Silylene-Bridged Dinuclear Iron Complexes [Cp(OC)2Fe]2SiX2 (X = H, F, Cl, Br, I). Synthesis, Molecular Structure, Vibrational Spectroscopy, and Theoretical Studies
Matthias Vögler; Ioana Pavel; Marco Hofmann; Damien Moigno; Martin Nieger; Wolfgang Kiefer; Wolfgang Malisch; Inorganic Chemistry 42 (2003) 3274–3284; doi:10.1021/ic026138v

data_4313636
_publ_contact_author
;
        Martin Nieger
        Institut f\"ur Anorganische Chemie
        Universit\"at Bonn
        Gerhard-Domagk-Str. 1
        D-53121 Bonn
        Bundesrepublik Deutschland
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_publ_contact_author_email       NIEGER@JOYX.JOENSUU.FI
_publ_contact_author_fax         '049 228 73-5327'
_publ_contact_author_phone       '049 228 73-5823'
_publ_section_title
;
 Silylene-Bridged Dinuclear Iron Complexes [Cp(OC)2Fe]2SiX2 (X = H, F, Cl,
 Br, I). Synthesis, Molecular Structure, Vibrational Spectroscopy, and
 Theoretical Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3274
_journal_page_last               3284
_journal_paper_doi               10.1021/ic026138v
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C14 H10 F2 Fe2 O4 Si'
_chemical_formula_sum            'C14 H10 F2 Fe2 O4 Si'
_chemical_formula_weight         420.01
_chemical_name_systematic
; 
 mu2-[(Difluoro)silanediyl]-bis[dicarbonyl(eta5-cyclopentadienyl)iron(II))] 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.500(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7190(1)
_cell_length_b                   16.9176(2)
_cell_length_c                   11.6193(2)
_cell_measurement_reflns_used    33836
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     1500.66(4)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       Collect
_computing_data_reduction        DENZO-SMn
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'rotation in phi and omega, 2 deg.'
_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  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0179
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            28456
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    2.050
_exptl_absorpt_correction_T_max  0.77003
_exptl_absorpt_correction_T_min  0.50328
_exptl_absorpt_correction_type   'empirical from multiple refl.'
_exptl_absorpt_process_details   'XEMP (SHELXTL-Plus)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2630
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0164
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0213P)^2^+0.6562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0432
_refine_ls_wR_factor_ref         0.0436
_reflns_number_gt                2503
_reflns_number_total             2630
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026138vsi20021029_032526_1.cif
_cod_data_source_block           wma57_a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:
data name '_publ_contact_autor' replaced with '_publ_contact_author'
as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
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_cod_database_code               4313636