From centrosymmetric to noncentrosymmetric: cation-directed structural evolution in X3ZnB5O10 (X = Na, K, Rb) and Cs12Zn4(B5O10)4 crystals
Baiheti, Tuohetijiang; Han, Shujuan; Tudi, AbuduKadi; Yang, Zhihua; Yu, H. H.; Pan, Shilie; Inorganic Chemistry Frontiers 6 (2019) 1461–; doi:10.1039/C9QI00285E

data_4350016
_publ_section_title
;
 From centrosymmetric to noncentrosymmetric: cation-directed structural
 evolution in X3ZnB5O10 (X = Na, K, Rb) and Cs12Zn4(B5O10)4 crystals
;
_journal_issue                   6
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1461
_journal_paper_doi               10.1039/C9QI00285E
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety         'B20 Cs12 O40 Zn4'
_chemical_formula_sum            'B20 Cs12 O40 Zn4'
_chemical_formula_weight         2712.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-18 deposited with the CCDC.	2019-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.520(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.739(16)
_cell_length_b                   19.326(16)
_cell_length_c                   14.495(12)
_cell_measurement_reflns_used    2806
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.09
_cell_measurement_theta_min      2.41
_cell_volume                     4948(7)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_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  0.0432
_diffrn_reflns_av_unetI/netI     0.0886
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14935
_diffrn_reflns_point_group_measured_fraction_full 0.831
_diffrn_reflns_point_group_measured_fraction_max 0.809
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.627
_diffrn_reflns_theta_min         2.306
_exptl_absorpt_coefficient_mu    10.723
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5349
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1268 before and 0.0559 after correction. The Ratio of minimum to maximum transmission is 0.7174. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.642
_exptl_crystal_description       block
_exptl_crystal_F_000             4800
_exptl_crystal_size_max          0.243
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.189
_refine_diff_density_max         1.846
_refine_diff_density_min         -1.923
_refine_diff_density_rms         0.276
_refine_ls_abs_structure_details
;
 Flack x determined using 2006 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         9328
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0351P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1068
_reflns_Friedel_coverage         0.632
_reflns_Friedel_fraction_full    0.663
_reflns_Friedel_fraction_max     0.627
_reflns_number_gt                7089
_reflns_number_total             9328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9qi00285e2.cif
_cod_data_source_block           123
_cod_database_code               4350016
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(B12) \\sim Ueq, Uanis(B19) \\sim Ueq, Uanis(B20) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
;
_shelx_res_checksum              49981
_shelx_hkl_checksum              8106
_olex2_submission_special_instructions 'No special instructions were received'