Reversible light-induced spin state switching in a dinuclear Fe(II) spin crossover complex.
Wang, Jun-Li; Zhou, Hang-Yue; Zhao, Liang; Meng, Yin-Shan; Liu, Tao; Dalton transactions (Cambridge, England : 2003) 53 (2024) 7669–7676; doi:10.1039/d3dt02691d

data_7715754
_publ_section_title
;
 Reversible light-induced spin state switching in a dinuclear Fe(II) spin
 crossover complex.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7669
_journal_page_last               7676
_journal_paper_doi               10.1039/d3dt02691d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C69 H50 Fe2 N24 S4, 2(C3 H7 N O), 2(H2 O)'
_chemical_formula_sum            'C75 H68 Fe2 N26 O4 S4'
_chemical_formula_weight         1637.49
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-09-16
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2023-12-11 deposited with the CCDC.	2024-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3484(10)
_cell_length_b                   20.7584(16)
_cell_length_c                   30.015(2)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.28
_cell_measurement_theta_min      2.35
_cell_volume                     7693.8(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      89.94
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0616
_diffrn_reflns_av_unetI/netI     0.1009
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            46847
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.394
_diffrn_reflns_theta_min         2.035
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.554
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1102 before and 0.0620 after correction.
The Ratio of minimum to maximum transmission is 0.9120.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       block
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 4244 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1047
_refine_ls_number_reflns         16849
_refine_ls_number_restraints     271
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0583
_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^)+(0.0490P)^2^+4.3267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1207
_reflns_Friedel_coverage         0.799
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.943
_reflns_number_gt                12480
_reflns_number_total             16849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02691d2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7715753--7715754.cif.'
_cod_original_cell_volume        7693.9(11)
_cod_database_code               7715754
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.937
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C21-C20 \\sim C21A-C20
 with sigma of 0.01
3. Rigid bond restraints
 N12, C20, C21, C22, C23, C24, C25, C30, C29, C28, C27, C26
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C21A \\sim C27A \\sim C29A \\sim C22A \\sim C30A \\sim C23A \\sim C28A \\sim
C24A \\sim C26A \\sim C25A \\sim C20: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
5. Rigid body (RIGU) restrains
 C21, C22, C23, C24, C25, C30, C29, C28, C27, C26, C20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C21A, C22A, C23A, C24A, C25A, C30A, C29A, C28A, C27A, C26A, C20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(H20A)=Sof(C21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=
 Sof(H24A)=Sof(C25A)=Sof(C30A)=Sof(C29A)=Sof(H29A)=Sof(C28A)=Sof(H28A)=
 Sof(C27A)=Sof(H27A)=Sof(C26A)=Sof(H26A)=1-FVAR(1)
 Sof(H20)=Sof(C21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=
 Sof(C25)=Sof(C30)=Sof(C29)=Sof(H29)=Sof(C28)=Sof(H28)=Sof(C27)=Sof(H27)=
 Sof(C26)=Sof(H26)=FVAR(1)
7.a Riding coordinates:
 C75(H2WA,H1WA,H1WB,H2WB)
7.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C20(H20A), C22(H22),
 C23(H23), C24(H24), C29(H29), C28(H28), C27(H27), C26(H26), C31(H31), C32(H32),
  C33(H33), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41),
 C42(H42), C44(H44), C45(H45), C46(H46), C48(H48), C49(H49), C50(H50), C52(H52),
  C53(H53), C54(H54), C55(H55), C57(H57), C58(H58), C59(H59), C61(H61),
 C62(H62), C63(H63), C65(H65), C66(H66), C67(H67), C68(H68), C70(H70), C73(H73),
  C22A(H22A), C23A(H23A), C24A(H24A), C29A(H29A), C28A(H28A), C27A(H27A),
 C26A(H26A)
7.c Naphthalene refined as free rotating group:
 C21(C22,C23,C24,C25,C30,C29,C28,C27,C26), C21A(C22A,C23A,C24A,C25A,C30A,C29A,
 C28A,C27A,C26A)
7.d Idealised Me refined as rotating group:
 C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C74(H74A,H74B,H74C), C75(H75A,H75B,
 H75C)
;
_shelx_res_checksum              53741
_olex2_submission_special_instructions 'No special instructions were received'