O3 2.7(4) . . . . ? C19 O4 C18 C11 -175.1(2) . . . . ? C12 C11 C18 O3 -17.6(4) . . . . ? C10 C11 C18 O3 161.4(3) . . . . ? C12 C11 C18 O4 160.0(2) . . . . ? C10 C11 C18 O4 -21.0(3) . . . . ? C18 O4 C19 C20 179.2(3) . . . . ? C25 N3 C21 C22 3.6(4) . . . . ? Fe1 N3 C21 C22 -164.8(2) . . . . ? N3 C21 C22 C23 0.1(4) . . . . ? C21 C22 C23 C24 -4.1(4) . . . . ? C21 C22 C23 C26 171.7(2) . . . . ? C22 C23 C24 C25 4.3(3) . . . . ? C26 C23 C24 C25 -171.3(2) . . . . ? C21 N3 C25 C24 -3.4(3) . . . . ? Fe1 N3 C25 C24 164.80(19) . . . . ? C23 C24 C25 N3 -0.6(4) . . . . ? C22 C23 C26 S1 138.4(2) . . . . ? C24 C23 C26 S1 -46.1(3) . . . . ? C27 S1 C26 C23 -62.7(2) . . . . ? C26 S1 C27 C28 -49.4(2) . . . . ? S1 C27 C28 C32 -57.7(3) . . . . ? S1 C27 C28 C29 118.7(2) . . . . ? C32 C28 C29 C30 1.8(4) . . . . ? C27 C28 C29 C30 -174.9(2) . . . . ? C31 N4 C30 C29 -2.6(4) . . . . ? Fe1 N4 C30 C29 165.7(2) 4_656 . . . ? C28 C29 C30 N4 1.0(4) . . . . ? C30 N4 C31 C32 1.6(4) . . . . ? Fe1 N4 C31 C32 -166.9(2) 4_656 . . . ? N4 C31 C32 C28 1.1(4) . . . . ? C29 C28 C32 C31 -2.7(4) . . . . ? C27 C28 C32 C31 173.9(2) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? #?# use this item for nonbonding or very weakly bonding contacts, e.g.: #?# Sb1 N13 3.906(13) . . ? #?# Mn Mn 3.253(2) . 2 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? _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. ; #:---------------------------------------------------------------------------- #:--------------------------ARCHIVING AND CHECKING---------------------------- #:---------------------------------------------------------------------------- _audit_block_code Fe_L1_bpms_mo231_Bauer _audit_creation_method 'form98_non/compatible with shelxl97-2' _chemical_name_systematic ; poly-(E,E)-[{diethyl-2,2'-[1,2-phenylenebis(iminomethylidyne)]bis[3-oxobutanato] (2-)-N,N',O^3,O^3'}(bis(4-pyridylmethyl)sulfide)iron(II) ; _chemical_formula_moiety 'C32 H34 Fe N4 O6 S' _chemical_formula_sum 'C32 H34 Fe N4 O6 S' _chemical_formula_weight 658.547 _chemical_melting_point ? _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.4446 _exptl_crystal_F_000 1376 #:---------------------------------------------------------------------------- #:---------------------------------------------------------------------------- data_oo194 _database_code_depnum_ccdc_archive 'CCDC 845683' _audit_update_record 21-Sep-11 _chemical_name_common '[FeL4(bpms)]LS' _chemical_compound_source ; The synthesis of (I) was carried out under argon using Schlenk tube techniques. [Fe(L1f)(MeOH)~2~] and Bis(4-pyridylmethyl)sulfide were dissolved in ethanol and heated to reflux for four hours. After 24 hours at room temperature the product was filtered off and washed two times with ice-cold ethanol. Crystals suitable for X-ray structure analysis were obtain after recrystallization. ; _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.46 #?# in millimeters _exptl_crystal_size_mid 0.36 #?# in millimeters _exptl_crystal_size_min 0.27 #?# in millimeters _exptl_crystal_density_method 'not measured' _exptl_crystal_density_meas 1.3546 _exptl_special_details ? #?# all that happened prior to measurement (crystal embedded in mother liquor) #:---------------------------------------------------------------------------- #:---------------------------DATA COLLECTION---------------------------------- #:---------------------------------------------------------------------------- _audit_author_name 'P. Mayer' #?# X-ray operator _audit_creation_date ; 'Wed Oct 27 07:13:18 2010' ; _diffrn_ambient_temperature 125(2) #?# in K _diffrn_source_type 'Spellman generator' _diffrn_source_power 2.00 #?# in kW _diffrn_source_voltage 50 #?# in kV _diffrn_source_current 40 #?# in mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation '0.5 mm collimator' _diffrn_measurement_device 'CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Oxford XCalibur' _diffrn_measurement_method '\w scans' _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -30.00 -2.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -20.4494 -94.0000 142.0000 28 #__ type_ start__ end____ width___ exp.time_ 2 omega -46.00 -8.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - -20.4494 38.0000 120.0000 38 #__ type_ start__ end____ width___ exp.time_ 3 omega -52.00 50.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ frames - 21.3869 -38.0000 -180.0000 102 ; _diffrn_detector_area_resol_mean 15.9809 _diffrn_special_details ? _diffrn_orient_matrix_type ? _diffrn_orient_matrix_UB_11 -0.0211267670 _diffrn_orient_matrix_UB_12 -0.0013753144 _diffrn_orient_matrix_UB_13 -0.0245153747 _diffrn_orient_matrix_UB_21 -0.0209695869 _diffrn_orient_matrix_UB_22 -0.0312773600 _diffrn_orient_matrix_UB_23 0.0082390093 _diffrn_orient_matrix_UB_31 -0.0325437899 _diffrn_orient_matrix_UB_32 0.0210174052 _diffrn_orient_matrix_UB_33 0.0106115099 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? ? _cell_length_a 18.8103(9) _cell_length_b 16.0825(7) _cell_length_c 25.3728(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7675.7(6) _cell_measurement_temperature 125(2) #?# in K _cell_measurement_reflns_used 7671 _cell_measurement_theta_min 4.2009 _cell_measurement_theta_max 26.2493 _cell_special_details ? #?# supposed (pseudo-)symmetries,subcells,deviation from standard setting loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? #?# same style as for the absorption correction routine, e.g.: #?# -1 0 -1 .0424 #:---------------------------------------------------------------------------- #:---------------------------ABSORPTION CORRECTION---------------------------- #:---------------------------------------------------------------------------- _exptl_absorpt_coefficient_mu 0.501 _exptl_absorpt_correction_type multi-scan #numerical (using crystal faces), refdelf (using DIFABS) _exptl_absorpt_correction_T_min 0.97309 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #?# 'XRed, rev. 1.09, Stoe (Darmstadt, Germany)' #:---------------------------------------------------------------------------- #:------------------------REFLECTION DATA ANALYSIS---------------------------- #:---------------------------------------------------------------------------- _diffrn_reflns_number 21310 #xl _diffrn_reflns_av_R_equivalents 0.0292 #xl _diffrn_reflns_av_sigmaI/netI 0.0537 #xl _diffrn_reflns_limit_h_min -20 #xl _diffrn_reflns_limit_h_max 18 #xl _diffrn_reflns_limit_k_min -20 #xl _diffrn_reflns_limit_k_max 23 #xl _diffrn_reflns_limit_l_min -31 #xl _diffrn_reflns_limit_l_max 31 #xl _diffrn_reflns_theta_min 4.22 #xl _diffrn_reflns_theta_max 26.27 #xl _diffrn_measured_fraction_theta_max 0.993 #xl _diffrn_reflns_theta_full 26.27 #xl _diffrn_measured_fraction_theta_full 0.993 #xl #:---------------------------------------------------------------------------- #:---------------------STRUCTURE SOLUTION AND REFINEMENT---------------------- #:---------------------------------------------------------------------------- _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _reflns_number_total 7753 #xl _reflns_number_gt 4851 #xl _reflns_threshold_expression >2sigma(I) #xl _reflns_special_details ? #?# "A description of reflection data not covered by the other data #?