Synthesis of thiazolidines via regioselective addition of unsymmetric thioureas to maleic acid derivatives
Pankova, Alena S.; Samartsev, Mikhail A.; Shulgin, Igor A.; Golubev, Pavel R.; Avdontceva, Margarita S.; Kuznetsov, Mikhail A.; RSC Adv. 4 (2014) 51780–; doi:10.1039/C4RA07840C

data_7218533
_publ_section_title
;
 Synthesis of thiazolidines via regioselective addition of unsymmetric
 thioureas to maleic acid derivatives
;
_journal_issue                   93
_journal_name_full               'RSC Adv.'
_journal_page_first              51780
_journal_paper_doi               10.1039/C4RA07840C
_journal_volume                  4
_journal_year                    2014
_chemical_formula_sum            'C20 H21 N3 O2 S'
_chemical_formula_weight         367.46
_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                71.1056(19)
_cell_angle_beta                 83.1820(19)
_cell_angle_gamma                86.6139(18)
_cell_formula_units_Z            2
_cell_length_a                   5.30469(13)
_cell_length_b                   12.5053(3)
_cell_length_c                   14.6627(3)
_cell_measurement_reflns_used    11535
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.5893
_cell_measurement_theta_min      3.2009
_cell_volume                     913.54(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3829
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18386
_diffrn_reflns_theta_full        71.00
_diffrn_reflns_theta_max         71.00
_diffrn_reflns_theta_min         3.20
_exptl_absorpt_coefficient_mu    1.731
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71274
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3539
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0364P)^2^+1.1562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0939
_reflns_number_gt                3339
_reflns_number_total             3539
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra07840c2.cif
_cod_data_source_block           shilgin_obr2
_cod_original_cell_volume        913.53(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7218533