# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Franc Meyer' 'Joachim Ballmann' 'Sebastian Dechert' 'Benjamin Schneider' 'Xianru Sun' _publ_contact_author_name 'Franc Meyer' _publ_contact_author_email FRANC.MEYER@CHEMIE.UNI-GOETTINGEN.DE _publ_section_title ; A Convenient Ligand Exchange Pathway to [2Fe-2S] Ferredoxin Analogues ; # Attachment '2009_DaltonTrans_JB.cif' #============================================================================== data_4c-ab44 _database_code_depnum_ccdc_archive 'CCDC 717459' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H36 Fe2 S6 2-, 2(C8 H20 N +)' _chemical_formula_sum 'C48 H76 Fe2 N2 S6' _chemical_formula_weight 985.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.8071(4) _cell_length_b 16.8841(4) _cell_length_c 13.2627(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.673(2) _cell_angle_gamma 90.00 _cell_volume 2545.64(13) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 30798 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 26.72 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.49 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1052 _exptl_absorpt_coefficient_mu 0.849 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5982 _exptl_absorpt_correction_T_max 0.7829 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30798 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0144 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 26.72 _reflns_number_total 5385 _reflns_number_gt 4954 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+1.3634P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5385 _refine_ls_number_parameters 270 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0683 _refine_ls_wR_factor_gt 0.0667 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.478754(18) 0.565043(12) 0.436997(16) 0.02104(6) Uani 1 1 d . . . S1 S 0.53058(4) 0.55989(2) 0.60913(3) 0.02592(9) Uani 1 1 d . . . S2 S 0.30374(3) 0.63525(2) 0.38994(3) 0.02764(9) Uani 1 1 d . . . S3 S 0.60552(3) 0.63542(2) 0.36599(3) 0.02714(9) Uani 1 1 d . . . C1 C 0.26914(14) 0.64508(9) 0.25105(12) 0.0271(3) Uani 1 1 d . . . C2 C 0.20859(14) 0.58462(10) 0.18588(13) 0.0304(3) Uani 1 1 d . . . C3 C 0.17972(16) 0.59478(12) 0.07750(14) 0.0391(4) Uani 1 1 d . . . H3 H 0.1421 0.5541 0.0339 0.080 Uiso 1 1 calc R . . C4 C 0.20620(18) 0.66455(13) 0.03390(14) 0.0440(4) Uani 1 1 d . . . H4 H 0.1858 0.6708 -0.0384 0.080 Uiso 1 1 calc R . . C5 C 0.26274(17) 0.72439(11) 0.09821(15) 0.0401(4) Uani 1 1 d . . . H5 H 0.2783 0.7717 0.0685 0.080 Uiso 1 1 calc R . . C6 C 0.29741(14) 0.71617(10) 0.20686(14) 0.0316(3) Uani 1 1 d . . . C7 C 0.17206(16) 0.50950(10) 0.22983(14) 0.0363(4) Uani 1 1 d . . . H7A H 0.2408 0.4815 0.2687 0.080 Uiso 1 1 calc R . . H7B H 0.1284 0.4768 0.1735 0.080 Uiso 1 1 calc R . . H7C H 0.1238 0.5224 0.2753 0.080 Uiso 1 1 calc R . . C8 C 0.36297(17) 0.78206(10) 0.27365(16) 0.0401(4) Uani 1 1 d . . . H8A H 0.3656 0.8273 0.2305 0.080 Uiso 1 1 calc R . . H8B H 0.4416 0.7650 0.3074 0.080 Uiso 1 1 calc R . . H8C H 0.3236 0.7960 0.3257 0.080 Uiso 1 1 calc R . . C9 C 0.67924(13) 0.56888(8) 0.30192(12) 0.0233(3) Uani 1 1 d . . . C10 C 0.63897(13) 0.55857(9) 0.19268(12) 0.0261(3) Uani 1 1 d . . . C11 C 0.70737(15) 0.51484(10) 0.14165(12) 0.0301(3) Uani 1 1 d . . . H11 H 0.6816 0.5080 0.0695 0.080 Uiso 1 1 calc R . . C12 C 0.81319(15) 0.48143(9) 0.19715(13) 0.0311(3) Uani 1 1 d . . . H12 H 0.8598 0.4545 0.1620 0.080 Uiso 1 1 calc R . . C13 C 0.84897(14) 0.48846(9) 0.30503(13) 0.0283(3) Uani 1 1 d . . . H13 H 0.9187 0.4645 0.3421 0.080 Uiso 1 1 calc R . . C14 C 0.78283(13) 0.53059(9) 0.35928(12) 0.0245(3) Uani 1 1 d . . . C15 C 0.52300(14) 0.59275(11) 0.13166(13) 0.0336(4) Uani 1 1 d . . . H15A H 0.5053 0.5748 0.0604 0.080 Uiso 1 1 calc R . . H15B H 0.5276 0.6495 0.1333 0.080 Uiso 1 1 calc R . . H15C H 0.4622 0.5757 0.1623 0.080 Uiso 1 1 calc R . . C16 C 0.81989(14) 0.53305(10) 0.47675(12) 0.0317(3) Uani 1 1 d . . . H16A H 0.8208 0.5870 0.4999 0.080 Uiso 1 1 calc R . . H16B H 0.8972 0.5108 0.5019 0.080 Uiso 1 1 calc R . . H16C H 0.7654 0.5030 0.5036 0.080 Uiso 1 1 calc R . . N1 N 0.43892(11) 0.74389(7) 0.78431(9) 0.0222(2) Uani 1 1 d . . . C21 C 0.34506(13) 0.68467(9) 0.73138(13) 0.0278(3) Uani 1 1 d . . . H21A H 0.3612 0.6667 0.6672 0.080 Uiso 1 1 calc R . . H21B H 0.3502 0.6390 0.7768 0.080 Uiso 1 1 calc R . . C22 C 0.22077(14) 0.71696(10) 0.70545(14) 0.0345(4) Uani 1 1 d . . . H22A H 0.2030 0.7336 0.7687 0.080 Uiso 1 1 calc R . . H22B H 0.1665 0.6764 0.6722 0.080 Uiso 1 1 calc R . . H22C H 0.2141 0.7614 0.6590 0.080 Uiso 1 1 calc R . . C23 C 0.43052(15) 0.81908(9) 0.71982(13) 0.0298(3) Uani 1 1 d . . . H23A H 0.3604 0.8478 0.7232 0.080 Uiso 1 1 calc R . . H23B H 0.4978 0.8523 0.7514 0.080 Uiso 1 1 calc R . . C24 C 0.42609(19) 0.80599(12) 0.60561(14) 0.0437(4) Uani 1 1 d . . . H24A H 0.4950 0.7777 0.6011 0.080 Uiso 1 1 calc R . . H24B H 0.4231 0.8563 0.5712 0.080 Uiso 1 1 calc R . . H24C H 0.3573 0.7758 0.5723 0.080 Uiso 1 1 calc R . . C25 C 0.55984(13) 0.70754(9) 0.79658(12) 0.0265(3) Uani 1 1 d . . . H25A H 0.5662 0.6920 0.7279 0.080 Uiso 1 1 calc R . . H25B H 0.6188 0.7479 0.8231 0.080 Uiso 1 1 calc R . . C26 C 0.58788(15) 0.63641(10) 0.86819(13) 0.0335(4) Uani 1 1 d . . . H26A H 0.5892 0.6520 0.9381 0.080 Uiso 1 1 calc R . . H26B H 0.6634 0.6156 0.8677 0.080 Uiso 1 1 calc R . . H26C H 0.5288 0.5965 0.8442 0.080 Uiso 1 1 calc R . . C27 C 0.42102(14) 0.76469(10) 0.89023(12) 0.0291(3) Uani 1 1 d . . . H27A H 0.3452 0.7904 0.8793 0.080 Uiso 1 1 calc R . . H27B H 0.4187 0.7160 0.9285 0.080 Uiso 1 1 calc R . . C28 C 0.51448(16) 0.81799(13) 0.95653(14) 0.0422(4) Uani 1 1 d . . . H28A H 0.5902 0.7935 0.9670 0.080 Uiso 1 1 calc R . . H28B H 0.4989 0.8265 1.0231 0.080 Uiso 1 1 calc R . . H28C H 0.5138 0.8679 0.9217 0.080 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 0.02583(12) 0.01917(11) 0.02185(11) 0.00057(7) 0.01285(8) 0.00218(8) S1 0.0359(2) 0.02234(18) 0.02236(18) -0.00347(13) 0.01267(15) 0.00293(14) S2 0.0310(2) 0.02664(19) 0.03026(19) 0.00430(15) 0.01676(15) 0.00802(15) S3 0.0309(2) 0.02331(18) 0.03295(19) 0.00160(14) 0.01839(16) -0.00016(14) C1 0.0272(8) 0.0269(7) 0.0319(8) 0.0067(6) 0.0163(6) 0.0082(6) C2 0.0277(8) 0.0306(8) 0.0354(8) 0.0042(7) 0.0129(7) 0.0062(6) C3 0.0394(10) 0.0441(10) 0.0344(9) 0.0009(8) 0.0109(7) 0.0042(8) C4 0.0486(11) 0.0545(11) 0.0313(9) 0.0108(8) 0.0147(8) 0.0082(9) C5 0.0443(10) 0.0395(9) 0.0437(10) 0.0180(8) 0.0243(8) 0.0102(8) C6 0.0315(8) 0.0274(8) 0.0415(9) 0.0077(7) 0.0195(7) 0.0074(6) C7 0.0347(9) 0.0303(8) 0.0431(9) 0.0038(7) 0.0089(7) -0.0008(7) C8 0.0449(10) 0.0254(8) 0.0560(11) 0.0063(8) 0.0238(9) 0.0032(7) C9 0.0242(7) 0.0218(7) 0.0275(7) 0.0024(5) 0.0133(6) -0.0028(5) C10 0.0251(7) 0.0259(7) 0.0288(7) 0.0024(6) 0.0099(6) -0.0037(6) C11 0.0340(8) 0.0308(8) 0.0280(7) -0.0040(6) 0.0130(6) -0.0053(6) C12 0.0327(8) 0.0260(8) 0.0403(9) -0.0049(6) 0.0193(7) -0.0015(6) C13 0.0251(8) 0.0230(7) 0.0385(8) 0.0019(6) 0.0115(6) -0.0003(6) C14 0.0243(7) 0.0222(7) 0.0290(7) 0.0035(6) 0.0108(6) -0.0041(6) C15 0.0279(8) 0.0419(9) 0.0309(8) 0.0032(7) 0.0074(6) 0.0004(7) C16 0.0298(8) 0.0373(9) 0.0290(8) 0.0072(7) 0.0096(6) -0.0022(7) N1 0.0231(6) 0.0208(6) 0.0244(6) -0.0044(5) 0.0096(5) -0.0009(5) C21 0.0262(8) 0.0223(7) 0.0339(8) -0.0063(6) 0.0063(6) -0.0035(6) C22 0.0257(8) 0.0309(8) 0.0428(9) -0.0060(7) 0.0024(7) -0.0016(6) C23 0.0359(8) 0.0217(7) 0.0343(8) 0.0006(6) 0.0138(7) -0.0007(6) C24 0.0570(12) 0.0440(10) 0.0355(9) 0.0084(8) 0.0220(9) 0.0029(9) C25 0.0237(7) 0.0256(7) 0.0336(8) -0.0049(6) 0.0136(6) 0.0003(6) C26 0.0296(8) 0.0340(9) 0.0382(9) 0.0018(7) 0.0112(7) 0.0073(7) C27 0.0266(8) 0.0382(9) 0.0245(7) -0.0056(6) 0.0101(6) 0.0044(6) C28 0.0313(9) 0.0590(12) 0.0344(9) -0.0213(9) 0.0057(7) 0.0042(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 S1 2.1908(4) 3_666 ? Fe1 S1 2.1998(4) . ? Fe1 S3 2.3024(4) . ? Fe1 S2 2.3169(4) . ? Fe1 Fe1 2.7232(4) 3_666 ? S1 Fe1 2.1908(4) 3_666 ? S2 C1 1.7835(16) . ? S3 C9 1.7724(15) . ? C1 C2 1.402(2) . ? C1 C6 1.415(2) . ? C2 C3 1.395(2) . ? C2 C7 1.507(2) . ? C3 C4 1.385(3) . ? C4 C5 1.373(3) . ? C5 C6 1.395(2) . ? C6 C8 1.500(3) . ? C9 C10 1.408(2) . ? C9 C14 1.411(2) . ? C10 C11 1.397(2) . ? C10 C15 1.505(2) . ? C11 C12 1.387(2) . ? C12 C13 1.383(2) . ? C13 C14 1.392(2) . ? C14 C16 1.501(2) . ? N1 C21 1.5167(18) . ? N1 C27 1.5171(18) . ? N1 C23 1.5189(19) . ? N1 C25 1.5218(18) . ? C21 C22 1.515(2) . ? C23 C24 1.518(2) . ? C25 C26 1.511(2) . ? C27 C28 1.509(2) . ? 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 S1 Fe1 S1 103.335(14) 3_666 . ? S1 Fe1 S3 111.837(16) 3_666 . ? S1 Fe1 S3 114.556(17) . . ? S1 Fe1 S2 116.328(17) 3_666 . ? S1 Fe1 S2 106.116(16) . . ? S3 Fe1 S2 104.879(16) . . ? S1 Fe1 Fe1 51.815(12) 3_666 3_666 ? S1 Fe1 Fe1 51.520(12) . 3_666 ? S3 Fe1 Fe1 129.417(16) . 3_666 ? S2 Fe1 Fe1 125.524(15) . 3_666 ? Fe1 S1 Fe1 76.665(14) 3_666 . ? C1 S2 Fe1 105.34(5) . . ? C9 S3 Fe1 109.06(5) . . ? C2 C1 C6 120.03(15) . . ? C2 C1 S2 120.35(12) . . ? C6 C1 S2 119.53(13) . . ? C3 C2 C1 119.17(15) . . ? C3 C2 C7 119.09(16) . . ? C1 C2 C7 121.73(15) . . ? C4 C3 C2 120.99(18) . . ? C5 C4 C3 119.55(17) . . ? C4 C5 C6 121.75(16) . . ? C5 C6 C1 118.44(16) . . ? C5 C6 C8 119.80(15) . . ? C1 C6 C8 121.76(15) . . ? C10 C9 C14 120.05(13) . . ? C10 C9 S3 119.90(11) . . ? C14 C9 S3 119.90(11) . . ? C11 C10 C9 119.02(14) . . ? C11 C10 C15 120.23(14) . . ? C9 C10 C15 120.74(14) . . ? C12 C11 C10 120.91(15) . . ? C13 C12 C11 119.58(14) . . ? C12 C13 C14 121.42(15) . . ? C13 C14 C9 118.77(14) . . ? C13 C14 C16 120.25(14) . . ? C9 C14 C16 120.96(13) . . ? C21 N1 C27 108.30(11) . . ? C21 N1 C23 111.22(12) . . ? C27 N1 C23 108.89(11) . . ? C21 N1 C25 109.31(11) . . ? C27 N1 C25 110.83(11) . . ? C23 N1 C25 108.30(11) . . ? C22 C21 N1 114.18(12) . . ? C24 C23 N1 114.82(13) . . ? C26 C25 N1 115.32(12) . . ? C28 C27 N1 114.50(13) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.72 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.294 _refine_diff_density_min -0.346 _refine_diff_density_rms 0.044 data_4d-ab40 _database_code_depnum_ccdc_archive 'CCDC 717460' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H36 Fe2 S6 2-, 2(C8 H20 N +)' _chemical_formula_sum 'C48 H76 Fe2 N2 S6' _chemical_formula_weight 985.