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_7132883
_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             2023-11-22
_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                   20.623(2)
_cell_length_b                   29.230(3)
_cell_length_c                   17.010(2)
_cell_measurement_reflns_used    9852
_cell_measurement_temperature    298.00
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.31
_cell_volume                     10253.8(19)
_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      298.00
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.1083
_diffrn_reflns_av_unetI/netI     0.0726
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48274
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.106
_diffrn_reflns_theta_max         25.106
_diffrn_reflns_theta_min         1.837
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1724 before and 0.0984 after correction.
The Ratio of minimum to maximum transmission is 0.6017.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_description       block
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.221
_exptl_crystal_size_min          0.194
_refine_diff_density_max         0.995
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4954
_refine_ls_number_restraints     618
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1400
_refine_ls_R_factor_gt           0.1184
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0933P)^2^+59.9317P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2564
_refine_ls_wR_factor_ref         0.2682
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3894
_reflns_number_total             4954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00673a2.cif
_cod_data_source_block           230519o_0m
_cod_depositor_comments
'Adding full bibliography for 7132879--7132883.cif.'
_cod_original_cell_volume        10254(2)
_cod_database_code               7132883
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.897
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C5A \\sim C6A \\sim C8A \\sim C7A \\sim C5 \\sim C6 \\sim C8 \\sim C7: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C13 \\sim C14 \\sim C12A \\sim C11A \\sim C12 \\sim C11 \\sim C13A \\sim C14A:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
O1 \\sim N6 \\sim N3 \\sim C2 \\sim N4 \\sim C3 \\sim N5 \\sim C4: within 8A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 8A
C11A \\sim C12A \\sim C13 \\sim C14 \\sim C12 \\sim C11 \\sim C14A \\sim C13A
\\sim C15 \\sim C16 \\sim C10: within 5A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 5A
Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N3) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N5) \\sim
Ueq, Uanis(N3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
3. Others
 Fixed Sof: C7A(0.5) H7A(0.5) C8A(0.5) H8A(0.5) C7(0.5) H7(0.5) C13A(0.5)
 H13A(0.5) C11(0.5) H11(0.5) C6A(0.5) H6A(0.5) C8(0.5) H8(0.5) C14A(0.5)
 H14A(0.5) C12(0.5) H12(0.5) C13(0.5) H13(0.5) C11A(0.5) H11A(0.5) C12A(0.5)
 H12A(0.5) C14(0.5) H14(0.5) C5A(0.5) H5A(0.5) C5(0.5) H5(0.5) C6(0.5) H6(0.5)
 C3(0.25) C4(0.25) N6(0.25) N5(0.25) O1(0.25) N4(0.25) C2(0.25) N3(0.25)
4.a Aromatic/amide H refined with riding coordinates:
 C7A(H7A), C8A(H8A), C7(H7), C13A(H13A), C11(H11), C6A(H6A), C8(H8),
 C14A(H14A), C12(H12), C13(H13), C11A(H11A), C12A(H12A), C14(H14), C5A(H5A),
 C5(H5), C6(H6)
;
_shelx_res_checksum              10570
_shelx_fab_checksum              7494
_olex2_submission_special_instructions 'No special instructions were received'