#------------------------------------------------------------------------------
#$Date: 2021-08-11 05:14:50 +0300 (Wed, 11 Aug 2021) $
#$Revision: 268022 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/38/2243890.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_2243890
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_iupac          'Li Na3 (S O4)2, 6H2 O'
_chemical_formula_moiety         '3(Na +), Li +, 2(O4 S 2-), 6(H2 O)'
_chemical_formula_sum            'H12 Li Na3 O14 S2'
_chemical_formula_weight         376.13
_chemical_name_common            'Sodium lithium sulfate hexahydrate'
_chemical_name_systematic
;
Lithium trisodium bis(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                   8.3876(13)
_cell_length_b                   8.3876(13)
_cell_length_c                   30.048(7)
_cell_measurement_reflns_used    2749
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      25.00
_cell_volume                     1830.7(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      90(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.987
_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  0.0273
_diffrn_reflns_av_unetI/netI     0.0096
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            12154
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.144
_diffrn_reflns_theta_min         3.123
_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    0.619
_exptl_absorpt_correction_T_max  0.9450
_exptl_absorpt_correction_T_min  0.9244
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Coppens (1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.047
_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         0.158
_refine_diff_density_min         -0.182
_refine_ls_abs_structure_details
;
Flack x determined using 539 quotients
[(I⁺)-(I⁻)]/[(I⁺)+(I⁻)]
(Parsons et al.,  2013)
;
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_coef       0.0037(7)
_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   1.144
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1089
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0131
_refine_ls_R_factor_gt           0.0131
_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)+(0.0238P)²+0.6042P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0360
_refine_ls_wR_factor_ref         0.0360
_reflns_number_gt                1089
_reflns_number_total             1089
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ru2076sup1.cif
_cod_data_source_block           Na3_Li_2SO4_6H2O-90K
_cod_original_cell_volume        1830.7(7)
_cod_database_code               2243890
_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 0.15432(13) 0.0085(7) Uani d 1 . .
Na Na1 0.23426(7) 0.26504(7) 0.06063(2) 0.00705(14) Uani d 1 . .
S S1 0.666667 0.333333 0.04323(2) 0.00332(12) Uani d 1 . .
S S2 0.333333 0.666667 0.12552(2) 0.00325(12) Uani d 1 . .
O O1 0.39254(13) 0.53800(12) 0.10892(3) 0.00609(18) Uani d 1 . .
O O2 0.51766(12) 0.36335(12) 0.02615(3) 0.00667(18) Uani d 1 . .
O O3 0.666667 0.333333 0.09154(6) 0.0095(4) Uani d 1 . .
O O4 0.333333 0.666667 0.17470(6) 0.0067(3) Uani d 1 . .
O O5 0.14513(13) 0.42897(12) 0.01016(3) 0.00656(17) Uani d 1 . .
H H5A 0.053(2) 0.429(3) 0.0194(7) 0.016(5) Uiso d 1 . .
H H5B 0.106(3) 0.363(3) -0.0120(6) 0.020(5) Uiso d 1 . .
O O6 -0.02932(13) 0.20979(13) 0.10180(3) 0.00744(19) Uani d 1 . .
H H6B -0.007(3) 0.316(2) 0.1019(8) 0.017(5) Uiso d 1 . .
H H6A -0.022(3) 0.190(3) 0.1279(5) 0.017(5) Uiso d 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'
Na Na 0.0362 0.0249 '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_554 110.37(11) ?
O3 Li1 O5 . 16_654 110.36(11) ?
O5 Li1 O5 18_554 16_654 108.56(12) ?
O3 Li1 O5 . 17_544 110.36(11) ?
O5 Li1 O5 18_554 17_544 108.56(12) ?
O5 Li1 O5 16_654 17_544 108.56(12) ?
O3 Li1 Na1 . 18_554 125.81(5) ?
O5 Li1 Na1 18_554 18_554 34.21(6) ?
O5 Li1 Na1 16_654 18_554 74.41(8) ?
O5 Li1 Na1 17_544 18_554 119.02(15) ?
O3 Li1 Na1 . 17_544 125.81(5) ?
O5 Li1 Na1 18_554 17_544 74.40(8) ?
O5 Li1 Na1 16_654 17_544 119.01(15) ?
O5 Li1 Na1 17_544 17_544 34.21(6) ?
Na1 Li1 Na1 18_554 17_544 89.23(7) ?
O3 Li1 Na1 . 16_654 125.81(5) ?
O5 Li1 Na1 18_554 16_654 119.02(15) ?
O5 Li1 Na1 16_654 16_654 34.21(6) ?
O5 Li1 Na1 17_544 16_654 74.40(8) ?
Na1 Li1 Na1 18_554 16_654 89.23(7) ?
Na1 Li1 Na1 17_544 16_654 89.23(7) ?
