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#$Date: 2022-07-01 01:36:09 +0300 (Fri, 01 Jul 2022) $
#$Revision: 276458 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/51/7245134.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_7245134
loop_
_publ_author_name
'Li, Qi-Yao'
'Li, Mao-Fan'
'Chen, Xiao-Xian'
'Gong, Ya-Ping'
'Liu, De-Xuan'
'Xu, Wei-Jian'
'Zhang, Wei-Xiong'
_publ_section_title
;
 Near-room-temperature dielectric switch and thermal expansion anomaly in
 a new hybrid crystal: (Me2NH2)[CsFe(CN)5(NO)]
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00754A
_journal_year                    2022
_chemical_formula_moiety         '0.25(C20 Cs4 Fe4 N24 O4), C2 H8 N'
_chemical_formula_sum            'C7 H8 Cs Fe N7 O'
_chemical_formula_weight         394.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-B 2b 2'
_space_group_name_H-M_alt        'B m m b'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-06-15 deposited with the CCDC.	2022-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2860(3)
_cell_length_b                   9.0586(4)
_cell_length_c                   18.0168(7)
_cell_measurement_reflns_used    8044
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.0960
_cell_measurement_theta_min      3.3040
_cell_volume                     1352.33(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            6738
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.995
_diffrn_reflns_theta_min         2.706
_exptl_absorpt_coefficient_mu    3.764
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.940
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.806
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       0.0018(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1108
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0388P)²+0.9483P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0712
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1005
_reflns_number_total             1108
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ce00754a2.cif
_cod_data_source_block           new
_cod_database_code               7245134
_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.
;
_shelx_estimated_absorpt_t_max   0.705
_shelx_estimated_absorpt_t_min   0.705
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N4-C4 = N4-C3
 1.5 with sigma of 0.02
 C4-C3
 2.55 with sigma of 0.02
 C1-N1 \\sim C1'-N1'
 with sigma of 0.02
 Fe1-N1 \\sim Fe1-N1'
 with sigma of 0.04
 Cs1-N1 \\sim Cs1-N1'
 with sigma of 0.02
 Cs1-C1 \\sim Cs1-C1'
 with sigma of 0.04
 Fe1-C1 \\sim Fe1-C1'
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C3 \\sim N4 \\sim C4: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(N1') \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C1') \\sim Ueq, Uanis(N1)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 C1, N1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N1', C1'
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C1')=Sof(N1')=1-FVAR(1)
 Sof(C1)=Sof(N1)=FVAR(1)
 Fixed Sof: C3(0.25) H3A(0.25) H3B(0.25) H3C(0.25) N4(0.25) H4A(0.25)
 H4B(0.25) C4(0.25) H4C(0.25) H4D(0.25) H4E(0.25)
6.a Secondary CH2 refined with riding coordinates:
 N4(H4A,H4B)
6.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4C,H4D,H4E)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z'
'x, -y, -z'
'-x, y+1/2, -z'
'x+1/2, y, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'-x, y, z'
'x, -y-1/2, z'
'-x+1/2, -y, -z+1/2'
'x+1/2, y-1/2, -z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, -y-1/2, z+1/2'
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
Cs1 Cs 0.0000 -0.2500 0.55922(2) 0.04807(14) Uani 1 4 d DS T P . .
Fe1 Fe 0.5000 0.2500 0.58570(3) 0.03355(16) Uani 1 4 d DS T P . .
O1 O 0.5000 0.2500 0.4315(2) 0.097(2) Uani 1 4 d S T P . .
C2 C 0.5000 0.2500 0.6933(3) 0.0447(10) Uani 1 4 d S T P A .
N3 N 0.5000 0.2500 0.4945(2) 0.0520(10) Uani 1 4 d S T P A .
C1 C 0.3495(11) 0.0870(10) 0.5910(8) 0.057(2) Uani 0.529(18) 1 d D U . A 1
N2 N 0.5000 0.2500 0.7569(3) 0.0789(19) Uani 1 4 d S T P . .
