New class of RSO2-NHC ligands and Pd/RSO2-NHC complexes with tailored electronic properties and high performance in catalytic C-C and C-N bonds formation
Pasyukov, Dmitry; Shevchenko, Maxim; Astakhov, Alexander Vladimirovich; Minyaev, Mikhail Evgenevich; Zhang, Yu; Chernyshev, Victor; Ananikov, Valentine P.; Dalton Transactions  (2023) –; doi:10.1039/D3DT02296J

data_7713573
_publ_section_title
;
 New class of RSO2-NHC ligands and Pd/RSO2-NHC complexes with tailored
 electronic properties and high performance in catalytic C-C and C-N bonds
 formation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02296J
_journal_year                    2023
_chemical_formula_moiety         'C38 H45 Cl2 N3 O2 Pd S, C H2 Cl2'
_chemical_formula_sum            'C39 H47 Cl4 N3 O2 Pd S'
_chemical_formula_weight         870.05
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-04-06
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-04-09 deposited with the CCDC.	2023-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.4290(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.69119(14)
_cell_length_b                   19.42369(17)
_cell_length_c                   18.9969(2)
_cell_measurement_reflns_used    69757
_cell_measurement_temperature    99.98(17)
_cell_measurement_theta_max      35.7020
_cell_measurement_theta_min      2.2360
_cell_volume                     4115.87(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(17)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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    -50.00  50.00   0.50    3.50    --   23.58 -72.00  86.00  200
  2  \w     -3.00  98.00   0.50    3.50    --   23.58  72.00-143.00  202
  3  \w    -97.00   0.00   0.50    3.50    --  -22.95 -57.00  30.00  194
  4  \w    -57.00   5.00   0.50    3.50    --   23.58 -19.00 -60.00  124
  5  \w     42.00 102.00   0.50    3.50    --   23.58 178.00 120.00  120
  6  \w    -57.00   5.00   0.50    3.50    --   23.58 -19.00 -30.00  124
  7  \w     42.00 102.00   0.50    3.50    --   23.58 178.00  90.00  120
  8  \w    -97.00   0.00   0.50    3.50    --  -22.95 -57.00 -60.00  194
  9  \w    -23.00   2.00   0.50    3.50    --   23.58 -99.00 -90.00   50
 10  \w     39.00 103.00   0.50    3.50    --   23.58-178.00 -60.00  128
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0202309000
_diffrn_orient_matrix_UB_12      0.0258057000
_diffrn_orient_matrix_UB_13      -0.0273230000
_diffrn_orient_matrix_UB_21      -0.0585617000
_diffrn_orient_matrix_UB_22      -0.0142080000
_diffrn_orient_matrix_UB_23      -0.0097296000
_diffrn_orient_matrix_UB_31      -0.0143530000
_diffrn_orient_matrix_UB_32      0.0215733000
