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_7124046
_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         'C64 H32 Ag8 Fe4 N32 O4, 6(C10 H8)'
_chemical_formula_sum            'C124 H80 Ag8 Fe4 N32 O4'
_chemical_formula_weight         3168.56
_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             2018-11-03
_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                67.033(2)
_cell_angle_beta                 76.138(2)
_cell_angle_gamma                87.708(3)
_cell_formula_units_Z            2
_cell_length_a                   27.8418(18)
_cell_length_b                   17.5236(14)
_cell_length_c                   13.7996(9)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    188(2)
_cell_measurement_theta_max      25.46
_cell_measurement_theta_min      2.44
_cell_volume                     6007.6(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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      188.12
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_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  0.1655
_diffrn_reflns_av_unetI/netI     0.1540
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            133997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.586
_diffrn_reflns_theta_min         2.264
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.807
_exptl_absorpt_correction_T_max  0.0949
_exptl_absorpt_correction_T_min  0.0631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0994 before and 0.0653 after correction.
The Ratio of minimum to maximum transmission is 0.6649.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_description       block
_exptl_crystal_F_000             3120
_exptl_crystal_size_max          0.079
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.045
_refine_diff_density_max         1.481
_refine_diff_density_min         -1.836
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1501
_refine_ls_number_reflns         27609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.2182
_refine_ls_R_factor_gt           0.0798
_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^)+(0.0096P)^2^+61.5636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1531
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10979
_reflns_number_total             27609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc06017k2.cif
_cod_data_source_block           1-naph-188K
_cod_database_code               7124046
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.923
_shelx_estimated_absorpt_t_min   0.870
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N13) = Uanis(C36)
Uanis(N21) = Uanis(C67)
Uanis(C15) = Uanis(C16)
Uanis(C78) = Uanis(C77)
Uanis(C88) = Uanis(C83)
Uanis(C109) = Uanis(C105)
Uanis(C108) = Uanis(C109)
Uanis(C25) = Uanis(C24)
3.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),
  C67(H67), C68(H68), C70(H70), C71(H71), C75(H75), C76(H76), C77(H77),
 C78(H78), C98(H98), C99(H99), C101(H101), C102(H102), C106(H106), C107(H107),
 C108(H108), C109(H109), 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), C79(H79), C80(H80), C81(H81), C82(H82),
  C84(H84), C85(H85), C86(H86), C87(H87), C89(H89), C90(H90), C91(H91),
 C92(H92), C110(H110), C111(H111), C112(H112), C113(H113), C115(H115),
 C116(H116), C117(H117), C118(H118), C120(H120), C121(H121), C122(H122),
 C123(H123)
;
_shelx_res_checksum              51924
_olex2_submission_special_instructions 'No special instructions were received'