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_7701839
_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 Se'
_chemical_formula_sum            'C25 H44 B N3 P2 Pd Se'
_chemical_formula_weight         644.74
_chemical_name_systematic        tBu-PBP-Pd-NCSe
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                 100.3090(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.8528(2)
_cell_length_b                   16.7026(2)
_cell_length_c                   21.5950(2)
_cell_measurement_reflns_used    10371
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      71.3810
_cell_measurement_theta_min      4.0600
_cell_volume                     5980.55(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 0.996
_diffrn_measured_fraction_theta_max 0.972
_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   -102.00 -77.00   1.00    5.71    --  -35.62 -42.00-115.00   25
  2  \w    -53.00  -5.00   1.00    5.71    --  -35.62  42.00  36.00   48
  3  \w    -44.00 -19.00   1.00    5.71    --  -35.62 -42.00-115.00   25
  4  \w     37.00  62.00   1.00    5.71    --   35.62  42.00  36.00   25
  5  \w     96.00 176.00   1.00   22.84    --  107.12  42.00  36.00   80
  6  \w     40.00 125.00   1.00   22.84    --  107.12 -42.00-115.00   85
  7  \w   -104.00 -35.00   1.00    5.71    --  -35.62-178.00  60.00   69
  8  \w    -53.00  31.00   1.00    5.71    --  -35.62  38.00 120.00   84
  9  \w    -76.00 -37.00   1.00    5.71    --  -35.62-178.00 -60.00   39
 10  \w     58.00 107.00   1.00    5.71    --   35.62 178.00  30.00   49
 11  \w     65.00 104.00   1.00    5.71    --   35.62 178.00 -60.00   39
 12  \w    -14.00  11.00   1.00    5.71    --   35.62 -42.00-115.00   25
 13  \w    116.00 174.00   1.00   22.84    --  107.12 111.00   0.00   58
 14  \w     74.00 177.00   1.00   22.84    --  107.12  15.00 -30.00  103
 15  \w     89.00 174.00   1.00   22.84    --  107.12  61.00-180.00   85
 16  \w     48.00 107.00   1.00   22.84    --  107.12 -95.00  60.00   59
 17  \w     97.00 122.00   1.00   22.84    --  107.12 -77.00  30.00   25
 18  \w     44.00 124.00   1.00   22.84    --  107.12 -45.00  30.00   80
;
_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      0.0263891000
_diffrn_orient_matrix_UB_12      0.0378725000
_diffrn_orient_matrix_UB_13      0.0655122000
_diffrn_orient_matrix_UB_21      -0.0774330000
_diffrn_orient_matrix_UB_22      -0.0314432000
_diffrn_orient_matrix_UB_23      0.0202479000
_diffrn_orient_matrix_UB_31      0.0440055000
_diffrn_orient_matrix_UB_32      -0.0779731000
_diffrn_orient_matrix_UB_33      0.0236673000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            13545
_diffrn_reflns_point_group_measured_fraction_full 0.761
_diffrn_reflns_point_group_measured_fraction_max 0.731
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.579
_diffrn_reflns_theta_min         3.756
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.531
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80210
_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    1.432
_exptl_crystal_description       block
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.018
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.011(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         8551
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0655P)^2^+11.7699P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.0979
_reflns_Friedel_coverage         0.503
_reflns_Friedel_fraction_full    0.525
_reflns_Friedel_fraction_max     0.490
_reflns_number_gt                8407
_reflns_number_total             8551
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03954f2.cif
_cod_data_source_block           dyz-20190712-1
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7701839
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 N1 P1 B1 Pd1 Se1'
_shelx_estimated_absorpt_t_max   0.465
_shelx_estimated_absorpt_t_min   0.398
_diffrn_oxdiff_digest_frames
;
017f1b26d059ac722bb8d24f7aa6eeddf50002790a1
;
_diffrn_oxdiff_digest_hkl
;
0168998e9aa51dd806018d12977896a4630092
;
_reflns_odcompleteness_completeness 99.64
_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), C50(H50A,H50B), C49(H49A,H49B), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C29(H29), C3(H3), C4(H4), C6(H6), C5(H5), C28(H28), C30(H30)
2.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C13(H13A,H13B,H13C), C25(H25A,H25B,H25C), C19(H19A,H19B,
 H19C), C42(H42A,H42B,H42C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C43(H43A,
 H43B,H43C), C21(H21A,H21B,H21C), C46(H46A,H46B,H46C), C38(H38A,H38B,H38C),
 C47(H47A,H47B,H47C), C40(H40A,H40B,H40C), C12(H12A,H12B,H12C), C48(H48A,H48B,
 H48C), C20(H20A,H20B,H20C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C35(H35A,
 H35B,H35C), C44(H44A,H44B,H44C), C11(H11A,H11B,H11C), C39(H39A,H39B,H39C),
 C24(H24A,H24B,H24C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              83252
_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 1.470
_oxdiff_exptl_absorpt_empirical_full_min 0.668