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_7705880
_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         'C44 H32 Co3 N24 O12, 4(C4 H9 N O), 3(H2 O)'
_chemical_formula_sum            'C60 H74 Co3 N28 O19'
_chemical_formula_weight         1668.26
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2020-10-16
_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                90
_cell_angle_beta                 95.6180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.46890(10)
_cell_length_b                   14.21320(10)
_cell_length_c                   19.8528(2)
_cell_measurement_reflns_used    15741
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.6860
_cell_measurement_theta_min      3.8200
_cell_volume                     3501.47(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.961
_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    -51.00  26.00   0.50    0.05    --  -46.37  78.00 -45.00  154
  2  \w     46.00  71.00   0.50    0.05    --   46.37  78.00 -45.00   50
  3  \w    137.00 163.00   0.50    0.20    --  107.00  45.00-120.00   52
  4  \w    143.00 169.00   0.50    0.20    --  107.00  78.00 -45.00   52
  5  \w     96.00 145.00   0.50    0.20    --  107.00  61.00   0.00   98
  6  \w     80.00 115.00   0.50    0.05    --   46.37  57.00 120.00   70
  7  \w     41.00  75.00   0.50    0.05    --   46.37  57.00 120.00   68
  8  \w     33.00  71.00   0.50    0.20    --  107.00 -30.00 150.00   76
  9  \w     33.00  69.00   0.50    0.20    --  107.00 -30.00  60.00   72
 10  \w     32.00  71.00   0.50    0.20    --  107.00 -30.00  30.00   78
 11  \w     43.00  71.00   0.50    0.20    --  107.00 -30.00 -30.00   56
 12  \w     46.00  72.00   0.50    0.20    --  107.00 -45.00 -60.00   52
 13  \w     38.00  64.00   0.50    0.20    --  107.00 -30.00-120.00   52
 14  \w     33.00  71.00   0.50    0.20    --  107.00 -30.00-180.00   76
 15  \w     42.00 130.00   0.50    0.20    --  107.00 -78.00-171.00  176
 16  \w     45.00  70.00   0.50    0.20    --  107.00 -45.00   0.00   50
 17  \w     37.00  68.00   0.50    0.20    --  107.00 -30.00   0.00   62
 18  \w     94.00 133.00   0.50    0.20    --  107.00  45.00-120.00   78
 19  \w     39.00  64.00   0.50    0.20    --  107.00 -45.00-150.00   50
 20  \w    -24.00  71.00   0.50    0.05    --   46.37 -78.00-171.00  190
 21  \w    -76.00 -51.00   0.50    0.20    -- -102.00  78.00 -45.00   50
 22  \w    -74.00 -29.00   0.50    0.20    -- -102.00  45.00 -30.00   90
 23  \w    -59.00 -34.00   0.50    0.20    -- -102.00  30.00 -60.00   50
 24  \w    -63.00 -37.00   0.50    0.20    -- -102.00  30.00 -30.00   52
 25  \w    -94.00 -69.00   0.50    0.05    --  -46.37 -78.00-171.00   50
 26  \w   -118.00 -71.00   0.50    0.05    --  -46.37-125.00 -30.00   94
 27  \w   -175.00 -78.00   0.50    0.20    -- -102.00 -78.00-171.00  194
 28  \w    -57.00 -32.00   0.50    0.20    -- -102.00  45.00-180.00   50
;
_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      -0.0714611000
_diffrn_orient_matrix_UB_12      -0.0293153000
_diffrn_orient_matrix_UB_13      0.0554754000
_diffrn_orient_matrix_UB_21      -0.0396597000
_diffrn_orient_matrix_UB_22      -0.0861327000
_diffrn_orient_matrix_UB_23      -0.0425418000
_diffrn_orient_matrix_UB_31      0.0933865000
_diffrn_orient_matrix_UB_32      -0.0589739000
_diffrn_orient_matrix_UB_33      0.0345494000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25354
