#------------------------------------------------------------------------------
#$Date: 2025-08-19 21:17:10 +0300 (Tue, 19 Aug 2025) $
#$Revision: 301807 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/03/2240305.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_2240305
loop_
_publ_author_name
'Kawasaki, Takeshi'
'Kitazawa, Takafumi'
_publ_section_title
;
 Crystal structure of
 dioxidobis(pentane-2,4-dionato-κ²O,O')[1-phenyl-3-(pyridin-4-yl)propane-κN]uranium(VI)
;
_journal_coeditor_code           CQ2012
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              42
_journal_page_last               44
_journal_paper_doi               10.1107/S2056989014026607
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[U (C5 H7 O2)2 O2 (C14 H15 N)]'
_chemical_formula_moiety         'C24 H29 N O6 U'
_chemical_formula_sum            'C24 H29 N O6 U'
_chemical_formula_weight         665.51
_chemical_name_systematic
Dioxidobis(pentane-2,4-dionato-κ²O,O')[1-phenyl-3-(pyridin-4-yl)propane-κN]uranium(VI)
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.67(3)
_cell_angle_beta                 98.50(3)
_cell_angle_gamma                100.81(3)
_cell_formula_units_Z            2
_cell_length_a                   8.2100(16)
_cell_length_b                   11.530(2)
_cell_length_c                   14.516(3)
_cell_measurement_reflns_used    4311
_cell_measurement_temperature    297
_cell_measurement_theta_max      28.5
_cell_measurement_theta_min      2.59
_cell_volume                     1246.4(5)
_computing_cell_refinement
;
SAINT (Bruker, 2007) and XSCANS (Bruker, 2007)
;
_computing_data_collection
;
APEX2 (Bruker, 2007) and XSCANS (Bruker, 2007)
;
_computing_data_reduction
;
APEX2 (Bruker, 2007) and SAINT (Bruker, 2007)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and ORTEP-3 for Windows (Farrugia,
2012)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      297
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       '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  0.0149
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9353
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.89
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    6.548
_exptl_absorpt_correction_T_max  0.2808
_exptl_absorpt_correction_T_min  0.1488
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(XPREP; Bruker, 2007)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.883
_refine_diff_density_min         -0.643
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         6948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0257P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0539
_refine_ls_wR_factor_ref         0.0560
_reflns_number_gt                6026
_reflns_number_total             6948
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cq2012sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        1246.4(4)
_cod_database_code               2240305
_cod_database_fobs_code          2240305
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_symmetry_multiplicity
U U1 0.488854(15) 0.690915(11) 0.372080(8) 0.03519(4) Uani d . 1 1
O O1 0.3391(3) 0.5504(2) 0.3581(2) 0.0535(6) Uani d . 1 1
O O2 0.6386(3) 0.8327(2) 0.38786(19) 0.0525(6) Uani d . 1 1
O O3 0.6977(3) 0.6473(3) 0.47398(18) 0.0566(7) Uani d . 1 1
