#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2004090.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2004090 loop_ _publ_author_name 'Tzou, J.-R.' 'Mullaney, M.' 'Norman, R. E.' 'Chang, S.-C.' _publ_section_title ; Hexakis(dimethyl sulfoxide-O)iron(III) Trinitrate ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 2249 _journal_page_last 2252 _journal_volume 51 _journal_year 1995 _chemical_formula_sum 'C12 H36 Fe N3 O15 S6' _chemical_formula_weight 710.64 _space_group_IT_number 148 _symmetry_cell_setting trigonal _symmetry_space_group_name_Hall '-R 3' _symmetry_space_group_name_H-M 'R -3 :H' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 3 _cell_length_a 11.5180(10) _cell_length_c 19.966(4) _cell_measurement_reflns_used 24 _cell_measurement_temperature 294 _cell_measurement_theta_max 29.50 _cell_measurement_theta_min 26.43 _cell_volume 2293.8(5) _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1988) ; _computing_data_reduction 'TEXSAN PROCESS (Molecular Structure Corporation, 1985)' _computing_publication_material 'TEXSAN FINISH' _computing_structure_refinement 'TEXSAN LS' _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_ambient_temperature 21.0 _diffrn_measurement_device 'Rigaku AFC-7R' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 2017 _diffrn_reflns_theta_max 32.4821 _diffrn_reflns_theta_min 4.57 _diffrn_standards_decay_% 0.03 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.947 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.909 _exptl_absorpt_correction_type 'empirical via \y scan' _exptl_absorpt_process_details \y-scan _exptl_crystal_colour 'pale yellow' _exptl_crystal_density_diffrn 1.543 _exptl_crystal_description irregular _exptl_crystal_F_000 1113.00 _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _refine_diff_density_max 0.593 _refine_diff_density_min -0.547 _refine_ls_extinction_coef 2.8E-7 _refine_ls_extinction_method 'Zachariasen type 2, Gaussian, isotropic' _refine_ls_goodness_of_fit_obs 5.165 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 62 _refine_ls_number_reflns 1408 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0435 _refine_ls_shift/esd_max 0.0781 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_obs 0.0540 _reflns_number_observed 1412 _reflns_number_total 1854 _reflns_observed_criterion >3\s(I) _[local]_cod_data_source_file bk1054.cif _[local]_cod_data_source_block TZOU28 _[local]_cod_cif_authors_sg_H-M 'R -3' _[local]_cod_chemical_formula_sum_orig 'C12 H36 Fe1 N3 O15 S6' _cod_database_code 2004090 loop_ _symmetry_equiv_pos_as_xyz x,y,z 2/3+x,1/3+y,1/3+z 1/3+x,2/3+y,2/3+z -y,x-y,z 2/3-y,1/3+x-y,1/3+z 1/3-y,2/3+x-y,2/3+z -x+y,-x,z 2/3-x+y,1/3-x,1/3+z 1/3-x+y,2/3-x,2/3+z -x,-y,-z 2/3-x,1/3-y,1/3-z 1/3-x,2/3-y,2/3-z y,-x+y,-z 2/3+y,1/3-x+y,1/3-z 1/3+y,2/3-x+y,2/3-z x-y,+x,-z 2/3+x-y,1/3+x,1/3-z 1/3+x-y,2/3+x,2/3-z 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 Fe1 .0283(4) .0283 .0373(7) .0142 .0000 .0000 S1 .0339(5) .0351(5) .0483(5) .0163(4) -.0051(4) .0028(4) O1 .0340(10) .0320(10) .0470(10) .0180(10) -.0080(10) -.0010(10) O2 .051(2) .051(2) .120(3) .018(2) -.004(2) .004(2) O3 .120(10) .170(10) .230(10) .073(8) .020(10) .030(10) N1 .039(2) .039 .069(4) .020 .0000 .0000 N2 .048(4) .048 .21(2) .024 .0000 .0000 C1 .047(2) .070(3) .047(2) .032(2) -.008(2) -.002(2) C2 .057(3) .068(3) .063(3) .039(3) -.001(2) -.008(2) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Fe1 0 0 0 .0313 Uani d . S1 .18212(9) -.08524(9) .07947(5) .0395 Uani d . O1 .1585(2) .0281(2) .05570(10) .0376 Uani d . O2 .1054(3) .1066(3) .2518(2) .0775 Uani d . O3 .0890(10) .0930(10) .4652(6) .1732 Uani d . N1 0 0 .2517(3) .0490 Uani d . N2 0 0 .5 .1010 Uani d . C1 .2724(4) -.0204(4) .1543(2) .0537 Uani d . C2 .3128(4) -.0705(5) .0276(2) .0594 Uani d . H1 .2935 -.0855 .1734 .0720 Uiso calc C1 H2 .3541 .0595 .1460 .0720 Uiso calc C1 H3 .2207 -.0049 .1860 .0720 Uiso calc C1 H4 .3355 -.1382 .0394 .0738 Uiso calc C2 H5 .2863 -.0832 -.0183 .0738 Uiso calc C2 H6 .3910 .0149 .0328 .0738 Uiso calc C2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.003 0.002 'International Tables' H 0.000 0.000 'International Tables' O 0.011 0.006 'International Tables' N 0.006 0.003 'International Tables' Fe 0.346 0.844 'International Tables' S 0.125 0.123 'International Tables' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 -5 5 4 -5 0 1 -5 3 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Fe1 O1 2_555 92.60(9) yes O1 Fe1 O1 5_555 87.40(9) yes O1 S1 C1 . 102.7(2) yes O1 S1 C2 . 104.0(2) yes C1 S1 C2 . 99.4(2) yes Fe1 O1 S1 . 124.30(10) yes O2 N1 O2 2_555 120.00(2) yes O3 N2 O3 5_556 92.6(8) yes O3 N2 O3 6_556 87.4(8) yes S1 C1 H1 . 109.1 no S1 C1 H2 . 110.8 no S1 C1 H3 . 110.8 no H1 C1 H2 . 107.9 no H1 C1 H3 . 107.8 no H2 C1 H3 . 110.4 no S1 C2 H4 . 109.9 no S1 C2 H5 . 111.0 no S1 C2 H6 . 110.9 no H4 C2 H5 . 107.7 no H4 C2 H6 . 107.9 no H5 C2 H6 . 109.2 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Fe1 O1 2.020(2) yes S1 O1 1.536(2) yes S1 C1 1.759(4) yes S1 C2 1.763(4) yes O2 N1 1.221(3) yes O3 N2 1.261(9) yes C1 H1 0.975 no C1 H2 0.944 no C1 H3 0.945 no C2 H4 0.969 no C2 H5 0.953 no C2 H6 0.950 no