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_7711730
_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         'C22 H41 N3 O3 P2 Pd, C4 H8 O'
_chemical_formula_sum            'C26 H49 N3 O4 P2 Pd'
_chemical_formula_weight         636.02
_chemical_name_systematic        tBu-PNCNP-Pd-NO3
_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   mixed
_atom_sites_solution_primary     iterative
_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                 95.3590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.34860(10)
_cell_length_b                   22.9353(2)
_cell_length_c                   11.59380(10)
_cell_measurement_reflns_used    8916
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      71.4050
_cell_measurement_theta_min      3.8560
_cell_volume                     3004.49(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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(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 0.984
_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   -103.00 -20.00   1.00    1.00    --  -35.62 -60.00-151.00   83
  2  \w     -4.00  24.00   1.00    1.00    --  -35.62  60.00 -11.00   28
  3  \w     19.00  50.00   1.00    1.00    --   35.62  60.00 -11.00   31
  4  \w    -13.00  12.00   1.00    1.00    --   35.62 -60.00-151.00   25
  5  \w     58.00 124.00   1.00    1.93    --  107.12 -60.00-151.00   66
  6  \w    124.00 174.00   1.00    1.93    --  107.12  60.00 -11.00   50
  7  \w    -68.00 -42.00   1.00    1.00    --  -35.62-178.00   0.00   26
  8  \w     24.00  74.00   1.00    1.00    --   35.62 -99.00-120.00   50
  9  \w     63.00 104.00   1.00    1.00    --   35.62 178.00-120.00   41
 10  \w      2.00  70.00   1.00    1.00    --   35.62 -99.00  30.00   68
 11  \w     68.00 103.00   1.00    1.00    --   35.62  60.00 -11.00   35
 12  \w     81.00 109.00   1.00    1.93    --  107.12 -95.00 150.00   28
 13  \w     39.00 110.00   1.00    1.93    --  107.12 -95.00  90.00   71
 14  \w    117.00 176.00   1.00    1.93    --  107.12  30.00 -90.00   59
 15  \w     92.00 142.00   1.00    1.93    --  107.12 -15.00 -90.00   50
 16  \w     37.00  78.00   1.00    1.93    --  107.12 -15.00 -90.00   41
 17  \w     87.00 169.00   1.00    1.93    --  107.12  77.00 -60.00   82
 18  \w     58.00  91.00   1.00    1.93    --  107.12 -95.00 -30.00   33
 19  \w     38.00 105.00   1.00    1.93    --  107.12 -95.00-120.00   67
 20  \w    118.00 170.00   1.00    1.93    --  107.12 111.00 -90.00   52
;
_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      -0.0121725000
_diffrn_orient_matrix_UB_12      0.0070619000
_diffrn_orient_matrix_UB_13      0.1305026000
_diffrn_orient_matrix_UB_21      -0.0976680000
_diffrn_orient_matrix_UB_22      -0.0468587000
_diffrn_orient_matrix_UB_23      -0.0076617000
_diffrn_orient_matrix_UB_31      0.0943538000
_diffrn_orient_matrix_UB_32      -0.0476018000
_diffrn_orient_matrix_UB_33      0.0268931000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13423
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.469
_diffrn_reflns_theta_min         3.855
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.266
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40218
_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    1.406
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.739
_refine_diff_density_min         -1.192
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         5747
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0531P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0878
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5270
_reflns_number_total             5747
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03131k2.cif
_cod_data_source_block           cjr-20211207
_cod_original_cell_volume        3004.48(5)
_cod_database_code               7711730
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 N1 P1 N1 O1 Pd1'
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.885
_diffrn_oxdiff_digest_frames
;
01c353fbbfe26f25ed72ab21f8f48b06f6000303e19
;
_diffrn_oxdiff_digest_hkl
;
0157bbce5127d6ee024c6fbd88ab43181e58f0
;
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C23(H23A,H23B), C26(H26A,H26B), C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C3(H3)
2.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C12(H12A,H12B,
 H12C), C17(H17A,H17B,H17C), C14(H14A,H14B,H14C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C21(H21A,H21B,H21C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C),
 C9(H9A,H9B,H9C)
;
_shelx_res_checksum              70484
_shelx_hkl_checksum              8584
_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 1.946
_oxdiff_exptl_absorpt_empirical_full_min 0.538