# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2007


data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Prof. Mercouri G. Kanatzidis'
_publ_contact_author_address     
;
Prof. Mercouri Kanatzidis
Department of Chemistry
Northwestern University
Evanston
IL
60208
UNITED STATES OF AMERICA
;

_publ_contact_author_email       m-kanatzidis@northwestern.edu

_publ_section_title              
;
Low Valent Phosphorus in the Molecular Anions [P5Se12]5-
and beta-[P6Se12]4-: Phase Change Behavior and Near Infrared
Second Harmonic Generation of Cs5P5Se12.
;
loop_
_publ_author_name
'In Chung.'
I.J.Jang
M.Kanatzidis

data_Cs5P5Se12
_database_code_depnum_ccdc_archive 'CCDC 650231'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Cesium selenophosphate
;
_chemical_name_common            'Cesium selenophosphate'
_chemical_melting_point          697
_chemical_formula_moiety         'P5 Se12, 5(Cs)'
_chemical_formula_sum            'Cs5 P5 Se12'
_chemical_formula_weight         1766.92

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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   P-4

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'

_cell_length_a                   13.9677(13)
_cell_length_b                   13.9677(13)
_cell_length_c                   7.5462(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1472.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    292(2)
_cell_measurement_reflns_used    6735
_cell_measurement_theta_min      2.70
_cell_measurement_theta_max      27.91

_exptl_crystal_description       'Irrgular block'
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.986
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1516
_exptl_absorpt_coefficient_mu    21.229
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
Because of the irregular shape, the crystal
dimension could not be measured
;

_diffrn_ambient_temperature      292(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  0.5
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12701
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.46
_diffrn_reflns_theta_max         28.25
_reflns_number_total             3424
_reflns_number_gt                3101
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 3.1d (Crystal Impact Gbr, 2006)'
_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.0473P)^2^+0.5352P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    none
_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   0.06(2)
_refine_ls_number_reflns         3424
_refine_ls_number_parameters     102
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0300
_refine_ls_wR_factor_ref         0.0855
_refine_ls_wR_factor_gt          0.0727
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_restrained_S_all      1.159
_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cs1 Cs 0.31243(5) 0.65471(4) 0.27117(9) 0.04649(17) Uani 1 1 d . . .
Cs2 Cs 0.32401(3) 0.03549(4) 0.25441(7) 0.03265(13) Uani 1 1 d . . .
Cs3 Cs 0.0000 0.0000 0.24769(11) 0.03908(18) Uani 1 2 d S . .
Se1 Se -0.03554(5) 0.31289(5) 0.25209(11) 0.02967(18) Uani 1 1 d . . .
Se2 Se 0.14920(6) 0.18562(6) 0.00900(11) 0.02966(18) Uani 1 1 d . . .
Se3 Se 0.14730(6) 0.17798(5) 0.49111(11) 0.02829(18) Uani 1 1 d . . .
Se4 Se 0.16509(6) 0.46436(6) 0.51329(11) 0.03188(19) Uani 1 1 d . . .
Se5 Se 0.12751(6) 0.47775(5) 0.04735(10) 0.02575(17) Uani 1 1 d . . .
Se6 Se 0.34663(6) 0.36982(8) 0.21322(13) 0.0441(3) Uani 1 1 d . . .
P1 P 0.11247(12) 0.25643(12) 0.2537(3) 0.0195(3) Uani 1 1 d . . .
P2 P 0.19941(12) 0.39238(12) 0.2678(3) 0.0217(4) Uani 1 1 d . . .
P3 P 0.0000 0.5000 0.2460(4) 0.0260(5) 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
Cs1 0.0590(4) 0.0411(3) 0.0393(3) -0.0075(3) 0.0016(3) -0.0134(3)
Cs2 0.0295(2) 0.0409(3) 0.0275(3) 0.0002(3) 0.0036(2) 0.0038(2)
Cs3 0.0412(4) 0.0476(4) 0.0285(4) 0.000 0.000 -0.0112(3)
Se1 0.0221(4) 0.0369(4) 0.0300(4) 0.0018(4) 0.0001(4) 0.0015(3)
Se2 0.0421(4) 0.0273(4) 0.0196(4) -0.0059(3) 0.0024(4) 0.0026(3)
Se3 0.0398(4) 0.0253(4) 0.0198(4) 0.0037(3) -0.0017(4) 0.0039(3)
Se4 0.0413(5) 0.0285(4) 0.0259(4) -0.0074(4) 0.0013(4) 0.0017(3)
Se5 0.0293(4) 0.0258(4) 0.0221(4) 0.0050(3) 0.0023(3) 0.0016(3)
Se6 0.0227(4) 0.0636(7) 0.0460(6) -0.0085(5) 0.0022(4) 0.0040(4)
P1 0.0243(8) 0.0179(7) 0.0162(8) -0.0006(8) 0.0008(8) 0.0024(6)
P2 0.0225(9) 0.0210(8) 0.0215(9) -0.0012(7) -0.0001(8) 0.0017(7)
P3 0.0237(12) 0.0355(14) 0.0189(12) 0.000 0.000 0.0047(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
Cs1 Se4 3.6722(11) 3_566 ?
Cs1 Se6 3.7422(13) 3_565 ?
Cs1 Se3 3.7938(11) 3_566 ?
Cs1 Se4 3.8265(11) . ?
Cs1 Se2 3.8870(11) 3_565 ?
Cs1 Se1 3.8966(10) 2_565 ?
Cs1 Se5 3.9539(10) . ?
Cs1 Se6 3.9727(14) 3_566 ?
Cs1 P2 3.9897(19) . ?
Cs1 Se6 4.0316(13) . ?
Cs1 P2 4.184(2) 3_566 ?
Cs1 Cs2 5.2790(10) 3_566 ?
Cs2 Se3 3.6392(10) . ?
Cs2 Se2 3.7133(10) . ?
Cs2 Se1 3.7273(12) 3_556 ?
Cs2 Se2 3.7872(11) 3 ?
Cs2 Se3 3.7904(10) 3_556 ?
Cs2 Se5 3.8084(9) 4_655 ?
Cs2 Se1 3.8253(12) 3 ?
Cs2 Se4 3.8425(10) 3_556 ?
Cs2 Se5 3.8704(10) 3 ?
Cs2 Se4 3.8842(10) 4_656 ?
Cs2 Cs3 4.5531(6) . ?
Cs2 Cs2 5.0153(10) 2_655 ?
Cs3 Se3 3.7131(9) 2 ?
Cs3 Se3 3.7131(9) . ?
Cs3 Cs3 3.7382(18) 3 ?
Cs3 Se3 3.7813(10) 3_556 ?
Cs3 Se3 3.7813(10) 4_556 ?
Cs3 Se2 3.7828(10) . ?
Cs3 Se2 3.7828(10) 2 ?
Cs3 Cs3 3.8080(18) 3_556 ?
Cs3 Se2 3.8493(9) 3 ?
Cs3 Se2 3.8493(9) 4 ?
Cs3 P1 3.9114(17) 2 ?
Cs3 P1 3.9114(17) . ?
Se1 P1 2.2127(18) . ?
Se1 P3 2.6606(8) . ?
Se1 Cs2 3.7273(12) 4_556 ?
Se1 Cs2 3.8253(12) 4 ?
Se1 Cs1 3.8965(10) 2_565 ?
Se2 P1 2.156(2) . ?
Se2 Cs2 3.7871(11) 4 ?
Se2 Cs3 3.8493(9) 3 ?
Se2 Cs1 3.8870(11) 4_655 ?
Se3 P1 2.156(2) . ?
Se3 Cs3 3.7813(10) 3_556 ?
Se3 Cs2 3.7904(10) 4_556 ?
Se3 Cs1 3.7937(11) 4_656 ?
Se4 P2 2.162(2) . ?
Se4 Cs1 3.6722(11) 4_656 ?
Se4 Cs2 3.8426(10) 4_556 ?
Se4 Cs2 3.8842(10) 3_566 ?
Se5 P2 2.280(2) . ?
Se5 P3 2.349(2) . ?
Se5 Cs2 3.8084(9) 3_565 ?
Se5 Cs2 3.8704(10) 4 ?
Se6 P2 2.1207(19) . ?
Se6 Cs1 3.7422(13) 4_655 ?
Se6 Cs1 3.9727(14) 4_656 ?
P1 P2 2.257(2) . ?
P2 Cs1 4.184(2) 4_656 ?
P3 Se5 2.349(2) 2_565 ?
P3 Se1 2.6605(8) 2_565 ?