N1 N 0.2011(10) 0.0495(13) 0.5979(4) 0.078(3) Uani 0.529(18) 1 d D U . A 1
C3 C 0.438(3) -0.355(4) 0.7545(12) 0.083(6) Uani 0.25 1 d D U . B -1
H3A H 0.5032 -0.4177 0.7238 0.124 Uiso 0.25 1 calc GR . . B -1
H3B H 0.3508 -0.3152 0.7257 0.124 Uiso 0.25 1 calc GR . . B -1
H3C H 0.3949 -0.4116 0.7951 0.124 Uiso 0.25 1 calc GR . . B -1
C1' C 0.3169(11) 0.1231(11) 0.5974(8) 0.052(2) Uani 0.471(18) 1 d D U . A 2
N1' N 0.2693(14) -0.0112(10) 0.6008(6) 0.082(3) Uani 0.471(18) 1 d D U . A 2
N4 N 0.535(2) -0.236(3) 0.7832(6) 0.111(6) Uani 0.25 1 d D U . B -1
H4A H 0.4766 -0.1923 0.8182 0.133 Uiso 0.25 1 calc R . . B -1
H4B H 0.6187 -0.2780 0.8061 0.133 Uiso 0.25 1 calc R . . B -1
C4 C 0.599(4) -0.122(4) 0.7377(15) 0.102(8) Uani 0.25 1 d D U . B -1
H4C H 0.5624 -0.1352 0.6876 0.152 Uiso 0.25 1 calc GR . . B -1
H4D H 0.7149 -0.1260 0.7389 0.152 Uiso 0.25 1 calc GR . . B -1
H4E H 0.5633 -0.0281 0.7559 0.152 Uiso 0.25 1 calc GR . . B -1
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'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'
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
N2 Cs1 N1 138.94(18) 13_556 10_556 y
N2 Cs1 N1 138.94(18) 13_556 4_546 y
N2 Cs1 N1 138.94(18) 13_556 9_556 y
N1 Cs1 N2 77.67(13) 11 13_556 y
N1 Cs1 N2 77.67(14) . 13_556 y
N1 Cs1 N2 77.67(13) 2_545 13_556 y
N1 Cs1 N2 77.67(13) 12 13_556 y
N1 Cs1 N1 112.7(4) 2_545 11 y
N1 Cs1 N1 109.69(16) . 10_556 y
N1 Cs1 N1 82.1(4) 10_556 9_556 y
N1 Cs1 N1 112.7(4) . 12 y
N1 Cs1 N1 142.3(2) 11 10_556 y
N1 Cs1 N1 62.0(3) 12 10_556 y
N1 Cs1 N1 155.3(3) . 2_545 y
N1 Cs1 N1 52.71(19) 4_546 10_556 y
N1 Cs1 N1 89.15(16) 2_545 10_556 y
N1 Cs1 N1 62.0(3) 11 9_556 y
N1 Cs1 N1 61.5(4) . 11 y
N1 Cs1 N1 61.5(4) 2_545 12 y
N1 Cs1 N1 155.3(3) 11 12 y
N1 Cs1 N1 89.15(16) . 9_556 y
N1 Cs1 N1 142.3(2) . 4_546 y
N1 Cs1 N1 142.3(2) 12 9_556 y
N1 Cs1 N1 62.0(3) 2_545 4_546 y
N1 Cs1 N1 57.9(3) 4_546 9_556 y
N1 Cs1 N1 109.69(16) 11 4_546 y
N1 Cs1 N1 89.15(16) 12 4_546 y
N1 Cs1 N1 109.69(16) 2_545 9_556 y
N1' Cs1 N2 76.46(18) 2_545 13_556 y
N1' Cs1 N2 76.46(18) 11 13_556 y
N1' Cs1 N2 76.46(18) 12 13_556 y
N1' Cs1 N2 76.46(18) . 13_556 y
N1' Cs1 N1' 152.9(4) . 2_545 y
N1' Cs1 N1' 152.9(4) 12 11 y
N1' Cs1 N1' 85.2(5) 2_545 11 y
N1' Cs1 N1' 88.5(5) 2_545 12 y
N1' Cs1 N1' 88.5(5) . 11 y
N1' Cs1 N1' 85.2(5) . 12 y
N3 Fe1 C2 180.0 . . y
N3 Fe1 C1 92.8(4) . . y
N3 Fe1 C1 92.8(4) . 2_655 y
N3 Fe1 C1 92.8(4) . 11_655 y
