Structural, Luminescence, and NMR Studies of the Reversible Binding of Acetate, Lactate, Citrate, and Selected Amino Acids to Chiral Diaqua Ytterbium, Gadolinium, and Europium Complexes
Rachel S. Dickins; Silvio Aime; Andrei S. Batsanov; Andrew Beeby; Mauro Botta; James I. Bruce; Judith A. K. Howard; Christine S. Love; David Parker; Robert D. Peacock; Horst Puschmann; Journal of the American Chemical Society 124 (2002) 12697–12705; doi:10.1021/ja020836x

data_4115229
_publ_contact_author             'Andrei S.Batsanov'
_publ_contact_author_email       a.s.batsanov@durham.ac.uk
_publ_section_title
;
 Structural, Luminescence, and NMR Studies of the Reversible Binding of
 Acetate, Lactate, Citrate, and Selected Amino Acids to Chiral Diaqua
 Ytterbium, Gadolinium, and Europium Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12697
_journal_page_last               12705
_journal_paper_doi               10.1021/ja020836x
_journal_volume                  124
_journal_year                    2002
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C40 H57 N8 O5 Yb 2+,2(C F3 O3 S 1-),C H4 O,2(H2 O)'
_chemical_formula_sum            'C43 H65 F6 N8 O14 S2 Yb'
_chemical_formula_weight         1269.19
_space_group_IT_number           1
_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                64.30(1)
_cell_angle_beta                 78.19(1)
_cell_angle_gamma                63.07(1)
_cell_formula_units_Z            1
_cell_length_a                   11.392(2)
_cell_length_b                   11.591(2)
_cell_length_c                   12.421(2)
_cell_measurement_reflns_used    985
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.11
_cell_measurement_theta_min      12.07
_cell_volume                     1317.6(4)
_computing_cell_refinement       'SMART version 5.625 (Bruker, 2001)'
_computing_data_collection       'SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT version 6.02A (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL version 6.12 (Bruker, 2001)'
_computing_publication_material  'SHELXTL version 6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'SMART 6000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_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  0.0204
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            39412
_diffrn_reflns_theta_full        37.50
_diffrn_reflns_theta_max         39.46
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.945
_exptl_absorpt_correction_T_max  0.7291
_exptl_absorpt_correction_T_min  0.5707
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'XPREP (SHELXTL), R(int)=0.039 before correction'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_description       block
_exptl_crystal_F_000             647
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_refine_diff_density_max         2.126
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.014(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         27144
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0225
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0497
_refine_ls_wR_factor_ref         0.0497
_reflns_Friedel_coverage         0.79
_reflns_number_gt                27134
_reflns_number_total             27144
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja020836x_3.cif
_cod_data_source_block           YbL1.glycinate
_cod_database_code               4115229