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_4327085
_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       'Tripier, Raphael'
_publ_contact_author_name        'Tripier, Raphael'
_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_compound_source        'synthesis as described'
_chemical_formula_moiety
'C64 H104 Eu2 F N16 O12, 3(Cl), 2(F), 18.16(O)'
_chemical_formula_sum            'C64 H104 Cl3 Eu2 F3 N16 O30.16'
_chemical_formula_weight         2047.45
_chemical_name_common            RTLIEU
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      13
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/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
_audit_creation_date             2011-06-04T20:20:38-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.018(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3092(3)
_cell_length_b                   16.5654(3)
_cell_length_c                   20.9868(4)
_cell_measurement_reflns_used    4915
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.13
_cell_measurement_theta_min      2.76
_cell_measurement_wavelength     0.71073
_cell_volume                     4627.01(16)
_computing_cell_refinement       'APEX2 v2011.4-1 (Bruker AXS, 2011)'
_computing_data_collection       'APEX2 v2011.4-1 (Bruker AXS, 2011)'
_computing_data_reduction        'APEX2 v2011.4-1 (Bruker AXS, 2011)'
_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    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8 kappa APEXII CCD'
_diffrn_measurement_method       'omega and phi 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  0.0675
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            84946
_diffrn_reflns_theta_full        29.39
_diffrn_reflns_theta_max         29.39
_diffrn_reflns_theta_min         0.97
_exptl_absorpt_coefficient_mu    1.516
_exptl_absorpt_correction_T_max  0.8879
_exptl_absorpt_correction_T_min  0.7714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER AXS - SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       prism
_exptl_crystal_F_000             2090.4
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.656
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.14
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         12766
_refine_ls_number_restraints     806
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+10.3248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1117
_reflns_number_gt                9325
_reflns_number_total             12766
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic201447c_si_001.cif
_cod_data_source_block           uc01tra2n
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               4327085