Palladium(II) complexes supported by PBP and POCOP pincer ligands: comparison of structure, property and catalytic activity
Ding, Yazhou; Ma, Qiang-Qiang; Kang, Jiaxin; Zhang, Jie; Li, Shujun; Chen, Xuenian; Dalton Transactions  (2019) –; doi:10.1039/C9DT03954F

data_7701843
_publ_section_title
;
 Palladium(II) complexes supported by PBP and POCOP pincer ligands:
 comparison of structure, property and catalytic activity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03954F
_journal_year                    2019
_chemical_formula_moiety         'C23 H39 N O2 P2 Pd Se'
_chemical_formula_sum            'C23 H39 N O2 P2 Pd Se'
_chemical_formula_weight         608.85
_chemical_name_systematic        tBu-POCOP-Pd-NCSe
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-09-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-06 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.098(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.1910(3)
_cell_length_b                   8.17200(10)
_cell_length_c                   26.5788(4)
_cell_measurement_reflns_used    7073
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      71.4150
_cell_measurement_theta_min      5.5000
_cell_volume                     5329.19(13)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.980
_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    -21.00   6.00   1.00    1.00    --  -35.62  42.00 -40.00   27
  2  \w    -67.00 -40.00   1.00    1.00    --  -35.62 -42.00 166.00   27
  3  \w     18.00 103.00   1.00    1.00    --   35.62  42.00 -40.00   85
  4  \w     45.00 125.00   1.00    3.80    --  107.12 -42.00 166.00   80
  5  \w    138.00 171.00   1.00    3.80    --  107.12  42.00 -40.00   33
  6  \w     93.00 120.00   1.00    3.80    --  107.12  42.00 -40.00   27
  7  \w   -107.00 -37.00   1.00    1.00    --  -35.62-178.00  30.00   70
  8  \w    -33.00  46.00   1.00    1.00    --   35.62 -38.00  30.00   79
  9  \w     10.00  49.00   1.00    1.00    --   35.62 -42.00 166.00   39
 10  \w     24.00  55.00   1.00    1.00    --   35.62  57.00-180.00   31
 11  \w     58.00  94.00   1.00    1.00    --   35.62  57.00-180.00   36
 12  \w    101.00 126.00   1.00    3.80    --  107.12 111.00-120.00   25
 13  \w    102.00 176.00   1.00    3.80    --  107.12  45.00-120.00   74
 14  \w    151.00 177.00   1.00    3.80    --  107.12 111.00-180.00   26
 15  \w     55.00 110.00   1.00    3.80    --  107.12 -95.00   0.00   55
 16  \w    111.00 138.00   1.00    3.80    --  107.12 111.00 -30.00   27
 17  \w    108.00 135.00   1.00    3.80    --  107.12 111.00-180.00   27
 18  \w    102.00 128.00   1.00    3.80    --  107.12  30.00  90.00   26
 19  \w     88.00 175.00   1.00    3.80    --  107.12  30.00   0.00   87
 20  \w     40.00 125.00   1.00    3.80    --  107.12 -45.00 -60.00   85
;
_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      -0.0596337000
_diffrn_orient_matrix_UB_12      -0.0453743000
_diffrn_orient_matrix_UB_13      -0.0012418000
_diffrn_orient_matrix_UB_21      -0.0042340000
_diffrn_orient_matrix_UB_22      -0.0874887000
_diffrn_orient_matrix_UB_23      -0.0521219000
_diffrn_orient_matrix_UB_31      0.0191992000
_diffrn_orient_matrix_UB_32      -0.1606557000
_diffrn_orient_matrix_UB_33      0.0287030000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            11096
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.468
_diffrn_reflns_theta_min         3.603
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.457
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62709
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       plate
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.123
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         5077
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0285
_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^)+(0.0430P)^2^+3.6193P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0747
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4823
_reflns_number_total             5077
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03954f2.cif
_cod_data_source_block           dyz-20190727-pocopsecn
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               7701843
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 N1 P1 Se1 Pd1 O1'
_shelx_estimated_absorpt_t_max   0.423
_shelx_estimated_absorpt_t_min   0.370
_diffrn_oxdiff_digest_frames
;
01f869084563ed5b4d8416b1e6c7c6f3790002994e9
;
_diffrn_oxdiff_digest_hkl
;
011d40bc52bce8069869d636d4e003d517656a
;
_reflns_odcompleteness_completeness 99.57
_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(H3), C4(H4), C5(H5)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C8(H8A,H8B,H8C), C22(H22A,H22B,
 H22C), C20(H20A,H20B,H20C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C18(H18A,
 H18B,H18C), C10(H10A,H10B,H10C), C17(H17A,H17B,H17C), C21(H21A,H21B,H21C),
 C16(H16A,H16B,H16C)
;
_shelx_res_checksum              69939
_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 1.358
_oxdiff_exptl_absorpt_empirical_full_min 0.546