Magnetic resonance thermometry using a Gd<sup>III</sup>-based contrast agent.
Subasinghe, S A Amali S; Romero, Jonathan; Ward, Cassandra L.; Bailey, Matthew D.; Zehner, Donna R.; Mehta, Prakrut J.; Carniato, Fabio; Botta, Mauro; Yustein, Jason T.; Pautler, Robia G.; Allen, Matthew J.; Chemical communications (Cambridge, England) 57 (2021) 1770–1773; doi:10.1039/d0cc06400a

data_7127849
_publ_section_title
;
 Magnetic resonance thermometry using a Gd<sup>III</sup>-based contrast
 agent.
;
_journal_issue                   14
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1770
_journal_page_last               1773
_journal_paper_doi               10.1039/d0cc06400a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C48 H52 F12 Gd N8 O5, 3(Cl), 3(H4 O2)'
_chemical_formula_sum            'C48 H66 Cl3 F12 Gd N8 O11'
_chemical_formula_weight         1422.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-20 deposited with the CCDC.	2021-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.247(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.8408(6)
_cell_length_b                   26.2799(13)
_cell_length_c                   11.5932(5)
_cell_measurement_reflns_used    6473
_cell_measurement_temperature    100
_cell_measurement_theta_max      19.622
_cell_measurement_theta_min      2.269
_cell_volume                     2936.4(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      100.1
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2448
_diffrn_reflns_av_unetI/netI     0.1202
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            73882
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.510
_diffrn_reflns_theta_min         0.775
_exptl_absorpt_coefficient_mu    1.366
_exptl_absorpt_correction_T_max  0.0916
_exptl_absorpt_correction_T_min  0.0589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1020 before and 0.0882 after correction. The Ratio of minimum to maximum transmission is 0.6430. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'light colourless'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       block
_exptl_crystal_F_000             1442
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.490
_refine_diff_density_min         -1.356
_refine_diff_density_rms         0.218
_refine_ls_extinction_coef       0.0068(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     687
_refine_ls_number_reflns         5522
_refine_ls_number_restraints     1729
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.1450
_refine_ls_R_factor_gt           0.1000
_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^)+(0.1612P)^2^+28.4565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2465
_refine_ls_wR_factor_ref         0.2788
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3806
_reflns_number_total             5522
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06400a2.cif
_cod_data_source_block           gdiiicf3_0m_4
_cod_depositor_comments
'Adding full bibliography for 7127849--7127850.cif.'
_cod_database_code               7127849
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.821
