3-Hydroxyphthalide and its adduct with dibutyltin oxide
Khoo, Lian Ee; Hazell, Alan; Acta Crystallographica Section C 55 (1999) 2070–2073; doi:10.1107/S0108270199009282

data_2009254
_publ_section_title
;
 3-Hydroxyphthalide and its adduct with dibutyltin oxide
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2070
_journal_page_last               2073
_journal_paper_doi               10.1107/S0108270199009282
_journal_volume                  55
_journal_year                    1999
_chemical_formula_sum            'C8 H6 O3'
_chemical_formula_weight         150.14
_chemical_melting_point          368.0(10)
_chemical_name_systematic
;
3-hydroxyphthalide
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90.0
_cell_angle_beta                 97.020(3)
_cell_angle_gamma                90.0
_cell_formula_units_Z            2
_cell_length_a                   3.9463(6)
_cell_length_b                   11.423(2)
_cell_length_c                   7.3270(11)
_cell_measurement_reflns_used    4235
_cell_measurement_temperature    120
_cell_measurement_theta_max      34.1
_cell_measurement_theta_min      2.8
_cell_volume                     327.81(9)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics
;
      ORTEPIII (Burnett & Johnson, 1996), KRYSTAL
;
_computing_publication_material  KRYSTAL
_computing_structure_refinement  'modified ORFLS (1962), KRYSTAL'
_computing_structure_solution
;
     SIR97 (Cascarano et al., 1996), KRYSTAL
;
_diffrn_ambient_temperature      120
_diffrn_measurement_device       'Siemens SMART CCD diffractometer'
_diffrn_measurement_method
;
\w rotation scans with narrow
frames
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'x-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6310
_diffrn_reflns_reduction_process 2204
_diffrn_reflns_theta_max         30.0
_diffrn_reflns_theta_min         2.8
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             156
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.27(4)
_refine_diff_density_min         -0.21(4)
_refine_ls_extinction_method
;
none
;
_refine_ls_goodness_of_fit_ref   1.700
_refine_ls_hydrogen_treatment    'see experimental'
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     103
_refine_ls_number_reflns         1004
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.028
_refine_ls_shift/su_max          0.00049
_refine_ls_shift/su_mean         0.00010
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.037
_reflns_number_gt                1004
_reflns_number_total             1006
_reflns_observed_criterion       I>0
_cod_data_source_file            fg1568.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '367-369' was changed to '368.0(10)'
- the average value was taken and precision was
estimated.

'_atom_site_thermal_displace_type' tag value 'Uij' was
replaced with 'Uani' value 11 times.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '367-369' was changed to '368.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '
1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^' was changed to 'calc'. New
tag '_refine_ls_weighting_details' was created. The value of the new
tag was set to 'w = 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        327.80(9)
_cod_original_sg_symbol_Hall     'P 2y1'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2009254
_cod_database_fobs_code          2009254