#------------------------------------------------------------------------------
#$Date: 2021-08-11 05:14:50 +0300 (Wed, 11 Aug 2021) $
#$Revision: 268022 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/38/2243893.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_2243893
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                   8.4337(17)
_cell_length_b                   8.4337(17)
_cell_length_c                   30.235(6)
_cell_measurement_reflns_used    10790
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.83
_cell_volume                     1862.4(6)
_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      273(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0351
_diffrn_reflns_av_unetI/netI     0.0144
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            8584
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.552
_diffrn_reflns_theta_min         3.098
_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    0.605
_exptl_absorpt_correction_T_max  0.8655
_exptl_absorpt_correction_T_min  0.7728
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Coppens (1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.012
_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         0.188
_refine_diff_density_min         -0.331
_refine_ls_abs_structure_details
;
Flack x determined using 551 quotients
[(I⁺)-(I⁻)]/[(I⁺)+(I⁻)]
(Parsons et al.,  2013)
;
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.277
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         1159
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.276
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0188
_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)+(0.0212P)²+1.6465P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0460
_refine_ls_wR_factor_ref         0.0528
_reflns_number_gt                1141
_reflns_number_total             1159
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ru2076sup1.cif
_cod_data_source_block           Na3_Li_2SO4_6H2O-273K
_cod_original_cell_volume        1862.4(8)
_cod_database_code               2243893
_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 0.666667 0.333333 0.1535(2) 0.0180(12) Uani d 1 . .
Na Na1 0.23496(12) 0.26693(13) 0.06069(4) 0.0207(2) Uani d 1 . .
S S1 0.666667 0.333333 0.04304(3) 0.01061(16) Uani d 1 . .
S S2 0.333333 0.666667 0.12574(3) 0.01110(16) Uani d 1 . .
O O1 0.3914(2) 0.5385(2) 0.10929(5) 0.0170(3) Uani d 1 . .
O O2 0.5185(2) 0.3624(2) 0.02624(6) 0.0193(3) Uani d 1 . .
O O3 0.666667 0.333333 0.09098(10) 0.0290(7) Uani d 1 . .
O O4 0.333333 0.666667 0.17459(9) 0.0190(5) Uani d 1 . .
O O5 0.1459(2) 0.4305(2) 0.00968(6) 0.0174(3) Uani d 1 . .
H H5A 0.047(6) 0.434(5) 0.0201(13) 0.034(10) Uiso d 1 . .
H H5B 0.108(5) 0.365(5) -0.0120(13) 0.030(9) Uiso d 1 . .
O O6 -0.0306(2) 0.2082(2) 0.10174(6) 0.0205(3) Uani d 1 . .
H H6B -0.009(6) 0.314(7) 0.1031(13) 0.043(11) Uiso d 1 . .
H H6A -0.023(7) 0.188(6) 0.1279(15) 0.051(12) 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 . 18_554 110.80(19) ?
O3 Li1 O5 . 16_654 110.80(19) ?
O5 Li1 O5 18_554 16_654 108.1(2) ?
O3 Li1 O5 . 17_544 110.80(19) ?
O5 Li1 O5 18_554 17_544 108.1(2) ?
O5 Li1 O5 16_654 17_544 108.1(2) ?
O3 Li1 Na1 . 18_554 126.29(8) ?
O5 Li1 Na1 18_554 18_554 34.22(10) ?
O5 Li1 Na1 16_654 18_554 73.93(13) ?
O5 Li1 Na1 17_544 18_554 118.2(3) ?
O3 Li1 Na1 . 17_544 126.29(8) ?
O5 Li1 Na1 18_554 17_544 73.93(13) ?
O5 Li1 Na1 16_654 17_544 118.2(3) ?
O5 Li1 Na1 17_544 17_544 34.22(10) ?
Na1 Li1 Na1 18_554 17_544 88.54(12) ?
O3 Li1 Na1 . 16_654 126.29(8) ?
O5 Li1 Na1 18_554 16_654 118.2(3) ?
O5 Li1 Na1 16_654 16_654 34.22(10) ?
O5 Li1 Na1 17_544 16_654 73.93(13) ?
Na1 Li1 Na1 18_554 16_654 88.54(12) ?
Na1 Li1 Na1 17_544 16_654 88.54(12) ?
O2 Na1 O6 . 3 94.65(7) ?
O2 Na1 O6 . . 171.96(7) ?
O6 Na1 O6 3 . 87.63(9) ?
O2 Na1 O5 . . 94.28(6) ?
O6 Na1 O5 3 . 162.35(7) ?
O6 Na1 O5 . . 85.62(7) ?
O2 Na1 O1 . . 88.05(7) ?
O6 Na1 O1 3 . 104.07(6) ?
