Bending the bonds: unveiling halogen interactions in the elastic polymorph of 2,5-bis(3-bromophenyl)furan
Dyk, Konrad; Kinzhybalo, Vasyl; Horak, Yuriy; Butenko, Serhii; Siczek, Miłosz; Kamiński, Daniel M.; Journal of Applied Crystallography 57 (2024) –; doi:10.1107/S1600576723010609

data_2300728
_publ_section_title
;
 Bending the bonds: unveiling halogen interactions in the elastic
 polymorph of 2,5-bis(3-bromophenyl)furan
;
_journal_issue                   1
_journal_name_full               'Journal of Applied Crystallography'
_journal_paper_doi               10.1107/S1600576723010609
_journal_volume                  57
_journal_year                    2024
_chemical_formula_moiety         'C16 H10 Br2 O'
_chemical_formula_sum            'C16 H10 Br2 O'
_chemical_formula_weight         378.06
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-21
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.217(3)
_cell_length_b                   30.110(8)
_cell_length_c                   7.180(3)
_cell_measurement_reflns_used    20762
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      29.1570
_cell_measurement_theta_min      2.8930
_cell_volume                     1344.1(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -19.00  91.00   1.00   13.50    --   13.31  57.00   0.00  110
  2  \w    -23.00  97.00   1.00   13.50    --   13.31  77.00 120.00  120
  3  \w    -18.00  93.00   1.00   13.50    --   13.31  37.00 -90.00  111
  4  \w    -78.00 -32.00   1.00   13.50    --   13.31 178.00 120.00   46
  5  \w    -65.00  46.00   1.00   13.50    --   13.31 -57.00-150.00  111
  6  \w    -97.00 -19.00   1.00   13.50    --  -14.40 160.00  37.75   78
  7  \w    -77.00  -1.00   1.00   13.50    --  -14.40 130.00-130.21   76
  8  \w     35.00 106.00   1.00   13.50    --   13.31 178.00-150.00   71
  9  \w    -25.00  57.00   1.00   13.50    --   13.31 -99.00  60.00   82
 10  \w    -18.00  93.00   1.00   13.50    --   13.31  37.00-180.00  111
 11  \w     35.00 106.00   1.00   13.50    --   13.31 178.00-120.00   71
 12  \w    -79.00 105.00   1.00   13.50    --   13.31   0.00-180.00  184
 13  \w     35.00 106.00   1.00   13.50    --   13.31 178.00  90.00   71
 14  \w    -79.00 105.00   1.00   13.50    --   13.31   0.00-120.00  184
 15  \w    -79.00  23.00   1.00   13.50    --   13.31   0.00 -90.00  102
 16  \w    -79.00 105.00   1.00   13.50    --   13.31   0.00-150.00  184
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0141276000
_diffrn_orient_matrix_UB_12      0.0013198000
_diffrn_orient_matrix_UB_13      -0.0978864000
_diffrn_orient_matrix_UB_21      0.0782695000
_diffrn_orient_matrix_UB_22      0.0171105000
_diffrn_orient_matrix_UB_23      -0.0044724000
_diffrn_orient_matrix_UB_31      0.0817714000
_diffrn_orient_matrix_UB_32      -0.0161360000
_diffrn_orient_matrix_UB_33      -0.0126845000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            53049
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.513
_diffrn_reflns_theta_min         2.706
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.018
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.868
_exptl_crystal_description       plate
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         1831
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+3.5330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0941
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1505
_reflns_number_total             1831
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ei5098sup1.cif
_cod_data_source_block           beta
_cod_database_code               2300728
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C16H10Br2O
_shelx_estimated_absorpt_t_max   0.714
_shelx_estimated_absorpt_t_min   0.187
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C4(H4), C5(H5), C2(H2)
;
_shelx_res_checksum              79004
_shelx_hkl_checksum              88851
_olex2_date_sample_data_collection 2021-12-15
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.027
_oxdiff_exptl_absorpt_empirical_full_min 0.775
_cod_database_fobs_code 2300728