The conformational analysis of 2-hydroxyaryl Schiff thiosemicarbazones
Krasowska, M.; Kochel, A.; Filarowski, A.; CrystEngComm 12 (2010) 1955–; doi:10.1039/b921402j

data_7212180
_publ_section_title
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 The conformational analysis of 2-hydroxyaryl Schiff thiosemicarbazones
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_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              1955
_journal_paper_doi               10.1039/b921402j
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         'C9 H11 N3 O3 S, 2(C2 H8 N), O4 S'
_chemical_formula_sum            'C13 H27 N5 O7 S2'
_chemical_formula_weight         429.54
_chemical_name_common
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1-(4-hydroxy-6-methyl-2-oxo-2H-pyran-3-yl) ethan-1-one 
thiosemicarbazone di dimethylaminium cation sulfate
;
_chemical_name_systematic
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1-(4-hydroxy-6-methyl-2-oxo-2H-pyran-3-yl) ethan-1-one 
thiosemicarbazone di dimethylaminium cation sulfate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 118.65(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.863(2)
_cell_length_b                   7.992(3)
_cell_length_c                   22.218(3)
_cell_measurement_reflns_used    5200
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.87
_cell_measurement_theta_min      2.75
_cell_volume                     2004.4(9)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, date)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, date)'
_computing_data_reduction        'CrysAlis RED '
_computing_molecular_graphics    'SHELXTL (Bruker, 1999)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  Km4-CCD
_diffrn_measurement_method       /w
_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  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            37694
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         36.87
_diffrn_reflns_theta_min         2.75
_exptl_absorpt_coefficient_mu    0.310
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'CrysAlis RED, Oxford Diffraction'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         9450
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0531P)^2^+0.0097P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.1094
_reflns_number_gt                5976
_reflns_number_total             9450
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b921402j.txt
_cod_data_source_block           olek7dc
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
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_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7212180