Lewis Base Mediated β-Elimination and Lewis Acid Mediated Insertion Reactions of Disilazido Zirconium Compounds
KaKing Yan; Juan J. Duchimaza Heredia; Arkady Ellern; Mark S. Gordon; Aaron D. Sadow; Journal of the American Chemical Society 135 (2013) 15225–15237; doi:10.1021/ja407950e

data_4120921
_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
;
 Lewis Base Mediated \b-Elimination and Lewis Acid Mediated Insertion
 Reactions of Disilazido Zirconium Compounds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15225
_journal_page_last               15237
_journal_paper_doi               10.1021/ja407950e
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C36 H26.5 B Br0.5 F18 N O3 S Si2 Zr'
_chemical_formula_weight         1093.31
_chemical_name_common            Sad183
_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 v2010.3-0'
_cell_angle_alpha                103.640(4)
_cell_angle_beta                 108.155(4)
_cell_angle_gamma                99.126(4)
_cell_formula_units_Z            2
_cell_length_a                   11.677(3)
_cell_length_b                   12.731(3)
_cell_length_c                   15.822(4)
_cell_measurement_temperature    173.(2)
_cell_volume                     2102.2(9)
_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_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21808
_diffrn_reflns_theta_full        28.44
_diffrn_reflns_theta_max         28.44
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.961
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
BRUKER SADABS
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_description       block
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.610
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         10431
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0532P)^2^+1.0030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1175
_reflns_number_gt                7483
_reflns_number_total             10431
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja407950e_si_003.cif
_cod_data_source_block           12-Cp2ZrNSiOTfSiH
_cod_original_formula_sum        'C36 H26.50 B Br0.50 F18 N O3 S Si2 Zr'
_cod_database_code               4120921