Tautomerism in Schiff bases derived from 3-hydroxysalicylaldehyde. Combined X-ray diffraction, solution and solid state NMR study
Pizzala, Helene; Carles, Micheline; Stone, William E. E.; Thevand, Andre; Journal of the Chemical Society, Perkin Transactions 2  (2000) 935–; doi:10.1039/b000756k

data_7213267
_publ_section_title
;
 Tautomerism in Schiff bases derived from 3-hydroxysalicylaldehyde.
 Combined X-ray diffraction, solution and solid state NMR study
;
_journal_issue                   5
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              935
_journal_paper_doi               10.1039/b000756k
_journal_year                    2000
_chemical_compound_source        'Local laboratory'
_chemical_formula_sum            'C13 H10 N2 O4'
_chemical_formula_weight         258.233
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                83.21(1)
_cell_angle_beta                 79.16(1)
_cell_angle_gamma                72.66(1)
_cell_formula_units_Z            2
_cell_length_a                   7.005(1)
_cell_length_b                   7.180(1)
_cell_length_c                   12.018(1)
_cell_measurement_reflns_used    3628
_cell_measurement_temperature    298
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1
_cell_volume                     565.44(13)
_computing_data_collection       KappaCCD
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Ortep (Johnson, 1976)'
_computing_publication_material  'maxus(Mackay et al., 1999)'
_computing_structure_refinement  'maxus(Mackay et al., 1999)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       phi-scan
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            1968
_diffrn_reflns_theta_max         26.36
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Cube
_exptl_crystal_F_000             268
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.18
_refine_diff_density_min         -0.18
_refine_diff_density_rms         0.04
_refine_ls_extinction_coef       39620(688)
_refine_ls_extinction_expression
'equ(22) p292 Crystallographic Computing (1970) '
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_all   1.266
_refine_ls_goodness_of_fit_gt    1.445
_refine_ls_goodness_of_fit_ref   1.445
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         1039
_refine_ls_R_factor_all          0.136
_refine_ls_R_factor_gt           0.074
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef F^2^
_refine_ls_weighting_details
;
w = 1 / ( s^2^(Fo^2^) + 0.03000 * Fo^2^)
;
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.150
_refine_ls_wR_factor_gt          0.150
_refine_ls_wR_factor_ref         0.150
_reflns_d_resolution_high        0.63
_reflns_d_resolution_low         1.76
_reflns_limit_h_max              8
_reflns_limit_h_min              0
_reflns_limit_k_max              8
_reflns_limit_k_min              -6
_reflns_limit_l_max              8
_reflns_limit_l_min              0
_reflns_number_gt                1039
_reflns_number_total             1968
_reflns_threshold_expression     'I> 3.00 sigma(I)'
_cod_data_source_file            b000756ksup1.cif
_cod_data_source_block           crystal_compound4
_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 
;
_cod_original_cell_volume        565.(2)
_cod_original_sg_symbol_H-M      'P -1           '
_cod_original_formula_sum        'C13 H10 N2 O4 '
_cod_database_code               7213267