2-[1-(2-Hydroxy-6-methoxyphenyl)ethylidene]-<i>N</i>-methylhydrazinecarbothioamide acetonitrile monosolvate
Anderson, Brian J.; Keeler, Alexander M.; O'Rourke, Kelly A.; Krauss, Shannon T.; Jasinski, Jerry P.; Acta Crystallographica Section E 69 (2013) o11–; doi:10.1107/S1600536812048799

data_2237214
_publ_section_title
;
 2-[1-(2-Hydroxy-6-methoxyphenyl)ethylidene]-<i>N</i>-methylhydrazinecarbothioamide
 acetonitrile monosolvate
;
_journal_coeditor_code           RK2388
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o11
_journal_paper_doi               10.1107/S1600536812048799
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C11 H15 N3 O2 S, C2 H3 N'
_chemical_formula_moiety         'C11 H15 N3 O2 S, C2 H3 N'
_chemical_formula_sum            'C13 H18 N4 O2 S'
_chemical_formula_weight         294.38
_chemical_melting_point_gt       415
_chemical_melting_point_lt       420
_chemical_name_systematic
;
2-[1-(2-Hydroxy-6-methoxyphenyl)ethylidene]-<i>N</i>-
methylhydrazinecarbothioamide acetonitrile monosolvate
;
_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                80.121(8)
_cell_angle_beta                 71.555(10)
_cell_angle_gamma                74.732(10)
_cell_formula_units_Z            2
_cell_length_a                   7.6232(10)
_cell_length_b                   9.4004(9)
_cell_length_c                   11.8031(12)
_cell_measurement_reflns_used    2112
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      72.2920
_cell_measurement_theta_min      3.9633
_cell_volume                     770.44(16)
_computing_cell_refinement       '<i>CrysAlis PRO</i> (Agilent, 2012)'
_computing_data_collection       '<i>CrysAlis PRO</i> (Agilent, 2012)'
_computing_data_reduction        '<i>CrysAlis RED</i> (Agilent, 2012)'
_computing_molecular_graphics    '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_publication_material  '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.0416
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Agilent Xcalibur (Eos, Gemini CCD)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X--ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4716
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         72.44
_diffrn_reflns_theta_min         3.97
_exptl_absorpt_coefficient_mu    1.934
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57507
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>CrysAlis PRO</i> and <i>CrysAlis RED</i>; Agilent, 2012)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             312
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.132
_refine_diff_density_min         -0.260
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2968
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0627
_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^)+(0.1150P)^2^+0.1027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1618
_refine_ls_wR_factor_ref         0.1702
_reflns_number_gt                2622
_reflns_number_total             2968
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rk2388.cif
_cod_data_source_block           I
_cod_database_code               2237214
_cod_database_fobs_code          2237214