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_7108648
_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         'C42 H46 Ir N4, C32 H12 B F24'
_chemical_formula_sum            'C74 H58 B F24 Ir N4'
_chemical_formula_weight         1662.28
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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             11-06-19
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                90
_cell_angle_beta                 104.8975(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9900(2)
_cell_length_b                   20.4349(2)
_cell_length_c                   21.0342(3)
_cell_measurement_reflns_used    16163
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     7057.37(15)
_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 0.993
_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  0.039
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31364
_diffrn_reflns_theta_full        26.908
_diffrn_reflns_theta_max         27.457
_diffrn_reflns_theta_min         5.109
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.001
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         2.04
_refine_diff_density_min         -1.13
_refine_ls_extinction_coef       180(20)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1073
_refine_ls_number_reflns         16000
_refine_ls_number_restraints     810
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.0184885
_refine_ls_shift/su_mean         0.0001961
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.03P)^2^ +15.23P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0923
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0923
_reflns_limit_h_max              21
_reflns_limit_h_min              -22
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                12251
_reflns_number_total             16000
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.27
_oxford_diffrn_Wilson_scale      132.91
_oxford_refine_ls_r_factor_ref   0.0662
_oxford_refine_ls_scale          0.092272(17)
_oxford_reflns_number_all        16000
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '4081615 163ct10'
_cod_data_source_file            c2cc35947b.txt
_cod_data_source_block           163CTMK11
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C74 H58 B1 F24 Ir1 N4'
_cod_database_code               7108648