#------------------------------------------------------------------------------
#$Date: 2021-08-11 05:14:50 +0300 (Wed, 11 Aug 2021) $
#$Revision: 268022 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/38/2243892.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_2243892
loop_
_publ_author_name
'Schmidt, Horst'
'Paschke, Iris'
'Voigt, Wolfgang'
_publ_section_title
;
 LiNa₃(SO₄)₂·6H₂O: a lithium double salt causing trouble in
 the industrial conversion of Li₂SO₄ into LiOH
;
_journal_coeditor_code           RU2076
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989021008057
_journal_volume                  77
_journal_year                    2021
_chemical_formula_moiety         '3(Na) Li 2(SO4) 6(H2O)'
_chemical_formula_sum            'H12 Li Na3 O14 S2'
_chemical_formula_weight         376.13
_chemical_name_systematic        Sodium-Lithium-Sulfate-Hexahydrate
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   8.426(2)
_cell_length_b                   8.426(2)
_cell_length_c                   30.197(4)
_cell_measurement_reflns_used    4304
_cell_measurement_temperature    260(2)
_cell_measurement_theta_max      21.00
_cell_measurement_theta_min      2.59
_cell_volume                     1856.7(7)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2015)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2015)
;
_computing_data_reduction
;
X-RED (Stoe & Cie, 2015)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2017)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      260(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            5068
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.176
_diffrn_reflns_theta_min         3.101
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_T_max  0.9382
_exptl_absorpt_correction_T_min  0.8637
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Coppens (1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.018
_exptl_crystal_description       needle
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.142
_refine_diff_density_min         -0.198
_refine_ls_abs_structure_details
;
Flack x determined using 437 quotients
[(I⁺)-(I⁻)]/[(I⁺)+(I⁻)]
(Parsons et al.,  2013)
;
_refine_ls_abs_structure_Flack   -0.04(6)
_refine_ls_extinction_coef       0.0031(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018/3 (Sheldrick 2015)
;
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         915
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0174
_refine_ls_R_factor_gt           0.0168
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0254P)²+0.5038P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0420
_refine_ls_wR_factor_ref         0.0426
_reflns_number_gt                906
_reflns_number_total             915
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ru2076sup1.cif
_cod_data_source_block           Na3_Li_2SO4_6H2O-260K
_cod_original_cell_volume        1856.6(10)
_cod_database_code               2243892
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Li Li1 0.333333 0.666667 0.8465(2) 0.0164(12) Uani d 1 . .
Na Na1 0.76508(11) 0.73321(11) 0.93934(4) 0.0204(2) Uani d 1 . .
S S1 0.333333 0.666667 0.95693(2) 0.01085(19) Uani d 1 . .
S S2 0.666667 0.333333 0.87429(2) 0.01117(19) Uani d 1 . .
O O1 0.6085(2) 0.46143(19) 0.89076(5) 0.0167(3) Uani d 1 . .
O O2 0.4815(2) 0.6374(2) 0.97377(5) 0.0188(3) Uani d 1 . .
O O3 0.333333 0.666667 0.90900(9) 0.0282(7) Uani d 1 . .
O O4 0.666667 0.333333 0.82539(8) 0.0181(6) Uani d 1 . .
O O5 0.8541(2) 0.56971(19) 0.99018(5) 0.0172(3) Uani d 1 . .
H H5A 0.949(5) 0.569(4) 0.9803(10) 0.027(8) Uiso d 1 . .
H H5B 0.890(4) 0.630(4) 1.0103(11) 0.027(8) Uiso d 1 . .
O O6 1.0306(2) 0.7917(2) 0.89835(6) 0.0200(3) Uani d 1 . .
H H6B 1.014(5) 0.690(6) 0.8961(11) 0.045(10) Uiso d 1 . .
H H6A 1.017(5) 0.807(5) 0.8738(12) 0.044(10) Uiso d 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 '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
_geom_angle_publ_flag
O3 Li1 O5 . 11_554 110.85(17) ?
O3 Li1 O5 . 10_564 110.85(17) ?
O5 Li1 O5 11_554 10_564 108.06(18) ?
O3 Li1 O5 . 12_454 110.85(17) ?
O5 Li1 O5 11_554 12_454 108.06(18) ?
O5 Li1 O5 10_564 12_454 108.06(18) ?
O3 Li1 Na1 . 12_454 126.24(8) ?
O5 Li1 Na1 11_554 12_454 118.2(2) ?
O5 Li1 Na1 10_564 12_454 73.96(12) ?
O5 Li1 Na1 12_454 12_454 34.14(9) ?
O3 Li1 Na1 . 11_554 126.24(8) ?
O5 Li1 Na1 11_554 11_554 34.14(9) ?
O5 Li1 Na1 10_564 11_554 118.2(2) ?
O5 Li1 Na1 12_454 11_554 73.96(12) ?
Na1 Li1 Na1 12_454 11_554 88.61(11) ?
O3 Li1 Na1 . 10_564 126.24(8) ?
O5 Li1 Na1 11_554 10_564 73.96(12) ?
O5 Li1 Na1 10_564 10_564 34.14(9) ?
