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#$Date: 2021-04-24 01:27:45 +0300 (Sat, 24 Apr 2021) $
#$Revision: 264490 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/39/4003916.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_4003916
loop_
_publ_author_name
'Xie, Yongfa'
'Zheng, Jingjing'
'Zheng, Kuangqi'
'Liu, Qing'
'Duan, Jie'
'Chen, Wei'
'Shao, Shuke'
'Cai, Hu'
_publ_section_title
;
 High-Temperature Switchable Nonlinear Optical and Dielectric Material
 Revealed by Molecular Modification
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.0c04220
_journal_year                    2021
_chemical_formula_moiety         'C8 H16 N, O4 Re'
_chemical_formula_sum            'C8 H16 N O4 Re'
_chemical_formula_weight         376.43
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   23.5948(5)
_cell_length_b                   23.5948(5)
_cell_length_c                   10.6826(3)
_cell_measurement_reflns_used    5425
_cell_measurement_temperature    300
_cell_measurement_theta_max      1.00000
_cell_measurement_theta_min      0.14416
_cell_volume                     5150.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15579
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.262
_diffrn_reflns_theta_min         1.726
_exptl_absorpt_coefficient_mu    10.607
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14416
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.185
_exptl_crystal_description       prism
_exptl_crystal_F_000             5529
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.896
_refine_diff_density_min         -5.268
_refine_diff_density_rms         0.342
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         3287
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0743
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1169P)²+244.8342P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2050
_refine_ls_wR_factor_ref         0.2213
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2425
_reflns_number_total             3287
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm0c04220_si_003.cif
_cod_data_source_block           '[N-Me-IsoQ]ReO4_300K'
_cod_original_cell_volume        5150.4(3)
_cod_database_code               4003916
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.93848(2) 0.59016(2) 0.10694(2) 0.04288(5) Uani 1 1 d . U . . .
O1 O 0.89537(15) 0.61883(15) 0.1883(3) 0.04288(5) Uani 1 1 d . U . . .
O3 O 0.88726(15) 0.53948(15) -0.0070(3) 0.04288(5) Uani 1 1 d . U . . .
O2 O 1.00688(15) 0.65675(15) 0.0454(3) 0.04288(5) Uani 1 1 d . U . . .
N1 N 0.0508(3) 0.2420(3) 0.6981(7) 0.0855(3) Uani 1 1 d . U . . .
H1A H 0.0328 0.2714 0.7034 0.103 Uiso 1 1 calc R U . . .
C1 C -0.0030(4) 0.1781(4) 0.6428(9) 0.0855(3) Uani 1 1 d . U . . .
H1 H -0.0109 0.1821 0.5541 0.103 Uiso 1 1 calc R U . . .
C2 C -0.0510(4) 0.1449(4) 0.8558(8) 0.0855(3) Uani 1 1 d . U . . .
H2A H -0.0619 0.1693 0.9145 0.103 Uiso 1 1 calc R U . . .
H2B H -0.0788 0.0986 0.8732 0.103 Uiso 1 1 calc R U . . .
C3 C -0.0619(4) 0.1597(4) 0.7227(8) 0.0855(3) Uani 1 1 d . U . . .
H3A H -0.0995 0.1215 0.6874 0.103 Uiso 1 1 calc R U . . .
H3B H -0.0713 0.1953 0.7233 0.103 Uiso 1 1 calc R U . . .
C4 C 0.0185(4) 0.1636(4) 0.8700(9) 0.0855(3) Uani 1 1 d . U . . .
H4 H 0.0271 0.1596 0.9584 0.103 Uiso 1 1 calc R U . . .
C5 C 0.0618(4) 0.2283(4) 0.8301(8) 0.0855(3) Uani 1 1 d . U . . .
H5A H 0.1064 0.2368 0.8377 0.103 Uiso 1 1 calc R U . . .
H5B H 0.0573 0.2584 0.8854 0.103 Uiso 1 1 calc R U . . .
O4 O 0.96008(15) 0.54681(15) 0.2040(3) 0.04288(5) Uani 1 1 d . U . . .
C6 C 0.0276(4) 0.1267(4) 0.6670(7) 0.0855(3) Uani 1 1 d . U . . .
H6A H -0.0002 0.0851 0.6262 0.103 Uiso 1 1 calc R U . . .
H6B H 0.0711 0.1457 0.6309 0.103 Uiso 1 1 calc R U . . .
C7 C 0.0306(4) 0.1169(4) 0.7948(8) 0.0855(3) Uani 1 1 d . U . . .
H7A H 0.0733 0.1231 0.8154 0.103 Uiso 1 1 calc R U . . .
H7B H -0.0020 0.0723 0.8161 0.103 Uiso 1 1 calc R U . . .
C8 C 0.1116(4) 0.2770(4) 0.6249(8) 0.0855(3) Uani 1 1 d . U . . .
H8A H 0.1462 0.3079 0.6777 0.128 Uiso 1 1 calc R U . . .
H8B H 0.1052 0.2996 0.5566 0.128 Uiso 1 1 calc R U . . .
H8C H 0.1232 0.2461 0.5925 0.128 Uiso 1 1 calc R U . . .
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
O4 Re1 O3 109.41(17) . . ?
O4 Re1 O1 110.07(18) . . ?
O3 Re1 O1 106.59(17) . . ?
O4 Re1 O2 110.76(16) . . ?
O3 Re1 O2 112.23(16) . . ?
O1 Re1 O2 107.68(16) . . ?
C8 N1 C5 113.3(7) . . ?
C8 N1 C1 116.4(7) . . ?
C5 N1 C1 107.4(6) . . ?
C3 C1 N1 105.0(7) . . ?
C3 C1 C6 111.6(7) . . ?
N1 C1 C6 101.8(7) . . ?
C4 C2 C3 108.6(7) . . ?
C1 C3 C2 111.1(8) . . ?
C5 C4 C2 112.8(9) . . ?
C5 C4 C7 109.3(8) . . ?
C2 C4 C7 108.4(7) . . ?
C4 C5 N1 114.0(7) . . ?
C7 C6 C1 109.8(8) . . ?
C6 C7 C4 111.1(9) . . ?
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 O4 1.704(4) . ?
Re1 O3 1.711(3) . ?
Re1 O1 1.713(4) . ?
Re1 O2 1.723(3) . ?
N1 C8 1.472(10) . ?
N1 C5 1.498(12) . ?
N1 C1 1.524(9) . ?
C1 C3 1.499(12) . ?
C1 C6 1.712(15) . ?
C2 C4 1.476(12) . ?
C2 C3 1.517(13) . ?
C4 C5 1.414(10) . ?
C4 C7 1.502(14) . ?
C6 C7 1.392(12) . ?
