Lanthanide Complexes Based on a 1,7-Diaza-12-crown-4 Platform Containing Picolinate Pendants: A New Structural Entry for the Design of Magnetic Resonance Imaging Contrast Agents
Marta Mato-Iglesias; Adrián Roca-Sabio; Zoltán Pálinkás; David Esteban-Gómez; Carlos Platas-Iglesias; Éva Tóth; Andrés de Blas; Teresa Rodríguez-Blas; Inorganic Chemistry 47 (2008) 7840–7851; doi:10.1021/ic800878x

data_4305953
_publ_section_title
;
Lanthanide Complexes Based on a 1,7-Diaza-12-crown-4 Platform Containing
Picolinate Pendants: A New Structural Entry for the Design of Magnetic
Resonance Imaging Contrast Agents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7840
_journal_page_last               7851
_journal_paper_doi               10.1021/ic800878x
_journal_volume                  47
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C22 H26 Lu N4 O6, Cl, C H4  O, 3(H2 O) '
_chemical_formula_sum            'C23 H36 Cl Lu N4 O10'
_chemical_formula_weight         738.98
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2007-06-19T10:53:40-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                99.883(4)
_cell_angle_beta                 91.113(4)
_cell_angle_gamma                98.435(4)
_cell_formula_units_Z            2
_cell_length_a                   8.6420(19)
_cell_length_b                   8.7926(19)
_cell_length_c                   18.355(4)
_cell_measurement_reflns_used    5295
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      25.5358
_cell_measurement_theta_min      2.2549
_cell_measurement_wavelength     0.71073
_cell_volume                     1357.7(5)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    DIRDIF99
_diffrn_ambient_temperature      100.0(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       'omega and  phi rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_av_unetI/netI     0.0858
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18640
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.13
_exptl_absorpt_coefficient_mu    3.796
_exptl_absorpt_correction_T_max  0.724
_exptl_absorpt_correction_T_min  0.514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SABADS, Bruker-AXS V2.03'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irrregular
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.761
_refine_diff_density_min         -1.271
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         6723
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0118P)^2^+2.6767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0747
_reflns_number_gt                5436
_reflns_number_total             6723
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800878x-file004.cif
_cod_data_source_block           12597s
_cod_database_code               4305953