1,2,4-triazine derived binuclear lead(ii) complexes: synthesis, spectroscopic and structural investigations and application in organic light-emitting diodes (OLEDs)
Arkak, Akbar; Sadr, Moayad Hossaini; Janghouri, Mohammad; Marandi, Farzin; Fuhrmann, Daniel; RSC Advances 14 (2024) 22006–22016; doi:10.1039/D4RA03383C

data_7249046
_publ_section_title
;
 1,2,4-triazine derived binuclear lead(ii) complexes: synthesis,
 spectroscopic and structural investigations and application in organic
 light-emitting diodes (OLEDs)
;
_journal_issue                   30
_journal_name_full               'RSC Advances'
_journal_page_first              22006
_journal_page_last               22016
_journal_paper_doi               10.1039/D4RA03383C
_journal_volume                  14
_journal_year                    2024
_chemical_formula_sum            'C36 H30 N10 O6 Pb2 S2'
_chemical_formula_weight         1177.2
_chemical_melting_point          478
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-07-10T18:33:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2024-04-23 deposited with the CCDC.	2024-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                81.463(5)
_cell_angle_beta                 68.068(5)
_cell_angle_gamma                86.765(5)
_cell_formula_units_Z            1
_cell_length_a                   9.7327(6)
_cell_length_b                   10.2844(6)
_cell_length_c                   10.5326(7)
_cell_measurement_reflns_used    10802
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.45
_cell_volume                     967.13(11)
_computing_cell_refinement
;
X-Area Recipe 1.36.0.0 (STOE, 2020)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 1.78.3.0 (STOE, 2020)
X-Area LANA 1.83.8.0 (STOE, 2020)
;
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.90, Darmstadt 2020
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'image plate (34 cm diameter / schwenk)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      ' 225 frames, detector distance = 110 mm'
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9247
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.939
_diffrn_reflns_theta_min         2.698
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40.000
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    8.88
_exptl_absorpt_correction_T_max  0.4198
_exptl_absorpt_correction_T_min  0.2185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.021
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_recrystallization_method 'Diffusion experiment'
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.671
_refine_diff_density_min         -1.57
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0334P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0572
_reflns_Friedel_coverage         0
_reflns_number_gt                3900
_reflns_number_total             4574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra03383c2.cif
_cod_data_source_block           ip2-2694_d15
_cod_database_code               7249046
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              45307