#------------------------------------------------------------------------------
#$Date: 2022-02-04 21:22:11 +0200 (Fri, 04 Feb 2022) $
#$Revision: 272621 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/41/7244199.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_7244199
loop_
_publ_author_name
'Wan, Min'
'Wang, Yan-Ning'
'Liu, Jing-Yuan'
'Tong, Liang'
'Ye, Si-Yu'
'Li, Jun-Yi'
'Chen, Li-Zhuang'
_publ_section_title
;
 High temperature molecular-based phase transition compounds with tunable
 and switchable dielectric properties
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              782
_journal_page_last               787
_journal_paper_doi               10.1039/D1CE01488A
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety         '2(O4 Re), C8 H17 Cl N2'
_chemical_formula_sum            'C8 H17 Cl N2 O8 Re2'
_chemical_formula_weight         677.09
_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   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-08-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-29 deposited with the CCDC.	2021-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                91.289(2)
_cell_angle_beta                 94.366(2)
_cell_angle_gamma                96.252(2)
_cell_formula_units_Z            4
_cell_length_a                   8.8362(5)
_cell_length_b                   12.7362(5)
_cell_length_c                   13.7512(5)
_cell_measurement_reflns_used    5138
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.488
_cell_measurement_theta_min      2.973
_cell_volume                     1533.15(12)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0428
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13422
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.33
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    15.988
_exptl_absorpt_correction_T_max  0.2722
_exptl_absorpt_correction_T_min  0.2304
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    2.933
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         4.018
_refine_diff_density_min         -2.922
_refine_diff_density_rms         0.434
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6962
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0317P)²+96.1882P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1601
_refine_ls_wR_factor_ref         0.1649
_reflns_number_gt                5786
_reflns_number_total             6962
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1ce01488a2.cif
_cod_data_source_block           ClEtdabcoReO4
_cod_depositor_comments
'Adding full bibliography for 7244198--7244201.cif.'
_cod_database_code               7244199
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
2. Restrained distances
 C36-C1
 1.54 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 N3(H3), N1(H1)
3.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C16(H16A,H16B), C17(H17A,H17B), C25(H25A,H25B), C26(H26A,
 H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C31(H31A,H31B),
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
  C39(H39A,H39B), C1(H1A,H1B)
;
_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'
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Re1 Re 0.46053(8) 0.17903(6) 0.47333(5) 0.02501(17) Uani 1 d . . .
Re2 Re 0.03796(8) 0.33607(6) 0.50435(5) 0.02625(18) Uani 1 d . . .
Re3 Re 0.49206(8) 0.20250(6) 0.04716(5) 0.02480(17) Uani 1 d . . .
Re4 Re 0.03062(8) 0.67892(6) 0.98854(5) 0.02346(17) Uani 1 d . . .
Cl2 Cl -0.3481(6) 1.0957(5) 0.7476(4) 0.0442(12) Uani 1 d . . .
Cl7 Cl 0.8574(7) 0.7026(4) 0.2256(5) 0.0522(15) Uani 1 d . . .
N4 N 0.5197(16) 0.5277(11) 0.2234(9) 0.020(3) Uani 1 d . . .
N3 N 0.2792(16) 0.5236(12) 0.3117(10) 0.024(3) Uani 1 d . . .
H3 H 0.1936 0.5221 0.3447 0.029 Uiso 1 calc . . R
O7 O -0.1328(16) 0.5942(12) 0.9953(11) 0.045(4) Uani 1 d . . .
N2 N -0.0110(15) 0.9654(10) 0.7748(9) 0.018(3) Uani 1 d . . .
O11 O 0.5636(16) 0.2985(11) 0.4649(11) 0.042(4) Uani 1 d . . .
O6 O 0.1077(17) 0.6510(11) 0.8818(10) 0.039(3) Uani 1 d . . .
O9 O 0.4240(16) 0.1547(10) 0.5930(9) 0.035(3) Uani 1 d . . .
N1 N 0.2368(17) 0.9694(13) 0.6929(11) 0.029(3) Uani 1 d . . .
H1 H 0.3252 0.9707 0.6628 0.035 Uiso 1 calc . . R
C12 C 0.115(2) 1.0134(15) 0.6248(13) 0.028(4) Uani 1 d . . .
H12A H 0.1549 1.0814 0.6013 0.033 Uiso 1 calc . . R
H12B H 0.0862 0.9656 0.5690 0.033 Uiso 1 calc . . R
O14 O -0.016(2) 0.2036(12) 0.5227(12) 0.054(4) Uani 1 d . . .
O16 O 0.024(2) 0.3583(12) 0.3813(10) 0.047(4) Uani 1 d . . .
O15 O 0.2255(17) 0.3684(13) 0.5505(11) 0.048(4) Uani 1 d . . .
C16 C 0.401(2) 0.4740(17) 0.3715(13) 0.031(4) Uani 1 d . . .
