Monomeric Ferrocene Bis-Imidazoline Bis-Palladacycles: Variation of Pd‒Pd Distances by an Interplay of Metallophilic, Dispersive, and Coulombic Interactions
Weber, Manuel; Klein, Johannes E. M. N.; Miehlich, Burkhard; Frey, Wolfgang; Peters, René; Organometallics 32 (2013) 5810–; doi:10.1021/om400360d

data_4081507
_publ_section_title
;
 Monomeric Ferrocene Bis-Imidazoline Bis-Palladacycles: Variation of
 Pd--Pd Distances by an Interplay of Metallophilic, Dispersive, and
 Coulombic Interactions
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5810
_journal_paper_doi               10.1021/om400360d
_journal_volume                  32
_journal_year                    2013
_chemical_absolute_configuration rd
_chemical_formula_moiety         'C64 H58 Fe N4 O8 Pd2 S2, 0.5(C5 H12)'
_chemical_formula_sum            'C66.5 H64 Fe N4 O8 Pd2 S2'
_chemical_formula_weight         1379.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.8177(12)
_cell_length_b                   32.078(2)
_cell_length_c                   9.8829(6)
_cell_measurement_reflns_used    9548
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      1.67
_cell_volume                     5965.7(6)
_computing_cell_refinement       'Bruker APEXII Software Suite, 2008'
_computing_data_collection       'Bruker APEXII Software Suite, 2008'
_computing_data_reduction        'Bruker APEXII Software Suite, 2008'
_computing_molecular_graphics    'SHELXTL-plus, XP (Sheldrick, 1991)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Kappa APEXII Duo'
_diffrn_measurement_method       'Omega + Phi Scans'
_diffrn_radiation_monochromator  Triumph
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            37210
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.967
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            light-red
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             2820
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.699
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.014(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         10465
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+7.4407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0732
_reflns_number_gt                9548
_reflns_number_total             10465
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400360d_si_004.cif
_cod_data_source_block           s1910lm
_cod_original_cell_volume        5965.7(7)
_cod_original_formula_sum        'C66.50 H64 Fe N4 O8 Pd2 S2'
_cod_database_code               4081507