Synthesis and characterisation of PCsp3P phosphine and phosphinite iridium complexes. Cyclometallation and dehydrogenation of a cyclohexyl ring
Arunachalampillai, Athimoolam; Olsson, Daniel; Wendt, Ola F.; Dalton Transactions  (2009) 8626–8630; doi:10.1039/b910798c

data_7002447
_publ_section_title
;
 Synthesis and characterisation of PCsp3P phosphine and phosphinite
 iridium complexes. Cyclometallation and dehydrogenation of a
 cyclohexyl ring
;
_journal_issue                   40
_journal_name_full               'Dalton Transactions'
_journal_page_first              8626
_journal_page_last               8630
_journal_paper_doi               10.1039/b910798c
_journal_year                    2009
_chemical_formula_sum            'C22 H39 Cl Ir O2 P2'
_chemical_formula_weight         625.12
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.461(5)
_cell_angle_beta                 95.623(5)
_cell_angle_gamma                104.395(6)
_cell_formula_units_Z            2
_cell_length_a                   8.2429(5)
_cell_length_b                   12.2217(8)
_cell_length_c                   13.4226(8)
_cell_measurement_reflns_used    4494
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.1231
_cell_measurement_theta_min      2.5704
_cell_volume                     1273.38(15)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1829
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measurement_device_type  'Oxford Diffraction XCalibur 3'
_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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.1780
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13293
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         33.20
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    5.488
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93492
_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            red
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             622
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.236
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.768
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         8453
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.768
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0253P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0681
_reflns_number_gt                4229
_reflns_number_total             8453
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b910798c.txt
_cod_data_source_block           athi53_complex5
_cod_original_cell_volume        1273.38(14)
_cod_database_code               7002447