data_waka_wc
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'As9 S14 Sb'
_chemical_formula_weight          1244.87
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'As'  'As'   0.0499   2.0058
 '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'
 'Sb'  'Sb'  -0.5866   1.5461
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            ?
_symmetry_space_group_name_H-M    ?
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, z+1/2'
 '-x+1/2, y+1/2, z+1/2'
 'x+1/2, -y+1/2, z'
 
_cell_length_a                    25.310(3)
_cell_length_b                    14.515(2)
_cell_length_c                    6.4988(5)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      2387.5(5)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        ?
_exptl_crystal_colour             ?
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     3.463
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              2288
_exptl_absorpt_coefficient_mu     14.752
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
 
_exptl_special_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   ?
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             26676
_diffrn_reflns_av_R_equivalents   0.0540
_diffrn_reflns_av_sigmaI/netI     0.0364
_diffrn_reflns_limit_h_min        -30
_diffrn_reflns_limit_h_max        35
_diffrn_reflns_limit_k_min        -20
_diffrn_reflns_limit_k_max        20
_diffrn_reflns_limit_l_min        -9
_diffrn_reflns_limit_l_max        9
_diffrn_reflns_theta_min          2.92
_diffrn_reflns_theta_max          30.10
_reflns_number_total              3746
_reflns_number_gt                 3187
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_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^)+(0.0304P)^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    -0.008(10)
_refine_ls_number_reflns          3746
_refine_ls_number_parameters      219
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.0578
_refine_ls_R_factor_gt            0.0244
_refine_ls_wR_factor_ref          0.0592
_refine_ls_wR_factor_gt           0.0250
_refine_ls_goodness_of_fit_ref    0.926
_refine_ls_restrained_S_all       0.926
_refine_ls_shift/su_max           0.085
_refine_ls_shift/su_mean          0.001
 
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
AS1 Sb -0.46952(2) -0.27935(4) -0.25057(13) 0.04017(18) Uani 0.030(6) 1 d P . .
SB1 As -0.46952(2) -0.27935(4) -0.25057(13) 0.04017(18) Uani 0.970(6) 1 d P . .
As2 As -0.43980(2) -0.22032(4) -0.74422(13) 0.04298(13) Uani 1 1 d . . .
AS3 Sb -0.37506(2) -0.43589(3) -0.75121(12) 0.04422(12) Uani 0.25 1 d P . .
SB3 As -0.37506(2) -0.43589(3) -0.75121(12) 0.04422(12) Uani 0.75 1 d P . .
As4 As -0.33090(2) -0.45034(4) -0.24656(13) 0.04259(13) Uani 1 1 d . . .
AS5 Sb -0.09483(2) -0.15587(4) -0.75155(12) 0.03908(18) Uani 0.023(5) 1 d P . .
SB5 As -0.09483(2) -0.15587(4) -0.75155(12) 0.03908(18) Uani 0.977(5) 1 d P . .
AS6 Sb -0.10988(2) -0.22948(4) -0.24633(14) 0.04427(19) Uani 0.026(6) 1 d P . .
SB6 As -0.10988(2) -0.22948(4) -0.24633(14) 0.04427(19) Uani 0.974(6) 1 d P . .
AS7 Sb -0.32938(4) -0.01352(6) -0.7589(2) 0.0760(4) Uani 0.021(8) 1 d P . .
SB7 As -0.32938(4) -0.01352(6) -0.7589(2) 0.0760(4) Uani 0.979(8) 1 d P . .
AS8 Sb -0.29530(5) -0.11547(8) -0.41049(19) 0.0843(4) Uani 0.011(8) 1 d P . .
SB8 As -0.29530(5) -0.11547(8) -0.41049(19) 0.0843(4) Uani 0.989(8) 1 d P . .
AS9 Sb -0.21253(3) -0.36229(4) -0.83727(12) 0.0443(2) Uani 0.042(6) 1 d P . .
SB9 As -0.21253(3) -0.36229(4) -0.83727(12) 0.0443(2) Uani 0.958(6) 1 d P . .
AS10 Sb -0.07637(3) -0.49819(5) -0.84154(11) 0.0509(2) Uani 0.023(7) 1 d P . .
SB10 As -0.07637(3) -0.49819(5) -0.84154(11) 0.0509(2) Uani 0.977(7) 1 d P . .
S1 S -0.49370(6) -0.17398(13) -0.0002(2) 0.0348(3) Uani 1 1 d . . .
