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_7701844
_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 H47.03 B1.76 Cl0.24 N2 P2 Pd'
_chemical_formula_sum            'C24 H47.03 B1.76 Cl0.24 N2 P2 Pd'
_chemical_formula_weight         559.63
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-10-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-31 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.07097(16)
_cell_length_b                   14.5114(2)
_cell_length_c                   32.0399(5)
_cell_measurement_reflns_used    7257
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.4170
_cell_measurement_theta_min      4.5750
_cell_volume                     5612.32(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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    'ShelXS (Sheldrick, 2008)'
_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 0.999
_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    -70.00  32.00   1.00    1.00    --  -40.77  63.00 134.00  102
  2  \w     74.00 176.00   1.00    3.02    --  103.55  63.00 134.00  102
  3  \w     73.00 159.00   1.00    3.02    --  103.55  76.00-103.00   86
  4  \w    106.00 173.00   1.00    3.02    --  103.55  83.00   5.00   67
  5  \w      1.00  55.00   1.00    1.00    --   40.77 -99.00   0.00   54
  6  \w     24.00  69.00   1.00    1.00    --   40.77-125.00 -90.00   45
  7  \w     48.00 129.00   1.00    3.02    --  103.55 -45.00-120.00   81
  8  \w    106.00 133.00   1.00    3.02    --  103.55 111.00  90.00   27
;
_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      0.1036688000
_diffrn_orient_matrix_UB_12      -0.0315104000
_diffrn_orient_matrix_UB_13      0.0241148000
_diffrn_orient_matrix_UB_21      0.0252678000
_diffrn_orient_matrix_UB_22      -0.0710294000
_diffrn_orient_matrix_UB_23      -0.0344485000
_diffrn_orient_matrix_UB_31      0.0699669000
_diffrn_orient_matrix_UB_32      0.0723332000
_diffrn_orient_matrix_UB_33      -0.0233402000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            18199
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.401
_diffrn_reflns_theta_min         4.587
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.712
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       block
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         5439
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+4.6230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0835
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4504
_reflns_number_total             5439
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03954f2.cif
_cod_data_source_block           dyz-20190308
_cod_original_cell_volume        5612.34(14)
_cod_database_code               7701844
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.553
_shelx_estimated_absorpt_t_min   0.500
_reflns_odcompleteness_completeness 99.86
_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 B(H,H,H,H) groups, All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Shared sites
{B1, Cl1}
3. Restrained distances
 H1B-Cl1 \\sim Cl1-H1A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C16)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.01
Uanis(C9A) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(B1) = Uanis(Cl1)
5. Rigid body (RIGU) restrains
 C9, C9A, C10, C10A, C12, C12A, C13, C13A, C14, C14A, C16, C16A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C9A)=Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(H11D)=Sof(H11E)=
 Sof(H11F)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C13A)=Sof(C14A)=
 Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16A)=
 Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(1)
 Sof(C9)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(H11A)=Sof(H11B)=Sof(H11C)=
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13)=Sof(C14)=Sof(H14A)=Sof(H14B)=
 Sof(H14C)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=
 FVAR(1)
 Sof(Cl1)=1-FVAR(2)
 Sof(B1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(H1D)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5)
7.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C10A(H10D,H10E,H10F), C11(H11A,H11B,H11C), C11(H11D,H11E,
 H11F), C12(H12A,H12B,H12C), C12A(H12D,H12E,H12F), C14(H14A,H14B,H14C),
 C14A(H14D,H14E,H14F), C15(H15A,H15B,H15C), C15(H15D,H15E,H15F), C16(H16A,H16B,
 H16C), C16A(H16D,H16E,H16F), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C),
 C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C)
;
_shelx_res_checksum              8668
_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 1.435
_oxdiff_exptl_absorpt_empirical_full_min 0.720