Oxidation of a Monomethylpalladium(II) Complex with O2 in Water: Tuning Reaction Selectivity to Form Ethane, Methanol, or Methylhydroperoxide.
Sberegaeva, Anna V.; Zavalij, Peter Y.; Vedernikov, Andrei N.; Journal of the American Chemical Society 138 (2016) 1446–1455; doi:10.1021/jacs.5b12832

data_4130027
_publ_section_title
;
 Oxidation of a Monomethylpalladium(II) Complex with O2 in Water: Tuning
 Reaction Selectivity to Form Ethane, Methanol, or Methylhydroperoxide.
;
_journal_issue                   4
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1446
_journal_page_last               1455
_journal_paper_doi               10.1021/jacs.5b12832
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C14 H18 N2 O3 Pd S2, C H4 O'
_chemical_formula_sum            'C15 H22 N2 O4 Pd S2'
_chemical_formula_weight         464.86
_chemical_name_common            Pd-complex
_chemical_name_systematic
;
Pd-complex 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 & ZCIF'
_cell_angle_alpha                90
_cell_angle_beta                 90.1712(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2940(8)
_cell_length_b                   11.7682(10)
_cell_length_c                   16.3112(14)
_cell_measurement_reflns_used    19995
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.1
_cell_measurement_theta_min      2.5
_cell_volume                     1784.0(3)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2010)'
_computing_data_reduction        Apex2
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  SHELXL-2012
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'ShelXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_detector_type            'Bruker Smart Apex II'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0468308
_diffrn_orient_matrix_UB_12      0.0763951
_diffrn_orient_matrix_UB_13      -0.0031687
_diffrn_orient_matrix_UB_21      -0.0046500
_diffrn_orient_matrix_UB_22      0.0030253
_diffrn_orient_matrix_UB_23      0.0612066
_diffrn_orient_matrix_UB_31      0.0967591
_diffrn_orient_matrix_UB_32      0.0370928
_diffrn_orient_matrix_UB_33      0.0016097
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29714
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.997
_diffrn_reflns_theta_min         2.134
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.296
_exptl_absorpt_correction_T_max  0.802
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             944
_exptl_crystal_id                'Vedern-Sbereg Pd-complex H2O,MeOH 150K'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.00080(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         5204
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0176
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+1.8450P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0393
_refine_ls_wR_factor_ref         0.0398
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4937
_reflns_number_total             5204
_reflns_threshold_expression     'I > 2\s(I)'
_iucr_refine_instructions_details 'See _shelx_res_file'
_cod_data_source_file            ja5b12832_si_001.cif
_cod_data_source_block           2340
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4130027
_diffrn_reflns_sigmai/neti       0.0129
_shelxl_version_number           2012-4
_shelx_res_checksum              88220
_shelx_hkl_checksum              19808