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_4302722
_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 N9 O5 Tm]3+, 3 (Cl O4)-, 4 (H2 O)'
_chemical_formula_sum            'C23 H47 Cl3 N9 O21 Tm'
_chemical_formula_weight         1060.98
_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                 98.456(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.8565(5)
_cell_length_b                   18.8304(6)
_cell_length_c                   13.0221(4)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.32
_cell_measurement_theta_min      2.51
_cell_volume                     3845.9(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX2'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source
'rotating anode, 50 kV, 40 mA, Multi-Layer Optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0137
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            441190
_diffrn_reflns_theta_full        35.00
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    2.609
_exptl_absorpt_correction_T_max  0.9028
_exptl_absorpt_correction_T_min  0.8384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2008/1'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent parallelepiped'
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.719
_refine_diff_density_min         -1.399
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         16916
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+6.2606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0587
_reflns_number_gt                15348
_reflns_number_total             16916
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900652y_si_002_1.cif
_cod_data_source_block           '[(1bttpam)Tm](ClO4)3*4H2O'
_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 
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_cod_database_code               4302722