# SUBMISSION DETAILS

_publ_contact_autor
;
     'V. Manri\´quez'
     Universidad de Chile   
      Facultad de Ciencias
      Departamento de Quimica 
      Casilla 653
      Santiago Chile
;
_publ_contact_author_phone        '056 02 6787252'
_publ_contact_author_fax          '056 02 2713888'
_publ_contact_author_email        vmanriqu@uchile.cl


_publ_requested_journal           
'Zeitschrift f\"ur Kristallographie-New Crystal Structures'
_publ_requested_coeditor_name     ?

_publ_contact_letter
; Dear Sirs,

 We would like to submit this CIF for publication in
  "Zeitschrift f\"ur Kristallographie" as a "New Crystal
  Structure". The next file is Figure of the manuscript.
;
#==============================================================================
#TITLE AND AUTHOR LIST

_publ_section_title
;
Crystal structure of potassium bismuth
hexathiodiphosphate, KBiP~2~S~6~
;

loop_
 _publ_author_name
 _publ_author_address
     ' Manriquez, Vi\´ctor'
;    Universidad de Chile   
     Facultad de Ciencias
     Departamento de Qui\´mica 
     Casilla 653
     Santiago Chile
;
     ' Galda\´mez, Antonio'
;    Universidad de Chile   
     Facultad de Ciencias
     Departamento de Qui\´mica 
     Casilla 653
     Santiago Chile
;    
     ' Leo\´n, D. Ruiz'
;    Universidad de Chile   
     Facultad de Ciencias
     Departamento de Qui\´mica 
     Casilla 653
     Santiago Chile
; 
     'Garland, M.T.'
;    Universidad de Chile   
     Facultad de Ciencias Fi\´sicas y Matema\´ticas
     Departamento de Fi\´sica 
     Casilla 487-3
     Santiago Chile
;             
     'Jime\´nez, M.'
;    Universidad de Chile   
     Facultad de Ciencias Fi\´sicas y Matema\´ticas
     Departamento de Fi\´sica 
     Casilla 487-3
     Santiago Chile
;     
#==============================================================================

# TEXT

_publ_section_abstract
;

;

_publ_section_comment
;
In the course of our work on Chalcophosphate[1,2], were have preparated the 
quaternary
bismuth hexathiodiphosphate KBiP~2~S~6~.  The title compound has a complicated 
layered structure, which contains the ethane-like [P~2~S~6~]^4-^ ligand. The 
structure 
can be characterized by layered of condensed S~6~ distorted octahedra 
alternately centered
by P~2 pairs and Bi atoms. The staircase layered of [BiP~2~S~6~]^1-^ groups in 
the a-b plane
are held together by a single layer of K^+^ ions. The bond lengths in the 
hexathiodiphosphate
[P~2~S~6~]^4-^ are d(P-P) = 2.219(3)\%A and d(P-S) range from 1.962(3)\%A to 
2.058(3)\%A.
The ethane-like [P~2~S~6~]^4-^ ligand chelates to 4 bi atoms, the bond lengths 
d(Bi-S) 
range from 2.706(2)\%A to 3.143(2)\%A. KBiP~2~S~6~ is structurally related to 
Na~0.16Bi~1.28P~2~S~6~ [3] and KBiP~2~Se~6~ [4]. 
;

_publ_section_experimental
;
All manipulations were carried out under Ar atmosphere. For the synthesis of
KBiP~2~S~6~ stoichiometric amounts of the corresponding high purity (99.99%)
elements, supplied by Aldrich, were mixed an sealed in quartz tubes after 
evacuation. 
The mixture was them heated at 1123K for two weeks. The reacted matter was 
slowly cooled
(0.4 K/min)to room temperature.
;

_publ_section_references
;
[1] Ruiz-León, D; Manriquez, V.; Kasaneva, J.; Avila, R.E.: Insertión of
trivalent cations in layered MPS~3~ (M=Mn, Cd) materials.
Mater. Res. Bull. 37(2002) 981-989.
  
[2] Galdámez, A.; Manriquez, V.; Kasaneva, J.; Avila, R.E.: synthesis, 
Characterization and electrical propierties of quaternary selenodiphosphates:
AMP~2~Se~6~ with A=Cu, Ag and M=Bi,Sb. Mater. Res. Bull. (2003) accepted.
 
