Field-induced slow magnetic relaxation from linear trinuclear Co<sup>III</sup>-Co<sup>II</sup>-Co<sup>III</sup> to grid [2 × 2] tetranuclear mixed-valence cobalt complexes.
Yang, Meng; Ouyang, Zhi-Jian; Zhong, Yun-Jing; Cai, Jia-Wei; Li, Xiao-Hui; Dong, Wen; Dalton transactions (Cambridge, England : 2003) 49 (2020) 17017–17025; doi:10.1039/d0dt02863k

data_7705879
_publ_section_title
;
 Field-induced slow magnetic relaxation from linear trinuclear
 Co<sup>III</sup>-Co<sup>II</sup>-Co<sup>III</sup> to grid [2 \\times 2]
 tetranuclear mixed-valence cobalt complexes.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17017
_journal_page_last               17025
_journal_paper_doi               10.1039/d0dt02863k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'2(C22 H12 Co N12 O4), C4 H16 O4, C66 H46 Co4 N34 O10, 8(C2 H6 O S)'
_chemical_formula_sum            'C130 H134 Co6 N58 O30 S8'
_chemical_formula_weight         3599.01
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-18 deposited with the CCDC.	2020-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                93.051(2)
_cell_angle_beta                 104.841(2)
_cell_angle_gamma                103.502(2)
_cell_formula_units_Z            1
_cell_length_a                   14.8320(3)
_cell_length_b                   16.1866(3)
_cell_length_c                   16.9537(4)
_cell_measurement_reflns_used    22355
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.3910
_cell_measurement_theta_min      2.7270
_cell_volume                     3797.95(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -14.00  36.00   0.50    0.51    --   45.75 -69.00   5.00  100
  2  \w     67.00  94.00   0.50    0.51    --   45.75-125.00 -90.00   54
  3  \w     34.00  76.00   0.50    4.68    --  106.06 -69.00   5.00   84
  4  \w     65.00  91.00   0.50    4.68    --  106.06 -94.00 -30.00   52
  5  \w     52.00  78.00   0.50    4.68    --  106.06-125.00 -30.00   52
  6  \w     34.00 108.00   0.50    4.68    --  106.06 -77.00  30.00  148
  7  \w     69.00 105.00   0.50    4.68    --  106.06 -94.00 120.00   72
  8  \w     36.00  70.00   0.50    4.68    --  106.06 -61.00 150.00   68
  9  \w     37.00  63.00   0.50    4.68    --  106.06 -94.00 120.00   52
 10  \w     33.00  62.00   0.50    4.68    --  106.06 -61.00  60.00   58
 11  \w     91.00 178.00   0.50    4.68    --  106.06  15.00  90.00  174
 12  \w    112.00 178.00   0.50    4.68    --  106.06  15.00 -60.00  132
 13  \w    101.00 171.00   0.50    4.68    --  106.06  30.00-120.00  140
 14  \w     77.00 108.00   0.50    4.68    --  106.06-108.00-152.47   62
 15  \w     66.00 124.00   0.50    4.68    --  106.06-142.00-158.05  116
 16  \w     46.00 103.00   0.50    4.68    --  106.06 -94.00-180.00  114
 17  \w     33.00  59.00   0.50    4.68    --  106.06-142.00-158.05   52
 18  \w     44.00 105.00   0.50    4.68    --  106.06 -94.00-120.00  122
 19  \w     35.00  72.00   0.50    4.68    --  106.06 -61.00-120.00   74
 20  \w     33.00 103.00   0.50    4.68    --  106.06 -94.00-150.00  140
 21  \w    -26.00  25.00   0.50    0.51    --   45.75 -19.00-150.00  102
 22  \w    -24.00  28.00   0.50    0.51    --  -45.75  19.00  90.00  104
 23  \w    -49.00 -14.00   0.50    0.51    --  -45.75 125.00 150.00   70
 24  \w    -65.00  22.00   0.50    0.51    --  -45.75  69.00 137.00  174
 25  \w     43.00 105.00   0.50    0.51    --   45.75  69.00 137.00  124
 26  \w     86.00 172.00   0.50    4.68    --  106.06  69.00 137.00  172
 27  \w     79.00 151.00   0.50    4.68    --  106.06 125.00 150.00  144
 28  \w    -63.00 -29.00   0.50    4.68    -- -102.00 125.00 150.00   68
 29  \w    -80.00 -55.00   0.50    4.68    -- -102.00  69.00 137.00   50
 30  \w    -90.00 -52.00   0.50    0.51    --  -45.75 125.00 150.00   76
 31  \w   -112.00 -54.00   0.50    4.68    -- -102.00 125.00  30.00  116
 32  \w    -67.00 -41.00   0.50    4.68    -- -102.00  61.00 -60.00   52
 33  \w    -69.00 -44.00   0.50    4.68    -- -102.00  61.00 -30.00   50
 34  \w    -66.00 -40.00   0.50    4.68    -- -102.00  61.00   0.00   52
 35  \w   -120.00 -43.00   0.50    4.68    -- -102.00 137.00 -89.92  154
 36  \w   -126.00 -69.00   0.50    4.68    -- -102.00 145.00 -74.29  114
 37  \w   -122.00 -46.00   0.50    4.68    -- -102.00 139.00  54.55  152
 38  \w   -173.00-148.00   0.50    4.68    -- -102.00 -45.00-120.00   50
