Dirhodium(II)-Catalyzed Sulfide Oxygenations: Catalyst Removal by Coprecipitation with Sulfoxides.
Zhao, Lili; Zhang, Hongyang; Wang, Yuanhua; The Journal of organic chemistry 81 (2016) 129–136; doi:10.1021/acs.joc.5b02400

data_4036517
_publ_section_title
;
 Dirhodium(II)-Catalyzed Sulfide Oxygenations: Catalyst Removal by
 Coprecipitation with Sulfoxides.
;
_journal_issue                   1
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              129
_journal_page_last               136
_journal_paper_doi               10.1021/acs.joc.5b02400
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         'C24 H30 O6 Rh S, C8 H10 O2 S'
_chemical_formula_sum            'C32 H40 O8 Rh S2'
_chemical_formula_weight         719.67
_space_group_crystal_system      triclinic
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_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
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_diffrn_ambient_temperature      208.26(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
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_diffrn_measurement_details
;
  1 omega   -1.00   83.00   1.0000   15.4400
omega____ theta____ kappa____ phi______ frames
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  2 omega  -54.00   85.00   1.0000   15.4400
omega____ theta____ kappa____ phi______ frames
    -       15.5694    0.0000  -30.0000 139

  3 omega  -11.00   83.00   1.0000   15.4400
omega____ theta____ kappa____ phi______ frames
    -       15.5694   77.0000  120.0000 94

  4 omega  -20.00   55.00   1.0000   15.4400
omega____ theta____ kappa____ phi______ frames
    -       15.5694  -99.0000   30.0000 75

  5 omega   -3.00   85.00   1.0000   15.4400
omega____ theta____ kappa____ phi______ frames
    -       15.5694   38.0000    0.0000 88

  6 omega  -63.00  -38.00   1.0000   15.4400
omega____ theta____ kappa____ phi______ frames
    -      -16.5069  112.0000  171.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_orient_matrix_UB_11      0.0626275000
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_diffrn_orient_matrix_UB_31      0.0139630000
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_diffrn_orient_matrix_UB_33      0.0109634000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_Laue_measured_fraction_full 0.985
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_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
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_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16561
_diffrn_reflns_point_group_measured_fraction_full 0.985
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_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.344
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.707
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_exptl_absorpt_correction_T_min  0.86623
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description
;
;
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_refine_ls_number_reflns         6506
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_refine_ls_restrained_S_all      1.050
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+1.4867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.0783
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_reflns_threshold_expression     'I > 2\s(I)'
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_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00M(H00d,H00f), C00P(H00g,H00j)
2.b Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00H(H00H), C00I(H00I), C00O(H00O), C00S(H00S), C00T(H00T),
 C00U(H00U), C00V(H00V), C00Z(H00Z), C014(H014), C015(H015), C016(H016)
2.c Idealised Me refined as rotating group:
 C00G(H00a,H00b,H00c), C00W(H00k,H00l,H00m), C00Y(H00n,H00p,H00q), C010(H01a,
 H01b,H01c), C011(H01d,H01e,H01f), C012(H01g,H01h,H01i), C013(H01j,H01k,H01l),
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;
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_olex2_submission_special_instructions 'No special instructions were received'