N-Methyl-2-{3-methyl-2-[(2Z)-pent-2-en-1-yl]cyclopent-2-en-1-ylidene}hydrazinecarbothioamide
Oliveira, Adriano Bof de; Bresolin, Leandro; Beck, Johannes; Daniels, Jörg; IUCrData 9 (2024) x240013–; doi:10.1107/S2414314624000130

data_1570750
_publ_section_title
;
 N-Methyl-2-{3-methyl-2-[(2Z)-pent-2-en-1-yl]cyclopent-2-en-1-ylidene}hydrazinecarbothioamide
;
_journal_issue                   1
_journal_name_full               IUCrData
_journal_page_first              x240013
_journal_paper_doi               10.1107/S2414314624000130
_journal_volume                  9
_journal_year                    2024
_chemical_formula_iupac          'C13 H21 N3 S'
_chemical_formula_moiety         'C13 H21 N3 S'
_chemical_formula_sum            'C13 H21 N3 S'
_chemical_formula_weight         251.39
_chemical_name_common            'cis-Jasmone 4-methylthiosemicarbazone'
_chemical_name_systematic
<i>N</i>-Methyl-2-{3-methyl-2-[(2<i>Z</i>)-pent-2-en-1-yl]cyclopent-2-en-1-ylidene}hydrazinecarbothioamide
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                83.0428(18)
_cell_angle_beta                 86.9392(13)
_cell_angle_gamma                76.5236(18)
_cell_formula_units_Z            4
_cell_length_a                   7.9583(2)
_cell_length_b                   11.2703(2)
_cell_length_c                   16.0080(5)
_cell_measurement_reflns_used    22795
_cell_measurement_temperature    223
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_volume                     1385.51(6)
_computing_cell_refinement
;
HKL Scalepack (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
COLLECT (Nonius, 1998)
;
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006), <i>Crystal Explorer 3.1</i> (Wolff <i>et
al.</i>,
2012)
;
_computing_publication_material
;
WinGX (Farrugia, 2012), publCIF (Westrip, 2010) and
enCIFer (Allen <i>et al.</i>,
2004)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR-92 (Altomare <i>et al.</i>,  1994)
;
_diffrn_ambient_temperature      223
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Enraf--Nonius FR590 Kappa CCD'
_diffrn_measurement_method
'CCD rotation images, thick slices, \k-goniostat'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0663
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23118
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.518
_diffrn_reflns_theta_min         2.959
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_T_max  0.9782
_exptl_absorpt_correction_T_min  0.9448
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(Alcock, 1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       prism
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.116
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.239
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         6319
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0556P)^2^+0.4261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1399
_reflns_number_gt                3700
_reflns_number_total             6319
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bt4146.cif
_cod_data_source_block           I
_cod_database_code               1570750
_shelx_estimated_absorpt_t_min   0.942
_shelx_estimated_absorpt_t_max   0.975
_shelx_hkl_checksum              40858
_shelx_res_checksum              38777