##############################################################################
###                                                                        ###
###        Electronic paper (Acta Crystallographica Section E)             ###
###                                                                        ###
##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section E. It conforms to the requirements of Notes      #
# for Authors for Section E, and has been peer reviewed under the auspices   #
# of the IUCr Commission on Journals.                                        #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
# cif/home.html                                                              #
#                                                                            #
#            Copyright International Union of Crystallography                #
#                                                                            #
##############################################################################
                                             
data_global
_audit_creation_method     'from SHELXL97 CIF'
_journal_date_recd_electronic     2004-06-09
_journal_date_accepted     2004-06-11
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2004
_journal_volume     60
_journal_issue      7
_journal_page_first     m973
_journal_page_last     m975
_journal_paper_category     EM
_publ_contact_author_name     'Dr. Thomas E. Albrecht-Schmitt'
_publ_contact_author_address
;
Department of Chemistry,
Auburn University,
Auburn,
Alabama,
USA 36849
;
_publ_contact_author_email     albreth@auburn.edu
_publ_contact_author_fax     ' 334 844 6959 '
_publ_contact_author_phone     ' 334 844 6948 '
_publ_section_title
;
Ethylenediammonium decafluorodineptunium
;
loop_
    _publ_author_name
    _publ_author_address
    'Sullens, Tyler A.'
;
Department of Chemistry and Leach Nuclear Science Center
Auburn University
Auburn
Alabama 36849
USA
;
    'Almond, Philip M.'
;
Department of Chemistry and Leach Nuclear Science Center
Auburn University
Auburn
Alabama 36849
USA
;
    'Albrecht-Schmitt, T. E.'
;
Department of Chemistry and Leach Nuclear Science Center
Auburn University
Auburn
Alabama 36849
USA
;
data_I
_audit_creation_method     SHELXL-97
_chemical_name_systematic
;
;
_chemical_name_common     'ethylene diammonium dineptunium decafluoride'
_chemical_formula_moiety     'F10 Np2, C2 H10 N2'
_chemical_formula_sum     'C2 H10 F10 N2 Np2'
_chemical_formula_iupac     '(C2 H10 N2) [Np2 F10]'
_chemical_formula_weight     726.12
_chemical_melting_point     ?
_symmetry_cell_setting     'monoclinic'
_symmetry_space_group_name_H-M     'C 2/c'
_symmetry_space_group_name_Hall     '-c_2yc'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, y, -z+1/2'
    'x+1/2, y+1/2, z'
    '-x+1/2, y+1/2, -z+1/2'
    '-x, -y, -z'
    'x, -y, z-1/2'
    '-x+1/2, -y+1/2, -z'
    'x+1/2, -y+1/2, z-1/2'
_cell_length_a     16.0190(11)
_cell_length_b     7.0570(5)
_cell_length_c     8.7203(6)
_cell_angle_alpha     90
_cell_angle_beta     91.5360(10)
_cell_angle_gamma     90
_cell_volume     985.44(12)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     4826
_cell_measurement_theta_min     3.15
_cell_measurement_theta_max     28.27
_cell_measurement_temperature     193(2)
_exptl_crystal_description     'prism'
_exptl_crystal_colour     'green'
_exptl_crystal_size_max     0.108
_exptl_crystal_size_mid     0.070
_exptl_crystal_size_min     0.050
_exptl_crystal_density_diffrn     4.894
_exptl_crystal_density_meas     'not measured'
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     1248
_exptl_absorpt_coefficient_mu     21.101
_exptl_absorpt_correction_type     'analytical'
_exptl_absorpt_process_details
;
SHELXPREP97 in SHELXTL97 (Sheldrick, 2000) and SADABS (Sheldrick, 1997)