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.1076(3) _cell_length_b 16.2036(4) _cell_length_c 15.7653(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.146(3) _cell_angle_gamma 90.00 _cell_volume 2555.98(13) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 31517 _cell_measurement_theta_min 1.81 _cell_measurement_theta_max 26.96 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1052 _exptl_absorpt_coefficient_mu 0.846 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6061 _exptl_absorpt_correction_T_max 0.7762 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31517 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 26.96 _reflns_number_total 5552 _reflns_number_gt 4999 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+4.1786P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5552 _refine_ls_number_parameters 257 _refine_ls_number_restraints 46 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1342 _refine_ls_wR_factor_gt 0.1310 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.47153(4) 0.44132(3) 0.55545(3) 0.02855(13) Uani 1 1 d . . . S1 S 0.53142(7) 0.57018(5) 0.58396(5) 0.03181(18) Uani 1 1 d . . . S2 S 0.25624(7) 0.40653(5) 0.57884(5) 0.03285(19) Uani 1 1 d . . . S3 S 0.62658(8) 0.36061(5) 0.63820(5) 0.0378(2) Uani 1 1 d . . . C1 C 0.2412(3) 0.39581(17) 0.68840(18) 0.0251(5) Uani 1 1 d . . . C2 C 0.3372(3) 0.42332(18) 0.7552(2) 0.0292(6) Uani 1 1 d . . . H2 H 0.4164 0.4466 0.7427 0.080 Uiso 1 1 calc R . . C3 C 0.3156(3) 0.41626(19) 0.8398(2) 0.0320(6) Uani 1 1 d . . . C4 C 0.1965(3) 0.38234(19) 0.85901(19) 0.0311(6) Uani 1 1 d . . . H4 H 0.1815 0.3786 0.9157 0.080 Uiso 1 1 calc R . . C5 C 0.0999(3) 0.35404(19) 0.79360(19) 0.0291(6) Uani 1 1 d . . . C6 C 0.1239(3) 0.36093(18) 0.70971(19) 0.0273(6) Uani 1 1 d . . . H6 H 0.0599 0.3417 0.6660 0.080 Uiso 1 1 calc R . . C7 C 0.4210(4) 0.4444(3) 0.9116(2) 0.0478(9) Uani 1 1 d . . . H7A H 0.4298 0.5033 0.9095 0.080 Uiso 1 1 calc R . . H7B H 0.5049 0.4191 0.9054 0.080 Uiso 1 1 calc R . . H7C H 0.3951 0.4286 0.9657 0.080 Uiso 1 1 calc R . . C8 C -0.0273(3) 0.3155(2) 0.8148(2) 0.0414(8) Uani 1 1 d . . . H8A H -0.0285 0.3182 0.8755 0.080 Uiso 1 1 calc R . . H8B H -0.0316 0.2589 0.7967 0.080 Uiso 1 1 calc R . . H8C H -0.1028 0.3449 0.7856 0.080 Uiso 1 1 calc R . . C9 C 0.5970(3) 0.2549(2) 0.61273(19) 0.0323(6) Uani 1 1 d . . . C10 C 0.6984(3) 0.1981(2) 0.6403(2) 0.0368(7) Uani 1 1 d . . . H10 H 0.7807 0.2175 0.6665 0.080 Uiso 1 1 calc R . . C11 C 0.6798(3) 0.1138(2) 0.6296(2) 0.0394(7) Uani 1 1 d . . . C12 C 0.5565(3) 0.0849(2) 0.5894(2) 0.0370(7) Uani 1 1 d . . . H12 H 0.5423 0.0285 0.5824 0.080 Uiso 1 1 calc R . . C13 C 0.4542(3) 0.1401(2) 0.55983(19) 0.0345(7) Uani 1 1 d . . . C14 C 0.4753(3) 0.2245(2) 0.5715(2) 0.0340(7) Uani 1 1 d . . . H14 H 0.4073 0.2612 0.5516 0.080 Uiso 1 1 calc R . . C15 C 0.7895(4) 0.0543(3) 0.6635(3) 0.0593(11) Uani 1 1 d . . . H15A H 0.8490 0.0473 0.6217 0.080 Uiso 1 1 calc R . . H15B H 0.7510 0.0020 0.6749 0.080 Uiso 1 1 calc R . . H15C H 0.8382 0.0758 0.7155 0.080 Uiso 1 1 calc R . . C16 C 0.3209(4) 0.1082(2) 0.5167(3) 0.0453(8) Uani 1 1 d . . . H16A H 0.2505 0.1425 0.5320 0.080 Uiso 1 1 calc R . . H16B H 0.3083 0.0526 0.5351 0.080 Uiso 1 1 calc R . . H16C H 0.3191 0.1091 0.4557 0.080 Uiso 1 1 calc R . . N1A N 0.9413(6) 0.3556(3) 0.3502(3) 0.0273(16) Uiso 0.510(6) 1 d PD A 1 C21A C 0.8582(6) 0.3035(4) 0.2800(4) 0.0409(16) Uiso 0.510(6) 1 d PD A 1 H21A H 0.8367 0.2511 0.3043 0.080 Uiso 0.510(6) 1 calc PR A 1 H21B H 0.9118 0.2923 0.2349 0.080 Uiso 0.510(6) 1 calc PR A 1 C22A C 0.7267(8) 0.3463(6) 0.2403(7) 0.050(2) Uiso 0.510(6) 1 d PD A 1 H22A H 0.6793 0.3111 0.1973 0.080 Uiso 0.510(6) 1 calc PR A 1 H22B H 0.7472 0.3976 0.2147 0.080 Uiso 0.510(6) 1 calc PR A 1 H22C H 0.6722 0.3566 0.2843 0.080 Uiso 0.510(6) 1 calc PR A 1 C23A C 0.9930(8) 0.4271(4) 0.3069(5) 0.0478(11) Uiso 0.510(6) 1 d PD A 1 H23A H 1.0168 0.4074 0.2530 0.080 Uiso 0.510(6) 1 calc PR A 1 H23B H 0.9193 0.4653 0.2929 0.080 Uiso 0.510(6) 1 calc PR A 1 C24A C 1.1022(9) 0.4729(6) 0.3472(7) 0.058(3) Uiso 0.510(6) 1 d PD A 1 H24A H 1.1230 0.5162 0.3096 0.080 Uiso 0.510(6) 1 calc PR A 1 H24B H 1.1783 0.4373 0.3603 0.080 Uiso 0.510(6) 1 calc PR A 1 H24C H 1.0800 0.4966 0.3992 0.080 Uiso 0.510(6) 1 calc PR A 1 C25A C 1.0516(5) 0.3014(4) 0.3952(4) 0.0406(16) Uiso 0.510(6) 1 d PD A 1 H25A H 1.0917 0.3299 0.4465 0.080 Uiso 0.510(6) 1 calc PR A 1 H25B H 1.0108 0.2515 0.4134 0.080 Uiso 0.510(6) 1 calc PR A 1 C26A C 1.1608(8) 0.2767(5) 0.3463(5) 0.0407(17) Uiso 0.510(6) 1 d PD A 1 H26A H 1.2239 0.2427 0.3817 0.080 Uiso 0.510(6) 1 calc PR A 1 H26B H 1.2051 0.3251 0.3294 0.080 Uiso 0.510(6) 1 calc PR A 1 H26C H 1.1238 0.2463 0.2962 0.080 Uiso 0.510(6) 1 calc PR A 1 C27A C 0.8533(7) 0.3800(4) 0.4165(4) 0.054(2) Uiso 0.510(6) 1 d PD A 1 H27A H 0.7611 0.3870 0.3906 0.080 Uiso 0.510(6) 1 calc PR A 1 H27B H 0.8845 0.4305 0.4456 0.080 Uiso 0.510(6) 1 calc PR A 1 C28A C 0.8702(10) 0.2987(5) 0.4842(6) 0.062(2) Uiso 0.510(6) 1 d PD A 1 H28A H 0.8180 0.3079 0.5296 0.080 Uiso 0.510(6) 1 calc PR A 1 H28B H 0.9625 0.2924 0.5078 0.080 Uiso 0.510(6) 1 calc PR A 1 H28C H 0.8396 0.2495 0.4535 0.080 Uiso 0.510(6) 1 calc PR A 1 N1B N 0.9108(6) 0.3568(4) 0.3458(4) 0.0286(17) Uiso 0.490(6) 1 d PD A 2 C21B C 0.7614(6) 0.3537(5) 0.3100(4) 0.051(2) Uiso 0.490(6) 1 d PD A 2 H21C H 0.7223 0.3056 0.3334 0.080 Uiso 0.490(6) 1 calc PR A 2 H21D H 0.7182 0.4021 0.3297 0.080 Uiso 0.490(6) 1 calc PR A 2 C22B C 0.7321(8) 0.3501(5) 0.2146(5) 0.0373(19) Uiso 0.490(6) 1 d PD A 2 H22D H 0.6371 0.3480 0.1974 0.080 Uiso 0.490(6) 1 calc PR A 2 H22E H 0.7726 0.3018 0.1943 0.080 Uiso 0.490(6) 1 calc PR A 2 H22F H 0.7676 0.3984 0.1906 0.080 Uiso 0.490(6) 1 calc PR A 2 C23B C 0.9734(8) 0.4334(4) 0.3111(5) 0.0478(11) Uiso 0.490(6) 1 d PD A 2 H23C H 0.9017 0.4720 0.2926 0.080 Uiso 0.490(6) 1 calc PR A 2 H23D H 1.0109 0.4169 0.2604 0.080 Uiso 0.490(6) 1 calc PR A 2 C24B C 1.0823(7) 0.4805(5) 0.3696(5) 0.0321(16) Uiso 0.490(6) 1 d PD A 2 H24D H 1.1113 0.5270 0.3393 0.080 Uiso 0.490(6) 1 calc PR A 2 H24E H 1.1568 0.4445 0.3867 0.080 Uiso 0.490(6) 1 calc PR A 2 H24F H 1.0470 0.4994 0.4196 0.080 Uiso 0.490(6) 1 calc PR A 2 C25B C 0.9779(6) 0.2805(4) 0.3170(4) 0.0382(16) Uiso 0.490(6) 1 d PD A 2 H25C H 0.9235 0.2334 0.3277 0.080 Uiso 0.490(6) 1 calc PR A 2 H25D H 0.9762 0.2844 0.2555 0.080 Uiso 0.490(6) 1 calc PR A 2 C26B C 1.1188(7) 0.2621(5) 0.3559(5) 0.0400(17) Uiso 0.490(6) 1 d PD A 2 H26D H 1.1480 0.2121 0.3317 0.080 Uiso 0.490(6) 1 calc PR A 2 H26E H 1.1229 0.2558 0.4167 0.080 Uiso 0.490(6) 1 calc PR A 2 H26F H 1.1759 0.3068 0.3440 0.080 Uiso 0.490(6) 1 calc PR A 2 C27B C 0.9225(7) 0.3621(5) 0.4428(4) 0.053(2) Uiso 0.490(6) 1 d PD A 2 H27C H 0.9260 0.4187 0.4629 0.080 Uiso 0.490(6) 1 calc PR A 2 H27D H 0.9993 0.3319 0.4710 0.080 Uiso 0.490(6) 1 calc PR A 2 C28B C 0.7864(9) 0.3186(6) 0.4547(6) 0.062(2) Uiso 0.490(6) 1 d PD A 2 H28D H 0.7778 0.3166 0.5146 0.080 Uiso 0.490(6) 1 calc PR A 2 H28E H 0.7855 0.2635 0.4323 0.080 Uiso 0.490(6) 1 calc PR A 2 H28F H 0.7132 0.3494 0.4246 0.080 Uiso 0.490(6) 1 calc PR A 2 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 0.0223(2) 0.0349(2) 0.0273(2) 0.00858(16) -0.00046(15) -0.00480(16) S1 0.0279(3) 0.0375(4) 0.0290(4) 0.0046(3) 0.0003(3) -0.0058(3) S2 0.0232(3) 0.0468(5) 0.0271(4) 0.0076(3) -0.0013(3) -0.0070(3) S3 0.0297(4) 0.0377(4) 0.0416(4) 0.0117(3) -0.0102(3) -0.0075(3) C1 0.0244(12) 0.0220(13) 0.0279(13) 0.0008(10) -0.0001(10) 0.0004(10) C2 0.0236(13) 0.0282(14) 0.0352(15) -0.0030(11) 0.0015(11) -0.0061(11) C3 0.0291(14) 0.0317(15) 0.0331(15) -0.0083(12) -0.0021(12) -0.0033(12) C4 0.0284(14) 0.0353(15) 0.0292(14) -0.0055(12) 0.0031(11) 0.0004(12) C5 0.0228(13) 0.0310(15) 0.0330(15) -0.0018(12) 0.0024(11) -0.0006(11) C6 0.0220(12) 0.0274(14) 0.0310(14) 0.0002(11) -0.0015(10) -0.0020(10) C7 0.0396(18) 0.064(2) 0.0367(18) -0.0129(16) -0.0047(14) -0.0157(17) C8 0.0290(15) 0.060(2) 0.0356(16) 0.0028(15) 0.0062(13) -0.0094(14) C9 0.0291(14) 0.0407(17) 0.0266(14) 0.0079(12) 0.0021(11) -0.0034(12) C10 0.0275(14) 0.0505(19) 0.0321(15) -0.0014(14) 0.0024(12) 0.0025(13) C11 0.0377(16) 0.0484(19) 0.0319(16) -0.0052(14) 0.0038(13) 0.0117(14) C12 0.0427(17) 0.0398(17) 0.0283(15) -0.0013(13) 0.0040(13) 0.0053(14) C13 0.0346(15) 0.0402(17) 0.0281(15) 0.0045(12) 0.0022(12) -0.0032(13) C14 0.0301(14) 0.0371(16) 0.0329(15) 0.0121(13) -0.0014(12) -0.0022(12) C15 0.051(2) 0.062(3) 0.061(3) -0.016(2) -0.0073(19) 0.025(2) C16 0.0400(18) 0.0406(19) 0.052(2) 0.0022(16) -0.0042(15) -0.0081(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 S1 2.2017(9) 3_666 ? Fe1 S1 2.2024(9) . ? Fe1 S3 2.2999(8) . ? Fe1 S2 2.3273(8) . ? Fe1 Fe1 2.6999(8) 3_666 ? S1 Fe1 2.2017(9) 3_666 ? S2 C1 1.764(3) . ? S3 C9 1.775(3) . ? C1 C6 1.396(4) . ? C1 C2 1.401(4) . ? C2 C3 1.387(4) . ? C3 C4 1.395(4) . ? C3 C7 1.510(4) . ? C4 C5 1.394(4) . ? C5 C6 1.383(4) . ? C5 C8 1.509(4) . ? C9 C14 1.397(4) . ? C9 C10 1.399(4) . ? C10 C11 1.387(5) . ? C11 C12 1.396(5) . ? C11 C15 1.509(5) . ? C12 C13 1.397(5) . ? C13 C14 1.391(5) . ? C13 C16 1.512(4) . ? N1A C23A 1.477(7) . ? N1A C25A 1.514(7) . ? N1A C27A 1.518(7) . ? N1A C21A 1.543(7) . ? C21A C22A 1.550(8) . ? C23A C24A 1.405(8) . ? C25A C26A 1.488(7) . ? C27A C28A 1.689(8) . ? N1B C25B 1.511(7) . ? N1B C27B 1.520(7) . ? N1B C23B 1.529(7) . ? N1B C21B 1.536(7) . ? C21B C22B 1.492(8) . ? C23B C24B 1.536(8) . ? C25B C26B 1.498(7) . ? C27B C28B 1.580(8) . ? 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 S1 Fe1 S1 104.38(3) 3_666 . ? S1 Fe1 S3 115.46(4) 3_666 . ? S1 Fe1 S3 106.13(3) . . ? S1 Fe1 S2 104.89(3) 3_666 . ? S1 Fe1 S2 115.68(4) . . ? S3 Fe1 S2 110.47(3) . . ? S1 Fe1 Fe1 52.20(2) 3_666 3_666 ? S1 Fe1 Fe1 52.18(2) . 3_666 ? S3 Fe1 Fe1 125.25(3) . 3_666 ? S2 Fe1 Fe1 124.27(3) . 3_666 ? Fe1 S1 Fe1 75.62(3) 3_666 . ? C1 S2 Fe1 113.04(9) . . ? C9 S3 Fe1 109.95(10) . . ? C6 C1 C2 118.0(3) . . ? C6 C1 S2 118.0(2) . . ? C2 C1 S2 124.0(2) . . ? C3 C2 C1 120.7(3) . . ? C2 C3 C4 120.0(3) . . ? C2 C3 C7 120.4(3) . . ? C4 C3 C7 119.7(3) . . ? C5 C4 C3 120.4(3) . . ? C6 C5 C4 118.8(3) . . ? C6 C5 C8 121.1(3) . . ? C4 C5 C8 120.2(3) . . ? C5 C6 C1 122.2(3) . . ? C14 C9 C10 118.1(3) . . ? C14 C9 S3 123.7(2) . . ? C10 C9 S3 118.2(2) . . ? C11 C10 C9 122.0(3) . . ? C10 C11 C12 118.9(3) . . ? C10 C11 C15 120.4(3) . . ? C12 C11 C15 120.7(3) . . ? C11 C12 C13 120.5(3) . . ? C14 C13 C12 119.5(3) . . ? C14 C13 C16 120.4(3) . . ? C12 C13 C16 120.1(3) . . ? C13 C14 C9 121.1(3) . . ? C23A N1A C25A 112.7(5) . . ? C23A N1A C27A 113.2(5) . . ? C25A N1A C27A 107.0(4) . . ? C23A N1A C21A 106.9(4) . . ? C25A N1A C21A 108.0(4) . . ? C27A N1A C21A 108.9(5) . . ? N1A C21A C22A 113.2(6) . . ? C24A C23A N1A 120.8(7) . . ? C26A C25A N1A 117.6(5) . . ? N1A C27A C28A 102.5(5) . . ? C25B N1B C27B 111.9(5) . . ? C25B N1B C23B 109.3(5) . . ? C27B N1B C23B 109.7(5) . . ? C25B N1B C21B 108.8(5) . . ? C27B N1B C21B 107.7(5) . . ? C23B N1B C21B 109.3(5) . . ? C22B C21B N1B 114.6(5) . . ? N1B C23B C24B 119.1(6) . . ? C26B C25B N1B 118.8(5) . . ? N1B C27B C28B 98.6(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.96 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.295 _refine_diff_density_min -0.745 _refine_diff_density_rms 0.078 data_4e-ab43 _database_code_depnum_ccdc_archive 'CCDC 717461' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H36 Fe2 S6 2-, 2(C8 H20 N +)' _chemical_formula_sum 'C48 H76 Fe2 N2 S6' _chemical_formula_weight 985.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.8954(4) _cell_length_b 18.6951(5) _cell_length_c 16.3160(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.047(2) _cell_angle_gamma 90.00 _cell_volume 5094.