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_7701838
_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         'C25 H44 B N3 P2 Pd S'
_chemical_formula_sum            'C25 H44 B N3 P2 Pd S'
_chemical_formula_weight         597.84
_chemical_name_systematic        tBu-PBP-Pd-NCS
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-28
_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                71.489(2)
_cell_angle_beta                 86.395(2)
_cell_angle_gamma                86.289(2)
_cell_formula_units_Z            4
_cell_length_a                   7.9460(2)
_cell_length_b                   16.5470(4)
_cell_length_c                   23.1657(6)
_cell_measurement_reflns_used    10137
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.4430
_cell_measurement_theta_min      4.1050
_cell_volume                     2879.36(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.42a (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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6296
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.978
_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    -87.00   9.00   1.00    1.00    --  -40.64 112.00-149.00   96
  2  \w     13.00  89.00   1.00    1.00    --   40.64-112.00 118.00   76
  3  \w    101.00 178.00   1.00    1.66    --  103.55 112.00-149.00   77
  4  \w     27.00 113.00   1.00    1.66    --  103.55-112.00 118.00   86
  5  \w   -115.00 -16.00   1.00    1.00    --  -40.64 -38.00  90.00   99
  6  \w   -117.00  -8.00   1.00    1.00    --  -40.64 -77.00   0.00  109
  7  \w    -32.00  69.00   1.00    1.00    --   40.64 -57.00-150.00  101
  8  \w     31.00 133.00   1.00    1.66    --  103.55 -61.00 -60.00  102
  9  \w     75.00 178.00   1.00    1.66    --  103.55  30.00 -90.00  103
 10  \w     21.00 109.00   1.00    1.66    --  103.55 -94.00-180.00   88
 11  \w     31.00 133.00   1.00    1.66    --  103.55 -61.00  90.00  102
 12  \w    106.00 178.00   1.00    1.66    --  103.55 111.00-180.00   72
 13  \w     86.00 112.00   1.00    1.66    --  103.55-111.00   0.00   26
 14  \w     27.00  64.00   1.00    1.66    --  103.55 -30.00 -90.00   37
 15  \w     68.00 120.00   1.00    1.66    --  103.55 -30.00 -90.00   52
 16  \w     64.00  92.00   1.00    1.66    --  103.55-111.00 -30.00   28
 17  \w     24.00  50.00   1.00    1.66    --  103.55 -94.00-150.00   26
 18  \w     63.00 109.00   1.00    1.66    --  103.55 -94.00-150.00   46
 19  \w    103.00 131.00   1.00    1.66    --  103.55 111.00 -30.00   28
 20  \w     31.00 124.00   1.00    1.66    --  103.55 -45.00-180.00   93
 21  \w     97.00 157.00   1.00    1.66    --  103.55  45.00 150.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0361153000
_diffrn_orient_matrix_UB_12      -0.0548778000
_diffrn_orient_matrix_UB_13      0.0665580000
_diffrn_orient_matrix_UB_21      0.0372051000
_diffrn_orient_matrix_UB_22      -0.0815421000
_diffrn_orient_matrix_UB_23      -0.0180363000
_diffrn_orient_matrix_UB_31      0.1874413000
_diffrn_orient_matrix_UB_32      0.0007882000
_diffrn_orient_matrix_UB_33      0.0131465000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            26389
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.490
_diffrn_reflns_theta_min         3.948
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.053
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.42a (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    1.379
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         11158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+4.6467P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9236
_reflns_number_total             11158
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03954f2.cif
_cod_data_source_block           dyz-20190506
_cod_database_code               7701838
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 N1 B1 P1 S1 Pd1 Cl1'
_shelx_estimated_absorpt_t_max   0.511
_shelx_estimated_absorpt_t_min   0.418
_diffrn_oxdiff_digest_frames
;
01ea7d67c00bdc6edfde17507d3dd77e620157194db
;
_diffrn_oxdiff_digest_hkl
;
017a318b1552cbd2d90f27a7800ba979cfee76
;
_reflns_odcompleteness_completeness 99.88
_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:
 C7(H7A,H7B), C8(H8A,H8B), C32(H32A,H32B), C33(H33A,H33B)
2.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C30(H30), C5(H5), C28(H28), C3(H3), C2(H2), C4(H4), C29(H29)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C35(H35A,H35B,H35C), C48(H48A,H48B,H48C), C19(H19A,H19B,
 H19C), C49(H49A,H49B,H49C), C23(H23A,H23B,H23C), C39(H39A,H39B,H39C), C15(H15A,
 H15B,H15C), C20(H20A,H20B,H20C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C),
 C16(H16A,H16B,H16C), C37(H37A,H37B,H37C), C47(H47A,H47B,H47C), C12(H12A,H12B,
 H12C), C22(H22A,H22B,H22C), C18(H18A,H18B,H18C), C11(H11A,H11B,H11C), C43(H43A,
 H43B,H43C), C36(H36A,H36B,H36C), C24(H24A,H24B,H24C), C14(H14A,H14B,H14C),
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C)
;
_shelx_res_checksum              63434
_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 1.813
_oxdiff_exptl_absorpt_empirical_full_min 0.579