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_4305362
_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         'C22H30F6N2O2PRhS2 *1/2 CH2Cl2'
_chemical_formula_sum            'C22.5 H31 Cl F6 N2 O2 P Rh S2'
_chemical_formula_weight         708.94
_chemical_name_common            '[Rh(BTSE)(1,10-phenanthroline)][PF6]'
_chemical_name_systematic
; 
[Rh(BTSE)(1,10-phenanthroline)][PF6] 14
;
_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                 109.557(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6477(10)
_cell_length_b                   10.7513(6)
_cell_length_c                   20.2994(16)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      50.8
_cell_measurement_theta_min      2.2
_cell_volume                     2806.7(4)
_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 0.932
_diffrn_measured_fraction_theta_max 0.932
_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  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0162
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25593
_diffrn_reflns_theta_full        25.90
_diffrn_reflns_theta_max         25.90
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.974
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.405
_refine_diff_density_min         -1.174
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         5084
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0627P)^2^+3.8919P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.0992
_reflns_number_gt                4505
_reflns_number_total             5084
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800354q-file001_1.cif
_cod_data_source_block           ts138x
_cod_original_cell_volume        2806.7(3)
_cod_original_formula_sum        'C22.50 H31 Cl F6 N2 O2 P Rh S2'
_cod_database_code               4305362