Synthesis and Structure of Palladium 1,2,3-Triazol-5-ylidene Mesoionic Carbene PEPPSI Complexes and Their Catalytic Applications in the Mizoroki‒Heck Reaction
Keske, Eric C.; Zenkina, Olena V.; Wang, Ruiyao; Crudden, Cathleen M.; Organometallics 31 (2012) 6215–; doi:10.1021/om3005228

data_4079146
_publ_section_title
;
 Synthesis and Structure of Palladium 1,2,3-Triazol-5-ylidene Mesoionic
 Carbene PEPPSI Complexes and Their Catalytic Applications in the
 Mizoroki--Heck Reaction
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              6215
_journal_paper_doi               10.1021/om3005228
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C46 H54 Cl4 N8 Pd2'
_chemical_formula_weight         1073.57
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 101.053(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.235(6)
_cell_length_b                   8.948(4)
_cell_length_c                   19.304(8)
_cell_measurement_reflns_used    1366
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      21.22
_cell_measurement_theta_min      2.52
_cell_volume                     2582.8(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      180(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0715
_diffrn_reflns_av_sigmaI/netI    0.1883
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            11408
_diffrn_reflns_theta_full        27.17
_diffrn_reflns_theta_max         27.17
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.941
_exptl_absorpt_correction_T_max  0.9633
_exptl_absorpt_correction_T_min  0.8341
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;Disordered CH2Cl2 removed by squeeze in platon PWT

;
_refine_diff_density_max         0.916
_refine_diff_density_min         -1.254
_refine_diff_density_rms         0.137
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.859
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         8347
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.859
_refine_ls_R_factor_all          0.1509
_refine_ls_R_factor_gt           0.0663
_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^)+(0.0643P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1340
_refine_ls_wR_factor_ref         0.1603
_reflns_number_gt                4039
_reflns_number_total             8347
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3005228_si_003.cif
_cod_data_source_block           a1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2582.8(18)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4079146