#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:34:44 +0100 (Fri 25 de Mar de 2016) $
#$Revision: 179902 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/98/7019864.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7019864
loop_
_publ_author_name
'Sankar, Cheriyedath Raj'
'Kuropatwa, Bryan A.'
'Assoud, Abdeljalil'
'Kleinke, Holger'
_publ_section_title
;
 Structures and properties of the ternary thallium chalcogenides
 Tl(2)MQ(3) (M = Zr, Hf; Q = S, Se).
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9646
_journal_page_last               9650
_journal_paper_doi               10.1039/c2dt30782k
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'Hf Se3 Tl2'
_chemical_formula_weight         824.11
_chemical_name_systematic
;
?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.435(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.1544(11)
_cell_length_b                   3.8812(5)
_cell_length_c                   10.6224(14)
_cell_measurement_temperature    296(2)
_cell_volume                     333.36(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_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  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0594
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2237
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.37
_exptl_absorpt_coefficient_mu    79.992
_exptl_absorpt_correction_T_max  0.298
_exptl_absorpt_correction_T_min  0.027
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    8.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.594
_refine_diff_density_min         -4.451
_refine_diff_density_rms         0.688
_refine_ls_extinction_coef       0.0065(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         1061
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0558P)²+2.4979P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1245
_refine_ls_wR_factor_ref         0.1284
_reflns_number_gt                967
_reflns_number_total             1061
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30782k.txt
_cod_data_source_block           Tl2HfSe3
_cod_original_sg_symbol_H-M      P21/m
_cod_database_code               7019864
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Tl1 Tl 0.06445(9) 0.2500 0.65805(7) 0.0228(2) Uani 1 2 d S
Tl2 Tl 0.74973(8) 0.2500 0.00293(6) 0.0217(2) Uani 1 2 d S
Hf1 Hf 0.40960(7) 0.2500 0.33423(5) 0.0078(2) Uani 1 2 d S
Se1 Se 0.13036(18) 0.2500 0.19044(15) 0.0130(4) Uani 1 2 d S
Se2 Se 0.45271(17) 0.2500 0.78917(13) 0.0086(3) Uani 1 2 d S
Se3 Se 0.69076(16) 0.2500 0.51355(12) 0.0066(3) Uani 1 2 d S
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Tl1 0.0223(4) 0.0216(4) 0.0246(4) 0.000 0.0033(3) 0.000
Tl2 0.0275(4) 0.0222(4) 0.0149(4) 0.000 0.0015(3) 0.000
Hf1 0.0101(3) 0.0067(3) 0.0064(4) 0.000 0.0005(2) 0.000
Se1 0.0116(7) 0.0125(7) 0.0134(7) 0.000 -0.0040(5) 0.000
Se2 0.0121(6) 0.0059(6) 0.0084(7) 0.000 0.0037(5) 0.000
Se3 0.0085(6) 0.0053(6) 0.0060(6) 0.000 0.0014(5) 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Se1 Tl1 Se1 77.84(4) 3_566 3_556
Se1 Tl1 Se3 74.36(4) 3_566 1_455
Se1 Tl1 Se3 74.36(4) 3_556 1_455
Se1 Tl1 Se2 108.12(4) 3_566 .
Se1 Tl1 Se2 108.12(4) 3_556 .
Se3 Tl1 Se2 176.71(4) 1_455 .
Se1 Tl2 Se1 78.23(4) 3_655 3_665
Se1 Tl2 Se2 78.26(4) 3_655 1_554
Se1 Tl2 Se2 78.26(4) 3_665 1_554
Se1 Hf1 Se2 96.01(4) . 3_656
Se1 Hf1 Se2 96.01(4) . 3_666
Se2 Hf1 Se2 93.27(4) 3_656 3_666
Se1 Hf1 Se3 92.39(4) . 3_666
Se2 Hf1 Se3 171.49(5) 3_656 3_666
Se2 Hf1 Se3 87.21(3) 3_666 3_666
Se1 Hf1 Se3 92.39(4) . 3_656
Se2 Hf1 Se3 87.21(3) 3_656 3_656
Se2 Hf1 Se3 171.49(5) 3_666 3_656
Se3 Hf1 Se3 91.08(4) 3_666 3_656
Se1 Hf1 Se3 173.36(5) . .
Se2 Hf1 Se3 88.54(4) 3_656 .
Se2 Hf1 Se3 88.54(4) 3_666 .
Se3 Hf1 Se3 82.98(4) 3_666 .
Se3 Hf1 Se3 82.98(4) 3_656 .
Hf1 Se1 Tl2 93.61(4) . 3_655
Hf1 Se1 Tl2 93.61(4) . 3_665
Tl2 Se1 Tl2 78.23(4) 3_655 3_665
Hf1 Se1 Tl1 99.56(5) . 3_556
Tl2 Se1 Tl1 100.424(16) 3_655 3_556
Tl2 Se1 Tl1 166.82(6) 3_665 3_556
Hf1 Se1 Tl1 99.56(5) . 3_566
Tl2 Se1 Tl1 166.82(6) 3_655 3_566
Tl2 Se1 Tl1 100.424(17) 3_665 3_566
Tl1 Se1 Tl1 77.84(4) 3_556 3_566
Hf1 Se2 Hf1 93.27(4) 3_656 3_666
Hf1 Se2 Tl2 91.22(4) 3_656 1_556
Hf1 Se2 Tl2 91.22(4) 3_666 1_556
Hf1 Se2 Tl1 103.59(4) 3_656 .
Hf1 Se2 Tl1 103.59(4) 3_666 .
Tl2 Se2 Tl1 158.21(5) 1_556 .
Hf1 Se3 Hf1 91.08(4) 3_666 3_656
Hf1 Se3 Hf1 97.02(4) 3_666 .
Hf1 Se3 Hf1 97.02(4) 3_656 .
Hf1 Se3 Tl1 93.18(4) 3_666 1_655
Hf1 Se3 Tl1 93.18(4) 3_656 1_655
Hf1 Se3 Tl1 165.41(5) . 1_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tl1 Se1 3.0888(14) 3_566
Tl1 Se1 3.0888(14) 3_556
Tl1 Se3 3.2297(16) 1_455
Tl1 Se2 3.2898(16) .
Tl2 Se1 3.0759(14) 3_655
Tl2 Se1 3.0759(14) 3_665
Tl2 Se2 3.0981(15) 1_554
Hf1 Se1 2.5725(16) .
Hf1 Se2 2.6694(10) 3_656
Hf1 Se2 2.6694(10) 3_666
Hf1 Se3 2.7189(10) 3_666
Hf1 Se3 2.7189(10) 3_656
Hf1 Se3 2.7847(14) .
Se1 Tl2 3.0759(14) 3_655
Se1 Tl2 3.0759(14) 3_665
Se1 Tl1 3.0888(14) 3_556
Se1 Tl1 3.0888(14) 3_566
Se2 Hf1 2.6694(10) 3_656
Se2 Hf1 2.6694(10) 3_666
Se2 Tl2 3.0981(15) 1_556
Se3 Hf1 2.7189(10) 3_666
Se3 Hf1 2.7189(10) 3_656
Se3 Tl1 3.2297(16) 1_655
