Positively Charged Lanthanide Complexes with Cyclen-Based Ligands: Synthesis, Solid-State and Solution Structure, and Fluoride Interaction
Luís M. P. Lima; Alexandre Lecointre; Jean-François Morfin; Andrés de Blas; Dimitris Visvikis; Loïc J. Charbonnière; Carlos Platas-Iglesias; Raphaël Tripier; Inorganic Chemistry 50 (2011) 12508–12521; doi:10.1021/ic201447c

data_4327086
_publ_contact_author_address
;
Laboratoire de chimie,
electrochimie moleculaire et chimie analytique (UMR 6521)
Universite de Bretagne occidentale
6, avenue Victor Le Gorgeu
CS 93837
F-29238 BREST cedex 3
FRANCE 
;
_publ_contact_author_email       raphael.tripier@univ-brest.fr
_publ_contact_author_fax         '+ 34 981 167065'
_publ_contact_author_name        'Tripier, Raphael'
_publ_contact_author_phone       '+ 34 981 167000'
_publ_section_title
;
 Positively Charged Lanthanide Complexes with Cyclen-Based Ligands:
 Synthesis, Solid-State and Solution Structure, and Fluoride Interaction
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12508
_journal_page_last               12521
_journal_paper_doi               10.1021/ic201447c
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C32 H64 Cl La N8 O12, 4(H2 O), , 2(Cl)'
_chemical_formula_sum            'C32 H71 Cl3 La N8 O16'
_chemical_formula_weight         1069.23
_space_group_IT_number           130
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      130
_symmetry_space_group_name_Hall  '-P 4a 2ac'
_symmetry_space_group_name_H-M   'P 4/n c c :2'
_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
_audit_creation_date             2011-06-29T14:10:13-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2869(4)
_cell_length_b                   14.2869(4)
_cell_length_c                   23.9665(11)
_cell_measurement_reflns_used    7686
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      31.6157
_cell_measurement_theta_min      2.845
_cell_volume                     4891.9(3)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
;
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 1980-2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3622
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Kappa-geometry diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0170339841
_diffrn_orient_matrix_UB_12      -0.0175847521
_diffrn_orient_matrix_UB_13      0.0257847834
_diffrn_orient_matrix_UB_21      0.0279434261
_diffrn_orient_matrix_UB_22      -0.0330767841
_diffrn_orient_matrix_UB_23      -0.0145291339
_diffrn_orient_matrix_UB_31      0.0374439374
_diffrn_orient_matrix_UB_32      0.0326525621
_diffrn_orient_matrix_UB_33      -0.0008275513
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0767
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            34445
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.85
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.106
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
        (compiled Nov  6 2009,16:24:50)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_description
;
;
_exptl_crystal_F_000             2220
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.908
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2507
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
 [0.00000+1.00000exp(1.42(sin\q/\l)^2^)]/
   [\s^2^(Fo^2^)+0.0221+0.0000*P+(0.0855P)^2^+0.0000sin\q/\l]
 where P = 0.32824Fo^2^ + 0.67176Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1381
_reflns_number_gt                1519
_reflns_number_total             2507
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic201447c_si_002.cif
_cod_data_source_block           sm20la-d0non-dedouble
_cod_original_sg_symbol_H-M      'P 4/n c c'
_cod_database_code               4327086