Pd-PEPPSI Complexes Bearing Bulky [(1,2-Di-(tert-butyl)acenaphthyl] (DtBu-An) on N-Heterocarbene Backbones: Highly Efficient for Suzuki‒Miyaura Cross-Coupling under Aerobic Conditions
Lan, Xiao-Bing; Chen, Fu-Min; Ma, Bei-Bei; Shen, Dong-Sheng; Liu, Feng-Shou; Organometallics 35 (2016) 3852–; doi:10.1021/acs.organomet.6b00723

data_4089117
_publ_section_title
;
 Pd-PEPPSI Complexes Bearing Bulky [(1,2-Di-(tert-butyl)acenaphthyl]
 (DtBu-An) on N-Heterocarbene Backbones: Highly Efficient for
 Suzuki--Miyaura Cross-Coupling under Aerobic Conditions
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              3852
_journal_paper_doi               10.1021/acs.organomet.6b00723
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C50 H63 Cl2 N3 Pd'
_chemical_formula_weight         883.33
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.1375(17)
_cell_angle_beta                 90.0769(19)
_cell_angle_gamma                103.6539(19)
_cell_formula_units_Z            4
_cell_length_a                   10.2847(3)
_cell_length_b                   20.8622(4)
_cell_length_c                   22.4773(5)
_cell_measurement_reflns_used    4781
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     4685.5(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku Pilatus 300K'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0807
_diffrn_reflns_av_sigmaI/netI    0.0832
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            38842
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  0.8987
_exptl_absorpt_correction_T_min  0.8987
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.597
_refine_diff_density_min         -1.344
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1037
_refine_ls_number_reflns         16201
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1084
_refine_ls_R_factor_gt           0.0840
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1586P)^2^+31.6185P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2353
_refine_ls_wR_factor_ref         0.2713
_reflns_number_gt                12751
_reflns_number_total             16201
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00723_si_002.cif
_cod_data_source_block           s
_cod_original_cell_volume        4685.45(18)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4089117