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_1548420
_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         'C26 H37 Br2 N O Si'
_chemical_formula_sum            'C26 H37 Br2 N O Si'
_chemical_formula_weight         567.47
_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                85.838(6)
_cell_angle_beta                 75.410(5)
_cell_angle_gamma                84.304(6)
_cell_formula_units_Z            2
_cell_length_a                   8.5127(2)
_cell_length_b                   9.9548(2)
_cell_length_c                   16.5298(12)
_cell_measurement_temperature    566(2)
_cell_volume                     1347.26(11)
_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      566(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0685
_diffrn_reflns_av_sigmaI/netI    0.0622
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17245
_diffrn_reflns_theta_full        65.98
_diffrn_reflns_theta_max         65.98
_diffrn_reflns_theta_min         6.64
_exptl_absorpt_coefficient_mu    4.366
_exptl_absorpt_correction_T_max  0.7215
_exptl_absorpt_correction_T_min  0.6224
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.810
_refine_diff_density_min         -1.764
_refine_diff_density_rms         0.166
_refine_ls_extinction_coef       0.045(3)
_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   1.153
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         4620
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0716
_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^)+(0.1603P)^2^+2.0495P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1961
_refine_ls_wR_factor_ref         0.2677
_reflns_number_gt                3835
_reflns_number_total             4620
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ncomms7913-s2.cif
_cod_data_source_block           1
_cod_depositor_comments
;

2019-03-25
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_moiety     'C52 H74 Br4 N2 O2 Si2'
_cod_original_formula_sum        'C52 H74 Br4 N2 O2 Si2'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     1134.95
_cod_database_code               1548420