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_7127850
_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 H66 Gd N8 O5, 2.95(I), H2 I0.05 O, H2 O'
_chemical_formula_sum            'C48 H70 Gd I3 N8 O7'
_chemical_formula_weight         1409.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-04
_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                 90.312(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.2967(7)
_cell_length_b                   11.2692(5)
_cell_length_c                   15.7712(7)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.36
_cell_measurement_theta_min      2.22
_cell_volume                     2718.6(2)
_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      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.0692
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            60168
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.785
_diffrn_reflns_theta_min         1.860
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.977
_exptl_absorpt_correction_T_max  0.2098
_exptl_absorpt_correction_T_min  0.1743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0618 before and 0.0556 after correction. The Ratio of minimum to maximum transmission is 0.8308. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_description       needle
_exptl_crystal_F_000             1386
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.011
_refine_diff_density_min         -1.032
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details
;
 Flack x determined using 4449 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         13946
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0265P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0729
_reflns_Friedel_coverage         0.879
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                11420
_reflns_number_total             13946
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06400a2.cif
_cod_data_source_block           amali_gdiiime_2
_cod_depositor_comments
'Adding full bibliography for 7127849--7127850.cif.'
_cod_database_code               7127850
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.616
_shelx_estimated_absorpt_t_min   0.512
_olex2_refinement_description
;
1. 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 C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H2WA-H2WB = H1WB_$1-H1WA_$1 = H3WB_$1-H3WA_$1
 1.34 with sigma of 0.02
 O3W-H3WA = O3W-H3WB = O2W_$2-H2WB_$2 = O2W_$2-H2WA_$2 = O1W-H1WA = O1W-H1WB
 0.84 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(I1) = Uanis(I1')
Uanis(I2) = Uanis(I2')
Uanis(I3) = Uanis(I3')
4. Others
 Sof(I1')=1-FVAR(1)
 Sof(I1)=FVAR(1)
 Sof(I2')=1-FVAR(2)
 Sof(I2)=FVAR(2)
 Sof(I3')=1-FVAR(3)
 Sof(I3)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B), C12(H12A,H12B), C14(H14A,H14B),
 C16(H16A,H16B), C17(H17A,H17B), C25(H25A,H25B), C33(H33A,H33B), C41(H41A,H41B)
5.b Aromatic/amide H refined with riding coordinates:
 N5(H5), N6(H6), N7(H7), N8(H8), C19(H19), C20(H20), C22(H22), C23(H23),
 C27(H27), C28(H28), C30(H30), C31(H31), C35(H35), C36(H36), C38(H38), C39(H39),
  C43(H43), C44(H44), C46(H46), C47(H47)
5.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C32(H32A,H32B,H32C), C40(H40A,H40B,H40C), C48(H48A,H48B,
 H48C)
;
_shelx_res_checksum              89461
_shelx_hkl_checksum              36009
_olex2_submission_special_instructions 'No special instructions were received'