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_7040000
_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         'C22 H29 Cl2 Ir N2'
_chemical_formula_sum            'C22 H29 Cl2 Ir N2'
_chemical_formula_weight         584.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-06
_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                 96.328(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.3524(4)
_cell_length_b                   8.7930(2)
_cell_length_c                   32.4934(11)
_cell_measurement_reflns_used    6178
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      30.7940
_cell_measurement_theta_min      3.5640
_cell_volume                     4359.7(2)
_computing_cell_refinement
;
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_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)'
_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      120.01(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 0.875
_diffrn_measurement_details
;
  1 omega    3.00   84.00   0.5000    1.1400
omega____ theta____ kappa____ phi______ frames
    -       13.1072   37.0000  -30.0000 162

  2 omega   30.00   56.00   0.5000    1.1400
omega____ theta____ kappa____ phi______ frames
    -       13.1072   37.0000  120.0000 52

  3 omega  -20.00   20.00   0.5000    1.1400
omega____ theta____ kappa____ phi______ frames
    -       13.1072   19.0000  -30.0000 80

  4 omega  -37.00  -10.00   0.5000    1.1400
omega____ theta____ kappa____ phi______ frames
    -       13.1072  -37.0000  -30.0000 54

  5 omega  -56.00   15.00   0.5000    1.1400
omega____ theta____ kappa____ phi______ frames
    -       13.1072  -37.0000  150.0000 142
;
_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      0.0285869000
_diffrn_orient_matrix_UB_12      -0.0031089000
_diffrn_orient_matrix_UB_13      0.0186752000
_diffrn_orient_matrix_UB_21      -0.0166200000
_diffrn_orient_matrix_UB_22      -0.0729353000
_diffrn_orient_matrix_UB_23      0.0042570000
_diffrn_orient_matrix_UB_31      0.0326634000
_diffrn_orient_matrix_UB_32      -0.0343686000
_diffrn_orient_matrix_UB_33      -0.0107390000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0667
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.875
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            15520
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.875
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.218
_diffrn_reflns_theta_min         3.019
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.380
_exptl_absorpt_correction_T_max  0.616
_exptl_absorpt_correction_T_min  0.330
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
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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    1.781
_exptl_crystal_description       block
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.204
_refine_diff_density_min         -1.876
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         6181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+21.3606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.1015
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5121
_reflns_number_total             6181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02079h2.cif
_cod_data_source_block           2d
_cod_depositor_comments
'Adding full bibliography for 7039998--7040005.cif.'
_cod_database_code               7040000
_chemical_oxdiff_formula         'C176 H232 Cl16 Ir8 N16'
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  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:
 C5(H5A,H5B), C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'