Hysteretic Four-Step Spin-Crossover in a 3D Hofmann-type Metal-Organic Framework with Aromatic Guest
Zhang, Cui-Juan; Lian, Kai-Ting; Huang, Guo-Zhang; Bala, Sukhen; Ni, Zhao-Ping; Tong, Ming-Liang; Chemical Communications  (2019) –; doi:10.1039/C9CC06017K

data_7124050
_publ_section_title
;
 Hysteretic Four-Step Spin-Crossover in a 3D Hofmann-type Metal-Organic
 Framework with Aromatic Guest
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC06017K
_journal_year                    2019
_chemical_formula_moiety         'C32 H16 Ag4 Fe2 N16 O2, 3(C10 H8)'
_chemical_formula_sum            'C62 H40 Ag4 Fe2 N16 O2'
_chemical_formula_weight         1584.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-30 deposited with the CCDC.    2019-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                67.038(4)
_cell_angle_beta                 90.558(4)
_cell_angle_gamma                64.872(4)
_cell_formula_units_Z            2
_cell_length_a                   15.5150(19)
_cell_length_b                   17.552(2)
_cell_length_c                   13.9024(16)
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    211(2)
_cell_measurement_theta_max      26.797
_cell_measurement_theta_min      2.409
_cell_volume                     3085.4(7)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      211.16
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-III CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0993
_diffrn_reflns_av_unetI/netI     0.0994
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            51532
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.599
_diffrn_reflns_theta_min         1.423
_exptl_absorpt_coefficient_mu    1.759
_exptl_absorpt_correction_T_max  0.0950
_exptl_absorpt_correction_T_min  0.0589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1045 before and 0.0793 after correction. The Ratio of minimum to maximum transmission is 0.6200. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.081
_refine_diff_density_max         2.908
_refine_diff_density_min         -3.449
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     769
_refine_ls_number_reflns         14107
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.1571
_refine_ls_R_factor_gt           0.1040
_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^)+(0.0853P)^2^+65.3088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2601
_refine_ls_wR_factor_ref         0.2843
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8925
_reflns_number_total             14107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc06017k2.cif
_cod_data_source_block           1-naph-211K
_cod_database_code               7124050
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.782
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 C40, C39
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C9, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C40 \\sim C39: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C9 \\sim C8: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(N16) = Uanis(C45)
4.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9), C13(H13), C14(H14), C15(H15), C16(H16),
 C36(H36), C37(H37), C39(H39), C40(H40), C44(H44), C45(H45), C46(H46), C47(H47),
  C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24),
 C25(H25), C27(H27), C28(H28), C29(H29), C30(H30), C48(H48), C49(H49), C50(H50),
  C51(H51), C53(H53), C54(H54), C55(H55), C56(H56), C58(H58), C59(H59),
 C60(H60), C61(H61)
;
_shelx_res_checksum              35338
_olex2_submission_special_instructions 'No special instructions were received'