Crystallographic characterization of ethylammonium salts of tetracyanopyridine (TCPy) and fluorescence determination of the degree of substitution of the amino nitrogen atom thereof
Ershov, Oleg V.; Chunikhin, Sergey S.; Ievlev, Mikhail Yu.; Belikov, Mikhail Yu.; Tafeenko, Viktor A.; CrystEngComm 21 (2019) 5500–; doi:10.1039/C9CE01089K

data_7233299
_publ_section_title
;
 Crystallographic characterization of ethylammonium salts of
 tetracyanopyridine (TCPy) and fluorescence determination of the degree of
 substitution of the amino nitrogen atom thereof
;
_journal_issue                   36
_journal_name_full               CrystEngComm
_journal_page_first              5500
_journal_paper_doi               10.1039/C9CE01089K
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C17 H4 N5, C4 H12 N'
_chemical_formula_sum            'C21 H16 N6'
_chemical_formula_weight         352.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-03-14 deposited with the CCDC.    2019-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.1192(6)
_cell_length_b                   17.6034(5)
_cell_length_c                   18.3391(6)
_cell_measurement_reflns_used    1768
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60
_cell_measurement_theta_min      4
_cell_volume                     1975.5(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      295
_diffrn_detector                 Pilatus100K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  STOE
_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  0.08
_diffrn_reflns_av_unetI/netI     0.1097
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_number            3564
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         68.857
_diffrn_reflns_theta_min         4.823
_diffrn_source                   'Cu GeniX 3D'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.595
_exptl_absorpt_correction_T_max  0.570
_exptl_absorpt_correction_T_min  0.484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             736
_exptl_crystal_size_max          .17
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .14
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 483 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.3(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3564
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1358
_refine_ls_R_factor_gt           0.0781
_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^)+(0.1299P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2019
_refine_ls_wR_factor_ref         0.2643
_reflns_Friedel_coverage         0.713
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     0.967
_reflns_number_gt                1697
_reflns_number_total             3564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01089k2.cif
_cod_data_source_block           ss34
_cod_depositor_comments
'Adding full bibliography for 7233297--7233300.cif.'
_cod_database_code               7233299
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              38853