O2 Na1 O6 . 3 95.05(4) ?
O2 Na1 O6 . . 170.96(4) ?
O6 Na1 O6 3 . 88.14(5) ?
O2 Na1 O5 . . 94.07(4) ?
O6 Na1 O5 3 . 162.69(4) ?
O6 Na1 O5 . . 85.10(4) ?
O2 Na1 O1 . . 87.29(4) ?
O6 Na1 O1 3 . 104.11(4) ?
O6 Na1 O1 . . 83.73(3) ?
O5 Na1 O1 . . 90.99(3) ?
O2 Na1 O4 . 10_554 103.31(4) ?
O6 Na1 O4 3 10_554 85.71(4) ?
O6 Na1 O4 . 10_554 85.34(4) ?
O5 Na1 O4 . 10_554 77.88(4) ?
O1 Na1 O4 . 10_554 165.02(3) ?
O2 Na1 Na1 . 2 149.40(3) ?
O6 Na1 Na1 3 2 85.68(3) ?
O6 Na1 Na1 . 2 39.18(3) ?
O5 Na1 Na1 . 2 79.01(3) ?
O1 Na1 Na1 . 2 122.28(3) ?
O4 Na1 Na1 10_554 2 46.16(3) ?
O2 Na1 Na1 . 3 102.41(3) ?
O6 Na1 Na1 3 3 39.55(3) ?
O6 Na1 Na1 . 3 85.42(3) ?
O5 Na1 Na1 . 3 123.78(3) ?
O1 Na1 Na1 . 3 142.40(2) ?
O4 Na1 Na1 10_554 3 46.16(3) ?
Na1 Na1 Na1 2 3 60.0 ?
O2 Na1 Li1 . 10_564 72.17(3) ?
O6 Na1 Li1 3 10_564 167.14(3) ?
O6 Na1 Li1 . 10_564 104.31(4) ?
O5 Na1 Li1 . 10_564 27.04(3) ?
O1 Na1 Li1 . 10_564 74.64(5) ?
O4 Na1 Li1 10_554 10_564 98.29(5) ?
Na1 Na1 Li1 2 10_564 105.94(2) ?
Na1 Na1 Li1 3 10_564 142.95(5) ?
O3 S1 O2 . 3_665 110.23(4) ?
O3 S1 O2 . . 110.23(4) ?
O2 S1 O2 3_665 . 108.71(5) ?
O3 S1 O2 . 2_655 110.23(4) ?
O2 S1 O2 3_665 2_655 108.70(5) ?
O2 S1 O2 . 2_655 108.71(5) ?
O4 S2 O1 . 2_665 109.66(4) ?
O4 S2 O1 . . 109.66(4) ?
O1 S2 O1 2_665 . 109.28(4) ?
O4 S2 O1 . 3_565 109.66(4) ?
O1 S2 O1 2_665 3_565 109.28(4) ?
O1 S2 O1 . 3_565 109.28(4) ?
S2 O1 Na1 . . 130.83(5) ?
S1 O2 Na1 . . 125.59(6) ?
S1 O3 Li1 . . 180.0 ?
S2 O4 Na1 . 17_554 126.89(4) ?
S2 O4 Na1 . 16_554 126.89(4) ?
Na1 O4 Na1 17_554 16_554 87.68(5) ?
S2 O4 Na1 . 18_554 126.89(4) ?
Na1 O4 Na1 17_554 18_554 87.68(5) ?
Na1 O4 Na1 16_554 18_554 87.68(5) ?
Li1 O5 Na1 10_564 . 118.75(8) ?
Na1 O6 Na1 2 . 101.27(4) ?
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 . 1.886(4) ?
Li1 O5 18_554 1.9434(17) ?
Li1 O5 16_654 1.9435(17) ?
Li1 O5 17_544 1.9435(17) ?
Li1 Na1 18_554 3.748(2) ?
Li1 Na1 17_544 3.748(2) ?
Li1 Na1 16_654 3.748(2) ?
Na1 O2 . 2.3331(10) ?
Na1 O6 3 2.3498(11) ?
Na1 O6 . 2.3682(11) ?
Na1 O5 . 2.4036(11) ?
Na1 O1 . 2.4638(10) ?
Na1 O4 10_554 2.6330(14) ?
Na1 Na1 2 3.6475(10) ?
Na1 Na1 3 3.6475(10) ?
S1 O3 . 1.4515(17) ?
S1 O2 3_665 1.4844(9) ?
S1 O2 . 1.4844(9) ?
S1 O2 2_655 1.4844(9) ?
S2 O4 . 1.4777(17) ?
S2 O1 2_665 1.4818(9) ?
S2 O1 . 1.4818(9) ?
S2 O1 3_565 1.4818(9) ?

_cod_database_fobs_code 2243890
