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_4109012
_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         'H2 O2 Tl4, 2(C36 H2 B2 F30 N), 4(C H2 Cl2)'
_chemical_formula_structural     '[Tl4(mu-OH)2][H2N{B(C6F5)3}2]2.4(CH2Cl2)'
_chemical_formula_sum            'C76 H14 B4 Cl8 F60 N2 O2 Tl4'
_chemical_formula_weight         3271.2
_chemical_name_common            'Compound 3'
_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                105.075(5)
_cell_angle_beta                 92.968(6)
_cell_angle_gamma                101.382(7)
_cell_formula_units_Z            1
_cell_length_a                   11.4827(11)
_cell_length_b                   14.1996(12)
_cell_length_c                   14.2725(8)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2189.7(3)
_computing_cell_refinement       'DENZO, COLLECT'
_computing_data_reduction        'DENZO, COLLECT'
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD Area Detector'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            53697
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.97
_diffrn_standards_decay_%        negligible
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    7.760
_exptl_absorpt_correction_T_max  0.5108
_exptl_absorpt_correction_T_min  0.2199
_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    2.480
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.710
_refine_diff_density_min         -2.417
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         10044
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0298P)^2^+9.5352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0844
_reflns_number_gt                9127
_reflns_number_total             10044
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0657105si20060816_114040_2.cif
_cod_data_source_block           2005src0804
_cod_database_code               4109012