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_2009253
_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_iupac          '[Sn4 (C4 H9)8 (C8 H5 O3)4(O)2]'
_chemical_formula_sum            'C64 H92 O14 Sn4'
_chemical_formula_weight         1560.14
_chemical_melting_point          404.0(10)
_chemical_name_systematic
;bis[(\m~3~-oxo)-\m~2~-(2-formylbenzoato-O,O')-(2-formylbenzoato-O)-bis(dibutyl-
tin(IV)]
;
_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_type_scat_source           IntTabIV
_cell_angle_alpha                83.7710(10)
_cell_angle_beta                 82.6720(10)
_cell_angle_gamma                62.8750(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1605(6)
_cell_length_b                   12.4140(6)
_cell_length_c                   25.0610(10)
_cell_measurement_reflns_used    8121
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.7
_cell_measurement_theta_min      1.6
_cell_volume                     3334.2(3)
_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  0.049
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            19727
_diffrn_reflns_reduction_process 19727
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.541
_exptl_absorpt_correction_T_max  0.775
_exptl_absorpt_correction_T_min  0.611
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'XPREP (Siemens, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.40(10)
_refine_diff_density_min         -1.30(10)
_refine_ls_extinction_coef       14E1(2)
_refine_ls_extinction_method
;
B-C type 1
Lorentzian isotropic (Becker & Coppens,1974)
;
_refine_ls_goodness_of_fit_ref   1.243
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     740
_refine_ls_number_reflns         10872
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.037
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_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                10872
_reflns_number_total             11985
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            fg1568.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '403-405' was changed to '404.0(10)'
- the average value was taken and precision was
estimated.

'_atom_site_thermal_displace_type' tag value 'Uij' was
replaced with 'Uani' value 82 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 '403-405' was changed to '404.0(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        3334.1(2)
_cod_database_code               2009253