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_4300026
_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_volume                  39
_journal_year                    2000
_chemical_formula_moiety         Bi9O7(OC6F5)13(toluene)2
_chemical_formula_sum            'C92 H16 Bi9 F65 O20'
_chemical_formula_weight         4556.87
_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-97
_cell_angle_alpha                86.04(3)
_cell_angle_beta                 81.79(3)
_cell_angle_gamma                61.98(3)
_cell_formula_units_Z            2
_cell_length_a                   14.123(3)
_cell_length_b                   14.578(3)
_cell_length_c                   29.487(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      6.05
_cell_measurement_theta_min      3.37
_cell_volume                     5304(2)
_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      193(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device       'Rigaku AFC5-S'
_diffrn_measurement_method       \wscans
_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  0.1204
_diffrn_reflns_av_sigmaI/netI    0.0976
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            14265
_diffrn_reflns_theta_full        22.54
_diffrn_reflns_theta_max         22.54
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    15.054
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3713
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.853
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4120
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         4.207
_refine_diff_density_min         -4.836
_refine_diff_density_rms         0.762
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1126
_refine_ls_number_reflns         13469
_refine_ls_number_restraints     405
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1382
_refine_ls_R_factor_gt           0.0764
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2161
_refine_ls_wR_factor_ref         0.2854
_reflns_number_gt                8948
_reflns_number_total             13469
_reflns_threshold_expression     >2sigma(I)
_cod_original_cell_volume        5304.4(18)
_cod_database_code               4300026
_journal_paper_doi 10.1021/ic990431m