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_7701837
_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 H44 B N5 P2 Pd'
_chemical_formula_sum            'C24 H44 B N5 P2 Pd'
_chemical_formula_weight         581.79
_chemical_name_systematic        tBu-PBP-Pd-N3
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-10-03
_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                 105.454(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2561(3)
_cell_length_b                   16.6838(3)
_cell_length_c                   14.5569(3)
_cell_measurement_reflns_used    8457
_cell_measurement_temperature    294.5(6)
_cell_measurement_theta_max      71.3500
_cell_measurement_theta_min      4.0980
_cell_volume                     2868.95(11)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.5(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.974
_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    -13.00  28.00   1.00    1.00    --  -35.62  86.00-163.00   41
  2  \w    -46.00 -20.00   1.00    1.00    --  -35.62  86.00-163.00   26
  3  \w     56.00 138.00   1.00    1.42    --  107.12 -86.00  77.00   82
  4  \w     99.00 175.00   1.00    1.42    --  107.12  86.00-163.00   76
  5  \w   -100.00 -37.00   1.00    1.00    --  -35.62-178.00  60.00   63
  6  \w   -101.00 -37.00   1.00    1.00    --  -35.62-178.00 -90.00   64
  7  \w    -98.00 -19.00   1.00    1.00    --  -35.62 -57.00  60.00   79
  8  \w     57.00  82.00   1.00    1.00    --   35.62 178.00 -30.00   25
  9  \w     57.00  99.00   1.00    1.00    --   35.62 178.00  60.00   42
 10  \w      2.00  27.00   1.00    1.00    --   35.62 -86.00  77.00   25
 11  \w     37.00 100.00   1.00    1.42    --  107.12-111.00  60.00   63
 12  \w     80.00 132.00   1.00    1.42    --  107.12 -77.00-120.00   52
 13  \w    105.00 158.00   1.00    1.42    --  107.12 111.00 -90.00   53
 14  \w     85.00 170.00   1.00    1.42    --  107.12  77.00 -60.00   85
 15  \w    104.00 171.00   1.00    1.42    --  107.12  77.00  60.00   67
 16  \w     41.00 128.00   1.00    1.42    --  107.12 -30.00 120.00   87
 17  \w     78.00 103.00   1.00    1.42    --  107.12 -30.00 150.00   25
 18  \w     48.00  73.00   1.00    1.42    --  107.12 -77.00-120.00   25
;
_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      -0.0866578000
_diffrn_orient_matrix_UB_12      -0.0590993000
_diffrn_orient_matrix_UB_13      -0.0603081000
_diffrn_orient_matrix_UB_21      -0.0210603000
_diffrn_orient_matrix_UB_22      0.0581033000
_diffrn_orient_matrix_UB_23      -0.0852892000
_diffrn_orient_matrix_UB_31      0.0951112000
_diffrn_orient_matrix_UB_32      -0.0408339000
_diffrn_orient_matrix_UB_33      -0.0337270000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12824
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.511
_diffrn_reflns_theta_min         4.117
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.421
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73904
_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    1.347
_exptl_crystal_description       block
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         5445
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0414P)^2^+1.5333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0841
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5007
_reflns_number_total             5445
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03954f2.cif
_cod_data_source_block           dyz20190726
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7701837
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 B1 N1 P1 Pd1'
_shelx_estimated_absorpt_t_max   0.566
_shelx_estimated_absorpt_t_min   0.391
_diffrn_oxdiff_digest_frames
;
01e68220c8b55d8a872f8f38eed7be34e300035d42d
;
_diffrn_oxdiff_digest_hkl
;
01242964658b09dab088d14869ba68a03c7003
;
_reflns_odcompleteness_completeness 99.70
_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:
 C8(H8A,H8B), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C4(H4)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C19(H19A,H19B,H19C), C24(H24A,H24B,
 H24C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C14(H14A,H14B,H14C), C11(H11A,
 H11B,H11C), C15(H15A,H15B,H15C), C10(H10A,H10B,H10C), C16(H16A,H16B,H16C),
 C12(H12A,H12B,H12C)
;
_shelx_res_checksum              54523
_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 1.297
_oxdiff_exptl_absorpt_empirical_full_min 0.857