Structural Study of the N,N'-Dimethylpropyleneurea Solvated Lanthanoid(III) Ions in Solution and Solid State with an Analysis of the Ionic Radii of Lanthanoid(III) Ions
Daniel Lundberg; Ingmar Persson; Lars Eriksson; Paola D'Angelo; Simone de Panfilis; Inorganic Chemistry 49 (2010) 4420–4432; doi:10.1021/ic100034q

data_4315471
_publ_contact_author_address
;Swedish University of Agricultural Sciences (SLU)
Dept. of Chemistry
P.O. Box 7015
S-750 07 Uppsala
Sweden
;
_publ_contact_author_email       daniel.lundberg@kemi.slu.se
_publ_contact_author_fax         +46-18-673476
_publ_contact_author_name        'Daniel Lundberg'
_publ_contact_author_phone       +46-18-671568
_publ_section_title
;
 Structural Study of the N,N'-Dimethylpropyleneurea Solvated
 Lanthanoid(III) Ions in Solution and Solid State with an Analysis of the
 Ionic Radii of Lanthanoid(III) Ions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4420
_journal_page_last               4432
_journal_paper_doi               10.1021/ic100034q
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C36 H72 La N12 O6, 3(C6 H12 N2 O), 3(I)'
_chemical_formula_structural     '(La (C6 H12 N2 O)6) (C6 H12 N2 O)3 I3'
_chemical_formula_sum            'C54 H108 I3 La N18 O9'
_chemical_formula_weight         1673.19
_chemical_name_common            'hexakis(dmpu)lanthanum(III) iodide'
_chemical_name_systematic
'hexakis[1,3-dimethyltetrahydropyrimidin-2(1H)-one-\kO]lanthanum(III) iodide'
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      176
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.000(10)
_cell_formula_units_Z            2
_cell_length_a                   13.33(1)
_cell_length_b                   13.33(1)
_cell_length_c                   23.32(1)
_cell_measurement_reflns_used    11255
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.88
_cell_measurement_theta_min      2.70
_cell_volume                     3589(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 12.65
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  MARCCD
_diffrn_measurement_method       '\f scan'
_diffrn_radiation_monochromator  silicon(111)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'I711, Maxlab'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.08700
_diffrn_reflns_av_R_equivalents  0.063
_diffrn_reflns_av_sigmaI/netI    0.1047
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10280
_diffrn_reflns_theta_full        31.88
_diffrn_reflns_theta_max         31.88
_diffrn_reflns_theta_min         2.70
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.982
_exptl_absorpt_correction_T_max  0.550
_exptl_absorpt_correction_T_min  0.171
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
'XABS2 (Parkin, S., Moezzi, B. and Hope H.  J. Appl. Cryst. (1995). 28, 53-56)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1692
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.066
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         1174
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+6.8050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1375
_reflns_number_gt                1158
_reflns_number_total             1174
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic100034q_si_002_1.cif
_cod_data_source_block           ccdc_La
_cod_database_code               4315471