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
Se4 Cs1 Se6 108.20(3) 3_566 3_565 ?
Se4 Cs1 Se3 64.97(2) 3_566 3_566 ?
Se6 Cs1 Se3 124.86(3) 3_565 3_566 ?
Se4 Cs1 Se4 125.14(2) 3_566 . ?
Se6 Cs1 Se4 125.32(2) 3_565 . ?
Se3 Cs1 Se4 90.83(2) 3_566 . ?
Se4 Cs1 Se2 91.22(2) 3_566 3_565 ?
Se6 Cs1 Se2 64.52(2) 3_565 3_565 ?
Se3 Cs1 Se2 61.18(2) 3_566 3_565 ?
Se4 Cs1 Se2 120.28(2) . 3_565 ?
Se4 Cs1 Se1 120.69(2) 3_566 2_565 ?
Se6 Cs1 Se1 100.20(3) 3_565 2_565 ?
Se3 Cs1 Se1 56.048(19) 3_566 2_565 ?
Se4 Cs1 Se1 64.18(2) . 2_565 ?
Se2 Cs1 Se1 56.35(2) 3_565 2_565 ?
Se4 Cs1 Se5 174.40(3) 3_566 . ?
Se6 Cs1 Se5 73.71(2) 3_565 . ?
Se3 Cs1 Se5 109.53(2) 3_566 . ?
Se4 Cs1 Se5 54.43(2) . . ?
Se2 Cs1 Se5 84.86(2) 3_565 . ?
Se1 Cs1 Se5 53.732(18) 2_565 . ?
Se4 Cs1 Se6 56.83(2) 3_566 3_566 ?
Se6 Cs1 Se6 155.98(4) 3_565 3_566 ?
Se3 Cs1 Se6 68.91(2) 3_566 3_566 ?
Se4 Cs1 Se6 68.75(2) . 3_566 ?
Se2 Cs1 Se6 128.90(3) 3_565 3_566 ?
Se1 Cs1 Se6 103.71(3) 2_565 3_566 ?
Se5 Cs1 Se6 123.18(2) . 3_566 ?
Se4 Cs1 P2 149.43(4) 3_566 . ?
Se6 Cs1 P2 94.24(3) 3_565 . ?
Se3 Cs1 P2 118.47(3) 3_566 . ?
Se4 Cs1 P2 32.02(3) . . ?
Se2 Cs1 P2 117.61(3) 3_565 . ?
Se1 Cs1 P2 73.36(3) 2_565 . ?
Se5 Cs1 P2 33.35(3) . . ?
Se6 Cs1 P2 94.69(3) 3_566 . ?
Se4 Cs1 Se6 131.00(3) 3_566 . ?
Se6 Cs1 Se6 82.17(2) 3_565 . ?
Se3 Cs1 Se6 146.04(3) 3_566 . ?
Se4 Cs1 Se6 55.232(19) . . ?
Se2 Cs1 Se6 133.67(3) 3_565 . ?
Se1 Cs1 Se6 103.19(2) 2_565 . ?
Se5 Cs1 Se6 54.131(19) . . ?
Se6 Cs1 Se6 94.45(3) 3_566 . ?
P2 Cs1 Se6 30.65(3) . . ?
Se4 Cs1 P2 31.08(3) 3_566 3_566 ?
Se6 Cs1 P2 139.25(3) 3_565 3_566 ?
Se3 Cs1 P2 51.97(3) 3_566 3_566 ?
Se4 Cs1 P2 94.87(3) . 3_566 ?
Se2 Cs1 P2 103.34(3) 3_565 3_566 ?
Se1 Cs1 P2 103.83(3) 2_565 3_566 ?
Se5 Cs1 P2 146.52(3) . 3_566 ?
Se6 Cs1 P2 30.00(3) 3_566 3_566 ?
P2 Cs1 P2 123.93(3) . 3_566 ?
Se6 Cs1 P2 122.63(3) . 3_566 ?
Se4 Cs1 Cs2 94.85(2) 3_566 3_566 ?
Se6 Cs1 Cs2 145.05(3) 3_565 3_566 ?
Se3 Cs1 Cs2 43.579(15) 3_566 3_566 ?
Se4 Cs1 Cs2 47.251(15) . 3_566 ?
Se2 Cs1 Cs2 89.73(2) 3_565 3_566 ?
Se1 Cs1 Cs2 44.865(16) 2_565 3_566 ?
Se5 Cs1 Cs2 81.155(17) . 3_566 ?
Se6 Cs1 Cs2 58.93(2) 3_566 3_566 ?
P2 Cs1 Cs2 76.47(3) . 3_566 ?
Se6 Cs1 Cs2 102.471(19) . 3_566 ?
P2 Cs1 Cs2 66.68(3) 3_566 3_566 ?
Se3 Cs2 Se2 59.33(2) . . ?
Se3 Cs2 Se1 58.75(2) . 3_556 ?
Se2 Cs2 Se1 118.09(2) . 3_556 ?
Se3 Cs2 Se2 106.50(2) . 3 ?
Se2 Cs2 Se2 77.72(2) . 3 ?
Se1 Cs2 Se2 120.22(2) 3_556 3 ?
Se3 Cs2 Se3 75.80(2) . 3_556 ?
Se2 Cs2 Se3 106.21(2) . 3_556 ?
Se1 Cs2 Se3 58.095(18) 3_556 3_556 ?
Se2 Cs2 Se3 62.12(2) 3 3_556 ?
Se3 Cs2 Se5 127.02(2) . 4_655 ?
Se2 Cs2 Se5 89.39(2) . 4_655 ?
Se1 Cs2 Se5 128.88(2) 3_556 4_655 ?
Se2 Cs2 Se5 106.69(2) 3 4_655 ?
Se3 Cs2 Se5 157.15(2) 3_556 4_655 ?
Se3 Cs2 Se1 117.57(2) . 3 ?
Se2 Cs2 Se1 58.326(19) . 3 ?
Se1 Cs2 Se1 175.29(3) 3_556 3 ?
Se2 Cs2 Se1 56.973(19) 3 3 ?
Se3 Cs2 Se1 118.98(2) 3_556 3 ?
Se5 Cs2 Se1 55.391(19) 4_655 3 ?
Se3 Cs2 Se4 121.39(3) . 3_556 ?
Se2 Cs2 Se4 167.09(2) . 3_556 ?
Se1 Cs2 Se4 64.251(19) 3_556 3_556 ?
Se2 Cs2 Se4 90.18(2) 3 3_556 ?
Se3 Cs2 Se4 63.404(19) 3_556 3_556 ?
Se5 Cs2 Se4 98.51(2) 4_655 3_556 ?
