A responsive Co(II) <sup>19</sup>F PARAShift probe: activation of Fermi contact interactions triggered by pH-dependent coordination changes.
Scott, Kathleen M.; Kadakia, Rahul T.; Hastings, Christopher D.; Barone, Georgia E. F.; Reyna, Jackson A.; Xiong, Jin; Guo, Yisong; Que, Emily L.; Chemical communications (Cambridge, England) 62 (2026) 6741–6745; doi:10.1039/d6cc00957c

data_7135584
_publ_section_title
;
 A responsive Co(II) <sup>19</sup>F PARAShift probe: activation of Fermi
 contact interactions triggered by pH-dependent coordination changes.
;
_journal_issue                   25
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              6741
_journal_page_last               6745
_journal_paper_doi               10.1039/d6cc00957c
_journal_volume                  62
_journal_year                    2026
_chemical_formula_moiety
'C19 H26 Co F5 N4 Na O6 S, 1.736(C H4 O), C0.264 H1.042 O0.264'
_chemical_formula_sum            'C21 H34 Co F5 N4 Na O8 S'
_chemical_formula_weight         679.50
_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             2020-03-03
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2026-02-12 deposited with the CCDC.	2026-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                64.957(4)
_cell_angle_beta                 69.304(4)
_cell_angle_gamma                75.254(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1113(4)
_cell_length_b                   11.8024(5)
_cell_length_c                   13.7663(5)
_cell_measurement_reflns_used    16032
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      73.1860
_cell_measurement_theta_min      4.1460
_cell_volume                     1381.63(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2940
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.982
_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   -116.00 -17.00   1.00    5.00    --  -41.59 -38.00  30.00   99
  2  \w     81.00 178.00   1.00   18.00    --  107.09  45.00-180.00   97
  3  \w    -66.00  33.00   1.00    5.00    --  -41.59  38.00-150.00   99
  4  \w     31.00 135.00   1.00   18.00    --  107.09 -30.00 120.00  104
  5  \w   -115.00 -13.00   1.00    5.00    --  -41.59 -57.00 -60.00  102
  6  \w     24.00 110.00   1.00   18.00    --  107.09 -94.00 150.00   86
  7  \w      1.00  82.00   1.00    5.00    --   41.59 -99.00 -60.00   81
  8  \w     23.00  98.00   1.00    5.00    --   41.59-125.00-180.00   75
  9  \w     23.00  98.00   1.00    5.00    --   41.59-125.00   0.00   75
 10  \w     35.00 136.00   1.00   18.00    --  107.09 -61.00-180.00  101
 11  \w     35.00 136.00   1.00   18.00    --  107.09 -61.00  30.00  101
 12  \w     31.00 135.00   1.00   18.00    --  107.09 -30.00 -60.00  104
 13  \w     34.00 118.00   1.00   18.00    --  107.09-125.00  90.00   84
 14  \w     34.00 118.00   1.00   18.00    --  107.09-125.00 -30.00   84
 15  \w     79.00 178.00   1.00   18.00    --  107.09  30.00 120.00   99
 16  \w     31.00 135.00   1.00   18.00    --  107.09 -30.00-150.00  104
 17  \w     24.00 110.00   1.00   18.00    --  107.09 -94.00   0.00   86
 18  \w   -118.00  -9.00   1.00    5.00    --  -41.59 -77.00 150.00  109
 19  \w   -118.00  -9.00   1.00    5.00    --  -41.59 -77.00  60.00  109
 20  \w   -115.00 -13.00   1.00    5.00    --  -41.59 -57.00-180.00  102
 21  \w   -118.00  -9.00   1.00    5.00    --  -41.59 -77.00-120.00  109
 22  \w      1.00  82.00   1.00    5.00    --   41.59 -99.00  90.00   81
 23  \w     79.00 178.00   1.00   18.00    --  107.09  30.00  30.00   99
 24  \w     75.00 178.00   1.00   18.00    --  107.09  77.00-180.00  103
 25  \w     79.00 178.00   1.00   18.00    --  107.09  30.00 -60.00   99
 26  \w     75.00 178.00   1.00   18.00    --  107.09  77.00 120.00  103
 27  \w     81.00 178.00   1.00   18.00    --  107.09  45.00  60.00   97
 28  \w     78.00 178.00   1.00   18.00    --  107.09  61.00 -30.00  100
 29  \w     78.00 178.00   1.00   18.00    --  107.09  61.00 -60.00  100
 30  \w     75.00 178.00   1.00   18.00    --  107.09  77.00   0.00  103
 31  \w     78.00 178.00   1.00   18.00    --  107.09  61.00-120.00  100
 32  \w     81.00 178.00   1.00   18.00    --  107.09  45.00-120.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1497073000
_diffrn_orient_matrix_UB_12      -0.0701385000
_diffrn_orient_matrix_UB_13      -0.0324416000
_diffrn_orient_matrix_UB_21      0.0672637000
_diffrn_orient_matrix_UB_22      0.1105354000
_diffrn_orient_matrix_UB_23      -0.0124819000
_diffrn_orient_matrix_UB_31      -0.0018207000
_diffrn_orient_matrix_UB_32      -0.0627953000
_diffrn_orient_matrix_UB_33      0.1238981000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24532
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.369
_diffrn_reflns_theta_min         3.692
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.519
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59085
_exptl_absorpt_correction_type   'gaussian and multi-scan'
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_description       prism
_exptl_crystal_F_000             702
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         5464
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0897P)^2^+0.6473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1314
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5125
_reflns_number_total             5464
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6cc00957c2.cif
_cod_data_source_block           co-sf5-deprovl
_cod_depositor_comments
'Adding full bibliography for 7135583--7135584.cif.'
_cod_database_code               7135584
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 H28 N4 O4 F5 S Co Na'
_shelx_estimated_absorpt_t_max   0.484
_shelx_estimated_absorpt_t_min   0.254
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H) groups
2. Restrained distances
 O6-H6
 0.85 with sigma of 0.01
 C19-H6
 1.891598 with sigma of 0.02
 Na1-H6
 2.998302 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O8 \\sim O8A \\sim C21 \\sim C21A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
4. Others
 Sof(O8A)=Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(1)
 Sof(O8)=Sof(H8)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(1)
 Fixed Sof: H8AA(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B)
5.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C17(H17), C18(H18)
5.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C21A(H21D,H21E,
 H21F)
5.d Idealised tetrahedral OH refined as rotating group:
 O8(H8), O8A(H8AA)
;
_shelx_res_checksum              95284
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.373
_oxdiff_exptl_absorpt_empirical_full_min 0.361