# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 1145/237 data_General _audit_creation_date 'Tue Mar 7 22:27:23 2000' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name ' Yoshiteru Sakata' _publ_contact_author_address ; The Institute of Scientific and Industrial Research (ISIR), Osaka University, 8-1 Mihogaoka, Ibaraki, Osaka 567-0047, Japan ; _publ_contact_author_email ' sakata@sanken.osaka-u.ac.jp ' _publ_contact_author_fax ' +(81)-6-6879-8479 ' _publ_contact_author_phone ' +(81)-6-6879-8475 ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' Submitted as a Full Paper of Journal of Materials Chemistry' _publ_requested_category ' supporting material' _publ_requested_coeditor_name ? #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; Ferrimagnetic Ordering of a Methylthio-Substituted Planar Porphyrin Based Electron Transfer Salt, Octakis(2,3,7,8,12,13,17,18-methylthio)porphyrinatomanganese(III) Tetracyanoethanide ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' Ken-ichi Sugiura ' ; ? ; ; The Institute of Scientific and Industrial Research (ISIR), Osaka University, 8-1 Mihogaoka, Ibaraki, Osaka 567-0047, Japan ; ' Kantaro Ushiroda ' ; ? ; ; The Institute of Scientific and Industrial Research (ISIR), Osaka University, 8-1 Mihogaoka, Ibaraki, Osaka 567-0047, Japan ; ' Mitchell T. Johnson ' ; ? ; ; Department of Chemistry, University of Utah, Salt Lake City, UT 84112-0850, U.S.A. ; ' Joel. S. Miller ' ; ? ; ; Department of Chemistry, University of Utah, Salt Lake City, UT 84112-0850, U.S.A. ; ' Yoshiteru Sakata ' ; ? ; ; The Institute of Scientific and Industrial Research (ISIR), Osaka University, 8-1 Mihogaoka, Ibaraki, Osaka 567-0047, Japan ; ' Ken-ichi Sugiura ' ; ? ; ; The Institute of Scientific and Industrial Research (ISIR), Osaka University, 8-1 Mihogaoka, Ibaraki, Osaka 567-0047, Japan ; _publ_section_synopsis ; ENTER SYNOPSIS ; #------------------------------------------------------------------------------ # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #------------------------------------------------------------------------------ data_OMTP-TCN #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C34 H28 N8 Mn S8 ' _chemical_formula_moiety '?' _chemical_formula_weight 860.07 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C 2/m 2/c 21/a' _symmetry_Int_Tables_number 64 loop_ _symmetry_equiv_pos_as_xyz x,y,z x,-y,-z x,1/2-y,1/2+z x,1/2+y,1/2-z -x,-y,-z -x,y,z -x,1/2+y,1/2-z -x,1/2-y,1/2+z 1/2+x,1/2+y,z 1/2+x,1/2-y,-z 1/2+x,-y,1/2+z 1/2+x,y,1/2-z 1/2-x,1/2-y,-z 1/2-x,1/2+y,z 1/2-x,y,1/2-z 1/2-x,-y,1/2+z _cell_length_a 25.495(2) _cell_length_b 9.3495(7) _cell_length_c 15.859(1) _cell_angle_alpha 89 _cell_angle_beta 89 _cell_angle_gamma 90 _cell_volume 3780.2(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 198.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.030 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.830 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-IV Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 0.010000 _diffrn_reflns_number 2077 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 27.51 _diffrn_measured_fraction_theta_max 0.8827 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.8827 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 0 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 1.5 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1965 _reflns_number_gt 1245 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.0634 _refine_ls_hydrogen_treatment ? _refine_ls_number_reflns 1397 _refine_ls_number_parameters 134 _refine_ls_goodness_of_fit_ref 1.856 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00040|Fo|^2^]' _refine_ls_shift/su_max 