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_1547864
_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         'C42 H38 Ir N4, C F3 O3 S'
_chemical_formula_sum            'C43 H38 F3 Ir N4 O3 S'
_chemical_formula_weight         940.03
_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     iterative
_audit_creation_date             2016-06-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-09-21 deposited with the CCDC.
2017-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.070(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7977(2)
_cell_length_b                   32.2237(6)
_cell_length_c                   12.8805(3)
_cell_measurement_reflns_used    16725
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.2058
_cell_measurement_theta_min      2.5232
_cell_volume                     3819.66(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.2096
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -96.00  -35.00   1.0000   38.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2468 -178.0000    0.0000 61

  2 omega   46.00   96.00   1.0000   38.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1843  178.0000  -60.0000 50

  3 omega   29.00   92.00   1.0000   38.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1843   38.0000  -60.0000 63

  4 omega  -52.00   21.00   1.0000   38.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1843  -19.0000    0.0000 73

  5 omega  -35.00   -9.00   1.0000   38.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2468   38.0000 -150.0000 26

  6 omega   23.00   49.00   1.0000   38.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2468   77.0000   90.0000 26

  7 omega    7.00   48.00   1.0000   38.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2468   38.0000 -150.0000 41

  8 omega  -31.00   -5.00   1.0000   38.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2468   77.0000   90.0000 26

  9 omega    3.00   88.00   1.0000   38.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1843   57.0000    0.0000 85

 10 omega    4.00   68.00   1.0000   38.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1843   57.0000 -120.0000 64
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0236129000
_diffrn_orient_matrix_UB_12      0.0165209000
_diffrn_orient_matrix_UB_13      0.0260983000
_diffrn_orient_matrix_UB_21      0.0710689000
_diffrn_orient_matrix_UB_22      0.0085080000
_diffrn_orient_matrix_UB_23      0.0177762000
_diffrn_orient_matrix_UB_31      -0.0181479000
_diffrn_orient_matrix_UB_32      0.0118240000
_diffrn_orient_matrix_UB_33      -0.0493528000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            39877
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.528
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.611
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_description       prism
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.794
_refine_diff_density_min         -1.985
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         8774
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0166P)^2^+6.1262P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0660
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7837
_reflns_number_total             8774
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cy02013a2.cif
_cod_data_source_block           103-5253-3718_ea15
_cod_original_cell_volume        3819.62(17)
_cod_database_code               1547864
_chemical_oxdiff_formula         'Ir N4 C32 H32'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50
_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:
 C4(H4), C6(H6), C14(H14), C16(H16), C21(H21), C22(H22), C23(H23), C24(H24),
 C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C34(H34), C35(H35), C36(H36),
  C39(H39), C40(H40), C41(H41), C42(H42)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 1456395223.25
_olex2_submission_special_instructions 'No special instructions were received'