# names. It should include details of the Friedel pairs." _refine_ls_structure_factor_coef Fsqd #xl _refine_ls_matrix_type full #xl _refine_ls_weighting_scheme calc #xl _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' #xl _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refU _refine_ls_extinction_method none #xl _refine_ls_extinction_coef ? #xl _refine_ls_abs_structure_details ? #xl _refine_ls_abs_structure_Flack ? #xl _refine_ls_number_reflns 7753 #xl _refine_ls_number_parameters 489 #xl _refine_ls_number_restraints 0 #xl _refine_ls_R_factor_all 0.0625 #xl _refine_ls_R_factor_gt 0.0324 #xl _refine_ls_wR_factor_ref 0.0771 #xl _refine_ls_wR_factor_gt 0.0723 #xl _refine_ls_goodness_of_fit_ref 0.879 #xl _refine_ls_restrained_S_all 0.879 #xl _refine_ls_shift/su_max 0.001 #xl _refine_ls_shift/su_mean 0.000 #xl _refine_diff_density_max 0.407 #xl _refine_diff_density_min -0.341 #xl _refine_diff_density_rms 0.050 #xl _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. Anisotrop refinement of all none-hydrogen atoms. Details of H atom refinement: riding with U(H)=1.2*U(C) for CH2 and CH, 1.5*U(C) for CH3 C-bonded H: constr ; #:---------------------------------------------------------------------------- #:-----------------------------REFERENCES------------------------------------- #:---------------------------------------------------------------------------- _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution ; A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A. Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for crystal structure determination and refinement; J. Appl. Crystallogr. 1999, 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ; ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid Plot Program for Crystal Structure Illustrations, Oak Ridge National Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ. Glasgow) used --- SCHAKAL (E. Keller, University of Freiburg (Breisgau), Germany, 1995). ; _computing_publication_material ; PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version). #-- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses). ; #:---------------------------------------------------------------------------- #:---------------------TABLES AND GEOMETRICAL DATA---------------------------- #:---------------------------------------------------------------------------- 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 0.011709(13) 0.248773(14) 0.073766(10) 0.01457(7) Uani 1 1 d . . . S1 S 0.00563(3) 0.07535(3) 0.326698(18) 0.02407(12) Uani 1 1 d . . . O1 O -0.06460(7) 0.30873(7) 0.10858(5) 0.0170(3) Uani 1 1 d . . . O2 O 0.08234(6) 0.31781(6) 0.10943(5) 0.0159(3) Uani 1 1 d . . . O3 O -0.26961(7) 0.16823(7) 0.04480(5) 0.0263(3) Uani 1 1 d . . . O4 O -0.27068(7) 0.24563(8) 0.11838(5) 0.0293(3) Uani 1 1 d . . . O5 O 0.29823(7) 0.19774(7) 0.04971(5) 0.0267(3) Uani 1 1 d . . . O6 O 0.29261(7) 0.27175(7) 0.12454(5) 0.0256(3) Uani 1 1 d . . . N1 N -0.05344(8) 0.18097(8) 0.03471(6) 0.0157(3) Uani 1 1 d . . . N2 N 0.08355(8) 0.18946(8) 0.03587(6) 0.0151(3) Uani 1 1 d . . . N3 N 0.01368(8) 0.16883(8) 0.13472(6) 0.0163(3) Uani 1 1 d . . . N4 N 0.00910(8) 0.16562(8) 0.51540(6) 0.0154(3) Uani 1 1 d . . . C1 C 0.14957(10) 0.31594(10) 0.10385(7) 0.0160(4) Uani 1 1 d . . . C2 C 0.18652(9) 0.25210(10) 0.07696(7) 0.0155(4) Uani 1 1 d . . . C3 C 0.15196(10) 0.19596(10) 0.04250(7) 0.0169(4) Uani 1 1 d . . . H3 H 0.1813 0.1598 0.0224 0.020 Uiso 1 1 calc R . . C4 C 0.05530(10) 0.13687(10) -0.00376(7) 0.0178(4) Uani 1 1 d . . . C5 C 0.09458(11) 0.09465(10) -0.04192(8) 0.0243(5) Uani 1 1 d . . . H5 H 0.1449 0.0994 -0.0425 0.029 Uiso 1 1 calc R . . C6 C 0.06055(12) 0.04609(11) -0.07873(8) 0.0294(5) Uani 1 1 d . . . H6 H 0.0876 0.0170 -0.1044 0.035 Uiso 1 1 calc R . . C7 C -0.01258(11) 0.03932(12) -0.07857(8) 0.0289(5) Uani 1 1 d . . . H7 H -0.0356 0.0053 -0.1040 0.035 Uiso 1 1 calc R . . C8 C -0.05244(11) 0.08183(10) -0.04169(8) 0.0230(5) Uani 1 1 d . . . H8 H -0.1028 0.0773 -0.0420 0.028 Uiso 1 1 calc R . . C9 C -0.01913(10) 0.13139(10) -0.00390(7) 0.0177(4) Uani 1 1 d . . . C10 C -0.12264(10) 0.18037(10) 0.03987(7) 0.0178(4) Uani 1 1 d . . . H10 H -0.1484 0.1414 0.0192 0.021 Uiso 1 1 calc R . . C11 C -0.16221(10) 0.23262(10) 0.07354(7) 0.0166(4) Uani 1 1 d . . . C12 C -0.13139(10) 0.29869(10) 0.10259(7) 0.0170(4) Uani 1 1 d . . . C13 C -0.23840(10) 0.21290(11) 0.07566(8) 0.0203(4) Uani 1 1 d . . . C14 C -0.34573(11) 0.22951(12) 0.12466(9) 0.0336(5) Uani 1 1 d . . . H14A H -0.3543 0.1693 0.1299 0.040 Uiso 1 1 calc R . . H14B H -0.3723 0.2480 0.0930 0.040 Uiso 1 1 calc R . . C15 C -0.36910(12) 0.27784(14) 0.17232(11) 0.0527(7) Uani 1 1 d . . . H15A H -0.3430 0.2582 0.2034 0.079 Uiso 1 1 calc R . . H15B H -0.4202 0.2698 0.1778 0.079 Uiso 1 1 calc R . . H15C H -0.3593 0.3371 0.1669 0.079 Uiso 1 1 calc R . . C16 C 0.26360(10) 0.23869(11) 0.08071(7) 0.0193(4) Uani 1 1 d . . . C17 C 0.36854(10) 0.25986(13) 0.13100(9) 0.0343(5) Uani 1 1 d . . . H17A H 0.3944 0.2797 0.0994 0.041 Uiso 1 1 calc R . . H17B H 0.3796 0.2003 0.1364 0.041 Uiso 1 1 calc R . . C18 C 0.38946(14) 0.30943(18) 0.17837(12) 0.0768(10) Uani 1 1 d . . . H18A H 0.3779 0.3681 0.1725 0.115 Uiso 1 1 calc R . . H18B H 0.4407 0.3037 0.1844 0.115 Uiso 1 1 calc R . . H18C H 0.3635 0.2890 0.2093 0.115 Uiso 1 1 calc R . . C19 C -0.17442(10) 0.36804(11) 0.12484(8) 0.0226(5) Uani 1 1 d . . . C20 C -0.17159(11) 0.38621(13) 0.17801(9) 0.0358(5) Uani 1 1 d . . . H20 H -0.1447 0.3518 0.2010 0.043 Uiso 1 1 calc R . . C21 C -0.20768(13) 0.45402(16) 0.19793(12) 0.0571(8) Uani 1 1 d . . . H21 H -0.2071 0.4650 0.2347 0.069 Uiso 1 1 calc R . . C22 C -0.24448(13) 0.50567(15) 0.16459(14) 0.0585(9) Uani 1 1 d . . . H22 H -0.2684 0.5530 0.1783 0.070 Uiso 1 1 calc R . . C23 C -0.24691(12) 0.48919(13) 0.11123(13) 0.0473(7) Uani 1 1 d . . . H23 H -0.2721 0.5253 0.0882 0.057 Uiso 1 1 calc R . . C24 C -0.21235(10) 0.41947(11) 0.09135(9) 0.0314(5) Uani 1 1 d . . . H24 H -0.2148 0.4072 0.0548 0.038 Uiso 1 1 calc R . . C25 C 0.18607(10) 0.39313(10) 0.12239(8) 0.0184(4) Uani 1 1 d . . . C26 C 0.16703(10) 0.43000(11) 0.16956(8) 0.0251(5) Uani 1 1 d . . . H26 H 0.1352 0.4023 0.1927 0.030 Uiso 1 1 calc R . . C27 C 0.19409(11) 0.50718(12) 0.18327(9) 0.0327(5) Uani 1 1 d . . . H27 H 0.1806 0.5322 0.2157 0.039 Uiso 1 1 calc R . . C28 C 0.24034(11) 0.54758(12) 0.15006(10) 0.0364(6) Uani 1 1 d . . . H28 H 0.2585 0.6006 0.1595 0.044 Uiso 1 1 calc R . . C29 C 0.26027(11) 0.51150(12) 0.10343(9) 0.0343(6) Uani 1 1 d . . . H29 H 0.2927 0.5393 0.0808 0.041 Uiso 1 1 calc R . . C30 C 0.23306(10) 0.43434(11) 0.08920(8) 0.0268(5) Uani 1 1 d . . . H30 H 0.2466 0.4097 0.0567 0.032 Uiso 1 1 calc R . . C31 C 0.07653(10) 0.09311(10) 0.20183(8) 0.0215(4) Uani 1 1 d . . . H31 H 0.1209 0.0792 0.2173 0.026 Uiso 1 1 calc R . . C32 C 0.07434(10) 0.14581(10) 0.15893(7) 0.0202(4) Uani 1 1 d . . . H32 H 0.1180 0.1670 0.1457 0.024 Uiso 1 1 calc R . . C33 C -0.04649(10) 0.13709(10) 0.15521(7) 0.0196(4) Uani 1 1 d . . . H33 H -0.0904 0.1521 0.1394 0.024 Uiso 1 1 calc R . . C34 C -0.04797(10) 0.08403(10) 0.19790(8) 0.0208(4) Uani 1 1 d . . . H34 H -0.0922 0.0636 0.2105 0.025 Uiso 1 1 calc R . . C35 C 0.01433(10) 0.06047(10) 0.22244(7) 0.0187(4) Uani 1 1 d . . . C36 C 0.01393(10) 0.00636(11) 0.27052(7) 0.0208(4) Uani 1 1 d . . . H36A H 0.0586 -0.0260 0.2728 0.025 Uiso 1 1 calc R . . H36B H -0.0266 -0.0329 0.2693 0.025 Uiso 1 1 calc R . . C37 C 0.00557(10) 0.00175(10) 0.38118(7) 0.0186(4) Uani 1 1 d . . . H37A H -0.0374 -0.0338 0.3800 0.022 Uiso 1 1 calc R . . H37B H 0.0482 -0.0343 0.3798 0.022 Uiso 1 1 calc R . . C38 C 0.00608(10) 0.05387(10) 0.43014(7) 0.0162(4) Uani 1 1 d . . . C39 C -0.05598(10) 0.08636(10) 0.45113(7) 0.0176(4) Uani 1 1 d . . . H39 H -0.1008 0.0709 0.4369 0.021 Uiso 1 1 calc R . . C40 C -0.05245(10) 0.14126(10) 0.49274(7) 0.0176(4) Uani 1 1 d . . . H40 H -0.0957 0.1632 0.5062 0.021 Uiso 1 1 calc R . . C41 C 0.06884(10) 0.13273(10) 0.49523(7) 0.0177(4) Uani 1 1 d . . . H41 H 0.1130 0.1484 0.5104 0.021 Uiso 1 1 calc R . . C42 C 0.06949(10) 0.07729(10) 0.45366(7) 0.0177(4) Uani 1 1 d . . . H42 H 0.1133 0.0553 0.4412 0.021 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 0.01275(13) 0.01671(13) 0.01424(13) 0.00116(11) -0.00029(12) -0.00077(12) S1 0.0388(3) 0.0184(2) 0.0150(2) 0.0005(2) 0.0001(2) -0.0001(2) O1 0.0151(7) 0.0193(6) 0.0166(7) 0.0000(5) -0.0005(6) -0.0020(5) O2 0.0129(7) 0.0186(6) 0.0161(7) 0.0011(5) 0.0012(6) 0.0007(5) O3 