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]∞1.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_4310093
_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            'C74 H152 N10 Na4 O24 Se8 Tl4'
_chemical_formula_weight         3107.18
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 94.17(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.768(3)
_cell_length_b                   16.635(3)
_cell_length_c                   21.254(4)
_cell_measurement_temperature    168(2)
_cell_volume                     5207.6(17)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      168(2)
_diffrn_measurement_device
;
 STOE Imaging Plate Diffractometer System (STOE, 1995)'
;
_diffrn_measurement_method       oscillation
_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  0.0667
_diffrn_reflns_av_sigmaI/netI    0.0806
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30330
_diffrn_reflns_theta_max         24.12
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    9.051
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_density_meas      1.92
_exptl_crystal_density_method    'floatation in perfluorodecaline'
_exptl_crystal_description       cube
_exptl_crystal_F_000             2996
_exptl_crystal_size_max          0.046
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.046
_refine_diff_density_max         1.137
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.860
_refine_ls_goodness_of_fit_obs   0.956
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         8169
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.867
_refine_ls_restrained_S_obs      0.956
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_obs          0.0331
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0065P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0446
_refine_ls_wR_factor_obs         0.0394
_reflns_number_observed          5478
_reflns_number_total             8226
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            ic0510922si20050825_035123_1.cif
_cod_data_source_block           '[2,2,2-crypt-Na]4[Tl4Se8].en'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0065P)^2^+0.0000P] 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^)+(0.0065P)^2^+0.0000P] 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        5207.6(18)
_cod_database_code               4310093