3-[(<i>R</i>)-3,3-Dichloro-2-hydroxypropyl]-8-hydroxy-6-methoxy-1<i>H</i>-isochromen-1-one
Huang, Hua-Rong; Fang, Yan-Xiong; Du, Zhi-Yun; Zhang, Kun; Lin, Yong-Cheng; Acta Crystallographica Section E 64 (2008) o1801–; doi:10.1107/S1600536808026391

data_2219465
_publ_section_title
3-[(<i>R</i>)-3,3-Dichloro-2-hydroxypropyl]-8-hydroxy-6-methoxy-1<i>H</i>-isochromen-1-one
_journal_coeditor_code           WW2128
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1801
_journal_paper_doi               10.1107/S1600536808026391
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C13 H12 Cl2 O5'
_chemical_formula_moiety         'C13 H12 Cl2 O5'
_chemical_formula_sum            'C13 H12 Cl2 O5'
_chemical_formula_weight         319.13
_chemical_melting_point          420
_chemical_name_systematic
;
3-[(<i>R</i>)-3,3-Dichloro-2-hydroxypropyl]-8-hydroxy-6-methoxy-\
1<i>H</i>-isochromen-1-one
;
_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_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.217(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.483(3)
_cell_length_b                   6.757(2)
_cell_length_c                   10.548(3)
_cell_measurement_reflns_used    1002
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      2.68
_cell_volume                     667.2(3)
_computing_cell_refinement       'SMART (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART 1K area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4190
_diffrn_reflns_theta_full        27.06
_diffrn_reflns_theta_max         27.06
_diffrn_reflns_theta_min         1.96
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.502
_exptl_absorpt_correction_T_max  0.9019
_exptl_absorpt_correction_T_min  0.7873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.394
_refine_ls_abs_structure_details 'Flack (1983), 931 Friedel pairs'
_refine_ls_abs_structure_Flack   0.06(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2524
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+0.1606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0953
_reflns_number_gt                2320
_reflns_number_total             2524
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ww2128.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_cell_volume        667.1(4)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2219465
_cod_database_fobs_code          2219465