_diffrn_orient_matrix_UB_33      0.0262713000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            97310
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.750
_diffrn_reflns_theta_min         2.105
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.797
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.79a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.48
_refine_diff_density_max         1.219
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.00084(9)
_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   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     774
_refine_ls_number_reflns         16385
_refine_ls_number_restraints     1013
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0286
_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^)+(0.0278P)^2^+2.4181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0704
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15026
_reflns_number_total             16385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02296j2.cif
_cod_data_source_block           sm-499
_cod_database_code               7713573
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C39H47Cl4N3O2PdS
_chemical_oxdiff_usercomment     sm-499
_shelx_estimated_absorpt_t_max   0.701
_shelx_estimated_absorpt_t_min   0.586
_olex2_refinement_description
;
1. 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
2. Restrained distances
 C4-C5 \\sim C4-C9 \\sim C4A-C5A \\sim C4A-C9A \\sim C4B-C5B \\sim C4B-C9B
 with sigma of 0.003
 C5-C6 \\sim C8-C9 \\sim C5A-C6A \\sim C8A-C9A \\sim C5B-C6B \\sim C8B-C9B
 with sigma of 0.003
 C6-C7 \\sim C7-C8 \\sim C6A-C7A \\sim C7A-C8A \\sim C6B-C7B \\sim C7B-C8B
 with sigma of 0.003
 C5-C10 \\sim C9-C13 \\sim C5A-C10A \\sim C9A-C13A \\sim C5B-C10B \\sim C9B-C13B
 with sigma of 0.003
 C4-C7 \\sim C5-C8 \\sim C6-C9 \\sim C4A-C7A \\sim C5A-C8A \\sim C6A-C9A \\sim
C4B-C7B \\sim C5B-C8B \\sim C6B-
 C9B
 with sigma of 0.03
 C10-C11 \\sim C10-C12 \\sim C13-C14 \\sim C13-C15 \\sim C10A-C11A \\sim
C10A-C12A \\sim C13A-C14A ~
 C13A-C15A \\sim C10B-C11B \\sim C10B-C12B \\sim C13B-C14B \\sim C13B-C15B
 with sigma of 0.003
 C11-C12 \\sim C14-C15 \\sim C11A-C12A \\sim C14A-C15A \\sim C11B-C12B \\sim
C14B-C15B
 with sigma of 0.03
 C16-C17 \\sim C16-C21 \\sim C16A-C17A \\sim C16A-C21A \\sim C16B-C17B \\sim
C16B-C21B
 with sigma of 0.003
 C17-C18 \\sim C20-C21 \\sim C17A-C18A \\sim C20A-C21A \\sim C17B-C18B \\sim
C20B-C21B
 with sigma of 0.003
 C18-C19 \\sim C19-C20 \\sim C18A-C19A \\sim C19A-C20A \\sim C18B-C19B \\sim
C19B-C20B
 with sigma of 0.003
 C17-C22 \\sim C21-C25 \\sim C17A-C22A \\sim C21A-C25A \\sim C17B-C22B \\sim
C21B-C25B
