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_1575143
_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         'C25 H25 O4 P Pd'
_chemical_formula_sum            'C25 H25 O4 P Pd'
_chemical_formula_weight         526.82
_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                 106.90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6970(3)
_cell_length_b                   9.2164(2)
_cell_length_c                   18.8878(4)
_cell_measurement_reflns_used    51495
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      28.323
_cell_measurement_theta_min      2.168
_cell_volume                     2281.37(9)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0258
_diffrn_reflns_av_unetI/netI     0.0112
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            69767
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.328
_diffrn_reflns_theta_min         2.254
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.912
_exptl_absorpt_correction_T_max  0.9819
_exptl_absorpt_correction_T_min  0.8036
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1056 before and 0.0440 after correction.
The Ratio of minimum to maximum transmission is 0.8184.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       Block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.303
_exptl_crystal_size_mid          0.269
_exptl_crystal_size_min          0.142
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.00174(18)
_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   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         5676
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0175
_refine_ls_R_factor_gt           0.0166
_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^)+(0.0141P)^2^+1.6112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0405
_refine_ls_wR_factor_ref         0.0410
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5471
_reflns_number_total             5676
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc02171e2.cif
_cod_data_source_block           acacpdacpph3_a
_cod_depositor_comments
'Adding full bibliography for 1575141--1575143.cif.'
_cod_original_cell_volume        2281.42(9)
_cod_database_code               1575143
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.881
_shelx_estimated_absorpt_t_min   0.770
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1A(0.042) H1B(0.042) H1C(0.042) H3(0.026) H5A(0.038) H5B(0.038)
 H5C(0.038) H7A(0.039) H7B(0.039) H7C(0.039) H9(0.021) H10(0.026) H11(0.026)
 H12(0.026) H13(0.021) H15(0.024) H16(0.028) H17(0.028) H18(0.026) H19(0.021)
 H21(0.029) H22(0.036) H23(0.031) H24(0.026) H25(0.021)
 Fixed X: H1A(0.518794) H1B(0.466448) H1C(0.583948) H3(0.336695) H5A(0.211002)
 H5B(0.196921) H5C(0.20173) H7A(0.600425) H7B(0.494912) H7C(0.494862)
 H9(0.858931) H10(0.882131) H11(0.776858) H12(0.644666) H13(0.619887)
 H15(0.724359) H16(0.817643) H17(0.938069) H18(0.965274) H19(0.875345)
 H21(0.879271) H22(0.970671) H23(0.927206) H24(0.789462) H25(0.696486)
 Fixed Y: H1A(0.729661) H1B(0.806561) H1C(0.759822) H3(0.635816) H5A(0.359306)
 H5B(0.506777) H5C(0.354754) H7A(-0.123244) H7B(-0.109945) H7C(-0.154892)
 H9(0.280325) H10(0.142533) H11(-0.057045) H12(-0.115114) H13(0.022488)
 H15(0.504369) H16(0.720085) H17(0.775912) H18(0.617138) H19(0.397982)
 H21(0.050696) H22(-0.065809) H23(-0.026964) H24(0.12255) H25(0.238193)
 Fixed Z: H1A(0.486867) H1B(0.409115) H1C(0.430467) H3(0.361046) H5A(0.256934)
 H5B(0.297616) H5C(0.339435) H7A(0.263633) H7B(0.199243) H7C(0.281073)
 H9(0.574297) H10(0.682373) H11(0.682544) H12(0.576701) H13(0.468545)
 H15(0.52291) H16(0.548919) H17(0.487171) H18(0.398496) H19(0.373897)
 H21(0.454942) H22(0.38403) H23(0.256354) H24(0.198722) H25(0.268909)
;
_shelx_res_checksum              45855
_olex2_submission_special_instructions 'No special instructions were received'