2,6-Dimethylmorpholin-4-yl 3,5-dimethyl-1<i>H</i>-pyrazole thioketone
Gerimário F. de Sousa; Inês S. Resck; Lariucci, Carlito; Sabino, Jose R.; Acta Crystallographica Section E 62 (2006) o3366–o3368; doi:10.1107/S1600536806026730

data_2209831
_publ_section_title
;
 2,6-Dimethylmorpholin-4-yl 3,5-dimethyl-1<i>H</i>-pyrazole thioketone
;
_journal_coeditor_code           EZ2013
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3366
_journal_page_last               o3368
_journal_paper_doi               10.1107/S1600536806026730
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C12 H19 N3 O S'
_chemical_formula_moiety         'C12 H19 N3 O S'
_chemical_formula_sum            'C12 H19 N3 O S'
_chemical_formula_weight         253.37
_chemical_name_systematic
;
2,6-Dimethylmorpholin-4-yl 3,5-dimethyl-1H-pyrazole thioketone
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                83.30(2)
_cell_angle_beta                 80.62(2)
_cell_angle_gamma                83.66(2)
_cell_formula_units_Z            2
_cell_length_a                   5.242(2)
_cell_length_b                   11.209(2)
_cell_length_c                   12.082(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      43.8
_cell_measurement_theta_min      13.1
_cell_volume                     692.6(3)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf--Nonius CAD4'
_diffrn_measurement_method       'non-profiled \w/2\q'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.016
_diffrn_reflns_av_sigmaI/netI    0.023
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            2875
_diffrn_reflns_theta_full        67.9
_diffrn_reflns_theta_max         67.9
_diffrn_reflns_theta_min         3.7
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.988
_exptl_absorpt_correction_T_max  0.857
_exptl_absorpt_correction_T_min  0.587
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North <i>et al.</i>,  1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             272
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.72
_refine_diff_density_min         -0.35
_refine_ls_extinction_coef       0.070(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2507
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.099
_refine_ls_R_factor_gt           0.081
_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^)+(0.1279P)^2^+0.6447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.230
_refine_ls_wR_factor_ref         0.248
_reflns_number_gt                1997
_reflns_number_total             2507
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ez2013.cif
_cod_data_source_block           I
_cod_database_code               2209831
_cod_database_fobs_code          2209831