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_7233297
_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         '4(c17 h8 n5),4(c6 n h16)'
_chemical_formula_sum            'C92 H96 N24'
_chemical_formula_weight         1537.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_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                 90.148(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.4174(2)
_cell_length_b                   18.7937(4)
_cell_length_c                   18.6491(4)
_cell_measurement_reflns_used    5673
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      60
_cell_measurement_theta_min      2
_cell_volume                     4352.11(15)
_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 0.994
_diffrn_measured_fraction_theta_max 0.988
_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  0.0225
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32098
_diffrn_reflns_point_group_measured_fraction_full 0.739
_diffrn_reflns_point_group_measured_fraction_max 0.726
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         73.307
_diffrn_reflns_theta_min         4.706
_diffrn_source                   'Cu GeniX 3D'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.574
_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    1.174
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          .21
_exptl_crystal_size_mid          .14
_exptl_crystal_size_min          .12
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 1796 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.08(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    ref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1063
_refine_ls_number_reflns         12691
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0634
_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^)+(0.1273P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1875
_refine_ls_wR_factor_ref         0.2027
_reflns_Friedel_coverage         0.425
_reflns_Friedel_fraction_full    0.466
_reflns_Friedel_fraction_max     0.447
_reflns_number_gt                7724
_reflns_number_total             12691
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01089k2.cif
_cod_data_source_block           ss13
_cod_depositor_comments
'Adding full bibliography for 7233297--7233300.cif.'
_cod_database_code               7233297
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              27673