Cleavage of acyclic diaminocarbene ligands at an iridium(iii) center. Recognition of a new reactivity mode for carbene ligands.
Kinzhalov, Mikhail A.; Eremina, Anzhelika A.; Smirnov, Andrey S.; Suslonov, Vitalii V.; Kukushkin, Vadim Yu; Luzyanin, Konstantin V.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 7571–7582; doi:10.1039/c9dt01138b

data_7049779
_publ_section_title
;
 Cleavage of acyclic diaminocarbene ligands at an iridium(iii) center.
 Recognition of a new reactivity mode for carbene ligands.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7571
_journal_page_last               7582
_journal_paper_doi               10.1039/c9dt01138b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C36 H24 Cl2 Ir N4, C F3 O3 S'
_chemical_formula_sum            'C37 H24 Cl2 F3 Ir N4 O3 S'
_chemical_formula_weight         924.76
_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             2018-06-01
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
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2018-06-01 deposited with the CCDC.    2019-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.734(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1328(3)
_cell_length_b                   14.0956(4)
_cell_length_c                   22.0626(7)
_cell_measurement_reflns_used    5832
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.7360
_cell_measurement_theta_min      3.1580
_cell_volume                     3401.56(17)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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 0.979
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
  1 omega  -91.00  -58.00   1.0000   23.3900
omega____ theta____ kappa____ phi______ frames
    -      -22.4241 -171.0000  144.0000 33

  2 omega   32.00   82.00   1.0000   23.3900
omega____ theta____ kappa____ phi______ frames
    -       23.3616 -134.0000   27.0000 50

  3 omega   68.00   94.00   1.0000   23.3900
omega____ theta____ kappa____ phi______ frames
    -       23.3616  171.0000  158.0000 26

  4 omega  -45.00   80.00   1.0000   23.3900
omega____ theta____ kappa____ phi______ frames
    -       23.3616    0.0000  -90.0000 125
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0037775000
_diffrn_orient_matrix_UB_12      -0.0435897000
_diffrn_orient_matrix_UB_13      0.0155767000
_diffrn_orient_matrix_UB_21      0.0150197000
_diffrn_orient_matrix_UB_22      0.0236624000
_diffrn_orient_matrix_UB_23      0.0287687000
_diffrn_orient_matrix_UB_31      -0.0630294000
_diffrn_orient_matrix_UB_32      0.0083034000
_diffrn_orient_matrix_UB_33      -0.0003677000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15740
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.663
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.205
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94246
_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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_description       prism
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.525
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         7603
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0151P)^2^+8.8311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0728
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6519
_reflns_number_total             7603
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01138b2.cif
_cod_data_source_block           ea-82
_cod_depositor_comments
'Adding full bibliography for 7049777--7049781.cif.'
_cod_original_cell_volume        3401.55(17)
_cod_database_code               7049779
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Ir Cl2 S O3 F3 N4 C26'
_reflns_odcompleteness_completeness 96.28
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.51
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C15(H15), C22(H22), C28(H28), C13(H13), C35(H35), C36(H36),
 C32(H32), C26(H26), C4(H4), C25(H25), C29(H29), C14(H14), C21(H21), C16(H16),
 C2(H2), C11(H11), C5(H5), C20(H20), C8(H8), C10(H10), C3(H3), C33(H33), C9(H9)
;
_shelx_res_checksum              91088
_olex2_submission_special_instructions 'No special instructions were received'