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_4300024
_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_sum            'C91.3 H32 Bi6 F60 O16'
_chemical_formula_weight         3778.65
_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                105.17(3)
_cell_angle_beta                 104.82(3)
_cell_angle_gamma                96.56(3)
_cell_formula_units_Z            2
_cell_length_a                   13.797(3)
_cell_length_b                   18.378(4)
_cell_length_c                   24.531(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      8.28
_cell_measurement_theta_min      3.64
_cell_volume                     5693(3)
_computing_cell_refinement       TEXSAN
_computing_data_collection       TEXSAN
_computing_data_reduction        TEXSAN
_computing_molecular_graphics    SHELXL-93
_computing_publication_material  'SHELXTL 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 0.720
_diffrn_measured_fraction_theta_max 0.720
_diffrn_measurement_device       'Rigaku AFC5-S'
_diffrn_measurement_method       2theta-\wscans
_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  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0648
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11135
_diffrn_reflns_theta_full        22.47
_diffrn_reflns_theta_max         22.47
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        3.1
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.397
_exptl_absorpt_correction_T_max  0.4534
_exptl_absorpt_correction_T_min  0.1649
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.204
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             3492
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.405
_refine_diff_density_min         -2.138
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           block
_refine_ls_number_parameters     1487
_refine_ls_number_reflns         10687
_refine_ls_number_restraints     501
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0747P)^2^+86.3624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1449
_reflns_number_gt                8481
_reflns_number_total             10687
_reflns_threshold_expression     >2sigma(I)
_cod_original_cell_volume        5693(2)
_cod_original_formula_sum        'C91.30 H32 Bi6 F60 O16'
_cod_database_code               4300024