#------------------------------------------------------------------------------ #$Date: 2016-03-22 10:07:20 +0000 (Tue, 22 Mar 2016) $ #$Revision: 178935 $ #$URL: svn://www.crystallography.net/cod/cif/4/11/64/4116488.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4116488 loop_ _publ_author_name 'Eduard Bernhardt' 'Bianca Bley' 'Rudolf Wartchow' 'Helge Willner' 'Eckhard Bill' 'Peter Kuhn' 'Iona H. T. Sham' 'Matthias Bodenbinder' 'Raimund Br\"ochler' 'Friedhelm Aubke' _publ_contact_author ; Concerning the supplementary material of the crystal structure : Rudolf Wartchow Institut f\"ur Anorganische Chemie Universit\"at Hannover Callinstr. 9 D-30167 Hannover ; _publ_contact_author_email wartchow@mbox.aca.uni-hannover.de _publ_contact_author_fax '0511 762 3006' _publ_contact_author_phone '0511 762 2216' _publ_section_title ; Hexakis(carbonyl)iron(II) Undecafluorodiantimonate(V), [Fe(CO)6][Sb2F11]2, and -Hexafluoroantimonate(V), [Fe(CO)6][SbF6]2, Their Syntheses, and Spectroscopic and Structural Characterization by Single Crystal X-ray Diffraction and Normal Coordinate Analysis ; _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 7188 _journal_page_last 7200 _journal_paper_doi 10.1021/ja990958y _journal_volume 121 _journal_year 1999 _chemical_compound_source synthetic _chemical_formula_moiety '[Fe(CO)6][SbF6]2' _chemical_formula_sum 'C6 F12 Fe O6 Sb2' _chemical_formula_weight 695.41 _chemical_name_systematic ; Hexakis(carbonyl)iron(II) hexafluoroantimonate(V), ; _space_group_IT_number 128 _symmetry_cell_setting tetragonal _symmetry_Int_Tables_number 128 _symmetry_space_group_name_Hall '-P 4 2n' _symmetry_space_group_name_H-M 'P 4/m n c' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 8.2580(10) _cell_length_b 8.2580(10) _cell_length_c 12.471(2) _cell_measurement_reflns_used 4794 _cell_measurement_temperature 300(2) _cell_measurement_theta_max 28.0 _cell_measurement_theta_min 2.9 _cell_volume 850.5(2) _computing_cell_refinement 'Stoe IPDS software' _computing_data_collection 'Stoe IPDS software' _computing_data_reduction 'Stoe IPDS software and SHELXL-93' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material ; The first CIF was issued by SHELXL-93. The edited CIF is finally treated with the program CIF2SX written by L. Farrugia, Univ. of Glasgow (1997) and a refinement cycle is repeated to assure that essential parameters are not changed ; _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_ambient_temperature 300(2) _diffrn_measurement_device 'Stoe IPDS area detector diffractometer' _diffrn_measurement_method '170 exposures, \D \f 1.5 \%' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0186 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 9353 _diffrn_reflns_theta_max 28.12 _diffrn_reflns_theta_min 2.96 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 4.142 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_correction_T_min 1.0 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.716 _exptl_crystal_description 'irregular shape' _exptl_crystal_F_000 640 _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.28 _refine_diff_density_max 0.605 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.102 _refine_ls_extinction_coef 