Intermolecular π-stacking stabilization of a new high-M/L-ratio coordination motif for a dinuclear Fe(III) complex supported by a "salen-type" Schiff base derivative of <i>o</i>-xylylenediamine.
Shutilov, Ilia D.; Volodin, Pavel A.; Ovsyannikov, Alexander S.; Pyataev, Andrew V.; Frantsuzova, Lyubov V.; Gerasimova, Daria P.; Khamatgalimov, Ayrat R.; Solovieva, Svetlana E.; Antipin, Igor S.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 10222–10226; doi:10.1039/d5dt00856e

data_7718850
_publ_section_title
;
 Intermolecular &#x3c0;-stacking stabilization of a new high-M/L-ratio
 coordination motif for a dinuclear Fe(III) complex supported by a
 "salen-type" Schiff base derivative of <i>o</i>-xylylenediamine.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10222
_journal_page_last               10226
_journal_paper_doi               10.1039/d5dt00856e
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C46 H42 Fe2 N4 O6'
_chemical_formula_sum            'C46 H42 Fe2 N4 O6'
_chemical_formula_weight         858.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-01-28
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2025-03-04 deposited with the CCDC.	2025-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.275(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0074(6)
_cell_length_b                   15.0503(9)
_cell_length_c                   11.4500(6)
_cell_measurement_reflns_used    5710
_cell_measurement_temperature    102.00
_cell_measurement_theta_max      24.37
_cell_measurement_theta_min      2.24
_cell_volume                     1885.50(18)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      102.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0909
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32043
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.243
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6683
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0928 before and 0.0699 after correction.
The Ratio of minimum to maximum transmission is 0.8958.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_description       prism
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.119
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0586
_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^)+(0.0444P)^2^+5.0863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1245
_refine_ls_wR_factor_ref         0.1324
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3003
_reflns_number_total             3713
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00856e2.cif
_cod_data_source_block           lub9_0m
_cod_depositor_comments
'Adding full bibliography for 7718850--7718852.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7718850
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.908
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C21(H21), C7(H7), C10(H10), C4(H4), C6(H6), C18(H18), C3(H3),
 C13(H13), C19(H19), C20(H20), C5(H5), C11(H11), C12(H12)
2.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C)
;
_shelx_res_checksum              28864
_shelx_hkl_checksum              70969
_olex2_submission_special_instructions 'No special instructions were received'