#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:51:08 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179493 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/90/4339047.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_4339047
loop_
_publ_author_name
'Wu, Yuandong'
'Bensch, Wolfgang'
_publ_section_title
;
 Rb(3)Ti(3)(P(4)S(13))(PS(4))(3) and Cs(2)Ti(2)(P(2)S(8))(PS(4))(2): two
 polar titanium thiophosphates with complex one-dimensional tunnels.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6170
_journal_page_last               6177
_journal_paper_doi               10.1021/ic700478r
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'P7 S25 Ti3, 2.718(Rb), 0.281(Rb)'
_chemical_formula_sum            'P7 Rb3 S25 Ti3'
_chemical_formula_weight         1418.40
_space_group_IT_number           173
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2006-11-20T08:54:18_00:00
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   18.2475(9)
_cell_length_b                   18.2475(9)
_cell_length_c                   6.8687(3)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2.2
_cell_volume                     1980.67(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Stoe Imaging Diffraction System'
_diffrn_measurement_method       'φ 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  0.0522
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            10951
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.862
_exptl_absorpt_correction_T_max  0.4548
_exptl_absorpt_correction_T_min  0.3951
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   X-Shape
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.015(9)
_refine_ls_extinction_coef       0.0037(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         3164
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0318
_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)+(0.0449P)²+0.5564P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0754
_reflns_number_gt                2856
_reflns_number_total             3164
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            wu417.cif
_cod_data_source_block           wu417
_cod_database_code               4339047
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
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
Rb1 Rb 0.12114(4) 0.60327(4) 0.35973(10) 0.03258(17) Uani 0.9064(14) 1 d P
Rb2 Rb 0.0000 0.0000 0.2314(9) 0.0491(14) Uani 0.281(4) 3 d SP
Ti1 Ti -0.08247(5) 0.69116(4) 0.26376(12) 0.01244(16) Uani 1 1 d .
P1 P 0.3333 0.6667 0.8572(3) 0.0131(3) Uani 1 3 d S
P2 P 0.06296(6) 0.80552(7) -0.01270(17) 0.0129(2) Uani 1 1 d .
P3 P 0.13274(6) 0.49434(6) 0.8575(2) 0.0142(2) Uani 1 1 d .
S1 S 0.06956(6) 0.75342(6) 0.24499(17) 0.0151(2) Uani 1 1 d .
S2 S 0.13916(8) 0.44537(7) 0.59616(18) 0.0177(2) Uani 1 1 d .
S3 S -0.06554(6) 0.80215(7) 0.48199(18) 0.0162(2) Uani 1 1 d .
S4 S -0.07501(7) 0.60781(7) 0.53777(17) 0.0170(2) Uani 1 1 d .
S5 S -0.06282(7) 0.76140(8) -0.04227(19) 0.0193(2) Uani 1 1 d .
S6 S 0.25549(6) 0.55129(7) -0.00054(18) 0.0162(2) Uani 1 1 d .
S7 S -0.22848(6) 0.65635(7) 0.27064(19) 0.0167(2) Uani 1 1 d .
S8 S 0.08777(7) 0.57154(7) 0.8509(2) 0.0234(3) Uani 1 1 d .
S9 S 0.3333 0.6667 0.5755(3) 0.0201(4) Uani 1 3 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Rb Rb -0.9393 2.9676 '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
S1 Rb1 S8 105.46(3) . .
S1 Rb1 S2 163.22(4) . .
S8 Rb1 S2 58.69(3) . .
S1 Rb1 S8 96.58(3) . 4_564
S8 Rb1 S8 81.05(3) . 4_564
S2 Rb1 S8 76.47(3) . 4_564
S1 Rb1 S8 79.00(3) . 1_554
S8 Rb1 S8 160.35(4) . 1_554
S2 Rb1 S8 113.98(3) . 1_554
S8 Rb1 S8 79.42(3) 4_564 1_554
S1 Rb1 S9 120.11(2) . .
S8 Rb1 S9 74.44(4) . .
S2 Rb1 S9 63.78(2) . .