;
_exptl_absorpt_correction_T_min     0.1256
_exptl_absorpt_correction_T_max     0.3710
_exptl_special_details
;
;
_diffrn_ambient_temperature     193(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Bruker APEX'
_diffrn_measurement_method     '0.3 ω exposures'
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     4826
_diffrn_reflns_av_R_equivalents     0.0216
_diffrn_reflns_av_sigmaI/netI     0.0188
_diffrn_reflns_theta_min     3.15
_diffrn_reflns_theta_max     28.27
_diffrn_reflns_theta_full     28.27
_diffrn_measured_fraction_theta_max     0.998
_diffrn_measured_fraction_theta_full     0.998
_diffrn_reflns_limit_h_min     -21
_diffrn_reflns_limit_h_max     21
_diffrn_reflns_limit_k_min     -9
_diffrn_reflns_limit_k_max     9
_diffrn_reflns_limit_l_min     -11
_diffrn_reflns_limit_l_max     11
_diffrn_standards_number     0
_diffrn_standards_interval_count     0
_diffrn_standards_interval_time     0
_diffrn_standards_decay_%     0
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_reflns_number_total     1224
_reflns_number_gt     1185
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0157
_refine_ls_R_factor_gt     0.0144
_refine_ls_wR_factor_gt     0.0327
_refine_ls_wR_factor_ref     0.0331
_refine_ls_goodness_of_fit_ref     1.151
_refine_ls_restrained_S_all     1.151
_refine_ls_number_reflns     1224
_refine_ls_number_parameters     74
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     mixed
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
     'calc w = 1/[σ²(Fo²)+(0.0131P)²+2.3052P] where P = (Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.002
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.843
_refine_diff_density_min     -0.741
_refine_ls_extinction_method     SHELXTL97
_refine_ls_extinction_coef     0.00049(5)
_refine_ls_extinction_expression
                                  'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
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'
    'Np' 'Np' -11.4937 4.1493
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'F' 'F' 0.0171 0.0103
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'SMART (Bruker, 2000)'
_computing_cell_refinement     'SMART and SAINT (Bruker, 1999)'
_computing_data_reduction     'SAINT'
_computing_structure_solution     'SHELXS97 in SHELXTL97 (Sheldrick, 2000)'
_computing_structure_refinement     'SHELXL97 in SHELXTL97'
_computing_molecular_graphics     'SHELXP97 in SHELXTL97'
_computing_publication_material     'SHELXCIF97 in in SHELXTL97'
loop_
    _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_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Np1 0.219411(7) -0.906689(17) 0.670144(13) 0.00792(7) Uani d . 1 . . Np
    F1 0.32224(12) -0.8217(3) 0.5047(2) 0.0121(4) Uani d . 1 . . F
    F2 0.31883(12) -0.7240(3) 0.7957(2) 0.0128(4) Uani d . 1 . . F
    F3 0.08169(13) -0.9249(3) 0.6639(2) 0.0151(4) Uani d . 1 . . F
    F4 0.19746(13) -0.9529(3) 0.9285(2) 0.0130(4) Uani d . 1 . . F
    F5 0.17109(13) -0.6151(3) 0.7876(2) 0.0125(4) Uani d . 1 . . F
    N1 0.54642(18) -0.7570(4) 0.4833(3) 0.0153(6) Uani d . 1 . . N
    H1A 0.5617 -0.6696 0.5554 0.023 Uiso calc R 1 . . H
    H1B 0.5065 -0.7069 0.4191 0.023 Uiso calc R 1 . . H
    H1E 0.5917 -0.7901 0.4284 0.023 Uiso calc R 1 . . H
    C1 0.5127(2) -0.9275(5) 0.5599(4) 0.0148(7) Uani d . 1 . . C
    H1C 0.4637 -0.8920 0.6206 0.018 Uiso calc R 1 . . H
    H1D 0.5557 -0.9818 0.6307 0.018 Uiso calc R 1 . . H
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    Np1 0.00944(9) 0.00774(9) 0.00655(8) -0.00003(4) -0.00027(5) 0.00017(4)
    F1 0.0119(9) 0.0119(10) 0.0126(9) 0.0014(7) 0.0018(7) 0.0007(7)
    F2 0.0122(10) 0.0112(9) 0.0146(9) 0.0015(7) -0.0032(8) -0.0018(8)
    F3 0.0123(10) 0.0138(10) 0.0191(11) 0.0003(7) 0.0003(8) 0.0018(8)
