Methoxyaryl Substituted Palladium bis-NHC Complexes - Synthesis and Electronic Effects
Allolio, Christoph; Doering, Katrin; Munz, Dominik; Poethig, Alexander; Doert, Thomas; Lang, Heinrich; Strassner, Thomas; Inorganica Chimica Acta 392 (2012) 204–210; doi:10.1016/j.ica.2012.06.009

data_1512604
_publ_contact_author_address
;Fachrichtung Chemie und Lebensmittelchemie
Professur fuer Physikalische Organische Chemie
TU Dresden
01062 Dresden
Germany
;
_publ_contact_author_email       thomas.strassner@chemie.tu-dresden.de
_publ_contact_author_fax         '+49 351 463 39679'
_publ_contact_author_name        'Thomas Strassner'
_publ_contact_author_phone       '+49 351 463 38571'
_publ_section_title
;
 Methoxyaryl Substituted Palladium bis-NHC Complexes - Synthesis and
 Electronic Effects
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              204
_journal_page_last               210
_journal_paper_doi               10.1016/j.ica.2012.06.009
_journal_volume                  392
_journal_year                    2012
_chemical_formula_moiety         'C25 H26 N6 O2 Pd, 2 (F6 P)'
_chemical_formula_sum            'C25 H26 F12 N6 O2 P2 Pd'
_chemical_formula_weight         838.86
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                90.000
_cell_angle_beta                 106.675(8)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   8.6060(13)
_cell_length_b                   18.876(3)
_cell_length_c                   20.4680(15)
_cell_measurement_reflns_used    379
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      22.726
_cell_measurement_theta_min      3.177
_cell_volume                     3185.1(7)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics
'Ortep III 1.0.3 (M.N.Burnett,C.K.Johnson,2000)'
_computing_publication_material  'XCIF 6.12 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 Altomare, 1999)'
_diffrn_ambient_pressure         101.3
_diffrn_ambient_temperature      198(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            48781
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         4.87
_exptl_absorpt_coefficient_mu    0.789
_exptl_absorpt_correction_T_max  0.9367
_exptl_absorpt_correction_T_min  0.8029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS 2.03.(Sheldrick,Bruker AXS Inc.,2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1672
_exptl_crystal_recrystallization_method acetonitrile/diethylether
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.950
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         6482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+7.1519P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0968
_reflns_number_gt                5241
_reflns_number_total             6482
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2012-392-204-210.cif
_cod_data_source_block           compund9
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1512604