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 52595 _cell_measurement_theta_min 1.63 _cell_measurement_theta_max 26.79 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.284 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 0.849 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5792 _exptl_absorpt_correction_T_max 0.7259 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52595 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0218 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 26.79 _reflns_number_total 10631 _reflns_number_gt 9649 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+2.4065P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10631 _refine_ls_number_parameters 571 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0318 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0721 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.548993(12) 0.549586(10) 0.986825(13) 0.01554(5) Uani 1 1 d . . . S1 S 0.43227(2) 0.513070(18) 0.89358(2) 0.01836(8) Uani 1 1 d . . . S2 S 0.63970(2) 0.53347(2) 0.91681(2) 0.02346(8) Uani 1 1 d . . . S3 S 0.54456(2) 0.666952(18) 1.02925(2) 0.01949(8) Uani 1 1 d . . . C1 C 0.73915(9) 0.54788(7) 0.98917(10) 0.0190(3) Uani 1 1 d . . . C2 C 0.80295(9) 0.53110(8) 0.96065(10) 0.0224(3) Uani 1 1 d . . . C3 C 0.88125(10) 0.53797(8) 1.02008(11) 0.0250(3) Uani 1 1 d . . . H3 H 0.9230 0.5266 1.0011 0.080 Uiso 1 1 calc R . . C4 C 0.90004(9) 0.56092(8) 1.10607(11) 0.0241(3) Uani 1 1 d . . . C5 C 0.83644(10) 0.58062(9) 1.13157(11) 0.0269(3) Uani 1 1 d . . . H5 H 0.8469 0.5984 1.1878 0.080 Uiso 1 1 calc R . . C6 C 0.75771(9) 0.57410(8) 1.07416(10) 0.0235(3) Uani 1 1 d . . . H6 H 0.7164 0.5876 1.0929 0.080 Uiso 1 1 calc R . . C7 C 0.78740(11) 0.50467(11) 0.86885(12) 0.0343(4) Uani 1 1 d . . . H7A H 0.8372 0.5011 0.8593 0.080 Uiso 1 1 calc R . . H7B H 0.7527 0.5376 0.8273 0.080 Uiso 1 1 calc R . . H7C H 0.7624 0.4585 0.8614 0.080 Uiso 1 1 calc R . . C8 C 0.98499(10) 0.56350(10) 1.17059(12) 0.0330(4) Uani 1 1 d . . . H8A H 1.0194 0.5385 1.1467 0.080 Uiso 1 1 calc R . . H8B H 0.9877 0.5413 1.2246 0.080 Uiso 1 1 calc R . . H8C H 1.0020 0.6124 1.1815 0.080 Uiso 1 1 calc R . . C9 C 0.51841(8) 0.72179(7) 0.93485(9) 0.0169(3) Uani 1 1 d . . . C10 C 0.50329(9) 0.79507(7) 0.94304(10) 0.0192(3) Uani 1 1 d . . . C11 C 0.48387(9) 0.83868(8) 0.86898(10) 0.0226(3) Uani 1 1 d . . . H11 H 0.4740 0.8869 0.8748 0.080 Uiso 1 1 calc R . . C12 C 0.47857(9) 0.81359(8) 0.78683(10) 0.0225(3) Uani 1 1 d . . . C13 C 0.49302(9) 0.74116(8) 0.77998(10) 0.0226(3) Uani 1 1 d . . . H13 H 0.4897 0.7225 0.7259 0.080 Uiso 1 1 calc R . . C14 C 0.51234(9) 0.69617(8) 0.85227(10) 0.0213(3) Uani 1 1 d . . . H14 H 0.5214 0.6479 0.8456 0.080 Uiso 1 1 calc R . . C15 C 0.50702(11) 0.82621(8) 1.02925(11) 0.0276(3) Uani 1 1 d . . . H15A H 0.4891 0.8750 1.0208 0.080 Uiso 1 1 calc R . . H15B H 0.5612 0.8245 1.0702 0.080 Uiso 1 1 calc R . . H15C H 0.4732 0.7991 1.0519 0.080 Uiso 1 1 calc R . . C16 C 0.45902(12) 0.86285(9) 0.70890(12) 0.0351(4) Uani 1 1 d . . . H16A H 0.4153 0.8935 0.7069 0.080 Uiso 1 1 calc R . . H16B H 0.4442 0.8350 0.6560 0.080 Uiso 1 1 calc R . . H16C H 0.5051 0.8915 0.7142 0.080 Uiso 1 1 calc R . . Fe2 Fe 0.059193(12) 0.540107(11) 0.490158(13) 0.01731(6) Uani 1 1 d . . . S11 S -0.06188(2) 0.52304(2) 0.39465(2) 0.02049(8) Uani 1 1 d . . . S12 S 0.14587(2) 0.49897(2) 0.42432(2) 0.02172(8) Uani 1 1 d . . . S13 S 0.09017(2) 0.65713(2) 0.53740(3) 0.02534(9) Uani 1 1 d . . . C21 C 0.24536(9) 0.50865(7) 0.49923(9) 0.0175(3) Uani 1 1 d . . . C22 C 0.30931(9) 0.49499(7) 0.47045(10) 0.0184(3) Uani 1 1 d . . . C23 C 0.38758(9) 0.50397(7) 0.52939(10) 0.0202(3) Uani 1 1 d . . . H23 H 0.4296 0.4942 0.5102 0.080 Uiso 1 1 calc R . . C24 C 0.40575(9) 0.52673(7) 0.61543(10) 0.0189(3) Uani 1 1 d . . . C25 C 0.34182(9) 0.53925(8) 0.64304(10) 0.0229(3) Uani 1 1 d . . . H25 H 0.3518 0.5541 0.7004 0.080 Uiso 1 1 calc R . . C26 C 0.26330(9) 0.52988(8) 0.58610(10) 0.0232(3) Uani 1 1 d . . . H26 H 0.2217 0.5380 0.6064 0.080 Uiso 1 1 calc R . . C27 C 0.29410(10) 0.47359(9) 0.37695(11) 0.0286(3) Uani 1 1 d . . . H27A H 0.2696 0.5127 0.3386 0.080 Uiso 1 1 calc R . . H27B H 0.2590 0.4329 0.3619 0.080 Uiso 1 1 calc R . . H27C H 0.3439 0.4615 0.3707 0.080 Uiso 1 1 calc R . . C28 C 0.49057(9) 0.53934(8) 0.67713(11) 0.0239(3) Uani 1 1 d . . . H28A H 0.5269 0.5144 0.6559 0.080 Uiso 1 1 calc R . . H28B H 0.4967 0.5220 0.7346 0.080 Uiso 1 1 calc R . . H28C H 0.5021 0.5896 0.6802 0.080 Uiso 1 1 calc R . . C29 C 0.04960(9) 0.71777(8) 0.44911(10) 0.0212(3) Uani 1 1 d . . . C30 C 0.04933(9) 0.79147(8) 0.46708(11) 0.0232(3) Uani 1 1 d . . . C31 C 0.01545(11) 0.83860(9) 0.39753(12) 0.0310(4) Uani 1 1 d . . . H31 H 0.0158 0.8872 0.4097 0.080 Uiso 1 1 calc R . . C32 C -0.01885(11) 0.81647(9) 0.31081(12) 0.0342(4) Uani 1 1 d . . . C33 C -0.01729(11) 0.74373(9) 0.29419(11) 0.0311(4) Uani 1 1 d . . . H33 H -0.0393 0.7272 0.2367 0.080 Uiso 1 1 calc R . . C34 C 0.01656(10) 0.69535(8) 0.36173(11) 0.0257(3) Uani 1 1 d . . . H34 H 0.0173 0.6470 0.3486 0.080 Uiso 1 1 calc R . . C35 C 0.08377(11) 0.81992(9) 0.55931(12) 0.0313(4) Uani 1 1 d . . . H35A H 0.0785 0.8710 0.5584 0.080 Uiso 1 1 calc R . . H35B H 0.1394 0.8073 0.5847 0.080 Uiso 1 1 calc R . . H35C H 0.0555 0.7996 0.5938 0.080 Uiso 1 1 calc R . . C36 C -0.05545(17) 0.86947(11) 0.23736(15) 0.0574(7) Uani 1 1 d . . . H36A H -0.0745 0.9104 0.2597 0.080 Uiso 1 1 calc R . . H36B H -0.0994 0.8474 0.1918 0.080 Uiso 1 1 calc R . . H36C H -0.0158 0.8844 0.2140 0.080 Uiso 1 1 calc R . . N1A N 0.25524(18) 0.69899(15) 0.8539(2) 0.0217(5) Uani 0.828(7) 1 d PD A 1 C41A C 0.31352(19) 0.70687(17) 0.8061(2) 0.0299(6) Uani 0.828(7) 1 d PD A 1 H41A H 0.3577 0.7367 0.8415 0.080 Uiso 0.828(7) 1 calc PR A 1 H41B H 0.3352 0.6600 0.8019 0.080 Uiso 0.828(7) 1 calc PR A 1 C42A C 0.27944(19) 0.7385(2) 0.7152(2) 0.0507(9) Uani 0.828(7) 1 d PD A 1 H42A H 0.2349 0.7102 0.6796 0.080 Uiso 0.828(7) 1 calc PR A 1 H42B H 0.3199 0.7390 0.6893 0.080 Uiso 0.828(7) 1 calc PR A 1 H42C H 0.2619 0.7866 0.7187 0.080 Uiso 0.828(7) 1 calc PR A 1 C43A C 0.18572(15) 0.65127(17) 0.80179(18) 0.0278(6) Uani 0.828(7) 1 d PD A 1 H43A H 0.1493 0.6472 0.8335 0.080 Uiso 0.828(7) 1 calc PR A 1 H43B H 0.1569 0.6741 0.7460 0.080 Uiso 0.828(7) 1 calc PR A 1 C44A C 0.2094(2) 0.57770(19) 0.7844(2) 0.0494(8) Uani 0.828(7) 1 d PD A 1 H44A H 0.2425 0.5808 0.7496 0.080 Uiso 0.828(7) 1 calc PR A 1 H44B H 0.1622 0.5504 0.7534 0.080 Uiso 0.828(7) 1 calc PR A 1 H44C H 0.2386 0.5546 0.8392 0.080 Uiso 0.828(7) 1 calc PR A 1 C45A C 0.3029(4) 0.6659(5) 0.9421(4) 0.0296(6) Uani 0.828(7) 1 d PD A 1 H45A H 0.3243 0.6204 0.9321 0.080 Uiso 0.828(7) 1 calc PR A 1 H45B H 0.3480 0.6968 0.9722 0.080 Uiso 0.828(7) 1 calc PR A 1 C46A C 0.2560(6) 0.6537(7) 1.0016(6) 0.0461(13) Uani 0.828(7) 1 d PD A 1 H46A H 0.2366 0.6986 1.0143 0.080 Uiso 0.828(7) 1 calc PR A 1 H46B H 0.2901 0.6320 1.0553 0.080 Uiso 0.828(7) 1 calc PR A 1 H46C H 0.2115 0.6227 0.9729 0.080 Uiso 0.828(7) 1 calc PR A 1 C47A C 0.21815(18) 0.76992(15) 0.8641(3) 0.0483(9) Uani 0.828(7) 1 d PD A 1 H47A H 0.1889 0.7889 0.8061 0.080 Uiso 0.828(7) 1 calc PR A 1 H47B H 0.1797 0.7611 0.8924 0.080 Uiso 0.828(7) 1 calc PR A 1 C48A C 0.2768(3) 0.82626(17) 0.9164(4) 0.0856(17) Uani 0.828(7) 1 d PD A 1 H48A H 0.3050 0.8088 0.9747 0.080 Uiso 0.828(7) 1 calc PR A 1 H48B H 0.2482 0.8690 0.9193 0.080 Uiso 0.828(7) 1 calc PR A 1 H48C H 0.3144 0.8366 0.8882 0.080 Uiso 0.828(7) 1 calc PR A 1 N1B N 0.2509(10) 0.7098(8) 0.8652(11) 0.0217(5) Uani 0.172(7) 1 d PD A 2 C41B C 0.3045(10) 0.7245(9) 0.8133(11) 0.0299(6) Uani 0.172(7) 1 d PD A 2 H41C H 0.3213 0.6792 0.7964 0.080 Uiso 0.172(7) 1 calc PR A 2 H41D H 0.3522 0.7493 0.8508 0.080 Uiso 0.172(7) 1 calc PR A 2 C42B C 0.2644(10) 0.7689(10) 0.7313(11) 0.0507(9) Uani 0.172(7) 1 d PD A 2 H42D H 0.2226 0.7414 0.6896 0.080 Uiso 0.172(7) 1 calc PR A 2 H42E H 0.3033 0.7822 0.7060 0.080 Uiso 0.172(7) 1 calc PR A 2 H42F H 0.2419 0.8112 0.7465 0.080 Uiso 0.172(7) 1 calc PR A 2 C43B C 0.1728(8) 0.6721(8) 0.8106(11) 0.0278(6) Uani 0.172(7) 1 d PD A 2 H43C H 0.1406 0.6661 0.8468 0.080 Uiso 0.172(7) 1 calc PR A 2 H43D H 0.1433 0.7030 0.7619 0.080 Uiso 0.172(7) 1 calc PR A 2 C44B C 0.1829(11) 0.6014(9) 0.7751(12) 0.0494(8) Uani 0.172(7) 1 d PD A 2 H44D H 0.2193 0.6057 0.7440 0.080 Uiso 0.172(7) 1 calc PR A 2 H44E H 0.1320 0.5847 0.7356 0.080 Uiso 0.172(7) 1 calc PR A 2 H44F H 0.2041 0.5680 0.8225 0.080 Uiso 0.172(7) 1 calc PR A 2 C45B C 0.303(2) 0.661(2) 0.940(2) 0.0296(6) Uani 0.172(7) 1 d PD A 2 H45C H 0.3107 0.6162 0.9149 0.080 Uiso 0.172(7) 1 calc PR A 2 H45D H 0.3546 0.6836 0.9674 0.080 Uiso 0.172(7) 1 calc PR A 2 C46B C 0.267(3) 0.646(4) 1.009(3) 0.0461(13) Uani 0.172(7) 1 d PD A 2 H46D H 0.2591 0.6908 1.0347 0.080 Uiso 0.172(7) 1 calc PR A 2 H46E H 0.3037 0.6170 1.0545 0.080 Uiso 0.172(7) 1 calc PR A 2 H46F H 0.2172 0.6221 0.9835 0.080 Uiso 0.172(7) 1 calc PR A 2 C47B C 0.2329(9) 0.7776(8) 0.9045(14) 0.0483(9) Uani 0.172(7) 1 d PD A 2 H47C H 0.1981 0.7665 0.9366 0.080 Uiso 0.172(7) 1 calc PR A 2 H47D H 0.2045 0.8103 0.8575 0.080 Uiso 0.172(7) 1 calc PR A 2 C48B C 0.3083(12) 0.8142(10) 0.9661(19) 0.0856(17) Uani 0.172(7) 1 d PD A 2 H48D H 0.3427 0.7792 1.0045 0.080 Uiso 0.172(7) 1 calc PR A 2 H48E H 0.2938 0.8495 1.0004 0.080 Uiso 0.172(7) 1 calc PR A 2 H48F H 0.3358 0.8368 0.9323 0.080 Uiso 0.172(7) 1 calc PR A 2 N2 N 0.75753(8) 0.71798(6) 0.40094(8) 0.0202(3) Uani 1 1 d . . . C51 C 0.83789(10) 0.68537(9) 0.45569(11) 0.0282(3) Uani 1 1 d . . . H51A H 0.8284 0.6438 0.4861 0.080 Uiso 1 1 calc R . . H51B H 0.8643 0.6691 0.4165 0.080 Uiso 1 1 calc R . . C52 C 0.89358(10) 0.73576(11) 0.52267(13) 0.0384(4) Uani 1 1 d . . . H52A H 0.9017 0.7781 0.4936 0.080 Uiso 1 1 calc R . . H52B H 0.9441 0.7126 0.5516 0.080 Uiso 1 1 calc R . . H52C H 0.8703 0.7486 0.5652 0.080 Uiso 1 1 calc R . . C53 C 0.77112(11) 0.77399(9) 0.34049(12) 0.0301(4) Uani 1 1 d . . . H53A H 0.8015 0.7524 0.3082 0.080 Uiso 1 1 calc R . . H53B H 0.8036 0.8121 0.3762 0.080 Uiso 1 1 calc R . . C54 C 0.69554(13) 0.80676(10) 0.27500(13) 0.0397(4) Uani 1 1 d . . . H54A H 0.6627 0.7697 0.2390 0.080 Uiso 1 1 calc R . . H54B H 0.7097 0.8404 0.2385 0.080 Uiso 1 1 calc R . . H54C H 0.6664 0.8309 0.3060 0.080 Uiso 1 1 calc R . . C55 C 0.70181(10) 0.65927(8) 0.34902(11) 0.0264(3) Uani 1 1 d . . . H55A H 0.6985 0.6226 0.3897 0.080 Uiso 1 1 calc R . . H55B H 0.6486 0.6793 0.3214 0.080 Uiso 1 1 calc R . . C56 C 0.72637(13) 0.62432(10) 0.27878(12) 0.0376(4) Uani 1 1 d . . . H56A H 0.7280 0.6597 0.2368 0.080 Uiso 1 1 calc R . . H56B H 0.6882 0.5879 0.2496 0.080 Uiso 1 1 calc R . . H56C H 0.7784 0.6032 0.3054 0.080 Uiso 1 1 calc R . . C57 C 0.71960(10) 0.75418(8) 0.45974(11) 0.0241(3) Uani 1 1 d . . . H57A H 0.7516 0.7956 0.4868 0.080 Uiso 1 1 calc R . . H57B H 0.6668 0.7712 0.4235 0.080 Uiso 1 1 calc R . . C58 C 0.71143(10) 0.70690(9) 0.53141(11) 0.0293(3) Uani 1 1 d . . . H58A H 0.6790 0.6661 0.5054 0.080 Uiso 1 1 calc R . . H58B H 0.6866 0.7335 0.5651 0.080 Uiso 1 1 calc R . . H58C H 0.7635 0.6912 0.5691 0.080 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 0.01626(10) 0.01446(10) 0.01453(10) 0.00082(7) 0.00388(8) -0.00036(7) S1 0.01881(17) 0.01864(16) 0.01431(16) 0.00187(12) 0.00193(13) -0.00027(12) S2 0.02047(18) 0.0321(2) 0.01745(18) -0.00392(14) 0.00633(14) 0.00136(14) S3 0.02744(19) 0.01548(16) 0.01504(17) 0.00040(12) 0.00701(14) -0.00014(13) C1 0.0211(7) 0.0173(6) 0.0188(7) 0.0024(5) 0.0075(6) 0.0016(5) C2 0.0246(8) 0.0241(7) 0.0203(8) 0.0008(6) 0.0104(6) 0.0021(6) C3 0.0238(8) 0.0274(8) 0.0275(8) 0.0015(6) 0.0139(7) 0.0023(6) C4 0.0214(7) 0.0259(7) 0.0250(8) 0.0022(6) 0.0084(6) -0.0014(6) C5 0.0250(8) 0.0357(8) 0.0205(8) -0.0043(6) 0.0089(6) -0.0025(6) C6 0.0216(7) 0.0292(8) 0.0217(8) -0.0014(6) 0.0100(6) 0.0003(6) C7 0.0317(9) 0.0498(11) 0.0250(9) -0.0067(7) 0.0147(7) 0.0045(8) C8 0.0218(8) 0.0453(10) 0.0306(9) -0.0006(7) 0.0077(7) -0.0020(7) C9 0.0165(6) 0.0173(6) 0.0159(7) 0.0002(5) 0.0046(5) -0.0014(5) C10 0.0200(7) 0.0183(6) 0.0186(7) -0.0011(5) 0.0061(6) 0.0001(5) C11 0.0268(8) 0.0166(6) 0.0231(8) 0.0014(6) 0.0075(6) 0.0011(5) C12 0.0242(7) 0.0224(7) 0.0203(7) 0.0044(6) 0.0071(6) -0.0007(6) C13 0.0269(8) 0.0241(7) 0.0160(7) -0.0008(6) 0.0069(6) -0.0004(6) C14 0.0267(8) 0.0170(6) 0.0194(7) -0.0009(5) 0.0071(6) 0.0006(5) C15 0.0388(9) 0.0210(7) 0.0238(8) -0.0022(6) 0.0122(7) 0.0061(6) C16 0.0530(11) 0.0278(8) 0.0247(9) 0.0081(7) 0.0139(8) 0.0043(7) Fe2 0.01413(10) 0.01947(10) 0.01531(10) -0.00071(7) 0.00163(8) 0.00073(7) S11 0.01623(17) 0.02500(18) 0.01584(17) 0.00129(13) 0.00041(13) 0.00012(13) S12 0.01814(17) 0.02849(19) 0.01636(17) -0.00525(14) 0.00358(14) -0.00049(13) S13 0.0288(2) 0.02058(17) 0.01878(18) -0.00251(14) -0.00094(15) 0.00171(14) C21 0.0182(7) 0.0164(6) 