Deprotonated diaminocarbene platinum complexes for thermoresponsive luminescent silicone materials: both catalysts and luminophores
Dobrynin, Mikhail V.; Kasatkina, Svetlana; Baykov, Sergey; Savko, Polina; Antonov, Nikita; Mikherdov, Alexander S.; Boyarskiy, Vadim; Islamova, Regina M.; Dalton Transactions  (2021) –; doi:10.1039/D1DT02823E

data_7708543
_publ_section_title
;
 Deprotonated diaminocarbene platinum complexes for thermoresponsive
 luminescent silicone materials: both catalysts and luminophores
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02823E
_journal_year                    2021
_chemical_formula_moiety         'C30 H30 Cl N5 O Pt'
_chemical_formula_sum            'C30 H30 Cl N5 O Pt'
_chemical_formula_weight         707.13
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-10 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.11700(10)
_cell_length_b                   14.11700(10)
_cell_length_c                   27.4755(3)
_cell_measurement_reflns_used    62658
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.3880
_cell_measurement_theta_min      3.1770
_cell_volume                     5475.58(8)
_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 (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_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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    -25.00   1.00   0.50    0.15    --  -47.13  52.00  47.00   52
  2  \w   -117.00 -87.00   0.50    0.15    --  -47.13 -52.00 -97.00   60
  3  \w    -15.00  40.00   0.50    0.15    --   47.13 -52.00 -97.00  110
  4  \w     38.00 112.00   0.50    0.15    --   47.13  52.00  47.00  148
  5  \w   -177.00-103.00   0.50    0.60    -- -105.31 -52.00 -97.00  148
  6  \w    -58.00 -33.00   0.50    0.60    -- -105.31  52.00  47.00   50
  7  \w     33.00  58.00   0.50    0.60    --  105.31 -52.00 -97.00   50
  8  \w     95.00 178.00   0.50    0.60    --  105.31  52.00  47.00  166
  9  \w    -95.00 -44.00   0.50    0.15    --  -47.13 125.00  60.00  102
 10  \w   -121.00 -34.00   0.50    0.15    --  -47.13 -19.00 120.00  174
 11  \w    -66.00  19.00   0.50    0.15    --  -47.13  77.00 -60.00  170
 12  \w     14.00  39.00   0.50    0.15    --   47.13-125.00 -90.00   50
 13  \w     69.00  95.00   0.50    0.15    --   47.13-125.00 -90.00   52
 14  \w     74.00 119.00   0.50    0.15    --   47.13 125.00-150.00   90
 15  \w    -27.00   4.00   0.50    0.15    --   47.13 -19.00 120.00   62
 16  \w   -128.00 -94.00   0.50    0.60    -- -105.31 148.00-139.50   68
 17  \w    -92.00 -47.00   0.50    0.60    -- -105.31  77.00  60.00   90
 18  \w   -106.00 -51.00   0.50    0.60    -- -105.31  77.00 -30.00  110
 19  \w    -70.00 -38.00   0.50    0.60    -- -105.31  61.00 -90.00   64
 20  \w   -174.00-130.00   0.50    0.60    -- -105.31 -61.00   0.00   88
 21  \w   -108.00 -69.00   0.50    0.60    -- -105.31 110.00-167.40   78
 22  \w   -176.00 -90.00   0.50    0.60    -- -105.31 -61.00 -30.00  172
 23  \w   -110.00 -38.00   0.50    0.60    -- -105.31 125.00-180.00  144
 24  \w   -107.00 -39.00   0.50    0.60    -- -105.31 110.00 -23.93  136
 25  \w    -67.00 -34.00   0.50    0.60    -- -105.31  77.00-150.00   66
 26  \w   -110.00 -79.00   0.50    0.60    -- -105.31 119.00  86.87   62
 27  \w   -107.00 -69.00   0.50    0.60    -- -105.31 105.00 172.64   76
 28  \w   -105.00 -79.00   0.50    0.60    -- -105.31  77.00-150.00   52
 29  \w   -153.00 -96.00   0.50    0.60    -- -105.31 -45.00 150.00  114
 30  \w   -101.00 -58.00   0.50    0.60    -- -105.31  77.00  30.00   86
 31  \w    -82.00 -41.00   0.50    0.60    -- -105.31 148.00-139.50   82
 32  \w     41.00  70.00   0.50    0.60    --  105.31 -61.00  90.00   58
 33  \w     63.00 117.00   0.50    0.60    --  105.31-133.00  85.71  108
 34  \w     39.00  68.00   0.50    0.60    --  105.31 -61.00-150.00   58
 35  \w     94.00 176.00   0.50    0.60    --  105.31  45.00 -30.00  164
 36  \w     36.00 107.00   0.50    0.60    --  105.31-125.00 150.00  142
 37  \w     35.00  76.00   0.50    0.60    --  105.31-125.00-150.00   82
 38  \w     71.00  96.00   0.50    0.60    --  105.31-133.00 -32.78   50
