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_4109039
_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         'C16 H40 O4 Tl, C36 H2 B2 F30 N'
_chemical_formula_structural     '[Tl(OEt2)4][H2N{B(C6F5)3}2]'
_chemical_formula_sum            'C52 H42 B2 F30 N O4 Tl'
_chemical_formula_weight         1540.86
_chemical_name_common            'Compound 2b'
_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                86.556(2)
_cell_angle_beta                 76.904(2)
_cell_angle_gamma                87.120(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2481(4)
_cell_length_b                   13.7603(5)
_cell_length_c                   17.3040(6)
_cell_measurement_temperature    120(2)
_cell_volume                     2833.38(17)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD Area Detector'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  'graphite OR 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  0.0881
_diffrn_reflns_av_sigmaI/netI    0.0680
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            57381
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.93
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.995
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.64
_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    1.806
_exptl_crystal_description       block
_exptl_crystal_F_000             1508
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.114
_refine_diff_density_min         -1.433
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     864
_refine_ls_number_reflns         12829
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0606P)^2^+5.6255P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1450
_reflns_number_gt                9058
_reflns_number_total             12829
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ja0657105subopt20060816_114040_1.cif
_cod_data_source_block           s0621
_cod_depositor_comments
;
 Replacing the _cod_related_optimal_structure data name with the shorter
 version (_cod_related_optimal_struct) that is formally defined in the
 'cif_cod' dictionary.

 Antanas Vaitkus,
 2018-11-16

 Removed the _cod_suboptimal_structure data item in preparation for
 its deprecation. The fact that the structure is a suboptimal one
 should be derived from the presence of the _cod_related_optimal_struct
 data item.

 Antanas Vaitkus,
 2019-05-21
;
_cod_related_optimal_struct      4109017
_cod_database_code               4109039