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_7712953
_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         'C34 H22 Cl2 Co F12 N2 O4'
_chemical_formula_sum            'C34 H22 Cl2 Co F12 N2 O4'
_chemical_formula_weight         880.384
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-03
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
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_audit_update_record
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2023-01-15 deposited with the CCDC.	2023-05-04 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 107.966(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.1173(9)
_cell_length_b                   14.4277(13)
_cell_length_c                   14.3485(14)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.75
_cell_measurement_theta_min      2.73
_cell_volume                     1795.4(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT V8.40A (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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9131
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II Ultra CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9131
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24070
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.9131
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         30.60
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.731
_exptl_absorpt_correction_T_max  0.6466
_exptl_absorpt_correction_T_min  0.5890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0563 before and 0.0408 after correction.
The Ratio of minimum to maximum transmission is 0.9109.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_description       block
_exptl_crystal_F_000             884.129
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.7641
_refine_diff_density_min         -0.5369
_refine_diff_density_rms         0.0765
_refine_ls_d_res_high            0.6982
_refine_ls_d_res_low             9.9151
_refine_ls_goodness_of_fit_ref   1.0508
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    21
_refine_ls_number_parameters     309
_refine_ls_number_reflns         5045
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.0456
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          -0.0008
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0115P)^2^+1.0388P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0566
_refine_ls_wR_factor_ref         0.0611
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -13
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              -8
_reflns_number_gt                4230
_reflns_number_total             5045
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt00990d2.cif
_cod_data_source_block           2
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7712953
_olex2_refinement_description
;
1. Restrained distances
 C8-H8
 1.083 with sigma of 0.02
 C15-H15
 1.083 with sigma of 0.02
 C11-H11
 1.083 with sigma of 0.02
 C6-H6a = C6-H6b
 1.092 with sigma of 0.02
 C1-H1
 1.083 with sigma of 0.02
 C9-H9
 1.083 with sigma of 0.02
 C2-H2
 1.083 with sigma of 0.02
 C12-H12
 1.083 with sigma of 0.02
 C4-H4
 1.083 with sigma of 0.02
 C5-H5
 1.083 with sigma of 0.02
 C13-F1 \\sim C13-F2 \\sim C13-F3 \\sim C13A-F1A \\sim C13A-F2A \\sim C13A-F3A
\\sim C17-F4 \\sim C17-F5 ~
 C17-F6 \\sim C17A-F4A \\sim C17A-F5A \\sim C17A-F6A
 with sigma of 0.02
 C14-C13 \\sim C14-C13A \\sim C16-C17 \\sim C16-C17A
 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
Uanis(C17) = Uanis(C17A)
Uanis(C13) = Uanis(C13A)
Uanis(F1) = Uanis(F1A)
Uanis(F2) = Uanis(F2A)
Uanis(F3) = Uanis(F3A)
Uanis(F4) = Uanis(F6A)
Uanis(F5A) = Uanis(F6)
Uanis(F4A) = Uanis(F5)
3. Rigid body (RIGU) restrains
 C17, F5, F6, F4, C13, F3, F2, F1, C17A, F5A, F6A, F4A, C13A, F2A, F3A, F1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C17A)=Sof(F5A)=Sof(F6A)=Sof(F4A)=1-FVAR(1)
 Sof(C17)=Sof(F5)=Sof(F6)=Sof(F4)=FVAR(1)
 Sof(C13A)=Sof(F2A)=Sof(F3A)=Sof(F1A)=1-FVAR(2)
 Sof(C13)=Sof(F3)=Sof(F2)=Sof(F1)=FVAR(2)
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_olex2_submission_special_instructions 'No special instructions were received'