Se1 Cs2 Se4 118.47(2) 3 3_556 ?
Se3 Cs2 Se5 170.67(2) . 3 ?
Se2 Cs2 Se5 113.80(2) . 3 ?
Se1 Cs2 Se5 127.66(2) 3_556 3 ?
Se2 Cs2 Se5 64.766(19) 3 3 ?
Se3 Cs2 Se5 101.56(2) 3_556 3 ?
Se5 Cs2 Se5 56.18(2) 4_655 3 ?
Se1 Cs2 Se5 55.581(18) 3 3 ?
Se4 Cs2 Se5 63.67(2) 3_556 3 ?
Se3 Cs2 Se4 92.28(2) . 4_656 ?
Se2 Cs2 Se4 117.54(2) . 4_656 ?
Se1 Cs2 Se4 65.21(2) 3_556 4_656 ?
Se2 Cs2 Se4 160.52(2) 3 4_656 ?
Se3 Cs2 Se4 119.66(2) 3_556 4_656 ?
Se5 Cs2 Se4 63.85(2) 4_655 4_656 ?
Se1 Cs2 Se4 118.80(2) 3 4_656 ?
Se4 Cs2 Se4 75.26(2) 3_556 4_656 ?
Se5 Cs2 Se4 96.74(2) 3 4_656 ?
Se3 Cs2 Cs3 52.472(15) . . ?
Se2 Cs2 Cs3 53.297(16) . . ?
Se1 Cs2 Cs3 88.267(19) 3_556 . ?
Se2 Cs2 Cs3 54.030(15) 3 . ?
Se3 Cs2 Cs3 52.943(15) 3_556 . ?
Se5 Cs2 Cs3 138.83(2) 4_655 . ?
Se1 Cs2 Cs3 87.050(19) 3 . ?
Se4 Cs2 Cs3 115.646(18) 3_556 . ?
Se5 Cs2 Cs3 118.743(19) 3 . ?
Se4 Cs2 Cs3 144.31(2) 4_656 . ?
Se3 Cs2 Cs2 140.622(19) . 2_655 ?
Se2 Cs2 Cs2 139.132(19) . 2_655 ?
Se1 Cs2 Cs2 92.342(14) 3_556 2_655 ?
Se2 Cs2 Cs2 111.448(18) 3 2_655 ?
Se3 Cs2 Cs2 113.226(18) 3_556 2_655 ?
Se5 Cs2 Cs2 49.760(15) 4_655 2_655 ?
Se1 Cs2 Cs2 92.282(14) 3 2_655 ?
Se4 Cs2 Cs2 49.890(14) 3_556 2_655 ?
Se5 Cs2 Cs2 48.687(14) 3 2_655 ?
Se4 Cs2 Cs2 49.166(15) 4_656 2_655 ?
Cs3 Cs2 Cs2 162.335(18) . 2_655 ?
Se3 Cs3 Se3 120.70(3) 2 . ?
Se3 Cs3 Cs3 119.651(17) 2 3 ?
Se3 Cs3 Cs3 119.651(17) . 3 ?
Se3 Cs3 Se3 75.055(12) 2 3_556 ?
Se3 Cs3 Se3 75.055(12) . 3_556 ?
Cs3 Cs3 Se3 121.419(18) 3 3_556 ?
Se3 Cs3 Se3 75.055(12) 2 4_556 ?
Se3 Cs3 Se3 75.056(12) . 4_556 ?
Cs3 Cs3 Se3 121.418(18) 3 4_556 ?
Se3 Cs3 Se3 117.16(4) 3_556 4_556 ?
Se3 Cs3 Se2 178.59(3) 2 . ?
Se3 Cs3 Se2 58.091(19) . . ?
Cs3 Cs3 Se2 61.566(18) 3 . ?
Se3 Cs3 Se2 105.01(2) 3_556 . ?
Se3 Cs3 Se2 103.738(19) 4_556 . ?
Se3 Cs3 Se2 58.091(19) 2 2 ?
Se3 Cs3 Se2 178.59(3) . 2 ?
Cs3 Cs3 Se2 61.566(18) 3 2 ?
Se3 Cs3 Se2 103.738(19) 3_556 2 ?
Se3 Cs3 Se2 105.01(2) 4_556 2 ?
Se2 Cs3 Se2 123.13(4) . 2 ?
Se3 Cs3 Cs3 60.349(17) 2 3_556 ?
Se3 Cs3 Cs3 60.349(17) . 3_556 ?
Cs3 Cs3 Cs3 180.0 3 3_556 ?
Se3 Cs3 Cs3 58.582(18) 3_556 3_556 ?
Se3 Cs3 Cs3 58.581(18) 4_556 3_556 ?
Se2 Cs3 Cs3 118.435(18) . 3_556 ?
Se2 Cs3 Cs3 118.434(18) 2 3_556 ?
Se3 Cs3 Se2 105.051(19) 2 3 ?
Se3 Cs3 Se2 103.78(2) . 3 ?
Cs3 Cs3 Se2 59.788(16) 3 3 ?
Se3 Cs3 Se2 61.636(19) 3_556 3 ?
Se3 Cs3 Se2 178.60(3) 4_556 3 ?
Se2 Cs3 Se2 76.137(12) . 3 ?
Se2 Cs3 Se2 76.137(12) 2 3 ?
Cs3 Cs3 Se2 120.212(16) 3_556 3 ?
Se3 Cs3 Se2 103.78(2) 2 4 ?
Se3 Cs3 Se2 105.051(19) . 4 ?
Cs3 Cs3 Se2 59.788(16) 3 4 ?
Se3 Cs3 Se2 178.60(3) 3_556 4 ?
Se3 Cs3 Se2 61.636(19) 4_556 4 ?
Se2 Cs3 Se2 76.137(12) . 4 ?
Se2 Cs3 Se2 76.137(12) 2 4 ?
Cs3 Cs3 Se2 120.212(16) 3_556 4 ?
Se2 Cs3 Se2 119.58(3) 3 4 ?
Se3 Cs3 P1 32.72(3) 2 2 ?
Se3 Cs3 P1 146.09(4) . 2 ?
Cs3 Cs3 P1 90.66(3) 3 2 ?
Se3 Cs3 P1 76.10(3) 3_556 2 ?
Se3 Cs3 P1 103.19(3) 4_556 2 ?
Se2 Cs3 P1 148.69(4) . 2 ?
Se2 Cs3 P1 32.50(3) 2 2 ?
Cs3 Cs3 P1 89.34(3) 3_556 2 ?
Se2 Cs3 P1 77.32(3) 3 2 ?
Se2 Cs3 P1 103.36(3) 4 2 ?
Se3 Cs3 P1 146.09(4) 2 . ?
Se3 Cs3 P1 32.72(3) . . ?
Cs3 Cs3 P1 90.66(3) 3 . ?
