#------------------------------------------------------------------------------
#$Date: 2021-08-11 05:14:50 +0300 (Wed, 11 Aug 2021) $
#$Revision: 268022 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/38/2243891.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_2243891
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                   8.4006(19)
_cell_length_b                   8.4006(19)
_cell_length_c                   30.111(9)
_cell_measurement_reflns_used    7724
_cell_measurement_temperature    180
_cell_measurement_theta_max      30.01
_cell_measurement_theta_min      2.83
_cell_volume                     1840.2(8)
_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      180(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.959
_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  0.0350
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_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            4345
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.465
_diffrn_reflns_theta_min         3.110
_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    0.612
_exptl_absorpt_correction_T_max  0.9408
_exptl_absorpt_correction_T_min  0.6823
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Coppens (1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.036
_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         0.227
_refine_diff_density_min         -0.327
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower
;
_refine_ls_abs_structure_Flack   -0.08(10)
_refine_ls_extinction_coef       0.055(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   1.176
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1088
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0214
_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)+(0.0413P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0534
_reflns_number_gt                1087
_reflns_number_total             1088
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ru2076sup1.cif
_cod_data_source_block           Na3_Li_2SO4_6H2O-180K
_cod_original_cell_volume        1840.3(10)
_cod_database_code               2243891
_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'
'-y, -x, z+1/2'
'-x+y, -x, z'
'x, x-y, z+1/2'
'-x+y, y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, -x+1/3, z+1/3'
'x+2/3, x-y+1/3, z+5/6'
'-x+y+2/3, 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'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, -x+2/3, z+2/3'
'x+1/3, x-y+2/3, z+7/6'
'-x+y+1/3, 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 0.15397(15) 0.0112(7) Uani d 1 . .
Na Na1 0.23455(8) 0.26585(8) 0.06065(3) 0.0123(2) Uani d 1 . .
S S1 0.666667 0.333333 0.04314(2) 0.00567(18) Uani d 1 . .
S S2 0.333333 0.666667 0.12563(2) 0.00580(18) Uani d 1 . .
O O1 0.39232(16) 0.53835(14) 0.10903(4) 0.0101(2) Uani d 1 . .
O O2 0.51801(14) 0.36299(14) 0.02615(4) 0.0116(2) Uani d 1 . .
O O3 0.666667 0.333333 0.09124(10) 0.0182(6) Uani d 1 . .
O O4 0.333333 0.666667 0.17460(9) 0.0113(5) Uani d 1 . .
O O5 0.14543(15) 0.42931(14) 0.00995(4) 0.0107(2) Uani d 1 . .
H H5A 0.057(4) 0.431(3) 0.0205(10) 0.019(6) Uiso d 1 . .
H H5B 0.106(4) 0.359(4) -0.0106(11) 0.021(5) Uiso d 1 . .
O O6 -0.02970(15) 0.20921(15) 0.10179(4) 0.0125(2) Uani d 1 . .
H H6B -0.011(4) 0.311(5) 0.1015(12) 0.029(8) Uiso d 1 . .
H H6A -0.023(4) 0.189(4) 0.1275(11) 0.019(6) 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 . 17_554 110.52(13) ?
O3 Li1 O5 . 15_654 110.52(13) ?
O5 Li1 O5 17_554 15_654 108.41(13) ?
O3 Li1 O5 . 18_544 110.52(13) ?
O5 Li1 O5 17_554 18_544 108.41(13) ?
O5 Li1 O5 15_654 18_544 108.40(13) ?
O3 Li1 Na1 . 15_654 126.01(6) ?
O5 Li1 Na1 17_554 15_654 118.70(17) ?
O5 Li1 Na1 15_654 15_654 34.19(6) ?
O5 Li1 Na1 18_544 15_654 74.26(9) ?
O3 Li1 Na1 . 18_544 126.01(6) ?
O5 Li1 Na1 17_554 18_544 74.26(9) ?
O5 Li1 Na1 15_654 18_544 118.70(17) ?
O5 Li1 Na1 18_544 18_544 34.19(6) ?
Na1 Li1 Na1 15_654 18_544 88.94(8) ?
O3 Li1 Na1 . 17_554 126.01(6) ?
O5 Li1 Na1 17_554 17_554 34.19(6) ?
O5 Li1 Na1 15_654 17_554 74.27(9) ?
O5 Li1 Na1 18_544 17_554 118.70(17) ?
Na1 Li1 Na1 15_654 17_554 88.94(8) ?
Na1 Li1 Na1 18_544 17_554 88.94(8) ?
O2 Na1 O6 . 4 94.92(4) ?
O2 Na1 O6 . . 171.37(5) ?