0.0161(7) 0.0007(5) 0.0042(5) 0.0002(5) C22 0.0225(7) 0.0165(6) 0.0172(7) -0.0009(5) 0.0082(6) -0.0002(5) C23 0.0200(7) 0.0202(7) 0.0225(7) 0.0003(5) 0.0100(6) 0.0000(5) C24 0.0181(7) 0.0172(6) 0.0192(7) 0.0030(5) 0.0039(6) 0.0004(5) C25 0.0211(7) 0.0303(8) 0.0152(7) -0.0023(6) 0.0038(6) 0.0021(6) C26 0.0186(7) 0.0327(8) 0.0182(7) -0.0026(6) 0.0066(6) 0.0027(6) C27 0.0286(8) 0.0390(9) 0.0207(8) -0.0078(7) 0.0118(7) -0.0031(7) C28 0.0189(7) 0.0267(7) 0.0227(8) 0.0012(6) 0.0035(6) -0.0006(6) C29 0.0170(7) 0.0219(7) 0.0228(8) -0.0001(6) 0.0050(6) -0.0004(5) C30 0.0201(7) 0.0230(7) 0.0265(8) -0.0021(6) 0.0083(6) -0.0015(5) C31 0.0351(9) 0.0205(7) 0.0365(10) 0.0015(6) 0.0120(8) 0.0008(6) C32 0.0384(10) 0.0277(8) 0.0310(9) 0.0063(7) 0.0059(8) 0.0011(7) C33 0.0341(9) 0.0310(8) 0.0225(8) 0.0017(6) 0.0031(7) -0.0025(7) C34 0.0289(8) 0.0225(7) 0.0228(8) -0.0007(6) 0.0058(6) -0.0015(6) C35 0.0357(9) 0.0248(8) 0.0314(9) -0.0077(7) 0.0099(7) -0.0037(7) C36 0.0850(18) 0.0314(10) 0.0390(12) 0.0112(9) 0.0019(12) 0.0046(10) N1A 0.0154(7) 0.0189(11) 0.0286(12) -0.0031(7) 0.0052(7) 0.0022(7) C41A 0.0210(11) 0.0354(17) 0.0310(11) 0.0005(11) 0.0066(8) -0.0048(10) C42A 0.0349(14) 0.070(2) 0.0389(15) 0.0167(15) 0.0030(11) -0.0164(15) C43A 0.0180(11) 0.0358(17) 0.0263(10) -0.0027(11) 0.0041(8) -0.0062(10) C44A 0.0474(19) 0.0408(18) 0.0524(16) -0.0255(14) 0.0085(15) -0.0144(13) C45A 0.0248(8) 0.0375(15) 0.0217(9) -0.0049(9) 0.0025(7) 0.0050(8) C46A 0.039(4) 0.070(4) 0.030(2) -0.0027(14) 0.012(2) -0.005(2) C47A 0.0329(14) 0.0251(11) 0.080(3) -0.0122(14) 0.0123(16) 0.0091(10) C48A 0.058(2) 0.0315(15) 0.160(5) -0.043(2) 0.030(3) -0.0009(14) N1B 0.0154(7) 0.0189(11) 0.0286(12) -0.0031(7) 0.0052(7) 0.0022(7) C41B 0.0210(11) 0.0354(17) 0.0310(11) 0.0005(11) 0.0066(8) -0.0048(10) C42B 0.0349(14) 0.070(2) 0.0389(15) 0.0167(15) 0.0030(11) -0.0164(15) C43B 0.0180(11) 0.0358(17) 0.0263(10) -0.0027(11) 0.0041(8) -0.0062(10) C44B 0.0474(19) 0.0408(18) 0.0524(16) -0.0255(14) 0.0085(15) -0.0144(13) C45B 0.0248(8) 0.0375(15) 0.0217(9) -0.0049(9) 0.0025(7) 0.0050(8) C46B 0.039(4) 0.070(4) 0.030(2) -0.0027(14) 0.012(2) -0.005(2) C47B 0.0329(14) 0.0251(11) 0.080(3) -0.0122(14) 0.0123(16) 0.0091(10) C48B 0.058(2) 0.0315(15) 0.160(5) -0.043(2) 0.030(3) -0.0009(14) N2 0.0224(6) 0.0189(6) 0.0220(6) 0.0019(5) 0.0112(5) 0.0035(5) C51 0.0225(8) 0.0316(8) 0.0314(9) 0.0034(7) 0.0110(7) 0.0087(6) C52 0.0222(8) 0.0539(11) 0.0381(10) -0.0023(9) 0.0096(8) -0.0023(8) C53 0.0373(9) 0.0273(8) 0.0322(9) 0.0072(7) 0.0203(8) 0.0002(7) C54 0.0527(12) 0.0352(9) 0.0360(10) 0.0174(8) 0.0218(9) 0.0101(8) C55 0.0294(8) 0.0238(7) 0.0255(8) -0.0009(6) 0.0091(7) -0.0012(6) C56 0.0521(12) 0.0330(9) 0.0291(9) -0.0061(7) 0.0162(8) 0.0010(8) C57 0.0270(8) 0.0235(7) 0.0263(8) 0.0009(6) 0.0152(7) 0.0069(6) C58 0.0283(8) 0.0378(9) 0.0255(8) 0.0064(7) 0.0141(7) 0.0057(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 S1 2.1959(4) 3_667 ? Fe1 S1 2.2048(4) . ? Fe1 S3 2.3107(4) . ? Fe1 S2 2.3158(4) . ? Fe1 Fe1 2.6905(4) 3_667 ? S1 Fe1 2.1959(4) 3_667 ? S2 C1 1.7677(15) . ? S3 C9 1.7678(14) . ? C1 C6 1.394(2) . ? C1 C2 1.414(2) . ? C2 C3 1.394(2) . ? C2 C7 1.505(2) . ? C3 C4 1.388(2) . ? C4 C5 1.394(2) . ? C4 C8 1.507(2) . ? C5 C6 1.389(2) . ? C9 C14 1.397(2) . ? C9 C10 1.4119(19) . ? C10 C11 1.394(2) . ? C10 C15 1.502(2) . ? C11 C12 1.391(2) . ? C12 C13 1.391(2) . ? C12 C16 1.506(2) . ? C13 C14 1.388(2) . ? Fe2 S11 2.1908(4) . ? Fe2 S11 2.2054(4) 3_566 ? Fe2 S12 2.3125(4) . ? Fe2 S13 2.3196(4) . ? Fe2 Fe2 2.7072(4) 3_566 ? S11 Fe2 2.2054(4) 3_566 ? S12 C21 1.7701(15) . ? S13 C29 1.7711(15) . ? C21 C26 1.394(2) . ? C21 C22 1.408(2) . ? C22 C23 1.395(2) . ? C22 C27 1.504(2) . ? C23 C24 1.389(2) . ? C24 C25 1.392(2) . ? C24 C28 1.508(2) . ? C25 C26 1.389(2) . ? C29 C34 1.397(2) . ? C29 C30 1.409(2) . ? C30 C31 1.392(2) . ? C30 C35 1.504(2) . ? C31 C32 1.388(3) . ? C32 C33 1.389(2) . ? C32 C36 1.511(2) . ? C33 C34 1.386(2) . ? N1A C41A 1.516(3) . ? N1A C45A 1.517(4) . ? N1A C47A 1.519(3) . ? N1A C43A 1.519(3) . ? C41A C42A 1.509(4) . ? C43A C44A 1.496(3) . ? C45A C46A 1.511(5) . ? C47A C48A 1.515(4) . ? N1B C47B 1.505(14) . ? N1B C41B 1.515(15) . ? N1B C45B 1.532(15) . ? N1B C43B 1.533(14) . ? C41B C42B 1.519(15) . ? C43B C44B 1.481(13) . ? C45B C46B 1.508(17) . ? C47B C48B 1.524(15) . ? N2 C53 1.5167(19) . ? N2 C57 1.5188(18) . ? N2 C55 1.520(2) . ? N2 C51 1.5216(19) . ? C51 C52 1.514(2) . ? C53 C54 1.519(3) . ? C55 C56 1.515(2) . ? C57 C58 1.514(2) . ? 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 S1 Fe1 S1 104.624(14) 3_667 . ? S1 Fe1 S3 104.539(15) 3_667 . ? S1 Fe1 S3 112.011(15) . . ? S1 Fe1 S2 117.294(16) 3_667 . ? S1 Fe1 S2 106.115(16) . . ? S3 Fe1 S2 112.140(16) . . ? S1 Fe1 Fe1 52.462(11) 3_667 3_667 ? S1 Fe1 Fe1 52.162(11) . 3_667 ? S3 Fe1 Fe1 120.799(15) . 3_667 ? S2 Fe1 Fe1 126.994(15) . 3_667 ? Fe1 S1 Fe1 75.376(14) 3_667 . ? C1 S2 Fe1 111.51(5) . . ? C9 S3 Fe1 108.45(5) . . ? C6 C1 C2 118.25(14) . . ? C6 C1 S2 122.76(12) . . ? C2 C1 S2 118.98(12) . . ? C3 C2 C1 118.62(14) . . ? C3 C2 C7 120.18(14) . . ? C1 C2 C7 121.18(14) . . ? C4 C3 C2 123.34(14) . . ? C3 C4 C5 117.12(15) . . ? C3 C4 C8 122.23(15) . . ? C5 C4 C8 120.65(15) . . ? C6 C5 C4 120.97(15) . . ? C5 C6 C1 121.56(14) . . ? C14 C9 C10 118.22(13) . . ? C14 C9 S3 123.10(11) . . ? C10 C9 S3 118.68(11) . . ? C11 C10 C9 118.81(13) . . ? C11 C10 C15 119.91(13) . . ? C9 C10 C15 121.28(13) . . ? C12 C11 C10 123.20(13) . . ? C13 C12 C11 117.11(13) . . ? C13 C12 C16 121.41(14) . . ? C11 C12 C16 121.48(14) . . ? C14 C13 C12 121.23(14) . . ? C13 C14 C9 121.43(13) . . ? S11 Fe2 S11 103.979(14) . 3_566 ? S11 Fe2 S12 106.148(16) . . ? S11 Fe2 S12 113.885(16) 3_566 . ? S11 Fe2 S13 115.535(16) . . ? S11 Fe2 S13 106.988(16) 3_566 . ? S12 Fe2 S13 110.356(16) . . ? S11 Fe2 Fe2 52.233(12) . 3_566 ? S11 Fe2 Fe2 51.746(12) 3_566 3_566 ? S12 Fe2 Fe2 123.704(15) . 3_566 ? S13 Fe2 Fe2 125.933(16) . 3_566 ? Fe2 S11 Fe2 76.021(14) . 3_566 ? C21 S12 Fe2 108.75(5) . . ? C29 S13 Fe2 110.75(5) . . ? C26 C21 C22 118.22(13) . . ? C26 C21 S12 122.58(11) . . ? C22 C21 S12 119.20(11) . . ? C23 C22 C21 118.90(13) . . ? C23 C22 C27 120.15(13) . . ? C21 C22 C27 120.91(13) . . ? C24 C23 C22 123.10(13) . . ? C23 C24 C25 117.21(13) . . ? C23 C24 C28 122.45(13) . . ? C25 C24 C28 120.33(14) . . ? C26 C25 C24 120.92(14) . . ? C25 C26 C21 121.61(14) . . ? C34 C29 C30 118.29(14) . . ? C34 C29 S13 122.52(11) . . ? C30 C29 S13 119.19(12) . . ? C31 C30 C29 118.84(15) . . ? C31 C30 C35 119.60(14) . . ? C29 C30 C35 121.56(14) . . ? C32 C31 C30 123.11(15) . . ? C31 C32 C33 117.28(15) . . ? C31 C32 C36 121.35(17) . . ? C33 C32 C36 121.37(17) . . ? C34 C33 C32 121.17(16) . . ? C33 C34 C29 121.31(15) . . ? C41A N1A C45A 105.7(3) . . ? C41A N1A C47A 112.3(2) . . ? C45A N1A C47A 111.8(4) . . ? C41A N1A C43A 110.2(2) . . ? C45A N1A C43A 111.1(4) . . ? C47A N1A C43A 105.8(2) . . ? C42A C41A N1A 115.7(3) . . ? C44A C43A N1A 114.55(19) . . ? C46A C45A N1A 114.7(4) . . ? C48A C47A N1A 115.3(2) . . ? C47B N1B C41B 111.2(13) . . ? C47B N1B C45B 108.6(18) . . ? C41B N1B C45B 103.2(16) . . ? C47B N1B C43B 110.2(12) . . ? C41B N1B C43B 112.7(13) . . ? C45B N1B C43B 110.7(19) . . ? N1B C41B C42B 113.4(13) . . ? C44B C43B N1B 115.1(11) . . ? C46B C45B N1B 114(2) . . ? N1B C47B C48B 112.6(12) . . ? C53 N2 C57 108.39(11) . . ? C53 N2 C55 111.25(13) . . ? C57 N2 C55 108.73(12) . . ? C53 N2 C51 108.66(12) . . ? C57 N2 C51 110.51(12) . . ? C55 N2 C51 109.30(12) . . ? C52 C51 N2 114.38(14) . . ? N2 C53 C54 115.19(14) . . ? C56 C55 N2 115.00(14) . . ? C58 C57 N2 114.63(12) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.79 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.420 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.053 data_4f-ab36 _database_code_depnum_ccdc_archive 'CCDC 717462' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H16 F4 Fe2 S6 2-, 2(C8 H20 N +)' _chemical_formula_sum 'C40 H56 F4 Fe2 N2 S6' _chemical_formula_weight 944.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 8.7961(2) _cell_length_b 15.7706(3) _cell_length_c 16.0927(3) _cell_angle_alpha 86.266(2) _cell_angle_beta 87.872(2) _cell_angle_gamma 80.465(2) _cell_volume 2196.07(8) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 68964 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 26.96 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 0.994 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5999 _exptl_absorpt_correction_T_max 0.9687 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68964 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 26.96 _reflns_number_total 18276 _reflns_number_gt 17248 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.617(6) _refine_ls_number_reflns 18276 _refine_ls_number_parameters 990 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0277 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0593 _refine_ls_wR_factor_gt 0.0587 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.79551(3) 0.352671(18) 0.329117(17) 0.01651(6) Uani 1 1 d . . . Fe2 Fe 0.80693(3) 0.219971(18) 0.444516(18) 0.01630(6) Uani 1 1 d . . . Fe11 Fe 0.24517(3) 0.828211(18) 0.920237(18) 0.01660(6) Uani 1 1 d . . . Fe12 Fe 0.26350(3) 0.703597(18) 0.812324(18) 0.01615(6) Uani 1 1 d . . . S1 S 0.85414(6) 0.21386(3) 0.31001(3) 0.01912(10) Uani 1 1 d . . . S2 S 0.76803(6) 0.35894(3) 0.46510(3) 0.01900(10) Uani 1 1 d . . . S3 S 0.99331(6) 0.41719(3) 0.27041(3) 0.02105(11) Uani 1 1 d . . . S4 S 0.56037(6) 0.41438(4) 0.27360(3) 0.02212(11) Uani 1 1 d . . . S5 S 1.01515(6) 0.13977(4) 0.51072(3) 0.02216(11) Uani 1 1 d . . . S6 S 0.58540(6) 0.16934(3) 0.49196(3) 0.02093(11) Uani 1 1 d . . . S11 S 0.23699(6) 0.84378(3) 0.78353(3) 0.01939(11) Uani 1 1 d . . . S12 S 0.27649(6) 0.68782(3) 0.94861(3) 0.01951(11) Uani 1 1 d . . . S13 S 0.45047(6) 0.87743(3) 0.97385(3) 0.01963(11) Uani 1 1 d . . . S14 S 0.01839(6) 0.89962(4) 0.97728(4) 0.02263(11) Uani 1 1 d . . . S15 S 0.48556(6) 0.62927(4) 0.75390(3) 0.02134(11) Uani 1 1 d . . . S16 S 0.05238(6) 0.65631(3) 0.76115(3) 0.02034(11) Uani 1 1 d . . . F1 F 0.9644(2) 0.76631(9) 0.38866(10) 0.0385(4) Uani 1 1 d . . . F2 F 0.55078(19) 0.41856(11) -0.09298(9) 0.0380(4) Uani 1 1 d . . . F3 F 0.92310(18) 0.12796(10) 0.87569(9) 0.0339(3) Uani 1 1 d . . . F4 F 0.5237(2) -0.16042(10) 0.35314(10) 0.0450(4) Uani 1 1 d . . . F11 F 0.4360(2) 1.24708(9) 0.88422(11) 0.0435(4) Uani 1 1 d . . . F12 F 0.0922(2) 0.94219(14) 1.33404(10) 0.0516(5) Uani 1 1 d . . . F13 F 0.44920(18) 0.64078(11) 0.38802(9) 0.0373(4) Uani 1 1 d . . . F14 F 0.0034(2) 0.30649(9) 0.90157(10) 0.0389(4) Uani 1 1 d . . . C1 C 0.9786(3) 0.52140(14) 0.30781(13) 0.0195(4) Uani 1 1 d . . . C2 C 1.1107(3) 0.56065(15) 0.30344(14) 0.0234(5) Uani 1 1 d . . . H2 H 1.2027 0.5314 0.2819 0.080 Uiso 1 1 calc R . . C3 C 1.1057(3) 0.64271(15) 0.33099(15) 0.0267(5) Uani 1 1 d . . . H3 H 1.1939 0.6683 0.3288 0.080 Uiso 1 1 calc R . . C4 C 0.9685(3) 0.68552(15) 0.36153(15) 0.0269(5) Uani 1 1 d . . . C5 C 0.8365(3) 0.64959(15) 0.36699(14) 0.0245(5) Uani 1 1 d . . . H5 H 0.7453 0.6796 0.3887 0.080 Uiso 1 1 calc R . . C6 C 0.8416(3) 0.56715(14) 0.33935(13) 0.0219(4) Uani 1 1 d . . . H6 H 0.7526 0.5424 0.3420 0.080 Uiso 1 1 calc R . . C7 C 0.5674(3) 0.41438(13) 0.16377(13) 0.0191(4) Uani 1 1 d . . . C8 C 0.6906(3) 0.37265(14) 0.11679(14) 0.0223(4) Uani 1 1 d . . . H8 H 0.7775 0.3436 0.1438 0.080 Uiso 1 1 calc R . . C9 C 0.6863(3) 0.37363(15) 0.03034(14) 0.0262(5) Uani 1 1 d . . . H9 H 0.7683 0.3451 -0.0005 0.080 Uiso 1 1 calc R . . C10 C 0.5569(3) 0.41810(15) -0.00829(14) 