A new multicomponent reaction: unexpected formation of derivatizable cyclic α-alkoxy isothioureas.
Brockmeyer, Fabian; Morosow, Valentin; Martens, Jürgen; Organic & biomolecular chemistry 13 (2015) 3341–3346; doi:10.1039/c4ob02608j

data_7154298
_publ_section_title
;
 A new multicomponent reaction: unexpected formation of derivatizable
 cyclic \a-alkoxy isothioureas.
;
_journal_issue                   11
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              3341
_journal_page_last               3346
_journal_paper_doi               10.1039/c4ob02608j
_journal_volume                  13
_journal_year                    2015
_chemical_formula_sum            'C12 H15 Cl N2 O S'
_chemical_formula_weight         270.77
_chemical_melting_point          388663.15
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-12-04 deposited with the CCDC.
2015-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                110.753(2)
_cell_angle_beta                 98.248(2)
_cell_angle_gamma                103.002(3)
_cell_formula_units_Z            2
_cell_length_a                   6.1948(3)
_cell_length_b                   10.9643(5)
_cell_length_c                   11.2530(5)
_cell_measurement_reflns_used    3302
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.61
_cell_measurement_theta_min      3.41
_cell_volume                     675.19(6)
_computing_cell_refinement       'Bruker AXS SAINT V7.60A'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker AXS SAINT V7.60A'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0575
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6165
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.423
_exptl_absorpt_correction_T_max  0.9916
_exptl_absorpt_correction_T_min  0.9354
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             284
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/n-hexane'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         6165
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0500P)^2^+0.5500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1253
_reflns_number_gt                4708
_reflns_number_total             6165
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ob02608j2.cif
_cod_data_source_block           svwfp16_5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '388390 C ' was changed to
'388663.15' - it was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 7154298.cif.
;
_cod_original_cell_volume        675.19(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7154298