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_4084369
_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         'C38 H54 N12 Pd2 2+, 2(F6 P -), 2(C2 H3 N)'
_chemical_formula_sum            'C42 H60 F12 N14 P2 Pd2'
_chemical_formula_weight         1263.78
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 92.004(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.8605(12)
_cell_length_b                   7.9596(2)
_cell_length_c                   28.0165(13)
_cell_measurement_reflns_used    51132
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.62
_cell_measurement_theta_min      1.45
_cell_volume                     5094.8(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0547
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            51132
_diffrn_reflns_theta_full        25.62
_diffrn_reflns_theta_max         25.62
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.860
_exptl_absorpt_correction_T_max  0.9467
_exptl_absorpt_correction_T_min  0.6559
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         9607
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0605
_reflns_number_gt                8258
_reflns_number_total             9607
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500351j_si_002.cif
_cod_data_source_block           LnBu2Pd2PF62-togu5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      'P 21/c'
_cod_database_code               4084369