0.0198(8) 0.0313(7) 0.0278(8) -0.0029(6) -0.0035(7) -0.0084(6) O4 0.0172(7) 0.0369(8) 0.0338(8) -0.0083(7) 0.0061(6) -0.0092(7) O5 0.0194(8) 0.0358(7) 0.0249(8) -0.0030(7) 0.0032(7) 0.0069(6) O6 0.0151(7) 0.0335(7) 0.0281(8) -0.0047(6) -0.0050(6) 0.0054(6) N1 0.0179(9) 0.0161(7) 0.0130(8) 0.0003(6) -0.0001(7) -0.0014(7) N2 0.0185(9) 0.0131(7) 0.0137(9) 0.0011(6) -0.0004(7) 0.0000(6) N3 0.0150(8) 0.0167(7) 0.0172(8) -0.0016(6) 0.0006(7) -0.0006(7) N4 0.0139(8) 0.0184(7) 0.0140(8) 0.0024(6) 0.0011(7) 0.0003(7) C1 0.0150(10) 0.0190(9) 0.0139(10) 0.0047(8) -0.0009(8) 0.0008(8) C2 0.0144(9) 0.0191(8) 0.0129(9) 0.0023(8) 0.0015(8) 0.0005(8) C3 0.0188(11) 0.0159(9) 0.0159(11) 0.0025(8) 0.0041(9) 0.0041(8) C4 0.0228(11) 0.0160(9) 0.0145(10) 0.0001(8) -0.0011(9) -0.0014(8) C5 0.0249(12) 0.0242(10) 0.0239(12) -0.0034(9) 0.0037(9) -0.0002(9) C6 0.0349(14) 0.0275(11) 0.0257(12) -0.0093(9) 0.0052(11) 0.0005(10) C7 0.0377(14) 0.0272(11) 0.0217(11) -0.0090(9) -0.0015(11) -0.0047(10) C8 0.0206(11) 0.0250(10) 0.0234(12) -0.0030(9) -0.0008(9) -0.0044(9) C9 0.0258(11) 0.0156(9) 0.0117(9) 0.0006(8) 0.0005(9) -0.0011(8) C10 0.0202(11) 0.0193(9) 0.0140(10) 0.0019(8) -0.0040(8) -0.0047(8) C11 0.0163(10) 0.0184(9) 0.0149(10) 0.0026(8) -0.0018(8) -0.0017(8) C12 0.0173(11) 0.0208(9) 0.0128(10) 0.0055(8) 0.0017(8) -0.0002(8) C13 0.0197(11) 0.0193(9) 0.0219(11) 0.0050(9) 0.0001(9) -0.0011(8) C14 0.0182(11) 0.0372(12) 0.0453(15) -0.0012(11) 0.0072(11) -0.0060(9) C15 0.0305(14) 0.0578(14) 0.070(2) -0.0143(14) 0.0243(14) -0.0046(12) C16 0.0180(10) 0.0207(10) 0.0191(10) 0.0027(9) 0.0019(9) 0.0003(9) C17 0.0150(11) 0.0474(13) 0.0405(14) -0.0031(11) -0.0063(10) 0.0048(10) C18 0.0320(16) 0.126(2) 0.073(2) -0.045(2) -0.0242(16) 0.0107(16) C19 0.0136(11) 0.0227(10) 0.0314(12) -0.0037(9) 0.0028(9) -0.0062(8) C20 0.0213(12) 0.0486(13) 0.0374(14) -0.0156(11) 0.0001(11) -0.0004(10) C21 0.0258(14) 0.0780(18) 0.068(2) -0.0461(16) 0.0049(14) 0.0003(14) C22 0.0222(14) 0.0382(14) 0.115(3) -0.0344(17) 0.0078(17) 0.0022(11) C23 0.0212(13) 0.0277(12) 0.093(2) 0.0064(14) 0.0068(15) -0.0002(10) C24 0.0189(12) 0.0263(10) 0.0489(15) 0.0059(10) 0.0046(10) -0.0006(9) C25 0.0133(10) 0.0175(9) 0.0243(11) 0.0011(8) -0.0044(8) 0.0031(8) C26 0.0173(11) 0.0285(10) 0.0294(12) -0.0034(9) -0.0011(9) -0.0017(9) C27 0.0266(12) 0.0318(11) 0.0396(14) -0.0136(10) -0.0066(11) 0.0045(10) C28 0.0243(13) 0.0228(11) 0.0622(17) -0.0067(11) -0.0126(12) -0.0022(10) C29 0.0274(13) 0.0276(11) 0.0479(15) 0.0083(11) 0.0003(11) -0.0054(10) C30 0.0233(12) 0.0250(10) 0.0322(13) 0.0028(9) 0.0016(10) -0.0001(9) C31 0.0187(11) 0.0254(10) 0.0206(11) 0.0027(9) -0.0034(9) 0.0025(9) C32 0.0156(11) 0.0222(10) 0.0228(11) 0.0009(9) 0.0008(9) -0.0006(8) C33 0.0159(11) 0.0223(10) 0.0207(11) -0.0015(9) -0.0008(9) -0.0012(8) C34 0.0175(11) 0.0247(10) 0.0202(11) 0.0001(9) 0.0004(9) -0.0039(9) C35 0.0222(11) 0.0172(9) 0.0168(9) -0.0034(8) 0.0005(9) 0.0001(8) C36 0.0246(11) 0.0215(9) 0.0162(9) 0.0001(8) 0.0010(9) 0.0014(9) C37 0.0214(11) 0.0164(9) 0.0180(9) 0.0019(8) -0.0010(9) -0.0011(8) C38 0.0188(11) 0.0154(9) 0.0143(9) 0.0032(8) 0.0009(9) -0.0004(8) C39 0.0149(10) 0.0197(9) 0.0181(11) 0.0016(8) -0.0035(8) -0.0021(8) C40 0.0133(10) 0.0207(9) 0.0188(11) 0.0030(8) 0.0011(8) 0.0002(8) C41 0.0137(10) 0.0216(9) 0.0178(11) 0.0016(8) -0.0017(9) -0.0007(8) C42 0.0153(10) 0.0195(9) 0.0182(11) 0.0014(8) 0.0020(8) 0.0044(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.9134(15) . ? Fe1 N1 1.9164(14) . ? Fe1 O1 1.9418(12) . ? Fe1 O2 1.9537(12) . ? Fe1 N3 2.0115(15) . ? Fe1 N4 2.0226(14) 8_565 ? S1 C36 1.8130(18) . ? S1 C37 1.8199(17) . ? O1 C12 1.276(2) . ? O2 C1 1.273(2) . ? O3 C13 1.214(2) . ? O4 C13 1.349(2) . ? O4 C14 1.444(2) . ? O5 C16 1.215(2) . ? O6 C16 1.348(2) . ? O6 C17 1.450(2) . ? N1 C10 1.308(2) . ? N1 C9 1.419(2) . ? N2 C3 1.302(2) . ? N2 C4 1.417(2) . ? N3 C33 1.346(2) . ? N3 C32 1.348(2) . ? N4 C41 1.343(2) . ? N4 C40 1.351(2) . ? N4 Fe1 2.0226(14) 8_566 ? C1 C2 1.415(2) . ? C1 C25 1.495(2) . ? C2 C3 1.415(2) . ? C2 C16 1.469(2) . ? C3 H3 0.9500 . ? C4 C5 1.394(2) . ? C4 C9 1.403(3) . ? C5 C6 1.375(3) . ? C5 H5 0.9500 . ? C6 C7 1.380(3) . ? C6 H6 0.9500 . ? C7 C8 1.380(3) . ? C7 H7 0.9500 . ? C8 C9 1.395(2) . ? C8 H8 0.9500 . ? C10 C11 1.411(2) . ? C10 H10 0.9500 . ? C11 C12 1.417(2) . ? C11 C13 1.469(2) . ? C12 C19 1.489(2) . ? C14 C15 1.503(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C17 C18 1.495(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.381(3) . ? C19 C24 1.384(3) . ? C20 C21 1.381(3) . ? C20 H20 0.9500 . ? C21 C22 1.373(4) . ? C21 H21 0.9500 . ? C22 C23 1.380(4) . ? C22 H22 0.9500 . ? C23 C24 1.391(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.383(3) . ? C25 C30 1.389(3) . ? C26 C27 1.386(2) . ? C26 H26 0.9500 . ? C27 C28 1.374(3) . ? C27 H27 0.9500 . ? C28 C29 1.370(3) . ? C28 H28 0.9500 . ? C29 C30 1.390(3) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.380(2) . ? C31 C35 1.385(2) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.379(2) . ? C33 H33 0.9500 . ? C34 C35 1.380(3) . ? C34 H34 0.9500 . ? C35 C36 1.499(2) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.499(2) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.385(2) . ? C38 C42 1.386(2) . ? C39 C40 1.378(2) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.381(2) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? 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 84.72(6) . . ? N2 Fe1 O1 176.68(6) . . ? N1 Fe1 O1 92.59(6) . . ? N2 Fe1 O2 92.05(6) . . ? N1 Fe1 O2 176.13(6) . . ? O1 Fe1 O2 90.56(5) . . ? N2 Fe1 N3 93.14(6) . . ? N1 Fe1 N3 92.61(6) . . ? O1 Fe1 N3 88.93(5) . . ? O2 Fe1 N3 89.69(5) . . ? N2 Fe1 N4 89.34(6) . 8_565 ? N1 Fe1 N4 89.61(6) . 8_565 ? O1 Fe1 N4 88.69(5) . 8_565 ? O2 Fe1 N4 88.21(5) . 8_565 ? N3 Fe1 N4 176.81(6) . 8_565 ? C36 S1 C37 101.48(8) . . ? C12 O1 Fe1 127.65(11) . . ? C1 O2 Fe1 127.64(11) . . ? C13 O4 C14 117.28(15) . . ? C16 O6 C17 116.09(15) . . ? C10 N1 C9 121.17(16) . . ? C10 N1 Fe1 126.07(13) . . ? C9 N1 Fe1 112.71(12) . . ? C3 N2 C4 120.68(16) . . ? C3 N2 Fe1 126.37(12) . . ? C4 N2 Fe1 112.91(12) . . ? C33 N3 C32 115.57(15) . . ? C33 N3 Fe1 121.60(12) . . ? C32 N3 Fe1 122.79(12) . . ? C41 N4 C40 116.15(15) . . ? C41 N4 Fe1 121.78(12) . 8_566 ? C40 N4 Fe1 122.00(12) . 8_566 ? O2 C1 C2 123.97(16) . . ? O2 C1 C25 113.68(15) . . ? C2 C1 C25 121.92(16) . . ? C3 C2 C1 122.35(16) . . ? C3 C2 C16 113.58(15) . . ? C1 C2 C16 124.05(16) . . ? N2 C3 C2 125.83(16) . . ? N2 C3 H3 117.1 . . ? C2 C3 H3 117.1 . . ? C5 C4 C9 119.77(17) . . ? C5 C4 N2 125.76(18) . . ? C9 C4 N2 114.43(16) . . ? C6 C5 C4 120.09(19) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 120.44(19) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C6 C7 C8 120.29(18) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C9 120.32(19) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C8 C9 C4 119.07(17) . . ? C8 C9 N1 126.25(18) . . ? C4 C9 N1 114.64(16) . . ? N1 C10 C11 125.52(17) . . ? N1 C10 H10 117.2 . . ? C11 C10 H10 117.2 . . ? C10 C11 C12 123.08(17) . . ? C10 C11 C13 114.10(16) . . ? C12 C11 C13 122.82(16) . . ? O1 C12 C11 124.04(16) . . ? O1 C12 C19 113.28(15) . . ? C11 C12 C19 122.44(17) . . ? O3 C13 O4 122.10(18) . . ? O3 C13 C11 125.16(18) . . ? O4 C13 C11 112.60(16) . . ? O4 C14 C15 106.36(17) . . ? O4 C14 H14A 110.5 . . ? C15 C14 H14A 110.5 . . ? O4 C14 H14B 110.5 . . ? C15 C14 H14B 110.5 . . ? H14A C14 H14B 108.6 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O5 C16 O6 122.06(17) . . ? O5 C16 C2 124.51(18) . . ? O6 C16 C2 113.28(15) . . ? O6 C17 C18 106.25(17) . . ? O6 C17 H17A 110.5 . . ? C18 C17 H17A 110.5 . . ? O6 C17 H17B 110.5 . . ? C18 C17 H17B 110.5 . . ? H17A C17 H17B 108.7 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 119.54(19) . . ? C20 C19 C12 120.51(18) . . ? C24 C19 C12 119.68(19) . . ? C21 C20 C19 