#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/79/2237973.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2237973
loop_
_publ_author_name
'Mereiter, Kurt'
_publ_section_title
;
 Trilithium thioarsenate octahydrate
;
_journal_coeditor_code           PJ2002
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i30
_journal_page_last               i31
_journal_paper_doi               10.1107/S1600536813010921
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'Li3 As S4, 8H2 O'
_chemical_formula_moiety         Li3AsS4.8H2O
_chemical_formula_sum            'As H16 Li3 O8 S4'
_chemical_formula_weight         368.11
_chemical_name_common            'Li3[AsS4].8H2O '
_chemical_name_systematic
;
Trilithium thioarsenate octahydrate
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.300(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.036(2)
_cell_length_b                   10.064(2)
_cell_length_c                   14.264(3)
_cell_measurement_reflns_used    34
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      26.2
_cell_measurement_theta_min      9.1
_cell_volume                     1375.5(5)
_computing_cell_refinement       'LLSQ (Mereiter, 1992)'
_computing_data_collection
;
Philips PW1100 software (Hornstra & Vossers, 1973)
;
_computing_data_reduction        'PWD (Mereiter, 1992)'
_computing_molecular_graphics
'Mercury (Macrae et al., 2006) and DIAMOND (Brandenburg, 2012)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Philips PW1100 four-circle'
_diffrn_measurement_method       'ω-2θ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5729
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        2.0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.090
_exptl_absorpt_correction_T_max  0.54
_exptl_absorpt_correction_T_min  0.51
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   '\mR = 0.45'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       oval
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.358
_refine_ls_extinction_coef       0.0081(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         4001
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0179P)²+0.5909P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0515
_refine_ls_wR_factor_ref         0.0573
_reflns_number_gt                2913
_reflns_number_total             4001
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            pj2002.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_original_formula_sum        'As H16 Li3 O8 S4 '
_cod_database_code               2237973
_cod_database_fobs_code          2237973
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'-x, -y, -z'
'-x, y, -z-1/2'
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_symmetry_multiplicity
Li Li1 0.5000 0.5000 0.5000 0.0393(13) Uani d S 1 2
Li Li2 0.2821(4) 0.7213(4) 0.5102(4) 0.0443(10) Uani d . 1 1
Li Li3 0.5000 0.5984(5) 0.7500 0.0311(11) Uani d S 1 2
