Charge density of 4-methyl-3-[(tetrahydro-2<i>H</i>-pyran-2-yl)oxy]thiazole-2(3<i>H</i>)-thione. A comprehensive multipole refinement, maximum entropy method and density functional theory study
Vénosová, Barbora; Koziskova, Julia; Kožíšek, Jozef; Herich, Peter; Lušpai, Karol; Petricek, Vaclav; Hartung, Jens; Müller, Mike; Hübschle, Christian B.; van Smaalen, Sander; Bucinsky, Lukas; Acta Crystallographica Section B 76 (2020) –; doi:10.1107/S2052520620005533

data_2108611
_publ_section_title
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 Charge density of
 4-methyl-3-[(tetrahydro-2<i>H</i>-pyran-2-yl)oxy]thiazole-2(3<i>H</i>)-thione.
 A comprehensive multipole refinement, maximum entropy method and density
 functional theory study
;
_journal_coeditor_code           PX5018SUP1
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520620005533
_journal_volume                  76
_journal_year                    2020
_chemical_formula_moiety         'C9 H13 N O2 S2'
_chemical_formula_sum            'C9 H13 N O2 S2'
_chemical_formula_weight         231.32
_chemical_name_systematic
;
4-Methyl-3-[(tetrahydro-2H-pyran-2-yl) oxy] thiazole-2(3H)-thione
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             '19-Jun-19 T06:24:30-00:00'
_audit_creation_method           'XD routine XDCIF'
_cell_angle_alpha                90
_cell_angle_beta                 91.7870(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.81060(10)
_cell_length_b                   10.53450(10)
_cell_length_c                   10.43120(10)
_cell_measurement_reflns_used    529944
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      46.07
_cell_measurement_theta_min      2.17
_cell_volume                     1077.538(18)
_computing_molecular_graphics    'Volkov et al, (2006)'
_computing_publication_material  'Volkov et al, (2006)'
_computing_structure_refinement  'Volkov et al, (2006)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      ' 24880 frames, detector distance = 60 mm'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_type           'Ag K\a'
_diffrn_radiation_wavelength     0.56083
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_number            440543
_diffrn_reflns_theta_full        19.664
_diffrn_reflns_theta_max         45.44
_diffrn_reflns_theta_min         2.17
_diffrn_source                   Ag-Ims
_exptl_absorpt_coefficient_mu    0.244
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.505
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.155
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.028
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.865
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         12400
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.041
_refine_ls_R_factor_gt           0.014
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;    calc w2 = q/[s^2^(Fo^2^) + (0.00 P)^2^ + 0.00 P + 0.00 + 0.00 sin(th)]
     where P = (0.3333 Fo^2^ + 0.6667 Fc^2^)
           q = 1.0
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.017
_reflns_limit_h_max              24
_reflns_limit_h_min              -22
_reflns_limit_k_max              26
_reflns_limit_k_min              -26
_reflns_limit_l_max              26
_reflns_limit_l_min              -24
_reflns_number_gt                11715
_reflns_number_total             18518
_reflns_threshold_expression     I>3u(I)
_cod_data_source_file            px5018sup1.cif
_cod_data_source_block           I
_cod_database_code               2108611