Field-induced slow magnetic relaxation behaviours in binuclear cobalt(II) metallocycles and exchange-coupled clusters.
Shao, Dong; Moorthy, Shruti; Zhou, Yue; Wu, Si-Tong; Zhu, Jing-Yan; Yang, Jiong; Wu, Dong-Qing; Tian, Zhengfang; Singh, Saurabh Kumar; Dalton transactions (Cambridge, England : 2003) 51 (2022) 9357–9368; doi:10.1039/d2dt01620f

data_7710459
_publ_section_title
;
 Field-induced slow magnetic relaxation behaviours in binuclear cobalt(II)
 metallocycles and exchange-coupled clusters.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9357
_journal_page_last               9368
_journal_paper_doi               10.1039/d2dt01620f
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C44 H48 Co2 N12 O8 S4, 3(C3 H7 N1 O1)'
_chemical_formula_sum            'C53 H69 Co2 N15 O11 S4'
_chemical_formula_weight         1338.33
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-12-06
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2021-12-06 deposited with the CCDC.	2022-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 125.5390(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.7630(16)
_cell_length_b                   9.1196(5)
_cell_length_c                   26.128(2)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      2.71
_cell_volume                     6352.4(7)
_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 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            29206
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.898
_diffrn_reflns_theta_min         2.374
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5079
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1428 before and 0.0755 after correction.
The Ratio of minimum to maximum transmission is 0.6812.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       block
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         7525
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+7.8109P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1024
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6654
_reflns_number_total             7525
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01620f2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7710458--7710459.cif.'
_cod_original_cell_volume        6352.6(7)
_cod_database_code               7710459
_shelx_shelxl_version_number     2014/7
_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
 C25-O5
 1.22 with sigma of 0.02
 C25-N7
 1.36 with sigma of 0.02
 N7-C13
 1.45 with sigma of 0.02
 N7-C27
 1.46 with sigma of 0.02
 C25-C13
 2.46 with sigma of 0.04
 C25-C27
 2.45 with sigma of 0.04
 N7-C13 \\sim N7-C27
 with sigma of 0.02
 N3-C3 \\sim N2-C15
 with sigma of 0.02
 C11-C23 \\sim C7-C29
 with sigma of 0.04
 O2-C11 \\sim O3-C7
 with sigma of 0.02
 C23-C3 \\sim C29-C15
 with sigma of 0.04
 C11-C3 \\sim C7-C15
 with sigma of 0.04
 O2-N3 \\sim O3-N2
 with sigma of 0.04
 N3-C11 \\sim N2-C7
 with sigma of 0.02
 N3-C23 \\sim N2-C29
 with sigma of 0.02
3. Restrained planarity
 O5, N7, C13, C25, C27
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O5 \\sim N7 \\sim C13 \\sim C25 \\sim C27: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uanis(C23) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.01
Uanis(O2) = Uanis(O3) = Uanis(C7) = Uanis(N2) = Uanis(C3) = Uanis(C11) =
Uanis(N3) = Uanis(C23) = Uanis(C29) = Uanis(C15)
5. Rigid body (RIGU) restrains
 O5, N7, C13, C25, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O3)=Sof(N2)=Sof(C7)=Sof(H7)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=1-FVAR(1)
 Sof(O2)=Sof(N3)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C11)=Sof(H11)=Sof(C23)=
 Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(1)
 Fixed Sof: O5(0.5) C13(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C25(0.5) H25(0.5)
 C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C24(H24A,H24B)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C8(H8), C10(H10), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21), C22(H22), C28(H28), C30(H30), C11(H11), C7(H7),
 C25(H25)
7.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C3(H3A,H3B,H3C), C23(H23A,H23B,
 H23C), C15(H15A,H15B,H15C), C29(H29A,H29B,H29C), C13(H13A,H13B,H13C), C27(H27A,
 H27B,H27C)
;
_shelx_res_checksum              1914
_olex2_submission_special_instructions 'No special instructions were received'