120.4(2) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C22 C21 C20 120.0(3) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 120.3(2) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 C24 119.7(2) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C19 C24 C23 120.0(2) . . ? C19 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C26 C25 C30 119.01(16) . . ? C26 C25 C1 120.64(17) . . ? C30 C25 C1 119.84(17) . . ? C25 C26 C27 120.40(19) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C28 C27 C26 120.1(2) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C29 C28 C27 120.15(19) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 120.1(2) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C25 C30 C29 120.18(19) . . ? C25 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C32 C31 C35 120.34(18) . . ? C32 C31 H31 119.8 . . ? C35 C31 H31 119.8 . . ? N3 C32 C31 123.61(17) . . ? N3 C32 H32 118.2 . . ? C31 C32 H32 118.2 . . ? N3 C33 C34 123.71(18) . . ? N3 C33 H33 118.1 . . ? C34 C33 H33 118.1 . . ? C33 C34 C35 120.47(18) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C34 C35 C31 116.30(17) . . ? C34 C35 C36 121.51(17) . . ? C31 C35 C36 122.11(17) . . ? C35 C36 S1 106.56(11) . . ? C35 C36 H36A 110.4 . . ? S1 C36 H36A 110.4 . . ? C35 C36 H36B 110.4 . . ? S1 C36 H36B 110.4 . . ? H36A C36 H36B 108.6 . . ? C38 C37 S1 105.41(11) . . ? C38 C37 H37A 110.7 . . ? S1 C37 H37A 110.7 . . ? C38 C37 H37B 110.7 . . ? S1 C37 H37B 110.7 . . ? H37A C37 H37B 108.8 . . ? C39 C38 C42 117.20(16) . . ? C39 C38 C37 121.62(17) . . ? C42 C38 C37 120.96(17) . . ? C40 C39 C38 119.71(17) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? N4 C40 C39 123.60(17) . . ? N4 C40 H40 118.2 . . ? C39 C40 H40 118.2 . . ? N4 C41 C42 123.54(17) . . ? N4 C41 H41 118.2 . . ? C42 C41 H41 118.2 . . ? C41 C42 C38 119.78(17) . . ? C41 C42 H42 120.1 . . ? C38 C42 H42 120.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Fe1 O1 C12 35.5(10) . . . . ? N1 Fe1 O1 C12 -0.35(14) . . . . ? O2 Fe1 O1 C12 177.40(14) . . . . ? N3 Fe1 O1 C12 -92.92(14) . . . . ? N4 Fe1 O1 C12 89.20(14) 8_565 . . . ? N2 Fe1 O2 C1 0.89(14) . . . . ? N1 Fe1 O2 C1 -32.6(9) . . . . ? O1 Fe1 O2 C1 -177.06(14) . . . . ? N3 Fe1 O2 C1 94.01(14) . . . . ? N4 Fe1 O2 C1 -88.39(14) 8_565 . . . ? N2 Fe1 N1 C10 176.51(15) . . . . ? O1 Fe1 N1 C10 -5.45(15) . . . . ? O2 Fe1 N1 C10 -149.9(7) . . . . ? N3 Fe1 N1 C10 83.59(15) . . . . ? N4 Fe1 N1 C10 -94.12(15) 8_565 . . . ? N2 Fe1 N1 C9 -6.19(11) . . . . ? O1 Fe1 N1 C9 171.85(11) . . . . ? O2 Fe1 N1 C9 27.4(8) . . . . ? N3 Fe1 N1 C9 -99.10(12) . . . . ? N4 Fe1 N1 C9 83.18(11) 8_565 . . . ? N1 Fe1 N2 C3 -175.28(15) . . . . ? O1 Fe1 N2 C3 148.7(8) . . . . ? O2 Fe1 N2 C3 6.86(15) . . . . ? N3 Fe1 N2 C3 -82.95(15) . . . . ? N4 Fe1 N2 C3 95.05(15) 8_565 . . . ? N1 Fe1 N2 C4 7.03(11) . . . . ? O1 Fe1 N2 C4 -28.9(10) . . . . ? O2 Fe1 N2 C4 -170.83(11) . . . . ? N3 Fe1 N2 C4 99.36(12) . . . . ? N4 Fe1 N2 C4 -82.64(12) 8_565 . . . ? N2 Fe1 N3 C33 -132.10(13) . . . . ? N1 Fe1 N3 C33 -47.25(13) . . . . ? O1 Fe1 N3 C33 45.29(13) . . . . ? O2 Fe1 N3 C33 135.86(13) . . . . ? N4 Fe1 N3 C33 86.9(11) 8_565 . . . ? N2 Fe1 N3 C32 50.36(14) . . . . ? N1 Fe1 N3 C32 135.22(14) . . . . ? O1 Fe1 N3 C32 -132.24(14) . . . . ? O2 Fe1 N3 C32 -41.68(14) . . . . ? N4 Fe1 N3 C32 -90.6(11) 8_565 . . . ? Fe1 O2 C1 C2 -11.8(2) . . . . ? Fe1 O2 C1 C25 160.82(11) . . . . ? O2 C1 C2 C3 16.5(3) . . . . ? C25 C1 C2 C3 -155.53(16) . . . . ? O2 C1 C2 C16 -165.10(17) . . . . ? C25 C1 C2 C16 22.9(3) . . . . ? C4 N2 C3 C2 173.41(15) . . . . ? Fe1 N2 C3 C2 -4.1(3) . . . . ? C1 C2 C3 N2 -8.2(3) . . . . ? C16 C2 C3 N2 173.28(16) . . . . ? C3 N2 C4 C5 -6.7(3) . . . . ? Fe1 N2 C4 C5 171.14(14) . . . . ? C3 N2 C4 C9 175.62(16) . . . . ? Fe1 N2 C4 C9 -6.54(19) . . . . ? C9 C4 C5 C6 -1.7(3) . . . . ? N2 C4 C5 C6 -179.23(17) . . . . ? C4 C5 C6 C7 0.6(3) . . . . ? C5 C6 C7 C8 0.5(3) . . . . ? C6 C7 C8 C9 -0.6(3) . . . . ? C7 C8 C9 C4 -0.4(3) . . . . ? C7 C8 C9 N1 177.17(17) . . . . ? C5 C4 C9 C8 1.6(3) . . . . ? N2 C4 C9 C8 179.40(14) . . . . ? C5 C4 C9 N1 -176.31(15) . . . . ? N2 C4 C9 N1 1.5(2) . . . . ? C10 N1 C9 C8 3.9(3) . . . . ? Fe1 N1 C9 C8 -173.51(14) . . . . ? C10 N1 C9 C4 -178.36(16) . . . . ? Fe1 N1 C9 C4 4.19(19) . . . . ? C9 N1 C10 C11 -173.91(16) . . . . ? Fe1 N1 C10 C11 3.2(3) . . . . ? N1 C10 C11 C12 6.4(3) . . . . ? N1 C10 C11 C13 -173.96(16) . . . . ? Fe1 O1 C12 C11 8.7(2) . . . . ? Fe1 O1 C12 C19 -165.69(11) . . . . ? C10 C11 C12 O1 -12.7(3) . . . . ? C13 C11 C12 O1 167.71(17) . . . . ? C10 C11 C12 C19 161.26(17) . . . . ? C13 C11 C12 C19 -18.4(3) . . . . ? C14 O4 C13 O3 -3.6(3) . . . . ? C14 O4 C13 C11 -179.53(15) . . . . ? C10 C11 C13 O3 -14.3(3) . . . . ? C12 C11 C13 O3 165.38(17) . . . . ? C10 C11 C13 O4 161.55(15) . . . . ? C12 C11 C13 O4 -18.8(2) . . . . ? C13 O4 C14 C15 -175.75(17) . . . . ? C17 O6 C16 O5 3.6(3) . . . . ? C17 O6 C16 C2 179.29(15) . . . . ? C3 C2 C16 O5 16.0(3) . . . . ? C1 C2 C16 O5 -162.54(17) . . . . ? C3 C2 C16 O6 -159.64(14) . . . . ? C1 C2 C16 O6 21.9(2) . . . . ? C16 O6 C17 C18 173.75(18) . . . . ? O1 C12 C19 C20 -61.2(2) . . . . ? C11 C12 C19 C20 124.3(2) . . . . ? O1 C12 C19 C24 112.82(19) . . . . ? C11 C12 C19 C24 -61.7(2) . . . . ? C24 C19 C20 C21 1.5(3) . . . . ? C12 C19 C20 C21 175.53(19) . . . . ? C19 C20 C21 C22 -2.5(3) . . . . ? C20 C21 C22 C23 1.4(4) . . . . ? C21 C22 C23 C24 0.5(4) . . . . ? C20 C19 C24 C23 0.4(3) . . . . ? C12 C19 C24 C23 -173.63(17) . . . . ? C22 C23 C24 C19 -1.4(3) . . . . ? O2 C1 C25 C26 43.8(2) . . . . ? C2 C1 C25 C26 -143.38(18) . . . . ? O2 C1 C25 C30 -127.95(18) . . . . ? C2 C1 C25 C30 44.9(2) . . . . ? C30 C25 C26 C27 0.4(3) . . . . ? C1 C25 C26 C27 -171.39(17) . . . . ? C25 C26 C27 C28 -0.2(3) . . . . ? C26 C27 C28 C29 -0.4(3) . . . . ? C27 C28 C29 C30 0.8(3) . . . . ? C26 C25 C30 C29 -0.1(3) . . . . ? C1 C25 C30 C29 171.84(17) . . . . ? C28 C29 C30 C25 -0.6(3) . . . . ? C33 N3 C32 C31 0.2(3) . . . . ? Fe1 N3 C32 C31 177.88(13) . . . . ? C35 C31 C32 N3 0.1(3) . . . . ? C32 N3 C33 C34 -0.3(2) . . . . ? Fe1 N3 C33 C34 -178.05(13) . . . . ? N3 C33 C34 C35 0.2(3) . . . . ? C33 C34 C35 C31 0.2(3) . . . . ? C33 C34 C35 C36 176.87(16) . . . . ? C32 C31 C35 C34 -0.3(3) . . . . ? C32 C31 C35 C36 -176.99(16) . . . . ? C34 C35 C36 S1 -87.51(18) . . . . ? C31 C35 C36 S1 89.01(18) . . . . ? C37 S1 C36 C35 179.79(13) . . . . ? C36 S1 C37 C38 174.58(13) . . . . ? S1 C37 C38 C39 83.56(17) . . . . ? S1 C37 C38 C42 -90.92(17) . . . . ? C42 C38 C39 C40 1.7(2) . . . . ? C37 C38 C39 C40 -172.95(15) . . . . ? C41 N4 C40 C39 -0.3(2) . . . . ? Fe1 N4 C40 C39 176.56(13) 8_566 . . . ? C38 C39 C40 N4 -0.7(3) . . . . ? C40 N4 C41 C42 0.2(2) . . . . ? Fe1 N4 C41 C42 -176.68(13) 8_566 . . . ? N4 C41 C42 C38 0.9(3) . . . . ? C39 C38 C42 C41 -1.8(2) . . . . ? C37 C38 C42 C41 172.88(15) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? #?# use this item for nonbonding or very weakly bonding contacts, e.g.: #?# Sb1 N13 3.906(13) . . ? #?# Mn Mn 3.253(2) . 2 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? #?# Do not(!) delete the #s to obtain a table header: # #D H A D - H H...A D...A D - H...A symm(A) publ_flag # #?# style: #?# N2 H721 O93 .72(4) 2.28(4) 2.868(4) 139(4) . ? #?# N2 H722 O1 .92(3) 2.44(3) 3.343(4) 171(3) 2_657 ? #?# #?# (1) This table may be copied from SHELXL97 (command HTAB D A_$n) #?# and rearranged (_geom_hbond_publ_flag missing); or #?# #?# (2) it may be copied from PLATON and rearranged; CAUTION! Check #?# symmetry operation numbers! They must(!) be identical from PLATON #?# and ACTA! "calc intra nomove" must(!) be used in PLATON runs! #?# Even then discrepancies may(!) occur! _geom_special_details ? #;Puckering parameters (\%A, \%) according to # D. Cremer, J. A. Pople, J. Am. Chem. Soc. 1975, 97, 1354--1358 #?# #?# style: #?# #?# Sb1 O2 C2 C3 O3 Q2 = 0.217(15) \f2 = 134(4) #?