2<i>H</i>-1-Benzopyrans. III. 4-Hydroxy-3-methoxycarbonyl-2-dimethoxyphosphoryl-2<i>H</i>-1-benzopyran
Olszak, Tomasz A.; Grabowski, Mieczysław J.; Modranka, R.; Kostka, K.; Olszak, Agnieszka; Acta Crystallographica Section C 54 (1998) 1459–1461; doi:10.1107/S0108270198005241

data_2007740
_publ_section_title
;
 2<i>H</i>-1-Benzopyrans. III.
 4-Hydroxy-3-methoxycarbonyl-2-dimethoxyphosphoryl-2<i>H</i>-1-benzopyran
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1459
_journal_page_last               1461
_journal_paper_doi               10.1107/S0108270198005241
_journal_volume                  54
_journal_year                    1998
_chemical_formula_analytical     'C13 H15 O7 P1'
_chemical_formula_moiety         'C13 H15 O7 P1'
_chemical_formula_structural     'C13 H15 O7 P1'
_chemical_formula_sum            'C13 H15 O7 P'
_chemical_formula_weight         314.23
_chemical_melting_point          389.0(10)
_chemical_name_systematic
;
4-Hydroxy-3-Methoxycarbonyl-2-Dimethoxyphosphoryl-2H-1-Benzopyran
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                96.458(6)
_cell_angle_beta                 99.231(8)
_cell_angle_gamma                75.480(4)
_cell_formula_units_Z            2
_cell_length_a                   9.0038(6)
_cell_length_b                   12.4130(5)
_cell_length_c                   6.6728(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      41.46
_cell_measurement_theta_min      30.95
_cell_volume                     710.57(10)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1989a)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1989b)'
_computing_molecular_graphics    'ORTEX3.1a (McArdle, 1995)'
_computing_publication_material  'PARST (Nardelli, 1983a)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku AFC-5S'
_diffrn_measurement_method       \w
_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  0.015
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            3831
_diffrn_reflns_theta_max         60.06
_diffrn_reflns_theta_min         3.69
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.023
_exptl_absorpt_correction_T_max  0.817
_exptl_absorpt_correction_T_min  0.657
_exptl_absorpt_correction_type
'empirical \y-scan correction (North et al., 1968)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_meas      1.466
_exptl_crystal_density_method
' Measured in carbon tetrachloride (CCl~4~) and tetralin (C~10~H~12~)'
_exptl_crystal_description       prism
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.439
_refine_ls_extinction_coef       0.074(5)
_refine_ls_extinction_method     SHELXL93
_refine_ls_goodness_of_fit_all   1.142
_refine_ls_goodness_of_fit_obs   1.231
_refine_ls_hydrogen_treatment    'H atoms: see below'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         2112
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_restrained_S_obs      1.231
_refine_ls_R_factor_all          0.055
_refine_ls_R_factor_obs          0.047
_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^)+(0.0964P)^2^+0.0470P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.142
_refine_ls_wR_factor_obs         0.139
_reflns_number_observed          1778
_reflns_number_total             2114
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            na1323.cif
_cod_data_source_block           na1323
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

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 2.4.1 from 2010-06-29.

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

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0964P)^2^+0.0470P] 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^)+(0.0964P)^2^+0.0470P] 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        710.60(10)
_cod_original_formula_sum        'C13 H15 O7 P1 '
_cod_database_code               2007740