Methyl 2-[(<i>tert</i>-butoxycarbonyl)amino]-3-(3-methyl-2-sulfanylidene-2,3-dihydro-1<i>H</i>-imidazol-1-yl)propanoate
Chan, Chin-Feng; Guo, Yi-Cin; Huang, Bor-Hunn; Chen, Ming-Jen; Acta Crystallographica Section E 68 (2012) o3206–; doi:10.1107/S1600536812043486

data_2236468
_publ_section_title
;
 Methyl
 2-[(<i>tert</i>-butoxycarbonyl)amino]-3-(3-methyl-2-sulfanylidene-2,3-dihydro-1<i>H</i>-imidazol-1-yl)propanoate
;
_journal_coeditor_code           LH5544
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3206
_journal_paper_doi               10.1107/S1600536812043486
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C13 H21 N3 O4 S'
_chemical_formula_moiety         'C13 H21 N3 O4 S'
_chemical_formula_sum            'C13 H21 N3 O4 S'
_chemical_formula_weight         315.39
_chemical_melting_point          379
_chemical_name_common            midazol-1-yl)propanoate
_chemical_name_systematic
;
Methyl 2-[(<i>tert</i>-butoxycarbonyl)amino]-3-(3-methyl-2-sulfanylidene-
2,3-dihydro-1<i>H</i>-imidazol-1-yl)propanoate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 98.4850(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.76360(10)
_cell_length_b                   19.1184(2)
_cell_length_c                   9.6735(2)
_cell_measurement_reflns_used    9755
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      71.4649
_cell_measurement_theta_min      4.6178
_cell_volume                     1603.02(4)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2010)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2010)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2010)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 16.0690
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Agilent Xcalibur (Sapphire3, Gemini)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0127
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12262
_diffrn_reflns_theta_full        71.60
_diffrn_reflns_theta_max         71.60
_diffrn_reflns_theta_min         4.63
_exptl_absorpt_coefficient_mu    1.968
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Agilent, 2010)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.531
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3093
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1200P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1370
_reflns_number_gt                2923
_reflns_number_total             3093
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5544.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2236468
_cod_database_fobs_code          2236468