H16A H 0.3576 0.4075 0.3963 0.037 Uiso 1 calc . . R
H16B H 0.4403 0.5204 0.4266 0.037 Uiso 1 calc . . R
C17 C -0.0227(18) 1.0255(15) 0.6820(11) 0.023(3) Uani 1 d . . .
H17A H -0.0276 1.0996 0.6974 0.027 Uiso 1 calc . . R
H17B H -0.1153 0.9987 0.6428 0.027 Uiso 1 calc . . R
O5 O 0.1558(18) 0.6635(12) 1.0875(11) 0.045(4) Uani 1 d . . .
O13 O -0.0796(18) 0.4104(12) 0.5644(12) 0.049(4) Uani 1 d . . .
O10 O 0.5714(19) 0.0859(12) 0.4341(12) 0.050(4) Uani 1 d . . .
O4 O 0.507(2) 0.3195(13) -0.0145(13) 0.055(5) Uani 1 d . . .
O12 O 0.2934(18) 0.1737(17) 0.4002(12) 0.064(5) Uani 1 d . . .
C25 C -0.161(2) 0.9561(15) 0.8231(14) 0.031(4) Uani 1 d . . .
H25A H -0.2359 0.9109 0.7814 0.037 Uiso 1 calc . . R
H25B H -0.1458 0.9203 0.8840 0.037 Uiso 1 calc . . R
C26 C 0.1216(17) 1.0167(14) 0.8427(12) 0.022(3) Uani 1 d . . .
H26A H 0.1407 0.9715 0.8971 0.027 Uiso 1 calc . . R
H26B H 0.0970 1.0838 0.8685 0.027 Uiso 1 calc . . R
C27 C 0.265(2) 1.0343(14) 0.7850(13) 0.029(4) Uani 1 d . . .
H27A H 0.2850 1.1085 0.7704 0.035 Uiso 1 calc . . R
H27B H 0.3527 1.0137 0.8234 0.035 Uiso 1 calc . . R
C28 C 0.242(2) 0.4649(14) 0.2152(14) 0.029(4) Uani 1 d . . .
H28A H 0.1517 0.4879 0.1816 0.035 Uiso 1 calc . . R
H28B H 0.2238 0.3895 0.2249 0.035 Uiso 1 calc . . R
C29 C 0.3793(19) 0.4893(14) 0.1562(12) 0.023(3) Uani 1 d . . .
H29A H 0.3589 0.5432 0.1098 0.028 Uiso 1 calc . . R
H29B H 0.3975 0.4262 0.1200 0.028 Uiso 1 calc . . R
O3 O 0.350(2) 0.1145(15) -0.0103(14) 0.064(5) Uani 1 d . . .
C31 C 0.499(2) 0.6378(14) 0.2595(13) 0.029(4) Uani 1 d . . .
H31A H 0.5111 0.6874 0.2074 0.035 Uiso 1 calc . . R
H31B H 0.5738 0.6603 0.3130 0.035 Uiso 1 calc . . R
O1 O 0.450(2) 0.2286(14) 0.1649(12) 0.059(5) Uani 1 d . . .
O2 O 0.6604(19) 0.1474(12) 0.0512(12) 0.049(4) Uani 1 d . . .
C34 C 0.529(2) 0.4550(15) 0.3071(12) 0.030(4) Uani 1 d . . .
H34A H 0.6273 0.4695 0.3442 0.036 Uiso 1 calc . . R
H34B H 0.5175 0.3821 0.2833 0.036 Uiso 1 calc . . R
C35 C 0.3362(19) 0.6341(14) 0.2938(14) 0.028(4) Uani 1 d . . .
H35A H 0.3379 0.6769 0.3533 0.034 Uiso 1 calc . . R
H35B H 0.2691 0.6625 0.2443 0.034 Uiso 1 calc . . R
C36 C 0.0221(19) 0.8544(14) 0.7476(13) 0.030(4) Uani 1 d . . D
H36A H -0.0528 0.8237 0.6968 0.036 Uiso 1 calc . . R
H36B H 0.0161 0.8102 0.8040 0.036 Uiso 1 calc . . R
C37 C 0.814(2) 0.5631(14) 0.2172(14) 0.032(4) Uani 1 d . . .
H37A H 0.8927 0.5332 0.1837 0.038 Uiso 1 calc . . R
H37B H 0.8160 0.5360 0.2826 0.038 Uiso 1 calc . . R
C38 C 0.660(2) 0.5263(15) 0.1642(13) 0.030(4) Uani 1 d . . .
H38A H 0.6632 0.4546 0.1396 0.036 Uiso 1 calc . . R
H38B H 0.6465 0.5702 0.1082 0.036 Uiso 1 calc . . R
C39 C -0.227(2) 1.0554(19) 0.8443(13) 0.038(5) Uani 1 d . . .
H39A H -0.1446 1.1112 0.8599 0.045 Uiso 1 calc . . R
H39B H -0.2846 1.0461 0.9014 0.045 Uiso 1 calc . . R
O8 O -0.0150(17) 0.8067(11) 0.9891(10) 0.039(3) Uani 1 d . . .