# O52 C12 C22 C32 C42 C52 Q = 0.577(5) \q = 3.2(6) \f = 271(9) #?# #?# or as a table: #?# #?# O5n - C1n - C2n - C3n - C4n - C5n #?# ------------------------------ #?# n Q theta phi #?# ------------------------------ #?# 11 .574(11) 6.3(11) 112(10) #?# 21 .557(10) 2.1(11) 86(22) #?# 31 .540(10) 6.2(11) 92(10) #?# 41 .571(10) 2.2(10) 221(34) #?# 51 .555(10) 10.6(10) 35(6) #?# 61 .571(10) 5.1(10) 13(13) #?# ------------------------------ #?# #?# least-squares planes be entered here, too #:---------------------------------------------------------------------------- #:--------------------------ARCHIVING AND CHECKING---------------------------- #:---------------------------------------------------------------------------- _audit_block_code Fe_L4_bpms_oo194_Bauer _audit_creation_method 'form98_non/compatible with shelxl97-2' _chemical_name_systematic ? _chemical_formula_moiety 'C42 H38 Fe N4 O6 S' _chemical_formula_sum 'C42 H38 Fe N4 O6 S' _chemical_formula_weight 782.685 _chemical_melting_point ? _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.3546 _exptl_crystal_F_000 3264 #:---------------------------------------------------------------------------- #:---------------------------------------------------------------------------- data_oo195 _database_code_depnum_ccdc_archive 'CCDC 845684' _audit_update_record 21-Sep-11 _chemical_name_common '[FeL4(bpms)]HS' _chemical_compound_source ; The synthesis of (I) was carried out under argon using Schlenk tube techniques. [Fe(L1f)(MeOH)~2~] and Bis(4-pyridylmethyl)sulfide were dissolved in ethanol and heated to reflux for four hours. After 24 hours at room temperature the product was filtered off and washed two times with ice-cold ethanol. Crystals suitable for X-ray structure analysis were obtain after recrystallization. ; _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.23 _exptl_crystal_density_method 'not measured' _exptl_crystal_density_meas 1.2908 _exptl_special_details ? #?# all that happened prior to measurement (crystal embedded in mother liquor) #:---------------------------------------------------------------------------- #:---------------------------DATA COLLECTION---------------------------------- #:---------------------------------------------------------------------------- _audit_author_name 'P. Mayer' _audit_creation_date ; 'Wed Oct 27 07:16:47 2010' ; _diffrn_ambient_temperature 250(2) #?# in K _diffrn_source_type 'Spellman generator' _diffrn_source_power 2.00 #?# in kW _diffrn_source_voltage 50 #?# in kV _diffrn_source_current 40 #?# in mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation '0.5 mm collimator' _diffrn_measurement_device 'CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Oxford XCalibur' _diffrn_measurement_method '\w scans' _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 60.00 89.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 21.3869 -138.0000 30.0000 29 #__ type_ start__ end____ width___ exp.time_ 2 omega 60.00 101.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 21.3869 179.0000 -180.0000 41 #__ type_ start__ end____ width___ exp.time_ 3 omega -7.00 48.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 21.3869 -77.0000 -120.0000 55 #__ type_ start__ end____ width___ exp.time_ 4 omega -53.00 64.00 1.0000 30.0000 omega____ theta____ kappa____ phi______ frames - 21.3869 0.0000 90.0000 117 ; _diffrn_detector_area_resol_mean 15.9809 _diffrn_special_details ? _diffrn_orient_matrix_type ? _diffrn_orient_matrix_UB_11 -0.0355337322 _diffrn_orient_matrix_UB_12 0.0118613322 _diffrn_orient_matrix_UB_13 0.0132598291 _diffrn_orient_matrix_UB_21 -0.0190924512 _diffrn_orient_matrix_UB_22 0.0074975796 _diffrn_orient_matrix_UB_23 -0.0240981481 _diffrn_orient_matrix_UB_31 -0.0165146097 _diffrn_orient_matrix_UB_32 -0.0341703875 _diffrn_orient_matrix_UB_33 -0.0006792936 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? ? _cell_length_a 19.2017(5) _cell_length_b 16.2729(8) _cell_length_c 25.7799(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8055.4(6) _cell_measurement_temperature 250(2) #?# in K _cell_measurement_reflns_used 8846 _cell_measurement_theta_min 4.2358 _cell_measurement_theta_max 26.2496 _cell_special_details ? #?# supposed (pseudo-)symmetries,subcells,deviation from standard setting loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? #?# same style as for the absorption correction routine, e.g.: #?# -1 0 -1 .0424 #:---------------------------------------------------------------------------- #:---------------------------ABSORPTION CORRECTION---------------------------- #:---------------------------------------------------------------------------- _exptl_absorpt_coefficient_mu 0.477 _exptl_absorpt_correction_type multi-scan #numerical (using crystal faces), refdelf (using DIFABS) _exptl_absorpt_correction_T_min 0.98238 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #?# 'XRed, rev. 1.09, Stoe (Darmstadt, Germany)' #:---------------------------------------------------------------------------- #:------------------------REFLECTION DATA ANALYSIS---------------------------- #:---------------------------------------------------------------------------- _diffrn_reflns_number 32198 #xl _diffrn_reflns_av_R_equivalents 0.0376 #xl _diffrn_reflns_av_sigmaI/netI 0.0625 #xl _diffrn_reflns_limit_h_min -19 #xl _diffrn_reflns_limit_h_max 20 #xl _diffrn_reflns_limit_k_min -23 #xl _diffrn_reflns_limit_k_max 15 #xl _diffrn_reflns_limit_l_min -32 #xl _diffrn_reflns_limit_l_max 28 #xl _diffrn_reflns_theta_min 4.24 #xl _diffrn_reflns_theta_max 26.27 #xl _diffrn_measured_fraction_theta_max 0.994 #xl _diffrn_reflns_theta_full 26.27 #xl _diffrn_measured_fraction_theta_full 0.994 #xl #:---------------------------------------------------------------------------- #:---------------------STRUCTURE SOLUTION AND REFINEMENT---------------------- #:---------------------------------------------------------------------------- _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _reflns_number_total 8144 #xl _reflns_number_gt 4323 #xl _reflns_threshold_expression >2sigma(I) #xl _reflns_special_details ? #?# "A description of reflection data not covered by the other data #?# names. It should include details of the Friedel pairs." _refine_ls_structure_factor_coef Fsqd #xl _refine_ls_matrix_type full #xl _refine_ls_weighting_scheme calc #xl _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' #xl _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refU _refine_ls_extinction_method none #xl _refine_ls_extinction_coef ? #xl _refine_ls_abs_structure_details ? #xl _refine_ls_abs_structure_Flack ? #xl _refine_ls_number_reflns 8144 #xl _refine_ls_number_parameters 489 #xl _refine_ls_number_restraints 0 #xl _refine_ls_R_factor_all 0.0815 #xl _refine_ls_R_factor_gt 0.0346 #xl _refine_ls_wR_factor_ref 0.0815 #xl _refine_ls_wR_factor_gt 0.0741 #xl _refine_ls_goodness_of_fit_ref 0.823 #xl _refine_ls_restrained_S_all 0.823 #xl _refine_ls_shift/su_max 0.001 #xl _refine_ls_shift/su_mean 0.000 #xl _refine_diff_density_max 0.388 #xl _refine_diff_density_min -0.255 #xl _refine_diff_density_rms 0.042 #xl _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. Anisotrop refinement of all none-hydrogen atoms. Details of H atom refinement: riding with U(H)=1.2*U(C) for CH2 and CH, 1.5*U(C) for CH3 C-bonded H: constr ; #:---------------------------------------------------------------------------- #:-----------------------------REFERENCES------------------------------------- #:---------------------------------------------------------------------------- _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution ; A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A. Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for crystal structure determination and refinement; J. Appl. Crystallogr. 