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_7711731
_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 H42 N2 O P2 Pd, 3(H2 O)'
_chemical_formula_sum            'C22 H48 N2 O4 P2 Pd'
_chemical_formula_weight         572.96
_chemical_name_systematic        tBu-PNCNP-Pd0OH
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.9062(2)
_cell_length_b                   14.9710(2)
_cell_length_c                   21.5306(3)
_cell_measurement_reflns_used    7457
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      71.4490
_cell_measurement_theta_min      4.4310
_cell_volume                     5449.45(12)
_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 0.981
_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    -71.00   7.00   1.00    1.22    --  -35.62  94.00 157.00   78
  2  \w      0.00  26.00   1.00    1.22    --   35.62 -95.00 -51.00   26
  3  \w    130.00 176.00   1.00    4.89    --  107.12  94.00 157.00   46
  4  \w     70.00 109.00   1.00    4.89    --  107.12 -95.00 -51.00   39
  5  \w     97.00 154.00   1.00    4.89    --  107.12  41.00 -50.00   57
  6  \w     63.00  90.00   1.00    4.89    --  107.12 -94.00  46.00   27
  7  \w    -74.00 -35.00   1.00    1.22    --  -35.62-178.00 150.00   39
  8  \w     70.00 100.00   1.00    1.22    --   35.62  77.00  90.00   30
  9  \w     63.00 107.00   1.00    1.22    --   35.62 178.00  90.00   44
 10  \w     64.00  89.00   1.00    1.22    --   35.62 178.00 -30.00   25
 11  \w     14.00  48.00   1.00    1.22    --   35.62  77.00  90.00   34
 12  \w     90.00 162.00   1.00    4.89    --  107.12  61.00  60.00   72
 13  \w    110.00 175.00   1.00    4.89    --  107.12 111.00 -60.00   65
 14  \w     71.00  97.00   1.00    4.89    --  107.12 -95.00-120.00   26
 15  \w     62.00  95.00   1.00    4.89    --  107.12 -95.00-150.00   33
;
_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      0.0280859000
_diffrn_orient_matrix_UB_12      -0.0198502000
_diffrn_orient_matrix_UB_13      -0.0666727000
_diffrn_orient_matrix_UB_21      0.0379185000
_diffrn_orient_matrix_UB_22      0.0934703000
_diffrn_orient_matrix_UB_23      -0.0036479000
_diffrn_orient_matrix_UB_31      0.0779153000
_diffrn_orient_matrix_UB_32      -0.0382740000
_diffrn_orient_matrix_UB_33      0.0257264000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14725
_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         71.455
_diffrn_reflns_theta_min         4.107
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.831
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71249
_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    1.397
_exptl_crystal_description       block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.012
_exptl_crystal_size_mid          0.011
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         5210
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0360P)^2^+3.7093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0785
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4653
_reflns_number_total             5210
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03131k2.cif
_cod_data_source_block           20211007-cjr
_cod_database_code               7711731
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 N1 P1 Pd1'
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.923
_diffrn_oxdiff_digest_frames
;
01ceeb07ab268c14b21fd3d029f13b2c83000361b0a
;
_diffrn_oxdiff_digest_hkl
;
01500877d8d1519637b8f1df0095198fbc5f9c
;
_reflns_odcompleteness_completeness 99.83
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O1-O2
 3.5 with sigma of 0.02
 H3B-H4A
 2.5 with sigma of 0.02
 H2B-H3B
 2.5 with sigma of 0.02
3.a Free rotating group:
 O2(H2A,H2B), O3(H3A,H3B), O4(H4A,H4B)
3.b Rotating group:
 O1(H1)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C3(H3)
3.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C22(H22A,H22B,H22C),
 C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C14(H14A,H14B,
 H14C), C21(H21A,H21B,H21C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C20(H20A,
 H20B,H20C)
;
_shelx_res_checksum              38768
_shelx_hkl_checksum              90233
_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 1.294
_oxdiff_exptl_absorpt_empirical_full_min 0.750