Efficient Pd-Catalyzed Dehydrogenative Coupling of P(O)H with RSH: A Precise Construction of P(O)-S Bonds.
Zhu, Yueyue; Chen, Tieqiao; Li, Shan; Shimada, Shigeru; Han, Li-Biao; Journal of the American Chemical Society 138 (2016) 5825–5828; doi:10.1021/jacs.6b03112

data_4130413
_publ_section_title
;
 Efficient Pd-Catalyzed Dehydrogenative Coupling of P(O)H with RSH: A
 Precise Construction of P(O)-S Bonds.
;
_journal_issue                   18
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5825
_journal_page_last               5828
_journal_paper_doi               10.1021/jacs.6b03112
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C24 H47 O3 P3 Pd S'
_chemical_formula_sum            'C24 H47 O3 P3 Pd S'
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_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
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_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 96.237(6)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   18.133(12)
_cell_length_b                   11.428(7)
_cell_length_c                   29.728(19)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      28.43
_cell_measurement_theta_min      2.18
_cell_volume                     6124(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
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_computing_structure_solution    'DIRDIF99-PATTY (Gould, et al., 1999)'
_diffrn_ambient_temperature      183(2)
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_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_type           'Mo K\a'
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_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_theta_max         28.461
_diffrn_reflns_theta_min         1.378
_diffrn_standards_decay_%        0.0
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_exptl_absorpt_correction_T_min  0.6759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
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_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bulk
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_exptl_crystal_size_max          0.500
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_refine_ls_number_reflns         7218
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_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0216P)^2^+7.8192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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