Exploring non-covalent interactions in binary aromatic complexes
Bear, Joseph C.; Cockcroft, Jeremy Karl; Rosu-Finsen, Alexander; Williams, Jeffrey Huw; CrystEngComm  (2025) –; doi:10.1039/D5CE00989H

data_7251330
_publ_section_title
;
 Exploring non-covalent interactions in binary aromatic complexes
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D5CE00989H
_journal_year                    2025
_chemical_formula_moiety         'C6 F4 I2, C6 H6'
_chemical_formula_sum            'C12 H6 F4 I2'
_chemical_formula_weight         479.97
_chemical_name_systematic        p-Tetrafluorodiidobenzene
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-08-14
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-08-28 deposited with the CCDC.	2025-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.058(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.6866(2)
_cell_length_b                   7.1907(2)
_cell_length_c                   10.5364(3)
_cell_measurement_reflns_used    4321
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.0490
_cell_measurement_theta_min      3.6680
_cell_volume                     658.13(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.130a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 44.114a 64-bit (release 13-06-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.43.130a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.826
_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    -22.00  20.00   0.50    2.50    --   -2.48  77.00  90.00   84
  2  \w    -56.00  14.00   0.50    2.50    --    2.48 -28.00 -76.80  140
  3  \w    -48.00  16.00   0.50    2.50    --    2.48 -26.00  43.89  128
  4  \w    -53.00  20.00   0.50    2.50    --    2.48 -23.00 -21.23  146
  5  \w      9.00  35.00   0.50    2.50    --    2.48 -99.00 -90.00   52
  6  \w    -16.00  36.00   0.50    2.50    --    2.48 -16.00 129.02  104
  7  \w      6.00  35.00   0.50    2.50    --    2.48 -99.00  90.00   58
  8  \w    -43.00  25.00   0.50    2.50    --    2.48 -19.00-150.00  136
  9  \w      9.00  34.00   0.50    2.50    --    2.48 -99.00  30.00   50
 10  \w    -24.00  42.00   0.50    2.50    --    2.48 -14.00  74.30  132
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0124382072
_diffrn_orient_matrix_UB_12      0.0354734910
_diffrn_orient_matrix_UB_13      0.0619657024
_diffrn_orient_matrix_UB_21      0.0162720960
_diffrn_orient_matrix_UB_22      0.0911362681
_diffrn_orient_matrix_UB_23      -0.0220036621
_diffrn_orient_matrix_UB_31      -0.0790244242
_diffrn_orient_matrix_UB_32      0.0131388547
_diffrn_orient_matrix_UB_33      -0.0143846379
_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  0.0524
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.826
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6531
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.826
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.454
_diffrn_reflns_theta_min         3.678
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.804
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.428
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.130a (Rigaku Oxford Diffraction, 2024)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.422
_exptl_crystal_description       plate
_exptl_crystal_F_000             440
_exptl_crystal_preparation
'0.5g of C6F4I2 dissolved in 0.75g of hot benzene a'
_exptl_crystal_recrystallization_method
'Bottle stood in hot water and allowed to cool at room temperature'
_exptl_crystal_size_max          0.308
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.058
_refine_diff_density_max         2.458
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     51
_refine_ls_number_reflns         969
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0490P)^2^+0.2854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0742
_reflns_Friedel_coverage         0.000
_reflns_number_gt                901
_reflns_number_total             969
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00989h2.cif
_cod_data_source_block           exp_1138
_cod_database_code               7251330
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C6H6C6F4I2
_shelx_estimated_absorpt_t_max   0.768
_shelx_estimated_absorpt_t_min   0.319
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5)
;
_shelx_res_checksum              34281
_olex2_exptl_crystal_mounting_method '0.3mm loop from Hampton Research'
_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 1.914
_oxdiff_exptl_absorpt_empirical_full_min 0.637