A Simple Route to Difluorocarbene and Perfluoroalkylidene Complexes of Iridium
Russell P. Hughes; Roman B. Laritchev; Jian Yuan; James A. Golen; Adam N. Rucker; Arnold L. Rheingold; Journal of the American Chemical Society 127 (2005) 15020–15021; doi:10.1021/ja055166k

data_4112045
_publ_section_title
;
 A Simple Route to Difluorocarbene and Perfluoroalkylidene Complexes of
 Iridium
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15020
_journal_page_last               15021
_journal_paper_doi               10.1021/ja055166k
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C21 H28 F3 I Ir P'
_chemical_formula_weight         687.50
_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                 91.5390(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.1786(5)
_cell_length_b                   9.1263(5)
_cell_length_c                   28.1355(17)
_cell_measurement_reflns_used    9544
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      2.23
_cell_volume                     2099.3(2)
_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      203(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_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  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            15933
_diffrn_reflns_theta_full        28.17
_diffrn_reflns_theta_max         28.17
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    7.937
_exptl_absorpt_correction_T_max  0.7419
_exptl_absorpt_correction_T_min  0.2997
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.175
_exptl_crystal_density_meas      0
_exptl_crystal_description       blade
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.083
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4860
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.615
_refine_ls_shift/su_mean         0.051
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+8.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0879
_reflns_number_gt                4123
_reflns_number_total             4860
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja055166ksi20050729_123415.cif
_cod_data_source_block           rph307
_cod_database_code               4112045