PC(sp3)P Pincer Carbonyl Complexes of Iridium(I) and Iridium(III)
Jonasson, Klara J.; Polukeev, Alexey; Wendt, Ola; RSC Adv.  (2015) –; doi:10.1039/C4RA15562A

data_7219386
_publ_section_title
;
 PC(sp3)P Pincer Carbonyl Complexes of Iridium(I) and Iridium(III)
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA15562A
_journal_year                    2015
_chemical_formula_sum            'C25 H49 Cl Ir O P2'
_chemical_formula_weight         655.23
_chemical_name_systematic
trans-[Iridium(hydrido)(carbonyl)Chloro{cis-1,3-Bis-((di-tert-butylphosphino)methyl)}-cyclohexane]
_chemical_properties_physical    Moisture-sensitive
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-10-15 deposited with the CCDC.
2015-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.996(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5453(2)
_cell_length_b                   15.2101(3)
_cell_length_c                   15.5649(3)
_cell_measurement_reflns_used    30747
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9626
_cell_measurement_theta_min      2.4168
_cell_volume                     2962.80(9)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'CrystalMaker (CrystalMaker, 2011)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1829
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_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  0.0594
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            70507
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.03
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    4.718
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51824
_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            colourless
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1324
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene/hexane'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.080
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.425
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         7422
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.425
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.1030
_reflns_number_gt                6467
_reflns_number_total             7422
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra15562a2.cif
_cod_data_source_block           kj3026b
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7219386