Se3 Cs3 P1 103.19(3) 3_556 . ?
Se3 Cs3 P1 76.10(3) 4_556 . ?
Se2 Cs3 P1 32.50(3) . . ?
Se2 Cs3 P1 148.69(4) 2 . ?
Cs3 Cs3 P1 89.34(3) 3_556 . ?
Se2 Cs3 P1 103.36(3) 3 . ?
Se2 Cs3 P1 77.32(3) 4 . ?
P1 Cs3 P1 178.68(6) 2 . ?
P1 Se1 P3 100.13(5) . . ?
P1 Se1 Cs2 90.54(6) . 4_556 ?
P3 Se1 Cs2 88.64(7) . 4_556 ?
P1 Se1 Cs2 91.13(6) . 4 ?
P3 Se1 Cs2 86.72(7) . 4 ?
Cs2 Se1 Cs2 175.29(3) 4_556 4 ?
P1 Se1 Cs1 165.59(5) . 2_565 ?
P3 Se1 Cs1 94.11(2) . 2_565 ?
Cs2 Se1 Cs1 87.62(2) 4_556 2_565 ?
Cs2 Se1 Cs1 91.85(2) 4 2_565 ?
P1 Se2 Cs2 89.34(5) . . ?
P1 Se2 Cs3 77.03(5) . . ?
Cs2 Se2 Cs3 74.796(19) . . ?
P1 Se2 Cs2 93.05(5) . 4 ?
Cs2 Se2 Cs2 176.29(3) . 4 ?
Cs3 Se2 Cs2 102.97(2) . 4 ?
P1 Se2 Cs3 127.66(6) . 3 ?
Cs2 Se2 Cs3 103.10(2) . 3 ?
Cs3 Se2 Cs3 58.65(3) . 3 ?
Cs2 Se2 Cs3 73.196(17) 4 3 ?
P1 Se2 Cs1 115.11(5) . 4_655 ?
Cs2 Se2 Cs1 93.74(2) . 4_655 ?
Cs3 Se2 Cs1 163.64(2) . 4_655 ?
Cs2 Se2 Cs1 87.82(2) 4 4_655 ?
Cs3 Se2 Cs1 114.50(2) 3 4_655 ?
P1 Se3 Cs2 91.32(5) . . ?
P1 Se3 Cs3 78.70(5) . . ?
Cs2 Se3 Cs3 76.518(18) . . ?
P1 Se3 Cs3 130.14(5) . 3_556 ?
Cs2 Se3 Cs3 105.39(2) . 3_556 ?
Cs3 Se3 Cs3 61.07(3) . 3_556 ?
P1 Se3 Cs2 89.75(5) . 4_556 ?
Cs2 Se3 Cs2 178.93(3) . 4_556 ?
Cs3 Se3 Cs2 103.75(2) . 4_556 ?
Cs3 Se3 Cs2 73.930(18) 3_556 4_556 ?
P1 Se3 Cs1 107.81(5) . 4_656 ?
Cs2 Se3 Cs1 90.48(2) . 4_656 ?
Cs3 Se3 Cs1 165.75(3) . 4_656 ?
Cs3 Se3 Cs1 118.40(3) 3_556 4_656 ?
Cs2 Se3 Cs1 89.15(2) 4_556 4_656 ?
P2 Se4 Cs1 87.64(5) . 4_656 ?
P2 Se4 Cs1 78.15(5) . . ?
Cs1 Se4 Cs1 104.15(3) 4_656 . ?
P2 Se4 Cs2 108.38(5) . 4_556 ?
Cs1 Se4 Cs2 90.16(2) 4_656 4_556 ?
Cs1 Se4 Cs2 164.67(3) . 4_556 ?
P2 Se4 Cs2 147.58(6) . 3_566 ?
Cs1 Se4 Cs2 124.01(3) 4_656 3_566 ?
Cs1 Se4 Cs2 86.41(2) . 3_566 ?
Cs2 Se4 Cs2 80.94(2) 4_556 3_566 ?
P2 Se5 P3 86.42(7) . . ?
P2 Se5 Cs2 164.84(6) . 3_565 ?
P3 Se5 Cs2 91.69(5) . 3_565 ?
P2 Se5 Cs2 113.47(5) . 4 ?
P3 Se5 Cs2 90.16(5) . 4 ?
Cs2 Se5 Cs2 81.55(2) 3_565 4 ?
P2 Se5 Cs1 74.19(5) . . ?
P3 Se5 Cs1 98.05(5) . . ?
Cs2 Se5 Cs1 91.22(2) 3_565 . ?
Cs2 Se5 Cs1 169.24(2) 4 . ?
P2 Se6 Cs1 102.51(6) . 4_655 ?
P2 Se6 Cs1 80.52(6) . 4_656 ?
Cs1 Se6 Cs1 155.98(4) 4_655 4_656 ?
P2 Se6 Cs1 73.58(5) . . ?
Cs1 Se6 Cs1 108.47(3) 4_655 . ?
Cs1 Se6 Cs1 95.30(3) 4_656 . ?
Se3 P1 Se2 115.14(8) . . ?
Se3 P1 Se1 113.35(9) . . ?
Se2 P1 Se1 112.41(9) . . ?
Se3 P1 P2 105.49(9) . . ?
Se2 P1 P2 107.36(9) . . ?
Se1 P1 P2 101.72(8) . . ?
Se3 P1 Cs3 68.58(5) . . ?
Se2 P1 Cs3 70.47(5) . . ?
Se1 P1 Cs3 87.19(5) . . ?
P2 P1 Cs3 170.86(8) . . ?
Se6 P2 Se4 116.78(9) . . ?
Se6 P2 P1 112.80(9) . . ?
Se4 P2 P1 108.22(9) . . ?
Se6 P2 Se5 111.29(9) . . ?
Se4 P2 Se5 106.52(8) . . ?
P1 P2 Se5 99.70(9) . . ?
Se6 P2 Cs1 75.76(6) . . ?
Se4 P2 Cs1 69.83(5) . . ?
P1 P2 Cs1 170.42(8) . . ?
Se5 P2 Cs1 72.46(5) . . ?
Se6 P2 Cs1 69.49(6) . 4_656 ?
Se4 P2 Cs1 61.28(5) . 4_656 ?
P1 P2 Cs1 94.40(7) . 4_656 ?
Se5 P2 Cs1 163.93(7) . 4_656 ?
Cs1 P2 Cs1 92.70(4) . 4_656 ?
Se5 P3 Se5 100.67(12) 2_565 . ?
Se5 P3 Se1 91.29(5) 2_565 2_565 ?
Se5 P3 Se1 89.97(5) . 2_565 ?
Se5 P3 Se1 89.97(5) 2_565 . ?
Se5 P3 Se1 91.29(5) . . ?
Se1 P3 Se1 178.02(13) 2_565 . ?

