 
data_cait85z

# TITLE AND AUTHOR LIST

_publ_section_title              
;\
Structure and spectroscopic evidence for neptunyl(VI) mono- and
dinitrate complexes in aqueous nitric acid
;
_publ_contact_author_name        
'Patric Lindqvist-Reis' # Name of author for correspondence
_publ_contact_author_address     # Address of author for correspondence
;
Institut für Nukleare Entsorgung
Karlsruhe Institute of Technology
P.O. Box 3640
76021 Karlsruhe
Germany
;
_publ_contact_author_email       'patric.lindqvist@kit.edu'
_publ_contact_author_phone       '+4972160822389'
_publ_contact_author_fax         ?
loop_
_publ_author_name
_publ_author_address
_publ_author_footnote
_publ_author_email
'Lindqvist-Reis, Patric'
;
Institut für Nukleare Entsorgung
Karlsruhe Institute of Technology
Hermann-von-Helmholtz-Platz 1
76344 Eggenstein-Leopoldshafen
Germany
;
.
.
'Apostolidis, Christos'
;
European Commission
Joint Research Centre
Institute for Transuranium Elements
Hermann-von-Helmholtz-Platz 1
76344 Eggenstein-Leopoldshafen
Germany
;
.
.
'Walter, Olaf'
;
Institut für Katalyseforschung und -technologie
Karlsruhe Institute of Technology
Hermann-von-Helmholtz-Platz 1
76344 Eggenstein-Leopoldshafen
Germany
;
.
.
'Marsak, Remi'
;
Institut für Nukleare Entsorgung
Karlsruhe Institute of Technology
Hermann-von-Helmholtz-Platz 1
76344 Eggenstein-Leopoldshafen
Germany
;
.
.
'Banik, Nidhu Lal'
;
Institut für Nukleare Entsorgung
Karlsruhe Institute of Technology
Hermann-von-Helmholtz-Platz 1
76344 Eggenstein-Leopoldshafen
Germany
;
.
.
'Skripkin, Mikhail Yu'
;
Department of Chemistry
St. Petersburg State University
Universitetsky pr., 26
198904 St. Petersburg
Russia
;
.
.
'Rothe, Joerg'
;
Institut für Nukleare Entsorgung
Karlsruhe Institute of Technology
Hermann-von-Helmholtz-Platz 1
76344 Eggenstein-Leopoldshafen
Germany
;
.
.
'Morgenstern, Alfred'
;
European Commission
Joint Research Centre
Institute for Transuranium Elements
Hermann-von-Helmholtz-Platz 1
76344 Eggenstein-Leopoldshafen
Germany
;
.
.
 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
;
 'tris-aqua-Neptunyldinitrate'
;
_chemical_name_common             'Trisaqua-Neptunyl-dinitrate'
_chemical_melting_point           ?
_chemical_formula_moiety          'H6 N2 Np O11'
_chemical_formula_sum
 'H6 N2 Np O11' 
_chemical_formula_weight          447.07

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 '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'
 'Np'  'Np' -11.4937   4.1493
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       triclinic
_space_group_IT_number            2
_space_group_name_H-M_alt         'P -1'
_space_group_name_Hall            '-P 1'
 
_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'
 '-x, -y, -z'
 
_cell_length_a                    7.0076(6)
_cell_length_b                    7.0747(6)
_cell_length_c                    9.9225(8)
_cell_angle_alpha                 82.3280(10)
_cell_angle_beta                  82.0830(10)
_cell_angle_gamma                 64.4870(10)
_cell_volume                      438.21(6)
_cell_formula_units_Z             2
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used     6725 
_cell_measurement_theta_min       6.403 
_cell_measurement_theta_max       59.15 
 