Li Li4 0.0724(5) 0.8832(5) 0.4126(5) 0.0610(14) Uani d . 1 1
As As1 0.0000 0.40273(3) 0.2500 0.01865(8) Uani d S 1 2
As As2 0.5000 0.91402(2) 0.2500 0.01887(8) Uani d S 1 2
S S1 -0.12581(5) 0.53147(5) 0.31185(4) 0.02508(11) Uani d . 1 1
S S2 0.13565(5) 0.27910(5) 0.36066(4) 0.02849(12) Uani d . 1 1
S S3 0.37068(5) 1.03848(5) 0.31147(4) 0.02615(12) Uani d . 1 1
S S4 0.64151(6) 0.79087(5) 0.35891(4) 0.02873(12) Uani d . 1 1
O O1 0.55849(15) 0.47247(15) 0.66032(12) 0.0297(3) Uani d G 1 1
H H1A 0.6400 0.4629 0.6874 0.054(6) Uiso d G 1 1
H H1B 0.5239 0.4023 0.6655 0.054(6) Uiso d G 1 1
O O2 0.28906(17) 0.51048(16) 0.50233(12) 0.0330(3) Uani d G 1 1
H H2A 0.2693 0.4923 0.5512 0.068(8) Uiso d G 1 1
H H2B 0.2494 0.4564 0.4627 0.068(8) Uiso d G 1 1
O O3 0.48739(17) 0.72351(17) 0.51911(12) 0.0359(4) Uani d G 1 1
H H3A 0.5233 0.7696 0.5654 0.077(8) Uiso d G 1 1
H H3B 0.5211 0.7466 0.4775 0.077(8) Uiso d G 1 1
O O4 0.33730(16) 0.70514(14) 0.67279(12) 0.0303(3) Uani d G 1 1
H H4A 0.2703 0.6689 0.6804 0.051(6) Uiso d G 1 1
H H4B 0.3423 0.7745 0.7010 0.051(6) Uiso d G 1 1
O O5 0.05507(17) 0.72354(16) 0.48637(12) 0.0344(4) Uani d G 1 1
H H5A 0.0167 0.6700 0.4459 0.059(7) Uiso d G 1 1
H H5B 0.0110 0.7247 0.5248 0.059(7) Uiso d G 1 1
O O6 0.2558(2) 0.9454(2) 0.49965(14) 0.0486(5) Uani d G 1 1
H H6A 0.2939 0.9720 0.4614 0.107(11) Uiso d G 1 1
H H6B 0.2680 1.0022 0.5406 0.107(11) Uiso d G 1 1
O O7 0.1906(2) 0.7739(2) 0.34519(16) 0.0535(5) Uani d G 1 1
H H7A 0.1517 0.7256 0.3009 0.112(12) Uiso d G 1 1
H H7B 0.2329 0.8251 0.3220 0.112(12) Uiso d G 1 1
O O8 -0.05671(19) 1.0198(2) 0.36351(18) 0.0573(6) Uani d G 1 1
H H8A -0.0190 1.0806 0.3455 0.102(11) Uiso d G 1 1
H H8B -0.1288 1.0100 0.3210 0.102(11) Uiso d G 1 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Li Li -0.0003 0.0001 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O2 Li1 O2 . 3_666 180.0
O2 Li1 O1 . 3_666 92.91(6)
O2 Li1 O1 3_666 3_666 87.09(6)
O2 Li1 O1 . . 87.09(6)
O2 Li1 O1 3_666 . 92.91(6)
O1 Li1 O1 3_666 . 180.0
O2 Li1 O3 . 3_666 98.16(6)
O2 Li1 O3 3_666 3_666 81.84(6)
O1 Li1 O3 3_666 3_666 90.41(6)
O1 Li1 O3 . 3_666 89.59(6)
O2 Li1 O3 . . 81.84(6)
O2 Li1 O3 3_666 . 98.16(6)
O1 Li1 O3 3_666 . 89.59(6)
O1 Li1 O3 . . 90.41(6)
O3 Li1 O3 3_666 . 180.0
O3 Li2 O2 . . 88.03(18)
O3 Li2 O5 . . 174.8(3)
O2 Li2 O5 . . 92.89(17)
O3 Li2 O4 . . 90.12(18)
O2 Li2 O4 . . 88.84(18)
O5 Li2 O4 . . 94.98(19)
O3 Li2 O6 . . 95.14(18)
O2 Li2 O6 . . 172.9(3)
O5 Li2 O6 . . 83.40(16)
O4 Li2 O6 . . 97.45(19)
O3 Li2 O7 . . 98.6(2)
O2 Li2 O7 . . 100.6(2)
O5 Li2 O7 . . 76.20(15)
O4 Li2 O7 . . 167.3(2)
O6 Li2 O7 . . 72.74(15)
O4 Li3 O4 4_657 . 114.7(3)
O4 Li3 O1 4_657 . 110.23(7)
O4 Li3 O1 . . 109.58(7)
O4 Li3 O1 4_657 4_657 109.58(7)
O4 Li3 O1 . 4_657 110.23(7)
O1 Li3 O1 . 4_657 101.7(2)
O8 Li4 O5 . . 129.8(3)
O8 Li4 O6 . . 114.2(3)
O5 Li4 O6 . . 97.9(3)
O8 Li4 O7 . . 130.4(3)
O5 Li4 O7 . . 88.2(2)
O6 Li4 O7 . . 84.6(2)