_diffrn_measured_fraction_theta_max 0.967
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.907
_refine_diff_density_min         -2.277
_refine_diff_density_rms         0.407
#=============================================END

data_Cs4P6Se12
_database_code_depnum_ccdc_archive 'CCDC 650232'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          697
_chemical_formula_moiety         'P6 Se12, 4(Cs)'
_chemical_formula_sum            'Cs4 P6 Se12'
_chemical_formula_weight         1664.98

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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.8363(11)
_cell_length_b                   10.5437(8)
_cell_length_c                   12.2731(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.661(8)
_cell_angle_gamma                90.00
_cell_volume                     1386.3(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      3.03
_cell_measurement_theta_max      29.99

_exptl_crystal_description       Block
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.065
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.031
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.989
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1436
_exptl_absorpt_coefficient_mu    21.309
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.3037
_exptl_absorpt_correction_T_max  0.6069
_exptl_absorpt_process_details   'face indexed'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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  'STOE IPDS II'
_diffrn_measurement_method       'incremental omega oscillation 1.0\%'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count 1.0
_diffrn_standards_interval_time  9
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8319
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         29.99
_reflns_number_total             3961
_reflns_number_gt                3810
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'X-Area Version 1.39 (STOE & Cie Gmbh, 2006)'
_computing_cell_refinement       'X-Area Version 1.39 (STOE & Cie Gmbh, 2006)'
_computing_data_reduction        'X-Area Version 1.39 (STOE & Cie Gmbh, 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 3.1d'
_computing_publication_material  ?

_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^)+(0.0764P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3961
_refine_ls_number_parameters     101
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0429
_refine_ls_wR_factor_ref         0.1403
_refine_ls_wR_factor_gt          0.1036
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cs1 Cs 0.49052(7) -0.00092(7) 0.24641(5) 0.01346(17) Uani 1 1 d . . .
Cs2 Cs 0.52386(7) 0.49950(8) 0.17741(5) 0.01543(19) Uani 1 1 d . . .
Se5 Se 0.23845(13) 0.23588(14) 0.27591(9) 0.0162(3) Uani 1 1 d . . .
Se2 Se 0.25519(12) 0.25395(13) 0.72496(9) 0.0135(3) Uani 1 1 d . . .
Se3 Se -0.00157(12) 0.28756(12) 0.49926(10) 0.0120(2) Uani 1 1 d . . .
Se4 Se 0.28711(12) -0.01166(13) 0.49034(9) 0.0136(2) Uani 1 1 d . . .
Se6 Se 0.49141(12) 0.25532(13) 0.50477(10) 0.0135(2) Uani 1 1 d . . .
Se1 Se 0.25941(11) 0.49992(14) 0.51441(9) 0.0138(2) Uani 1 1 d . . .
P1 P 0.1948(3) 0.2999(3) 0.5557(2) 0.0106(6) Uani 1 1 d . . .
P2 P 0.2954(3) 0.1819(3) 0.4429(2) 0.0116(6) Uani 1 1 d . . .
P3 P 0.4334(3) 0.4502(3) 0.4359(2) 0.0139(6) Uani 1 1 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
Cs1 0.0122(3) 0.0157(4) 0.0124(3) -0.0003(3) 0.0017(2) -0.0009(3)
Cs2 0.0157(4) 0.0176(4) 0.0127(3) -0.0001(3) 0.0013(2) 0.0022(3)
Se5 0.0171(6) 0.0206(7) 0.0108(5) 0.0011(4) 0.0020(4) 0.0059(6)
Se2 0.0150(5) 0.0157(6) 0.0089(5) -0.0001(4) -0.0008(4) 0.0011(5)
Se3 0.0097(5) 0.0127(5) 0.0133(4) -0.0002(4) 0.0013(4) 0.0013(5)
Se4 0.0146(5) 0.0111(6) 0.0143(5) 0.0005(4) 0.0003(4) 0.0025(5)
Se6 0.0089(5) 0.0155(6) 0.0160(5) 0.0020(5) 0.0018(4) 0.0018(5)
Se1 0.0096(5) 0.0133(6) 0.0192(5) 0.0011(5) 0.0040(4) 0.0011(5)
P1 0.0110(13) 0.0128(15) 0.0082(12) -0.0017(10) 0.0021(10) 0.0016(12)
P2 0.0095(14) 0.0158(16) 0.0092(12) 0.0001(10) 0.0004(10) 0.0024(12)
P3 0.0119(14) 0.0163(16) 0.0136(13) 0.0037(11) 0.0025(10) 0.0017(13)

