#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/67/2216731.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2216731
loop_
_publ_author_name
'Ludmila Yu. Alikberova'
'Dmitry V. Albov'
'Denis V. Golubev'
'Valery V. Kravchenko'
'Nataliya S. Rukk'
_publ_section_title
;
 Tetraaquatetraureaneodymium(III) triiodide
;
_journal_coeditor_code           RK2058
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m3078
_journal_page_last               m3078
_journal_paper_doi               10.1107/S1600536807058643
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Nd (C1 H4 N2 O1)4 (H2 O1)4] I3'
_chemical_formula_moiety         'C4 H24 N8 Nd O8 3+, 3(I -)'
_chemical_formula_sum            'C4 H24 I3 N8 Nd O8'
_chemical_formula_weight         837.25
_chemical_melting_point          371
_chemical_name_systematic
;
Tetraaquatetraureaneodymium(III) triiodide
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.136(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.7633(19)
_cell_length_b                   10.597(4)
_cell_length_c                   15.140(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      14
_cell_volume                     1183.7(6)
_computing_cell_refinement       'CAD-4 Express (Enraf--Nonius, 1994)'
_computing_data_collection       'CAD-4 Express (Enraf--Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'κ--geometry diffractometer'
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       'non--profiled ω--scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine--focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            3446
_diffrn_reflns_theta_full        29.96
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  120
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    6.145
_exptl_absorpt_correction_T_max  0.304
_exptl_absorpt_correction_T_min  0.293
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
(North et al.,  1968)
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    2.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             774
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.731
_refine_diff_density_min         -0.548
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         3446
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0298P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0696
_reflns_number_gt                2589
_reflns_number_total             3446
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            rk2058.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               2216731
_cod_database_fobs_code          2216731
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Nd Nd1 0.5000 0.15416(3) 0.2500 0.03067(8) Uani d S 1
I I1 0.0000 0.53143(5) 0.2500 0.05980(15) Uani d S 1
I I2 0.82533(5) 0.78527(3) 0.49371(3) 0.05522(11) Uani d . 1
O O1 0.3857(6) 0.3168(4) 0.1427(3) 0.0869(14) Uani d . 1
C C1 0.3636(7) 0.4170(5) 0.0989(4) 0.0535(13) Uani d . 1
N N11 0.2203(6) 0.4292(5) 0.0241(4) 0.0677(13) Uani d . 1
H H11A 0.1446 0.3680 0.0067 0.081 Uiso calc R 1
H H11B 0.2030 0.4984 -0.0072 0.081 Uiso calc R 1
N N12 0.4807(7) 0.5126(5) 0.1217(4) 0.0891(19) Uani d . 1
H H12A 0.5769 0.5061 0.1688 0.107 Uiso calc R 1
H H12B 0.4600 0.5807 0.0892 0.107 Uiso calc R 1
O O2 0.4141(5) -0.0102(3) 0.3359(3) 0.0595(10) Uani d . 1
C C2 0.3219(7) -0.1020(6) 0.3391(5) 0.0649(16) Uani d . 1
