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_4102507
_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            'C28.5 H47 B N4 O3 Si2 Zn'
_chemical_formula_weight         626.06
_chemical_melting_point          505
_chemical_name_common            ToMZnN(SiHMe2)2
_chemical_name_systematic
'tris(4,4-dimethyl-2-oxazolinyl)phenylborato tetramethyldisilazato zinc'
_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           'APEX2 v2009.7-0'
_cell_angle_alpha                97.8930(10)
_cell_angle_beta                 98.3800(10)
_cell_angle_gamma                106.9340(10)
_cell_formula_units_Z            4
_cell_length_a                   9.9164(7)
_cell_length_b                   15.0927(10)
_cell_length_c                   24.2345(16)
_cell_measurement_reflns_used    8669
_cell_measurement_temperature    153.(2)
_cell_measurement_theta_max      28.2242
_cell_measurement_theta_min      2.1907
_cell_volume                     3370.3(4)
_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      153.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'BRUKER APEX2 CCD Diffractometer'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0526
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            34655
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.833
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs Version 2008/1'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.624
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     756
_refine_ls_number_reflns         16487
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.053
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+0.7448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1161
_reflns_number_gt                12196
_reflns_number_total             16487
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja102323g_si_003.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C28.50 H47 B N4 O3 Si2 Zn'
_cod_database_code               4102507