Conformational Analysis and Assignments of Relative Stereocenter Configurations in Fluoroalkyl-Iridium Complexes Using 19F{1H} HOESY Experiments. Comparison with Solid-State X-ray Structural Results
Russell P. Hughes; Donghui Zhang; Antony J. Ward; Lev N. Zakharov; Arnold L. Rheingold; Journal of the American Chemical Society 126 (2004) 6169–6178; doi:10.1021/ja049225q

data_4112562
_publ_section_title
;
 Conformational Analysis and Assignments of Relative Stereocenter
 Configurations in Fluoroalkyl-Iridium Complexes Using 19F{1H} HOESY
 Experiments. Comparison with Solid-State X-ray Structural Results
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6169
_journal_page_last               6178
_journal_paper_doi               10.1021/ja049225q
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C15 H15 F9 I Ir O'
_chemical_formula_weight         701.37
_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                 95.585(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5210(7)
_cell_length_b                   15.2085(12)
_cell_length_c                   14.6563(12)
_cell_measurement_temperature    173(2)
_cell_volume                     1890.3(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.851
_diffrn_measured_fraction_theta_max 0.851
_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  0.0638
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9099
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    8.783
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Orange/Yellow
_exptl_crystal_density_diffrn    2.464
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.414
_refine_diff_density_min         -1.579
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4029
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0698P)^2^+19.6464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1280
_reflns_number_gt                3529
_reflns_number_total             4029
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja049225qsi20040316_115930_2.cif
_cod_data_source_block           rph148_compound3
_cod_database_code               4112562