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_4089118
_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 H62 Cl3 N3 Pd'
_chemical_formula_weight         917.78
_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                 103.412(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5167(3)
_cell_length_b                   22.5311(5)
_cell_length_c                   20.9505(5)
_cell_measurement_reflns_used    8017
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      74.2080
_cell_measurement_theta_min      3.9020
_cell_volume                     4828.9(2)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1099
_diffrn_reflns_av_sigmaI/netI    0.0917
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15404
_diffrn_reflns_theta_full        59.00
_diffrn_reflns_theta_max         59.00
_diffrn_reflns_theta_min         3.92
_exptl_absorpt_coefficient_mu    4.885
_exptl_absorpt_correction_T_max  0.5479
_exptl_absorpt_correction_T_min  0.4129
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.158
_refine_diff_density_min         -2.354
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         6934
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.1145
_refine_ls_R_factor_gt           0.1031
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2658
_refine_ls_wR_factor_ref         0.2863
_reflns_number_gt                5569
_reflns_number_total             6934
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00723_si_002.cif
_cod_data_source_block           exp_554
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4089118