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_4305365
_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 O4 Rh S4, F6 P, C3 H6 O'
_chemical_formula_sum            'C23 H50 F6 O5 P Rh S4'
_chemical_formula_weight         782.79
_chemical_name_common            '[Rh(BTSE)2][PF6]'
_chemical_name_systematic
; 
[Rh(BTSE)2][PF6] 3
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.6747(2)
_cell_length_b                   22.5346(3)
_cell_length_c                   24.0876(4)
_cell_measurement_reflns_used    9360
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.55
_cell_volume                     6879.88(18)
_computing_cell_refinement       HKL
_computing_data_collection       'Collect package Bruker - Nonius'
_computing_data_reduction        HKL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.061
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9478
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_T_max  0.9200
_exptl_absorpt_correction_T_min  0.7849
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SHELXL-97 (Sheldrick, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3248
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.057
_refine_diff_density_min         -1.355
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         6491
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0702
_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^)+(0.0719P)^2^+45.9072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1790
_refine_ls_wR_factor_ref         0.1841
_reflns_number_gt                5474
_reflns_number_total             6491
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800354q-file001_4.cif
_cod_data_source_block           m806a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_Hall     -P2n2ab
_cod_database_code               4305365