[3] McCarthy, T.; Kanatzidis, M.: Synthesis in molten alkali metal polythiophsphate
fluxes.The new quaternary bismuth an antimony thiophaspates ABiP~2~S~7~(A=K,Rb), 
A~3~M(PS~4~)~2~(A=K,Rb, Cs; M=Sb,Bi), Cs~3~Bi~2~(PS~4~) and Na~0.16Bi~1.28P~2~S~6~.
J. Alloys Compounds 236 (1996) 70-85.  

[4] Breshears, J.; Kanatzidis, M.: B-KBiP~2~Se~6~(M=Sb,Bi): Kinetically 
Accessible Phases Obtained from rapid crystallization of amorphous precursors.
J. Am. Chem. Soc. 122 (2000) 7839-7840.  

[5] Sheldrick, G. M.: SHELXL-97. Program for crystal structure refinement.
University of G\"ottingen, Germany 1997.

[6] Dowty, E.: ATOMS (V 3.0).A Complete Programa for displaying Atomic
structures. By Shape Software, Kingsport, USA 1994.
;

_publ_section_figure_captions
;

;

_publ_section_acknowledgements
;
This work was supported by FONDECYT through operating grants 
N\% 1020683, "Beca Apoyo Tesis 2002" and Fundación Andes for the single 
crystal diffractometer
;

#==============================================================================

data_KBiP2S6 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
potassium bismuth hexathiodiphosphate
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural   'K Bi P2 S6' 
_chemical_formula_sum   'Bi1 K1 P2 S6' 
_chemical_formula_weight          502.38 
 
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' 
 'K'  'K'   0.2009   0.2494 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Bi'  'Bi'  -4.1077  10.2566 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    p1211
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z' 
 
_cell_length_a                    6.6200(6) 
_cell_length_b                    7.4058(7) 
_cell_length_c                    9.9002(9) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  92.1080(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      485.04(8) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        prism  
_exptl_crystal_colour             'red dark' 
_exptl_crystal_size_max           0.2 
_exptl_crystal_size_mid           0.075 
_exptl_crystal_size_min           0.075 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     3.440 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              456 
_exptl_absorpt_coefficient_mu     20.148 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Siemens SMART CCD'  
_diffrn_measurement_method        'phi/omega' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             3908 
_diffrn_reflns_av_R_equivalents   0.0342 
_diffrn_reflns_av_sigmaI/netI     0.0855 
_diffrn_reflns_limit_h_min        -8 
_diffrn_reflns_limit_h_max        8 
_diffrn_reflns_limit_k_min        -9 
_diffrn_reflns_limit_k_max        9 
_diffrn_reflns_limit_l_min        -13 
_diffrn_reflns_limit_l_max        13 
_diffrn_reflns_theta_min          2.06 
_diffrn_reflns_theta_max          28.00 
_reflns_number_total              2071 
_reflns_number_gt                 1901 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'Bruker SMART (BRUKER 1996)' 
_computing_cell_refinement        'Bruker SAINTPLUS V6.02 (BRUKER 1997)' 
_computing_data_reduction         'Bruker SHELXTL V6.10(BRUKER 2000)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Atoms 3.0 (Dowty E., 1994)' 
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)' 
 
_refine_special_details 
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.012(7) 
_refine_ls_number_reflns          2071 
_refine_ls_number_parameters      91 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.0290 
_refine_ls_R_factor_gt            0.0265 
_refine_ls_wR_factor_ref          0.0595 
_refine_ls_wR_factor_gt           0.0586 
_refine_ls_goodness_of_fit_ref    0.676 
_refine_ls_restrained_S_all       0.675 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
 
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_Wyckoff_symbol
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Bi Bi 0.79399(4) 0.77391(6) 0.98012(3) 0.02185(9) Uani 1 2 a d . . . 
K K 0.7017(3) 1.0236(3) 0.5016(2) 0.0312(5) Uani 1 2 a d . . . 
P1 P 0.6876(3) 0.3148(2) 0.8258(2) 0.0147(5) Uani 1 2 a d . . . 
P2 P 0.7956(3) 0.5409(3) 0.7003(2) 0.0142(4) Uani 1 2 a d . . . 
S1 S 0.6585(3) 0.4287(3) 1.0136(2) 0.0194(4) Uani 1 2 a d . . . 
S2 S 0.9127(3) 0.1262(3) 0.8259(2) 0.0180(4) Uani 1 2 a d . . . 
S3 S 0.4251(3) 0.2268(2) 0.7458(2) 0.0193(5) Uani 1 2 a d . . . 
S4 S 1.0521(3) 0.6229(3) 0.8071(2) 0.0190(4) Uani 1 2 a d . . . 
S5 S 0.5845(3) 0.7341(2) 0.7305(2) 0.0203(5) Uani 1 2 a d . . . 
S6 S 0.8230(4) 0.4592(3) 0.5134(2) 0.0240(5) Uani 1 2 a d . . . 
 
