Macrocyclic transition-metal parashift complexes for MRI at clinical and pre-clinical magnetic fields.
Rogers, Nicola J.; Ashok Kumar, Chowan; Alexander, Carlson; Bowdery, Daniel; Pavlovskaya, Galina; Harvey, Peter; Dalton transactions (Cambridge, England : 2003) 54 (2025) 11036–11046; doi:10.1039/d5dt01149c

data_7718954
_publ_section_title
;
 Macrocyclic transition-metal parashift complexes for MRI at clinical and
 pre-clinical magnetic fields.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11036
_journal_page_last               11046
_journal_paper_doi               10.1039/d5dt01149c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C36.55 H54 Fe N6, Cl6 Fe2 O, C4 H8 O2'
_chemical_formula_sum            'C40.55 H62 Cl6 Fe3 N6 O3'
_chemical_formula_weight         1061.81
_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             2025-04-24
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-04-24 deposited with the CCDC.	2025-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                82.332(4)
_cell_angle_beta                 76.998(3)
_cell_angle_gamma                83.372(3)
_cell_formula_units_Z            2
_cell_length_a                   12.4242(10)
_cell_length_b                   12.5408(11)
_cell_length_c                   16.2487(15)
_cell_measurement_reflns_used    9179
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      27.183
_cell_measurement_theta_min      2.204
_cell_volume                     2435.2(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8V'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0797
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            134627
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.533
_diffrn_reflns_theta_min         2.251
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.253
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1293 before and 0.0787 after correction.
The Ratio of minimum to maximum transmission is 0.8852.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dull dark red'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       needle
_exptl_crystal_F_000             1103
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.129
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         11143
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0525P)^2^+3.0111P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1159
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8880
_reflns_number_total             11143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01149c2.cif
_cod_data_source_block           FeL1b
_cod_depositor_comments
'Adding full bibliography for 7718951--7718957.cif.'
_cod_database_code               7718954
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.634
_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
2. Restrained distances
 C01C-H01L \\sim C01D-H01P \\sim C01D-H01N
 with sigma of 0.02
 C01D-H01P \\sim C01C-H01L \\sim C01I-H01T
 with sigma of 0.02
3. Others
 Fixed Sof: C2(0.55)
4.a Secondary CH2 refined with riding coordinates:
 C00L(H00A,H00B), C00N(H00C,H00D), C00P(H00E,H00F), C00R(H00G,H00H), C00V(H00I,
 H00K), C00W(H00L,H00N), C00Z(H00O,H00P), C011(H01A,H01B), C016(H01C,H01D),
 C01E(H1,H), C01F(H2,HA), C01H(H3,HB), C01K(H4,HC)
4.b Aromatic/amide H refined with riding coordinates:
 C00J(H00J), C00M(H00M), C00Q(H00Q), C00X(H00X), C00Y(H00Y), C013(H013),
 C014(H014), C015(H015), C018(H018)
4.c Idealised Me refined as rotating group:
 C01A(H01E,H01F,H01G), C01B(H01H,H01I,H01J), C01G(H01Q,H01R,H01S), C01J(H01W,
 H01X,H01Y), C01L(H01Z,HD,HE), C01M(H01,HF,HG)
;
_shelx_res_checksum              73776
_shelx_hkl_checksum              17191
_olex2_submission_special_instructions 'No special instructions were received'