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#$Date: 2025-08-22 00:26:11 +0300 (Fri, 22 Aug 2025) $
#$Revision: 301853 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/89/7108979.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_7108979
loop_
_publ_author_name
'Florian Dulong'
'Jacky Pouessel'
'Pierre Thuery'
'Jean-Claude Berthet'
'Michel Ephritikhine'
'Thibault Cantat'
_publ_section_title
;
 Nitrite complexes of uranium and thorium
;
_journal_name_full               Chem.Commun.
_journal_page_first              2412
_journal_paper_doi               10.1039/c3cc39163a
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C48 H40 N4 O10 P2 U'
_chemical_formula_weight         1132.81
_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                99.5411(7)
_cell_angle_beta                 93.7891(7)
_cell_angle_gamma                114.6103(9)
_cell_formula_units_Z            1
_cell_length_a                   10.0718(2)
_cell_length_b                   10.7528(2)
_cell_length_c                   11.7809(3)
_cell_measurement_reflns_used    71913
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.25
_cell_volume                     1130.86(4)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and twelve ω scans with 1° steps (1531 frames)'
_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  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_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            71913
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.723
_exptl_absorpt_correction_T_max  0.771
_exptl_absorpt_correction_T_min  0.613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             558
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.537
_refine_diff_density_min         -1.140
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         6903
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0214
_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)+(0.0191P)²+0.1655P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0514
_reflns_number_gt                6859
_reflns_number_total             6903
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc39163a.txt
_cod_data_source_block           2
_cod_database_code               7108979
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
U U 0.0000 0.5000 0.0000 0.02393(3) Uani 1 2 d S
P1 P 0.62025(5) 0.69519(5) 0.31839(4) 0.02120(9) Uani 1 1 d .
O1 O -0.16520(16) 0.50718(18) -0.05091(12) 0.0319(3) Uani 1 1 d .
O2 O -0.1204(2) 0.36010(19) 0.14848(14) 0.0420(4) Uani 1 1 d .
O3 O -0.03933(19) 0.5763(2) 0.20649(12) 0.0378(4) Uani 1 1 d .
O4 O 0.11157(17) 0.74657(18) 0.07273(13) 0.0357(3) Uani 1 1 d .
O5 O 0.2981(2) 0.9359(2) 0.15000(17) 0.0523(5) Uani 1 1 d .
N1 N -0.1003(3) 0.4585(3) 0.23179(16) 0.0421(5) Uani 1 1 d .
N2 N 0.2539(2) 0.8128(2) 0.10699(17) 0.0422(5) Uani 1 1 d .
C1 C 0.7144(2) 0.8269(2) 0.23843(14) 0.0225(3) Uani 1 1 d .
C2 C 0.8485(2) 0.8375(2) 0.20239(15) 0.0254(4) Uani 1 1 d .
H2 H 0.8858 0.7750 0.2174 0.030 Uiso 1 1 calc R
C3 C 0.9245(2) 0.9417(2) 0.14440(16) 0.0293(4) Uani 1 1 d .
H3 H 1.0126 0.9484 0.1197 0.035 Uiso 1 1 calc R
C4 C 0.8704(2) 1.0365(2) 0.12271(15) 0.0298(4) Uani 1 1 d .
H4 H 0.9232 1.1075 0.0853 0.036 Uiso 1 1 calc R
C5 C 0.7371(2) 1.0247(2) 0.15699(16) 0.0291(4) Uani 1 1 d .
H5 H 0.7003 1.0874 0.1416 0.035 Uiso 1 1 calc R
C6 C 0.6587(2) 0.9207(2) 0.21380(15) 0.0257(4) Uani 1 1 d .
H6 H 0.5690 0.9128 0.2357 0.031 Uiso 1 1 calc R
C7 C 0.4952(2) 0.7420(2) 0.39795(15) 0.0243(3) Uani 1 1 d .
C8 C 0.5300(2) 0.7931(2) 0.51799(16) 0.0296(4) Uani 1 1 d .
H8 H 0.6140 0.7957 0.5584 0.036 Uiso 1 1 calc R
C9 C 0.4394(3) 0.8399(3) 0.57716(18) 0.0364(5) Uani 1 1 d .
H9 H 0.4621 0.8735 0.6574 0.044 Uiso 1 1 calc R
C10 C 0.3156(2) 0.8364(3) 0.5167(2) 0.0383(5) Uani 1 1 d .
H10 H 0.2568 0.8709 0.5560 0.046 Uiso 1 1 calc R
C11 C 0.2779(2) 0.7823(3) 0.3980(2) 0.0361(5) Uani 1 1 d .
H11 H 0.1925 0.7781 0.3585 0.043 Uiso 1 1 calc R
C12 C 0.3670(2) 0.7341(2) 0.33761(18) 0.0301(4) Uani 1 1 d .