S2 S -0.00350(6) -0.32319(13) -0.5001(2) 0.0359(3) Uani 1 1 d . . .
S3 S -0.45905(5) -0.37440(9) -0.7339(3) 0.0381(3) Uani 1 1 d . . .
S4 S -0.34053(7) -0.33285(12) 0.0016(3) 0.0380(3) Uani 1 1 d . . .
S5 S -0.33536(6) -0.34650(10) -0.5002(3) 0.0346(3) Uani 1 1 d . . .
S6 S -0.41687(4) -0.49741(9) -0.2479(2) 0.0341(2) Uani 1 1 d . . .
S7 S -0.16252(6) -0.15700(10) 0.0012(3) 0.0305(3) Uani 1 1 d . . .
S8 S -0.15932(7) -0.16995(12) -0.4981(3) 0.0380(3) Uani 1 1 d . . .
S9 S -0.04256(5) -0.12266(8) -0.2358(3) 0.0344(2) Uani 1 1 d . . .
S10 S -0.25296(5) -0.00011(11) -0.2598(3) 0.0443(3) Uani 1 1 d . . .
S11 S -0.20719(7) -0.37970(12) -0.1805(3) 0.0504(4) Uani 1 1 d . . .
S12 S -0.12588(5) -0.37766(9) -0.7274(3) 0.0372(3) Uani 1 1 d . . .
S13 S -0.08908(8) -0.49894(14) -0.1843(3) 0.0569(4) Uani 1 1 d . . .
S14 S -0.37293(6) -0.12101(10) -0.2398(3) 0.0431(3) 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
AS1 0.0397(3) 0.0400(3) 0.0409(3) -0.0001(3) 0.0000(3) 0.0000(2)
SB1 0.0397(3) 0.0400(3) 0.0409(3) -0.0001(3) 0.0000(3) 0.0000(2)
As2 0.0428(3) 0.0422(3) 0.0440(3) -0.0001(3) 0.0003(4) 0.0002(2)
AS3 0.0438(2) 0.0439(2) 0.0449(2) 0.0001(3) 0.0000(3) -0.0001(2)
SB3 0.0438(2) 0.0439(2) 0.0449(2) 0.0001(3) 0.0000(3) -0.0001(2)
As4 0.0421(3) 0.0423(3) 0.0434(3) 0.0000(4) -0.0001(4) -0.0003(2)
AS5 0.0387(3) 0.0390(3) 0.0396(3) -0.0001(3) 0.0000(3) 0.0005(2)
SB5 0.0387(3) 0.0390(3) 0.0396(3) -0.0001(3) 0.0000(3) 0.0005(2)
AS6 0.0441(3) 0.0442(3) 0.0446(3) -0.0004(4) 0.0000(3) 0.0005(2)
SB6 0.0441(3) 0.0442(3) 0.0446(3) -0.0004(4) 0.0000(3) 0.0005(2)
AS7 0.0760(6) 0.0754(6) 0.0767(6) -0.0002(6) -0.0004(6) 0.0011(4)
SB7 0.0760(6) 0.0754(6) 0.0767(6) -0.0002(6) -0.0004(6) 0.0011(4)
AS8 0.0842(8) 0.0845(7) 0.0840(7) 0.0000(6) -0.0001(6) -0.0001(6)
SB8 0.0842(8) 0.0845(7) 0.0840(7) 0.0000(6) -0.0001(6) -0.0001(6)
AS9 0.0440(3) 0.0438(3) 0.0452(3) -0.0005(3) -0.0002(3) -0.0005(3)
SB9 0.0440(3) 0.0438(3) 0.0452(3) -0.0005(3) -0.0002(3) -0.0005(3)
AS10 0.0506(4) 0.0504(4) 0.0516(4) -0.0001(4) 0.0004(3) -0.0001(4)
SB10 0.0506(4) 0.0504(4) 0.0516(4) -0.0001(4) 0.0004(3) -0.0001(4)
S1 0.0344(7) 0.0343(7) 0.0358(7) -0.0004(5) -0.0002(6) -0.0001(6)
S2 0.0351(7) 0.0347(8) 0.0380(8) -0.0005(6) 0.0006(7) 0.0007(6)
S3 0.0368(6) 0.0384(6) 0.0391(6) -0.0010(8) 0.0007(7) 0.0000(5)
