Evidence for Suzuki-Miyaura cross-couplings catalyzed by ligated Pd<sub>3</sub>-clusters: from cradle to grave.
Jeddi, Neda; Scott, Neil W. J.; Tanner, Theo; Beaumont, Simon K.; Fairlamb, Ian J. S.; Chemical science 15 (2024) 2763–2777; doi:10.1039/d3sc06447f

data_1570781
_publ_section_title
;
 Evidence for Suzuki-Miyaura cross-couplings catalyzed by ligated
 Pd<sub>3</sub>-clusters: from cradle to grave.
;
_journal_issue                   8
_journal_name_full               'Chemical science'
_journal_page_first              2763
_journal_page_last               2777
_journal_paper_doi               10.1039/d3sc06447f
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C78 H65 Cl P5 Pd3, F6 Sb'
_chemical_formula_sum            'C78 H65 Cl F6 P5 Pd3 Sb'
_chemical_formula_weight         1747.55
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-07-12 deposited with the CCDC.	2024-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.5087(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.28922(15)
_cell_length_b                   16.70934(13)
_cell_length_c                   27.2586(2)
_cell_measurement_reflns_used    13102
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      70.8370
_cell_measurement_theta_min      4.1820
_cell_volume                     6950.78(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (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 0.998
_diffrn_measured_fraction_theta_max 0.980
_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    -30.00  16.00   1.00    2.50    --    0.00  77.00-180.00   46
  2  \w    -26.00  39.00   1.00    2.50    --    0.00  77.00   0.00   65
  3  \w     35.00 121.00   1.00   10.00    --   54.00  57.00-180.00   86
  4  \w     35.00  75.00   1.00   10.00    --   54.00 -57.00 150.00   40
  5  \w     10.00 119.00   1.00   10.00    --   54.00  19.00 120.00  109
  6  \w     54.00  98.00   1.00   10.00    --   54.00-125.00 -90.00   44
  7  \w     29.00  56.00   1.00   10.00    --   54.00-125.00 150.00   27
  8  \w    108.00 149.00   1.00   10.00    --  108.00  77.00   0.00   41
  9  \w    104.00 152.00   1.00   10.00    --  108.00  77.00  60.00   48
 10  \w     38.00  79.00   1.00   10.00    --  108.00 -77.00  30.00   41
 11  \w     64.00 127.00   1.00   10.00    --  108.00 -63.00  30.00   63
 12  \w     61.00 142.00   1.00   10.00    --  108.00 178.00  30.00   81
 13  \w     84.00 175.00   1.00   10.00    --  108.00  37.00-180.00   91
 14  \w    110.00 177.00   1.00   10.00    --  108.00  77.00  30.00   67
 15  \w     89.00 114.00   1.00   10.00    --  108.00 -77.00  30.00   25
 16  \w     67.00 132.00   1.00   10.00    --  108.00 178.00  60.00   65
;
_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      -0.0991324000
_diffrn_orient_matrix_UB_12      0.0101839000
_diffrn_orient_matrix_UB_13      -0.0120613000
_diffrn_orient_matrix_UB_21      0.0190184000
_diffrn_orient_matrix_UB_22      0.0572718000
_diffrn_orient_matrix_UB_23      -0.0423410000
_diffrn_orient_matrix_UB_31      0.0011359000
_diffrn_orient_matrix_UB_32      -0.0715335000
_diffrn_orient_matrix_UB_33      -0.0356089000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            28086
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.214
_diffrn_reflns_theta_min         3.923
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.152
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.63a (Rigaku Oxford Diffraction, 2019)
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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       plate
_exptl_crystal_F_000             3472
_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.036
_refine_diff_density_max         1.164
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         13206
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+4.7090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0827
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11559
_reflns_number_total             13206
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06447f2.cif
_cod_data_source_block           ijsf1923
_cod_depositor_comments          'Adding full bibliography for 1570781.cif.'
_cod_original_cell_volume        6950.79(11)
_cod_database_code               1570781
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'c78 h65 Cl1 f6 p5 Pd3 Sb1'
_chemical_oxdiff_usercomment     'Neda Jeddi NEJ-1-ab62-low concentrated'
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C36(H36), C66(H66), C38(H38), C60(H60), C2(H2), C65(H65), C56(H56), C54(H54),
 C71(H71), C68(H68), C20(H20), C26(H26), C17(H17), C51(H51), C53(H53), C4(H4),
 C62(H62), C59(H59), C72(H72), C42(H42), C76(H76), C39(H39), C78(H78), C27(H27),
  C63(H63), C77(H77), C64(H64), C35(H35), C34(H34), C48(H48), C14(H14),
 C32(H32), C3(H3), C30(H30), C52(H52), C18(H18), C40(H40), C44(H44), C57(H57),
 C41(H41), C28(H28), C8(H8), C6(H6), C5(H5), C69(H69), C58(H58), C33(H33),
 C50(H50), C74(H74), C45(H45), C9(H9), C21(H21), C24(H24), C12(H12), C22(H22),
 C70(H70), C11(H11), C75(H75), C16(H16), C29(H29), C47(H47), C15(H15), C23(H23),
  C46(H46), C10(H10)
;
_shelx_res_checksum              98880
_olex2_date_sample_data_collection 2019-11-15
_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 1.424
_oxdiff_exptl_absorpt_empirical_full_min 0.779