O6 Na1 O1 . . 83.92(6) ?
O5 Na1 O1 . . 91.41(6) ?
O2 Na1 O4 . 10_554 102.93(7) ?
O6 Na1 O4 3 10_554 85.39(6) ?
O6 Na1 O4 . 10_554 84.92(6) ?
O5 Na1 O4 . 10_554 77.80(6) ?
O1 Na1 O4 . 10_554 165.02(5) ?
O2 Na1 Na1 . 2 149.02(5) ?
O6 Na1 Na1 3 2 85.31(5) ?
O6 Na1 Na1 . 2 38.80(5) ?
O5 Na1 Na1 . 2 79.22(5) ?
O1 Na1 Na1 . 2 122.09(5) ?
O4 Na1 Na1 10_554 2 46.13(4) ?
O2 Na1 Na1 . 3 101.65(6) ?
O6 Na1 Na1 3 3 39.26(5) ?
O6 Na1 Na1 . 3 84.99(5) ?
O5 Na1 Na1 . 3 123.70(5) ?
O1 Na1 Na1 . 3 142.09(4) ?
O4 Na1 Na1 10_554 3 46.13(4) ?
Na1 Na1 Na1 2 3 60.0 ?
O2 Na1 Li1 . 10_564 72.56(5) ?
O6 Na1 Li1 3 10_564 167.19(6) ?
O6 Na1 Li1 . 10_564 104.94(7) ?
O5 Na1 Li1 . 10_564 26.85(5) ?
O1 Na1 Li1 . 10_564 75.37(9) ?
O4 Na1 Li1 10_554 10_564 97.99(9) ?
Na1 Na1 Li1 2 10_564 105.97(4) ?
Na1 Na1 Li1 3 10_564 142.53(8) ?
O3 S1 O2 . 2_655 110.10(8) ?
O3 S1 O2 . . 110.10(8) ?
O2 S1 O2 2_655 . 108.83(8) ?
O3 S1 O2 . 3_665 110.10(8) ?
O2 S1 O2 2_655 3_665 108.83(8) ?
O2 S1 O2 . 3_665 108.83(8) ?
O4 S2 O1 . 3_565 109.66(7) ?
O4 S2 O1 . 2_665 109.66(7) ?
O1 S2 O1 3_565 2_665 109.28(7) ?
O4 S2 O1 . . 109.66(7) ?
O1 S2 O1 3_565 . 109.28(7) ?
O1 S2 O1 2_665 . 109.28(7) ?
S2 O1 Na1 . . 131.18(9) ?
S1 O2 Na1 . . 126.18(10) ?
S1 O3 Li1 . . 180.0 ?
S2 O4 Na1 . 17_554 126.84(6) ?
S2 O4 Na1 . 16_554 126.84(6) ?
Na1 O4 Na1 17_554 16_554 87.75(8) ?
S2 O4 Na1 . 18_554 126.84(6) ?
Na1 O4 Na1 17_554 18_554 87.75(8) ?
Na1 O4 Na1 16_554 18_554 87.75(8) ?
Li1 O5 Na1 10_564 . 118.93(13) ?
Na1 O6 Na1 2 . 101.94(8) ?
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 . 1.889(7) ?
Li1 O5 18_554 1.948(3) ?
Li1 O5 16_654 1.948(3) ?
Li1 O5 17_544 1.948(3) ?
Li1 Na1 18_554 3.775(4) ?
Li1 Na1 17_544 3.775(4) ?
Li1 Na1 16_654 3.775(4) ?
Na1 O2 . 2.3509(19) ?
Na1 O6 3 2.362(2) ?
Na1 O6 . 2.386(2) ?
Na1 O5 . 2.4253(18) ?
Na1 O1 . 2.4745(18) ?
Na1 O4 10_554 2.661(2) ?
Na1 Na1 2 3.6879(18) ?
Na1 Na1 3 3.6879(18) ?
S1 O3 . 1.449(3) ?
S1 O2 2_655 1.4783(16) ?
S1 O2 . 1.4783(16) ?
S1 O2 3_665 1.4783(16) ?
S2 O4 . 1.477(3) ?
S2 O1 3_565 1.4781(16) ?
S2 O1 2_665 1.4781(16) ?
S2 O1 . 1.4781(16) ?
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
_geom_hbond_publ_flag
O6 H6A O2 16_554 0.77(5) 2.00(5) 2.764(11) 170(5) yes
O6 H6B O1 . 0.83(4) 2.15(4) 2.937(7) 157(4) yes
O5 H5B O1 12_454 0.79(4) 1.92(4) 2.694(7) 165(4) yes
O5 H5A O2 3_565 0.89(4) 1.97(4) 2.828(6) 163(3) yes

_cod_database_fobs_code 2243893
