Elucidating the role of the o-methoxy group in the lower rim appended salicylideneamine substituents of calix[4]arene ligands on the molecular and electronic structures of dinuclear Fe(iii)-based diamond-core complexes
Strelnikova, Iuliia V.; Shutilov, Ilya D.; Ovsyannikov, Alexander S.; Islamov, Daut R.; Pyataev, Andrew V.; Gerasimova, Tatiana P.; Khamatgalimov, Ayrat R.; Khrizanforov, Mikhail N.; Gubaidullin, Aidar T.; Burilov, Vladimir A.; Solovieva, Svetlana E.; Antipin, Igor S.; CrystEngComm 26 (2024) 3973–3988; doi:10.1039/D4CE00347K

data_7248903
_publ_section_title
;
 Elucidating the role of the o-methoxy group in the lower rim appended
 salicylideneamine substituents of calix[4]arene ligands on the molecular
 and electronic structures of dinuclear Fe(iii)-based diamond-core
 complexes
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              3973
_journal_page_last               3988
_journal_paper_doi               10.1039/D4CE00347K
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C130 H158 Fe2 N4 O14, 5(C H2 Cl2)'
_chemical_formula_sum            'C135 H168 Cl10 Fe2 N4 O14'
_chemical_formula_weight         2536.92
_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             2023-04-16
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-02-02 deposited with the CCDC.	2024-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.41(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.900(5)
_cell_length_b                   12.187(2)
_cell_length_c                   52.643(11)
_cell_measurement_reflns_used    652
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.012
_cell_measurement_theta_min      2.012
_cell_volume                     14534(5)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  synchro
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7454
_diffrn_reflns_av_R_equivalents  0.2064
_diffrn_reflns_av_unetI/netI     0.1696
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_number            109055
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.567
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         1.436
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.933
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange-red
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_description       prism
_exptl_crystal_F_000             5360
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.423
_refine_diff_density_min         -1.445
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1552
_refine_ls_number_reflns         30396
_refine_ls_number_restraints     145
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.2338
_refine_ls_R_factor_gt           0.1214
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3118
_refine_ls_wR_factor_ref         0.3953
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12443
_reflns_number_total             30396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00347k2.cif
_cod_data_source_block           kmv474
_cod_depositor_comments          'Adding full bibliography for 7248903.cif.'
_cod_database_code               7248903
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.865
_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, All O(H) groups
2. Restrained distances
 C125-C31 \\sim C31-C129
 with sigma of 0.001
 C63-C31 \\sim C31-C127
 with sigma of 0.001
 C143-C116 \\sim C116-C139
 with sigma of 0.001
 C123-C31 \\sim C31-C2
 with sigma of 0.001
 C131-C53 \\sim C53-C135
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C143) = Uanis(C139)
Uanis(C125) = Uanis(C127)
Uanis(C2) = Uanis(C63)
Uanis(C129) = Uanis(C123)
