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_7701840
_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         'C22 H39 N3 O2 P2 Pd'
_chemical_formula_sum            'C22 H39 N3 O2 P2 Pd'
_chemical_formula_weight         545.90
_chemical_name_systematic        tBu-POCOP-Pd-N3
_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             2019-10-02
_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                99.726(2)
_cell_angle_beta                 95.763(2)
_cell_angle_gamma                102.906(2)
_cell_formula_units_Z            2
_cell_length_a                   8.4289(2)
_cell_length_b                   11.8643(3)
_cell_length_c                   13.2820(4)
_cell_measurement_reflns_used    10684
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      71.4350
_cell_measurement_theta_min      4.6490
_cell_volume                     1262.82(6)
_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 1.000
_diffrn_measured_fraction_theta_max 0.987
_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    -76.00  18.00   1.00    1.00    --  -35.62 102.00-161.00   94
  2  \w      4.00  76.00   1.00    1.00    --   35.62-102.00  95.00   72
  3  \w     37.00 111.00   1.00    1.00    --  107.12-102.00  95.00   74
  4  \w    101.00 177.00   1.00    1.00    --  107.12 102.00-161.00   76
  5  \w   -103.00  -9.00   1.00    1.00    --  -35.62 -77.00   0.00   94
  6  \w   -105.00 -17.00   1.00    1.00    --  -35.62 -38.00  90.00   88
  7  \w    -34.00  55.00   1.00    1.00    --   35.62 -38.00-180.00   89
  8  \w     17.00 105.00   1.00    1.00    --   35.62  38.00  60.00   88
  9  \w     17.00 105.00   1.00    1.00    --   35.62  38.00 150.00   88
 10  \w      1.00  75.00   1.00    1.00    --   35.62 -99.00 -90.00   74
 11  \w     19.00 103.00   1.00    1.00    --   35.62  57.00 -30.00   84
 12  \w     40.00 125.00   1.00    1.00    --  107.12 -61.00  60.00   85
 13  \w     38.00 110.00   1.00    1.00    --  107.12 -95.00-150.00   72
 14  \w     38.00 110.00   1.00    1.00    --  107.12 -95.00   0.00   72
 15  \w     90.00 176.00   1.00    1.00    --  107.12  45.00  30.00   86
 16  \w     37.00 113.00   1.00    1.00    --  107.12-111.00 150.00   76
 17  \w     40.00 125.00   1.00    1.00    --  107.12 -61.00 -60.00   85
 18  \w     39.00 125.00   1.00    1.00    --  107.12 -45.00 150.00   86
 19  \w     89.00 174.00   1.00    1.00    --  107.12  61.00 150.00   85
 20  \w     90.00 176.00   1.00    1.00    --  107.12  45.00-180.00   86
 21  \w     86.00 177.00   1.00    1.00    --  107.12  30.00 -60.00   91
 22  \w     37.00 113.00   1.00    1.00    --  107.12-111.00   0.00   76
 23  \w     90.00 176.00   1.00    1.00    --  107.12  45.00  90.00   86
 24  \w     40.00 125.00   1.00    1.00    --  107.12 -61.00-150.00   85
 25  \w     38.00 110.00   1.00    1.00    --  107.12 -95.00 -60.00   72
 26  \w     89.00 174.00   1.00    1.00    --  107.12  61.00 120.00   85
 27  \w    -55.00  34.00   1.00    1.00    --  -35.62  38.00 150.00   89
 28  \w    -32.00  52.00   1.00    1.00    --   35.62 -57.00 -30.00   84
 29  \w     19.00 103.00   1.00    1.00    --   35.62  57.00-120.00   84
;
_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      0.1326792000
_diffrn_orient_matrix_UB_12      0.0520949000
_diffrn_orient_matrix_UB_13      0.0951488000
_diffrn_orient_matrix_UB_21      0.0989700000
_diffrn_orient_matrix_UB_22      0.0822390000
_diffrn_orient_matrix_UB_23      -0.0620515000
_diffrn_orient_matrix_UB_31      -0.0922097000
_diffrn_orient_matrix_UB_32      0.0948027000
_diffrn_orient_matrix_UB_33      0.0351741000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14092
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.540
_diffrn_reflns_theta_min         3.412
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.300
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70820
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       block
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         4863
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0253
_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^)+(0.0265P)^2^+0.8585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0620
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4652
_reflns_number_total             4863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03954f2.cif
_cod_data_source_block           dyz-pocop-pdn3
_cod_database_code               7701840
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 P1 N1 O1 Pd1'
_shelx_estimated_absorpt_t_max   0.501
_shelx_estimated_absorpt_t_min   0.370
_diffrn_oxdiff_digest_frames
;
01218a14438953b9fda73884460ad10c550003065fa
;
_diffrn_oxdiff_digest_hkl
;
0174973a237a881b963699257d0e57cc619dac
;
_reflns_odcompleteness_completeness 100.00
_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. Uiso/Uaniso restraints and constraints
Uanis(N1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N3A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: N1A(0.5) N1(0.5) N3(0.5) N3A(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C5(H5)
4.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C13(H13A,H13B,H13C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C12(H12A,
 H12B,H12C), C14(H14A,H14B,H14C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C)
;
_shelx_res_checksum              55813
_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 1.195
_oxdiff_exptl_absorpt_empirical_full_min 0.793