_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
Cs1 Se5 3.7051(17) 2_545 ?
Cs1 Se4 3.7308(18) 3_656 ?
Cs1 Se5 3.7581(16) . ?
Cs1 Se3 3.7667(15) 2_545 ?
Cs1 Se3 3.7878(15) 4_665 ?
Cs1 Se2 3.8135(16) 3_656 ?
Cs1 Se1 3.8692(19) 2_545 ?
Cs1 Se2 3.9119(16) 4_665 ?
Cs1 P2 3.942(3) . ?
Cs1 Se4 3.9776(17) . ?
Cs1 Se6 4.0471(16) 3_656 ?
Cs1 P1 4.054(3) 4_665 ?
Cs2 P3 3.497(3) . ?
Cs2 Se2 3.6141(17) 3_666 ?
Cs2 Se2 3.6504(16) 4_665 ?
Cs2 Se4 3.6767(18) 2 ?
Cs2 Se3 3.7184(16) 2 ?
Cs2 Se3 3.7196(16) 4_665 ?
Cs2 Se5 3.8872(17) 2 ?
Cs2 Se4 3.9240(17) 4_665 ?
Cs2 P2 4.039(4) 2 ?
Cs2 P1 4.057(3) 4_665 ?
Cs2 Se1 4.1408(19) 3_666 ?
Cs2 Cs2 4.3072(16) 3_665 ?
Se5 P2 2.127(2) . ?
Se5 Cs1 3.7052(16) 2 ?
Se5 Cs2 3.8872(17) 2_545 ?
Se2 P1 2.137(2) . ?
Se2 Cs2 3.6141(17) 3_666 ?
Se2 Cs2 3.6504(16) 4_566 ?
Se2 Cs1 3.8135(16) 3_656 ?
Se2 Cs1 3.9119(16) 4_566 ?
Se3 P1 2.140(2) . ?
Se3 Cs2 3.7183(16) 2_545 ?
Se3 Cs2 3.7197(16) 4_566 ?
Se3 Cs1 3.7667(15) 2 ?
Se3 Cs1 3.7878(15) 4_566 ?
Se4 P2 2.128(2) . ?
Se4 Cs2 3.6767(18) 2_545 ?
Se4 Cs1 3.7307(18) 3_656 ?
Se4 Cs2 3.9239(17) 4_566 ?
Se6 P3 2.274(2) . ?
Se6 P2 2.281(2) . ?
Se6 Cs1 4.0471(16) 3_656 ?
Se1 P1 2.303(2) . ?
Se1 P3 2.303(2) . ?
Se1 Cs1 3.8693(19) 2 ?
Se1 Cs2 4.1408(19) 3_666 ?
P1 P2 2.260(2) . ?
P1 Cs1 4.054(3) 4_566 ?
P1 Cs2 4.057(3) 4_566 ?
P2 Cs2 4.039(4) 2_545 ?
P3 P3 2.232(2) 3_666 ?