0.0056(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_all 1.026 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 39 _refine_ls_number_reflns 545 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.026 _refine_ls_restrained_S_obs 1.130 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0259 _refine_ls_shift/esd_mean 0.000 _refine_ls_shift/su_max 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0668 _refine_ls_wR_factor_ref 0.0626 _reflns_number_gt 405 _reflns_number_total 545 _reflns_observed_criterion >2sigma(I) _cod_data_source_file ja990958y_2.cif _cod_data_source_block wart_bern3 _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_database_code 4116488 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' '-x, -y, z' 'y, -x, z' '-x+1/2, y+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'y, -x, -z' 'x, y, -z' '-y, x, -z' 'x-1/2, -y-1/2, -z-1/2' '-y-1/2, -x-1/2, -z-1/2' '-x-1/2, y-1/2, -z-1/2' 'y-1/2, x-1/2, -z-1/2' 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 0.0315(4) 0.0315(4) 0.0250(6) 0.000 0.000 0.000 C1 0.041(2) 0.041(2) 0.032(3) 0.000 0.000 0.000 O1 0.075(3) 0.075(3) 0.032(3) 0.000 0.000 0.000 C2 0.042(3) 0.038(3) 0.025(2) 0.000 0.000 0.007(3) O2 0.041(2) 0.049(2) 0.045(2) 0.000 0.000 -0.007(2) Sb1 0.0350(2) 0.0350(2) 0.0282(3) 0.000 0.000 -0.0061(2) F1 0.095(2) 0.109(3) 0.049(2) 0.002(2) 0.022(2) -0.051(2) F2 0.127(4) 0.127(4) 0.121(5) 0.014(3) 0.014(3) 0.087(5) 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags Fe1 Fe 0.0000 0.0000 0.0000 0.0293(3) Uani 1 d S C1 C 0.0000 0.0000 0.1537(6) 0.0383(15) Uani 1 d S O1 O 0.0000 0.0000 0.2416(4) 0.060(2) Uani 1 d S C2 C 0.1905(7) 0.1296(7) 0.0000 0.0347(12) Uani 1 d S O2 O 0.3035(6) 0.2033(6) 0.0000 0.0449(9) Uani 1 d S Sb1 Sb 0.5000 0.0000 0.2500 0.0327(2) Uani 1 d S F1 F 0.6179(4) 0.1024(4) 0.1435(2) 0.0844(11) Uani 1 d . F2 F 0.3431(4) 0.1569(4) 0.2500 0.125(3) Uani 1 d S 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' Sb Sb -0.5866 1.5461 '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' C C 0.0033 0.0016 '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' 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 C2 Fe1 C2 180.0 . 9 C2 Fe1 C2 90.0 . 10 C2 Fe1 C2 90.0 9 10 C2 Fe1 C2 90.0 . 2 C2 Fe1 C2 90.0 9 2 C2 Fe1 C2 180.0 10 2 C2 Fe1 C1 90.0 . 9 C2 Fe1 C1 90.0 9 9 C2 Fe1 C1 90.0 10 9 C2 Fe1 C1 90.0 2 9 C2 Fe1 C1 90.0 . . C2 Fe1 C1 90.0 9 . C2 Fe1 C1 90.0 10 . C2 Fe1 C1 90.0 2 . C1 Fe1 C1 180.0 9 . O1 C1 Fe1 180.0 . . O2 C2 Fe1 178.9(5) . . F2 Sb1 F2 180.0 . 3_655 F2 Sb1 F1 92.82(12) . . F2 Sb1 F1 87.18(12) 3_655 . F2 Sb1 F1 87.18(12) . 3_655 F2 Sb1 F1 92.82(12) 3_655 3_655 F1 Sb1 F1 88.3(2) . 3_655 F2 Sb1 F1 87.18(12) . 16_656 F2 Sb1 F1 92.82(12) 3_655 16_656 F1 Sb1 F1 92.0(2) . 16_656 F1 Sb1 F1 174.4(2) 3_655 16_656 F2 Sb1 F1 92.82(12) . 14_666 F2 Sb1 F1 87.18(12) 3_655 14_666 F1 Sb1 F1 174.4(2) . 14_666 F1 Sb1 F1 92.0(2) 3_655 14_666 F1 Sb1 F1 88.3(2) 16_656 14_666 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Fe1 C2 1.903(6) . Fe1 C2 1.903(6) 9 Fe1 C2 1.903(6) 10 Fe1 C2 1.903(6) 2 Fe1 C1 1.917(7) 9 Fe1 C1 1.917(7) . C1 O1 1.097(8) . C2 O2 1.114(7) . Sb1 F2 1.832(5) . Sb1 F2 1.832(5) 3_655 Sb1 F1 1.851(3) . Sb1 F1 1.851(3) 3_655 Sb1 F1 1.851(3) 16_656 Sb1 F1 1.851(3) 14_666