Lanthanide(III) Complexes of Pyridine-N-Oxide Analogues of DOTA in Solution and in the Solid State. A New Kind of Isomerism in Complexes of DOTA-like Ligands
Miloslav Polášek; Jan Kotek; Petr Hermann; Ivana Císařová; Koen Binnemans; Ivan Lukeš; Inorganic Chemistry 48 (2009) 466–475; doi:10.1021/ic801597z

data_4301207
_publ_section_title
;
Lanthanide(III) Complexes of Pyridine-N-Oxide Analogues of DOTA in Solution
and in the Solid State. A New Kind of Isomerism in Complexes of DOTA-like
Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              466
_journal_page_last               475
_journal_paper_doi               10.1021/ic801597z
_journal_volume                  48
_journal_year                    2009
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'C20 H28 N5 O7 Tm, 3(H2 O)'
_chemical_formula_sum            'C20 H34 N5 O10 Tm'
_chemical_formula_weight         673.45
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.7654(12)
_cell_angle_beta                 86.6648(15)
_cell_angle_gamma                89.6355(16)
_cell_formula_units_Z            2
_cell_length_a                   7.31450(10)
_cell_length_b                   10.6758(3)
_cell_length_c                   15.7482(4)
_cell_measurement_reflns_used    22733
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1215.01(5)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Nonius KappaCCD area detector'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21850
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.31
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.716
_exptl_absorpt_correction_T_max  0.608
_exptl_absorpt_correction_T_min  0.214
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.841
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.084
_refine_diff_density_min         -2.346
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       0.0056(4)
_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   1.195
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5539
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0053P)^2^+4.9089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0732
_reflns_number_gt                5381
_reflns_number_total             5539
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801597z_si_002_2.cif
_cod_data_source_block           tmmil
_cod_database_code               4301207