Oxidative addition of activated aryl-carboxylates to Pd(0): divergent reactivity dependant on temperature and structure.
Becica, Joseph; Gaube, Gregory; Sabbers, William A.; Leitch, David C.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 16067–16071; doi:10.1039/d0dt01119c

data_7704088
_publ_section_title
;
 Oxidative addition of activated aryl-carboxylates to Pd(0): divergent
 reactivity dependant on temperature and structure.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16067
_journal_page_last               16071
_journal_paper_doi               10.1039/d0dt01119c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C44 H74 O4 P2 Pd'
_chemical_formula_sum            'C44 H74 O4 P2 Pd'
_chemical_formula_weight         835.37
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-08-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-11 deposited with the CCDC.	2020-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5817(11)
_cell_length_b                   17.9358(17)
_cell_length_c                   21.123(2)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.850
_cell_measurement_theta_min      2.24
_cell_volume                     4387.8(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.04
_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  0.0303
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            86378
_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         27.869
_diffrn_reflns_theta_min         1.489
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.534
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0519 before and 0.0370 after correction. The Ratio of minimum to maximum transmission is 0.9551. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.410(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         10479
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0190
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0188P)^2^+1.3486P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0428
_refine_ls_wR_factor_ref         0.0435
_reflns_Friedel_coverage         0.810
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                10106
_reflns_number_total             10479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01119c2.cif
_cod_data_source_block           solve_a
_cod_depositor_comments
'Adding full bibliography for 7704088--7704089.cif.'
_cod_original_cell_volume        4387.9(7)
_cod_database_code               7704088
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.901
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.590(13)
 0.410(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C9(H9), C39(H39), C21(H21), C15(H15), C33(H33), C27(H27)
3.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B), C10(H10A,H10B), C20(H20A,
 H20B), C35(H35A,H35B), C22(H22A,H22B), C26(H26A,H26B), C17(H17A,H17B),
 C19(H19A,H19B), C44(H44A,H44B), C34(H34A,H34B), C40(H40A,H40B), C36(H36A,H36B),
  C16(H16A,H16B), C18(H18A,H18B), C38(H38A,H38B), C37(H37A,H37B), C13(H13A,
 H13B), C25(H25A,H25B), C24(H24A,H24B), C23(H23A,H23B), C43(H43A,H43B),
 C31(H31A,H31B), C41(H41A,H41B), C32(H32A,H32B), C28(H28A,H28B), C42(H42A,H42B),
  C29(H29A,H29B), C30(H30A,H30B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              49239
_olex2_submission_special_instructions 'No special instructions were received'