Near-room-temperature dielectric switch and thermal expansion anomaly in a new hybrid crystal: (Me2NH2)[CsFe(CN)5(NO)]
Li, Qi-Yao; Li, Mao-Fan; Chen, Xiao-Xian; Gong, Ya-Ping; Liu, De-Xuan; Xu, Wei-Jian; Zhang, Wei-Xiong; CrystEngComm  (2022) –; doi:10.1039/D2CE00754A

data_7245134
_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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0388P)^2^+0.9483P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(I)'
_cod_data_source_file            d2ce00754a2.cif
_cod_data_source_block           new
_cod_database_code               7245134
_shelx_shelxl_version_number     2014/7
_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)
;
_shelx_res_checksum              20827
_olex2_submission_special_instructions 'No special instructions were received'