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_7124047
_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         'C16 H8 Ag2 Fe N8 O, 2(C7 H5)'
_chemical_formula_sum            'C30 H18 Ag2 Fe N8 O'
_chemical_formula_weight         778.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-03
_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                90
_cell_angle_beta                 107.917(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.695(3)
_cell_length_b                   13.6288(10)
_cell_length_c                   14.3844(10)
_cell_measurement_reflns_used    9832
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.69
_cell_volume                     5352.6(8)
_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      120.01
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0465
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            54075
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.517
_diffrn_reflns_theta_min         2.691
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.026
_exptl_absorpt_correction_T_max  0.0949
_exptl_absorpt_correction_T_min  0.0654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0852 before and 0.0521 after correction. The Ratio of minimum to maximum transmission is 0.6891. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_description       block
_exptl_crystal_F_000             3056
_exptl_crystal_size_max          0.109
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.069
_refine_diff_density_max         4.581
_refine_diff_density_min         -1.398
_refine_diff_density_rms         0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         6146
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0922
_refine_ls_R_factor_gt           0.0786
_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^)+(0.0307P)^2^+346.7917P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1784
_refine_ls_wR_factor_ref         0.1853
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5113
_reflns_number_total             6146
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc06017k2.cif
_cod_data_source_block           1-anth-120K
_cod_original_cell_volume        5352.6(7)
_cod_database_code               7124047
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.873
_shelx_estimated_absorpt_t_min   0.809
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C17-C23
 2.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C28 \\sim C27 \\sim C26 \\sim C25 \\sim C30 \\sim C29: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C21) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C24) \\sim Ueq,
Uanis(C23) \\sim Ueq, : with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C18) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C27) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C28) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Riding coordinates:
 C27(H27), C26(H26)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9), C13(H13), C14(H14), C15(H15), C16(H16),
 C19(H19), C20(H20), C17(H17), C18(H18), C23(H23), C24(H24), C25(H25), C28(H28),
  C31(H31)
4.c Fitted hexagon refined as free rotating group:
 C19(C20,C21,C22,C17,C18), C25(C30,C29,C28,C27,C26)
;
_shelx_res_checksum              72427
_olex2_submission_special_instructions 'No special instructions were received'