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###        Electronic paper (Acta Crystallographica Section E)             ###
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#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section E. It conforms to the requirements of Notes      #
# for Authors for Section E, and has been peer reviewed under the auspices   #
# of the IUCr Commission on Journals.                                        #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
# cif/home.html                                                              #
#                                                                            #
##############################################################################
                                             
data_I
_audit_creation_method     SHELXL-97
_chemical_name_systematic
;
dicerium pentathiosilicate
;
_chemical_name_common     ?
_chemical_formula_moiety     ?
_chemical_formula_sum     'La2 S5 Si'
_chemical_formula_structural     'La2 Si S5'
_chemical_formula_iupac     'La2 Si S5'
_chemical_formula_weight     466.21
_chemical_melting_point     ?
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'P 21/c'
_symmetry_space_group_name_Hall     '-P 2ybc'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, y+1/2, -z+1/2'
    '-x, -y, -z'
    'x, -y-1/2, z-1/2'
_cell_length_a     7.6208(12)
_cell_length_b     12.6407(15)
_cell_length_c     7.8998(12)
_cell_angle_alpha     90.00
_cell_angle_beta     101.559(13)
_cell_angle_gamma     90.00
_cell_volume     745.57(19)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     1465
_cell_measurement_theta_min     3.09
_cell_measurement_theta_max     28.28
_cell_measurement_temperature     293(2)
_exptl_crystal_description     prism
_exptl_crystal_colour     yellow
_exptl_crystal_size_max     0.13
_exptl_crystal_size_mid     0.09
_exptl_crystal_size_min     0.06
_exptl_crystal_density_diffrn     4.153
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     832
_exptl_absorpt_coefficient_mu     12.753
_exptl_absorpt_correction_type     numerical
_exptl_absorpt_process_details     '(CrysAlis-RED; Oxford Diffraction, 2006)'
_exptl_absorpt_correction_T_min     0.2084
_exptl_absorpt_correction_T_max     0.5665
_exptl_special_details
;
 ?
;
_diffrn_ambient_temperature     293(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'KUMA KM-4 with CCD area-detector'
_diffrn_measurement_method     'ω-scan'
_diffrn_detector_area_resol_mean     '1024x1024 with blocks 2x2, 33.133pixel/mm'
_diffrn_reflns_number     9434
_diffrn_reflns_av_R_equivalents     0.0515
_diffrn_reflns_av_sigmaI/netI     0.0473
_diffrn_reflns_theta_min     3.09
_diffrn_reflns_theta_max     28.28
_diffrn_reflns_theta_full     28.28
_diffrn_measured_fraction_theta_max     0.986
_diffrn_measured_fraction_theta_full     0.986
_diffrn_reflns_limit_h_min     -10
_diffrn_reflns_limit_h_max     9
_diffrn_reflns_limit_k_min     -15
_diffrn_reflns_limit_k_max     16
_diffrn_reflns_limit_l_min     -9
_diffrn_reflns_limit_l_max     10
_diffrn_standards_number     0
_diffrn_standards_interval_count     .
_diffrn_standards_interval_time     .
_diffrn_standards_decay_%     ?
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_reflns_number_total     1818
_reflns_number_gt     1465
_reflns_threshold_expression     'I>2σ(I)'
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0359
_refine_ls_R_factor_gt     0.0230
_refine_ls_wR_factor_gt     0.0385
_refine_ls_wR_factor_ref     0.0403
_refine_ls_goodness_of_fit_ref     0.966
_refine_ls_restrained_S_all     0.966
_refine_ls_number_reflns     1818
_refine_ls_number_parameters     73
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     .
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
                      'w=1/[σ²(Fo²)+(0.0134P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.001
_refine_ls_shift/su_mean     '<0.001'
_refine_diff_density_max     '0.974'
_refine_diff_density_min     '-1.219'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'Si' 'Si' 0.0817 0.0704
                         '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'
    'La' 'La' -0.2871 2.4523
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_cell_refinement     'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_reduction     'CrysAlis RED'
_computing_structure_solution     'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics     'DIAMOND (Brandenburg, 2005)'
_computing_publication_material     'publCIF (Westrip, 2007)'
loop_
    _atom_site_type_symbol
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    La La1 0.74054(4) 0.09529(2) 0.04559(3) 0.00735(8) Uani d . 1 . .
