Cu(OAc)2-Promoted Cascade Carboamination/Oxidative Cyclization of C-Acylimines with Alkenes.
Dang, Ling; Liang, Libo; Qian, Cheng; Fu, Meiqin; Ma, Tongmei; Xu, Dingguo; Jiang, Huanfeng; Zeng, Wei; The Journal of organic chemistry 79 (2014) 769–776; doi:10.1021/jo402705w

data_4028982
_publ_section_title
;
 Cu(OAc)2-Promoted Cascade Carboamination/Oxidative Cyclization of
 C-Acylimines with Alkenes.
;
_journal_issue                   2
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              769
_journal_page_last               776
_journal_paper_doi               10.1021/jo402705w
_journal_volume                  79
_journal_year                    2014
_chemical_formula_sum            'C30 H29 N3 O7 S'
_chemical_formula_weight         575.62
_chemical_name_common            Bridged-bisheterocycle_(3a)
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.45(3)
_cell_angle_beta                 79.49(3)
_cell_angle_gamma                72.23(3)
_cell_formula_units_Z            2
_cell_length_a                   10.893(2)
_cell_length_b                   11.806(2)
_cell_length_c                   11.988(2)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.05
_cell_volume                     1421.8(5)
_computing_cell_refinement       'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13883
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  0.9675
_exptl_absorpt_correction_T_min  0.9518
_exptl_crystal_colour            blown
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6427
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1503P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1707
_refine_ls_wR_factor_ref         0.2369
_reflns_number_gt                4043
_reflns_number_total             6427
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo402705w_si_002.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        1421.7(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4028982