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#$Date: 2024-02-04 13:58:44 +0200 (Sun, 04 Feb 2024) $
#$Revision: 289510 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/47/7714703.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_7714703
loop_
_publ_author_name
'Lundberg, Daniel'
'Lindqvist-Reis, Patric'
'Łyczko, Krzysztof'
'Eriksson, Lars'
'Persson, Ingmar'
_publ_section_title
;
 Coordination chemistry effects of the space-demanding solvent molecule
 N,N'-dimethylpropyleneurea.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1817
_journal_page_last               1832
_journal_paper_doi               10.1039/d3dt03193d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C36 H72 N12 O6 Pr, I, 2(I3)'
_chemical_formula_sum            'C36 H72 I7 N12 O6 Pr'
_chemical_formula_weight         1798.26
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-09-25 deposited with the CCDC.	2023-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   11.6236(18)
_cell_length_b                   11.6236(18)
_cell_length_c                   12.2134(12)
_cell_measurement_reflns_used    3001
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.2976
_cell_measurement_theta_min      3.8701
_cell_volume                     1429.1(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.5467
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Excalibur-III κ diffractometer with Sapphire-3 CCD'
_diffrn_measurement_method       'ω scans at different φ'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0992
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11630
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.269
_diffrn_reflns_theta_min         3.883
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.681
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.090
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             850
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.012
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.00131(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.703
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         2370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.703
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0241
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0150P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0398
_refine_ls_wR_factor_ref         0.0412
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1328
_reflns_number_total             2370
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt03193d2.cif
_cod_data_source_block           Pr_dmpu6_I7
_cod_depositor_comments
'Adding full bibliography for 7714702--7714710.cif.'
_cod_original_cell_volume        1429.1(5)
_cod_database_code               7714703
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.000000 0.000000 0.000000 0.01241(13) Uani 1 6 d S T P . .
I1 I 0.000000 0.000000 0.500000 0.0361(2) Uani 1 6 d S T P . .
I21 I 0.333333 0.666667 0.58379(4) 0.02731(15) Uani 1 3 d S T P . .
I22 I 0.333333 0.666667 1.06001(4) 0.02739(15) Uani 1 3 d S T P . .
I23 I 0.333333 0.666667 0.82288(4) 0.01946(12) Uani 1 3 d S T P . .
O1 O 0.0935(2) -0.0975(2) 0.11004(18) 0.0164(6) Uani 1 1 d . . . . .
C1 C 0.1620(4) -0.1092(3) 0.1852(3) 0.0169(9) Uani 1 1 d . . . . .
N11 N 0.1027(3) -0.1878(3) 0.2715(2) 0.0185(7) Uani 1 1 d . . . . .
N12 N 0.2954(3) -0.0442(3) 0.1772(2) 0.0164(7) Uani 1 1 d . . . . .
C11 C -0.0426(3) -0.2645(4) 0.2790(3) 0.0266(10) Uani 1 1 d . . . . .
H11A H -0.074176 -0.215304 0.323014 0.040 Uiso 1 1 calc R U . . .
H11B H -0.069739 -0.350367 0.313750 0.040 Uiso 1 1 calc R U . . .
H11C H -0.080877 -0.279095 0.205414 0.040 Uiso 1 1 calc R U . . .
C12 C 0.3558(3) 0.0210(4) 0.0743(3) 0.0221(9) Uani 1 1 d . . . . .
H12A H 0.303309 -0.035391 0.013144 0.033 Uiso 1 1 calc R U . . .
H12B H 0.446440 0.035719 0.070172 0.033 Uiso 1 1 calc R U . . .
H12C H 0.358556 0.106506 0.070312 0.033 Uiso 1 1 calc R U . . .
C13 C 0.1771(4) -0.1958(4) 0.3650(3) 0.0268(10) Uani 1 1 d . . . . .
H13A H 0.187473 -0.274908 0.357235 0.032 Uiso 1 1 calc R U . . .
H13B H 0.127199 -0.205594 0.433363 0.032 Uiso 1 1 calc R U . . .
C14 C 0.3106(4) -0.0741(4) 0.3719(3) 0.0217(9) Uani 1 1 d . . . . .
