C-H Bond Activations by New Labile η6-Arene Complexes of Iridium
Francisco Torres; Eduardo Sola; Marta Martín; José A. López; Fernando J. Lahoz; Luis A. Oro; Journal of the American Chemical Society 121 (1999) 10632–10633; doi:10.1021/ja9923890

data_4116584
_publ_contact_author
;
  Dr. Fernando J. Lahoz
  Departamento de Qu\'imica Inorg\'anica
  Facultad de Ciencias
  Universidad de Zaragoza
  50009 Zaragoza, Spain
;
_publ_contact_author_email       lahoz@posta.unizar.es
_publ_section_title
;
 C-H Bond Activations by New Labile \h6-Arene Complexes of Iridium
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10632
_journal_page_last               10633
_journal_paper_doi               10.1021/ja9923890
_journal_volume                  121
_journal_year                    1999
_chemical_formula_moiety         'C18 H35 Ir P 1+, B F4 1-'
_chemical_formula_sum            'C18 H35 B F4 Ir P'
_chemical_formula_weight         561.44
_chemical_name_systematic
;
 dihydride-triisopropylphosphine-1,3,5-trimethylbenzene-iridium(III)
tetrafluoro borate
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.454(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.1477(7)
_cell_length_b                   13.8943(12)
_cell_length_c                   10.1659(9)
_cell_measurement_reflns_used    60
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      15
_cell_volume                     1085.14(18)
_computing_cell_refinement       'XSCANS v. 2.1 (Siemens)'
_computing_data_collection       'XSCANS v. 2.1 (Siemens)'
_computing_data_reduction        'XSCANS v. 2.1 (Siemens)'
_computing_molecular_graphics    'XP, SHELXTL v.5 (Siemens)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '\w-2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal focus Mo sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4286
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.258
_exptl_absorpt_correction_T_max  0.3988
_exptl_absorpt_correction_T_min  0.2116
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 Azimuthal psi-scans of 30 reflections (15 + Friedel pairs) at 10\% intervals.
 Data corrected with the program: XPREP, SHELXTL v. 5 (Siemens)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.026(14)
_refine_ls_extinction_coef       0.0059(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3842
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+8.8796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0833
_reflns_number_gt                3675
_reflns_number_total             3842
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9923890.cif
_cod_data_source_block           compound4
_cod_original_cell_volume        1085.14(16)
_cod_database_code               4116584