Unveiling the Relationship between Counterion Size and Spin Crossover Dynamics in Hexadentate Schiff-Base Manganese(III) Complexes
Shang, Meng-Jia; Chen, Duyong; Zhou, Ren-He; Lu, Han-Han; Ma, Lin; Xiao, Jingyi; Zhao, Liang; Meng, Yin-Shan; Liu, Tao; Dalton Transactions  (2025) –; doi:10.1039/D5DT01347J

data_7719160
_publ_section_title
;
 Unveiling the Relationship between Counterion Size and Spin Crossover
 Dynamics in Hexadentate Schiff-Base Manganese(III) Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D5DT01347J
_journal_year                    2025
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C22 H26 F2 Mn N4 O2, N O3'
_chemical_formula_sum            'C22 H26 F2 Mn N5 O5'
_chemical_formula_weight         533.42
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-07-03
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-07-05 deposited with the CCDC.	2025-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0868(7)
_cell_length_b                   16.1944(15)
_cell_length_c                   18.3469(15)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      25.090
_cell_measurement_theta_min      2.220
_cell_volume                     2402.7(4)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      300(2)
_diffrn_detector                 'Bruker PHOTON-II area detector'
_diffrn_detector_area_resol_mean 7.4
_diffrn_detector_type            'CMOS-PHOTONII area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTON-II area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24035
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.684
_diffrn_reflns_theta_min         2.220
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           1.6
_diffrn_source_power             0.08
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1168 before and 0.0448 after correction.
The Ratio of minimum to maximum transmission is 0.8994.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic blackish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.236
_refine_diff_density_min         -0.146
_refine_diff_density_rms         0.031
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.48(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         4539
_refine_ls_number_restraints     724
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0309
_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^)+(0.0376P)^2^+0.4021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0777
_reflns_Friedel_coverage         0.749
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                4008
_reflns_number_total             4539
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01347j2.cif
_cod_data_source_block           2441909
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_database_code               7719160
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.888
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.52(3)
 0.48(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
3. Restrained planarity
 O2, F2A, C15A, C16A, C17A, C18A, C19A, C21A, C22A
 with sigma of 0.01
 C6A, C4A, C3A, C1A, C5A, C2A, F1A, O1, C7A
 with sigma of 0.01
 C6, C4, C3, C1, C5, C2, F1, O1, C7
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
O1 \\sim N4 \\sim F1 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6
\\sim C7 \\sim N4 \\sim F1A \\sim C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A
\\sim C6A \\sim C7A: within 2A with sigma of 0.02 and sigma for terminal atoms
of 0.04 within 2A
O2 \\sim N3 \\sim F2 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim
C21 \\sim C22 \\sim F2A \\sim C15A \\sim C16A \\sim C17A \\sim C18A \\sim C19A
\\sim C21A \\sim C22A: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 2A
O3 \\sim O4 \\sim O5 \\sim N5 \\sim O3A \\sim O4A \\sim O5A \\sim N5A: within
2A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
5. Same fragment restrains
{O1, N4, F1A, C1A, C2A, C3A, C4A, C5A, C6A, C7A} sigma for 1-2: 0.01, 1-3: 0.04
as in
{O1, N4, F1, C1, C2, C3, C4, C5, C6, C7}
{O2, N3, F2A, C15A, C16A, C17A, C18A, C19A, C21A, C22A} sigma for 1-2: 0.01,
1-3: 0.04
as in
{O2, N3, F2, C15, C16, C17, C18, C19, C21, C22}
{O3A, O4A, O5A, N5A} sigma for 1-2: 0.01, 1-3: 0.04
as in
{O3, O4, O5, N5}
6. Others
 Sof(O3A)=Sof(O4A)=Sof(O5A)=Sof(N5A)=1-FVAR(1)
 Sof(O3)=Sof(O4)=Sof(O5)=Sof(N5)=FVAR(1)
 Sof(F2A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=
 Sof(H18A)=Sof(C19A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=1-FVAR(2)
 Sof(F2)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=
 Sof(C19)=Sof(C21)=Sof(H21)=Sof(C22)=FVAR(2)
 Sof(F1A)=Sof(C1A)=Sof(C2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=
 Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7A)=1-FVAR(3)
 Sof(F1)=Sof(C1)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(C6)=
 Sof(H6)=Sof(C7)=Sof(H7)=FVAR(3)
7.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2)
7.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C14(H14A,H14B), C20(H20A,H20B)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C15(H15), C17(H17), C18(H18), C21(H21),
 C3A(H3A), C4A(H4A), C6A(H6A), C7A(H7A), C15A(H15A), C17A(H17A), C18A(H18A),
 C21A(H21A)
;
_shelx_res_checksum              12123
_shelx_hkl_checksum              85075
_olex2_submission_special_instructions 'No special instructions were received'