Magnetic anisotropy and slow relaxation of magnetisation in double salts containing four- and six-coordinate cobalt(II) complex ions.
Juráková, Jana; Santana, Vinicius Tadeu; Pavlik, Ján; Moncoľ, Ján; Nemec, Ivan; Clemente-León, Miguel; Kuppusamy, Senthil Kumar; Ruben, Mario; Čižmár, Erik; Šalitroš, Ivan; Dalton transactions (Cambridge, England : 2003) 53 (2024) 12962–12972; doi:10.1039/d4dt01509f

data_7716575
_publ_section_title
;
 Magnetic anisotropy and slow relaxation of magnetisation in double salts
 containing four- and six-coordinate cobalt(II) complex ions.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12962
_journal_page_last               12972
_journal_paper_doi               10.1039/d4dt01509f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C62 H74 Co N10, C4 Co N4 O4'
_chemical_formula_sum            'C66 H74 Co2 N14 O4'
_chemical_formula_weight         1245.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-18
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2024-05-01 deposited with the CCDC.	2024-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                109.687(4)
_cell_angle_beta                 90.185(4)
_cell_angle_gamma                117.019(4)
_cell_formula_units_Z            2
_cell_length_a                   15.6926(7)
_cell_length_b                   15.7264(6)
_cell_length_c                   16.0729(8)
_cell_measurement_reflns_used    30456
_cell_measurement_temperature    293
_cell_measurement_theta_max      66.65
_cell_measurement_theta_min      4.73
_cell_volume                     3268.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  XtaLAB
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33249
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.592
_diffrn_reflns_theta_min         2.972
_exptl_absorpt_coefficient_mu    4.431
_exptl_absorpt_correction_T_max  0.896
_exptl_absorpt_correction_T_min  0.563
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.57a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
_diffrn_measurement_device_type   
 'XtaLAB Synergy, Single source at home/near, HyPix3000'
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_description       block
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         11853
_refine_ls_number_restraints     975
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0629
_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^)+(0.1266P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1822
_refine_ls_wR_factor_ref         0.2009
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8244
_reflns_number_total             11853
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01509f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7716575--7716578.cif.'
_cod_database_code               7716575
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.777
_shelx_estimated_absorpt_t_min   0.556
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C46-C45
 1.5 with sigma of 0.02
 C11-C38 \\sim C11A-C38A
 with sigma of 0.02
 C30-C1 \\sim C30A-C1A
 with sigma of 0.04
 C1-C2 \\sim C1A-C2A
 with sigma of 0.02
 C38-C46 \\sim C38A-C46A
 with sigma of 0.04
 C19-C53 \\sim C19A-C53A
 with sigma of 0.04
 C26-C53 \\sim C26A-C53A
 with sigma of 0.02
 C62-C13 \\sim C13-C19 \\sim C19-C26
 with sigma of 0.02
 C38-C45 \\sim C38A-C45A
 with sigma of 0.02
 C45-C46 \\sim C45A-C46A
 with sigma of 0.02
 C29-C2 \\sim C29A-C2A
 with sigma of 0.04
 C4-C38 \\sim C4A-C38A
 with sigma of 0.04
 C28-C29 \\sim C28A-C29A
 with sigma of 0.02
 C29-C30 \\sim C29A-C30A
 with sigma of 0.02
 C28-C30 \\sim C28A-C30A
 with sigma of 0.04
 C27-C28 \\sim C27-C28A
 with sigma of 0.02
 C30-C2 \\sim C30A-C2A
 with sigma of 0.02
