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_7040004
_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         'C19 H37 B10 Cl2 Ir N2'
_chemical_formula_sum            'C19 H37 B10 Cl2 Ir N2'
_chemical_formula_weight         664.70
_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     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                90
_cell_angle_beta                 92.623(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3551(4)
_cell_length_b                   15.9601(8)
_cell_length_c                   23.705(2)
_cell_measurement_reflns_used    3172
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      72.0910
_cell_measurement_theta_min      3.3970
_cell_volume                     2779.8(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
  1 omega -114.00  -50.00   1.0000    4.7500
omega____ theta____ kappa____ phi______ frames
    -      -40.7934  -37.0000 -120.0000 64

  2 omega  -64.00   14.00   1.0000    4.7500
omega____ theta____ kappa____ phi______ frames
    -      -40.7934   57.0000   60.0000 78

  3 omega   26.00   76.00   1.0000    4.7500
omega____ theta____ kappa____ phi______ frames
    -       40.7934   37.0000  150.0000 50

  4 omega   19.00   61.00   1.0000    4.7500
omega____ theta____ kappa____ phi______ frames
    -       40.7934   37.0000    0.0000 42

  5 omega   36.00  112.00   1.0000   21.2500
omega____ theta____ kappa____ phi______ frames
    -      104.4397  -61.0000 -180.0000 76

  6 omega  127.00  174.00   1.0000   21.2500
omega____ theta____ kappa____ phi______ frames
    -      104.4397   61.0000  -30.0000 47

  7 omega   37.00  134.00   1.0000   21.2500
omega____ theta____ kappa____ phi______ frames
    -      104.4397  -65.0000  -30.0069 97

  8 omega   79.00  144.00   1.0000   21.2500
omega____ theta____ kappa____ phi______ frames
    -      104.4397   45.0000   90.0000 65

  9 omega   80.00  174.00   1.0000   21.2500
omega____ theta____ kappa____ phi______ frames
    -      104.4397   61.0000  120.0000 94

 10 omega   51.00   85.00   1.0000   21.2500
omega____ theta____ kappa____ phi______ frames
    -      104.4397  -45.0000  -30.0000 34
;
_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      -0.0007845000
_diffrn_orient_matrix_UB_12      -0.0683336000
_diffrn_orient_matrix_UB_13      0.0458751000
_diffrn_orient_matrix_UB_21      0.1159010000
_diffrn_orient_matrix_UB_22      -0.0568722000
_diffrn_orient_matrix_UB_23      -0.0366558000
_diffrn_orient_matrix_UB_31      0.1748427000
_diffrn_orient_matrix_UB_32      0.0374139000
_diffrn_orient_matrix_UB_33      0.0280407000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0823
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            6983
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.033
_diffrn_reflns_theta_min         3.339
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.134
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.874
_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    1.588
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.911
_refine_diff_density_min         -1.882
_refine_diff_density_rms         0.245
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         6983
_refine_ls_number_restraints     447
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1095
_refine_ls_R_factor_gt           0.0739
_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^)+(0.0272P)^2^+107.2053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1894
_refine_ls_wR_factor_ref         0.2022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4560
_reflns_number_total             6983
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02079h2.cif
_cod_data_source_block           2c
_cod_depositor_comments
'Adding full bibliography for 7039998--7040005.cif.'
_cod_database_code               7040004
_chemical_oxdiff_formula         C20H30B10N2IrCl2
_diffrn_oxdiff_twin_integration_method simultaneous
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6695(18) 0.3305(18)
2. 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
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C9(H9A,H9B,H9C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
4.d Boron cage BH refined with riding coordinates:
 B3(H3), B4(H4), B5(H5), B6(H6A), B7(H7A), B8(H8), B9(H9), B10(H10), B11(H11),
 B12(H12)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'