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_4120922
_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            'C17 H31 N O Si2 Zr'
_chemical_formula_weight         412.83
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'APEX2 v2012.4-3'
_cell_angle_alpha                90
_cell_angle_beta                 96.440(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3458(12)
_cell_length_b                   15.4989(19)
_cell_length_c                   14.4616(18)
_cell_measurement_reflns_used    3414
_cell_measurement_temperature    173.(2)
_cell_measurement_theta_max      24.0659
_cell_measurement_theta_min      2.4741
_cell_volume                     2081.5(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0611
_diffrn_reflns_av_sigmaI/netI    0.0578
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21875
_diffrn_reflns_theta_full        28.74
_diffrn_reflns_theta_max         28.74
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.645
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       plate
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.580
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         5397
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+0.7267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0857
_reflns_number_gt                3982
_reflns_number_total             5397
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja407950e_si_004.cif
_cod_data_source_block           I
_cod_database_code               4120922