Synthesis and structure of trans-bis(1,4-dimesityl-3-methyl-1,2,3-triazol-5-ylidene)palladium(II) dichloride and diacetate. Suzuki-Miyaura coupling of polybromoarenes with high catalytic turnover efficiencies.
Shaik, Jeelani Basha; Ramkumar, Venkatachalam; Varghese, Babu; Sankararaman, Sethuraman; Beilstein journal of organic chemistry 9 (2013) 698–704; doi:10.3762/bjoc.9.79

data_4029698
_publ_section_title
;
 Synthesis and structure of
 trans-bis(1,4-dimesityl-3-methyl-1,2,3-triazol-5-ylidene)palladium(II)
 dichloride and diacetate. Suzuki-Miyaura coupling of polybromoarenes with
 high catalytic turnover efficiencies.
;
_journal_name_full               'Beilstein journal of organic chemistry'
_journal_page_first              698
_journal_page_last               704
_journal_paper_doi               10.3762/bjoc.9.79
_journal_volume                  9
_journal_year                    2013
_chemical_formula_moiety         '(C42 H50 Cl2 N6 Pd).2(C2 H3 N)'
_chemical_formula_sum            'C46 H56 Cl2 N8 Pd'
_chemical_formula_weight         898.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           142
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.7337(4)
_cell_length_b                   14.7337(4)
_cell_length_c                   43.098(3)
_cell_measurement_reflns_used    5040
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.1
_cell_measurement_theta_min      2.8
_cell_volume                     9355.8(7)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altornare et al., 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker axs kappa apex2 CCD Diffractometer'
_diffrn_measurement_method       '\w and \f scan'
_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  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            39193
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.550
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1999)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.00028(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.329
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         2072
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.333
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0599
_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^)+(0.0269P)^2^+66.1200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1366
_refine_ls_wR_factor_ref         0.1459
_reflns_number_gt                1595
_reflns_number_total             2072
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1860-5397-9-79-S2.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        9355.9(7)
_cod_original_sg_symbol_H-M      I41/acd
_cod_database_code               4029698