Switchable colossal anisotropic thermal expansion in a spin crossover framework
Wu, Si-Guo; Cui, Wen; Ruan, Ze-Yu; Ni, Zhao-Ping; Tong, Ming-Liang; Chemical Science 16 (2025) 8845–8852; doi:10.1039/D4SC08032G

data_1574372
_publ_section_title
;
 Switchable colossal anisotropic thermal expansion in a spin crossover
 framework
;
_journal_issue                   20
_journal_name_full               'Chemical Science'
_journal_page_first              8845
_journal_page_last               8852
_journal_paper_doi               10.1039/D4SC08032G
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C14 H9 Au2 Fe N7, C4 H10 O'
_chemical_formula_sum            'C18 H19 Au2 Fe N7 O'
_chemical_formula_weight         799.18
_space_group_crystal_system      orthorhombic
_space_group_IT_number           73
_space_group_name_Hall           '-I 2b 2c'
_space_group_name_H-M_alt        'I b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2024-05-09
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-25 deposited with the CCDC.	2025-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.465(7)
_cell_length_b                   15.754(7)
_cell_length_c                   22.263(19)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    120.01
_cell_measurement_theta_max      27.14
_cell_measurement_theta_min      2.77
_cell_volume                     4372(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.01
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_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  0.0489
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            23211
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.138
_diffrn_reflns_theta_min         2.586
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.068
_exptl_absorpt_correction_T_max  0.6941
_exptl_absorpt_correction_T_min  0.2503
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1258 before and 0.0702 after correction.
The Ratio of minimum to maximum transmission is 0.3606.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.428
_exptl_crystal_description       block
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.185
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2407
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+15.7435P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1140
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2060
_reflns_number_total             2407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc08032g2.cif
_cod_data_source_block           final
_cod_depositor_comments
'Adding full bibliography for 1574366--1574373.cif.'
_cod_database_code               1574372
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.334
_shelx_estimated_absorpt_t_min   0.181
_olex2_refinement_description
;
1. Shared sites
{C11, O1}
2. Uiso/Uaniso restraints and constraints
C10 \\sim C9 \\sim C11 \\sim O1: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(C11) = Uanis(O1)
3. Others
 Fixed Sof: H4(0.5) N5(0.5) H5A(0.5) H5B(0.5) C11(0.5) H11A(0.5) H11B(0.5)
 H11C(0.5) O1(0.5) H1(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8)
4.b X=CH2 refined with riding coordinates:
 N5(H5A,H5B)
4.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C)
4.d Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_olex2_submission_special_instructions 'No special instructions were received'