N3 Fe1 C1 92.8(4) . 12_565 y
N3 Fe1 C1' 96.3(4) . 2_655 y
N3 Fe1 C1' 96.3(4) . . y
N3 Fe1 C1' 96.3(4) . 11_655 y
N3 Fe1 C1' 96.3(4) . 12_565 y
C1 Fe1 C2 87.2(4) . . y
C1 Fe1 C2 87.2(4) 2_655 . y
C1 Fe1 C2 87.2(4) 12_565 . y
C1 Fe1 C2 87.2(4) 11_655 . y
C1 Fe1 C1 174.4(8) 11_655 12_565 y
C1 Fe1 C1 99.5(7) 2_655 11_655 y
C1 Fe1 C1 174.4(8) 2_655 . y
C1 Fe1 C1 99.5(7) 12_565 . y
C1 Fe1 C1 80.3(7) 11_655 . y
C1 Fe1 C1 80.3(7) 2_655 12_565 y
C1' Fe1 C2 83.7(4) 2_655 . y
C1' Fe1 C2 83.7(4) . . y
C1' Fe1 C2 83.7(4) 11_655 . y
C1' Fe1 C2 83.7(4) 12_565 . y
C1' Fe1 C1' 167.4(8) 2_655 . y
C1' Fe1 C1' 167.4(8) 11_655 12_565 y
C1' Fe1 C1' 73.8(7) 2_655 11_655 y
C1' Fe1 C1' 104.8(7) 2_655 12_565 y
C1' Fe1 C1' 73.8(7) 12_565 . y
C1' Fe1 C1' 104.8(7) 11_655 . y
N2 C2 Fe1 180.0 . . ?
O1 N3 Fe1 180.0 . . ?
N1 C1 Fe1 145.6(12) . . ?
C2 N2 Cs1 180.0 . 13_556 ?
Cs1 N1 Cs1 90.85(16) . 9_556 ?
C1 N1 Cs1 103.0(9) . 9_556 ?
C1 N1 Cs1 133.7(10) . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N4 C3 H3A 109.5 . . ?
N4 C3 H3B 109.5 . . ?
N4 C3 H3C 109.5 . . ?
N1' C1' Fe1 145.1(12) . . ?
C1' N1' Cs1 147.9(11) . . ?
C3 N4 H4A 106.6 . . ?
C3 N4 H4B 106.6 . . ?
H4A N4 H4B 106.5 . . ?
C4 N4 C3 123.1(13) . . ?
C4 N4 H4A 106.6 . . ?
C4 N4 H4B 106.6 . . ?
N4 C4 H4C 109.5 . . ?
N4 C4 H4D 109.5 . . ?
N4 C4 H4E 109.5 . . ?
H4C C4 H4D 109.5 . . ?
H4C C4 H4E 109.5 . . ?
H4D C4 H4E 109.5 . . ?
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
Cs1 N2 3.314(5) 13_556 y
Cs1 N1 3.259(7) . y
Cs1 N1 3.753(10) 4_546 y
Cs1 N1 3.259(7) 12 y
Cs1 N1 3.259(7) 2_545 y
Cs1 N1 3.753(10) 10_556 y
Cs1 N1 3.259(7) 11 y
Cs1 N1 3.753(10) 9_556 y
Cs1 N1' 3.196(7) 12 y
Cs1 N1' 3.196(7) . y
Cs1 N1' 3.196(7) 2_545 y
Cs1 N1' 3.196(7) 11 y
Fe1 C2 1.939(5) . y
Fe1 N3 1.643(4) . y
Fe1 C1 1.935(7) 12_565 y
Fe1 C1 1.935(7) 2_655 y
Fe1 C1 1.935(7) . y
Fe1 C1 1.935(7) 11_655 y
Fe1 C1' 1.915(7) 11_655 y
Fe1 C1' 1.915(7) 2_655 y
Fe1 C1' 1.915(7) 12_565 y
Fe1 C1' 1.915(7) . y
O1 N3 1.136(6) . ?
C2 N2 1.145(7) . ?
C1 N1 1.282(10) . ?
N2 Cs1 3.314(5) 13_556 y
N1 Cs1 3.753(10) 9_556 y
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C3 N4 1.439(16) . ?
C1' N1' 1.280(11) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 C4 1.423(16) . ?
C4 H4C 0.9600 . ?
C4 H4D 0.9600 . ?
C4 H4E 0.9600 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 C1 N1 Cs1 160.2(11) . . . . ?
Fe1 C1 N1 Cs1 56(2) . . . 9_556 ?
Fe1 C1' N1' Cs1 -141.8(13) . . . . ?
