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_4312878
_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[Ce(DOTA)]^.^6H~2~O^.^0.5KCl
_chemical_formula_sum            'C13.5 H35 Cl0.5 K1.5 N4 O14 Tm'
_chemical_formula_weight         722.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 111.09(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   37.550(6)
_cell_length_b                   8.981(3)
_cell_length_c                   16.783(5)
_cell_measurement_temperature    293(2)
_cell_volume                     5281(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.456
_diffrn_measured_fraction_theta_max 0.456
_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  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8489
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.21
_exptl_absorpt_coefficient_mu    3.715
_exptl_crystal_density_diffrn    1.818
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2896
_refine_diff_density_max         1.271
_refine_diff_density_min         -1.296
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.00010(5)
_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   1.223
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         4541
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.223
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+42.0475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0876
_reflns_number_gt                4536
_reflns_number_total             4541
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025790n_s1_5.cif
_cod_data_source_block           tmdotap
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+42.0475P] 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^)+(0.0263P)^2^+42.0475P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C13.50 H35 Cl0.50 K1.50 N4 O14 Tm'
_cod_database_code               4312878