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_7116477
_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         'C25 H36 Cl Ir N3, B F4'
_chemical_formula_sum            'C25 H36 B Cl F4 Ir N3'
_chemical_formula_weight         693.03
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 110.9360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.1698(9)
_cell_length_b                   20.5501(8)
_cell_length_c                   14.5843(6)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      34.06
_cell_measurement_theta_min      2.48
_cell_volume                     6205.8(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50764
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.081
_diffrn_reflns_theta_min         1.396
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    4.429
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.5676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       prism
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;
 The residual electron density was assigned to one molecule of the
 diethyl ether solvent [348/8 = 44 e per asymmetric unit; one molecule
 of C4H10O would give 42e].
;
_refine_diff_density_max         3.074
_refine_diff_density_min         -2.275
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         12686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0324P)^2^+23.5269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0812
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10025
_reflns_number_total             12686
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc10109j2.cif
_cod_data_source_block           pbfh141126
_cod_database_code               7116477
_shelx_estimated_absorpt_t_min   0.306
_shelx_estimated_absorpt_t_max   0.471
_shelxl_version_number           2013-4
_shelx_res_checksum              45934