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_1569520
_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 H49 B N2 O2 P2 Pd'
_chemical_formula_sum            'C27 H49 B N2 O2 P2 Pd'
_chemical_formula_weight         612.83
_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'
_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                90
_cell_angle_beta                 112.762(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8927(7)
_cell_length_b                   19.9252(9)
_cell_length_c                   13.4943(8)
_cell_measurement_reflns_used    18120
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      27.6010
_cell_measurement_theta_min      1.9180
_cell_volume                     2948.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (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  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      93.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_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     39.00  70.00   0.50   40.00    --   20.00  54.00  60.00   62
  2  \w    -74.00 -25.00   0.50   40.00    --   20.00  54.00-180.00   98
  3  \w     81.00 107.00   0.50   40.00    --   20.00  54.00-180.00   52
  4  \w    -63.00   4.00   0.50   40.00    --   20.00  54.00-120.00  134
  5  \w     38.00  63.00   0.50   40.00    --   20.00  54.00-120.00   50
  6  \w    -68.00 110.00   0.50   40.00    --   20.00  54.00   0.00  356
  7  \w    -74.00 108.00   0.50   40.00    --   20.00  54.00 120.00  364
  8  \w    -66.00 -36.00   0.50   40.00    --   20.00  54.00-150.00   60
  9  \w     23.00  60.00   0.50   40.00    --   20.00  54.00-150.00   74
 10  \w    -72.00 -44.00   0.50   40.00    --   20.00  54.00 -30.00   56
 11  \w    -25.00   2.00   0.50   40.00    --   20.00  54.00 -30.00   54
 12  \w     26.00  58.00   0.50   40.00    --   20.00  54.00 -30.00   64
 13  \w    -65.00 -11.00   0.50   40.00    --   20.00  54.00 -90.00  108
 14  \w     -2.00  24.00   0.50   40.00    --   20.00  54.00 -90.00   52
 15  \w     43.00  68.00   0.50   40.00    --   20.00  54.00 -90.00   50
 16  \w     74.00  99.00   0.50   40.00    --   20.00  54.00 -90.00   50
 17  \w    -10.00  61.00   0.50   40.00    --   20.00  54.00  30.00  142
 18  \w     33.00  58.00   0.50   40.00    --   20.00  54.00  90.00   50
 19  \w    -70.00 -44.00   0.50   40.00    --   20.00  54.00  60.00   52
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0276125000
_diffrn_orient_matrix_UB_12      0.0144742000
_diffrn_orient_matrix_UB_13      -0.0330590000
_diffrn_orient_matrix_UB_21      0.0560923000
_diffrn_orient_matrix_UB_22      0.0026300000
_diffrn_orient_matrix_UB_23      0.0451277000
_diffrn_orient_matrix_UB_31      0.0166836000
_diffrn_orient_matrix_UB_32      -0.0324513000
_diffrn_orient_matrix_UB_33      -0.0109584000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            41375
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         1.930
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
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    1.380
_exptl_crystal_description       plate
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         6766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0295
_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^)+(0.0272P)^2^+1.2630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0627
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5659
_reflns_number_total             6766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01459b3.cif
_cod_data_source_block           mini2-22004
_cod_depositor_comments
'Adding full bibliography for 1569513--1569521.cif.'
_cod_database_code               1569520
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.832
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C10(H10A,H10B), C11(H11A,H11B)
1.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8)
1.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), 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              27615
_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 1.430
_oxdiff_exptl_absorpt_empirical_full_min 0.844