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_4036516
_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 H27.36 O6 Rh S'
_chemical_formula_sum            'C24 H30 O6 Rh S'
_chemical_formula_weight         549.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
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Olex2 1.2
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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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_computing_data_reduction
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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_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_diffrn_detector                 'CCD plate'
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;
  1 omega  -11.00   83.00   1.0000   42.5400
omega____ theta____ kappa____ phi______ frames
    -       15.5694   77.0000  -60.0000 94

  2 omega  -11.00   83.00   1.0000   42.5400
omega____ theta____ kappa____ phi______ frames
    -       15.5694   77.0000   60.0000 94

  3 omega  -11.00   83.00   1.0000   42.5400
omega____ theta____ kappa____ phi______ frames
    -       15.5694   77.0000 -180.0000 94

  4 omega    8.00   44.00   1.0000   42.5400
omega____ theta____ kappa____ phi______ frames
    -      -16.5069   77.0000 -180.0000 36
;
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_orient_matrix_UB_33      -0.0379556000
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.867
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
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_diffrn_reflns_number            16528
_diffrn_reflns_point_group_measured_fraction_full 0.998
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.231
_diffrn_reflns_theta_min         3.383
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.814
_exptl_absorpt_correction_T_max  1.00000
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
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Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            'dull reddish red'
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_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.482
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;
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_exptl_crystal_F_000             1132
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_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.983
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_restraints     0
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_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+0.2090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           201506-qy-1
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_cod_database_code               4036516
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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. Others
 Sof(H00O)=Sof(H00Q)=Sof(H00R)=Sof(S0)=1-FVAR(1)
 Sof(S002)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C00G(H00A,H00B), C00O(H00M,H00N)
3.b Me refined with riding coordinates:
 C00Q(H00O,H00Q,H00R)
3.c Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00H(H00H), C00J(H00J), C00L(H00L), C00P(H00P), C00R(H00S),
 C00S(H00T)
3.d Idealised Me refined as rotating group:
 C00M(H00C,H00D,H00F), C00N(H00G,H00I,H00K), C00T(H00U,H00V,H00W), C00U(H00X,
 H00Y,H), C00W(H00,HA,HB)
;
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_olex2_date_sample_data_collection 2015-06-09
_olex2_submission_special_instructions 'No special instructions were received'