#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:56:08 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179354 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/51/4325125.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_4325125
loop_
_publ_author_name
'Andrew J. Gaunt'
'Iain May'
'Mary P. Neu'
'Sean D. Reilly'
'Brian L. Scott'
_publ_section_title
;
 Structural and Spectroscopic Characterization of Plutonyl(VI) Nitrate
 under Acidic Conditions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4244
_journal_page_last               4246
_journal_paper_doi               10.1021/ic200525u
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'H6 N2 O11 Pu'
_chemical_formula_weight         449.05
_chemical_name_systematic
; 
 ? 
;
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.158(3)
_cell_angle_beta                 82.011(3)
_cell_angle_gamma                65.129(2)
_cell_formula_units_Z            2
_cell_length_a                   6.9924(3)
_cell_length_b                   7.0456(3)
_cell_length_c                   9.9252(5)
_cell_measurement_temperature    141(2)
_cell_volume                     438.31(4)
_computing_cell_refinement       'SAINT 4.05 (Bruker, 1996)'
_computing_data_collection       'SMART 4.210 (Bruker, 1996)'
_computing_data_reduction        'SAINT 4.05 (Bruker, 1996)'
_computing_molecular_graphics    'SHELXTL 6.10 (Bruker, 2001)'
_computing_publication_material  'SHELXTL 6.10 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      141(2)
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'Bruker SMART 1k CCD'
_diffrn_measurement_method       'φ 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  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6604
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.575
_exptl_absorpt_correction_T_max  0.7515
_exptl_absorpt_correction_T_min  0.5180
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.425
_exptl_crystal_description       block
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.411
_refine_diff_density_min         -3.588
_refine_diff_density_rms         0.299
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         1459
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0551P)²+1.6821P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0870
_reflns_number_gt                1168
_reflns_number_total             1459
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200525u_si_002.cif
_cod_data_source_block           ccd853
_cod_original_cell_volume        438.31(3)
_cod_database_code               4325125
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
Pu1 Pu 0.5000 0.5000 0.5000 0.01674(17) Uani 1 2 d SU
Pu2 Pu 0.5000 0.0000 1.0000 0.01930(17) Uani 1 2 d SU
N1 N 0.1724(10) 0.8831(9) 0.6103(6) 0.0237(14) Uani 1 1 d U
N2 N 0.2554(11) -0.2342(10) 0.9535(7) 0.0288(16) Uani 1 1 d U
O1 O 0.4053(8) 0.5828(8) 0.3420(5) 0.0282(12) Uani 1 1 d U
O2 O 0.3483(8) 0.8793(7) 0.5535(5) 0.0245(12) Uani 1 1 d U
O3 O 0.0344(9) 1.0381(9) 0.6574(7) 0.0354(15) Uani 1 1 d U
O4 O 0.1473(8) 0.7158(7) 0.6116(5) 0.0267(12) Uani 1 1 d U
O5 O 0.2598(12) 0.3287(10) 0.5583(8) 0.0354(16) Uani 1 1 d U
O6 O 0.3191(9) 0.2230(8) 0.9215(6) 0.0331(13) Uani 1 1 d U
O7 O 0.2329(12) -0.1527(12) 1.0678(7) 0.0336(16) Uani 1 1 d U
O8 O 0.1483(9) -0.3234(9) 0.9346(6) 0.0398(15) Uani 1 1 d U
O9 O 0.3940(9) -0.2108(9) 0.8655(6) 0.0381(15) Uani 1 1 d U
O10 O 0.2931(8) 0.1022(8) 1.2186(5) 0.0297(13) Uani 1 1 d U
O11 O 0.9358(9) 0.4672(9) 0.7690(6) 0.0301(14) Uani 1 1 d U
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pu Pu -9.4100 4.3056 '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 Pu1 O1 179.999(1) 2_666 .
O1 Pu1 O5 90.0(2) 2_666 .
O1 Pu1 O5 90.0(2) . .
O1 Pu1 O5 90.0(2) 2_666 2_666
O1 Pu1 O5 90.0(2) . 2_666
O5 Pu1 O5 180.000(1) . 2_666
O1 Pu1 O4 90.2(2) 2_666 2_666
O1 Pu1 O4 89.8(2) . 2_666
O5 Pu1 O4 115.85(19) . 2_666
O5 Pu1 O4 64.15(19) 2_666 2_666
O1 Pu1 O4 89.8(2) 2_666 .
O1 Pu1 O4 90.2(2) . .
O5 Pu1 O4 64.15(19) . .
O5 Pu1 O4 115.85(19) 2_666 .
O4 Pu1 O4 180.00(19) 2_666 .
O1 Pu1 O2 91.9(2) 2_666 .
O1 Pu1 O2 88.1(2) . .
O5 Pu1 O2 115.1(2) . .
O5 Pu1 O2 64.9(2) 2_666 .
O4 Pu1 O2 129.03(15) 2_666 .
O4 Pu1 O2 50.97(15) . .
O1 Pu1 O2 88.1(2) 2_666 2_666
O1 Pu1 O2 91.9(2) . 2_666
O5 Pu1 O2 64.9(2) . 2_666
O5 Pu1 O2 115.1(2) 2_666 2_666
O4 Pu1 O2 50.97(15) 2_666 2_666
O4 Pu1 O2 129.03(15) . 2_666
O2 Pu1 O2 180.0 . 2_666
O1 Pu1 N1 90.4(2) 2_666 .
