Flexible Steric Bulky Bis(Imino)acenaphthene (BIAN)-Supported N-Heterocyclic Carbene Palladium Precatalysts: Catalytic Application in Buchwald-Hartwig Amination in Air.
Lan, Xiao-Bing; Li, Yinwu; Li, Yan-Fang; Shen, Dong-Sheng; Ke, Zhuofeng; Liu, Feng-Shou; The Journal of organic chemistry 82 (2017) 2914–2925; doi:10.1021/acs.joc.6b02867

data_4032420
_publ_section_title
;
 Flexible Steric Bulky Bis(Imino)acenaphthene (BIAN)-Supported
 N-Heterocyclic Carbene Palladium Precatalysts: Catalytic Application in
 Buchwald-Hartwig Amination in Air.
;
_journal_issue                   6
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              2914
_journal_page_last               2925
_journal_paper_doi               10.1021/acs.joc.6b02867
_journal_volume                  82
_journal_year                    2017
_chemical_formula_sum            'C255 H226 Cl14 N12 Pd4'
_chemical_formula_weight         4380.38
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 96.562(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.2100(11)
_cell_length_b                   26.743(2)
_cell_length_c                   31.090(2)
_cell_measurement_temperature    296(2)
_cell_volume                     10911.4(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1735
_diffrn_reflns_av_sigmaI/netI    0.1177
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            152779
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.554
_exptl_absorpt_correction_T_max  0.9570
_exptl_absorpt_correction_T_min  0.9264
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4520
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.515
_refine_diff_density_min         -1.241
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1139
_refine_ls_number_reflns         20921
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1840
_refine_ls_R_factor_gt           0.0971
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1478P)^2^+52.4672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2473
_refine_ls_wR_factor_ref         0.3110
_reflns_number_gt                10644
_reflns_number_total             20921
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo6b02867_si_002.cif
_cod_data_source_block           C2
_cod_original_cell_volume        10911.2(15)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4032420