0.0254(5) Uani 1 1 d . . . C11 C 0.4340(3) 0.46067(16) 0.03489(15) 0.0282(5) Uani 1 1 d . . . H11 H 0.3486 0.4904 0.0071 0.080 Uiso 1 1 calc R . . C12 C 0.4392(3) 0.45861(15) 0.12133(15) 0.0257(5) Uani 1 1 d . . . H12 H 0.3560 0.4871 0.1514 0.080 Uiso 1 1 calc R . . C13 C 0.9743(2) 0.13646(14) 0.61880(14) 0.0201(4) Uani 1 1 d . . . C14 C 1.0609(3) 0.07092(14) 0.66917(14) 0.0219(4) Uani 1 1 d . . . H14 H 1.1322 0.0292 0.6443 0.080 Uiso 1 1 calc R . . C15 C 1.0419(3) 0.06730(15) 0.75500(15) 0.0250(5) Uani 1 1 d . . . H15 H 1.0996 0.0236 0.7877 0.080 Uiso 1 1 calc R . . C16 C 0.9369(3) 0.12914(16) 0.79100(14) 0.0250(5) Uani 1 1 d . . . C17 C 0.8468(3) 0.19357(16) 0.74451(15) 0.0274(5) Uani 1 1 d . . . H17 H 0.7749 0.2343 0.7702 0.080 Uiso 1 1 calc R . . C18 C 0.8659(3) 0.19635(15) 0.65816(15) 0.0256(5) Uani 1 1 d . . . H18 H 0.8049 0.2391 0.6261 0.080 Uiso 1 1 calc R . . C19 C 0.5738(3) 0.07011(14) 0.44910(13) 0.0204(4) Uani 1 1 d . . . C20 C 0.6959(3) 0.02214(14) 0.40580(14) 0.0229(4) Uani 1 1 d . . . H20 H 0.7894 0.0422 0.3986 0.080 Uiso 1 1 calc R . . C21 C 0.6787(3) -0.05576(15) 0.37322(15) 0.0281(5) Uani 1 1 d . . . H21 H 0.7597 -0.0876 0.3442 0.080 Uiso 1 1 calc R . . C22 C 0.5401(3) -0.08409(15) 0.38508(15) 0.0306(5) Uani 1 1 d . . . C23 C 0.4175(3) -0.03933(17) 0.42732(16) 0.0304(5) Uani 1 1 d . . . H23 H 0.3248 -0.0604 0.4342 0.080 Uiso 1 1 calc R . . C24 C 0.4344(3) 0.03810(15) 0.45962(15) 0.0242(5) Uani 1 1 d . . . H24 H 0.3522 0.0690 0.4886 0.080 Uiso 1 1 calc R . . C101 C 0.4406(3) 0.98847(14) 0.94534(13) 0.0187(4) Uani 1 1 d . . . C102 C 0.5767(3) 1.02367(14) 0.94473(14) 0.0204(4) Uani 1 1 d . . . H102 H 0.6691 0.9885 0.9583 0.080 Uiso 1 1 calc R . . C103 C 0.5749(3) 1.11110(15) 0.92389(15) 0.0264(5) Uani 1 1 d . . . H103 H 0.6652 1.1346 0.9231 0.080 Uiso 1 1 calc R . . C104 C 0.4374(3) 1.16135(15) 0.90469(15) 0.0272(5) Uani 1 1 d . . . C105 C 0.2997(3) 1.13006(15) 0.90581(15) 0.0260(5) Uani 1 1 d . . . H105 H 0.2078 1.1661 0.8929 0.080 Uiso 1 1 calc R . . C106 C 0.3028(3) 1.04305(14) 0.92686(14) 0.0218(4) Uani 1 1 d . . . H106 H 0.2112 1.0207 0.9287 0.080 Uiso 1 1 calc R . . C107 C 0.0543(3) 0.91165(15) 1.08291(14) 0.0216(4) Uani 1 1 d . . . C108 C -0.0207(3) 0.98587(16) 1.11992(16) 0.0285(5) Uani 1 1 d . . . H108 H -0.0793 1.0292 1.0873 0.080 Uiso 1 1 calc R . . C109 C -0.0091(3) 0.99582(17) 1.20432(17) 0.0329(6) Uani 1 1 d . . . H109 H -0.0609 1.0446 1.2288 0.080 Uiso 1 1 calc R . . C110 C 0.0804(3) 0.93210(19) 1.25075(16) 0.0343(6) Uani 1 1 d . . . C111 C 0.1605(3) 0.85949(18) 1.21709(16) 0.0325(6) Uani 1 1 d . . . H111 H 0.2230 0.8181 1.2500 0.080 Uiso 1 1 calc R . . C112 C 0.1461(3) 0.84929(16) 1.13301(16) 0.0268(5) Uani 1 1 d . . . H112 H 0.1986 0.8001 1.1095 0.080 Uiso 1 1 calc R . . C113 C 0.4637(3) 0.63422(14) 0.64478(14) 0.0200(4) Uani 1 1 d . . . C114 C 0.5665(3) 0.57614(14) 0.59885(14) 0.0213(4) Uani 1 1 d . . . H114 H 0.6398 0.5360 0.6265 0.080 Uiso 1 1 calc R . . C115 C 0.5604(3) 0.57773(14) 0.51256(14) 0.0245(5) Uani 1 1 d . . . H115 H 0.6284 0.5389 0.4824 0.080 Uiso 1 1 calc R . . C116 C 0.4522(3) 0.63760(16) 0.47291(14) 0.0263(5) Uani 1 1 d . . . C117 C 0.3476(3) 0.69558(17) 0.51512(15) 0.0284(5) Uani 1 1 d . . . H117 H 0.2739 0.7348 0.4867 0.080 Uiso 1 1 calc R . . C118 C 0.3555(3) 0.69370(15) 0.60165(14) 0.0238(5) Uani 1 1 d . . . H118 H 0.2870 0.7330 0.6311 0.080 Uiso 1 1 calc R . . C119 C 0.0449(3) 0.55036(14) 0.80365(13) 0.0176(4) Uani 1 1 d . . . C120 C -0.0905(3) 0.51743(15) 0.79477(15) 0.0232(5) Uani 1 1 d . . . H120 H -0.1725 0.5507 0.7668 0.080 Uiso 1 1 calc R . . C121 C -0.1041(3) 0.43461(15) 0.82761(15) 0.0272(5) Uani 1 1 d . . . H121 H -0.1940 0.4121 0.8213 0.080 Uiso 1 1 calc R . . C122 C 0.0172(3) 0.38750(14) 0.86915(15) 0.0266(5) Uani 1 1 d . . . C123 C 0.1531(3) 0.41710(14) 0.87892(14) 0.0241(5) Uani 1 1 d . . . H123 H 0.2343 0.3831 0.9068 0.080 Uiso 1 1 calc R . . C124 C 0.1664(3) 0.49969(14) 0.84582(13) 0.0217(4) Uani 1 1 d . . . H124 H 0.2574 0.5211 0.8520 0.080 Uiso 1 1 calc R . . N1 N 0.3704(2) 0.16036(11) 0.18740(11) 0.0188(4) Uani 1 1 d . . . C33 C 0.3001(3) 0.24213(15) 0.13815(15) 0.0282(5) Uani 1 1 d . . . H33A H 0.3076 0.2910 0.1704 0.080 Uiso 1 1 calc R . . H33B H 0.3610 0.2477 0.0872 0.080 Uiso 1 1 calc R . . C34 C 0.1328(3) 0.2465(2) 0.11545(17) 0.0397(6) Uani 1 1 d . . . H34A H 0.1239 0.1993 0.0821 0.080 Uiso 1 1 calc R . . H34B H 0.0983 0.2999 0.0845 0.080 Uiso 1 1 calc R . . H34C H 0.0704 0.2429 0.1654 0.080 Uiso 1 1 calc R . . C27 C 0.3631(3) 0.08300(15) 0.13647(13) 0.0226(4) Uani 1 1 d . . . H27A H 0.2557 0.0776 0.1310 0.080 Uiso 1 1 calc R . . H27B H 0.4050 0.0942 0.0810 0.080 Uiso 1 1 calc R . . C28 C 0.4488(3) -0.00216(15) 0.17236(16) 0.0312(5) Uani 1 1 d . . . H28A H 0.5559 0.0017 0.1768 0.080 Uiso 1 1 calc R . . H28B H 0.4385 -0.0470 0.1364 0.080 Uiso 1 1 calc R . . H28C H 0.4062 -0.0151 0.2266 0.080 Uiso 1 1 calc R . . C29 C 0.5357(3) 0.16755(15) 0.20507(14) 0.0232(4) Uani 1 1 d . . . H29A H 0.5745 0.1222 0.2462 0.080 Uiso 1 1 calc R . . H29B H 0.5368 0.2222 0.2291 0.080 Uiso 1 1 calc R . . C30 C 0.6442(3) 0.16128(16) 0.12902(16) 0.0289(5) Uani 1 1 d . . . H30A H 0.6535 0.1048 0.1084 0.080 Uiso 1 1 calc R . . H30B H 0.7439 0.1715 0.1442 0.080 Uiso 1 1 calc R . . H30C H 0.6038 0.2036 0.0864 0.080 Uiso 1 1 calc R . . C31 C 0.2833(3) 0.14833(15) 0.26959(14) 0.0235(4) Uani 1 1 d . . . H31A H 0.1781 0.1428 0.2578 0.080 Uiso 1 1 calc R . . H31B H 0.3303 0.0947 0.2979 0.080 Uiso 1 1 calc R . . C32 C 0.2790(3) 0.22018(16) 0.32808(15) 0.0273(5) Uani 1 1 d . . . H32A H 0.3824 0.2263 0.3404 0.080 Uiso 1 1 calc R . . H32B H 0.2247 0.2066 0.3788 0.080 Uiso 1 1 calc R . . H32C H 0.2271 0.2731 0.3022 0.080 Uiso 1 1 calc R . . N2 N 0.7606(2) 0.66729(11) 0.08604(11) 0.0165(3) Uani 1 1 d . . . C35 C 0.7929(3) 0.70285(14) -0.00227(13) 0.0207(4) Uani 1 1 d . . . H35A H 0.7521 0.7639 -0.0065 0.080 Uiso 1 1 calc R . . H35B H 0.9037 0.6965 -0.0118 0.080 Uiso 1 1 calc R . . C36 C 0.7250(3) 0.65970(17) -0.07005(15) 0.0299(5) Uani 1 1 d . . . H36A H 0.7529 0.5983 -0.0618 0.080 Uiso 1 1 calc R . . H36B H 0.7642 0.6783 -0.1234 0.080 Uiso 1 1 calc R . . H36C H 0.6147 0.6751 -0.0680 0.080 Uiso 1 1 calc R . . C37 C 0.8256(3) 0.57219(13) 0.09674(14) 0.0224(5) Uani 1 1 d . . . H37A H 0.7658 0.5408 0.0640 0.080 Uiso 1 1 calc R . . H37B H 0.8124 0.5533 0.1547 0.080 Uiso 1 1 calc R . . C38 C 0.9945(3) 0.54857(17) 0.07155(17) 0.0349(6) Uani 1 1 d . . . H38A H 1.0066 0.5576 0.0123 0.080 Uiso 1 1 calc R . . H38B H 1.0299 0.4891 0.0877 0.080 Uiso 1 1 calc R . . H38C H 1.0538 0.5840 0.0988 0.080 Uiso 1 1 calc R . . C39 C 0.8356(3) 0.71651(15) 0.14604(14) 0.0236(5) Uani 1 1 d . . . H39A H 0.9417 0.7168 0.1275 0.080 Uiso 1 1 calc R . . H39B H 0.8376 0.6858 0.2003 0.080 Uiso 1 1 calc R . . C40 C 0.7584(3) 0.80894(15) 0.15593(16) 0.0299(5) Uani 1 1 d . . . H40A H 0.7467 0.8389 0.1021 0.080 Uiso 1 1 calc R . . H40B H 0.8210 0.8370 0.1894 0.080 Uiso 1 1 calc R . . H40C H 0.6589 0.8094 0.1826 0.080 Uiso 1 1 calc R . . C41 C 0.5867(3) 0.67835(14) 0.10108(13) 0.0198(4) Uani 1 1 d . . . H41A H 0.5448 0.6426 0.0639 0.080 Uiso 1 1 calc R . . H41B H 0.5430 0.7378 0.0863 0.080 Uiso 1 1 calc R . . C42 C 0.5344(3) 0.65580(15) 0.18997(14) 0.0238(5) Uani 1 1 d . . . H42A H 0.5742 0.5966 0.2049 0.080 Uiso 1 1 calc R . . H42B H 0.4238 0.6647 0.1936 0.080 Uiso 1 1 calc R . . H42C H 0.5724 0.6920 0.2274 0.080 Uiso 1 1 calc R . . N3 N 0.2603(2) 0.38754(11) 0.59937(11) 0.0187(4) Uani 1 1 d . . . C43 C 0.2324(3) 0.35696(15) 0.51424(14) 0.0242(5) Uani 1 1 d . . . H43A H 0.2719 0.2958 0.5135 0.080 Uiso 1 1 calc R . . H43B H 0.1222 0.3648 0.5060 0.080 Uiso 1 1 calc R . . C44 C 0.3069(3) 0.40349(17) 0.44282(15) 0.0299(5) Uani 1 1 d . . . H44A H 0.2825 0.4645 0.4484 0.080 Uiso 1 1 calc R . . H44B H 0.2688 0.3896 0.3911 0.080 Uiso 1 1 calc R . . H44C H 0.4167 0.3859 0.4435 0.080 Uiso 1 1 calc R . . C45 C 0.1771(3) 0.33763(17) 0.66478(15) 0.0306(5) Uani 1 1 d . . . H45A H 0.1734 0.3660 0.7167 0.080 Uiso 1 1 calc R . . H45B H 0.0717 0.3400 0.6479 0.080 Uiso 1 1 calc R . . C46 C 0.2486(4) 0.24421(18) 0.68059(17) 0.0387(6) Uani 1 1 d . . . H46A H 0.2563 0.2157 0.6293 0.080 Uiso 1 1 calc R . . H46B H 0.1852 0.2166 0.7201 0.080 Uiso 1 1 calc R . . H46C H 0.3496 0.2409 0.7024 0.080 Uiso 1 1 calc R . . C47 C 0.1985(3) 0.48320(15) 0.60391(15) 0.0257(5) Uani 1 1 d . . . H47A H 0.2050 0.4986 0.6609 0.080 Uiso 1 1 calc R . . H47B H 0.2649 0.5153 0.5696 0.080 Uiso 1 1 calc R . . C48 C 0.0338(3) 0.51142(19) 0.57642(19) 0.0396(7) Uani 1 1 d . . . H48A H 0.0290 0.5057 0.5176 0.080 Uiso 1 1 calc R . . H48B H 0.0001 0.5705 0.5886 0.080 Uiso 1 1 calc R . . H48C H -0.0319 0.4759 0.6057 0.080 Uiso 1 1 calc R . . C49 C 0.4320(3) 0.37274(14) 0.61401(13) 0.0210(4) Uani 1 1 d . . . H49A H 0.4800 0.4087 0.5732 0.080 Uiso 1 1 calc R . . H49B H 0.4732 0.3132 0.6039 0.080 Uiso 1 1 calc R . . C50 C 0.4787(3) 0.39094(15) 0.70008(14) 0.0264(5) Uani 1 1 d . . . H50A H 0.4358 0.4491 0.7119 0.080 Uiso 1 1 calc R . . H50B H 0.5891 0.3835 0.7020 0.080 Uiso 1 1 calc R . . H50C H 0.4408 0.3518 0.7408 0.080 Uiso 1 1 calc R . . N4 N 0.7426(2) 0.88881(12) 0.65965(11) 0.0196(4) Uani 1 1 d . . . C51 C 0.7051(3) 0.84481(15) 0.74347(14) 0.0258(5) Uani 1 1 d . . . H51A H 0.5944 0.8566 0.7536 0.080 Uiso 1 1 calc R . . H51B H 0.7346 0.7830 0.7402 0.080 Uiso 1 1 calc R . . C52 C 0.7832(3) 0.87254(17) 0.81601(15) 0.0296(5) Uani 1 1 d . . . H52A H 0.8920 0.8517 0.8118 0.080 Uiso 1 1 calc R . . H52B H 0.7419 0.8493 0.8670 0.080 Uiso 1 1 calc R . . H52C H 0.7658 0.9343 0.8156 0.080 Uiso 1 1 calc R . . C53 C 0.6609(3) 0.85323(18) 0.59281(16) 0.0335(6) Uani 1 1 d . . . H53A H 0.6652 0.8899 0.5423 0.080 Uiso 1 1 calc R . . H53B H 0.5533 0.8564 0.6097 0.080 Uiso 1 1 calc R . . C54 C 0.7237(4) 0.76187(19) 0.57282(18) 0.0408(7) Uani 1 1 d . . . H54A H 0.8249 0.7594 0.5477 0.080 Uiso 1 1 calc R . . H54B H 0.6569 0.7425 0.5349 0.080 Uiso 1 1 calc R . . H54C H 0.7293 0.7255 0.6232 0.080 Uiso 1 1 calc R . . C55 C 0.9172(3) 0.87093(15) 0.64447(14) 0.0240(5) Uani 1 1 d . . . H55A H 0.9654 0.8985 0.6863 0.080 Uiso 1 1 calc R . . H55B H 0.9521 0.8094 0.6523 0.080 Uiso 1 1 calc R . . C56 C 0.9728(3) 0.90129(16) 0.55934(15) 0.0273(5) Uani 1 1 d . . . H56A H 0.9324 0.8712 0.5174 0.080 Uiso 1 1 calc R . . H56B H 1.0834 0.8899 0.5563 0.080 Uiso 1 1 calc R . . H56C H 0.9377 0.9620 0.5503 0.080 Uiso 1 1 calc R . . C57 C 0.6919(3) 0.98580(15) 0.66010(16) 0.0279(5) Uani 1 1 d . . . H57A H 0.7578 1.0087 0.6969 0.080 Uiso 1 1 calc R . . H57B H 0.7078 1.0109 0.6044 0.080 Uiso 1 1 calc R . . C58 C 0.5259(4) 1.01446(19) 0.6871(2) 0.0411(7) Uani 1 1 d . . . H58A H 0.4594 0.9895 0.6533 0.080 Uiso 1 1 calc R . . H58B H 0.5015 1.0761 0.6808 0.080 Uiso 1 1 calc R . . H58C H 0.5113 0.9959 0.7445 0.080 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 0.01875(15) 0.01480(13) 0.01523(14) 0.00073(11) -0.00086(11) -0.00106(11) Fe2 0.01835(15) 0.01458(13) 0.01546(13) 0.00037(10) -0.00171(11) -0.00139(11) Fe11 0.01757(15) 0.01466(14) 0.01753(14) -0.00302(11) -0.00131(11) -0.00151(11) Fe12 0.01745(15) 0.01451(14) 0.01642(14) -0.00281(11) -0.00148(11) -0.00147(11) S1 0.0226(3) 0.0170(2) 0.0176(2) -0.00335(18) -0.0003(2) -0.0018(2) S2 0.0239(3) 0.0156(2) 0.0168(2) -0.00164(18) -0.0005(2) -0.00085(19) S3 0.0211(3) 0.0174(2) 0.0235(3) -0.0003(2) 0.0038(2) -0.0010(2) S4 0.0195(3) 0.0268(3) 0.0176(2) 0.0019(2) -0.0002(2) 0.0019(2) S5 0.0186(3) 0.0232(3) 0.0225(3) 0.0028(2) -0.0010(2) 0.0014(2) S6 0.0194(3) 0.0193(2) 0.0238(3) -0.0025(2) 0.0016(2) -0.0023(2) S11 0.0225(3) 0.0160(2) 