Fe- and Ln-DOTAm-F12 Are Effective Paramagnetic Fluorine Contrast Agents for MRI in Water and Blood.
Srivastava, Kriti; Weitz, Evan A.; Peterson, Katie L.; Marjańska, Małgorzata; Pierre, Valérie C; Inorganic chemistry 56 (2017) 1546–1557; doi:10.1021/acs.inorgchem.6b02631

data_4345048
_publ_section_title
;
 Fe- and Ln-DOTAm-F12 Are Effective Paramagnetic Fluorine Contrast Agents
 for MRI in Water and Blood.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1546
_journal_page_last               1557
_journal_paper_doi               10.1021/acs.inorgchem.6b02631
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C24 H38 F12 N8 O5 Tm, 4(Cl)'
_chemical_formula_sum            'C24 H38 Cl4 F12 N8 O5 Tm'
_chemical_formula_weight         1057.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c e'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.5559(18)
_cell_length_b                   18.5893(13)
_cell_length_c                   18.6003(14)
_cell_measurement_reflns_used    2823
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      68.115
_cell_measurement_theta_min      6.191
_cell_volume                     8836.4(11)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEX II, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker D8 Photon 100 CMOS'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_monochromator  'normal parabolic mirrors'
_diffrn_radiation_source         'micro-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0184
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            46172
_diffrn_reflns_theta_full        68.30
_diffrn_reflns_theta_max         68.30
_diffrn_reflns_theta_min         3.46
_exptl_absorpt_coefficient_mu    6.819
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5364
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4184
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
The Squeeze results are consistent with 5 water molecules per asymmetric unit.
;
_refine_diff_density_max         3.791
_refine_diff_density_min         -1.558
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4109
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1210P)^2^+79.7163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1853
_refine_ls_wR_factor_ref         0.1928
_reflns_number_gt                3496
_reflns_number_total             4109
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b02631_si_002.cif
_cod_data_source_block           13251sqz
_cod_depositor_comments          'Adding full bibliography for 4345048.cif.'
_cod_original_sg_symbol_H-M      Cmca
_cod_database_code               4345048