# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jun Tao' _publ_contact_author_email TAOJUN@XMU.EDU.CN _publ_section_title ; An Iron(II) Incomplete Spin-Crossover Compound: Pressure Effects and Mossbauer Spectra Study ; loop_ _publ_author_name 'Jun Tao.' 'Yasuaki Einaga' 'Taro Hanajima' 'Rong-Bin Huang.' 'Bao Li.' ; Feng-Lei Yang ; 'Lan-Sun Zheng.' data_1 _database_code_depnum_ccdc_archive 'CCDC 755408' #TrackingRef '105K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H40 Fe N12 O7 S2' _chemical_formula_weight 896.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 11.9078(2) _cell_length_b 9.94740(10) _cell_length_c 17.7290(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.361(2) _cell_angle_gamma 90.00 _cell_volume 2051.35(5) _cell_formula_units_Z 2 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used 2643 _cell_measurement_theta_min 3.80 _cell_measurement_theta_max 62.22 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 932 _exptl_absorpt_coefficient_mu 4.445 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.3053 _exptl_absorpt_correction_T_max 0.6649 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008, 18:23:10) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 105(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\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 9679 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.80 _diffrn_reflns_theta_max 62.22 _reflns_number_total 3240 _reflns_number_gt 2643 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. The solvent water molecules are difficult to be identified, so the data were refined with PLATONT SQUEEZE. The S1 atom is highly disordered. Checkcif reports 301 A**3 voids , which is attributed to the unidentified solvent water molecules. Checkcif also reports a lower than usual U(eq) value for C19. This is probably due to reason that it is able to move about its position slightly. ; _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^)+(0.1067P)^2^+1.5389P] 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 3240 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0736 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1890 _refine_ls_wR_factor_gt 0.1803 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.5000 0.52760(7) 0.7500 0.0428(3) Uani 1 2 d S . . N1 N 0.3912(3) 0.6750(3) 0.77995(18) 0.0502(8) Uani 1 1 d . . . N2 N 0.3880(3) 1.3800(3) 0.77583(18) 0.0475(8) Uani 1 1 d . . . N3 N -0.3066(4) 1.0412(6) 0.9631(2) 0.0824(14) Uani 1 1 d . . . N4 N 0.0629(3) 0.9211(4) 0.87063(19) 0.0567(9) Uani 1 1 d . . . H4B H 0.0449 0.8402 0.8805 0.068 Uiso 1 1 calc R . . N5 N 0.0556(3) 1.1422(3) 0.86022(18) 0.0506(8) Uani 1 1 d . . . C1 C 0.3473(4) 0.6600(4) 0.8447(2) 0.0583(11) Uani 1 1 d . . . H1A H 0.3707 0.5860 0.8763 0.070 Uiso 1 1 calc R . . C2 C 0.2711(4) 0.7476(4) 0.8655(2) 0.0585(11) Uani 1 1 d . . . H2A H 0.2414 0.7310 0.9091 0.070 Uiso 1 1 calc R . . C3 C 0.2384(4) 0.8611(4) 0.8214(2) 0.0521(10) Uani 1 1 d . . . C4 C 