First Examples of Thallium Chalcogenide Cages. Syntheses,77Se,203Tl, and 205Tl NMR Study of the Tl4Se54- and Tl4Se64- Anions, the X-ray Crystal Structure of (2,2,2-crypt-K+)3Tl5Se53-, and Theoretical Studies
Janette Campbell; Hélène P. A. Mercier; David P. Santry; Reijo J. Suontamo; Horst Borrmann; Gary J. Schrobilgen; Inorganic Chemistry 40 (2001) 233–254; doi:10.1021/ic000779d

data_4319175
_publ_section_title
;
 First Examples of Thallium Chalcogenide Cages. Syntheses,77Se,203Tl, and
 205Tl NMR Study of the Tl4Se54- and Tl4Se64- Anions, the X-ray Crystal
 Structure of (2,2,2-crypt-K+)3Tl5Se53-, and Theoretical Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              233
_journal_page_last               254
_journal_paper_doi               10.1021/ic000779d
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C54 H108 K3 N6 O18 Se5 Tl5'
_chemical_formula_weight         2663.41
_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
_cell_angle_alpha                82.56(3)
_cell_angle_beta                 88.62(3)
_cell_angle_gamma                68.95(3)
_cell_formula_units_Z            2
_cell_length_a                   11.818(2)
_cell_length_b                   16.118(3)
_cell_length_c                   25.765(5)
_cell_measurement_temperature    293(2)
_cell_volume                     4540.4(17)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0916
_diffrn_reflns_av_sigmaI/netI    0.0842
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            22628
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         4.45
_exptl_absorpt_coefficient_mu    11.039
_exptl_crystal_density_diffrn    1.948
_exptl_crystal_F_000             2500
_refine_diff_density_max         7.302
_refine_diff_density_min         -4.081
_refine_diff_density_rms         0.490
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.179
_refine_ls_goodness_of_fit_obs   1.275
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         13271
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.233
_refine_ls_restrained_S_obs      1.314
_refine_ls_R_factor_all          0.1699
_refine_ls_R_factor_obs          0.1418
_refine_ls_shift/esd_max         -2.893
_refine_ls_shift/esd_mean        0.038
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1020P)^2^+831.3787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3690
_refine_ls_wR_factor_obs         0.3447
_reflns_number_observed          10391
_reflns_number_total             13465
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000779d.cif
_cod_data_source_block           tl5se5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1020P)^2^+831.3787P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1020P)^2^+831.3787P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4540.1(16)
_cod_database_code               4319175