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 
Bi 0.02447(16) 0.01881(14) 0.02227(16) -0.00475(18) 0.00087(11) -0.00115(18) 
K 0.0315(13) 0.0354(12) 0.0264(12) 0.0003(9) -0.0014(10) -0.0025(9) 
P1 0.0172(10) 0.0139(12) 0.0130(10) 0.0005(7) -0.0014(8) -0.0003(7) 
P2 0.0150(10) 0.0139(9) 0.0135(10) 0.0004(8) -0.0017(8) -0.0008(8) 
S1 0.0260(11) 0.0197(11) 0.0126(10) -0.0015(8) 0.0015(9) -0.0044(9) 
S2 0.0187(11) 0.0153(9) 0.0199(11) -0.0003(9) -0.0028(9) 0.0016(8) 
S3 0.0179(10) 0.0203(12) 0.0195(11) -0.0004(8) -0.0033(8) -0.0050(7) 
S4 0.0145(10) 0.0231(10) 0.0194(11) -0.0024(9) -0.0010(8) -0.0013(8) 
S5 0.0212(10) 0.0185(13) 0.0210(10) -0.0008(8) -0.0048(8) 0.0043(8) 
S6 0.0290(13) 0.0306(12) 0.0125(11) -0.0020(9) 0.0017(9) -0.0036(10) 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
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 
Bi S4 2.706(2) . ? 
Bi S1 2.734(2) . ? 
Bi S5 2.804(2) . ? 
Bi S2 2.895(2) 2_757 ? 
Bi S2 3.138(2) 1_565 ? 
Bi S3 3.143(2) 2_657 ? 
K S6 3.191(3) 2_756 ? 
K S5 3.235(3) . ? 
K S5 3.314(3) 2_656 ? 
K S6 3.325(3) 1_565 ? 
K S3 3.374(3) 2_656 ? 
K S3 3.433(3) 1_565 ? 
K S6 3.504(3) 2_656 ? 
K S2 3.536(3) 1_565 ? 
K S4 3.592(3) 2_756 ? 
P1 S3 1.992(3) . ? 
P1 S2 2.042(3) . ? 
P1 S1 2.057(3) . ? 
P1 P2 2.219(3) . ? 
P2 S6 1.962(3) . ? 
P2 S5 2.030(3) . ? 
P2 S4 2.058(3) . ? 
S2 Bi 2.895(2) 2_747 ? 
S2 K 3.536(3) 1_545 ? 
S3 K 3.374(3) 2_646 ? 
S3 K 3.433(3) 1_545 ? 
S4 K 3.592(3) 2_746 ? 
S5 K 3.314(3) 2_646 ? 
S6 K 3.191(3) 2_746 ? 
S6 K 3.325(3) 1_545 ? 
S6 K 3.504(3) 2_646 ? 
 
