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_7040003
_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         'C21 H39 B10 Ir N2'
_chemical_formula_sum            'C21 H39 B10 Ir N2'
_chemical_formula_weight         619.84
_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
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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                 110.343(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1388(4)
_cell_length_b                   18.2073(6)
_cell_length_c                   13.5279(5)
_cell_measurement_reflns_used    9590
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      30.9680
_cell_measurement_theta_min      3.7110
_cell_volume                     2572.44(17)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_computing_data_reduction
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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)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_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 0.897
_diffrn_measurement_details
;
  1 omega   -6.00   45.00   1.0000   95.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509   37.0000    0.0000 51

  2 omega  -12.00   81.00   1.0000   95.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509   57.0000   60.0000 93

  3 omega  -28.00   -1.00   1.0000   95.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509  -57.0000    0.0000 27

  4 omega  -34.00   52.00   1.0000   95.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7322    0.0000  150.0000 86

  5 omega  -42.00  -17.00   1.0000   95.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7322  -57.0000  -30.0000 25

  6 omega  -52.00  -27.00   1.0000   95.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509  -57.0000 -120.0000 25

  7 omega    2.00   27.00   1.0000   95.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509  -37.0000 -180.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
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_diffrn_orient_matrix_UB_11      -0.0155340000
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_diffrn_orient_matrix_UB_13      -0.0005226000
_diffrn_orient_matrix_UB_21      0.0351548000
_diffrn_orient_matrix_UB_22      0.0072288000
_diffrn_orient_matrix_UB_23      -0.0337137000
_diffrn_orient_matrix_UB_31      -0.0559585000
_diffrn_orient_matrix_UB_32      -0.0059942000
_diffrn_orient_matrix_UB_33      -0.0445709000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.897
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25348
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.187
_diffrn_reflns_theta_min         3.035
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.205
_exptl_absorpt_correction_T_max  0.852
_exptl_absorpt_correction_T_min  0.737
_exptl_absorpt_correction_type   gaussian
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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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.033
_refine_diff_density_min         -0.958
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         7490
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0183P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_gt                6050
_reflns_number_total             7490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02079h2.cif
_cod_data_source_block           4a
_cod_depositor_comments
'Adding full bibliography for 7039998--7040005.cif.'
_cod_original_cell_volume        2572.45(18)
_cod_database_code               7040003
_chemical_oxdiff_formula         'C84 H156 B40 Ir4 N8'
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_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.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C4(H4A,H4B), C3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6)
2.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C9(H9A,H9B,H9C), C17(H17A,H17B,H17C), C10(H10A,H10B,H10C)
2.d Boron cage BH refined with riding coordinates:
 B10(H10), C1(H1), B12(H12), B8(H8), B7(H7), B11(H11), B5(H5A), B3(H3), B4(H4),
  B9(H9)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'