1999, 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ; ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid Plot Program for Crystal Structure Illustrations, Oak Ridge National Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ. Glasgow) used --- SCHAKAL (E. Keller, University of Freiburg (Breisgau), Germany, 1995). ; _computing_publication_material ; PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version). #-- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses). ; #:---------------------------------------------------------------------------- #:---------------------TABLES AND GEOMETRICAL DATA---------------------------- #:---------------------------------------------------------------------------- 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 0.010469(12) 0.253499(17) 0.079860(10) 0.03136(9) Uani 1 1 d . . . S1 S 0.00495(3) 0.06473(4) 0.32928(2) 0.05317(16) Uani 1 1 d . . . O1 O -0.07441(6) 0.30388(8) 0.11131(5) 0.0365(3) Uani 1 1 d . . . O2 O 0.09099(6) 0.31300(8) 0.11230(5) 0.0348(3) Uani 1 1 d . . . O3 O -0.26868(6) 0.16234(10) 0.04196(6) 0.0559(4) Uani 1 1 d . . . O4 O -0.27382(7) 0.23749(9) 0.11460(6) 0.0568(4) Uani 1 1 d . . . O5 O 0.29547(7) 0.18892(10) 0.04680(6) 0.0563(4) Uani 1 1 d . . . O6 O 0.29314(6) 0.25996(9) 0.12121(6) 0.0518(4) Uani 1 1 d . . . N1 N -0.05606(7) 0.17981(9) 0.03621(6) 0.0314(4) Uani 1 1 d . . . N2 N 0.08319(7) 0.18780(9) 0.03709(6) 0.0319(4) Uani 1 1 d . . . N3 N 0.01181(8) 0.16371(10) 0.14518(6) 0.0359(4) Uani 1 1 d . . . N4 N 0.00757(7) 0.15251(9) 0.51662(6) 0.0325(4) Uani 1 1 d . . . C1 C 0.15622(9) 0.30981(12) 0.10373(7) 0.0322(5) Uani 1 1 d . . . C2 C 0.18798(8) 0.24505(12) 0.07634(7) 0.0322(4) Uani 1 1 d . . . C3 C 0.15057(9) 0.19155(12) 0.04313(8) 0.0351(5) Uani 1 1 d . . . H3 H 0.1772 0.1547 0.0233 0.042 Uiso 1 1 calc R . . C4 C 0.05290(10) 0.13774(12) -0.00149(8) 0.0352(5) Uani 1 1 d . . . C5 C 0.08949(11) 0.09614(14) -0.03976(9) 0.0492(6) Uani 1 1 d . . . H5 H 0.1383 0.1005 -0.0406 0.059 Uiso 1 1 calc R . . C6 C 0.05680(13) 0.04905(15) -0.07620(9) 0.0600(7) Uani 1 1 d . . . H6 H 0.0831 0.0210 -0.1013 0.072 Uiso 1 1 calc R . . C7 C -0.01451(12) 0.04280(15) -0.07606(9) 0.0597(7) Uani 1 1 d . . . H7 H -0.0371 0.0099 -0.1009 0.072 Uiso 1 1 calc R . . C8 C -0.05253(11) 0.08447(14) -0.03977(9) 0.0492(6) Uani 1 1 d . . . H8 H -0.1014 0.0807 -0.0405 0.059 Uiso 1 1 calc R . . C9 C -0.02085(10) 0.13252(12) -0.00167(8) 0.0345(5) Uani 1 1 d . . . C10 C -0.12379(9) 0.17704(12) 0.04091(8) 0.0348(5) Uani 1 1 d . . . H10 H -0.1473 0.1379 0.0205 0.042 Uiso 1 1 calc R . . C11 C -0.16556(9) 0.22696(11) 0.07358(7) 0.0328(5) Uani 1 1 d . . . C12 C -0.13896(9) 0.29309(12) 0.10260(7) 0.0334(5) Uani 1 1 d . . . C13 C -0.24017(10) 0.20587(13) 0.07347(9) 0.0406(5) Uani 1 1 d . . . C14 C -0.34740(10) 0.22213(16) 0.11877(11) 0.0688(8) Uani 1 1 d . . . H14A H -0.3561 0.1632 0.1233 0.083 Uiso 1 1 calc R . . H14B H -0.3714 0.2406 0.0873 0.083 Uiso 1 1 calc R . . C15 C -0.37294(13) 0.2688(2) 0.16480(12) 0.1054(12) Uani 1 1 d . . . H15A H -0.3489 0.2497 0.1956 0.158 Uiso 1 1 calc R . . H15B H -0.4226 0.2600 0.1688 0.158 Uiso 1 1 calc R . . H15C H -0.3639 0.3269 0.1599 0.158 Uiso 1 1 calc R . . C16 C 0.26358(10) 0.22940(13) 0.07829(9) 0.0399(5) Uani 1 1 d . . . C17 C 0.36761(10) 0.24940(17) 0.12653(11) 0.0717(8) Uani 1 1 d . . . H17A H 0.3917 0.2709 0.0959 0.086 Uiso 1 1 calc R . . H17B H 0.3791 0.1910 0.1302 0.086 Uiso 1 1 calc R . . C18 C 0.38894(14) 0.2954(2) 0.17343(13) 0.1317(15) Uani 1 1 d . . . H18A H 0.3780 0.3531 0.1690 0.198 Uiso 1 1 calc R . . H18B H 0.4387 0.2890 0.1787 0.198 Uiso 1 1 calc R . . H18C H 0.3642 0.2741 0.2033 0.198 Uiso 1 1 calc R . . C19 C -0.18278(9) 0.36237(13) 0.12203(9) 0.0428(6) Uani 1 1 d . . . C20 C -0.18022(11) 0.38424(18) 0.17375(11) 0.0761(9) Uani 1 1 d . . . H20 H -0.1548 0.3519 0.1973 0.091 Uiso 1 1 calc R . . C21 C -0.21493(15) 0.4536(3) 0.19088(16) 0.1236(16) Uani 1 1 d . . . H21 H -0.2146 0.4672 0.2263 0.148 Uiso 1 1 calc R . . C22 C -0.24970(17) 0.5022(2) 0.1562(2) 0.1241(18) Uani 1 1 d . . . H22 H -0.2723 0.5501 0.1678 0.149 Uiso 1 1 calc R . . C23 C -0.25172(13) 0.48173(18) 0.10498(19) 0.0961(12) Uani 1 1 d . . . H23 H -0.2755 0.5155 0.0813 0.115 Uiso 1 1 calc R . . C24 C -0.21872(10) 0.41105(14) 0.08777(11) 0.0596(7) Uani 1 1 d . . . H24 H -0.2210 0.3964 0.0525 0.072 Uiso 1 1 calc R . . C25 C 0.19415(9) 0.38556(12) 0.11977(8) 0.0362(5) Uani 1 1 d . . . C26 C 0.17722(10) 0.42414(15) 0.16583(9) 0.0513(6) Uani 1 1 d . . . H26 H 0.1464 0.3986 0.1891 0.062 Uiso 1 1 calc R . . C27 C 0.20535(13) 0.50028(17) 0.17806(11) 0.0687(8) Uani 1 1 d . . . H27 H 0.1938 0.5260 0.2095 0.082 Uiso 1 1 calc R . . C28 C 0.25014(13) 0.53779(16) 0.14400(14) 0.0740(9) Uani 1 1 d . . . H28 H 0.2690 0.5896 0.1520 0.089 Uiso 1 1 calc R . . C29 C 0.26724(12) 0.50029(17) 0.09889(13) 0.0724(8) Uani 1 1 d . . . H29 H 0.2983 0.5261 0.0759 0.087 Uiso 1 1 calc R . . C30 C 0.23949(10) 0.42440(14) 0.08623(10) 0.0530(6) Uani 1 1 d . . . H30 H 0.2516 0.3992 0.0547 0.064 Uiso 1 1 calc R . . C31 C 0.07291(10) 0.08421(14) 0.20846(9) 0.0507(6) Uani 1 1 d . . . H31 H 0.1160 0.0693 0.2230 0.061 Uiso 1 1 calc R . . C32 C 0.07052(10) 0.13910(14) 0.16813(9) 0.0496(6) Uani 1 1 d . . . H32 H 0.1128 0.1607 0.1559 0.060 Uiso 1 1 calc R . . C33 C -0.04613(10) 0.13002(14) 0.16343(8) 0.0458(6) Uani 1 1 d . . . H33 H -0.0885 0.1449 0.1478 0.055 Uiso 1 1 calc R . . C34 C -0.04803(10) 0.07481(14) 0.20370(8) 0.0481(6) Uani 1 1 d . . . H34 H -0.0909 0.0533 0.2149 0.058 Uiso 1 1 calc R . . C35 C 0.01235(10) 0.05112(12) 0.22748(8) 0.0388(5) Uani 1 1 d . . . C36 C 0.01212(10) -0.00381(13) 0.27439(8) 0.0462(5) Uani 1 1 d . . . H36A H 0.0553 -0.0358 0.2763 0.055 Uiso 1 1 calc R . . H36B H -0.0274 -0.0418 0.2733 0.055 Uiso 1 1 calc R . . C37 C 0.00396(9) -0.00601(12) 0.38328(7) 0.0383(5) Uani 1 1 d . . . H37A H -0.0381 -0.0402 0.3824 0.046 Uiso 1 1 calc R . . H37B H 0.0449 -0.0420 0.3823 0.046 Uiso 1 1 calc R . . C38 C 0.00490(9) 0.04616(11) 0.43109(7) 0.0324(5) Uani 1 1 d . . . C39 C -0.05577(9) 0.07955(12) 0.45130(8) 0.0365(5) Uani 1 1 d . . . H39 H -0.0991 0.0669 0.4364 0.044 Uiso 1 1 calc R . . C40 C -0.05195(9) 0.13107(12) 0.49316(8) 0.0372(5) Uani 1 1 d . . . H40 H -0.0937 0.1528 0.5063 0.045 Uiso 1 1 calc R . . C41 C 0.06577(9) 0.12046(12) 0.49639(8) 0.0363(5) Uani 1 1 d . . . H41 H 0.1085 0.1344 0.5118 0.044 Uiso 1 1 calc R . . C42 C 0.06666(9) 0.06844(12) 0.45454(8) 0.0368(5) Uani 1 1 d . . . H42 H 0.1092 0.0480 0.4419 0.044 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 0.02725(14) 0.03543(16) 0.03140(15) -0.00043(15) -0.00019(12) -0.00099(13) S1 0.0929(4) 0.0368(3) 0.0299(3) 0.0040(3) 0.0012(3) 0.0000(3) O1 0.0294(7) 0.0419(8) 0.0381(9) -0.0055(8) -0.0008(6) -0.0042(6) O2 0.0295(7) 0.0397(8) 0.0353(9) -0.0043(7) 0.0008(6) 0.0013(6) O3 0.0424(8) 0.0675(11) 0.0579(11) -0.0107(10) -0.0073(7) -0.0175(8) O4 0.0356(8) 0.0653(11) 0.0695(12) -0.0184(10) 0.0130(7) -0.0172(7) O5 0.0393(8) 0.0735(12) 0.0560(11) -0.0092(10) 0.0064(7) 0.0159(8) O6 0.0325(7) 0.0642(11) 0.0588(10) -0.0106(9) -0.0100(7) 0.0110(7) N1 0.0343(9) 0.0313(9) 0.0285(10) 0.0013(9) -0.0003(7) -0.0046(7) N2 0.0339(9) 0.0318(9) 0.0301(10) 0.0007(9) 0.0022(7) 0.0006(7) N3 0.0348(9) 0.0401(10) 0.0326(9) 0.0010(9) 0.0011(8) 0.0003(8) N4 0.0300(9) 0.0357(9) 0.0319(9) 0.0038(8) -0.0001(7) 0.0009(7) C1 0.0281(10) 0.0382(12) 0.0302(12) 0.0064(11) -0.0019(8) 0.0009(9) C2 0.0285(9) 0.0355(11) 0.0328(11) 0.0010(11) 0.0023(8) 0.0010(10) C3 0.0376(11) 0.0330(12) 0.0347(13) 0.0021(11) 0.0080(9) 0.0087(9) C4 0.0446(12) 0.0305(12) 0.0304(13) -0.0021(11) -0.0001(9) -0.0038(10) C5 0.0518(13) 0.0506(15) 0.0452(15) -0.0143(14) 0.0069(11) 0.0008(11) C6 0.0662(16) 0.0614(16) 0.0522(17) -0.0257(15) 0.0101(13) -0.0024(13) C7 0.0752(17) 0.0555(15) 0.0486(16) -0.0246(14) -0.0026(13) -0.0095(13) C8 0.0505(13) 