0.0190(2) -0.00006(19) -0.0028(2) -0.0010(2) S12 0.0243(3) 0.0160(2) 0.0181(2) -0.00040(19) -0.0022(2) -0.0029(2) S13 0.0193(3) 0.0154(2) 0.0238(3) -0.00139(19) -0.0062(2) -0.0004(2) S14 0.0180(3) 0.0245(3) 0.0248(3) -0.0057(2) 0.0000(2) -0.0002(2) S15 0.0180(3) 0.0238(3) 0.0209(3) -0.0043(2) -0.0023(2) 0.0021(2) S16 0.0192(3) 0.0178(2) 0.0240(3) 0.0003(2) -0.0055(2) -0.0022(2) F1 0.0507(10) 0.0264(7) 0.0414(9) -0.0112(6) 0.0024(7) -0.0124(7) F2 0.0439(9) 0.0536(10) 0.0178(7) 0.0016(6) -0.0048(6) -0.0121(8) F3 0.0324(8) 0.0478(9) 0.0214(7) 0.0058(6) -0.0033(6) -0.0081(7) F4 0.0692(12) 0.0301(8) 0.0410(9) -0.0092(7) -0.0104(8) -0.0187(8) F11 0.0533(10) 0.0181(7) 0.0591(11) 0.0100(7) -0.0043(8) -0.0105(7) F12 0.0528(11) 0.0803(13) 0.0264(8) -0.0217(8) 0.0010(7) -0.0185(10) F13 0.0361(9) 0.0587(10) 0.0190(7) -0.0094(7) 0.0032(6) -0.0112(7) F14 0.0480(9) 0.0207(7) 0.0475(9) 0.0051(6) 0.0112(7) -0.0093(6) C1 0.0226(11) 0.0199(10) 0.0150(10) 0.0024(8) -0.0026(8) -0.0011(8) C2 0.0206(11) 0.0251(11) 0.0227(11) 0.0018(9) -0.0012(9) 0.0000(9) C3 0.0247(12) 0.0283(12) 0.0290(12) 0.0005(9) -0.0048(9) -0.0102(10) C4 0.0379(14) 0.0220(11) 0.0215(11) -0.0041(9) -0.0020(10) -0.0060(10) C5 0.0283(12) 0.0240(11) 0.0201(11) -0.0017(8) 0.0032(9) -0.0017(9) C6 0.0226(11) 0.0251(11) 0.0177(10) 0.0002(8) 0.0006(8) -0.0039(9) C7 0.0203(11) 0.0163(9) 0.0212(10) 0.0027(8) -0.0027(8) -0.0054(8) C8 0.0213(11) 0.0231(11) 0.0212(11) 0.0019(8) -0.0010(9) -0.0011(9) C9 0.0286(12) 0.0289(12) 0.0210(11) -0.0016(9) 0.0025(9) -0.0055(10) C10 0.0330(13) 0.0306(12) 0.0144(10) 0.0030(8) -0.0045(9) -0.0112(10) C11 0.0315(13) 0.0269(12) 0.0258(12) 0.0036(9) -0.0115(10) -0.0031(10) C12 0.0237(12) 0.0253(11) 0.0265(12) -0.0022(9) -0.0022(9) 0.0017(9) C13 0.0175(10) 0.0198(10) 0.0235(11) 0.0033(8) -0.0039(8) -0.0057(8) C14 0.0225(11) 0.0169(10) 0.0266(11) 0.0003(8) -0.0062(9) -0.0033(8) C15 0.0278(12) 0.0213(11) 0.0274(12) 0.0048(9) -0.0110(9) -0.0086(9) C16 0.0248(12) 0.0310(12) 0.0206(11) 0.0054(9) -0.0052(9) -0.0109(10) C17 0.0225(12) 0.0315(12) 0.0259(12) 0.0021(9) -0.0008(9) 0.0009(10) C18 0.0201(11) 0.0279(12) 0.0272(12) 0.0024(9) -0.0032(9) 0.0000(9) C19 0.0206(11) 0.0220(11) 0.0177(10) 0.0036(8) -0.0048(8) -0.0021(9) C20 0.0251(12) 0.0231(11) 0.0206(10) 0.0000(8) -0.0019(9) -0.0040(9) C21 0.0398(14) 0.0239(11) 0.0194(11) -0.0015(9) -0.0015(10) -0.0013(10) C22 0.0463(15) 0.0220(11) 0.0256(12) -0.0003(9) -0.0135(11) -0.0092(11) C23 0.0332(14) 0.0310(13) 0.0294(12) 0.0072(10) -0.0118(10) -0.0132(11) C24 0.0212(11) 0.0241(11) 0.0271(11) 0.0058(9) -0.0052(9) -0.0049(9) C101 0.0228(11) 0.0168(10) 0.0163(10) -0.0033(7) -0.0003(8) -0.0022(8) C102 0.0190(11) 0.0215(11) 0.0207(11) -0.0047(8) 0.0017(8) -0.0026(8) C103 0.0289(12) 0.0260(12) 0.0260(12) -0.0047(9) 0.0051(10) -0.0094(10) C104 0.0374(14) 0.0176(11) 0.0267(12) 0.0032(9) -0.0001(10) -0.0068(10) C105 0.0296(12) 0.0201(11) 0.0276(12) 0.0015(9) -0.0084(9) -0.0013(9) C106 0.0220(11) 0.0203(10) 0.0227(11) -0.0016(8) -0.0062(9) -0.0012(9) C107 0.0189(11) 0.0237(11) 0.0239(11) -0.0054(8) 0.0025(9) -0.0076(9) C108 0.0243(12) 0.0255(12) 0.0369(13) -0.0104(10) 0.0028(10) -0.0048(9) C109 0.0306(13) 0.0318(13) 0.0388(14) -0.0173(11) 0.0076(11) -0.0084(11) C110 0.0341(14) 0.0484(16) 0.0253(12) -0.0138(11) 0.0032(11) -0.0172(12) C111 0.0308(14) 0.0401(14) 0.0278(13) -0.0036(10) 0.0005(10) -0.0087(11) C112 0.0251(12) 0.0250(12) 0.0301(12) -0.0044(9) 0.0036(10) -0.0041(9) C113 0.0178(10) 0.0196(10) 0.0236(11) -0.0031(8) 0.0022(8) -0.0059(8) C114 0.0189(11) 0.0185(10) 0.0270(11) -0.0024(8) 0.0055(9) -0.0051(8) C115 0.0272(12) 0.0210(11) 0.0268(11) -0.0085(9) 0.0112(9) -0.0086(9) C116 0.0272(12) 0.0361(13) 0.0190(11) -0.0080(9) 0.0047(9) -0.0136(10) C117 0.0243(12) 0.0348(13) 0.0253(12) -0.0008(10) -0.0020(10) -0.0023(10) C118 0.0199(11) 0.0289(12) 0.0214(11) -0.0058(9) 0.0005(9) 0.0008(9) C119 0.0177(10) 0.0179(10) 0.0165(10) -0.0035(8) 0.0019(8) -0.0005(8) C120 0.0200(11) 0.0237(11) 0.0257(11) -0.0068(9) 0.0016(9) -0.0016(9) C121 0.0254(12) 0.0254(11) 0.0320(13) -0.0072(9) 0.0079(10) -0.0076(9) C122 0.0368(13) 0.0157(10) 0.0269(12) -0.0011(8) 0.0095(10) -0.0056(9) C123 0.0314(13) 0.0188(10) 0.0203(11) -0.0002(8) -0.0001(9) 0.0003(9) C124 0.0236(11) 0.0215(10) 0.0197(10) -0.0032(8) -0.0019(9) -0.0020(9) N1 0.0203(9) 0.0188(9) 0.0172(8) -0.0001(7) -0.0042(7) -0.0022(7) C33 0.0324(13) 0.0244(11) 0.0250(12) 0.0023(9) -0.0032(10) 0.0027(10) C34 0.0316(14) 0.0500(17) 0.0307(13) 0.0001(12) -0.0066(11) 0.0139(12) C27 0.0262(12) 0.0251(11) 0.0187(10) -0.0063(8) -0.0017(9) -0.0081(9) C28 0.0444(15) 0.0193(11) 0.0304(12) -0.0046(9) -0.0021(11) -0.0053(10) C29 0.0232(11) 0.0241(11) 0.0234(11) -0.0049(8) -0.0050(9) -0.0048(9) C30 0.0227(12) 0.0327(12) 0.0336(13) -0.0105(10) 0.0008(10) -0.0085(10) C31 0.0244(11) 0.0274(11) 0.0186(10) -0.0022(8) 0.0009(9) -0.0038(9) C32 0.0285(12) 0.0282(12) 0.0232(11) -0.0065(9) -0.0027(9) 0.0036(10) N2 0.0187(9) 0.0142(8) 0.0158(8) 0.0018(6) -0.0010(7) -0.0012(7) C35 0.0237(11) 0.0202(10) 0.0165(10) 0.0044(8) 0.0001(8) -0.0010(9) C36 0.0332(14) 0.0378(14) 0.0187(11) -0.0044(10) 0.0013(10) -0.0055(11) C37 0.0253(12) 0.0141(10) 0.0254(11) 0.0036(8) 0.0001(9) 0.0018(8) C38 0.0327(14) 0.0304(13) 0.0341(14) 0.0097(10) 0.0089(11) 0.0099(11) C39 0.0243(12) 0.0262(11) 0.0221(11) -0.0014(9) -0.0060(9) -0.0078(9) C40 0.0379(14) 0.0247(12) 0.0300(12) -0.0077(9) 0.0033(11) -0.0125(11) C41 0.0160(10) 0.0216(10) 0.0210(10) 0.0013(8) -0.0019(8) -0.0019(8) C42 0.0228(11) 0.0253(11) 0.0225(11) 0.0026(9) 0.0033(9) -0.0042(9) N3 0.0203(9) 0.0203(9) 0.0165(8) -0.0044(7) 0.0037(7) -0.0057(7) C43 0.0292(12) 0.0233(11) 0.0210(11) -0.0071(8) -0.0018(9) -0.0048(9) C44 0.0327(13) 0.0374(13) 0.0196(11) -0.0033(9) -0.0026(10) -0.0049(11) C45 0.0332(13) 0.0378(13) 0.0249(12) -0.0030(10) 0.0072(10) -0.0187(11) C46 0.0498(17) 0.0366(14) 0.0350(14) 0.0091(11) -0.0076(12) -0.0254(13) C47 0.0280(12) 0.0226(11) 0.0264(11) -0.0092(9) 0.0013(9) -0.0008(9) C48 0.0325(14) 0.0439(17) 0.0397(15) -0.0139(13) -0.0073(12) 0.0075(12) C49 0.0210(11) 0.0200(10) 0.0219(11) -0.0014(8) 0.0007(8) -0.0033(8) C50 0.0309(13) 0.0262(11) 0.0234(11) -0.0009(9) -0.0044(9) -0.0085(10) N4 0.0220(10) 0.0204(9) 0.0170(9) 0.0033(7) -0.0041(7) -0.0067(7) C51 0.0307(13) 0.0246(11) 0.0218(11) 0.0056(9) 0.0006(9) -0.0063(10) C52 0.0320(13) 0.0351(13) 0.0192(11) 0.0003(9) 0.0010(10) 0.0007(11) C53 0.0367(15) 0.0438(15) 0.0242(12) -0.0005(10) -0.0076(10) -0.0186(12) C54 0.0527(18) 0.0428(16) 0.0351(14) -0.0153(12) 0.0074(13) -0.0284(14) C55 0.0227(12) 0.0245(11) 0.0246(11) 0.0020(9) -0.0032(9) -0.0036(9) C56 0.0307(13) 0.0278(12) 0.0255(12) 0.0000(9) 0.0020(10) -0.0118(10) C57 0.0339(14) 0.0202(11) 0.0281(12) 0.0037(9) -0.0031(10) -0.0015(10) C58 0.0357(15) 0.0383(15) 0.0427(16) 0.0056(12) 0.0014(12) 0.0102(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 S2 2.1995(6) . ? Fe1 S1 2.2034(6) . ? Fe1 S3 2.3009(6) . ? Fe1 S4 2.3196(6) . ? Fe1 Fe2 2.6975(4) . ? Fe2 S1 2.1942(6) . ? Fe2 S2 2.2062(6) . ? Fe2 S5 2.3003(6) . ? Fe2 S6 2.3115(6) . ? Fe11 S11 2.2003(6) . ? Fe11 S12 2.2049(6) . ? Fe11 S13 2.2968(6) . ? Fe11 S14 2.3118(6) . ? Fe11 Fe12 2.6875(4) . ? Fe12 S12 2.1961(6) . ? Fe12 S11 2.2047(6) . ? Fe12 S15 2.3069(6) . ? Fe12 S16 2.3099(6) . ? S3 C1 1.770(2) . ? S4 C7 1.766(2) . ? S5 C13 1.762(2) . ? S6 C19 1.770(2) . ? S13 C101 1.770(2) . ? S14 C107 1.768(2) . ? S15 C113 1.769(2) . ? S16 C119 1.774(2) . ? F1 C4 1.368(3) . ? F2 C10 1.365(3) . ? F3 C16 1.363(3) . ? F4 C22 1.370(3) . ? F11 C104 1.369(3) . ? F12 C110 1.370(3) . ? F13 C116 1.365(3) . ? F14 C122 1.371(3) . ? C1 C6 1.394(3) . ? C1 C2 1.401(3) . ? C2 C3 1.388(3) . ? C3 C4 1.372(4) . ? C4 C5 1.371(4) . ? C5 C6 1.395(3) . ? C7 C8 1.396(3) . ? C7 C12 1.400(3) . ? C8 C9 1.392(3) . ? C9 C10 1.380(4) . ? C10 C11 1.367(4) . ? C11 C12 1.391(3) . ? C13 C18 1.392(3) . ? C13 C14 1.407(3) . ? C14 C15 1.384(3) . ? C15 C16 1.370(4) . ? C16 C17 1.377(3) . ? C17 C18 1.392(3) . ? C19 C20 1.398(3) . ? C19 C24 1.403(3) . ? C20 C21 1.399(3) . ? C21 C22 1.370(4) . ? C22 C23 1.371(4) . ? C23 C24 1.390(4) . ? C101 C106 1.395(3) . ? C101 C102 1.400(3) . ? C102 C103 1.395(3) . ? C103 C104 1.365(4) . ? C104 C105 1.381(3) . ? C105 C106 1.388(3) . ? C107 C112 1.397(4) . ? C107 C108 1.402(3) . ? C108 C109 1.387(4) . ? C109 C110 1.368(4) . ? C110 C111 1.373(4) . ? C111 C112 1.386(4) . ? C113 C118 1.391(3) . ? C113 C114 1.403(3) . ? C114 C115 1.390(3) . ? C115 C116 1.368(4) . ? C116 C117 1.379(3) . ? C117 C118 1.395(3) . ? C119 C120 1.392(3) . ? C119 C124 1.393(3) . ? C120 C121 1.399(3) . ? C121 C122 1.365(4) . ? C122 C123 1.371(4) . ? C123 C124 1.396(3) . ? N1 C29 1.516(3) . ? N1 C33 1.521(3) . ? N1 C31 1.521(3) . ? N1 C27 1.525(3) . ? C33 C34 1.519(4) . ? C27 C28 1.517(3) . ? C29 C30 1.522(3) . ? C31 C32 1.514(3) . ? N2 C39 1.512(3) . ? N2 C37 1.515(3) . ? N2 C41 1.523(3) . ? N2 C35 1.528(3) . ? C35 C36 1.513(3) . ? C37 C38 1.517(3) . ? C39 C40 1.518(3) . ? C41 C42 1.524(3) . ? N3 C45 1.513(3) . ? N3 C49 1.515(3) . ? N3 C47 1.522(3) . ? N3 C43 1.523(3) . ? C43 C44 1.511(3) . ? C45 C46 1.512(4) . ? C47 C48 1.517(4) . ? C49 C50 1.518(3) . ? N4 C53 1.503(3) . ? N4 C57 1.521(3) . ? N4 C51 1.527(3) . ? N4 C55 1.528(3) . ? C51 C52 1.501(4) . ? C53 C54 1.506(4) . ? C55 C56 1.512(3) . ? C57 C58 1.512(4) . ? 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 S2 Fe1 S1 104.18(2) . . ? S2 Fe1 S3 114.65(2) . . ? S1 Fe1 S3 107.30(2) . . ? S2 Fe1 S4 106.62(2) . . ? S1 Fe1 S4 112.73(2) . . ? S3 Fe1 S4 111.28(2) . . ? S2 Fe1 Fe2 52.359(16) . . ? S1 Fe1 Fe2 52.009(16) . . ? S3 Fe1 Fe2 129.25(2) . . ? S4 Fe1 Fe2 119.453(18) . . ? S1 Fe2 S2 104.26(2) . . ? S1 Fe2 S5 107.28(2) . . ? S2 Fe2 S5 115.38(2) . . ? S1 Fe2 S6 114.86(2) . . ? S2 Fe2 S6 106.34(2) . . ? S5 Fe2 S6 108.91(2) . . ? S1 Fe2 Fe1 52.319(16) . . ? S2 Fe2 Fe1 52.134(16) . . ? S5 Fe2 Fe1 129.966(19) . . ? S6 Fe2 Fe1 121.127(19) . . ? S11 Fe11 S12 104.68(2) . . ? S11 Fe11 S13 113.57(2) . . ? S12 Fe11 S13 107.42(2) . . ? S11 Fe11 S14 109.29(2) . . ? S12 Fe11 S14 112.66(2) . . ? S13 Fe11 S14 109.23(2) . . ? S11 Fe11 Fe12 52.477(16) . . ? S12 Fe11 Fe12 52.215(16) . . ? S13 Fe11 Fe12 125.781(18) . . ? S14 Fe11 Fe12 124.962(19) . . ? S12 Fe12 S11 104.83(2) . . ? S12 Fe12 S15 108.97(2) . . ? S11 Fe12 S15 112.87(2) . . ? S12 Fe12 S16 113.45(2) . . ? S11 Fe12 S16 107.63(2) . . ? S15 Fe12 S16 109.13(2) . . ? S12 Fe12 Fe11 52.512(16) . . ? S11 Fe12 Fe11 52.329(16) . . ? S15 Fe12 Fe11 126.703(19) . . ? S16 Fe12 Fe11 124.158(19) . . ? Fe2 S1 Fe1 75.672(19) . . ? Fe1 S2 Fe2 75.506(19) . . ? C1 S3 Fe1 108.81(7) . . ? C7 S4 Fe1 111.22(8) . . ? C13 S5 Fe2 108.38(8) . . ? C19 S6 Fe2 110.68(8) . . ? Fe11 S11 Fe12 75.195(19) . . ? Fe12 S12 Fe11 75.274(19) . . ? C101 S13 Fe11 109.56(8) . . ? C107 S14 Fe11 106.51(8) . . ? C113 S15 Fe12 107.91(8) . . ? C119 S16 Fe12 109.05(8) . . ? C6 C1 C2 118.5(2) . . ? C6 C1 S3 123.34(17) . . ? C2 C1 S3 118.17(17) . . ? C3 C2 C1 120.7(2) . . ? C4 C3 C2 118.9(2) . . ? F1 C4 C5 119.1(2) . . ? F1 C4 C3 118.6(2) . . ? C5 C4 C3 122.3(2) . . ? C4 C5 C6 118.7(2) . . ? C1 C6 C5 120.8(2) . . ? C8 C7 C12 118.0(2) . . ? C8 C7 S4 124.59(17) . . ? C12 C7 S4 117.38(17) . . ? C9 C8 C7 121.4(2) . . ? C10 C9 C8 118.2(2) . . ? F2 C10 C11 118.7(2) . . ? F2 C10 C9 118.6(2) . . ? C11 C10 C9 122.6(2) . . ? C10 C11 C12 118.6(2) . . ? C11 C12 C7 121.2(2) . . ? C18 C13 C14 117.7(2) . . ? C18 C13 S5 124.28(17) . . ? C14 C13 S5 118.00(17) . . ? C15 C14 C13 121.3(2) . . ? C16 C15 C14 118.9(2) . . ? F3 C16 C15 118.9(2) . . ? F3 C16 C17 118.9(2) . . ? C15 C16 C17 122.2(2) . . ? C16 