Locked guest PAHs by soft–cavity–type host assembled via halogen bond to form luminescent cocrystals
Wu, Wen Xin; Wang, Hui; Jin, Wei Jun; CrystEngComm  (2020) –; doi:10.1039/D0CE00965B

data_7240998
_publ_section_title
;
 Locked guest PAHs by soft--cavity--type host assembled via halogen bond
 to form luminescent cocrystals
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00965B
_journal_year                    2020
_chemical_formula_moiety         '2(C6 F4 I2), 2(C11 H9 N O), C16 H10'
_chemical_formula_sum            'C50 H28 F8 I4 N2 O2'
_chemical_formula_weight         1348.34
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-07-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-03 deposited with the CCDC.	2020-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                69.005(5)
_cell_angle_beta                 75.360(5)
_cell_angle_gamma                84.308(5)
_cell_formula_units_Z            2
_cell_length_a                   11.5999(7)
_cell_length_b                   12.8903(8)
_cell_length_c                   17.2206(10)
_cell_measurement_reflns_used    6219
_cell_measurement_temperature    271(2)
_cell_measurement_theta_max      25.8330
_cell_measurement_theta_min      3.4560
_cell_volume                     2325.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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      271(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -11.00  80.00   1.00    6.00    --   12.61  37.00 -60.00   91
  2  \w      7.00  64.00   1.00    6.00    --   12.61  57.00-150.00   57
  3  \w     -1.00  25.00   1.00    6.00    --   12.61  57.00-120.00   26
  4  \w    -19.00  89.00   1.00    6.00    --   12.61  77.00  30.00  108
  5  \w      9.00  34.00   1.00    6.00    --   12.61 -99.00 -30.00   25
  6  \w    -55.00  35.00   1.00    6.00    --   12.61 -57.00 120.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0099658000
_diffrn_orient_matrix_UB_12      -0.0536670000
_diffrn_orient_matrix_UB_13      0.0004988000
_diffrn_orient_matrix_UB_21      0.0476812000
_diffrn_orient_matrix_UB_22      0.0075951000
_diffrn_orient_matrix_UB_23      -0.0366032000
_diffrn_orient_matrix_UB_31      0.0402697000
_diffrn_orient_matrix_UB_32      -0.0231572000
_diffrn_orient_matrix_UB_33      0.0268125000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21180
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.350
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.179
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.754
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70330
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.925
_exptl_crystal_description       block
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         8484
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+0.9552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0903
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5768
_reflns_number_total             8484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00965b2.cif
_cod_data_source_block           20170612c
_cod_original_cell_volume        2325.8(2)
_cod_database_code               7240998
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         c1h1n1o1i1f1
_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. Restrained distances
 C18-C19
 1.38 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C20(H20), C22(H22), C23(H23), C21(H21), C19(H19), C48(H48), C49(H49),
 C44(H44), C37(H37), C42(H42), C50(H50), C43(H43), C33(H33), C39(H39), C34(H34),
  C35(H35), C32(H32), C13(H13), C28(H28), C36(H36), C24(H24), C31(H31),
 C15(H15), C26(H26), C27(H27), C16(H16), C25(H25), C14(H14)
3.b Fitted hexagon refined as free rotating group:
 C18(C20,C22,C23,C21,C19)
;
_shelx_res_checksum              12909
_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 1.537
_oxdiff_exptl_absorpt_empirical_full_min 0.691