Novel TCNQ-stacking motifs in (12-crown-4)-complexes of alkali metal TCNQ salts
Yan, Bingjia; Horton, Peter N.; Weston, Simon C.; Russell, Andrea E.; Grossel, Martin C.; CrystEngComm 23 (2021) 6755–6760; doi:10.1039/D1CE01075A

data_7243510
_publ_section_title
;
 Novel TCNQ-stacking motifs in (12-crown-4)-complexes of alkali metal TCNQ
 salts
;
_journal_issue                   38
_journal_name_full               CrystEngComm
_journal_page_first              6755
_journal_page_last               6760
_journal_paper_doi               10.1039/D1CE01075A
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C16 H32 K O8, 2(C12 H4 N4)'
_chemical_formula_sum            'C40 H40 K N8 O8'
_chemical_formula_weight         799.90
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-05-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2021-08-06 deposited with the CCDC.	2021-08-31 downloaded from the CCDC.
;
_cell_angle_alpha                80.507(2)
_cell_angle_beta                 85.505(2)
_cell_angle_gamma                85.457(2)
_cell_formula_units_Z            2
_cell_length_a                   8.0221(2)
_cell_length_b                   13.6455(3)
_cell_length_c                   18.3816(5)
_cell_measurement_reflns_used    16176
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.7950
_cell_measurement_theta_min      2.8530
_cell_volume                     1973.99(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection
'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_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 0.996
_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    -69.00  73.00   1.00   35.00    --  -17.00   0.00  30.00  142
  2  \w    -25.00  73.00   1.00   35.00    --  -17.00  72.00-120.00   98
  3  \w    -78.00  22.00   1.00   35.00    --  -17.00 -72.00 150.00  100
  4  \w    -68.00  22.00   1.00   35.00    --  -17.00 -72.00 -30.00   90
  5  \w      2.00  22.00   1.00   35.00    --  -17.00 -72.00   0.00   20
  6  \w    -89.00  20.00   1.00   35.00    --  -17.00   0.00 -90.00  109
;
_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      0.0518010000
_diffrn_orient_matrix_UB_12      -0.0183876000
_diffrn_orient_matrix_UB_13      -0.0285154000
_diffrn_orient_matrix_UB_21      0.0421468000
_diffrn_orient_matrix_UB_22      -0.0344401000
_diffrn_orient_matrix_UB_23      0.0268420000
_diffrn_orient_matrix_UB_31      -0.0586707000
_diffrn_orient_matrix_UB_32      -0.0355806000
_diffrn_orient_matrix_UB_33      -0.0019479000
_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  0.0241
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25643
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_min         2.721
_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    0.198
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       block
_exptl_crystal_F_000             838
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         9014
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0515P)^2^+0.3848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1042
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6853
_reflns_number_total             9014
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01075a2.cif
_cod_data_source_block           MCG5
_cod_depositor_comments
'Adding full bibliography for 7243509--7243513.cif.'
_cod_database_code               7243510
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C12H4N4 C8H16O4 K'
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.979
_reflns_odcompleteness_completeness 99.42
_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 Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C56(H56A,
 H56B), C58(H58A,H58B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B),
 C64(H64A,H64B), C65(H65A,H65B), C67(H67A,H67B), C68(H68A,H68B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C32(H32), C33(H33), C35(H35), C36(H36)
;
_shelx_res_checksum              93848
_shelx_hkl_checksum              19011
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_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 1.469
_oxdiff_exptl_absorpt_empirical_full_min 0.750