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_7241000
_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         '3(C6 F4 I2), 3(C11 H9 N O), 2(C10 H6)'
_chemical_formula_sum            'C71 H39 F12 I6 N3 O3'
_chemical_formula_weight         1971.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 111.263(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9947(5)
_cell_length_b                   16.3335(3)
_cell_length_c                   21.9920(5)
_cell_measurement_reflns_used    29141
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.5060
_cell_measurement_theta_min      3.7130
_cell_volume                     6358.5(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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_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      0.00  25.00   1.00    4.00    --   12.76 -37.00  60.00   25
  2  \w      4.00  54.00   1.00    4.00    --   12.76 -19.00  60.00   50
  3  \w     27.00  86.00   1.00    4.00    --   12.76  37.00 -60.00   59
  4  \w      6.00  34.00   1.00    4.00    --   12.76  37.00-180.00   28
  5  \w    -11.00  79.00   1.00    4.00    --   12.76  37.00-120.00   90
  6  \w    -19.00  30.00   1.00    4.00    --  -11.04 -99.00 -90.00   49
  7  \w    -19.00  32.00   1.00    4.00    --   12.76 -99.00 150.00   51
  8  \w     49.00 100.00   1.00    4.00    --   12.76-178.00 120.00   51
  9  \w     50.00  76.00   1.00    4.00    --   12.76-178.00 -60.00   26
 10  \w    -62.00 -27.00   1.00    4.00    --   12.76 -37.00  60.00   35
 11  \w    -63.00 -38.00   1.00    4.00    --   12.76 -19.00  60.00   25
 12  \w     48.00  73.00   1.00    4.00    --   12.76 178.00   0.00   25
;
_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      -0.0189907000
_diffrn_orient_matrix_UB_12      0.0356767000
_diffrn_orient_matrix_UB_13      -0.0161709000
_diffrn_orient_matrix_UB_21      0.0301951000
_diffrn_orient_matrix_UB_22      0.0245200000
_diffrn_orient_matrix_UB_23      0.0203036000
_diffrn_orient_matrix_UB_31      0.0182511000
_diffrn_orient_matrix_UB_32      -0.0034442000
_diffrn_orient_matrix_UB_33      -0.0228859000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            68868
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         3.281
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.019
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77230
_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 yellow'
_exptl_crystal_density_diffrn    2.059
_exptl_crystal_description       block
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.622
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     868
_refine_ls_number_reflns         11604
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0156P)^2^+36.7581P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0735
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9598
_reflns_number_total             11604
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00965b2.cif
_cod_data_source_block           20170531a
_cod_database_code               7241000
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         c1h1n1o1i1f1
_reflns_odcompleteness_completeness 99.71
_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. Uiso/Uaniso restraints and constraints
Uanis(C59) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C56)
\\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C53) \\sim Ueq,
Uanis(C52) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C67)
\\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq,
Uanis(C72) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C62) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C28(H28), C50(H50), C38(H38), C39(H39), C40(H40), C37(H37), C27(H27),
 C33(H33), C26(H26), C34(H34), C51(H51), C29(H29), C67(H67), C48(H48), C68(H68),
  C49(H49), C31(H31), C63(H63), C23(H23), C54(H54), C64(H64), C32(H32),
 C45(H45), C55(H55), C69(H69), C22(H22), C43(H43), C42(H42), C44(H44), C30(H30),
  C59(H59), C57(H57), C65(H65), C53(H53), C41(H41), C58(H58)
;
_shelx_res_checksum              81525
_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 1.137
_oxdiff_exptl_absorpt_empirical_full_min 0.838