0.0495(14) 0.0475(15) -0.0140(14) -0.0032(11) -0.0084(11) C9 0.0439(12) 0.0296(11) 0.0302(12) -0.0018(10) 0.0009(9) -0.0015(9) C10 0.0403(12) 0.0329(12) 0.0313(13) 0.0009(11) -0.0061(9) -0.0095(9) C11 0.0300(10) 0.0350(11) 0.0333(12) 0.0015(11) -0.0037(9) -0.0039(8) C12 0.0307(11) 0.0396(12) 0.0299(12) 0.0051(11) 0.0004(8) -0.0008(9) C13 0.0361(12) 0.0398(13) 0.0459(15) 0.0040(13) -0.0025(10) -0.0042(10) C14 0.0359(13) 0.0718(17) 0.099(2) -0.0053(18) 0.0148(13) -0.0129(12) C15 0.0669(18) 0.115(3) 0.134(3) -0.033(3) 0.0460(18) -0.0132(17) C16 0.0336(11) 0.0421(14) 0.0440(14) 0.0034(13) 0.0015(10) 0.0038(9) C17 0.0333(12) 0.093(2) 0.089(2) -0.0087(19) -0.0150(12) 0.0098(13) C18 0.0631(19) 0.198(4) 0.134(3) -0.063(3) -0.0448(19) 0.015(2) C19 0.0274(11) 0.0465(14) 0.0545(16) -0.0120(14) 0.0028(10) -0.0065(10) C20 0.0485(14) 0.105(2) 0.075(2) -0.039(2) 0.0005(13) 0.0082(15) C21 0.059(2) 0.167(4) 0.145(4) -0.109(3) 0.006(2) 0.011(2) C22 0.0470(18) 0.088(3) 0.237(6) -0.087(3) 0.009(3) 0.0005(16) C23 0.0476(16) 0.0497(19) 0.191(4) -0.003(2) -0.001(2) 0.0014(14) C24 0.0391(12) 0.0454(15) 0.094(2) 0.0023(16) 0.0017(13) 0.0013(11) C25 0.0260(10) 0.0388(12) 0.0437(14) -0.0021(12) -0.0048(9) 0.0035(9) C26 0.0390(12) 0.0608(16) 0.0543(16) -0.0138(15) -0.0025(11) -0.0029(11) C27 0.0625(17) 0.0675(18) 0.076(2) -0.0312(17) -0.0136(14) 0.0002(14) C28 0.0566(17) 0.0484(16) 0.117(3) -0.012(2) -0.0174(17) -0.0091(13) C29 0.0626(17) 0.0525(17) 0.102(3) 0.0059(19) 0.0064(15) -0.0116(14) C30 0.0513(13) 0.0436(14) 0.0642(18) 0.0030(14) 0.0056(12) -0.0046(11) C31 0.0420(13) 0.0638(16) 0.0464(16) 0.0174(14) -0.0042(10) 0.0081(11) C32 0.0343(12) 0.0610(16) 0.0536(16) 0.0161(15) 0.0044(11) -0.0018(11) C33 0.0367(12) 0.0586(15) 0.0420(15) 0.0090(13) -0.0055(10) -0.0057(11) C34 0.0454(13) 0.0587(16) 0.0403(15) 0.0079(14) 0.0008(10) -0.0123(12) C35 0.0526(12) 0.0367(12) 0.0271(11) -0.0026(10) 0.0013(10) 0.0014(11) C36 0.0601(13) 0.0445(13) 0.0339(12) 0.0036(11) 0.0011(10) 0.0011(11) C37 0.0500(12) 0.0345(11) 0.0304(11) 0.0042(10) -0.0007(9) 0.0009(10) C38 0.0452(12) 0.0273(10) 0.0249(10) 0.0074(9) 0.0013(9) -0.0004(9) C39 0.0325(11) 0.0417(13) 0.0352(13) 0.0008(12) -0.0044(9) -0.0032(10) C40 0.0309(11) 0.0415(13) 0.0393(14) -0.0004(12) 0.0014(9) 0.0034(10) C41 0.0290(10) 0.0456(13) 0.0342(13) 0.0007(12) -0.0029(9) 0.0009(9) C42 0.0323(11) 0.0420(13) 0.0360(13) 0.0016(12) 0.0034(9) 0.0062(10) 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 O1 1.9966(12) . ? Fe1 O2 2.0070(12) . ? Fe1 N2 2.0757(15) . ? Fe1 N1 2.0823(15) . ? Fe1 N3 2.2297(16) . ? Fe1 N4 2.2362(16) 8_565 ? S1 C37 1.807(2) . ? S1 C36 1.807(2) . ? O1 C12 1.2718(19) . ? O2 C1 1.2729(19) . ? O3 C13 1.209(2) . ? O4 C13 1.344(2) . ? O4 C14 1.439(2) . ? O5 C16 1.212(2) . ? O6 C16 1.339(2) . ? O6 C17 1.447(2) . ? N1 C10 1.307(2) . ? N1 C9 1.415(2) . ? N2 C3 1.305(2) . ? N2 C4 1.411(2) . ? N3 C33 1.327(2) . ? N3 C32 1.335(2) . ? N4 C41 1.339(2) . ? N4 C40 1.339(2) . ? N4 Fe1 2.2362(16) 8_566 ? C1 C2 1.407(2) . ? C1 C25 1.490(3) . ? C2 C3 1.417(2) . ? C2 C16 1.475(2) . ? C3 H3 0.9400 . ? C4 C5 1.387(3) . ? C4 C9 1.419(2) . ? C5 C6 1.365(3) . ? C5 H5 0.9400 . ? C6 C7 1.373(3) . ? C6 H6 0.9400 . ? C7 C8 1.367(3) . ? C7 H7 0.9400 . ? C8 C9 1.395(3) . ? C8 H8 0.9400 . ? C10 C11 1.419(2) . ? C10 H10 0.9400 . ? C11 C12 1.407(3) . ? C11 C13 1.473(2) . ? C12 C19 1.493(3) . ? C14 C15 1.492(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C17 C18 1.480(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C24 1.373(3) . ? C19 C20 1.381(3) . ? C20 C21 1.383(4) . ? C20 H20 0.9400 . ? C21 C22 1.368(5) . ? C21 H21 0.9400 . ? C22 C23 1.363(5) . ? C22 H22 0.9400 . ? C23 C24 1.386(4) . ? C23 H23 0.9400 . ? C24 H24 0.9400 . ? C25 C30 1.380(3) . ? C25 C26 1.382(3) . ? C26 C27 1.388(3) . ? C26 H26 0.9400 . ? C27 C28 1.372(4) . ? C27 H27 0.9400 . ? C28 C29 1.354(4) . ? C28 H28 0.9400 . ? C29 C30 1.384(3) . ? C29 H29 0.9400 . ? C30 H30 0.9400 . ? C31 C32 1.372(3) . ? C31 C35 1.372(3) . ? C31 H31 0.9400 . ? C32 H32 0.9400 . ? C33 C34 1.373(3) . ? C33 H33 0.9400 . ? C34 C35 1.367(3) . ? C34 H34 0.9400 . ? C35 C36 1.504(3) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 C38 1.497(3) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C38 C42 1.380(2) . ? C38 C39 1.387(2) . ? C39 C40 1.368(2) . ? C39 H39 0.9400 . ? C40 H40 0.9400 . ? C41 C42 1.371(3) . ? C41 H41 0.9400 . ? C42 H42 0.9400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O2 105.16(5) . . ? O1 Fe1 N2 167.53(6) . . ? O2 Fe1 N2 87.23(5) . . ? O1 Fe1 N1 87.43(6) . . ? O2 Fe1 N1 167.34(6) . . ? N2 Fe1 N1 80.15(6) . . ? O1 Fe1 N3 88.39(5) . . ? O2 Fe1 N3 89.57(6) . . ? N2 Fe1 N3 93.20(6) . . ? N1 Fe1 N3 92.18(6) . . ? O1 Fe1 N4 89.71(5) . 8_565 ? O2 Fe1 N4 89.60(5) . 8_565 ? N2 Fe1 N4 88.96(6) . 8_565 ? N1 Fe1 N4 89.12(6) . 8_565 ? N3 Fe1 N4 177.65(6) . 8_565 ? C37 S1 C36 102.17(10) . . ? C12 O1 Fe1 131.85(12) . . ? C1 O2 Fe1 131.76(12) . . ? C13 O4 C14 117.68(18) . . ? C16 O6 C17 116.94(17) . . ? C10 N1 C9 121.37(16) . . ? C10 N1 Fe1 125.47(13) . . ? C9 N1 Fe1 113.14(11) . . ? C3 N2 C4 121.33(16) . . ? C3 N2 Fe1 125.42(13) . . ? C4 N2 Fe1 113.23(11) . . ? C33 N3 C32 115.29(17) . . ? C33 N3 Fe1 121.93(13) . . ? C32 N3 Fe1 122.76(13) . . ? C41 N4 C40 115.78(17) . . ? C41 N4 Fe1 121.98(12) . 8_566 ? C40 N4 Fe1 121.92(12) . 8_566 ? O2 C1 C2 122.95(17) . . ? O2 C1 C25 113.51(17) . . ? C2 C1 C25 123.15(16) . . ? C1 C2 C3 122.93(16) . . ? C1 C2 C16 122.60(18) . . ? C3 C2 C16 114.43(17) . . ? N2 C3 C2 127.14(17) . . ? N2 C3 H3 116.4 . . ? C2 C3 H3 116.4 . . ? C5 C4 N2 125.03(18) . . ? C5 C4 C9 118.29(19) . . ? N2 C4 C9 116.63(18) . . ? C6 C5 C4 122.0(2) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C7 119.9(2) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C8 C7 C6 119.8(2) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C7 C8 C9 121.8(2) . . ? C7 C8 H8 119.1 . . ? C9 C8 H8 119.1 . . ? C8 C9 N1 125.61(18) . . ? C8 C9 C4 118.10(19) . . ? N1 C9 C4 116.24(17) . . ? N1 C10 C11 126.71(18) . . ? N1 C10 H10 116.6 . . ? C11 C10 H10 116.6 . . ? C12 C11 C10 123.28(16) . . ? C12 C11 C13 122.16(18) . . ? C10 C11 C13 114.53(18) . . ? O1 C12 C11 123.60(17) . . ? O1 C12 C19 112.68(17) . . ? C11 C12 C19 123.47(16) . . ? O3 C13 O4 122.46(19) . . ? O3 C13 C11 125.3(2) . . ? O4 C13 C11 112.14(19) . . ? O4 C14 C15 107.1(2) . . ? O4 C14 H14A 110.3 . . ? C15 C14 H14A 110.3 . . ? O4 C14 H14B 110.3 . . ? C15 C14 H14B 110.3 . . ? H14A C14 H14B 108.6 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O5 C16 O6 122.76(18) . . ? O5 C16 C2 124.7(2) . . ? O6 C16 C2 112.41(18) . . ? O6 C17 C18 106.9(2) . . ? O6 C17 H17A 110.3 . . ? C18 C17 H17A 110.3 . . ? O6 C17 H17B 110.3 . . ? C18 C17 H17B 110.3 . . ? H17A C17 H17B 108.6 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 119.4(2) . . ? C24 C19 C12 120.2(2) . . ? C20 C19 C12 119.9(2) . . ? C19 C20 C21 120.1(3) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 119.9(4) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C21 120.3(3) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 120.0(3) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C19 C24 C23 120.2(3) . . ? C19 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C30 C25 C26 118.6(2) . . ? C30 C25 C1 120.9(2) . . ? C26 C25 C1 119.95(18) . . ? C25 C26 C27 120.6(2) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C28 C27 C26 119.7(3) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C29 C28 C27 120.1(2) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 120.8(3) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C25 C30 C29 120.3(2) . . ? C25 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C32 C31 C35 119.88(19) . . ? C32 C31 H31 120.1 . . ? C35 C31 H31 120.1 . . ? N3 C32 C31 124.03(18) . . ? N3 C32 H32 118.0 . . ? C31 C32 H32 118.0 . . ? N3 C33 C34 124.11(18) . . ? N3 C33 H33 117.9 . . ? C34 C33 H33 117.9 . . ? C35 C34 C33 120.07(19) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C31 116.60(19) . . ? C34 C35 C36 121.73(18) . . ? C31 C35 C36 121.54(19) . . ? C35 C36 S1 105.25(14) . . ? C35 C36 H36A 110.7 . . ? S1 C36 H36A 110.7 . . ? C35 C36 H36B 110.7 . . ? S1 C36 H36B 110.7 . . ? H36A C36 H36B 108.8 . . ? C38 C37 S1 105.84(13) . . ? C38 C37 H37A 110.6 . . ? S1 C37 H37A 110.6 . . ? C38 C37 H37B 110.6 . . ? S1 C37 H37B 110.6 . . ? H37A C37 H37B 108.7 . . ? C42 C38 C39 117.03(18) . . ? C42 C38 C37 121.35(17) . . ? C39 C38 C37 121.43(17) . . ? C40 C39 C38 119.41(17) . . ? C40 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? N4 C40 C39 124.16(17) . . ? N4 C40 H40 117.9 . . ? C39 C40 H40 117.9 . . ? N4 C41 C42 123.86(17) . . ? N4 C41 H41 118.1 . . ? C42 C41 H41 118.1 . . ? C41 C42 C38 119.75(17) . . ? C41 C42 H42 120.1 . . ? C38 C42 H42 120.