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_4315473
_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       +46-18-671549
_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 N12 Nd O6, 3(C6 H12 N2 O), 3(I)'
_chemical_formula_structural     '(Nd (C6 H12 N2 O)6) (C6 H12 N2 O)3 I3'
_chemical_formula_sum            'C54 H108 I3 N18 Nd O9'
_chemical_formula_weight         1678.52
_chemical_name_common            'hexakis(dmpu)neodymium(III) iodide'
_chemical_name_systematic
'hexakis[1,3-dimethyltetrahydropyrimidin-2(1H)-one-\kO]neodymium(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                120.00
_cell_formula_units_Z            2
_cell_length_a                   13.2344(3)
_cell_length_b                   13.2344(3)
_cell_length_c                   23.2595(3)
_cell_measurement_reflns_used    23594
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.7318
_cell_measurement_theta_min      3.9153
_cell_volume                     3528.09(12)
_computing_cell_refinement       'Crysalis RED (Oxford diffraction, 2008)'
_computing_data_collection       'Crysalis CCD (Oxford diffraction, 2008)'
_computing_data_reduction        'Crysalis RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.5467
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'GONIOMETER OXFORD DIFFRACTION KM4 XCALIBUR2'
_diffrn_measurement_method       '\w scans at different \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            37448
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         3.93
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.110
_exptl_absorpt_correction_T_max  0.82817
_exptl_absorpt_correction_T_min  0.80031
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Crysalis RED (Oxford Diffraction, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1698
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.018
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.00221(19)
_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   1.177
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         3661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+5.3924P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0752
_reflns_number_gt                3174
_reflns_number_total             3661
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic100034q_si_002_3.cif
_cod_data_source_block           ccdc_Nd
_cod_database_code               4315473