Electronic effects in iridium C-H borylations: insights from unencumbered substrates and variation of boryl ligand substituents.
Vanchura, 2nd, Britt A; Preshlock, Sean M.; Roosen, Philipp C.; Kallepalli, Venkata A.; Staples, Richard J.; Maleczka, Jr, Robert E; Singleton, Daniel A.; Smith, 3rd, Milton R; Chemical communications (Cambridge, England) 46 (2010) 7724–7726; doi:10.1039/c0cc02041a

data_7112899
_publ_section_title
;
 Electronic effects in iridium C-H borylations: insights from unencumbered
 substrates and variation of boryl ligand substituents.
;
_journal_issue                   41
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7724
_journal_page_last               7726
_journal_paper_doi               10.1039/c0cc02041a
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         'C56 H91 B3 Ir O6 P2, 0.5(C8 H18)'
_chemical_formula_sum            'C60 H100 B3 Ir O6 P2'
_chemical_formula_weight         1203.97
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                78.098(2)
_cell_angle_beta                 85.375(2)
_cell_angle_gamma                65.636(2)
_cell_formula_units_Z            2
_cell_length_a                   14.715(2)
_cell_length_b                   14.882(2)
_cell_length_c                   17.249(2)
_cell_measurement_reflns_used    8142
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.14
_cell_measurement_theta_min      2.21
_cell_volume                     3366.9(8)
_computing_cell_refinement       'APEX2 (BRUKER, V2008.5-0, 2006)'
_computing_data_collection       'COSMO (BRUKER, V1.58, 2006)'
_computing_data_reduction        'SAINT (BRUKER, V7.34A, 2006)'
_computing_molecular_graphics
'SHELXTL (Sheldrick, Acta Cryst. A64 2008, 112-122)'
_computing_publication_material
'SHELXTL (Sheldrick, Acta Cryst. A64 2008, 112-122)'
_computing_structure_refinement
'SHELXL (Sheldrick, Acta Cryst. A64 2008, 112-122)'
_computing_structure_solution
'SHELXS (Sheldrick, Acta Cryst. A64 2008, 112-122)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w,and/f 0.5 deg'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_sigmaI/netI    0.1105
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25455
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.52
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.072
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.057
_refine_diff_density_max         2.234
_refine_diff_density_min         -1.193
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         11719
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1120P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1740
_refine_ls_wR_factor_ref         0.1883
_reflns_number_gt                8967
_reflns_number_total             11719
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc02041a.txt
_cod_data_source_block           p1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        3366.7(8)
_cod_database_code               7112899