NMR, Relaxometric, and Structural Studies of the Hydration and Exchange Dynamics of Cationic Lanthanide Complexes of Macrocyclic Tetraamide Ligands
Silvio Aime; Alessandro Barge; James I. Bruce; Mauro Botta; Judith A. K. Howard; Janet M. Moloney; David Parker; Alvaro S. de Sousa; Mark Woods; Journal of the American Chemical Society 121 (1999) 5762–5771; doi:10.1021/ja990225d

data_4116425
_publ_contact_author             'Professor David Parker'
_publ_contact_author_email       david.parker@durham.ac.uk
_publ_section_title
;
 NMR, Relaxometric, and Structural Studies of the Hydration and Exchange
 Dynamics of Cationic Lanthanide Complexes of Macrocyclic Tetraamide
 Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5762
_journal_page_last               5771
_journal_paper_doi               10.1021/ja990225d
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C20 H43 N8 O5.5'
_chemical_formula_weight         483.62
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 106.13(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.517(7)
_cell_length_b                   8.7230(17)
_cell_length_c                   18.638(4)
_cell_measurement_temperature    150(2)
_cell_volume                     5078(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0884
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            2676
_diffrn_reflns_theta_full        49.99
_diffrn_reflns_theta_max         49.99
_diffrn_reflns_theta_min         4.94
_exptl_absorpt_coefficient_mu    0.769
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_F_000             2104
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         2618
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0765
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1307P)^2^+16.2567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1956
_refine_ls_wR_factor_ref         0.2179
_reflns_number_gt                2043
_reflns_number_total             2618
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja990225d_3.cif
_cod_data_source_block           97srv012
_cod_original_cell_volume        5078.5(17)
_cod_original_formula_sum        'C20 H43 N8 O5.50'
_cod_database_code               4116425