_exptl_crystal_description        quader 
_exptl_crystal_colour             red 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     3.388          
_exptl_crystal_F_000              402
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.272
_exptl_crystal_size_mid           0.213
_exptl_crystal_size_min           0.145
_exptl_absorpt_coefficient_mu     11.912
_shelx_estimated_absorpt_T_min    0.140
_shelx_estimated_absorpt_T_max    0.277
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.2924 
_exptl_absorpt_correction_T_max   0.7459 
_exptl_absorpt_process_details    (sadabs) 
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       173(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'fine-focus sealed tube'                       
_diffrn_measurement_device_type   'Bruker Apex II Quazar' 
_diffrn_measurement_method        'combined omega- and phi-scan' 
_diffrn_detector_area_resol_mean  66 
_diffrn_reflns_number             10954
_diffrn_reflns_av_unetI/netI      0.0340
_diffrn_reflns_av_R_equivalents   0.0441
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -9
_diffrn_reflns_limit_k_max        9
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_limit_l_max        13
_diffrn_reflns_theta_min          2.079
_diffrn_reflns_theta_max          29.582
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.999
_diffrn_measured_fraction_theta_full  0.998
_diffrn_reflns_Laue_measured_fraction_max    0.999
_diffrn_reflns_Laue_measured_fraction_full   0.998
_diffrn_reflns_point_group_measured_fraction_max   0.999
_diffrn_reflns_point_group_measured_fraction_full  0.998
_reflns_number_total              2464
_reflns_number_gt                 2159
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'APEX II (Bruker, 2007)'
_computing_cell_refinement        'APEX II (Bruker, 2007)'
_computing_data_reduction         'SAINT (Bruker, 2007)'
_computing_structure_solution     'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement   'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics      
'XPMA (Zsolnai, 1996), ORTEP (Farrugia, 1997)' 
_computing_publication_material   ?
 
_refine_special_details
;
 ?
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0378P)²+0.1087P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     refall
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.204(5)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          2464
_refine_ls_number_parameters      155
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0286
_refine_ls_R_factor_gt            0.0266
_refine_ls_wR_factor_ref          0.0751
_refine_ls_wR_factor_gt           0.0719
_refine_ls_goodness_of_fit_ref    1.191
_refine_ls_restrained_S_all       1.191
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
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
Np1 Np 0.5000 0.5000 0.5000 0.00818(12) Uani 1 2 d S . P . .
Np2 Np 0.5000 0.0000 1.0000 0.00971(12) Uani 1 2 d S . P . .
N1 N 0.1740(3) 0.8843(3) 0.6106(2) 0.0149(5) Uani 1 1 d . . . . .
N2 N 0.2575(4) -0.2332(4) 0.9542(3) 0.0179(5) Uani 1 1 d . . . . .
O1 O 0.4012(3) 0.5893(3) 0.34039(19) 0.0185(4) Uani 1 1 d . . . . .
O2 O 0.3498(3) 0.8800(3) 0.5537(2) 0.0178(4) Uani 1 1 d . . . . .
O3 O 0.0366(5) 1.0398(4) 0.6596(4) 0.0241(6) Uani 1 1 d . . . . .
O4 O 0.1497(3) 0.7171(3) 0.6121(2) 0.0195(4) Uani 1 1 d . . . . .
O5 O 0.2595(7) 0.3309(7) 0.5610(5) 0.0217(8) Uani 1 1 d . . . . .
O6 O 0.3119(3) 0.2237(3) 0.9193(2) 0.0232(5) Uani 1 1 d . . . . .
O7 O 0.2343(8) -0.1534(8) 1.0657(4) 0.0208(8) Uani 1 1 d . . . . .
O8 O 0.1507(4) -0.3207(4) 0.9328(2) 0.0284(5) Uani 1 1 d . . . . .
O9 O 0.3989(3) -0.2121(4) 0.8664(2) 0.0263(5) Uani 1 1 d . . . . .
O10 O 0.2915(3) 0.1001(3) 1.2172(2) 0.0202(5) Uani 1 1 d . . . . .
O11 O 0.9330(4) 0.4716(4) 0.7679(3) 0.0192(5) Uani 1 1 d . . . . .
H5A H 0.294(7) 0.218(7) 0.552(4) 0.034(11) Uiso 1 1 d . . . . .
H5B H 0.161(10) 0.370(10) 0.612(6) 0.07(2) Uiso 1 1 d . . . . .
H10A H 0.190(9) 0.043(9) 1.266(5) 0.071(15) Uiso 1 1 d . . . . .
H10B H 0.241(8) 0.221(8) 1.230(5) 0.051(13) Uiso 1 1 d . . . . .
H11A H 0.867(9) 0.397(9) 0.782(6) 0.075(18) Uiso 1 1 d . . . . .
H11B H 0.994(12) 0.447(12) 0.864(8) 0.08(3) Uiso 1 1 d . . . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
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
Np1 O1 1.7450(19) . ?
Np1 O1 1.7450(19) 2_666 ?
Np1 O5 2.429(4) 2_666 ?
Np1 O5 2.429(4) . ?
Np1 O4 2.4651(18) 2_666 ?
Np1 O4 2.4651(18) . ?
Np1 O2 2.5319(18) . ?
Np1 O2 2.5319(18) 2_666 ?
Np1 N1 2.928(2) 2_666 ?
Np1 N1 2.928(2) . ?
Np2 O6 1.7433(19) 2_657 ?
Np2 O6 1.7433(19) . ?
Np2 O10 2.435(2) 2_657 ?
Np2 O10 2.435(2) . ?
Np2 O9 2.493(2) 2_657 ?
Np2 O9 2.493(2) . ?
Np2 O7 2.507(4) 2_657 ?
Np2 O7 2.507(4) . ?
Np2 N2 2.940(2) . ?
Np2 N2 2.940(2) 2_657 ?
N1 O3 1.214(3) . ?
N1 O4 1.264(3) . ?
N1 O2 1.272(3) . ?
N2 O8 1.211(3) . ?
N2 O7 1.268(5) . ?
N2 O9 1.272(3) . ?
O5 H5A 0.74(5) . ?
O5 H5B 0.76(6) . ?
O10 H10A 1.00(6) . ?
O10 H10B 0.80(5) . ?
O11 H11A 0.83(6) . ?
O11 H11B 1.07(8) . ?
 
