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_7132882
_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
'C51 H32 Fe2 N10 O, 7[H2O], 6[C5H11NO], 1[C2H6O]'
_chemical_formula_sum            'C83 H118 Fe2 N16 O15'
_chemical_formula_weight         1691.63
_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             2023-07-17
_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                   19.818(2)
_cell_length_b                   29.050(3)
_cell_length_c                   16.4847(18)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      26.10
_cell_measurement_theta_min      2.34
_cell_volume                     9490.5(17)
_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      120.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.985
_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  0.0953
_diffrn_reflns_av_unetI/netI     0.0916
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37621
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.009
_diffrn_reflns_theta_min         1.869
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.371
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1154 before and 0.0722 after correction.
The Ratio of minimum to maximum transmission is 0.7242.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_description       block
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.191
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.131
_refine_diff_density_max         1.122
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         6128
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0778
_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^)+(0.1527P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2378
_refine_ls_wR_factor_ref         0.2545
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3882
_reflns_number_total             6128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00673a2.cif
_cod_data_source_block           230331a_0m
_cod_depositor_comments
'Adding full bibliography for 7132879--7132883.cif.'
_cod_original_cell_volume        9490.4(18)
_cod_database_code               7132882
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.932
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Fixed Sof: C5A(0.5) H5A(0.5) C6A(0.5) H6A(0.5) C8A(0.5) H8A(0.5) C7A(0.5)
 H7A(0.5) C13(0.5) H13(0.5) C14(0.5) H14(0.5) C12(0.5) H12(0.5) C11(0.5)
 H11(0.5) C7(0.5) H7(0.5) C8(0.5) H8(0.5) C13A(0.5) H13A(0.5) C5(0.5) H5(0.5)
 C6(0.5) H6(0.5) C11A(0.5) H11A(0.5) C14A(0.5) H14A(0.5) C12A(0.5) H12A(0.5)
 N6(0.25) O1(0.25) N4(0.25) C4(0.25) C3(0.25) N5(0.25) N3(0.25) C2(0.25)
4.a Aromatic/amide H refined with riding coordinates:
 C5A(H5A), C6A(H6A), C8A(H8A), C7A(H7A), C13(H13), C14(H14), C12(H12),
 C11(H11), C7(H7), C8(H8), C13A(H13A), C5(H5), C6(H6), C11A(H11A), C14A(H14A),
 C12A(H12A)
4.b Fitted hexagon refined as free rotating group:
 N2(C5A,C6A,C9,C8A,C7A), C10(C13,C14,C15,C12,C11)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              94137
_shelx_fab_checksum              61695
_olex2_submission_special_instructions 'No special instructions were received'