Syntheses; 77Se, 203Tl, and 205Tl NMR; and Theoretical Studies of the Tl2Se66-, Tl3Se65-, and Tl3Se75- Anions and the X-ray Crystal Structures of [2,2,2-crypt-Na]4[Tl4Se8].en and [2,2,2-crypt-Na]2[Tl2Se4]\ιnfty1.en
Ayaaz M. Pirani; Hélène P. A. Mercier; Reijo J. Suontamo; Gary J. Schrobilgen; David P. Santry; Horst Borrmann; Inorganic Chemistry 44 (2005) 8770–8785; doi:10.1021/ic0510922

data_4310094
_publ_section_title
;
Syntheses; 77Se, 203Tl, and 205Tl NMR; and Theoretical Studies of the
Tl2Se66-, Tl3Se65-, and Tl3Se75- Anions and the X-ray Crystal Structures of
[2,2,2-crypt-Na]4[Tl4Se8].en and [2,2,2-crypt-Na]2[Tl2Se4]\\infty1.en
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8770
_journal_page_last               8785
_journal_paper_doi               10.1021/ic0510922
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C38 H80 N6 Na2 O12 Se4 Tl2'
_chemical_formula_weight         1583.64
_chemical_name_systematic
; 
 ? 
;
_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                 99.87(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.246(3)
_cell_length_b                   14.360(3)
_cell_length_c                   26.673(5)
_cell_measurement_temperature    293(2)
_cell_volume                     5375.8(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0565
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            43412
_diffrn_reflns_theta_full        24.09
_diffrn_reflns_theta_max         24.09
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    8.770
_exptl_crystal_density_diffrn    1.957
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3064
_refine_diff_density_max         2.830
_refine_diff_density_min         -1.343
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.483
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         8460
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.483
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.176
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1133
_reflns_number_gt                6764
_reflns_number_total             8460
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0510922si20050825_035123_2.cif
_cod_data_source_block           '[2,2,2-crypt-Na]2[Tl2Se4].en'
_cod_database_code               4310094