Exceptional structural phase transition near room temperature in an organic-inorganic hybrid ferroelectric
Wang, Ping; Tong, Yu-Qiao; Yin, Shi Qing; Gu, Qian Jun; Huang, Bo; Zhu, Ai-Xin; Chemical Communications  (2023) –; doi:10.1039/D3CC04186G

data_7132248
_publ_section_title
;
 Exceptional structural phase transition near room temperature in an
 organic-inorganic hybrid ferroelectric
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC04186G
_journal_year                    2023
_chemical_formula_moiety         'Hg I4, 2(C8 H12 N)'
_chemical_formula_sum            'C16 H24 Hg I4 N2'
_chemical_formula_weight         952.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-09-20 deposited with the CCDC.	2023-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.809(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.663(3)
_cell_length_b                   8.316(3)
_cell_length_c                   13.502(4)
_cell_measurement_reflns_used    10866
_cell_measurement_temperature    270(2)
_cell_measurement_theta_max      27.58
_cell_measurement_theta_min      2.27
_cell_volume                     1183.1(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      270
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10520
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.622
_diffrn_reflns_theta_min         1.933
_exptl_absorpt_coefficient_mu    11.724
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ABSCOR
_exptl_crystal_colour            light
_exptl_crystal_density_diffrn    2.674
_exptl_crystal_description       block
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   0.096
_exptl_transmission_factor_min   0.075
_refine_diff_density_max         1.833
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.396(6)
_refine_ls_extinction_coef       0.0043(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         5261
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0243
_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^)+(0.0148P)^2^+1.1516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0602
_reflns_Friedel_coverage         0.872
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                5165
_reflns_number_total             5261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04186g2.cif
_cod_data_source_block           mo_b221207a_0m_b
_cod_original_cell_volume        1183.2(6)
_cod_database_code               7132248
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.096
_shelx_estimated_absorpt_t_min   0.075
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.604(6)
 0.396(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C1(H1D,H1E), C10(H10A,H10B), C2(H2D,H2E)
3.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C16(H16), C4(H4), C13(H13), C12(H12), C8(H8), C15(H15), C5(H5),
 C6(H6), C7(H7)
3.c Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N1(H1A,H1B,H1C)
;
_shelx_res_checksum              12859
_shelx_hkl_checksum              69781
_olex2_submission_special_instructions 'No special instructions were received'