Chelating N-heterocyclic carbene-carboranes offer flexible ligand coordination to Ir(III), Rh(III) and Ru(II): effect of ligand cyclometallation in catalytic transfer hydrogenation.
Holmes, Jordan; Pask, Christopher M.; Willans, Charlotte E.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 15818–15827; doi:10.1039/c6dt02079h

data_7040001
_publ_section_title
;
 Chelating N-heterocyclic carbene-carboranes offer flexible ligand
 coordination to Ir(III), Rh(III) and Ru(II): effect of ligand
 cyclometallation in catalytic transfer hydrogenation.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15818
_journal_page_last               15827
_journal_paper_doi               10.1039/c6dt02079h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C18 H34 B10 Br0.7 Cl0.3 Ir N2'
_chemical_formula_sum            'C18 H34 B10 Br0.7 Cl0.3 Ir N2'
_chemical_formula_weight         645.34
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-06 deposited with the CCDC.
2016-07-11 downloaded from the CCDC.
;
_cell_angle_alpha                95.466(4)
_cell_angle_beta                 93.488(4)
_cell_angle_gamma                106.566(4)
_cell_formula_units_Z            2
_cell_length_a                   8.0693(4)
_cell_length_b                   10.6249(4)
_cell_length_c                   14.7046(7)
_cell_measurement_reflns_used    7034
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      30.4630
_cell_measurement_theta_min      3.6170
_cell_volume                     1197.76(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measurement_details
;
  1 omega  -33.00   56.00   1.0000   11.5700
omega____ theta____ kappa____ phi______ frames
    -      -13.8884   37.0000   60.0000 89

  2 omega   -2.00   25.00   1.0000   11.5700
omega____ theta____ kappa____ phi______ frames
    -       13.1072   37.0000  150.0000 27

  3 omega  -13.00   82.00   1.0000   11.5700
omega____ theta____ kappa____ phi______ frames
    -       13.1072   63.0000  173.0000 95

  4 omega  -52.00  -25.00   1.0000   11.5700
omega____ theta____ kappa____ phi______ frames
    -       13.1072  -57.0000  120.0000 27

  5 omega    1.00   50.00   1.0000   11.5700
omega____ theta____ kappa____ phi______ frames
    -       13.1072   57.0000  -90.0000 49

  6 omega   -3.00   22.00   1.0000   11.5700
omega____ theta____ kappa____ phi______ frames
    -       13.1072  -37.0000 -150.0000 25

  7 omega  -80.00   11.00   1.0000   11.5700
omega____ theta____ kappa____ phi______ frames
    -      -13.8884  -62.0000  -94.0887 91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0416135000
_diffrn_orient_matrix_UB_12      0.0652521000
_diffrn_orient_matrix_UB_13      -0.0093150000
_diffrn_orient_matrix_UB_21      0.0678213000
_diffrn_orient_matrix_UB_22      0.0050886000
_diffrn_orient_matrix_UB_23      0.0344411000
_diffrn_orient_matrix_UB_31      0.0463786000
_diffrn_orient_matrix_UB_32      -0.0252092000
_diffrn_orient_matrix_UB_33      -0.0330945000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0766
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14195
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.336
_diffrn_reflns_theta_min         3.141
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.786
_exptl_absorpt_correction_T_max  0.650
_exptl_absorpt_correction_T_min  0.283
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_description       irregular
_exptl_crystal_F_000             625
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.067
_refine_diff_density_min         -1.785
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         6744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0491P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1005
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5699
_reflns_number_total             6744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02079h2.cif
_cod_data_source_block           7b
_cod_depositor_comments
'Adding full bibliography for 7039998--7040005.cif.'
_cod_original_formula_sum        'C18 H34 B10 Br0.70 Cl0.30 Ir N2'
_cod_database_code               7040001
_chemical_oxdiff_formula         'C36 H68 B20 Br2 Ir2 N4'
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Br1, Cl1}
3. Uiso/Uaniso restraints and constraints
Uanis(Br1) = Uanis(Cl1)
4. Others
 Fixed Sof: Br1(0.7) Cl1(0.3)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3A,H3B)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5A), C6(H6)
5.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
5.d Boron cage BH refined with riding coordinates:
 B4(H4), B5(H5), B3(H3), B8(H8), B7(H7), B10(H10), B11(H11), B6(H6A), B9(H9),
 B12(H12)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'