Imine-functionalised protic NHC complexes of Ir: direct formation by C-H activation.
He, Fan; Braunstein, Pierre; Wesolek, Marcel; Danopoulos, Andreas A.; Chemical communications (Cambridge, England) 51 (2015) 2814–; doi:10.1039/c4cc10109j

data_7116479
_publ_section_title
;
 Imine-functionalised protic NHC complexes of Ir: direct formation by C-H
 activation.
;
_journal_issue                   14
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2814
_journal_paper_doi               10.1039/c4cc10109j
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C50 H68 Ir2 N6'
_chemical_formula_sum            'C50 H68 Ir2 N6'
_chemical_formula_weight         1137.50
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-12-16 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                86.542(2)
_cell_angle_beta                 72.600(2)
_cell_angle_gamma                62.575(4)
_cell_formula_units_Z            2
_cell_length_a                   12.2904(3)
_cell_length_b                   13.3290(5)
_cell_length_c                   19.4944(6)
_cell_measurement_reflns_used    30741
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2693.60(18)
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_molecular_graphics    'PLATON 98 (Spek, 1998)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Superflip (Palatinus, 2007)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29513
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.478
_diffrn_reflns_theta_min         1.099
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.970
_exptl_absorpt_correction_T_max  0.33442
_exptl_absorpt_correction_T_min  0.28056
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULscanABS in PLATON (Spek, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       prism
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
 The residual electron density was assigned to four molecules of the
 diethyl ether solvent [318/2 = 159 e per asymmetric unit; four molecules
 of C4H10O would give 168e].
;
_refine_diff_density_max         1.529
_refine_diff_density_min         -2.862
_refine_diff_density_rms         0.310
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         12243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0656P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1169
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9499
_reflns_number_total             12243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc10109j2.cif
_cod_data_source_block           pbfh140901
_cod_original_cell_volume        2693.61(17)
_cod_database_code               7116479
_shelxl_version_number           2013-4
_shelx_res_checksum              87354