S8 Rb1 S9 139.93(3) 4_564 .
S8 Rb1 S9 120.45(4) 1_554 .
S1 Rb1 S4 54.41(3) . .
S8 Rb1 S4 66.38(3) . .
S2 Rb1 S4 110.33(3) . .
S8 Rb1 S4 55.06(3) 4_564 .
S8 Rb1 S4 103.46(3) 1_554 .
S9 Rb1 S4 134.50(4) . .
S1 Rb1 S6 77.36(3) . 3_565
S8 Rb1 S6 140.06(3) . 3_565
S2 Rb1 S6 117.97(3) . 3_565
S8 Rb1 S6 138.81(4) 4_564 3_565
S8 Rb1 S6 59.39(3) 1_554 3_565
S9 Rb1 S6 70.40(3) . 3_565
S4 Rb1 S6 131.64(3) . 3_565
S1 Rb1 S6 120.44(3) . .
S8 Rb1 S6 131.36(3) . .
S2 Rb1 S6 76.33(3) . .
S8 Rb1 S6 107.04(3) 4_564 .
S8 Rb1 S6 54.21(3) 1_554 .
S9 Rb1 S6 69.49(3) . .
S4 Rb1 S6 155.94(3) . .
S6 Rb1 S6 49.08(3) 3_565 .
S1 Rb1 P3 134.42(3) . .
S8 Rb1 P3 29.10(3) . .
S2 Rb1 P3 30.46(3) . .
S8 Rb1 P3 82.42(3) 4_564 .
S8 Rb1 P3 143.74(3) 1_554 .
S9 Rb1 P3 60.92(3) . .
S4 Rb1 P3 91.14(3) . .
S6 Rb1 P3 130.59(3) 3_565 .
S6 Rb1 P3 102.94(3) . .
S1 Rb1 P3 107.57(3) . 1_554
S8 Rb1 P3 143.76(3) . 1_554
S2 Rb1 P3 86.61(3) . 1_554
S8 Rb1 P3 80.78(3) 4_564 1_554
S8 Rb1 P3 28.92(2) 1_554 1_554
S9 Rb1 P3 100.91(3) . 1_554
S4 Rb1 P3 124.33(3) . 1_554
S6 Rb1 P3 63.21(2) 3_565 1_554
S6 Rb1 P3 31.64(2) . 1_554
P3 Rb1 P3 117.08(3) . 1_554
S1 Rb1 P3 68.72(2) . 4_564
S8 Rb1 P3 82.05(3) . 4_564
S2 Rb1 P3 101.51(3) . 4_564
S8 Rb1 P3 28.86(2) 4_564 4_564
S8 Rb1 P3 81.90(3) 1_554 4_564
S9 Rb1 P3 156.32(4) . 4_564
S4 Rb1 P3 29.84(2) . 4_564
S6 Rb1 P3 132.61(3) 3_565 4_564
S6 Rb1 P3 127.45(3) . 4_564
P3 Rb1 P3 96.74(3) . 4_564
P3 Rb1 P3 96.33(3) 1_554 4_564
Rb2 Rb2 Rb2 180.0 4_554 4
Rb2 Rb2 S3 61.73(8) 4_554 5_444
Rb2 Rb2 S3 118.28(9) 4 5_444
Rb2 Rb2 S3 61.73(8) 4_554 4_564
Rb2 Rb2 S3 118.27(8) 4 4_564
S3 Rb2 S3 99.41(11) 5_444 4_564
Rb2 Rb2 S3 61.72(8) 4_554 6_654
Rb2 Rb2 S3 118.27(8) 4 6_654
S3 Rb2 S3 99.41(11) 5_444 6_654
S3 Rb2 S3 99.40(11) 4_564 6_654
Rb2 Rb2 S3 118.38(8) 4_554 3_455
Rb2 Rb2 S3 61.62(8) 4 3_455
S3 Rb2 S3 80.664(11) 5_444 3_455
S3 Rb2 S3 80.663(11) 4_564 3_455
S3 Rb2 S3 179.89(17) 6_654 3_455
Rb2 Rb2 S3 118.38(8) 4_554 1_545
Rb2 Rb2 S3 61.62(8) 4 1_545
S3 Rb2 S3 80.663(11) 5_444 1_545
S3 Rb2 S3 179.89(17) 4_564 1_545
S3 Rb2 S3 80.662(11) 6_654 1_545
S3 Rb2 S3 99.27(11) 3_455 1_545
Rb2 Rb2 S3 118.38(8) 4_554 2_665
Rb2 Rb2 S3 61.62(8) 4 2_665
S3 Rb2 S3 179.89(17) 5_444 2_665
S3 Rb2 S3 80.662(11) 4_564 2_665
S3 Rb2 S3 80.661(11) 6_654 2_665
S3 Rb2 S3 99.27(11) 3_455 2_665
S3 Rb2 S3 99.27(11) 1_545 2_665
S5 Ti1 S7 90.47(5) . .
