C-H Activation of 2,4,6-Triphenylphosphinine: Synthesis and Characterization of the First Homoleptic Phosphinine-Iridium(III) Complex fac-[Ir(C^P)3]
Leen E. E. Broeckx; Wylliam Delaunay; Camille Latouche; Martin Lutz; Abdou Boucekkine; Muriel Hissler; Christian Müller; Inorganic Chemistry 52 (2013) 10738–10740; doi:10.1021/ic401933m

data_4336358
_publ_contact_author_address
; Bijvoet Center for Biomolecular Research
  Crystal and Structural Chemistry
  Utrecht University
  Padualaan 8
  3584 CH Utrecht
  The Netherlands
;
_publ_contact_author_email       m.lutz@uu.nl
_publ_contact_author_fax         '[+31] 30 2533940'
_publ_contact_author_name        'Martin Lutz'
_publ_contact_author_phone       '[+31] 30 2533902'
_publ_section_title
;
 C-H Activation of 2,4,6-Triphenylphosphinine: Synthesis and
 Characterization of the First Homoleptic Phosphinine-Iridium(III) Complex
 fac-[Ir(C^P)3]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10738
_journal_page_last               10740
_journal_paper_doi               10.1021/ic401933m
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C69 H48 Ir P3'
_chemical_formula_sum            'C69 H48 Ir P3'
_chemical_formula_weight         1162.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 92.2338(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   13.7200(12)
_cell_length_b                   13.5181(12)
_cell_length_c                   51.965(5)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.35
_cell_measurement_theta_min      2.16
_cell_volume                     9630.5(15)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       Apex2
_computing_data_reduction        'SAINT V7.68A, SADABS-2008/1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa ApexII'
_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  0.0706
_diffrn_reflns_av_sigmaI/netI    0.0624
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            140000
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    2.190
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.6644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       needle
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
;
_refine_diff_density_max         0.985
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.022(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2065
_refine_ls_number_reflns         27578
_refine_ls_number_restraints     277
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0785
_reflns_number_gt                24091
_reflns_number_total             27578
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic401933m_si_002.cif
_cod_data_source_block           l0144a
_cod_original_cell_volume        9630.4(15)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4336358