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_7718852
_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         'C28 H32 Br2 Cl2 Fe2 N2 O8'
_chemical_formula_sum            'C28 H32 Br2 Cl2 Fe2 N2 O8'
_chemical_formula_weight         866.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-02-21
_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                 110.849(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9195(13)
_cell_length_b                   13.4258(14)
_cell_length_c                   12.5162(13)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      29.52
_cell_measurement_theta_min      2.31
_cell_volume                     1871.8(3)
_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      150.00
_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  0.0615
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            35651
_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         25.998
_diffrn_reflns_theta_min         2.309
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.096
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.7519
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1408 before and 0.0679 after correction.
The Ratio of minimum to maximum transmission is 0.8101.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       prism
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.408
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.064
_refine_diff_density_max         1.449
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3681
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0561P)^2^+6.2818P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1298
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3058
_reflns_number_total             3681
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00856e2.cif
_cod_data_source_block           lub148_0m
_cod_depositor_comments
'Adding full bibliography for 7718850--7718852.cif.'
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               7718852
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.826
_shelx_estimated_absorpt_t_min   0.365
_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. Rigid bond restraints
 O4, Fe1, O3, O2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
Fe1 \\sim O4 \\sim O3 \\sim O2: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 2A
4. Rigid body (RIGU) restrains
 Fe1, O4, O3, O2
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C4(H4), C6(H6), C10(H10), C11(H11)
5.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              93155
_shelx_hkl_checksum              1201
_shelx_fab_checksum              46029
_olex2_submission_special_instructions 'No special instructions were received'