O1 Pu1 N1 89.6(2) . .
O5 Pu1 N1 89.4(2) . .
O5 Pu1 N1 90.6(2) 2_666 .
O4 Pu1 N1 154.69(15) 2_666 .
O4 Pu1 N1 25.30(15) . .
O2 Pu1 N1 25.67(16) . .
O2 Pu1 N1 154.33(16) 2_666 .
O1 Pu1 N1 89.6(2) 2_666 2_666
O1 Pu1 N1 90.4(2) . 2_666
O5 Pu1 N1 90.6(2) . 2_666
O5 Pu1 N1 89.4(2) 2_666 2_666
O4 Pu1 N1 25.31(15) 2_666 2_666
O4 Pu1 N1 154.69(15) . 2_666
O2 Pu1 N1 154.33(16) . 2_666
O2 Pu1 N1 25.67(16) 2_666 2_666
N1 Pu1 N1 180.000(1) . 2_666
O6 Pu2 O6 179.999(1) . 2_657
O6 Pu2 O10 89.4(2) . .
O6 Pu2 O10 90.6(2) 2_657 .
O6 Pu2 O10 90.6(2) . 2_657
O6 Pu2 O10 89.4(2) 2_657 2_657
O10 Pu2 O10 179.999(2) . 2_657
O6 Pu2 O9 92.0(2) . 2_657
O6 Pu2 O9 88.0(2) 2_657 2_657
O10 Pu2 O9 63.94(18) . 2_657
O10 Pu2 O9 116.06(18) 2_657 2_657
O6 Pu2 O9 88.0(2) . .
O6 Pu2 O9 92.0(2) 2_657 .
O10 Pu2 O9 116.06(18) . .
O10 Pu2 O9 63.94(18) 2_657 .
O9 Pu2 O9 180.000(1) 2_657 .
O6 Pu2 O7 87.3(3) . 2_657
O6 Pu2 O7 92.7(3) 2_657 2_657
O10 Pu2 O7 114.78(19) . 2_657
O10 Pu2 O7 65.22(19) 2_657 2_657
O9 Pu2 O7 51.1(2) 2_657 2_657
O9 Pu2 O7 128.9(2) . 2_657
O6 Pu2 O7 92.7(3) . .
O6 Pu2 O7 87.3(3) 2_657 .
O10 Pu2 O7 65.22(19) . .
O10 Pu2 O7 114.78(19) 2_657 .
O9 Pu2 O7 128.9(2) 2_657 .
O9 Pu2 O7 51.1(2) . .
O7 Pu2 O7 180.000(2) 2_657 .
O6 Pu2 N2 89.9(2) . .
O6 Pu2 N2 90.1(2) 2_657 .
O10 Pu2 N2 90.94(18) . .
O10 Pu2 N2 89.06(17) 2_657 .
O9 Pu2 N2 154.78(17) 2_657 .
O9 Pu2 N2 25.22(17) . .
O7 Pu2 N2 154.1(2) 2_657 .
O7 Pu2 N2 25.9(2) . .
O6 Pu2 N2 90.1(2) . 2_657
O6 Pu2 N2 89.9(2) 2_657 2_657
O10 Pu2 N2 89.06(18) . 2_657
O10 Pu2 N2 90.94(18) 2_657 2_657
O9 Pu2 N2 25.22(17) 2_657 2_657
O9 Pu2 N2 154.78(17) . 2_657
O7 Pu2 N2 25.9(2) 2_657 2_657
O7 Pu2 N2 154.1(2) . 2_657
N2 Pu2 N2 180.0 . 2_657
O3 N1 O4 121.4(6) . .
O3 N1 O2 122.5(6) . .
O4 N1 O2 116.1(6) . .
O3 N1 Pu1 178.3(5) . .
O4 N1 Pu1 57.0(3) . .
O2 N1 Pu1 59.2(3) . .
O8 N2 O9 123.7(6) . .
O8 N2 O7 121.2(7) . .
O9 N2 O7 115.1(6) . .
O8 N2 Pu2 177.5(5) . .
O9 N2 Pu2 57.2(3) . .
O7 N2 Pu2 57.9(4) . .
N1 O2 Pu1 95.1(3) . .
N1 O4 Pu1 97.7(4) . .
N2 O7 Pu2 96.2(5) . .
N2 O9 Pu2 97.5(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pu1 O1 1.727(5) 2_666
Pu1 O1 1.727(5) .
Pu1 O5 2.425(7) .
Pu1 O5 2.425(7) 2_666
Pu1 O4 2.472(5) 2_666
Pu1 O4 2.472(5) .
Pu1 O2 2.519(5) .
Pu1 O2 2.519(5) 2_666
Pu1 N1 2.922(6) .
Pu1 N1 2.922(6) 2_666
Pu2 O6 1.728(5) .
Pu2 O6 1.728(5) 2_657
Pu2 O10 2.438(5) .
Pu2 O10 2.438(5) 2_657
Pu2 O9 2.492(5) 2_657
Pu2 O9 2.492(5) .
Pu2 O7 2.503(7) 2_657
Pu2 O7 2.503(7) .
Pu2 N2 2.938(6) .
Pu2 N2 2.938(6) 2_657
N1 O3 1.205(8) .
N1 O4 1.260(7) .
N1 O2 1.271(8) .
N2 O8 1.206(8) .
N2 O9 1.263(8) .
N2 O7 1.292(9) .
