data_ecke
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_mineral 'eckerite'
_chemical_compound_source 'Lengenbach, Binn'
_chemical_melting_point ?
_chemical_formula_moiety
'Ag17.68 As8 Cu6.32 S24'
_chemical_formula_sum
'Ag17.68 As8 Cu6.32 S24'
_chemical_formula_weight 3677.58
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'Ag' 'Ag' -0.8971 1.1015
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'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'
'Cu' 'Cu' 0.3201 1.2651
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting 'monoclinic'
_space_group_IT_number 15
_symmetry_space_group_name_H-M 'C 2/c'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 11.8643(3)
_cell_length_b 6.23380(10)
_cell_length_c 16.6785(4)
_cell_angle_alpha 90.00
_cell_angle_beta 110.842(3)
_cell_angle_gamma 90.00
_cell_volume 1152.82(4)
_cell_formula_units_Z 1
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 1456
_cell_measurement_theta_min 10.1
_cell_measurement_theta_max 25.8
_exptl_crystal_description block
_exptl_crystal_colour red
_exptl_crystal_size_max 0.110
_exptl_crystal_size_mid 0.090
_exptl_crystal_size_min 0.080
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 5.297
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1662.2
_exptl_absorpt_coefficient_mu 16.952
_exptl_absorpt_correction_type 'gaussian'
_exptl_absorpt_correction_T_min 0.096
_exptl_absorpt_correction_T_max 0.159
_exptl_absorpt_process_details
'(ABSPACK; Oxford Diffraction, 2006)'
_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 'Oxford Xcalibur 3'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count .
_diffrn_standards_interval_time .
_diffrn_standards_decay_% ?
_diffrn_reflns_number 17445
_diffrn_reflns_av_R_equivalents 0.0581
_diffrn_reflns_av_sigmaI/netI 0.0355
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_theta_min 2.93
_diffrn_reflns_theta_max 34.63
_reflns_number_total 2488
_reflns_number_gt 1606
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)'
_computing_cell_refinement 'CrysAlis (Oxford Diffraction, 2006)'
_computing_data_reduction 'CrysAlis (Oxford Diffraction, 2006)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)'
_computing_publication_material 'SHELXL-97 (Sheldrick, 2008)'
_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^)+(0.0912P)^2^+35.7140P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens .
_refine_ls_hydrogen_treatment .
_refine_ls_extinction_method none
_refine_ls_extinction_coef 0.0013(2)
_refine_ls_extinction_expression
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns 2488
_refine_ls_number_parameters 67
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0769
_refine_ls_R_factor_gt 0.0825
_refine_ls_wR_factor_ref 0.2195
_refine_ls_wR_factor_gt 0.2325
_refine_ls_goodness_of_fit_ref 1.312
_refine_ls_restrained_S_all 1.312
_refine_ls_shift/su_max 0.025
_refine_ls_shift/su_mean 0.010
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
Ag1 Ag 0.14310(17) 0.0350(3) 0.21371(9) 0.0668(8) Uani 0.84(2) 1 d P . .
Cu1 Cu 0.14310(17) 0.0350(3) 0.21371(9) 0.0668(8) Uani 0.16(2) 1 d P . .
Ag2 Ag 0.05860(18) 0.9218(5) 0.43279(15) 0.0842(12) Uani 0.37(2) 1 d P . .
Cu2 Cu 0.05860(18) 0.9218(5) 0.43279(15) 0.0842(12) Uani 0.63(2) 1 d P . .
Ag3 Ag 0.35956(13) 0.0264(2) 0.13538(16) 0.0776(7) Uani 1 1 d . . .
As As 0.35360(11) 0.04631(18) 0.43332(8) 0.0258(3) Uani 1 1 d . . .
S1 S 0.1513(3) 0.1797(5) 0.0765(2) 0.0372(7) Uani 1 1 d . . .
S2 S 0.4260(3) 0.1404(6) 0.3294(2) 0.0347(7) Uani 1 1 d . . .
S3 S 0.1573(3) 0.1253(5) 0.3600(2) 0.0343(7) 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
Ag1 0.0697(12) 0.0875(15) 0.0403(9) -0.0060(7) 0.0159(7) -0.0109(9)
Cu1 0.0697(12) 0.0875(15) 0.0403(9) -0.0060(7) 0.0159(7) -0.0109(9)
Ag2 0.0468(12) 0.119(2) 0.0689(15) 0.0532(13) -0.0009(9) -0.0300(11)
Cu2 0.0468(12) 0.119(2) 0.0689(15) 0.0532(13) -0.0009(9) -0.0300(11)
Ag3 0.0335(7) 0.0460(8) 0.1435(18) 0.0002(9) 0.0193(8) -0.0004(5)
As 0.0252(5) 0.0247(6) 0.0275(6) -0.0013(4) 0.0095(4) -0.0022(4)
S1 0.0330(15) 0.0241(13) 0.054(2) -0.0045(13) 0.0151(14) -0.0007(11)
S2 0.0324(15) 0.0413(16) 0.0342(15) 0.0039(12) 0.0165(12) 0.0007(12)
S3 0.0235(13) 0.0309(14) 0.0478(18) 0.0014(13) 0.0120(12) 0.0009(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
Ag1 S3 2.451(4) . ?
