#------------------------------------------------------------------------------ #$Date: 2016-02-20 03:06:23 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/08/2200804.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_2200804 loop_ _publ_author_name 'Brennessel, William W.' 'Brooks, Neil R.' 'Mehn, Mark P.' 'Que Jr, Lawrence' 'Young Jr, Victor G.' _publ_section_title ; Hexakis(acetonitrile)iron(II) hexafluoroantimonate ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m545 _journal_page_last m546 _journal_paper_doi 10.1107/S1600536801017585 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Fe (C2 H3 N)6] [Sb F6]2' _chemical_formula_moiety 'C12 H18 Fe N6 2+, 2F6 Sb 1-' _chemical_formula_sum 'C12 H18 F12 Fe N6 Sb2' _chemical_formula_weight 773.67 _chemical_name_common '(MeCN)6Fe (SbF6)2' _chemical_name_systematic ; hexakis(acetonitrile) iron(II) hexafluoroantimonate ; _space_group_IT_number 148 _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall '-R 3' _symmetry_space_group_name_H-M 'R -3 :H' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 3 _cell_length_a 11.3398(6) _cell_length_b 11.3398(6) _cell_length_c 17.3584(11) _cell_measurement_reflns_used 4001 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 2.4 _cell_volume 1933.09(19) _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_collection 'SMART (Bruker, 2000)' _computing_data_reduction SAINT _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1998)' _computing_publication_material 'SHELXTL/PC and PLATON (Spek, 2001)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full .998 _diffrn_measured_fraction_theta_max .998 _diffrn_measurement_device_type 'Bruker CCD area-detector' _diffrn_measurement_method '\f and \w' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .028 _diffrn_reflns_av_sigmaI/netI .016 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 5690 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 2.4 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.73 _exptl_absorpt_correction_T_max .900 _exptl_absorpt_correction_T_min .602 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Blessing, 1995; Sheldrick, 2000)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.994 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'block cut from hexagonal prism' _exptl_crystal_F_000 1104 _exptl_crystal_size_max .40 _exptl_crystal_size_mid .30 _exptl_crystal_size_min .30 _refine_diff_density_max .55 _refine_diff_density_min -.47 _refine_ls_extinction_coef .0107(5) _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.12 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 53 _refine_ls_number_reflns 996 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.12 _refine_ls_R_factor_all .025 _refine_ls_R_factor_gt .024 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0368P)^2^+4.867P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .069 _reflns_number_gt 933 _reflns_number_total 996 _reflns_threshold_expression I>2\s(I) _cod_data_source_file ya6066.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 1933.1(2) _cod_original_sg_symbol_H-M 'R -3' _cod_database_code 2200804 _cod_database_fobs_code 2200804 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' 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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Fe1 .6667 .3333 .3333 .02141(19) Uani d S 1 . . Fe N1 .6659(2) .4906(2) .40253(12) .0321(5) Uani d . 1 . . N C1 .6658(2) .5774(2) .43437(14) .0288(5) Uani d . 1 . . C C2 .6651(3) .6881(3) .4763(2) .0424(7) Uani d . 1 . . C H2A .6723 .6760 .5316 .064 Uiso calc R 1 . . H H2B .5800 .6878 .4657 .064 Uiso calc R 1 . . H H2C .7425 .7751 .4597 .064 Uiso calc R 1 . . H Sb1 .6667 .3333 .661838(14) .02892(17) Uani d S 1 . . Sb F1 .6682(3) .1981(3) .7195(2) .1068(11) Uani d . 1 . . F F2 .5350(3) .1968(3) .60083(19) .0921(9) Uani d . 1 . . F 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 .0214(2) .0214(2) .0215(4) .01069(12) .000 .000 N1 .0328(10) .0315(10) .0331(10) .0171(8) -.0006(8) -.0040(8) C1 .0252(10) .0299(11) .0313(11) .0137(9) -.0021(8) -.0033(9) C2 .0416(16) .0364(13) .054(2) .0230(13) -.0058(11) -.0167(13) Sb1 .03148(19) .03148(19) .0238(2) .01574(9) .000 .000 F1 .111(2) .094(2) .118(2) .0533(18) -.0103(19) .0595(19) F2 .0745(16) .0736(16) .120(2) .0309(13) -.0527(16) -.0450(16) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe .3463 .8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -.5866 1.5461 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle N1 Fe1 N1 18_545 3_665 180.0 N1 Fe1 N1 18_545 2_655 88.10(8) N1 Fe1 N1 3_665 2_655 91.91(8) N1 Fe1 N1 18_545 . 88.10(8) N1 Fe1 N1 3_665 . 91.91(8) N1 Fe1 N1 2_655 . 91.91(8) N1 Fe1 N1 18_545 17 91.91(8) N1 Fe1 N1 3_665 17 88.09(8) N1 Fe1 N1 2_655 17 180.0 N1 Fe1 N1 . 17 88.10(8) N1 Fe1 N1 18_545 16_655 91.90(8) N1 Fe1 N1 3_665 16_655 88.09(8) N1 Fe1 N1 2_655 16_655 88.10(8) N1 Fe1 N1 . 16_655 180.0 N1 Fe1 N1 17 16_655 91.90(8) C1 N1 Fe1 . . 175.4(2) N1 C1 C2 . . 179.3(3) C1 C2 H2A . . 109.5 C1 C2 H2B . . 109.5 H2A C2 H2B . . 109.5 C1 C2 H2C . . 109.5 H2A C2 H2C . . 109.5 H2B C2 H2C . . 109.5 F1 Sb1 F1 . 2_655 93.15(17) F1 Sb1 F1 . 3_665 93.15(17) F1 Sb1 F1 2_655 3_665 93.15(17) F1 Sb1 F2 . 2_655 88.85(16) F1 Sb1 F2 2_655 2_655 87.37(16) F1 Sb1 F2 3_665 2_655 177.90(13) F1 Sb1 F2 . . 87.37(16) F1 Sb1 F2 2_655 . 177.90(13) F1 Sb1 F2 3_665 . 88.85(16) F2 Sb1 F2 2_655 . 90.60(16) F1 Sb1 F2 . 3_665 177.90(13) F1 Sb1 F2 2_655 3_665 88.85(16) F1 Sb1 F2 3_665 3_665 87.37(15) F2 Sb1 F2 2_655 3_665 90.60(16) F2 Sb1 F2 . 3_665 90.60(16) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 N1 18_545 2.153(2) ? Fe1 N1 3_665 2.153(2) ? Fe1 N1 2_655 2.153(2) ? Fe1 N1 . 2.153(2) ? Fe1 N1 17 2.153(2) ? Fe1 N1 16_655 2.153(2) ? N1 C1 . 1.129(3) ? C1 C2 . 1.455(4) ? C2 H2A . .9800 ? C2 H2B . .9800 ? C2 H2C . .9800 ? Sb1 F1 . 1.839(2) ? Sb1 F1 2_655 1.839(2) ? Sb1 F1 3_665 1.839(2) ? Sb1 F2 2_655 1.854(2) ? Sb1 F2 . 1.854(2) ? Sb1 F2 3_665 1.854(2) ?