Synthetic and Structural Studies of Cyclodistib(V)azanes
May C. Copsey; Sabrina B. Gallon; Sara K. Grocott; John C. Jeffery; Christopher A. Russell; John M. Slattery; Inorganic Chemistry 44 (2005) 5495–5500; doi:10.1021/ic050127v

data_4309252
_publ_section_title
;
Synthetic and Structural Studies of Cyclodistib(V)azanes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5495
_journal_page_last               5500
_journal_paper_doi               10.1021/ic050127v
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C25 H22 Bi0 N Sb'
_chemical_formula_weight         458.19
_chemical_name_systematic
; 
 ? 
;
_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                70.90(3)
_cell_angle_beta                 74.33(3)
_cell_angle_gamma                71.59(3)
_cell_formula_units_Z            2
_cell_length_a                   9.0485(18)
_cell_length_b                   10.702(2)
_cell_length_c                   11.459(2)
_cell_measurement_temperature    293(2)
_cell_volume                     977.5(4)
_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_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  0.0215
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11047
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    1.420
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.87
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0206
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0473
_refine_ls_wR_factor_ref         0.0479
_reflns_number_gt                4089
_reflns_number_total             4473
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050127vsi20050127_032156_1.cif
_cod_data_source_block           sunnym
_cod_original_cell_volume        977.5(3)
_cod_database_code               4309252