Two quasi-spherical molecules [1,4-diazabicyclo(3.2.2)nonane]X (X = ClO4, ReO4) exhibit switchable phase transition, dielectric and second-harmonic-generation properties
You, Xiuli; Rao, Wenjun; Han, Keke; Wang, Lingyu; Zhang, Mengxia; Wei, Zhenhong; New Journal of Chemistry 46 (2022) 14404–14409; doi:10.1039/D2NJ02531K

data_7061629
_publ_section_title
;
 Two quasi-spherical molecules [1,4-diazabicyclo(3.2.2)nonane]X (X = ClO4,
 ReO4) exhibit switchable phase transition, dielectric and
 second-harmonic-generation properties
;
_journal_issue                   30
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14404
_journal_page_last               14409
_journal_paper_doi               10.1039/D2NJ02531K
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C7 H15 N2, O4 Re'
_chemical_formula_sum            'C7 H15 N2 O4 Re'
_chemical_formula_weight         377.42
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-12-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-12-13 deposited with the CCDC.	2022-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.725(2)
_cell_length_b                   13.750(2)
_cell_length_c                   10.9708(17)
_cell_measurement_reflns_used    2659
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.80
_cell_volume                     2070.4(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_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  0.0292
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5922
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.561
_diffrn_reflns_theta_min         2.801
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    11.731
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4204
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1239 before and 0.0377 after correction.
The Ratio of minimum to maximum transmission is 0.5638.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.303
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.187
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_coef       0.00016(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2194
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0088P)^2^+35.7523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0715
_reflns_Friedel_coverage         0.899
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                1921
_reflns_number_total             2395
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj02531k2.cif
_cod_data_source_block           t_CCDC2
_cod_depositor_comments
;
Adding full bibliography for 7061626--7061629.cif.

2025-03-29
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C14 H30 N4 O8 Re2'
_cod_original_formula_weight         754.84
_cod_original_formula_moiety         'C14 H30 N4, 2(O4 Re)'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_original_sg_symbol_H-M      'A b a 2'
_cod_database_code               7061629
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C1(H1)
1.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C4(H4A,H4B), C2(H2A,H2B), C3(H3A,H3B), C7(H7A,H7B), C5(H5A,H5B),
 N2(H2C,H2D)
;
_shelx_res_checksum              59148
_olex2_submission_special_instructions 'No special instructions were received'