<i>S</i>-Phenyl <i>N</i>,<i>N</i>'-dimethyl-^13^C~2~-thiooxamate: a by-product in the synthesis of ethyl <i>N</i>,<i>N</i>'-dimethyl-^13^C~2~-oxamate
Asani, Ernest M.; Khrustalev, Victor N.; Juarez, Ernesto; Martinez, Rodolfo A.; Timofeeva, Tatiana V.; Acta Crystallographica Section E 63 (2007) o1802–o1804; doi:10.1107/S1600536807011324

data_2212755
_publ_section_title
;
 <i>S</i>-Phenyl <i>N</i>,<i>N</i>'-dimethyl-^13^C~2~-thiooxamate: a
 by-product in the synthesis of ethyl
 <i>N</i>,<i>N</i>'-dimethyl-^13^C~2~-oxamate
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1802
_journal_page_last               o1804
_journal_paper_doi               10.1107/S1600536807011324
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C10 H11 N O2 S'
_chemical_formula_moiety         'C10 H11 N O2 S'
_chemical_formula_sum            'C10 H11 N O2 S'
_chemical_formula_weight         209.26
_chemical_name_systematic
;
S-Phenyl N,N'-dimethyl-^13^C~2~-thiooxamate
;
_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                73.332(4)
_cell_angle_beta                 86.321(4)
_cell_angle_gamma                78.345(4)
_cell_formula_units_Z            2
_cell_length_a                   5.8925(16)
_cell_length_b                   7.950(2)
_cell_length_c                   11.332(3)
_cell_measurement_reflns_used    3343
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.15
_cell_measurement_theta_min      2.73
_cell_volume                     498.1(2)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD area-detector'
_diffrn_measurement_method       '\f and omega scans'
_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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6584
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.297
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             220
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         2360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.04P)^2^+0.07P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0729
_reflns_number_gt                2006
_reflns_number_total             2360
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            at2236.cif
_cod_data_source_block           3
_cod_database_code               2212755
_cod_database_fobs_code          2212755