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_1569515
_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         'C27 H51 B N2 P2 Pd'
_chemical_formula_sum            'C27 H51 B N2 P2 Pd'
_chemical_formula_weight         582.84
_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             2023-02-20
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-02-21 deposited with the CCDC.	2023-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                104.2180(10)
_cell_angle_beta                 94.7470(10)
_cell_angle_gamma                100.4430(10)
_cell_formula_units_Z            2
_cell_length_a                   7.85480(10)
_cell_length_b                   11.08790(10)
_cell_length_c                   17.8239(2)
_cell_measurement_reflns_used    10726
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      77.7390
_cell_measurement_theta_min      2.5770
_cell_volume                     1466.62(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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_temperature      93.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.999
_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     38.00 109.00   0.50    0.21    --   99.22-125.00  30.00  142
  2  \w     49.00 105.00   0.50    0.21    --   99.22-125.00-150.00  112
  3  \w    -26.00  35.00   0.50    0.21    --  -47.25  19.00 -60.00  122
  4  \w    -26.00  33.00   0.50    0.21    --  -47.25  19.00   0.00  118
  5  \w    -26.00  36.00   0.50    0.21    --  -47.25  19.00  60.00  124
  6  \w     32.00  57.00   0.50    0.21    --   46.75-106.00  58.00   50
  7  \w     85.00 111.00   0.50    0.21    --  109.90-125.00 -30.00   52
  8  \w     47.00  97.00   0.50    0.21    --  109.90 -95.00-150.00  100
  9  \w     45.00 104.00   0.50    0.21    --   99.22-106.00  58.00  118
 10  \w     46.00  72.00   0.50    0.21    --  109.90-106.00  58.00   52
 11  \w     81.00 107.00   0.50    0.21    --   88.00-104.00 176.22   52
 12  \w     23.00  48.00   0.50    0.21    --   88.00-104.00 176.22   50
 13  \w     43.00  98.00   0.50    0.21    --  109.90 -77.00  90.00  110
 14  \w     36.00  67.00   0.50    0.21    --  109.90 -61.00  30.00   62
 15  \w     45.00  70.00   0.50    0.21    --  109.90 -61.00 -30.00   50
 16  \w     28.00  64.00   0.50    0.21    --   99.22 -61.00 -90.00   72
 17  \w     18.00  43.00   0.50    0.21    --   99.22 -45.00-150.00   50
 18  \w     19.00  51.00   0.50    0.21    --   99.22 -45.00-180.00   64
 19  \w     42.00  85.00   0.50    0.21    --  109.90 -77.00-120.00   86
 20  \w     33.00  58.00   0.50    0.21    --  109.90 -61.00 -60.00   50
 21  \w     24.00  50.00   0.50    0.21    --   99.22 -45.00  60.00   52
 22  \w     18.00  46.00   0.50    0.21    --   99.22 -45.00  90.00   56
 23  \w    125.00 174.00   0.50    0.21    --  109.90  45.00 -60.00   98
 24  \w    123.00 177.00   0.50    0.21    --  109.90  30.00-180.00  108
 25  \w     85.00 111.00   0.50    0.21    --  109.90  30.00-180.00   52
 26  \w    128.00 178.00   0.50    0.21    --  109.90  30.00  60.00  100
 27  \w     80.00 106.00   0.50    0.21    --  109.90  30.00  60.00   52
 28  \w    122.00 147.00   0.50    0.21    --  109.90 106.00 156.00   50
 29  \w    115.00 140.00   0.50    0.21    --   99.22 106.00 156.00   50
 30  \w     95.00 120.00   0.50    0.21    --   99.22 125.00  60.00   50
 31  \w    141.00 167.00   0.50    0.21    --   99.22 125.00  60.00   52
 32  \w    -69.00  -7.00   0.50    0.21    --  -84.11  61.00 150.00  124
 33  \w    -33.00  -2.00   0.50    0.21    --  -84.11  30.00  90.00   62
 34  \w    -34.00  -3.00   0.50    0.21    --  -84.11  30.00  60.00   62
 35  \w    -35.00 -10.00   0.50    0.21    --  -84.11  30.00 120.00   50
 36  \w    -35.00 -10.00   0.50    0.21    --  -84.11  30.00  30.00   50
 37  \w    -35.00  -1.00   0.50    0.21    --  -84.11  30.00   0.00   68
 38  \w    -32.00  -1.00   0.50    0.21    --  -84.11  30.00 -30.00   62
 39  \w    -35.00 -10.00   0.50    0.21    --  -84.11  30.00 -90.00   50
 40  \w    -33.00  -1.00   0.50    0.21    --  -84.11  30.00-150.00   64
 41  \w    -82.00 -20.00   0.50    0.21    --  -84.11 125.00-150.00  124
 42  \w    -57.00   0.00   0.50    0.21    --  -47.25 106.00 156.00  114
 43  \w    -69.00 -44.00   0.50    0.21    --  -84.11 106.00 156.00   50
 44  \w   -145.00-120.00   0.50    0.21    --  -84.11-106.00  58.00   50
 45  \w   -111.00 -85.00   0.50    0.21    --  -47.25-125.00  30.00   52
;
_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      0.0260947000
_diffrn_orient_matrix_UB_12      -0.1185684000
_diffrn_orient_matrix_UB_13      0.0262532000
_diffrn_orient_matrix_UB_21      0.0324578000
_diffrn_orient_matrix_UB_22      -0.0641058000
_diffrn_orient_matrix_UB_23      -0.0830621000
_diffrn_orient_matrix_UB_31      0.1968786000
_diffrn_orient_matrix_UB_32      0.0575423000
_diffrn_orient_matrix_UB_33      0.0224912000
_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  0.0389
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15470
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.589
_diffrn_reflns_theta_max         66.589
_diffrn_reflns_theta_min         2.580
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.247
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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    1.320
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         5183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0249
_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^)+(0.0229P)^2^+0.5164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0605
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4831
_reflns_number_total             5183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01459b3.cif
_cod_data_source_block           syn-23013_auto
_cod_depositor_comments
'Adding full bibliography for 1569513--1569521.cif.'
_cod_database_code               1569515
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N B P Pd'
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.574
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C12(H12A,H12B), C19(H19A,H19B)
1.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17)
1.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), 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              99807
_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 1.485
_oxdiff_exptl_absorpt_empirical_full_min 0.710