Spin-Crossover Modulation via Single-Crystal to Single-Crystal Photochemical [2+2] Reaction in Hofmann-Type Frameworks
Wang, Long-Fei; Zhuang, Wei-Man; Guo-Zhang, Huang; Chen, Yan-Cong; Qiu, Jiang-Zhen; Ni, Zhao-Ping; Tong, Ming-Liang; Chemical Science  (2019) –; doi:10.1039/C9SC02274K

data_1551945
_publ_section_title
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 Spin-Crossover Modulation via Single-Crystal to Single-Crystal
 Photochemical [2+2] Reaction in Hofmann-Type Frameworks
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_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02274K
_journal_year                    2019
_chemical_formula_moiety         '0.5(C60 H44 Ag4 Fe2 N12)'
_chemical_formula_sum            'C30 H22 Ag2 Fe N6'
_chemical_formula_weight         738.12
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-11-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-18 deposited with the CCDC.    2019-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3342(6)
_cell_length_b                   14.4997(7)
_cell_length_c                   15.8603(8)
_cell_measurement_reflns_used    8451
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.52
_cell_volume                     2836.5(2)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22470
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.534
_diffrn_reflns_theta_min         2.568
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.902
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0695 before and 0.0526 after correction. The Ratio of minimum to maximum transmission is 0.9072. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.061
_refine_diff_density_max         0.707
_refine_diff_density_min         -1.482
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3245
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0171P)^2^+7.9177P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0742
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2619
_reflns_number_total             3245
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02274k2.cif
_cod_data_source_block           120k
_cod_database_code               1551945
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.893
_shelx_estimated_absorpt_t_min   0.774
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{N1, N1A}
3. Uiso/Uaniso restraints and constraints
Uanis(C5A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1) = Uanis(N1A)
Uanis(C1) = Uanis(C1A)
Uanis(C2) = Uanis(C2A)
Uanis(C3) = Uanis(C3A)
Uanis(C4) = Uanis(C4A)
Uanis(C5) = Uanis(C5A)
Uanis(C6) = Uanis(C6A)
Uanis(C7) = Uanis(C7A)
Uanis(C8) = Uanis(C8A)
Uanis(C9) = Uanis(C9A)
Uanis(C10) = Uanis(C10A)
Uanis(C11) = Uanis(C11A)
Uanis(C12) = Uanis(C12A)
Uanis(C13) = Uanis(C13A)
4. Same fragment restrains
{N1A, C1A, C2A, C3A, C4A, C5A} sigma for 1-2: 0.02, 1-3: 0.04
{N1, C5, C4, C3, C2, C1} sigma for 1-2: 0.02, 1-3: 0.04
as
{N1, C1, C2, C3, C4, C5}
5. Others
 Fixed Sof: N1(0.66) C1(0.66) H1(0.66) C2(0.66) H2(0.66) C3(0.66) C4(0.66)
 H4(0.66) C5(0.66) H5(0.66) C6(0.66) H6(0.66) C7(0.66) H7(0.66) C8(0.66)
 C9(0.66) H9(0.66) C10(0.66) H10(0.66) C11(0.66) H11(0.66) C12(0.66) H12(0.66)
 C13(0.66) H13(0.66) N1A(0.34) C1A(0.34) H1A(0.34) C2A(0.34) H2A(0.34)
 C3A(0.34) C4A(0.34) H4A(0.34) C5A(0.34) H5A(0.34) C6A(0.34) H6A(0.34)
 C7A(0.34) H7A(0.34) C8A(0.34) C9A(0.34) H9A(0.34) C10A(0.34) H10A(0.34)
 C11A(0.34) H11A(0.34) C12A(0.34) H12A(0.34) C13A(0.34) H13A(0.34)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C1A(H1A), C2A(H2A), C4A(H4A), C5A(H5A), C6A(H6A), C7A(H7A),
  C9A(H9A), C10A(H10A), C11A(H11A), C12A(H12A), C13A(H13A)
6.b Fitted hexagon refined as free rotating group:
 C8(C9,C10,C11,C12,C13), C8A(C9A,C10A,C11A,C12A,C13A)
;
_shelx_res_checksum              65283
_olex2_submission_special_instructions 'No special instructions were received'