A mononuclear Fe(III) complex showing thermally induced spin crossover and slow magnetic relaxation with reciprocating thermal behaviour.
Bridová, Terézia; Rajnák, Cyril; Titiš, Ján; Samoľová, Erika; Tran, Kevin; Malina, Ondřéj; Bieńko, Alina; Renz, Franz; Gembický, Milan; Boča, Roman; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10824–10828; doi:10.1039/d4dt00642a

data_7716294
_publ_section_title
;
 A mononuclear Fe(III) complex showing thermally induced spin crossover
 and slow magnetic relaxation with reciprocating thermal behaviour.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10824
_journal_page_last               10828
_journal_paper_doi               10.1039/d4dt00642a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C24 H29 Fe N4 O4 Se'
_chemical_formula_sum            'C24 H29 Fe N4 O4 Se'
_chemical_formula_weight         572.32
_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             2021-06-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-03-28 deposited with the CCDC.	2024-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.079(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.4057(17)
_cell_length_b                   13.593(2)
_cell_length_c                   24.030(3)
_cell_measurement_reflns_used    4771
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      22.01
_cell_measurement_theta_min      2.20
_cell_volume                     5024.9(11)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            136965
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.726
_diffrn_reflns_theta_min         1.534
_exptl_absorpt_coefficient_mu    2.086
_exptl_absorpt_correction_T_max  0.4903
_exptl_absorpt_correction_T_min  0.4524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0947 before and 0.0604 after correction.
The Ratio of minimum to maximum transmission is 0.9227.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       block
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         9548
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0539P)^2^+4.3418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1159
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6980
_reflns_number_total             9548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00642a2.cif
_cod_data_source_block           rajnak_tlcr39_rt
_cod_depositor_comments
'Adding full bibliography for 7716293--7716294.cif.'
_cod_original_cell_volume        5024.8(12)
_cod_database_code               7716294
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.788
_shelx_estimated_absorpt_t_min   0.705
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C26-O5 \\sim C26-O5A
 with sigma of 0.03
 C40-O8 \\sim C40-O8A
 with sigma of 0.03
 C2-O1 \\sim C2-O1A
 with sigma of 0.03
3. Uiso/Uaniso restraints and constraints
Uanis(C44A) = Uanis(C44)
Uanis(O5) = Uanis(O5A)
Uanis(O1) = Uanis(O1A)
Uanis(C20) = Uanis(C20A)
Uanis(C45A) = Uanis(C45)
4. Same fragment restrains
{O4, C22, C23} sigma for 1-2: 0.01, 1-3: 0.02
as in
{O1, C20, C21}
{O4, C22, C23} sigma for 1-2: 0.01, 1-3: 0.02
as in
{O5, C44, C45}
{O4, C22, C23} sigma for 1-2: 0.01, 1-3: 0.02
as in
{O8, C46, C47}
{O4, C22, C23} sigma for 1-2: 0.01, 1-3: 0.02
as in
{O1A, C20A, C21A}
{O4, C22, C23} sigma for 1-2: 0.01, 1-3: 0.02
as in
{O5A, C44A, C45A}
{O4, C22, C23} sigma for 1-2: 0.01, 1-3: 0.02
as in
{O8A, C46A, C47A}
5. Others
 Sof(O1A)=Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(C21A)=Sof(H21D)=Sof(H21E)=
 Sof(H21F)=1-FVAR(1)
 Sof(O1)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=
 FVAR(1)
 Sof(O5A)=Sof(C44A)=Sof(H44C)=Sof(H44D)=Sof(C45A)=Sof(H45D)=Sof(H45E)=
 Sof(H45F)=1-FVAR(2)
 Sof(O5)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=
 FVAR(2)
 Sof(O8A)=Sof(C46A)=Sof(H46C)=Sof(H46D)=Sof(C47A)=Sof(H47D)=Sof(H47E)=
 Sof(H47F)=1-FVAR(3)
 Sof(O8)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=
 FVAR(3)
6.a Ternary CH refined with riding coordinates:
 N2(H2), N6(H6)
6.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
  C22(H22A,H22B), C20(H20A,H20B), C44(H44A,H44B), C46(H46A,H46B), C20A(H20C,
 H20D), C44A(H44C,H44D), C46A(H46C,H46D)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C13(H13), C17(H17), C18(H18), C19(H19),
 C27(H27), C28(H28), C29(H29), C31(H31), C37(H37), C41(H41), C42(H42), C43(H43)
6.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C21(H21A,H21B,H21C), C45(H45A,H45B,H45C), C47(H47A,H47B,
 H47C), C21A(H21D,H21E,H21F), C45A(H45D,H45E,H45F), C47A(H47D,H47E,H47F)
;
_shelx_res_checksum              20359
_olex2_submission_special_instructions 'No special instructions were received'