#------------------------------------------------------------------------------
#$Date: 2025-08-23 00:35:05 +0200 (Sat 23 de Aug de 2025) $
#$Revision: 301870 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/23/7242393.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7242393
loop_
_publ_author_name
'Liu, Kaitong'
'Han, Jian'
'Huang, Junben'
'Wei, Zhonglei'
'Yang, Zhihua'
'Pan, Shilie'
_publ_section_title
;
 SrTi(IO3)6·2H2O and SrSn(IO3)6: distinct arrangements of lone pair
 electrons leading to large birefringences
;
_journal_issue                   17
_journal_name_full               'RSC Advances'
_journal_page_first              10309
_journal_page_last               10315
_journal_paper_doi               10.1039/D0RA10726C
_journal_volume                  11
_journal_year                    2021
_chemical_formula_sum            'H6 I6 O20 Ti'
_chemical_formula_weight         1135.35
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2020-07-06 deposited with the CCDC.	2021-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   11.31(3)
_cell_length_b                   11.31(3)
_cell_length_c                   11.36(3)
_cell_measurement_reflns_used    555
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.94
_cell_measurement_theta_min      2.76
_cell_volume                     1258(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2567
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.189
_diffrn_reflns_theta_min         2.746
_exptl_absorpt_coefficient_mu    11.657
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   face-index
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1518
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.219
_refine_ls_extinction_coef       0.00038(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         628
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0259
_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)+(0.0067P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0360
_refine_ls_wR_factor_ref         0.0382
_reflns_Friedel_coverage         0.000
_reflns_number_gt                512
_reflns_number_total             628
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ra10726c2.cif
_cod_data_source_block           111
_cod_original_cell_volume        1258(7)
_cod_database_code               7242393
_shelx_shelxl_version_number     2016/6
_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. 
;
_shelx_res_file
; 
TITL ASDFA in R-3 
    111.res 
    created by SHELXL-2016/6 at 17:58:36 on 30-May-2020 
CELL 0.71073  11.30720  11.30720  11.36420  90.0000  90.0000 120.0000 
ZERR   3.00   0.02720   0.02720   0.02810   0.0000   0.0000   0.0000 
LATT 3 
SYMM -Y, X-Y, Z 
SYMM -X+Y, -X, Z 
SFAC O  H  Ti I 
UNIT 60  18  3  18 
OMIT -1 2 0 
L.S. 10 
ACTA 
BOND 
FMAP 2 
PLAN 10 
DFIX 0.84 0.01 O1 H1 
TEMP 23.000 
WGHT    0.006700 
EXTI    0.000383 
FVAR       0.04845 
TI1   3    1.000000    1.000000    0.000000    10.16667    0.02438    0.02438 = 
         0.01793    0.00000    0.00000    0.01219 
I1    4    0.684301    0.737869    0.107780    11.00000    0.02443    0.01729 = 
         0.01116   -0.00091   -0.00134    0.01384 
O1    1    0.333333    0.666667    0.024851    10.33333    0.02301    0.02301 = 
         0.06986    0.00000    0.00000    0.01151 
O2    1    0.840591    0.909356    0.101616    11.00000    0.02731    0.01950 = 
         0.02188   -0.00196    0.00712    0.00428 
O3    1    0.600848    0.787572    0.214395    11.00000    0.01745    0.01873 = 
         0.02124   -0.00456    0.00079    0.00864 
O4    1    0.612386    0.758696   -0.027276    11.00000    0.05679    0.02184 = 
         0.01840    0.00293   -0.00851    0.02136 
H1    2    0.368221    0.629092    0.064164    11.00000    0.23448 
HKLF 4 
  
  
  
  
REM  ASDFA in R-3 
REM R1 =  0.0259 for     512 Fo > 4sig(Fo)  and  0.0361 for all     628 data 
REM     47 parameters refined using      1 restraints 
  