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 Np1 O1 180.00(5) . 2_666 ?
O1 Np1 O5 89.54(14) . 2_666 ?
O1 Np1 O5 90.46(14) 2_666 2_666 ?
O1 Np1 O5 90.46(14) . . ?
O1 Np1 O5 89.54(14) 2_666 . ?
O5 Np1 O5 180.0 2_666 . ?
O1 Np1 O4 89.74(8) . 2_666 ?
O1 Np1 O4 90.26(8) 2_666 2_666 ?
O5 Np1 O4 64.20(11) 2_666 2_666 ?
O5 Np1 O4 115.80(11) . 2_666 ?
O1 Np1 O4 90.26(8) . . ?
O1 Np1 O4 89.74(8) 2_666 . ?
O5 Np1 O4 115.80(11) 2_666 . ?
O5 Np1 O4 64.20(11) . . ?
O4 Np1 O4 180.0 2_666 . ?
O1 Np1 O2 88.06(8) . . ?
O1 Np1 O2 91.94(8) 2_666 . ?
O5 Np1 O2 64.91(11) 2_666 . ?
O5 Np1 O2 115.09(11) . . ?
O4 Np1 O2 129.07(6) 2_666 . ?
O4 Np1 O2 50.93(6) . . ?
O1 Np1 O2 91.94(8) . 2_666 ?
O1 Np1 O2 88.06(8) 2_666 2_666 ?
O5 Np1 O2 115.09(11) 2_666 2_666 ?
O5 Np1 O2 64.91(11) . 2_666 ?
O4 Np1 O2 50.93(6) 2_666 2_666 ?
O4 Np1 O2 129.07(6) . 2_666 ?
O2 Np1 O2 180.0 . 2_666 ?
O1 Np1 N1 90.44(8) . 2_666 ?
O1 Np1 N1 89.56(8) 2_666 2_666 ?
O5 Np1 N1 89.48(11) 2_666 2_666 ?
O5 Np1 N1 90.52(11) . 2_666 ?
O4 Np1 N1 25.29(6) 2_666 2_666 ?
O4 Np1 N1 154.71(6) . 2_666 ?
O2 Np1 N1 154.35(6) . 2_666 ?
O2 Np1 N1 25.65(6) 2_666 2_666 ?
O1 Np1 N1 89.56(8) . . ?
O1 Np1 N1 90.44(8) 2_666 . ?
O5 Np1 N1 90.52(11) 2_666 . ?
O5 Np1 N1 89.48(11) . . ?
O4 Np1 N1 154.71(6) 2_666 . ?
O4 Np1 N1 25.29(6) . . ?
O2 Np1 N1 25.65(6) . . ?
O2 Np1 N1 154.35(6) 2_666 . ?
N1 Np1 N1 180.00(7) 2_666 . ?
O6 Np2 O6 180.0 2_657 . ?
O6 Np2 O10 89.02(9) 2_657 2_657 ?
O6 Np2 O10 90.98(9) . 2_657 ?
O6 Np2 O10 90.98(9) 2_657 . ?
O6 Np2 O10 89.02(9) . . ?
O10 Np2 O10 180.00(11) 2_657 . ?
O6 Np2 O9 87.52(9) 2_657 2_657 ?
O6 Np2 O9 92.48(9) . 2_657 ?
O10 Np2 O9 115.95(7) 2_657 2_657 ?
O10 Np2 O9 64.05(7) . 2_657 ?
O6 Np2 O9 92.48(9) 2_657 . ?
