Solvent induced conformational polymorphism
Dyk, Konrad; Kinzhybalo, Vasyl; Czernel, Grzegorz; Grudziński, Wojciech; Horak, Yuriy; Butenko, Serhii; Kamiński, Daniel M.; CrystEngComm 25 (2023) 971–980; doi:10.1039/D2CE01681H

data_7246100
_publ_section_title
;
 Solvent induced conformational polymorphism
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              971
_journal_page_last               980
_journal_paper_doi               10.1039/D2CE01681H
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C16 H10 Br2 O'
_chemical_formula_sum            'C16 H10 Br2 O'
_chemical_formula_weight         378.06
_chemical_name_systematic        2,5-bis(3-bromophenyl)furan
_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
_audit_creation_date             2022-07-08
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-07-08 deposited with the CCDC.	2023-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.278(3)
_cell_length_b                   13.527(4)
_cell_length_c                   12.503(4)
_cell_measurement_reflns_used    11746
_cell_measurement_temperature    295
_cell_measurement_theta_max      25.1180
_cell_measurement_theta_min      2.9830
_cell_volume                     1400.0(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      295
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.963
_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   -107.00 -35.00   1.00   20.00    --  -14.40-178.00 -90.00   72
  2  \w    -98.00  22.00   1.00   20.00    --  -14.40 -77.00-180.00  120
  3  \w    -25.00  57.00   1.00   20.00    --   13.31 -99.00-120.00   82
  4  \w    -65.00  46.00   1.00   20.00    --   13.31 -57.00  90.00  111
  5  \w    -18.00  93.00   1.00   20.00    --   13.31  37.00 150.00  111
  6  \w    -19.00  91.00   1.00   20.00    --   13.31  57.00  30.00  110
  7  \w    -78.00 -32.00   1.00   20.00    --   13.31 178.00  90.00   46
  8  \w   -105.00 -32.00   1.00   20.00    --  -14.40 178.00-150.00   73
  9  \w    -25.00  57.00   1.00   20.00    --   13.31 -99.00  60.00   82
 10  \w    -62.00   0.00   1.00   20.00    --  -14.40 105.00 104.00   62
;
_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      -0.0414942000
_diffrn_orient_matrix_UB_12      0.0352254000
_diffrn_orient_matrix_UB_13      -0.0317928000
_diffrn_orient_matrix_UB_21      0.0049075000
_diffrn_orient_matrix_UB_22      -0.0322481000
_diffrn_orient_matrix_UB_23      -0.0445956000
_diffrn_orient_matrix_UB_31      -0.0748382000
_diffrn_orient_matrix_UB_32      -0.0216465000
_diffrn_orient_matrix_UB_33      0.0147223000
_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  0.0341
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29237
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.436
_diffrn_reflns_theta_min         2.885
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.778
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.794
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             736
_exptl_crystal_recrystallization_method 'Crystallization from ethanol'
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 1061 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3626
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0240P)^2^+0.4762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0605
_reflns_Friedel_coverage         0.858
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.900
_reflns_number_gt                2693
_reflns_number_total             3626
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01681h2.cif
_cod_data_source_block           metafuran
_cod_depositor_comments
'Adding full bibliography for 7246100--7246102.cif.'
_cod_database_code               7246100
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHOBr
_shelx_estimated_absorpt_t_max   0.624
_shelx_estimated_absorpt_t_min   0.185
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C14(H14), C2(H2), C9(H9), C8(H8), C6(H6), C3(H3), C10(H10),
 C13(H13), C12(H12)
;
_shelx_res_checksum              96394
_olex2_date_sample_data_collection 2021-07-27
_olex2_exptl_crystal_mounting_method 'Crystal mounted on nail polish'
_olex2_submission_original_sample_id 2,5-bis(3-bromophenyl)furan
_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 2.833
_oxdiff_exptl_absorpt_empirical_full_min 0.683