Series of charge transfer complexes obtained as crystals in a confined environment
Sanda Bawa, Ali; Meunier-Prest, Rita; Rousselin, Yoann; Couvercelle, Jean-Pierre; Christine, Stern; Malézieux, Bernard; Bouvet, Marcel; CrystEngComm  (2021) –; doi:10.1039/D1CE00929J

data_7243403
_publ_section_title
;
 Series of charge transfer complexes obtained as crystals in a confined
 environment
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D1CE00929J
_journal_year                    2021
_chemical_formula_moiety         'C10 H2 N4, C6 H6 O2'
_chemical_formula_sum            'C16 H8 N4 O2'
_chemical_formula_weight         288.26
_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     dual
_audit_creation_date             2019-11-19
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-01 deposited with the CCDC.	2021-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                108.309(5)
_cell_angle_beta                 109.791(4)
_cell_angle_gamma                92.810(5)
_cell_formula_units_Z            1
_cell_length_a                   6.3120(4)
_cell_length_b                   7.4057(5)
_cell_length_c                   8.1661(5)
_cell_measurement_reflns_used    1700
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      66.59
_cell_measurement_theta_min      6.15
_cell_volume                     335.79(4)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 CMOS
_diffrn_detector_area_resol_mean '1024 x 1024'
_diffrn_detector_type            'Photon 100'
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans''
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'QUAZAR MX multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_unetI/netI     0.0734
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2906
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        66.706
_diffrn_reflns_theta_max         66.706
_diffrn_reflns_theta_min         6.153
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              'high brilliance microfocus sealed tube, Cu'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.817
_exptl_absorpt_correction_T_max  0.9287
_exptl_absorpt_correction_T_min  0.7394
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1231 before and 0.0720 after correction.
The Ratio of minimum to maximum transmission is 0.7962.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       plate
_exptl_crystal_F_000             148
_exptl_crystal_recrystallization_method
'The material was recrystallised by sublimation'
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.061
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.290
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1163
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.290
_refine_ls_R_factor_all          0.1149
_refine_ls_R_factor_gt           0.0934
_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^)+0.9100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1831
_refine_ls_wR_factor_ref         0.1915
_reflns_Friedel_coverage         0.000
_reflns_number_gt                927
_reflns_number_total             1163
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00929j2.cif
_cod_data_source_block           TCNB-H2Q
_cod_database_code               7243403
_publcif_datablock.id            {0bb0e9a7-9b7e-4a94-8f6c-62024d4e67ff}
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.882
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C1(H1)
2.b Idealised tetrahedral OH refined as rotating group:
 O1(H1A)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder oil'
_olex2_submission_special_instructions 'No special instructions were received'