    La La2 0.66488(4) 0.66522(2) 0.13363(4) 0.00926(8) Uani d . 1 . .
    Si Si 0.83032(18) 0.38347(10) 0.09619(16) 0.0080(3) Uani d . 1 . .
    S S1 1.02312(17) 0.27396(9) 0.05064(15) 0.0111(3) Uani d . 1 . .
    S S2 0.92134(17) 0.50034(9) 0.28160(15) 0.0092(3) Uani d . 1 . .
    S S3 0.36080(16) 0.12101(9) 0.00203(15) 0.0085(3) Uani d . 1 . .
    S S4 0.67558(17) 0.47033(9) -0.11162(15) 0.0103(3) Uani d . 1 . .
    S S5 0.62829(17) 0.29811(9) 0.19537(15) 0.0100(3) Uani d . 1 . .
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    La1 0.00743(15) 0.00657(14) 0.00813(14) 0.00046(11) 0.00170(11) 0.00066(11)
    La2 0.00955(16) 0.00836(15) 0.00978(14) 0.00071(12) 0.00175(12) 0.00164(11)
    Si 0.0087(7) 0.0075(7) 0.0078(6) -0.0011(5) 0.0019(5) -0.0009(5)
    S1 0.0101(7) 0.0090(6) 0.0154(6) -0.0001(5) 0.0056(5) -0.0010(5)
    S2 0.0098(7) 0.0081(6) 0.0094(6) -0.0015(5) 0.0011(5) -0.0023(5)
    S3 0.0071(6) 0.0074(6) 0.0110(6) 0.0005(5) 0.0021(5) -0.0007(5)
    S4 0.0119(7) 0.0107(6) 0.0078(6) 0.0013(5) 0.0012(5) -0.0003(5)
    S5 0.0111(7) 0.0084(6) 0.0109(6) -0.0025(5) 0.0029(5) -0.0009(5)
_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_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    La1 S1 . 3.1154(13) y
    La1 S2 2_745 2.9213(13) y
    La1 S2 4_565 2.9767(13) y
    La1 S3 3_655 2.8456(12) y
    La1 S3 . 2.8635(13) y
    La1 S4 4_566 2.9670(13) y
    La1 S5 . 3.0184(13) y
    La1 S5 4_565 3.0420(13) y
    La2 S1 3_765 3.1226(14) y
    La2 S2 . 2.9350(13) y
    La2 S3 3_665 2.8991(12) y
    La2 S3 2_655 2.9767(13) y
    La2 S4 3_665 3.0850(13) y
    La2 S4 . 3.1453(12) y
    La2 S5 3_665 3.1040(13) y
    La2 S5 2_655 3.2936(13) y
    La2 S1 2_755 3.3745(13) y
    Si S1 . 2.1015(18) y
    Si S2 . 2.0980(17) y
    Si S4 . 2.1249(18) y
    Si S5 . 2.1522(19) y
    S1 La2 3_765 3.1226(13) ?
    S1 La2 2_745 3.3745(13) ?
    S2 La1 2_755 2.9213(13) ?
    S2 La1 4_566 2.9767(13) ?
    S3 La1 3_655 2.8456(12) ?
    S3 La2 3_665 2.8991(12) ?
    S3 La2 2_645 2.9767(13) ?
    S4 La1 4_565 2.9670(13) ?
    S4 La2 3_665 3.0850(13) ?
    S5 La1 4_566 3.0420(13) ?
    S5 La2 3_665 3.1040(13) ?
    S5 La2 2_645 3.2936(13) ?
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    S3 La1 S3 3_655 . 81.50(4) ?
    S3 La1 S2 3_655 2_745 81.81(3) ?
    S3 La1 S2 . 2_745 151.44(4) ?
    S3 La1 S4 3_655 4_566 76.21(3) ?
    S3 La1 S4 . 4_566 77.99(4) ?
