Structural Variations Across the Lanthanide Series of Macrocyclic DOTA Complexes: Insights into the Design of Contrast Agents for Magnetic Resonance Imaging
F. Benetollo; Gabriella Bombieri; L. Calabi; S. Aime; M. Botta; Inorganic Chemistry 42 (2003) 148–157; doi:10.1021/ic025790n

data_4312875
_publ_contact_author
;
      Bombieri Gabriella
      Istituto Chimica Farmaceutica
      Viale Abruzzi 42
      20131 Milano
      Italy
;
_publ_contact_author_email       gabriella.bombieri@unimi.it
_publ_contact_author_fax         '++39 02 50317565'
_publ_contact_author_phone       '++39 02 50317516'
_publ_section_title
;
 Structural Variations Across the Lanthanide Series of Macrocyclic DOTA
 Complexes: Insights into the Design of Contrast Agents for Magnetic
 Resonance Imaging
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              148
_journal_page_last               157
_journal_paper_doi               10.1021/ic025790n
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         Na[Pr(DOTA)(H~2~O)]^.^4H~2~O
_chemical_formula_sum            'C16 H34 N4 Na O13 Pr'
_chemical_formula_weight         654.37
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.74(3)
_cell_angle_beta                 84.93(3)
_cell_angle_gamma                80.98(2)
_cell_formula_units_Z            2
_cell_length_a                   8.715(2)
_cell_length_b                   9.188(2)
_cell_length_c                   15.880(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1242.7(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_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  0.0098
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4844
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    2.047
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             664
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.0018(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         4668
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          1.382
_refine_ls_shift/su_mean         0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.3058P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0620
_reflns_number_gt                4668
_reflns_number_total             4668
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025790n_s1_2.cif
_cod_data_source_block           pr-dota
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.3058P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.3058P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1242.7(7)
_cod_database_code               4312875