(In situ) spectroscopic studies on state-of-the-art Pd(ii) catalysts in solution for the alkoxycarbonylation of alkenes
Kucmierczyk, Peter; Behrens, Stephan; Kubis, Christoph; Baumann, Wolfgang; Wei, Zhihong; Jiao, Haijun; Dong, Kaiwu; Spannenberg, Anke; Neumann, Helfried; Jackstell, Ralf; Börner, Armin; Franke, Robert; Beller, Matthias; Catalysis Science & Technology 12 (2022) 3175–3189; doi:10.1039/D0CY02248A

data_1566690
_publ_section_title
;
 (In situ) spectroscopic studies on state-of-the-art Pd(ii) catalysts in
 solution for the alkoxycarbonylation of alkenes
;
_journal_issue                   10
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              3175
_journal_page_last               3189
_journal_paper_doi               10.1039/D0CY02248A
_journal_volume                  12
_journal_year                    2022
_chemical_formula_sum            'C28 H34 F6 N2 O6 P2 Pd S2'
_chemical_formula_weight         841.03
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-06-19 deposited with the CCDC.	2022-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                73.9005(13)
_cell_angle_beta                 72.8892(13)
_cell_angle_gamma                73.6404(12)
_cell_formula_units_Z            2
_cell_length_a                   11.2734(7)
_cell_length_b                   12.1729(7)
_cell_length_c                   13.5903(8)
_cell_measurement_reflns_used    9027
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.31
_cell_volume                     1671.40(17)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0107
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            55544
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         1.604
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.853
_exptl_absorpt_correction_T_max  0.76
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       prism
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.432
_exptl_crystal_size_mid          0.402
_exptl_crystal_size_min          0.336
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         8068
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0201
_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^)+(0.0233P)^2^+1.1737P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0501
_refine_ls_wR_factor_ref         0.0506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7804
_reflns_number_total             8068
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cy02248a2.cif
_cod_data_source_block           AX1611
_cod_depositor_comments
'Adding full bibliography for 1566688--1566690.cif.'
_cod_database_code               1566690
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              82385