Solution Structure of Ln(III) Complexes with Macrocyclic Ligands Through Theoretical Evaluation of 1H NMR Contact Shifts
Aurora Rodríguez-Rodríguez; David Esteban-Gómez; Andrés de Blas; Teresa Rodríguez-Blas; Mauro Botta; Raphaël Tripier; Carlos Platas-Iglesias; Inorganic Chemistry 51 (2012) 13419–13429; doi:10.1021/ic302322r

data_4331382
_publ_contact_author_address
;
Departamento de Quimica Fundamental
Facultade de Ciencias
Universidade da Coru\~na
Rua da Fraga 10
15008 A Coru\~na
Spain
;
_publ_contact_author_email       andres.blas@udc.es
_publ_contact_author_fax         '+ 34 981 167065'
_publ_contact_author_name        'De Blas, Andr\'es'
_publ_contact_author_phone       '+ 34 981 167000'
_publ_section_title
;
 Solution Structure of Ln(III) Complexes with Macrocyclic Ligands Through
 Theoretical Evaluation of 1H NMR Contact Shifts
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13419
_journal_page_last               13429
_journal_paper_doi               10.1021/ic302322r
_journal_volume                  51
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C24 H32 Lu N6 O4, F6 P, 2(H2 O)'
_chemical_formula_sum            'C24 H36 F6 Lu N6 O6 P'
_chemical_formula_weight         824.53
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-06-20T13:20:04-00:00
_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                   13.5298(5)
_cell_length_b                   15.8653(7)
_cell_length_c                   13.5839(5)
_cell_measurement_reflns_used    6005
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.636
_cell_measurement_theta_min      2.4811
_cell_measurement_wavelength     0.71073
_cell_volume                     2915.8(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    'DIRDIF2008, P.T. Beurskens ET AL. (2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_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  0.0652
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_limit_h_max       16
_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            31179
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         9.52
_exptl_absorpt_coefficient_mu    3.53
_exptl_absorpt_correction_T_max  0.6119
_exptl_absorpt_correction_T_min  0.4576
_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    1.878
_exptl_crystal_description       plate
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.029
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.09
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         2825
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0211
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0075P)^2^+4.2976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0403
_refine_ls_wR_factor_ref         0.0447
_reflns_number_gt                2065
_reflns_number_total             2825
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic302322r_si_002_1.cif
_cod_data_source_block           1217160_b1_2s
_cod_database_code               4331382