Elucidating mechanochemical reactivity of a ternary halogen-bonded cocrystal system by computational and calorimetric studies.
Kumar, Lavanya; Dash, Sibananda G.; Leko, Katarina; Trzybiński, Damian; Bregović, Nikola; Cinčić, Dominik; Arhangelskis, Mihails; Physical chemistry chemical physics : PCCP 25 (2023) 28576–28580; doi:10.1039/d3cp04358d

data_7247572
_publ_section_title
;
 Elucidating mechanochemical reactivity of a ternary halogen-bonded
 cocrystal system by computational and calorimetric studies.
;
_journal_issue                   42
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              28576
_journal_page_last               28580
_journal_paper_doi               10.1039/d3cp04358d
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C18 H15 P S, 2(C6 F3 I3), C4 H4 N2'
_chemical_formula_sum            'C34 H19 F6 I6 N2 P S'
_chemical_formula_weight         1394.000
_chemical_name_systematic
'triphenylphospine sulfide pyrazine bis(1,3,5-trifluro-2,4,6-triiodobenzene)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_Int_Tables_number      11
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-08-16
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-18 deposited with the CCDC.	2023-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.873(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.2546(1)
_cell_length_b                   28.9120(4)
_cell_length_c                   9.1504(1)
_cell_measurement_reflns_used    13584
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      28.9320
_cell_measurement_theta_min      2.3250
_cell_volume                     1916.84(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.36a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.36a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.36a (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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0026
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.9992
_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    -90.00 -55.00   1.00    2.50    --  -18.75 147.00 160.78   35
  2  \w    -82.00   3.00   1.00    2.50    --  -18.75 -57.00-180.00   85
  3  \w    -42.00   7.00   1.00    2.50    --  -18.75 -77.00   0.00   49
  4  \w    -88.00  -2.00   1.00    2.50    --  -18.75 -57.00  90.00   86
  5  \w      4.00  50.00   1.00    2.50    --  -18.75  57.00-120.00   46
  6  \w    -37.00  49.00   1.00    2.50    --  -18.75  57.00  90.00   86
  7  \w    -86.00   7.00   1.00    2.50    --  -18.75 -37.00 -90.00   93
  8  \w    -39.00  43.00   1.00    2.50    --  -18.75  57.00-150.00   82
  9  \w    -93.00 -64.00   1.00    2.50    --  -18.75 151.00   9.92   29
 10  \w    -47.00  39.00   1.00    2.50    --   18.75 -57.00 -30.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0549309000
_diffrn_orient_matrix_UB_12      -0.0172467000
_diffrn_orient_matrix_UB_13      -0.0360929000
_diffrn_orient_matrix_UB_21      -0.0775707000
_diffrn_orient_matrix_UB_22      0.0149299000
_diffrn_orient_matrix_UB_23      -0.0000938000
_diffrn_orient_matrix_UB_31      0.0234038000
_diffrn_orient_matrix_UB_32      0.0090301000
_diffrn_orient_matrix_UB_33      -0.0687152000
_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  0.0364
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.9992
_diffrn_reflns_Laue_measured_fraction_max 0.9992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            25064
_diffrn_reflns_point_group_measured_fraction_full 0.9992
_diffrn_reflns_point_group_measured_fraction_max 0.9992
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.23
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.016
_exptl_absorpt_correction_T_max  0.613
_exptl_absorpt_correction_T_min  0.424
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.36a (Rigaku Oxford Diffraction, 2021)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.415
_exptl_crystal_description       block
_exptl_crystal_F_000             1276.376
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.227
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.116
_refine_diff_density_max         0.7535
_refine_diff_density_min         -0.7457
_refine_diff_density_rms         0.1629
_refine_ls_d_res_high            0.8000
_refine_ls_d_res_low             9.1389
_refine_ls_goodness_of_fit_ref   1.1528
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    20
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3982
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.1528
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+0.5877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0486
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              36
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_gt                3634
_reflns_number_total             3982
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3cp04358d2.cif
_cod_data_source_block           3-comp
_cod_depositor_comments          'Adding full bibliography for 7247572.cif.'
_cod_database_code               7247572
_chemical_oxdiff_formula         'C34 H19 F6 I6 N2 P S'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17),
 C18(H18), C7(H7), C8(H8)
;
_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 1.175
_oxdiff_exptl_absorpt_empirical_full_min 0.853