Trifunctional pNHC, Imine, Pyridine Pincer-Type Iridium(III) Complexes: Synthetic, Structural, and Reactivity Studies
He, Fan; Danopoulos, Andreas A.; Braunstein, Pierre; Organometallics 35 (2015) 198–; doi:10.1021/acs.organomet.5b00926

data_4088195
_publ_section_title
;
 Trifunctional pNHC, Imine, Pyridine Pincer-Type Iridium(III) Complexes:
 Synthetic, Structural, and Reactivity Studies
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              198
_journal_paper_doi               10.1021/acs.organomet.5b00926
_journal_volume                  35
_journal_year                    2015
_chemical_formula_moiety         'C31 H48 Cl Ir N4 P, B F4, C H2 Cl2'
_chemical_formula_sum            'C32 H50 B Cl3 F4 Ir N4 P'
_chemical_formula_weight         907.09
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                93.175(5)
_cell_angle_beta                 93.492(5)
_cell_angle_gamma                93.730(5)
_cell_formula_units_Z            2
_cell_length_a                   9.234(5)
_cell_length_b                   12.118(5)
_cell_length_c                   18.115(5)
_cell_measurement_reflns_used    9789
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.71
_cell_measurement_theta_min      2.21
_cell_volume                     2015.4(15)
_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  0.0336
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            52682
_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         31.974
_diffrn_reflns_theta_min         1.687
_diffrn_source                   'fine focus sea'
_exptl_absorpt_coefficient_mu    3.596
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.5682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       plate
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
 The residual electron density was assigned to half a molecule of the
 diethyl ether solvent [34/2 = 17 e per asymmetric unit; half a molecule
 of C4H10O would give 21e].
;
_refine_diff_density_max         1.518
_refine_diff_density_min         -1.361
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         13891
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+0.4536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0774
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11780
_reflns_number_total             13891
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00926_si_001.cif
_cod_data_source_block           pbfh150521
_cod_database_code               4088195
_shelxl_version_number           2013-4
_shelx_res_checksum              7068
_shelx_hkl_checksum              5523