Synthesis of Alkali Metal Salts of Borylsilyl Anions Utilizing Highly Crowded Silylboranes and Their Properties#
Kajiwara, Takashi; Takeda, Nobuhiro; Sasamori, Takahiro; Tokitoh, Norihiro; Organometallics 27 (2008) 880–; doi:10.1021/om7008974

data_4070636
_publ_section_title
;
 Synthesis of Alkali Metal Salts of Borylsilyl Anions Utilizing Highly
 Crowded Silylboranes and Their Properties#
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              880
_journal_paper_doi               10.1021/om7008974
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C45 H91 B O2 Si8 '
_chemical_formula_sum            'C45 H91 B O2 Si8'
_chemical_formula_weight         899.71
_chemical_name_common            BSiTMS
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                65.154(12)
_cell_angle_beta                 78.169(12)
_cell_angle_gamma                88.869(18)
_cell_formula_units_Z            4
_cell_length_a                   13.100(7)
_cell_length_b                   20.193(10)
_cell_length_c                   24.014(11)
_cell_measurement_temperature    103(2)
_cell_volume                     5626(5)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0640
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            31913
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.96
_exptl_absorpt_coefficient_mu    0.222
_exptl_absorpt_correction_T_max  0.9569
_exptl_absorpt_correction_T_min  0.9569
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.062
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1065
_refine_ls_number_reflns         18704
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0605
_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^)+(0.0625P)^2^+3.7118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1368
_refine_ls_wR_factor_ref         0.1475
_reflns_number_gt                15139
_reflns_number_total             18704
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7008974-file001.cif
_cod_data_source_block           bsitms
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
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_cod_database_code               4070636