Metal control of selectivity in acetate-assisted C‒H bond activation: an experimental and computational study of heterocyclic, vinylic and phenylic C(sp2)‒H bonds at Ir and Rh
Carr, Kevin J. T.; Davies, David L.; Macgregor, Stuart A.; Singh, Kuldip; Villa-Marcos, Barbara; Chemical Science 5 (2014) 2340–; doi:10.1039/c4sc00738g

data_1516545
_publ_section_title
;
 Metal control of selectivity in acetate-assisted C--H bond activation: an
 experimental and computational study of heterocyclic, vinylic and
 phenylic C(sp2)--H bonds at Ir and Rh
;
_journal_issue                   6
_journal_name_full               'Chemical Science'
_journal_page_first              2340
_journal_paper_doi               10.1039/c4sc00738g
_journal_volume                  5
_journal_year                    2014
_chemical_formula_moiety         '(C23 H27 Cl N S Ir) (C H2 Cl2)'
_chemical_formula_sum            'C24 H29 Cl3 Ir N S'
_chemical_formula_weight         662.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 104.557(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.730(2)
_cell_length_b                   14.462(3)
_cell_length_c                   16.791(4)
_cell_measurement_reflns_used    1016
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.51
_cell_volume                     2521.9(9)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex 2000 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  0.1584
_diffrn_reflns_av_sigmaI/netI    0.0879
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20722
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    5.707
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.292
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
absorption correction based on 13901 reflections(SADABS);Rint 0.2008 before
correction and 0.0851 after.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.805
_refine_diff_density_min         -1.924
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         5498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0434P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.0995
_reflns_number_gt                4688
_reflns_number_total             5498
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4sc00738g1.cif
_cod_data_source_block           04158a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/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        2521.8(9)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1516545