Insights into the mechanism of active catalyst generation for the Pd<sup>II</sup>(acac)<sub>2</sub>/PPh<sub>3</sub> system in the context of telomerization of 1,3-butadiene.
Bouley, Bailey S.; Bae, Dae Young; Chakrabarti, Sagnik; Rosen, Mari; Kennedy, Robert D.; Mirica, Liviu M.; Chemical science 16 (2025) 15486–15498; doi:10.1039/d5sc02171e

data_1575142
_publ_section_title
;
 Insights into the mechanism of active catalyst generation for the
 Pd<sup>II</sup>(acac)<sub>2</sub>/PPh<sub>3</sub> system in the context
 of telomerization of 1,3-butadiene.
;
_journal_issue                   34
_journal_name_full               'Chemical science'
_journal_page_first              15486
_journal_page_last               15498
_journal_paper_doi               10.1039/d5sc02171e
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C30 H33 O6 P Pd'
_chemical_formula_sum            'C30 H33 O6 P Pd'
_chemical_formula_weight         626.93
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-08-09 deposited with the CCDC.	2025-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.2350(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9495(4)
_cell_length_b                   15.9935(6)
_cell_length_c                   16.2962(6)
_cell_measurement_reflns_used    8664
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.27
_cell_volume                     2816.81(18)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture/Photon II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25172
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.367
_diffrn_reflns_theta_min         2.274
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6541
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0768 before and 0.0596 after correction.
The Ratio of minimum to maximum transmission is 0.8778.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.136
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.053
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       0.00021(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         5167
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0081P)^2^+4.7524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0664
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4188
_reflns_number_total             5167
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc02171e2.cif
_cod_data_source_block           p21n_a
_cod_depositor_comments
'Adding full bibliography for 1575141--1575143.cif.'
_cod_database_code               1575142
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.904
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C21(H21)
1.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C28(H28)
1.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              74043
_olex2_submission_special_instructions 'No special instructions were received'