"Inverted" hysteresis in a bilayer Fe(II) spin crossover system.
Tołoczko, Aleksandra; Kaźmierczak, Marcin; Maliuzhenko, Vladyslav; Siczek, Miłosz; Weselski, Marek; Bronisz, Robert; Chemical communications (Cambridge, England) 62 (2026) 6110–6113; doi:10.1039/d6cc00357e

data_7135405
_publ_section_title
;
 "Inverted" hysteresis in a bilayer Fe(II) spin crossover system.
;
_journal_issue                   22
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              6110
_journal_page_last               6113
_journal_paper_doi               10.1039/d6cc00357e
_journal_volume                  62
_journal_year                    2026
_chemical_formula_moiety
'C200 H352 Fe2 N48 O16, 4(B F4), 0.46(H2 O), 2(C25 H44 N6 O2), 4(C2 H3 N)'
_chemical_formula_sum            'C258 H452.92 B4 F16 Fe2 N64 O20.46'
_chemical_formula_weight         5238.04
_chemical_melting_point          ?
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-12-11
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-12-11 deposited with the CCDC.	2026-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                77.55(2)
_cell_angle_beta                 85.89(2)
_cell_angle_gamma                72.53(2)
_cell_formula_units_Z            1
_cell_length_a                   13.001(4)
_cell_length_b                   18.757(5)
_cell_length_c                   33.217(8)
_cell_measurement_reflns_used    15895
_cell_measurement_temperature    250(1)
_cell_measurement_theta_max      36.6050
_cell_measurement_theta_min      2.2610
_cell_volume                     7545(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 44.116a 64-bit (release 30-06-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      250(1)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.998
_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     13.00  38.00   0.50    2.90    --    0.05  39.00 -35.38   50
  2  \w     16.00  42.00   0.50    2.90    --    0.05  52.00 -43.52   52
  3  \w     13.00  39.00   0.50    2.90    --    0.05  60.00  33.35   52
  4  \w     15.00  44.00   0.50    2.90    --    0.05  49.00  69.35   58
  5  \w      9.00  34.00   0.50    2.90    --    0.05  64.00 148.86   50
  6  \w     -7.00  19.00   0.50    2.90    --    0.05  96.00 160.46   52
  7  \w     -6.00  23.00   0.50    2.90    --    0.05  91.00  87.08   58
  8  \w    -11.00  17.00   0.50    2.90    --    0.05  98.00  -5.50   56
  9  \w    -13.00  12.00   0.50    2.90    --    0.05 101.00 -66.66   50
 10  \w     -9.00  16.00   0.50    2.90    --    0.05  96.00 -88.20   50
 11  \w     -5.00  23.00   0.50    2.90    --    0.05  91.00-137.67   56
 12  \w      9.00  42.00   0.50    2.90    --    0.05  60.00-179.27   66
 13  \w     -8.00  18.00   0.50    2.90    --    0.05  97.00-121.10   52
 14  \w    -11.00  16.00   0.50    2.90    --    0.05  98.00-160.07   54
 15  \w    -24.00   8.00   0.50    2.90    --  -37.06  19.00-120.00   64
 16  \w    -19.00   7.00   0.50    2.90    --  -37.06  19.00-180.00   52
 17  \w    -45.00 -11.00   0.50    2.90    --    0.05 -44.00-153.33   68
 18  \w    -24.00   2.00   0.50    2.90    --  -37.06  19.00 -30.00   52
 19  \w    -24.00   1.00   0.50    2.90    --  -37.06  19.00  30.00   50
 20  \w    -21.00   5.00   0.50    2.90    --  -37.06  19.00   0.00   52
 21  \w     -7.00  18.00   0.50    2.90    --    0.05  93.00 -20.96   50
 22  \w    -46.00   0.00   0.50    2.90    --  -37.06  96.00 129.00   92
 23  \w      1.00  27.00   0.50    2.90    --   37.16 -19.00  30.00   52
 24  \w     11.00  45.00   0.50    2.90    --   37.16 -96.00  20.00   68
 25  \w    -24.00   1.00   0.50    2.90    --  -37.06  19.00 120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            191638
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.700
_diffrn_reflns_theta_min         1.908
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.378
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.144a (Rigaku Oxford Diffraction, 2024)
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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2829
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1864
_refine_ls_number_reflns         38902
_refine_ls_number_restraints     210
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0980
_refine_ls_R_factor_gt           0.0685
_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^)+(0.0854P)^2^+4.4425P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1855
_refine_ls_wR_factor_ref         0.2007
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27611
_reflns_number_total             38902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6cc00357e2.cif
_cod_data_source_block           cooling_01_250k
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7135405--7135407.cif.
