The Bridged Binding Mode as a New, Versatile Template for the Selective Activation of Carbon-Fluorine Bonds in Fluoroolefins: Activation of Trifluoroethylene
Michael E. Slaney; D. Jason Anderson; Michael J. Ferguson; Robert McDonald; Martin Cowie; Journal of the American Chemical Society 132 (2010) 16544–16558; doi:10.1021/ja106723u

data_4103543
_publ_section_title
;
 The Bridged Binding Mode as a New, Versatile Template for the Selective
 Activation of Carbon-Fluorine Bonds in Fluoroolefins: Activation of
 Trifluoroethylene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16544
_journal_page_last               16558
_journal_paper_doi               10.1021/ja106723u
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety
'C55 H46 F3 Ir2 O6 P4 S, C F3 O3 S, 2(C H2 Cl2)'
_chemical_formula_sum            'C58 H50 Cl4 F6 Ir2 O9 P4 S2'
_chemical_formula_weight         1719.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   20.9533(10)
_cell_length_b                   23.2733(11)
_cell_length_c                   54.433(3)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.84
_cell_measurement_theta_min      2.16
_cell_volume                     26544(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w 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  0.0995
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_number            207019
_diffrn_reflns_theta_full        26.44
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    4.395
_exptl_absorpt_correction_T_max  0.5988
_exptl_absorpt_correction_T_min  0.4858
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             13408
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
Attempts to refine peaks of residual electron density as 
disordered or partial-occupancy solvent dichloromethane or diethylether
carbon, chlorine or oxygen atoms were unsuccessful.  The data were corrected 
for disordered electron density through use of the SQUEEZE procedure (Sluis, 
P. van der; Spek, A. L. Acta Crystallogr. 1990, A46, 194-201) as implemented 
in PLATON (Spek, A. L. Acta Crystallogr. 1990, A46, C34; Spek, A. L. J. 
Appl. Cryst. 2003, 36, 7-13.  PLATON - a multipurpose crystallographic 
tool.  Utrecht University, Utrecht, The Netherlands).  A total 
solvent-accessible void volume of 4905 cubic Angstroms with a total electron
count of 982 (consistent with 24 molecules of solvent dichloromethane, or 1.5 
molecules per formula unit of the diiridium complex) was found in the unit 
cell.
;
_refine_diff_density_max         2.857
_refine_diff_density_min         -1.794
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1450
_refine_ls_number_reflns         27266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+215.5532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1165
_reflns_number_gt                19998
_reflns_number_total             27266
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja106723u_si_001_3.cif
_cod_data_source_block           13
_cod_database_code               4103543