Palladium(II) Complexes with Anionic N-Heterocyclic Carbene‒Borate Ligands as Catalysts for the Amination of Aryl Halides
Winkler, Andrea; Brandhorst, Kai; Freytag, Matthias; Jones, Peter G.; Tamm, Matthias; Organometallics 35 (2016) 1160–; doi:10.1021/acs.organomet.6b00217

data_4088587
_publ_section_title
;
 Palladium(II) Complexes with Anionic N-Heterocyclic Carbene--Borate
 Ligands as Catalysts for the Amination of Aryl Halides
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1160
_journal_paper_doi               10.1021/acs.organomet.6b00217
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C56 H50 B F15 N2 Pd'
_chemical_formula_weight         1153.19
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.7286(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.77451(10)
_cell_length_b                   18.90823(10)
_cell_length_c                   25.13604(16)
_cell_measurement_reflns_used    85321
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.6850
_cell_measurement_theta_min      3.5410
_cell_volume                     5061.58(6)
_computing_cell_refinement
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44)  
;
_computing_data_collection
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_data_reduction
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3543
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0152
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            132991
_diffrn_reflns_theta_full        75.00
_diffrn_reflns_theta_max         75.79
_diffrn_reflns_theta_min         3.56
_exptl_absorpt_coefficient_mu    3.803
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.543
_refine_diff_density_min         -1.163
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         10516
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+3.8680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0820
_reflns_number_gt                10229
_reflns_number_total             10516
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00217_si_002.cif
_cod_data_source_block           andre42
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4088587