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_7716211
_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 H12 Fe N6 S6, 2(Cl O4), C H4 O'
_chemical_formula_sum            'C19 H16 Cl2 Fe N6 O9 S6'
_chemical_formula_weight         791.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-13
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2024-01-13 deposited with the CCDC.	2024-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.0130(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.90780(10)
_cell_length_b                   21.8512(3)
_cell_length_c                   12.7772(2)
_cell_measurement_reflns_used    34803
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      33.8750
_cell_measurement_theta_min      3.3130
_cell_volume                     2766.23(6)
_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 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9982
_diffrn_measured_fraction_theta_max 0.9017
_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    -22.00  30.00   0.50    6.31    --   13.19 -97.00 155.00  104
  2  \w    -28.00   8.00   0.50    6.31    --  -13.50 -97.00 155.00   72
  3  \w    -36.00 -10.00   0.50    6.31    --  -13.50  97.00 -96.00   52
  4  \w    -53.00  27.00   0.50    6.31    --   13.19 -57.00  90.00  160
  5  \w      3.00  54.00   0.50    6.31    --   13.19  57.00 -60.00  102
  6  \w    -25.00  18.00   0.50    6.31    --   13.19 -77.00   0.00   86
  7  \w     -7.00  46.00   0.50    6.31    --   13.19 -99.00-150.00  106
  8  \w     -9.00  17.00   0.50    6.31    --   13.19  77.00  60.00   52
  9  \w     49.00  77.00   0.50    6.31    --   13.19 178.00  90.00   56
 10  \w     50.00  86.00   0.50    6.31    --   13.19-178.00   0.00   72
 11  \w     -3.00  37.00   0.50    6.31    --   13.19 -99.00  30.00   80
 12  \w     21.00  58.00   0.50    6.31    --   13.19  57.00   0.00   74
 13  \w    -57.00   1.00   0.50    6.31    --  -13.50 -57.00 120.00  116
 14  \w    -53.00  -1.00   0.50    6.31    --  -13.50 -57.00   0.00  104
;
_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      -0.0406135000
_diffrn_orient_matrix_UB_12      0.0264751000
_diffrn_orient_matrix_UB_13      0.0062744000
_diffrn_orient_matrix_UB_21      0.0545275000
_diffrn_orient_matrix_UB_22      0.0151674000
_diffrn_orient_matrix_UB_23      0.0249594000
_diffrn_orient_matrix_UB_31      0.0224263000
_diffrn_orient_matrix_UB_32      0.0110875000
_diffrn_orient_matrix_UB_33      -0.0491776000
_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  0.0477
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            47278
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         3.201
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.255
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.582
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.85a (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 dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_description       block
_exptl_crystal_F_000             1528.000
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'slow evaporation of methanol solution'
_exptl_crystal_size_max          0.335
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.162
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         6844
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0495
_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^)+14.3628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1070
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6004
_reflns_number_total             6844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00308j2.cif
_cod_data_source_block           str2-100K
_cod_depositor_comments
'Adding full bibliography for 7716207--7716213.cif.'
_cod_database_code               7716211
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         FeS6Cl2O8N6C18H12
_chemical_oxdiff_usercomment
'same xtal as at 300K and 230K, cooled down from 230 K to 100 K at the rate of 1K/min'
_shelx_estimated_absorpt_t_max   0.823
_shelx_estimated_absorpt_t_min   0.679
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. 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) groups
2. Restrained distances
 C1M-O1M
 1.43 with sigma of 0.001
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14),
 C15(H15), C17(H17), C18(H18)
3.b Idealised Me refined as rotating group:
 C1M(H1MA,H1MB,H1MC)
3.c Idealised tetrahedral OH refined as rotating group:
 O1M(H1M)
;
_shelx_res_checksum              1639
_shelx_hkl_checksum              42785
_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 1.568
_oxdiff_exptl_absorpt_empirical_full_min 0.787