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_1569519
_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         'C32 H53 B N2 O P2 Pd, C5 H12'
_chemical_formula_sum            'C37 H65 B N2 O P2 Pd'
_chemical_formula_weight         733.06
_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                 105.439(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9723(7)
_cell_length_b                   11.4923(6)
_cell_length_c                   23.5265(14)
_cell_measurement_reflns_used    12290
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      30.1300
_cell_measurement_theta_min      1.8180
_cell_volume                     3902.0(4)
_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                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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    -15.00  28.00   0.50   23.00    --   20.00  54.00 -30.00   86
  2  \w     57.00 106.00   0.50   23.00    --   20.00  54.00 -30.00   98
  3  \w    -74.00 109.00   0.50   23.00    --   20.00  54.00-120.00  366
  4  \w    -74.00 108.00   0.50   23.00    --   20.00  54.00 171.87  364
  5  \w    -41.00 -16.00   0.50   23.00    --   20.00  54.00   0.00   50
  6  \w     41.00  67.00   0.50   23.00    --   20.00  54.00   0.00   52
  7  \w     -1.00  56.00   0.50   23.00    --   20.00  54.00 -90.00  114
  8  \w     35.00  60.00   0.50   23.00    --   20.00  54.00 -60.00   50
  9  \w    -67.00 -42.00   0.50   23.00    --   20.00  54.00 -30.00   50
;
_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      -0.0323947000
_diffrn_orient_matrix_UB_12      -0.0024113000
_diffrn_orient_matrix_UB_13      -0.0281395000
_diffrn_orient_matrix_UB_21      0.0360265000
_diffrn_orient_matrix_UB_22      -0.0160005000
_diffrn_orient_matrix_UB_23      -0.0128463000
_diffrn_orient_matrix_UB_31      -0.0083092000
_diffrn_orient_matrix_UB_32      -0.0595586000
_diffrn_orient_matrix_UB_33      0.0046100000
_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  0.0515
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            31758
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.265
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.587
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90512
_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    1.248
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         7971
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0243P)^2^+2.2124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0741
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6106
_reflns_number_total             7971
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01459b3.cif
_cod_data_source_block           mini2-22012
_cod_depositor_comments
'Adding full bibliography for 1569513--1569521.cif.'
_cod_database_code               1569519
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C48H51N2P2Pd1O1B1
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.799
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C17(H17A,H17B), C25(H25A,H25B), C35(H35A,H35B), C36(H36A,H36B),
 C37(H37A,H37B)
1.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C20(H20), C21(H21), C22(H22), C23(H23)
1.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C27(H27A,
 H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C38(H38A,H38B,
 H38C)
;
_shelx_res_checksum              66227
_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 1.188
_oxdiff_exptl_absorpt_empirical_full_min 0.893