Isolation of Reactive Intermediate in Deprotonation Reaction with Zinc Alkyls
Victoria P. Colquhoun; Christian Unkelbach; Carsten Strohmann; Chem.Commun. 48 (2012) 5034–; doi:10.1039/c2cc32057f

data_7107697
_publ_section_title
;
 Isolation of Reactive Intermediate in Deprotonation Reaction with Zinc
 Alkyls
;
_journal_name_full               Chem.Commun.
_journal_page_first              5034
_journal_paper_doi               10.1039/c2cc32057f
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C16 H38 N2 Si Zn'
_chemical_formula_weight         351.94
_chemical_name_common
;adduct of diethylzinc and (tert
butylamino)(piperidinomethyl)dimethylsilane
;
_chemical_name_systematic
;
adduct of diethylzinc and (tert butylamino)(piperidinomethyl)dimethylsilane
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-02-22T11:21:41-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 106.918(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.126(5)
_cell_length_b                   10.691(5)
_cell_length_c                   16.231(7)
_cell_measurement_reflns_used    4390
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.99
_cell_measurement_theta_min      2.31
_cell_volume                     2013.1(15)
_computing_cell_refinement       'SAINT-Plus (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus (Bruker, 1999)'
_computing_molecular_graphics
;
Ortep-3 (Farrugia, 1997) and Schakal 92
(Keller 1992)
;
_computing_publication_material  'wingx (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS90 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'Bruker APEXCCD'
_diffrn_measurement_method       \w
_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  0.0417
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43766
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    1.275
_exptl_absorpt_correction_T_max  0.7846
_exptl_absorpt_correction_T_min  0.5151
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.163
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         4390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+0.5125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0715
_reflns_number_gt                3869
_reflns_number_total             4390
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc32057f.txt
_cod_data_source_block           compound_2
_cod_original_cell_volume        2013.3(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7107697