Tris(tert-butoxy)siloxy Derivatives of Boron, Including the Boronous Acid HOB[OSi(OtBu)3]2 and the Metal (Siloxy)boryloxide Complex Cp2Zr(Me)OB[OSi(OtBu)3]2: A Remarkable Crystal Structure with 18 Independent Molecules in Its Asymmetric Unit
Kyle L. Fujdala; Allen G. Oliver; Frederick J. Hollander; T. Don Tilley; Inorganic Chemistry 42 (2003) 1140–1150; doi:10.1021/ic0205482

data_4313118
_publ_section_title
;
 Tris(tert-butoxy)siloxy Derivatives of Boron, Including the Boronous Acid
 HOB[OSi(OtBu)3]2 and the Metal (Siloxy)boryloxide Complex
 Cp2Zr(Me)OB[OSi(OtBu)3]2: A Remarkable Crystal Structure with 18
 Independent Molecules in Its Asymmetric Unit
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1140
_journal_page_last               1150
_journal_paper_doi               10.1021/ic0205482
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C28 H63 B O9 Si2'
_chemical_formula_sum            'C28 H63 B O9 Si2'
_chemical_formula_weight         610.77
_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
_cell_angle_alpha                93.089(3)
_cell_angle_beta                 101.8720(10)
_cell_angle_gamma                101.340(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4639(5)
_cell_length_b                   11.8965(4)
_cell_length_c                   17.8225(11)
_cell_measurement_reflns_used    2530
_cell_measurement_temperature    159(2)
_cell_measurement_theta_max      23.0
_cell_measurement_theta_min      1.75
_cell_volume                     1916.00(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL-XP'(Bruker, 1995)'
_computing_structure_refinement  'SHELXTL-XL (Bruker, 1995)'
_computing_structure_solution    'SHELXTL-XS (Bruker, 1995)'
_diffrn_ambient_temperature      159(2)
_diffrn_measurement_device       'SMART CCD'
_diffrn_measurement_method       \w-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  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0901
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8698
_diffrn_reflns_theta_max         22.99
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.134
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.333
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.059
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.983
_refine_ls_goodness_of_fit_obs   1.127
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         5153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_restrained_S_obs      1.127
_refine_ls_R_factor_all          0.1356
_refine_ls_R_factor_obs          0.0825
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1568P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2475
_refine_ls_wR_factor_obs         0.2116
_reflns_number_observed          3089
_reflns_number_total             5239
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0205482_1.cif
_cod_data_source_block           BOSi2_compound_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1568P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1568P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1916.0(2)
_cod_database_code               4313118