H14A H 0.364383 -0.086213 0.428690 0.026 Uiso 1 1 calc R U . . .
H14B H 0.300835 0.002795 0.392905 0.026 Uiso 1 1 calc R U . . .
C15 C 0.3801(4) -0.0476(4) 0.2630(3) 0.0243(10) Uani 1 1 d . . . . .
H15A H 0.464265 0.038459 0.265557 0.029 Uiso 1 1 calc R U . . .
H15B H 0.401644 -0.118194 0.246962 0.029 Uiso 1 1 calc R U . . .
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'
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'
Pr Pr -0.2180 2.8214 '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 89.56(8) . 5 ?
O1 Pr1 O1 90.44(8) . 2 ?
O1 Pr1 O1 180.00(14) 5 2 ?
O1 Pr1 O1 180.0 . 4 ?
O1 Pr1 O1 90.44(8) 5 4 ?
O1 Pr1 O1 89.56(8) 2 4 ?
O1 Pr1 O1 89.56(8) . 6 ?
O1 Pr1 O1 90.44(8) 5 6 ?
O1 Pr1 O1 89.56(8) 2 6 ?
O1 Pr1 O1 90.44(8) 4 6 ?
O1 Pr1 O1 90.44(8) . 3 ?
O1 Pr1 O1 89.56(8) 5 3 ?
O1 Pr1 O1 90.44(8) 2 3 ?
O1 Pr1 O1 89.56(8) 4 3 ?
O1 Pr1 O1 180.0(2) 6 3 ?
I22 I23 I21 180.0 . . ?
C1 O1 Pr1 159.2(2) . . ?
O1 C1 N11 120.5(3) . . ?
O1 C1 N12 119.8(3) . . ?
N11 C1 N12 119.7(3) . . ?
C1 N11 C13 122.7(3) . . ?
C1 N11 C11 120.5(3) . . ?
C13 N11 C11 116.7(3) . . ?
C1 N12 C15 122.6(3) . . ?
C1 N12 C12 118.4(3) . . ?
C15 N12 C12 118.7(3) . . ?
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(3) . . ?
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 . . ?
C13 C14 C15 110.0(3) . . ?
C13 C14 H14A 109.7 . . ?
C15 C14 H14A 109.7 . . ?
C13 C14 H14B 109.7 . . ?
C15 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
N12 C15 C14 109.9(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 . . ?
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 2.346(2) . ?
Pr1 O1 2.346(2) 5 ?
Pr1 O1 2.346(2) 2 ?
Pr1 O1 2.346(2) 4 ?
Pr1 O1 2.346(2) 6 ?
Pr1 O1 2.346(2) 3 ?
I21 I23 2.9202(7) . ?
I22 I23 2.8961(7) . ?
O1 C1 1.266(4) . ?
C1 N11 1.339(4) . ?
C1 N12 1.346(4) . ?
N11 C13 1.463(4) . ?
N11 C11 1.466(4) . ?
N12 C15 1.452(4) . ?
N12 C12 1.454(4) . ?
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 1.490(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.506(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 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
Pr1 O1 C1 N11 109.5(6) . . . . ?
Pr1 O1 C1 N12 -71.8(7) . . . . ?
O1 C1 N11 C13 -174.5(3) . . . . ?
N12 C1 N11 C13 6.8(5) . . . . ?
O1 C1 N11 C11 1.7(5) . . . . ?
N12 C1 N11 C11 -177.0(3) . . . . ?
O1 C1 N12 C15 176.7(3) . . . . ?
N11 C1 N12 C15 -4.6(5) . . . . ?
O1 C1 N12 C12 -9.6(5) . . . . ?
N11 C1 N12 C12 169.1(3) . . . . ?
C1 N11 C13 C14 22.3(5) . . . . ?
C11 N11 C13 C14 -154.1(3) . . . . ?
N11 C13 C14 C15 -51.4(4) . . . . ?
C1 N12 C15 C14 -26.0(5) . . . . ?
C12 N12 C15 C14 160.3(3) . . . . ?
C13 C14 C15 N12 53.1(4) . . . . ?
