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_7708542
_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         'C26 H28 Cl N5 O Pt, 0.356(H2 O)'
_chemical_formula_sum            'C26 H28.71 Cl N5 O1.36 Pt'
_chemical_formula_weight         663.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-10-04 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.9090(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.0902(3)
_cell_length_b                   12.0056(2)
_cell_length_c                   22.7916(3)
_cell_measurement_reflns_used    14300
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.2550
_cell_measurement_theta_min      2.7410
_cell_volume                     5111.16(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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   -106.00 -26.00   0.50    0.52    --  -38.82 -33.00  49.00  160
  2  \w     27.00 107.00   0.50    0.52    --   38.82  33.00-151.00  160
  3  \w     16.00  48.00   0.50    0.52    --   38.82 -33.00  49.00   64
  4  \w    130.00 156.00   0.50    2.08    --  100.00  33.00-151.00   52
  5  \w     97.00 126.00   0.50    2.08    --  100.00  33.00-151.00   58
  6  \w     32.00 112.00   0.50    2.08    --  100.00 -33.00  49.00  160
  7  \w    -90.00 -50.00   0.50    0.52    --  -38.82 138.00 -60.00   80
  8  \w    -45.00 -15.00   0.50    0.52    --  -38.82 138.00 -60.00   60
  9  \w    -59.00 -21.00   0.50    0.52    --  -38.82 -21.00 -90.00   76
 10  \w    -60.00 -25.00   0.50    0.52    --  -38.82 -32.00-150.00   70
 11  \w    -29.00  12.00   0.50    0.52    --  -38.82  65.00 -30.00   82
 12  \w    -60.00 -35.00   0.50    0.52    --  -38.82  65.00 -30.00   50
 13  \w   -108.00 -64.00   0.50    0.52    --  -38.82 -21.00 -90.00   88
 14  \w    -44.00 -19.00   0.50    0.52    --  -38.82  33.00-151.00   50
 15  \w     73.00 101.00   0.50    0.52    --   38.82  54.00-120.00   56
 16  \w     19.00  64.00   0.50    0.52    --   38.82  54.00-120.00   90
 17  \w    -17.00   8.00   0.50    0.52    --   38.82 -43.00 -30.00   50
 18  \w     32.00 103.00   0.50    0.52    --   38.82  43.00 -30.00  142
 19  \w     36.00  61.00   0.50    0.52    --   38.82  32.00   0.00   50
 20  \w     83.00 108.00   0.50    0.52    --   38.82  32.00   0.00   50
 21  \w     14.00  46.00   0.50    0.52    --   38.82 -43.00 -30.00   64
 22  \w    101.00 141.00   0.50    2.08    --  100.00  93.00 -90.00   80
 23  \w     65.00 117.00   0.50    2.08    --  100.00 -45.00-150.00  104
 24  \w     36.00 115.00   0.50    2.08    --  100.00 -61.00  90.00  158
 25  \w     36.00  61.00   0.50    2.08    --  100.00 -45.00-150.00   50
 26  \w     73.00  99.00   0.50    2.08    --  100.00  15.00 120.00   52
 27  \w     76.00 114.00   0.50    2.08    --  100.00 -30.00-120.00   76
 28  \w     26.00 126.00   0.50    2.08    --  100.00 -15.00-180.00  200
 29  \w     35.00  72.00   0.50    2.08    --  100.00 -30.00-120.00   74
 30  \w    103.00 156.00   0.50    2.08    --  100.00  30.00-180.00  106
 31  \w     38.00 122.00   0.50    2.08    --  100.00 -77.00-150.00  168
 32  \w     61.00 118.00   0.50    2.08    --  100.00 -45.00 -90.00  114
 33  \w     96.00 153.00   0.50    2.08    --  100.00  45.00  90.00  114
 34  \w     42.00  85.00   0.50    2.08    --  100.00 -45.00-180.00   86
 35  \w     60.00 104.00   0.50    2.08    --  100.00-111.00   0.00   88
 36  \w     79.00 105.00   0.50    2.08    --  100.00  15.00  30.00   52
 37  \w     42.00  72.00   0.50    2.08    --  100.00-111.00 -60.00   60
 38  \w    106.00 154.00   0.50    2.08    --  100.00  45.00-120.00   96
 39  \w    119.00 144.00   0.50    2.08    --  100.00  15.00  30.00   50
 40  \w     88.00 113.00   0.50    2.08    --  100.00 -61.00-180.00   50
 41  \w    -49.00 -23.00   0.50    0.52    --  -38.82  33.00-151.00   52
 42  \w    -41.00 -15.00   0.50    0.52    --  -38.82 -65.00 -90.00   52
 43  \w    -55.00 -29.00   0.50    0.52    --  -38.82 -65.00 -60.00   52
 44  \w    -48.00 -23.00   0.50    0.52    --  -38.82 -54.00 -60.00   50
 45  \w    -36.00  33.00   0.50    0.52    --  -38.82  21.00   0.00  138
 46  \w     17.00  42.00   0.50    0.52    --   38.82  65.00 -60.00   50
 47  \w     23.00  49.00   0.50    0.52    --   38.82  65.00 -30.00   52
 48  \w    -27.00  -1.00   0.50    0.52    --   38.82 -89.00  30.00   52
 49  \w     30.00  70.00   0.50    0.52    --   38.82 -89.00  30.00   80
 50  \w     16.00  55.00   0.50    0.52    --   38.82  65.00  30.00   78
 51  \w     17.00  55.00   0.50    0.52    --   38.82  65.00   0.00   76
 52  \w     79.00 104.00   0.50    0.52    --   38.82  65.00   0.00   50
 53  \w    -32.00  18.00   0.50    0.52    --   38.82 -21.00 -90.00  100
 54  \w     29.00  55.00   0.50    0.52    --   38.82  32.00 -60.00   52
 55  \w    119.00 150.00   0.50    2.08    --  100.00  69.00 -60.00   62
 56  \w     29.00  54.00   0.50    2.08    --  100.00 -22.00 120.00   50
