#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:10:54 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179234 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/54/4315472.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_4315472
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 O6 Pr, 3(C6 H12 N2 O), 3(I)'
_chemical_formula_structural     '(Pr (C6 H12 N2 O)6) (C6 H12 N2 O)3 I3'
_chemical_formula_sum            'C54 H108 I3 N18 O9 Pr'
_chemical_formula_weight         1675.19
_chemical_name_common            'hexakis(dmpu)praseodymium(III) iodide'
_chemical_name_systematic
'hexakis[1,3-dimethyltetrahydropyrimidin-2(1H)-one-\kO]praseodymium(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                   13.2345(5)
_cell_length_b                   13.2345(5)
_cell_length_c                   23.2798(12)
_cell_measurement_reflns_used    2022
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.3864
_cell_measurement_theta_min      3.6597
_cell_volume                     3531.2(3)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1851
_diffrn_reflns_av_sigmaI/netI    0.1643
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            23435
_diffrn_reflns_theta_full        25.67
_diffrn_reflns_theta_max         25.67
_diffrn_reflns_theta_min         3.66
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.063
_exptl_absorpt_correction_T_max  0.90000
_exptl_absorpt_correction_T_min  0.7915563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Crysalis RED (Oxford Diffraction, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.00024(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.761
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         2285
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      0.757
_refine_ls_R_factor_all          0.1146
_refine_ls_R_factor_gt           0.0404
_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/[σ²(Fo²)+(0.0140P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0535
_refine_ls_wR_factor_ref         0.0618
_reflns_number_gt                1186
_reflns_number_total             2285
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic100034q_si_002_2.cif
_cod_data_source_block           ccdc_Pr
_cod_database_code               4315472
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 0.6667 0.3333 0.7500 0.0215(3) Uani 1 6 d S . .
I3 I 0.6667 0.3333 0.46351(3) 0.0315(2) Uani 1 3 d S . .
Pr1 Pr 0.0000 0.0000 0.5000 0.0122(2) Uani 1 6 d SU . .
O1 O -0.1358(3) 0.0156(3) 0.55836(15) 0.0180(10) Uani 1 1 d U . .
C1 C -0.1992(5) 0.0532(5) 0.5785(3) 0.0162(13) Uani 1 1 d U . .
N11 N -0.1712(5) 0.1087(5) 0.6296(2) 0.0256(14) Uani 1 1 d U . .
N12 N -0.2926(4) 0.0402(4) 0.5504(2) 0.0218(12) Uani 1 1 d U . .
C11 C -0.0804(5) 0.1095(5) 0.6658(3) 0.0238(15) Uani 1 1 d U . .
H11A H -0.0722 0.1533 0.7011 0.036 Uiso 1 1 calc R . .
H11B H -0.0061 0.1465 0.6449 0.036 Uiso 1 1 calc R . .
H11C H -0.1020 0.0291 0.6756 0.036 Uiso 1 1 calc R . .
C12 C -0.3276(5) -0.0238(5) 0.4967(3) 0.0343(17) Uani 1 1 d U . .
H12A H -0.3969 -0.0240 0.4818 0.051 Uiso 1 1 calc R . .
H12B H -0.3457 -0.1043 0.5033 0.051 Uiso 1 1 calc R . .
H12C H -0.2639 0.0136 0.4688 0.051 Uiso 1 1 calc R . .
C13 C -0.2458(6) 0.1453(7) 0.6580(3) 0.040(2) Uani 1 1 d U . .
H13A H -0.1976 0.2141 0.6825 0.048 Uiso 1 1 calc R . .
H13B H -0.3026 0.0816 0.6829 0.048 Uiso 1 1 calc R . .
C14 C -0.3100(6) 0.1755(6) 0.6146(3) 0.0424(19) Uani 1 1 d U . .
H14A H -0.3675 0.1905 0.6343 0.051 Uiso 1 1 calc R . .
H14B H -0.2543 0.2474 0.5939 0.051 Uiso 1 1 calc R . .
C15 C -0.3713(5) 0.0777(6) 0.5728(3) 0.0294(16) Uani 1 1 d U . .
H15A H -0.4382 0.0112 0.5920 0.035 Uiso 1 1 calc R . .
H15B H -0.4020 0.1034 0.5406 0.035 Uiso 1 1 calc R . .
O2 O 0.6961(5) 0.8996(5) 0.7500 0.0315(17) Uani 1 2 d SU . .
C2 C 0.6240(7) 0.7950(8) 0.7500 0.020(2) Uani 1 2 d SU . .
N21 N 0.5836(5) 0.7338(5) 0.6992(2) 0.0291(14) Uani 1 1 d U . .
C21 C 0.6168(7) 0.7974(7) 0.6459(3) 0.049(2) Uani 1 1 d U . .
H21A H 0.5809 0.7429 0.6138 0.074 Uiso 1 1 calc R . .
H21B H 0.7019 0.8381 0.6420 0.074 Uiso 1 1 calc R . .
H21C H 0.5902 0.8544 0.6457 0.074 Uiso 1 1 calc R . .
C23 C 0.4962(7) 0.6126(6) 0.6981(4) 0.062(3) Uani 1 1 d U . .
H23A H 0.5127 0.5747 0.6656 0.075 Uiso 1 1 calc R . .
H23B H 0.4193 0.6059 0.6909 0.075 Uiso 1 1 calc R . .
C24 C 0.4895(13) 0.5510(10) 0.7500 0.112(6) Uani 1 2 d SU . .
H24A H 0.5538 0.5331 0.7500 0.135 Uiso 1 2 calc SR . .
H24B H 0.4151 0.4758 0.7500 0.135 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'
Pr Pr -0.2180 2.8214 '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 Pr1 O1 90.27(13) 5 7_556 ?