END 
  
WGHT      0.0067      0.0000 
  
REM Highest difference peak  0.740,  deepest hole -0.877,  1-sigma level  0.219 
Q1    1   0.9187  0.9160  0.2062  11.00000  0.05    0.74 
Q2    1   0.8083  0.7735  0.0606  11.00000  0.05    0.73 
Q3    1   0.5816  0.8482  0.1111  11.00000  0.05    0.72 
Q4    1   0.5017  0.7000  0.2232  11.00000  0.05    0.71 
Q5    1   0.6176  0.6407  0.0062  11.00000  0.05    0.70 
Q6    1   0.7318  0.7867 -0.0976  11.00000  0.05    0.69 
Q7    1   0.2762  0.5697 -0.0370  11.00000  0.05    0.65 
Q8    1   0.4692  0.6195  0.0048  11.00000  0.05    0.64 
Q9    1   0.6449  0.6734  0.1485  11.00000  0.05    0.62 
Q10   1   0.7992  0.9222  0.0100  11.00000  0.05    0.62 
;
_shelx_res_checksum              77670
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'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'
'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'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-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'
'-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'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 1.000000 1.000000 0.000000 0.0222(6) Uani 1 6 d S T P . .
I1 I 0.68430(4) 0.73787(4) 0.10778(3) 0.01611(14) Uani 1 1 d . . . . .
O1 O 0.333333 0.666667 0.0249(9) 0.039(2) Uani 1 3 d DS T P . .
O2 O 0.8406(4) 0.9094(4) 0.1016(3) 0.0262(10) Uani 1 1 d . . . . .
O3 O 0.6008(4) 0.7876(4) 0.2144(3) 0.0193(9) Uani 1 1 d . . . . .
O4 O 0.6124(5) 0.7587(4) -0.0273(3) 0.0316(11) Uani 1 1 d . . . . .
H1 H 0.368(19) 0.629(19) 0.064(7) 0.23(6) Uiso 1 1 d D . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ti1 0.0244(10) 0.0244(10) 0.0179(15) 0.000 0.000 0.0122(5)
I1 0.0244(3) 0.0173(2) 0.0112(2) -0.00091(16) -0.00134(16) 0.0138(2)
O1 0.023(3) 0.023(3) 0.070(6) 0.000 0.000 0.0115(14)
O2 0.027(3) 0.019(2) 0.022(2) -0.0020(19) 0.0071(19) 0.004(2)
O3 0.017(2) 0.019(2) 0.021(2) -0.0046(18) 0.0008(17) 0.0086(18)
O4 0.057(3) 0.022(2) 0.018(2) 0.0029(19) -0.009(2) 0.021(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ti1 O2 180.00(17) 12_655 3_675 ?
O2 Ti1 O2 88.4(2) 12_655 11_565 ?
O2 Ti1 O2 91.6(2) 3_675 11_565 ?
O2 Ti1 O2 91.6(2) 12_655 2_765 ?
O2 Ti1 O2 88.4(2) 3_675 2_765 ?
O2 Ti1 O2 180.0 11_565 2_765 ?
O2 Ti1 O2 88.4(2) 12_655 10_775 ?
O2 Ti1 O2 91.6(2) 3_675 10_775 ?
O2 Ti1 O2 88.4(2) 11_565 10_775 ?
O2 Ti1 O2 91.6(2) 2_765 10_775 ?
O2 Ti1 O2 91.6(2) 12_655 . ?
O2 Ti1 O2 88.4(2) 3_675 . ?
O2 Ti1 O2 91.6(2) 11_565 . ?
O2 Ti1 O2 88.4(2) 2_765 . ?
O2 Ti1 O2 180.0 10_775 . ?
O3 I1 O4 101.1(3) . . ?
O3 I1 O2 94.21(17) . . ?
O4 I1 O2 94.99(18) . . ?
I1 O2 Ti1 135.9(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O2 1.946(5) 12_655 ?
Ti1 O2 1.946(5) 3_675 ?
Ti1 O2 1.946(5) 11_565 ?
Ti1 O2 1.946(5) 2_765 ?
Ti1 O2 1.946(5) 10_775 ?
Ti1 O2 1.946(5) . ?
I1 O3 1.790(5) . ?
I1 O4 1.807(5) . ?
I1 O2 1.860(6) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168342056
