#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/80/2238073.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_2238073
loop_
_publ_author_name
'Kamaha, Shouassi'
'Reuter, Hans'
_publ_section_title
;
 Dilithium hexahydroxidostannate(IV) dihydrate, a second monoclinic
 modification with a layer structure
;
_journal_coeditor_code           WM2733
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i25
_journal_paper_doi               10.1107/S1600536813008416
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'Li2 [Sn (O H)6], 2H2 O'
_chemical_formula_sum            'H10 Li2 O8 Sn'
_chemical_formula_weight         270.65
_chemical_name_systematic
;
Dilithium hexahydroxidostannate(IV) dihydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 118.2490(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.1028(2)
_cell_length_b                   10.4708(3)
_cell_length_c                   6.0003(2)
_cell_measurement_reflns_used    9252
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.24
_cell_measurement_theta_min      3.79
_cell_volume                     337.760(19)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics
'DIAMOND (Brandenburg, 2006) and Mercury (Macrae et al., 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'phi and omega 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  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0100
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            11484
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.79
_exptl_absorpt_coefficient_mu    3.778
_exptl_absorpt_correction_T_max  0.6813
_exptl_absorpt_correction_T_min  0.6011
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             260
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.386
_refine_ls_extinction_coef       0.0094(10)
_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   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         986
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0134
_refine_ls_R_factor_gt           0.0130
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0111P)²+0.5571P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0321
_refine_ls_wR_factor_ref         0.0323
_reflns_number_gt                964
_reflns_number_total             986
_reflns_threshold_expression     I>2sigma(I)
_iucr_refine_instructions_details
;
TITL O008_0ma in P2(1)/c
CELL 0.71073   6.1028  10.4708   6.0003  90.000 118.249  90.000
ZERR       2   0.0002   0.0003   0.0002   0.000   0.001   0.000
LATT  1
SYMM -X, 0.5+Y, 0.5-Z
SFAC LI H O SN
UNIT 4 20 16 2
OMIT -3 60
OMIT 0 4 0
TEMP -173
ACTA
HTAB
HTAB O1 O4_$5
HTAB O2 O1_$4
HTAB O3 O4_$6
HTAB O4 O3_$7
HTAB O4 O2_$8
EQIV $5 -x+1, -y+1, -z
EQIV $6 -x+1, y+1/2, -z+1/2
EQIV $7 -x+1, -y+1, -z+1
EQIV $8 x+1, y, z
EQIV $4 -x+1, y-1/2, -z+1/2
L.S. 10
BOND $H
FMAP 2
PLAN 5
Size  0.15  0.14  0.11
WGHT    0.011100    0.557100
EXTI    0.009377
FVAR       0.93521   0.04515
MOLE   1
SN1   4    0.500000    0.500000    0.500000    10.50000    0.00660    0.00674 =
         0.00670    0.00009    0.00314    0.00001
O1    3    0.592426    0.613501    0.277287    11.00000    0.00911    0.01031 =
         0.00811    0.00070    0.00392   -0.00086
AFIX   3
H1    2    0.434435    0.620774    0.127751    11.00000   21.00000
AFIX   0
O2    3    0.293037    0.382275    0.194422    11.00000    0.00956    0.00882 =
         0.00841   -0.00034    0.00349    0.00047
AFIX   3
H2    2    0.343807    0.294679    0.206118    11.00000   21.00000
AFIX   0
O3    3    0.178006    0.604085    0.392600    11.00000    0.00855    0.00746 =
