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_7715822
_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 H30 Co N11 P S3, H O0.5, O, C H3.25 O'
_chemical_formula_sum            'C36 H37 Co N11 O2.5 P S3'
_chemical_formula_weight         849.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2023-09-11
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-02-23 deposited with the CCDC.	2024-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.188(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.919(3)
_cell_length_b                   13.9992(13)
_cell_length_c                   20.960(2)
_cell_measurement_reflns_used    9763
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.285
_cell_measurement_theta_min      2.650
_cell_volume                     7826.2(13)
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_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  0.0417
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            44118
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.371
_diffrn_reflns_theta_min         2.433
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.690
_exptl_absorpt_correction_T_max  0.9010
_exptl_absorpt_correction_T_min  0.8397
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0800 before and 0.0580 after correction.
The Ratio of minimum to maximum transmission is 0.9320.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3520
_exptl_crystal_size_max          0.369
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.162
_refine_diff_density_max         1.254
_refine_diff_density_min         -1.121
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.00146(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         9704
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0436P)^2^+29.0729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1231
_refine_ls_wR_factor_ref         0.1292
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8230
_reflns_number_total             9704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00622d2.cif
_cod_data_source_block           compound_3
_cod_depositor_comments
'Adding full bibliography for 7715819--7715822.cif.'
_cod_original_cell_volume        7826.2(14)
_cod_original_formula_sum        'C36 H37 Co N11 O2.50 P S3'
_cod_database_code               7715822
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.896
_shelx_estimated_absorpt_t_min   0.785
_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, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O3) = Uanis(O3A)
Uanis(O2) = Uanis(O2A)
3. Same fragment restrains
{N8, C16, C17, C18, C19, C20, C21, C22, C23, C24} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N9A, C25A, C26A, C27A, C28A, C29A, C30A, C31A, C32A, C33A}
{N8, C16, C17, C18, C19, C20, C21, C22, C23, C24} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N9, C25, C26, C27, C28, C29, C30, C31, C32, C33}
4. Others
 Fixed Sof: H6A(0.5) H6B(0.5) N9(0.5) C25(0.5) C26(0.5) C27(0.5) H27(0.5)
 C28(0.5) H28(0.5) C29(0.5) H29(0.5) C30(0.5) H30(0.5) C31(0.5) C32(0.5)
 H32(0.5) C33(0.5) H33(0.5) N9A(0.5) C25A(0.5) C26A(0.5) C27A(0.5) H27A(0.5)
 C28A(0.5) H28A(0.5) C29A(0.5) H29A(0.5) C30A(0.5) H30A(0.5) C31A(0.5)
 C32A(0.5) H32A(0.5) C33A(0.5) H33A(0.5) O3(0.5) O3A(0.5) O2(0.75) H2(0.75)
 H36A(0.75) H36B(0.75) H36C(0.75) O2A(0.25) H2AA(0.25)
5.a Riding coordinates:
 O1(H1)
5.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C5(H5), C10(H10), C9(H9), C11(H11), C6(H6A), C6(H6B), C4(H4),
 C12(H12), C15(H15), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24),
  C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C27A(H27A),
 C28A(H28A), C29A(H29A), C30A(H30A), C32A(H32A), C33A(H33A)
5.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C1(H1A,H1B,H1C), C36(H36A,H36B,H36C)
5.d Idealised tetrahedral OH refined as rotating group:
 O2(H2), O2A(H2AA)
;
_shelx_res_checksum              136
_olex2_submission_special_instructions 'No special instructions were received'