[2 + 2] Photocyclization converts thermally induced spin crossover effect into “hidden hysteresis” one
Kaźmierczak, Marcin; Weselski, Marek; Siczek, Miłosz; Wolny, Juliusz A.; Schünemann, Volker; Bronisz, Robert; Chemical Science 16 (2025) 7884–7893; doi:10.1039/D4SC05587J

data_1574232
_publ_section_title
;
 [2 + 2] Photocyclization converts thermally induced spin crossover effect
 into &#x201C;hidden hysteresis&#x201D; one
;
_journal_issue                   18
_journal_name_full               'Chemical Science'
_journal_page_first              7884
_journal_page_last               7893
_journal_paper_doi               10.1039/D4SC05587J
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C22 H16 N8 O4'
_chemical_formula_sum            'C22 H16 N8 O4'
_chemical_formula_weight         456.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-06-13
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-06-13 deposited with the CCDC.	2025-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                101.07(3)
_cell_angle_beta                 99.32(3)
_cell_angle_gamma                97.21(2)
_cell_formula_units_Z            2
_cell_length_a                   6.597(2)
_cell_length_b                   12.473(4)
_cell_length_c                   12.691(4)
_cell_measurement_reflns_used    8452
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.0410
_cell_measurement_theta_min      3.5890
_cell_volume                     998.0(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     86.00 111.00   0.50    0.12    --   79.25  30.00 120.00   50
  2  \w     66.00 120.00   0.50    0.12    --   82.00  24.00   7.03  108
  3  \w     80.00 105.00   0.50    0.12    --   79.25  30.00 -60.00   50
  4  \w     53.00  83.00   0.50    0.12    --   83.00   4.00  43.66   60
  5  \w     58.00  83.00   0.50    0.12    --   83.00   4.00  99.34   50
  6  \w     93.00 126.00   0.50    0.12    --   83.00   4.00  99.34   66
  7  \w     56.00 108.00   0.50    0.12    --   83.00  12.00 -60.90  104
  8  \w     65.00 121.00   0.50    0.12    --   83.00  23.00-176.29  112
  9  \w     45.00 105.00   0.50    0.12    --   83.00   3.00-174.42  120
 10  \w     63.00 104.00   0.50    0.12    --   59.59  30.00-120.00   82
 11  \w     78.00 103.00   0.50    0.12    --   79.25 126.00   0.00   50
 12  \w     86.00 122.00   0.50    0.12    --   79.25 126.00 120.00   72
 13  \w     79.00 111.00   0.50    0.12    --   79.25 126.00 -30.00   64
 14  \w     83.00 111.00   0.50    0.12    --   79.25 126.00-180.00   56
 15  \w     11.00  37.00   0.50    0.12    --   59.59 -30.00 -90.00   52
 16  \w     40.00  72.00   0.50    0.12    --   83.00 -63.00-169.38   64
 17  \w     89.00 121.00   0.50    0.12    --   83.00-137.00 -26.30   64
 18  \w     42.00  86.00   0.50    0.12    --   83.00-137.00 -26.30   88
 19  \w     50.00 116.00   0.50    0.12    --   83.00-130.00  48.20  132
 20  \w     69.00  95.00   0.50    0.12    --   83.00-145.00  72.07   52
 21  \w     78.00 103.00   0.50    0.12    --   79.25-126.00  90.00   50
 22  \w     85.00 111.00   0.50    0.12    --   79.25-126.00 120.00   52
 23  \w     46.00  71.00   0.50    0.12    --   83.00 -65.00 160.93   50
 24  \w     43.00  69.00   0.50    0.12    --   79.25-126.00  90.00   52
 25  \w     34.00  63.00   0.50    0.12    --   79.25-126.00-120.00   58
 26  \w     57.00 101.00   0.50    0.12    --   79.25-126.00-150.00   88
 27  \w     85.00 111.00   0.50    0.12    --   79.25-126.00-180.00   52
 28  \w     82.00 111.00   0.50    0.12    --   79.25-126.00-120.00   58
 29  \w     48.00  86.00   0.50    0.12    --   79.25 -95.00 -30.00   76
 30  \w     65.00  90.00   0.50    0.12    --   79.25 -95.00-120.00   50
 31  \w     50.00  85.00   0.50    0.12    --   79.25 -95.00  60.00   70
 32  \w     47.00  82.00   0.50    0.12    --   79.25 -95.00  90.00   70
 33  \w     51.00  86.00   0.50    0.12    --   79.25 -95.00 120.00   70
 34  \w     49.00  74.00   0.50    0.12    --   79.25 -95.00 150.00   50
 35  \w     24.00  69.00   0.50    0.12    --   59.59 -95.00  90.00   90
 36  \w     43.00  68.00   0.50    0.12    --   79.25 -95.00   0.00   50
 37  \w     35.00  63.00   0.50    0.12    --   74.19 -95.00   0.00   56
 38  \w     36.00  84.00   0.50    0.12    --   74.19 -95.00 -30.00   96
 39  \w     34.00  84.00   0.50    0.12    --   74.19 -95.00-120.00  100
 40  \w     46.00  71.00   0.50    0.12    --   79.25 -95.00 -90.00   50
 41  \w   -121.00 -41.00   0.50    0.12    --  -74.77 -15.00 -30.00  160
 42  \w   -107.00 -62.00   0.50    0.12    --  -61.35 -30.00 120.00   90
 43  \w   -106.00 -81.00   0.50    0.12    --  -79.25 -87.00-104.17   50
 44  \w   -116.00 -91.00   0.50    0.12    --  -79.25 -43.00 -66.55   50
 45  \w   -112.00 -59.00   0.50    0.12    --  -75.31   0.00-150.00  106
 46  \w    -87.00 -61.00   0.50    0.12    --  -79.25 111.00 -88.79   52
 47  \w    -64.00 -33.00   0.50    0.12    --  -75.31 126.00  60.00   62
 48  \w   -100.00 -74.00   0.50    0.12    --  -75.31 126.00  60.00   52
 49  \w    -71.00 -44.00   0.50    0.12    --  -79.25  62.00 155.25   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0807611000
_diffrn_orient_matrix_UB_12      -0.1117342000
_diffrn_orient_matrix_UB_13      -0.0121392000
_diffrn_orient_matrix_UB_21      -0.0327797000
_diffrn_orient_matrix_UB_22      -0.0066736000
_diffrn_orient_matrix_UB_23      0.1163145000
_diffrn_orient_matrix_UB_31      -0.2234743000
_diffrn_orient_matrix_UB_32      -0.0614662000
_diffrn_orient_matrix_UB_33      -0.0473196000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14010
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.573
_diffrn_reflns_theta_max         66.573
_diffrn_reflns_theta_min         3.615
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.919
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.618
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
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            colourless
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       plate
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0514
_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^)+(0.1101P)^2^+0.1277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1452
_refine_ls_wR_factor_ref         0.1497
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3123
_reflns_number_total             3512
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05587j10.cif
_cod_data_source_block           206bv
_cod_depositor_comments
'Adding full bibliography for 1574226--1574232.cif.'
_cod_database_code               1574232
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C22H16N8O4
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.766
_reflns_odcompleteness_completeness 98.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C13(H13), C14(H14)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C21(H21A,H21B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C11(H11), C16(H16), C17(H17), C19(H19), C22(H22)
;
_shelx_res_checksum              18741
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.903
_oxdiff_exptl_absorpt_empirical_full_min 0.581