Oligomerization and Oxide Formation in Bismuth Aryl Alkoxides: Synthesis and Characterization of Bi4(μ4-O)(μ-OC6F5)6{μ3-OBi(μ-OC6F5)3}2(C6H5CH3), Bi8(μ4-O)2(μ3-O)2(μ-OC6F5)16, Bi6(μ3-O)4(μ3-OC6F5){μ3-OBi(OC6F5)4}3, NaBi4(μ3-O)2(OC6F5)9(THF)2, and Na2Bi4(μ3-O)2(OC6F5)10(THF)2
Kenton H. Whitmire; Silke Hoppe; Orson Sydora; Jennifer L. Jolas; Carolyn M. Jones; Inorganic Chemistry 39 (2000) 85–97; doi:10.1021/ic990431m

data_4300025
_publ_contact_author
;
Dr. Kenton. H. Whitmire
Chemistry Department MS 60
Rice University
Houston TX 77251-1892
U.S.A.
;
_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
;
Oligomerization and Oxide Formation in Bismuth Aryl Alkoxides: Synthesis
and Characterization of
Bi4(\m4-O)(\m-OC6F5)6{\m3-OBi(\m-OC6F5)3}2(C6H5CH3),
Bi8(\m4-O)2(\m3-O)2(\m-OC6F5)16, Bi6(\m3-O)4(\m3-OC6F5){\m3-OBi(OC6F5)4}3,
NaBi4(\m3-O)2(OC6F5)9(THF)2, and Na2Bi4(\m3-O)2(OC6F5)10(THF)2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              85
_journal_page_last               97
_journal_paper_doi               10.1021/ic990431m
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         Bi8O4(OC6F5)16(CH2Cl2)3.37(H2O)2
_chemical_formula_sum            'C99.37 H10.74 Bi8 Cl6.74 F80 O22'
_chemical_formula_weight         4987.03
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                112.19(3)
_cell_angle_beta                 104.46(3)
_cell_angle_gamma                100.58(3)
_cell_formula_units_Z            1
_cell_length_a                   14.292(3)
_cell_length_b                   15.111(3)
_cell_length_c                   17.545(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      7.15
_cell_measurement_theta_min      3.41
_cell_volume                     3230.0(18)
_computing_cell_refinement       'TEXSAN 5.0'
_computing_data_collection       'TEXSAN 5.0'
_computing_data_reduction        'TEXSAN 5.0'
_computing_molecular_graphics    SHELXL-93
_computing_publication_material  'SHELXL Plus'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measurement_device       'Rigaku 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     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8840
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        4.3
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    11.175
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5593
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.564
_exptl_crystal_description       prism
_exptl_crystal_F_000             2282
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.70
_refine_diff_density_max         1.727
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.048
_refine_ls_goodness_of_fit_obs   1.089
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     967
_refine_ls_number_reflns         8452
_refine_ls_number_restraints     236
_refine_ls_restrained_S_all      1.051
_refine_ls_restrained_S_obs      1.090
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_obs          0.0397
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+23.1196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1015
_refine_ls_wR_factor_obs         0.0931
_reflns_number_observed          6795
_reflns_number_total             8453
_reflns_observed_criterion       >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+23.1196P] 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^)+(0.0364P)^2^+23.1196P] 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        3230.0(11)
_cod_database_code               4300025