Access to Cyclobutene-Fused Azepines through Au-Catalyzed Cycloisomerization of Stable Alkyne Tethered Ketene N,N-Acetals.
Nayak, Sanatan; Ghosh, Nayan; Sahoo, Akhila K.; Organic letters 16 (2014) 2996–2999; doi:10.1021/ol501125r

data_1516131
_publ_section_title
;
 Access to Cyclobutene-Fused Azepines through Au-Catalyzed
 Cycloisomerization of Stable Alkyne Tethered Ketene N,N-Acetals.
;
_journal_issue                   11
_journal_name_full               'Organic letters'
_journal_page_first              2996
_journal_page_last               2999
_journal_paper_doi               10.1021/ol501125r
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C39 H38 N2 O8 S2'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 79.626(11)
_cell_angle_gamma                82.116(11)
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_cell_length_b                   12.6893(16)
_cell_length_c                   16.278(2)
_cell_measurement_reflns_used    1287
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      20.8560
_cell_measurement_theta_min      2.8640
_cell_volume                     1765.6(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.840
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_h_max       10
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_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
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_diffrn_reflns_limit_l_min       -22
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_diffrn_reflns_theta_max         29.22
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    0.208
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_exptl_absorpt_correction_T_min  0.93252
_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.20
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_refine_diff_density_max         0.397
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.0011(2)
_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   0.841
_refine_ls_hydrogen_treatment    mixed
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_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^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.1458
_reflns_number_gt                2180
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_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ol501125r_si_005.cif
_cod_data_source_block           aks96
_cod_depositor_comments
'Adding full bibliography for 1516129--1516131.cif.'
_cod_original_cell_volume        1765.5(4)
_cod_database_code               1516131