A New Anhydrous Polar Rare-Earth Iodate Fluoride, Ce(IO3)2F2, Exhibiting a Large Second-Harmonic-Generation Effect and Improved Overall Performance
Zhang, Xiao-Han; Yang, Bing-Ping; Hu, Chun-Li; Chen, Jin; Huang, Qian-Ming; Mao, Jiang-Gao; Chemistry of Materials 33 (2021) 2894–2900; doi:10.1021/acs.chemmater.1c00222

data_4003917
_publ_section_title
;
 A New Anhydrous Polar Rare-Earth Iodate Fluoride, Ce(IO3)2F2, Exhibiting
 a Large Second-Harmonic-Generation Effect and Improved Overall
 Performance
;
_journal_issue                   8
_journal_name_full               'Chemistry of Materials'
_journal_page_first              2894
_journal_page_last               2900
_journal_paper_doi               10.1021/acs.chemmater.1c00222
_journal_volume                  33
_journal_year                    2021
_chemical_formula_moiety         'Ce F2 I2 O6'
_chemical_formula_sum            'Ce F2 I2 O6'
_chemical_formula_weight         527.92
_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_primary     dual
_audit_creation_date             2021-01-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0451(8)
_cell_length_b                   6.8485(5)
_cell_length_c                   11.7325(10)
_cell_measurement_reflns_used    2227
_cell_measurement_temperature    100.01(15)
_cell_measurement_theta_max      30.0190
_cell_measurement_theta_min      3.3870
_cell_volume                     646.42(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(15)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3468
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -10.00  75.00   1.00    1.62    --   11.29  77.00 150.00   85
  2  \w    -82.00  11.00   1.00    1.62    --  -12.07 -57.00-120.00   93
  3  \w    -39.00  58.00   1.00    1.62    --  -12.07  57.00  30.00   97
;
_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      -0.0365044000
_diffrn_orient_matrix_UB_12      0.0177505000
_diffrn_orient_matrix_UB_13      -0.0540670000
_diffrn_orient_matrix_UB_21      0.0154131000
_diffrn_orient_matrix_UB_22      -0.0982790000
_diffrn_orient_matrix_UB_23      -0.0158824000
_diffrn_orient_matrix_UB_31      -0.0787536000
_diffrn_orient_matrix_UB_32      -0.0274379000
_diffrn_orient_matrix_UB_33      0.0219046000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4527
_diffrn_reflns_point_group_measured_fraction_full 0.856
_diffrn_reflns_point_group_measured_fraction_max 0.830
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.084
_diffrn_reflns_theta_min         3.445
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    16.619
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.794
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46c (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    5.425
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.136
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.985
_refine_diff_density_min         -1.455
_refine_diff_density_rms         0.270
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.05(5)
_refine_ls_extinction_coef       0.0040(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1189
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0291
_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/[\s^2^(Fo^2^)+(0.0324P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0644
_reflns_Friedel_coverage         0.581
_reflns_Friedel_fraction_full    0.696
_reflns_Friedel_fraction_max     0.643
_reflns_number_gt                1141
_reflns_number_total             1189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm1c00222_si_002.cif
_cod_data_source_block           1
_cod_database_code               4003917
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Ce F I O'
_shelx_estimated_absorpt_t_max   0.490
_shelx_estimated_absorpt_t_min   0.211
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
;
_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 1.590
_oxdiff_exptl_absorpt_empirical_full_min 0.613