5-Chloro-6-hydroxy-7,8-dimethylchroman-2-one
Cameron, Scott A.; Goswami, Shailesh K.; Hanton, Lyall R.; McAdam, C. John; Moratti, Stephen C.; Simpson, Jim; Acta Crystallographica Section E 67 (2011) o2141–o2142; doi:10.1107/S1600536811029345

data_2231217
_publ_section_title
;
 5-Chloro-6-hydroxy-7,8-dimethylchroman-2-one
;
_journal_coeditor_code           LH5289
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2141
_journal_page_last               o2142
_journal_paper_doi               10.1107/S1600536811029345
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C11 H11 Cl O3'
_chemical_formula_moiety         'C11 H11 Cl O3'
_chemical_formula_sum            'C11 H11 Cl O3'
_chemical_formula_weight         226.65
_chemical_name_systematic
;
5-Chloro-6-hydroxy-7,8-dimethylchroman-2-one
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.1375(6)
_cell_length_b                   16.1375(6)
_cell_length_c                   7.5887(6)
_cell_measurement_reflns_used    1966
_cell_measurement_temperature    89(2)
_cell_measurement_theta_max      20.57
_cell_measurement_theta_min      2.52
_cell_volume                     1976.24(19)
_computing_cell_refinement       'SAINT (Bruker 2009)'
_computing_data_collection       'APEX2 (Bruker 2009)'
_computing_data_reduction        'SAINT (Bruker 2009)'
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008), enCIFer (Allen <i>et al.</i>, 2004),
PLATON (Spek, 2009) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008) and TITAN2000 (Hunter & Simpson,
1999)
;
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      89(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       \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  0.0950
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            22360
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         3.90
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.368
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.7923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.392
_refine_ls_abs_structure_details
;
Flack (1983), 859 Friedel pairs
;
_refine_ls_abs_structure_Flack   -0.04(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2030
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0781P)^2^+0.6384P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1313
_refine_ls_wR_factor_ref         0.1425
_reflns_number_gt                1618
_reflns_number_total             2030
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5289.cif
_cod_data_source_block           I
_cod_database_code               2231217
_cod_database_fobs_code          2231217