α- and β-Fluorine Elimination Reactions Induced by Reduction of Iridium−Fluoroalkyl Complexes. Selective Formation of Fluoroalkylidene and Hydrofluoroalkene Ligands
Bourgeois, Cheryl J.; Hughes, Russell P.; Yuan, Jian; DiPasquale, Antonio G.; Rheingold, Arnold L.; Organometallics 25 (2006) 2908–; doi:10.1021/om060243l

data_4075354
_publ_section_title
;
 \a- and \b-Fluorine Elimination Reactions Induced by Reduction of
 Iridium&#x2212;Fluoroalkyl Complexes. Selective Formation of
 Fluoroalkylidene and Hydrofluoroalkene Ligands
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2908
_journal_paper_doi               10.1021/om060243l
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C13 H17 F2 Ir O'
_chemical_formula_weight         419.47
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 103.519(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.299(4)
_cell_length_b                   11.283(6)
_cell_length_c                   8.262(5)
_cell_measurement_reflns_used    3480
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.98
_cell_measurement_theta_min      2.54
_cell_volume                     661.6(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3873
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    10.095
_exptl_absorpt_correction_T_max  0.4317
_exptl_absorpt_correction_T_min  0.1517
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.106
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.336
_refine_diff_density_min         -1.119
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         1590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0224
_refine_ls_shift/su_max          0.465
_refine_ls_shift/su_mean         0.074
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0596
_reflns_number_gt                1544
_reflns_number_total             1590
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060243lsi20060427_010511.cif
_cod_data_source_block           rph348_compound_11
_cod_original_sg_symbol_H-M      P2(1)/m
_cod_database_code               4075354