 with sigma of 0.003
 C22-C23 \\sim C22-C24 \\sim C25-C26 \\sim C25-C27 \\sim C22A-C23A \\sim
C22A-C24A \\sim C25A-C26A ~
 C25A-C27A \\sim C22B-C23B \\sim C22B-C24B \\sim C25B-C26B \\sim C25B-C27B
 with sigma of 0.003
 C23-C24 \\sim C26-C27 \\sim C23A-C24A \\sim C26A-C27A \\sim C23B-C24B \\sim
C26B-C27B
 with sigma of 0.03
 C16-C19 \\sim C17-C20 \\sim C18-C21 \\sim C16A-C19A \\sim C17A-C20A \\sim
C18A-C21A \\sim C16B-C19B ~
 C17B-C20B \\sim C18B-C21B
 with sigma of 0.03
 C28-C29 \\sim C28-C33 \\sim C28A-C29A \\sim C28A-C33A \\sim C28B-C29B \\sim
C28B-C33B
 with sigma of 0.003
 C29-C30 \\sim C32-C33 \\sim C29A-C30A \\sim C32A-C33A \\sim C29B-C30B \\sim
C32B-C33B
 with sigma of 0.003
 C30-C31 \\sim C31-C32 \\sim C30A-C31A \\sim C31A-C32A \\sim C30B-C31B \\sim
C31B-C32B
 with sigma of 0.003
 C28-C31 \\sim C29-C32 \\sim C30-C33 \\sim C28A-C31A \\sim C29A-C32A \\sim
C30A-C33A \\sim C28B-C31B ~
 C29B-C32B \\sim C30B-C33B
 with sigma of 0.03
 N3-C34 \\sim N3-C38 \\sim N3A-C34A \\sim N3A-C38A \\sim N3B-C34B \\sim N3B-C38B
 with sigma of 0.003
 C34-C35 \\sim C37-C38 \\sim C34A-C35A \\sim C37A-C38A \\sim C34B-C35B \\sim
C37B-C38B
 with sigma of 0.003
 C35-C36 \\sim C36-C37 \\sim C35A-C36A \\sim C36A-C37A \\sim C35B-C36B \\sim
C36B-C37B
 with sigma of 0.003
 C39-Cl3 \\sim C39A-Cl3A \\sim C39B-Cl3B
 with sigma of 0.003
 C39-Cl4 \\sim C39A-Cl4A \\sim C39B-Cl4B
 with sigma of 0.003
 Cl3-Cl4 \\sim Cl3A-Cl4A \\sim Cl3B-Cl4B
 with sigma of 0.03
3. Restrained planarity
 N1, N2, C1, C2, C3
 with sigma of 0.005
 N1A, N2A, C1A, C2A, C3A
 with sigma of 0.005
 N1B, N2B, C1B, C2B, C3B
 with sigma of 0.005
 C4, C5, C6, C7, C8, C9
 with sigma of 0.005
 C4A, C5A, C6A, C7A, C8A, C9A
 with sigma of 0.005
 C4B, C5B, C6B, C7B, C8B, C9B
 with sigma of 0.005
 C16, C17, C18, C19, C20, C21
 with sigma of 0.005
 C16A, C17A, C18A, C19A, C20A, C21A
 with sigma of 0.005
 C16B, C17B, C18B, C19B, C20B, C21B
 with sigma of 0.005
 C28, C29, C30, C31, C32, C33
 with sigma of 0.005
 C28A, C29A, C30A, C31A, C32A, C33A
 with sigma of 0.005
 C28B, C29B, C30B, C31B, C32B, C33B
 with sigma of 0.005
 N3, C34, C35, C36, C37, C38
 with sigma of 0.005
 N3A, C34A, C35A, C36A, C37A, C38A
 with sigma of 0.005
 N3B, C34B, C35B, C36B, C37B, C38B
 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq,
Uanis(C16) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(C15) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C25) \\sim Ueq:
with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C26)
\\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.002 and sigma for terminal
atoms of 0.004
Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31)