S4 0.0374(7) 0.0369(7) 0.0396(7) -0.0008(7) 0.0006(7) 0.0001(6)
S5 0.0347(7) 0.0339(7) 0.0353(7) -0.0013(7) 0.0003(6) -0.0004(6)
S6 0.0341(5) 0.0342(5) 0.0340(5) 0.0001(9) 0.0000(6) 0.0002(5)
S7 0.0305(6) 0.0295(6) 0.0314(6) -0.0002(6) 0.0001(6) 0.0009(5)
S8 0.0373(7) 0.0377(7) 0.0390(7) 0.0002(7) 0.0000(7) -0.0001(6)
S9 0.0343(5) 0.0338(5) 0.0350(6) -0.0008(7) 0.0002(7) 0.0006(5)
S10 0.0438(6) 0.0445(6) 0.0446(6) -0.0012(10) 0.0006(7) -0.0003(7)
S11 0.0494(8) 0.0493(8) 0.0526(9) 0.0017(7) -0.0017(7) -0.0016(7)
S12 0.0374(6) 0.0366(6) 0.0377(7) 0.0003(7) 0.0009(7) -0.0001(5)
S13 0.0585(8) 0.0533(8) 0.0590(10) 0.0000(9) 0.0004(7) -0.0002(10)
S14 0.0430(6) 0.0426(6) 0.0436(7) -0.0001(9) 0.0003(9) -0.0008(6)
 
_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
AS1 S1 2.3156(18) . ?
AS1 S9 2.3345(13) 4_445 ?
AS1 S2 2.3634(18) 4_445 ?
As2 S1 2.2539(18) 1_554 ?
As2 S3 2.2899(14) . ?
As2 S2 2.3483(17) 4_445 ?
AS3 S3 2.3082(14) . ?
AS3 S5 2.3142(18) . ?
AS3 S4 2.362(2) 1_554 ?
As4 S5 2.2363(19) . ?
As4 S6 2.2806(13) . ?
As4 S4 2.360(2) . ?
AS5 S6 2.3192(14) 3_454 ?
AS5 S8 2.328(2) . ?
AS5 S7 2.3489(18) 1_554 ?
AS6 S8 2.234(2) . ?
AS6 S9 2.3047(13) . ?
AS6 S7 2.3386(17) . ?
AS7 S13 2.130(2) 3_454 ?
AS7 S11 2.211(2) 3_454 ?
AS7 AS8 2.8391(19) . ?
AS8 S10 2.216(2) . ?
AS8 S14 2.258(2) . ?
AS9 S10 2.2403(17) 3_444 ?
AS9 S11 2.2487(19) 1_554 ?
AS9 S12 2.3172(15) . ?
AS10 S13 2.2506(19) 1_554 ?
AS10 S12 2.2761(16) . ?
AS10 S14 2.2940(17) 3_444 ?
S1 As2 2.2538(18) 1_556 ?
S2 As2 2.3483(17) 4_545 ?
S2 AS1 2.3634(18) 4_545 ?
S2 SB1 2.3634(18) 4_545 ?
S4 SB3 2.362(2) 1_556 ?
S4 AS3 2.362(2) 1_556 ?
S6 SB5 2.3192(14) 3_445 ?
S6 AS5 2.3192(14) 3_445 ?
S7 SB5 2.3489(18) 1_556 ?
S7 AS5 2.3489(18) 1_556 ?
S9 SB1 2.3345(13) 4_545 ?
S9 AS1 2.3345(13) 4_545 ?
S10 SB9 2.2403(17) 3_455 ?
S10 AS9 2.2403(17) 3_455 ?
S11 SB7 2.211(2) 3_445 ?
S11 AS7 2.211(2) 3_445 ?
S11 SB9 2.2487(19) 1_556 ?
S11 AS9 2.2487(19) 1_556 ?
S13 SB7 2.130(2) 3_445 ?
S13 AS7 2.130(2) 3_445 ?
S13 SB10 2.2506(18) 1_556 ?
S13 AS10 2.2506(18) 1_556 ?
S14 SB10 2.2940(17) 3_455 ?
S14 AS10 2.2940(17) 3_455 ?
 
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 AS1 S9 99.46(6) . 4_445 ?
S1 AS1 S2 88.29(5) . 4_445 ?
S9 AS1 S2 97.10(6) 4_445 4_445 ?
S1 As2 S3 100.62(7) 1_554 . ?