O O4 0.6471(3) 0.5741(2) 0.27211(18) 0.0521(6) Uani d . 1 1
O O5 0.3569(4) 0.6784(3) 0.21310(17) 0.0579(7) Uani d . 1 1
O O6 0.2846(3) 0.8105(3) 0.38825(18) 0.0567(7) Uani d . 1 1
N N1 0.4613(4) 0.7730(3) 0.55740(19) 0.0397(6) Uani d . 1 1
C C1 0.9705(6) 0.6794(5) 0.5706(3) 0.0810(14) Uani d . 1 1
H H1A 0.9878 0.7680 0.6071 0.121 Uiso calc R 1 1
H H1B 1.0774 0.6618 0.5601 0.121 Uiso calc R 1 1
H H1C 0.9231 0.6316 0.6080 0.121 Uiso calc R 1 1
C C2 0.8488(5) 0.6426(3) 0.4705(3) 0.0493(9) Uani d . 1 1
C C3 0.9047(5) 0.6043(4) 0.3827(3) 0.0573(10) Uani d . 1 1
H H3 1.0188 0.6043 0.3872 0.069 Uiso calc R 1 1
C C4 0.8004(5) 0.5661(3) 0.2886(3) 0.0497(9) Uani d . 1 1
C C5 0.8646(7) 0.5049(5) 0.1981(4) 0.0757(14) Uani d . 1 1
H H5A 0.7867 0.4249 0.1584 0.114 Uiso calc R 1 1
H H5B 0.9744 0.4920 0.2186 0.114 Uiso calc R 1 1
H H5C 0.8738 0.5586 0.1595 0.114 Uiso calc R 1 1
C C6 0.2066(7) 0.6847(5) 0.0645(3) 0.0796(15) Uani d . 1 1
H H6A 0.3049 0.7172 0.0433 0.119 Uiso calc R 1 1
H H6B 0.1140 0.7170 0.0434 0.119 Uiso calc R 1 1
H H6C 0.1752 0.5940 0.0354 0.119 Uiso calc R 1 1
C C7 0.2466(5) 0.7251(4) 0.1764(3) 0.0496(9) Uani d . 1 1
C C8 0.1637(5) 0.8067(4) 0.2321(3) 0.0560(10) Uani d . 1 1
H H8 0.0878 0.8375 0.1980 0.067 Uiso calc R 1 1
C C9 0.1856(4) 0.8459(3) 0.3350(3) 0.0473(8) Uani d . 1 1
C C10 0.0891(6) 0.9354(4) 0.3879(3) 0.0670(12) Uani d . 1 1
H H10A -0.0194 0.8881 0.3894 0.101 Uiso calc R 1 1
H H10B 0.0723 0.9919 0.3531 0.101 Uiso calc R 1 1
H H10C 0.1526 0.9833 0.4549 0.101 Uiso calc R 1 1
C C11 0.4545(5) 0.6962(3) 0.6101(3) 0.0449(8) Uani d . 1 1
H H11 0.4583 0.6129 0.5791 0.054 Uiso calc R 1 1
C C12 0.4422(5) 0.7361(4) 0.7083(3) 0.0479(8) Uani d . 1 1
H H12 0.4371 0.6798 0.7421 0.058 Uiso calc R 1 1
C C13 0.4373(4) 0.8594(3) 0.7568(2) 0.0434(8) Uani d . 1 1
C C14 0.4484(5) 0.9381(3) 0.7028(3) 0.0476(8) Uani d . 1 1
H H14 0.4501 1.0227 0.7333 0.057 Uiso calc R 1 1
C C15 0.4570(5) 0.8929(3) 0.6042(3) 0.0470(8) Uani d . 1 1
H H15 0.4599 0.9474 0.5688 0.056 Uiso calc R 1 1
C C16 0.4135(6) 0.9028(4) 0.8628(3) 0.0576(10) Uani d . 1 1
H H16A 0.4701 0.9919 0.8956 0.069 Uiso calc R 1 1
H H16B 0.4675 0.8568 0.8984 0.069 Uiso calc R 1 1
C C17 0.2268(6) 0.8831(4) 0.8692(3) 0.0586(10) Uani d . 1 1
H H17A 0.1655 0.7980 0.8253 0.070 Uiso calc R 1 1
H H17B 0.2195 0.8901 0.9367 0.070 Uiso calc R 1 1
C C18 0.1404(5) 0.9765(4) 0.8412(3) 0.0536(9) Uani d . 1 1
H H18A 0.1565 0.9747 0.7759 0.064 Uiso calc R 1 1
H H18B 0.0192 0.9492 0.8361 0.064 Uiso calc R 1 1
C C19 0.2056(5) 1.1116(4) 0.9144(3) 0.0488(8) Uani d . 1 1
C C20 0.1846(6) 1.1420(4) 1.0114(3) 0.0621(11) Uani d . 1 1
H H20 0.1317 1.0788 1.0318 0.075 Uiso calc R 1 1
C C21 0.2424(6) 1.2672(5) 1.0796(3) 0.0750(14) Uani d . 1 1
H H21 0.2255 1.2868 1.1442 0.090 Uiso calc R 1 1
C C22 0.3239(6) 1.3604(5) 1.0503(4) 0.0772(14) Uani d . 1 1
H H22 0.3654 1.4431 1.0952 0.093 Uiso calc R 1 1
C C23 0.3428(7) 1.3292(5) 0.9534(4) 0.0796(14) Uani d . 1 1
H H23 0.3952 1.3923 0.9328 0.096 Uiso calc R 1 1
C C24 0.2867(6) 1.2082(4) 0.8869(3) 0.0627(11) Uani d . 1 1
H H24 0.3030 1.1900 0.8222 0.075 Uiso calc R 1 1
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'
U U -9.6767 9.6646 '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_publ_flag
O1 U1 O2 179.19(11) y
O1 U1 O3 91.86(12) ?