H12 H 0.3416 0.6971 0.2579 0.036 Uiso 1 1 calc R
C13 C 0.5235(2) 0.5248(2) 0.22660(15) 0.0235(3) Uani 1 1 d .
C14 C 0.3994(2) 0.4262(2) 0.25931(17) 0.0330(4) Uani 1 1 d .
H14 H 0.3583 0.4526 0.3220 0.040 Uiso 1 1 calc R
C15 C 0.3369(3) 0.2882(3) 0.19805(19) 0.0405(5) Uani 1 1 d .
H15 H 0.2531 0.2220 0.2189 0.049 Uiso 1 1 calc R
C16 C 0.3999(3) 0.2490(3) 0.10540(18) 0.0380(5) Uani 1 1 d .
H16 H 0.3597 0.1560 0.0658 0.046 Uiso 1 1 calc R
C17 C 0.5217(2) 0.3475(3) 0.07182(17) 0.0339(5) Uani 1 1 d .
H17 H 0.5622 0.3209 0.0089 0.041 Uiso 1 1 calc R
C18 C 0.5842(2) 0.4863(2) 0.13156(15) 0.0273(4) Uani 1 1 d .
H18 H 0.6656 0.5529 0.1084 0.033 Uiso 1 1 calc R
C19 C 0.7575(2) 0.6919(2) 0.42217(14) 0.0224(3) Uani 1 1 d .
C20 C 0.7564(2) 0.5664(2) 0.43690(16) 0.0259(4) Uani 1 1 d .
H20 H 0.6884 0.4823 0.3895 0.031 Uiso 1 1 calc R
C21 C 0.8585(2) 0.5672(3) 0.52364(17) 0.0311(4) Uani 1 1 d .
H21 H 0.8590 0.4834 0.5336 0.037 Uiso 1 1 calc R
C22 C 0.9580(2) 0.6914(3) 0.59424(17) 0.0325(4) Uani 1 1 d .
H22 H 1.0244 0.6910 0.6528 0.039 Uiso 1 1 calc R
C23 C 0.9605(2) 0.8178(2) 0.57892(16) 0.0305(4) Uani 1 1 d .
H23 H 1.0288 0.9016 0.6265 0.037 Uiso 1 1 calc R
C24 C 0.8608(2) 0.8183(2) 0.49246(15) 0.0268(4) Uani 1 1 d .
H24 H 0.8626 0.9025 0.4812 0.032 Uiso 1 1 calc R
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'
U U -9.6767 9.6646 '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'
P P 0.1023 0.0942 '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
O1 U O1 180.0 . 2_565
O1 U O4 90.18(6) . 2_565
O1 U O4 89.82(6) 2_565 2_565
O1 U O4 89.82(6) . .
O1 U O4 90.18(6) 2_565 .
O4 U O4 180.00(9) 2_565 .
O1 U O2 92.29(6) . .
O1 U O2 87.71(6) 2_565 .
O4 U O2 66.29(5) 2_565 .
O4 U O2 113.71(5) . .
O1 U O2 87.71(6) . 2_565
O1 U O2 92.29(7) 2_565 2_565
O4 U O2 113.71(5) 2_565 2_565
O4 U O2 66.29(5) . 2_565
O2 U O2 180.00(8) . 2_565
O1 U O3 91.88(6) . 2_565
O1 U O3 88.12(6) 2_565 2_565
O4 U O3 65.38(6) 2_565 2_565
O4 U O3 114.62(6) . 2_565
O2 U O3 131.48(6) . 2_565
O2 U O3 48.52(6) 2_565 2_565
O1 U O3 88.12(6) . .
O1 U O3 91.88(6) 2_565 .
O4 U O3 114.62(6) 2_565 .
O4 U O3 65.38(6) . .
O2 U O3 48.52(6) . .
O2 U O3 131.48(6) 2_565 .
O3 U O3 180.00(9) 2_565 .
C13 P1 C1 112.46(8) . .
C13 P1 C19 108.51(9) . .
C1 P1 C19 107.54(9) . .
C13 P1 C7 110.39(9) . .
C1 P1 C7 109.81(9) . .
C19 P1 C7 107.99(8) . .
N1 O2 U 99.67(14) . .
N1 O3 U 99.11(12) . .
N2 O4 U 119.69(14) . .
O3 N1 O2 112.61(18) . .
O5 N2 O4 114.5(2) . .
C6 C1 C2 119.60(18) . .
C6 C1 P1 121.37(14) . .
C2 C1 P1 119.01(14) . .
C3 C2 C1 119.46(18) . .
C3 C2 H2 120.3 . .
C1 C2 H2 120.3 . .
C2 C3 C4 120.61(18) . .
