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_7049778
_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 H30 Cl2 Ir N6, C F3 O3 S, C H Cl3'
_chemical_formula_sum            'C38 H31 Cl5 F3 Ir N6 O3 S'
_chemical_formula_weight         1078.20
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-05-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-01 deposited with the CCDC.    2019-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.392(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0467(8)
_cell_length_b                   30.1504(13)
_cell_length_c                   10.5444(5)
_cell_measurement_reflns_used    6989
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.5580
_cell_measurement_theta_min      2.8150
_cell_volume                     4079.7(4)
_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    '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 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -99.00  -36.00   1.0000   36.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4241  178.0000  150.0000 63

  2 omega   46.00   86.00   1.0000   36.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616  178.0000  -90.0000 40

  3 omega  -11.00   93.00   1.0000   36.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616   19.0000   60.0000 104

  4 omega   55.00   93.00   1.0000   36.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616   77.0000   60.0000 38

  5 omega  -95.00  -89.00   1.0000   36.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4241  -19.0000 -150.0000 6
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0447739000
_diffrn_orient_matrix_UB_12      -0.0148886000
_diffrn_orient_matrix_UB_13      -0.0159772000
_diffrn_orient_matrix_UB_21      -0.0182732000
_diffrn_orient_matrix_UB_22      0.0073799000
_diffrn_orient_matrix_UB_23      -0.0520314000
_diffrn_orient_matrix_UB_31      0.0484237000
_diffrn_orient_matrix_UB_32      0.0166739000
_diffrn_orient_matrix_UB_33      0.0091766000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_unetI/netI     0.1011
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19969
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.821
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.711
_exptl_absorpt_correction_T_max  0.587
_exptl_absorpt_correction_T_min  0.293
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_description       prism
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.5167
_exptl_crystal_size_mid          0.3092
_exptl_crystal_size_min          0.1857
_refine_diff_density_max         2.446
_refine_diff_density_min         -3.115
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.312
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         9344
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.312
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0762
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+22.7804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1319
_refine_ls_wR_factor_ref         0.1368
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8060
_reflns_number_total             9344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01138b2.cif
_cod_data_source_block           ea-102
_cod_depositor_comments
'Adding full bibliography for 7049777--7049781.cif.'
_cod_database_code               7049778
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Ir Cl5 S F3 O3 C38 N6'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.51
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C24) = Uanis(C27)
Uanis(C2S) = Uanis(C1S)
Uanis(C23) = Uanis(N3)
Uanis(Cl1) = Uanis(C27) = Uanis(C24)
Uanis(C12) = Uanis(N2)
Uanis(C1) = Uanis(N1)
Uanis(C31) = Uanis(N6)
Uanis(C18) = Uanis(C17)
3. Others
 Fixed Sof: Cl1S(0.5) Cl2S(0.5) Cl4S(0.5) Cl5S(0.5) C1S(0.5) H1S(0.5) C2S(0.5)
 H2S(0.5)
4.a Riding coordinates:
 N4(H4), N3(H3A,H3B), N5(H5A,H5B), N6(H6)
4.b Ternary CH refined with riding coordinates:
 C1S(H1S), C2S(H2S)
4.c Aromatic/amide H refined with riding coordinates:
 C29(H29), C28(H28), C26(H26), C25(H25), C36(H36), C35(H35), C33(H33),
 C32(H32), C11(H11), C10(H10), C9(H9), C8(H8), C5(H5), C4(H4A), C3(H3), C2(H2),
 C13(H13), C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22)
;
_shelx_res_checksum              23174
_olex2_date_sample_data_collection 1476866297.99
_olex2_submission_special_instructions 'No special instructions were received'