Ag1 S1 2.494(4) . ?
Ag1 S2 2.612(4) 4_545 ?
Ag1 Cu2 2.835(3) 2_545 ?
Ag1 Ag2 2.835(3) 2_545 ?
Ag1 Ag3 3.270(3) . ?
Ag2 S3 2.338(4) 1_565 ?
Ag2 S1 2.341(4) 6_566 ?
Ag2 S2 2.568(4) 3_455 ?
Ag2 Ag1 2.835(3) 2_565 ?
Ag2 Cu1 2.835(3) 2_565 ?
Ag2 S1 2.922(4) 2_565 ?
Ag2 Ag3 3.016(4) 4 ?
Ag2 Cu2 3.182(6) 5_576 ?
Ag2 Ag2 3.182(6) 5_576 ?
Ag3 S2 2.502(4) 2_655 ?
Ag3 S1 2.501(4) . ?
Ag3 S3 2.512(4) 4_545 ?
Ag3 Ag2 3.016(4) 4_545 ?
Ag3 Cu2 3.016(4) 4_545 ?
As S3 2.266(3) . ?
As S2 2.268(3) . ?
As S1 2.291(3) 4_545 ?
S1 As 2.291(3) 4 ?
S1 Cu2 2.341(4) 6_565 ?
S1 Ag2 2.341(4) 6_565 ?
S1 Ag2 2.922(4) 2_545 ?
S2 Ag3 2.502(4) 2_655 ?
S2 Cu2 2.568(4) 3_545 ?
S2 Ag2 2.568(4) 3_545 ?
S2 Ag1 2.612(4) 4 ?
S2 Cu1 2.612(4) 4 ?
S3 Cu2 2.338(4) 1_545 ?
S3 Ag2 2.338(4) 1_545 ?
S3 Ag3 2.512(4) 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
S3 Ag1 S1 145.02(14) . . ?
S3 Ag1 S2 113.22(12) . 4_545 ?
S1 Ag1 S2 101.45(11) . 4_545 ?
S3 Ag1 Cu2 130.80(11) . 2_545 ?
S1 Ag1 Cu2 66.14(11) . 2_545 ?
S2 Ag1 Cu2 56.09(10) 4_545 2_545 ?
S3 Ag1 Ag2 130.80(11) . 2_545 ?
S1 Ag1 Ag2 66.14(11) . 2_545 ?
S2 Ag1 Ag2 56.09(10) 4_545 2_545 ?
Cu2 Ag1 Ag2 0.00(15) 2_545 2_545 ?
S3 Ag1 Ag3 128.02(10) . . ?
S1 Ag1 Ag3 49.20(9) . . ?
S2 Ag1 Ag3 95.08(9) 4_545 . ?
Cu2 Ag1 Ag3 101.17(8) 2_545 . ?
Ag2 Ag1 Ag3 101.17(8) 2_545 . ?
S3 Ag2 S1 122.59(14) 1_565 6_566 ?
S3 Ag2 S2 108.82(15) 1_565 3_455 ?
S1 Ag2 S2 117.08(14) 6_566 3_455 ?
S3 Ag2 Ag1 80.94(10) 1_565 2_565 ?
S1 Ag2 Ag1 153.51(14) 6_566 2_565 ?
S2 Ag2 Ag1 57.56(10) 3_455 2_565 ?
S3 Ag2 Cu1 80.94(10) 1_565 2_565 ?
S1 Ag2 Cu1 153.51(14) 6_566 2_565 ?
S2 Ag2 Cu1 57.56(10) 3_455 2_565 ?
Ag1 Ag2 Cu1 0.00(7) 2_565 2_565 ?
S3 Ag2 S1 104.42(13) 1_565 2_565 ?
S1 Ag2 S1 106.51(14) 6_566 2_565 ?
S2 Ag2 S1 91.89(12) 3_455 2_565 ?
Ag1 Ag2 S1 51.32(9) 2_565 2_565 ?
Cu1 Ag2 S1 51.32(9) 2_565 2_565 ?
S3 Ag2 Ag3 87.69(13) 1_565 4 ?
S1 Ag2 Ag3 93.91(12) 6_566 4 ?
S2 Ag2 Ag3 52.51(10) 3_455 4 ?
Ag1 Ag2 Ag3 99.48(10) 2_565 4 ?
Cu1 Ag2 Ag3 99.48(10) 2_565 4 ?
S1 Ag2 Ag3 144.32(11) 2_565 4 ?
S3 Ag2 Cu2 128.66(18) 1_565 5_576 ?
S1 Ag2 Cu2 61.66(11) 6_566 5_576 ?
S2 Ag2 Cu2 111.42(11) 3_455 5_576 ?
Ag1 Ag2 Cu2 94.85(11) 2_565 5_576 ?
Cu1 Ag2 Cu2 94.85(11) 2_565 5_576 ?
