Alkali metal salts of a tetracyanopyridine (TCPy) derivative: structure characterization and luminescence properties
Chunikhin, Sergey S.; Ershov, Oleg V.; Yatsenko, Alexandr V.; Tafeenko, Viktor A.; Dmitrieva, Natalia E.; Ievlev, Mikhail Yu.; CrystEngComm 23 (2021) 2816–2824; doi:10.1039/D1CE00028D

data_7242363
_publ_section_title
;
 Alkali metal salts of a tetracyanopyridine (TCPy) derivative: structure
 characterization and luminescence properties
;
_journal_issue                   15
_journal_name_full               CrystEngComm
_journal_page_first              2816
_journal_page_last               2824
_journal_paper_doi               10.1039/D1CE00028D
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         '2(C19 H11 K N6)'
_chemical_formula_sum            'C38 H22 K2 N12'
_chemical_formula_weight         724.88
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2020-05-01 deposited with the CCDC.	2021-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.6080(5)
_cell_length_b                   7.2325(2)
_cell_length_c                   23.9944(5)
_cell_measurement_reflns_used    3606
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      65.3
_cell_measurement_theta_min      7.2
_cell_volume                     3576.30(15)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      295
_diffrn_detector                 Pilatus100K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'stadivari pilatus100k'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  none
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.1112
_diffrn_reflns_av_unetI/netI     0.1971
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            13535
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.119
_diffrn_reflns_theta_max         67.119
_diffrn_reflns_theta_min         3.684
_diffrn_source                   'Cu GeniX 3D'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.719
_exptl_absorpt_correction_T_max  0.857
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          .19
_exptl_crystal_size_mid          .16
_exptl_crystal_size_min          .15
_refine_diff_density_max         1.277
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.40(5)
_refine_ls_extinction_coef       0.0029(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   0.807
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         5063
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.807
_refine_ls_R_factor_all          0.1611
_refine_ls_R_factor_gt           0.0736
_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^)+(0.0906P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1604
_refine_ls_wR_factor_ref         0.1980
_reflns_Friedel_coverage         0.954
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                2012
_reflns_number_total             5063
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00028d2.cif
_cod_data_source_block           ss140_k
_cod_depositor_comments
'Adding full bibliography for 7242361--7242365.cif.'
_cod_database_code               7242363
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              88150
_shelx_hkl_checksum              9661