A Cationic Terminal Methylene Complex of Ir(I) Supported by a Pincer Ligand
Campos, Jesus; Peloso, Riccardo; Brookhart, Maurice; Carmona, Ernesto; Organometallics 32 (2013) 3423–; doi:10.1021/om400383s

data_4089538
_publ_contact_author
;
        Jesus Campos
        Instituto de Investigaciones Qu\'imicas
        CSIC-Universidad de Sevilla
        Am\'erico Vespucio, 49
        Isla de la Cartuja 
        41092 SEVILLA
        Spain
;
_publ_section_title
;
 A Cationic Terminal Methylene Complex of Ir(I) Supported by a Pincer
 Ligand
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              3423
_journal_paper_doi               10.1021/om400383s
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety
'2(C25 H50 Ir N O2 P3), 2(C24 B F20), C5 H12, C6 H5 F'
_chemical_formula_sum            'C109 H117 B2 F41 Ir2 N2 O4 P6'
_chemical_formula_weight         2889.93
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                109.711(2)
_cell_angle_beta                 111.838(2)
_cell_angle_gamma                93.720(2)
_cell_formula_units_Z            1
_cell_length_a                   13.4159(8)
_cell_length_b                   15.4284(16)
_cell_length_c                   16.2092(9)
_cell_measurement_reflns_used    9027
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.86
_cell_measurement_theta_min      2.43
_cell_volume                     2861.4(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type
;
 Bruker-Nonius X8kappa APEX II CCD area detector'
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            53022
_diffrn_reflns_theta_full        29.90
_diffrn_reflns_theta_max         29.90
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    2.526
_exptl_absorpt_correction_T_max  0.6551
_exptl_absorpt_correction_T_min  0.4670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS, Bruker (2006). APEX 2. Version 2.1. Bruker Analytical
 X-ray Solutions, Madison, Wisconsin, USA. 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.615
_refine_diff_density_min         -0.968
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.627
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         16406
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.624
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0556
_reflns_number_gt                14655
_reflns_number_total             16406
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400383s_si_002.cif
_cod_data_source_block           jcm0311a
_cod_database_code               4089538