 
data_luca_quadra-p
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'Ag2 As1.50 Cd0 Mn2 Pb0 S6 Sb0.50'
_chemical_formula_weight          691.23
 
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'
 'Mn'  'Mn'   0.3368   0.7283
 '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'
 'Cd'  'Cd'  -0.8075   1.2024
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Pb'  'Pb'  -3.3944  10.1111
 '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'
 '-y, x, z+3/4'
 '-x, -y, z+1/2'
 'y, -x, z+1/4'
 'x, -y, -z+1/2'
 'y, x, -z+1/4'
 '-x, y, -z'
 '-y, -x, -z+3/4'
 
_cell_length_a                    5.5229(4)
_cell_length_b                    5.5229(4)
_cell_length_c                    33.399(5)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      1018.75(18)
_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     4.507
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1260
_exptl_absorpt_coefficient_mu     13.504
_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             2324
_diffrn_reflns_av_R_equivalents   0.0225
_diffrn_reflns_av_sigmaI/netI     0.1465
_diffrn_reflns_limit_h_min        0
_diffrn_reflns_limit_h_max        7
_diffrn_reflns_limit_k_min        0
_diffrn_reflns_limit_k_max        7
_diffrn_reflns_limit_l_min        0
_diffrn_reflns_limit_l_max        46
_diffrn_reflns_theta_min          2.44
_diffrn_reflns_theta_max          29.97
_reflns_number_total              1485
_reflns_number_gt                 558
_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^)+(0.0497P)^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    0.5(2)
_refine_ls_number_reflns          1485
_refine_ls_number_parameters      60
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0608
_refine_ls_R_factor_gt            0.0484
_refine_ls_wR_factor_ref          0.1080
_refine_ls_wR_factor_gt           0.1067
_refine_ls_goodness_of_fit_ref    0.665
_refine_ls_restrained_S_all       0.665
_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
Ag1 Ag 0.7483(16) 0.2355(18) 0.03365(10) 0.0240(6) Uani 0.787(4) 1 d P . .
Pb1 Pb 0.740(3) 0.242(4) 0.0417(2) 0.0240(6) Uani 0.213(4) 1 d P . .
M1CD Cd 0.2429(3) 0.2429(3) 0.1250 0.0237(3) Uani 0.58 2 d SP . .
M1AG Ag 0.2429(3) 0.2429(3) 0.1250 0.0237(3) Uani 0.42 2 d SP . .
M2 Cd 0.7382(3) 0.7382(3) 0.1250 0.0235(3) Uani 1 2 d S . .
As As 0.2559(3) 0.7443(3) 0.04947(3) 0.0208(2) Uani 1 1 d . . .
S1 S 0.2220(7) 0.7364(8) 0.11861(7) 0.0201(6) Uani 1 1 d . . .
S2 S 0.6646(6) 0.7249(8) 0.04735(10) 0.0254(9) Uani 1 1 d . . .
S3 S 0.2334(7) 0.1620(6) 0.04691(8) 0.0208(8) 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 0.0247(8) 0.0286(7) 0.0188(14) 0.003(2) -0.0002(19) -0.0012(9)
Pb1 0.0247(8) 0.0286(7) 0.0188(14) 0.003(2) -0.0002(19) -0.0012(9)
M1CD 0.0246(4) 0.0246(4) 0.0220(5) 0.0001(4) -0.0001(4) 0.0012(18)
M1AG 0.0246(4) 0.0246(4) 0.0220(5) 0.0001(4) -0.0001(4) 0.0012(18)
M2 0.0227(4) 0.0227(4) 0.0249(5) 0.0003(4) -0.0003(4) -0.0012(18)
As 0.0206(6) 0.0212(6) 0.0205(4) 0.0000(7) -0.0007(7) -0.0005(10)
S1 0.0236(18) 0.0176(14) 0.0192(11) 0.0018(14) 0.0032(13) 0.0017(16)
S2 0.0283(16) 0.0222(19) 0.0258(16) -0.0009(16) -0.0039(11) 0.0020(17)
S3 0.0158(15) 0.0329(17) 0.0137(13) 0.0014(10) 0.0025(15) 0.0019(17)
 
