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_7245133
_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         'C5 Cs Fe N6 O, 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           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-03-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-03-21 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                   8.3288(3)
_cell_length_b                   8.9675(3)
_cell_length_c                   17.7852(7)
_cell_measurement_reflns_used    8044
_cell_measurement_temperature    249.99(13)
_cell_measurement_theta_max      30.0960
_cell_measurement_theta_min      3.3040
_cell_volume                     1328.35(8)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      249.99(13)
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -41.00  17.00   1.00   13.59    --  -12.93 -77.00 -60.00   58
  2  \w    -43.00  18.00   1.00   13.59    --  -12.93  77.00  60.00   61
  3  \w      4.00  87.00   1.00   13.59    --   14.02  38.00 -60.00   83
  4  \w    -39.00  36.00   1.00   13.59    --   14.02 -77.00-180.00   75
  5  \w    -50.00  -2.00   1.00   13.59    --   14.02 -38.00 120.00   48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.912
_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       24
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12283
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.660
_diffrn_reflns_theta_min         3.226
_exptl_absorpt_coefficient_mu    3.832
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69760
_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    1.975
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.09(3)
_refine_ls_extinction_coef       0.00153(17)
_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   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         3607
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0204
_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^)+(0.0186P)^2^+0.3353P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0432
_refine_ls_wR_factor_ref         0.0443
_reflns_Friedel_coverage         0.746
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.909
_reflns_number_gt                3382
_reflns_number_total             3607
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00754a2.cif
_cod_data_source_block           a21042303a0249_250k
_cod_database_code               7245133
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.701
_shelx_estimated_absorpt_t_min   0.701
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H7A(0.056) H7B(0.056) H6A(0.073) H6B(0.073) H6C(0.073) H7C(0.103)
 H7D(0.103) H7E(0.103)
 Fixed X: H7A(0.3697) H7B(0.3678) H6A(0.4931) H6B(0.3243) H6C(0.4804)
 H7C(0.6369) H7D(0.6344) H7E(0.561)
 Fixed Y: H7A(0.0577) H7B(0.0428) H6A(-0.1642) H6B(-0.1782) H6C(-0.1809)
 H7C(0.0733) H7D(0.0576) H7E(0.1995)
 Fixed Z: H7A(0.4664) H7B(0.5468) H6A(0.4543) H6B(0.4927) H6C(0.5419)
 H7C(0.4649) H7D(0.5527) H7E(0.5144)
;
_shelx_res_checksum              49535
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;