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#$Date: 2025-08-20 23:21:57 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301837 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/54/4315473.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4315473
loop_
_publ_author_name
'Daniel Lundberg'
'Ingmar Persson'
'Lars Eriksson'
'Paola D'Angelo'
'Simone de Panfilis'
_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       'ω scans at different φ'
_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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0361P)²+5.3924P] where P=(Fo²+2Fc²)/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>2σ(I)
_cod_data_source_file            ic100034q_si_002_3.cif
_cod_data_source_block           ccdc_Nd
_cod_database_code               4315473
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.3333 0.6667 0.2500 0.01966(10) Uani 1 6 d S . .
I2 I 0.3333 0.6667 0.536343(13) 0.03117(10) Uani 1 3 d S . .
Nd1 Nd 0.0000 1.0000 0.5000 0.00950(7) Uani 1 6 d S . .
O1 O 0.14988(15) 1.01535(16) 0.55775(7) 0.0175(3) Uani 1 1 d . . .
C1 C 0.2520(2) 1.0538(2) 0.57890(10) 0.0165(4) Uani 1 1 d . . .
N11 N 0.2790(2) 1.1094(2) 0.62987(9) 0.0216(4) Uani 1 1 d . . .
N12 N 0.3321(2) 1.0410(2) 0.54975(9) 0.0214(4) Uani 1 1 d . . .
C11 C 0.1885(3) 1.1092(3) 0.66541(11) 0.0256(6) Uani 1 1 d . . .
H11A H 0.2236 1.1543 0.7005 0.038 Uiso 1 1 calc R . .
H11B H 0.1308 1.0287 0.6757 0.038 Uiso 1 1 calc R . .
H11C H 0.1501 1.1444 0.6440 0.038 Uiso 1 1 calc R . .
C12 C 0.3023(3) 0.9761(3) 0.49588(13) 0.0339(7) Uani 1 1 d . . .
H12A H 0.3712 0.9760 0.4806 0.051 Uiso 1 1 calc R . .
H12B H 0.2753 1.0131 0.4680 0.051 Uiso 1 1 calc R . .
H12C H 0.2401 0.8956 0.5027 0.051 Uiso 1 1 calc R . .
C13 C 0.3903(3) 1.1458(3) 0.65839(12) 0.0367(8) Uani 1 1 d . . .
H13A H 0.3831 1.0821 0.6835 0.044 Uiso 1 1 calc R . .
H13B H 0.4112 1.2148 0.6828 0.044 Uiso 1 1 calc R . .
C14 C 0.4850(3) 1.1756(4) 0.61437(13) 0.0406(9) Uani 1 1 d . . .
H14A H 0.5005 1.2468 0.5932 0.049 Uiso 1 1 calc R . .
H14B H 0.5579 1.1914 0.6340 0.049 Uiso 1 1 calc R . .
C15 C 0.4482(2) 1.0761(3) 0.57288(13) 0.0315(7) Uani 1 1 d . . .
H15A H 0.5053 1.1004 0.5410 0.038 Uiso 1 1 calc R . .
H15B H 0.4466 1.0092 0.5928 0.038 Uiso 1 1 calc R . .
O2 O 0.1000(3) 0.3047(3) 0.7500 0.0322(7) Uani 1 2 d S . .
C2 C 0.2053(3) 0.3759(3) 0.7500 0.0224(7) Uani 1 2 d S . .
N21 N 0.2656(2) 0.4161(2) 0.69982(11) 0.0322(6) Uani 1 1 d . . .
C21 C 0.2013(4) 0.3851(3) 0.64582(13) 0.0481(10) Uani 1 1 d . . .
H21A H 0.2562 0.4199 0.6138 0.072 Uiso 1 1 calc R . .
H21B H 0.1465 0.4145 0.6458 0.072 Uiso 1 1 calc R . .
H21C H 0.1582 0.3000 0.6416 0.072 Uiso 1 1 calc R . .
C22 C 0.3886(4) 0.5037(4) 0.6978(2) 0.0589(12) Uani 1 1 d . . .
H22A H 0.3964 0.5814 0.6920 0.071 Uiso 1 1 calc R . .
H22B H 0.4251 0.4878 0.6645 0.071 Uiso 1 1 calc R . .
C23 C 0.4507(5) 0.5061(7) 0.7500 0.087(3) Uani 1 2 d S . .
H23A H 0.5284 0.5775 0.7500 0.104 Uiso 1 2 calc SR . .
H23B H 0.4627 0.4380 0.7500 0.104 Uiso 1 2 calc SR . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Nd1 O1 89.81(6) 7_576 9_456 ?
O1 Nd1 O1 180.0 7_576 . ?
O1 Nd1 O1 90.19(6) 9_456 . ?
O1 Nd1 O1 90.19(6) 7_576 5_465 ?
O1 Nd1 O1 90.19(6) 9_456 5_465 ?
O1 Nd1 O1 89.81(6) . 5_465 ?
O1 Nd1 O1 90.19(6) 7_576 3_675 ?
O1 Nd1 O1 180.00(7) 9_456 3_675 ?
O1 Nd1 O1 89.81(6) . 3_675 ?
O1 Nd1 O1 89.81(6) 5_465 3_675 ?
O1 Nd1 O1 89.81(6) 7_576 11_666 ?
O1 Nd1 O1 89.81(6) 9_456 11_666 ?
