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_7715821
_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         'C33 H30 Co N9 P S, 2(Cl O4), 2(C H4 O)'
_chemical_formula_sum            'C35 H38 Cl2 Co N9 O10 P S'
_chemical_formula_weight         937.60
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-08
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-08 deposited with the CCDC.	2024-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.7780(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7990(7)
_cell_length_b                   15.1731(6)
_cell_length_c                   17.5313(7)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      28.201
_cell_measurement_theta_min      2.403
_cell_volume                     4063.6(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'four-circle diffractomenter'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45118
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.280
_diffrn_reflns_theta_min         2.403
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8722
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0863 before and 0.0576 after correction.
The Ratio of minimum to maximum transmission is 0.8722.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1932
_exptl_crystal_size_max          0.129
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.061
_refine_diff_density_max         1.343
_refine_diff_density_min         -1.298
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         10053
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1161
_refine_ls_R_factor_gt           0.0819
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0908P)^2^+21.3891P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1981
_refine_ls_wR_factor_ref         0.2237
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7233
_reflns_number_total             10053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00622d2.cif
_cod_data_source_block           compound_4
_cod_depositor_comments
'Adding full bibliography for 7715819--7715822.cif.'
_cod_database_code               7715821
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 Cl1-O1 = Cl1-O2 = Cl1-O3 = Cl1-O4
 1.44 with sigma of 0.01
 Cl1A-O1A = Cl1A-O2A = Cl1A-O3A = Cl1A-O4A
 1.44 with sigma of 0.01
 O1-O2 = O1-O3 = O1-O4 = O2-O3 = O2-O4 = O3-O4
 2.35 with sigma of 0.01
 O1A-O2A = O1A-O3A = O1A-O4A = O2A-O3A = O2A-O4A = O3A-O4A
 2.35 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O1A \\sim O2A \\sim O3A \\sim O4A: within
2.6A with sigma of 0.04 and sigma for terminal atoms of 0.04 within 2.6A
4. Others
 Fixed Sof: O3(0.7) O4(0.7) Cl1(0.7) Cl1A(0.3) O2(0.7) O1(0.7) O4A(0.3)
 O2A(0.3) O1A(0.3) O3A(0.3)
5.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C23(H23), C9(H9), C24(H24), C14(H14), C15(H15), C18(H18),
 C21(H21), C33(H33), C10(H10), C12(H12), C27(H27), C19(H19), C11(H11), C6(H6),
 C20(H20), C30(H30), C29(H29), C32(H32), C28(H28)
5.b Idealised Me refined as rotating group:
 C00X(H00A,H00B,H00C), C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C35(H35A,H35B,H35C),
 C34(H34A,H34B,H34C)
5.c Idealised tetrahedral OH refined as rotating group:
 O10(H10A), O9(H9A)
;
_shelx_res_checksum              59070
_olex2_submission_special_instructions 'No special instructions were received'