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_7708541
_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         'C27 H30 Cl N5 O Pt'
_chemical_formula_sum            'C27 H30 Cl N5 O Pt'
_chemical_formula_weight         671.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-04-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-10 deposited with the CCDC.	2021-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.3680(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.55950(10)
_cell_length_b                   29.0139(4)
_cell_length_c                   11.9767(2)
_cell_measurement_reflns_used    7392
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.2220
_cell_measurement_theta_min      3.0280
_cell_volume                     2575.32(7)
_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 (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 0.997
_diffrn_measured_fraction_theta_max 0.992
_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    -82.00 -44.00   0.50    0.20    --  -38.82 120.00 -63.00   76
  2  \w    -78.00 -26.00   0.50    0.20    --  -38.82 155.00  94.00  104
  3  \w     23.00  83.00   0.50    0.20    --   38.82-155.00  55.00  120
  4  \w     20.00  45.00   0.50    0.20    --   38.82-120.00-147.00   50
  5  \w     85.00 115.00   0.50    0.71    --  100.00-155.00  55.00   60
  6  \w     48.00  74.00   0.50    0.71    --  100.00-120.00-147.00   52
  7  \w     95.00 134.00   0.50    0.71    --  100.00 120.00 -63.00   78
  8  \w    -56.00 -23.00   0.50    0.20    --  -38.82  54.00 -60.00   66
  9  \w    -19.00  14.00   0.50    0.20    --  -38.82  54.00 -60.00   66
 10  \w    -63.00 -27.00   0.50    0.20    --  -38.82  77.00-120.00   72
 11  \w     -3.00  27.00   0.50    0.20    --  -38.82  77.00-120.00   60
 12  \w      3.00  29.00   0.50    0.20    --  -38.82  32.00  90.00   52
 13  \w    -44.00 -16.00   0.50    0.20    --  -38.82  32.00  90.00   56
 14  \w    -52.00 -15.00   0.50    0.20    --  -38.82  32.00-180.00   74
 15  \w   -105.00 -35.00   0.50    0.20    --  -38.82 -43.00-180.00  140
 16  \w     21.00  91.00   0.50    0.20    --   38.82-138.00 -30.00  140
 17  \w     33.00 105.00   0.50    0.20    --   38.82  32.00 -60.00  144
 18  \w     70.00 104.00   0.50    0.20    --   38.82  43.00 150.00   68
 19  \w     26.00  56.00   0.50    0.20    --   38.82  32.00  30.00   60
 20  \w     33.00  62.00   0.50    0.20    --   38.82  43.00 150.00   58
 21  \w     26.00  57.00   0.50    0.71    --  100.00 -93.00-150.00   62
 22  \w     57.00  83.00   0.50    0.71    --  100.00 178.00   0.00   52
 23  \w     31.00 114.00   0.50    0.71    --  100.00 -30.00-180.00  166
 24  \w     86.00 113.00   0.50    0.71    --  100.00 -77.00-120.00   54
 25  \w     93.00 119.00   0.50    0.71    --  100.00  77.00 -60.00   52
 26  \w     31.00 107.00   0.50    0.71    --  100.00-111.00  30.00  152
 27  \w    101.00 140.00   0.50    0.71    --  100.00 111.00 -90.00   78
 28  \w     37.00  71.00   0.50    0.71    --  100.00-111.00 -30.00   68
 29  \w     93.00 118.00   0.50    0.71    --  100.00-133.00-180.00   50
 30  \w     80.00 157.00   0.50    0.71    --  100.00  53.00 120.00  154
 31  \w     35.00  62.00   0.50    0.71    --  100.00 -77.00-120.00   54
 32  \w     36.00  94.00   0.50    0.71    --  100.00-133.00 -30.00  116
 33  \w     47.00  77.00   0.50    0.71    --  100.00-133.00-180.00   60
 34  \w     84.00 109.00   0.50    0.71    --  100.00  77.00-180.00   50
 35  \w     88.00 157.00   0.50    0.71    --  100.00  37.00  90.00  138
 36  \w    100.00 139.00   0.50    0.71    --  100.00 178.00   0.00   78
 37  \w     57.00 105.00   0.50    0.71    --  100.00 -93.00 150.00   96
 38  \w     71.00 106.00   0.50    0.71    --  100.00-111.00-120.00   70
 39  \w     85.00 152.00   0.50    0.71    --  100.00  93.00 120.00  134
 40  \w    108.00 153.00   0.50    0.71    --  100.00  77.00-120.00   90
 41  \w     88.00 113.00   0.50    0.71    --  100.00-133.00   0.00   50
 42  \w     54.00  72.50   0.50    0.71    --  100.00 -61.00-180.00   37
;
_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      -0.0357665000
_diffrn_orient_matrix_UB_12      0.0140266000
_diffrn_orient_matrix_UB_13      0.1176207000
_diffrn_orient_matrix_UB_21      0.0343847000
_diffrn_orient_matrix_UB_22      0.0508362000
_diffrn_orient_matrix_UB_23      -0.0262335000
_diffrn_orient_matrix_UB_31      -0.2018476000
_diffrn_orient_matrix_UB_32      0.0061524000
_diffrn_orient_matrix_UB_33      -0.0518990000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14904
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.424
_diffrn_reflns_theta_min         3.046
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.378
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83463
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_description       prism
_exptl_crystal_F_000             1320
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 1,2-dichloroethane'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.159
_refine_diff_density_min         -1.274
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         4890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+0.9747P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0717
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4399
_reflns_number_total             4890
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02823e2.cif
_cod_data_source_block           bsc-450
_cod_database_code               7708541
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C27 H30 Cl N5 O Pt '
_shelx_estimated_absorpt_t_max   0.396
_shelx_estimated_absorpt_t_min   0.209
_reflns_odcompleteness_completeness 98.18
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     70.93
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C18(H18), C11(H11), C1(H1), C4(H4), C9(H9), C19(H19), C20(H20),
 C10(H10)
1.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              32249
_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 1.389
_oxdiff_exptl_absorpt_empirical_full_min 0.782