    S2 La1 S4 2_745 4_566 75.61(4) ?
    S3 La1 S2 3_655 4_565 70.65(3) ?
    S3 La1 S2 . 4_565 124.09(4) ?
    S2 La1 S2 2_745 4_565 70.84(4) ?
    S4 La1 S2 4_566 4_565 135.33(3) ?
    S3 La1 S5 3_655 . 141.01(4) ?
    S3 La1 S5 . . 65.90(3) ?
    S2 La1 S5 2_745 . 117.29(3) ?
    S4 La1 S5 4_566 . 76.55(3) ?
    S2 La1 S5 4_565 . 145.78(3) ?
    S3 La1 S5 3_655 4_565 106.62(3) ?
    S3 La1 S5 . 4_565 75.35(4) ?
    S2 La1 S5 2_745 4_565 131.91(4) ?
    S4 La1 S5 4_566 4_565 152.37(4) ?
    S2 La1 S5 4_565 4_565 68.16(3) ?
    S5 La1 S5 . 4_565 85.99(2) ?
    S3 La1 S1 3_655 . 150.10(3) ?
    S3 La1 S1 . . 126.77(3) ?
    S2 La1 S1 2_745 . 75.47(3) ?
    S4 La1 S1 4_566 . 115.61(3) ?
    S2 La1 S1 4_565 . 83.54(3) ?
    S5 La1 S1 . . 68.20(3) ?
    S5 La1 S1 4_565 . 76.01(3) ?
    S3 La2 S2 3_665 . 143.07(4) ?
    S3 La2 S3 3_665 2_655 121.32(3) ?
    S2 La2 S3 . 2_655 69.46(3) ?
    S3 La2 S4 3_665 3_665 120.21(3) ?
    S2 La2 S4 . 3_665 96.52(3) ?
    S3 La2 S4 2_655 3_665 74.50(3) ?
    S3 La2 S5 3_665 3_665 64.36(3) ?
    S2 La2 S5 . 3_665 138.56(3) ?
    S3 La2 S5 2_655 3_665 131.45(4) ?
    S4 La2 S5 3_665 3_665 65.14(3) ?
    S3 La2 S1 3_665 3_765 66.39(3) ?
    S2 La2 S1 . 3_765 81.49(3) ?
    S3 La2 S1 2_655 3_765 134.48(3) ?
    S4 La2 S1 3_665 3_765 145.17(3) ?
    S5 La2 S1 3_665 3_765 93.47(4) ?
    S3 La2 S4 3_665 . 120.70(3) ?
    S2 La2 S4 . . 65.91(3) ?
    S3 La2 S4 2_655 . 117.61(3) ?
    S4 La2 S4 3_665 . 69.85(4) ?
    S5 La2 S4 3_665 . 72.80(3) ?
    S1 La2 S4 3_765 . 77.85(3) ?
    S3 La2 S5 3_665 2_655 71.04(3) ?
    S2 La2 S5 . 2_655 130.63(3) ?
    S3 La2 S5 2_655 2_655 61.17(3) ?
    S4 La2 S5 3_665 2_655 71.00(3) ?
    S5 La2 S5 3_665 2_655 80.42(3) ?
    S1 La2 S5 3_765 2_655 135.08(3) ?
    S4 La2 S5 . 2_655 139.07(3) ?
    S3 La2 S1 3_665 2_755 83.05(3) ?
    S2 La2 S1 . 2_755 71.37(3) ?
    S3 La2 S1 2_655 2_755 62.28(3) ?
    S4 La2 S1 3_665 2_755 136.72(3) ?
    S5 La2 S1 3_665 2_755 147.19(3) ?
    S1 La2 S1 3_765 2_755 75.80(3) ?
    S4 La2 S1 . 2_755 132.30(3) ?
    S5 La2 S1 2_655 2_755 85.67(3) ?
    S2 Si S1 . . 116.02(8) ?
    S2 Si S4 . . 103.31(7) ?
    S1 Si S4 . . 120.45(8) ?
    S2 Si S5 . . 105.04(7) ?
    S1 Si S5 . . 107.93(7) ?
