Lanthanide(iii) complexes of a pyridine N-oxide analogue of DOTA: exclusive M isomer formation induced by a six-membered chelate ring
Polášek, Miloslav; Rudovský, Jakub; Hermann, Petr; Lukeš, Ivan; Elst, Luce Vander; Muller, Robert N.; Chemical Communications  (2004) 2602–2603; doi:10.1039/b409996f

data_7111452
_publ_section_title
;
 Lanthanide(iii) complexes of a pyridine N-oxide analogue of DOTA:
 exclusive M isomer formation induced by a six-membered chelate ring
;
_journal_issue                   22
_journal_name_full               'Chemical Communications'
_journal_page_first              2602
_journal_page_last               2603
_journal_paper_doi               10.1039/b409996f
_journal_year                    2004
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'C20 H28 Dy N5 O7, 3(H2O)'
_chemical_formula_sum            'C20 H34 Dy N5 O10'
_chemical_formula_weight         667.02
_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                82.0772(12)
_cell_angle_beta                 86.8978(12)
_cell_angle_gamma                90.0588(10)
_cell_formula_units_Z            2
_cell_length_a                   7.29510(10)
_cell_length_b                   10.7100(2)
_cell_length_c                   15.7375(3)
_cell_measurement_reflns_used    16569
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     1216.01(4)
_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(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0404
_diffrn_reflns_av_sigmaI/netI    0.0277
_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            21215
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         3.02
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.137
_exptl_absorpt_correction_T_max  0.537
_exptl_absorpt_correction_T_min  0.246
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.635
_refine_diff_density_min         -1.435
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         5585
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0192
_refine_ls_R_factor_gt           0.0181
_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^)+(0.0182P)^2^+1.2995P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0460
_refine_ls_wR_factor_ref         0.0463
_reflns_number_gt                5478
_reflns_number_total             5585
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b409996fsup1.cif
_cod_data_source_block           dypol
_cod_original_cell_volume        1216.03(4)
_cod_database_code               7111452