Structural phase transition and dielectric relaxation in an organic-inorganic hybrid compound: [(CH3)3NH]4[Fe(SCN)6]Cl
Wang, Ping; Chen, Ming-Kun; Tong, Yu-Qiao; Yin, Shi-Qing; Huang, Bo; CrystEngComm  (2022) –; doi:10.1039/D2CE01150F

data_7245503
_publ_section_title
;
 Structural phase transition and dielectric relaxation in an
 organic-inorganic hybrid compound: [(CH3)3NH]4[Fe(SCN)6]Cl
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01150F
_journal_year                    2022
_chemical_formula_moiety         'C6 Fe N6 S6, Cl, 4(C3 H10 N1)'
_chemical_formula_sum            'C18 H40 Cl Fe N10 S6'
_chemical_formula_weight         680.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-08-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.806(2)
_cell_length_b                   16.361(3)
_cell_length_c                   17.171(3)
_cell_measurement_reflns_used    5863
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      3.32
_cell_volume                     3597.7(11)
_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      213(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_unetI/netI     0.0793
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9771
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.498
_diffrn_reflns_theta_min         3.182
_exptl_absorpt_coefficient_mu    0.866
_exptl_absorpt_correction_T_max  0.9053
_exptl_absorpt_correction_T_min  0.8626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ABSCOR
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       bulk
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   1.000
_exptl_transmission_factor_min   0.099
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.08(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3378
_refine_ls_number_restraints     280
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1668
_refine_ls_R_factor_gt           0.0805
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1303P)^2^+0.0799P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2031
_refine_ls_wR_factor_ref         0.2632
_reflns_Friedel_coverage         0.935
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                1498
_reflns_number_total             3378
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01150f3.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        3597.4(11)
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_database_code               7245503
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.08(9)
 -0.08(9)
2. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N4'-C4' \\sim N4'-C5' \\sim N4'-C6'
 with sigma of 0.02
 N4-C4 \\sim N4-C5 \\sim N4-C6
 with sigma of 0.02
 C4-C5 \\sim C4-C6 \\sim C5-C6 \\sim C4'-C5' \\sim C4'-C6' \\sim C5'-C6'
 with sigma of 0.02
 N5-C7 \\sim N5-C8 \\sim N5-C9 \\sim N5'-C7' \\sim N5'-C8' \\sim N5'-C9'
 with sigma of 0.02
 C7-C8 \\sim C8-C9 \\sim C7-C9 \\sim C7'-C8' \\sim C8'-C9' \\sim C7'-C9'
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
S1 \\sim S2 \\sim S3 \\sim N1 \\sim N2 \\sim N3 \\sim C1 \\sim C2 \\sim C3
\\sim Cl1 \\sim N4 \\sim C4 \\sim C5 \\sim C6 \\sim N4' \\sim C4' \\sim C5'
\\sim C6' \\sim N5 \\sim C7 \\sim C8 \\sim C9 \\sim N5' \\sim C7' \\sim C8':
within 2.2A with sigma of 0.04 and sigma for terminal atoms of 0.04
5. Others
 Fixed Sof: N4(0.7) H4(0.7) C4(0.7) H4A(0.7) H4B(0.7) H4C(0.7) C5(0.7)
 H5A(0.7) H5B(0.7) H5C(0.7) C6(0.7) H6A(0.7) H6B(0.7) H6C(0.7) N4'(0.3)
 H4'(0.3) C4'(0.3) H4'A(0.3) H4'B(0.3) H4'C(0.3) C5'(0.3) H5'A(0.3) H5'B(0.3)
 H5'C(0.3) C6'(0.3) H6'A(0.3) H6'B(0.3) H6'C(0.3) N5(0.5) H5(0.5) C7(0.5)
 H7A(0.5) H7B(0.5) H7C(0.5) C8(0.5) H8A(0.5) H8B(0.5) H8C(0.5) C9(0.5) H9A(0.5)
 H9B(0.5) H9C(0.5) N5'(0.5) H5'(0.5) C7'(0.5) H7'A(0.5) H7'B(0.5) H7'C(0.5)
 C8'(0.5) H8'A(0.5) H8'B(0.5) H8'C(0.5) C9'(0.5) H9'A(0.5) H9'B(0.5) H9'C(0.5)
6.a Ternary CH refined with riding coordinates:
 N4(H4), N4'(H4'), N5(H5), N5'(H5')
6.b Me refined with riding coordinates:
 C6'(H6'A,H6'B,H6'C)
6.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C4'(H4'A,H4'B,H4'C),
 C5'(H5'A,H5'B,H5'C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C7'(H7'A,H7'B,H7'C), C8'(H8'A,H8'B,H8'C), C9'(H9'A,H9'B,H9'C)
;
_shelx_res_checksum              27786
_shelx_hkl_checksum              33922
_olex2_submission_special_instructions 'No special instructions were received'