C17 C18 118.5(2) . . ? C13 C18 C17 121.4(2) . . ? C20 C19 C24 118.5(2) . . ? C20 C19 S6 123.61(17) . . ? C24 C19 S6 117.87(18) . . ? C19 C20 C21 120.7(2) . . ? C22 C21 C20 118.5(2) . . ? C21 C22 F4 118.4(2) . . ? C21 C22 C23 122.8(2) . . ? F4 C22 C23 118.8(2) . . ? C22 C23 C24 118.7(2) . . ? C23 C24 C19 120.8(2) . . ? C106 C101 C102 118.6(2) . . ? C106 C101 S13 123.06(17) . . ? C102 C101 S13 118.28(17) . . ? C103 C102 C101 120.6(2) . . ? C104 C103 C102 118.4(2) . . ? C103 C104 F11 118.3(2) . . ? C103 C104 C105 123.2(2) . . ? F11 C104 C105 118.5(2) . . ? C104 C105 C106 117.9(2) . . ? C105 C106 C101 121.3(2) . . ? C112 C107 C108 118.0(2) . . ? C112 C107 S14 123.80(18) . . ? C108 C107 S14 118.13(19) . . ? C109 C108 C107 121.2(2) . . ? C110 C109 C108 118.4(2) . . ? C109 C110 F12 118.3(2) . . ? C109 C110 C111 122.8(2) . . ? F12 C110 C111 118.9(3) . . ? C110 C111 C112 118.4(3) . . ? C111 C112 C107 121.2(2) . . ? C118 C113 C114 118.2(2) . . ? C118 C113 S15 124.37(17) . . ? C114 C113 S15 117.37(18) . . ? C115 C114 C113 121.0(2) . . ? C116 C115 C114 118.7(2) . . ? F13 C116 C115 118.6(2) . . ? F13 C116 C117 118.7(2) . . ? C115 C116 C117 122.7(2) . . ? C116 C117 C118 118.1(2) . . ? C113 C118 C117 121.3(2) . . ? C120 C119 C124 119.0(2) . . ? C120 C119 S16 117.65(18) . . ? C124 C119 S16 123.33(17) . . ? C119 C120 C121 120.4(2) . . ? C122 C121 C120 118.7(2) . . ? C121 C122 F14 118.5(2) . . ? C121 C122 C123 122.9(2) . . ? F14 C122 C123 118.5(2) . . ? C122 C123 C124 118.2(2) . . ? C119 C124 C123 120.8(2) . . ? C29 N1 C33 107.96(17) . . ? C29 N1 C31 109.00(17) . . ? C33 N1 C31 111.57(17) . . ? C29 N1 C27 111.14(17) . . ? C33 N1 C27 109.07(17) . . ? C31 N1 C27 108.12(16) . . ? C34 C33 N1 115.2(2) . . ? C28 C27 N1 115.08(19) . . ? N1 C29 C30 114.50(18) . . ? C32 C31 N1 115.00(19) . . ? C39 N2 C37 109.70(17) . . ? C39 N2 C41 111.50(17) . . ? C37 N2 C41 108.30(16) . . ? C39 N2 C35 107.97(16) . . ? C37 N2 C35 110.85(16) . . ? C41 N2 C35 108.54(16) . . ? C36 C35 N2 114.37(18) . . ? N2 C37 C38 114.96(18) . . ? N2 C39 C40 115.5(2) . . ? N2 C41 C42 115.24(18) . . ? C45 N3 C49 110.90(18) . . ? C45 N3 C47 108.97(17) . . ? C49 N3 C47 108.61(16) . . ? C45 N3 C43 108.43(17) . . ? C49 N3 C43 109.16(16) . . ? C47 N3 C43 110.78(17) . . ? C44 C43 N3 113.74(18) . . ? C46 C45 N3 115.0(2) . . ? C48 C47 N3 115.3(2) . . ? N3 C49 C50 115.81(18) . . ? C53 N4 C57 109.84(19) . . ? C53 N4 C51 108.67(17) . . ? C57 N4 C51 110.80(18) . . ? C53 N4 C55 110.87(19) . . ? C57 N4 C55 108.27(17) . . ? C51 N4 C55 108.38(17) . . ? C52 C51 N4 114.42(19) . . ? N4 C53 C54 115.6(2) . . ? C56 C55 N4 115.2(2) . . ? C58 C57 N4 115.2(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.96 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.258 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.046 data_5-ab4 _database_code_depnum_ccdc_archive 'CCDC 717463' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H8 Cl8 Fe2 O4 S2 2-, 2(C8 H20 N +), 3(C4 H8 O)' _chemical_formula_sum 'C52 H72 Cl8 Fe2 N2 O7 S2' _chemical_formula_weight 1296.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1684(5) _cell_length_b 16.8066(8) _cell_length_c 20.4441(10) _cell_angle_alpha 79.572(4) _cell_angle_beta 81.551(4) _cell_angle_gamma 77.079(4) _cell_volume 3001.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 55140 _cell_measurement_theta_min 1.49 _cell_measurement_theta_max 24.79 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1348 _exptl_absorpt_coefficient_mu 0.958 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4952 _exptl_absorpt_correction_T_max 0.7767 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55140 _diffrn_reflns_av_R_equivalents 0.0918 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 24.79 _reflns_number_total 10268 _reflns_number_gt 8180 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-AREA (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10268 _refine_ls_number_parameters 666 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0983 _refine_ls_wR_factor_gt 0.0950 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.50277(4) 0.05284(2) 0.041068(18) 0.02231(10) Uani 1 1 d . . . Fe2 Fe 0.58263(4) 0.42678(2) 0.484516(18) 0.02025(10) Uani 1 1 d . . . S1 S 0.65291(8) -0.06926(4) 0.03528(3) 0.02696(16) Uani 1 1 d . . . S2 S 0.64664(7) 0.54953(4) 0.46091(3) 0.02421(15) Uani 1 1 d . . . Cl1 Cl 0.47171(8) -0.08329(4) 0.22430(3) 0.03061(16) Uani 1 1 d . . . Cl2 Cl 0.60313(10) 0.13119(5) 0.36272(4) 0.0450(2) Uani 1 1 d . . . Cl3 Cl 0.34417(13) 0.47061(5) 0.09626(5) 0.0619(3) Uani 1 1 d . . . Cl4 Cl 0.65355(9) 0.26732(5) -0.07315(4) 0.0423(2) Uani 1 1 d . . . Cl11 Cl 0.66637(8) 0.44989(5) 0.27337(4) 0.0424(2) Uani 1 1 d . . . Cl12 Cl 1.14908(8) 0.20191(4) 0.26523(4) 0.03646(18) Uani 1 1 d . . . Cl13 Cl 0.79025(10) -0.01313(4) 0.57158(4) 0.0435(2) Uani 1 1 d . . . Cl14 Cl 0.64913(8) 0.27311(4) 0.66882(3) 0.03028(16) Uani 1 1 d . . . N1 N -0.0068(2) -0.02442(14) 0.17325(11) 0.0267(5) Uani 1 1 d . . . N2 N 0.8494(2) 0.51057(13) 0.65639(11) 0.0252(5) Uani 1 1 d . . . O1 O 0.3904(2) 0.06493(11) 0.12570(9) 0.0255(4) Uani 1 1 d . . . O2 O 0.6164(2) 0.13564(11) 0.04000(9) 0.0256(4) Uani 1 1 d . . . O4 O 0.8673(3) 0.66232(16) 0.20960(13) 0.0564(7) Uani 1 1 d . . . O5 O 0.7667(3) 0.87058(17) 0.37280(12) 0.0580(7) Uani 1 1 d . . . O6 O 0.0315(4) 0.3915(2) 0.12697(17) 0.0818(10) Uani 1 1 d . . . O11 O 0.59785(19) 0.36898(10) 0.41141(9) 0.0232(4) Uani 1 1 d . . . O12 O 0.72999(19) 0.34716(10) 0.53048(8) 0.0215(4) Uani 1 1 d . . . C1 C 0.4538(3) 0.07906(16) 0.17508(13) 0.0243(6) Uani 1 1 d . . . C2 C 0.4869(3) 0.01659(16) 0.23064(13) 0.0252(6) Uani 1 1 d . . . C3 C 0.5336(3) 0.03080(17) 0.28760(13) 0.0294(6) Uani 1 1 d . . . H3 H 0.5512 -0.0113 0.3236 0.080 Uiso 1 1 calc R . . C4 C 0.5537(3) 0.10934(18) 0.28993(13) 0.0300(6) Uani 1 1 d . . . C5 C 0.5370(3) 0.17052(17) 0.23472(14) 0.0290(6) Uani 1 1 d . . . H5 H 0.5577 0.2218 0.2362 0.080 Uiso 1 1 calc R . . C6 C 0.4893(3) 0.15631(16) 0.17675(13) 0.0255(6) Uani 1 1 d . . . C7 C 0.4793(3) 0.22409(16) 0.11852(13) 0.0267(6) Uani 1 1 d . . . C8 C 0.4145(4) 0.30454(17) 0.12980(15) 0.0342(7) Uani 1 1 d . . . H8 H 0.3661 0.3137 0.1719 0.080 Uiso 1 1 calc R . . C9 C 0.4213(4) 0.37022(17) 0.07943(16) 0.0385(7) Uani 1 1 d . . . C10 C 0.4929(4) 0.36005(18) 0.01669(15) 0.0392(7) Uani 1 1 d . . . H10 H 0.4988 0.4051 -0.0169 0.080 Uiso 1 1 calc R . . C11 C 0.5559(3) 0.28038(17) 0.00535(14) 0.0306(6) Uani 1 1 d . . . C12 C 0.5503(3) 0.21051(16) 0.05375(13) 0.0253(6) Uani 1 1 d . . . C13 C 0.1160(3) -0.05144(19) 0.11799(15) 0.0340(7) Uani 1 1 d . . . H13A H 0.1580 -0.0040 0.0962 0.080 Uiso 1 1 calc R . . H13B H 0.1961 -0.0921 0.1383 0.080 Uiso 1 1 calc R . . C14 C 0.0638(4) -0.0877(2) 0.06562(15) 0.0404(8) Uani 1 1 d . . . H14A H 0.0388 -0.1401 0.0850 0.080 Uiso 1 1 calc R . . H14B H 0.1427 -0.0953 0.0295 0.080 Uiso 1 1 calc R . . H14C H -0.0235 -0.0510 0.0489 0.080 Uiso 1 1 calc R . . C15 C -0.1241(3) 0.04777(17) 0.14499(15) 0.0325(7) Uani 1 1 d . . . H15A H -0.1653 0.0313 0.1096 0.080 Uiso 1 1 calc R . . H15B H -0.2058 0.0596 0.1801 0.080 Uiso 1 1 calc R . . C16 C -0.0664(4) 0.12645(19) 0.11717(18) 0.0459(8) Uani 1 1 d . . . H16A H -0.0300 0.1451 0.1522 0.080 Uiso 1 1 calc R . . H16B H -0.1468 0.1683 0.0996 0.080 Uiso 1 1 calc R . . H16C H 0.0140 0.1157 0.0821 0.080 Uiso 1 1 calc R . . C17 C 0.0702(3) -0.00080(19) 0.22524(15) 0.0347(7) Uani 1 1 d . . . H17A H 0.1424 -0.0488 0.2426 0.080 Uiso 1 1 calc R . . H17B H 0.1259 0.0413 0.2035 0.080 Uiso 1 1 calc R . . C18 C -0.0341(4) 0.0311(2) 0.28340(16) 0.0428(8) Uani 1 1 d . . . H18A H -0.0962 0.0832 0.2679 0.080 Uiso 1 1 calc R . . H18B H 0.0244 0.0382 0.3164 0.080 Uiso 1 1 calc R . . H18C H -0.0966 -0.0078 0.3029 0.080 Uiso 1 1 calc R . . C19 C -0.0898(3) -0.09362(17) 0.20403(15) 0.0320(6) Uani 1 1 d . . . H19A H -0.1670 -0.0739 0.2385 0.080 Uiso 1 1 calc R . . H19B H -0.1401 -0.1061 0.1697 0.080 Uiso 1 1 calc R . . C20 C 0.0078(4) -0.17257(19) 0.23436(18) 0.0469(8) Uani 1 1 d . . . H20A H 0.0907 -0.1900 0.2021 0.080 Uiso 1 1 calc R . . H20B H -0.0508 -0.2147 0.2472 0.080 Uiso 1 1 calc R . . H20C H 0.0456 -0.1632 0.2731 0.080 Uiso 1 1 calc R . . C21 C 0.7269(3) 0.33184(15) 0.38087(13) 0.0215(5) Uani 1 1 d . . . C22 C 0.7715(3) 0.35934(16) 0.31363(13) 0.0252(6) Uani 1 1 d . . . C23 C 0.8984(3) 0.32043(17) 0.27658(13) 0.0273(6) Uani 1 1 d . . . H23 H 0.9228 0.3402 0.2317 0.080 Uiso 1 1 calc R . . C24 C 0.9867(3) 0.25125(16) 0.30924(13) 0.0261(6) Uani 1 1 d . . . C25 C 0.9509(3) 0.22281(15) 0.37550(13) 0.0256(6) Uani 1 1 d . . . H25 H 1.0143 0.1771 0.3965 0.080 Uiso 1 1 calc R . . C26 C 0.8211(3) 0.26089(15) 0.41249(13) 0.0216(5) Uani 1 1 d . . . C27 C 0.7844(3) 0.22114(15) 0.48261(12) 0.0216(5) Uani 1 1 d . . . C28 C 0.8006(3) 0.13537(15) 0.49438(13) 0.0243(6) Uani 1 1 d . . . H28 H 0.8305 0.1058 0.4587 0.080 Uiso 1 1 calc R . . C29 C 0.7729(3) 0.09371(15) 0.55831(14) 0.0277(6) Uani 1 1 d . . . C30 C 0.7294(3) 0.13560(16) 0.61240(14) 0.0272(6) Uani 1 1 d . . . H30 H 0.7123 0.1075 0.6554 0.080 Uiso 1 1 calc R . . C31 C 0.7119(3) 0.22033(15) 0.60073(13) 0.0233(6) Uani 1 1 d . . . C32 C 0.7398(3) 0.26609(14) 0.53701(13) 0.0210(5) Uani 1 1 d . . . C33 C 0.8513(3) 0.43809(15) 0.62081(14) 0.0262(6) Uani 1 1 d . . . H33A H 0.7639 0.4145 0.6391 0.080 Uiso 1 1 calc R . . H33B H 0.8420 0.4588 0.5738 0.080 Uiso 1 1 calc R . . C34 C 0.9910(3) 0.37002(16) 0.62615(14) 0.0308(6) Uani 1 1 d . . . H34A H 1.0776 0.3914 0.6046 0.080 Uiso 1 1 calc R . . H34B H 0.9804 0.3256 0.6047 0.080 Uiso 1 1 calc R . . H34C H 1.0032 0.3499 0.6725 0.080 Uiso 1 1 calc R . . C35 C 0.9736(3) 0.55569(17) 0.62471(15) 0.0299(6) Uani 1 1 d . . . H35A H 0.9773 0.5966 0.6521 0.080 Uiso 1 1 calc R . . H35B H 1.0689 0.5164 0.6252 0.080 Uiso 1 1 calc R . . C36 C 0.9580(4) 0.59830(18) 0.55411(16) 0.0377(7) Uani 1 1 d . . . H36A H 0.9438 0.5598 0.5274 0.080 Uiso 1 1 calc R . . H36B H 1.0475 0.6189 0.5360 0.080 Uiso 1 1 calc R . . H36C H 0.8728 0.6435 0.5538 0.080 Uiso 1 1 calc R . . C37 C 0.8723(4) 0.48101(19) 0.72937(14) 0.0364(7) Uani 1 1 d . . . H37A H 0.9748 0.4503 0.7319 0.080 Uiso 1 1 calc R . . H37B H 0.8607 0.5289 0.7514 0.080 Uiso 1 1 calc R . . C38 C 0.7663(4) 0.4272(2) 0.76736(16) 0.0485(9) Uani 1 1 d . . . H38A H 0.6643 0.4574 0.7663 0.080 Uiso 1 1 calc R . . H38B H 0.7884 0.4115 0.8129 0.080 Uiso 1 1 calc R . . H38C H 0.7788 0.3786 0.7470 0.080 Uiso 1 1 calc R . . C39 C 0.6962(3) 0.56691(16) 0.64858(14) 0.0289(6) Uani 1 1 d . . . H39A H 0.6851 0.5822 0.6012 0.080 Uiso 1 1 calc R . . H39B H 0.6190 0.5360 0.6687 0.080 Uiso 1 1 calc R . . C40 C 0.6687(4) 0.64516(19) 0.67941(18) 0.0448(8) Uani 1 1 d . . . H40A H 0.6730 0.6310 0.7268 0.080 Uiso 1 1 calc R . . H40B H 0.5712 0.6777 0.6709 0.080 Uiso 1 1 calc R . . H40C H 0.7445 0.6764 0.6601 0.080 Uiso 1 1 calc R . . C41 C 0.7144(4) 0.6789(2) 0.23842(19) 0.0554(10) Uani 1 1 d . . . H41A H 0.6890 0.7329 0.2524 0.080 Uiso 1 1 calc R . . H41B H 0.6980 0.6377 0.2771 0.080 Uiso 1 1 calc R . . C42 C 0.6205(5) 0.6761(3) 0.1861(2) 0.0681(12) Uani 1 1 d . . . H42A H 0.5294 0.7185 0.1879 0.080 Uiso 1 1 calc R . . H42B H 0.5926 0.6226 0.1921 0.080 Uiso 1 1 calc R . . C43 C 0.7171(5) 0.6911(3) 0.1202(2) 0.0683(12) Uani 1 1 d . . . H43A H 0.7243 0.6473 0.0940 0.080 Uiso 1 1 calc R . . H43B H 0.6761 0.7435 0.0942 0.080 Uiso 1 1 calc R . . C44 C 0.8675(6) 0.6917(3) 0.1399(2) 0.0772(13) Uani 1 1 d . . . H44A H 0.9462 0.6565 0.1149 0.080 Uiso 1 1 calc R . . H44B H 0.8866 0.7474 0.1300 0.080 Uiso 1 1 calc R . . C51 C 0.6837(4) 0.80621(19) 0.38682(17) 0.0410(8) Uani 1 1 