O5 Li1 Na1 12_454 10_564 118.2(2) ?
Na1 Li1 Na1 12_454 10_564 88.61(11) ?
Na1 Li1 Na1 11_554 10_564 88.61(11) ?
O2 Na1 O6 . 3_675 94.66(6) ?
O2 Na1 O6 . . 171.88(7) ?
O6 Na1 O6 3_675 . 87.76(9) ?
O2 Na1 O5 . . 94.30(6) ?
O6 Na1 O5 3_675 . 162.39(7) ?
O6 Na1 O5 . . 85.48(7) ?
O2 Na1 O1 . . 87.96(6) ?
O6 Na1 O1 3_675 . 104.13(6) ?
O6 Na1 O1 . . 83.93(6) ?
O5 Na1 O1 . . 91.31(6) ?
O2 Na1 O4 . 16_664 103.01(6) ?
O6 Na1 O4 3_675 16_664 85.37(6) ?
O6 Na1 O4 . 16_664 84.90(6) ?
O5 Na1 O4 . 16_664 77.85(6) ?
O1 Na1 O4 . 16_664 165.00(5) ?
O2 Na1 Na1 . 3_675 101.74(5) ?
O6 Na1 Na1 3_675 3_675 39.26(5) ?
O6 Na1 Na1 . 3_675 85.03(4) ?
O5 Na1 Na1 . 3_675 123.73(5) ?
O1 Na1 Na1 . 3_675 142.14(4) ?
O4 Na1 Na1 16_664 3_675 46.11(4) ?
O2 Na1 Na1 . 2_765 149.08(5) ?
O6 Na1 Na1 3_675 2_765 85.36(5) ?
O6 Na1 Na1 . 2_765 38.79(4) ?
O5 Na1 Na1 . 2_765 79.18(5) ?
O1 Na1 Na1 . 2_765 122.10(5) ?
O4 Na1 Na1 16_664 2_765 46.11(4) ?
Na1 Na1 Na1 3_675 2_765 60.0000(10) ?
O2 Na1 Li1 . 16_654 72.52(5) ?
O6 Na1 Li1 3_675 16_654 167.16(6) ?
O6 Na1 Li1 . 16_654 104.84(6) ?
O5 Na1 Li1 . 16_654 26.88(5) ?
O1 Na1 Li1 . 16_654 75.28(8) ?
O4 Na1 Li1 16_664 16_654 98.04(8) ?
Na1 Na1 Li1 3_675 16_654 142.58(7) ?
Na1 Na1 Li1 2_765 16_654 105.97(3) ?
O3 S1 O2 . . 110.11(7) ?
O3 S1 O2 . 2_665 110.12(7) ?
O2 S1 O2 . 2_665 108.82(7) ?
O3 S1 O2 . 3_565 110.12(7) ?
O2 S1 O2 . 3_565 108.82(7) ?
O2 S1 O2 2_665 3_565 108.82(7) ?
O4 S2 O1 . 3_665 109.68(7) ?
O4 S2 O1 . 2_655 109.68(7) ?
O1 S2 O1 3_665 2_655 109.26(7) ?
O4 S2 O1 . . 109.69(6) ?
O1 S2 O1 3_665 . 109.26(7) ?
O1 S2 O1 2_655 . 109.26(7) ?
S2 O1 Na1 . . 131.17(9) ?
S1 O2 Na1 . . 126.11(9) ?
S1 O3 Li1 . . 180.0 ?
S2 O4 Na1 . 11_544 126.82(5) ?
S2 O4 Na1 . 10_664 126.82(5) ?
Na1 O4 Na1 11_544 10_664 87.78(7) ?
S2 O4 Na1 . 12_454 126.82(5) ?
Na1 O4 Na1 11_544 12_454 87.78(7) ?
Na1 O4 Na1 10_664 12_454 87.78(7) ?
Li1 O5 Na1 16_654 . 118.98(12) ?
Na1 O6 Na1 2_765 . 101.95(7) ?
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 O3 . 1.888(6) ?
Li1 O5 11_554 1.948(3) ?
Li1 O5 10_564 1.948(3) ?
Li1 O5 12_454 1.948(3) ?
Li1 Na1 12_454 3.770(4) ?
Li1 Na1 11_554 3.770(4) ?
Li1 Na1 10_564 3.770(4) ?
Na1 O2 . 2.3478(17) ?
Na1 O6 3_675 2.3584(18) ?
Na1 O6 . 2.3825(19) ?
Na1 O5 . 2.4188(16) ?
Na1 O1 . 2.4727(17) ?
Na1 O4 16_664 2.656(2) ?
Na1 Na1 3_675 3.6830(17) ?
Na1 Na1 2_765 3.6830(17) ?
S1 O3 . 1.447(3) ?
S1 O2 . 1.4788(15) ?
S1 O2 2_665 1.4788(15) ?
S1 O2 3_565 1.4788(15) ?
S2 O4 . 1.477(2) ?
S2 O1 3_665 1.4769(14) ?
S2 O1 2_655 1.4769(14) ?
S2 O1 . 1.4769(14) ?

_cod_database_fobs_code 2243892
