Isolation of a Bismuth Chloride-Iron Carbonyl Adduct: Synthesis and Structural Characterization of [PhCH2NMe3]2[Bi2Cl4(μ-Cl)2{μ-Fe(CO)4}]
Jeffrey R. Eveland; Kenton H. Whitmire; Jean-Yves Saillard; Inorganic Chemistry 35 (1996) 4400–4405; doi:10.1021/ic951262i

data_4323857
_publ_contact_author
;
Dr. Kenton H. Whitmire
Chemistry Department, MS 60
Rice University
Houston, TX 77251-1892
U.S.A.
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_publ_contact_author_email       whitmir@rice.edu
_publ_contact_author_fax         (1)-713-737-5652
_publ_contact_author_phone       (1)-713-737-5650
_publ_section_title
;
 Isolation of a Bismuth Chloride-Iron Carbonyl Adduct: Synthesis and
 Structural Characterization of [PhCH2NMe3]2[Bi2Cl4(\m-Cl)2{\m-Fe(CO)4}]
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4400
_journal_page_last               4405
_journal_paper_doi               10.1021/ic951262i
_journal_volume                  35
_journal_year                    1996
_chemical_formula_structural     (C~10~H~16~N)~2~[Bi~2~Cl~6~Fe~(CO)~4~]
_chemical_formula_sum            'C24 H32 Bi2 Cl6 Fe N2 O4'
_chemical_formula_weight         1099.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           32
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 -2ab'
_symmetry_space_group_name_H-M   'P b a 2'
_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                   14.562(3)
_cell_length_b                   17.062(3)
_cell_length_c                   7.2210(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      8
_cell_measurement_theta_min      4
_cell_volume                     1794.1(5)
_computing_cell_refinement       'Texray 5.0 (MSC)'
_computing_data_collection       'Texray 5.0 (MSC)'
_computing_data_reduction        'Texray 5.0 (MSC)'
_computing_molecular_graphics    'SHELXTL-PC (Siemens, 1992)'
_computing_publication_material  'SHELXTL-PC (Siemens, 1992)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku AFC5S'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0643
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3176
_diffrn_reflns_theta_max         23.98
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    10.660
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6728
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.034
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.873
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.27(2)
_refine_ls_extinction_coef       0.0008(4)
_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   1.030
_refine_ls_goodness_of_fit_obs   1.062
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         2823
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.110
_refine_ls_restrained_S_obs      1.050
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_obs          0.0521
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+8.9484P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1514
_refine_ls_wR_factor_obs         0.1257
_reflns_number_observed          2194
_reflns_number_total             2824
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic951262i.cif
_cod_data_source_block           jre22
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+8.9484P] 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^)+(0.0712P)^2^+8.9484P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4323857