Cyclohexane-Based Phosphinite Iridium Pincer Complexes: Synthesis, Characterization, Carbene Formation, and Catalytic Activity in Dehydrogenation Reactions
Polukeev, Alexey V.; Wendt, Ola F.; Organometallics 36 (2017) 639–; doi:10.1021/acs.organomet.6b00846

data_4087125
_publ_section_title
;
 Cyclohexane-Based Phosphinite Iridium Pincer Complexes: Synthesis,
 Characterization, Carbene Formation, and Catalytic Activity in
 Dehydrogenation Reactions
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              639
_journal_paper_doi               10.1021/acs.organomet.6b00846
_journal_volume                  36
_journal_year                    2017
_chemical_formula_sum            'C22 H44 Cl Ir O2 P2'
_chemical_formula_weight         630.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 113.090(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0591(9)
_cell_length_b                   15.1140(9)
_cell_length_c                   15.2086(11)
_cell_measurement_reflns_used    1970
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.9730
_cell_measurement_theta_min      2.6273
_cell_volume                     2761.3(4)
_computing_structure_refinement  'SHELXL-2014/7 (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 0.932
_diffrn_measurement_device_type  'Oxford Xcalibur 3'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1762
_diffrn_reflns_av_unetI/netI     0.2578
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27648
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         33.048
_diffrn_reflns_theta_min         2.633
_exptl_absorpt_coefficient_mu    5.062
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92206
_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            violet
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_description       plate
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.03
_refine_diff_density_max         4.648
_refine_diff_density_min         -1.478
_refine_diff_density_rms         0.258
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         9738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.2713
_refine_ls_R_factor_gt           0.1331
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0700P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2001
_refine_ls_wR_factor_ref         0.2557
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4196
_reflns_number_total             9738
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00846_si_002.cif
_cod_data_source_block           comp6
_cod_database_code               4087125
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              97538
_shelx_hkl_checksum              78764