Smallest molecular chalcogenidometalate anions of the heaviest metals: syntheses, structures, and their interconversion.
Thiele, G.; Donsbach, C.; Riedel, R.; Marsch, M.; Harms, K.; Dehnen, S.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 5958–5967; doi:10.1039/c5dt03996g

data_7037269
_publ_section_title
;
 Smallest molecular chalcogenidometalate anions of the heaviest metals:
 syntheses, structures, and their interconversion.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5958
_journal_page_last               5967
_journal_paper_doi               10.1039/c5dt03996g
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         '0.25(K3.77 Se8 Tl4), 0.03(Tl2)'
_chemical_formula_sum            'K0.94 Se2 Tl1.06'
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_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_Hall           '-I 4 2c'
_space_group_name_H-M_alt        'I 4/m c m'
_symmetry_space_group_name_Hall  '-I 4 2c'
_symmetry_space_group_name_H-M   'I 4/m c m'
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-10-12 deposited with the CCDC.
2015-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
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_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDSII'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1902
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
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_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            3160
_diffrn_reflns_point_group_measured_fraction_full 1.000
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.672
_diffrn_reflns_theta_min         3.598
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    54.829
_exptl_absorpt_correction_T_max  0.1154
_exptl_absorpt_correction_T_min  0.0091
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_exptl_crystal_colour_primary    black
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_exptl_crystal_description       block
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_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
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_refine_ls_extinction_coef       0.0049(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.232
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     11
_refine_ls_number_reflns         147
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.232
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0111P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0565
_refine_ls_wR_factor_ref         0.0567
_reflns_Friedel_coverage         0.000
_reflns_number_gt                145
_reflns_number_total             147
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03996g2.cif
_cod_data_source_block           Compound7
_cod_depositor_comments
'Adding full bibliography for 7037263--7037272.cif.'
_cod_original_cell_volume        449.51(15)
_cod_database_code               7037269
_olex2_refinement_description
;
1. Shared sites
{K1, Tl2}
2. Uiso/Uaniso restraints and constraints
Uanis(K1) = Uanis(Tl2)
3. Others
 Sof(Tl2)=0.125*(1-FVAR(2))
 Sof(K1)=0.125*FVAR(2)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'