Analysis of Solid-State Emission of the p-Bis(2,2-dicyanovinyl)benzene Analogue through Combined X-ray, Synchrotron, and Microcrystal Electron Diffraction
Deka, Poonam; Jaiswal, Shilpi; Sarma, Parishmita; Bora, Debajit; Nakane, Takanori; Kawamoto, Akihiro; Kurisu, Genji; Mahanta, Sanjeev Pran; Patra, Abhijit; Ichiyanagi, Kouhei; Sasaki, Toshiyuki; Thakuria, Ranjit; Crystal Growth & Design 24 (2024) 7222–7234; doi:10.1021/acs.cgd.4c00856

data_3000470
_publ_section_title
;
 Analysis of Solid-State Emission of the p-Bis(2,2-dicyanovinyl)benzene
 Analogue through Combined X-ray, Synchrotron, and Microcrystal Electron
 Diffraction
;
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              7222
_journal_page_last               7234
_journal_paper_doi               10.1021/acs.cgd.4c00856
_journal_volume                  24
_journal_year                    2024
_chemical_formula_moiety         '2(O), C20 H10 N4'
_chemical_formula_sum            'C20 H10 N4 O2'
_chemical_formula_weight         338.33
_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   difmap
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-11-03
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                97.17
_cell_angle_beta                 96.81
_cell_angle_gamma                99.79
_cell_formula_units_Z            2
_cell_length_a                   3.795
_cell_length_b                   14.526
_cell_length_c                   17.715
_cell_measurement_reflns_used    5084
_cell_measurement_temperature    79
_cell_measurement_theta_max      0.870595921720824
_cell_measurement_theta_min      0.10288693714916029
_cell_volume                     945.003
_computing_cell_refinement
'dials.two_theta_refine (Waterman et al., 2016)'
_computing_data_collection
'Verlox (Thermo Fisher Scientific) and SerialEM (Mastronarde, 2005)'
_computing_data_reduction        'dials.scale (Beilsten-Edmands et al., 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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      79
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
;
Talos Arctica G2
;
_diffrn_radiation_type           electrons
_diffrn_radiation_wavelength     0.02508
_diffrn_reflns_av_R_equivalents  0.2838
_diffrn_reflns_av_unetI/netI     0.2347
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31259
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        0.845
_diffrn_reflns_theta_max         0.845
_diffrn_reflns_theta_min         0.104
_exptl_absorpt_coefficient_mu    0.000
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_description       plate
_exptl_crystal_F_000             135
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.180
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       38194(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.281
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         3221
_refine_ls_number_restraints     228
_refine_ls_restrained_S_all      1.241
_refine_ls_R_factor_all          0.2225
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4048
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1615
_reflns_number_total             3221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            BP1_ADD.cif
_cod_data_source_block           bp1
_cod_depositor_comments
'Releasing structure 3000470 into public domain as published material.'
_cod_original_cell_volume        945.0
_cod_database_code               3000470
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 C17-H17 \\sim C18-H18 \\sim C15-H15 \\sim C14-H14 \\sim C8-H8 \\sim C7-H7
\\sim C5-H5 \\sim C4-H4 \\sim C2-H2
 \\sim C12-H12
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(O2B) \\sim Ueq, Uanis(O2A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O2B)=1-FVAR(1)
 Sof(O2A)=FVAR(1)
;
_shelx_res_checksum              95028
_shelx_hkl_checksum              7737
_olex2_submission_special_instructions 'No special instructions were received'