#------------------------------------------------------------------------------ #$Date: 2008-06-20 14:44:24 +0100 (Fri, 20 Jun 2008) $ #$Revision: 397 $ #$URL: svn://www.crystallography.net/cod/cif/2/2103786.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_2103786 loop_ _publ_author_name 'Clemente, Dore Augusto' 'Marzotto, Armando' _publ_section_title ; 22 Space-group changes ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 43 _journal_page_last 50 _journal_volume 59 _journal_year 2003 _chemical_formula_sum 'C7 H5 As F6 Fe O4 S' _chemical_formula_weight 429.94 _chemical_name_systematic ; Dicarbonyl-(eta$5!-cyclopentadienyl)-(sulfur dioxide)-iron(iii) hexafluoroarsenate ; _space_group_IT_number 36 _symmetry_space_group_name_Hall 'C 2c -2' _symmetry_space_group_name_H-M 'C m c 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.068(2) _cell_length_b 13.904(4) _cell_length_c 11.285(2) _cell_measurement_temperature 293(2) _cell_volume 1265.9(5) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.247 _diffrn_measured_fraction_theta_max 0.247 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71070 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0897 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 7020 _diffrn_reflns_theta_full 53.09 _diffrn_reflns_theta_max 53.09 _diffrn_reflns_theta_min 2.92 _exptl_absorpt_coefficient_mu 4.033 _exptl_crystal_density_diffrn 2.256 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _refine_diff_density_max 0.185 _refine_diff_density_min -0.266 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.0108(18) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.146 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 60 _refine_ls_number_reflns 1916 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 0.146 _refine_ls_R_factor_all 0.0048 _refine_ls_R_factor_gt 0.0046 _refine_ls_shift/su_max 2.807 _refine_ls_shift/su_mean 0.047 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0225 _refine_ls_wR_factor_ref 0.0239 _reflns_number_gt 1903 _reflns_number_total 1916 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file an0613.cif _[local]_cod_data_source_block bogpiw loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, z' '-x, -y, z+1/2' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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' F F 0.0171 0.0103 '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' 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' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Fe1 0.0000 0.184900(11) 0.257400(13) 0.02000(3) Uiso d S 1 Fe As1 0.5000 0.072700(7) 0.063800(9) 0.02000(2) Uiso d S 1 As F1 0.5000 0.05280(5) -0.08470(5) 0.02000(10) Uiso d S 1 F F2 0.35070(4) 0.16060(3) 0.04350(4) 0.02000(7) Uiso d . 1 F F3 0.34890(4) -0.01220(3) 0.08470(4) 0.02000(7) Uiso d . 1 F F5 0.5000 0.09780(5) 0.21090(5) 0.02000(9) Uiso d S 1 F S1 0.0000 0.172300(17) 0.07120(2) 0.02000(4) Uiso d S 1 S O1 0.0000 0.08190(5) 0.01370(7) 0.02000(10) Uiso d S 1 O O2 0.0000 0.25750(5) 0.00080(7) 0.02000(10) Uiso d S 1 O C1 0.13670(7) 0.10800(6) 0.38110(6) 0.02000(9) Uiso d . 1 C C2 0.0000 0.14200(7) 0.43320(9) 0.02000(14) Uiso d S 1 C C5 0.08820(6) 0.04820(6) 0.29260(6) 0.02000(9) Uiso d . 1 C C6 0.16640(6) 0.27390(5) 0.25760(7) 0.02000(9) Uiso d . 1 C O3 0.27090(5) 0.32580(3) 0.26000(5) 0.02000(8) Uiso d . 1 O H1 0.2489(12) 0.1230(5) 0.4023(9) 0.020(3) Uiso d . 1 H H2 0.0000 0.1852(9) 0.4994(14) 0.020(4) Uiso d S 1 H H5 0.1592(12) 0.0127(7) 0.2401(8) 0.020(2) Uiso d . 1 H loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Fe1 C6 . 1.8258(7) Fe1 C6 2 1.8258(7) Fe1 C5 . 2.0680(10) Fe1 C5 2 2.0680(10) Fe1 C2 . 2.0716(11) Fe1 C1 . 2.0756(8) Fe1 C1 2 2.0756(8) Fe1 S1 . 2.1086(5) As1 F5 . 1.6963(7) As1 F1 . 1.6985(7) As1 F3 . 1.7133(5) As1 F3 2_655 1.7133(5) As1 F2 2_655 1.7312(5) As1 F2 . 1.7312(5) S1 O1 . 1.4145(9) S1 O2 . 1.4264(9) C1 C2 . 1.3362(9) C1 C5 . 1.3572(10) C2 C1 2 1.3362(9) C5 C5 2 1.4232(11) C6 O3 . 1.1101(8) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle C6 Fe1 C6 . 2 94.66(4) C6 Fe1 C5 . . 111.69(3) C6 Fe1 C5 2 . 151.13(3) C6 Fe1 C5 . 2 151.13(3) C6 Fe1 C5 2 2 111.69(3) C5 Fe1 C5 . 2 40.25(3) C6 Fe1 C2 . . 101.18(3) C6 Fe1 C2 2 . 101.18(3) C5 Fe1 C2 . . 63.35(3) C5 Fe1 C2 2 . 63.35(3) C6 Fe1 C1 . . 87.57(3) C6 Fe1 C1 2 . 137.65(3) C5 Fe1 C1 . . 38.24(3) C5 Fe1 C1 2 . 65.18(3) C2 Fe1 C1 . . 37.59(2) C6 Fe1 C1 . 2 137.65(3) C6 Fe1 C1 2 2 87.57(3) C5 Fe1 C1 . 2 65.18(3) C5 Fe1 C1 2 2 38.24(3) C2 Fe1 C1 . 2 37.59(2) C1 Fe1 C1 . 2 64.19(4) C6 Fe1 S1 . . 93.30(2) C6 Fe1 S1 2 . 93.30(2) C5 Fe1 S1 . . 96.61(2) C5 Fe1 S1 2 . 96.61(2) C2 Fe1 S1 . . 158.50(3) C1 Fe1 S1 . . 128.86(2) C1 Fe1 S1 2 . 128.86(2) F5 As1 F1 . . 177.50(3) F5 As1 F3 . . 90.40(2) F1 As1 F3 . . 91.35(2) F5 As1 F3 . 2_655 90.40(2) F1 As1 F3 . 2_655 91.35(2) F3 As1 F3 . 2_655 90.72(3) F5 As1 F2 . 2_655 89.10(2) F1 As1 F2 . 2_655 89.11(2) F3 As1 F2 . 2_655 178.639(18) F3 As1 F2 2_655 2_655 90.55(3) F5 As1 F2 . . 89.10(2) F1 As1 F2 . . 89.11(2) F3 As1 F2 . . 90.55(3) F3 As1 F2 2_655 . 178.639(18) F2 As1 F2 2_655 . 88.18(3) O1 S1 O2 . . 118.85(5) O1 S1 Fe1 . . 122.07(4) O2 S1 Fe1 . . 119.08(4) C2 C1 C5 . . 107.61(6) C2 C1 Fe1 . . 71.04(5) C5 C1 Fe1 . . 70.58(5) C1 C2 C1 2 . 111.25(9) C1 C2 Fe1 2 . 71.37(5) C1 C2 Fe1 . . 71.37(5) C1 C5 C5 . 2 106.76(3) C1 C5 Fe1 . . 71.19(5) C5 C5 Fe1 2 . 69.874(17) O3 C6 Fe1 . . 177.51(6)