#------------------------------------------------------------------------------
#$Date: 2016-02-19 23:18:51 +0100 (vie 19 de feb de 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/95/2019549.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2019549
loop_
_publ_author_name
'Pavlyuk, Volodymyr'
'Dmytriv, Grygoriy'
'Szyrej, Malgorzata'
'Levkovets, Sergii'
'Parasyuk, Oleh'
_publ_section_title
;
 A new semiconducting quaternary mixed halogenide: pentathallium dimercury
 pentabromide tetraiodide, Tl₅Hg₂Br₅I₄
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229614009966
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'Tl5 Hg2 Br5 I4'
_chemical_formula_moiety         '2(Br2 Hg I2), Br, 5(Tl)'
_chemical_formula_sum            'Br5 Hg2 I4 Tl5'
_chemical_formula_weight         2330.18
_chemical_name_systematic
;
Pentathallium dimercury pentabromide tetraiodide
;
_space_group_IT_number           140
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4 2c'
_symmetry_space_group_name_H-M   'I 4/m c m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5611(6)
_cell_length_b                   8.5611(6)
_cell_length_c                   30.227(2)
_cell_measurement_reflns_used    804
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.32
_cell_measurement_theta_min      3.37
_cell_volume                     2215.4(3)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2008)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2008)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur3 CCD'
_diffrn_measurement_method       'ω scans'
_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  0.0681
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            6153
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.32
_diffrn_reflns_theta_min         3.37
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    64.606
_exptl_absorpt_correction_T_max  0.517
_exptl_absorpt_correction_T_min  0.101
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    6.986
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3808.0
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.215
_refine_diff_density_min         -1.978
_refine_ls_extinction_coef       0.000074(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_matrix_type           full
_refine_ls_number_parameters     29
_refine_ls_number_reflns         804
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0392P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0637
_reflns_number_gt                725
_reflns_number_total             804
_reflns_threshold_expression     I>2sigma(I)
_iucr_refine_instructions_details
;
TITL Tl5Hg2Br5I4  in     I4/mcm
CELL  0.71073    8.5611    8.5611   30.2270    90.000    90.000    90.000
ZERR 1           0.0006    0.0006    0.0020     0.000     0.000     0.000
LATT   2
SYMM             - Y ,              X ,              Z
SYMM             - X ,            - Y ,              Z
SYMM               Y ,            - X ,              Z
SYMM               X ,            - Y ,    0.50000 - Z
SYMM               Y ,              X ,    0.50000 - Z
SYMM             - X ,              Y ,    0.50000 - Z
SYMM             - Y ,            - X ,    0.50000 - Z
SFAC I HG TL BR
UNIT 16 12 12 20
L.S. 4
BOND
FMAP 2
PLAN 20
merg 2
acta 55
WGHT    0.039200
EXTI    0.000074
FVAR       0.03418
TL1   3    0.350011    0.149989    0.000000    10.25000    0.01697    0.01697 =
         0.03130    0.00000    0.00000    0.00055
TL2   3    0.000000    0.000000    0.109198    10.25000    0.02407    0.02407 =
         0.02781    0.00000    0.00000    0.00000
TL3   3    0.000000    0.000000    0.250000    10.12500    0.03025    0.03025 =
         0.02955    0.00000    0.00000    0.00000
HG1    2    0.000000    0.500000    0.141681    10.25000    0.02260    0.02260 =
         0.02097    0.00000    0.00000   -0.00604
I1     1   -0.189660    0.310340    0.189376    10.50000    0.01927    0.01927 =
         0.02762    0.00362    0.00362   -0.00122
BR1   4    0.156870    0.343130    0.076016    10.50000    0.01452    0.01452 =
         0.02161   -0.00150    0.00150    0.00013