O1 Nd1 O1 90.19(6) . 11_666 ?
O1 Nd1 O1 180.00(9) 5_465 11_666 ?
O1 Nd1 O1 90.19(6) 3_675 11_666 ?
C1 O1 Nd1 160.73(16) . . ?
O1 C1 N12 120.0(2) . . ?
O1 C1 N11 119.6(2) . . ?
N12 C1 N11 120.3(2) . . ?
C1 N11 C11 120.4(2) . . ?
C1 N11 C13 121.9(2) . . ?
C11 N11 C13 115.9(2) . . ?
C1 N12 C12 120.7(2) . . ?
C1 N12 C15 123.0(2) . . ?
C12 N12 C15 115.8(2) . . ?
N11 C11 H11A 109.5 . . ?
N11 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N11 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N12 C12 H12A 109.5 . . ?
N12 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N12 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N11 C13 C14 110.3(2) . . ?
N11 C13 H13A 109.6 . . ?
C14 C13 H13A 109.6 . . ?
N11 C13 H13B 109.6 . . ?
C14 C13 H13B 109.6 . . ?
H13A C13 H13B 108.1 . . ?
C15 C14 C13 110.1(3) . . ?
C15 C14 H14A 109.6 . . ?
C13 C14 H14A 109.6 . . ?
C15 C14 H14B 109.6 . . ?
C13 C14 H14B 109.6 . . ?
H14A C14 H14B 108.2 . . ?
N12 C15 C14 110.0(3) . . ?
N12 C15 H15A 109.7 . . ?
C14 C15 H15A 109.7 . . ?
N12 C15 H15B 109.7 . . ?
C14 C15 H15B 109.7 . . ?
H15A C15 H15B 108.2 . . ?
O2 C2 N21 121.08(18) . 10_557 ?
O2 C2 N21 121.08(18) . . ?
N21 C2 N21 117.8(4) 10_557 . ?
C2 N21 C22 122.9(3) . . ?
C2 N21 C21 118.9(3) . . ?
C22 N21 C21 117.5(3) . . ?
N21 C21 H21A 109.5 . . ?
N21 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N21 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N21 C22 C23 112.7(4) . . ?
N21 C22 H22A 109.1 . . ?
C23 C22 H22A 109.1 . . ?
N21 C22 H22B 109.1 . . ?
C23 C22 H22B 109.1 . . ?
H22A C22 H22B 107.8 . . ?
C22 C23 C22 112.8(6) . 10_557 ?
C22 C23 H23A 109.0 . . ?
C22 C23 H23A 109.0 10_557 . ?
C22 C23 H23B 109.0 . . ?
C22 C23 H23B 109.0 10_557 . ?
H23A C23 H23B 107.8 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 O1 2.3189(17) 7_576 ?
Nd1 O1 2.3189(16) 9_456 ?
Nd1 O1 2.3189(17) . ?
Nd1 O1 2.3189(17) 5_465 ?
Nd1 O1 2.3189(16) 3_675 ?
Nd1 O1 2.3189(17) 11_666 ?
O1 C1 1.280(3) . ?
C1 N12 1.339(3) . ?
C1 N11 1.346(3) . ?
N11 C11 1.454(4) . ?
N11 C13 1.461(3) . ?
N12 C12 1.458(4) . ?
N12 C15 1.467(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.510(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.503(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
O2 C2 1.231(5) . ?
C2 N21 1.363(3) 10_557 ?
C2 N21 1.363(3) . ?
N21 C22 1.452(5) . ?
N21 C21 1.456(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.457(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C22 1.457(6) 10_557 ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Nd1 O1 C1 97.7(5) 9_456 . . . ?
O1 Nd1 O1 C1 -172.1(5) 5_465 . . . ?
O1 Nd1 O1 C1 -82.3(5) 3_675 . . . ?
O1 Nd1 O1 C1 7.9(5) 11_666 . . . ?
Nd1 O1 C1 N12 -73.8(6) . . . . ?
Nd1 O1 C1 N11 104.7(5) . . . . ?
O1 C1 N11 C11 10.3(4) . . . . ?
N12 C1 N11 C11 -171.3(2) . . . . ?
O1 C1 N11 C13 174.5(3) . . . . ?
N12 C1 N11 C13 -7.1(4) . . . . ?
O1 C1 N12 C12 -4.5(4) . . . . ?
N11 C1 N12 C12 177.1(3) . . . . ?
O1 C1 N12 C15 -176.0(3) . . . . ?
N11 C1 N12 C15 5.5(4) . . . . ?
C1 N11 C13 C14 31.5(4) . . . . ?
C11 N11 C13 C14 -163.7(3) . . . . ?
N11 C13 C14 C15 -52.9(4) . . . . ?
C1 N12 C15 C14 -28.6(4) . . . . ?
C12 N12 C15 C14 159.5(3) . . . . ?
C13 C14 C15 N12 51.2(4) . . . . ?
O2 C2 N21 C22 177.3(4) . . . . ?
N21 C2 N21 C22 -3.4(6) 10_557 . . . ?
O2 C2 N21 C21 7.6(6) . . . . ?
N21 C2 N21 C21 -173.1(3) 10_557 . . . ?
C2 N21 C22 C23 25.3(6) . . . . ?
C21 N21 C22 C23 -164.8(5) . . . . ?
N21 C22 C23 C22 -46.3(8) . . . 10_557 ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139131992