 39  \w   -135.00-103.00   0.50    4.68    -- -102.00 -45.00-120.00   64
 40  \w   -115.00 -82.00   0.50    0.51    --  -45.75-125.00-180.00   66
 41  \w   -104.00 -25.00   0.50    0.51    --  -45.75 -69.00   5.00  158
 42  \w   -131.00 -88.00   0.50    4.68    -- -102.00 -69.00   5.00   86
 43  \w   -175.00-150.00   0.50    4.68    -- -102.00 -69.00   5.00   50
 44  \w   -167.00-114.00   0.50    4.68    -- -102.00 -45.00  60.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0908221000
_diffrn_orient_matrix_UB_12      -0.0755726000
_diffrn_orient_matrix_UB_13      -0.0242816000
_diffrn_orient_matrix_UB_21      0.0351452000
_diffrn_orient_matrix_UB_22      -0.0345893000
_diffrn_orient_matrix_UB_23      -0.0699379000
_diffrn_orient_matrix_UB_31      0.0535892000
_diffrn_orient_matrix_UB_32      -0.0530418000
_diffrn_orient_matrix_UB_33      0.0590387000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            52437
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.925
_diffrn_reflns_theta_min         2.716
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.822
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.59a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       block
_exptl_crystal_F_000             1850
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   0.279
_exptl_transmission_factor_min   0.256
_refine_diff_density_max         2.617
_refine_diff_density_min         -1.210
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1090
_refine_ls_number_reflns         15400
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0856
_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^)+(0.1000P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2157
_refine_ls_wR_factor_ref         0.2226
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13244
_reflns_number_total             16053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02863k2.cif
_cod_data_source_block           Co4
_cod_database_code               7705879
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N S Co'
_shelx_estimated_absorpt_t_max   0.342
_shelx_estimated_absorpt_t_min   0.315
_diffrn_oxdiff_digest_frames
;
012244c24945fccc540cb648aca3427e6100040e584
;
_diffrn_oxdiff_digest_hkl
;
0188b8bc4b2c7b90fb0748d9faa039c15f3c2c
;
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H16A of O16
 At 1.5 times of:
  All C(H,H,H) groups, H12 of O12, H4 of O4, H1 of O1, H6 of O6, H8 of O8,
  All O(H,H) groups
2. Restrained distances
 S4-O10
 1.48 with sigma of 0.01
 S4-C63A = S4-C64A
 1.78 with sigma of 0.01
 S4-C63A = S4-C63B
 1.78 with sigma of 0.01
 S4-C64A = S4-C64B
 1.78 with sigma of 0.01
 S3-C61
 1.78 with sigma of 0.01
 S3-C59
 1.78 with sigma of 0.01
 O16-C12
 1.5 with sigma of 0.001
 O12-C65
 1.38 with sigma of 0.01
 C12-O16
 1.38 with sigma of 0.01
 S4-O10 \\sim S4-O11
 with sigma of 0.02
 S4-C63B \\sim S4-C63A
 with sigma of 0.02
 S4-C64B \\sim S4-C64A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O12) \\sim Ueq, Uanis(O16) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
Uanis(C64A) \\sim Ueq, Uanis(C64B) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
Uanis(C65) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C12) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
4. Others
 Fixed Sof: O10(0.5) C63A(0.5) H63A(0.5) H63B(0.5) H63C(0.5) C64A(0.5)
 H64A(0.5) H64B(0.5) H64C(0.5) O11(0.5) C63B(0.5) H63D(0.5) H63E(0.5) H63F(0.5)
 C64B(0.5) H64D(0.5) H64E(0.5) H64F(0.5)
5.a Riding coordinates:
 O16(H16A)
5.b Rotating group:
 O14(H14A,H14B)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4A), C5(H5), C7(H7), C8(H8A), C10(H10), C15(H15), C16(H16), C18(H18),
 C19(H19), C22(H22), C28(H28), C29(H29), C31(H31), C32(H32), C34(H34), C41(H41),
  C42(H42), C44(H44), C45(H45), C47(H47), C49(H49), C50(H50), C51(H51),
 C53(H53), C54(H54), C55(H55), C57(H57), C58(H58), C60(H60)
5.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C26(H26A,H26B,
 H26C), C37(H37A,H37B,H37C), C59(H59A,H59B,H59C), C61(H61A,H61B,H61C),
 C63A(H63A,H63B,H63C), C64A(H64A,H64B,H64C), C63B(H63D,H63E,H63F), C64B(H64D,
 H64E,H64F), C65(H65A,H65B,H65C)
5.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O4(H4), O6(H6), O8(H8), O12(H12)
;
_shelx_res_checksum              7481
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.696
_oxdiff_exptl_absorpt_empirical_full_min 0.719