C-H Activation of 2,4,6-Triphenylphosphinine: Unprecedented Formation of Cyclometalated [(P^C)Ir(III)] and [(P^C)Rh(III)] Complexes
Leen E. E. Broeckx; Martin Lutz; Dieter Vogt; Christian Muller; Chem.Commun. 47 (2011) 2003–; doi:10.1039/c0cc04660d

data_7105977
_publ_section_title
;
 C-H Activation of 2,4,6-Triphenylphosphinine: Unprecedented Formation of
 Cyclometalated [(P^C)Ir(III)] and [(P^C)Rh(III)] Complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              2003
_journal_paper_doi               10.1039/c0cc04660d
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C33 H31 Cl Ir P'
_chemical_formula_sum            'C33 H31 Cl Ir P'
_chemical_formula_weight         686.20
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.1991(8)
_cell_length_b                   14.1332(15)
_cell_length_c                   25.829(3)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.77
_cell_volume                     2628.0(5)
_computing_cell_refinement       Saint
_computing_data_collection       ApexII
_computing_data_reduction        'Saint, Sadabs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker ApexII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            31203
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    5.264
_exptl_absorpt_correction_T_max  0.8571
_exptl_absorpt_correction_T_min  0.3433
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.982
_refine_diff_density_min         -1.333
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.016(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         6014
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0261
_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^)+(0.0331P)^2^+0.3335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0610
_reflns_number_gt                5582
_reflns_number_total             6014
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            C0CC04660D.TXT
_cod_data_source_block           l0094a
_cod_database_code               7105977