0.2843(4) 0.8800(4) 0.7562(2) 0.0524(10) Uani 1 1 d . . . H4A H 0.2654 0.9560 0.7256 0.063 Uiso 1 1 calc R . . C5 C 0.3583(4) 0.7846(4) 0.7376(2) 0.0511(9) Uani 1 1 d . . . H5A H 0.3867 0.7976 0.6932 0.061 Uiso 1 1 calc R . . C6 C 0.4243(4) 1.2719(4) 0.8189(2) 0.0527(10) Uani 1 1 d . . . H6A H 0.5031 1.2604 0.8362 0.063 Uiso 1 1 calc R . . C7 C 0.3525(3) 1.1763(4) 0.8395(2) 0.0505(9) Uani 1 1 d . . . H7A H 0.3828 1.1025 0.8692 0.061 Uiso 1 1 calc R . . C8 C 0.2338(3) 1.1920(4) 0.8150(2) 0.0465(9) Uani 1 1 d . . . C9 C 0.1954(3) 1.3049(4) 0.7707(2) 0.0479(9) Uani 1 1 d . . . H9A H 0.1170 1.3200 0.7536 0.057 Uiso 1 1 calc R . . C10 C 0.2729(3) 1.3935(4) 0.7523(2) 0.0488(9) Uani 1 1 d . . . H10A H 0.2449 1.4672 0.7218 0.059 Uiso 1 1 calc R . . C11 C -0.2617(4) 1.1531(7) 0.9397(3) 0.0783(15) Uani 1 1 d . . . H11A H -0.3006 1.2338 0.9411 0.094 Uiso 1 1 calc R . . C12 C -0.1597(4) 1.1550(5) 0.9134(2) 0.0648(12) Uani 1 1 d . . . H12A H -0.1315 1.2352 0.8980 0.078 Uiso 1 1 calc R . . C13 C -0.1002(4) 1.0345(5) 0.9105(2) 0.0587(11) Uani 1 1 d . . . C14 C -0.1465(5) 0.9188(6) 0.9360(3) 0.0701(13) Uani 1 1 d . . . H14A H -0.1097 0.8365 0.9353 0.084 Uiso 1 1 calc R . . C15 C -0.2466(5) 0.9270(7) 0.9620(3) 0.0833(17) Uani 1 1 d . . . H15A H -0.2749 0.8488 0.9800 0.100 Uiso 1 1 calc R . . C16 C 0.1564(4) 0.9580(4) 0.8421(2) 0.0516(10) Uani 1 1 d . . . C17 C 0.0042(4) 1.0323(4) 0.8806(2) 0.0535(10) Uani 1 1 d . . . C18 C 0.1527(3) 1.0966(4) 0.8366(2) 0.0488(9) Uani 1 1 d . . . N6 N 0.5900(3) 0.5278(3) 0.8583(2) 0.0495(8) Uani 1 1 d . . . C19 C 0.6393(6) 0.5424(5) 0.9188(4) 0.0830(16) Uani 1 1 d . . . S1 S 0.7077(4) 0.5629(3) 1.00887(12) 0.227(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0522(5) 0.0254(4) 0.0471(5) 0.000 0.0026(4) 0.000 N1 0.068(2) 0.0301(16) 0.0469(18) 0.0040(13) -0.0006(15) 0.0005(15) N2 0.0513(18) 0.0378(17) 0.0509(18) -0.0031(14) 0.0053(14) 0.0074(14) N3 0.074(3) 0.117(4) 0.056(2) 0.003(2) 0.011(2) -0.022(3) N4 0.067(2) 0.0431(19) 0.055(2) 0.0060(16) 0.0027(17) -0.0044(17) N5 0.0548(19) 0.0479(18) 0.0469(17) 0.0019(14) 0.0057(15) 0.0005(16) C1 0.089(3) 0.0291(19) 0.053(2) 0.0018(17) 0.005(2) 0.005(2) C2 0.083(3) 0.039(2) 0.051(2) -0.0006(18) 0.009(2) 0.000(2) C3 0.067(2) 0.035(2) 0.050(2) -0.0042(16) 0.0023(19) -0.0006(18) C4 0.065(2) 0.033(2) 0.052(2) 0.0027(17) -0.0014(19) 0.0050(18) C5 0.063(2) 0.036(2) 0.050(2) -0.0005(16) 0.0020(18) -0.0023(18) C6 0.053(2) 0.040(2) 0.061(2) -0.0012(18) 0.0043(19) 0.0083(18) C7 0.055(2) 0.034(2) 0.059(2) 0.0041(17) 0.0042(18) 0.0082(17) C8 0.055(2) 0.0368(19) 0.045(2) -0.0066(16) 0.0051(17) 0.0037(17) C9 0.050(2) 0.039(2) 0.050(2) -0.0008(17) 0.0016(17) 0.0076(17) C10 0.057(2) 0.0334(19) 0.053(2) 0.0007(16) 0.0039(18) 0.0097(17) C11 0.068(3) 0.110(4) 0.055(3) 0.001(3) 0.009(2) 0.002(3) C12 0.064(3) 0.080(3) 0.049(2) 0.007(2) 0.010(2) -0.002(2) C13 0.063(3) 0.067(3) 0.041(2) 0.0048(19) 0.0010(19) -0.008(2) C14 0.084(3) 0.074(3) 0.048(2) 0.004(2) 0.002(2) -0.020(3) C15 0.086(4) 