S1 Ag2 Cu2 44.85(10) 2_565 5_576 ?
Ag3 Ag2 Cu2 142.74(11) 4 5_576 ?
S3 Ag2 Ag2 128.66(18) 1_565 5_576 ?
S1 Ag2 Ag2 61.66(11) 6_566 5_576 ?
S2 Ag2 Ag2 111.42(11) 3_455 5_576 ?
Ag1 Ag2 Ag2 94.85(11) 2_565 5_576 ?
Cu1 Ag2 Ag2 94.85(11) 2_565 5_576 ?
S1 Ag2 Ag2 44.85(10) 2_565 5_576 ?
Ag3 Ag2 Ag2 142.74(11) 4 5_576 ?
Cu2 Ag2 Ag2 0.00(6) 5_576 5_576 ?
S2 Ag3 S1 139.80(13) 2_655 . ?
S2 Ag3 S3 111.16(12) 2_655 4_545 ?
S1 Ag3 S3 108.29(11) . 4_545 ?
S2 Ag3 Ag2 54.51(9) 2_655 4_545 ?
S1 Ag3 Ag2 86.87(10) . 4_545 ?
S3 Ag3 Ag2 149.87(12) 4_545 4_545 ?
S2 Ag3 Cu2 54.51(9) 2_655 4_545 ?
S1 Ag3 Cu2 86.87(10) . 4_545 ?
S3 Ag3 Cu2 149.87(12) 4_545 4_545 ?
Ag2 Ag3 Cu2 0.00(12) 4_545 4_545 ?
S2 Ag3 Ag1 141.20(12) 2_655 . ?
S1 Ag3 Ag1 49.01(10) . . ?
S3 Ag3 Ag1 85.51(9) 4_545 . ?
Ag2 Ag3 Ag1 122.77(7) 4_545 . ?
Cu2 Ag3 Ag1 122.77(7) 4_545 . ?
S3 As S2 97.32(13) . . ?
S3 As S1 100.55(13) . 4_545 ?
S2 As S1 102.15(14) . 4_545 ?
As S1 Cu2 101.87(16) 4 6_565 ?
As S1 Ag2 101.87(16) 4 6_565 ?
Cu2 S1 Ag2 0.00(6) 6_565 6_565 ?
As S1 Ag1 114.72(15) 4 . ?
Cu2 S1 Ag1 133.20(17) 6_565 . ?
Ag2 S1 Ag1 133.20(17) 6_565 . ?
As S1 Ag3 113.93(14) 4 . ?
Cu2 S1 Ag3 109.73(15) 6_565 . ?
Ag2 S1 Ag3 109.73(15) 6_565 . ?
Ag1 S1 Ag3 81.79(13) . . ?
As S1 Ag2 123.07(14) 4 2_545 ?
Cu2 S1 Ag2 73.49(14) 6_565 2_545 ?
Ag2 S1 Ag2 73.49(14) 6_565 2_545 ?
Ag1 S1 Ag2 62.54(10) . 2_545 ?
Ag3 S1 Ag2 121.01(14) . 2_545 ?
As S2 Ag3 112.16(14) . 2_655 ?
As S2 Cu2 88.39(12) . 3_545 ?
Ag3 S2 Cu2 72.98(12) 2_655 3_545 ?
As S2 Ag2 88.39(12) . 3_545 ?
Ag3 S2 Ag2 72.98(12) 2_655 3_545 ?
Cu2 S2 Ag2 0.00(10) 3_545 3_545 ?
As S2 Ag1 106.70(13) . 4 ?
Ag3 S2 Ag1 121.68(14) 2_655 4 ?
Cu2 S2 Ag1 66.35(11) 3_545 4 ?
Ag2 S2 Ag1 66.35(11) 3_545 4 ?
As S2 Cu1 106.70(13) . 4 ?
Ag3 S2 Cu1 121.68(14) 2_655 4 ?
Cu2 S2 Cu1 66.35(11) 3_545 4 ?
Ag2 S2 Cu1 66.35(11) 3_545 4 ?
Ag1 S2 Cu1 0.00(13) 4 4 ?
As S3 Cu2 102.15(14) . 1_545 ?
As S3 Ag2 102.15(14) . 1_545 ?
Cu2 S3 Ag2 0.00(12) 1_545 1_545 ?
As S3 Ag1 100.41(13) . . ?
Cu2 S3 Ag1 121.51(17) 1_545 . ?
Ag2 S3 Ag1 121.51(17) 1_545 . ?
As S3 Ag3 106.11(13) . 4 ?
Cu2 S3 Ag3 117.66(17) 1_545 4 ?
Ag2 S3 Ag3 117.66(17) 1_545 4 ?
Ag1 S3 Ag3 106.32(15) . 4 ?
_diffrn_measured_fraction_theta_max 1.008
_diffrn_reflns_theta_full 34.63
_diffrn_measured_fraction_theta_full 1.008
_refine_diff_density_max 3.757
_refine_diff_density_min -3.592
_refine_diff_density_rms 0.328