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_7248690
_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, 2(C10 H20 O5), 2(H4 N0.5)'
_chemical_formula_sum            'C20 H48 N O14 Re'
_chemical_formula_weight         712.79
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_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                83.4460(10)
_cell_angle_beta                 88.6520(10)
_cell_angle_gamma                87.6340(10)
_cell_formula_units_Z            2
_cell_length_a                   8.7695(3)
_cell_length_b                   8.9474(3)
_cell_length_c                   17.6798(5)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    108(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.29
_cell_volume                     1376.74(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)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      108.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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_unetI/netI     0.0736
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_number            5626
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.412
_diffrn_reflns_theta_min         2.293
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.479
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0865 before and 0.0676 after correction.
 
For component 2:
 wR2(int) was 0.0899 before and 0.0677 after correction.
 The Ratio of minimum to maximum transmission is 0.72.

Final HKLF 4 output contains 26879 reflections, Rint = 0.0730
 (20455 with I > 3sig(I), Rint = 0.0671)
;
_exptl_crystal_colour            clear
_exptl_crystal_colour_lustre     clear
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_description       block
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.783
_refine_diff_density_min         -1.838
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         5626
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+13.8552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1084
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4800
_reflns_number_total             5626
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00435c2.cif
_cod_data_source_block           224
_cod_depositor_comments
'Adding full bibliography for 7248686--7248690.cif.'
_cod_database_code               7248690
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.553
_shelx_estimated_absorpt_t_min   0.468
_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
 O6-C11A = O6-C11 = O7-C12A = O7-C12
 1.425 with sigma of 0.02
 C12-C11 = C11A-C12A
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C11 \\sim C11A \\sim C12 \\sim C12A: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
Uanis(C12A) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C11A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(C12A)=Sof(H12C)=Sof(H12D)=1-FVAR(1)
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=FVAR(1)
5.a Riding coordinates:
 N1(H1C,H1D,H1E), N1(H1F), N2(H2C,H2D,H2E), N2(H2F)
5.b 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),
 C11A(H11C,H11D), C12(H12A,H12B), C12A(H12C,H12D), C13(H13A,H13B), C14(H14A,
 H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B),
 C19(H19A,H19B), C20(H20A,H20B)
;
_shelx_res_checksum              52884
_olex2_submission_special_instructions 'No special instructions were received'