Trifluoroborate-appended cyclen complexes of paramagnetic transition metals (Ni<sup>2+</sup>, Co<sup>2+</sup>) as fast-relaxing <sup>19</sup>F MRI probes.
Sire, Charline; Garello, Francesca; Lalaoui, Noémie; Saffon-Merceron, Nathalie; Le Poul, Nicolas; Tripier, Raphaël; Tei, Lorenzo; Troadec, Thibault; Dalton transactions (Cambridge, England : 2003) 54 (2025) 13053–13056; doi:10.1039/d5dt01834j

data_7719304
_publ_section_title
;
 Trifluoroborate-appended cyclen complexes of paramagnetic transition
 metals (Ni<sup>2+</sup>, Co<sup>2+</sup>) as fast-relaxing <sup>19</sup>F
 MRI probes.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13053
_journal_page_last               13056
_journal_paper_doi               10.1039/d5dt01834j
_journal_volume                  54
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_sum            'C22 H36 B2 Co F6 N6 O2'
_chemical_formula_weight         611.12
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-06-02 deposited with the CCDC.	2025-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1182(9)
_cell_length_b                   9.0791(5)
_cell_length_c                   16.9809(8)
_cell_measurement_reflns_used    9000
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.54
_cell_volume                     2639.1(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT (Sheldrick 2015)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker D8-Venture Photon III-C14 detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            117993
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.304
_diffrn_reflns_theta_min         2.809
_diffrn_source                   'Fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       plate
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
; 
 Flack x determined using 2715 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.003(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         6193
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0217
_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^)+(0.0366P)^2^+0.4304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0573
_refine_ls_wR_factor_ref         0.0577
_reflns_Friedel_coverage         0.842
_reflns_Friedel_fraction_full    0.908
_reflns_Friedel_fraction_max     0.892
_reflns_number_gt                6069
_reflns_number_total             6193
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01834j2.cif
_cod_data_source_block           Co(Do2pyBF3)
_cod_depositor_comments
'Adding full bibliography for 7719303--7719304.cif.'
_cod_database_code               7719304
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.760
_shelx_estimated_absorpt_t_max   0.931
_exptl_absorpt_special_details
;
SADABS-2016/2 - Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_shelx_res_checksum              30410
_shelx_hkl_checksum              4805