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_7715753
_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         '4(C69 H50 Fe2 N24 S4), 8(C3 H7 N O), 5(H2 O)'
_chemical_formula_sum            'C300 H266 Fe8 N104 O13 S16'
_chemical_formula_weight         6495.91
_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             2023-09-17
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2024-02-27 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            1
_cell_length_a                   12.5490(15)
_cell_length_b                   21.076(3)
_cell_length_c                   30.415(4)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    291.81
_cell_measurement_theta_max      23.29
_cell_measurement_theta_min      2.32
_cell_volume                     8044.2(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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)'
_computing_structure_solution    'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      291.81
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0825
_diffrn_reflns_av_unetI/netI     0.0868
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            48489
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.004
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.528
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6284
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.1458 before and 0.0725 after correction.
The Ratio of minimum to maximum transmission is 0.8428.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       block
_exptl_crystal_F_000             3362
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         14185
_refine_ls_number_restraints     1996
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1178
_refine_ls_R_factor_gt           0.0666
_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^)+(0.0859P)^2^+0.9827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1601
_refine_ls_wR_factor_ref         0.1816
_reflns_Friedel_coverage         0.822
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                9011
_reflns_number_total             14185
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02691d2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7715753--7715754.cif.'
_cod_original_cell_volume        8044.3(17)
_cod_database_code               7715753
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.939
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.93(3)
 0.07(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Restrained distances
 C60-C61
 1.35 with sigma of 0.02
 C9-C8
 1.5 with sigma of 0.01
 N7-N8
 1.35 with sigma of 0.02
 C62-C65 = C63-C66 = C64-C67
 2.78 with sigma of 0.02
 C62-C63 = C63-C64 = C64-C65 = C65-C66 = C66-C67 = C67-C62
 1.39 with sigma of 0.02
 C61-C68 = C67-C70 = C62-C69
 2.78 with sigma of 0.02
 C61-C62 = C62-C67 = C67-C68 = C68-C69 = C69-C70 = C70-C61
 1.39 with sigma of 0.02
 N24A-N23 = N24-N23
 1.488 with sigma of 0.02
 N24-C60 \\sim N24A-C60A
 with sigma of 0.1
 C61A-C60A \\sim C61-C60
 with sigma of 0.1
 N24A-N23 \\sim N24-N23
 with sigma of 0.1
4. Rigid bond restraints
 C8, C9, C10, C11, C12, C13, C14, C15, C16, C17, C18, N7, N8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10
\\sim C11 \\sim C12 \\sim C13 \\sim C18 \\sim C17 \\sim C16 \\sim C15 \\sim C14
\\sim C19 \\sim C20 \\sim C21 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28
\\sim C23 \\sim C22 \\sim C31 \\sim C30 \\sim C29 \\sim C32 \\sim C33 \\sim C34
\\sim C35 \\sim C44 \\sim C43 \\sim C42 \\sim C41 \\sim C36 \\sim C37 \\sim C38
\\sim C39 \\sim C40 \\sim C45 \\sim C46 \\sim C47 \\sim C50 \\sim C51 \\sim C52
\\sim C53 \\sim C54 \\sim C49 \\sim C48 \\sim C57 \\sim C56 \\sim C55 \\sim C58
\\sim C59 \\sim C60 \\sim C61 \\sim C70 \\sim C69 \\sim C68 \\sim C67 \\sim C62
\\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C71 \\sim C72 \\sim C73 \\sim C74
\\sim C75 \\sim C76 \\sim C60A \\sim C61A \\sim C70A \\sim C69A \\sim C68A
\\sim C67A \\sim C62A \\sim C63A \\sim C64A \\sim C65A \\sim C66A: within 2.8A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2.8A
O2 \\sim C76 \\sim N26 \\sim C75 \\sim C74: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Uanis(O2W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(N26) \\sim Ueq, Uanis(C75)
\\sim Ueq, Uanis(C74) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
6. Rigid body (RIGU) restrains
 N24, C68, C66, C67, C70, C65, C62, C60, C63, C69, C61, C64
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N24A, C64A, C62A, C63A, C66A, C67A, C70A, C60A, C69A, C65A, C61A, C68A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
7. Others
 Sof(N24A)=Sof(C60A)=Sof(H60A)=Sof(C61A)=Sof(C70A)=Sof(H70A)=Sof(C69A)=
 Sof(H69A)=Sof(C68A)=Sof(H68A)=Sof(C67A)=Sof(C62A)=Sof(C63A)=Sof(H63A)=
 Sof(C64A)=Sof(H64A)=Sof(C65A)=Sof(H65A)=Sof(C66A)=Sof(H66A)=1-FVAR(1)
 Sof(N24)=Sof(C60)=Sof(H60)=Sof(C61)=Sof(C70)=Sof(H70)=Sof(C69)=Sof(H69)=
 Sof(C68)=Sof(H68)=Sof(C67)=Sof(C62)=Sof(C63)=Sof(H63)=Sof(C64)=Sof(H64)=
 Sof(C65)=Sof(H65)=Sof(C66)=Sof(H66)=FVAR(1)
 Fixed Sof: O2W(0.25) H2WA(0.25) H2WB(0.25)
8.a Riding coordinates:
 O2W(H2WA,H2WB)
8.b Free rotating group:
 O1W(H1WA,H1WB)
8.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12), C17(H17), C16(H16),
 C15(H15), C14(H14), C19(H19), C20(H20), C21(H21), C24(H24), C25(H25), C26(H26),
  C27(H27), C31(H31), C30(H30), C29(H29), C32(H32), C33(H33), C34(H34),
 C44(H44), C43(H43), C42(H42), C37(H37), C38(H38), C39(H39), C40(H40), C45(H45),
  C46(H46), C47(H47), C50(H50), C51(H51), C52(H52), C53(H53), C57(H57),
 C56(H56), C55(H55), C58(H58), C59(H59), C60(H60), C70(H70), C69(H69), C68(H68),
  C63(H63), C64(H64), C65(H65), C66(H66), C73(H73), C76(H76), C60A(H60A),
 C70A(H70A), C69A(H69A), C68A(H68A), C63A(H63A), C64A(H64A), C65A(H65A),
 C66A(H66A)
8.d Naphthalene refined as free rotating group:
 C9(C10,C11,C12,C13,C18,C17,C16,C15,C14), C24(C25,C26,C27,C28,C23,C22,C31,C30,
 C29), C35(C44,C43,C42,C41,C36,C37,C38,C39,C40), C50(C51,C52,C53,C54,C49,C48,
 C57,C56,C55), C61(C70,C69,C68,C67,C62,C63,C64,C65,C66), C61A(C70A,C69A,C68A,
 C67A,C62A,C63A,C64A,C65A,C66A)
8.e 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              49643
_olex2_submission_special_instructions 'No special instructions were received'