_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 2.723(4) 7_655 ?
Ag1 S3 2.745(10) 1_655 ?
Ag1 S2 2.780(11) . ?
Ag1 S2 2.894(11) 1_545 ?
Ag1 S3 2.907(9) . ?
Pb1 S2 2.71(2) . ?
Pb1 S3 2.767(19) 1_655 ?
Pb1 S3 2.836(19) . ?
Pb1 S2 2.89(2) 1_545 ?
Pb1 S3 2.994(9) 7_655 ?
Pb1 S1 2.999(8) 6 ?
M1CD S3 2.647(3) 6 ?
M1CD S3 2.647(3) . ?
M1CD S1 2.736(5) . ?
M1CD S1 2.736(5) 6 ?
M1CD S1 2.808(5) 6_455 ?
M1CD S1 2.808(5) 1_545 ?
M2 S2 2.626(3) 6 ?
M2 S2 2.626(3) . ?
M2 S1 2.680(4) 6_565 ?
M2 S1 2.680(4) 1_655 ?
M2 S1 2.859(4) . ?
M2 S1 2.859(4) 6 ?
As S2 2.261(4) . ?
As S3 2.312(4) 1_565 ?
As S1 2.317(3) . ?
S1 M2 2.680(4) 1_455 ?
S1 M1AG 2.808(5) 1_565 ?
S1 M1CD 2.808(5) 1_565 ?
S1 Pb1 2.999(8) 6 ?
S2 Pb1 2.89(2) 1_565 ?
S2 Ag1 2.894(11) 1_565 ?
S3 As 2.312(4) 1_545 ?
S3 Ag1 2.723(4) 7_655 ?
S3 Ag1 2.745(10) 1_455 ?
S3 Pb1 2.767(19) 1_455 ?
S3 Pb1 2.994(9) 7_655 ?
 