O1 Pr1 O1 180.00(18) 5 11_556 ?
O1 Pr1 O1 89.73(13) 7_556 11_556 ?
O1 Pr1 O1 89.73(13) 5 3 ?
O1 Pr1 O1 90.27(13) 7_556 3 ?
O1 Pr1 O1 90.27(13) 11_556 3 ?
O1 Pr1 O1 89.73(13) 5 . ?
O1 Pr1 O1 180.00(14) 7_556 . ?
O1 Pr1 O1 90.27(13) 11_556 . ?
O1 Pr1 O1 89.73(13) 3 . ?
O1 Pr1 O1 90.27(13) 5 9_556 ?
O1 Pr1 O1 89.73(13) 7_556 9_556 ?
O1 Pr1 O1 89.73(13) 11_556 9_556 ?
O1 Pr1 O1 180.000(1) 3 9_556 ?
O1 Pr1 O1 90.27(13) . 9_556 ?
C1 O1 Pr1 160.3(4) . . ?
O1 C1 N12 121.6(6) . . ?
O1 C1 N11 119.2(6) . . ?
N12 C1 N11 119.2(6) . . ?
C1 N11 C13 122.2(6) . . ?
C1 N11 C11 120.8(5) . . ?
C13 N11 C11 115.3(5) . . ?
C1 N12 C12 120.3(5) . . ?
C1 N12 C15 123.8(5) . . ?
C12 N12 C15 115.7(5) . . ?
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 110.6(6) . . ?
N11 C13 H13A 109.5 . . ?
C14 C13 H13A 109.5 . . ?
N11 C13 H13B 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
C15 C14 C13 110.0(6) . . ?
C15 C14 H14A 109.7 . . ?
C13 C14 H14A 109.7 . . ?
C15 C14 H14B 109.7 . . ?
C13 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
N12 C15 C14 111.0(5) . . ?
N12 C15 H15A 109.4 . . ?
C14 C15 H15A 109.4 . . ?
N12 C15 H15B 109.4 . . ?
C14 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
O2 C2 N21 121.1(4) . . ?
O2 C2 N21 121.1(4) . 10_557 ?
N21 C2 N21 117.8(9) . 10_557 ?
C2 N21 C23 122.1(6) . . ?
C2 N21 C21 118.7(6) . . ?
C23 N21 C21 118.5(6) . . ?
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 C23 C24 114.0(8) . . ?
N21 C23 H23A 108.8 . . ?
C24 C23 H23A 108.8 . . ?
N21 C23 H23B 108.8 . . ?
C24 C23 H23B 108.8 . . ?
H23A C23 H23B 107.7 . . ?
C23 C24 C23 114.7(12) . 10_557 ?
C23 C24 H24A 108.6 . . ?
C23 C24 H24A 108.6 10_557 . ?
C23 C24 H24B 108.6 . . ?
C23 C24 H24B 108.6 10_557 . ?
H24A C24 H24B 107.6 . . ?
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
Pr1 O1 2.342(4) 5 ?
Pr1 O1 2.342(4) 7_556 ?
Pr1 O1 2.342(4) 11_556 ?
Pr1 O1 2.342(4) 3 ?
Pr1 O1 2.342(4) . ?
Pr1 O1 2.342(4) 9_556 ?
O1 C1 1.261(6) . ?
C1 N12 1.332(7) . ?
C1 N11 1.349(7) . ?
N11 C13 1.457(8) . ?
N11 C11 1.463(7) . ?
N12 C12 1.449(8) . ?
N12 C15 1.456(7) . ?
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 1.497(9) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.494(8) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
O2 C2 1.227(9) . ?
C2 N21 1.381(7) . ?
C2 N21 1.381(7) 10_557 ?
N21 C23 1.434(8) . ?
N21 C21 1.439(8) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C23 C24 1.436(10) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C23 1.436(10) 10_557 ?
C24 H24A 0.9900 . ?
C24 H24B 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 Pr1 O1 C1 84.6(12) 5 . . . ?
O1 Pr1 O1 C1 -95.4(12) 11_556 . . . ?
O1 Pr1 O1 C1 174.3(11) 3 . . . ?
O1 Pr1 O1 C1 -5.7(11) 9_556 . . . ?
Pr1 O1 C1 N12 72.5(13) . . . . ?
Pr1 O1 C1 N11 -107.1(11) . . . . ?
O1 C1 N11 C13 -174.4(6) . . . . ?
N12 C1 N11 C13 6.0(9) . . . . ?
O1 C1 N11 C11 -9.7(8) . . . . ?
N12 C1 N11 C11 170.7(5) . . . . ?
O1 C1 N12 C12 3.3(8) . . . . ?
N11 C1 N12 C12 -177.1(5) . . . . ?
O1 C1 N12 C15 177.4(5) . . . . ?
N11 C1 N12 C15 -3.0(8) . . . . ?
C1 N11 C13 C14 -31.5(9) . . . . ?
C11 N11 C13 C14 163.1(6) . . . . ?
N11 C13 C14 C15 52.2(8) . . . . ?
C1 N12 C15 C14 25.9(8) . . . . ?
C12 N12 C15 C14 -159.7(6) . . . . ?
C13 C14 C15 N12 -49.5(7) . . . . ?
O2 C2 N21 C23 -177.7(7) . . . . ?
N21 C2 N21 C23 4.6(12) 10_557 . . . ?
O2 C2 N21 C21 -7.4(11) . . . . ?
N21 C2 N21 C21 174.8(5) 10_557 . . . ?
C2 N21 C23 C24 -24.0(12) . . . . ?
C21 N21 C23 C24 165.7(10) . . . . ?
N21 C23 C24 C23 43.1(17) . . . 10_557 ?
