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_4302724
_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_absolute_configuration unk
_chemical_formula_moiety         '(C18 H36 Eu N10 O6), 3 (Cl O4), 3 (H2 O)'
_chemical_formula_sum            'C18 H42 Cl3 Eu N10 O21'
_chemical_formula_weight         992.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   13.2178(4)
_cell_length_b                   23.9498(8)
_cell_length_c                   45.210(2)
_cell_measurement_temperature    100(2)
_cell_volume                     14311.8(9)
_computing_cell_refinement       'Collect, Bruker AXS'
_computing_data_collection       'Collect, Bruker AXS'
_computing_data_reduction        'Collect, Bruker AXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
'774 images at 0.3 deg stepwise rotation in omega and phi, 9 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode, 50 kV, 80 mA'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0975
_diffrn_reflns_av_sigmaI/netI    0.0829
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            92795
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    2.073
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.660
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   XPREP
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.843
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent block'
_exptl_crystal_F_000             8032
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.429
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.153
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2118
_refine_ls_number_reflns         23894
_refine_ls_number_restraints     4295
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+74.0502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1504
_reflns_number_gt                18498
_reflns_number_total             23894
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900652y_si_002_3.cif
_cod_data_source_block           '[(ttham)Eu](ClO4)3*3H2O'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' 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               4302724