Degradation of the active species in the catalytic system Pd(OAc)2/NEt3
Sanmartin, Jesus; Gonzalez, Concepcion; Briones-Miguéns, Lucía; Fondo, Matilde; Garcia-Deibe, Ana M.; RSC Adv.  (2016) –; doi:10.1039/C6RA20886J

data_7226934
_publ_section_title
;
 Degradation of the active species in the catalytic system Pd(OAc)2/NEt3
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA20886J
_journal_year                    2016
_chemical_formula_moiety         'C28 H30 N4 O4 Pd S2'
_chemical_formula_sum            'C28 H30 N4 O4 Pd S2'
_chemical_formula_weight         657.08
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2016-09-05 deposited with the CCDC.
2016-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.652(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.8995(15)
_cell_length_b                   8.5875(19)
_cell_length_c                   22.797(4)
_cell_measurement_reflns_used    1268
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.758
_cell_measurement_theta_min      2.538
_cell_volume                     1335.3(5)
_computing_cell_refinement       'BRUKER APEX2'
_computing_data_collection       'BRUKER APEX2'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2016/4 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8 KappaAPEXII'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_unetI/netI     0.0939
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9929
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.707
_diffrn_reflns_theta_max         24.707
_diffrn_reflns_theta_min         1.807
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.895
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_description       needle
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.388
_refine_diff_density_min         -1.466
_refine_diff_density_rms         0.195
_refine_ls_extinction_coef       0.0048(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2264
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0692
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0894P)^2^+4.2760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1561
_refine_ls_wR_factor_ref         0.1794
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1593
_reflns_number_total             2264
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra20886j2.cif
_cod_data_source_block           pdAts_2
_cod_original_cell_volume        1335.4(5)
_cod_database_code               7226934
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.739
_shelx_estimated_absorpt_t_max   0.965
_shelx_res_checksum              14504