Cyanometallic charge engineering in spin crossover metal-organic frameworks.
Lyu, Bang-Heng; Xie, Kai-Ping; Cui, Wen; Chen, Yan-Cong; Chen, Guan-Xi; Wu, Si-Guo; Tong, Ming-Liang; Chemical communications (Cambridge, England) 60 (2024) 4318–4321; doi:10.1039/d4cc00673a

data_7132879
_publ_section_title
;
 Cyanometallic charge engineering in spin crossover metal-organic
 frameworks.
;
_journal_issue                   32
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4318
_journal_page_last               4321
_journal_paper_doi               10.1039/d4cc00673a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C48 H32 Au Fe N6, Br, 1[H2O], 4.5[C2H2Cl4]'
_chemical_formula_sum            'C57 H43 Au Br Cl18 Fe N6 O'
_chemical_formula_weight         1798.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           65
_space_group_name_Hall           '-C 2 2'
_space_group_name_H-M_alt        'C m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-01-12 deposited with the CCDC.	2024-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0212(8)
_cell_length_b                   28.7967(13)
_cell_length_c                   16.6677(7)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    91.0
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.37
_cell_volume                     9609.7(7)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      91.00
_diffrn_measured_fraction_theta_full 0.998
_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  0.0424
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50587
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.896
_diffrn_reflns_theta_min         1.740
_exptl_absorpt_coefficient_mu    2.623
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0759 before and 0.0630 after correction.
The Ratio of minimum to maximum transmission is 0.7992.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_description       block
_exptl_crystal_F_000             3524
_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.192
_exptl_crystal_size_min          0.155
_refine_diff_density_max         3.081
_refine_diff_density_min         -1.756
_refine_diff_density_rms         0.152
_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     204
_refine_ls_number_reflns         6171
_refine_ls_number_restraints     258
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0937P)^2^+68.0571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1620
_refine_ls_wR_factor_ref         0.1641
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5626
_reflns_number_total             6171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00673a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7132879--7132883.cif.'
_cod_database_code               7132879
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.687
_shelx_estimated_absorpt_t_min   0.548
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 C7, C12, C11, C10, C9, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C5A, C4A, N2, C2A, C3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C7, C12, C10A, C11A, C9A, C8A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, N2, C4, C2, C5, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Br1B \\sim Br1A \\sim Br1: within 1.7A with sigma of 0.005 and sigma for
terminal atoms of 0.001 within 1.7A
C3A \\sim C2A \\sim C4A \\sim C5A \\sim C6 \\sim N2: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C9 \\sim C8 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C10A \\sim C11A \\sim C9A \\sim C8A \\sim C12: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C3 \\sim C2 \\sim C5 \\sim C4 \\sim C6 \\sim N2: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
C7 \\sim C10A \\sim C11A \\sim C12 \\sim C9A \\sim C8A \\sim C10 \\sim C11
\\sim C9 \\sim C8: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
4. Others
 Fixed Sof: C3(0.5) H3(0.5) C2(0.5) H2(0.5) C4(0.5) H4(0.5) C5(0.5) H5(0.5)
 C5A(0.5) H5A(0.5) C4A(0.5) H4A(0.5) C2A(0.5) H2A(0.5) C3A(0.5) H3A(0.5)
 C10A(0.5) H10A(0.5) C11A(0.5) H11A(0.5) C9A(0.5) H9A(0.5) C8A(0.5) H8A(0.5)
 C10(0.5) H10(0.5) C11(0.5) H11(0.5) C9(0.5) H9(0.5) C8(0.5) H8(0.5)
 Br1(0.0625) Br1A(0.0625) Br1B(0.125)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C4(H4), C5(H5), C5A(H5A), C4A(H4A), C2A(H2A), C3A(H3A),
 C10A(H10A), C11A(H11A), C9A(H9A), C8A(H8A), C10(H10), C11(H11), C9(H9), C8(H8)
5.b Fitted hexagon refined as free rotating group:
 C6(C3,C2,N2,C4,C5), C7(C10A,C11A,C12,C9A,C8A)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1562 electrons were 
found in a volume of 5686\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[H2O], 4[C2H2Cl4] per Formula Unit 
which account for 1352 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              53417
_shelx_fab_checksum              26647
_olex2_submission_special_instructions 'No special instructions were received'