Structure and Stereodynamics of N,N-Bis(silyloxy)enamines
Alexander A. Tishkov; Alexander D. Dilman; Valery I. Faustov; Arsenij A. Birukov; Konstantin S. Lysenko; Paul A. Belyakov; Sema L. Ioffe; Yury A. Strelenko; Michael Yu. Antipin; Journal of the American Chemical Society 124 (2002) 11358–11367; doi:10.1021/ja026548i

data_4115163
_publ_section_title
;
 Structure and Stereodynamics of N,N-Bis(silyloxy)enamines
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11358
_journal_page_last               11367
_journal_paper_doi               10.1021/ja026548i
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         'C20 H36 N2 O4 Si2'
_chemical_formula_sum            'C20 H36 N2 O4 Si2'
_chemical_formula_weight         424.69
_chemical_melting_point          301(2)
_chemical_name_systematic
; 
4-Methyl-2-N,N-bis(t-butyldimethylsilyloxy)amino-3-trimethylsilyloxy-pent-1-ene
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.34(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.149(4)
_cell_length_b                   14.155(4)
_cell_length_c                   14.586(5)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      5
_cell_volume                     2467.6(14)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'SHELXTL ver. 5.1 (Sheldrick, 1998a)'
_computing_molecular_graphics    'SHELXTL ver. 5.1 (Sheldrick, 1998a)'
_computing_publication_material  'SHELXTL ver. 5.1 (Sheldrick, 1998a)'
_computing_structure_refinement  'SHELXTL ver. 5.1 (Sheldrick, 1998a)'
_computing_structure_solution    'SHELXTL ver. 5.1 (Sheldrick, 1998a)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_method       '\q/2\q 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  0.0555
_diffrn_reflns_av_sigmaI/netI    0.1081
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5934
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        4
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_description       prism
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.852
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5674
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.852
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1117
_reflns_number_gt                3434
_reflns_number_total             5674
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja026548i_s4.cif
_cod_data_source_block           comp1o
_cod_database_code               4115163