;
_cod_database_code               7135405
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.905
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C82-N80
 2.34 with sigma of 0.02
 C72-N70
 2.34 with sigma of 0.02
 N60-C62
 2.34 with sigma of 0.02
 N40-C42
 2.34 with sigma of 0.02
 O1-H1A
 0.85 with sigma of 0.01
 O1-H1B
 0.85 with sigma of 0.01
 H1A-H1B
 1.38 with sigma of 0.02
 C438-C437 \\sim C439-C438
 with sigma of 0.008
 C339-C338 \\sim C638-C339
 with sigma of 0.008
 C338-C337 \\sim C638-C337
 with sigma of 0.008
 C337-C336 \\sim C636-C337
 with sigma of 0.008
 C636-C335 \\sim C336-C335
 with sigma of 0.008
 C335-C334 \\sim C634-C335
 with sigma of 0.008
 C334-C333 \\sim C634-C333
 with sigma of 0.008
 C333-C332 \\sim C632-C333
 with sigma of 0.008
 C332-C331 \\sim C632-C331
 with sigma of 0.008
 C331-C330 \\sim C630-C331
 with sigma of 0.008
 C330-C329 \\sim C630-C329
 with sigma of 0.008
 C329-C328 \\sim C628-C329
 with sigma of 0.008
 C328-C327 \\sim C628-C327
 with sigma of 0.008
 C327-C326 \\sim C626-C327
 with sigma of 0.008
 C326-C325 \\sim C626-C625
 with sigma of 0.008
 C625-C624 \\sim C325-C324
 with sigma of 0.008
 C624-C623 \\sim C324-C323
 with sigma of 0.008
 C623-C322 \\sim C323-C322
 with sigma of 0.008
3. Rigid body (RIGU) restrains
 F1, F2, F3, F4, B1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F5, F6, F7, F8, B2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F9, F10, F11, F12, B3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F13, F14, F15, F16, B4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N60, C61, C62
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N40, C41, C42
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N50, C51, C52
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N70, C71, C72
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N80, C81, C82
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N90, C91, C92
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{F1, F2, F3, F4, B1} sigma for 1-2: 0.008, 1-3: 0.04
as in
{F5, F6, F7, F8, B2}
{N90, C91, C92} sigma for 1-2: 0.004, 1-3: 0.04
as in
{N70, C71, C72}
{N90, C91, C92} sigma for 1-2: 0.004, 1-3: 0.04
as in
{N60, C61, C62}
{N90, C91, C92} sigma for 1-2: 0.004, 1-3: 0.04
as in
{N80, C81, C82}
{N90, C91, C92} sigma for 1-2: 0.004, 1-3: 0.04
as in
{N50, C51, C52}
{N90, C91, C92} sigma for 1-2: 0.004, 1-3: 0.04
as in
{N40, C41, C42}
{F9, F10, F11, F12, B3} sigma for 1-2: 0.02, 1-3: 0.04
as in
{F13, F14, F15, F16, B4}
5. Others
 Sof(F5)=Sof(F6)=Sof(F7)=Sof(F8)=Sof(B2)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(B1)=FVAR(1)
 Sof(H32K)=Sof(H32L)=Sof(H32Q)=Sof(H32R)=Sof(H33E)=Sof(H33F)=Sof(H33K)=
 Sof(H33L)=Sof(H33Q)=Sof(H33R)=Sof(H33W)=Sof(H33X)=Sof(HC)=Sof(HD)=Sof(HE)=
 Sof(C623)=Sof(H62A)=Sof(H62B)=Sof(C624)=Sof(H62C)=Sof(H62D)=Sof(C625)=
 Sof(H62E)=Sof(H62F)=Sof(C626)=Sof(H62G)=Sof(H62H)=Sof(C628)=Sof(H62I)=
 Sof(H62J)=Sof(C630)=Sof(H63A)=Sof(H63B)=Sof(C632)=Sof(H63C)=Sof(H63D)=
 Sof(C634)=Sof(H63E)=Sof(H63F)=Sof(C636)=Sof(H63G)=Sof(H63H)=Sof(C638)=
 Sof(H63I)=Sof(H63J)=1-FVAR(2)
 Sof(C323)=Sof(H32A)=Sof(H32B)=Sof(C324)=Sof(H32C)=Sof(H32D)=Sof(C325)=
 Sof(H32E)=Sof(H32F)=Sof(C326)=Sof(H32G)=Sof(H32H)=Sof(H32I)=Sof(H32J)=
 Sof(C328)=Sof(H32M)=Sof(H32N)=Sof(H32O)=Sof(H32P)=Sof(C330)=Sof(H33A)=
 Sof(H33B)=Sof(H33C)=Sof(H33D)=Sof(C332)=Sof(H33G)=Sof(H33H)=Sof(H33I)=
 Sof(H33J)=Sof(C334)=Sof(H33M)=Sof(H33N)=Sof(H33O)=Sof(H33P)=Sof(C336)=
