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_7248689
_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         'C24 H48 K2 O20 Re2'
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2022-07-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-01-29 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                   8.382(5)
_cell_length_b                   15.736(8)
_cell_length_c                   14.815(8)
_cell_measurement_reflns_used    4651
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.65
_cell_measurement_theta_min      2.43
_cell_volume                     1954.1(19)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0482
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9458
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.988
_diffrn_reflns_theta_max         24.988
_diffrn_reflns_theta_min         2.430
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.474
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3487
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1331 before and 0.0675 after correction.
The Ratio of minimum to maximum transmission is 0.4677.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.882
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.197
_refine_diff_density_min         -2.272
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.298
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         1785
_refine_ls_number_restraints     157
_refine_ls_restrained_S_all      1.271
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0501
_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^)+33.3506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1314
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1632
_reflns_number_total             1785
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00435c2.cif
_cod_data_source_block           213
_cod_depositor_comments
'Adding full bibliography for 7248686--7248690.cif.'
_cod_original_cell_volume        1954.2(18)
_cod_database_code               7248689
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.593
_shelx_estimated_absorpt_t_min   0.536
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 C11-C12
 1.5 with sigma of 0.02
 C2-C1
 1.5 with sigma of 0.02
3. Rigid bond restraints
 Re1, O9, Re1, O9A, Re1, O7, Re1, O8, Re1, O8A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 Re1, O7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(O5) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C5)
\\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C1) \\sim Ueq,
Uanis(C10) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C12) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(K1) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim
Ueq, Uanis(O6) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq,
Uanis(C7) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C12) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(O4)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O7) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O9) \\sim Ueq, Uanis(O9A) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O8A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(O8A)=1-FVAR(1)
 Sof(O9A)=0.5*(1-FVAR(2))
 Sof(O9)=0.5*FVAR(2)
 Sof(O8)=FVAR(1)
 Fixed Sof: O3(0.5) O1(0.5) O2(0.5) O6(0.5) C6(0.5) H6A(0.5) H6B(0.5) O5(0.5)
 C3(0.5) H3A(0.5) H3B(0.5) C8(0.5) H8A(0.5) H8B(0.5) C5(0.5) H5A(0.5) H5B(0.5)
 O7(0.5) C4(0.5) H4A(0.5) H4B(0.5) C7(0.5) H7A(0.5) H7B(0.5) C1(0.5) H1A(0.5)
 H1B(0.5) C10(0.5) H10A(0.5) H10B(0.5) C2(0.5) H2A(0.5) H2B(0.5) C12(0.5)
 H12A(0.5) H12B(0.5) C9(0.5) H9A(0.5) H9B(0.5) C11(0.5) H11A(0.5) H11B(0.5)
 O4(0.5)
6.a Riding coordinates:
 C6(H6A,H6B), C3(H3A,H3B), C8(H8A,H8B), C5(H5A,H5B), C4(H4A,H4B), C7(H7A,H7B),
 C1(H1A,H1B), C10(H10A,H10B), C2(H2A,H2B), C12(H12A,H12B), C9(H9A,H9B),
 C11(H11A,H11B)
;
_shelx_res_checksum              45893
_olex2_submission_special_instructions 'No special instructions were received'