#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:47:59 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179155 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/16/4311685.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_4311685
loop_
_publ_author_name
'Navid Soheilnia'
'Katja M. Kleinke'
'Enkhtsetseg Dashjav'
'Heather L. Cuthbert'
'John E. Greedan'
'Holger Kleinke'
_publ_section_title
;
 Crystal Structure and Physical Properties of a New CuTi2S4 Modification
 in Comparison to the Thiospinel
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6473
_journal_page_last               6478
_journal_paper_doi               10.1021/ic0495113
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'Cu S4 Ti2'
_chemical_formula_weight         287.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           166
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_hydrogens   geom
_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                120.00
_cell_formula_units_Z            12
_cell_length_a                   7.0242(4)
_cell_length_b                   7.0242(4)
_cell_length_c                   34.834(4)
_cell_measurement_temperature    293(2)
_cell_volume                     1488.4(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.804
_diffrn_measured_fraction_theta_max 0.804
_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  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            2505
_diffrn_reflns_theta_full        33.15
_diffrn_reflns_theta_max         33.15
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    8.891
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.850
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.786
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.173
_refine_ls_extinction_coef       0.00029(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     36
_refine_ls_number_reflns         619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0322
_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)+(0.0225P)²+14.3484P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0686
_reflns_number_gt                528
_reflns_number_total             619
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0495113si20040414_120533.cif
_cod_data_source_block           CuTi2S4_rhombohedral
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               4311685
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.0000 0.0000 0.18759(3) 0.0120(3) Uani 1 6 d S . .
Cu2 Cu 0.0000 0.0000 0.35449(3) 0.0116(2) Uani 1 6 d S . .
Ti1 Ti 0.0000 0.0000 0.0000 0.0142(5) Uani 1 12 d S . .
Ti2 Ti 0.0000 0.0000 0.5000 0.0218(5) Uani 1 12 d S . .
Ti3 Ti 0.34224(11) 0.17112(6) 0.08568(3) 0.0101(2) Uani 1 2 d S . .
S1 S 0.0000 0.0000 0.12320(6) 0.0078(4) Uani 1 6 d S . .
S2 S 0.0000 0.0000 0.28892(6) 0.0087(4) Uani 1 6 d S . .
S3 S 0.15702(8) 0.31404(15) 0.04234(4) 0.0083(2) Uani 1 2 d S . .
S4 S 0.16020(8) 0.32040(16) 0.45437(4) 0.0097(2) Uani 1 2 d S . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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
_geom_angle_publ_flag
S1 Cu1 S4 112.22(4) . 31 ?
S1 Cu1 S4 112.22(4) . 32_445 ?
S4 Cu1 S4 106.58(4) 31 32_445 ?
S1 Cu1 S4 112.22(4) . 33_545 ?
S4 Cu1 S4 106.58(4) 31 33_545 ?
S4 Cu1 S4 106.58(4) 32_445 33_545 ?
S1 Cu1 Ti3 136.67(2) . 25 ?
S4 Cu1 Ti3 53.65(3) 31 25 ?
S4 Cu1 Ti3 111.10(6) 32_445 25 ?
S4 Cu1 Ti3 53.65(3) 33_545 25 ?
S1 Cu1 Ti3 136.67(2) . 27_445 ?
S4 Cu1 Ti3 111.10(6) 31 27_445 ?
S4 Cu1 Ti3 53.65(3) 32_445 27_445 ?
S4 Cu1 Ti3 53.65(3) 33_545 27_445 ?
Ti3 Cu1 Ti3 72.92(4) 25 27_445 ?
S1 Cu1 Ti3 136.67(2) . 26_455 ?
S4 Cu1 Ti3 53.65(3) 31 26_455 ?
S4 Cu1 Ti3 53.65(3) 32_445 26_455 ?
S4 Cu1 Ti3 111.10(6) 33_545 26_455 ?
Ti3 Cu1 Ti3 72.92(4) 25 26_455 ?
Ti3 Cu1 Ti3 72.92(4) 27_445 26_455 ?
S3 Cu2 S3 109.95(4) 8 7_445 ?
S3 Cu2 S3 109.95(4) 8 9_455 ?
S3 Cu2 S3 109.95(4) 7_445 9_455 ?
S3 Cu2 S2 108.98(4) 8 . ?
S3 Cu2 S2 108.98(4) 7_445 . ?
S3 Cu2 S2 108.98(4) 9_455 . ?
S3 Ti1 S3 180.00(5) 19 . ?
S3 Ti1 S3 86.55(4) 19 21 ?
S3 Ti1 S3 93.45(4) . 21 ?
S3 Ti1 S3 86.55(4) 19 20 ?
S3 Ti1 S3 93.45(4) . 20 ?
S3 Ti1 S3 86.55(4) 21 20 ?
S3 Ti1 S3 93.45(4) 19 3 ?
S3 Ti1 S3 86.55(4) . 3 ?
S3 Ti1 S3 180.00(5) 21 3 ?
S3 Ti1 S3 93.45(4) 20 3 ?
S3 Ti1 S3 93.45(4) 19 2 ?
S3 Ti1 S3 86.55(4) . 2 ?
S3 Ti1 S3 93.45(4) 21 2 ?
S3 Ti1 S3 180.00(5) 20 2 ?
S3 Ti1 S3 86.55(4) 3 2 ?
S4 Ti2 S4 180.0 20_556 2 ?
S4 Ti2 S4 84.31(4) 20_556 21_556 ?
S4 Ti2 S4 95.69(4) 2 21_556 ?
S4 Ti2 S4 95.69(4) 20_556 3 ?
S4 Ti2 S4 84.31(4) 2 3 ?
S4 Ti2 S4 180.00(4) 21_556 3 ?
