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_7712523
_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         'C24 H27 Cl N4 O Pt'
_chemical_formula_sum            'C24 H27 Cl N4 O Pt'
_chemical_formula_weight         618.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-02-01
_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                90
_cell_angle_beta                 97.6964(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.05120(15)
_cell_length_b                   11.10207(8)
_cell_length_c                   24.15392(17)
_cell_measurement_reflns_used    22126
_cell_measurement_temperature    100.01(11)
_cell_measurement_theta_max      70.2810
_cell_measurement_theta_min      2.6710
_cell_volume                     5328.46(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -16.00  16.00   0.50    0.20    --  -38.82  49.00 171.00   64
  2  \w    -61.00 -35.00   0.50    0.20    --  -38.82 -49.00  24.00   52
  3  \w   -101.00 -73.00   0.50    0.20    --  -38.82 -49.00  24.00   56
  4  \w     83.00 116.00   0.50    0.50    --  100.00 -49.00  24.00   66
  5  \w     35.00  79.00   0.50    0.50    --  100.00 -49.00  24.00   88
  6  \w     96.00 141.00   0.50    0.50    --  100.00  49.00 171.00   90
  7  \w     -5.00  31.00   0.50    0.20    --  -38.82  21.00-180.00   72
  8  \w    -37.00 -12.00   0.50    0.20    --  -38.82  21.00-180.00   50
  9  \w   -106.00 -61.00   0.50    0.20    --  -38.82 -32.00  30.00   90
 10  \w    -57.00 -31.00   0.50    0.20    --  -38.82 -32.00  30.00   52
 11  \w   -102.00 -24.00   0.50    0.20    --  -38.82 -54.00 -60.00  156
 12  \w    -97.00 -21.00   0.50    0.20    --  -38.82 -54.00-150.00  152
 13  \w    -47.00 -21.00   0.50    0.20    --  -38.82 -21.00  60.00   52
 14  \w   -109.00 -63.00   0.50    0.20    --  -38.82 -21.00  60.00   92
 15  \w    -24.00   1.00   0.50    0.20    --   38.82 -32.00-120.00   50
 16  \w     52.00 108.00   0.50    0.20    --   38.82  32.00   0.00  112
 17  \w     -7.00  18.00   0.50    0.20    --   38.82 -89.00-150.00   50
 18  \w    -22.00  48.00   0.50    0.20    --   38.82 -32.00-150.00  140
 19  \w     77.00 102.00   0.50    0.20    --   38.82  49.00 171.00   50
 20  \w     -2.00  46.00   0.50    0.20    --   38.82 -49.00  24.00   96
 21  \w     33.00  58.00   0.50    0.20    --   38.82  49.00 171.00   50
 22  \w     34.00  68.00   0.50    0.20    --   38.82 -89.00-150.00   68
 23  \w     46.00  90.00   0.50    0.50    --  100.00 -53.00   0.00   88
 24  \w    108.00 134.00   0.50    0.50    --  100.00  30.00 150.00   52
 25  \w     26.00  52.00   0.50    0.50    --  100.00 -93.00-150.00   52
 26  \w     50.00 118.00   0.50    0.50    --  100.00 -61.00-150.00  136
 27  \w     70.00 101.00   0.50    0.50    --  100.00  15.00  60.00   62
 28  \w     29.00  67.00   0.50    0.50    --  100.00 -22.00 -30.00   76
 29  \w     82.00 134.00   0.50    0.50    --  100.00  45.00-150.00  104
 30  \w     52.00 114.00   0.50    0.50    --  100.00 -30.00  30.00  124
 31  \w    108.00 157.00   0.50    0.50    --  100.00  15.00  60.00   98
 32  \w     57.00 102.00   0.50    0.50    --  100.00-133.00   0.00   90
 33  \w    132.00 157.00   0.50    0.50    --  100.00  61.00 -60.00   50
 34  \w     78.00 127.00   0.50    0.50    --  100.00  61.00 -60.00   98
 35  \w     85.00 111.00   0.50    0.50    --  100.00  22.00 -30.00   52
 36  \w     86.00 131.00   0.50    0.50    --  100.00  22.00 120.00   90
 37  \w     30.00  56.00   0.50    0.50    --  100.00 -93.00 -60.00   52
 38  \w     69.00 156.00   0.50    0.50    --  100.00   7.00 -30.00  174
 39  \w     66.00 112.00   0.50    0.50    --  100.00 -30.00-180.00   92
 40  \w    104.00 151.00   0.50    0.50    --  100.00  30.00-150.00   94
 41  \w     76.00 125.00   0.50    0.50    --  100.00 -69.00 120.00   98
 42  \w     94.00 151.00   0.50    0.50    --  100.00  53.00-120.00  114
 43  \w     84.00 143.00   0.50    0.50    --  100.00  77.00  90.00  118
 44  \w     86.00 129.00   0.50    0.50    --  100.00  37.00-120.00   86
 45  \w     59.00  85.00   0.50    0.50    --  100.00 -22.00-180.00   52
 46  \w     39.00 101.00   0.50    0.50    --  100.00-133.00  30.00  124
 47  \w    -40.00 -14.00   0.50    0.20    --  -38.82  49.00 171.00   52
 48  \w    -75.00 -49.00   0.50    0.20    --  -38.82 -43.00-120.00   52
 49  \w    -11.00  15.00   0.50    0.20    --  -38.82  32.00  30.00   52
 50  \w    -70.00 -45.00   0.50    0.20    --  -38.82 104.00 150.00   50
 51  \w      1.00  12.50   0.50    0.20    --  -38.82  49.00 171.00   23
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0771639000
_diffrn_orient_matrix_UB_12      0.0113969000
_diffrn_orient_matrix_UB_13      -0.0112723000
_diffrn_orient_matrix_UB_21      -0.0064227000
_diffrn_orient_matrix_UB_22      -0.0829925000
_diffrn_orient_matrix_UB_23      0.0501270000
_diffrn_orient_matrix_UB_31      0.0032051000
_diffrn_orient_matrix_UB_32      0.1107491000
_diffrn_orient_matrix_UB_33      0.0387432000
_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  0.0422
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35514
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.997
_diffrn_reflns_theta_max         66.997
_diffrn_reflns_theta_min         3.075
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.932
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_description       prism
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.552
_refine_diff_density_min         -1.634
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         9492
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+16.8211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0782
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9073
_reflns_number_total             9492
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00080j2.cif
_cod_data_source_block           15400_ksa524_m
_cod_original_cell_volume        5328.47(7)
_cod_database_code               7712523
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 H27 Cl1 N4 Pt1'
_shelx_estimated_absorpt_t_max   0.475
_shelx_estimated_absorpt_t_min   0.197
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C21(H21A,H21B), C23(H23A,H23B), C24(H24A,H24B), C48(H48A,
 H48B), C47(H47A,H47B), C45(H45A,H45B), C46(H46A,H46B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C42(H42), C3(H3), C11(H11), C18(H18), C41(H41), C14(H14), C2(H2A),
 C17(H17), C5(H5), C9(H9), C35(H35), C4(H4), C10(H10), C39(H39), C8(H8),
 C38(H38), C29(H29), C26(H26), C27(H27), C32(H32), C34(H34), C28(H28), C33(H33)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C43(H43A,H43B,H43C), C19(H19A,H19B,H19C), C44(H44A,H44B,
 H44C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 364 electrons were 
found in a volume of 1112\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[CH2Cl2] per Formula Unit 
which account for 336 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              45781
_shelx_hkl_checksum              84796
_shelx_fab_checksum              86265
_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 2.142
_oxdiff_exptl_absorpt_empirical_full_min 0.756