Control of the geometry and anisotropy driven by the combination of steric and anion coordination effects in Co<sup>II</sup> complexes with N<sub>6</sub>-tripodal ligands: the impact of the size of the ligand on the magnetization relaxation time.
Landart, Aritz; Quesada-Moreno, María Mar; Palacios, María A; Li, Yanling; Ozerov, Mykhaylo; Krzystek, J.; Colacio, Enrique; Dalton transactions (Cambridge, England : 2003) 53 (2024) 12876–12892; doi:10.1039/d4dt00622d

data_7715819
_publ_section_title
;
 Control of the geometry and anisotropy driven by the combination of
 steric and anion coordination effects in Co<sup>II</sup> complexes with
 N<sub>6</sub>-tripodal ligands: the impact of the size of the ligand on
 the magnetization relaxation time.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12876
_journal_page_last               12892
_journal_paper_doi               10.1039/d4dt00622d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C35.5 H30.007 Co N11 O P S3, 0.75(C O), 1.5(O)'
_chemical_formula_sum            'C36.25 H30.01 Co N11 O3.25 P S3'
_chemical_formula_weight         857.80
_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             2024-02-22
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-02-23 deposited with the CCDC.	2024-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                77.604(2)
_cell_angle_beta                 79.837(2)
_cell_angle_gamma                85.377(2)
_cell_formula_units_Z            2
_cell_length_a                   7.5558(6)
_cell_length_b                   16.3975(14)
_cell_length_c                   18.6509(15)
_cell_measurement_reflns_used    7235
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      20.823
_cell_measurement_theta_min      2.362
_cell_volume                     2219.3(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'four-circle diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20748
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        20.925
_diffrn_reflns_theta_max         20.925
_diffrn_reflns_theta_min         2.267
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.610
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8546
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0862 before and 0.0551 after correction.
The Ratio of minimum to maximum transmission is 0.8546.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             881
_exptl_crystal_size_max          0.448
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.022
_refine_diff_density_max         1.490
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         4662
_refine_ls_number_restraints     256
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0738
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1056P)^2^+19.7660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2018
_refine_ls_wR_factor_ref         0.2179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3802
_reflns_number_total             4662
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00622d2.cif
_cod_data_source_block           compound_1
_cod_depositor_comments
'Adding full bibliography for 7715819--7715822.cif.'
_cod_database_code               7715819
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.772
_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
 C6-C25 \\sim C6-C25A
 with sigma of 0.02
 N9-C25 \\sim N9A-C25A
 with sigma of 0.02
 N9-C33 \\sim N9A-C33A
 with sigma of 0.02
 C30-C32 \\sim C30A-C32A
 with sigma of 0.04
 C25-C26 \\sim C25A-C26A
 with sigma of 0.02
 C26-C28 \\sim C26A-C28A
 with sigma of 0.04
 C27-C29 \\sim C27A-C29A
 with sigma of 0.04
 C26-C27 \\sim C26A-C27A
 with sigma of 0.02
 C27-C28 \\sim C27A-C28A
 with sigma of 0.02
 C28-C30 \\sim C28A-C30A
 with sigma of 0.04
 C28-C29 \\sim C28A-C29A
 with sigma of 0.02
 C28-C33 \\sim C28A-C33A
 with sigma of 0.02
 C29-C31 \\sim C29A-C31A
 with sigma of 0.04
 C31-C33 \\sim C31A-C33A
 with sigma of 0.04
 C29-C30 \\sim C29A-C30A
 with sigma of 0.02
