Lewis Acid-Mediated β-Hydride Abstraction Reactions of Divalent M(C(SiHMe2)3)2THF2(M = Ca, Yb)
KaKing Yan; Brianna M. Upton; Arkady Ellern; Aaron D. Sadow; Journal of the American Chemical Society 131 (2009) 15110–15111; doi:10.1021/ja9070865

data_4105210
_publ_contact_author_address
;1605 Gilman Hall
Department of Chemistry
Iowa State University
Ames IA 50011
;
_publ_contact_author_email       sadow@iastate.edu
_publ_contact_author_fax         5152940105
_publ_contact_author_name        'Aaron D. Sadow'
_publ_contact_author_phone       5152948069
_publ_section_title
;
 Lewis Acid-Mediated \b-Hydride Abstraction Reactions of Divalent
 M(C(SiHMe2)3)2THF2(M = Ca, Yb)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15110
_journal_page_last               15111
_journal_paper_doi               10.1021/ja9070865
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C14 H40 Si6'
_chemical_formula_weight         377.00
_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           SHELXL-97
_cell_angle_alpha                104.555(19)
_cell_angle_beta                 91.47(2)
_cell_angle_gamma                114.49(2)
_cell_formula_units_Z            1
_cell_length_a                   8.512(7)
_cell_length_b                   8.569(7)
_cell_length_c                   9.253(9)
_cell_measurement_reflns_used    715
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.73
_cell_volume                     588.0(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3013
_diffrn_reflns_av_sigmaI/netI    0.2229
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3026
_diffrn_reflns_theta_full        21.00
_diffrn_reflns_theta_max         21.00
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             208
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         1275
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_gt           0.0771
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1379P)^2^+0.6066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1992
_refine_ls_wR_factor_ref         0.2429
_reflns_number_gt                859
_reflns_number_total             1275
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9070865_si_004.cif
_cod_data_source_block           disilacyclobutane
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_database_code               4105210