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_4109018
_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         'C21 H24 Tl, C36 H2 B2 F30 N'
_chemical_formula_structural     '[Tl(toluene)3][H2N{B(C6F5)3}2]'
_chemical_formula_sum            'C57 H26 B2 F30 N Tl'
_chemical_formula_weight         1520.78
_chemical_name_common            'Compound 4b'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 91.68(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.781(5)
_cell_length_b                   18.151(8)
_cell_length_c                   21.698(14)
_cell_measurement_reflns_used    13191
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      2.91
_cell_volume                     5425(5)
_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    'SIR2002 (Giacovazzo, 2002)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD Area Detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            91366
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.60
_diffrn_standards_decay_%        negligible
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    3.123
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.75
_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    1.862
_exptl_crystal_description       block
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.088
_refine_diff_density_min         -1.138
_refine_diff_density_rms         0.086
_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     823
_refine_ls_number_reflns         12426
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0111P)^2^+12.5301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0810
_reflns_number_gt                9689
_reflns_number_total             12426
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0657105si20061102_033921_3.cif
_cod_data_source_block           s0399x
_cod_depositor_comments
;
 Adding a reference to a suboptimal entry.

 Antanas Vaitkus,
 2018-11-16
;
_cod_related_suboptimal_struct   4109040
_cod_database_code               4109018