#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/18/7051804.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_7051804
loop_
_publ_author_name
'Ye, Chengfeng'
'Gao, Haixiang'
'Twamley, Brendan'
'Shreeve, Jean’ne M.'
_publ_section_title
;
 Dense energetic salts of N,N′-dinitrourea (DNU)
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              317
_journal_paper_doi               10.1039/b712417a
_journal_volume                  32
_journal_year                    2008
_chemical_formula_moiety         'C1 H2 N4 O5'
_chemical_formula_sum            'C H2 N4 O5'
_chemical_formula_weight         150.07
_chemical_name_common            DNU
_chemical_name_systematic
;
?
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.0015(9)
_cell_length_b                   17.6425(13)
_cell_length_c                   4.5555(4)
_cell_measurement_reflns_used    2824
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      4.10
_cell_volume                     964.57(13)
_computing_cell_refinement       'Bruker, 2006; APEX2, SAINT+ v.7.23a'
_computing_data_collection       'Bruker, 2006; APEX2v2.1-RC12'
_computing_data_reduction        'Bruker, 2006; APEX2, SAINT+ v.7.23a'
_computing_molecular_graphics    'Bruker, 2003; XP, SHELXTL v.6.14'
_computing_publication_material  'Bruker, 2001; APEX2, XCIF v.6.12'
_computing_structure_refinement  'Bruker, 2003; XL,SHELXTL v.6.14''
_computing_structure_solution    'Bruker, 2003; XS, SHELXTL v.6.14'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker/Siemens SMART APEX'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0100
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            3712
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         4.11
_exptl_absorpt_coefficient_mu    0.210
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2004/1 ; Bruker, 2004'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.067
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         389
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0236
_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)+(0.0406P)²+0.7359P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0617
_refine_ls_wR_factor_ref         0.0620
_reflns_number_gt                379
_reflns_number_total             389
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b712417a.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      Fdd2
_cod_original_formula_sum        'C1 H2 N4 O5'
_cod_database_code               7051804
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'
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
C1 C 1.0000 0.0000 0.3458(5) 0.0102(4) Uani 1 2 d S . .
O1 O 0.83007(9) 0.09249(6) 0.1687(3) 0.0172(3) Uani 1 1 d . . .
O2 O 0.74402(8) 0.07043(6) 0.5793(3) 0.0174(3) Uani 1 1 d . . .
O3 O 1.0000 0.0000 0.0808(4) 0.0135(3) Uani 1 2 d S . .
N1 N 0.82298(9) 0.06486(6) 0.4120(3) 0.0113(2) Uani 1 1 d . . .
N2 N 0.91170(9) 0.02257(7) 0.5221(3) 0.0113(2) Uani 1 1 d . . .
H2A H 0.9117 0.0098 0.7088 0.014 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0099(8) 0.0110(7) 0.0097(9) 0.000 0.000 -0.0007(6)
O1 0.0192(5) 0.0202(5) 0.0120(5) 0.0054(4) 0.0012(4) 0.0055(4)
O2 0.0131(4) 0.0239(5) 0.0151(5) 0.0010(5) 0.0043(4) 0.0053(4)
O3 0.0136(6) 0.0184(6) 0.0087(6) 0.000 0.000 0.0023(5)
N1 0.0107(5) 0.0115(5) 0.0115(5) -0.0010(5) -0.0013(5) 0.0014(4)
N2 0.0104(5) 0.0156(5) 0.0079(5) 0.0017(4) -0.0002(4) 0.0031(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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0000 '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
O3 C1 N2 125.35(9) . 2_755 ?
O3 C1 N2 125.35(9) . . ?
N2 C1 N2 109.29(18) 2_755 . ?
O1 N1 O2 126.34(12) . . ?
O1 N1 N2 119.34(12) . . ?
O2 N1 N2 114.32(12) . . ?
C1 N2 N1 121.92(12) . . ?
C1 N2 H2A 119.0 . . ?
N1 N2 H2A 119.0 . . ?
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
C1 O3 1.207(3) . ?
C1 N2 1.3880(17) 2_755 ?
C1 N2 1.3880(17) . ?
O1 N1 1.2135(17) . ?
O2 N1 1.2200(16) . ?
N1 N2 1.3936(15) . ?
N2 H2A 0.8800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2A O3 0.88 2.01 2.786(2) 147.0 1_556