d . . . H51A H 0.7436 0.7568 0.3708 0.080 Uiso 1 1 calc R . . H51B H 0.5926 0.8228 0.3647 0.080 Uiso 1 1 calc R . . C52 C 0.6449(4) 0.7896(2) 0.46127(18) 0.0517(9) Uani 1 1 d . . . H52A H 0.6566 0.7308 0.4772 0.080 Uiso 1 1 calc R . . H52B H 0.5424 0.8168 0.4743 0.080 Uiso 1 1 calc R . . C53 C 0.7566(6) 0.8255(2) 0.4878(2) 0.0634(11) Uani 1 1 d . . . H53A H 0.7120 0.8490 0.5279 0.080 Uiso 1 1 calc R . . H53B H 0.8451 0.7836 0.4982 0.080 Uiso 1 1 calc R . . C54 C 0.7952(6) 0.8893(3) 0.4340(2) 0.0781(14) Uani 1 1 d . . . H54A H 0.7351 0.9428 0.4418 0.080 Uiso 1 1 calc R . . H54B H 0.9006 0.8914 0.4322 0.080 Uiso 1 1 calc R . . C61 C -0.0681(5) 0.4650(3) 0.1087(2) 0.0806(15) Uani 1 1 d . . . H61A H -0.0158 0.5025 0.0772 0.080 Uiso 1 1 calc R . . H61B H -0.1095 0.4912 0.1479 0.080 Uiso 1 1 calc R . . C62 C -0.1903(6) 0.4469(4) 0.0780(3) 0.0908(17) Uani 1 1 d . . . H62A H -0.2184 0.4889 0.0402 0.080 Uiso 1 1 calc R . . H62B H -0.2784 0.4434 0.1102 0.080 Uiso 1 1 calc R . . C63 C -0.1217(8) 0.3641(3) 0.0557(4) 0.124(3) Uani 1 1 d . . . H63A H -0.1779 0.3226 0.0783 0.080 Uiso 1 1 calc R . . H63B H -0.1212 0.3679 0.0077 0.080 Uiso 1 1 calc R . . C64 C 0.0362(6) 0.3430(3) 0.0745(3) 0.0826(15) Uani 1 1 d . . . H64A H 0.0652 0.2844 0.0908 0.080 Uiso 1 1 calc R . . H64B H 0.1070 0.3578 0.0365 0.080 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 0.0201(2) 0.02603(19) 0.02096(19) -0.00529(15) -0.00109(14) -0.00444(15) Fe2 0.01673(19) 0.01881(17) 0.02343(19) -0.00400(14) 0.00152(14) -0.00167(14) S1 0.0245(3) 0.0284(3) 0.0271(3) -0.0053(3) -0.0061(3) -0.0006(3) S2 0.0186(3) 0.0216(3) 0.0303(3) -0.0039(3) 0.0045(3) -0.0043(2) Cl1 0.0305(4) 0.0280(3) 0.0322(4) -0.0007(3) -0.0004(3) -0.0086(3) Cl2 0.0522(5) 0.0524(4) 0.0326(4) -0.0133(3) -0.0139(3) -0.0039(4) Cl3 0.0844(7) 0.0295(4) 0.0618(6) -0.0074(4) 0.0089(5) -0.0013(4) Cl4 0.0461(5) 0.0457(4) 0.0273(4) 0.0020(3) 0.0061(3) -0.0058(3) Cl11 0.0322(4) 0.0456(4) 0.0332(4) 0.0117(3) 0.0033(3) 0.0070(3) Cl12 0.0277(4) 0.0393(4) 0.0404(4) -0.0152(3) 0.0102(3) -0.0046(3) Cl13 0.0659(5) 0.0219(3) 0.0415(4) -0.0027(3) -0.0101(4) -0.0055(3) Cl14 0.0383(4) 0.0298(3) 0.0229(3) -0.0070(3) 0.0056(3) -0.0108(3) N1 0.0184(11) 0.0316(11) 0.0285(12) -0.0019(9) -0.0006(9) -0.0053(9) N2 0.0222(12) 0.0261(11) 0.0275(12) -0.0053(9) -0.0027(9) -0.0043(9) O1 0.0223(10) 0.0316(9) 0.0238(9) -0.0044(8) -0.0014(7) -0.0082(8) O2 0.0221(9) 0.0282(9) 0.0262(10) -0.0060(8) 0.0009(7) -0.0052(8) O4 0.0444(15) 0.0567(14) 0.0632(16) -0.0046(12) -0.0131(12) 0.0011(12) O5 0.0675(18) 0.0792(18) 0.0385(13) -0.0071(12) -0.0061(12) -0.0397(15) O6 0.076(2) 0.083(2) 0.078(2) 0.0088(18) -0.0052(17) -0.0174(18) O11 0.0181(9) 0.0260(9) 0.0232(9) -0.0063(7) -0.0002(7) 0.0005(7) O12 0.0200(9) 0.0200(8) 0.0243(9) -0.0054(7) -0.0007(7) -0.0029(7) C1 0.0190(13) 0.0294(13) 0.0219(13) -0.0054(10) 0.0035(10) -0.0018(11) C2 0.0197(13) 0.0290(13) 0.0250(13) -0.0042(11) 0.0030(10) -0.0047(11) C3 0.0261(15) 0.0353(15) 0.0227(14) -0.0022(11) 0.0012(11) -0.0020(12) C4 0.0263(15) 0.0400(15) 0.0233(14) -0.0092(12) -0.0019(11) -0.0029(12) C5 0.0277(15) 0.0302(14) 0.0291(15) -0.0100(11) 0.0000(11) -0.0037(12) C6 0.0213(13) 0.0292(13) 0.0233(13) -0.0064(11) 0.0035(10) -0.0012(11) C7 0.0247(14) 0.0282(13) 0.0275(14) -0.0067(11) -0.0007(11) -0.0055(11) C8 0.0405(17) 0.0299(14) 0.0302(15) -0.0072(12) 0.0003(13) -0.0036(13) C9 0.0450(19) 0.0248(14) 0.0423(18) -0.0065(13) 0.0011(14) -0.0025(13) C10 0.0466(19) 0.0312(15) 0.0354(17) 0.0030(13) -0.0017(14) -0.0069(14) C11 0.0297(15) 0.0353(15) 0.0247(14) -0.0012(12) 0.0001(11) -0.0067(12) C12 0.0222(14) 0.0299(13) 0.0255(14) -0.0046(11) -0.0042(11) -0.0074(11) C13 0.0186(14) 0.0444(16) 0.0338(16) -0.0026(13) 0.0048(12) -0.0033(12) C14 0.0291(16) 0.0531(18) 0.0360(17) -0.0122(14) 0.0055(13) -0.0034(14) C15 0.0231(15) 0.0331(14) 0.0378(16) -0.0006(12) -0.0074(12) 0.0003(12) C16 0.048(2) 0.0371(16) 0.052(2) 0.0051(15) -0.0149(16) -0.0093(15) C17 0.0274(15) 0.0405(16) 0.0385(17) -0.0028(13) -0.0102(13) -0.0098(13) C18 0.0436(19) 0.0525(19) 0.0371(17) -0.0094(14) -0.0045(14) -0.0180(15) C19 0.0277(15) 0.0326(14) 0.0345(16) -0.0022(12) 0.0035(12) -0.0108(12) C20 0.054(2) 0.0352(16) 0.0472(19) 0.0038(14) -0.0053(16) -0.0086(15) C21 0.0185(13) 0.0246(12) 0.0224(13) -0.0070(10) -0.0016(10) -0.0040(10) C22 0.0221(13) 0.0258(13) 0.0264(14) -0.0020(11) -0.0038(11) -0.0028(11) C23 0.0230(14) 0.0349(14) 0.0248(14) -0.0072(11) 0.0008(11) -0.0073(11) C24 0.0210(14) 0.0305(13) 0.0283(14) -0.0127(11) 0.0045(11) -0.0064(11) C25 0.0228(14) 0.0226(12) 0.0305(14) -0.0077(11) -0.0014(11) -0.0012(11) C26 0.0194(13) 0.0220(12) 0.0239(13) -0.0076(10) 0.0000(10) -0.0038(10) C27 0.0172(12) 0.0237(12) 0.0223(13) -0.0026(10) -0.0039(10) -0.0005(10) C28 0.0225(13) 0.0245(13) 0.0258(14) -0.0073(11) -0.0030(11) -0.0017(11) C29 0.0309(15) 0.0205(12) 0.0314(15) -0.0029(11) -0.0067(12) -0.0032(11) C30 0.0268(15) 0.0267(13) 0.0266(14) 0.0001(11) -0.0026(11) -0.0056(11) C31 0.0227(13) 0.0258(13) 0.0208(13) -0.0059(10) -0.0010(10) -0.0027(11) C32 0.0154(12) 0.0196(12) 0.0264(13) -0.0034(10) -0.0019(10) -0.0005(10) C33 0.0244(14) 0.0241(13) 0.0316(14) -0.0066(11) -0.0004(11) -0.0078(11) C34 0.0299(15) 0.0262(13) 0.0345(15) -0.0021(11) -0.0016(12) -0.0053(12) C35 0.0211(14) 0.0288(13) 0.0422(17) -0.0090(12) -0.0036(12) -0.0072(11) C36 0.0316(16) 0.0359(15) 0.0454(18) -0.0026(13) 0.0031(14) -0.0144(13) C37 0.0396(17) 0.0410(16) 0.0274(15) -0.0080(13) -0.0074(13) -0.0007(14) C38 0.056(2) 0.0507(19) 0.0327(17) -0.0026(15) 0.0049(15) -0.0087(17) C39 0.0182(14) 0.0309(14) 0.0364(15) -0.0076(12) -0.0015(11) -0.0017(11) C40 0.0400(19) 0.0414(17) 0.054(2) -0.0248(15) -0.0094(15) 0.0064(15) C41 0.046(2) 0.062(2) 0.055(2) -0.0057(18) -0.0102(17) -0.0043(18) C42 0.060(3) 0.093(3) 0.051(2) -0.002(2) -0.0117(19) -0.020(2) C43 0.062(3) 0.081(3) 0.059(3) -0.005(2) -0.011(2) -0.010(2) C44 0.069(3) 0.113(4) 0.060(3) -0.022(3) -0.001(2) -0.038(3) C51 0.0367(18) 0.0378(16) 0.0499(19) -0.0084(14) -0.0132(15) -0.0034(14) C52 0.054(2) 0.055(2) 0.052(2) 0.0011(17) -0.0153(17) -0.0246(17) C53 0.092(3) 0.057(2) 0.053(2) 0.0041(18) -0.023(2) -0.039(2) C54 0.108(4) 0.103(3) 0.047(2) 0.003(2) -0.023(2) -0.071(3) C61 0.064(3) 0.099(4) 0.062(3) 0.000(3) 0.000(2) 0.002(3) C62 0.071(3) 0.111(4) 0.075(3) -0.002(3) -0.012(3) 0.006(3) C63 0.116(5) 0.078(3) 0.194(7) 0.014(4) -0.096(5) -0.033(4) C64 0.074(3) 0.074(3) 0.092(4) -0.003(3) -0.004(3) -0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.8992(17) . ? Fe1 O2 1.9112(19) . ? Fe1 S1 2.2073(8) 2_655 ? Fe1 S1 2.2129(7) . ? Fe1 Fe1 2.6688(8) 2_655 ? Fe2 O11 1.8976(18) . ? Fe2 O12 1.8996(17) . ? Fe2 S2 2.2179(7) 2_666 ? Fe2 S2 2.2207(7) . ? Fe2 Fe2 2.7146(7) 2_666 ? S1 Fe1 2.2073(8) 2_655 ? S2 Fe2 2.2179(7) 2_666 ? Cl1 C2 1.745(3) . ? Cl2 C4 1.739(3) . ? Cl3 C9 1.752(3) . ? Cl4 C11 1.744(3) . ? Cl11 C22 1.745(2) . ? Cl12 C24 1.743(2) . ? Cl13 C29 1.741(3) . ? Cl14 C31 1.743(3) . ? N1 C17 1.511(4) . ? N1 C15 1.520(3) . ? N1 C19 1.523(4) . ? N1 C13 1.527(3) . ? N2 C35 1.511(4) . ? N2 C37 1.515(4) . ? N2 C39 1.520(3) . ? N2 C33 1.523(3) . ? O1 C1 1.317(3) . ? O2 C12 1.329(3) . ? O4 C44 1.422(5) . ? O4 C41 1.426(4) . ? O5 C54 1.417(5) . ? O5 C51 1.423(4) . ? O6 C61 1.389(5) . ? O6 C64 1.451(6) . ? O11 C21 1.332(3) . ? O12 C32 1.329(3) . ? C1 C6 1.415(4) . ? C1 C2 1.418(4) . ? C2 C3 1.374(4) . ? C3 C4 1.383(4) . ? C4 C5 1.384(4) . ? C5 C6 1.398(4) . ? C6 C7 1.489(4) . ? C7 C8 1.396(4) . ? C7 C12 1.421(4) . ? C8 C9 1.372(4) . ? C9 C10 1.374(4) . ? C10 C11 1.381(4) . ? C11 C12 1.397(4) . ? C13 C14 1.505(5) . ? C15 C16 1.518(4) . ? C17 C18 1.511(4) . ? C19 C20 1.510(4) . ? C21 C22 1.400(4) . ? C21 C26 1.418(3) . ? C22 C23 1.391(4) . ? C23 C24 1.382(4) . ? C24 C25 1.370(4) . ? C25 C26 1.403(3) . ? C26 C27 1.492(3) . ? C27 C28 1.395(4) . ? C27 C32 1.417(4) . ? C28 C29 1.383(4) . ? C29 C30 1.380(4) . ? C30 C31 1.377(4) . ? C31 C32 1.408(4) . ? C33 C34 1.517(4) . ? C35 C36 1.502(4) . ? C37 C38 1.510(5) . ? C39 C40 1.515(4) . ? C41 C42 1.481(6) . ? C42 C43 1.514(6) . ? C43 C44 1.496(6) . ? C51 C52 1.501(5) . ? C52 C53 1.505(6) . ? C53 C54 1.454(5) . ? C61 C62 1.474(8) . ? C62 C63 1.515(8) . ? C63 C64 1.502(7) . ? 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 96.31(8) . . ? O1 Fe1 S1 109.50(6) . 2_655 ? O2 Fe1 S1 119.50(6) . 2_655 ? O1 Fe1 S1 115.12(6) . . ? O2 Fe1 S1 110.96(6) . . ? S1 Fe1 S1 105.72(3) 2_655 . ? O1 Fe1 Fe1 128.91(6) . 2_655 ? O2 Fe1 Fe1 134.74(6) . 2_655 ? S1 Fe1 Fe1 52.95(2) 2_655 2_655 ? S1 Fe1 Fe1 52.76(2) . 2_655 ? O11 Fe2 O12 95.29(7) . . ? O11 Fe2 S2 113.79(6) . 2_666 ? O12 Fe2 S2 115.99(6) . 2_666 ? O11 Fe2 S2 116.43(6) . . ? O12 Fe2 S2 111.13(6) . . ? S2 Fe2 S2 104.59(2) 2_666 . ? O11 Fe2 Fe2 133.93(5) . 2_666 ? O12 Fe2 Fe2 130.76(6) . 2_666 ? S2 Fe2 Fe2 52.34(2) 2_666 2_666 ? S2 Fe2 Fe2 52.25(2) . 2_666 ? Fe1 S1 Fe1 74.28(3) 2_655 . ? Fe2 S2 Fe2 75.41(2) 2_666 . ? C17 N1 C15 111.2(2) . . ? C17 N1 C19 110.7(2) . . ? C15 N1 C19 106.5(2) . . ? C17 N1 C13 106.9(2) . . ? C15 N1 C13 110.5(2) . . ? C19 N1 C13 111.1(2) . . ? C35 N2 C37 107.9(2) . . ? C35 N2 C39 110.4(2) . . ? C37 N2 C39 111.5(2) . . ? C35 N2 C33 110.9(2) . . ? C37 N2 C33 110.8(2) . . ? C39 N2 C33 105.4(2) . . ? C1 O1 Fe1 120.60(16) . . ? C12 O2 Fe1 121.53(17) . . ? C44 O4 C41 106.8(3) . . ? C54 O5 C51 109.0(3) . . ? C61 O6 C64 104.7(4) . . ? C21 O11 Fe2 124.59(17) . . ? C32 O12 Fe2 123.85(17) . . ? O1 C1 C6 122.8(2) . . ? O1 C1 C2 120.6(2) . . ? C6 C1 C2 116.6(3) . . ? C3 C2 C1 123.2(3) . . ? C3 C2 Cl1 119.2(2) . . ? C1 C2 Cl1 117.5(2) . . ? C2 C3 C4 118.3(2) . . ? C3 C4 C5 120.8(3) . . ? C3 C4 Cl2 119.7(2) . . ? C5 C4 Cl2 119.6(2) . . ? C4 C5 C6 120.9(3) . . ? C5 C6 C1 119.6(2) . . ? C5 C6 C7 117.9(2) . . ? C1 C6 C7 122.6(2) . . ? C8 C7 C12 119.3(2) . . ? C8 C7 C6 118.7(2) . . ? C12 C7 C6 121.6(2) . . ? C9 C8 C7 120.6(3) . . ? C8 C9 C10 121.9(3) . . ? C8 C9 Cl3 119.3(2) . . ? C10 C9 Cl3 118.7(2) . . ? C9 C10 C11 117.4(3) . . ? C10 C11 C12 123.8(3) . . ? C10 C11 Cl4 117.6(2) . . ? C12 C11 Cl4 118.6(2) . . ? O2 C12 C11 120.7(2) . . ? O2 C12 C7 122.3(2) . . ? C11 C12 C7 116.9(2) . . ? C14 C13 N1 114.7(2) . . ? C16 C15 N1 114.9(2) . . ? C18 C17 N1 115.0(3) . . ? C20 C19 N1 115.1(2) . . ? O11 C21 C22 120.5(2) . . ? O11 C21 C26 122.8(2) . . ? C22 C21 C26 116.7(2) . . ? C23 C22 C21 124.2(2) . . ? C23 C22 Cl11 117.0(2) . . ? C21 C22 Cl11 118.83(19) . . ? C24 C23 C22 117.3(2) . . ? C25 C24 C23 121.2(2) . . ? C25 C24 Cl12 120.0(2) . . ? C23 C24 Cl12 118.8(2) . . ? C24 C25 C26 121.6(2) . . ? C25 C26 C21 119.1(2) . . ? C25 C26 C27 117.7(2) . . ? C21 C26 C27 123.1(2) . . ? C28 C27 C32 119.5(2) . . ? C28 C27 C26 117.5(2) . . ? C32 C27 C26 123.0(2) . . ? C29 C28 C27 120.9(2) . . ? C30 C29 C28 121.1(2) . . ? C30 C29 Cl13 118.8(2) . . ? C28 C29 Cl13 120.1(2) . . ? C31 C30 C29 118.0(2) . . ? C30 C31 C32 123.6(2) . . ? C30 C31 Cl14 117.7(2) . . ? C32 C31 Cl14 118.73(19) . . ? O12 C32 C31 119.9(2) . . ? O12 C32 C27 123.1(2) . . ? C31 C32 C27 116.9(2) . . ? C34 C33 N2 114.9(2) . . ? C36 C35 N2 115.1(2) . . ? C38 C37 N2 115.0(3) . . ? C40 C39 N2 115.1(2) . . ? O4 C41 C42 106.8(3) . . ? C41 C42 C43 105.6(4) . . ? C44 C43 C42 104.2(4) . . ? O4 C44 C43 108.3(4) . . ? O5 C51 C52 107.5(3) . . ? C51 C52 C53 103.4(3) . . ? C54 C53 C52 104.6(3) . . ? O5 C54 C53 108.6(3) . . ? O6 C61 C62 108.8(5) . . ? C61 C62 C63 103.2(4) . . ? C64 C63 C62 105.3(5) . . ? O6 C64 C63 104.4(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.79 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.622 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.072