#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:05:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179092 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/54/4305462.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_4305462
loop_
_publ_author_name
'Jean-Claude Berthet'
'Pierre Thuéry'
'Jean-Pierre Dognon'
'Denis Guillaneux'
'Michel Ephritikhine'
_publ_contact_author_address
;
      CEA/Saclay, SCM (CNRS URA 331)
      Bât. 125
      91191 Gif-sur-Yvette
      France
;
_publ_contact_author_email       jean-claude.berthet@cea.fr
_publ_contact_author_fax         '33 1 69 08 66 40'
_publ_contact_author_name        'J. C. Berthet'
_publ_contact_author_phone       '33 01 69 08 64 36'
_publ_section_title
;
Sterically Congested Uranyl Complexes with Seven-Coordination of the
UO2 Unit: the Peculiar Ligation Mode of Nitrate in [UO2(NO3)2(Rbtp)]
Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6850
_journal_page_last               6862
_journal_paper_doi               10.1021/ic8004486
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C17 H18 N10 O8 U'
_chemical_formula_weight         728.44
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.861(3)
_cell_angle_beta                 98.721(2)
_cell_angle_gamma                102.410(3)
_cell_formula_units_Z            2
_cell_length_a                   8.7996(4)
_cell_length_b                   9.2294(5)
_cell_length_c                   15.5220(9)
_cell_measurement_reflns_used    44575
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.91
_cell_volume                     1161.09(11)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'two φ and six ω scans with 2° steps'
_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  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0179
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            44575
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.91
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.056
_exptl_absorpt_correction_T_max  0.494
_exptl_absorpt_correction_T_min  0.342
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    2.084
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         4403
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0175
_refine_ls_R_factor_gt           0.0168
_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)+(0.0273P)²+0.9935P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0431
_refine_ls_wR_factor_ref         0.0433
_reflns_number_gt                4280
_reflns_number_total             4403
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8004486.file003_4.cif
_cod_data_source_block           5.MeCN
_cod_database_code               4305462
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
_atom_site_disorder_assembly
_atom_site_disorder_group
U U 0.532313(10) 0.828887(10) 0.671187(6) 0.01576(4) Uani 1 1 d . . .
O1 O 0.5756(2) 0.6476(2) 0.63464(14) 0.0225(4) Uani 1 1 d . . .
O2 O 0.4660(2) 1.0000(2) 0.69022(14) 0.0227(4) Uani 1 1 d . . .
O3 O 0.7038(2) 0.9670(2) 0.58376(14) 0.0252(4) Uani 1 1 d . . .
O4 O 0.8218(2) 0.9675(3) 0.71490(14) 0.0259(5) Uani 1 1 d . . .
O5 O 0.9613(2) 1.0695(2) 0.63031(16) 0.0286(5) Uani 1 1 d . . .
O6 O 0.6332(2) 0.9766(2) 0.83955(14) 0.0251(4) Uani 1 1 d . . .
O7 O 0.7202(3) 0.7732(3) 0.80976(17) 0.0360(5) Uani 1 1 d . . .
O8 O 0.7781(3) 0.9267(3) 0.94949(17) 0.0492(7) Uani 1 1 d . . .
N1 N 0.2236(3) 0.7168(3) 0.60365(15) 0.0165(5) Uani 1 1 d . . .
N2 N 0.5328(3) 0.7260(3) 0.44147(16) 0.0191(5) Uani 1 1 d . . .
N3 N 0.4264(3) 0.7443(3) 0.49504(16) 0.0176(5) Uani 1 1 d . . .
N4 N 0.2125(3) 0.6672(3) 0.36532(16) 0.0190(5) Uani 1 1 d . . .
N5 N 0.4168(3) 0.7221(3) 0.85552(16) 0.0201(5) Uani 1 1 d . . .
N6 N 0.3485(3) 0.7286(3) 0.77270(16) 0.0184(5) Uani 1 1 d . . .
N7 N 0.0939(3) 0.6976(3) 0.81127(16) 0.0184(5) Uani 1 1 d . . .
N8 N 0.8347(3) 1.0054(3) 0.64244(17) 0.0210(5) Uani 1 1 d . . .
N9 N 0.7147(3) 0.8925(3) 0.86962(18) 0.0265(6) Uani 1 1 d . . .
C1 C 0.1209(3) 0.7047(3) 0.65964(19) 0.0174(5) Uani 1 1 d . . .
C2 C -0.0414(3) 0.6866(3) 0.6326(2) 0.0196(6) Uani 1 1 d . . .
H2 H -0.1076 0.6788 0.6734 0.023 Uiso 1 1 calc R . .
