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_7245410
_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         'C20 H24 K O6, 2(C12 H4 N4)'
_chemical_formula_sum            'C44 H32 K N8 O6'
_chemical_formula_weight         807.87
_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     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                96.6200(10)
_cell_angle_beta                 93.222(2)
_cell_angle_gamma                101.779(2)
_cell_formula_units_Z            2
_cell_length_a                   7.8459(3)
_cell_length_b                   14.5336(4)
_cell_length_c                   17.8334(4)
_cell_measurement_reflns_used    8496
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.0
_cell_volume                     1970.77(10)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b31 (Rigaku, 2014)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b31 (Rigaku, 2014)
;
_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      120(2)
_diffrn_detector                 'Image plate'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_type            'Rigaku Curved Fujifilm'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       'three-circle quarter \c goniometer'
_diffrn_measurement_device_type
'Rigaku R-AXIS SPIDER IP equipped with a three-circle quarter \c goniometer'
_diffrn_measurement_method       'profile data from oscillation \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  graphite
_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  0.0769
_diffrn_reflns_av_unetI/netI     0.0818
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24504
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.591
_diffrn_reflns_theta_min         2.558
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_size              '12mm x 0.4 mm long fine-focus'
_diffrn_source_target            Mo
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear-SM Expert 2.1 b31 (Rigaku, 2014)'
_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    1.361
_exptl_crystal_description       plate
_exptl_crystal_F_000             838
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         8943
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.1159
_refine_ls_R_factor_gt           0.0842
_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^)+(0.0288P)^2^+2.2897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1545
_refine_ls_wR_factor_ref         0.1698
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6598
_reflns_number_total             8943
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00773h2.cif
_cod_data_source_block           MCG4_dibenzo18c6
_cod_database_code               7245410
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.940
_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:
 C317(H317), C318(H318), C319(H319), C320(H320)
2.b Secondary CH2 refined with riding coordinates:
 C307(H30A,H30B), C308(H30C,H30D), C309(H30E,H30F), C310(H31A,H31B), C313(H31C,
 H31D), C314(H31E,H31F), C315(H31G,H31H), C316(H31I,H31J)
2.c Aromatic/amide H refined with riding coordinates:
 C302(H302), C303(H303), C304(H304), C305(H305), C102(H102), C103(H103),
 C105(H105), C106(H106), C202(H202), C203(H203), C205(H205), C206(H206)
;
_shelx_res_checksum              79342
_shelx_hkl_checksum              88367
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'