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
Se5 Cs1 Se4 115.38(4) 2_545 3_656 ?
Se5 Cs1 Se5 90.94(2) 2_545 . ?
Se4 Cs1 Se5 106.08(4) 3_656 . ?
Se5 Cs1 Se3 66.36(3) 2_545 2_545 ?
Se4 Cs1 Se3 128.32(4) 3_656 2_545 ?
Se5 Cs1 Se3 125.57(4) . 2_545 ?
Se5 Cs1 Se3 118.77(4) 2_545 4_665 ?
Se4 Cs1 Se3 125.65(4) 3_656 4_665 ?
Se5 Cs1 Se3 77.70(4) . 4_665 ?
Se3 Cs1 Se3 72.74(4) 2_545 4_665 ?
Se5 Cs1 Se2 87.10(4) 2_545 3_656 ?
Se4 Cs1 Se2 65.26(3) 3_656 3_656 ?
Se5 Cs1 Se2 168.96(3) . 3_656 ?
Se3 Cs1 Se2 63.25(4) 2_545 3_656 ?
Se3 Cs1 Se2 112.71(4) 4_665 3_656 ?
Se5 Cs1 Se1 64.09(3) 2_545 2_545 ?
Se4 Cs1 Se1 175.38(3) 3_656 2_545 ?
Se5 Cs1 Se1 69.50(3) . 2_545 ?
Se3 Cs1 Se1 56.07(3) 2_545 2_545 ?
Se3 Cs1 Se1 55.50(3) 4_665 2_545 ?
Se2 Cs1 Se1 118.94(4) 3_656 2_545 ?
Se5 Cs1 Se2 169.48(3) 2_545 4_665 ?
Se4 Cs1 Se2 69.52(3) 3_656 4_665 ?
Se5 Cs1 Se2 96.61(4) . 4_665 ?
Se3 Cs1 Se2 103.19(4) 2_545 4_665 ?
Se3 Cs1 Se2 56.33(4) 4_665 4_665 ?
Se2 Cs1 Se2 86.84(2) 3_656 4_665 ?
Se1 Cs1 Se2 111.82(3) 2_545 4_665 ?
Se5 Cs1 P2 89.80(6) 2_545 . ?
Se4 Cs1 P2 77.80(5) 3_656 . ?
Se5 Cs1 P2 31.96(5) . . ?
Se3 Cs1 P2 149.76(6) 2_545 . ?
Se3 Cs1 P2 106.17(6) 4_665 . ?
Se2 Cs1 P2 137.09(5) 3_656 . ?
Se1 Cs1 P2 97.58(5) 2_545 . ?
Se2 Cs1 P2 100.48(6) 4_665 . ?
Se5 Cs1 Se4 66.01(3) 2_545 . ?
Se4 Cs1 Se4 73.02(4) 3_656 . ?
Se5 Cs1 Se4 56.85(3) . . ?
Se3 Cs1 Se4 132.35(4) 2_545 . ?
Se3 Cs1 Se4 134.55(3) 4_665 . ?
Se2 Cs1 Se4 112.67(3) 3_656 . ?
Se1 Cs1 Se4 102.98(3) 2_545 . ?
Se2 Cs1 Se4 124.37(3) 4_665 . ?
P2 Cs1 Se4 31.17(5) . . ?
Se5 Cs1 Se6 61.00(4) 2_545 3_656 ?
Se4 Cs1 Se6 54.45(3) 3_656 3_656 ?
Se5 Cs1 Se6 108.72(4) . 3_656 ?
Se3 Cs1 Se6 101.99(4) 2_545 3_656 ?
Se3 Cs1 Se6 173.49(3) 4_665 3_656 ?
Se2 Cs1 Se6 60.96(3) 3_656 3_656 ?
Se1 Cs1 Se6 125.04(4) 2_545 3_656 ?
Se2 Cs1 Se6 122.64(4) 4_665 3_656 ?
P2 Cs1 Se6 80.32(5) . 3_656 ?
Se4 Cs1 Se6 51.87(3) . 3_656 ?
Se5 Cs1 P1 140.07(5) 2_545 4_665 ?
Se4 Cs1 P1 98.27(5) 3_656 4_665 ?
Se5 Cs1 P1 100.15(6) . 4_665 ?
Se3 Cs1 P1 76.20(5) 2_545 4_665 ?
Se3 Cs1 P1 31.45(5) 4_665 4_665 ?
Se2 Cs1 P1 88.24(6) 3_656 4_665 ?
Se1 Cs1 P1 84.04(5) 2_545 4_665 ?
Se2 Cs1 P1 31.06(5) 4_665 4_665 ?
P2 Cs1 P1 119.17(7) . 4_665 ?
Se4 Cs1 P1 149.56(6) . 4_665 ?
Se6 Cs1 P1 144.46(6) 3_656 4_665 ?
P3 Cs2 Se2 93.93(7) . 3_666 ?
P3 Cs2 Se2 91.48(6) . 4_665 ?
Se2 Cs2 Se2 93.95(3) 3_666 4_665 ?
P3 Cs2 Se4 98.31(6) . 2 ?
Se2 Cs2 Se4 135.58(4) 3_666 2 ?
Se2 Cs2 Se4 127.99(4) 4_665 2 ?
P3 Cs2 Se3 130.38(7) . 2 ?
Se2 Cs2 Se3 65.64(4) 3_666 2 ?
Se2 Cs2 Se3 132.37(4) 4_665 2 ?
Se4 Cs2 Se3 74.10(4) 2 2 ?
P3 Cs2 Se3 113.96(7) . 4_665 ?
Se2 Cs2 Se3 140.08(4) 3_666 4_665 ?
Se2 Cs2 Se3 59.11(4) 4_665 4_665 ?
Se4 Cs2 Se3 70.38(3) 2 4_665 ?
Se3 Cs2 Se3 109.23(3) 2 4_665 ?
P3 Cs2 Se5 69.54(6) . 2 ?
Se2 Cs2 Se5 87.28(4) 3_666 2 ?
Se2 Cs2 Se5 161.01(3) 4_665 2 ?
Se4 Cs2 Se5 58.28(3) 2 2 ?
Se3 Cs2 Se5 65.01(3) 2 2 ?
Se3 Cs2 Se5 128.12(4) 4_665 2 ?
P3 Cs2 Se4 149.70(6) . 4_665 ?
Se2 Cs2 Se4 70.54(3) 3_666 4_665 ?
Se2 Cs2 Se4 64.87(3) 4_665 4_665 ?
Se4 Cs2 Se4 111.05(3) 2 4_665 ?
Se3 Cs2 Se4 67.74(3) 2 4_665 ?
Se3 Cs2 Se4 71.26(3) 4_665 4_665 ?
Se5 Cs2 Se4 132.65(4) 2 4_665 ?
P3 Cs2 P2 93.47(7) . 2 ?
Se2 Cs2 P2 105.49(6) 3_666 2 ?
Se2 Cs2 P2 159.54(6) 4_665 2 ?
Se4 Cs2 P2 31.57(5) 2 2 ?
Se3 Cs2 P2 54.62(5) 2 2 ?
Se3 Cs2 P2 100.89(6) 4_665 2 ?
Se5 Cs2 P2 31.06(5) 2 2 ?
Se4 Cs2 P2 115.39(5) 4_665 2 ?
P3 Cs2 P1 115.10(7) . 4_665 ?
Se2 Cs2 P1 111.42(6) 3_666 4_665 ?
Se2 Cs2 P1 31.64(5) 4_665 4_665 ?
Se4 Cs2 P1 101.52(5) 2 4_665 ?
Se3 Cs2 P1 114.46(5) 2 4_665 ?
