15N NMR and crystal structure studies of 5-(2-pyridylmethylene)pseudothiohydantoin;† dipolar dephasing experiments for establishing the preferred tautomer in the solid and solution states
Chowdhry, Mubarik M.; Mingos, D. Michael P.; White, Andrew J. P.; Williams, David J.; Journal of the Chemical Society, Perkin Transactions 2  (2000) 2265–; doi:10.1039/b004368k

data_7213391
_publ_section_title
;
 15N NMR and crystal structure studies of
 5-(2-pyridylmethylene)pseudothiohydantoin;&#x2020; dipolar dephasing
 experiments for establishing the preferred tautomer in the solid and
 solution states
;
_journal_issue                   11
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              2265
_journal_paper_doi               10.1039/b004368k
_journal_year                    2000
_chemical_formula_sum            'C9 H7 N3 O S'
_chemical_formula_weight         205.24
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                71.480(15)
_cell_angle_beta                 79.503(15)
_cell_angle_gamma                73.308(15)
_cell_formula_units_Z            2
_cell_length_a                   6.6773(14)
_cell_length_b                   8.191(2)
_cell_length_c                   9.319(2)
_cell_measurement_temperature    298(2)
_cell_volume                     460.60(19)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1493
_diffrn_reflns_theta_max         62.92
_diffrn_reflns_theta_min         5.03
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.869
_exptl_absorpt_correction_T_max  0.7909
_exptl_absorpt_correction_T_min  0.6464
_exptl_absorpt_correction_type   'Face-indexed numerical'
_exptl_crystal_colour            Yellow/red
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       Dichroic
_exptl_crystal_F_000             212
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.178
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.0102(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.039
_refine_ls_goodness_of_fit_obs   1.038
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1487
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.128
_refine_ls_restrained_S_obs      1.037
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_obs          0.0350
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+0.1672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1056
_refine_ls_wR_factor_obs         0.0942
_reflns_number_observed          1406
_reflns_number_total             1493
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b004368ksup1.cif
_cod_data_source_block           MM9550
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+0.1672P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+0.1672P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        460.6(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7213391