Comparing the structures and photophysical properties of two charge transfer co-crystals.
Abou Taka, Ali; Reynolds, 3rd, Joseph E; Cole-Filipiak, Neil C; Shivanna, Mohana; Yu, Christine J.; Feng, Patrick; Allendorf, Mark D.; Ramasesha, Krupa; Stavila, Vitalie; McCaslin, Laura M.; Physical chemistry chemical physics : PCCP 25 (2023) 27065–27074; doi:10.1039/d3cp03720g

data_7247438
_publ_section_title
;
 Comparing the structures and photophysical properties of two charge
 transfer co-crystals.
;
_journal_issue                   40
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              27065
_journal_page_last               27074
_journal_paper_doi               10.1039/d3cp03720g
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C17 H13 N, 1.5(C12 H4 N4)'
_chemical_formula_sum            'C35 H19 N7'
_chemical_formula_weight         537.57
_chemical_name_systematic        3TCNQ2NPE
_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     direct
_audit_creation_date             2022-06-28
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-08-03 deposited with the CCDC.	2023-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                93.827(3)
_cell_angle_beta                 93.940(3)
_cell_angle_gamma                111.868(4)
_cell_formula_units_Z            2
_cell_length_a                   9.8862(4)
_cell_length_b                   11.8127(5)
_cell_length_c                   12.3102(5)
_cell_measurement_reflns_used    9179
_cell_measurement_temperature    102(3)
_cell_measurement_theta_max      72.7970
_cell_measurement_theta_min      3.5720
_cell_volume                     1324.38(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      102(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2358
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.972
_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   -117.00 -18.00   1.00    2.50    --  -42.59 -38.00  90.00   99
  2  \w    -87.00  -6.00   1.00    2.50    --  -42.59 125.00-120.00   81
  3  \w   -123.00  -2.00   1.00    2.50    --  -42.59 -19.00 150.00  121
  4  \w     27.00  99.00   1.00    2.50    --   42.59-125.00  60.00   72
  5  \w     27.00  99.00   1.00    2.50    --   42.59-125.00   0.00   72
  6  \w     31.00 130.00   1.00    7.50    --  104.03 -45.00-150.00   99
  7  \w     78.00 177.00   1.00    7.50    --  104.03  45.00-120.00   99
  8  \w    103.00 178.00   1.00    7.50    --  104.03  77.00 -90.00   75
  9  \w     31.00 112.00   1.00    7.50    --  104.03-125.00 -30.00   81
 10  \w     22.00 106.00   1.00    7.50    --  104.03 -95.00  60.00   84
 11  \w     78.00 177.00   1.00    7.50    --  104.03  45.00 -30.00   99
 12  \w     78.00 177.00   1.00    7.50    --  104.03  45.00-180.00   99
 13  \w     22.00 106.00   1.00    7.50    --  104.03 -95.00 120.00   84
 14  \w     22.00 106.00   1.00    7.50    --  104.03 -95.00   0.00   84
 15  \w     28.00 137.00   1.00    7.50    --  104.03 -77.00-180.00  109
 16  \w     28.00 132.00   1.00    7.50    --  104.03 -30.00 -60.00  104
 17  \w   -116.00 -14.00   1.00    2.50    --  -42.59 -57.00  60.00  102
 18  \w   -116.00 -14.00   1.00    2.50    --  -42.59 -57.00 -30.00  102
 19  \w     14.00 116.00   1.00    2.50    --   42.59  57.00 -60.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0112428000
_diffrn_orient_matrix_UB_12      0.0175216000
_diffrn_orient_matrix_UB_13      -0.1227225000
_diffrn_orient_matrix_UB_21      0.0382017000
_diffrn_orient_matrix_UB_22      0.1380527000
_diffrn_orient_matrix_UB_23      0.0287893000
_diffrn_orient_matrix_UB_31      0.1640097000
_diffrn_orient_matrix_UB_32      0.0240970000
_diffrn_orient_matrix_UB_33      -0.0020083000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14402
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.000
_diffrn_reflns_theta_min         3.617
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.660
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.628
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       prism
_exptl_crystal_F_000             556
_exptl_crystal_recrystallization_method '1:1 (DMF/MeCN)'
_exptl_crystal_size_max          0.421
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5154
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0650P)^2^+0.1666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1073
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4451
_reflns_number_total             5154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cp03720g2.cif
_cod_data_source_block           Npe-TCNQ
_cod_depositor_comments
'Adding full bibliography for 7247438--7247439.cif.'
_cod_original_cell_volume        1324.40(9)
_cod_database_code               7247438
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         N4C18H18
_chemical_oxdiff_usercomment     'Solvent MeCN. 1:1 NVP:TCNQ'
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.769
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11),
 C13(H13), C14(H14), C15(H15), C16(H16), C22(H22), C23(H23), C25(H25), C26(H26),
  C34(H34), C35(H35)
;
_shelx_res_checksum              74300
_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 1.150
_oxdiff_exptl_absorpt_empirical_full_min 0.885