C3 C -0.1035(3) 0.6802(3) 0.54348(19) 0.0195(6) Uani 1 1 d . . .
H3 H -0.2117 0.6695 0.5238 0.023 Uiso 1 1 calc R . .
C4 C -0.0006(3) 0.6902(3) 0.48467(19) 0.0192(6) Uani 1 1 d . . .
H4 H -0.0386 0.6858 0.4245 0.023 Uiso 1 1 calc R . .
C5 C 0.1608(3) 0.7070(3) 0.51711(18) 0.0170(5) Uani 1 1 d . . .
C6 C 0.2737(3) 0.7086(3) 0.45614(19) 0.0167(5) Uani 1 1 d . . .
C7 C 0.3166(3) 0.6590(3) 0.31257(19) 0.0197(6) Uani 1 1 d . . .
C8 C 0.4805(3) 0.6837(3) 0.3524(2) 0.0193(6) Uani 1 1 d . . .
C9 C 0.1921(3) 0.7095(3) 0.75290(18) 0.0162(5) Uani 1 1 d . . .
C10 C 0.1619(3) 0.7005(3) 0.89415(19) 0.0192(6) Uani 1 1 d . . .
C11 C 0.3265(3) 0.7064(3) 0.91495(19) 0.0202(6) Uani 1 1 d . . .
C12 C 0.2575(4) 0.6216(4) 0.2122(2) 0.0274(6) Uani 1 1 d . . .
H12A H 0.1445 0.6094 0.1990 0.041 Uiso 1 1 calc R . .
H12B H 0.2798 0.5267 0.1815 0.041 Uiso 1 1 calc R . .
H12C H 0.3100 0.7045 0.1915 0.041 Uiso 1 1 calc R . .
C13 C 0.5998(4) 0.6627(4) 0.2946(2) 0.0263(6) Uani 1 1 d . . .
H13A H 0.7040 0.6890 0.3331 0.039 Uiso 1 1 calc R . .
H13B H 0.5992 0.7292 0.2561 0.039 Uiso 1 1 calc R . .
H13C H 0.5729 0.5563 0.2573 0.039 Uiso 1 1 calc R . .
C14 C 0.0613(4) 0.6967(4) 0.9629(2) 0.0248(6) Uani 1 1 d . . .
H14A H -0.0364 0.7202 0.9421 0.037 Uiso 1 1 calc R . .
H14B H 0.1176 0.7723 1.0201 0.037 Uiso 1 1 calc R . .
H14C H 0.0376 0.5951 0.9708 0.037 Uiso 1 1 calc R . .
C15 C 0.4074(4) 0.6966(4) 1.0043(2) 0.0267(6) Uani 1 1 d . . .
H15A H 0.5177 0.7024 1.0045 0.040 Uiso 1 1 calc R . .
H15B H 0.3570 0.5997 1.0128 0.040 Uiso 1 1 calc R . .
H15C H 0.3995 0.7812 1.0529 0.040 Uiso 1 1 calc R . .
N10 N 0.1549(4) 0.3564(3) 0.8729(2) 0.0372(7) Uani 1 1 d . . .
C16 C 0.1635(4) 0.2316(4) 0.8584(2) 0.0254(6) Uani 1 1 d . . .
C17 C 0.1761(4) 0.0726(3) 0.8405(2) 0.0291(7) Uani 1 1 d . . .
H17A H 0.2068 0.0412 0.7832 0.044 Uiso 1 1 calc R . .
H17B H 0.0749 0.0050 0.8379 0.044 Uiso 1 1 calc R . .
H17C H 0.2550 0.0665 0.8885 0.044 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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 U O2 170.49(9) . . ?
O1 U O4 91.14(8) . . ?
O2 U O4 95.13(8) . . ?
O1 U O6 116.15(8) . . ?
O2 U O6 73.06(8) . . ?
O4 U O6 65.77(7) . . ?
O1 U O3 96.92(8) . . ?
O2 U O3 81.72(8) . . ?
O4 U O3 50.34(7) . . ?
O6 U O3 107.66(7) . . ?
O1 U N3 77.16(8) . . ?
O2 U N3 93.87(8) . . ?
O4 U N3 111.33(7) . . ?
O6 U N3 165.90(7) . . ?
O3 U N3 64.18(7) . . ?
O1 U N6 91.94(8) . . ?
O2 U N6 89.70(8) . . ?
O4 U N6 128.78(7) . . ?
O6 U N6 67.19(7) . . ?
O3 U N6 171.09(7) . . ?
N3 U N6 119.17(7) . . ?
O1 U N1 94.61(8) . . ?
O2 U N1 78.04(8) . . ?
O4 U N1 168.76(7) . . ?
O6 U N1 119.58(7) . . ?
