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_7246101
_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_melting_point          398
_chemical_name_common            MBFP
_chemical_name_systematic        2,5-bis(3-bromophenyl)furan
_chemical_properties_physical    'Metastable polymorph'
_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             2021-10-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6403)
;
_audit_update_record
;
2022-05-11 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                   6.3129(3)
_cell_length_b                   30.1720(12)
_cell_length_c                   7.2937(4)
_cell_measurement_reflns_used    10338
_cell_measurement_temperature    295
_cell_measurement_theta_max      26.5640
_cell_measurement_theta_min      2.6770
_cell_volume                     1389.25(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 0.977
_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   17.50    --   13.31  57.00  60.00  110
  2  \w    -23.00  97.00   1.00   17.50    --   13.31  77.00-180.00  120
  3  \w    -18.00  93.00   1.00   17.50    --   13.31  37.00 -30.00  111
  4  \w    -57.00  31.00   1.00   17.50    --  -14.40  94.00  37.00   88
  5  \w    -47.00  64.00   1.00   17.50    --  -14.40  57.00 -60.00  111
  6  \w    -50.00  70.00   1.00   17.50    --  -14.40  77.00-180.00  120
  7  \w    -76.00   1.00   1.00   17.50    --  -14.40 128.00-131.49   77
  8  \w    -79.00 105.00   1.00   17.50    --   13.31   0.00-180.00  184
  9  \w    -25.00  57.00   1.00   17.50    --   13.31 -99.00 150.00   82
 10  \w    -78.00 -32.00   1.00   17.50    --   13.31 178.00-120.00   46
 11  \w    -74.00   3.00   1.00   17.50    --  -14.40 125.00 -54.17   77
 12  \w    -55.00  37.00   1.00   17.50    --  -14.40  90.00-138.77   92
 13  \w    -57.00  31.00   1.00   17.50    --  -14.40  94.00 107.66   88
 14  \w    -79.00 105.00   1.00   17.50    --   13.31   0.00-120.00  184
 15  \w    -79.00 -27.00   1.00   17.50    --   13.31   0.00 -90.00   52
 16  \w    -79.00 105.00   1.00   17.50    --   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      0.0104527000
_diffrn_orient_matrix_UB_12      0.0208175000
_diffrn_orient_matrix_UB_13      0.0442704000
_diffrn_orient_matrix_UB_21      -0.0732327000
_diffrn_orient_matrix_UB_22      -0.0068456000
_diffrn_orient_matrix_UB_23      0.0680907000
_diffrn_orient_matrix_UB_31      0.0845641000
_diffrn_orient_matrix_UB_32      -0.0085046000
_diffrn_orient_matrix_UB_33      0.0535052000
_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  0.0844
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            55420
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.471
_diffrn_reflns_theta_min         2.700
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.823
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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    1.808
_exptl_crystal_description       plate
_exptl_crystal_F_000             736
_exptl_crystal_recrystallization_method 'Crystallization from acetonitrille'
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.640
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         1925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0578
_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^)+(0.0420P)^2^+3.2277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1354
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1262
_reflns_number_total             1925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01681h2.cif
_cod_data_source_block           metafuranacn
_cod_depositor_comments
'Adding full bibliography for 7246100--7246102.cif.'
_cod_database_code               7246101
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O Br'
_shelx_estimated_absorpt_t_max   0.622
_shelx_estimated_absorpt_t_min   0.250
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C4(H4), C6(H6), C2(H2), C5(H5)
;
_shelx_res_checksum              75429
_olex2_date_sample_data_collection 2021-09-28
_olex2_exptl_crystal_mounting_method 'Mounted on polish nail'
_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 2.245
_oxdiff_exptl_absorpt_empirical_full_min 0.755