Rhodium and Iridium Complexes of Bulky Tertiary Phosphine Ligands. Searching for Isolable Cationic MIIIAlkylidenes
Campos, Jesús; Carmona, Ernesto; Organometallics 34 (2015) 2212–; doi:10.1021/om500910t

data_4084948
_publ_section_title
;
 Rhodium and Iridium Complexes of Bulky Tertiary Phosphine Ligands.
 Searching for Isolable Cationic MIIIAlkylidenes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2212
_journal_paper_doi               10.1021/om500910t
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C32 H12 B F24, C24 H37 Ir P'
_chemical_formula_sum            'C56 H49 B F24 Ir P'
_chemical_formula_weight         1411.93
_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                74.310(2)
_cell_angle_beta                 68.576(2)
_cell_angle_gamma                81.856(2)
_cell_formula_units_Z            4
_cell_length_a                   18.1609(9)
_cell_length_b                   18.2151(9)
_cell_length_c                   19.2306(10)
_cell_measurement_reflns_used    9771
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.05
_cell_measurement_theta_min      2.29
_cell_volume                     5694.8(5)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            98961
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         1.17
_exptl_absorpt_coefficient_mu    2.488
_exptl_absorpt_correction_T_max  0.8258
_exptl_absorpt_correction_T_min  0.5126
_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            red
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.08
_refine_diff_density_max         5.154
_refine_diff_density_min         -2.994
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1621
_refine_ls_number_reflns         20497
_refine_ls_number_restraints     483
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0291P)^2^+21.2501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0880
_reflns_number_gt                16681
_reflns_number_total             20497
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500910t_si_001.cif
_cod_data_source_block           jc00110a
_cod_depositor_comments
'Adding full bibliography for 4084945--4084954.cif.'
_cod_database_code               4084948