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_4079147
_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            'C26.75 H31.5 Cl3.5 N4 Pd'
_chemical_formula_weight         639.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.601(2)
_cell_angle_beta                 98.819(2)
_cell_angle_gamma                100.718(2)
_cell_formula_units_Z            4
_cell_length_a                   10.5239(3)
_cell_length_b                   15.6327(4)
_cell_length_c                   21.1539(6)
_cell_measurement_reflns_used    7353
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      2.86
_cell_volume                     3132.62(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23037
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.912
_exptl_absorpt_correction_T_max  0.9473
_exptl_absorpt_correction_T_min  0.7716
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1302
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
Difference electron density maps revealed the presence of disordered 
CH2Cl2 molecules, which were ultimately modeled through the
use of the SQUEEZE subroutine of the PLATON software suite. PLATON 
Reference: P. v.d. Sluis & A.L. Spek. Acta Cryst. (1990), A46, 194. 
One solvent accessible void per lattice were found, comprising a 
total volume of 685 A3 and contributing a total of 129 electrons. 
The void was thus assigned to 3 disordered CH2Cl2 molecules, which 
contribute 3x42 = 126 electrons, and ocuppy about 180 A3 in space. 
The larger volume of the void may be a result of the disorder. The
contributions have been included in all derived crystal quantities.
;
_refine_diff_density_max         2.434
_refine_diff_density_min         -1.090
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         12132
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0584
_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^)+(0.0980P)^2^+1.1282P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1585
_refine_ls_wR_factor_ref         0.1678
_reflns_number_gt                9120
_reflns_number_total             12132
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3005228_si_004.cif
_cod_data_source_block           cc138a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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        3132.62(15)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C26.75 H31.50 Cl3.50 N4 Pd'
_cod_database_code               4079147