S5 Ti1 S3 100.03(5) . .
S7 Ti1 S3 82.52(4) . .
S5 Ti1 S1 82.65(4) . .
S7 Ti1 S1 168.99(5) . .
S3 Ti1 S1 90.20(4) . .
S5 Ti1 S2 90.34(5) . 4_564
S7 Ti1 S2 83.82(5) . 4_564
S3 Ti1 S2 162.88(5) . 4_564
S1 Ti1 S2 104.72(5) . 4_564
S5 Ti1 S4 163.89(5) . .
S7 Ti1 S4 102.53(5) . .
S3 Ti1 S4 91.16(5) . .
S1 Ti1 S4 85.78(4) . .
S2 Ti1 S4 81.79(4) 4_564 .
S9 P1 S6 117.71(6) . 3_566
S9 P1 S6 117.71(6) . 1_556
S6 P1 S6 100.12(8) 3_566 1_556
S9 P1 S6 117.71(6) . 2_666
S6 P1 S6 100.12(8) 3_566 2_666
S6 P1 S6 100.11(8) 1_556 2_666
S7 P2 S5 114.68(8) 6_664 .
S7 P2 S3 102.99(6) 6_664 6_664
S5 P2 S3 112.49(7) . 6_664
S7 P2 S1 110.39(7) 6_664 .
S5 P2 S1 102.75(7) . .
S3 P2 S1 113.93(7) 6_664 .
S8 P3 S2 115.67(8) . .
S8 P3 S4 117.55(8) . 4_565
S2 P3 S4 104.55(6) . 4_565
S8 P3 S6 111.72(7) . 1_556
S2 P3 S6 109.50(7) . 1_556
S4 P3 S6 95.89(7) 4_565 1_556
S8 P3 Rb1 58.51(6) . .
S2 P3 Rb1 59.65(5) . .
S4 P3 Rb1 147.08(6) 4_565 .
S6 P3 Rb1 116.26(5) 1_556 .
S8 P3 Rb1 61.37(6) . 1_556
S2 P3 Rb1 176.68(6) . 1_556
S4 P3 Rb1 78.52(5) 4_565 1_556
S6 P3 Rb1 71.13(5) 1_556 1_556
Rb1 P3 Rb1 117.08(3) . 1_556
S8 P3 Rb1 61.08(5) . 4_565
S2 P3 Rb1 96.58(5) . 4_565
S4 P3 Rb1 68.95(4) 4_565 4_565
S6 P3 Rb1 152.66(7) 1_556 4_565
Rb1 P3 Rb1 83.62(3) . 4_565
Rb1 P3 Rb1 83.30(2) 1_556 4_565
P2 S1 Ti1 86.80(5) . .
P2 S1 Rb1 132.84(6) . .
Ti1 S1 Rb1 108.86(4) . .
P3 S2 Ti1 86.81(6) . 4_565
P3 S2 Rb1 89.89(5) . .
Ti1 S2 Rb1 153.79(5) 4_565 .
P2 S3 Ti1 86.23(5) 5_455 .