BR2   4    0.500000    0.500000    0.000000    10.12500    0.01331    0.01331 =
         0.02478    0.00000    0.00000    0.00000
hklf 4
REM  Tl5Hg2Br5I4 in     I4/mcm
REM R1 =  0.0271 for    725 Fo > 4sig(Fo)  and  0.0289 for all    804 data
REM     29 parameters refined using      0 restraints
END
WGHT      0.0391      0.0000
REM Highest difference peak  2.215,  deepest hole -1.978,  1-sigma level  0.391
Q1    1   0.0000  0.0000  0.2207  10.25000  0.05    2.21
Q2    1   0.4115  0.2171  0.0000  10.50000  0.05    2.13
Q3    1   0.0769  0.0565  0.1091  11.00000  0.05    2.01
Q4    1   0.4173  0.0827  0.0000  10.25000  0.05    1.93
Q5    1   0.0603  0.4397  0.1405  10.50000  0.05    1.75
Q6    1   0.0693  0.0693  0.2500  10.50000  0.05    1.69
Q7    1  -0.0780  0.4220  0.1343  10.50000  0.05    1.57
Q8    1   0.1172  0.2943  0.0739  11.00000  0.05    1.52
Q9    1   0.1367  0.2860  0.0776  11.00000  0.05    1.38
Q10   1   0.1504  0.3496  0.0989  10.50000  0.05    1.26
Q11   1   0.5737  0.1742  0.0000  10.50000  0.05    1.16
Q12   1   0.0000  0.5000  0.1711  10.25000  0.05    1.14
Q13   1  -0.2685  0.3345  0.2320  11.00000  0.05    1.09
Q14   1   0.4571 -0.0429  0.0000  10.25000  0.05    1.05
Q15   1   0.2806  0.2194  0.0000  10.25000  0.05    1.05
Q16   1  -0.1166  0.4906  0.1619  11.00000  0.05    1.03
Q17   1  -0.1233  0.2297  0.1812  11.00000  0.05    1.02
Q18   1  -0.2732  0.1055  0.2099  11.00000  0.05    1.01
Q19   1   0.0991  0.4009  0.0783  10.50000  0.05    1.01
Q20   1   0.2481  0.1052  0.0374  11.00000  0.05    0.98
;
_cod_data_source_file            yp3061sup1.cf
_cod_data_source_block           I
_cod_database_code               2019549
_cod_database_fobs_code          2019549
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -y, -z+1/2'
'y, x, -z+1/2'
'-x, y, -z+1/2'
'-y, -x, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1'
'y+1/2, x+1/2, -z+1'
'-x+1/2, y+1/2, -z+1'
'-y+1/2, -x+1/2, -z+1'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, y, z-1/2'
'-y, -x, z-1/2'
'x, -y, z-1/2'
'y, x, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, z'
'-y+1/2, -x+1/2, z'
'x+1/2, -y+1/2, z'
'y+1/2, x+1/2, z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Tl Tl1 0.35001(4) 0.14999(4) 0.0000 0.02175(17) Uani d S 1 4
Tl Tl2 0.0000 0.0000 0.109198(17) 0.02532(17) Uani d S 1 4
Tl Tl3 0.0000 0.0000 0.2500 0.0300(2) Uani d S 1 8
Hg Hg1 0.0000 0.5000 0.141681(16) 0.02206(17) Uani d S 1 4
I I1 -0.18966(5) 0.31034(5) 0.18938(2) 0.02205(18) Uani d S 1 2
Br Br1 0.15687(6) 0.34313(6) 0.07602(3) 0.0169(2) Uani d S 1 2
Br Br2 0.5000 0.5000 0.0000 0.0171(4) Uani d S 1 8
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Tl1 0.0170(2) 0.0170(2) 0.0313(3) 0.00055(17) 0.000 0.000
Tl2 0.0241(2) 0.0241(2) 0.0278(3) 0.000 0.000 0.000
Tl3 0.0303(3) 0.0303(3) 0.0295(4) 0.000 0.000 0.000
Hg1 0.0226(2) 0.0226(2) 0.0210(3) -0.00604(17) 0.000 0.000
I1 0.0193(2) 0.0193(2) 0.0276(3) -0.0012(2) 0.00362(15) 0.00362(15)
Br1 0.0145(3) 0.0145(3) 0.0216(5) 0.0001(3) 0.0015(2) -0.0015(2)
Br2 0.0133(5) 0.0133(5) 0.0248(9) 0.000 0.000 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
Br2 Tl1 Br2 . 13_454 136.393(15)
Br2 Tl1 Br1 . 19 74.637(8)
Br2 Tl1 Br1 13_454 19 74.637(8)
Br2 Tl1 Br1 . . 74.637(8)
Br2 Tl1 Br1 13_454 . 74.637(8)
Br1 Tl1 Br1 19 . 88.99(3)
Br2 Tl1 Tl1 . 17_655 111.804(8)
Br2 Tl1 Tl1 13_454 17_655 111.804(8)
Br1 Tl1 Tl1 19 17_655 135.503(16)
Br1 Tl1 Tl1 . 17_655 135.503(16)
I1 Hg1 I1 3_565 . 115.76(3)
I1 Hg1 Br1 3_565 . 112.593(11)
I1 Hg1 Br1 . . 112.593(11)
I1 Hg1 Br1 3_565 3_565 112.593(11)
I1 Hg1 Br1 . 3_565 112.593(11)
Br1 Hg1 Br1 . 3_565 87.48(4)
Hg1 Br1 Tl1 . . 178.24(3)
Tl1 Br2 Tl1 . 17_665 180.000(5)
Tl1 Br2 Tl1 . 18_565 90.0
Tl1 Br2 Tl1 17_665 18_565 90.0
Tl1 Br2 Tl1 . 2_655 90.0
Tl1 Br2 Tl1 17_665 2_655 90.0
Tl1 Br2 Tl1 18_565 2_655 180.0
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Tl1 Br2 . 3.2600(3)
Tl1 Br2 13_454 3.2600(3)
Tl1 Br1 19 3.2784(9)
Tl1 Br1 . 3.2784(9)
Tl1 Tl1 17_655 3.6319(10)
Hg1 I1 3_565 2.7113(6)
Hg1 I1 . 2.7113(6)
Hg1 Br1 . 2.7472(9)
Hg1 Br1 3_565 2.7472(9)
Br2 Tl1 17_665 3.2600(3)
Br2 Tl1 18_565 3.2600(3)
Br2 Tl1 2_655 3.2600(3)
