Activation of a PARACEST Agent for MRI through Selective Outersphere Interactions with Phosphate Diesters
Ching-Hui Huang; Jacob Hammell; S. James Ratnakar; A. Dean Sherry; Janet R. Morrow; Inorganic Chemistry 49 (2010) 5963–5970; doi:10.1021/ic1004616

data_4315912
_publ_section_title
;
 Activation of a PARACEST Agent for MRI through Selective Outersphere
 Interactions with Phosphate Diesters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5963
_journal_page_last               5970
_journal_paper_doi               10.1021/ic1004616
_journal_volume                  49
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C20 H46 Eu N4 O5, 2(C12 H8 N2 O8 P), C F3 O3 S, C3 H8 O, 2(H2 O)'
_chemical_formula_sum            'C48 H74 Eu F3 N8 O27 P2 S'
_chemical_formula_weight         1498.11
_chemical_name_common            ubjm01
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 112.122(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.491(5)
_cell_length_b                   9.8057(18)
_cell_length_c                   27.192(5)
_cell_measurement_reflns_used    3833
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      26.98
_cell_measurement_theta_min      2.23
_cell_volume                     6296(2)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0803
_diffrn_reflns_av_sigmaI/netI    0.0787
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            136522
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         1.39
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.178
_exptl_absorpt_correction_T_max  0.9327
_exptl_absorpt_correction_T_min  0.7339
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3080
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.931
_refine_diff_density_min         -3.732
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details
'Flack H D (1983), 16689 Friedel pairs, Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.042(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1635
_refine_ls_number_reflns         35308
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0763
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0144P)^2^+31.8870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1440
_reflns_number_gt                29118
_reflns_number_total             35308
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1004616_si_001.cif
_cod_data_source_block           ubjm01
_cod_database_code               4315912