Just at the limit: binding studies with neutral brominated terphenyl-derived halogen bond donors
Stoesser, Julian; Engelage, Elric; Belmonte, Debora; Huber, Stefan M.; CrystEngComm 25 (2023) 1501–1506; doi:10.1039/D2CE01629J

data_7246256
_publ_section_title
;
 Just at the limit: binding studies with neutral brominated
 terphenyl-derived halogen bond donors
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              1501
_journal_page_last               1506
_journal_paper_doi               10.1039/D2CE01629J
_journal_volume                  25
_journal_year                    2023
_chemical_formula_sum            'C18 Br2 F12'
_chemical_formula_weight         603.98
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_primary     'dual space'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-07-04 deposited with the CCDC.	2023-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.8665(2)
_cell_length_b                   20.2579(3)
_cell_length_c                   22.2780(4)
_cell_measurement_reflns_used    3127
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      66.5
_cell_measurement_theta_min      4.0
_cell_volume                     3550.19(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_molecular_graphics
;
 Diamond 4 - Crystal and Molecular Structure Visualization
  Crystal Impact - Dr. H. Putz & Dr. K. Brandenburg GbR, 
  Kreuzherrenstr. 102, 53227 Bonn, Germany
  http://www.crystalimpact.com/diamond
 Mercury CSD 2.0 - New Features for the Visualization 
 and Investigation of Crystal Structures
  C. F. Macrae, I. J. Bruno, J. A. Chisholm, P. R. Edgington, P. McCabe,
  E. Pidcock, 
  L. Rodriguez-Monge, R. Taylor, J. van de Streek and P. A. Wood, 
  J. Appl. Cryst., 41, 466-470, 2008
;
_computing_publication_material
'WinGX L. J. Farrugia, J. Appl. Crystallogr., 1999, 32, 837-838.'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution
;
 shelXT  G. M. Sheldrick, Acta Crystallogr., Sect. A: Found. Crystallogr.,
 2008, 64, 112-122.
 shelXle C. B. Huebschle, G. M. Sheldrick and B. Dittrich J. Appl. Cryst.
  (2011). 44, 1281-1284
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -69.00  19.00   0.50    0.83    --  -47.45  75.00 -66.00  176
  2  \w   -134.00 -96.00   0.50    3.34    --  -86.25 -95.00  70.00   76
  3  \w    -48.00 -23.00   0.50    3.34    --  -86.25  55.00  81.00   50
  4  \w     41.00  66.00   0.50    3.34    --  106.49 -55.00 -61.00   50
  5  \w     89.00 178.00   0.50    3.34    --  106.49  75.00 -66.00  178
  6  \w   -118.00 -87.00   0.50    0.83    --  -47.45-125.00-120.00   62
  7  \w    -23.00   6.00   0.50    0.83    --  -47.45  19.00 150.00   58
  8  \w    -11.00  27.00   0.50    0.83    --   47.45 -19.00 150.00   76
  9  \w     35.00  65.00   0.50    3.34    --  106.49 -61.00  90.00   60
 10  \w    114.00 140.00   0.50    3.34    --  106.49  30.00  60.00   52
 11  \w    146.00 178.00   0.50    3.34    --  106.49  30.00  60.00   64
 12  \w     47.00  73.00   0.50    3.34    --  106.49 -61.00 150.00   52
 13  \w     37.00  74.00   0.50    3.34    --  106.49 -61.00   0.00   74
 14  \w     45.00  70.00   0.50    3.34    --  106.49 -61.00  60.00   50
 15  \w     36.00  71.00   0.50    3.34    --  106.49 -61.00-180.00   70
 16  \w     34.00  59.00   0.50    3.34    --  106.49 -61.00-150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1046029000
_diffrn_orient_matrix_UB_12      -0.0405879000
_diffrn_orient_matrix_UB_13      0.0453433000
_diffrn_orient_matrix_UB_21      -0.1500039000
_diffrn_orient_matrix_UB_22      -0.0480685000
_diffrn_orient_matrix_UB_23      0.0076324000
_diffrn_orient_matrix_UB_31      0.0699129000
_diffrn_orient_matrix_UB_32      -0.0426534000
_diffrn_orient_matrix_UB_33      -0.0517114000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            12960
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.494
_diffrn_reflns_theta_max         66.494
_diffrn_reflns_theta_min         3.969
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.029
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.709
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.20a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent colourless'
_exptl_crystal_density_diffrn    2.260
_exptl_crystal_description       'cut plate'
_exptl_crystal_F_000             2288
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Slow evaporation of pentane'
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         3127
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+10.9787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1074
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2844
_reflns_number_total             3127
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01629j3.cif
_cod_data_source_block           JS-1-4-2Br4-Br
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7246252--7246257.cif.
;
_cod_database_code               7246256
_shelx_shelxl_version_number     2018/3
_oxdiff_exptl_absorpt_empirical_full_min 0.703
_oxdiff_exptl_absorpt_empirical_full_max 1.384
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_shelx_res_checksum              2114