S2 As1 S2 4_556 . 109.21(3)
S2 As1 S1 4_556 4_556 111.42(2)
S2 As1 S1 . 4_556 109.04(2)
S2 As1 S1 4_556 . 109.04(2)
S2 As1 S1 . . 111.42(2)
S1 As1 S1 4_556 . 106.72(3)
S4 As2 S4 4_656 . 109.87(4)
S4 As2 S3 4_656 . 106.15(2)
S4 As2 S3 . . 112.69(2)
S4 As2 S3 4_656 4_656 112.69(2)
S4 As2 S3 . 4_656 106.15(2)
S3 As2 S3 . 4_656 109.40(3)
Li3 O1 Li1 . . 122.93(10)
Li3 O1 H1A . . 102.7
Li1 O1 H1A . . 115.8
Li3 O1 H1B . . 106.3
Li1 O1 H1B . . 102.6
H1A O1 H1B . . 105.0
Li2 O2 Li1 . . 95.65(13)
Li2 O2 H2A . . 99.3
Li1 O2 H2A . . 120.5
Li2 O2 H2B . . 134.3
Li1 O2 H2B . . 104.1
H2A O2 H2B . . 105.0
Li2 O3 Li1 . . 94.22(14)
Li2 O3 H3A . . 105.0
Li1 O3 H3A . . 130.2
Li2 O3 H3B . . 127.1
Li1 O3 H3B . . 98.5
H3A O3 H3B . . 105.0
Li3 O4 Li2 . . 121.68(14)
Li3 O4 H4A . . 105.3
Li2 O4 H4A . . 102.5
Li3 O4 H4B . . 105.9
Li2 O4 H4B . . 114.8
H4A O4 H4B . . 105.0
Li4 O5 Li2 . . 80.7(2)
Li4 O5 H5A . . 105.4
Li2 O5 H5A . . 111.0
Li4 O5 H5B . . 120.8
Li2 O5 H5B . . 130.7
H5A O5 H5B . . 105.0
Li4 O6 Li2 . . 78.26(19)
Li4 O6 H6A . . 102.8
Li2 O6 H6A . . 107.9
Li4 O6 H6B . . 126.3
Li2 O6 H6B . . 132.2
H6A O6 H6B . . 105.0
Li4 O7 Li2 . . 75.9(2)
Li4 O7 H7A . . 118.8
Li2 O7 H7A . . 128.0
Li4 O7 H7B . . 107.4
Li2 O7 H7B . . 117.9
H7A O7 H7B . . 105.0
Li4 O8 H8A . . 109.9
Li4 O8 H8B . . 124.1
H8A O8 H8B . . 105.0
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
Li1 O2 . 2.130(2) y
Li1 O2 3_666 2.130(2) ?
Li1 O1 . 2.203(2) y
Li1 O1 3_666 2.203(2) ?
Li1 O3 . 2.274(2) y
Li1 O3 3_666 2.274(2) ?
Li2 O3 . 2.026(4) y
Li2 O2 . 2.127(5) y
Li2 O5 . 2.202(4) y
Li2 O4 . 2.225(5) y
Li2 O6 . 2.271(5) y
Li2 O7 . 2.319(5) y
Li3 O4 4_657 1.991(3) ?
Li3 O4 . 1.991(3) y
Li3 O1 . 2.009(4) y
Li3 O1 4_657 2.009(4) ?
Li4 O8 . 1.876(5) y
Li4 O5 . 1.957(5) y
Li4 O6 . 1.990(6) y
Li4 O7 . 2.054(6) y
As1 S2 4_556 2.1482(6) ?
As1 S2 . 2.1482(6) y
As1 S1 4_556 2.1711(6) ?
As1 S1 . 2.1711(6) y
As2 S4 4_656 2.1574(6) ?
As2 S4 . 2.1574(6) y
As2 S3 . 2.1677(6) y
As2 S3 4_656 2.1677(6) ?
O1 H1A . 0.80 ?
O1 H1B . 0.80 ?
O2 H2A . 0.80 ?
O2 H2B . 0.80 ?
O3 H3A . 0.80 ?
O3 H3B . 0.80 ?
O4 H4A . 0.80 ?
O4 H4B . 0.80 ?
O5 H5A . 0.80 ?
O5 H5B . 0.80 ?
O6 H6A . 0.80 ?
O6 H6B . 0.80 ?
O7 H7A . 0.80 ?
O7 H7B . 0.80 ?
O8 H8A . 0.80 ?
O8 H8B . 0.80 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1 H1A S1 2_665 0.80 2.49 3.262(2) 162.7
O1 H1B S4 3_666 0.80 2.51 3.287(2) 163.2
O2 H2A S1 3_566 0.80 2.76 3.531(2) 162.3
O2 H2B S2 . 0.80 2.37 3.167(2) 173.4
O3 H3A S3 3_676 0.80 2.61 3.400(2) 167.5
O3 H3B S4 . 0.80 2.39 3.190(2) 172.5
O4 H4A S1 3_566 0.80 2.51 3.240(2) 153.3
O4 H4B S3 2_575 0.80 2.42 3.207(2) 170.2
O5 H5A S1 . 0.80 2.45 3.247(2) 171.6
O5 H5B S2 3_566 0.80 2.50 3.303(2) 177.2
O6 H6A S3 . 0.80 2.57 3.354(2) 168.0
O6 H6B S4 3_676 0.80 2.54 3.307(2) 161.7
O7 H7A S1 4_556 0.80 2.49 3.244(2) 156.5
O7 H7B S3 . 0.80 2.58 3.333(2) 156.9
O8 H8A S2 1_565 0.80 2.50 3.253(2) 157.4
O8 H8B S3 4_556 0.80 2.61 3.394(2) 166.3
