A Joint Experimental and Theoretical Study of Cation-π Interactions: Multiple-Decker Sandwich Complexes of Ferrocene with Alkali Metal Ions (Li+, Na+, K+, Rb+, Cs+)
Alireza Haghiri Ilkhechi; Jose M. Mercero; Iñaki Silanes; Michael Bolte; Matthias Scheibitz; Hans-Wolfram Lerner; Jesus M. Ugalde; Matthias Wagner; Journal of the American Chemical Society 127 (2005) 10656–10666; doi:10.1021/ja051544+

data_4111856
_publ_section_title
;
 A Joint Experimental and Theoretical Study of Cation-\p Interactions:
 Multiple-Decker Sandwich Complexes of Ferrocene with Alkali Metal Ions
 (Li+, Na+, K+, Rb+, Cs+)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10656
_journal_page_last               10666
_journal_paper_doi               10.1021/ja051544+
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C36 H58 B2 Fe N4 O4 Rb2'
_chemical_formula_weight         859.27
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.13(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.309(3)
_cell_length_b                   15.248(5)
_cell_length_c                   12.259(4)
_cell_measurement_reflns_used    4701
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.4
_cell_measurement_theta_min      3.6
_cell_volume                     2101.9(11)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_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  0.1834
_diffrn_reflns_av_sigmaI/netI    0.2032
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10870
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.72
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.699
_exptl_absorpt_correction_T_max  0.7378
_exptl_absorpt_correction_T_min  0.5882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULABS (Spek, 1990; Blessing, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_description       needle
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         3700
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.2266
_refine_ls_R_factor_gt           0.0978
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0846P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1932
_refine_ls_wR_factor_ref         0.2475
_reflns_number_gt                1356
_reflns_number_total             3700
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0515442Bsi20050324_023555.cif
_cod_data_source_block           wa313
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4111856