Comparative study of CO<sub>2</sub> insertion into pincer supported palladium alkyl and aryl complexes.
Deziel, Anthony P.; Gahlawat, Sahil; Hazari, Nilay; Hopmann, Kathrin H.; Mercado, Brandon Q.; Chemical science 14 (2023) 8164–8179; doi:10.1039/d3sc01459b

data_1569516
_publ_section_title
;
 Comparative study of CO<sub>2</sub> insertion into pincer supported
 palladium alkyl and aryl complexes.
;
_journal_issue                   30
_journal_name_full               'Chemical science'
_journal_page_first              8164
_journal_page_last               8179
_journal_paper_doi               10.1039/d3sc01459b
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C54 H98 B2 N4 P4 Pd2, 4(C6 H6)'
_chemical_formula_sum            'C78 H122 B2 N4 P4 Pd2'
_chemical_formula_weight         1474.09
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     SHELXT
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-05-23
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-05-23 deposited with the CCDC.	2023-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                85.337(2)
_cell_angle_beta                 79.407(3)
_cell_angle_gamma                89.959(2)
_cell_formula_units_Z            1
_cell_length_a                   9.9648(3)
_cell_length_b                   13.3134(4)
_cell_length_c                   14.9073(4)
_cell_measurement_reflns_used    16009
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.5810
_cell_measurement_theta_min      3.1030
_cell_volume                     1937.34(10)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.988
_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     88.00 118.00   0.50    0.54    --  110.65  61.00 150.00   60
  2  \w    101.00 165.00   0.50    0.54    --  110.65  61.00  90.00  128
  3  \w     98.00 177.00   0.50    0.54    --  110.65  30.00  60.00  158
  4  \w     34.00  92.00   0.50    0.54    --  110.65   0.00 -90.00  116
  5  \w     96.00 133.00   0.50    0.54    --  110.65   0.00 -90.00   74
  6  \w    146.00 172.00   0.50    0.54    --  110.65   0.00 -90.00   52
  7  \w     91.00 134.00   0.50    0.54    --  110.65  45.00   0.00   86
  8  \w    106.00 136.00   0.50    0.54    --  110.65  96.00 100.00   60
  9  \w     34.00  74.00   0.50    0.54    --  110.65 -61.00 150.00   80
 10  \w     34.00  72.00   0.50    0.54    --  110.65 -61.00   0.00   76
 11  \w     36.00  63.00   0.50    0.54    --  110.65 -61.00-150.00   54
 12  \w     41.00  68.00   0.50    0.54    --  110.65 -77.00-150.00   54
 13  \w     67.00 105.00   0.50    0.54    --  110.65 -95.00-150.00   76
 14  \w     37.00  67.00   0.50    0.54    --  110.65-125.00-120.00   60
 15  \w     40.00 110.00   0.50    0.54    --  110.65-125.00 -60.00  140
 16  \w     42.00 105.00   0.50    0.54    --  110.65-125.00 -30.00  126
 17  \w     51.00  76.00   0.50    0.54    --  113.75-107.00  78.14   50
 18  \w     80.00 108.00   0.50    0.54    --  113.75-107.00  78.14   56
 19  \w     82.00 107.00   0.50    0.54    --  113.75-105.00 139.78   50
 20  \w     44.00  69.00   0.50    0.54    --  113.75-105.00 139.78   50
 21  \w     39.00 105.00   0.50    0.54    --  110.65 -95.00 150.00  132
 22  \w      6.00  33.00   0.50    0.14    --   46.49 -96.00  -8.00   54
 23  \w     47.00  72.00   0.50    0.54    --  110.65 -96.00  -8.00   50
 24  \w     38.00 105.00   0.50    0.54    --  110.65 -95.00 -30.00  134
 25  \w     79.00 106.00   0.50    0.54    --  113.75 -95.00   7.35   54
 26  \w     48.00  73.00   0.50    0.54    --  113.75 -95.00   7.35   50
 27  \w     37.00 102.00   0.50    0.54    --  110.65 -95.00  90.00  130
 28  \w    -19.00  35.00   0.50    0.14    --  -47.24  19.00-150.00  108
 29  \w    -48.00  -7.00   0.50    0.54    --  -84.13  45.00-150.00   82
 30  \w    -68.00 -43.00   0.50    0.54    --  -84.13  61.00-150.00   50