_shelx_estimated_absorpt_t_min   0.772
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.910(3)
 0.090(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 O1W-H1WB = O1W-H1WA = O2W-H2WB = O2W-H2WA = O3W-H3WB = O3W-H3WA = O4W-H4WB =
 O4W-H4WA
 0.83 with sigma of 0.02
 H1WB-H1WA = H2WB-H2WA = H4WB-H4WA = H3WB-H3WA
 1.33 with sigma of 0.04
 N1B-C2A \\sim N1B-C2B \\sim N1B-C7B \\sim N1B-C7A \\sim N1B-C3B \\sim N1B-C3A
\\sim N2B-C4A \\sim N2B-C4B
 \\sim N2B-C5B \\sim N2B-C5A
 with sigma of 0.02
 C6B-C5B \\sim C6A-C5A \\sim C3A-C4A \\sim C4B-C3B \\sim C7B-C8B \\sim C7A-C8A
\\sim C2A-C1A \\sim C1B-C2B
 with sigma of 0.02
 N4B-C6B \\sim N3A-C6A \\sim N3B-C8B \\sim N4A-C8A
 with sigma of 0.02
 N4B-C16B \\sim N3A-C16A \\sim N3B-C9B \\sim N4A-C9A
 with sigma of 0.02
 C10A-C9A \\sim C10B-C9B \\sim C16A-C17A \\sim C17B-C16B
 with sigma of 0.02
 C17B-C18B \\sim C22A-C17A \\sim C17B-C22B \\sim C18A-C17A \\sim C22B-C21B
\\sim C18A-C19A \\sim C19B-
 C18B \\sim C19B-C20B \\sim C21B-C20B \\sim C20A-C19A \\sim C20A-C21A \\sim
C21A-C22A \\sim C10A-C15A ~
 C10A-C11A \\sim C12A-C11A \\sim C12A-C13A \\sim C15B-C14B \\sim C13A-C14A
\\sim C15A-C14A \\sim C15B-
 C10B \\sim C12B-C11B \\sim C12B-C13B \\sim C13B-C14B \\sim C10B-C11B
 with sigma of 0.02
 C16A-C18A \\sim C9A-C11A \\sim C16B-C22B \\sim C9B-C15B
 with sigma of 0.02
 C16A-C22A \\sim C9A-C15A \\sim C16B-C18B \\sim C9B-C11B
 with sigma of 0.02
 C11B-C15B \\sim C10B-C14B \\sim C15B-C13B \\sim C12B-C14B \\sim C13B-C11B
\\sim C12B-C10B \\sim C17B-
 C19B \\sim C18B-C20B \\sim C19B-C21B \\sim C20B-C22B \\sim C21B-C17B \\sim
C22B-C18B \\sim C11A-C15A ~
 C10A-C14A \\sim C15A-C13A \\sim C12A-C14A \\sim C13A-C11A \\sim C12A-C10A
\\sim C17A-C19A \\sim C18A-
 C20A \\sim C19A-C21A \\sim C20A-C22A \\sim C21A-C17A \\sim C22A-C18A
 with sigma of 0.02
 C24A-C20A \\sim C23B-C13B \\sim C20B-C24B \\sim C23A-C13A
 with sigma of 0.005
 C23B-F6B \\sim C23B-F4B \\sim C23B-F5B \\sim C23A-F6A \\sim C23A-F5A \\sim
C23A-F4A \\sim C24B-F3B ~
 C24B-F1B \\sim C24B-F2B \\sim C24A-F1A \\sim C24A-F2A \\sim C24A-F3A
 with sigma of 0.005
 F5B-F4B \\sim F4B-F6B \\sim F6B-F5B \\sim F4A-F6A \\sim F6A-F5A \\sim F5A-F4A
\\sim F2B-F3B \\sim F3B-F1B
 \\sim F1B-F2B \\sim F1A-F2A \\sim F2A-F3A \\sim F3A-F1A
 with sigma of 0.005
 C13B-F5B \\sim C13B-F4B \\sim C13B-F6B \\sim C13A-F5A \\sim C13A-F6A \\sim
C13A-F4A \\sim C20B-F1B ~
 C20B-F2B \\sim C20B-F3B \\sim C20A-F2A \\sim C20A-F3A \\sim C20A-F1A
 with sigma of 0.005
4. Restrained planarity
 C17A, C22A, C21A, C20A, C19A, C18A
 with sigma of 0.1
 C17B, C22B, C21B, C20B, C19B, C18B
 with sigma of 0.1
 C10A, C15A, C14A, C13A, C12A, C11A
 with sigma of 0.1
 C10B, C15B, C14B, C13B, C12B, C11B
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
F1A \\sim F2A \\sim F3A \\sim F4A \\sim F5A \\sim F6A \\sim O1A \\sim O1A \\sim
O1B \\sim O1B \\sim O1B \\sim O2A \\sim O2A \\sim O2B \\sim O2B \\sim O2B \\sim
N1B \\sim N2B \\sim N3A \\sim N3B \\sim N3B \\sim N3B \\sim N4A \\sim N4B \\sim
N4B \\sim N4B \\sim C1A \\sim C1A \\sim C1B \\sim C2A \\sim C2A \\sim C2B \\sim
C3A \\sim C3A \\sim C3A \\sim C3B \\sim C4A \\sim C4A \\sim C4A \\sim C5A \\sim
