Exploring a new short-wavelength nonlinear optical fluoride material featuring unprecedented polar <i>cis</i>-[Zr<sub>6</sub>F<sub>34</sub>]<sup>10-</sup> clusters.
Yan, Mei; Tang, Ru-Ling; Yao, Wen-Dong; Liu, Wenlong; Guo, Sheng-Ping; Chemical science 15 (2024) 2883–2888; doi:10.1039/d3sc06683e

data_1570780
_publ_section_title
;
 Exploring a new short-wavelength nonlinear optical fluoride material
 featuring unprecedented polar
 <i>cis</i>-[Zr<sub>6</sub>F<sub>34</sub>]<sup>10-</sup> clusters.
;
_journal_issue                   8
_journal_name_full               'Chemical science'
_journal_page_first              2883
_journal_page_last               2888
_journal_paper_doi               10.1039/d3sc06683e
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'Ba2 F31 K3 Zr6'
_chemical_formula_sum            'Ba2 F31 K3 Zr6'
_chemical_formula_weight         1528.30
_space_group_crystal_system      hexagonal
_space_group_IT_number           185
_space_group_name_Hall           'P 6c -2'
_space_group_name_H-M_alt        'P 63 c m'
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-01
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-11-02 deposited with the CCDC.	2024-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   9.4435(3)
_cell_length_b                   9.4435(3)
_cell_length_c                   15.3288(6)
_cell_measurement_reflns_used    8881
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.536
_cell_measurement_theta_min      2.489
_cell_volume                     1183.87(7)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11097
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.545
_diffrn_reflns_theta_min         2.490
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    6.566
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1458 before and 0.0637 after correction.
The Ratio of minimum to maximum transmission is 0.6788.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.287
_exptl_crystal_description       prism
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.07(2)
_refine_ls_extinction_coef       0.0091(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1012
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0163
_refine_ls_R_factor_gt           0.0163
_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^)+(0.0209P)^2^+0.7056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0376
_refine_ls_wR_factor_ref         0.0377
_reflns_Friedel_coverage         0.913
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                1010
_reflns_number_total             1012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06683e2.cif
_cod_data_source_block           a
_cod_depositor_comments          'Adding full bibliography for 1570780.cif.'
_cod_original_cell_volume        1183.87(9)
_cod_database_code               1570780
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.532
_shelx_estimated_absorpt_t_min   0.482
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.93(2)
 0.07(2)
;
_shelx_res_checksum              25635
_olex2_submission_special_instructions 'No special instructions were received'