Four-Component Reaction for the Synthesis of Dithiocarbamates Starting from Cyclic Imines.
Schlüter, Torben; Ziyaei Halimehjani, Azim; Wachtendorf, Daniel; Schmidtmann, Marc; Martens, Jürgen; ACS combinatorial science 18 (2016) 456–460; doi:10.1021/acscombsci.6b00029

data_4513909
_publ_section_title
;
 Four-Component Reaction for the Synthesis of Dithiocarbamates Starting
 from Cyclic Imines.
;
_journal_issue                   8
_journal_name_full               'ACS combinatorial science'
_journal_page_first              456
_journal_page_last               460
_journal_paper_doi               10.1021/acscombsci.6b00029
_journal_volume                  18
_journal_year                    2016
_chemical_formula_structural     C17H24N2OS3
_chemical_formula_sum            'C17 H24 N2 O S3'
_chemical_formula_weight         368.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90
_cell_angle_beta                 98.6470(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6665(7)
_cell_length_b                   8.8044(3)
_cell_length_c                   12.3437(5)
_cell_measurement_reflns_used    9637
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.33
_cell_measurement_theta_min      2.33
_cell_volume                     1898.15(13)
_computing_cell_refinement       'Bruker SAINT V8.34A'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT V8.34A'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0104
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            96731
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.316
_diffrn_reflns_theta_min         2.332
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.396
_exptl_absorpt_correction_T_max  0.9478
_exptl_absorpt_correction_T_min  0.8634
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS-2014/5 (Sheldrick)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         9213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.6000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0787
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8362
_reflns_number_total             9213
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            co6b00029_si_001.cif
_cod_data_source_block           tos1429
_cod_depositor_comments          'Adding full bibliography for 4513909.cif.'
_cod_database_code               4513909
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.851
_shelx_estimated_absorpt_t_max   0.932
_exptl_absorpt_special_details
;
 numerical absorption correction followed by correction based on
 symmetry-related measurements (multi-scan)
;
_shelx_res_checksum              25308
_shelx_hkl_checksum              79610