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_4305952
_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 Gd N4 O6, C H4 O, Cl '
_chemical_formula_sum            'C23 H30 Cl Gd N4 O7'
_chemical_formula_weight         667.21
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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             2007-09-20T13:11:44-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 102.7540(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1596(6)
_cell_length_b                   11.5025(7)
_cell_length_c                   23.3465(13)
_cell_measurement_reflns_used    7318
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      28.2719
_cell_measurement_theta_min      2.5171
_cell_measurement_wavelength     0.71073
_cell_volume                     2922.9(3)
_computing_cell_refinement       'APEX2 and SAINT V7.12A (Bruker Nonius 2004)'
_computing_data_collection       'Apex2 (Bruker Nonius, 2004)'
_computing_data_reduction
'SAINT and XPREP Version 6.14 COPYRIGHT(c) 2003 Bruker-AXS'
_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 program system. P. T. Beurskens et al. 1999.'
_diffrn_ambient_temperature      100.0(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker X8 APEX II CCD'
_diffrn_measurement_method       'omega and phi rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            31016
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    2.404
_exptl_absorpt_correction_T_max  0.598
_exptl_absorpt_correction_T_min  0.438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;Sheldrick, G. M. (2004). SADABS Version 2.10. 
University of G\"ottingen, Germany'
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.416
_exptl_crystal_size_mid          0.345
_exptl_crystal_size_min          0.214
_platon_squeeze_details
;
;
_refine_diff_density_max         2.523
_refine_diff_density_min         -4.919
_refine_diff_density_rms         0.339
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.312
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         7145
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.312
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0439P)^2^+16.4131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1179
_reflns_number_gt                6741
_reflns_number_total             7145
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800878x-file003.cif
_cod_data_source_block           mmigdl6c_0s
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4305952