Reactions and catalytic applications of a PNCNP pincer palladium hydride complex
Chang, Jiarui; Ding, Man; Mao, Jia-Xue; Zhang, Jie; Chen, Xuenian; Dalton Transactions  (2022) –; doi:10.1039/D2DT03131K

data_7711729
_publ_section_title
;
 Reactions and catalytic applications of a PNCNP pincer palladium hydride
 complex
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT03131K
_journal_year                    2022
_chemical_formula_moiety         'C24 H45 N3 O P2 Pd, 2(C2 H3 N)'
_chemical_formula_sum            'C28 H51 N5 O P2 Pd'
_chemical_formula_weight         642.07
_chemical_name_systematic        tBu-PNCNP-Pd-NHCOCH3
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2022-10-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-10-25 deposited with the CCDC.	2022-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.1230(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.71590(10)
_cell_length_b                   14.45290(10)
_cell_length_c                   19.6929(2)
_cell_measurement_reflns_used    9679
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      71.3790
_cell_measurement_theta_min      3.7960
_cell_volume                     3321.25(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_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    -52.00  -3.00   1.00    1.00    --  -35.62  61.00 -46.00   49
  2  \w   -103.00 -31.00   1.00    1.00    --  -35.62 -61.00 174.00   72
  3  \w     76.00 102.00   1.00    1.00    --   35.62  61.00 -46.00   26
  4  \w    -13.00  12.00   1.00    1.00    --   35.62 -61.00 174.00   25
  5  \w    107.00 132.00   1.00    1.16    --  107.12  61.00 -46.00   25
  6  \w     41.00 124.00   1.00    1.16    --  107.12 -61.00 174.00   83
  7  \w    -74.00 -35.00   1.00    1.00    --  -35.62-178.00-120.00   39
  8  \w     16.00  73.00   1.00    1.00    --   35.62 -99.00-150.00   57
  9  \w     68.00 107.00   1.00    1.00    --   35.62 178.00-150.00   39
 10  \w     80.00 107.00   1.00    1.00    --   35.62-178.00-150.00   27
 11  \w    -34.00  41.00   1.00    1.00    --   35.62 -38.00  60.00   75
 12  \w     75.00 105.00   1.00    1.16    --  107.12 -95.00 -90.00   30
 13  \w     37.00 113.00   1.00    1.16    --  107.12-111.00-150.00   76
 14  \w    103.00 159.00   1.00    1.16    --  107.12 111.00 150.00   56
 15  \w     40.00  78.00   1.00    1.16    --  107.12 -61.00  30.00   38
 16  \w     90.00 174.00   1.00    1.16    --  107.12  61.00 -60.00   84
 17  \w     90.00 173.00   1.00    1.16    --  107.12  61.00 -90.00   83
 18  \w     82.00 109.00   1.00    1.16    --  107.12 -95.00  30.00   27
 19  \w     64.00  97.00   1.00    1.16    --  107.12 -95.00 120.00   33
 20  \w     64.00 111.00   1.00    1.16    --  107.12-111.00  30.00   47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0571891000
_diffrn_orient_matrix_UB_12      -0.0335467000
_diffrn_orient_matrix_UB_13      0.0691219000
_diffrn_orient_matrix_UB_21      -0.0994029000
_diffrn_orient_matrix_UB_22      -0.0684257000
_diffrn_orient_matrix_UB_23      0.0062722000
_diffrn_orient_matrix_UB_31      0.0654501000
_diffrn_orient_matrix_UB_32      -0.0745242000
_diffrn_orient_matrix_UB_33      -0.0367419000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            14789
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.500
_diffrn_reflns_theta_min         3.788
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.622
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_description       plate
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.00010(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         6346
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0387P)^2^+3.1646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0849
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5840
_reflns_number_total             6346
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03131k2.cif
_cod_data_source_block           cjr-20211203
_cod_database_code               7711729
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 P1 N1 Pd1'
_shelx_estimated_absorpt_t_max   0.577
_shelx_estimated_absorpt_t_min   0.552
_diffrn_oxdiff_digest_frames
;
01122d244cb9873a6217dc3df1e9c2956f0002729d4
;
_diffrn_oxdiff_digest_hkl
;
0125bee59f62fdb4a7c05e123eeb630ecd9748
;
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C4(H4)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C24(H24A,H24B,
 H24C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C19(H19A,H19B,H19C), C22(H22A,
 H22B,H22C), C18(H18A,H18B,H18C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C),
 C12(H12A,H12B,H12C), C28(H28A,H28B,H28C), C11(H11A,H11B,H11C), C26(H26A,H26B,
 H26C)
;
_shelx_res_checksum              26420
_shelx_hkl_checksum              17070
_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 1.300
_oxdiff_exptl_absorpt_empirical_full_min 0.741