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_1551947
_publ_section_title
;
 Spin-Crossover Modulation via Single-Crystal to Single-Crystal
 Photochemical [2+2] Reaction in Hofmann-Type Frameworks
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02274K
_journal_year                    2019
_chemical_formula_moiety         'C14 H10 Ag Fe0.5 N4'
_chemical_formula_sum            'C14 H10 Ag Fe0.5 N4'
_chemical_formula_weight         370.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-11-05
_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                 122.644(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.296(5)
_cell_length_b                   16.684(9)
_cell_length_c                   12.654(7)
_cell_measurement_reflns_used    3310
_cell_measurement_temperature    300
_cell_measurement_theta_max      27.605
_cell_measurement_theta_min      2.268
_cell_volume                     1474.8(15)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      300
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0912
_diffrn_reflns_av_unetI/netI     0.0764
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12007
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         2.441
_exptl_absorpt_coefficient_mu    1.831
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5554
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1357 before and 0.0774 after correction. The Ratio of minimum to maximum transmission is 0.7449. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'light gray'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    gray
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.987
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2731
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1591
_refine_ls_R_factor_gt           0.0908
_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^)+(0.0977P)^2^+13.3905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2161
_refine_ls_wR_factor_ref         0.2666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1500
_reflns_number_total             2731
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02274k2.cif
_cod_data_source_block           a_CCDC3
_cod_original_cell_volume        1474.9(14)
_cod_original_formula_sum        'C14 H10 Ag Fe0.50 N4'
_cod_database_code               1551947
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.827
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N3-C7A = C6A-C5 = C4A-C3A
 1.39 with sigma of 0.002
 C7A-C6A = C5-C4A = C3A-N3
 1.39 with sigma of 0.002
 C3A-C6A = C7A-C4A
 2.78 with sigma of 0.002
 C10-C9 \\sim C9-C10A
 with sigma of 0.01
 N4-C9 \\sim C9-C11
 with sigma of 0.02
3. Restrained planarity
 C7A, N3, C6A, C5, C4A, C3A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C4A) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C7A)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C7A) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C3A)
\\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
Uanis(C10) \\sim Ueq, Uanis(C10A) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C11A)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(N4) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C14A) \\sim Ueq, Uanis(N4A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C13) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C12A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7A) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C3A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7A) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C4A)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C10) = Uanis(C11) = Uanis(C12) = Uanis(C13) = Uanis(C14) = Uanis(N4)
Uanis(C10A) = Uanis(C11A) = Uanis(C12A) = Uanis(C13A) = Uanis(C14A) = Uanis(N4A)
Uanis(C3A) = Uanis(C4A) = Uanis(C6A) = Uanis(C7A)
5. Others
 Fixed Sof: C7(0.5) H7(0.5) C6(0.5) H6(0.5) C4(0.5) H4(0.5) C3(0.5) H3(0.5)
 H9B(0.5) H9A(0.5) C10A(0.5) N4A(0.5) C14A(0.5) H14A(0.5) C13A(0.5) H13A(0.5)
 C12A(0.5) H12A(0.5) C11A(0.5) H11A(0.5) C7A(0.5) H7A(0.5) C6A(0.5) H6A(0.5)
 C4A(0.5) H4A(0.5) C3A(0.5) H3A(0.5) C10(0.5) N4(0.5) C14(0.5) H14(0.5)
 C13(0.5) H13(0.5) C12(0.5) H12(0.5) C11(0.5) H11(0.5)
6.a Ternary CH refined with riding coordinates:
 C9(H9B), C9(H9A), C8(H8)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C4(H4), C3(H3), C14A(H14A), C13A(H13A), C12A(H12A),
 C11A(H11A), C7A(H7A), C6A(H6A), C4A(H4A), C3A(H3A), C14(H14), C13(H13),
 C12(H12), C11(H11)
6.c Fitted hexagon refined as free rotating group:
 N3(C7,C6,C5,C4,C3), C10A(N4A,C14A,C13A,C12A,C11A), C10(N4,C14,C13,C12,C11)
;
_shelx_res_checksum              74912
_olex2_submission_special_instructions 'No special instructions were received'