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_7719303
_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 H32 B2 F6 N6 Ni'
_chemical_formula_weight         574.86
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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            8
_cell_length_a                   14.1872(6)
_cell_length_b                   14.1872(6)
_cell_length_c                   23.9442(12)
_cell_measurement_reflns_used    9869
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.13
_cell_measurement_theta_min      2.93
_cell_volume                     4819.4(4)
_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_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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  0.0807
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            209774
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.318
_diffrn_reflns_theta_min         2.872
_diffrn_source                   'Fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_T_max  0.6417
_exptl_absorpt_correction_T_min  0.4755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_description       prism
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.133(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         5988
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+4.7925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.736
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5819
_reflns_number_total             5988
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01834j2.cif
_cod_data_source_block           Ni(Do2pyBF3)
_cod_depositor_comments
'Adding full bibliography for 7719303--7719304.cif.'
_cod_original_cell_volume        4819.4(5)
_cod_database_code               7719303
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.791
_shelx_estimated_absorpt_t_max   0.844
_shelx_res_checksum              11695
_shelx_hkl_checksum              51668