 57  \w     76.00 102.00   0.50    2.08    --  100.00  69.00 -60.00   52
 58  \w     80.00 114.00   0.50    2.08    --  100.00  53.00   0.00   68
 59  \w     80.00 107.00   0.50    2.08    --  100.00  53.00 -30.00   54
 60  \w     78.00 108.00   0.50    2.08    --  100.00  61.00-120.00   60
 61  \w     80.00 137.00   0.50    2.08    --  100.00  53.00 -90.00  114
 62  \w     86.00 157.00   0.50    2.08    --  100.00  45.00 -30.00  142
 63  \w    115.00 145.00   0.50    2.08    --  100.00  45.00   0.00   60
 64  \w     92.00 117.00   0.50    2.08    --  100.00  61.00 120.00   50
 65  \w    122.00 155.00   0.50    2.08    --  100.00  61.00 120.00   66
 66  \w     78.00 104.00   0.50    2.08    --  100.00  61.00 -30.00   52
 67  \w     78.00 104.00   0.50    2.08    --  100.00  61.00   0.00   52
 68  \w     83.00 111.00   0.50    2.08    --  100.00  77.00   0.00   56
 69  \w     94.00 119.00   0.50    2.08    --  100.00 -22.00 120.00   50
 70  \w     78.00 155.00   0.50    2.08    --  100.00  61.00 -90.00  154
 71  \w     81.00 123.00   0.50    2.08    --  100.00  53.00-120.00   84
 72  \w     85.00 111.00   0.50    2.08    --  100.00  45.00 -90.00   52
 73  \w     83.00 109.00   0.50    2.08    --  100.00  77.00  90.00   52
 74  \w    131.00 157.00   0.50    2.08    --  100.00  37.00  60.00   52
 75  \w     76.00 101.00   0.50    2.08    --  100.00  69.00 -30.00   50
 76  \w     83.00 108.00   0.50    2.08    --  100.00  77.00 -30.00   50
 77  \w    128.00 155.00   0.50    2.08    --  100.00  69.00 -79.93   54
 78  \w     76.00 101.00   0.50    2.08    --  100.00  69.00 -79.93   50
 79  \w     80.00 118.00   0.50    2.08    --  100.00  67.00 -75.32   76
 80  \w     76.00 102.00   0.50    2.08    --  100.00  69.00 -90.00   52
 81  \w    132.00 157.00   0.50    2.08    --  100.00  77.00  90.00   50
 82  \w    117.00 144.00   0.50    2.08    --  100.00  69.00-120.00   54
 83  \w     85.00 111.00   0.50    2.08    --  100.00  45.00   0.00   52
 84  \w    112.00 138.00   0.50    2.08    --  100.00  61.00  30.00   52
 85  \w     78.00 103.00   0.50    2.08    --  100.00  61.00  30.00   50
 86  \w     76.00 102.00   0.50    2.08    --  100.00  69.00-120.00   52
 87  \w     76.00 133.00   0.50    2.08    --  100.00  69.00   0.00  114
 88  \w    129.00 154.00   0.50    2.08    --  100.00  53.00-180.00   50
 89  \w     83.00 108.00   0.50    2.08    --  100.00-111.00 120.00   50
 90  \w     77.00 102.00   0.50    2.08    --  100.00  65.00  29.76   50
 91  \w    132.00 157.00   0.50    2.08    --  100.00  61.00 -60.00   50
 92  \w     78.00 104.00   0.50    2.08    --  100.00  61.00 -60.00   52
;
_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      0.0441138000
_diffrn_orient_matrix_UB_12      0.0340711000
_diffrn_orient_matrix_UB_13      -0.0466023000
_diffrn_orient_matrix_UB_21      -0.0605810000
_diffrn_orient_matrix_UB_22      -0.0415304000
_diffrn_orient_matrix_UB_23      -0.0507811000
_diffrn_orient_matrix_UB_31      -0.0344989000
_diffrn_orient_matrix_UB_32      0.1165094000
_diffrn_orient_matrix_UB_33      -0.0045000000
_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  0.0414
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28786
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.987
_diffrn_reflns_theta_min         3.964
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.469
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.71a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_description       prism
_exptl_crystal_F_000             2604
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 1,2-dichloroethane'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.842
_refine_diff_density_min         -2.730
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         4833
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+14.6490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4360
_reflns_number_total             4833
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02823e2.cif
_cod_data_source_block           bsc-355
_cod_database_code               7708542
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C28 H28 Cl N5 O Pt '
_shelx_estimated_absorpt_t_max   0.365
_shelx_estimated_absorpt_t_min   0.246
_reflns_odcompleteness_completeness 98.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     70.93
_olex2_refinement_description
;
1. Others
 Sof(O1S)=Sof(H1SA)=Sof(H1SB)=FVAR(1)
2.a Riding coordinates:
 O1S(H1SA,H1SB)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C11(H11), C10(H10), C20(H20),
 C18(H18), C19(H19)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C26(H26A,H26B,H26C), C14(H14A,H14B,H14C), C22(H22A,H22B,
 H22C), C25(H25A,H25B,H25C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              59429
_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 2.027
_oxdiff_exptl_absorpt_empirical_full_min 0.515