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_7705881
_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
'C66 H46 Co4 N34 O10, 2(C22 H12 Co N12 O4), 8(C3 H7 N O), 6(H2 O)'
_chemical_formula_sum            'C134 H138 Co6 N66 O32'
_chemical_formula_weight         3538.68
_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     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                91.460(2)
_cell_angle_beta                 105.601(2)
_cell_angle_gamma                101.919(2)
_cell_formula_units_Z            1
_cell_length_a                   15.3105(3)
_cell_length_b                   15.6182(3)
_cell_length_c                   16.7603(4)
_cell_measurement_reflns_used    17910
_cell_measurement_temperature    100.0(4)
_cell_measurement_theta_max      30.8020
_cell_measurement_theta_min      2.5150
_cell_volume                     3762.90(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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      100.0(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_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    -44.00  18.00   0.50    6.46    --    4.91 -50.00   5.00  124
  2  \w    -21.00   4.00   0.50    6.46    --   -6.94 -99.00  90.00   50
  3  \w    -20.00  13.00   0.50    6.46    --   -6.94 -99.00 -30.00   66
  4  \w    -20.00  34.00   0.50    6.46    --    4.91 -99.00-120.00  108
  5  \w    -21.00   5.00   0.50    6.46    --   -6.94 -99.00-150.00   52
  6  \w    -70.00  20.00   0.50    6.46    --    4.91 -19.00-120.00  180
  7  \w    -11.00  72.00   0.50    6.46    --    4.91  57.00  30.00  166
  8  \w      9.00  78.00   0.50    6.46    --    4.91  50.00 152.00  138
;
_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      -0.0221650000
_diffrn_orient_matrix_UB_12      -0.0432813000
_diffrn_orient_matrix_UB_13      0.0050845000
_diffrn_orient_matrix_UB_21      -0.0225179000
_diffrn_orient_matrix_UB_22      0.0171565000
_diffrn_orient_matrix_UB_23      0.0265408000
_diffrn_orient_matrix_UB_31      -0.0378781000
_diffrn_orient_matrix_UB_32      0.0016824000
_diffrn_orient_matrix_UB_33      -0.0348532000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0681
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            54866
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.223
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_description       block
_exptl_crystal_F_000             1822
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1108
_refine_ls_number_reflns         17106
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0513P)^2^+0.6037P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1117
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12455
_reflns_number_total             17106
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02863k2.cif
_cod_data_source_block           Co3
_cod_original_cell_volume        3762.90(14)
_cod_database_code               7705881
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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, All O(H,H) groups
2. Restrained distances
 H15B-O15
 0.8 with sigma of 0.01
 H12A-H15B
 2 with sigma of 0.01
3. Rigid bond restraints
 O1, O4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N17, N16
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N14, C30
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N14, C31
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N16, C26
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(O17)=Sof(H17A)=Sof(H17B)=1-FVAR(1)
 Sof(O15)=Sof(H15A)=Sof(H15B)=FVAR(1)
5.a Riding coordinates:
 O17(H17A,H17B)
5.b Free rotating group:
 O13(H13A,H13B), O12(H12A,H12B), O15(H15A)
5.c Rotating group:
 O5(H5A,H5B)
5.d Aromatic/amide H refined with riding coordinates:
 C49(H49), C15(H15), C48(H48), C54(H54), C21(H21), C16(H16), C10(H10), C4(H4A),
  C43(H43), C31(H31), C52(H52), C38(H38), C37(H37), C7(H7), C33(H33), C5(H5),
 C29(H29), C51(H51), C23(H23), C40(H40), C25(H25), C41(H41), C32(H32), C19(H19),
  C18(H18), C27(H27), C65(H65), C8(H8), C24(H24), C28(H28), C56(H56), C62(H62),
 C59(H59)
5.e Idealised Me refined as rotating group:
 C66(H66A,H66B,H66C), C57(H57A,H57B,H57C), C63(H63A,H63B,H63C), C64(H64A,H64B,
 H64C), C58(H58A,H58B,H58C), C67(H67A,H67B,H67C), C60(H60A,H60B,H60C), C61(H61A,
 H61B,H61C)
5.f Idealised tetrahedral OH refined as rotating group:
 O9(H9), O4(H4), O2(H2), O7(H7A)
;
_shelx_res_checksum              54290
_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 1.572
_oxdiff_exptl_absorpt_empirical_full_min 0.564