    S4 Si S5 . . 102.33(8) ?
    Si S1 La1 . . 88.54(6) ?
    Si S1 La2 . 3_765 122.78(6) ?
    La1 S1 La2 . 3_765 139.60(4) ?
    Si S1 La2 . 2_745 123.71(6) ?
    La1 S1 La2 . 2_745 95.57(3) ?
    La2 S1 La2 3_765 2_745 87.44(3) ?
    Si S2 La1 . 2_755 138.84(7) ?
    Si S2 La2 . . 96.97(6) ?
    La1 S2 La2 2_755 . 110.42(4) ?
    Si S2 La1 . 4_566 93.92(6) ?
    La1 S2 La1 2_755 4_566 109.16(4) ?
    La2 S2 La1 . 4_566 101.69(4) ?
    La1 S3 La1 3_655 . 98.50(4) ?
    La1 S3 La2 3_655 3_665 148.24(5) ?
    La1 S3 La2 . 3_665 98.16(4) ?
    La1 S3 La2 3_655 2_645 103.86(4) ?
    La1 S3 La2 . 2_645 99.54(4) ?
    La2 S3 La2 3_665 2_645 99.78(3) ?
    Si S4 La1 . 4_565 113.10(6) ?
    Si S4 La2 . 3_665 94.98(6) ?
    La1 S4 La2 4_565 3_665 94.91(3) ?
    Si S4 La2 . . 90.44(5) ?
    La1 S4 La2 4_565 . 144.17(4) ?
    La2 S4 La2 3_665 . 110.15(4) ?
    Si S5 La1 . . 90.20(6) ?
    Si S5 La1 . 4_566 91.02(5) ?
    La1 S5 La1 . 4_566 133.05(4) ?
    Si S5 La2 . 3_665 93.88(5) ?
    La1 S5 La2 . 3_665 90.66(3) ?
    La1 S5 La2 4_566 3_665 136.01(4) ?
    Si S5 La2 . 2_645 176.92(6) ?
    La1 S5 La2 . 2_645 89.79(3) ?
    La1 S5 La2 4_566 2_645 86.74(3) ?
    La2 S5 La2 3_665 2_645 89.20(3) ?
data_global
_journal_date_recd_electronic     2007-11-08
_journal_date_accepted     2007-11-13
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2007
_journal_volume     63
_journal_issue     12
_journal_page_first     i197
_journal_page_last     i197
_journal_paper_category     QI
_journal_coeditor_code     WM2163
_publ_contact_author_name     'M. Daszkiewicz'
_publ_contact_author_address
;
W. Trzebiatowski Institute of Low Temperature and Structure Research, Polish
Academy of Sciences, Okólna str. 2, P.O. Box 1410, 50-950 Wrocław, Poland
;
_publ_contact_author_email     m.daszkiewicz@int.pan.wroc.pl
_publ_contact_author_fax     '+48 71 344 10 29'
_publ_contact_author_phone     '+48 71 344 50 21, 145'
_publ_section_title
;
La₂SiS₅
;
loop_
    _publ_author_name
    _publ_author_footnote
    _publ_author_address
    'Daszkiewicz, M.' .
;
W. Trzebiatowski Institute of Low Temperature and Structure Research,
Polish Academy of Sciences, Okólna str. 2, PO Box 1410, 50-950 Wrocław,
Poland
;
    'Gulay, L. D.' .
;
Department of Ecology and Protection of Environment, Volyn State University,
Voli Ave 13, 43009 Lutsk, Ukraine
;
    'Ruda, I. R.' .
;
Department of Physical and Colloidal Chemistry, Volyn State University,
Voli Ave 13, 43009 Lutsk, Ukraine
;
    'Marchuk, O. V.' .
;
Department of Physical and Colloidal Chemistry, Volyn State University,
Voli Ave 13, 43009 Lutsk, Ukraine
;
    'Pietraszko, A.' .
;
W. Trzebiatowski Institute of Low Temperature and Structure Research,
Polish Academy of Sciences, Okólna str. 2, PO Box 1410, 50-950 Wrocław,
Poland
;
