Enhancing catalytic activity towards Heck-reaction by using 4,5,9,10-tetra(arylimino)pyrenylidenyldipalladium tetrachlorides
Zhao, Tong; Xing, Qifeng; Song, Kuifeng; Ban, Qing; Liang, Tongling; Liu, Qingbin; Sun, Wen Hua; RSC Adv.  (2015) –; doi:10.1039/C4RA16193A

data_7219369
_publ_section_title
;
 Enhancing catalytic activity towards Heck-reaction by using
 4,5,9,10-tetra(arylimino)pyrenylidenyldipalladium tetrachlorides
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA16193A
_journal_year                    2015
_chemical_formula_moiety         'C48 H42 Cl2 N4 Pd'
_chemical_formula_sum            'C48 H42 Cl2 N4 Pd'
_chemical_formula_weight         852.16
_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
_audit_update_record
;
2014-11-27 deposited with the CCDC.
2015-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 106.27(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.764(4)
_cell_length_b                   12.137(2)
_cell_length_c                   21.618(4)
_cell_measurement_temperature    173(2)
_cell_volume                     4726.1(17)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_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  0.1035
_diffrn_reflns_av_sigmaI/netI    0.1041
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26306
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.13
_exptl_absorpt_coefficient_mu    0.539
_exptl_absorpt_correction_T_max  0.9596
_exptl_absorpt_correction_T_min  0.8919
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         8255
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1265
_refine_ls_R_factor_gt           0.1000
_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^)+(0.1482P)^2^+16.7121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2662
_refine_ls_wR_factor_ref         0.2883
_reflns_number_gt                6308
_reflns_number_total             8255
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra16193a1.cif
_cod_data_source_block           C1
_cod_original_cell_volume        4726.2(16)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7219369