Dinuclear Palladium Complexes of Pyrazole-Bridged Bis(NHC) Ligands: A Delicate Balance between Normal and Abnormal Carbene Coordination
Guo, Tongxun; Dechert, Sebastian; Meyer, Franc; Organometallics 33 (2014) 5145–; doi:10.1021/om500351j

data_4084372
_publ_section_title
;
 Dinuclear Palladium Complexes of Pyrazole-Bridged Bis(NHC) Ligands: A
 Delicate Balance between Normal and Abnormal Carbene Coordination
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5145
_journal_paper_doi               10.1021/om500351j
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C15 H19 Cl3 N6 Pd2, 0.5(C2 H3 N)'
_chemical_formula_sum            'C16 H20.5 Cl3 N6.5 Pd2'
_chemical_formula_weight         623.04
_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                82.860(7)
_cell_angle_beta                 69.725(6)
_cell_angle_gamma                71.791(6)
_cell_formula_units_Z            2
_cell_length_a                   8.4677(7)
_cell_length_b                   11.5408(10)
_cell_length_c                   11.9833(10)
_cell_measurement_reflns_used    20273
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      1.81
_cell_volume                     1043.32(16)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       \w
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0684
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20273
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    2.124
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.3879
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.983
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             610
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.536
_refine_diff_density_min         -1.521
_refine_diff_density_rms         0.266
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         20273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1267
_refine_ls_R_factor_gt           0.0995
_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^)+(0.1970P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2685
_refine_ls_wR_factor_ref         0.2852
_reflns_number_gt                13636
_reflns_number_total             20273
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500351j_si_002.cif
_cod_data_source_block           LEtPd2Cl3-togu10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/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 

 Adding full bibliography for 4084368--4084374.cif.
;
_cod_original_cell_volume        1043.32(15)
_cod_original_formula_sum        'C16 H20.50 Cl3 N6.50 Pd2'
_cod_database_code               4084372