Tandem C‒F and C‒H Bond Activation in Fluoroolefins Promoted by a Bis(diethylphosphino)methane-Bridged Diiridium Complex: Role of Water in the Activation Processes
Slaney, Michael E.; Ferguson, Michael J.; McDonald, Robert; Cowie, Martin; Organometallics 31 (2012) 1384–; doi:10.1021/om2011968

data_4068197
_publ_section_title
;
 Tandem C--F and C--H Bond Activation in Fluoroolefins Promoted by a
 Bis(diethylphosphino)methane-Bridged Diiridium Complex: Role of Water in
 the Activation Processes
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1384
_journal_paper_doi               10.1021/om2011968
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C23 H47 Ir2 O3 P4, C32 H12 B F24'
_chemical_formula_sum            'C55 H59 B F24 Ir2 O3 P4'
_chemical_formula_weight         1743.11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                76.3985(15)
_cell_angle_beta                 84.0521(16)
_cell_angle_gamma                86.3437(16)
_cell_formula_units_Z            2
_cell_length_a                   12.5007(16)
_cell_length_b                   14.6611(18)
_cell_length_c                   18.491(2)
_cell_measurement_reflns_used    7504
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.11
_cell_measurement_theta_min      2.18
_cell_volume                     3273.4(7)
_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    'DIRDIF-2008 (Beurskens et al., 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0144
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29059
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    4.268
_exptl_absorpt_correction_T_max  0.5155
_exptl_absorpt_correction_T_min  0.2729
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.166
_refine_diff_density_min         -1.444
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         14991
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0229
_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^)+(0.0258P)^2^+4.3209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0578
_reflns_number_gt                13501
_reflns_number_total             14991
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om2011968_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3273.5(7)
_cod_database_code               4068197