S4 Ti2 S4 95.69(4) 20_556 . ?
S4 Ti2 S4 84.31(4) 2 . ?
S4 Ti2 S4 95.69(4) 21_556 . ?
S4 Ti2 S4 84.31(4) 3 . ?
S4 Ti2 S4 84.31(4) 20_556 19_556 ?
S4 Ti2 S4 95.69(4) 2 19_556 ?
S4 Ti2 S4 84.31(4) 21_556 19_556 ?
S4 Ti2 S4 95.69(4) 3 19_556 ?
S4 Ti2 S4 180.00(4) . 19_556 ?
S4 Ti3 S4 99.75(6) 15_554 13_544 ?
S4 Ti3 S2 89.55(4) 15_554 25 ?
S4 Ti3 S2 89.55(4) 13_544 25 ?
S4 Ti3 S1 93.00(4) 15_554 . ?
S4 Ti3 S1 93.00(4) 13_544 . ?
S2 Ti3 S1 176.05(7) 25 . ?
S4 Ti3 S3 171.41(4) 15_554 3 ?
S4 Ti3 S3 88.83(3) 13_544 3 ?
S2 Ti3 S3 90.50(4) 25 3 ?
S1 Ti3 S3 86.53(4) . 3 ?
S4 Ti3 S3 88.83(3) 15_554 . ?
S4 Ti3 S3 171.41(4) 13_544 . ?
S2 Ti3 S3 90.50(4) 25 . ?
S1 Ti3 S3 86.53(4) . . ?
S3 Ti3 S3 82.58(5) 3 . ?
S4 Ti3 Cu1 50.19(3) 15_554 25 ?
S4 Ti3 Cu1 50.19(3) 13_544 25 ?
S2 Ti3 Cu1 82.74(5) 25 25 ?
S1 Ti3 Cu1 101.21(5) . 25 ?
S3 Ti3 Cu1 138.28(3) 3 25 ?
S3 Ti3 Cu1 138.28(3) . 25 ?
Cu1 S1 Ti3 122.12(4) . 3 ?
Cu1 S1 Ti3 122.12(4) . . ?
Ti3 S1 Ti3 94.36(6) 3 . ?
Cu1 S1 Ti3 122.12(4) . 2 ?
Ti3 S1 Ti3 94.36(6) 3 2 ?
Ti3 S1 Ti3 94.36(6) . 2 ?
Cu2 S2 Ti3 126.07(4) . 27_445 ?
Cu2 S2 Ti3 126.07(4) . 25 ?
Ti3 S2 Ti3 88.86(6) 27_445 25 ?
Cu2 S2 Ti3 126.07(4) . 26_455 ?
Ti3 S2 Ti3 88.86(6) 27_445 26_455 ?
Ti3 S2 Ti3 88.86(6) 25 26_455 ?
Cu2 S3 Ti1 123.35(6) 13_554 . ?
Cu2 S3 Ti3 121.59(3) 13_554 2 ?
Ti1 S3 Ti3 95.37(3) . 2 ?
Cu2 S3 Ti3 121.59(3) 13_554 . ?
Ti1 S3 Ti3 95.37(3) . . ?
Ti3 S3 Ti3 91.96(5) 2 . ?
Cu1 S4 Ti3 76.16(4) 31 8 ?
Cu1 S4 Ti3 76.16(4) 31 7_455 ?
Ti3 S4 Ti3 91.52(5) 8 7_455 ?
Cu1 S4 Ti2 118.58(6) 31 . ?
Ti3 S4 Ti2 133.63(2) 8 . ?
Ti3 S4 Ti2 133.63(2) 7_455 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 S1 2.243(2) . ?
Cu1 S4 2.2754(11) 31 ?
Cu1 S4 2.2754(11) 32_445 ?
Cu1 S4 2.2754(11) 33_545 ?
Cu1 Ti3 2.8762(12) 25 ?
Cu1 Ti3 2.8762(12) 27_445 ?
Cu1 Ti3 2.8762(12) 26_455 ?
Cu2 S3 2.2684(10) 8 ?
Cu2 S3 2.2684(10) 7_445 ?
Cu2 S3 2.2685(10) 9_455 ?
Cu2 S2 2.284(2) . ?
Ti1 S3 2.4134(11) 19 ?
Ti1 S3 2.4134(11) . ?
Ti1 S3 2.4134(11) 21 ?
Ti1 S3 2.4134(11) 20 ?
Ti1 S3 2.4134(11) 3 ?
Ti1 S3 2.4134(11) 2 ?
Ti2 S4 2.5150(11) 20_556 ?
Ti2 S4 2.5150(11) 2 ?
Ti2 S4 2.5150(11) 21_556 ?
Ti2 S4 2.5150(11) 3 ?
Ti2 S4 2.5150(11) . ?
Ti2 S4 2.5150(11) 19_556 ?
Ti3 S4 2.3856(9) 15_554 ?
Ti3 S4 2.3856(9) 13_544 ?
Ti3 S2 2.4415(15) 25 ?
Ti3 S1 2.4581(13) . ?
Ti3 S3 2.5073(10) 3 ?
Ti3 S3 2.5073(10) . ?
Ti3 Cu1 2.8762(12) 25 ?
S1 Ti3 2.4581(13) 3 ?
S1 Ti3 2.4581(13) 2 ?
S2 Ti3 2.4415(15) 27_445 ?
S2 Ti3 2.4415(15) 25 ?
S2 Ti3 2.4416(15) 26_455 ?
S3 Cu2 2.2684(10) 13_554 ?
S3 Ti3 2.5073(10) 2 ?
S4 Cu1 2.2754(11) 31 ?
S4 Ti3 2.3856(9) 8 ?
S4 Ti3 2.3856(9) 7_455 ?
