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_1552097
_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         'C52 H46 O4 P2 Pd2'
_chemical_formula_sum            'C52 H46 O4 P2 Pd2'
_chemical_formula_weight         1009.63
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-31 deposited with the CCDC.    2019-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.5561(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0527(2)
_cell_length_b                   23.8864(4)
_cell_length_c                   17.0272(2)
_cell_measurement_reflns_used    7467
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      70.8940
_cell_measurement_theta_min      5.4970
_cell_volume                     4432.96(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      110.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -67.00  26.00   1.00    5.00    --    0.00 -37.00   0.00   93
  2  \w    -11.00  25.00   1.00    5.00    --    0.00  57.00 -30.00   36
  3  \w    -16.00  28.00   1.00   18.00    --   54.00 -77.00-180.00   44
  4  \w     37.00  85.00   1.00   18.00    --   54.00  57.00 120.00   48
  5  \w     29.00 118.00   1.00   18.00    --   54.00  37.00 -90.00   89
  6  \w     40.00  99.00   1.00   18.00    --   54.00-125.00-150.00   59
  7  \w     28.00  70.00   1.00   18.00    --   54.00-128.00 -21.00   42
  8  \w     51.00 130.00   1.00   18.00    --  108.00 -50.00 -60.00   79
  9  \w     83.00 110.00   1.00   18.00    --  108.00-111.00  60.00   27
 10  \w    101.00 171.00   1.00   18.00    --  108.00  63.00   0.00   70
 11  \w    106.00 140.00   1.00   18.00    --  108.00 -91.00 -60.00   34
 12  \w     82.00 109.00   1.00   18.00    --  108.00-111.00   0.00   27
 13  \w     44.00 100.00   1.00   18.00    --  108.00 -91.00 -60.00   56
 14  \w    105.00 173.00   1.00   18.00    --  108.00  63.00  60.00   68
 15  \w     37.00  63.00   1.00   18.00    --  108.00-111.00   0.00   26
 16  \w    111.00 177.00   1.00   18.00    --  108.00  50.00  30.00   66
 17  \w    105.00 177.00   1.00   18.00    --  108.00 111.00-120.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0396391000
_diffrn_orient_matrix_UB_12      -0.0618537000
_diffrn_orient_matrix_UB_13      0.0015795000
_diffrn_orient_matrix_UB_21      -0.1352585000
_diffrn_orient_matrix_UB_22      -0.0179453000
_diffrn_orient_matrix_UB_23      -0.0223039000
_diffrn_orient_matrix_UB_31      0.0104684000
_diffrn_orient_matrix_UB_32      0.0034703000
_diffrn_orient_matrix_UB_33      -0.0889799000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16871
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.069
_diffrn_reflns_theta_max         67.069
_diffrn_reflns_theta_min         3.701
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.587
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.358
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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 light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       needle
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.028
_exptl_crystal_size_min          0.019
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         7909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0243
_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^)+(0.0243P)^2^+1.5463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6909
_reflns_number_total             7909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01847f2.cif
_cod_data_source_block           ijsf1818
_cod_original_cell_volume        4432.98(13)
_cod_database_code               1552097
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C52 H46 O4 P2 Pd2'
_chemical_oxdiff_usercomment     'Neil NWJS-4-273-precipitate2'
_reflns_odcompleteness_completeness 99.91
_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:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32),
 C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42),
  C43(H43), C44(H44), C45(H45), C46(H46), C48(H48), C49(H49), C50(H50),
 C51(H51), C52(H52)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              24277
_olex2_date_sample_data_collection 2018-09-19
_olex2_exptl_crystal_mounting_method 'oil on 200 micrometre micromount'
_olex2_submission_original_sample_id NWJS-4-273-precipitate2
_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 1.507
_oxdiff_exptl_absorpt_empirical_full_min 0.796