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_7251328
_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 F5 I, C4 H5'
_chemical_formula_sum            'C10 H5 F5 I'
_chemical_formula_weight         347.04
_chemical_name_systematic        Iodofluorobenzene:p-xylene
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-08-28 deposited with the CCDC.	2025-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                74.629(2)
_cell_angle_beta                 89.584(2)
_cell_angle_gamma                89.675(2)
_cell_formula_units_Z            2
_cell_length_a                   6.0419(2)
_cell_length_b                   8.9855(2)
_cell_length_c                   9.9890(3)
_cell_measurement_reflns_used    7680
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.1010
_cell_measurement_theta_min      3.5450
_cell_volume                     522.88(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.60a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.60a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.60a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120
_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 0.801
_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     44.00  77.00   0.50    0.60    --    3.31-161.00 -24.00   66
  2  \w     10.00  51.00   0.50    0.60    --    3.31-118.00 165.29   82
  3  \w    -12.00  67.00   0.50    0.60    --    3.31  77.00-180.00  158
  4  \w     24.00  51.00   0.50    0.60    --    3.31-117.00 132.08   54
  5  \w     21.00  46.00   0.50    0.60    --    3.31-109.00-140.79   50
  6  \w     13.00  39.00   0.50    0.60    --    3.31 -99.00  90.00   52
  7  \w    -13.00  41.00   0.50    0.60    --    3.31-102.00 -96.95  108
  8  \w     29.00  54.00   0.50    0.60    --    3.31-123.00  40.87   50
  9  \w    -67.00  15.00   0.50    0.60    --    3.31 -57.00-150.00  164
 10  \w    -70.00  36.00   0.50    0.60    --    3.31 -19.00   0.00  212
 11  \w    -39.00  43.00   0.50    0.60    --   -3.63  19.00   0.00  164
 12  \w    -59.00  29.00   0.50    0.60    --   -3.63 -19.00-150.00  176
;
_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      0.0241124000
_diffrn_orient_matrix_UB_12      -0.0137901000
_diffrn_orient_matrix_UB_13      0.0716489000
_diffrn_orient_matrix_UB_21      0.0539317000
_diffrn_orient_matrix_UB_22      0.0724250000
_diffrn_orient_matrix_UB_23      -0.0135098000
_diffrn_orient_matrix_UB_31      -0.1014538000
_diffrn_orient_matrix_UB_32      0.0355908000
_diffrn_orient_matrix_UB_33      0.0103564000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.801
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12848
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.801
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.133
_diffrn_reflns_theta_min         3.372
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.100
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.181
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.60a (Rigaku Oxford Diffraction, 2022)
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    2.204
_exptl_crystal_description       block
_exptl_crystal_F_000             326
_exptl_crystal_preparation       'Grown in situ from melt'
_exptl_crystal_recrystallization_method 'Grown in situ from melt'
_exptl_crystal_size_max          0.922
_exptl_crystal_size_mid          0.372
_exptl_crystal_size_min          0.357
_refine_diff_density_max         0.640
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2691
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0268
_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^)+(0.0227P)^2^+0.0474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0578
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2448
_reflns_number_total             2691
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00989h2.cif
_cod_data_source_block           exp_78
_cod_database_code               7251328
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C8 H10 (C6 F5 I)2'
_chemical_oxdiff_usercomment     '0.3mm capillary'
_shelx_estimated_absorpt_t_max   0.404
_shelx_estimated_absorpt_t_min   0.162
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_shelx_res_checksum              35875
_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 1.958
_oxdiff_exptl_absorpt_empirical_full_min 0.707