 31  \w    -72.00 -33.00   0.50    0.54    --  -84.13  77.00-120.00   78
 32  \w    -33.00  -8.00   0.50    0.54    --  -84.13  45.00 -90.00   50
 33  \w   -101.00 -61.00   0.50    0.54    --  -84.13  77.00   0.00   80
 34  \w   -101.00 -31.00   0.50    0.54    --  -84.13  77.00  60.00  140
 35  \w    -33.00  -1.00   0.50    0.54    --  -84.13  30.00 120.00   64
 36  \w    -32.00  -4.00   0.50    0.54    --  -84.13  30.00  90.00   56
 37  \w    -31.00  -2.00   0.50    0.54    --  -84.13  30.00  60.00   58
 38  \w    -33.00  -1.00   0.50    0.54    --  -84.13  30.00  30.00   64
 39  \w    -33.00  -1.00   0.50    0.54    --  -84.13  30.00   0.00   64
 40  \w    -33.00  -2.00   0.50    0.54    --  -84.13  30.00 -30.00   62
 41  \w    -20.00  36.00   0.50    0.14    --  -47.24  19.00 -30.00  112
 42  \w    -33.00  -8.00   0.50    0.54    --  -84.13  30.00 -60.00   50
 43  \w    -33.00  -8.00   0.50    0.54    --  -84.13  30.00 -90.00   50
 44  \w    -28.00  -1.00   0.50    0.54    --  -84.13  30.00-120.00   54
 45  \w   -150.00-108.00   0.50    0.54    --  -84.13 -96.00  -8.00   84
 46  \w   -122.00 -73.00   0.50    0.14    --  -47.24-125.00 -60.00   98
 47  \w   -100.00 -75.00   0.50    0.14    --  -47.24-125.00 150.00   50
 48  \w   -113.00 -77.00   0.50    0.14    --  -47.24-125.00 120.00   72
 49  \w    -80.00  -5.00   0.50    0.14    --  -47.24  96.00 100.00  150
 50  \w    -69.00 -41.00   0.50    0.54    --  -84.13  96.00 100.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0477240000
_diffrn_orient_matrix_UB_12      -0.0788218000
_diffrn_orient_matrix_UB_13      -0.0687551000
_diffrn_orient_matrix_UB_21      0.0662983000
_diffrn_orient_matrix_UB_22      0.0844502000
_diffrn_orient_matrix_UB_23      -0.0711010000
_diffrn_orient_matrix_UB_31      0.1344241000
_diffrn_orient_matrix_UB_32      -0.0116924000
_diffrn_orient_matrix_UB_33      0.0367092000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17232
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.604
_diffrn_reflns_theta_min         3.026
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.841
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87240
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.961
_refine_diff_density_min         -1.051
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         17232
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0806P)^2^+0.1100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1160
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15357
_reflns_number_total             17232
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9447\% 
around [-0.00 1.00 0.00] (reciprocal) or [0.02 1.00 -0.07] (direct)
;
_cod_data_source_file            d3sc01459b3.cif
_cod_data_source_block           syn-23079
_cod_depositor_comments
'Adding full bibliography for 1569513--1569521.cif.'
_cod_database_code               1569516
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.643
_shelx_estimated_absorpt_t_min   0.219
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5716(7)
 0.4284(7)
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 Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C10(H10A,H10B), C11(H11A,H11B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C7(H7), C8(H8), C28(H28), C29(H29), C30(H30),
 C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
  C39(H39)
3.c X=CH2 refined with riding coordinates:
 C3(H3A,H3B)
3.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,
 H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C),
 C27(H27A,H27B,H27C)
;
_shelx_res_checksum              70883
_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 1.304
_oxdiff_exptl_absorpt_empirical_full_min 0.732
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2