    F4 0.0184(10) 0.0112(9) 0.0096(9) 0.0003(8) 0.0012(8) 0.0014(8)
    F5 0.0143(10) 0.0110(9) 0.0121(10) 0.0000(7) -0.0009(8) -0.0016(7)
    N1 0.0138(14) 0.0162(16) 0.0157(14) -0.0010(11) -0.0024(11) 0.0015(12)
    C1 0.0129(17) 0.0177(18) 0.0137(17) -0.0014(13) 0.0009(13) 0.0010(13)
_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_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Np1 F3 . 2.209(2) yes
    Np1 F1 . 2.2981(19) yes
    Np1 F2 . 2.3029(19) yes
    Np1 F1 7_536 2.3053(19) yes
    Np1 F5 4_546 2.311(2) yes
    Np1 F4 . 2.3124(19) yes
    Np1 F2 4_546 2.343(2) yes
    Np1 F4 6_535 2.3467(19) yes
    Np1 F5 . 2.4341(19) yes
    Np1 Np1 7_536 3.8487(3) yes
    Np1 Np1 4_556 3.9086(3) yes
    N1 C1 . 1.485(4) no
    N1 H1A . 0.9100 no
    N1 H1B . 0.9100 no
    N1 H1E . 0.9100 no
    C1 C1 5_636 1.511(7) no
    C1 H1C . 0.9900 no
    C1 H1D . 0.9900 no
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    F3 Np1 F1 . . 137.04(7) no
    F3 Np1 F2 . . 136.20(7) no
    F1 Np1 F2 . . 69.77(7) no
    F3 Np1 F1 . 7_536 75.72(7) no
    F1 Np1 F1 . 7_536 66.54(8) no
    F2 Np1 F1 . 7_536 96.16(7) no
    F3 Np1 F5 . 4_546 136.06(7) no
    F1 Np1 F5 . 4_546 73.28(7) no
    F2 Np1 F5 . 4_546 76.61(7) no
    F1 Np1 F5 7_536 4_546 139.06(7) no
    F3 Np1 F4 . . 80.67(8) no
    F1 Np1 F4 . . 141.13(7) no
    F2 Np1 F4 . . 74.76(7) no
    F1 Np1 F4 7_536 . 133.96(7) no
    F5 Np1 F4 4_546 . 83.66(7) no
    F3 Np1 F2 . 4_546 71.52(7) no
    F1 Np1 F2 . 4_546 121.57(7) no
    F2 Np1 F2 . 4_546 130.88(5) no
    F1 Np1 F2 7_536 4_546 132.88(7) no
    F5 Np1 F2 4_546 4_546 64.61(7) no
    F4 Np1 F2 . 4_546 72.20(7) no
    F3 Np1 F4 . 6_535 80.08(7) no
    F1 Np1 F4 . 6_535 68.85(7) no
    F2 Np1 F4 . 6_535 138.45(7) no
    F1 Np1 F4 7_536 6_535 70.58(7) no
    F5 Np1 F4 4_546 6_535 88.23(7) no
    F4 Np1 F4 . 6_535 142.40(5) no
    F2 Np1 F4 4_546 6_535 71.16(7) no
    F3 Np1 F5 . . 74.40(7) no
    F1 Np1 F5 . . 106.56(7) no
    F2 Np1 F5 . . 63.28(7) no
    F1 Np1 F5 7_536 . 66.28(7) no
    F5 Np1 F5 4_546 . 136.01(3) no
    F4 Np1 F5 . . 69.56(7) no
    F2 Np1 F5 4_546 . 131.86(7) no
    F4 Np1 F5 6_535 . 133.89(7) no
    F3 Np1 Np1 . 7_536 106.81(5) no
    F1 Np1 Np1 . 7_536 33.33(5) no
    F2 Np1 Np1 . 7_536 81.82(5) no
    F1 Np1 Np1 7_536 7_536 33.21(5) no
    F5 Np1 Np1 4_546 7_536 106.30(5) no
    F4 Np1 Np1 . 7_536 151.72(5) no
    F2 Np1 Np1 4_546 7_536 136.07(5) no
    F4 Np1 Np1 6_535 7_536 65.51(5) no
    F5 Np1 Np1 . 7_536 85.94(5) no
    F3 Np1 Np1 . 4_556 107.58(5) no
    F1 Np1 Np1 . 4_556 79.11(5) no
    F2 Np1 Np1 . 4_556 33.03(5) no
    F1 Np1 Np1 7_536 4_556 70.72(5) no
    F5 Np1 Np1 4_546 4_556 109.62(5) no
    F4 Np1 Np1 . 4_556 79.83(5) no
    F2 Np1 Np1 4_546 4_556 151.83(5) no
    F4 Np1 Np1 6_535 4_556 137.00(5) no
    F5 Np1 Np1 . 4_556 33.53(5) no
    Np1 Np1 Np1 7_536 4_556 71.905(6) no
    F3 Np1 Np1 . 4_546 101.35(5) no
    F1 Np1 Np1 . 4_546 106.39(5) no
    F2 Np1 Np1 . 4_546 99.93(5) no
    F1 Np1 Np1 7_536 4_546 158.79(5) no
    F5 Np1 Np1 4_546 4_546 35.58(5) no
    F4 Np1 Np1 . 4_546 64.46(5) no
    F2 Np1 Np1 4_546 4_546 32.40(5) no
    F4 Np1 Np1 6_535 4_546 88.22(5) no
    F5 Np1 Np1 . 4_546 133.84(5) no
    Np1 Np1 Np1 7_536 4_546 136.624(7) no
    Np1 Np1 Np1 4_556 4_546 129.045(8) no
    Np1 F1 Np1 . 7_536 113.46(8) no
    Np1 F2 Np1 . 4_556 114.56(8) no
    Np1 F4 Np1 . 6_536 155.69(10) no
    Np1 F5 Np1 4_556 . 110.89(8) no
    C1 N1 H1A . . 109.5 no
    C1 N1 H1B . . 109.5 no
    H1A N1 H1B . . 109.5 no
    C1 N1 H1E . . 109.5 no
    H1A N1 H1E . . 109.5 no
    H1B N1 H1E . . 109.5 no
    N1 C1 C1 . 5_636 109.4(4) no
    N1 C1 H1C . . 109.8 no
    C1 C1 H1C 5_636 . 109.8 no
    N1 C1 H1D . . 109.8 no
    C1 C1 H1D 5_636 . 109.8 no
    H1C C1 H1D . . 108.2 no