 Sof(H33S)=Sof(H33T)=Sof(H33U)=Sof(H33V)=Sof(C338)=Sof(H33Y)=Sof(H)=Sof(H33Z)=
 Sof(HA)=Sof(HB)=FVAR(2)
 Sof(F13)=Sof(F14)=Sof(F15)=Sof(F16)=Sof(B4)=1-FVAR(3)
 Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=Sof(B3)=FVAR(3)
 Fixed Sof: O1(0.23) H1A(0.23) H1B(0.23) N90(0.5) C91(0.5) C92(0.5) H92O(0.5)
 H92P(0.5) H92Q(0.5) N40(0.25) C41(0.25) C42(0.25) H42O(0.25) H42P(0.25)
 H42Q(0.25) N50(0.5) C51(0.5) C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5) N60(0.25)
 C61(0.25) C62(0.25) H62K(0.25) H62L(0.25) H62M(0.25) N70(0.25) C71(0.25)
 C72(0.25) H72A(0.25) H72B(0.25) H72C(0.25) N80(0.25) C81(0.25) C82(0.25)
 H82A(0.25) H82B(0.25) H82C(0.25)
6.a Ternary CH refined with riding coordinates:
 C102(H102), C202(H202), C302(H302), C402(H402), C902(H902)
6.b Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B), C103(H10C,H10D), C123(H12A,H12B), C124(H12C,H12D), C125(H12E,
 H12F), C126(H12G,H12H), C127(H12I,H12J), C128(H12K,H12L), C129(H12M,H12N),
 C130(H13A,H13B), C131(H13C,H13D), C132(H13E,H13F), C133(H13G,H13H), C134(H13I,
 H13J), C135(H13K,H13L), C136(H13M,H13N), C137(H13O,H13P), C138(H13Q,H13R),
 C201(H20A,H20B), C203(H20C,H20D), C223(H22A,H22B), C224(H22C,H22D), C225(H22E,
 H22F), C226(H22G,H22H), C227(H22I,H22J), C228(H22K,H22L), C229(H22M,H22N),
 C230(H23A,H23B), C231(H23C,H23D), C232(H23E,H23F), C233(H23G,H23H), C234(H23I,
 H23J), C235(H23K,H23L), C236(H23M,H23N), C237(H23O,H23P), C238(H23Q,H23R),
 C301(H30A,H30B), C303(H30C,H30D), C323(H32A,H32B), C324(H32C,H32D), C325(H32E,
 H32F), C326(H32G,H32H), C327(H32I,H32J), C327(H32K,H32L), C328(H32M,H32N),
 C329(H32O,H32P), C329(H32Q,H32R), C330(H33A,H33B), C331(H33C,H33D), C331(H33E,
 H33F), C332(H33G,H33H), C333(H33I,H33J), C333(H33K,H33L), C334(H33M,H33N),
 C335(H33O,H33P), C335(H33Q,H33R), C336(H33S,H33T), C337(H33U,H33V), C337(H33W,
 H33X), C338(H33Y,H), C401(H40A,H40B), C403(H40C,H40D), C423(H42A,H42B),
 C424(H42C,H42D), C425(H42E,H42F), C426(H42G,H42H), C427(H42I,H42J), C428(H42K,
 H42L), C429(H42M,H42N), C430(H43A,H43B), C431(H43C,H43D), C432(H43E,H43F),
 C433(H43G,H43H), C434(H43I,H43J), C435(H43K,H43L), C436(H43M,H43N), C437(H43O,
 H43P), C438(H43Q,H43R), C623(H62A,H62B), C624(H62C,H62D), C625(H62E,H62F),
 C626(H62G,H62H), C628(H62I,H62J), C630(H63A,H63B), C632(H63C,H63D), C634(H63E,
 H63F), C636(H63G,H63H), C638(H63I,H63J), C901(H90A,H90B), C903(H90C,H90D),
 C923(H92A,H92B), C924(H92C,H92D), C925(H92E,H92F), C926(H92G,H92H), C927(H92I,
 H92J), C928(H92K,H92L), C929(H92M,H92N), C930(H93A,H93B), C931(H93C,H93D),
 C932(H93E,H93F), C933(H93G,H93H), C934(H93I,H93J), C935(H93K,H93L), C936(H93M,
 H93N), C937(H93O,H93P), C938(H93Q,H93R)
6.c Aromatic/amide H refined with riding coordinates:
 C114(H114), C115(H115), C116(H116), C117(H117), C214(H214), C215(H215),
 C216(H216), C217(H217), C314(H314), C315(H315), C316(H316), C317(H317),
 C414(H414), C415(H415), C416(H416), C417(H417), C914(H914), C915(H915),
 C916(H916), C917(H917)
6.d Idealised Me refined as rotating group:
 C139(H13S,H13T,H13U), C239(H23S,H23T,H23U), C339(H33Z,HA,HB), C339(HC,HD,HE),
 C439(H43S,H43T,H43U), C939(H93S,H93T,H93U), C92(H92O,H92P,H92Q), C42(H42O,H42P,
 H42Q), C52(H52A,H52B,H52C), C62(H62K,H62L,H62M), C72(H72A,H72B,H72C), C82(H82A,
 H82B,H82C)
;
_shelx_res_checksum              99388
_shelx_hkl_checksum              22562
_olex2_exptl_crystal_mounting_method 'glass capillar'
_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
;