Complexation of Ln(3+) Ions with Cyclam Dipicolinates: A Small Bridge that Makes Huge Differences in Structure, Equilibrium, and Kinetic Properties.
Rodríguez-Rodríguez, Aurora; Regueiro-Figueroa, Martín; Esteban-Gómez, David; Tripier, Raphaël; Tircsó, Gyula; Kálmán, Ferenc Krisztián; Bényei, Attila Csaba; Tóth, Imre; de Blas, Andrés; Rodríguez-Blas, Teresa; Platas-Iglesias, Carlos; Inorganic chemistry 55 (2016) 2227–2239; doi:10.1021/acs.inorgchem.5b02627

data_4347022
_publ_section_title
;
 Complexation of Ln(3+) Ions with Cyclam Dipicolinates: A Small Bridge
 that Makes Huge Differences in Structure, Equilibrium, and Kinetic
 Properties.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2227
_journal_page_last               2239
_journal_paper_doi               10.1021/acs.inorgchem.5b02627
_journal_volume                  55
_journal_year                    2016
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C26 H34 Cl La N6 O4, 5(H2 O)'
_chemical_formula_sum            'C26 H44 Cl La N6 O9'
_chemical_formula_weight         759.03
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-03-27T14:09:21-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 102.195(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5447(6)
_cell_length_b                   16.3852(6)
_cell_length_c                   14.1598(6)
_cell_measurement_reflns_used    5352
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      25.0392
_cell_measurement_theta_min      2.6524
_cell_measurement_wavelength     0.71073
_cell_volume                     3071.6(2)
_computing_cell_refinement
'SAINT V7.68A (Bruker: Madison, 2009 ) in Apex2 suite.'
_computing_data_collection       'Apex2, Bruker Instrument Service v2010, 1-2'
_computing_data_reduction
'SAINT and XPREP Version 2008/2 (Sheldrick, Bruker AXS Inc.)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'BRUKER-NONIUS X8 APEX KAPPA CCD'
_diffrn_measurement_method       'omega and  phi rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14091
_diffrn_reflns_theta_full        25.1
_diffrn_reflns_theta_max         25.1
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    1.539
_exptl_absorpt_correction_T_max  0.8249
_exptl_absorpt_correction_T_min  0.7762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS Version 2008/1 (Sheldrick, Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.72
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.1
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         2743
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.023
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0197P)^2^+6.5707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0528
_reflns_number_gt                2548
_reflns_number_total             2743
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic5b02627_si_002.cif
_cod_data_source_block           compound_3
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4347022