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_7105978
_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 P Rh'
_chemical_formula_sum            'C33 H31 Cl P Rh'
_chemical_formula_weight         596.91
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.867(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.33421(12)
_cell_length_b                   16.3287(4)
_cell_length_c                   22.9799(3)
_cell_measurement_reflns_used    46565
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      1.54
_cell_volume                     2719.14(9)
_computing_cell_refinement       Peakref
_computing_data_collection       Apex
_computing_data_reduction        'Eval15, Sadabs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa 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  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0136
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            49748
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         6249
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0216
_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^)+(0.0275P)^2^+1.7007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0574
_reflns_number_gt                5694
_reflns_number_total             6249
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            C0CC04660D.TXT
_cod_data_source_block           l0121a
_cod_original_cell_volume        2719.14(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7105978