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_1574373
_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 N7 Zn, C3 H8 O'
_chemical_formula_sum            'C17 H17 Au2 N7 O Zn'
_chemical_formula_weight         794.68
_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             2025-03-17
_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                   11.2926(9)
_cell_length_b                   17.4255(14)
_cell_length_c                   22.7813(19)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    103.00
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.34
_cell_volume                     4482.9(6)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      103.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_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  0.0497
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            23436
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.342
_diffrn_reflns_theta_min         2.796
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.140
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1121 before and 0.0771 after correction.
The Ratio of minimum to maximum transmission is 0.6737.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.355
_exptl_crystal_description       block
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.106
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.062
_refine_diff_density_max         1.678
_refine_diff_density_min         -0.984
_refine_diff_density_rms         0.248
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2786
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+73.6143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0756
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2299
_reflns_number_total             2786
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc08032g2.cif
_cod_data_source_block           Zn_iPrOH_103K
_cod_depositor_comments
'Adding full bibliography for 1574366--1574373.cif.'
_cod_original_sg_symbol_H-M      Ibca
_cod_database_code               1574373
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.474
_shelx_estimated_absorpt_t_min   0.316
_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-O1
 1.45 with sigma of 0.02
 C11-C10
 1.45 with sigma of 0.02
 C10-C9
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1 \\sim C9 \\sim C10 \\sim C11: within 3A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 3A
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 Rotating group:
 N5(H5A,H5B)
5.b Ternary CH refined with riding coordinates:
 C10(H10)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7A(H7A), C8A(H8A), C7B(H7B), C8B(H8B)
5.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C)
5.e Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_olex2_submission_special_instructions 'No special instructions were received'