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_4084952
_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, C25 H39 Cl2 P Rh'
_chemical_formula_sum            'C57 H51 B Cl2 F24 P Rh'
_chemical_formula_weight         1407.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.468(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.835(2)
_cell_length_b                   35.645(5)
_cell_length_c                   13.161(2)
_cell_measurement_reflns_used    9483
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.30
_cell_volume                     6015.6(16)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0722
_diffrn_reflns_av_sigmaI/netI    0.0582
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            52988
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    0.511
_exptl_absorpt_correction_T_max  0.4381
_exptl_absorpt_correction_T_min  0.2847
_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    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.975
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     808
_refine_ls_number_reflns         10855
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0684P)^2^+12.9088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1413
_refine_ls_wR_factor_ref         0.1627
_reflns_number_gt                7474
_reflns_number_total             10855
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500910t_si_001.cif
_cod_data_source_block           jc00210a
_cod_depositor_comments
'Adding full bibliography for 4084945--4084954.cif.'
_cod_original_cell_volume        6015.7(17)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4084952