Structural Consequences of the Use of Hard and Soft Tripodal Ligands during Metathesis Reactions: Synthesis of the [Bis(hydrotris(methimazolyl)borato]bismuth(III) [Bis(hydrotris(pyrazolyl)borato]sodiate
John Reglinski; Mark D. Spicer; Mark Garner; Alan R. Kennedy; Journal of the American Chemical Society 121 (1999) 2317–2318; doi:10.1021/ja983637f

data_4116317
_publ_contact_author
;
          Dr. J. Reglinski
     Department of Pure and Applied Chemistry
            University of Strathclyde
            295 Cathedral Street
            GLASGOW  G1 1XL
            UK
;
_publ_section_title
;
 Structural Consequences of the Use of Hard and Soft Tripodal Ligands
 during Metathesis Reactions: Synthesis of the
 [Bis(hydrotris(methimazolyl)borato]bismuth(III)
 [Bis(hydrotris(pyrazolyl)borato]sodiate
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2317
_journal_page_last               2318
_journal_paper_doi               10.1021/ja983637f
_journal_volume                  121
_journal_year                    1999
_chemical_formula_analytical     'C24 H32 B2 Bi0.5 cl5 N12 Na0.5 S3'
_chemical_formula_sum            'C48 H64 B4 Bi Cl10 N24 Na S6'
_chemical_formula_weight         899.65
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Tue Oct  6 13:34:56 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                109.21(3)
_cell_angle_beta                 95.38(3)
_cell_angle_gamma                114.22(2)
_cell_formula_units_Z            2
_cell_length_a                   12.968(4)
_cell_length_b                   13.279(5)
_cell_length_c                   12.825(3)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    123.2
_cell_measurement_theta_max      20.4
_cell_measurement_theta_min      13.5
_cell_volume                     1833.6(12)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      123.2
_diffrn_measurement_device       AFC7S
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      -0.00214
_diffrn_orient_matrix_UB_12      -0.07680
_diffrn_orient_matrix_UB_13      -0.00210
_diffrn_orient_matrix_UB_21      -0.03501
_diffrn_orient_matrix_UB_22      -0.03894
_diffrn_orient_matrix_UB_23      -0.08476
_diffrn_orient_matrix_UB_31      0.08039
_diffrn_orient_matrix_UB_32      0.02723
_diffrn_orient_matrix_UB_33      -0.01215
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  3.19
_diffrn_reflns_av_sigmaI/netI    0.051
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7014
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.5
_diffrn_standards_decay_%        -1.99
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    29.94
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.636
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_meas      0.000
_exptl_crystal_description       plate
_exptl_crystal_F_000             900.00
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.70
_refine_diff_density_min         -2.75
_refine_ls_extinction_coef       1.60513
_refine_ls_extinction_method     Zachariasen_type_2_gaussian_isotropic
_refine_ls_goodness_of_fit_obs   1.412
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     431
_refine_ls_number_reflns         5047
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_obs          0.0538
_refine_ls_shift/esd_max         0.195
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_all         0.1093
_refine_ls_wR_factor_obs         0.0641
_reflns_number_observed          5047
_reflns_number_total             6413
_reflns_observed_criterion       2.00
_cod_data_source_file            ja983637f.cif
_cod_data_source_block           C48H64B4BiCl10N24NaS6
_cod_original_cell_volume        1833(1)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C48 H64 B4 Bi Cl10 N24 Na S6 '
_cod_database_code               4116317