Catalyst and Solvent Free Domino Ring Opening Cyclization: A Greener and Atom Economic Route to 2-Iminothiazolidines
Dahiya, Anjali; Ali, Wajid; Patel, Bhisma K.; ACS Sustainable Chemistry & Engineering 6 (2018) 4272–; doi:10.1021/acssuschemeng.7b04723

data_4517026
_publ_section_title
;
 Catalyst and Solvent Free Domino Ring Opening Cyclization: A Greener and
 Atom Economic Route to 2-Iminothiazolidines
;
_journal_issue                   3
_journal_name_full               'ACS Sustainable Chemistry &amp; Engineering'
_journal_page_first              4272
_journal_paper_doi               10.1021/acssuschemeng.7b04723
_journal_volume                  6
_journal_year                    2018
_chemical_formula_sum            'C21 H24 N2 O S'
_chemical_formula_weight         352.48
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.6334(5)
_cell_length_b                   17.0832(16)
_cell_length_c                   20.6455(19)
_cell_measurement_reflns_used    5553
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.82
_cell_measurement_theta_min      2.38
_cell_volume                     1986.9(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.1096
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            51091
_diffrn_reflns_theta_full        24.75
_diffrn_reflns_theta_max         24.75
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.12(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.821
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3413
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.821
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0697
_refine_ls_shift/su_max          0.000
_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^+5.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1508
_reflns_number_gt                2406
_reflns_number_total             3413
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            sc7b04723_si_002.cif
_cod_data_source_block           p2
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               4517026