Exploring the scope of the isothiourea-mediated synthesis of dihydropyridinones.
Yeh, Pei-Pei; Daniels, David S. B.; Fallan, Charlene; Gould, Eoin; Simal, Carmen; Taylor, James E.; Slawin, Alexandra M. Z.; Smith, Andrew D.; Organic & biomolecular chemistry 13 (2015) 2177–2191; doi:10.1039/c4ob02408g

data_7154263
_publ_section_title
;
 Exploring the scope of the isothiourea-mediated synthesis of
 dihydropyridinones.
;
_journal_issue                   7
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2177
_journal_page_last               2191
_journal_paper_doi               10.1039/c4ob02408g
_journal_volume                  13
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C27 H25 N O6 S'
_chemical_formula_sum            'C27 H25 N O6 S'
_chemical_formula_weight         491.56
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_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_update_record
;
2014-11-13 deposited with the CCDC.
2014-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                66.024(17)
_cell_angle_beta                 83.58(3)
_cell_angle_gamma                78.23(2)
_cell_formula_units_Z            1
_cell_length_a                   5.5082(17)
_cell_length_b                   10.112(2)
_cell_length_c                   11.961(2)
_cell_measurement_reflns_used    2277
_cell_measurement_temperature    93
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.24
_cell_volume                     595.6(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 rc13'
_computing_data_collection
'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 rc13'
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3716
_diffrn_reflns_point_group_measured_fraction_full 0.649
_diffrn_reflns_point_group_measured_fraction_max 0.640
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.295
_diffrn_reflns_theta_min         2.239
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.180
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             258.00
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.67
_refine_diff_density_min         -0.33
_refine_ls_abs_structure_details
;
 Flack x determined using 621 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, S., Flack, H.D. and Wagner, T. Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     316
_refine_ls_number_reflns         2782
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0574P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                2644
_reflns_number_total             2782
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c4ob02408g2.cif
_cod_data_source_block           31
_cod_depositor_comments
'Adding full bibliography for 7154263--7154264.cif.'
_cod_database_code               7154263
_shelx_res_checksum              66735