The ubiquitous cross-coupling catalyst system ‘Pd(OAc)2’/2PPh3 forms a unique dinuclear PdI complex: an important entry point into catalytically competent cyclic Pd3 clusters
Scott, Neil W. J.; Ford, Mark J.; Schotes, Christoph; Parker, Rachel R.; Whitwood, Adrian C.; Fairlamb, Ian J. S.; Chemical Science  (2019) –; doi:10.1039/C9SC01847F

data_1552096
_publ_section_title
;
 The ubiquitous cross-coupling catalyst system
 &#x2018;Pd(OAc)2&#x2019;/2PPh3 forms a unique dinuclear PdI complex: an
 important entry point into catalytically competent cyclic Pd3 clusters
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC01847F
_journal_year                    2019
_chemical_formula_moiety         'C40 H36 O4 P2 Pd'
_chemical_formula_sum            'C40 H36 O4 P2 Pd'
_chemical_formula_weight         749.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-01-31 deposited with the CCDC.    2019-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.765(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6975(2)
_cell_length_b                   15.0053(3)
_cell_length_c                   19.3767(3)
_cell_measurement_reflns_used    5912
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      70.5410
_cell_measurement_theta_min      4.7970
_cell_volume                     3389.33(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -28.00  21.00   1.00    1.50    --    0.00 -57.00 -30.00   49
  2  \w     32.00 107.00   1.00    4.50    --   54.00-125.00  60.00   75
  3  \w     49.00  77.00   1.00    4.50    --  108.00-111.00  60.00   28
  4  \w     37.00 114.00   1.00    4.50    --  108.00-111.00 120.00   77
  5  \w     46.00 136.00   1.00    4.50    --  108.00 -77.00 150.00   90
  6  \w    130.00 156.00   1.00    4.50    --  108.00  25.00   0.00   26
  7  \w    108.00 172.00   1.00    4.50    --  108.00  62.00 -61.00   64
  8  \w     99.00 140.00   1.00    4.50    --  108.00 -25.00-150.00   41
  9  \w     48.00  97.00   1.00    4.50    --  108.00 -50.00 -90.00   49
 10  \w     35.00  84.00   1.00    4.50    --  108.00 -25.00-150.00   49
 11  \w     23.00  78.00   1.00    4.50    --   54.00-125.00 -60.00   55
 12  \w      9.00  69.00   1.00    4.50    --   54.00 -57.00 120.00   60
 13  \w     90.00 148.00   1.00    4.50    --  108.00  50.00  60.00   58
 14  \w     68.00  96.00   1.00    4.50    --  108.00 178.00 -30.00   28
 15  \w     31.00 123.00   1.00    4.50    --   54.00  77.00  90.00   92
 16  \w    -26.00  15.00   1.00    1.50    --    0.00  91.00 171.00   41
 17  \w    -61.00 -34.00   1.00    1.50    --    0.00 -57.00 -30.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1005092000
_diffrn_orient_matrix_UB_12      -0.0483546000
_diffrn_orient_matrix_UB_13      0.0304178000
_diffrn_orient_matrix_UB_21      -0.0184754000
_diffrn_orient_matrix_UB_22      -0.0565909000
_diffrn_orient_matrix_UB_23      -0.0663276000
_diffrn_orient_matrix_UB_31      0.0836956000
_diffrn_orient_matrix_UB_32      -0.0707040000
_diffrn_orient_matrix_UB_33      0.0323649000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12675
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.065
_diffrn_reflns_theta_max         67.065
_diffrn_reflns_theta_min         3.731
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.641
_exptl_absorpt_correction_T_max  0.865
_exptl_absorpt_correction_T_min  0.698
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.193
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.066
_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         6044
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0334P)^2^+1.5655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0743
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5295
_reflns_number_total             6044
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01847f2.cif
_cod_data_source_block           ijsf1807a
_cod_database_code               1552096
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C86 H73 O2 P5 Pd3'
_chemical_oxdiff_usercomment     'Neil Scott nwjs-3-204-recryst'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C36(H36), C14(H14), C9(H9), C16(H16), C12(H12), C17(H17), C15(H15), C32(H32),
 C35(H35), C10(H10), C18(H18), C2(H2), C24(H24), C8(H8), C20(H20), C34(H34),
 C11(H11), C6(H6), C29(H29), C22(H22), C28(H28), C33(H33), C25(H25), C27(H27),
 C23(H23), C21(H21), C5(H5), C3(H3), C4(H4), C26(H26)
2.b Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C40(H40A,H40B,H40C)
;
_olex2_date_sample_data_collection 2018-03-16
_olex2_date_sample_submission    2018-03-12
_olex2_exptl_crystal_mounting_method 'oil on micromount '
_olex2_submission_original_sample_id 'Neil Scott -3-204-recrys'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.765
_oxdiff_exptl_absorpt_empirical_full_min 0.814