 C30-C31 \\sim C30A-C31A
 with sigma of 0.02
 C31-C32 \\sim C31A-C32A
 with sigma of 0.02
 C32-C33 \\sim C32A-C33A
 with sigma of 0.02
 C27-C33 \\sim C27A-C33A
 with sigma of 0.04
 C28-C32 \\sim C28A-C32A
 with sigma of 0.04
 C29-C33 \\sim C29A-C33A
 with sigma of 0.04
 C6-N9 \\sim C6-N9A
 with sigma of 0.04
 C6-C26 \\sim C6-C26A
 with sigma of 0.04
 N9-C26 \\sim N9A-C26A
 with sigma of 0.04
 N9-C28 \\sim N9A-C28A
 with sigma of 0.04
 N9-C32 \\sim N9A-C32A
 with sigma of 0.04
 C25-C27 \\sim C25A-C27A
 with sigma of 0.04
 C25-C33 \\sim C25A-C33A
 with sigma of 0.04
 C16A-C18 \\sim C16-C18A
 with sigma of 0.04
 C18-C20 \\sim C18A-C20A
 with sigma of 0.04
 C19-C21 \\sim C19A-C21A
 with sigma of 0.04
 C20-C22 \\sim C20A-C22A
 with sigma of 0.04
 C21-C23 \\sim C21A-C23A
 with sigma of 0.04
 C5-C16A \\sim C5-C16
 with sigma of 0.02
 N8-C16A \\sim N8A-C16
 with sigma of 0.02
 N8-C24 \\sim N8A-C24A
 with sigma of 0.02
 C16A-C17 \\sim C16-C17A
 with sigma of 0.02
 C17-C18 \\sim C17A-C18A
 with sigma of 0.02
 C22-C24 \\sim C22A-C24A
 with sigma of 0.04
 C18-C19 \\sim C18A-C19A
 with sigma of 0.02
 C16A-C24 \\sim C16-C24A
 with sigma of 0.04
 C19-C20 \\sim C19A-C20A
 with sigma of 0.02
 C19-C24 \\sim C19A-C24A
 with sigma of 0.02
 C17-C19 \\sim C17A-C19A
 with sigma of 0.04
 C18-C24 \\sim C18A-C24A
 with sigma of 0.04
 C20-C21 \\sim C20A-C21A
 with sigma of 0.02
 C19-C23 \\sim C19A-C23A
 with sigma of 0.04
 C21-C22 \\sim C21A-C22A
 with sigma of 0.02
 C22-C23 \\sim C22A-C23A
 with sigma of 0.02
 C20-C24 \\sim C20A-C24A
 with sigma of 0.04
 C23-C24 \\sim C23A-C24A
 with sigma of 0.02
 C5-N8 \\sim C5-N8A
 with sigma of 0.04
 C5-C17 \\sim C5-C17A
 with sigma of 0.04
 N8-C17 \\sim N8A-C17A
 with sigma of 0.04
 N8-C19 \\sim N8A-C19A
 with sigma of 0.04
 N8-C23 \\sim N8A-C23A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C35) = Uanis(C35A)
Uiso(C31) = Uiso(C30A)
Uiso(C16) = Uiso(C16A)
Uiso(C17) = Uiso(C17A)
Uiso(C19) = Uiso(C19A)
Uiso(C20) = Uiso(C20A)
Uiso(C21) = Uiso(C21A)
Uiso(C22) = Uiso(C22A)
Uiso(C23) = Uiso(C23A)
Uiso(C24) = Uiso(C24A)
Uiso(N8) = Uiso(N8A)
Uiso(C18) = Uiso(C18A)
Uiso(C26) = Uiso(C26A)
Uiso(C27) = Uiso(C27A)
Uiso(C28) = Uiso(C28A)
Uiso(C29) = Uiso(C29A)
Uiso(C30) = Uiso(C30A)
Uiso(C31) = Uiso(C31A)
Uiso(C32) = Uiso(C32A)
Uiso(C33) = Uiso(C33A)
Uiso(N9) = Uiso(N9A)
Uiso(C25) = Uiso(C25A)
4. Same fragment restrains
{N7, C7, C8, C9, C10, C11, C12, C13, C14, C15} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N9, C25, C26, C27, C28, C29, C30, C31, C32, C33}
{N7, C7, C8, C9, C10, C11, C12, C13, C14, C15} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N8, C16A, C17, C18, C19, C20, C21, C22, C23, C24}
5. Others
 Sof(H5B)=Sof(C24A)=1-FVAR(1)
 Sof(H5A)=Sof(C22)=Sof(H22)=FVAR(1)
 Fixed Sof: H6A(0.5) H6B(0.5) N8(0.5) C16A(0.5) C17(0.5) H17(0.5) C18(0.5)
 H18(0.5) C19(0.5) C20(0.5) H20(0.5) C21(0.5) H21(0.5) C23(0.5) H23(0.5)
 C24(0.5) N9(0.5) C25(0.5) C26(0.5) H26(0.5) C27(0.5) H27(0.5) C28(0.5)
 C29(0.5) H29(0.5) C30(0.5) H30(0.5) C31(0.5) H31(0.5) C32(0.5) H32(0.5)
 C33(0.5) C35(0.5) S3(0.5) C35A(0.5) S3A(0.5) C26A(0.5) H26A(0.5) C27A(0.5)
 H27A(0.5) C28A(0.5) C29A(0.5) H29A(0.5) C30A(0.5) H30A(0.5) C31A(0.5)
 H31A(0.5) C32A(0.5) H32A(0.5) C33A(0.5) N9A(0.5) C25A(0.5) C17A(0.5) H17A(0.5)
 C16(0.5) N8A(0.5) C19A(0.5) C18A(0.5) H18A(0.5) C20A(0.5) H20A(0.5) C21A(0.5)
 H21A(0.5) C22A(0.5) H22A(0.5) C23A(0.5) H23A(0.5) O3(0.75) O2(0.5) C37(0.75)
 C36(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6A), C6(H6B), C5(H5A), C5(H5B), C8(H8), C9(H9), C11(H11),
 C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22),
  C23(H23), C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32),
 C26A(H26A), C27A(H27A), C29A(H29A), C30A(H30A), C31A(H31A), C32A(H32A),
 C17A(H17A), C18A(H18A), C20A(H20A), C21A(H21A), C22A(H22A), C23A(H23A)
6.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              25392
_olex2_submission_special_instructions 'No special instructions were received'