Evidence for C−H···X−Ir (X = Cl or I) Hydrogen Bonding between Imidazolium Salts and Iridium-Bound Halides and Formation of Ir(I) NHC Complexes†
Zuo, Weiwei; Braunstein, Pierre; Organometallics 29 (2010) 5535–; doi:10.1021/om100496x

data_4066497
_publ_section_title
;
 Evidence for C&#x2212;H&#x00B7;&#x00B7;&#x00B7;X&#x2212;Ir (X = Cl or I)
 Hydrogen Bonding between Imidazolium Salts and Iridium-Bound Halides and
 Formation of Ir(I) NHC Complexes&#x2020;
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              5535
_journal_paper_doi               10.1021/om100496x
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C42 H55 Cl0.70 I0.30 Ir N4, C2 H3 N, I'
_chemical_formula_sum            'C44 H58 Cl0.7 I1.3 Ir N5'
_chemical_formula_weight         1038.96
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.8880(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5090(2)
_cell_length_b                   29.9709(6)
_cell_length_c                   14.7927(3)
_cell_measurement_reflns_used    6915
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.103
_cell_measurement_theta_min      0.998
_cell_volume                     4155.48(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0853
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15197
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         3.16
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.227
_exptl_absorpt_correction_T_max  0.675
_exptl_absorpt_correction_T_min  0.570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'L. Spek, J. Appl.Cryst. 2003, 36, 7, B. Blessing, Acta Cryst, 1995, A51, 33'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2059.2
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.751
_refine_diff_density_min         -1.418
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         9108
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0950
_reflns_number_gt                6085
_reflns_number_total             9108
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100496x_si_002.cif
_cod_data_source_block           ZwIr4
_cod_original_cell_volume        4155.48(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C44 H58 Cl0.70 I1.30 Ir N5'
_cod_database_code               4066497