N N21 0.2945(10) -0.1930(6) 0.2739(5) 0.121(3) Uani d . 1
H H21A 0.3421 -0.1863 0.2299 0.145 Uiso calc R 1
H H21B 0.2293 -0.2578 0.2764 0.145 Uiso calc R 1
N N22 0.2716(12) -0.1279(7) 0.4085(6) 0.165(4) Uani d . 1
H H22A 0.3023 -0.0796 0.4565 0.198 Uiso calc R 1
H H22B 0.2065 -0.1938 0.4078 0.198 Uiso calc R 1
O O3 0.2249(5) 0.2324(4) 0.2831(3) 0.0635(10) Uani d D 1
H H3A 0.179 0.303 0.262 0.076 Uiso calc R 1
H H3B 0.207 0.225 0.3356 0.076 Uiso calc R 1
O O4 0.2283(5) 0.0663(4) 0.1314(3) 0.0709(12) Uani d D 1
H H4A 0.131 0.107 0.105 0.085 Uiso calc R 1
H H4B 0.209 -0.008 0.109 0.085 Uiso calc R 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Nd1 0.03188(14) 0.02026(13) 0.03909(17) 0.000 0.00991(12) 0.000
I1 0.0509(3) 0.0385(2) 0.0817(4) 0.000 0.0085(2) 0.000
I2 0.0559(2) 0.03773(17) 0.0624(2) 0.00232(14) 0.00431(16) 0.00285(15)
O1 0.083(3) 0.062(3) 0.113(4) 0.021(2) 0.027(3) 0.057(3)
C1 0.052(3) 0.042(3) 0.068(3) 0.010(2) 0.020(3) 0.023(3)
N11 0.059(3) 0.055(3) 0.081(3) -0.005(2) 0.009(3) 0.020(3)
N12 0.064(3) 0.064(3) 0.108(4) -0.012(3) -0.018(3) 0.030(3)
O2 0.0502(19) 0.048(2) 0.077(3) -0.0097(16) 0.0149(18) 0.0219(19)
C2 0.056(3) 0.049(3) 0.087(4) -0.006(3) 0.020(3) 0.025(3)
N21 0.152(7) 0.087(5) 0.120(6) -0.049(5) 0.039(5) -0.008(4)
N22 0.234(10) 0.125(7) 0.209(10) -0.068(6) 0.175(9) -0.025(6)
O3 0.063(2) 0.053(2) 0.086(3) 0.0198(19) 0.039(2) 0.016(2)
O4 0.056(2) 0.053(2) 0.079(3) 0.0128(18) -0.0164(19) -0.027(2)
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'
I I -0.4742 1.8119 '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'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-2 5 -5
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Nd1 O1 2_655 . 85.4(3)
O1 Nd1 O2 2_655 . 105.55(16)
O1 Nd1 O2 . . 143.45(14)
O1 Nd1 O2 . 2_655 105.55(16)
O2 Nd1 O2 . 2_655 86.4(2)
O1 Nd1 O3 . 2_655 77.19(16)
O2 Nd1 O3 . 2_655 139.17(13)
O1 Nd1 O3 . . 74.39(15)
O2 Nd1 O3 . . 74.34(13)
O2 Nd1 O3 2_655 . 139.17(13)
O3 Nd1 O3 2_655 . 140.99(19)
O1 Nd1 O4 2_655 . 145.93(14)
O1 Nd1 O4 . . 73.87(16)
O2 Nd1 O4 . . 78.60(15)
O2 Nd1 O4 2_655 . 69.62(12)
O3 Nd1 O4 2_655 . 124.67(16)
O3 Nd1 O4 . . 71.41(15)
O1 Nd1 O4 . 2_655 145.93(14)
O2 Nd1 O4 . 2_655 69.62(12)
O3 Nd1 O4 . 2_655 124.67(16)
O4 Nd1 O4 . 2_655 136.01(18)
C1 O1 Nd1 . . 164.4(4)
O1 C1 N11 . . 118.9(5)
O1 C1 N12 . . 123.0(5)
N11 C1 N12 . . 118.1(5)
C1 N11 H11A . . 120.0
C1 N11 H11B . . 120.0
H11A N11 H11B . . 120.0
C1 N12 H12A . . 120.0
C1 N12 H12B . . 120.0
H12A N12 H12B . . 120.0
C2 O2 Nd1 . . 150.6(4)
O2 C2 N22 . . 123.1(8)
O2 C2 N21 . . 120.2(6)
N22 C2 N21 . . 115.8(7)
C2 N21 H21A . . 120.0
C2 N21 H21B . . 120.0
H21A N21 H21B . . 120.0
C2 N22 H22A . . 120.0
C2 N22 H22B . . 120.0
H22A N22 H22B . . 120.0
Nd1 O3 H3A . . 121
Nd1 O3 H3B . . 124
H3A O3 H3B . . 105.1
Nd1 O4 H4A . . 125
Nd1 O4 H4B . . 130
H4A O4 H4B . . 105.2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Nd1 O1 2_655 2.345(4)
Nd1 O1 . 2.345(4)
Nd1 O2 . 2.389(3)
Nd1 O2 2_655 2.389(3)
Nd1 O3 2_655 2.484(3)
Nd1 O3 . 2.484(3)
Nd1 O4 . 2.487(3)
Nd1 O4 2_655 2.487(3)
O1 C1 . 1.235(6)
C1 N11 . 1.324(7)
C1 N12 . 1.333(7)
N11 H11A . 0.8600
N11 H11B . 0.8600
N12 H12A . 0.8600
N12 H12B . 0.8600
O2 C2 . 1.218(6)
C2 N22 . 1.259(9)
C2 N21 . 1.348(9)
N21 H21A . 0.8600
N21 H21B . 0.8600
N22 H22A . 0.8600
N22 H22B . 0.8600
O3 H3A . 0.8500
O3 H3B . 0.8500
O4 H4A . 0.8500
O4 H4B . 0.8500
