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_4313119
_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         'C35 H67 B O9 Si2 Zr'
_chemical_formula_sum            'C35 H67 B O9 Si2 Zr'
_chemical_formula_weight         790.10
_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                103.1340(10)
_cell_angle_beta                 92.8090(10)
_cell_angle_gamma                118.2060(10)
_cell_formula_units_Z            36
_cell_length_a                   33.0365(6)
_cell_length_b                   34.9417(7)
_cell_length_c                   40.9629(8)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    155(2)
_cell_measurement_theta_max      23.33
_cell_measurement_theta_min      1.75
_cell_volume                     39900.9(14)
_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      155(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  '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  0.0606
_diffrn_reflns_av_sigmaI/netI    0.1373
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            185691
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    0.346
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.603
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular prism'
_exptl_crystal_F_000             15192
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.134
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     7648
_refine_ls_number_reflns         112301
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.1630
_refine_ls_R_factor_gt           0.0674
_refine_ls_shift/su_max          0.525
_refine_ls_shift/su_mean         0.066
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1544
_refine_ls_wR_factor_ref         0.2038
_reflns_number_gt                53974
_reflns_number_total             112301
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0205482_2.cif
_cod_data_source_block           Cp2ZrOB_compound_4
_cod_original_cell_volume        39900.9(13)
_cod_database_code               4313119