Cyclometalated Platinum(II) Complexes with Acyclic Diaminocarbene Ligands for OLED Application
Katkova, Svetlana; Kozina, Daria O.; Kisel, Kristina S.; Sandzhieva, Maria A.; Tarvanen, Dmitriy; Makarov, Sergey; Porsev, Vitaly Veniaminovich; Tunik, Sergey P.; Kinzhalov, Mikhail A.; Dalton Transactions  (2023) –; doi:10.1039/D3DT00080J

data_7712520
_publ_section_title
;
 Cyclometalated Platinum(II) Complexes with Acyclic Diaminocarbene Ligands
 for OLED Application
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00080J
_journal_year                    2023
_chemical_formula_moiety         'C23 H21 Cl F3.002 N3 O Pt'
_chemical_formula_sum            'C23 H21 Cl F3 N3 O Pt'
_chemical_formula_weight         642.97
_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   mixed
_audit_creation_date             2023-02-03
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-03 deposited with the CCDC.	2023-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                89.573(3)
_cell_angle_beta                 72.113(4)
_cell_angle_gamma                69.091(4)
_cell_formula_units_Z            2
_cell_length_a                   9.9036(5)
_cell_length_b                   9.9576(5)
_cell_length_c                   12.3123(5)
_cell_measurement_reflns_used    10992
_cell_measurement_temperature    296.00(10)
_cell_measurement_theta_max      32.0390
_cell_measurement_theta_min      3.3150
_cell_volume                     1072.26(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.00(10)
_diffrn_detector_area_resol_mean 16.2096
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_details
;
  1 omega  -57.00    3.00   1.0000    3.9900
omega____ theta____ kappa____ phi______ frames
    -      -25.4311  -77.0000   90.0000 60

  2 omega  -79.00  -35.00   1.0000    3.9900
omega____ theta____ kappa____ phi______ frames
    -      -25.4311 -178.0000 -180.0000 44

  3 omega   48.00  100.00   1.0000    3.9900
omega____ theta____ kappa____ phi______ frames
    -       26.3686  178.0000  -60.0000 52

  4 omega  -24.00   68.00   1.0000    3.9900
omega____ theta____ kappa____ phi______ frames
    -       26.3686  -99.0000    0.0000 92

  5 omega   34.00   67.00   1.0000    3.9900
omega____ theta____ kappa____ phi______ frames
    -       26.3686  -99.0000 -120.0000 33

  6 omega  -18.00   96.00   1.0000    3.9900
omega____ theta____ kappa____ phi______ frames
    -       26.3686   19.0000  120.0000 114

  7 omega   50.00   95.00   1.0000    3.9900
omega____ theta____ kappa____ phi______ frames
    -       26.3686   57.0000  150.0000 45

  8 omega  -83.00   -4.00   1.0000    3.9900
omega____ theta____ kappa____ phi______ frames
    -      -25.4311  -57.0000  -30.0000 79

  9 omega  -96.00    4.00   1.0000    3.9900
omega____ theta____ kappa____ phi______ frames
    -      -25.4311  -77.0000  -90.0000 100

 10 omega  -62.00   -4.00   1.0000    3.9900
omega____ theta____ kappa____ phi______ frames
    -      -25.4311  -57.0000  150.0000 58

 11 omega  -55.00   38.00   1.0000    3.9900
omega____ theta____ kappa____ phi______ frames
    -      -25.4311   77.0000  120.0000 93

 12 omega  -35.00   52.00   1.0000    3.9900
omega____ theta____ kappa____ phi______ frames
    -       26.3686  -38.0000    0.0000 87
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0576070000
_diffrn_orient_matrix_UB_12      0.0532064000
_diffrn_orient_matrix_UB_13      -0.0166962000
_diffrn_orient_matrix_UB_21      0.0495145000
_diffrn_orient_matrix_UB_22      0.0380795000
_diffrn_orient_matrix_UB_23      -0.0204556000
_diffrn_orient_matrix_UB_31      0.0283995000
_diffrn_orient_matrix_UB_32      -0.0401447000
_diffrn_orient_matrix_UB_33      -0.0549211000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22956
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.276
_diffrn_reflns_theta_min         2.652
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.715
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.991
_exptl_crystal_description       prism
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.001
_refine_diff_density_min         -1.205
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         6998
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0144P)^2^+0.1252P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0452
_refine_ls_wR_factor_ref         0.0471
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6463
_reflns_number_total             6998
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00080j2.cif
_cod_data_source_block           14533_rsa520m
_cod_original_cell_volume        1072.26(9)
_cod_database_code               7712520
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C23 H21 Cl F3 N3 Pt'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 F3-F1 \\sim F3'-F1'
 with sigma of 0.04
 F3-F2 \\sim F3'-F2'
 with sigma of 0.04
 F1-F2 \\sim F1'-F2'
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(F3') \\sim Ueq, Uanis(F1') \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 F3', C19, F1', F2'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F3, F1, F2, C14, C18, C16, C15, C19, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C9(H9), C11(H11), C2(H2A), C10(H10), C14(H14), C18(H18),
 C15(H15), C17(H17), C4(H4), C3(H3)
;
_shelx_res_checksum              1902
_shelx_hkl_checksum              26891
_olex2_submission_special_instructions 'No special instructions were received'