(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_1566688
_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            'C29.4 H40.8 Cl8.8 N2 P2 Pd'
_chemical_formula_weight         902.54
_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'
_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                90
_cell_angle_beta                 108.5348(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2620(6)
_cell_length_b                   12.8154(5)
_cell_length_c                   20.9917(8)
_cell_measurement_reflns_used    9858
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      2.59
_cell_volume                     3892.8(3)
_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  0.0269
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            50050
_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         1.453
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.187
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       prism
_exptl_crystal_F_000             1827
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.255
_exptl_crystal_size_min          0.162
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         9395
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+4.0629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0837
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8028
_reflns_number_total             9395
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cy02248a2.cif
_cod_data_source_block           AX1608
_cod_depositor_comments
'Adding full bibliography for 1566688--1566690.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C29.40 H40.80 Cl8.80 N2 P2 Pd'
_cod_database_code               1566688
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              26610