Lanthanide Complexes of Triethylenetetramine Tetra-, Penta-, and Hexaacetamide Ligands as Paramagnetic Chemical Exchange-Dependent Saturation Transfer Contrast Agents for Magnetic Resonance Imaging: Nona- versus Decadentate Coordination
Dirk Burdinski; Jeroen A. Pikkemaat; Johan Lub; Peter de Peinder; Lidia Nieto Garrido; Thomas Weyhermüller; Inorganic Chemistry 48 (2009) 6692–6712; doi:10.1021/ic900652y

data_4302723
_publ_section_title
;
Lanthanide Complexes of Triethylenetetramine Tetra-, Penta-, and
Hexaacetamide Ligands as Paramagnetic Chemical Exchange-Dependent
Saturation Transfer Contrast Agents for Magnetic Resonance Imaging: Nona-
versus Decadentate Coordination
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6692
_journal_page_last               6712
_journal_paper_doi               10.1021/ic900652y
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety
'[C23 H39 Eu N9 O5]3+, 3 (Cl O4)-, 3.65 (H2 O)'
_chemical_formula_sum            'C23 H46.3 Cl3 Eu N9 O20.65'
_chemical_formula_weight         1037.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 98.482(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.0701(6)
_cell_length_b                   18.7910(6)
_cell_length_c                   13.0930(4)
_cell_measurement_temperature    100(2)
_cell_volume                     3910.5(2)
_computing_cell_refinement       'Bruker SAINT 7.34A'
_computing_data_collection       'Bruker SAINT 7.34A'
_computing_data_reduction        'Bruker SAINT 7.34A'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
'1678 images at 0.5 deg. stepwise rotation in omega and phi, 43 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode, 50 kV, 40 mA'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            77466
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    1.900
_exptl_absorpt_correction_T_max  0.8327
_exptl_absorpt_correction_T_min  0.6738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent parallelepiped'
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         6.528
_refine_diff_density_min         -3.323
_refine_diff_density_rms         0.175
_refine_ls_extinction_coef       0.00032(9)
_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   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         14130
_refine_ls_number_restraints     151
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0117P)^2^+36.9598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1338
_reflns_number_gt                12014
_reflns_number_total             14130
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900652y_si_002_2.cif
_cod_data_source_block           '[(1bttpam)Eu](ClO4)3*3.65H2O'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4302723