0.110(5) 0.050(3) 0.000(3) 0.007(3) -0.048(4) C16 0.061(2) 0.041(2) 0.048(2) 0.0018(17) 0.0008(19) 0.0019(18) C17 0.057(2) 0.050(2) 0.047(2) 0.0012(18) -0.0019(18) -0.0039(19) C18 0.055(2) 0.046(2) 0.043(2) -0.0001(17) 0.0044(17) 0.0026(18) N6 0.061(2) 0.0396(18) 0.0443(19) -0.0040(14) 0.0019(16) -0.0016(15) C19 0.115(5) 0.043(3) 0.090(4) 0.014(3) 0.019(4) -0.016(3) S1 0.387(5) 0.163(2) 0.0781(12) 0.0371(13) -0.071(2) -0.145(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 N6 1.989(4) 2_656 ? Fe1 N6 1.989(4) . ? Fe1 N1 2.099(3) 2_656 ? Fe1 N1 2.099(3) . ? Fe1 N2 2.099(3) 1_545 ? Fe1 N2 2.099(3) 2_646 ? N1 C5 1.334(5) . ? N1 C1 1.368(5) . ? N2 C6 1.337(5) . ? N2 C10 1.351(5) . ? N2 Fe1 2.099(3) 1_565 ? N3 C11 1.339(7) . ? N3 C15 1.344(8) . ? N4 C17 1.340(6) . ? N4 C16 1.368(5) . ? N5 C17 1.340(5) . ? N5 C18 1.387(5) . ? C1 C2 1.365(6) . ? C2 C3 1.381(6) . ? C3 C4 1.394(6) . ? C3 C16 1.473(6) . ? C4 C5 1.382(6) . ? C6 C7 1.378(6) . ? C7 C8 1.397(5) . ? C8 C9 1.390(5) . ? C8 C18 1.463(6) . ? C9 C10 1.365(6) . ? C11 C12 1.391(6) . ? C12 C13 1.399(7) . ? C13 C14 1.393(7) . ? C13 C17 1.452(6) . ? C14 C15 1.370(8) . ? C16 C18 1.382(6) . ? N6 C19 1.116(7) . ? C19 S1 1.642(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 N6 Fe1 N6 179.91(18) 2_656 . ? N6 Fe1 N1 89.38(13) 2_656 2_656 ? N6 Fe1 N1 90.55(13) . 2_656 ? N6 Fe1 N1 90.55(13) 2_656 . ? N6 Fe1 N1 89.38(13) . . ? N1 Fe1 N1 91.34(18) 2_656 . ? N6 Fe1 N2 88.57(13) 2_656 1_545 ? N6 Fe1 N2 91.50(13) . 1_545 ? N1 Fe1 N2 177.95(12) 2_656 1_545 ? N1 Fe1 N2 88.74(12) . 1_545 ? N6 Fe1 N2 91.50(13) 2_656 2_646 ? N6 Fe1 N2 88.57(13) . 2_646 ? N1 Fe1 N2 88.74(12) 2_656 2_646 ? N1 Fe1 N2 177.95(12) . 2_646 ? N2 Fe1 N2 91.25(17) 1_545 2_646 ? C5 N1 C1 116.3(3) . . ? C5 N1 Fe1 123.5(3) . . ? C1 N1 Fe1 120.2(2) . . ? C6 N2 C10 116.0(3) . . ? C6 N2 Fe1 123.0(3) . 1_565 ? C10 N2 Fe1 120.9(3) . 1_565 ? C11 N3 C15 116.7(5) . . ? C17 N4 C16 108.4(3) . . ? C17 N5 C18 105.8(3) . . ? C2 C1 N1 123.6(4) . . ? C1 C2 C3 119.5(4) . . ? C2 C3 C4 117.8(4) . . ? C2 C3 C16 121.1(4) . . ? C4 C3 C16 121.1(4) . . ? C5 C4 C3 119.3(4) . . ? N1 C5 C4 123.5(4) . . ? N2 C6 C7 124.3(4) . . ? C6 C7 C8 119.0(4) . . ? C9 C8 C7 117.0(4) . . ? C9 C8 C18 121.1(3) . . ? C7 C8 C18 121.8(3) . . ? C10 C9 C8 119.9(4) . . ? N2 C10 C9 123.7(3) . . ? N3 C11 C12 123.4(6) . . ? C11 C12 C13 119.1(5) . . ? C14 C13 C12 117.2(5) . . ? C14 C13 C17 122.4(5) . . ? C12 C13 C17 120.4(4) . . ? C15 C14 C13 119.6(6) . . ? N3 C15 C14 123.9(5) . . ? N4 C16 C18 106.1(4) . . ? N4 C16 C3 123.4(3) . . ? C18 C16 C3 130.4(4) . . ? N5 C17 N4 110.9(4) . . ? N5 C17 C13 124.2(4) . . ? N4 C17 C13 124.9(4) . . ? C16 C18 N5 108.7(4) . . ? C16 C18 C8 130.7(4) . . ? N5 C18 C8 120.4(3) . . ? C19 N6 Fe1 172.5(4) . . ? N6 C19 S1 178.0(6) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 62.22 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.606 _refine_diff_density_min -0.915 _refine_diff_density_rms 0.062 #_eof #End of Crystallographic Information File