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_7248687
_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         'O4 Re, 0.25(H16 N4), 4(C5 H10 O2.5)'
_chemical_formula_sum            'C20 H44 N O14 Re'
_chemical_formula_weight         708.76
_space_group_crystal_system      tetragonal
_space_group_IT_number           84
_space_group_name_Hall           '-P 4c'
_space_group_name_H-M_alt        'P 42/m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-07-11
_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                   9.100(3)
_cell_length_b                   9.100(3)
_cell_length_c                   17.743(6)
_cell_measurement_reflns_used    1616
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.84
_cell_measurement_theta_min      2.24
_cell_volume                     1469.3(8)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0501
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7609
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.008
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         2.238
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.197
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3776
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1213 before and 0.0530 after correction.
The Ratio of minimum to maximum transmission is 0.5064.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_description       needle
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.016(3)
_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   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         1347
_refine_ls_number_restraints     396
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1333
_refine_ls_R_factor_gt           0.0838
_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^)+(0.0980P)^2^+7.1859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2257
_refine_ls_wR_factor_ref         0.2607
_reflns_Friedel_coverage         0.000
_reflns_number_gt                724
_reflns_number_total             1347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00435c2.cif
_cod_data_source_block           224_0m
_cod_depositor_comments
'Adding full bibliography for 7248686--7248690.cif.'
_cod_original_cell_volume        1469.2(11)
_cod_database_code               7248687
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.704
_shelx_estimated_absorpt_t_min   0.655
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H,H) groups
2. Restrained distances
 O1-C2
 1.45 with sigma of 0.02
 C2-C3
 1.5 with sigma of 0.02
 C3-O2
 1.45 with sigma of 0.02
 O2-C4
 1.45 with sigma of 0.02
 C4-O2
 1.45 with sigma of 0.02
 C4-C5
 1.5 with sigma of 0.02
 C5-O3
 1.45 with sigma of 0.02
 O1-C1
 1.45 with sigma of 0.02
 C3A-C2A
 1.5 with sigma of 0.02
 C2A-O1A
 1.45 with sigma of 0.02
 C2A-C1A
 2.45 with sigma of 0.02
 O1A-C1A
 1.45 with sigma of 0.02
 O1A_$1-C1A
 2.38 with sigma of 0.02
 O1A_$1-C2A_$1
 1.45 with sigma of 0.02
 C2A_$1-C3A_$1
 1.5 with sigma of 0.02
 C3A_$1-O2A_$1
 1.455 with sigma of 0.02
 C5A_$1-O3A
 1.45 with sigma of 0.02
 C5A-O3A
 1.45 with sigma of 0.02
 O2A-C3A
 1.45 with sigma of 0.02
 C4A-C5A
 1.5 with sigma of 0.02
 C5A_$1-C5A
 2.36 with sigma of 0.02
 O3-C4
 2.45 with sigma of 0.02
 C5-O2
 2.38 with sigma of 0.02
 C4-C3
 2.38 with sigma of 0.02
 N1-H1E
 0.82 with sigma of 0.02
 N1-H1C
 0.82 with sigma of 0.02
 N1-H1F
 0.82 with sigma of 0.02
 H1D-N1
 0.82 with sigma of 0.02
 H1E-H1C
 1.32 with sigma of 0.02
 H1E-H1F
 1.32 with sigma of 0.02
 H1E-H1D
 1.32 with sigma of 0.02
 H1C-H1F
 1.32 with sigma of 0.02
 H1C-H1D
 1.32 with sigma of 0.02
 H1F-H1D
 1.32 with sigma of 0.02
3. Rigid bond restraints
 O1, O2, O3, C1, C2, C3, C4, C5, O1A, O2A, O3A, C1A, C2A, C3A, C4A, C5A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O1 \\sim O2 \\sim O3 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim O1A
\\sim O2A \\sim O3A \\sim C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O5) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C3) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C4) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O2)
\\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C2) \\sim Ueq,
Uanis(O1) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C1) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3A) \\sim Ueq, Uanis(O1A) \\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(C1A)
\\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(C4A) \\sim Ueq,
Uanis(C5A) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(O2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(O1)
\\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: O4(0.25) O5(0.75) H1C(0.25) H1D(0.25) H1E(0.25) H1F(0.25) O1(0.5)
 O2(0.5) O3(0.25) C1(0.5) H1B(0.5) H1A(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) O1A(0.5)
 O2A(0.5) O3A(0.25) C1A(0.5) H1AA(0.5) H1AB(0.5) C2A(0.5) H2AB(0.5) H2AA(0.5)
 C3A(0.5) H3AB(0.5) H3AA(0.5) C4A(0.5) H4AB(0.5) H4AA(0.5) C5A(0.5) H5AA(0.5)
 H5AB(0.5)
6.a Riding coordinates:
 N1(H1C,H1D,H1E,H1F)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1B,H1A), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C1A(H1AA,
 H1AB), C2A(H2AB,H2AA), C3A(H3AB,H3AA), C4A(H4AB,H4AA), C5A(H5AA,H5AB)
;
_shelx_res_checksum              90828
_olex2_submission_special_instructions 'No special instructions were received'