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_7716208
_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(C6 H5 N3 S), 2(Cl1 O4)'
_chemical_formula_sum            'C30 H25 Cl2 Fe N15 O8 S5'
_chemical_formula_weight         1010.70
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-17
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_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            4
_cell_length_a                   14.9806(6)
_cell_length_b                   15.5610(6)
_cell_length_c                   17.7708(7)
_cell_measurement_reflns_used    10257
_cell_measurement_temperature    230.00(10)
_cell_measurement_theta_max      33.3070
_cell_measurement_theta_min      3.4890
_cell_volume                     4142.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (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 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      230.00(10)
_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     38.00  69.00   0.50   21.68    --   16.36-154.00-121.00   62
  2  \w     -6.00  51.00   0.50   21.68    --  -16.68  53.00  52.00  114
  3  \w      0.00  25.00   0.50   21.68    --   16.36  77.00 150.00   50
  4  \w     -3.00  22.00   0.50   21.68    --   16.36  57.00 -60.00   50
  5  \w     46.00  93.00   0.50   21.68    --   16.36-178.00  90.00   94
  6  \w    -10.00  19.00   0.50   21.68    --   16.36  77.00  90.00   58
  7  \w    -32.00   2.00   0.50   21.68    --  -16.68 -57.00-180.00   68
;
_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      -0.0097161000
_diffrn_orient_matrix_UB_12      0.0274731000
_diffrn_orient_matrix_UB_13      0.0307528000
_diffrn_orient_matrix_UB_21      -0.0460108000
_diffrn_orient_matrix_UB_22      -0.0099711000
_diffrn_orient_matrix_UB_23      -0.0033952000
_diffrn_orient_matrix_UB_31      0.0055895000
_diffrn_orient_matrix_UB_32      -0.0349601000
_diffrn_orient_matrix_UB_33      0.0252260000
_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  0.0269
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25464
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.280
_diffrn_reflns_theta_min         3.229
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.813
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.566
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       block
_exptl_crystal_F_000             2056
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile, diethyl ether'
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.139
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         5129
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0381P)^2^+3.2577P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1183
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3891
_reflns_number_total             5129
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00308j2.cif
_cod_data_source_block           str3-230K
_cod_depositor_comments
'Adding full bibliography for 7716207--7716213.cif.'
_cod_database_code               7716208
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Fe S15 H16 Cl2 O8 C30 H30'
_chemical_oxdiff_usercomment     230K
_shelx_estimated_absorpt_t_max   0.895
_shelx_estimated_absorpt_t_min   0.821
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Shared sites
{C17A, N5}
{Cl1A, Cl1B}
{C15, N9B}
{C11, N7B}
3. Restrained distances
 C12B-C14
 1.37 with sigma of 0.01
 C16-C12A
 1.38 with sigma of 0.01
 C12B-C13
 1.37 with sigma of 0.01
 C9-C8
 1.37 with sigma of 0.01
 C12A-C10
 1.38 with sigma of 0.01
 C8-C7
 1.37 with sigma of 0.01
 O1A-O2A \\sim O3A-O4A
 with sigma of 0.02
 O1B-O2B \\sim O3B-O4B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C15) = Uanis(N9B)
Uanis(C12B) = Uanis(C12A)
Uanis(C17A) = Uanis(N5)
Uanis(Cl1A) = Uanis(Cl1B)
Uiso(C11) = Uiso(N7B)
5. Others
 Sof(S3A)=1-FVAR(1)
 Sof(S3B)=FVAR(1)
 Sof(Cl1B)=Sof(O4B)=Sof(O2B)=Sof(O1B)=Sof(O3B)=1-FVAR(2)
 Sof(Cl1A)=Sof(O3A)=Sof(O1A)=Sof(O2A)=Sof(O4A)=FVAR(2)
 Fixed Sof: S2(0.5) N7B(0.5) H7B(0.5) N9B(0.5) H9B(0.5) N5(0.5) H5(0.5)
 C12B(0.5) H12B(0.5) C15(0.5) H15(0.5) C11(0.5) H11(0.5) C12A(0.5) H12A(0.5)
 C17A(0.5) H17A(0.5) C8(0.5) H8(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N7B(H7B), N9B(H9B), N5(H5), C2(H2), C5(H5A), C6(H6), C3(H3A),
 C12B(H12B), C15(H15), C11(H11), C12A(H12A), C17A(H17A), C8(H8)
;
_shelx_res_checksum              84030
_shelx_hkl_checksum              59502
_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 1.150
_oxdiff_exptl_absorpt_empirical_full_min 0.793