C2 C3 H3 119.7 . .
C4 C3 H3 119.7 . .
C5 C4 C3 119.8(2) . .
C5 C4 H4 120.1 . .
C3 C4 H4 120.1 . .
C6 C5 C4 120.50(19) . .
C6 C5 H5 119.7 . .
C4 C5 H5 119.7 . .
C5 C6 C1 119.99(18) . .
C5 C6 H6 120.0 . .
C1 C6 H6 120.0 . .
C8 C7 C12 120.10(17) . .
C8 C7 P1 120.35(14) . .
C12 C7 P1 119.46(14) . .
C9 C8 C7 119.97(18) . .
C9 C8 H8 120.0 . .
C7 C8 H8 120.0 . .
C10 C9 C8 119.74(19) . .
C10 C9 H9 120.1 . .
C8 C9 H9 120.1 . .
C9 C10 C11 120.71(19) . .
C9 C10 H10 119.6 . .
C11 C10 H10 119.6 . .
C10 C11 C12 120.21(19) . .
C10 C11 H11 119.9 . .
C12 C11 H11 119.9 . .
C11 C12 C7 119.21(19) . .
C11 C12 H12 120.4 . .
C7 C12 H12 120.4 . .
C14 C13 C18 120.40(19) . .
C14 C13 P1 119.48(14) . .
C18 C13 P1 119.57(16) . .
C15 C14 C13 119.68(19) . .
C15 C14 H14 120.2 . .
C13 C14 H14 120.2 . .
C14 C15 C16 119.9(2) . .
C14 C15 H15 120.1 . .
C16 C15 H15 120.1 . .
C17 C16 C15 120.3(2) . .
C17 C16 H16 119.8 . .
C15 C16 H16 119.8 . .
C16 C17 C18 120.3(2) . .
C16 C17 H17 119.8 . .
C18 C17 H17 119.8 . .
C17 C18 C13 119.3(2) . .
C17 C18 H18 120.3 . .
C13 C18 H18 120.3 . .
C20 C19 C24 120.30(17) . .
C20 C19 P1 120.93(15) . .
C24 C19 P1 118.68(14) . .
C19 C20 C21 119.41(19) . .
C19 C20 H20 120.3 . .
C21 C20 H20 120.3 . .
C22 C21 C20 120.2(2) . .
C22 C21 H21 119.9 . .
C20 C21 H21 119.9 . .
C21 C22 C23 120.59(18) . .
C21 C22 H22 119.7 . .
C23 C22 H22 119.7 . .
C24 C23 C22 119.7(2) . .
C24 C23 H23 120.2 . .
C22 C23 H23 120.2 . .
C23 C24 C19 119.82(19) . .
C23 C24 H24 120.1 . .
C19 C24 H24 120.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U O1 1.7676(13) .
U O1 1.7677(13) 2_565
U O4 2.3800(17) 2_565
U O4 2.3800(17) .
U O2 2.5349(17) .
U O2 2.5349(17) 2_565
U O3 2.5465(14) 2_565
U O3 2.5465(14) .
P1 C13 1.7871(19) .
P1 C1 1.798(2) .
P1 C19 1.7995(17) .
P1 C7 1.8014(18) .
O2 N1 1.255(3) .
O3 N1 1.254(3) .
O4 N2 1.305(3) .
O5 N2 1.211(3) .
C1 C6 1.400(3) .
C1 C2 1.408(2) .
C2 C3 1.384(3) .
C2 H2 0.9300 .
C3 C4 1.390(3) .
C3 H3 0.9300 .
C4 C5 1.389(3) .
C4 H4 0.9300 .
C5 C6 1.380(3) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 C8 1.393(3) .
C7 C12 1.396(3) .
C8 C9 1.387(3) .
C8 H8 0.9300 .
C9 C10 1.378(3) .
C9 H9 0.9300 .
C10 C11 1.384(3) .
C10 H10 0.9300 .
C11 C12 1.389(3) .
C11 H11 0.9300 .
C12 H12 0.9300 .
C13 C14 1.390(3) .
C13 C18 1.395(3) .
C14 C15 1.388(3) .
C14 H14 0.9300 .
C15 C16 1.390(3) .
C15 H15 0.9300 .
C16 C17 1.380(3) .
C16 H16 0.9300 .
C17 C18 1.389(3) .
C17 H17 0.9300 .
C18 H18 0.9300 .
C19 C20 1.385(3) .
C19 C24 1.396(3) .
C20 C21 1.397(3) .
C20 H20 0.9300 .
C21 C22 1.374(3) .
C21 H21 0.9300 .
C22 C23 1.390(3) .
C22 H22 0.9300 .
C23 C24 1.385(3) .
C23 H23 0.9300 .
C24 H24 0.9300 .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139183049
