Ethyl (2<i>S</i>,4<i>R</i>)-4-(4-bromophenyl)-2-hydroxy-5,10-dioxo-3,4,5,10-tetrahydro-2<i>H</i>-benzo[<i>g</i>]chromene-2-carboxylate
Zhang, Wei; Wang, Yifeng; Zhang, Guangcun; Xu, Xiangsheng; Acta Crystallographica Section E 66 (2010) o388–; doi:10.1107/S1600536810001315

data_2225153
_publ_section_title
;Ethyl
 (2<i>S</i>,4<i>R</i>)-4-(4-bromophenyl)-2-hydroxy-5,10-dioxo-3,4,5,10-tetrahydro-2<i>H</i>-benzo[<i>g</i>]chromene-2-carboxylate
;
_journal_coeditor_code           ZQ2026
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o388
_journal_paper_doi               10.1107/S1600536810001315
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C22 H17 Br O6'
_chemical_formula_moiety         'C22 H17 Br O6'
_chemical_formula_sum            'C22 H17 Br O6'
_chemical_formula_weight         457.27
_chemical_name_systematic
;
Ethyl (2<i>S</i>,4<i>R</i>)-4-(4-bromophenyl)-2-hydroxy-5,10-dioxo-3,4,5,10-
tetrahydro-2<i>H</i>-benzo[<i>g</i>]chromene-2-carboxylate
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 96.323(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.2993(6)
_cell_length_b                   9.9445(7)
_cell_length_c                   12.4884(10)
_cell_measurement_reflns_used    6026
_cell_measurement_temperature    296.0(10)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.1
_cell_volume                     1024.43(13)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 2006)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 2006)'
_computing_data_reduction        'CrystalStructure (Rigaku, 2007)'
_computing_molecular_graphics    'ORTEP-3 for windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.0(10)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rolling anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0672
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9887
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    2.042
_exptl_absorpt_correction_T_max  0.5645
_exptl_absorpt_correction_T_min  0.5201
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.372
_refine_ls_abs_structure_details 'Flack (1983), 2082 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.008(11)
_refine_ls_extinction_coef       0.032(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4549
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1084
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0455P)^2^+0.1250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.1220
_reflns_number_gt                2257
_reflns_number_total             4549
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zq2026.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2225153
_cod_database_fobs_code          2225153