Methyl 3-[3-(ethoxycarbonyl)thioureido]-1<i>H</i>-pyrazole-5-carboxylate
Huang, Buwen; Kung, Pei-Pei; Rheingold, Arnold L.; DiPasquale, Antonio; Yanovsky, Alex; Acta Crystallographica Section E 65 (2009) o1249–; doi:10.1107/S1600536809016742

data_2221993
_publ_section_title
;
 Methyl
 3-[3-(ethoxycarbonyl)thioureido]-1<i>H</i>-pyrazole-5-carboxylate
;
_journal_coeditor_code           DN2451
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1249
_journal_paper_doi               10.1107/S1600536809016742
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C9 H12 N4 O4 S'
_chemical_formula_moiety         'C9 H12 N4 O4 S'
_chemical_formula_sum            'C9 H12 N4 O4 S'
_chemical_formula_weight         272.29
_chemical_name_systematic
;
Methyl 3-[3-(ethoxycarbonyl)thioureido]-1<i>H</i>-pyrazole-5-carboxylate
;
_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
_cell_angle_alpha                64.5100(10)
_cell_angle_beta                 82.2940(10)
_cell_angle_gamma                78.7160(10)
_cell_formula_units_Z            2
_cell_length_a                   8.0855(8)
_cell_length_b                   9.0035(8)
_cell_length_c                   9.5959(9)
_cell_measurement_reflns_used    3767
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      2.5
_cell_volume                     617.39(10)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'ORTEP-32 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla <i>et al.</i>,  2005)'
_diffrn_ambient_temperature      208(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_device_type  'Siemens P4 diffractometer with APEX CCD'
_diffrn_measurement_method       '\f and \w 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  0.044
_diffrn_reflns_av_sigmaI/netI    0.052
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5852
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         28.2
_diffrn_reflns_theta_min         2.4
_exptl_absorpt_coefficient_mu    0.276
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             284
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.39
_refine_diff_density_min         -0.28
_refine_ls_extinction_coef       0.064(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.047
_refine_ls_R_factor_gt           0.040
_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^)+(0.0521P)^2^+0.1805P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.106
_refine_ls_wR_factor_ref         0.113
_reflns_number_gt                2255
_reflns_number_total             2653
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn2451.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2221993
_cod_database_fobs_code          2221993