O1 U1 O4 91.38(11) ?
O1 U1 O5 89.82(12) ?
O1 U1 O6 92.85(12) ?
O2 U1 O3 87.91(12) ?
O2 U1 O4 89.27(11) ?
O2 U1 O5 90.77(12) ?
O2 U1 O6 86.82(11) ?
O3 U1 O4 70.88(9) y
O3 U1 O5 149.99(9) ?
O3 U1 O6 138.83(9) y
O4 U1 O5 79.13(9) y
O4 U1 O6 149.71(9) ?
O5 U1 O6 70.91(9) y
O1 U1 N1 86.45(11) y
O2 U1 N1 92.74(11) y
O3 U1 N1 69.37(9) y
O4 U1 N1 140.08(8) ?
O5 U1 N1 140.62(9) ?
O6 U1 N1 70.15(9) y
C2 O3 U1 132.2(2) ?
C4 O4 U1 132.7(2) ?
C7 O5 U1 137.4(2) ?
C9 O6 U1 139.2(2) ?
C11 N1 C15 117.5(3) ?
C11 N1 U1 120.6(2) ?
C15 N1 U1 121.9(2) ?
C2 C1 H1A 109.5 ?
C2 C1 H1B 109.5 ?
H1A C1 H1B 109.5 ?
C2 C1 H1C 109.5 ?
H1A C1 H1C 109.5 ?
H1B C1 H1C 109.5 ?
O3 C2 C3 123.9(4) ?
O3 C2 C1 115.6(4) ?
C3 C2 C1 120.5(4) ?
C2 C3 C4 123.8(3) ?
C2 C3 H3 118.1 ?
C4 C3 H3 118.1 ?
O4 C4 C3 124.5(3) ?
O4 C4 C5 115.8(4) ?
C3 C4 C5 119.7(4) ?
C4 C5 H5A 109.5 ?
C4 C5 H5B 109.5 ?
H5A C5 H5B 109.5 ?
C4 C5 H5C 109.5 ?
H5A C5 H5C 109.5 ?
H5B C5 H5C 109.5 ?
C7 C6 H6A 109.5 ?
C7 C6 H6B 109.5 ?
H6A C6 H6B 109.5 ?
C7 C6 H6C 109.5 ?
H6A C6 H6C 109.5 ?
H6B C6 H6C 109.5 ?
O5 C7 C8 124.5(3) ?
O5 C7 C6 115.5(4) ?
C8 C7 C6 120.0(3) ?
C7 C8 C9 124.8(3) ?
C7 C8 H8 117.6 ?
C9 C8 H8 117.6 ?
O6 C9 C8 122.9(3) ?
O6 C9 C10 116.8(3) ?
C8 C9 C10 120.3(3) ?
C9 C10 H10A 109.5 ?
C9 C10 H10B 109.5 ?
H10A C10 H10B 109.5 ?
C9 C10 H10C 109.5 ?
H10A C10 H10C 109.5 ?
H10B C10 H10C 109.5 ?
N1 C11 C12 122.5(3) ?
N1 C11 H11 118.8 ?
C12 C11 H11 118.8 ?
C11 C12 C13 120.3(3) ?
C11 C12 H12 119.8 ?
C13 C12 H12 119.8 ?
C14 C13 C12 116.7(3) ?
C14 C13 C16 122.3(3) ?
C12 C13 C16 121.0(3) ?
C15 C14 C13 120.7(3) ?
