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_4089676
_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_compound_source        'see text'
_chemical_formula_moiety         'C19 H20 Br2 N2 Pd, C2 H6 O S'
_chemical_formula_sum            'C21 H26 Br2 N2 O Pd S'
_chemical_formula_weight         620.71
_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
_cell_angle_alpha                106.268(3)
_cell_angle_beta                 102.414(2)
_cell_angle_gamma                99.185(2)
_cell_formula_units_Z            2
_cell_length_a                   9.0983(4)
_cell_length_b                   10.1476(4)
_cell_length_c                   13.3960(5)
_cell_measurement_reflns_used    9557
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.9930
_cell_measurement_theta_min      2.2421
_cell_volume                     1127.19(8)
_computing_cell_refinement       'SAINT (Bruker, 2012)'
_computing_data_collection       'APEX II Control Software (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2012)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2004)'
_computing_structure_refinement
'SHELXL2013 (Sheldrick, 2013), 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 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  'MONTEL optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'rotating anode FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0793
_diffrn_reflns_av_sigmaI/netI    0.0696
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22191
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    4.475
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.829
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.144
_refine_diff_density_max         1.604
_refine_diff_density_min         -1.449
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         5158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'W=1/[\S^2^(FO^2^)+(0.0645P)^2^] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1129
_reflns_number_gt                4117
_reflns_number_total             5158
_reflns_threshold_expression     i>2\s(i)
_cod_data_source_file            om500738d_si_002.cif
_cod_data_source_block           Compound_3e_DMSO
_cod_database_code               4089676