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_4347023
_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         '2(C26 H34 Gd N6 O4), 2(F6 P), 5(H2 O)'
_chemical_formula_sum            'C52 H78 F12 Gd2 N12 O13 P2'
_chemical_formula_weight         1683.7
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2014-02-12T13:01:09-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.9271(8)
_cell_length_b                   21.5806(12)
_cell_length_c                   41.373(2)
_cell_measurement_reflns_used    2453
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.09
_cell_measurement_theta_min      2.4
_cell_measurement_wavelength     0.71073
_cell_volume                     12434.9(12)
_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, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.866
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'BRUKER-NONIUS X8 APEX KAPPA CCD'
_diffrn_measurement_method       'omega and phi rotation with narrow frames'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2041
_diffrn_reflns_Laue_measured_fraction_full 0.866
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            116346
_diffrn_reflns_point_group_measured_fraction_full 0.866
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.411
_diffrn_reflns_theta_min         8.631
_exptl_absorpt_coefficient_mu    2.274
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.664
_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    1.799
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6752
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.907
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     900
_refine_ls_number_reflns         9752
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+26.7705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.1035
_reflns_number_gt                6520
_reflns_number_total             9752
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02627_si_002.cif
_cod_data_source_block           compound_4
_cod_original_cell_volume        12435.0(12)
_cod_database_code               4347023
_shelx_estimated_absorpt_t_min   0.6
_shelx_estimated_absorpt_t_max   0.915