Se3 Cs2 P1 31.57(5) 4_665 4_665 ?
Se5 Cs2 P1 159.66(6) 2 4_665 ?
Se4 Cs2 P1 52.95(5) 4_665 4_665 ?
P2 Cs2 P1 130.49(7) 2 4_665 ?
P3 Cs2 Se1 50.93(6) . 3_666 ?
Se2 Cs2 Se1 55.93(3) 3_666 3_666 ?
Se2 Cs2 Se1 64.76(3) 4_665 3_666 ?
Se4 Cs2 Se1 149.03(3) 2 3_666 ?
Se3 Cs2 Se1 120.63(4) 2 3_666 ?
Se3 Cs2 Se1 121.31(4) 4_665 3_666 ?
Se5 Cs2 Se1 101.02(3) 2 3_666 ?
Se4 Cs2 Se1 99.91(3) 4_665 3_666 ?
P2 Cs2 Se1 132.07(5) 2 3_666 ?
P1 Cs2 Se1 96.31(5) 4_665 3_666 ?
P3 Cs2 Cs2 155.50(7) . 3_665 ?
Se2 Cs2 Cs2 107.83(4) 3_666 3_665 ?
Se2 Cs2 Cs2 97.96(4) 4_665 3_665 ?
Se4 Cs2 Cs2 58.24(3) 2 3_665 ?
Se3 Cs2 Cs2 54.63(3) 2 3_665 ?
Se3 Cs2 Cs2 54.60(3) 4_665 3_665 ?
Se5 Cs2 Cs2 99.69(4) 2 3_665 ?
Se4 Cs2 Cs2 52.81(3) 4_665 3_665 ?
P2 Cs2 Cs2 70.33(5) 2 3_665 ?
P1 Cs2 Cs2 67.77(5) 4_665 3_665 ?
Se1 Cs2 Cs2 152.71(3) 3_666 3_665 ?
P2 Se5 Cs1 111.44(10) . 2 ?
P2 Se5 Cs1 78.78(10) . . ?
Cs1 Se5 Cs1 168.19(4) 2 . ?
P2 Se5 Cs2 78.40(10) . 2_545 ?
Cs1 Se5 Cs2 89.70(4) 2 2_545 ?
Cs1 Se5 Cs2 98.42(4) . 2_545 ?
P1 Se2 Cs2 104.47(10) . 3_666 ?
P1 Se2 Cs2 84.72(10) . 4_566 ?
Cs2 Se2 Cs2 169.82(3) 3_666 4_566 ?
P1 Se2 Cs1 111.05(10) . 3_656 ?
Cs2 Se2 Cs1 92.25(4) 3_666 3_656 ?
Cs2 Se2 Cs1 88.39(4) 4_566 3_656 ?
P1 Se2 Cs1 78.13(9) . 4_566 ?
Cs2 Se2 Cs1 87.41(4) 3_666 4_566 ?
Cs2 Se2 Cs1 90.30(4) 4_566 4_566 ?
Cs1 Se2 Cs1 170.54(3) 3_656 4_566 ?
P1 Se3 Cs2 102.26(10) . 2_545 ?
P1 Se3 Cs2 82.93(10) . 4_566 ?
Cs2 Se3 Cs2 70.77(3) 2_545 4_566 ?
P1 Se3 Cs1 94.21(9) . 2 ?
Cs2 Se3 Cs1 91.37(4) 2_545 2 ?
Cs2 Se3 Cs1 160.71(4) 4_566 2 ?
P1 Se3 Cs1 81.14(9) . 4_566 ?
Cs2 Se3 Cs1 160.87(4) 2_545 4_566 ?
Cs2 Se3 Cs1 91.21(4) 4_566 4_566 ?
Cs1 Se3 Cs1 107.25(4) 2 4_566 ?
P2 Se4 Cs2 83.63(10) . 2_545 ?
P2 Se4 Cs1 98.88(10) . 3_656 ?
Cs2 Se4 Cs1 154.39(4) 2_545 3_656 ?
P2 Se4 Cs2 101.14(9) . 4_566 ?
Cs2 Se4 Cs2 68.95(3) 2_545 4_566 ?
Cs1 Se4 Cs2 85.63(3) 3_656 4_566 ?
P2 Se4 Cs1 73.48(8) . . ?
Cs2 Se4 Cs1 98.20(4) 2_545 . ?
Cs1 Se4 Cs1 106.98(4) 3_656 . ?
Cs2 Se4 Cs1 166.79(4) 4_566 . ?
P3 Se6 P2 89.50(8) . . ?
P3 Se6 Cs1 149.16(9) . 3_656 ?
P2 Se6 Cs1 87.88(9) . 3_656 ?
P3 Se6 Cs1 109.52(9) . . ?
P2 Se6 Cs1 68.35(8) . . ?
Cs1 Se6 Cs1 97.98(4) 3_656 . ?
P1 Se1 P3 100.29(8) . . ?
P1 Se1 Cs1 88.96(9) . 2 ?
P3 Se1 Cs1 99.68(9) . 2 ?
P1 Se1 Cs2 87.12(8) . 3_666 ?
P3 Se1 Cs2 89.73(9) . 3_666 ?
Cs1 Se1 Cs2 170.32(3) 2 3_666 ?
Se2 P1 Se3 116.42(8) . . ?
Se2 P1 P2 111.43(8) . . ?
Se3 P1 P2 108.43(8) . . ?
Se2 P1 Se1 111.26(9) . . ?
Se3 P1 Se1 107.74(9) . . ?
P2 P1 Se1 100.29(8) . . ?
Se2 P1 Cs1 70.80(8) . 4_566 ?
Se3 P1 Cs1 67.41(8) . 4_566 ?
P2 P1 Cs1 175.80(15) . 4_566 ?
Se1 P1 Cs1 81.87(9) . 4_566 ?
Se2 P1 Cs2 63.64(9) . 4_566 ?
Se3 P1 Cs2 65.49(9) . 4_566 ?
P2 P1 Cs2 94.96(13) . 4_566 ?
Se1 P1 Cs2 164.68(12) . 4_566 ?
Cs1 P1 Cs2 82.82(6) 4_566 4_566 ?
Se5 P2 Se4 120.15(8) . . ?
Se5 P2 P1 110.26(8) . . ?
Se4 P2 P1 108.43(8) . . ?
Se5 P2 Se6 110.52(8) . . ?
Se4 P2 Se6 108.07(8) . . ?
P1 P2 Se6 96.90(8) . . ?
Se5 P2 Cs1 69.26(8) . . ?
Se4 P2 Cs1 75.35(9) . . ?
P1 P2 Cs1 175.32(16) . . ?
Se6 P2 Cs1 79.12(9) . . ?
Se5 P2 Cs2 70.54(10) . 2_545 ?
Se4 P2 Cs2 64.80(9) . 2_545 ?
P1 P2 Cs2 91.16(13) . 2_545 ?
Se6 P2 Cs2 170.74(13) . 2_545 ?
Cs1 P2 Cs2 93.00(7) . 2_545 ?
P3 P3 Se6 92.84(8) 3_666 . ?
P3 P3 Se1 94.64(8) 3_666 . ?
Se6 P3 Se1 104.36(8) . . ?
P3 P3 Cs2 109.25(18) 3_666 . ?
Se6 P3 Cs2 111.84(12) . . ?
Se1 P3 Cs2 134.81(13) . . ?

_diffrn_measured_fraction_theta_max 0.712
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         2.157
_refine_diff_density_min         -1.767
_refine_diff_density_rms         0.466