Switching of the redox centers of a tris-2-mercaptophenolato chromium(III) metalloligand by a guest metal ion.
Wakizaka, Masanori; Matsumoto, Takeshi; Chang, Ho-Chol; Dalton transactions (Cambridge, England : 2003) 52 (2023) 1538–1542; doi:10.1039/d2dt03502b

data_7712156
_publ_section_title
;
 Switching of the redox centers of a tris-2-mercaptophenolato
 chromium(III) metalloligand by a guest metal ion.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1538
_journal_page_last               1542
_journal_paper_doi               10.1039/d2dt03502b
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety
'C18 H12 Co0.5 Cr O3 S3, C18 H12 Co1.9 Cr K0.2 O12.5 S3, 10(O)'
_chemical_formula_sum            'C36 H24 Co2.4 Cr2 K0.2 O25.5 S6'
_chemical_formula_weight         1310.16
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-25
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2021-12-25 deposited with the CCDC.	2023-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                70.242(2)
_cell_angle_beta                 73.531(2)
_cell_angle_gamma                88.9980(10)
_cell_formula_units_Z            2
_cell_length_a                   12.6211(2)
_cell_length_b                   14.7753(3)
_cell_length_c                   16.6912(3)
_cell_measurement_reflns_used    41813
_cell_measurement_temperature    120
_cell_measurement_theta_max      31.9180
_cell_measurement_theta_min      3.1640
_cell_volume                     2798.56(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.893
_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     38.00  64.00   0.50    6.00    --   -0.30  45.00  30.00   52
  2  \w    -88.00  49.00   0.50    6.00    --   -0.30  45.00 120.00  274
  3  \w    -89.00  72.00   0.50    6.00    --   -0.30  45.00 -19.77  322
  4  \w    -88.00  80.00   0.50    6.00    --   -0.30  45.00 150.00  336
  5  \w    -84.00 -59.00   0.50    6.00    --   -0.30  45.00  60.00   50
  6  \w    -51.00  23.00   0.50    6.00    --   -0.30  45.00  60.00  148
  7  \w     35.00  60.00   0.50    6.00    --   -0.30  45.00   0.00   50
  8  \w    -28.00  -3.00   0.50    6.00    --   -0.30  45.00  90.00   50
  9  \w    -80.00 -55.00   0.50    6.00    --   -0.30  45.00  30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0201188000
_diffrn_orient_matrix_UB_12      0.0149040000
_diffrn_orient_matrix_UB_13      -0.0471172000
_diffrn_orient_matrix_UB_21      -0.0346202000
_diffrn_orient_matrix_UB_22      -0.0377495000
_diffrn_orient_matrix_UB_23      0.0007269000
_diffrn_orient_matrix_UB_31      -0.0430950000
_diffrn_orient_matrix_UB_32      0.0312169000
_diffrn_orient_matrix_UB_33      -0.0035517000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            89620
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.909
_diffrn_reflns_theta_min         2.941
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.390
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull dark violet'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       plate
_exptl_crystal_F_000             1313
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.235
_refine_diff_density_min         -1.588
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         17209
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0620
_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^)+(0.0948P)^2^+9.4223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1753
_refine_ls_wR_factor_ref         0.1817
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15104
_reflns_number_total             17209
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03502b2.cif
_cod_data_source_block           c_120k
_cod_depositor_comments          'Adding full bibliography for 7712156.cif.'
_cod_original_formula_sum        'C36 H24 Co2.40 Cr2 K0.20 O25.50 S6'
_cod_database_code               7712156
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cr Co K C8 H8 O8 S8'
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.769
_diffrn_oxdiff_digest_frames
;
013da251702c711e91df7dbd863b74866e00026f47c
;
_diffrn_oxdiff_digest_hkl
;
01d36a2f4f9f8f14e514321cd9360c53764e5b
;
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: Co3(0.95) Co5(0.2) Co4(0.2) O19(0.8) O26(0.8) O25(0.8) O18(0.8)
 O15(0.8) O22(0.5) O27(0.8) Co6(0.05) K1(0.2) O14(0.2)
3.a Aromatic/amide H refined with riding coordinates:
 C30(H30), C15(H15), C21(H21), C23(H23), C18(H18), C12(H12), C24(H24),
 C22(H22), C35(H35), C36(H36), C33(H33), C16(H16), C29(H29), C17(H17), C9(H9),
 C6(H6), C10(H10), C5(H5), C11(H11), C27(H27), C28(H28), C34(H34), C3(H3),
 C4(H4)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              95575
_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 1.358
_oxdiff_exptl_absorpt_empirical_full_min 0.781