         0.01066    0.00058    0.00467    0.00065
AFIX   3
H3    2    0.196514    0.692957    0.365867    11.00000   21.00000
AFIX   0
LI1   1    0.828404    0.565707    0.156112    11.00000    0.01356    0.01211 =
         0.01167   -0.00062    0.00628   -0.00009
O4    3    0.849741    0.372290    0.179502    11.00000    0.00942    0.01158 =
         0.00962   -0.00043    0.00482   -0.00025
AFIX   3
H41   2    0.864336    0.377109    0.345762    11.00000   21.00000
H42   2    1.017559    0.365102    0.207059    11.00000   21.00000
HKLF 4
;
_cod_data_source_file            wm2733.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2238073
_cod_database_fobs_code          2238073
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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
Sn Sn1 0.5000 0.5000 0.5000 0.00669(7) Uani d S 1 2
O O1 0.5924(2) 0.61350(11) 0.2773(2) 0.0092(2) Uani d . 1 1
H H1 0.4344 0.6208 0.1278 0.045(4) Uiso d R 1 1
O O2 0.2930(2) 0.38228(11) 0.1944(2) 0.0092(2) Uani d . 1 1
H H2 0.3438 0.2947 0.2061 0.045(4) Uiso d R 1 1
O O3 0.1780(2) 0.60408(11) 0.3926(2) 0.0088(2) Uani d . 1 1
H H3 0.1965 0.6930 0.3659 0.045(4) Uiso d R 1 1
Li Li1 0.8284(5) 0.5657(3) 0.1561(6) 0.0123(5) Uani d . 1 1
O O4 0.8497(2) 0.37229(11) 0.1795(2) 0.0101(2) Uani d . 1 1
H H41 0.8643 0.3771 0.3458 0.045(4) Uiso d R 1 1
H H42 1.0175 0.3651 0.2071 0.045(4) Uiso d R 1 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Sn1 0.00660(8) 0.00674(9) 0.00670(9) 0.00001(4) 0.00314(6) 0.00009(5)
O1 0.0091(5) 0.0103(5) 0.0081(5) -0.0009(4) 0.0039(4) 0.0007(4)
O2 0.0096(5) 0.0088(5) 0.0084(5) 0.0005(4) 0.0035(4) -0.0003(4)
O3 0.0085(5) 0.0075(5) 0.0107(5) 0.0006(4) 0.0047(4) 0.0006(4)
Li1 0.0136(12) 0.0121(13) 0.0117(13) -0.0001(10) 0.0063(11) -0.0006(10)
O4 0.0094(5) 0.0116(5) 0.0096(5) -0.0002(4) 0.0048(4) -0.0004(4)
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'
H H 0.0000 0.0000 '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'
Sn Sn -0.6537 1.4246 '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
O1 Sn1 O1 3_666 . 180.0
O1 Sn1 O3 3_666 3_666 90.31(4)
O1 Sn1 O3 . 3_666 89.69(4)
O1 Sn1 O3 3_666 . 89.69(4)
O1 Sn1 O3 . . 90.31(4)
O3 Sn1 O3 3_666 . 180.0
O1 Sn1 O2 3_666 3_666 90.49(4)
O1 Sn1 O2 . 3_666 89.51(4)
O3 Sn1 O2 3_666 3_666 86.92(4)
O3 Sn1 O2 . 3_666 93.08(4)
O1 Sn1 O2 3_666 . 89.51(4)
O1 Sn1 O2 . . 90.49(4)
O3 Sn1 O2 3_666 . 93.08(4)
O3 Sn1 O2 . . 86.92(4)
O2 Sn1 O2 3_666 . 180.0
Li1 O1 Sn1 . . 124.68(10)
Li1 O1 H1 . . 105.2
Sn1 O1 H1 . . 101.0
Li1 O2 Sn1 3_665 . 123.42(11)
Li1 O2 H2 3_665 . 106.9
Sn1 O2 H2 . . 117.6
Li1 O3 Sn1 1_455 . 131.67(10)
Li1 O3 H3 1_455 . 104.5
Sn1 O3 H3 . . 113.2
O2 Li1 O1 3_665 . 110.99(15)
O2 Li1 O3 3_665 1_655 116.79(15)
O1 Li1 O3 . 1_655 114.65(15)
O2 Li1 O4 3_665 . 109.44(15)
O1 Li1 O4 . . 105.27(14)
O3 Li1 O4 1_655 . 98.16(13)
Li1 O4 H41 . . 89.5
Li1 O4 H42 . . 96.8
H41 O4 H42 . . 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
Sn1 O1 3_666 2.0567(11) ?
Sn1 O1 . 2.0567(11) yes
Sn1 O3 3_666 2.0654(11) ?
Sn1 O3 . 2.0654(11) yes
Sn1 O2 3_666 2.0699(11) ?
Sn1 O2 . 2.0699(11) yes
O1 Li1 . 1.961(3) yes
O1 H1 . 0.9600 ?
O2 Li1 3_665 1.948(3) yes
O2 H2 . 0.9600 ?
O3 Li1 1_455 1.965(3) yes
O3 H3 . 0.9600 ?
Li1 O2 3_665 1.948(3) ?
Li1 O3 1_655 1.965(3) ?
Li1 O4 . 2.030(3) yes
O4 H41 . 0.9600 ?
O4 H42 . 0.9600 ?
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 H1 O4 3_665 0.96 1.84 2.7955(16) 173.2
O2 H2 O1 2_645 0.96 1.93 2.8853(16) 173.4
O3 H3 O4 2_655 0.96 1.90 2.8343(16) 164.0
O4 H41 O3 3_666 0.96 1.72 2.6634(16) 167.2
O4 H42 O2 1_655 0.96 1.73 2.6662(16) 164.8
