Crystal structure and Hirshfeld surface analysis of dimethyl 4′-bromo-3-oxo-5-(thiophen-2-yl)-3,4,5,6-tetrahydro-[1,1′-biphenyl]-2,4-dicarboxylate
Naghiyev, Farid N.; Khrustalev, Victor N.; Akkurt, Mehmet; Asadov, Khammed A.; Bhattarai, Ajaya; Khalilov, Ali N.; Mamedov, İbrahim G.; Acta Crystallographica Section E Crystallographic Communications 80 (2024) –; doi:10.1107/S2056989024002858

data_2023078
_publ_section_title
;
 Crystal structure and Hirshfeld surface analysis of dimethyl
 4&#x2032;-bromo-3-oxo-5-(thiophen-2-yl)-3,4,5,6-tetrahydro-[1,1&#x2032;-biphenyl]-2,4-dicarboxylate
;
_journal_coeditor_code           NX2007
_journal_issue                   5
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989024002858
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          'C20 H17 Br O5 S'
_chemical_formula_moiety         'C20 H17 Br O5 S'
_chemical_formula_sum            'C20 H17 Br O5 S'
_chemical_formula_weight         449.30
_chemical_name_systematic
;Dimethyl
4'-bromo-3-oxo-5-(thiophen-2-yl)-3,4,5,6-tetrahydro-[1,1'-biphenyl]-2,4-dicarboxylate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 105.135(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4670(2)
_cell_length_b                   8.4852(2)
_cell_length_c                   20.4823(4)
_cell_measurement_reflns_used    16653
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.9180
_cell_measurement_theta_min      2.4180
_cell_volume                     1923.80(7)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)
;
_computing_data_reduction
;
CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
PLATON (Spek, 2020)
;
_computing_structure_refinement
;
<i>SHELXL2019/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            36460
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.499
_diffrn_reflns_theta_min         2.377
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.274
_exptl_absorpt_correction_T_max  0.749
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2022)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.172
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.127
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.973
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         6958
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+1.2510P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0863
_reflns_number_gt                5872
_reflns_number_total             6958
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nx2007.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2023078
_shelx_estimated_absorpt_t_min   0.696
_shelx_estimated_absorpt_t_max   0.761
_shelx_hkl_checksum              85880
_shelx_res_checksum              87846