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_7049780
_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 H25 Cl2 Ir N5, C1 F3 O3 S1'
_chemical_formula_sum            'C37 H25 Cl2 F3 Ir N5 O3 S'
_chemical_formula_weight         939.78
_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   geom
_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                 94.676(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3436(7)
_cell_length_b                   22.3709(10)
_cell_length_c                   13.9967(8)
_cell_measurement_reflns_used    6390
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.1780
_cell_measurement_theta_min      3.2670
_cell_volume                     3540.1(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -52.00   18.00   1.0000   69.5200
omega____ theta____ kappa____ phi______ frames
    -      -22.4241   77.0000 -180.0000 70

  2 omega   72.00   99.00   1.0000   69.5200
omega____ theta____ kappa____ phi______ frames
    -       23.3616  178.0000 -180.0000 27

  3 omega  -28.00   91.00   1.0000   69.5200
omega____ theta____ kappa____ phi______ frames
    -       23.3616    0.0000  -90.0000 119

  4 omega   64.00   99.00   1.0000   69.5200
omega____ theta____ kappa____ phi______ frames
    -       23.3616  178.0000  120.0000 35

  5 omega  -15.00   43.00   1.0000   69.5200
omega____ theta____ kappa____ phi______ frames
    -      -22.4241   19.0000  120.0000 58

  6 omega  -36.00  -14.00   1.0000   69.5200
omega____ theta____ kappa____ phi______ frames
    -      -22.4241  -90.0000   -4.0000 22
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0312061000
_diffrn_orient_matrix_UB_12      -0.0173553000
_diffrn_orient_matrix_UB_13      0.0361889000
_diffrn_orient_matrix_UB_21      0.0068402000
_diffrn_orient_matrix_UB_22      -0.0231792000
_diffrn_orient_matrix_UB_23      -0.0337028000
_diffrn_orient_matrix_UB_31      0.0539102000
_diffrn_orient_matrix_UB_32      0.0129433000
_diffrn_orient_matrix_UB_33      -0.0119623000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23108
_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         27.500
_diffrn_reflns_theta_min         2.875
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.043
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72490
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_description       prism
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.659
_refine_diff_density_min         -2.323
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         8132
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0714
_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^)+(0.0449P)^2^+51.2724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1589
_refine_ls_wR_factor_ref         0.1687
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6736
_reflns_number_total             8132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01138b2.cif
_cod_data_source_block           ea-100
_cod_depositor_comments
'Adding full bibliography for 7049777--7049781.cif.'
_cod_database_code               7049780
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Ir C36 H26 N5'
_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(O1C) = Uanis(O2C) = Uanis(O3C) = Uanis(C1C) = Uanis(F3C) = Uanis(F2C) =
Uanis(F1C) = Uanis(S1C)
Uanis(F2A) = Uanis(O2A) = Uanis(C1A) = Uanis(F3A) = Uanis(O3A) = Uanis(S1A) =
Uanis(F1A) = Uanis(O1A) = Uanis(F2B) = Uanis(O1B) = Uanis(C1B) = Uanis(F1B) =
Uanis(O3B) = Uanis(S1B) = Uanis(O2B) = Uanis(F3B)
3. Others
 Fixed Sof: F2A(0.4793) O2A(0.4793) C1A(0.4793) F3A(0.4793) O3A(0.4793)
 S1A(0.4793) F1A(0.4793) O1A(0.4793) F2B(0.1159) O1B(0.1159) C1B(0.1159)
 F1B(0.1159) O3B(0.1159) S1B(0.1159) F3B(0.1159) O2B(0.1159) S1C(0.4048)
 O1C(0.4048) O2C(0.4048) O3C(0.4048) C1C(0.4048) F3C(0.4048) F2C(0.4048)
 F1C(0.4048)
4.a Free rotating group:
 F2A(O2A,C1A,F3A,O3A,S1A,F1A,O1A), F2B(O1B,C1B,F1B,O3B,S1B,F3B,O2B), S1C(O1C,
 O2C,O3C,C1C,F3C,F2C,F1C)
4.b Aromatic/amide H refined with riding coordinates:
 C13(H13), N4(H4), C36(H36), C21(H21), C3(H3), C15(H15), C19(H19), C11(H11),
 C25(H25), C32(H32), C35(H35), C5(H5), C8(H8), C10(H10), C33(H33), C9(H9),
 C20(H20), C22(H22), C2(H2), C4(H4A), C26(H26), C29(H29), C28(H28)
4.c X=CH2 refined with riding coordinates:
 N3(H3A,H3B)
;
_shelx_res_checksum              80172
_olex2_submission_special_instructions 'No special instructions were received'