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_7701836
_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 Cl N2 P2 Pd, C H2 Cl2, C3 H7'
_chemical_formula_sum            'C28 H53 B Cl3 N2 P2 Pd'
_chemical_formula_weight         703.22
_chemical_name_systematic        tBu-PBP-Pd-Cl
_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
_atom_sites_solution_primary     iterative
_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                 93.997(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1561(2)
_cell_length_b                   30.3997(7)
_cell_length_c                   14.3424(3)
_cell_measurement_reflns_used    12921
_cell_measurement_temperature    289.00(10)
_cell_measurement_theta_max      28.3440
_cell_measurement_theta_min      3.9650
_cell_volume                     3547.45(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_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      air
_diffrn_ambient_temperature      289.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0528
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.905
_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    -53.00  35.00   1.00    7.49    --   15.98 -38.00-120.00   88
  2  \w    -20.00  55.00   1.00    7.49    --   15.98 -99.00 -60.00   75
  3  \w     -3.00  85.00   1.00    7.49    --   15.98  38.00 150.00   88
  4  \w    -55.00  45.00   1.00    7.49    --   15.98 -19.00 -30.00  100
  5  \w    -13.00  87.00   1.00    7.49    --   15.98  19.00  60.00  100
;
_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      -0.0402950000
_diffrn_orient_matrix_UB_12      0.0012194000
_diffrn_orient_matrix_UB_13      -0.0453815000
_diffrn_orient_matrix_UB_21      -0.0563305000
_diffrn_orient_matrix_UB_22      0.0154838000
_diffrn_orient_matrix_UB_23      0.0164092000
_diffrn_orient_matrix_UB_31      0.0529202000
_diffrn_orient_matrix_UB_32      0.0174107000
_diffrn_orient_matrix_UB_33      -0.0114010000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            35003
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.063
_diffrn_reflns_theta_min         3.441
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
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    1.317
_exptl_crystal_description       block
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.121
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         8576
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0605
_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^)+(0.0342P)^2^+7.5337P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1326
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6708
_reflns_number_total             8576
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03954f2.cif
_cod_data_source_block           pbp-pdcl-mq
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7701836
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C1 H1 N1 P1 B1 Pd1 Cl1'
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.834
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 C29-C30
 1.5 with sigma of 0.02
 C29-C31
 2.3 with sigma of 0.02
 C30-C31
 1.6 with sigma of 0.02
3. Rigid bond restraints
 C29, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C29, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C30, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C29, C30, 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
C29 \\sim C30 \\sim C31: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C25(H25A,H25B), C29(H29A,H29B), C30(H30A,H30B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C3(H3), C4(H4)
5.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C23(H23A,H23B,H23C), C14(H14A,H14B,H14C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C24(H24A,
 H24B,H24C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C),
 C15(H15A,H15B,H15C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              39779
_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 1.460
_oxdiff_exptl_absorpt_empirical_full_min 0.642