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
Eduard Bernhardt; Bianca Bley; Rudolf Wartchow; Helge Willner; Eckhard Bill; Peter Kuhn; Iona H. T. Sham; Matthias Bodenbinder; Raimund Bröchler; Friedhelm Aubke; Journal of the American Chemical Society 121 (1999) 7188–7200; doi:10.1021/ja990958y

data_4116488
_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