Comprehensively understanding the distinct properties of crystal structure, phase transition and dielectrics in [M(crown)n]ReO4 (M+ = Na+, K+, NH4+; crown = 15-crown-5, 18-crown-6; n = 1 or 2)
Yuan, Guo-Jun; Pan, Xue-Wei; Gao, Yan; Jiang, You-Fang; Li, Li; Ren, Xiao-Ming; CrystEngComm 26 (2024) 3704–3713; doi:10.1039/D4CE00435C

data_7248688
_publ_section_title
;
 Comprehensively understanding the distinct properties of crystal
 structure, phase transition and dielectrics in [M(crown)n]ReO4 (M+ = Na+,
 K+, NH4+; crown = 15-crown-5, 18-crown-6; n = 1 or 2)
;
_journal_issue                   27
_journal_name_full               CrystEngComm
_journal_page_first              3704
_journal_page_last               3713
_journal_paper_doi               10.1039/D4CE00435C
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         '0.5(C48 H96 K4 O40 Re4)'
_chemical_formula_sum            'C24 H48 K2 O20 Re2'
_chemical_formula_weight         1107.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-02-02
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-02-02 deposited with the CCDC.	2024-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.3113(2)
_cell_length_b                   15.5506(4)
_cell_length_c                   14.6792(4)
_cell_measurement_reflns_used    9788
_cell_measurement_temperature    108(2)
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.62
_cell_volume                     1897.22(8)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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)'
_diffrn_ambient_temperature      108.15
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13918
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.620
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.668
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.3664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1120 before and 0.0778 after correction.
The Ratio of minimum to maximum transmission is 0.4915.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            clear
_exptl_crystal_colour_lustre     clear
_exptl_crystal_density_diffrn    1.938
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.835
_refine_diff_density_min         -3.299
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.312
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         1721
_refine_ls_number_restraints     375
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0437
_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^)+48.7244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1220
_refine_ls_wR_factor_ref         0.1226
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1661
_reflns_number_total             1721
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00435c2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7248686--7248690.cif.'
_cod_database_code               7248688
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.555
_shelx_estimated_absorpt_t_min   0.349
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 O7-O8 \\sim O7-O9 \\sim O7-O10 \\sim O8-O9 \\sim O8-O10 \\sim O9-O10
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim C1 \\sim C2 \\sim C3
\\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim
C12: within 3.5A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 3.5A
Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim
Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C1) \\sim Ueq,
Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Fixed Sof: O1(0.5) O2(0.5) O3(0.5) O4(0.5) O5(0.5) O6(0.5) O7(0.5) O8(0.5)
 O9(0.5) O10(0.5) C1(0.5) H1A(0.5) H1B(0.5) C2(0.5) H2A(0.5) H2B(0.5) C3(0.5)
 H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5) H4B(0.5) C5(0.5) H5A(0.5) H5B(0.5) C6(0.5)
 H6A(0.5) H6B(0.5) C7(0.5) H7A(0.5) H7B(0.5) C8(0.5) H8A(0.5) H8B(0.5) C9(0.5)
 H9A(0.5) H9B(0.5) C10(0.5) H10A(0.5) H10B(0.5) C11(0.5) H11A(0.5) H11B(0.5)
 C12(0.5) H12A(0.5) H12B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B)
;
_shelx_res_checksum              93472
_olex2_submission_special_instructions 'No special instructions were received'