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_4347020
_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_formula_moiety         'C26  H36  N6  O4  Cl1  Lu1, Cl1 O4'
_chemical_formula_sum            'C26 H38 Cl2 N6 O12'
_chemical_formula_weight         697.52
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_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             2014-04-23T14:51:12-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 99.33(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.838(3)
_cell_length_b                   18.252(7)
_cell_length_c                   18.672(7)
_cell_measurement_reflns_used    541
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.21
_cell_measurement_theta_min      2.42
_cell_measurement_wavelength     0.71073
_cell_volume                     2972.2(19)
_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    'SIR-2011 (Burla et al., 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.95
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1204
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.95
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16855
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.95
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.211
_exptl_absorpt_coefficient_mu    0.294
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.59
_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    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       0.0031(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     428
_refine_ls_number_reflns         5775
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1595
_refine_ls_R_factor_gt           0.0797
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0747P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1686
_refine_ls_wR_factor_ref         0.2086
_reflns_number_gt                2926
_reflns_number_total             5775
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02627_si_002.cif
_cod_data_source_block           '_compound_1'
_cod_original_cell_volume        2972.1(19)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4347020
_shelx_estimated_absorpt_t_min   0.927
_shelx_estimated_absorpt_t_max   0.974