0.0002 _refine_diff_density_max 0.36 _refine_diff_density_min -0.94 _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0025(5) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Mn' 'Mn' 0.337 0.728 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn(1) Mn 0.5000 0.0000 0.5000 0.0541(4) Uani 1.00 d S . . S(1) S 0.39512(5) 0.3379(1) 0.23906(10) 0.0760(4) Uani 1.00 d . . . S(2) S 0.29540(4) 0.1707(1) 0.3662(1) 0.0883(5) Uani 1.00 d . . . N(1) N 0.4442(1) 0.0910(3) 0.4286(2) 0.0553(10) Uani 1.00 d . . . N(2) N 0.5000 0.2097(6) 0.5794(4) 0.069(2) Uani 1.00 d S . . N(3) N 0.3824(3) 0.5000 0.5000 0.150(4) Uani 1.00 d S . . C(1) C 0.5000 0.2198(6) 0.3280(5) 0.058(2) Uani 1.00 d S . . C(2) C 0.4518(1) 0.1812(4) 0.3601(3) 0.059(1) Uani 1.00 d . . . C(3) C 0.4019(2) 0.2252(4) 0.3261(3) 0.059(1) Uani 1.00 d . . . C(4) C 0.3639(2) 0.1631(4) 0.3749(3) 0.063(1) Uani 1.00 d . . . C(5) C 0.3905(1) 0.0788(4) 0.4389(3) 0.057(1) Uani 1.00 d . . . C(6) C 0.3659(2) 0.0000 0.5000 0.063(2) Uani 1.00 d S . . C(7) C 0.3615(3) 0.2239(7) 0.1679(5) 0.134(3) Uani 1.00 d . . . C(8) C 0.2828(3) 0.3552(7) 0.3773(6) 0.154(3) Uani 1.00 d . . . C(9) C 0.5000 0.3215(8) 0.5521(6) 0.090(3) Uani 1.00 d S . . C(10) C 0.4802(3) 0.4556(9) 0.5170(8) 0.073(3) Uani 0.50 d P . . C(11) C 0.4263(3) 0.5000 0.5000 0.094(3) Uani 1.00 d S . . H(1) H 0.5000 0.275(5) 0.275(3) 0.03(1) Uiso 1.00 calc S . . H(2) H 0.331(3) 0.0000 0.5000 0.08(2) Uiso 1.00 calc S . . H(3) H 0.3823 0.1418 0.1567 0.1610 Uiso 1.00 calc . . . H(4) H 0.3550 0.2736 0.1167 0.1610 Uiso 1.00 calc . . . H(5) H 0.3291 0.1951 0.1922 0.1610 Uiso 1.00 calc . . . H(6) H 0.3003 0.4062 0.3338 0.1848 Uiso 1.00 calc . . . H(7) H 0.2461 0.3718 0.3734 0.1848 Uiso 1.00 calc . . . H(8) H 0.2951 0.3869 0.4306 0.1848 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mn(1) 0.0386(6) 0.0268(6) 0.097(1) 0.0000 0.0000 -0.0060(7) S(1) 0.0627(7) 0.0462(6) 0.119(1) 0.0009(6) -0.0063(7) 0.0106(7) S(2) 0.0435(6) 0.0522(7) 0.169(2) 0.0025(6) -0.0101(7) 0.0106(8) N(1) 0.039(2) 0.029(2) 0.098(2) 0.000(1) 0.000(2) -0.008(2) N(2) 0.053(3) 0.038(3) 0.114(5) 0.0000 0.0000 -0.017(3) N(3) 0.057(4) 0.171(9) 0.222(9) 0.0000 0.0000 0.022(8) C(1) 0.049(3) 0.037(3) 0.086(5) 0.0000 0.0000 0.000(3) C(2) 0.046(2) 0.029(2) 0.101(3) 0.003(2) -0.003(2) -0.009(2) C(3) 0.048(2) 0.034(2) 0.095(3) 0.003(2) -0.006(2) -0.006(2) C(4) 0.046(2) 0.034(2) 0.109(4) 0.003(2) -0.005(2) -0.010(2) C(5) 0.039(2) 0.028(2) 0.105(3) 0.003(2) -0.005(2) -0.009(2) C(6) 0.040(3) 0.030(3) 0.120(5) 0.0000 0.0000 -0.008(4) C(7) 0.164(7) 0.080(4) 0.158(6) -0.031(5) -0.076(5) 0.035(5) C(8) 0.067(4) 0.078(4) 0.32(1) 0.027(3) 0.007(5) -0.019(6) C(9) 0.114(6) 0.035(4) 0.120(7) 0.0000 0.0000 -0.024(4) C(10) 0.058(4) 0.044(5) 0.118(9) -0.001(3) 0.000(5) -0.018(6) C(11) 0.069(5) 0.046(4) 0.168(8) 0.0000 0.0000 -0.021(5) #------------------------------------------------------------------------------ _computing_data_collection 'PROCESS' _computing_cell_refinement 'PROCESS' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag ? ? ? ? ? ? # -- ENTER BONDS HERE, ONE PER LINE -- # e.g. C1 C2 1.541(1) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag # -- ENTER ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 109.4(3) . . . yes ? ? ? ? ? ? ? ? #------------------------------------------------------------------------------ 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 # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 109.4(3) . . . . yes ? ? ? ? ? ? ? ? ? ? #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? # -- ENTER BONDS HERE, ONE PER LINE -- # e.g. O1 N1 1.541(1) . . yes #------------------------------------------------------------------------------