P2 S3 Rb2 103.96(5) 5_455 4_565
Ti1 S3 Rb2 166.42(8) . 4_565
P2 S3 Rb2 104.95(5) 5_455 1_565
Ti1 S3 Rb2 112.43(9) . 1_565
Rb2 S3 Rb2 56.657(16) 4_565 1_565
P3 S4 Ti1 86.44(6) 4_564 .
P3 S4 Rb1 81.21(5) 4_564 .
Ti1 S4 Rb1 96.33(4) . .
P2 S5 Ti1 87.79(6) . .
P1 S6 P3 106.83(7) 1_554 1_554
P1 S6 Rb1 106.73(5) 1_554 2_665
P3 S6 Rb1 145.85(5) 1_554 2_665
P1 S6 Rb1 104.03(5) 1_554 .
P3 S6 Rb1 77.23(5) 1_554 .
Rb1 S6 Rb1 100.51(3) 2_665 .
P2 S7 Ti1 86.60(5) 5_455 .
P3 S8 Rb1 92.39(7) . .
P3 S8 Rb1 90.07(5) . 4_565
Rb1 S8 Rb1 100.92(4) . 4_565
P3 S8 Rb1 89.70(6) . 1_556
Rb1 S8 Rb1 160.35(4) . 1_556
Rb1 S8 Rb1 98.61(4) 4_565 1_556
P1 S9 Rb1 113.29(3) . .
P1 S9 Rb1 113.29(3) . 3_565
Rb1 S9 Rb1 105.40(4) . 3_565
P1 S9 Rb1 113.29(3) . 2_665
Rb1 S9 Rb1 105.40(4) . 2_665
Rb1 S9 Rb1 105.40(4) 3_565 2_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rb1 S1 3.4050(12) .
Rb1 S8 3.4255(17) .
Rb1 S2 3.4633(13) .
Rb1 S8 3.5427(13) 4_564
Rb1 S8 3.5453(17) 1_554
Rb1 S9 3.7479(11) .
Rb1 S4 3.8225(13) .
Rb1 S6 3.8353(12) 3_565
Rb1 S6 3.9189(13) .
Rb1 P3 4.0134(14) .
Rb1 P3 4.0391(15) 1_554
Rb1 P3 4.0475(12) 4_564
Rb2 Rb2 3.43434(15) 4_554
Rb2 Rb2 3.43436(15) 4
Rb2 S3 3.617(3) 5_444
Rb2 S3 3.617(3) 4_564
Rb2 S3 3.617(3) 6_654
Rb2 S3 3.621(3) 3_455
Rb2 S3 3.621(3) 1_545
Rb2 S3 3.621(3) 2_665
Ti1 S5 2.3938(15) .
Ti1 S7 2.4108(13) .
Ti1 S3 2.4121(14) .
Ti1 S1 2.4189(13) .
Ti1 S2 2.4546(13) 4_564
Ti1 S4 2.4659(14) .
P1 S9 1.935(3) .
P1 S6 2.1008(15) 3_566
P1 S6 2.1009(15) 1_556
P1 S6 2.1010(15) 2_666
P2 S7 2.0244(17) 6_664
P2 S5 2.0272(15) .
P2 S3 2.0399(15) 6_664
P2 S1 2.0409(16) .
P3 S8 1.9533(15) .
P3 S2 2.0347(18) .
P3 S4 2.0379(16) 4_565
P3 S6 2.1726(15) 1_556
P3 Rb1 4.0391(15) 1_556
P3 Rb1 4.0475(12) 4_565
S2 Ti1 2.4546(13) 4_565
S3 P2 2.0399(14) 5_455
S3 Rb2 3.617(3) 4_565
S3 Rb2 3.621(3) 1_565
S4 P3 2.0379(16) 4_564
S6 P1 2.1009(15) 1_554
S6 P3 2.1725(15) 1_554
S6 Rb1 3.8354(12) 2_665
S7 P2 2.0245(17) 5_455
S8 Rb1 3.5427(13) 4_565
S8 Rb1 3.5454(17) 1_556
S9 Rb1 3.7479(11) 3_565
S9 Rb1 3.7479(11) 2_665
