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_7701842
_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 S'
_chemical_formula_sum            'C23 H39 N O2 P2 Pd S'
_chemical_formula_weight         561.95
_chemical_name_systematic        tBu-POCOP-Pd-NCS
_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
_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                90
_cell_angle_beta                 103.0320(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.0749(3)
_cell_length_b                   8.12790(10)
_cell_length_c                   26.3766(4)
_cell_measurement_reflns_used    8157
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      71.9650
_cell_measurement_theta_min      3.5950
_cell_volume                     5237.26(12)
_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      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6296
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.976
_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    -74.00 -49.00   1.00    4.05    --  -40.64 128.00-172.00   25
  2  \w    -98.00 -69.00   1.00    4.05    --  -40.64-142.00 -58.00   29
  3  \w     70.00  95.00   1.00    4.05    --   40.64-142.00 -58.00   25
  4  \w     42.00  95.00   1.00    4.05    --   40.64-128.00 113.00   53
  5  \w     97.00 163.00   1.00   16.50    --  103.55 128.00-172.00   66
  6  \w     77.00 126.00   1.00   16.50    --  103.55-142.00 -58.00   49
  7  \w    106.00 132.00   1.00   16.50    --  103.55 142.00  -1.00   26
  8  \w     87.00 114.00   1.00   16.50    --  103.55-128.00 113.00   27
  9  \w    -65.00  32.00   1.00    4.05    --  -40.64  38.00 -30.00   97
 10  \w    -34.00  63.00   1.00    4.05    --   40.64 -38.00  60.00   97
 11  \w    150.00 177.00   1.00   16.50    --  103.55  45.00-180.00   27
 12  \w     34.00 109.00   1.00   16.50    --  103.55 -94.00 120.00   75
 13  \w     78.00 177.00   1.00   16.50    --  103.55  45.00   0.00   99
 14  \w    100.00 178.00   1.00   16.50    --  103.55 111.00 -60.00   78
 15  \w     99.00 124.00   1.00   16.50    --  103.55 -45.00-120.00   25
 16  \w    100.00 163.00   1.00   16.50    --  103.55 111.00  30.00   63
 17  \w     53.00  79.00   1.00   16.50    --  103.55 -45.00-120.00   26
;
_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      -0.0300793000
_diffrn_orient_matrix_UB_12      -0.1646199000
_diffrn_orient_matrix_UB_13      -0.0146289000
_diffrn_orient_matrix_UB_21      -0.0504899000
_diffrn_orient_matrix_UB_22      0.0936550000
_diffrn_orient_matrix_UB_23      -0.0305413000
_diffrn_orient_matrix_UB_31      0.0228653000
_diffrn_orient_matrix_UB_32      -0.0091410000
_diffrn_orient_matrix_UB_33      -0.0494399000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            13254
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.361
_diffrn_reflns_theta_min         3.619
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.760
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77936
_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    1.425
_exptl_crystal_description       plate
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         5045
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0159P)^2^+27.3728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0774
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4506
_reflns_number_total             5045
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03954f2.cif
_cod_data_source_block           dyz-20190522
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               7701842
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 H1'
_shelx_estimated_absorpt_t_max   0.482
_shelx_estimated_absorpt_t_min   0.370
_diffrn_oxdiff_digest_frames
;
01de5a28c01c6f35220df64961204a0cf700027696a
;
_diffrn_oxdiff_digest_hkl
;
0114a526ba96681a6addee57a73d317cb36ae1
;
_reflns_odcompleteness_completeness 99.56
_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:
 C4(H4), C3(H3), C5(H5)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C13(H13A,H13B,H13C), C22(H22A,H22B,
 H22C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C), C17(H17A,
 H17B,H17C), C18(H18A,H18B,H18C), C8(H8A,H8B,H8C), C20(H20A,H20B,H20C),
 C16(H16A,H16B,H16C)
;
_shelx_res_checksum              39586
_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 1.506
_oxdiff_exptl_absorpt_empirical_full_min 0.698