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_1548423
_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         'C45 H62 N4 O9 Si2'
_chemical_formula_sum            'C45 H62 N4 O9 Si2'
_chemical_formula_weight         859.17
_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
_cell_angle_alpha                83.987(6)
_cell_angle_beta                 80.786(6)
_cell_angle_gamma                68.014(5)
_cell_formula_units_Z            2
_cell_length_a                   10.94190(10)
_cell_length_b                   13.4756(2)
_cell_length_c                   18.1470(12)
_cell_measurement_temperature    293(2)
_cell_volume                     2446.21(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33733
_diffrn_reflns_theta_full        69.17
_diffrn_reflns_theta_max         69.17
_diffrn_reflns_theta_min         6.58
_exptl_absorpt_coefficient_mu    1.100
_exptl_absorpt_correction_T_max  0.8100
_exptl_absorpt_correction_T_min  0.8100
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.0144(4)
_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    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         8794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0220P)^2^+1.6700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1403
_reflns_number_gt                6134
_reflns_number_total             8794
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ncomms7913-s5.cif
_cod_data_source_block           xy
_cod_original_cell_volume        2446.21(17)
_cod_database_code               1548423