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_7107699
_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_absolute_configuration syn
_chemical_formula_sum            'C20 H47 N3 Si Zn'
_chemical_formula_weight         423.07
_chemical_name_common
;
adduct of diethylzinc and (tert butylamino)-(N,N?,N?-
trimethylcyclohexyl-1R,2R-diamino-N-methyl)-dimethylsilane
;
_chemical_name_systematic
;
adduct of diethylzinc and (tert
butylamino)-(N,N?,N?-trimethylcyclohexyl-1R,2R-diamino-N-methyl)-dimethylsilane
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-02-23T09:49:22-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 107.870(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7303(5)
_cell_length_b                   10.1126(3)
_cell_length_c                   17.4314(6)
_cell_measurement_reflns_used    4845
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.46
_cell_volume                     2471.34(15)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET)
(compiled Oct 24 2008,09:44:38)'
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET)
(compiled Oct 24 2008,09:44:38)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET)
(compiled Oct 24 2008,09:44:38)
;
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'Xcalibur S Oxford Diffraction'
_diffrn_measurement_method       Omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22745
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    1.05
_exptl_absorpt_correction_T_max  0.7435
_exptl_absorpt_correction_T_min  0.7435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd. Empirical absorption correction using
spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.184
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.010(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         4845
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.01
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0546
_reflns_number_gt                4495
_reflns_number_total             4845
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc32057f.txt
_cod_data_source_block           compounds_4
_cod_original_cell_volume        2471.35(13)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7107699