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_7712521
_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         'C35 H40 N5 O2 Pt, B F4, 0.9[CHCl3]'
_chemical_formula_sum            'C35 H40 B F4 N5 O2 Pt'
_chemical_formula_weight         844.62
_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
_atom_sites_solution_primary     dual
_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                80.977(4)
_cell_angle_beta                 83.061(4)
_cell_angle_gamma                68.144(5)
_cell_formula_units_Z            2
_cell_length_a                   11.6565(7)
_cell_length_b                   11.9574(7)
_cell_length_c                   15.1337(7)
_cell_measurement_reflns_used    9381
_cell_measurement_temperature    99.99(18)
_cell_measurement_theta_max      73.4380
_cell_measurement_theta_min      2.9740
_cell_volume                     1929.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(18)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3829
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -66.00  33.00   1.00    1.50    --  -41.19  38.00-150.00   99
  2  \w   -107.00 -17.00   1.00    1.50    --  -41.19 -57.00 -90.00   90
  3  \w    -64.00  32.00   1.00    1.50    --  -41.19  57.00  60.00   96
  4  \w     90.00 127.00   1.00    1.50    --   41.19 178.00 -90.00   37
  5  \w     17.00  44.00   1.00    1.50    --   41.19 -99.00 150.00   27
  6  \w    132.00 159.00   1.00    6.50    --  106.94  15.00  60.00   27
  7  \w     67.00 108.00   1.00    6.50    --  106.94  15.00  60.00   41
  8  \w     55.00 153.00   1.00    6.50    --  106.94  15.00 -30.00   98
  9  \w     36.00 110.00   1.00    6.50    --  106.94-126.00-180.00   74
 10  \w     44.00  80.00   1.00    6.50    --  106.94-126.00 -30.00   36
 11  \w    104.00 173.00   1.00    6.50    --  106.94  77.00-180.00   69
 12  \w     36.00 131.00   1.00    6.50    --  106.94 -61.00 -30.00   95
 13  \w     66.00 114.00   1.00    6.50    --  106.94-126.00 -60.00   48
 14  \w     85.00 113.00   1.00    6.50    --  106.94-126.00 120.00   28
 15  \w     34.00 132.00   1.00    6.50    --  106.94 -45.00 120.00   98
 16  \w     27.00 106.00   1.00    6.50    --  106.94 -95.00 -30.00   79
 17  \w     82.00 109.00   1.00    6.50    --  106.94  45.00 120.00   27
 18  \w    152.00 177.00   1.00    6.50    --  106.94  45.00 120.00   25
 19  \w     97.00 123.00   1.00    6.50    --  106.94 -84.00 110.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0601684000
_diffrn_orient_matrix_UB_12      -0.0525878000
_diffrn_orient_matrix_UB_13      0.0899294000
_diffrn_orient_matrix_UB_21      0.0647212000
_diffrn_orient_matrix_UB_22      0.0933693000
_diffrn_orient_matrix_UB_23      -0.0149304000
_diffrn_orient_matrix_UB_31      -0.1120809000
_diffrn_orient_matrix_UB_32      0.0898609000
_diffrn_orient_matrix_UB_33      0.0486148000
_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  0.0627
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12973
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.492
_diffrn_reflns_theta_max         67.492
_diffrn_reflns_theta_min         4.013
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.266
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.95a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       prism
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.836
_refine_diff_density_min         -1.843
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         6932
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0561P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0893
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6454
_reflns_number_total             6932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00080j2.cif
_cod_data_source_block           17878_ksa527_m
_cod_database_code               7712521
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C38 H50 B1 F4 N5 O2 Pt1'
_shelx_estimated_absorpt_t_max   0.530
_shelx_estimated_absorpt_t_min   0.274
_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. Restrained distances
 H2-N2
 0.75 with sigma of 0.002
3.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C32(H32A,H32B), C21(H21A,H21B), C22(H22A,H22B), C35(H35A,
 H35B), C34(H34A,H34B), C23(H23A,H23B), C24(H24A,H24B)
3.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C29(H29), C10(H10), C11(H11), C26(H26), C19(H19), C27(H27),
 C18(H18), C2(H2A), C15(H15), C3(H3), C16(H16), C9(H9), C8(H8), C5(H5), C4(H4A)
3.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C20(H20A,H20B,H20C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 104 electrons were 
found in a volume of 350\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.9[CHCl3] per Formula Unit 
which account for 104 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              3762
_shelx_hkl_checksum              57710
_shelx_fab_checksum              85196
_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 2.261
_oxdiff_exptl_absorpt_empirical_full_min 0.455