C1 C 0.1811(19) 0.8602(14) 0.7119(14) 0.029(4) Uani 1 d . . D
H1A H 0.2500 0.8325 0.7608 0.035 Uiso 1 calc . . R
H1B H 0.1785 0.8171 0.6526 0.035 Uiso 1 calc . . R
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'
Cl Cl 0.1484 0.1585 '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
O11 Re1 O9 110.9(7) . . ?
O11 Re1 O10 106.6(8) . . ?
O11 Re1 O12 109.9(9) . . ?
O10 Re1 O9 108.4(7) . . ?
O12 Re1 O9 110.8(8) . . ?
O12 Re1 O10 110.2(9) . . ?
O16 Re2 O14 109.2(8) . . ?
O16 Re2 O15 109.1(8) . . ?
O16 Re2 O13 110.9(8) . . ?
O15 Re2 O14 109.3(8) . . ?
O13 Re2 O14 108.6(8) . . ?
O13 Re2 O15 109.7(8) . . ?
O3 Re3 O4 110.0(10) . . ?
O3 Re3 O1 109.7(8) . . ?
O1 Re3 O4 108.8(9) . . ?
O2 Re3 O4 110.6(8) . . ?
O2 Re3 O3 109.0(9) . . ?
O2 Re3 O1 108.6(9) . . ?
O7 Re4 O8 109.1(8) . . ?
O6 Re4 O7 108.1(7) . . ?
O6 Re4 O5 111.2(7) . . ?
O6 Re4 O8 109.7(7) . . ?
O5 Re4 O7 109.5(8) . . ?
O5 Re4 O8 109.2(7) . . ?
C29 N4 C38 107.9(12) . . ?
C31 N4 C29 106.8(13) . . ?
C31 N4 C38 112.3(13) . . ?
C34 N4 C29 108.6(13) . . ?
C34 N4 C31 110.3(13) . . ?
C34 N4 C38 110.7(13) . . ?
C16 N3 C28 110.1(14) . . ?
C35 N3 C16 109.0(14) . . ?
C35 N3 C28 108.9(13) . . ?
C17 N2 C25 111.3(12) . . ?
C17 N2 C26 109.9(12) . . ?
C17 N2 C36 107.4(13) . . ?
C26 N2 C25 112.2(13) . . ?
C36 N2 C25 107.7(13) . . ?
C36 N2 C26 108.3(12) . . ?
C27 N1 C12 110.1(14) . . ?
C1 N1 C12 107.5(14) . . ?
C1 N1 C27 111.1(14) . . ?
C17 C12 N1 108.1(13) . . ?
N3 C16 C34 108.9(13) . . ?
N2 C17 C12 109.9(13) . . ?
C39 C25 N2 117.3(15) . . ?
N2 C26 C27 108.8(13) . . ?
N1 C27 C26 108.5(13) . . ?
N3 C28 C29 106.7(13) . . ?
C28 C29 N4 110.1(13) . . ?
N4 C31 C35 107.5(14) . . ?
N4 C34 C16 107.6(14) . . ?
N3 C35 C31 109.1(14) . . ?
N2 C36 C1 108.8(13) . . ?
C38 C37 Cl7 114.0(13) . . ?
C37 C38 N4 116.8(15) . . ?
C25 C39 Cl2 114.0(15) . . ?
N1 C1 C36 110.2(14) . . ?
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 O11 1.698(14) . ?
Re1 O9 1.729(12) . ?
Re1 O10 1.721(13) . ?
Re1 O12 1.717(14) . ?
Re2 O14 1.732(15) . ?
Re2 O16 1.719(14) . ?
Re2 O15 1.732(15) . ?
Re2 O13 1.722(14) . ?
Re3 O4 1.729(14) . ?
Re3 O3 1.722(14) . ?
Re3 O1 1.723(15) . ?
Re3 O2 1.710(15) . ?
Re4 O7 1.716(13) . ?
Re4 O6 1.711(13) . ?
Re4 O5 1.716(14) . ?
Re4 O8 1.718(13) . ?
Cl2 C39 1.763(19) . ?
Cl7 C37 1.776(19) . ?
N4 C29 1.52(2) . ?
N4 C31 1.51(2) . ?
N4 C34 1.50(2) . ?
N4 C38 1.54(2) . ?
N3 C16 1.50(2) . ?
N3 C28 1.50(2) . ?
N3 C35 1.47(2) . ?
N2 C17 1.505(19) . ?
N2 C25 1.52(2) . ?
N2 C26 1.521(19) . ?
N2 C36 1.52(2) . ?
N1 C12 1.53(2) . ?
N1 C27 1.49(2) . ?
N1 C1 1.46(2) . ?
C12 C17 1.52(2) . ?
C16 C34 1.53(2) . ?
C25 C39 1.48(3) . ?
C26 C27 1.54(2) . ?
C28 C29 1.52(2) . ?
C31 C35 1.54(2) . ?
C36 C1 1.518(16) . ?
C37 C38 1.51(3) . ?