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 S3 95.8(2) 7_655 1_655 ?
S3 Ag1 S2 108.3(3) 7_655 . ?
S3 Ag1 S2 106.2(3) 1_655 . ?
S3 Ag1 S2 91.0(3) 7_655 1_545 ?
S3 Ag1 S2 89.2(3) 1_655 1_545 ?
S2 Ag1 S2 153.5(3) . 1_545 ?
S3 Ag1 S3 99.6(3) 7_655 . ?
S3 Ag1 S3 155.4(3) 1_655 . ?
S2 Ag1 S3 87.0(3) . . ?
S2 Ag1 S3 71.5(2) 1_545 . ?
S2 Pb1 S3 107.6(7) . 1_655 ?
S2 Pb1 S3 89.8(6) . . ?
S3 Pb1 S3 160.6(8) 1_655 . ?
S2 Pb1 S2 161.2(7) . 1_545 ?
S3 Pb1 S2 88.9(6) 1_655 1_545 ?
S3 Pb1 S2 72.6(5) . 1_545 ?
S2 Pb1 S3 102.8(5) . 7_655 ?
S3 Pb1 S3 89.4(4) 1_655 7_655 ?
S3 Pb1 S3 95.0(4) . 7_655 ?
S2 Pb1 S3 85.8(5) 1_545 7_655 ?
S2 Pb1 S1 88.0(4) . 6 ?
S3 Pb1 S1 86.4(4) 1_655 6 ?
S3 Pb1 S1 85.8(4) . 6 ?
S2 Pb1 S1 84.1(4) 1_545 6 ?
S3 Pb1 S1 169.2(8) 7_655 6 ?
S3 M1CD S3 164.68(18) 6 . ?
S3 M1CD S1 95.13(10) 6 . ?
S3 M1CD S1 95.18(9) . . ?
S3 M1CD S1 95.18(9) 6 6 ?
S3 M1CD S1 95.13(10) . 6 ?
S1 M1CD S1 95.16(18) . 6 ?
S3 M1CD S1 75.89(9) 6 6_455 ?
S3 M1CD S1 92.77(10) . 6_455 ?
S1 M1CD S1 90.278(11) . 6_455 ?
S1 M1CD S1 169.97(12) 6 6_455 ?
S3 M1CD S1 92.77(10) 6 1_545 ?
S3 M1CD S1 75.89(9) . 1_545 ?
S1 M1CD S1 169.97(12) . 1_545 ?
S1 M1CD S1 90.278(11) 6 1_545 ?
S1 M1CD S1 85.65(18) 6_455 1_545 ?
S2 M2 S2 165.13(19) 6 . ?
S2 M2 S1 94.34(9) 6 6_565 ?
S2 M2 S1 96.08(11) . 6_565 ?
S2 M2 S1 96.08(11) 6 1_655 ?
S2 M2 S1 94.34(9) . 1_655 ?
S1 M2 S1 90.8(2) 6_565 1_655 ?
S2 M2 S1 92.59(11) 6 . ?
S2 M2 S1 76.81(10) . . ?
S1 M2 S1 90.327(10) 6_565 . ?
S1 M2 S1 171.15(10) 1_655 . ?
S2 M2 S1 76.81(10) 6 6 ?
S2 M2 S1 92.59(11) . 6 ?
S1 M2 S1 171.15(10) 6_565 6 ?
S1 M2 S1 90.327(10) 1_655 6 ?
S1 M2 S1 89.9(2) . 6 ?
S2 As S3 95.73(14) . 1_565 ?
S2 As S1 96.38(13) . . ?
S3 As S1 92.94(14) 1_565 . ?
As S1 M2 99.20(12) . 1_455 ?
As S1 M1CD 95.34(14) . . ?
M2 S1 M1CD 92.26(11) 1_455 . ?
As S1 M1AG 93.08(13) . 1_565 ?
M2 S1 M1AG 91.78(17) 1_455 1_565 ?
M1CD S1 M1AG 169.97(12) . 1_565 ?
As S1 M1CD 93.08(13) . 1_565 ?
M2 S1 M1CD 91.78(17) 1_455 1_565 ?
M1CD S1 M1CD 169.97(12) . 1_565 ?
M1AG S1 M1CD 0.000(5) 1_565 1_565 ?
As S1 M2 89.64(11) . . ?
M2 S1 M2 171.15(10) 1_455 . ?
M1CD S1 M2 87.47(16) . . ?
M1AG S1 M2 87.13(10) 1_565 . ?
M1CD S1 M2 87.13(10) 1_565 . ?
As S1 Pb1 173.1(4) . 6 ?
M2 S1 Pb1 87.5(4) 1_455 6 ?
M1CD S1 Pb1 85.8(4) . 6 ?
M1AG S1 Pb1 85.2(4) 1_565 6 ?
M1CD S1 Pb1 85.2(4) 1_565 6 ?
M2 S1 Pb1 83.7(4) . 6 ?
As S2 M2 97.03(13) . . ?
As S2 Pb1 101.6(4) . . ?
M2 S2 Pb1 94.2(2) . . ?
As S2 Ag1 102.6(2) . . ?
M2 S2 Ag1 99.45(15) . . ?
Pb1 S2 Ag1 5.5(2) . . ?
As S2 Pb1 95.7(4) . 1_565 ?
M2 S2 Pb1 90.9(2) . 1_565 ?
Pb1 S2 Pb1 161.2(7) . 1_565 ?
Ag1 S2 Pb1 157.7(3) . 1_565 ?
As S2 Ag1 96.8(2) . 1_565 ?
M2 S2 Ag1 95.98(15) . 1_565 ?
Pb1 S2 Ag1 157.6(3) . 1_565 ?
Ag1 S2 Ag1 153.5(3) . 1_565 ?
Pb1 S2 Ag1 5.4(2) 1_565 1_565 ?
As S3 M1CD 97.51(11) 1_545 . ?
As S3 Ag1 100.6(2) 1_545 7_655 ?
M1CD S3 Ag1 161.4(3) . 7_655 ?
As S3 Ag1 101.9(3) 1_545 1_455 ?
M1CD S3 Ag1 98.82(13) . 1_455 ?
Ag1 S3 Ag1 81.6(2) 7_655 1_455 ?
As S3 Pb1 102.4(5) 1_545 1_455 ?
M1CD S3 Pb1 93.2(2) . 1_455 ?
Ag1 S3 Pb1 87.1(2) 7_655 1_455 ?
Ag1 S3 Pb1 5.7(2) 1_455 1_455 ?
As S3 Pb1 96.0(4) 1_545 . ?
M1CD S3 Pb1 90.9(2) . . ?
Ag1 S3 Pb1 83.1(2) 7_655 . ?
Ag1 S3 Pb1 158.3(2) 1_455 . ?
Pb1 S3 Pb1 160.6(8) 1_455 . ?
As S3 Ag1 95.3(2) 1_545 . ?
M1CD S3 Ag1 96.16(14) . . ?
Ag1 S3 Ag1 78.0(3) 7_655 . ?
Ag1 S3 Ag1 155.4(3) 1_455 . ?
Pb1 S3 Ag1 158.8(3) 1_455 . ?
Pb1 S3 Ag1 5.3(2) . . ?
As S3 Pb1 100.4(4) 1_545 7_655 ?
M1CD S3 Pb1 161.4(4) . 7_655 ?
Ag1 S3 Pb1 0.7(5) 7_655 7_655 ?
Ag1 S3 Pb1 82.4(4) 1_455 7_655 ?
Pb1 S3 Pb1 87.9(4) 1_455 7_655 ?
Pb1 S3 Pb1 82.4(4) . 7_655 ?
Ag1 S3 Pb1 77.3(3) . 7_655 ?
 
_diffrn_measured_fraction_theta_max    1.000
_diffrn_reflns_theta_full              29.97
_diffrn_measured_fraction_theta_full   1.000
_refine_diff_density_max    4.452
_refine_diff_density_min   -5.004
_refine_diff_density_rms    0.583
