Fluorinated EuII-based multimodal contrast agent for temperature- and redox-responsive magnetic resonance imaging
Basal, Lina A.; Bailey, Matthew D.; Romero, Jonathan; Ali, Meser M.; Kurenbekova, Lyazat; Yustein, Jason; Pautler, Robia G.; Allen, Matthew J.; Chem. Sci.  (2017) –; doi:10.1039/C7SC03142D

data_1547802
_publ_section_title
;
 Fluorinated EuII-based multimodal contrast agent for temperature- and
 redox-responsive magnetic resonance imaging
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC03142D
_journal_year                    2017
_chemical_formula_moiety         'C48 H46 Eu F12 N8 O4.5, 2(Cl), 2.17(O)'
_chemical_formula_sum            'C48 H46 Cl2 Eu F12 N8 O6.66'
_chemical_formula_weight         1292.43
_chemical_properties_physical
Air-sensitive,Oxygen-sensitive,Light-sensitive,Photo-sensitive
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n'
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-10-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-10-04 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.2597(12)
_cell_length_b                   14.2597(12)
_cell_length_c                   17.793(2)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.17
_cell_measurement_theta_min      2.29
_cell_volume                     3618.0(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.1
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1721
_diffrn_reflns_av_unetI/netI     0.0732
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            65731
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.663
_diffrn_reflns_theta_min         1.830
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.013
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4121
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1297
_exptl_crystal_size_max          0.667
_exptl_crystal_size_mid          0.512
_exptl_crystal_size_min          0.289
_refine_diff_density_max         1.264
_refine_diff_density_min         -2.546
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         3797
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.1261
_refine_ls_R_factor_gt           0.0986
_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^)+(0.1812P)^2^+39.9231P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2713
_refine_ls_wR_factor_ref         0.2933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2937
_reflns_number_total             3797
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc03142d2.cif
_cod_data_source_block           2EuII
_cod_original_cell_volume        3618.0(7)
_cod_database_code               1547802
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.758
_shelx_estimated_absorpt_t_min   0.551
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C17) \\sim Ueq,
Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of
0.06 and sigma for terminal atoms of 0.12
3. Others
 Fixed Sof: Cl02(0.25) F1(0.5) F3(0.5) F2(0.5) O1(0.5) N2(0.5) H2(0.5)
 O2(0.125) N1(0.5) C9(0.5) C6(0.5) C12(0.5) C4(0.5) C1(0.5) H1(0.5) C3(0.5)
 H3A(0.5) H3B(0.5) C5(0.5) H5A(0.5) H5B(0.5) C8(0.5) H8(0.5) C11(0.5) H11(0.5)
 C2(0.5) H2A(0.5) H2B(0.5) C7(0.5) H7(0.5) C10(0.5) H10(0.5) O5(0.125) O6(0.5)
 N4(0.5) C17(0.5) H17A(0.5) H17B(0.5) C19(0.5) H19(0.5) C18(0.5) C23(0.5)
 H23(0.5) C20(0.5) H20(0.5) C22(0.5) F5(0.5) F4(0.5) C21(0.5) H21(0.5) C24(0.5)
 F6(0.5) N3(0.5) C13(0.5) H13A(0.5) H13B(0.5) C14(0.5) H14(0.5) C16(0.5)
 Cl2(0.25) C15(0.5) H15A(0.5) H15B(0.5) O0AA(0.33333) O1AA(0.08333)
4.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C5(H5A,H5B), C2(H2A,H2B), C17(H17A,H17B), C13(H13A,H13B),
 C15(H15A,H15B)
4.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C1(H1), C8(H8), C11(H11), C7(H7), C10(H10), C19(H19), C23(H23),
 C20(H20), C21(H21), C14(H14)
;
_shelx_res_checksum              34591
_olex2_submission_special_instructions 'No special instructions were received'