 39  \w     59.00 101.00   0.50    0.60    --  105.31 -94.00  60.00   84
 40  \w    132.00 178.00   0.50    0.60    --  105.31  30.00-180.00   92
 41  \w     94.00 173.00   0.50    0.60    --  105.31  45.00   0.00  158
 42  \w     93.00 123.00   0.50    0.60    --  105.31  30.00-180.00   60
 43  \w     38.00 107.00   0.50    0.60    --  105.31-110.00  92.49  138
 44  \w     35.00  63.00   0.50    0.60    --  105.31 -61.00  60.00   56
 45  \w     53.00  78.00   0.50    0.15    --   47.13  52.00  47.00   50
 46  \w    -43.00 -18.00   0.50    0.15    --    8.00 132.00 107.23   50
 47  \w    -42.00 -15.00   0.50    0.15    --    8.00 129.00  39.69   54
 48  \w    -28.00  -3.00   0.50    0.15    --   12.00 111.00 172.22   50
 49  \w    -18.00   7.00   0.50    0.15    --   16.00 100.00 -26.36   50
 50  \w     -1.00  26.00   0.50    0.15    --   24.00  84.00-101.88   54
 51  \w      1.00  26.00   0.50    0.15    --   32.00  94.00 -33.39   50
 52  \w     16.00  41.00   0.50    0.15    --   44.00  89.00  81.67   50
 53  \w     15.00  40.00   0.50    0.15    --   44.00  90.00-142.38   50
 54  \w     15.00  40.00   0.50    0.15    --   44.00  90.00 -37.47   50
 55  \w     16.00  41.00   0.50    0.15    --   44.00  89.00  -0.54   50
 56  \w     14.00  39.00   0.50    0.15    --   44.00  92.00 154.90   50
 57  \w     11.00  37.00   0.50    0.15    --   47.13 -37.00 120.00   52
 58  \w     30.00  75.00   0.50    0.15    --   52.00  77.00-157.37   90
 59  \w     29.00  83.00   0.50    0.15    --   52.00  77.00 -79.45  108
 60  \w     80.00 106.00   0.50    0.15    --   52.00  77.00-157.37   52
 61  \w     35.00  63.00   0.50    0.15    --   56.00  74.00  12.65   56
 62  \w     34.00  74.00   0.50    0.15    --   56.00  76.00 -40.33   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0845632000
_diffrn_orient_matrix_UB_12      0.0270749000
_diffrn_orient_matrix_UB_13      0.0325383000
_diffrn_orient_matrix_UB_21      0.0115068000
_diffrn_orient_matrix_UB_22      0.1043825000
_diffrn_orient_matrix_UB_23      -0.0149453000
_diffrn_orient_matrix_UB_31      -0.0682265000
_diffrn_orient_matrix_UB_32      -0.0159627000
_diffrn_orient_matrix_UB_33      -0.0431368000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0777
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            93936
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.745
_diffrn_reflns_theta_min         3.520
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.742
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49543
_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            'metallic orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_description       prism
_exptl_crystal_F_000             2784
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 1,2-dichloroethane'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.871
_refine_diff_density_min         -1.234
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Flack x determined using 2221 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.017(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0286P)^2^+22.2399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0832
_reflns_Friedel_coverage         0.722
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                5492
_reflns_number_total             5721
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02823e2.cif
_cod_data_source_block           bsc-461
_cod_original_cell_volume        5475.58(10)
_cod_database_code               7708543
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H30 Cl N5 O Pt '
_shelx_estimated_absorpt_t_max   0.359
_shelx_estimated_absorpt_t_min   0.235
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C29(H29), C27(H27), C30(H30), C11(H11), C28(H28), C20(H20),
 C10(H10), C19(H19), C9(H9), C18(H18)
2.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C13(H13A,H13B,H13C), C23(H23A,H23B,H23C), C25(H25A,H25B,
 H25C), C14(H14A,H14B,H14C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              66123
_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 1.973
_oxdiff_exptl_absorpt_empirical_full_min 0.650