A new polar alkaline earth−rare earth−iodate, Ba2Ce(IO3)8(H2O)
Zhang, Xue-Ying; Zhang, Xiao-Han; Yang, Bing-Ping; Mao, Jiang-Gao; Dalton Transactions  (2023) –; doi:10.1039/D3DT00326D

data_7712370
_publ_section_title
;
 A new polar alkaline earth&#x2212;rare earth&#x2212;iodate,
 Ba2Ce(IO3)8(H2O)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00326D
_journal_year                    2023
_chemical_formula_moiety         'Ba2 Ce H2 I8 O25'
_chemical_formula_sum            'Ba2 Ce H2 I8 O25'
_chemical_formula_weight         1832.02
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-09-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-01-25 deposited with the CCDC.	2023-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5042(5)
_cell_length_b                   7.8841(3)
_cell_length_c                   19.5359(8)
_cell_measurement_reflns_used    9536
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.6770
_cell_measurement_theta_min      3.5180
_cell_volume                     2388.00(15)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -3.00  22.00   1.00    2.27    --   13.00-105.00-162.00   25
  2  \w     -4.00  22.00   1.00    2.27    --  -13.94-105.00-162.00   26
  3  \w    -57.00 -32.00   1.00    2.27    --  -13.94 105.00 -62.00   25
  4  \w     35.00 102.00   1.00    2.27    --   13.00 178.00 150.00   67
  5  \w    -16.00  10.00   1.00    2.27    --   13.00 -99.00   0.00   26
  6  \w    -18.00  28.00   1.00    2.27    --  -13.94 -99.00 -30.00   46
  7  \w    -89.00 -64.00   1.00    2.27    --  -13.94 -38.00 -90.00   25
  8  \w    -51.00   7.00   1.00    2.27    --  -13.94 -38.00 -90.00   58
  9  \w   -101.00 -58.00   1.00    2.27    --  -13.94 178.00-120.00   43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0414011000
_diffrn_orient_matrix_UB_12      -0.0134267000
_diffrn_orient_matrix_UB_13      0.0189268000
_diffrn_orient_matrix_UB_21      -0.0187558000
_diffrn_orient_matrix_UB_22      -0.0323625000
_diffrn_orient_matrix_UB_23      0.0173964000
_diffrn_orient_matrix_UB_31      0.0052765000
_diffrn_orient_matrix_UB_32      -0.0095053000
_diffrn_orient_matrix_UB_33      -0.0862014000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16163
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         3.355
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    15.587
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    5.096
_exptl_crystal_description       prism
_exptl_crystal_F_000             3184
_exptl_crystal_size_max          1.75
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.956
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.262
_refine_ls_abs_structure_details
;
 Flack x determined using 1630 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         4016
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0261P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0527
_refine_ls_wR_factor_ref         0.0548
_reflns_Friedel_coverage         0.844
_reflns_Friedel_fraction_full    0.898
_reflns_Friedel_fraction_max     0.898
_reflns_number_gt                3782
_reflns_number_total             4016
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00326d2.cif
_cod_data_source_block           1
_cod_original_formula_sum        'Ba2 H2 Ce I8 O25'
_cod_database_code               7712370
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ba Ce I O'
_shelx_estimated_absorpt_t_max   0.574
_shelx_estimated_absorpt_t_min   0.015
_reflns_odcompleteness_completeness 99.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Restrained distances
 Ce1-H4A \\sim Ce1-H4B
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(O11) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O2) \\sim
Ueq, Uanis(O23) \\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O15) \\sim Ueq,
Uanis(O14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O11)
\\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O24) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O20) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
3.a Free rotating group:
 O4(H4A,H4B)
;
_shelx_res_checksum              8463
_shelx_hkl_checksum              41336
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.733
_oxdiff_exptl_absorpt_empirical_full_min 0.742