Hydrogen shuttling: synthesis and reactivity of a 14-electron iridium complex featuring a bis(alkyl) tethered N-heterocyclic carbene ligand
Christina Y. Tang; Nicholas Phillips; Michael J. Kelly; Simon Aldridge; Chem.Commun. 48 (2012) 11999–; doi:10.1039/c2cc35947b

data_7108646
_publ_section_title
;
 Hydrogen shuttling: synthesis and reactivity of a 14-electron iridium
 complex featuring a bis(alkyl) tethered N-heterocyclic carbene ligand
;
_journal_name_full               Chem.Commun.
_journal_page_first              11999
_journal_paper_doi               10.1039/c2cc35947b
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C48 H68 B Ir N5, C32 H12 B F24'
_chemical_formula_sum            'C80 H80 B2 F24 Ir N5'
_chemical_formula_weight         1781.34
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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             11-06-29
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                84.6300(4)
_cell_angle_beta                 87.2490(4)
_cell_angle_gamma                89.4415(5)
_cell_formula_units_Z            2
_cell_length_a                   12.45280(10)
_cell_length_b                   16.8943(2)
_cell_length_c                   19.4968(2)
_cell_measurement_reflns_used    17112
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     4079.00(7)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30117
_diffrn_reflns_theta_full        26.956
_diffrn_reflns_theta_max         27.506
_diffrn_reflns_theta_min         5.102
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.737
_exptl_absorpt_correction_T_max  0.56
_exptl_absorpt_correction_T_min  0.51
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1796
_exptl_crystal_size_max          0.560
_exptl_crystal_size_mid          0.390
_exptl_crystal_size_min          0.330
_refine_diff_density_max         2.35
_refine_diff_density_min         -1.47
_refine_ls_extinction_coef       110(20)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9901
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1172
_refine_ls_number_reflns         18572
_refine_ls_number_restraints     972
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.0321426
_refine_ls_shift/su_mean         0.0004039
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.05P)^2^ +11.35P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1100
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1100
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              21
_reflns_limit_k_min              -21
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                15506
_reflns_number_total             18572
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.04
_oxford_diffrn_Wilson_scale      60.97
_oxford_refine_ls_r_factor_ref   0.0631
_oxford_refine_ls_scale          0.13822(4)
_oxford_reflns_number_all        18572
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '5190028 199ct10'
_cod_data_source_file            c2cc35947b.txt
_cod_data_source_block           199CTMK10
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C80 H80 B2 F24 Ir1 N5'
_cod_database_code               7108646