S1 As2 S2 90.15(6) 1_554 4_445 ?
S3 As2 S2 95.55(7) . 4_445 ?
S3 AS3 S5 98.55(6) . . ?
S3 AS3 S4 97.42(6) . 1_554 ?
S5 AS3 S4 87.92(5) . 1_554 ?
S5 As4 S6 98.68(6) . . ?
S5 As4 S4 90.65(5) . . ?
S6 As4 S4 96.92(6) . . ?
S6 AS5 S8 99.75(6) 3_454 . ?
S6 AS5 S7 96.14(5) 3_454 1_554 ?
S8 AS5 S7 88.40(5) . 1_554 ?
S8 AS6 S9 100.11(6) . . ?
S8 AS6 S7 90.61(5) . . ?
S9 AS6 S7 95.64(6) . . ?
S13 AS7 S11 105.42(8) 3_454 3_454 ?
S13 AS7 AS8 99.48(7) 3_454 . ?
S11 AS7 AS8 98.44(7) 3_454 . ?
S10 AS8 S14 103.33(8) . . ?
S10 AS8 AS7 96.06(7) . . ?
S14 AS8 AS7 98.40(7) . . ?
S10 AS9 S11 98.40(7) 3_444 1_554 ?
S10 AS9 S12 102.35(6) 3_444 . ?
S11 AS9 S12 103.75(7) 1_554 . ?
S13 AS10 S12 104.33(7) 1_554 . ?
S13 AS10 S14 101.64(8) 1_554 3_444 ?
S12 AS10 S14 101.27(6) . 3_444 ?
As2 S1 AS1 99.30(7) 1_556 . ?
As2 S2 AS1 92.54(6) 4_545 4_545 ?
As2 S2 SB1 92.54(6) 4_545 4_545 ?
AS1 S2 SB1 0.00(3) 4_545 4_545 ?
As2 S3 AS3 100.39(5) . . ?
As4 S4 SB3 92.61(6) . 1_556 ?
As4 S4 AS3 92.61(6) . 1_556 ?
SB3 S4 AS3 0.00(4) 1_556 1_556 ?
As4 S5 AS3 99.42(6) . . ?
As4 S6 SB5 100.10(5) . 3_445 ?
As4 S6 AS5 100.10(5) . 3_445 ?
SB5 S6 AS5 0.00(5) 3_445 3_445 ?
AS6 S7 SB5 93.33(6) . 1_556 ?
AS6 S7 AS5 93.33(6) . 1_556 ?
SB5 S7 AS5 0.00(3) 1_556 1_556 ?
AS6 S8 AS5 99.18(7) . . ?
AS6 S9 SB1 100.04(5) . 4_545 ?
AS6 S9 AS1 100.04(5) . 4_545 ?
SB1 S9 AS1 0.00(4) 4_545 4_545 ?
AS8 S10 SB9 112.75(8) . 3_455 ?
AS8 S10 AS9 112.75(8) . 3_455 ?
SB9 S10 AS9 0.00(3) 3_455 3_455 ?
SB7 S11 AS7 0.00(4) 3_445 3_445 ?
SB7 S11 SB9 110.64(9) 3_445 1_556 ?
AS7 S11 SB9 110.64(9) 3_445 1_556 ?
SB7 S11 AS9 110.64(9) 3_445 1_556 ?
AS7 S11 AS9 110.64(9) 3_445 1_556 ?
SB9 S11 AS9 0.000(5) 1_556 1_556 ?
AS10 S12 AS9 119.65(7) . . ?
SB7 S13 AS7 0.00(7) 3_445 3_445 ?
SB7 S13 SB10 111.35(9) 3_445 1_556 ?
AS7 S13 SB10 111.35(9) 3_445 1_556 ?
SB7 S13 AS10 111.35(9) 3_445 1_556 ?
AS7 S13 AS10 111.35(9) 3_445 1_556 ?
SB10 S13 AS10 0.00(3) 1_556 1_556 ?
AS8 S14 SB10 108.51(8) . 3_455 ?
AS8 S14 AS10 108.51(8) . 3_455 ?
SB10 S14 AS10 0.00(5) 3_455 3_455 ?
 
_diffrn_measured_fraction_theta_max    0.996
_diffrn_reflns_theta_full              30.10
_diffrn_measured_fraction_theta_full   0.996
_refine_diff_density_max    0.930
_refine_diff_density_min   -0.919