\\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq: with sigma of 0.003 and
sigma for terminal atoms of 0.006
Uanis(N3) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq: with sigma of 0.003 and
sigma for terminal atoms of 0.006
Uanis(Pd1) = Uanis(Pd1A) = Uanis(Pd1B)
Uanis(Cl1) = Uanis(Cl1A) = Uanis(Cl1B)
Uanis(Cl2) = Uanis(Cl2A) = Uanis(Cl2B)
Uanis(N1) = Uanis(N1A) = Uanis(N1B)
Uanis(N2) = Uanis(N2A) = Uanis(N2B)
Uanis(C1) = Uanis(C1A) = Uanis(C1B)
Uanis(C2) = Uanis(C2A) = Uanis(C2B)
Uanis(C3) = Uanis(C3A) = Uanis(C3B)
Uanis(C4) = Uanis(C4A) = Uanis(C4B)
Uanis(C5) = Uanis(C5A) = Uanis(C5B)
Uanis(C6) = Uanis(C6A) = Uanis(C6B)
Uanis(C7) = Uanis(C7A) = Uanis(C7B)
Uanis(C8) = Uanis(C8A) = Uanis(C8B)
Uanis(C9) = Uanis(C9A) = Uanis(C9B)
Uanis(C10) = Uanis(C10A) = Uanis(C10B)
Uanis(C11) = Uanis(C11A) = Uanis(C11B)
Uanis(C12) = Uanis(C12A) = Uanis(C12B)
Uanis(C13) = Uanis(C13A) = Uanis(C13B)
Uanis(C14) = Uanis(C14A) = Uanis(C14B)
Uanis(C15) = Uanis(C15A) = Uanis(C15B)
Uanis(C16) = Uanis(C16A) = Uanis(C16B)
Uanis(C17) = Uanis(C17A) = Uanis(C17B)
Uanis(C18) = Uanis(C18A) = Uanis(C18B)
Uanis(C19) = Uanis(C19A) = Uanis(C19B)
Uanis(C20) = Uanis(C20A) = Uanis(C20B)
Uanis(C21) = Uanis(C21A) = Uanis(C21B)
Uanis(C22) = Uanis(C22A) = Uanis(C22B)
Uanis(C23) = Uanis(C23A) = Uanis(C23B)
Uanis(C24) = Uanis(C24A) = Uanis(C24B)
Uanis(C25) = Uanis(C25A) = Uanis(C25B)
Uanis(C26) = Uanis(C26A) = Uanis(C26B)
Uanis(C27) = Uanis(C27A) = Uanis(C27B)
Uanis(S1) = Uanis(S1A) = Uanis(S1B)
Uanis(O1) = Uanis(O1A) = Uanis(O1B)
Uanis(O2) = Uanis(O2A) = Uanis(O2B)
Uanis(C28) = Uanis(C28A) = Uanis(C28B)
Uanis(C29) = Uanis(C29A) = Uanis(C29B)
Uanis(C30) = Uanis(C30A) = Uanis(C30B)
Uanis(C31) = Uanis(C31A) = Uanis(C31B)
Uanis(C32) = Uanis(C32A) = Uanis(C32B)
Uanis(C33) = Uanis(C33A) = Uanis(C33B)
Uanis(N3) = Uanis(N3A) = Uanis(N3B)
Uanis(C34) = Uanis(C34A) = Uanis(C34B)
Uanis(C35) = Uanis(C35A) = Uanis(C35B)
Uanis(C36) = Uanis(C36A) = Uanis(C36B)
Uanis(C37) = Uanis(C37A) = Uanis(C37B)
Uanis(C38) = Uanis(C38A) = Uanis(C38B)
Uanis(Cl3) = Uanis(Cl3A) = Uanis(Cl3B)
Uanis(Cl4) = Uanis(Cl4A) = Uanis(Cl4B)
Uanis(C39) = Uanis(C39A) = Uanis(C39B)
5. Same fragment restrains
{Pd1, Cl1, Cl2, S1, O1, O2, N1, C1, N2, C2, C3, C4, C5, C6, C7, C8, C9, C10,
C11, C12, C13, C14, C15, C16, C17, C18, C19, C20, C21, C22, C23, C24, C25, C26,
C27, C28, C29, C30, C31, C32, C33, N3, C34, C35, C36, C37, C38} sigma for 1-2:
0.003, 1-3: 0.03
as in
{Pd1A, Cl1A, Cl2A, S1A, O1A, O2A, N1A, C1A, N2A, C2A, C3A, C4A, C5A, C6A, C7A,
C8A, C9A, C10A, C11A, C12A, C13A, C14A, C15A, C16A, C17A, C18A, C19A, C20A,
C21A, C22A, C23A, C24A, C25A, C26A, C27A, C28A, C29A, C30A, C31A, C32A, C33A,
N3A, C34A, C35A, C36A, C37A, C38A}
