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_7701841
_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         'C24 H45 B N2 P2 Pd S, 2(C6 H6)'
_chemical_formula_sum            'C36 H57 B N2 P2 Pd S'
_chemical_formula_weight         729.04
_chemical_name_systematic        tBu-PBP-Pd-SH
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-23
_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                 107.062(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2903(3)
_cell_length_b                   17.5028(3)
_cell_length_c                   15.0487(3)
_cell_measurement_reflns_used    8912
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      71.2300
_cell_measurement_theta_min      5.0330
_cell_volume                     3850.13(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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(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     -1.00  31.00   1.00    1.16    --  -35.62  68.00-162.00   32
  2  \w   -102.00 -22.00   1.00    1.16    --  -35.62 -68.00  64.00   80
  3  \w     53.00 102.00   1.00    1.16    --   35.62  68.00-162.00   49
  4  \w    -28.00  13.00   1.00    1.16    --   35.62 -68.00  64.00   41
  5  \w     48.00 120.00   1.00    4.64    --  107.12 -68.00  64.00   72
  6  \w     95.00 158.00   1.00    4.64    --  107.12  68.00-162.00   63
  7  \w      2.00  73.00   1.00    1.16    --   35.62 -99.00 -90.00   71
  8  \w     67.00  94.00   1.00    1.16    --   35.62 178.00  30.00   27
  9  \w    -31.00  50.00   1.00    1.16    --   35.62 -57.00 120.00   81
 10  \w     59.00 108.00   1.00    1.16    --   35.62-178.00 120.00   49
 11  \w     56.00  83.00   1.00    4.64    --  107.12 -95.00   0.00   27
 12  \w    101.00 165.00   1.00    4.64    --  107.12 111.00  60.00   64
 13  \w    127.00 176.00   1.00    4.64    --  107.12  45.00 120.00   49
 14  \w     57.00 126.00   1.00    4.64    --  107.12 -30.00  60.00   69
 15  \w     39.00 105.00   1.00    4.64    --  107.12-111.00  90.00   66
 16  \w     41.00  88.00   1.00    4.64    --  107.12 -95.00-150.00   47
 17  \w    101.00 159.00   1.00    4.64    --  107.12 111.00 150.00   58
 18  \w     40.00 105.00   1.00    4.64    --  107.12 -95.00 -90.00   65
;
_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      -0.0907312000
_diffrn_orient_matrix_UB_12      -0.0443490000
_diffrn_orient_matrix_UB_13      -0.0196749000
_diffrn_orient_matrix_UB_21      -0.0425260000
_diffrn_orient_matrix_UB_22      0.0516517000
_diffrn_orient_matrix_UB_23      -0.0846179000
_diffrn_orient_matrix_UB_31      0.0329060000
_diffrn_orient_matrix_UB_32      -0.0556991000
_diffrn_orient_matrix_UB_33      -0.0626393000
_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     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17318
_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         71.372
_diffrn_reflns_theta_min         3.940
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.360
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79150
_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    1.258
_exptl_crystal_description       plate
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.183
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         7351
_refine_ls_number_restraints     164
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0646P)^2^+6.5055P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1278
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6340
_reflns_number_total             7351
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03954f2.cif
_cod_data_source_block           dyz20190703
_cod_original_cell_volume        3850.12(13)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7701841
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 N1 B1 P1 Pd1 S1'
_shelx_estimated_absorpt_t_max   0.521
_shelx_estimated_absorpt_t_min   0.399
_diffrn_oxdiff_digest_frames
;
019c22dc9ae83ffec58308ccee3607b59900034d55c
;
_diffrn_oxdiff_digest_hkl
;
016f868a94939a344262e5f9bb1a8ef3390d1a
;
_reflns_odcompleteness_completeness 99.94
_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. Restrained distances
 C25-C26 = C27-C28 = C29-C30
 1.4 with sigma of 0.02
 C31-C32 = C33-C34 = C35-C36
 1.4 with sigma of 0.02
 C31-C36
 1.4 with sigma of 0.02
 C25-C30
 1.45 with sigma of 0.02
3. Rigid bond restraints
 C36, C35, C34, C33, C32, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C36 \\sim C35 \\sim C34 \\sim C33 \\sim C32 \\sim C31: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
C26 \\sim C25 \\sim C30 \\sim C29 \\sim C28 \\sim C27: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(C36) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C35) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C28) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C25) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C36) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C33)
\\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C31) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C26) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C4(H4), C5(H5), C25(H25), C30(H30), C29(H29), C28(H28),
 C27(H27), C26(H26), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
5.c Fitted hexagon refined as free rotating group:
 C25(C30,C29,C28,C27,C26), C31(C32,C33,C34,C35,C36)
5.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C19(H19A,H19B,
 H19C), C18(H18A,H18B,H18C), C23(H23A,H23B,H23C), C20(H20A,H20B,H20C), C22(H22A,
 H22B,H22C), C10(H10A,H10B,H10C), C15(H15A,H15B,H15C), C24(H24A,H24B,H24C),
 C12(H12A,H12B,H12C)
;
_shelx_res_checksum              95889
_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 1.446
_oxdiff_exptl_absorpt_empirical_full_min 0.792