#------------------------------------------------------------------------------
#$Date: 2022-08-06 14:58:11 +0300 (Sat, 06 Aug 2022) $
#$Revision: 277133 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/16/7061628.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7061628
loop_
_publ_author_name
'You, Xiuli'
'Rao, Wenjun'
'Han, Keke'
'Wang, Lingyu'
'Zhang, Mengxia'
'Wei, Zhenhong'
_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         'O4 Re, 2(C7)'
_chemical_formula_sum            'C14 O4 Re'
_chemical_formula_weight         418.35
_space_group_crystal_system      tetragonal
_space_group_IT_number           111
_space_group_name_Hall           'P -4 2'
_space_group_name_H-M_alt        'P -4 2 m'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_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                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   6.8907(5)
_cell_length_b                   6.8907(5)
_cell_length_c                   5.8523(10)
_cell_measurement_reflns_used    2659
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.80
_cell_volume                     277.88(6)
_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      413(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0239
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            1655
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.96
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    10.937
_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 λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.5
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             191
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.5(3)
_refine_ls_extinction_coef       0.004(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.325
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     16
_refine_ls_number_reflns         314
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.325
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0417
_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/[σ²(Fo²)+(0.0497P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1081
_reflns_number_gt                212
_reflns_number_total             314
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d2nj02531k2.cif
_cod_data_source_block           t_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7061626--7061629.cif.'
_cod_database_code               7061628
_olex2_refinement_description
;
1. Others
 Fixed Sof: Re1(0.125) C2(0.25) O2(0.25) O1(0.25) C3(0.5)
 Fixed U12: Re1(0)
 Fixed U13: Re1(0)
 Fixed U23: Re1(0)
 Fixed X: Re1(0.5) C2(0) O2(0.5) O1(0.5) C3(0)
 Fixed Y: Re1(0.5) C2(0) O2(0.5)
 Fixed Z: Re1(0) O1(0) C3(0.5)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, z'
3 'y, -x, -z'
4 '-y, x, -z'
5 '-x, y, -z'
6 'x, -y, -z'
7 '-y, -x, z'
8 'y, x, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.5000 0.5000 0.0000 0.1482(8) Uani 1 8 d S . .
C2 C 0.0000 0.0000 0.250(5) 0.179(8) Uiso 1 4 d S . .
C1 C -0.053(6) 0.183(4) 0.307(4) 0.263(13) Uiso 1 1 d . . .
O2 O 0.5000 0.5000 0.234(14) 0.40(3) Uiso 1 4 d S . .
O1 O 0.5000 0.258(9) 0.0000 0.285(18) Uiso 0.50 2 d SP . .
C3 C 0.0000 0.289(13) 0.5000 0.44(4) Uiso 1 2 d S . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Re1 0.1433(8) 0.1433(8) 0.1581(12) 0.000 0.000 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Re1 O2 179.999(3) . 3_565 ?
O2 Re1 O1 90.0 3_565 . ?
O2 Re1 O1 90.000(8) . 4_655 ?
O2 Re1 O1 90.000(8) . 3_565 ?
O2 Re1 O1 90.0 3_565 2_665 ?
O2 Re1 O1 90.001(8) 3_565 3_565 ?
O2 Re1 O1 89.999(8) 3_565 4_655 ?
O2 Re1 O1 90.0 . . ?
O2 Re1 O1 90.0 . 2_665 ?
O1 Re1 O1 179.999(7) . 2_665 ?
O1 Re1 O1 90.001(5) 3_565 2_665 ?
O1 Re1 O1 90.0 . 4_655 ?
O1 Re1 O1 89.999(9) 2_665 4_655 ?
O1 Re1 O1 90.000(5) 3_565 . ?
O1 Re1 O1 180.0 3_565 4_655 ?
C1 C2 C1 151(4) 2 . ?
C1 C2 C1 151(4) 8 7 ?
C1 C2 C1 116(3) 2 7 ?
C1 C2 C1 56(3) 2 8 ?
C1 C2 C1 116(3) . 8 ?
C1 C2 C1 56(3) . 7 ?
C1 C1 C2 62.1(16) 7 . ?
C1 C1 C3 124(2) 7 . ?
C3 C1 C2 128(4) . . ?
C1 C3 C1 117(7) 5_556 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 O2 1.37(8) . ?
Re1 O2 1.37(8) 3_565 ?
Re1 O1 1.67(6) 4_655 ?
Re1 O1 1.67(6) . ?
Re1 O1 1.67(6) 3_565 ?
Re1 O1 1.67(6) 2_665 ?
C2 C1 1.36(3) . ?
C2 C1 1.36(3) 7 ?
C2 C1 1.36(3) 8 ?
C2 C1 1.36(3) 2 ?
C1 C1 1.27(7) 7 ?
C1 C3 1.39(5) . ?
C3 C1 1.39(5) 5_556 ?
