Structure and Dynamics of Imidazolium- and Pyridinium-Substituted η3-Cycloheptatrienide-Pd Complexes
Jandl, Christian; Öfele, Karl; Kühn, Fritz E.; Herrmann, Wolfgang A.; Pöthig, Alexander; Organometallics 33 (2014) 6398–; doi:10.1021/om500738d

data_4089672
_publ_section_title
;
 Structure and Dynamics of Imidazolium- and Pyridinium-Substituted
 \h3-Cycloheptatrienide-Pd Complexes
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6398
_journal_paper_doi               10.1021/om500738d
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C17 H16 Br2 N2 Pd'
_chemical_formula_sum            'C17 H16 Br2 N2 Pd'
_chemical_formula_weight         514.52
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                94.676(2)
_cell_angle_beta                 91.954(2)
_cell_angle_gamma                103.620(2)
_cell_formula_units_Z            2
_cell_length_a                   7.9127(3)
_cell_length_b                   8.8284(4)
_cell_length_c                   12.3548(6)
_cell_measurement_reflns_used    6442
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.5726
_cell_measurement_theta_min      2.6526
_cell_volume                     834.73(6)
_computing_cell_refinement       'SAINT (Bruker, 2008b)'
_computing_data_collection       'APEX II Control Software (Bruker, 2008a)'
_computing_data_reduction        'SAINT (Bruker, 2008b)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2004)'
_computing_structure_refinement
'SHELXL97 (Sheldrick, 1997), SHELXLE (Huebschle, 2011)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25093
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    5.895
_exptl_absorpt_correction_T_max  0.666
_exptl_absorpt_correction_T_min  0.357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.047
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         4863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0178P)^2^+0.1522P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0465
_refine_ls_wR_factor_ref         0.0514
_reflns_number_gt                3599
_reflns_number_total             4863
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om500738d_si_002.cif
_cod_data_source_block           Compound_2d
_cod_database_code               4089672