O6 Na1 O6 4 . 87.90(6) ?
O2 Na1 O5 . . 94.13(4) ?
O6 Na1 O5 4 . 162.50(5) ?
O6 Na1 O5 . . 85.35(5) ?
O2 Na1 O1 . . 87.57(4) ?
O6 Na1 O1 4 . 104.10(4) ?
O6 Na1 O1 . . 83.82(4) ?
O5 Na1 O1 . . 91.21(4) ?
O2 Na1 O4 . 9_554 103.11(6) ?
O6 Na1 O4 4 9_554 85.59(5) ?
O6 Na1 O4 . 9_554 85.22(5) ?
O5 Na1 O4 . 9_554 77.78(5) ?
O1 Na1 O4 . 9_554 165.06(3) ?
O2 Na1 Na1 . 4 102.10(4) ?
O6 Na1 Na1 4 4 39.43(3) ?
O6 Na1 Na1 . 4 85.26(3) ?
O5 Na1 Na1 . 4 123.70(3) ?
O1 Na1 Na1 . 4 142.29(3) ?
O4 Na1 Na1 9_554 4 46.17(4) ?
O2 Na1 Na1 . 2 149.23(3) ?
O6 Na1 Na1 4 2 85.51(3) ?
O6 Na1 Na1 . 2 39.06(3) ?
O5 Na1 Na1 . 2 79.08(3) ?
O1 Na1 Na1 . 2 122.25(3) ?
O4 Na1 Na1 9_554 2 46.17(4) ?
Na1 Na1 Na1 4 2 60.0 ?
O2 Na1 Li1 . 9_564 72.31(3) ?
O6 Na1 Li1 4 9_564 167.18(4) ?
O6 Na1 Li1 . 9_564 104.59(4) ?
O5 Na1 Li1 . 9_564 26.99(3) ?
O1 Na1 Li1 . 9_564 74.93(6) ?
O4 Na1 Li1 9_554 9_564 98.14(7) ?
Na1 Na1 Li1 4 9_564 142.78(5) ?
Na1 Na1 Li1 2 9_564 105.95(2) ?
O3 S1 O2 . . 110.20(6) ?
O3 S1 O2 . 2_655 110.21(6) ?
O2 S1 O2 . 2_655 108.73(6) ?
O3 S1 O2 . 4_665 110.21(6) ?
O2 S1 O2 . 4_665 108.73(6) ?
O2 S1 O2 2_655 4_665 108.73(6) ?
O4 S2 O1 . . 109.74(6) ?
O4 S2 O1 . 4_565 109.74(6) ?
O1 S2 O1 . 4_565 109.20(6) ?
O4 S2 O1 . 2_665 109.74(6) ?
O1 S2 O1 . 2_665 109.20(6) ?
O1 S2 O1 4_565 2_665 109.20(6) ?
S2 O1 Na1 . . 130.92(7) ?
S1 O2 Na1 . . 125.78(7) ?
S1 O3 Li1 . . 180.0 ?
S2 O4 Na1 . 18_554 126.90(6) ?
S2 O4 Na1 . 15_554 126.90(6) ?
Na1 O4 Na1 18_554 15_554 87.67(9) ?
S2 O4 Na1 . 17_554 126.90(6) ?
Na1 O4 Na1 18_554 17_554 87.67(9) ?
Na1 O4 Na1 15_554 17_554 87.67(9) ?
Li1 O5 Na1 9_564 . 118.83(9) ?
Na1 O6 Na1 2 . 101.51(5) ?
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(6) ?
Li1 O5 17_554 1.9454(19) ?
Li1 O5 15_654 1.9455(19) ?
Li1 O5 18_544 1.9455(19) ?
Li1 Na1 15_654 3.756(3) ?
Li1 Na1 18_544 3.756(3) ?
Li1 Na1 17_554 3.756(3) ?
Na1 O2 . 2.3393(12) ?
Na1 O6 4 2.3546(13) ?
Na1 O6 . 2.3734(13) ?
Na1 O5 . 2.4093(13) ?
Na1 O1 . 2.4669(12) ?
Na1 O4 9_554 2.644(2) ?
Na1 Na1 4 3.6617(13) ?
Na1 Na1 2 3.6618(13) ?
S1 O3 . 1.448(3) ?
S1 O2 . 1.4813(11) ?
S1 O2 2_655 1.4814(11) ?
S1 O2 4_665 1.4814(11) ?
S2 O4 . 1.474(3) ?
S2 O1 . 1.4804(11) ?
S2 O1 4_565 1.4804(11) ?
S2 O1 2_665 1.4804(11) ?

_cod_database_fobs_code 2243891
