Thallium(I) Sandwich, Multidecker, and Ether Complexes Stabilized by Weakly-Coordinating Anions: A Spectroscopic, Structural, and Theoretical Investigation
Yann Sarazin; David L. Hughes; Nikolas Kaltsoyannis; Joseph A. Wright; Manfred Bochmann; Journal of the American Chemical Society 129 (2007) 881–894; doi:10.1021/ja0657105

data_4109014
_publ_section_title
;
 Thallium(I) Sandwich, Multidecker, and Ether Complexes Stabilized by
 Weakly-Coordinating Anions: A Spectroscopic, Structural, and Theoretical
 Investigation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              881
_journal_page_last               894
_journal_paper_doi               10.1021/ja0657105
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety
'2(C36 H2 B2 F30 N), C11 H12 Cl2 Fe Tl, 2(C10 H10 Fe), 4(C H2 Cl2), Tl'
_chemical_formula_structural     '[Tl2(FeCp2)3][H2N{B(C6F5)3}2]2.5CH2Cl2'
_chemical_formula_sum            'C107 H44 B4 Cl10 F60 Fe3 N2 Tl2'
_chemical_formula_weight         3471.47
_chemical_name_common            'Compound 6'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.719(7)
_cell_angle_beta                 81.749(7)
_cell_angle_gamma                84.366(7)
_cell_formula_units_Z            1
_cell_length_a                   10.0625(9)
_cell_length_b                   11.6162(10)
_cell_length_c                   24.6374(19)
_cell_measurement_reflns_used    14076
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      29.83
_cell_measurement_theta_min      3.74
_cell_volume                     2817.6(4)
_computing_cell_refinement
'CrysAlis RED (Oxford Diffraction Ltd., 2005)'
_computing_data_collection
'CrysAlis CCD (Oxford Diffraction Ltd., 2005)'
_computing_data_reduction
'CrysAlis RED (Oxford Diffraction Ltd., 2005)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
;
PLATON (Spek, 2003)
ENCIFER (Allen, 2004)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, 1992)'
_diffrn_ambient_temperature      140(1)
_diffrn_detector_area_resol_mean 16.0050
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3/CCD'
_diffrn_measurement_method       'Thin slice \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_sigmaI/netI    0.1237
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            38083
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.83
_diffrn_reflns_theta_min         3.74
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.615
_exptl_absorpt_correction_T_max  0.8689
_exptl_absorpt_correction_T_min  0.4194
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSPACK (Oxford Diffraction Ltd., 2005)'
_exptl_crystal_colour            'light orange'
_exptl_crystal_density_diffrn    2.046
_exptl_crystal_description       plate
_exptl_crystal_F_000             1670
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.357
_refine_diff_density_min         -1.542
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     916
_refine_ls_number_reflns         14076
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.1511
_refine_ls_R_factor_gt           0.0669
_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^)+(0.0888P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1590
_refine_ls_wR_factor_ref         0.1770
_reflns_number_gt                6527
_reflns_number_total             14076
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0657105si20060816_114040_5.cif
_cod_data_source_block           06jaw003
_cod_database_code               4109014