# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Martha Elena Sosa-Torres' _publ_contact_author_email MEST@SERVIDOR.UNAM.MX _publ_section_title ; Magnetic and high-frequency EPR studies of an octahedral Fe(III) compound with unusual zero field splitting parameters ; loop_ _publ_author_name 'Martha Elena Sosa-Torres' 'Hassane El-Mkami' 'Roberto Escudero' 'Herbert Hopfl' ; J.P.Saucedo-Vazquez ; 'Graham Smith' 'A Solano-Peralta' # Attachment 'zuntresm3.cif' data_zuntresm _database_code_depnum_ccdc_archive 'CCDC 659005' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H36 Fe O6 S6, 3 (N O3)' _chemical_formula_sum 'C12 H36 Fe N3 O15 S6' _chemical_formula_weight 710.65 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' 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 11.3913(6) _cell_length_b 11.3913(6) _cell_length_c 19.6535(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2208.6(2) _cell_formula_units_Z 3 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4611 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 28.1 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1113 _exptl_absorpt_coefficient_mu 1.004 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6896 _exptl_absorpt_correction_T_max 0.8169 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6452 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0132 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 25.00 _reflns_number_total 864 _reflns_number_gt 842 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+8.8007P] 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 864 _refine_ls_number_parameters 76 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0306 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0795 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 1.0000 1.0000 0.0000 0.0157(2) Uani 1 6 d S . . S1 S 0.73066(6) 0.81643(5) 0.07946(3) 0.0194(2) Uani 1 1 d . . . O1 O 0.87054(15) 0.84107(15) 0.05619(8) 0.0193(4) Uani 1 1 d . . . C1 C 0.6121(2) 0.6849(3) 0.02578(13) 0.0274(6) Uani 1 1 d . . . H1A H 0.6213 0.7192 -0.0208 0.035(8) Uiso 1 1 calc R . . H1B H 0.5200 0.6539 0.0422 0.046(9) Uiso 1 1 calc R . . H1C H 0.6297 0.6090 0.0263 0.043(9) Uiso 1 1 calc R . . C2 C 0.7022(3) 0.7241(3) 0.15604(12) 0.0296(6) Uani 1 1 d . . . H2A H 0.7110 0.6441 0.1475 0.030(7) Uiso 1 1 calc R . . H2B H 0.6108 0.6954 0.1729 0.052(10) Uiso 1 1 calc R . . H2C H 0.7691 0.7817 0.1901 0.034(8) Uiso 1 1 calc R . . N1 N 0.6667 0.3333 0.08254(17) 0.0220(7) Uani 1 3 d S . . O2 O 0.66524(18) 0.44223(18) 0.08259(9) 0.0305(4) Uani 1 1 d . . . N2 N 0.3333 0.6667 0.1667 0.0437(16) Uani 1 6 d SD . . O3A O 0.2862(10) 0.6883(12) 0.1139(4) 0.058(2) Uani 0.167 1 d PD . . O3B O 0.2551(8) 0.5839(13) 0.2097(5) 0.058(2) Uani 0.167 1 d PD . . O3C O 0.45831(18) 0.7183(13) 0.1736(6) 0.058(2) Uani 0.167 1 d PD . . 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 0.0145(3) 0.0145(3) 0.0181(4) 0.000 0.000 0.00727(14) S1 0.0198(3) 0.0170(3) 0.0213(3) 0.0019(2) 0.0040(2) 0.0090(2) O1 0.0171(8) 0.0182(8) 0.0226(8) 0.0035(6) 0.0020(6) 0.0087(6) C1 0.0225(12) 0.0258(13) 0.0298(13) 0.0003(10) -0.0060(10) 0.0091(10) C2 0.0351(14) 0.0259(13) 0.0182(12) 0.0044(10) 0.0047(10) 0.0079(11) N1 0.0222(11) 0.0222(11) 0.0218(17) 0.000 0.000 0.0111(6) O2 0.0298(10) 0.0209(9) 0.0435(11) 0.0013(8) 0.0017(8) 0.0147(8) N2 0.0240(18) 0.0240(18) 0.083(5) 0.000 0.000 0.0120(9) O3A 0.075(6) 0.059(7) 0.049(4) 0.005(5) 0.009(5) 0.042(6) O3B 0.075(6) 0.059(7) 0.049(4) 0.005(5) 0.009(5) 0.042(6) O3C 0.075(6) 0.059(7) 0.049(4) 0.005(5) 0.009(5) 0.042(6) _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 2.0006(15) 11_565 ? S1 O1 1.5426(16) . ? S1 C2 1.771(2) . ? S1 C1 1.777(2) . ? N1 O2 1.2487(17) 3_665 ? N2 O3C 1.2465(9) 14_455 ? N2 O3A 1.2472(9) . ? O3A O3B 0.41(2) 14_455 ? 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 O1 87.54(6) 11_565 3_675 ? O1 Fe1 O1 180.00(10) 11_565 2_765 ? O1 Fe1 O1 92.46(6) 3_675 2_765 ? O1 Fe1 O1 87.54(6) 11_565 . ? O1 S1 C2 103.05(11) . . ? O1 S1 C1 104.93(11) . . ? C2 S1 C1 99.65(12) . . ? S1 O1 Fe1 123.73(9) . . ? O2 N1 O2 120.000(2) 3_665 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 S1 O1 Fe1 -151.88(12) . . . . ? C1 S1 O1 Fe1 104.24(13) . . . . ? O1 Fe1 O1 S1 -42.88(8) 11_565 . . . ? O1 Fe1 O1 S1 44.55(14) 3_675 . . . ? O1 Fe1 O1 S1 137.12(8) 2_765 . . . ? O1 Fe1 O1 S1 -135.45(14) 12_655 . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.652 _refine_diff_density_min -0.692 _refine_diff_density_rms 0.066