KBa<sub>3</sub>M<sub>2</sub>F<sub>14</sub>Cl (M = Zr, Hf): novel short-wavelength mixed metal halides with the largest second-harmonic generation responses contributed by mixed functional moieties.
Yan, Mei; Hu, Chun-Li; Tang, Ru-Ling; Yao, Wen-Dong; Liu, Wenlong; Guo, Sheng-Ping; Chemical science 15 (2024) 8500–8505; doi:10.1039/d4sc01259c

data_1571503
_publ_section_title
;
 KBa<sub>3</sub>M<sub>2</sub>F<sub>14</sub>Cl (M = Zr, Hf): novel
 short-wavelength mixed metal halides with the largest second-harmonic
 generation responses contributed by mixed functional moieties.
;
_journal_issue                   22
_journal_name_full               'Chemical science'
_journal_page_first              8500
_journal_page_last               8505
_journal_paper_doi               10.1039/d4sc01259c
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'Ba3 Cl F14 K Zr2'
_chemical_formula_sum            'Ba3 Cl F14 K Zr2'
_chemical_formula_weight         935.01
_space_group_crystal_system      tetragonal
_space_group_IT_number           115
_space_group_name_Hall           'P -4 -2'
_space_group_name_H-M_alt        'P -4 m 2'
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-02
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2024-04-08 deposited with the CCDC.	2024-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   5.7502(2)
_cell_length_b                   5.7502(2)
_cell_length_c                   10.2521(7)
_cell_measurement_reflns_used    2491
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      3.54
_cell_volume                     338.98(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       '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 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0236
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2424
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.465
_diffrn_reflns_theta_min         1.986
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    10.720
_exptl_absorpt_correction_T_max  0.2214
_exptl_absorpt_correction_T_min  0.0888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1058 before and 0.0423 after correction.
The Ratio of minimum to maximum transmission is 0.4011.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.580
_exptl_crystal_description       block
_exptl_crystal_F_000             410
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.29(2)
_refine_ls_extinction_coef       0.065(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     36
_refine_ls_number_reflns         427
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0103
_refine_ls_R_factor_gt           0.0102
_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^)+(0.0082P)^2^+0.1294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0236
_refine_ls_wR_factor_ref         0.0236
_reflns_Friedel_coverage         0.688
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                425
_reflns_number_total             427
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01259c2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1571503--1571504.cif.'
_cod_database_code               1571503
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.414
_shelx_estimated_absorpt_t_min   0.223
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.71(2)
 0.29(2)
;
_shelx_res_checksum              21461
_olex2_submission_special_instructions 'No special instructions were received'