{Pd1, Cl1, Cl2, S1, O1, O2, N1, C1, N2, C2, C3, C4, C5, C6, C7, C8, C9, C10,
C11, C12, C13, C14, C15, C16, C17, C18, C19, C20, C21, C22, C23, C24, C25, C26,
C27, C28, C29, C30, C31, C32, C33, N3, C34, C35, C36, C37, C38} sigma for 1-2:
0.003, 1-3: 0.03
{Pd1A, Cl1A, Cl2A, S1A, O1A, O2A, N1A, C1A, N2A, C2A, C3A, C4A, C5A, C6A, C7A,
C8A, C9A, C10A, C11A, C12A, C13A, C14A, C15A, C16A, C17A, C18A, C19A, C20A,
C21A, C22A, C23A, C24A, C25A, C26A, C27A, C28A, C29A, C30A, C31A, C32A, C33A,
N3A, C34A, C35A, C36A, C37A, C38A} sigma for 1-2: 0.003, 1-3: 0.03
as in
{Pd1B, Cl1B, Cl2B, S1B, O1B, O2B, N1B, C1B, N2B, C2B, C3B, C4B, C5B, C6B, C7B,
C8B, C9B, C10B, C11B, C12B, C13B, C14B, C15B, C16B, C17B, C18B, C19B, C20B,
C21B, C22B, C23B, C24B, C25B, C26B, C27B, C28B, C29B, C30B, C31B, C32B, C33B,
N3B, C34B, C35B, C36B, C37B, C38B}
6. Others
 1*[Sof(Pd1)+Sof(Cl1)+Sof(Cl2)+Sof(S1)+Sof(O1)+Sof(O2)+Sof(N1)+Sof(C1)+Sof(N2)+
 Sof(C2)+Sof(C3)+Sof(H3)+Sof(C4)+Sof(C5)+Sof(C6)+Sof(H6)+Sof(C7)+Sof(H7)+
 Sof(C8)+Sof(H8)+Sof(C9)+Sof(C10)+Sof(H10)+Sof(C11)+Sof(H11A)+Sof(H11B)+
 Sof(H11C)+Sof(C12)+Sof(H12A)+Sof(H12B)+Sof(H12C)+Sof(C13)+Sof(H13)+Sof(C14)+
 Sof(H14A)+Sof(H14B)+Sof(H14C)+Sof(C15)+Sof(H15A)+Sof(H15B)+Sof(H15C)+Sof(C16)+
 Sof(C17)+Sof(C18)+Sof(H18)+Sof(C19)+Sof(H19)+Sof(C20)+Sof(H20)+Sof(C21)+
 Sof(C22)+Sof(H22)+Sof(C23)+Sof(H23A)+Sof(H23B)+Sof(H23C)+Sof(C24)+Sof(H24A)+
 Sof(H24B)+Sof(H24C)+Sof(C25)+Sof(H25)+Sof(C26)+Sof(H26A)+Sof(H26B)+Sof(H26C)+
 Sof(C27)+Sof(H27A)+Sof(H27B)+Sof(H27C)+Sof(C28)+Sof(C29)+Sof(H29)+Sof(C30)+
 Sof(H30)+Sof(C31)+Sof(H31)+Sof(C32)+Sof(H32)+Sof(C33)+Sof(H33)+Sof(N3)+
 Sof(C34)+Sof(H34)+Sof(C35)+Sof(H35)+Sof(C36)+Sof(H36)+Sof(C37)+Sof(H37)+
 Sof(C38)+Sof(H38)]+1*[Sof(Pd1A)+Sof(Cl1A)+Sof(Cl2A)+Sof(S1A)+Sof(O1A)+Sof(O2A)+
 Sof(N1A)+Sof(C1A)+Sof(N2A)+Sof(C2A)+Sof(C3A)+Sof(H3A)+Sof(C4A)+Sof(C5A)+
 Sof(C6A)+Sof(H6A)+Sof(C7A)+Sof(H7A)+Sof(C8A)+Sof(H8A)+Sof(C9A)+Sof(C10A)+
 Sof(H10A)+Sof(C11A)+Sof(H11D)+Sof(H11E)+Sof(H11F)+Sof(C12A)+Sof(H12D)+
 Sof(H12E)+Sof(H12F)+Sof(C13A)+Sof(H13A)+Sof(C14A)+Sof(H14D)+Sof(H14E)+
 Sof(H14F)+Sof(C15A)+Sof(H15D)+Sof(H15E)+Sof(H15F)+Sof(C16A)+Sof(C17A)+
 Sof(C18A)+Sof(H18A)+Sof(C19A)+Sof(H19A)+Sof(C20A)+Sof(H20A)+Sof(C21A)+
 Sof(C22A)+Sof(H22A)+Sof(C23A)+Sof(H23D)+Sof(H23E)+Sof(H23F)+Sof(C24A)+
 Sof(H24D)+Sof(H24E)+Sof(H24F)+Sof(C25A)+Sof(H25A)+Sof(C26A)+Sof(H26D)+
 Sof(H26E)+Sof(H26F)+Sof(C27A)+Sof(H27D)+Sof(H27E)+Sof(H27F)+Sof(C28A)+
 Sof(C29A)+Sof(H29A)+Sof(C30A)+Sof(H30A)+Sof(C31A)+Sof(H31A)+Sof(C32A)+
 Sof(H32A)+Sof(C33A)+Sof(H33A)+Sof(N3A)+Sof(C34A)+Sof(H34A)+Sof(C35A)+Sof(H35A)+
 Sof(C36A)+Sof(H36A)+Sof(C37A)+Sof(H37A)+Sof(C38A)+Sof(H38A)]+1*[Sof(Pd1B)+
