Architectural diversity in the solid-state behaviour of crown ether and [2.2.2]-cryptand complexes of K+TCNQ•– salts
Yan, Bingjia; Horton, Peter; Weston, Simon C.; Wedge, Christopher J.; Russell, Andrea E.; Grossel, Martin C.; CrystEngComm  (2022) –; doi:10.1039/D2CE00773H

data_7245409
_publ_section_title
;
 Architectural diversity in the solid-state behaviour of crown ether and
 [2.2.2]-cryptand complexes of K+TCNQ&#x2022;-- salts
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00773H
_journal_year                    2022
_chemical_formula_moiety         'C16 H24 K O6, 2(C12 H4 N4)'
_chemical_formula_sum            'C40 H32 K N8 O6'
_chemical_formula_weight         759.83
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-11-02 deposited with the CCDC.	2022-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.840(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.44420(10)
_cell_length_b                   35.1206(6)
_cell_length_c                   8.0868(2)
_cell_measurement_reflns_used    15135
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.7950
_cell_measurement_theta_min      2.6120
_cell_volume                     1803.31(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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    -85.00  57.00   1.00   50.00    --  -17.00   0.00  90.00  142
  2  \w    -98.00  22.00   1.00   50.00    --  -17.00 -72.00 -90.00  120
  3  \w    -68.00  22.00   1.00   50.00    --  -17.00 -72.00  90.00   90
  4  \w    -15.00  70.00   1.00   50.00    --  -17.00  54.00-150.00   85
  5  \w      2.00  22.00   1.00   50.00    --  -17.00 -72.00 -60.00   20
  6  \w   -107.00  -3.00   1.00   50.00    --  -17.00 -72.00-150.00  104
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with HF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0014150000
_diffrn_orient_matrix_UB_12      -0.0182538000
_diffrn_orient_matrix_UB_13      0.0377283000
_diffrn_orient_matrix_UB_21      0.0475172000
_diffrn_orient_matrix_UB_22      0.0079185000
_diffrn_orient_matrix_UB_23      0.0779783000
_diffrn_orient_matrix_UB_31      -0.1011131000
_diffrn_orient_matrix_UB_32      0.0034750000
_diffrn_orient_matrix_UB_33      0.0203898000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            20813
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.556
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.209
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.105a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark blue'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       needle
_exptl_crystal_F_000             790
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4212
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0468P)^2^+0.7271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0908
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3771
_reflns_number_total             4212
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00773h2.cif
_cod_data_source_block           MCG3_benzo18c6
_cod_database_code               7245409
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C40H40N8 O12 K'
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.944
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O22-C26B_$1 \\sim O22-C26 \\sim O23-C27 \\sim O23B_$1-C27B_$1 \\sim O23-C28
\\sim O23B_$1-C28B_$1
 \\sim O22-C25
 with sigma of 0.02
 C27-C26 \\sim C27B_$1-C26B_$1 \\sim C28B_$1-C28_$1 \\sim C25-C24
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O23 \\sim C26 \\sim C27 \\sim C28B \\sim C28 \\sim O23B \\sim C26B \\sim C27B:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C26) = Uanis(C26B)
4. Rigid body (RIGU) restrains
 O23, C26, C27, C28B, C28, O23B, C26B, C27B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O23(0.5) C26(0.5) H26A(0.5) H26B(0.5) C27(0.5) H27A(0.5) H27B(0.5)
 C28B(0.5) H28A(0.5) H28B(0.5) C28(0.5) H28C(0.5) H28D(0.5) O23B(0.5) C26B(0.5)
 H26C(0.5) H26D(0.5) C27B(0.5) H27C(0.5) H27D(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C24(H24A,H24B), C26(H26A,H26B), C27(H27A,H27B), C28B(H28A,
 H28B), C28(H28C,H28D), C26B(H26C,H26D), C27B(H27C,H27D)
6.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C21(H21), C22(H22), C3(H3), C2(H2)
;
_shelx_res_checksum              701
_shelx_hkl_checksum              42917
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.283
_oxdiff_exptl_absorpt_empirical_full_min 0.595