Crystal structure of 4-bromo-5,7-dimethoxy-2,3-dihydro-1H-inden-1-one
Galla, Sri Hari; Sridhar, Jayalakshmi; Mague, Joel T.; Zhang, Xiaodong; White, Kira D.; Zhang, Qiang; Donahue, James P.; Acta Crystallographica Section E Crystallographic Communications 80 (2024) –; doi:10.1107/S2056989024006522

data_2023206
_publ_section_title
;
 Crystal structure of 4-bromo-5,7-dimethoxy-2,3-dihydro-1H-inden-1-one
;
_journal_coeditor_code           JY2050
_journal_issue                   8
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989024006522
_journal_volume                  80
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_iupac          'C11 H11 Br O3'
_chemical_formula_moiety         'C11 H11 Br O3'
_chemical_formula_sum            'C11 H11 Br O3'
_chemical_formula_weight         271.11
_chemical_name_systematic
;
4-Bromo-5,7-dimethoxy-2,3-dihydro-1<i>H</i>-inden-1-one
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.0928(5)
_cell_length_b                   14.3933(10)
_cell_length_c                   10.0419(7)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.2367
_cell_measurement_theta_min      2.8305
_cell_volume                     1025.17(12)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2021)
;
_computing_data_collection
;
<i>APEX4</i> (Bruker, 2021)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2021)
;
_computing_molecular_graphics
;
<i>DIAMOND</i> (Brandenburg & Putz, 2012)
;
_computing_publication_material
;
<i>SHELXTL</i> (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2019/1</i> (L\"ubben <i>et al.</i>, 2019; Sheldrick,
2015b)
;
_computing_structure_solution
;
<i>SHELXT/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker D8 QUEST PHOTON 3 diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON 3 diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13923
_diffrn_reflns_theta_full        28.279
_diffrn_reflns_theta_max         28.279
_diffrn_reflns_theta_min         2.830
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.50
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.992
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.031
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.386
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1025 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013). Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.039(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2534
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+0.0970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0562
_reflns_number_gt                2366
_reflns_number_total             2534
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jy2050.cif
_cod_data_source_block           I
_cod_database_code               2023206
_shelx_estimated_absorpt_t_min   0.479
_shelx_estimated_absorpt_t_max   0.886
_shelx_hkl_checksum              5716
_shelx_res_checksum              36268