 Sof(Cl1B)+Sof(Cl2B)+Sof(S1B)+Sof(O1B)+Sof(O2B)+Sof(N1B)+Sof(C1B)+Sof(N2B)+
 Sof(C2B)+Sof(C3B)+Sof(H3B)+Sof(C4B)+Sof(C5B)+Sof(C6B)+Sof(H6B)+Sof(C7B)+
 Sof(H7B)+Sof(C8B)+Sof(H8B)+Sof(C9B)+Sof(C10B)+Sof(H10B)+Sof(C11B)+Sof(H11G)+
 Sof(H11H)+Sof(H11I)+Sof(C12B)+Sof(H12G)+Sof(H12H)+Sof(H12I)+Sof(C13B)+
 Sof(H13B)+Sof(C14B)+Sof(H14G)+Sof(H14H)+Sof(H14I)+Sof(C15B)+Sof(H15G)+
 Sof(H15H)+Sof(H15I)+Sof(C16B)+Sof(C17B)+Sof(C18B)+Sof(H18B)+Sof(C19B)+
 Sof(H19B)+Sof(C20B)+Sof(H20B)+Sof(C21B)+Sof(C22B)+Sof(H22B)+Sof(C23B)+
 Sof(H23G)+Sof(H23H)+Sof(H23I)+Sof(C24B)+Sof(H24G)+Sof(H24H)+Sof(H24I)+
 Sof(C25B)+Sof(H25B)+Sof(C26B)+Sof(H26G)+Sof(H26H)+Sof(H26I)+Sof(C27B)+
 Sof(H27G)+Sof(H27H)+Sof(H27I)+Sof(C28B)+Sof(C29B)+Sof(H29B)+Sof(C30B)+
 Sof(H30B)+Sof(C31B)+Sof(H31B)+Sof(C32B)+Sof(H32B)+Sof(C33B)+Sof(H33B)+Sof(N3B)+
 Sof(C34B)+Sof(H34B)+Sof(C35B)+Sof(H35B)+Sof(C36B)+Sof(H36B)+Sof(C37B)+
 Sof(H37B)+Sof(C38B)+Sof(H38B)]=1 with esd of 0.000001
 1*[Sof(Cl3)+Sof(Cl4)+Sof(C39)+Sof(H39A)+Sof(H39B)]+1*[Sof(Cl3A)+Sof(Cl4A)+
 Sof(C39A)+Sof(H1)+Sof(H2)]+1*[Sof(Cl3B)+Sof(Cl4B)+Sof(C39B)+Sof(H39C)+
 Sof(H39D)]=1 with esd of 0.000001
 Sof(Pd1)=Sof(Cl1)=Sof(Cl2)=Sof(S1)=Sof(O1)=Sof(O2)=Sof(N1)=Sof(C1)=Sof(N2)=
 Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=
 Sof(C8)=Sof(H8)=Sof(C9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11A)=Sof(H11B)=
 Sof(H11C)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13)=Sof(H13)=Sof(C14)=
 Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)=
 Sof(C17)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=Sof(C21)=
 Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=
 Sof(H24B)=Sof(H24C)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C28)=Sof(C29)=Sof(H29)=Sof(C30)=
 Sof(H30)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(N3)=
 Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35)=Sof(C36)=Sof(H36)=Sof(C37)=Sof(H37)=
 Sof(C38)=Sof(H38)=FVAR(1)
 Sof(Pd1A)=Sof(Cl1A)=Sof(Cl2A)=Sof(S1A)=Sof(O1A)=Sof(O2A)=Sof(N1A)=Sof(C1A)=
 Sof(N2A)=Sof(C2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(C5A)=Sof(C6A)=Sof(H6A)=
 Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=
 Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=
 Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C15A)=
 Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16A)=Sof(C17A)=Sof(C18A)=Sof(H18A)=
 Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(C22A)=Sof(H22A)=
 Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24A)=Sof(H24D)=Sof(H24E)=
 Sof(H24F)=Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=
 Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C28A)=Sof(C29A)=Sof(H29A)=
 Sof(C30A)=Sof(H30A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=
