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_4112563
_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            'C17 H24 F9 I Ir P'
_chemical_formula_weight         749.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.160(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4637(7)
_cell_length_b                   15.4169(7)
_cell_length_c                   14.9804(9)
_cell_measurement_temperature    173(2)
_cell_volume                     2185.6(2)
_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 0.850
_diffrn_measured_fraction_theta_max 0.850
_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  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5251
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    7.671
_exptl_absorpt_correction_T_max  0.3091
_exptl_absorpt_correction_T_min  0.1494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Orange/Yellow
_exptl_crystal_density_diffrn    2.278
_exptl_crystal_description       Block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.531
_refine_diff_density_min         -1.528
_refine_diff_density_rms         0.206
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.034(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         3485
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0619P)^2^+24.5955P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.0961
_reflns_number_gt                3450
_reflns_number_total             3485
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja049225qsi20040316_115930_3.cif
_cod_data_source_block           rph147_compound4
_cod_database_code               4112563