Synthesis, Structure, and Reactivity of Rhodium and Iridium Complexes of the Chelating Bis-Sulfoxide tBuSOC2H4SOtBu. Selective O-H Activation of 2-Hydroxy-isopropyl-pyridine
Thomas Schaub; Yael Diskin-Posner; Udo Radius; David Milstein; Inorganic Chemistry 47 (2008) 6502–6512; doi:10.1021/ic800354q

data_4305364
_publ_contact_author_address
;Department of Organic Chemistry
Weizmann Institute of Science
76100 Rehovot
Israel
;
_publ_contact_author_email       david.milstein@weizmann.ac.il
_publ_contact_author_name        'David Milstein'
_publ_section_title
;
Synthesis, Structure, and Reactivity of Rhodium and Iridium Complexes of
the Chelating Bis-Sulfoxide tBuSOC2H4SOtBu. Selective O-H Activation of
2-Hydroxy-isopropyl-pyridine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6502
_journal_page_last               6512
_journal_paper_doi               10.1021/ic800354q
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C20 H44 Cl2 Ir2 O4 S4'
_chemical_formula_sum            'C20 H44 Cl2 Ir2 O4 S4'
_chemical_formula_weight         932.09
_chemical_name_common            '[Ir2(BTSE)2Cl2]'
_chemical_name_systematic
; 
[Ir2(BTSE)2Cl2] 2
;
_space_group_IT_number           170
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 65'
_symmetry_space_group_name_H-M   'P 65'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   21.6261(8)
_cell_length_b                   21.6261(8)
_cell_length_c                   11.7931(15)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      25.6
_cell_measurement_theta_min      2.0
_cell_volume                     4776.6(7)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'STOE IPDS 1'
_diffrn_measurement_method       rotation
_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  0.0561
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            37326
_diffrn_reflns_theta_full        25.96
_diffrn_reflns_theta_max         25.96
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    8.802
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.944
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.515
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.160
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.013(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         6165
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0208
_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^)+(0.0349P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0573
_refine_ls_wR_factor_ref         0.0584
_reflns_number_gt                3097
_reflns_number_total             3285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800354q-file001_3.cif
_cod_data_source_block           ts108z
_cod_original_cell_volume        4776.6(6)
_cod_database_code               4305364