 Sof(H33A)=Sof(N3A)=Sof(C34A)=Sof(H34A)=Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36A)=
 Sof(C37A)=Sof(H37A)=Sof(C38A)=Sof(H38A)=FVAR(2)
 Sof(Pd1B)=Sof(Cl1B)=Sof(Cl2B)=Sof(S1B)=Sof(O1B)=Sof(O2B)=Sof(N1B)=Sof(C1B)=
 Sof(N2B)=Sof(C2B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(C5B)=Sof(C6B)=Sof(H6B)=
 Sof(C7B)=Sof(H7B)=Sof(C8B)=Sof(H8B)=Sof(C9B)=Sof(C10B)=Sof(H10B)=Sof(C11B)=
 Sof(H11G)=Sof(H11H)=Sof(H11I)=Sof(C12B)=Sof(H12G)=Sof(H12H)=Sof(H12I)=
 Sof(C13B)=Sof(H13B)=Sof(C14B)=Sof(H14G)=Sof(H14H)=Sof(H14I)=Sof(C15B)=
 Sof(H15G)=Sof(H15H)=Sof(H15I)=Sof(C16B)=Sof(C17B)=Sof(C18B)=Sof(H18B)=
 Sof(C19B)=Sof(H19B)=Sof(C20B)=Sof(H20B)=Sof(C21B)=Sof(C22B)=Sof(H22B)=
 Sof(C23B)=Sof(H23G)=Sof(H23H)=Sof(H23I)=Sof(C24B)=Sof(H24G)=Sof(H24H)=
 Sof(H24I)=Sof(C25B)=Sof(H25B)=Sof(C26B)=Sof(H26G)=Sof(H26H)=Sof(H26I)=
 Sof(C27B)=Sof(H27G)=Sof(H27H)=Sof(H27I)=Sof(C28B)=Sof(C29B)=Sof(H29B)=
 Sof(C30B)=Sof(H30B)=Sof(C31B)=Sof(H31B)=Sof(C32B)=Sof(H32B)=Sof(C33B)=
 Sof(H33B)=Sof(N3B)=Sof(C34B)=Sof(H34B)=Sof(C35B)=Sof(H35B)=Sof(C36B)=Sof(H36B)=
 Sof(C37B)=Sof(H37B)=Sof(C38B)=Sof(H38B)=FVAR(3)
 Sof(Cl3)=Sof(Cl4)=Sof(C39)=Sof(H39A)=Sof(H39B)=FVAR(4)
 Sof(Cl3A)=Sof(Cl4A)=Sof(C39A)=Sof(H1)=Sof(H2)=FVAR(5)
 Sof(Cl3B)=Sof(Cl4B)=Sof(C39B)=Sof(H39C)=Sof(H39D)=FVAR(6)
7.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25), C10A(H10A), C13A(H13A), C22A(H22A),
 C25A(H25A), C10B(H10B), C13B(H13B), C22B(H22B), C25B(H25B)
7.b Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C39A(H1,H2), C39B(H39C,H39D)
7.c Me refined with riding coordinates:
 C23A(H23D,H23E,H23F), C24A(H24D,H24E,H24F), C26A(H26D,H26E,H26F), C27A(H27D,
 H27E,H27F), C23B(H23G,H23H,H23I), C24B(H24G,H24H,H24I), C26B(H26G,H26H,H26I),
 C27B(H27G,H27H,H27I)
7.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C29(H29),
 C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37),
  C38(H38), C3A(H3A), C6A(H6A), C7A(H7A), C8A(H8A), C18A(H18A), C19A(H19A),
 C20A(H20A), C29A(H29A), C30A(H30A), C31A(H31A), C32A(H32A), C33A(H33A),
 C34A(H34A), C35A(H35A), C36A(H36A), C37A(H37A), C38A(H38A), C3B(H3B), C6B(H6B),
  C7B(H7B), C8B(H8B), C18B(H18B), C19B(H19B), C20B(H20B), C29B(H29B),
 C30B(H30B), C31B(H31B), C32B(H32B), C33B(H33B), C34B(H34B), C35B(H35B),
 C36B(H36B), C37B(H37B), C38B(H38B)
7.e Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C11A(H11D,H11E,H11F), C12A(H12D,H12E,H12F), C14A(H14D,H14E,H14F),
 C15A(H15D,H15E,H15F), C11B(H11G,H11H,H11I), C12B(H12G,H12H,H12I), C14B(H14G,
 H14H,H14I), C15B(H15G,H15H,H15I)
;
_shelx_res_checksum              98329
_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 1.333
_oxdiff_exptl_absorpt_empirical_full_min 0.749