Trinuclear [FeIII2-Mg<sup>II</sup>] compounds with aminopyridines as precursors for supported CC bond hydrogenation catalysts at atmospheric pressure in a plug-flow reactor.
Koshenskova, Kseniya A.; Tigai, Yana A.; Nebykov, Denis N.; Lagutina, Anastasia V.; Mokhov, Vladimir M.; Dolgushin, Fedor M.; Razvorotneva, Lada S.; Efimov, Nikolay N.; Babeshkin, Konstantin A.; Gogoleva, Natalia V.; Imshennik, Vladimir K.; Novichikhin, Sergey V.; Eremenko, Igor L.; Lutsenko, Irina A.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 9329–9337; doi:10.1039/d5dt00653h

data_7718784
_publ_section_title
;
 Trinuclear [FeIII2-Mg<sup>II</sup>] compounds with aminopyridines as
 precursors for supported C&#xe001;C bond hydrogenation catalysts at
 atmospheric pressure in a plug-flow reactor.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9329
_journal_page_last               9337
_journal_paper_doi               10.1039/d5dt00653h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C35 H62 Fe2 Mg N2 O14, 1.5(C2 H3 N)'
_chemical_formula_sum            'C38 H66.5 Fe2 Mg N3.5 O14'
_chemical_formula_weight         932.45
_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   mixed
_audit_creation_date             2024-10-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2025-03-08 deposited with the CCDC.	2025-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.078(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.358(4)
_cell_length_b                   28.564(8)
_cell_length_c                   13.605(4)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.219
_cell_measurement_theta_min      2.483
_cell_volume                     5094(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_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)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            48153
_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         27.999
_diffrn_reflns_theta_min         2.109
_exptl_absorpt_coefficient_mu    0.640
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0766 before and 0.0400 after correction.
The Ratio of minimum to maximum transmission is 0.8913.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       prism
_exptl_crystal_F_000             1980
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         12287
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0378P)^2^+7.3250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1187
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9723
_reflns_number_total             12287
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00653h2.cif
_cod_data_source_block           mo_yan1_0m
_cod_depositor_comments
'Adding full bibliography for 7718784--7718785.cif.'
_cod_original_formula_sum        'C38 H66.50 Fe2 Mg N3.50 O14'
_cod_database_code               7718784
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.872
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C22'-C23'
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C24) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C3) = Uanis(C3')
Uanis(C4) = Uanis(C4')
Uanis(C5) = Uanis(C5')
Uanis(C7) = Uanis(C7')
Uanis(C8) = Uanis(C8')
Uanis(C9) = Uanis(C9')
Uanis(C10) = Uanis(C10')
Uanis(C13) = Uanis(C13')
Uanis(C14) = Uanis(C14')
Uanis(C15) = Uanis(C15')
Uanis(C18) = Uanis(C18')
Uanis(C19) = Uanis(C19')
Uanis(C20) = Uanis(C20')
Uanis(C22) = Uanis(C22')
Uanis(C23) = Uanis(C23')
Uanis(C24) = Uanis(C24')
Uanis(C25) = Uanis(C25')
Uanis(C27) = Uanis(C27')
Uanis(C28) = Uanis(C28')
Uanis(C29) = Uanis(C29')
Uanis(C30) = Uanis(C30')
Uanis(N1S) = Uanis(C1S) = Uanis(C2S) = Uanis(N1S') = Uanis(C1S') = Uanis(C2S')
Uanis(N2S) = Uanis(C3S) = Uanis(C4S) = Uanis(N2S') = Uanis(C3S') = Uanis(C4S')
4. Others
 Sof(C3')=Sof(H3'A)=Sof(H3'B)=Sof(H3'C)=Sof(C4')=Sof(H4'A)=Sof(H4'B)=Sof(H4'C)=
 Sof(C5')=Sof(H5'A)=Sof(H5'B)=Sof(H5'C)=1-FVAR(1)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5)=
 Sof(H5A)=Sof(H5B)=Sof(H5C)=FVAR(1)
 Sof(C7')=Sof(C8')=Sof(H8'A)=Sof(H8'B)=Sof(H8'C)=Sof(C9')=Sof(H9'A)=Sof(H9'B)=
 Sof(H9'C)=Sof(C10')=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(2)
 Sof(C7)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(2)
 Sof(C13')=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14')=Sof(H14D)=Sof(H14E)=
 Sof(H14F)=Sof(C15')=Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(3)
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(3)
 Sof(C18')=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19')=Sof(H19D)=Sof(H19E)=
 Sof(H19F)=Sof(C20')=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(4)
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(4)
 Sof(C22')=Sof(C23')=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24')=Sof(H24D)=
 Sof(H24E)=Sof(H24F)=Sof(C25')=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(5)
 Sof(C22)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=
 Sof(H24C)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(5)
 Sof(C27')=Sof(C28')=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29')=Sof(H29D)=
 Sof(H29E)=Sof(H29F)=Sof(C30')=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(6)
 Sof(C27)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(H29A)=Sof(H29B)=
 Sof(H29C)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(6)
 Sof(N1S')=Sof(C1S')=Sof(C2S')=Sof(H2SD)=Sof(H2SE)=Sof(H2SF)=1-FVAR(7)
 Sof(N1S)=Sof(C1S)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=Sof(H2SC)=FVAR(7)
 Fixed Sof: N2S(0.3) C3S(0.3) C4S(0.3) H4SA(0.3) H4SB(0.3) H4SC(0.3) N2S'(0.2)
 C3S'(0.2) C4S'(0.2) H4SD(0.2) H4SE(0.2) H4SF(0.2)
5.a Me refined with riding coordinates:
 C4S(H4SA,H4SB,H4SC), C4S'(H4SD,H4SE,H4SF)
5.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C33(H33), C34(H34), C35(H35)
5.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3'(H3'A,H3'B,H3'C),
 C4'(H4'A,H4'B,H4'C), C5'(H5'A,H5'B,H5'C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C8'(H8'A,H8'B,H8'C), C9'(H9'A,H9'B,H9'C), C10'(H10D,H10E,
 H10F), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C13'(H13D,H13E,H13F), C14'(H14D,H14E,H14F), C15'(H15D,H15E,H15F), C18(H18A,
 H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C18'(H18D,H18E,H18F),
 C19'(H19D,H19E,H19F), C20'(H20D,H20E,H20F), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C23'(H23D,H23E,H23F), C24'(H24D,H24E,H24F),
 C25'(H25D,H25E,H25F), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C28'(H28D,H28E,H28F), C29'(H29D,H29E,H29F), C30'(H30D,H30E,H30F),
 C2S(H2SA,H2SB,H2SC), C2S'(H2SD,H2SE,H2SF)
;
_shelx_res_checksum              64311
_shelx_hkl_checksum              53236
_olex2_submission_special_instructions 'No special instructions were received'