Iridium(III)-catalysed cross-linking of polysiloxanes leading to the thermally resistant luminescent silicone rubbers
Islamova, Regina M. M; Dobrynin, Mikhail V.; Vlasov, Andrey V.; Eremina, Anzhelika A.; Kinzhalov, Mikhail A.; Kolesnikov, Ilya E.; Zolotarev, Andrei; Masloborodova, Eleonora A.; Luzyanin, Konstantin; Catalysis Science & Technology  (2017) –; doi:10.1039/C7CY02013A

data_1547865
_publ_section_title
;
 Iridium(III)-catalysed cross-linking of polysiloxanes leading to the
 thermally resistant luminescent silicone rubbers
;
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_paper_doi               10.1039/C7CY02013A
_journal_year                    2017
_chemical_formula_moiety         'C31 H25 Cl Ir N3, C H2 Cl2'
_chemical_formula_sum            'C32 H27 Cl3 Ir N3'
_chemical_formula_weight         752.12
_chemical_name_systematic
;
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-27
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2016-10-06 deposited with the CCDC.
2017-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 112.277(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.7446(4)
_cell_length_b                   8.57762(18)
_cell_length_c                   21.5557(5)
_cell_measurement_reflns_used    13222
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.9890
_cell_measurement_theta_min      2.8840
_cell_volume                     2864.94(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 10.3829
_diffrn_measured_fraction_theta_full 0.9907
_diffrn_measured_fraction_theta_max 0.9907
_diffrn_measurement_details
;
  1 omega  -40.00   30.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787   38.0000 -120.0000 70

  2 omega  -36.00   25.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787   38.0000  120.0000 61

  3 omega -130.00  -88.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787 -178.0000    0.0000 42

  4 omega  -41.00   30.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787   38.0000 -180.0000 71

  5 omega  105.00  130.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3787  178.0000   90.0000 25

  6 omega   88.00  169.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000  -60.0000 81

  7 omega   29.00   54.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000 -120.0000 25

  8 omega   59.00   89.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -60.0000 30

  9 omega  113.00  146.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000   60.0000 33

 10 omega   73.00  103.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000  150.0000 30

 11 omega   54.00  135.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   15.0000  120.0000 81

 12 omega   35.00   61.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  120.0000 26

 13 omega   38.00   96.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000 -180.0000 58

 14 omega   35.00   74.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000 -150.0000 39

 15 omega   57.00   90.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000    0.0000 33

 16 omega   50.00   94.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  150.0000 44

 17 omega   86.00  131.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  120.0000 45

 18 omega   39.00   86.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  120.0000 47

 19 omega  122.00  177.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000  -30.0000 55

 20 omega  116.00  144.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000  120.0000 28

 21 omega   90.00  115.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000 -150.0000 25

 22 omega   85.00  111.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000 -180.0000 26

 23 omega   37.00   83.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000  -90.0000 46

 24 omega   84.00  114.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000   30.0000 30

 25 omega   99.00  126.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000  -60.0000 27

 26 omega   83.00  134.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000 -180.0000 51

 27 omega   89.00  114.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000 -180.0000 25

 28 omega  132.00  177.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000 -180.0000 45

 29 omega   83.00  115.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000  120.0000 32

 30 omega   35.00   60.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -90.0000 25

 31 omega   66.00   92.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000   90.0000 26

 32 omega   54.00   82.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000 -150.0000 28

 33 omega   90.00  115.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000 -120.0000 25

 34 omega   60.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000  -30.0000 44

 35 omega  112.00  146.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000  150.0000 34

 36 omega   82.00  108.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  178.0000  -30.0000 26

 37 omega   57.00   82.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -77.0000  150.0000 25

 38 omega  -60.00  -14.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -77.0000  120.0000 46

 39 omega  -51.00  -25.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -38.0000   60.0000 26

 40 omega  -81.00  -33.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -38.0000  -90.0000 48

 41 omega  -51.00  -25.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -57.0000   60.0000 26

 42 omega  -70.00   -6.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -26.0000  150.7207 64

 43 omega  -65.00   -8.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -77.0000 -180.0000 57

 44 omega  -54.00  -24.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -77.0000   90.0000 30

 45 omega  -79.00  -54.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -57.0000  120.0000 25

 46 omega  -51.00  -26.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -57.0000    0.0000 25

 47 omega  -43.00  -14.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -57.0000  -90.0000 29

 48 omega  -37.00  -11.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787   57.0000  -30.0000 26

 49 omega  -71.00  -11.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -57.0000  -60.0000 60

 50 omega  -52.00  -26.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -77.0000 -150.0000 26

 51 omega  -57.00  -18.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -57.0000 -150.0000 39

 52 omega   80.00  106.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   72.0000  147.4109 26

 53 omega  140.00  165.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   66.0000 -100.0253 25

 54 omega  142.00  168.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   51.0000 -158.4443 26

 55 omega   82.00  108.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   66.0000 -100.0253 26

 56 omega   81.00  107.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   68.0000 -147.2346 26

 57 omega   84.00  109.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   51.0000 -158.4443 25

 58 omega   82.00  108.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   63.0000 -146.8273 26

 59 omega   83.00  109.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000 -120.0000 26

 60 omega   79.00  108.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000 -150.0000 29

 61 omega   79.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000 -120.0000 25

 62 omega   83.00  134.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000 -150.0000 51

 63 omega   83.00  109.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  150.0000 26

 64 omega  123.00  149.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  150.0000 26

 65 omega   78.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -15.0000  -60.0000 26

 66 omega   79.00  104.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000 -180.0000 25

 67 omega   83.00  110.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  -90.0000 27

 68 omega   84.00  110.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000 -180.0000 26
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0080618000
_diffrn_orient_matrix_UB_12      -0.1782357000
_diffrn_orient_matrix_UB_13      0.0094406000
_diffrn_orient_matrix_UB_21      -0.0900877000
_diffrn_orient_matrix_UB_22      -0.0057535000
_diffrn_orient_matrix_UB_23      0.0036052000
_diffrn_orient_matrix_UB_31      -0.0413225000
_diffrn_orient_matrix_UB_32      -0.0223638000
_diffrn_orient_matrix_UB_33      -0.0765492000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            37122
_diffrn_reflns_theta_full        72.48
_diffrn_reflns_theta_max         72.48
_diffrn_reflns_theta_min         2.87
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.802
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.312
_refine_diff_density_min         -1.420
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         5634
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+8.2494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1114
_reflns_number_gt                4867
_reflns_number_total             5634
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cy02013a2.cif
_cod_data_source_block           km857
_cod_original_cell_volume        2864.94(12)
_cod_database_code               1547865
_chemical_oxdiff_formula         'Ir1 N3 Cl1 C15 h20'
_reflns_odcompleteness_completeness 93.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     80.95