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 
S4 Bi S1 84.70(6) . . ? 
S4 Bi S5 72.66(6) . . ? 
S1 Bi S5 81.65(6) . . ? 
S4 Bi S2 80.80(6) . 2_757 ? 
S1 Bi S2 77.36(6) . 2_757 ? 
S5 Bi S2 147.43(6) . 2_757 ? 
S4 Bi S2 81.97(6) . 1_565 ? 
S1 Bi S2 157.80(6) . 1_565 ? 
S5 Bi S2 77.48(6) . 1_565 ? 
S2 Bi S2 117.59(4) 2_757 1_565 ? 
S4 Bi S3 145.39(6) . 2_657 ? 
S1 Bi S3 68.14(6) . 2_657 ? 
S5 Bi S3 121.34(6) . 2_657 ? 
S2 Bi S3 72.84(6) 2_757 2_657 ? 
S2 Bi S3 130.11(5) 1_565 2_657 ? 
S6 K S5 101.29(8) 2_756 . ? 
S6 K S5 125.28(9) 2_756 2_656 ? 
S5 K S5 130.69(7) . 2_656 ? 
S6 K S6 84.80(7) 2_756 1_565 ? 
S5 K S6 133.02(9) . 1_565 ? 
S5 K S6 72.49(7) 2_656 1_565 ? 
S6 K S3 95.06(8) 2_756 2_656 ? 
S5 K S3 90.99(8) . 2_656 ? 
S5 K S3 71.48(6) 2_656 2_656 ? 
S6 K S3 135.29(9) 1_565 2_656 ? 
S6 K S3 130.58(9) 2_756 1_565 ? 
S5 K S3 69.47(6) . 1_565 ? 
S5 K S3 88.63(7) 2_656 1_565 ? 
S6 K S3 71.61(7) 1_565 1_565 ? 
S3 K S3 132.21(7) 2_656 1_565 ? 
S6 K S6 162.79(12) 2_756 2_656 ? 
S5 K S6 71.13(7) . 2_656 ? 
S5 K S6 59.61(6) 2_656 2_656 ? 
S6 K S6 111.80(9) 1_565 2_656 ? 
S3 K S6 70.17(7) 2_656 2_656 ? 
S3 K S6 62.35(6) 1_565 2_656 ? 
S6 K S2 73.57(7) 2_756 1_565 ? 
S5 K S2 66.63(6) . 1_565 ? 
S5 K S2 136.48(9) 2_656 1_565 ? 
S6 K S2 70.91(7) 1_565 1_565 ? 
S3 K S2 151.46(9) 2_656 1_565 ? 
S3 K S2 57.96(6) 1_565 1_565 ? 
S6 K S2 115.19(7) 2_656 1_565 ? 
S6 K S4 60.79(6) 2_756 2_756 ? 
S5 K S4 149.29(9) . 2_756 ? 
S5 K S4 65.13(6) 2_656 2_756 ? 
S6 K S4 73.42(7) 1_565 2_756 ? 
S3 K S4 67.93(6) 2_656 2_756 ? 
S3 K S4 141.25(9) 1_565 2_756 ? 
S6 K S4 118.17(7) 2_656 2_756 ? 
S2 K S4 123.50(8) 1_565 2_756 ? 
S3 P1 S2 113.72(12) . . ? 
S3 P1 S1 112.60(13) . . ? 
S2 P1 S1 111.87(13) . . ? 
S3 P1 P2 108.58(12) . . ? 
S2 P1 P2 105.42(12) . . ? 
S1 P1 P2 103.83(11) . . ? 
S6 P2 S5 116.39(14) . . ? 
S6 P2 S4 118.17(14) . . ? 
S5 P2 S4 106.02(12) . . ? 
S6 P2 P1 109.76(13) . . ? 
S5 P2 P1 102.22(12) . . ? 
S4 P2 P1 102.24(12) . . ? 
P1 S1 Bi 103.42(10) . . ? 
P1 S2 Bi 102.34(10) . 2_747 ? 
P1 S2 K 83.26(9) . 1_545 ? 
Bi S2 K 156.40(8) 2_747 1_545 ? 
P1 S3 K 105.40(10) . 2_646 ? 
P1 S3 K 86.76(10) . 1_545 ? 
P2 S4 Bi 85.34(9) . . ? 
P2 S4 K 83.94(9) . 2_746 ? 
Bi S4 K 160.09(9) . 2_746 ? 
P2 S5 Bi 83.28(9) . . ? 
P2 S5 K 100.36(10) . . ? 
Bi S5 K 115.10(8) . . ? 
P2 S5 K 86.87(10) . 2_646 ? 
Bi S5 K 155.81(8) . 2_646 ? 
P2 S6 K 97.08(11) . 2_746 ? 
P2 S6 K 107.56(12) . 1_545 ? 
P2 S6 K 82.65(10) . 2_646 ? 

 
_diffrn_measured_fraction_theta_max    0.927 
_diffrn_reflns_theta_full              28.00 
_diffrn_measured_fraction_theta_full   0.927 
_refine_diff_density_max    1.209 
_refine_diff_density_min   -1.435 
_refine_diff_density_rms    0.201 

