Easy-axis magnetic anisotropy in tetragonally elongated cobalt(II) complexes beyond the spin-Hamiltonian formalism
Mičová, Romana; Rajnák, Cyril; Titis, Jan; Bieńko, Alina; Moncol, Jan; Samolova, Erika; Boca, Roman; Dalton Transactions  (2023) –; doi:10.1039/D3DT00990D

data_7712952
_publ_section_title
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 Easy-axis magnetic anisotropy in tetragonally elongated cobalt(II)
 complexes beyond the spin-Hamiltonian formalism
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00990D
_journal_year                    2023
_chemical_formula_moiety         'C24 H20 Co F12 N2 O4'
_chemical_formula_sum            'C24 H20 Co F12 N2 O4'
_chemical_formula_weight         687.351
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-15
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
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2023-01-15 deposited with the CCDC.	2023-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.335(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.9911(18)
_cell_length_b                   9.202(2)
_cell_length_c                   20.709(5)
_cell_measurement_reflns_used    3240
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      23.82
_cell_measurement_theta_min      2.43
_cell_volume                     1498.1(6)
_computing_cell_refinement       'SAINT v8.40B (Bruker, 2019)'
_computing_data_collection       'APEX4 v2022.1-1 (Bruker, 2022)'
_computing_data_reduction        'SAINT v8.40B (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.9992
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II Ultra'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.9992
_diffrn_reflns_Laue_measured_fraction_max 0.9992
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8689
_diffrn_reflns_point_group_measured_fraction_full 0.9992
_diffrn_reflns_point_group_measured_fraction_max 0.9992
_diffrn_reflns_theta_full        25.0244
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0904 before and 0.0378 after correction.
The Ratio of minimum to maximum transmission is 0.9407.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'orangish red'
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       block
_exptl_crystal_F_000             691.462
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.4161
_refine_diff_density_min         -0.2901
_refine_diff_density_rms         0.0525
_refine_ls_d_res_high            0.8401
_refine_ls_d_res_low             10.1867
_refine_ls_goodness_of_fit_ref   1.0645
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    35
_refine_ls_number_parameters     223
_refine_ls_number_reflns         2643
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.0584
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          -0.0010
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0864P)^2^+0.5342P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1459
_refine_ls_wR_factor_ref         0.1621
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                2017
_reflns_number_total             2643
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt00990d2.cif
_cod_data_source_block           1c
_cod_original_cell_volume        1498.2(6)
_cod_database_code               7712952
_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. Restrained distances
 C8-C11 \\sim C8-C11A
 with sigma of 0.02
 C1-F1 \\sim C1-F2 \\sim C1-F3 \\sim C1-F1A \\sim C1-F2A \\sim C1-F3A
 with sigma of 0.02
 C5-F4 \\sim C5-F5 \\sim C5-F6 \\sim C5-F4A \\sim C5-F5A \\sim C5-F6A
 with sigma of 0.02
 F1-F2 \\sim F1-F3 \\sim F2-F3 \\sim F1A-F2A \\sim F1A-F3A \\sim F2A-F3A
 with sigma of 0.04
 F4-F5 \\sim F4-F6 \\sim F5-F6 \\sim F4A-F5A \\sim F4A-F6A \\sim F5A-F6A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C11) = Uanis(C11A)
Uanis(C12) = Uanis(C12A)
Uanis(F1) = Uanis(F1A)
Uanis(F2) = Uanis(F2A)
Uanis(F3) = Uanis(F3A)
Uanis(F4) = Uanis(F4A)
Uanis(F5) = Uanis(F5A)
Uanis(F6) = Uanis(F6A)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{C11A, C12A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{C11, C12}
6. Others
 Sof(C11A)=Sof(H11c)=Sof(H11d)=Sof(C12A)=Sof(H12d)=Sof(H12e)=Sof(H12f)=1-FVAR(1)
 Sof(C11)=Sof(H11a)=Sof(H11b)=Sof(C12)=Sof(H12a)=Sof(H12b)=Sof(H12c)=FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(2)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(3)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(3)
7.a Secondary CH2 refined with riding coordinates:
 C11(H11a,H11b), C11A(H11c,H11d)
7.b Me refined with riding coordinates:
 C12(H12a,H12b,H12c), C12A(H12d,H12e,H12f)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C9(H9), C10(H10)
;
_olex2_submission_special_instructions 'No special instructions were received'