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_4115483
_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            'C108 H204 Bi6 K6 Mo4 N16 O42'
_chemical_formula_weight         4271.11
_chemical_name_systematic
;
K(K-crypt)5[Bi3Mo2(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                91.602(6)
_cell_angle_beta                 102.387(6)
_cell_angle_gamma                91.953(6)
_cell_formula_units_Z            2
_cell_length_a                   12.635(4)
_cell_length_b                   21.115(6)
_cell_length_c                   29.197(8)
_cell_measurement_temperature    170(2)
_cell_volume                     7599(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0947
_diffrn_reflns_av_sigmaI/netI    0.1762
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            69305
_diffrn_reflns_theta_full        26.47
_diffrn_reflns_theta_max         26.47
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    7.479
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.697553
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_description       irregular
_exptl_crystal_F_000             4160
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.15
_refine_diff_density_max         4.295
_refine_diff_density_min         -1.765
_refine_diff_density_rms         0.366
_refine_ls_extinction_coef       0.00121(7)
_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_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1640
_refine_ls_number_reflns         30953
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1724
_refine_ls_R_factor_gt           0.1303
_refine_ls_shift/su_max          0.850
_refine_ls_shift/su_mean         0.021
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+646.6719P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3148
_refine_ls_wR_factor_ref         0.3386
_reflns_number_gt                19907
_reflns_number_total             30953
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0038732_1.cif
_cod_data_source_block           Bi3Mo2(CO)6
_cod_database_code               4115483