Light-induced spin-state switching in Fe(II) spin-crossover complexes with thiazole-based chelating ligands.
Jo, Minyoung; Amanyazova, Botagoz; Yergeshbayeva, Sandugash; Gakiya-Teruya, Miguel; Üngör, Ökten; Lopez Rivera, Paola; Jen, Natalie; Lukyanenko, Evgeny; Kurkin, Alexander V.; Erkasov, Rakhmetulla; Meisel, Mark W.; Hauser, Andreas; Chakraborty, Pradip; Shatruk, Michael; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10511–10520; doi:10.1039/d4dt00308j

data_7716213
_publ_section_title
;
 Light-induced spin-state switching in Fe(II) spin-crossover complexes
 with thiazole-based chelating ligands.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10511
_journal_page_last               10520
_journal_paper_doi               10.1039/d4dt00308j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C18 H15 Fe N9 S3, 2(Cl O4), 2(C6 H5 N3 S)'
_chemical_formula_sum            'C30 H25 Cl2 Fe N15 O8 S5'
_chemical_formula_weight         1010.70
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-01-13
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-13 deposited with the CCDC.	2024-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   17.8075(6)
_cell_length_b                   15.1011(3)
_cell_length_c                   44.5307(8)
_cell_measurement_reflns_used    16016
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      31.0030
_cell_measurement_theta_min      3.2660
_cell_volume                     11974.9(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -9.00  35.08   0.38   38.99    --    4.78 -94.00-113.00  116
  2  \w    -34.00   1.34   0.38   38.99    --   -5.09 -94.00-113.00   93
  3  \w    -35.00  -4.98   0.38   38.99    --   -5.09  94.00  -2.00   79
  4  \w    -25.00  26.30   0.38   38.99    --    4.78 -77.00   0.00  135
  5  \w     -7.00  33.28   0.38   38.99    --    4.78 -99.00-180.00  106
  6  \w     -7.00  18.08   0.38   38.99    --    4.78 -99.00 120.00   66
  7  \w    -53.00  19.20   0.38   38.99    --    4.78 -57.00 120.00  190
  8  \w    -14.00  26.28   0.38   38.99    --    4.78 -77.00  30.00  106
  9  \w    -25.00  15.28   0.38   38.99    --   -5.09 -77.00 -60.00  106
 10  \w     -7.00  26.06   0.38   38.99    --   -5.09 -99.00  90.00   87
 11  \w    -23.00   5.12   0.38   38.99    --   -5.09 -77.00 -30.00   74
 12  \w    -52.00  -7.92   0.38   38.99    --   -5.09 -57.00  60.00  116
 13  \w    -27.00  10.24   0.38   38.99    --   -5.09  77.00-180.00   98
 14  \w    -28.00   5.06   0.38   38.99    --   -5.09  77.00-120.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0237718000
_diffrn_orient_matrix_UB_12      -0.0016833000
_diffrn_orient_matrix_UB_13      -0.0346386000
_diffrn_orient_matrix_UB_21      -0.0376526000
_diffrn_orient_matrix_UB_22      -0.0209813000
_diffrn_orient_matrix_UB_23      -0.0172833000
_diffrn_orient_matrix_UB_31      -0.0176993000
_diffrn_orient_matrix_UB_32      0.0421077000
_diffrn_orient_matrix_UB_33      -0.0099375000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            170932
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         3.225
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.844
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_description       block
_exptl_crystal_F_000             6168
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile, diethyl ether'
_exptl_crystal_size_max          0.368
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.117
_refine_diff_density_max         3.657
_refine_diff_density_min         -1.482
_refine_diff_density_rms         0.263
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.56(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.853
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     872
_refine_ls_number_reflns         24344
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.853
_refine_ls_R_factor_all          0.1580
_refine_ls_R_factor_gt           0.1494
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4148
_refine_ls_wR_factor_ref         0.4222
_reflns_Friedel_coverage         0.968
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                21568
_reflns_number_total             24344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00308j2.cif
_cod_data_source_block           str3-100K
_cod_depositor_comments
'Adding full bibliography for 7716207--7716213.cif.'
