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_1569521
_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         'C30 H49 B N2 P2 Pd'
_chemical_formula_sum            'C30 H49 B N2 P2 Pd'
_chemical_formula_weight         616.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                 103.208(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.5512(13)
_cell_length_b                   8.0925(2)
_cell_length_c                   21.4368(6)
_cell_measurement_reflns_used    36116
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      68.5360
_cell_measurement_theta_min      2.3920
_cell_volume                     6173.1(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-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93.15
_diffrn_detector_area_resol_mean 22.2
_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    -48.00 132.00   2.00    2.00    --   42.00   0.00   0.00   90 
  2  \w    -48.00 132.00   2.00    2.00    --   42.00   0.00 180.00   90 
  3  \w    -48.00 132.00   2.00    2.00    --   42.00  54.00 220.00   90 
  4  \w    -48.00 132.00   2.00    2.00    --   42.00  54.00  55.00   90 
  5  \w    -48.00 132.00   2.00    2.00    --   42.00  54.00 320.00   90 
  6  \w    -48.00 132.00   2.00    2.00    --   42.00  54.00 110.00   90 
  7  \w    -48.00 132.00   2.00    2.00    --   42.00  54.00   0.00   90 
  8  \w    -48.00 132.00   2.00    2.00    --   42.00  54.00 275.00   90 
  9  \w    -48.00 132.00   2.00    2.00    --   42.00  54.00 200.00   90 
 10  \w    -48.00 132.00   2.00    2.00    --   42.00  54.00 180.00   90 
 11  \w    -48.00 132.00   2.00    2.00    --   42.00  54.00 165.00   90 
 12  \w      0.00 180.00   2.00    6.00    --   90.00   0.00   0.00   90 
 13  \w      0.00 180.00   2.00    6.00    --   90.00   0.00 180.00   90 
 14  \w      0.00 180.00   2.00    6.00    --   90.00  54.00  50.00   90 
 15  \w      0.00 180.00   2.00    6.00    --   90.00  54.00 125.00   90 
 16  \w      0.00 180.00   2.00    6.00    --   90.00  54.00 225.00   90 
 17  \w      0.00 180.00   2.00    6.00    --   90.00  54.00 300.00   90 
 18  \w      0.00 180.00   2.00    6.00    --   90.00  54.00 250.00   90 
 19  \w      0.00 180.00   2.00    6.00    --   90.00  54.00 150.00   90 
 20  \w      0.00 180.00   2.00    6.00    --   90.00  54.00  75.00   90 
 21  \w      0.00 180.00   2.00    6.00    --   90.00  54.00 350.00   90 
 22  \w      0.00 180.00   2.00    6.00    --   90.00  54.00  25.00   90 
 23  \w      0.00 180.00   2.00    6.00    --   90.00  54.00 175.00   90 
 24  \w      0.00 180.00   2.00    6.00    --   90.00  54.00   0.00   90 
 25  \w      0.00 180.00   2.00    6.00    --   90.00  54.00 325.00   90 
 26  \w      0.00 180.00   2.00    6.00    --   90.00  54.00 275.00   90 
 27  \w      0.00 180.00   2.00    6.00    --   90.00  54.00 100.00   90 
 28  \w      0.00 180.00   2.00    6.00    --   90.00  54.00 200.00   90 
;
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0130942000
_diffrn_orient_matrix_UB_12      0.1069069000
_diffrn_orient_matrix_UB_13      0.0504423000
_diffrn_orient_matrix_UB_21      -0.0262930000
_diffrn_orient_matrix_UB_22      0.0974597000
_diffrn_orient_matrix_UB_23      -0.0540161000
_diffrn_orient_matrix_UB_31      -0.0316163000
_diffrn_orient_matrix_UB_32      -0.1238160000
_diffrn_orient_matrix_UB_33      0.0010798000
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            103894
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.594
_diffrn_reflns_theta_max         66.594
_diffrn_reflns_theta_min         2.483
_diffrn_source                   'microfocus rotating anode'
_exptl_absorpt_coefficient_mu    5.971
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85065
_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    1.327
_exptl_crystal_description       block
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5461
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0311P)^2^+24.9596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5152
_reflns_number_total             5461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01459b3.cif
_cod_data_source_block           007a-22028
_cod_depositor_comments
'Adding full bibliography for 1569513--1569521.cif.'
_cod_database_code               1569521
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C30 H49 B N2 P2 Pd'
_shelx_estimated_absorpt_t_max   0.381
_shelx_estimated_absorpt_t_min   0.381
_olex2_refinement_description
;
1. Restrained distances
 C28A-C27A \\sim C28B-C27B \\sim C29A-C27A \\sim C27B-C29B \\sim C30A-C27A
\\sim C30B-C27B
 with sigma of 0.02
 P2-C27A \\sim P2-C27B
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(C30A) = Uanis(C30B)
Uanis(C29A) = Uanis(C29B)
Uanis(C27A) = Uanis(C27B)
Uanis(C28A) = Uanis(C28B)
3. Others
 Sof(C27B)=Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29B)=Sof(H29D)=
 Sof(H29E)=Sof(H29F)=Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C27)=Sof(H27A)=
 Sof(H27B)=Sof(H27C)=Sof(C28)=Sof(H28G)=Sof(H28H)=Sof(H28I)=1-FVAR(1)
 Sof(C27A)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29A)=Sof(H29A)=
 Sof(H29B)=Sof(H29C)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C26)=Sof(H26A)=
 Sof(H26B)=Sof(H26C)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C22(H22A,H22B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C17(H17), C18(H18), C19(H19), C20(H20)
4.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C24(H24A,H24B,H24C), C28A(H28A,H28B,
 H28C), C29A(H29A,H29B,H29C), C30A(H30A,H30B,H30C), C28B(H28D,H28E,H28F),
 C29B(H29D,H29E,H29F), C30B(H30D,H30E,H30F), C26(H26A,H26B,H26C), C25(H25A,H25B,
 H25C), C27(H27A,H27B,H27C), C28(H28G,H28H,H28I)
;
_shelx_res_checksum              38495
_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 
- Detector area scaling 
;
_oxdiff_exptl_absorpt_empirical_full_max 2.070
_oxdiff_exptl_absorpt_empirical_full_min 0.620