Uanis(C131) = Uanis(C135)
4. Rigid body (RIGU) restrains
 C69, C139, C35, C141, C71, C143, C9, C145
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C65, C131, C33, C133, C67, C135, C17, C137
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C123, C31, C125, C63, C127, C2, C129
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C25, C7, C57, C115
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl2, C61, Cl9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl7, C121, Cl3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C127)=Sof(H12N)=Sof(H12O)=Sof(H12P)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=
 Sof(C129)=Sof(H12Q)=Sof(H12R)=Sof(H12S)=1-FVAR(1)
 Sof(C123)=Sof(H12H)=Sof(H12I)=Sof(H12J)=Sof(C125)=Sof(H12K)=Sof(H12L)=
 Sof(H12M)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=FVAR(1)
 Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(H65C)=Sof(C131)=Sof(C33)=Sof(H33A)=Sof(H33B)=
 Sof(H33C)=Sof(C133)=Sof(H13J)=Sof(H13K)=Sof(H13L)=1-FVAR(2)
 Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(H67C)=Sof(C135)=Sof(C17)=Sof(H17A)=Sof(H17B)=
 Sof(H17C)=Sof(C137)=Sof(H13M)=Sof(H13N)=Sof(H13O)=FVAR(2)
 Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=Sof(C139)=Sof(C35)=Sof(H35A)=Sof(H35B)=
 Sof(H35C)=Sof(C141)=Sof(H14C)=Sof(H14D)=Sof(H14E)=1-FVAR(3)
 Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=Sof(C143)=Sof(C9)=Sof(H9A)=Sof(H9B)=
 Sof(H9C)=Sof(C145)=Sof(H14F)=Sof(H14G)=Sof(H14H)=FVAR(3)
6.a Free rotating group:
 Cl1(Cl4,C59), Cl6(Cl8,C119), Cl10(Cl5,C15), Cl3(Cl7,C121), Cl2(Cl9,C61),
 C123(C31,C125,C63), C65(C131,C33,C133), C67(C135,C17,C137), C69(C139,C35,C141),
  C71(C143,C9,C145)
6.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C30(H30A,H30B), C50(H50A,H50B), C58(H58A,H58B), C70(H70A,
 H70B), C80(H80A,H80B), C88(H88A,H88B), C92(H92A,H92B), C108(H10A,H10B),
 C120(H12A,H12B), C126(H12F,H12G), C130(H13A,H13B), C136(H13F,H13G), C140(H14A,
 H14B), C77(H77A,H77B), C41(H41A,H41B), C21(H21A,H21B), C85(H85A,H85B),
 C11(H11A,H11B), C13(H13H,H13I), C59(H59A,H59B), C119(H11I,H11J), C15(H15A,
 H15B), C121(H12T,H12U), C61(H61A,H61B)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C10(H10), C24(H24), C42(H42), C48(H48), C54(H54), C60(H60),
 C68(H68), C74(H74), C76(H76), C78(H78), C96(H96), C104(H104), C110(H110),
 C118(H118), C128(H128), C142(H142), C146(H146), C39(H39), C5(H5), C81(H81),
 C83(H83), C91(H91), C23(H23), C47(H47), C3(H3A), C49(H49), C51(H51),
 C103(H103), C107(H107), C27(H27), C109(H109), C55(H55), C111(H111), C113(H113)
6.d Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C124(H12C,H12D,H12E), C132(H13C,H13D,H13E), C37(H37A,
 H37B,H37C), C19(H19A,H19B,H19C), C87(H87A,H87B,H87C), C89(H89A,H89B,H89C),
 C45(H45A,H45B,H45C), C95(H95A,H95B,H95C), C97(H97A,H97B,H97C), C99(H99A,H99B,
 H99C), C101(H10C,H10D,H10E), C7(H7A,H7B,H7C), C57(H57A,H57B,H57C), C115(H11C,
 H11D,H11E), C29(H29A,H29B,H29C), C117(H11F,H11G,H11H), C123(H12H,H12I,H12J),
 C125(H12K,H12L,H12M), C63(H63A,H63B,H63C), C127(H12N,H12O,H12P), C2(H2A,H2B,
 H2C), C129(H12Q,H12R,H12S), C65(H65A,H65B,H65C), C33(H33A,H33B,H33C),
 C133(H13J,H13K,H13L), C67(H67A,H67B,H67C), C17(H17A,H17B,H17C), C137(H13M,H13N,
 H13O), C69(H69A,H69B,H69C), C35(H35A,H35B,H35C), C141(H14C,H14D,H14E),
 C71(H71A,H71B,H71C), C9(H9A,H9B,H9C), C145(H14F,H14G,H14H)
6.e Idealised tetrahedral OH refined as rotating group:
 O2(H2), O9(H9), O3(H3), O13(H13)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              27794
_shelx_fab_checksum              8026
_olex2_submission_special_instructions 'No special instructions were received'