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_7039998
_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 Cl2 N2 Ru'
_chemical_formula_sum            'C18 H34 B10 Cl2 N2 Ru'
_chemical_formula_weight         558.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'I -2ya'
_space_group_name_H-M_alt        'I 1 a 1'
_symmetry_space_group_name_Hall  'I -2ya'
_symmetry_space_group_name_H-M   'I 1 a 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                 112.782(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8583(3)
_cell_length_b                   19.1551(4)
_cell_length_c                   12.2719(3)
_cell_measurement_reflns_used    3479
_cell_measurement_temperature    119.99(12)
_cell_measurement_theta_max      73.1650
_cell_measurement_theta_min      4.4970
_cell_volume                     2570.06(12)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.99(12)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
  1 omega  -12.00   31.00   1.0000    9.0100
omega____ theta____ kappa____ phi______ frames
    -      -41.0434   37.0000    0.0000 43

  2 omega  -34.00   12.00   1.0000    9.0100
omega____ theta____ kappa____ phi______ frames
    -      -41.0434   37.0000 -120.0000 46

  3 omega  -39.00   31.00   1.0000    9.0100
omega____ theta____ kappa____ phi______ frames
    -      -41.0434   37.0000  -60.0000 70

  4 omega  -44.00    9.00   1.0000    9.0100
omega____ theta____ kappa____ phi______ frames
    -      -41.0434   37.0000   90.0000 53

  5 omega   44.00   73.00   1.0000   36.0500
omega____ theta____ kappa____ phi______ frames
    -      106.0180  -45.0000 -180.0000 29

  6 omega   48.00   95.00   1.0000   36.0500
omega____ theta____ kappa____ phi______ frames
    -      106.0180  -45.0000 -150.0000 47

  7 omega   31.00   85.00   1.0000   36.0500
omega____ theta____ kappa____ phi______ frames
    -      106.0180  -30.0000  -30.0000 54

  8 omega   61.00   90.00   1.0000   36.0500
omega____ theta____ kappa____ phi______ frames
    -      106.0180  -30.0000   60.0000 29

  9 omega   85.00  171.00   1.0000   36.0500
omega____ theta____ kappa____ phi______ frames
    -      106.0180   45.0000   90.0000 86

 10 omega  126.00  178.00   1.0000   36.0500
omega____ theta____ kappa____ phi______ frames
    -      106.0180   45.0000   30.0000 52

 11 omega   34.00   90.00   1.0000   36.0500
omega____ theta____ kappa____ phi______ frames
    -      106.0180  -30.0000  -90.0000 56

 12 omega   30.00   90.00   1.0000   36.0500
omega____ theta____ kappa____ phi______ frames
    -      106.0180  -30.0000  120.0000 60
;
_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      0.0205956000
_diffrn_orient_matrix_UB_12      0.0227417000
_diffrn_orient_matrix_UB_13      -0.1112206000
_diffrn_orient_matrix_UB_21      -0.0963057000
_diffrn_orient_matrix_UB_22      0.0580166000
_diffrn_orient_matrix_UB_23      -0.0221543000
_diffrn_orient_matrix_UB_31      0.1008176000
_diffrn_orient_matrix_UB_32      0.0508854000
_diffrn_orient_matrix_UB_33      0.0752075000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4773
_diffrn_reflns_point_group_measured_fraction_full 0.585
_diffrn_reflns_point_group_measured_fraction_max 0.564
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.344
_diffrn_reflns_theta_min         4.539
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.907
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.581
_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    1.444
_exptl_crystal_description       needle
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.909
_refine_diff_density_min         -1.954
_refine_diff_density_rms         0.170
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.010(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         2923
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0905P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1245
_refine_ls_wR_factor_ref         0.1258
_reflns_Friedel_coverage         0.165
_reflns_Friedel_fraction_full    0.170
_reflns_Friedel_fraction_max     0.160
_reflns_number_gt                2839
_reflns_number_total             2923
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02079h2.cif
_cod_data_source_block           6b
_cod_depositor_comments
'Adding full bibliography for 7039998--7040005.cif.'
_cod_original_cell_volume        2570.05(13)
_cod_database_code               7039998
_chemical_oxdiff_formula         C18H37B10N2RuCl2
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Rigid body (RIGU) restrains
 C9, C14, C13, C12, C11, C10
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3.a Ternary CH refined with riding coordinates:
 C16(H16)
3.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C11(H11), C10(H10), C13(H13), C14(H14), C6(H6)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
3.e Boron cage BH refined with riding coordinates:
 C1(H1), B4(H4), B3(H3), B8(H8), B5(H5A), B12(H12), B9(H9), B10(H10A), B6(H6A),
  B11(H11A), B7(H7)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'