Stabilization of Ozone-like [Bi3]3- in the Heteroatomic closo-Clusters [Bi3Cr2(CO)6]3- and [Bi3Mo2(CO)6]3-
Li Xu; Angel Ugrinov; Slavi C. Sevov; Journal of the American Chemical Society 123 (2001) 4091–4092; doi:10.1021/ja0038732

data_4115484
_publ_section_title
;
 Stabilization of Ozone-like [Bi3]3- in the Heteroatomic closo-Clusters
 [Bi3Cr2(CO)6]3- and [Bi3Mo2(CO)6]3-
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4091
_journal_page_last               4092
_journal_paper_doi               10.1021/ja0038732
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C106 H196 Bi6 Cr4 K6 N14 O42'
_chemical_formula_weight         4035.25
_chemical_name_systematic
;
K(K-crypt)5[Bi3Cr2(CO)6]2*3en
;
_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                71.310(10)
_cell_angle_beta                 81.37(3)
_cell_angle_gamma                78.82(2)
_cell_formula_units_Z            1
_cell_length_a                   12.679(3)
_cell_length_b                   17.724(2)
_cell_length_c                   18.254(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      11
_cell_volume                     3794.9(11)
_computing_cell_refinement       'CAD4-ARGUS, (Enraf-Nonius, 1994)'
_computing_data_collection       'CAD4-ARGUS, (Enraf-Nonius, 1994)'
_computing_data_reduction        'xcad4 (Harms, 1996)'
_computing_molecular_graphics    'SHELXTL-V5.1 (Siemens, 1994)'
_computing_publication_material  'SHELXTL-V5.1 (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       omega-2theta
_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  0.0482
_diffrn_reflns_av_sigmaI/netI    0.1328
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13265
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.442
_exptl_absorpt_correction_T_max  1.234
_exptl_absorpt_correction_T_min  0.631
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Xabs
_exptl_crystal_colour            brown-red
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_description       needle
_exptl_crystal_F_000             1974
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.802
_refine_diff_density_min         -1.053
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     826
_refine_ls_number_reflns         13265
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1899
_refine_ls_R_factor_gt           0.0765
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0961P)^2^+7.3805P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1665
_refine_ls_wR_factor_ref         0.2175
_reflns_number_gt                5928
_reflns_number_total             13265
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0038732_2.cif
_cod_data_source_block           Bi3Cr2(CO)6
_cod_database_code               4115484