_cod_database_code               7716213
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         FeC34H34Cl2O8S6N6
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.44(5)
 0.56(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
3. Shared sites
{N9, C13A}
{C13, N9A}
{N18, C18A}
{C31, N31A}
{N27, C27A}
{C49, N49A}
4. Restrained distances
 C16-C17
 1.38 with sigma of 0.01
 C18-C17
 1.38 with sigma of 0.01
 C14-C17A
 1.38 with sigma of 0.01
 C15-C17A
 1.38 with sigma of 0.01
 C34-C35
 1.38 with sigma of 0.01
 C36-C35
 1.38 with sigma of 0.01
 C32-C35A
 1.38 with sigma of 0.01
 C33-C35A
 1.38 with sigma of 0.01
 C50-C53
 1.38 with sigma of 0.01
 C51-C53
 1.38 with sigma of 0.01
 C52-C53A
 1.38 with sigma of 0.01
 C54-C53A
 1.38 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(S3) = Uanis(S3A) = Uanis(C17) = Uanis(C17A)
Uanis(S6) = Uanis(S6A) = Uanis(C35) = Uanis(C35A)
Uanis(S9) = Uanis(S9A) = Uanis(C53) = Uanis(C53A)
Uiso(N9) = Uiso(C13A)
Uiso(C13) = Uiso(N9A)
Uiso(N18) = Uiso(C18A)
Uiso(C31) = Uiso(N31A)
Uiso(N27) = Uiso(C27A)
Uiso(C49) = Uiso(N49A)
6. Others
 Sof(S6A)=Sof(N31A)=Sof(H31A)=Sof(C18A)=Sof(H18C)=Sof(H32A)=Sof(C35A)=
 Sof(H35A)=Sof(H36A)=1-FVAR(1)
 Sof(S6)=Sof(N18)=Sof(H18B)=Sof(C31)=Sof(H31)=Sof(H32)=Sof(C35)=Sof(H35)=
 Sof(H36)=FVAR(1)
 Sof(S3A)=Sof(N9A)=Sof(H9A)=Sof(C13A)=Sof(H13A)=Sof(H14A)=Sof(C17A)=Sof(H17A)=
 Sof(H18A)=1-FVAR(2)
 Sof(S3)=Sof(N9)=Sof(H9)=Sof(C13)=Sof(H13)=Sof(H14)=Sof(C17)=Sof(H17)=Sof(H18)=
 FVAR(2)
 Sof(S9A)=Sof(N49A)=Sof(H49A)=Sof(C27A)=Sof(H27A)=Sof(H50A)=Sof(C53A)=
 Sof(H53A)=Sof(H54A)=1-FVAR(3)
 Sof(S9)=Sof(N27)=Sof(H27)=Sof(C49)=Sof(H49)=Sof(H50)=Sof(C53)=Sof(H53)=
 Sof(H54)=FVAR(3)
7.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6), N9(H9), N9A(H9A), N12(H12A), N15(H15), N18(H18B), N21(H21),
 N24(H24A), N27(H27), N30(H30A), N31A(H31A), N33(H33), N36(H36B), N39(H39),
 N42(H42A), N45(H45), N49A(H49A), C1(H1), C2(H2), C5(H5), C6(H6A), C7(H7),
 C8(H8), C11(H11), C12(H12), C13(H13), C13A(H13A), C14(H14), C14(H14A),
 C17(H17), C17A(H17A), C18(H18A), C18(H18), C18A(H18C), C19(H19), C20(H20),
 C23(H23), C24(H24), C25(H25), C26(H26), C27A(H27A), C29(H29), C30(H30),
 C31(H31), C32(H32A), C32(H32), C35(H35), C35A(H35A), C36(H36A), C36(H36),
 C37(H37), C38(H38), C41(H41), C42(H42), C43(H43), C44(H44), C47(H47), C48(H48),
  C49(H49), C50(H50A), C50(H50), C53(H53), C53A(H53A), C54(H54), C54(H54A),
 C55(H55), C56(H56), C59(H59), C60(H60), C61(H61), C62(H62), C65(H65), C66(H66),
  C67(H67), C68(H68), C71(H71), C72(H72), C73(H73), C74(H74), C77(H77),
 C78(H78), C79(H79), C80(H80), C83(H83), C84(H84), C85(H85), C86(H86), C89(H89),
  C90(H90)
;
_shelx_res_checksum              24893
_shelx_hkl_checksum              32082
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.748
_oxdiff_exptl_absorpt_empirical_full_min 0.458