Phosphine-Triggered Tandem Annulation between Morita-Baylis-Hillman Carbonates and Dinucleophiles: Facile Syntheses of Oxazepanes, Thiazepanes, and Diazepanes.
Zhou, Rong; Wang, Jianfang; Duan, Chong; He, Zhengjie; Organic letters 14 (2012) 6134–6137; doi:10.1021/ol302696e

data_1508750
_publ_section_title
;
 Phosphine-Triggered Tandem Annulation between Morita-Baylis-Hillman
 Carbonates and Dinucleophiles: Facile Syntheses of Oxazepanes,
 Thiazepanes, and Diazepanes.
;
_journal_issue                   24
_journal_name_full               'Organic letters'
_journal_page_first              6134
_journal_page_last               6137
_journal_paper_doi               10.1021/ol302696e
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C26 H28 N2 O6 S2'
_chemical_formula_weight         528.62
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.173(12)
_cell_angle_beta                 68.081(12)
_cell_angle_gamma                79.230(14)
_cell_formula_units_Z            2
_cell_length_a                   10.868(2)
_cell_length_b                   11.564(2)
_cell_length_c                   11.8448(19)
_cell_measurement_reflns_used    3883
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.9
_cell_volume                     1271.3(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 14.22
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13507
_diffrn_reflns_theta_full        27.89
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.254
_exptl_absorpt_correction_T_max  0.9750
_exptl_absorpt_correction_T_min  0.9653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.14
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_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.489
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         5991
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_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                3466
_reflns_number_total             5991
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol302696e_si_002.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1271.4(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1508750