Halide Ion Addition to Bismuth-Containing Iron Carbonyl Compounds: Synthesis and Characterization of the Two Bridged-Butterfly Cluster Compounds [Et4N][(μ-H)Fe2(CO)6Bi2{μ-Fe(CO)4}] and [{PhCH2NMe3}{(μ-H)Fe2(CO)6Bi2(μ-Cl)2}]∞and Stabilization of Reduced-Hypervalent Bismuth Centers by Coordination to a Metal Center in [PhCH2NMe3]3[Bi3Cl4(μ-Cl)4{Fe(CO)3}]
Jeffrey R. Eveland; Jean-Yves Saillard; Kenton H. Whitmire; Inorganic Chemistry 36 (1997) 4387–4396; doi:10.1021/ic9609721

data_4323579
_publ_contact_author
;
Prof. Kenton H. Whitmire
Chemistry Department MS 60
Rice University
Houston TX 77005-1892
U.S.A.
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_publ_contact_author_email       whitmire@rice.edu
_publ_contact_author_fax         (1)-713-737-5652
_publ_contact_author_phone       (1)-713-737-5650
_publ_section_title
;
 Halide Ion Addition to Bismuth-Containing Iron Carbonyl Compounds:
 Synthesis and Characterization of the Two Bridged-Butterfly Cluster
 Compounds [Et4N][(\m-H)Fe2(CO)6Bi2{\m-Fe(CO)4}] and
 [{PhCH2NMe3}{(\m-H)Fe2(CO)6Bi2(\m-Cl)2}]\\infty and Stabilization of
 Reduced-Hypervalent Bismuth Centers by Coordination to a Metal Center in
 [PhCH2NMe3]3[Bi3Cl4(\m-Cl)4{Fe(CO)3}]
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4387
_journal_page_last               4396
_journal_paper_doi               10.1021/ic9609721
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C36.44 H56.6 Bi3 Cl8 Fe N3 O3.86'
_chemical_formula_weight         1564.88
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   20.801(4)
_cell_length_b                   19.937(4)
_cell_length_c                   25.480(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.41
_cell_measurement_theta_min      7.17
_cell_volume                     10567(4)
_computing_cell_refinement       'TEXSAN 5.0'
_computing_data_collection       'TEXSAN 5.0'
_computing_data_reduction        'TEXSAN 5.0'
_computing_molecular_graphics    'SHELXTL PC'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       AFC5-S
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2055
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            5490
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         2.04
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    10.671
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.180
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.967
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             5905
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.5
_refine_diff_density_max         2.288
_refine_diff_density_min         -1.153
_refine_diff_density_rms         0.228
_refine_ls_extinction_coef       0.000000(10)
_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   1.022
_refine_ls_goodness_of_fit_obs   1.157
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         5471
_refine_ls_number_restraints     642
_refine_ls_restrained_S_all      0.987
_refine_ls_restrained_S_obs      1.036
_refine_ls_R_factor_all          0.1979
_refine_ls_R_factor_obs          0.0691
_refine_ls_shift/esd_max         -0.198
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0695P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1894
_refine_ls_wR_factor_obs         0.1417
_reflns_number_observed          2670
_reflns_number_total             5490
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9609721_3.cif
_cod_data_source_block           '[PhCH2NMe3]3[Fe(CO)3Bi3Cl8].0.87Et2O'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0695P)^2^+0.0000P] 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^)+(0.0695P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        10566.8(36)
_cod_original_formula_sum        'C36.44 H56.60 Bi3 Cl8 Fe N3 O3.86'
_cod_database_code               4323579