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_7245412
_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         'C44 H44 K N8 O6, C12 H4 N4'
_chemical_formula_sum            'C56 H48 K N12 O6'
_chemical_formula_weight         1024.16
_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     iterative
_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                87.136(2)
_cell_angle_beta                 79.011(2)
_cell_angle_gamma                80.148(3)
_cell_formula_units_Z            1
_cell_length_a                   7.9514(2)
_cell_length_b                   9.9644(3)
_cell_length_c                   16.7703(4)
_cell_measurement_reflns_used    14379
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.9420
_cell_measurement_theta_min      2.6200
_cell_volume                     1284.92(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
;
Superflip  (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_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 0.997
_diffrn_measured_fraction_theta_max 0.994
_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    -35.00  73.00   1.00   10.00    --  -17.00  72.00   0.00  108
  2  \w    -69.00  20.00   1.00   10.00    --  -17.00 -72.00-120.00   89
  3  \w    -64.00  22.00   1.00   10.00    --  -17.00 -72.00  60.00   86
  4  \w    -54.00   8.00   1.00   10.00    --  -17.00   0.00  30.00   62
  5  \w    -32.00 -12.00   1.00   10.00    --  -17.00  54.00-150.00   20
  6  \w    -31.00  73.00   1.00   10.00    --  -17.00  72.00  30.00  104
  7  \w    -69.00  22.00   1.00   10.00    --  -17.00 -72.00 -90.00   91
  8  \w    -66.00 -45.00   1.00   10.00    --  -17.00 -72.00  90.00   21
;
_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      0.0128030000
_diffrn_orient_matrix_UB_12      -0.0721544000
_diffrn_orient_matrix_UB_13      0.0029992000
_diffrn_orient_matrix_UB_21      0.0171445000
_diffrn_orient_matrix_UB_22      -0.0037238000
_diffrn_orient_matrix_UB_23      -0.0429856000
_diffrn_orient_matrix_UB_31      0.0896115000
_diffrn_orient_matrix_UB_32      -0.0012229000
_diffrn_orient_matrix_UB_33      -0.0004018000
_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  0.0164
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16871
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.478
_diffrn_reflns_theta_min         2.397
_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    0.168
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86925
_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 violet'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       plate
_exptl_crystal_F_000             535
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         5852
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+0.3995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.0979
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5173
_reflns_number_total             5852
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00773h2.cif
_cod_data_source_block           MCG5_dicyclohexano18c6
_cod_original_cell_volume        1284.91(7)
_cod_database_code               7245412
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C40H50N10O12K
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.948
_reflns_odcompleteness_completeness 99.41
_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.a Ternary CH refined with riding coordinates:
 C304(H304), C309(H309)
2.b Secondary CH2 refined with riding coordinates:
 C301(H30A,H30B), C302(H30C,H30D), C303(H30E,H30F), C305(H30G,H30H), C306(H30I,
 H30J), C307(H30K,H30L), C308(H30M,H30N), C310(H31A,H31B)
2.c Aromatic/amide H refined with riding coordinates:
 C102(H102), C103(H103), C105(H105), C106(H106), C202(H202), C206(H206)
;
_shelx_res_checksum              93868
_shelx_hkl_checksum              59119
_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 1.515
_oxdiff_exptl_absorpt_empirical_full_min 0.702