 C27-C29 \\sim C27-C29A
 with sigma of 0.04
 C4-C11 \\sim C4A-C11A
 with sigma of 0.02
 C63-C11 \\sim C63-C11A
 with sigma of 0.04
 C63-C4 \\sim C63-C4A
 with sigma of 0.02
 C11-C45 \\sim C11A-C45A
 with sigma of 0.04
 C19-C26 \\sim C19A-C26A
 with sigma of 0.02
 C61-C62 \\sim C61-C62A
 with sigma of 0.02
 C13-C19 \\sim C13A-C19A
 with sigma of 0.02
 C61-C13 \\sim C61-C13A
 with sigma of 0.04
 C62-C19 \\sim C62A-C19A
 with sigma of 0.04
 C62-C13 \\sim C62A-C13A
 with sigma of 0.02
 C13-C26 \\sim C13A-C26A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C19A \\sim C19 \\sim C26 \\sim C26A \\sim C53A \\sim C53: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 2A
C4 \\sim C4A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
C28A \\sim C29 \\sim C29A \\sim C28: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C62A \\sim C62 \\sim C13A \\sim C13: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(C11A) = Uanis(C11) = Uanis(C46) = Uanis(C46A) = Uanis(C45A) = Uanis(C45)
= Uanis(C38A) = Uanis(C38)
Uanis(C30A) = Uanis(C30) = Uanis(C2A) = Uanis(C2) = Uanis(C1A) = Uanis(C1)
Uanis(C19) = Uanis(C19A)
Uanis(C26) = Uanis(C26A)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(H27C)=Sof(H27D)=Sof(C28A)=Sof(H28C)=Sof(H28D)=Sof(C29A)=Sof(H29C)=
 Sof(H29D)=Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C1A)=
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=1-FVAR(1)
 Sof(H27A)=Sof(H27B)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C29)=Sof(H29A)=Sof(H29B)=
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=
 Sof(H2A)=Sof(H2B)=FVAR(1)
 Sof(H63C)=Sof(H63D)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C11A)=Sof(H11C)=
 Sof(H11D)=Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C45A)=Sof(H45C)=Sof(H45D)=
 Sof(C46A)=Sof(H46D)=Sof(H46E)=Sof(H46F)=1-FVAR(2)
 Sof(H63A)=Sof(H63B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C11)=Sof(H11A)=Sof(H11B)=
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=
 Sof(H46B)=Sof(H46C)=FVAR(2)
 Sof(H61C)=Sof(H61D)=Sof(C62A)=Sof(H62C)=Sof(H62D)=Sof(C13A)=Sof(H13C)=
 Sof(H13D)=Sof(C19A)=Sof(H19C)=Sof(H19D)=Sof(C26A)=Sof(H26C)=Sof(H26D)=
 Sof(C53A)=Sof(H53D)=Sof(H53E)=Sof(H53F)=1-FVAR(3)
 Sof(H61A)=Sof(H61B)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(C13)=Sof(H13A)=Sof(H13B)=
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C53)=Sof(H53A)=
 Sof(H53B)=Sof(H53C)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C63(H63A,H63B), C63(H63C,H63D), C32(H32A,H32B), C27(H27A,
 H27B), C27(H27C,H27D), C33(H33A,H33B), C61(H61A,H61B), C61(H61C,H61D),
 C34(H34A,H34B), C28(H28A,H28B), C62(H62A,H62B), C35(H35A,H35B), C29(H29A,H29B),
  C30(H30A,H30B), C2(H2A,H2B), C13(H13A,H13B), C28A(H28C,H28D), C29A(H29C,H29D),
  C30A(H30C,H30D), C2A(H2AA,H2AB), C4(H4A,H4B), C11(H11A,H11B), C38(H38A,H38B),
 C45(H45A,H45B), C4A(H4AA,H4AB), C11A(H11C,H11D), C38A(H38C,H38D), C45A(H45C,
 H45D), C19(H19A,H19B), C26(H26A,H26B), C62A(H62C,H62D), C13A(H13C,H13D),
 C19A(H19C,H19D), C26A(H26C,H26D)
6.b Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C1A(H1AA,H1AB,H1AC), C46(H46A,H46B,H46C), C53(H53A,H53B,
 H53C), C53A(H53D,H53E,H53F)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C15(H15), C43(H43), C9(H9), C7(H7), C50(H50), C48(H48), C8(H8),
 C16(H16), C49(H49), C23(H23), C24(H24), C17(H17), C58(H58), C55(H55), C42(H42),
  C21(H21), C56(H56), C40(H40), C57(H57), C41(H41), C22(H22)
6.d Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C46A(H46D,H46E,H46F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              31118
_shelx_hkl_checksum              3841
_shelx_fab_checksum              29970
_olex2_submission_special_instructions 'No special instructions were received'