Reaction of [2-(SiH3)C6H4]2SiH2 with Ni(Et2PCH2CH2PEt2)(PEt3)2: Characterization of η2-(Si-H)Ni and NiIV-H Complexes
Wanzhi Chen; Shigeru Shimada; Masato Tanaka; Yuka Kobayashi; Kazuhiko Saigo; Journal of the American Chemical Society 126 (2004) 8072–8073; doi:10.1021/ja039244k

data_4112709
_publ_contact_author_address
;
National Institute of Advanced Industrial Science and Technology,
Tukuba Central 5, Tsukuba, Ibaraki 305-8565, Japan
;
_publ_contact_author_email       s-shimada@aist.go.jp
_publ_contact_author_fax         +81-29-861-4511
_publ_contact_author_name        'Shigeru Shimada'
_publ_contact_author_phone       +81-29-861-6257
_publ_section_title
;
 Reaction of [2-(SiH3)C6H4]2SiH2 with Ni(Et2PCH2CH2PEt2)(PEt3)2:
 Characterization of \h2-(Si-H)Ni and NiIV-H Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8072
_journal_page_last               8073
_journal_paper_doi               10.1021/ja039244k
_journal_volume                  126
_journal_year                    2004
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C22 H38 Ni P2 Si3 '
_chemical_formula_sum            'C22 H38 Ni P2 Si3'
_chemical_formula_weight         507.45
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2004-02-02
_audit_creation_method           'by CrystalStructure 3.6.0'
_cell_angle_alpha                90
_cell_angle_beta                 101.7990(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.2218(4)
_cell_length_b                   14.3152(6)
_cell_length_c                   9.8666(4)
_cell_measurement_reflns_used    6183
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      28.257
_cell_measurement_theta_min      2.544
_cell_volume                     1274.99(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 2003'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean '8.366 [pixels/mm]'
_diffrn_measured_fraction_theta_full 0.9967
_diffrn_measured_fraction_theta_max 0.9967
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            8989
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_exptl_absorpt_coefficient_mu    1.035
_exptl_absorpt_correction_T_max  0.9405
_exptl_absorpt_correction_T_min  0.9036
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS; Sheldrick 1996'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             540.00
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.45
_refine_diff_density_min         -1.07
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.016(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     370
_refine_ls_number_reflns         8974
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[0.9030\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0690
_reflns_number_gt                8626
_reflns_number_total             8974
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja039244ksi20040206_044714.cif
_cod_data_source_block           General
_cod_original_sg_symbol_Hall     p_2yb
_cod_original_formula_sum        'C22 H38 Ni P2 Si3 '
_cod_database_code               4112709