O6 Np2 O9 87.52(9) . . ?
O10 Np2 O9 64.05(7) 2_657 . ?
O10 Np2 O9 115.95(7) . . ?
O9 Np2 O9 180.0 2_657 . ?
O6 Np2 O7 91.29(14) 2_657 2_657 ?
O6 Np2 O7 88.71(14) . 2_657 ?
O10 Np2 O7 65.45(11) 2_657 2_657 ?
O10 Np2 O7 114.55(11) . 2_657 ?
O9 Np2 O7 50.75(11) 2_657 2_657 ?
O9 Np2 O7 129.25(11) . 2_657 ?
O6 Np2 O7 88.72(14) 2_657 . ?
O6 Np2 O7 91.29(14) . . ?
O10 Np2 O7 114.55(11) 2_657 . ?
O10 Np2 O7 65.45(11) . . ?
O9 Np2 O7 129.25(11) 2_657 . ?
O9 Np2 O7 50.75(11) . . ?
O7 Np2 O7 180.0 2_657 . ?
O6 Np2 N2 91.35(9) 2_657 . ?
O6 Np2 N2 88.65(9) . . ?
O10 Np2 N2 89.40(7) 2_657 . ?
O10 Np2 N2 90.60(7) . . ?
O9 Np2 N2 154.58(6) 2_657 . ?
O9 Np2 N2 25.42(6) . . ?
O7 Np2 N2 154.65(11) 2_657 . ?
O7 Np2 N2 25.35(11) . . ?
O6 Np2 N2 88.65(9) 2_657 2_657 ?
O6 Np2 N2 91.35(9) . 2_657 ?
O10 Np2 N2 90.60(7) 2_657 2_657 ?
O10 Np2 N2 89.40(7) . 2_657 ?
O9 Np2 N2 25.42(6) 2_657 2_657 ?
O9 Np2 N2 154.58(6) . 2_657 ?
O7 Np2 N2 25.35(11) 2_657 2_657 ?
O7 Np2 N2 154.65(11) . 2_657 ?
N2 Np2 N2 180.0 . 2_657 ?
O3 N1 O4 121.8(2) . . ?
O3 N1 O2 122.3(2) . . ?
O4 N1 O2 115.9(2) . . ?
O3 N1 Np1 177.9(2) . . ?
O4 N1 Np1 56.43(11) . . ?
O2 N1 Np1 59.51(12) . . ?
O8 N2 O7 122.2(3) . . ?
O8 N2 O9 122.7(2) . . ?
O7 N2 O9 115.1(3) . . ?
O8 N2 Np2 177.0(2) . . ?
O7 N2 Np2 57.9(2) . . ?
O9 N2 Np2 57.24(13) . . ?
N1 O2 Np1 94.84(14) . . ?
N1 O4 Np1 98.28(14) . . ?
Np1 O5 H5A 122(3) . . ?
Np1 O5 H5B 125(5) . . ?
H5A O5 H5B 110(5) . . ?
N2 O7 Np2 96.8(3) . . ?
N2 O9 Np2 97.35(15) . . ?
Np2 O10 H10A 127(3) . . ?
Np2 O10 H10B 117(3) . . ?
H10A O10 H10B 107(4) . . ?
H11A O11 H11B 100(5) . . ?
 
_refine_diff_density_max    2.128
_refine_diff_density_min   -3.927
_refine_diff_density_rms    0.352

_shelxl_version_number 2013-2