C15 C14 H14 119.6 ?
C13 C14 H14 119.6 ?
N1 C15 C14 122.3(3) ?
N1 C15 H15 118.9 ?
C14 C15 H15 118.9 ?
C13 C16 C17 113.2(3) ?
C13 C16 H16A 108.9 ?
C17 C16 H16A 108.9 ?
C13 C16 H16B 108.9 ?
C17 C16 H16B 108.9 ?
H16A C16 H16B 107.7 ?
C18 C17 C16 113.9(3) ?
C18 C17 H17A 108.8 ?
C16 C17 H17A 108.8 ?
C18 C17 H17B 108.8 ?
C16 C17 H17B 108.8 ?
H17A C17 H17B 107.7 ?
C19 C18 C17 114.2(3) ?
C19 C18 H18A 108.7 ?
C17 C18 H18A 108.7 ?
C19 C18 H18B 108.7 ?
C17 C18 H18B 108.7 ?
H18A C18 H18B 107.6 ?
C20 C19 C24 117.9(4) ?
C20 C19 C18 120.4(4) ?
C24 C19 C18 121.7(4) ?
C19 C20 C21 120.9(4) ?
C19 C20 H20 119.5 ?
C21 C20 H20 119.5 ?
C22 C21 C20 119.7(5) ?
C22 C21 H21 120.1 ?
C20 C21 H21 120.1 ?
C21 C22 C23 118.8(5) ?
C21 C22 H22 120.6 ?
C23 C22 H22 120.6 ?
C24 C23 C22 121.7(5) ?
C24 C23 H23 119.1 ?
C22 C23 H23 119.1 ?
C23 C24 C19 120.8(4) ?
C23 C24 H24 119.6 ?
C19 C24 H24 119.6 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
U1 O1 1.773(3) y
U1 O2 1.777(3) y
U1 O3 2.330(2) y
U1 O4 2.360(2) y
U1 O5 2.348(2) y
U1 O6 2.354(2) y
U1 N1 2.610(3) y
O3 C2 1.260(4) ?
O4 C4 1.272(4) ?
O5 C7 1.271(4) ?
O6 C9 1.251(4) ?
N1 C11 1.342(4) ?
N1 C15 1.342(4) ?
C1 C2 1.519(5) ?
C1 H1A 0.9600 ?
C1 H1B 0.9600 ?
C1 H1C 0.9600 ?
C2 C3 1.384(6) ?
C3 C4 1.386(6) ?
C3 H3 0.9300 ?
C4 C5 1.501(5) ?
C5 H5A 0.9600 ?
C5 H5B 0.9600 ?
C5 H5C 0.9600 ?
C6 C7 1.505(5) ?
C6 H6A 0.9600 ?
C6 H6B 0.9600 ?
C6 H6C 0.9600 ?
C7 C8 1.385(5) ?
C8 C9 1.388(5) ?
C8 H8 0.9300 ?
C9 C10 1.504(5) ?
C10 H10A 0.9600 ?
C10 H10B 0.9600 ?
C10 H10C 0.9600 ?
C11 C12 1.376(5) ?
C11 H11 0.9300 ?
C12 C13 1.382(5) ?
C12 H12 0.9300 ?
C13 C14 1.375(5) ?
C13 C16 1.512(5) ?
C14 C15 1.375(5) ?
C14 H14 0.9300 ?
C15 H15 0.9300 ?
C16 C17 1.528(6) ?
C16 H16A 0.9700 ?
C16 H16B 0.9700 ?
C17 C18 1.519(5) ?
C17 H17A 0.9700 ?
C17 H17B 0.9700 ?
C18 C19 1.517(6) ?
C18 H18A 0.9700 ?
C18 H18B 0.9700 ?
C19 C20 1.382(5) ?
C19 C24 1.389(6) ?
C20 C21 1.407(6) ?
C20 H20 0.9300 ?
C21 C22 1.375(7) ?
C21 H21 0.9300 ?
C22 C23 1.375(7) ?
C22 H22 0.9300 ?
C23 C24 1.362(6) ?
C23 H23 0.9300 ?
C24 H24 0.9300 ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139087176
