Development of highly efficient and selective palladium catalysts for telomerization of 1,3-butadiene with alcohols
Souza, Edson Leonardo Scarpa de; Ahrens, Sebastian; Spannenberg, Anke; Neumann, Helfried; Junge, Kathrin; Correia, Carlos Roque Duarte; Jackstell, Ralf; Beller, Matthias; Chemical Communications 61 (2025) 9083–9086; doi:10.1039/D5CC01036E

data_7134492
_publ_section_title
;
 Development of highly efficient and selective palladium catalysts for
 telomerization of 1,3-butadiene with alcohols
;
_journal_issue                   50
_journal_name_full               'Chemical Communications'
_journal_page_first              9083
_journal_page_last               9086
_journal_paper_doi               10.1039/D5CC01036E
_journal_volume                  61
_journal_year                    2025
_chemical_formula_sum            'C11 H13 O3 P'
_chemical_formula_weight         224.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/1
_audit_update_record
;
2024-03-11 deposited with the CCDC.	2025-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.8044(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5361(4)
_cell_length_b                   8.4344(3)
_cell_length_c                   12.6771(5)
_cell_measurement_reflns_used    9619
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      68.19
_cell_measurement_theta_min      5.09
_cell_volume                     1113.28(7)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         microfocus
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14767
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.208
_diffrn_reflns_theta_min         4.246
_exptl_absorpt_coefficient_mu    2.080
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       prism
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 1780 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4055
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0250
_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^)+(0.0483P)^2^+0.0743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0681
_refine_ls_wR_factor_ref         0.0692
_reflns_Friedel_coverage         0.852
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                3937
_reflns_number_total             4055
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01036e2.cif
_cod_data_source_block           AX2646
_cod_depositor_comments          'Adding full bibliography for 7134492.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7134492
_shelx_shelxl_version_number     2019/1
_shelx_res_checksum              78867
_shelx_hkl_checksum              86886