Iridium Hydride Complexes with Cyclohexyl-Based Pincer Ligands: Fluxionality and Deuterium Exchange
Polukeev, Alexey V.; Marcos, Rocío; Ahlquist, Mårten S. G.; Wendt, Ola F.; Organometallics 35 (2016) 2600–; doi:10.1021/acs.organomet.6b00324

data_4088699
_publ_section_title
;
 Iridium Hydride Complexes with Cyclohexyl-Based Pincer Ligands:
 Fluxionality and Deuterium Exchange
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              2600
_journal_paper_doi               10.1021/acs.organomet.6b00324
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C24 H53 Ir P2'
_chemical_formula_sum            'C24 H53 Ir P2'
_chemical_formula_weight         595.80
_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   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                103.610(4)
_cell_angle_beta                 100.537(4)
_cell_angle_gamma                110.861(4)
_cell_formula_units_Z            2
_cell_length_a                   8.4709(4)
_cell_length_b                   11.7388(5)
_cell_length_c                   15.6404(7)
_cell_measurement_reflns_used    9535
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8459
_cell_measurement_theta_min      2.5809
_cell_volume                     1350.23(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1829
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17856
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.909
_diffrn_reflns_theta_min         2.586
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.070
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.327
_refine_diff_density_min         -1.706
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         6237
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+9.2698P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0721
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5861
_reflns_number_total             6237
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00324_si_002.cif
_cod_data_source_block           compound2
_cod_original_cell_volume        1350.23(11)
_cod_database_code               4088699
_shelxl_version_number           2014-3
_shelx_res_checksum              54647
_shelx_hkl_checksum              73864