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_7061626
_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_absolute_configuration unk
_chemical_formula_moiety         'C7 H15 N2, Cl O4'
_chemical_formula_sum            'C7 H15 Cl N2 O4'
_chemical_formula_weight         226.66
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-08-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-17 deposited with the CCDC.	2022-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                77.838(3)
_cell_angle_beta                 88.700(3)
_cell_angle_gamma                81.931(3)
_cell_formula_units_Z            2
_cell_length_a                   6.7331(3)
_cell_length_b                   8.6522(3)
_cell_length_c                   8.8761(3)
_cell_measurement_reflns_used    4598
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.1500
_cell_measurement_theta_min      2.3740
_cell_volume                     500.46(3)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'multiwire proportional'
_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  0.0218
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5249
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.35
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.374
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             240
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.23(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.274
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         2899
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.276
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1009P)^2^+0.0357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1660
_refine_ls_wR_factor_ref         0.1762
_reflns_number_gt                2420
_reflns_number_total             3508
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d2nj02531k2.cif
_cod_data_source_block           t
_cod_depositor_comments
'Adding full bibliography for 7061626--7061629.cif.'
_cod_original_cell_volume        500.47(3)
_cod_database_code               7061626
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.052) H1A(0.052) H1B(0.052) H2A(0.052) H2B(0.052) H3A(0.064)
 H3B(0.064) H4A(0.053) H4B(0.053) H5(0.056) H6A(0.051) H6B(0.051) H7A(0.051)
 H7B(0.051) H8A(0.065) H8B(0.065) H9A(0.061) H9B(0.061) H10A(0.058) H10B(0.058)
 H11A(0.053) H11B(0.053) H12A(0.052) H12B(0.052) H13A(0.064) H13B(0.064)
 H14(0.05)
 Fixed X: H1A(-0.0757) H1B(0.1401) H2A(0.4011) H2B(0.3963) H3A(0.5528)
 H3B(0.4776) H4A(0.0539) H4B(0.24) H5(0.3611) H6A(0.0868) H6B(-0.0843) H7A(-
 0.0623) H7B(-0.1167) H8A(-0.3961) H8B(-0.3277) H9A(-0.2444) H9B(-0.2458)
 H10A(0.02) H10B(0.2356) H11A(-0.0809) H11B(0.1062) H12A(0.2501) H12B(0.0841)
 H13A(0.2739) H13B(0.2185) H14(-0.1999)
 Fixed Y: H1A(0.2467) H1B(0.2269) H2A(0.1917) H2B(0.3081) H3A(0.4517)
 H3B(0.371) H4A(0.6941) H4B(0.6449) H5(0.6561) H6A(0.4605) H6B(0.4942)
 H7A(0.4282) H7B(0.5189) H8A(-0.0542) H8B(0.0295) H9A(0.0946) H9B(0.209)
 H10A(0.1695) H10B(0.1471) H11A(-0.2549) H11B(-0.3071) H12A(-0.1009) H12B(-
 0.0695) H13A(-0.1215) H13B(-0.0286) H14(-0.2553)
 Fixed Z: H1A(0.8777) H1B(0.8083) H2A(0.9896) H2B(1.1037) H3A(0.919)
 H3B(0.7925) H4A(0.9104) H4B(1.0213) H5(0.7837) H6A(1.1528) H6B(1.0284)
 H7A(0.6444) H7B(0.7781) H8A(0.3137) H8B(0.4404) H9A(0.1305) H9B(0.2461)
 H10A(0.4219) H10B(0.3534) H11A(0.2128) H11B(0.3234) H12A(0.2068) H12B(0.0788)
 H13A(0.4544) H13B(0.5861) H14(0.458)
;
_olex2_submission_special_instructions 'No special instructions were received'