C5B \\sim C5B \\sim C5B \\sim C6A \\sim C6B \\sim C6B \\sim C6B \\sim C7A \\sim
C7B \\sim C7B \\sim C7B \\sim C8A \\sim C8B \\sim C8B \\sim C8B \\sim C9A \\sim
C9B \\sim C9B \\sim C9B \\sim C10A \\sim C10B \\sim C10B \\sim C10B \\sim C11A
\\sim C11B \\sim C11B \\sim C11B \\sim C12A \\sim C12B \\sim C12B \\sim C12B
\\sim C13A \\sim C13B \\sim C13B \\sim C13B \\sim C14A \\sim C14A \\sim C14B
\\sim C14B \\sim C14B \\sim C15A \\sim C15A \\sim C15B \\sim C15B \\sim C16A
\\sim C16A \\sim C16B \\sim C16B \\sim C17A \\sim C17A \\sim C17B \\sim C17B
\\sim C18A \\sim C18A \\sim C18B \\sim C18B \\sim C19A \\sim C19A \\sim C19B
\\sim C19B \\sim C20A \\sim C20A \\sim C20B \\sim C20B \\sim C21A \\sim C21A
\\sim C21B \\sim C21B \\sim C22A \\sim C22B \\sim C22B \\sim C23B \\sim C23B
\\sim C23B \\sim C24B \\sim C24B \\sim Cl1 \\sim Cl2 \\sim O1W: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.002
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.002
6. Others
 Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=Sof(O1B)=Sof(O2B)=
 Sof(N3B)=Sof(H3B)=Sof(N4B)=Sof(H4B)=Sof(C5B)=Sof(H5BA)=Sof(H5BB)=Sof(C6B)=
 Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(C8B)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(C10B)=
 Sof(C11B)=Sof(H11B)=Sof(C12B)=Sof(H12B)=Sof(C13B)=Sof(C14B)=Sof(H14B)=
 Sof(C15B)=Sof(H15B)=Sof(C16B)=Sof(H16C)=Sof(H16D)=Sof(C17B)=Sof(C18B)=
 Sof(H18B)=Sof(C19B)=Sof(H19B)=Sof(C20B)=Sof(C21B)=Sof(H21B)=Sof(C22B)=
 Sof(H22B)=Sof(C23B)=Sof(C24B)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(O1A)=Sof(O2A)=
 Sof(N3A)=Sof(H3A)=Sof(N4A)=Sof(H4A)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C6A)=
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=
 Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(C14A)=Sof(H14A)=
 Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(C17A)=Sof(C18A)=
 Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=
 Sof(H22A)=Sof(C23A)=Sof(C24A)=FVAR(1)
 Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C3B)=Sof(H3BA)=
 Sof(H3BB)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=1-FVAR(2)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=
 Sof(H3AB)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=FVAR(2)
 Fixed Sof: H1WA(0.5) H1WB(0.5) H2WA(0.5) H2WB(0.5)
7.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB)
7.b Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C1B(H1BA,H1BB), C2A(H2AA,H2AB), C2B(H2BA,H2BB), C3A(H3AA,
 H3AB), C3B(H3BA,H3BB), C4A(H4AA,H4AB), C4B(H4BA,H4BB), C5A(H5AA,H5AB),
 C5B(H5BA,H5BB), C7A(H7AA,H7AB), C7B(H7BA,H7BB), C9A(H9AA,H9AB), C9B(H9BA,H9BB),
  C16A(H16A,H16B), C16B(H16C,H16D)
7.c Aromatic/amide H refined with riding coordinates:
 N3A(H3A), N3B(H3B), N4A(H4A), N4B(H4B), C11A(H11A), C11B(H11B), C12A(H12A),
 C12B(H12B), C14A(H14A), C14B(H14B), C15A(H15A), C15B(H15B), C18A(H18A),
 C18B(H18B), C19A(H19A), C19B(H19B), C21A(H21A), C21B(H21B), C22A(H22A),
 C22B(H22B)
;
_shelx_res_checksum              76437
_shelx_hkl_checksum              79167
_olex2_submission_special_instructions 'No special instructions were received'