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_7219385
_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 H50 Cl Ir O P2'
_chemical_formula_weight         656.24
_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           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.3770(2)
_cell_length_b                   15.3452(2)
_cell_length_c                   28.8663(4)
_cell_measurement_reflns_used    15219
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.0600
_cell_measurement_theta_min      2.2238
_cell_volume                     5482.51(14)
_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_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 0.934
_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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0587
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            39527
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    5.100
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             2656
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane/toluene'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         4.404
_refine_diff_density_min         -3.284
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         9768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1221
_reflns_number_gt                6122
_reflns_number_total             9768
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra15562a2.cif
_cod_data_source_block           abs3
_cod_database_code               7219385