An organic-inorganic hybrid ferroelastic with a near-room-temperature phase transition.
Bai, Yong-Ju; Qi, Jun-Chao; Hou, Ya-Ru; Xia, Zhang-Tian; Shen, Xin; Peng, Hang; Lu, Yan-Zi; Qin, Yan; Lv, Hui-Peng; Liao, Wei-Qiang; Dalton transactions (Cambridge, England : 2003) 54 (2025) 2386–2392; doi:10.1039/d4dt03193h

data_7717704
_publ_section_title
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 An organic-inorganic hybrid ferroelastic with a near-room-temperature
 phase transition.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2386
_journal_page_last               2392
_journal_paper_doi               10.1039/d4dt03193h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C16 H28 N4 O2, Br4 Zn'
_chemical_formula_sum            'C16 H28 Br4 N4 O2 Zn'
_chemical_formula_weight         693.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-11-11
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-11-12 deposited with the CCDC.	2024-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                70.636(2)
_cell_angle_beta                 86.5060(10)
_cell_angle_gamma                89.6140(10)
_cell_formula_units_Z            8
_cell_length_a                   10.1213(2)
_cell_length_b                   20.2424(3)
_cell_length_c                   25.7250(5)
_cell_measurement_reflns_used    41903
_cell_measurement_temperature    233.14
_cell_measurement_theta_max      73.9040
_cell_measurement_theta_min      2.3070
_cell_volume                     4962.62(17)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      233.14
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0874
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            84491
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.594
_diffrn_reflns_theta_max         66.594
_diffrn_reflns_theta_min         1.824
_diffrn_source                   'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.067
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear yellowish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.856
_exptl_crystal_description       needle
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.988
_refine_diff_density_min         -1.567
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     993
_refine_ls_number_reflns         17445
_refine_ls_number_restraints     266
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0671
_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^)+(0.1235P)^2^+27.3856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1983
_refine_ls_wR_factor_ref         0.2052
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14654
_reflns_number_total             17445
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03193h2.cif
_cod_data_source_block           EE_BPHDZnBr4_LTP
_cod_depositor_comments
'Adding full bibliography for 7717703--7717704.cif.'
_cod_original_cell_volume        4962.63(17)
_cod_database_code               7717704
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.464
_shelx_estimated_absorpt_t_min   0.264
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 Br5-Zn2 \\sim Br5A-Zn2
 with sigma of 0.02
 Zn1-Br3A \\sim Zn1-Br3B
 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Br3A \\sim Br4 \\sim Br2 \\sim Br1: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Br5 \\sim Br5A \\sim Zn2 \\sim Br6 \\sim Br7 \\sim Br8: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Br3A \\sim Br3B \\sim Br2 \\sim Zn1 \\sim Br4 \\sim Br1: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
5. Others
 Sof(Br5A)=1-FVAR(1)
 Sof(Br5)=FVAR(1)
 Sof(Br3B)=1-FVAR(2)
 Sof(Br3A)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 N5(H5), N8(H8A), N13(H13), N16(H16), N9(H9A), N12(H12), N1(H1), N4(H4)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C12(H12A,
 H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
 C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B),
  C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,
 H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B),
 C53(H53A,H53B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B),
  C64(H64A,H64B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,
 H20B), C21(H21A,H21B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
 C31(H31A,H31B), C32(H32A,H32B)
6.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), N6(H6), N7(H7A), C39(H39), C40(H40),
 C41(H41), C42(H42), N14(H14), N15(H15), C55(H55), C56(H56), C57(H57), C58(H58),
  N10(H10A), N11(H11), C23(H23), C24(H24), C25(H25), C26(H26), N2(H2), N3(H3)
;
_shelx_res_checksum              7148
_olex2_submission_special_instructions 'No special instructions were received'