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_7125131
_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         'C48 H37 B I N O2 P2 Pd, 3(C6 H6)'
_chemical_formula_sum            'C66 H55 B I N O2 P2 Pd'
_chemical_formula_weight         1200.16
_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
_audit_creation_date             2016-03-07
_audit_creation_method
;
Olex2 1.2
(compiled Feb 16 2016 13:09:46 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-03-27 deposited with the CCDC.
2016-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.077(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.188(3)
_cell_length_b                   20.733(4)
_cell_length_c                   18.380(4)
_cell_measurement_reflns_used    2904
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      21.15
_cell_measurement_theta_min      2.29
_cell_volume                     5469.9(19)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1144
_diffrn_reflns_av_unetI/netI     0.0975
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            49698
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.536
_diffrn_reflns_theta_min         1.529
_diffrn_source_current           600.0
_diffrn_source_power             30.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.009
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1965 before and 0.0914 after correction.
The Ratio of minimum to maximum transmission is 0.7440.
The \l/2 correction factor is 0.0015.
;
_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    1.457
_exptl_crystal_description       plate
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.795
_refine_diff_density_min         -1.333
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       0.00085(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         11278
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0250P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1079
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8219
_reflns_number_total             11278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc07079e2.cif
_cod_data_source_block           n16_a48sad
_cod_original_cell_volume        5469.8(19)
_cod_database_code               7125131
_shelx_estimated_absorpt_t_max   0.897
_shelx_estimated_absorpt_t_min   0.765
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C21(H21), C22(H22), C23(H23),
 C24(H24), C25(H25), C31(H31), C32(H32), C33(H33), C34(H34), C41(H41), C42(H42),
  C43(H43), C44(H44), C45(H45), C51(H51), C52(H52), C53(H53), C54(H54),
 C55(H55), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C71(H71), C72(H72),
  C73(H73), C74(H74), C75(H75), C81(H81), C82(H82), C84(H84), C85(H85),
 C100(H100), C101(H101), C102(H102), C103(H103), C104(H104), C105(H105),
 C90(H90), C91(H91), C92(H92), C93(H93), C94(H94), C95(H95), C110(H110),
 C111(H111), C112(H112), C113(H113), C114(H114), C115(H115)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'