Conversion of a Zinc Disilazide to a Zinc Hydride Mediated by LiCl
Debabrata Mukherjee; Arkady Ellern; Aaron D. Sadow; Journal of the American Chemical Society 132 (2010) 7582–7583; doi:10.1021/ja102323g

data_4102511
_publ_contact_author_address
;Department of Chemistry
1605 Gilman Hall
Iowa State University
Ames, IA 50011
;
_publ_contact_author_email       sadow@iastate.edu
_publ_contact_author_fax         515-294-0105
_publ_contact_author_name        'Aaron D. Sadow'
_publ_contact_author_phone       515-294-8069
_publ_section_title
;
 Conversion of a Zinc Disilazide to a Zinc Hydride Mediated by LiCl
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7582
_journal_page_last               7583
_journal_paper_doi               10.1021/ja102323g
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C41 H79 B Cl N5 O3 Si2 Zn'
_chemical_formula_weight         857.90
_chemical_melting_point          459
_chemical_name_common            '[NBu4][ToMZn(Cl)N(SiHMe2)2]'
_chemical_name_systematic
'[NBu4]chloro tris(4,4-Me-2-oxazolinyl)phenylborato tetramethyldisilazato zinc'
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.8574(9)
_cell_length_b                   14.4461(6)
_cell_length_c                   15.6143(6)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.34
_cell_volume                     4930.3(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48288
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.69
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.639
_exptl_absorpt_correction_T_max  0.9330
_exptl_absorpt_correction_T_min  0.8936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
_exptl_crystal_recrystallization_method THF
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         12227
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0342P)^2^+0.1431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0754
_reflns_number_gt                10299
_reflns_number_total             12227
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja102323g_si_007.cif
_cod_data_source_block           sad133
_cod_database_code               4102511