Influence of neutral auxiliary ligands on crystal structure and magnetic behaviour of new [MnII2MnIII2] clusters supported by p-adamantylcalix[4]arene
Ovsyannikov, Alexander S.; Strelnikova, Iuliia V.; Samigullina, Aida I.; Islamov, Daut R.; Cherosov, Mikhail A.; Batulin, Ruslan G.; Kiiamov, Airat G.; Gubaidullin, Aidar T.; Dorovatovskii, Pavel V.; Solovieva, Svetlana E.; Antipin, Igor S.; New Journal of Chemistry 48 (2024) 203–215; doi:10.1039/D3NJ04809H

data_7062887
_publ_section_title
;
 Influence of neutral auxiliary ligands on crystal structure and magnetic
 behaviour of new [MnII2MnIII2] clusters supported by
 p-adamantylcalix[4]arene
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              203
_journal_page_last               215
_journal_paper_doi               10.1039/D3NJ04809H
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C156 H170 Mn4 N4 O10, 4(C3 H7 N O)'
_chemical_formula_sum            'C168 H198 Mn4 N8 O14'
_chemical_formula_weight         2773.09
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-08-10
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2023-11-15 deposited with the CCDC.	2023-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.27(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.357(3)
_cell_length_b                   25.859(5)
_cell_length_c                   18.043(4)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.936
_cell_measurement_theta_min      1.999
_cell_volume                     7599(3)
_computing_data_collection       'XDS (Kabsh, 2010)'
_computing_data_reduction        'XDS (Kabsh, 2010)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.79313
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            41227
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        28.417
_diffrn_reflns_theta_max         30.936
_diffrn_reflns_theta_min         1.999
_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_T_max  0
_exptl_absorpt_correction_T_min  0
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XDS (Kabsh, 2010)'
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       prism
_exptl_crystal_F_000             2948
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.441
_refine_diff_density_min         -0.971
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.0049(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     964
_refine_ls_number_reflns         16429
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0924P)^2^+5.3300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1628
_refine_ls_wR_factor_ref         0.1820
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11340
_reflns_number_total             16429
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj04809h2.cif
_cod_data_source_block           kmv287
_cod_depositor_comments
'Adding full bibliography for 7062886--7062889.cif.'
_cod_original_cell_volume        7600(3)
_cod_database_code               7062887
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.903
_olex2_refinement_description
;
1. Restrained distances
 H5-O5
 0.9 with sigma of 0.01
 C49-C54 \\sim C49-C53
 with sigma of 0.02
 C49-C52 \\sim C49-C51
 with sigma of 0.02
 C49-C50 \\sim C49-C55
 with sigma of 0.02
 C58-C60 \\sim C67-C57
 with sigma of 0.02
 C58-C56 \\sim C67-C66
 with sigma of 0.02
 C63-C65 \\sim C62-C64
 with sigma of 0.02
 C63-C61 \\sim C62-C59
 with sigma of 0.02
 C63-C54 \\sim C62-C53
 with sigma of 0.02
 C65-C56 \\sim C64-C66
 with sigma of 0.02
 C61-C60 \\sim C59-C57
 with sigma of 0.02
 C60-C52 \\sim C57-C51
 with sigma of 0.02
 C56-C50 \\sim C66-C55
 with sigma of 0.02
 C49-C63 \\sim C49-C62
 with sigma of 0.04
 C49-C60 \\sim C49-C57
 with sigma of 0.04
 C49-C56 \\sim C49-C66
 with sigma of 0.04
 C58-C65 \\sim C67-C64
 with sigma of 0.04
 C58-C61 \\sim C67-C59
 with sigma of 0.04
 C58-C52 \\sim C67-C51
 with sigma of 0.04
 C58-C50 \\sim C67-C55
 with sigma of 0.04
 C63-C60 \\sim C62-C57
 with sigma of 0.04
 C63-C56 \\sim C62-C66
 with sigma of 0.04
 C65-C61 \\sim C64-C59
 with sigma of 0.04
 C65-C54 \\sim C64-C53
 with sigma of 0.04
 C65-C50 \\sim C64-C55
 with sigma of 0.04
 C61-C54 \\sim C59-C53
 with sigma of 0.04
 C61-C52 \\sim C59-C51
 with sigma of 0.04
 C60-C56 \\sim C57-C66
 with sigma of 0.04
 C52-C49 \\sim C49-C53
 with sigma of 0.02
 C53-C49 \\sim C49-C54
 with sigma of 0.02
 C54-C49 \\sim C49-C55
 with sigma of 0.02
 C55-C49 \\sim C49-C50
 with sigma of 0.02
 C50-C49 \\sim C49-C51
 with sigma of 0.02
 C51-C49 \\sim C49-C52
 with sigma of 0.02
2. Others
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C62)=Sof(H62)=Sof(C59)=Sof(H59A)=Sof(H59B)=
 Sof(C57)=Sof(H57)=Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(C66)=Sof(H66)=Sof(C64)=
 Sof(H64A)=Sof(H64B)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(C51)=Sof(H51A)=Sof(H51B)=
 1-FVAR(1)
 Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(C63)=Sof(H63)=Sof(C65)=Sof(H65A)=Sof(H65B)=
 Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(C60)=Sof(H60)=Sof(C56)=Sof(H56)=Sof(C54)=
 Sof(H54A)=Sof(H54B)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(C50)=Sof(H50A)=Sof(H50B)=
 FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C76(H76), C74(H74), C72(H72), C47(H47), C43(H43), C45(H45), C63(H63),
 C37(H37), C35(H35), C60(H60), C56(H56), C33(H33), C62(H62), C57(H57), C66(H66)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C22(H22A,H22B), C15(H15A,H15B), C70(H70A,H70B), C8(H8A,H8B),
 C71(H71A,H71B), C69(H69A,H69B), C42(H42A,H42B), C40(H40A,H40B), C41(H41A,H41B),
  C73(H73A,H73B), C77(H77A,H77B), C75(H75A,H75B), C48(H48A,H48B), C58(H58A,
 H58B), C46(H46A,H46B), C44(H44A,H44B), C32(H32A,H32B), C30(H30A,H30B),
 C65(H65A,H65B), C31(H31A,H31B), C61(H61A,H61B), C36(H36A,H36B), C34(H34A,H34B),
  C54(H54A,H54B), C38(H38A,H38B), C52(H52A,H52B), C50(H50A,H50B), C53(H53A,
 H53B), C59(H59A,H59B), C67(H67A,H67B), C64(H64A,H64B), C55(H55A,H55B),
 C51(H51A,H51B)
3.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C26(H26), C5(H5A), C12(H12), C19(H19), C10(H10), C3(H3), C17(H17),
 C84(H84), C87(H87), C78(H78), C93(H93), C86(H86), C81(H81), C90(H90), C79(H79),
  C80(H80), C85(H85)
3.d Idealised Me refined as rotating group:
 C88(H88A,H88B,H88C), C89(H89A,H89B,H89C), C91(H91A,H91B,H91C), C92(H92A,H92B,
 H92C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              82652
_shelx_hkl_checksum              74925
_shelx_fab_checksum              46997
_olex2_submission_special_instructions 'No special instructions were received'