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.996
_diffrn_reflns_theta_min         3.831
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.298
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.582
_exptl_crystal_description       block
_exptl_crystal_F_000             1726
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.00105(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         7119
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0724P)^2^+2.9251P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1230
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6594
_reflns_number_total             7119
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02863k2.cif
_cod_data_source_block           Co1
_cod_database_code               7705880
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Fe C H O N'
_shelx_estimated_absorpt_t_max   0.572
_shelx_estimated_absorpt_t_min   0.366
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H2A,H2B} of O2, {H1A,H1B} of O1, {H9A,H9B} of O9, All
  O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H10A,H10B} of O10
2. Restrained distances
 O7-C27 \\sim O7A-C27A
 with sigma of 0.02
 N13-C27 \\sim N13A-C27A
 with sigma of 0.02
 N13-C29 \\sim N13A-C29A
 with sigma of 0.02
 N13-C30 \\sim N13A-C30A
 with sigma of 0.02
 C27-C28 \\sim C27A-C28A
 with sigma of 0.02
 O7-N13 \\sim O7A-N13A
 with sigma of 0.04
 O7-C28 \\sim O7A-C28A
 with sigma of 0.04
 N13-C28 \\sim N13A-C28A
 with sigma of 0.04
 C27-C29 \\sim C27A-C29A
 with sigma of 0.04
 C27-C30 \\sim C27A-C30A
 with sigma of 0.04
 C29-C30 \\sim C29A-C30A
 with sigma of 0.04
 C23-C25 \\sim C23A-C25A
 with sigma of 0.04
 C25-C26 \\sim C25A-C26A
 with sigma of 0.04
 O8-C24 \\sim O8A-C24A
 with sigma of 0.04
 C23-C26 \\sim C23A-C26A
 with sigma of 0.04
 O8-C23 \\sim O8A-C23A
 with sigma of 0.02
 C23-C24 \\sim C23A-C24A
 with sigma of 0.02
 O8-N14 \\sim O8A-N14A
 with sigma of 0.04
 N14-C24 \\sim N14A-C24A
 with sigma of 0.04
 N14-C23 \\sim N14A-C23A
 with sigma of 0.02
 N14-C25 \\sim N14A-C25A
 with sigma of 0.02
 N14-C26 \\sim N14A-C26A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N14A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O7) = Uanis(O7A)
4. Others
 Sof(O7A)=Sof(N13A)=Sof(C27A)=Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=
 Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C30A)=Sof(H30D)=Sof(H30E)=
 Sof(H30F)=1-FVAR(1)
 Sof(O7)=Sof(N13)=Sof(C27)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=
 Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
 Fixed Sof: O8(0.6) N14(0.6) C23(0.6) C24(0.6) H24A(0.6) H24B(0.6) H24C(0.6)
 C25(0.6) H25A(0.6) H25B(0.6) H25C(0.6) C26(0.6) H26A(0.6) H26B(0.6) H26C(0.6)
 O9(0.5) H9A(0.5) H9B(0.5) C23A(0.4) O8A(0.4) N14A(0.4) C24A(0.4) H24D(0.4)
 H24E(0.4) H24F(0.4) C25A(0.4) H25D(0.4) H25E(0.4) H25F(0.4) C26A(0.4)
 H26D(0.4) H26E(0.4) H26F(0.4)
5.a Riding coordinates:
 O5(H5), O6(H6), O2(H2A,H2B), O1(H1A,H1B), O9(H9A,H9B), O10(H10A,H10B)
5.b Me refined with riding coordinates:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C28A(H28D,H28E,H28F),
 C29A(H29D,H29E,H29F), C30A(H30D,H30E,H30F), C24A(H24D,H24E,H24F), C25A(H25D,
 H25E,H25F), C26A(H26D,H26E,H26F)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5A), C7(H7), C8(H8), C10(H10), C15(H15), C16(H16), C18(H18),
 C19(H19), C21(H21)
;
_shelx_res_checksum              13894
_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 1.461
_oxdiff_exptl_absorpt_empirical_full_min 0.786