Coordinatively Saturated Tris(oxazolinyl)borato Zinc Hydride-Catalyzed Cross Dehydrocoupling of Silanes and Alcohols
Mukherjee, Debabrata; Thompson, Richard R.; Ellern, Arkady; Sadow, Aaron D.; ACS Catalysis 1 (2011) 698–; doi:10.1021/cs2001016

data_4501451
_publ_section_title
;
 Coordinatively Saturated Tris(oxazolinyl)borato Zinc Hydride-Catalyzed
 Cross Dehydrocoupling of Silanes and Alcohols
;
_journal_issue                   7
_journal_name_full               'ACS Catalysis'
_journal_page_first              698
_journal_paper_doi               10.1021/cs2001016
_journal_volume                  1
_journal_year                    2011
_chemical_formula_sum            'C31 H42 B N3 O4.5 Zn'
_chemical_formula_weight         604.86
_chemical_name_common            Sad225
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'APEX2 v2010.11-3'
_cell_angle_alpha                90
_cell_angle_beta                 106.292(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.569(9)
_cell_length_b                   9.896(4)
_cell_length_c                   15.813(7)
_cell_measurement_reflns_used    2931
_cell_measurement_temperature    173.(2)
_cell_measurement_theta_max      20.8730
_cell_measurement_theta_min      2.2811
_cell_volume                     3240(2)
_computing_cell_refinement       'SAINT V7.66A (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 Suite (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.66A (Bruker AXS, 2009)'
_computing_molecular_graphics    'XSHELL (Bruker AXS, 2007)'
_computing_publication_material  'APEX2 Suite (Bruker AXS, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  ' BRUKER APEX2 CCD Diffractometer'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_sigmaI/netI    0.0512
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16141
_diffrn_reflns_theta_full        20.81
_diffrn_reflns_theta_max         20.81
_diffrn_reflns_theta_min         0.98
_exptl_absorpt_coefficient_mu    0.797
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
High peaks of electron density were observed in voids, 
however, all attempts to model disordered by inversion center
 solvent molecule failed. SQUEEZE indicated approximately a
 half of THF solvent per asymmetric unit therefore
 correspondent values were added to final  formula to obtain
 true metric values in outputs. R factor dropped by 0.02.
;
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.337
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.834
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         3390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.834
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0796P)^2^+4.3631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1123
_reflns_number_gt                2668
_reflns_number_total             3390
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs2001016_si_003.cif
_cod_data_source_block           I
_cod_original_cell_volume        3240.(2)
_cod_original_formula_sum        'C31 H42 B N3 O4.50 Zn'
_cod_database_code               4501451