O3 U N1 119.19(7) . . ?
N3 U N1 60.86(7) . . ?
N6 U N1 60.74(7) . . ?
O1 U O7 68.48(8) . . ?
O2 U O7 120.87(8) . . ?
O4 U O7 61.79(7) . . ?
O6 U O7 47.87(7) . . ?
O3 U O7 110.26(7) . . ?
N3 U O7 144.41(7) . . ?
N6 U O7 72.14(7) . . ?
N1 U O7 129.38(7) . . ?
N8 O3 U 96.73(15) . . ?
N8 O4 U 98.74(15) . . ?
N9 O6 U 103.22(16) . . ?
N9 O7 U 94.21(17) . . ?
C5 N1 C1 116.7(2) . . ?
C5 N1 U 120.66(17) . . ?
C1 N1 U 120.56(18) . . ?
C8 N2 N3 118.2(2) . . ?
C6 N3 N2 118.9(2) . . ?
C6 N3 U 123.11(17) . . ?
N2 N3 U 117.78(16) . . ?
C7 N4 C6 115.8(2) . . ?
C11 N5 N6 118.6(2) . . ?
C9 N6 N5 118.4(2) . . ?
C9 N6 U 121.71(17) . . ?
N5 N6 U 118.83(17) . . ?
C10 N7 C9 115.9(2) . . ?
O5 N8 O3 123.4(2) . . ?
O5 N8 O4 122.5(2) . . ?
O3 N8 O4 114.1(2) . . ?
O8 N9 O7 123.8(3) . . ?
O8 N9 O6 121.5(3) . . ?
O7 N9 O6 114.7(2) . . ?
N1 C1 C2 123.4(3) . . ?
N1 C1 C9 115.5(2) . . ?
C2 C1 C9 121.1(2) . . ?
C1 C2 C3 119.0(3) . . ?
C4 C3 C2 118.4(3) . . ?
C3 C4 C5 118.9(3) . . ?
N1 C5 C4 123.4(2) . . ?
N1 C5 C6 115.4(2) . . ?
C4 C5 C6 121.2(2) . . ?
N3 C6 N4 125.6(2) . . ?
N3 C6 C5 116.7(2) . . ?
N4 C6 C5 117.6(2) . . ?
N4 C7 C8 119.7(3) . . ?
N4 C7 C12 118.4(3) . . ?
C8 C7 C12 122.0(3) . . ?
N2 C8 C7 121.4(2) . . ?
N2 C8 C13 117.3(3) . . ?
C7 C8 C13 121.3(3) . . ?
N6 C9 N7 125.7(3) . . ?
N6 C9 C1 116.7(2) . . ?
N7 C9 C1 117.6(2) . . ?
N7 C10 C11 119.8(2) . . ?
N7 C10 C14 118.2(3) . . ?
C11 C10 C14 122.0(3) . . ?
N5 C11 C10 121.2(3) . . ?
N5 C11 C15 116.3(3) . . ?
C10 C11 C15 122.6(3) . . ?
N10 C16 C17 179.4(4) . . ?
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
U O1 1.766(2) . ?
U O2 1.770(2) . ?
U O4 2.493(2) . ?
U O6 2.535(2) . ?
U O3 2.535(2) . ?
U N3 2.603(2) . ?
U N6 2.614(2) . ?
U N1 2.631(2) . ?
U O7 2.735(3) . ?
O3 N8 1.274(3) . ?
O4 N8 1.274(3) . ?
O5 N8 1.210(3) . ?
O6 N9 1.287(3) . ?
O7 N9 1.261(4) . ?
O8 N9 1.209(4) . ?
N1 C5 1.345(4) . ?
N1 C1 1.353(3) . ?
N2 C8 1.315(4) . ?
N2 N3 1.353(3) . ?
N3 C6 1.319(4) . ?
N4 C7 1.320(4) . ?
N4 C6 1.352(4) . ?
N5 C11 1.321(4) . ?
N5 N6 1.356(3) . ?
N6 C9 1.327(4) . ?
N7 C10 1.325(4) . ?
N7 C9 1.352(3) . ?
C1 C2 1.387(4) . ?
C1 C9 1.473(4) . ?
C2 C3 1.389(4) . ?
C3 C4 1.386(4) . ?
C4 C5 1.394(4) . ?
C5 C6 1.473(4) . ?
C7 C8 1.425(4) . ?
C7 C12 1.489(4) . ?
C8 C13 1.493(4) . ?
C10 C11 1.422(4) . ?
C10 C14 1.489(4) . ?
C11 C15 1.494(4) . ?
N10 C16 1.137(4) . ?
C16 C17 1.454(4) . ?
