Isolation and properties of a palladium PBP pincer complex featuring an ambiphilic boryl site.
Schuhknecht, Danny; Ritter, Florian; Tauchert, Michael E.; Chemical communications (Cambridge, England) 52 (2016) 11823–11826; doi:10.1039/c6cc07079e

data_7125127
_publ_section_title
;
 Isolation and properties of a palladium PBP pincer complex featuring an
 ambiphilic boryl site.
;
_journal_issue                   79
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11823
_journal_page_last               11826
_journal_paper_doi               10.1039/c6cc07079e
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C40 H40 B P3 Pd'
_chemical_formula_sum            'C40 H40 B P3 Pd'
_chemical_formula_weight         730.84
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-08-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-03-27 deposited with the CCDC.
2016-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.699(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6783(16)
_cell_length_b                   18.823(3)
_cell_length_c                   17.516(3)
_cell_measurement_reflns_used    6275
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.21
_cell_volume                     3488.9(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multi opitcal layer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0784
_diffrn_reflns_av_unetI/netI     0.0746
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39214
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.57
_diffrn_reflns_theta_min         2.16
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1574 before and 0.0839 after correction.
The Ratio of minimum to maximum transmission is 0.6042.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.002
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         10149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.6040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.1003
_reflns_number_gt                8011
_reflns_number_total             10149
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc07079e2.cif
_cod_data_source_block           a15_a52sad
_cod_original_cell_volume        3489.0(9)
_cod_database_code               7125127
_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.a Aromatic/amide H refined with riding coordinates:
 C25(H25), C45(H45), C55(H55), C61(H61), C65(H65), C12(H12), C64(H64),
 C51(H51), C22(H22), C33(H33), C15(H15), C62(H62), C24(H24), C32(H32), C63(H63),
  C23(H23), C41(H41), C44(H44), C52(H52), C13(H13), C31(H31), C14(H14),
 C53(H53), C43(H43), C1AA(H1AA), C54(H54), C34(H34), C42(H42)
2.b Idealised Me refined as rotating group:
 C80(H80A,H80B,H80C), C82(H82A,H82B,H82C), C81(H81A,H81B,H81C), C70(H70A,H70B,
 H70C)
;
_olex2_submission_special_instructions 'No special instructions were received'