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_7108647
_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         'C45 H58 B Ir1 N5, C32 H12 B1 F24'
_chemical_formula_sum            'C77 H70 B2 F24 Ir N5'
_chemical_formula_weight         1735.23
_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             11-08-04
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                80.1426(3)
_cell_angle_beta                 82.4277(3)
_cell_angle_gamma                89.6505(3)
_cell_formula_units_Z            2
_cell_length_a                   13.57800(10)
_cell_length_b                   16.55140(10)
_cell_length_c                   17.81450(10)
_cell_measurement_reflns_used    16072
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3909.48(4)
_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 0.990
_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  0.021
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17704
_diffrn_reflns_theta_full        26.899
_diffrn_reflns_theta_max         27.448
_diffrn_reflns_theta_min         5.101
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.810
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_platon_squeeze_details
;The discrete Fourier transform of the void region
were treated as contributions to the A and B parts
of the calculated structure factors.
;
_refine_diff_density_max         1.68
_refine_diff_density_min         -1.55
_refine_ls_extinction_coef       192(14)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.8202
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1091
_refine_ls_number_reflns         17704
_refine_ls_number_restraints     648
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.0240896
_refine_ls_shift/su_mean         0.0004017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
12.6 16.4 5.50
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0883
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0883
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              21
_reflns_limit_k_min              -20
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                16035
_reflns_number_total             17704
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.66
_oxford_diffrn_Wilson_scale      22.26
_oxford_refine_ls_r_factor_ref   0.0408
_oxford_refine_ls_scale          0.22591(10)
_oxford_reflns_number_all        17704
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '6191540 205CT10'
_cod_data_source_file            c2cc35947b.txt
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C77 H70 B2 F24 Ir1 N5'
_cod_database_code               7108647