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_1574371
_publ_section_title
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 Switchable colossal anisotropic thermal expansion in a spin crossover
 framework
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_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, C3 H8 O'
_chemical_formula_sum            'C17 H17 Au2 Fe N7 O'
_chemical_formula_weight         785.16
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-03-12
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-03-17 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                   11.8527(7)
_cell_length_b                   17.0385(11)
_cell_length_c                   22.9573(16)
_cell_measurement_reflns_used    7340
_cell_measurement_temperature    298
_cell_measurement_theta_max      27.65
_cell_measurement_theta_min      2.74
_cell_volume                     4636.3(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      298
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            19100
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.335
_diffrn_reflns_theta_min         2.744
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.263
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0984 before and 0.0466 after correction.
The Ratio of minimum to maximum transmission is 0.6582.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.250
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.00040(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2876
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.200
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0086P)^2^+24.3407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0566
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2253
_reflns_number_total             2876
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc08032g2.cif
_cod_data_source_block           1Fe_298K
_cod_depositor_comments
'Adding full bibliography for 1574366--1574373.cif.'
_cod_original_sg_symbol_H-M      Ibca
_cod_database_code               1574371
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.534
_shelx_estimated_absorpt_t_min   0.345
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C10-C11
 1.45 with sigma of 0.02
 C9-C10
 1.45 with sigma of 0.02
 C10-O1
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C9 \\sim C10 \\sim C11 \\sim O1: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
Uanis(N5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C7B)=Sof(H7B)=Sof(C8B)=Sof(H8B)=1-FVAR(1)
 Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=FVAR(1)
 Fixed Sof: H4(0.5) N5(0.5) H5A(0.5) H5B(0.5) O1(0.5) H1(0.5) C9(0.5) H9A(0.5)
 H9B(0.5) H9C(0.5) C10(0.5) H10(0.5) C11(0.5) H11A(0.5) H11B(0.5) H11C(0.5)
5.a Riding coordinates:
 C11(H11A,H11B,H11C)
5.b Ternary CH refined with riding coordinates:
 C10(H10)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7B(H7B), C7A(H7A), C8B(H8B), C8A(H8A)
5.d X=CH2 refined with riding coordinates:
 N5(H5A,H5B)
5.e Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C)
5.f Idealised tetrahedral OH refined as rotating group:
 O1(H1)
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_olex2_submission_special_instructions 'No special instructions were received'