Synthesis of tetrasubstituted 1-silyloxy-3-aminobutadienes and chemistry beyond Diels-Alder reactions
Xijian Li; Siyu Peng; Li Li; Yong Huang; Nature Communications 6 (2015) 6913–; doi:10.1038/ncomms7913

data_1548422
_publ_section_title
;
 Synthesis of tetrasubstituted 1-silyloxy-3-aminobutadienes and chemistry
 beyond Diels-Alder reactions
;
_journal_name_full               'Nature Communications'
_journal_page_first              6913
_journal_paper_doi               10.1038/ncomms7913
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C27 H37 N O2 Si'
_chemical_formula_sum            'C27 H37 N O2 Si'
_chemical_formula_weight         435.67
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 100.544(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.8831(6)
_cell_length_b                   7.8642(3)
_cell_length_c                   19.9523(7)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      62.67
_cell_measurement_theta_min      3.79
_cell_volume                     2604.38(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21402
_diffrn_reflns_theta_full        62.67
_diffrn_reflns_theta_max         62.67
_diffrn_reflns_theta_min         3.79
_exptl_absorpt_coefficient_mu    0.953
_exptl_absorpt_correction_T_max  0.834
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.111
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.038
_refine_ls_extinction_coef       0.00250(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         4157
_refine_ls_number_restraints     333
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0633
_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^)+(0.0000P)^2^+2.6500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1176
_reflns_number_gt                3509
_reflns_number_total             4157
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ncomms7913-s4.cif
_cod_data_source_block           x
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               1548422