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_4029697
_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         'C46 H56 N6 O4 Pd'
_chemical_formula_sum            'C46 H56 N6 O4 Pd'
_chemical_formula_weight         863.37
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_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                 106.720(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.426(2)
_cell_length_b                   10.1901(18)
_cell_length_c                   16.699(3)
_cell_measurement_reflns_used    682
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      17.97
_cell_measurement_theta_min      2.55
_cell_volume                     2188.0(6)
_computing_cell_refinement       APEXII,Bruker,2004
_computing_data_collection       APEXII,Bruker,2004
_computing_data_reduction        SAINT,Bruker,2004
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEXII 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  0.0901
_diffrn_reflns_av_sigmaI/netI    0.0827
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8624
_diffrn_reflns_theta_full        21.21
_diffrn_reflns_theta_max         21.21
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_T_max  0.9325
_exptl_absorpt_correction_T_min  0.8910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker,2004)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         2386
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.1014
_reflns_number_gt                1518
_reflns_number_total             2386
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1860-5397-9-79-S3.cif
_cod_data_source_block           new
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/Beilstein/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        2188.1(6)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               4029697