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_4109013
_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         'C24 H36 Tl, C36 H2 B2 F30 N, 2.5(C H2 Cl2)'
_chemical_formula_structural     '[Tl(C6Me6)2][H2N{B(C6F5)3}2].2.5(CH2Cl2)'
_chemical_formula_sum            'C62.5 H43 B2 Cl5 F30 N Tl'
_chemical_formula_weight         1781.22
_chemical_name_common            'Compound 5b'
_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 and CrysAlis RED'
_cell_angle_alpha                84.244(2)
_cell_angle_beta                 86.754(3)
_cell_angle_gamma                87.660(3)
_cell_formula_units_Z            2
_cell_length_a                   12.2427(5)
_cell_length_b                   13.9012(4)
_cell_length_c                   19.1784(6)
_cell_measurement_temperature    140(1)
_cell_volume                     3240.24(19)
_computing_cell_refinement
;
 CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p5 beta 
;
_computing_data_collection
;
 CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.27p5 beta 
;
_computing_data_reduction
;
 CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p5 beta 
;
_computing_molecular_graphics    'ORTEP (Johnson, 1971)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997b)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      140(1)
_diffrn_detector_area_resol_mean 16.0050
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0473
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35169
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.47
_exptl_absorpt_coefficient_mu    2.828
_exptl_absorpt_correction_T_max  1.049
_exptl_absorpt_correction_T_min  0.960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10 (Sheldrick, G.M., 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.826
_exptl_crystal_description       prism
_exptl_crystal_F_000             1742
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.167
_refine_diff_density_min         -1.174
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     949
_refine_ls_number_reflns         11290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0753
_reflns_number_gt                9319
_reflns_number_total             11290
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ja0657105si20060816_114040_4.cif
_cod_data_source_block           yanns17
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C62.50 H43 B2 Cl5 F30 N Tl'
_cod_database_code               4109013