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_7241002
_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), C18 H12, 2(C11 H9 N O)'
_chemical_formula_sum            'C52 H30 F8 I4 N2 O2'
_chemical_formula_weight         1374.38
_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   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                90
_cell_angle_beta                 114.181(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.8703(5)
_cell_length_b                   34.1971(7)
_cell_length_c                   17.3770(4)
_cell_measurement_reflns_used    7602
_cell_measurement_temperature    292.49(10)
_cell_measurement_theta_max      73.0320
_cell_measurement_theta_min      4.7230
_cell_volume                     9687.5(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.6a (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    'XS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.49(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_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    -57.00  30.00   1.00    3.00    --  -41.49  57.00 -90.00   87
  2  \w   -103.00 -76.00   1.00    3.00    --  -41.49 -57.00-150.00   27
  3  \w   -114.00 -13.00   1.00    3.00    --  -41.49 -57.00   0.00  101
  4  \w   -110.00 -83.00   1.00    3.00    --  -41.49 -37.00  90.00   27
  5  \w     60.00 103.00   1.00    3.00    --  107.52 -30.00  30.00   43
  6  \w     88.00 165.00   1.00    3.00    --  107.52  30.00 -90.00   77
  7  \w    114.00 149.00   1.00    3.00    --  107.52  77.00-180.00   35
  8  \w     90.00 177.00   1.00    3.00    --  107.52  61.00 -30.00   87
  9  \w     34.00 130.00   1.00    3.00    --  107.52 -45.00-180.00   96
 10  \w     29.00 102.00   1.00    3.00    --  107.52 -94.00  60.00   73
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0854901000
_diffrn_orient_matrix_UB_12      -0.0145748000
_diffrn_orient_matrix_UB_13      0.0113868000
_diffrn_orient_matrix_UB_21      -0.0029766000
_diffrn_orient_matrix_UB_22      -0.0315735000
_diffrn_orient_matrix_UB_23      0.0619537000
_diffrn_orient_matrix_UB_31      -0.0401508000
_diffrn_orient_matrix_UB_32      -0.0286146000
_diffrn_orient_matrix_UB_33      -0.0740416000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0622
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37327
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.321
_diffrn_reflns_theta_min         3.746
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.846
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.6a (Rigaku Oxford Diffraction, 2015)
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    1.885
_exptl_crystal_description       block
_exptl_crystal_F_000             5248
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.015
_refine_diff_density_min         -2.005
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       0.000049(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1214
_refine_ls_number_reflns         18962
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0637
_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^)+(0.0892P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1593
_refine_ls_wR_factor_ref         0.1927
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12292
_reflns_number_total             18962
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00965b2.cif
_cod_data_source_block           20170301b
_cod_depositor_comments
;

2024-11-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        9687.5(4)
_cod_original_formula_moiety     '4(C6 F4 I2), 2(C18 H12), 4(C11 H9 N O)'
_cod_original_formula_sum        'C104 H60 F16 I8 N4 O4'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     2748.76
_cod_database_code               7241002
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         c1h1n1o1i1f1
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C41) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C44)
\\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C45) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C52) \\sim Ueq, Uanis(C63) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C75(H75), C86(H86), C85(H85), C82(H82), C73(H73), C76(H76), C79(H79),
 C74(H74), C81(H81), C80(H80), C102(H102), C100(H100), C99(H99), C90(H90),
 C34(H34), C35(H35), C88(H88), C32(H32), C89(H89), C96(H96), C33(H33), C36(H36),
  C56(H56), C101(H101), C69(H69), C87(H87), C42(H42), C43(H43), C44(H44),
 C45(H45), C46(H46), C59(H59), C53(H53), C38(H38), C55(H55), C37(H37), C67(H67),
  C39(H39), C58(H58), C70(H70), C27(H27), C28(H28), C54(H54), C51(H51),
 C29(H29), C26(H26), C25(H25), C95(H95), C68(H68), C52(H52), C94(H94), C93(H93),
  C48(H48), C47(H47), C57(H57), C64(H64), C66(H66), C62(H62), C65(H65), C63(H63)
3.b Fitted hexagon refined as free rotating group:
 C41(C42,C43,C44,C45,C46)
;
_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 2.047
_oxdiff_exptl_absorpt_empirical_full_min 0.514