Equilibria and structure of the lanthanide(III)-2-hydroxy-1,3-diaminopropane-N,N,N',N'-tetraacetate complexes: formation of alkoxo-bridged dimers in solid state and solution.
Tircsó, Gyula; Bényei, Attila; Brücher, Ernõ; Kis, Anita; Kiraly, Róbert; Inorganic chemistry 45 (2006) 4951–4962; doi:10.1021/ic0517321

data_4350124
_publ_section_title
;
 Equilibria and structure of the
 lanthanide(III)-2-hydroxy-1,3-diaminopropane-N,N,N',N'-tetraacetate
 complexes: formation of alkoxo-bridged dimers in solid state and
 solution.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4951
_journal_page_last               4962
_journal_paper_doi               10.1021/ic0517321
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C11 H23 K2 N2 Nd1 O14, 3(H2 O)'
_chemical_formula_sum            'C11 H29 K2 N2 Nd O17'
_chemical_formula_weight         683.8
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2005-07-04T08:49:42-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                78.693(10)
_cell_angle_beta                 71.953(10)
_cell_angle_gamma                82.483(10)
_cell_formula_units_Z            2
_cell_length_a                   9.5072(10)
_cell_length_b                   10.2779(10)
_cell_length_c                   13.497(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.76
_cell_measurement_theta_min      11.43
_cell_volume                     1226.1(3)
_computing_cell_refinement       'MACH3/PC (Enraf Nonius, 1996)'
_computing_data_collection       'MACH3/PC (Enraf Nonius, 1996)'
_computing_data_reduction        'PROFIT (Streltsov & Zavodnik, 1989)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Enraf Nonius MACH3'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.014
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4854
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         2.03
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        -1
_diffrn_standards_interval_count 67
_diffrn_standards_interval_time  28
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.534
_exptl_absorpt_correction_T_max  0.4417
_exptl_absorpt_correction_T_min  0.2911
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
        Number of psi-scan sets used was   4
        Theta correction was applied.
        Averaged transmission function was used.
        Fourier smoothing - Window value   5
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.852
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             686
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.162
_refine_diff_density_min         -1.453
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.503
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         4495
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.5
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+3.8505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1316
_refine_ls_wR_factor_ref         0.1365
_reflns_number_gt                4143
_reflns_number_total             4495
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0517321si20051005_075650.cif
_cod_data_source_block           0325b
_cod_database_code               4350124