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_4116424
_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            'C16 H40 Cl2 N4 O13'
_chemical_formula_weight         567.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.30(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.018(2)
_cell_length_b                   20.019(4)
_cell_length_c                   11.822(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      20
_cell_volume                     2606.9(8)
_computing_cell_refinement       'MCS/AFC. Molecular Structure Corporation'
_computing_data_collection       'MSC/AFC. Molecular Structure Corporation'
_computing_data_reduction        'Texsan (Molecular Structure Corporation)'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.895
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_device       'Rigaku AFC6S'
_diffrn_measurement_method       '/w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5021
_diffrn_reflns_theta_full        74.98
_diffrn_reflns_theta_max         74.98
_diffrn_reflns_theta_min         4.34
_diffrn_standards_decay_%        0.6
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.852
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       'orthogonal block'
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.750
_exptl_crystal_size_mid          0.675
_exptl_crystal_size_min          0.375
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4801
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0815
_refine_ls_shift/su_max          0.141
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1500P)^2^+6.2610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2293
_refine_ls_wR_factor_ref         0.2501
_reflns_number_gt                4388
_reflns_number_total             4801
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja990225d_2.cif
_cod_data_source_block           99srv036
_cod_original_cell_volume        2606.9(9)
_cod_database_code               4116424