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Fe1 O1 C12 175.26(16) . . . . ? N2 Fe1 O1 C12 1.9(4) . . . . ? N1 Fe1 O1 C12 -3.38(16) . . . . ? N3 Fe1 O1 C12 -95.63(17) . . . . ? N4 Fe1 O1 C12 85.75(16) 8_565 . . . ? O1 Fe1 O2 C1 -174.24(15) . . . . ? N2 Fe1 O2 C1 4.32(16) . . . . ? N1 Fe1 O2 C1 -0.5(4) . . . . ? N3 Fe1 O2 C1 97.55(16) . . . . ? N4 Fe1 O2 C1 -84.65(16) 8_565 . . . ? O1 Fe1 N1 C10 -5.57(15) . . . . ? O2 Fe1 N1 C10 -179.5(2) . . . . ? N2 Fe1 N1 C10 175.59(16) . . . . ? N3 Fe1 N1 C10 82.71(15) . . . . ? N4 Fe1 N1 C10 -95.32(15) 8_565 . . . ? O1 Fe1 N1 C9 172.68(12) . . . . ? O2 Fe1 N1 C9 -1.3(3) . . . . ? N2 Fe1 N1 C9 -6.16(12) . . . . ? N3 Fe1 N1 C9 -99.03(12) . . . . ? N4 Fe1 N1 C9 82.94(12) 8_565 . . . ? O1 Fe1 N2 C3 -179.7(2) . . . . ? O2 Fe1 N2 C3 6.71(15) . . . . ? N1 Fe1 N2 C3 -174.35(16) . . . . ? N3 Fe1 N2 C3 -82.70(16) . . . . ? N4 Fe1 N2 C3 96.36(15) 8_565 . . . ? O1 Fe1 N2 C4 1.5(3) . . . . ? O2 Fe1 N2 C4 -172.01(13) . . . . ? N1 Fe1 N2 C4 6.92(12) . . . . ? N3 Fe1 N2 C4 98.58(12) . . . . ? N4 Fe1 N2 C4 -82.37(12) 8_565 . . . ? O1 Fe1 N3 C33 40.60(15) . . . . ? O2 Fe1 N3 C33 145.78(15) . . . . ? N2 Fe1 N3 C33 -127.02(15) . . . . ? N1 Fe1 N3 C33 -46.77(16) . . . . ? O1 Fe1 N3 C32 -140.44(16) . . . . ? O2 Fe1 N3 C32 -35.26(16) . . . . ? N2 Fe1 N3 C32 51.94(16) . . . . ? N1 Fe1 N3 C32 132.19(16) . . . . ? Fe1 O2 C1 C2 -16.9(3) . . . . ? Fe1 O2 C1 C25 156.13(13) . . . . ? O2 C1 C2 C3 19.3(3) . . . . ? C25 C1 C2 C3 -153.07(19) . . . . ? O2 C1 C2 C16 -163.18(18) . . . . ? C25 C1 C2 C16 24.4(3) . . . . ? C4 N2 C3 C2 172.98(18) . . . . ? Fe1 N2 C3 C2 -5.7(3) . . . . ? C1 C2 C3 N2 -7.7(3) . . . . ? C16 C2 C3 N2 174.58(19) . . . . ? C3 N2 C4 C5 -7.8(3) . . . . ? Fe1 N2 C4 C5 171.01(17) . . . . ? C3 N2 C4 C9 174.51(17) . . . . ? Fe1 N2 C4 C9 -6.7(2) . . . . ? N2 C4 C5 C6 -179.6(2) . . . . ? C9 C4 C5 C6 -1.9(3) . . . . ? C4 C5 C6 C7 0.9(4) . . . . ? C5 C6 C7 C8 0.7(4) . . . . ? C6 C7 C8 C9 -1.3(4) . . . . ? C7 C8 C9 N1 177.72(19) . . . . ? C7 C8 C9 C4 0.3(3) . . . . ? C10 N1 C9 C8 5.4(3) . . . . ? Fe1 N1 C9 C8 -172.95(16) . . . . ? C10 N1 C9 C4 -177.19(17) . . . . ? Fe1 N1 C9 C4 4.5(2) . . . . ? C5 C4 C9 C8 1.2(3) . . . . ? N2 C4 C9 C8 179.10(17) . . . . ? C5 C4 C9 N1 -176.40(17) . . . . ? N2 C4 C9 N1 1.5(3) . . . . ? C9 N1 C10 C11 -173.40(18) . . . . ? Fe1 N1 C10 C11 4.7(3) . . . . ? N1 C10 C11 C12 6.1(3) . . . . ? N1 C10 C11 C13 -175.86(18) . . . . ? Fe1 O1 C12 C11 13.6(3) . . . . ? Fe1 O1 C12 C19 -160.77(14) . . . . ? C10 C11 C12 O1 -15.6(3) . . . . ? C13 C11 C12 O1 166.51(18) . . . . ? C10 C11 C12 C19 158.18(19) . . . . ? C13 C11 C12 C19 -19.7(3) . . . . ? C14 O4 C13 O3 -3.8(3) . . . . ? C14 O4 C13 C11 179.30(18) . . . . ? C12 C11 C13 O3 163.5(2) . . . . ? C10 C11 C13 O3 -14.5(3) . . . . ? C12 C11 C13 O4 -19.6(3) . . . . ? C10 C11 C13 O4 162.33(17) . . . . ? C13 O4 C14 C15 -175.6(2) . . . . ? C17 O6 C16 O5 5.8(3) . . . . ? C17 O6 C16 C2 -178.82(18) . . . . ? C1 C2 C16 O5 -161.2(2) . . . . ? C3 C2 C16 O5 16.5(3) . . . . ? C1 C2 C16 O6 23.5(3) . . . . ? C3 C2 C16 O6 -158.79(17) . . . . ? C16 O6 C17 C18 174.1(2) . . . . ? O1 C12 C19 C24 114.4(2) . . . . ? C11 C12 C19 C24 -60.0(3) . . . . ? O1 C12 C19 C20 -57.2(3) . . . . ? C11 C12 C19 C20 128.4(2) . . . . ? C24 C19 C20 C21 1.4(4) . . . . ? C12 C19 C20 C21 173.2(2) . . . . ? C19 C20 C21 C22 -2.4(5) . . . . ? C20 C21 C22 C23 1.5(5) . . . . ? C21 C22 C23 C24 0.3(5) . . . . ? C20 C19 C24 C23 0.4(3) . . . . ? C12 C19 C24 C23 -171.32(19) . . . . ? C22 C23 C24 C19 -1.3(4) . . . . ? O2 C1 C25 C30 -130.02(19) . . . . ? C2 C1 C25 C30 43.0(3) . . . . ? O2 C1 C25 C26 41.1(3) . . . . ? C2 C1 C25 C26 -145.81(19) . . . . ? C30 C25 C26 C27 -0.1(3) . . . . ? C1 C25 C26 C27 -171.45(19) . . . . ? C25 C26 C27 C28 0.3(3) . . . . ? C26 C27 C28 C29 -0.6(4) . . . . ? C27 C28 C29 C30 0.6(4) . . . . ? C26 C25 C30 C29 0.1(3) . . . . ? C1 C25 C30 C29 171.4(2) . . . . ? C28 C29 C30 C25 -0.4(4) . . . . ? C33 N3 C32 C31 -1.2(3) . . . . ? Fe1 N3 C32 C31 179.78(17) . . . . ? C35 C31 C32 N3 0.1(4) . . . . ? C32 N3 C33 C34 1.3(3) . . . . ? Fe1 N3 C33 C34 -179.67(16) . . . . ? N3 C33 C34 C35 -0.2(3) . . . . ? C33 C34 C35 C31 -0.9(3) . . . . ? C33 C34 C35 C36 174.99(19) . . . . ? C32 C31 C35 C34 1.0(3) . . . . ? C32 C31 C35 C36 -174.91(19) . . . . ? C34 C35 C36 S1 -88.2(2) . . . . ? C31 C35 C36 S1 87.5(2) . . . . ? C37 S1 C36 C35 179.30(13) . . . . ? C36 S1 C37 C38 174.77(12) . . . . ? S1 C37 C38 C42 -91.35(18) . . . . ? S1 C37 C38 C39 83.45(18) . . . . ? C42 C38 C39 C40 -0.9(3) . . . . ? C37 C38 C39 C40 -175.92(17) . . . . ? C41 N4 C40 C39 0.4(3) . . . . ? Fe1 N4 C40 C39 173.91(15) 8_566 . . . ? C38 C39 C40 N4 0.2(3) . . . . ? C40 N4 C41 C42 -0.3(3) . . . . ? Fe1 N4 C41 C42 -173.86(15) 8_566 . . . ? N4 C41 C42 C38 -0.3(3) . . . . ? C39 C38 C42 C41 1.0(3) . . . . ? C37 C38 C42 C41 175.97(17) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? #?# use this item for nonbonding or very weakly bonding contacts, e.g.: #?# Sb1 N13 3.906(13) . . ? #?# Mn Mn 3.253(2) . 2 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? #?# Do not(!) delete the #s to obtain a table header: # #D H A D - H H...A D...A D - H...A symm(A) publ_flag # #?# style: #?# N2 H721 O93 .72(4) 2.28(4) 2.868(4) 139(4) . ? #?# N2 H722 O1 .92(3) 2.44(3) 3.343(4) 171(3) 2_657 ? #?# #?# (1) This table may be copied from SHELXL97 (command HTAB D A_$n) #?# and rearranged (_geom_hbond_publ_flag missing); or #?# #?# (2) it may be copied from PLATON and rearranged; CAUTION! Check #?# symmetry operation numbers! They must(!) be identical from PLATON #?# and ACTA! "calc intra nomove" must(!) be used in PLATON runs! #?# Even then discrepancies may(!) occur! _geom_special_details ? #;Puckering parameters (\%A, \%) according to # D. Cremer, J. A. Pople, J. Am. Chem. Soc. 1975, 97, 1354--1358 #?# #?# style: #?# #?# Sb1 O2 C2 C3 O3 Q2 = 0.217(15) \f2 = 134(4) #?# O52 C12 C22 C32 C42 C52 Q = 0.577(5) \q = 3.2(6) \f = 271(9) #?# #?# or as a table: #?# #?# O5n - C1n - C2n - C3n - C4n - C5n #?# ------------------------------ #?# n Q theta phi #?# ------------------------------ #?# 11 .574(11) 6.3(11) 112(10) #?# 21 .557(10) 2.1(11) 86(22) #?# 31 .540(10) 6.2(11) 92(10) #?# 41 .571(10) 2.2(10) 221(34) #?# 51 .555(10) 10.6(10) 35(6) #?# 61 .571(10) 5.1(10) 13(13) #?# ------------------------------ #?# #?# least-squares planes be entered here, too #:---------------------------------------------------------------------------- #:--------------------------ARCHIVING AND CHECKING---------------------------- #:---------------------------------------------------------------------------- _audit_block_code Fe_L4_bpms_oo195_Bauer _audit_creation_method 'form98_non/compatible with shelxl97-2' _chemical_name_systematic ? _chemical_formula_moiety 'C42 H38 Fe N4 O6 S' _chemical_formula_sum 'C42 H38 Fe N4 O6 S' _chemical_formula_weight 782.685 _chemical_melting_point ? _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.2908 _exptl_crystal_F_000 3264