#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:16:27 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179369 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/66/4326617.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_4326617
loop_
_publ_author_name
'Richard E. Wilson'
'S. Skanthakumar'
'C. L. Cahill'
'L. Soderholm'
_publ_section_title
;
 Structural Studies Coupling X-ray Diffraction and High-Energy X-ray
 Scattering in the UO22+-HBraq System
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10748
_journal_page_last               10754
_journal_paper_doi               10.1021/ic201265s
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'Br4 N2 O4 U'
_chemical_formula_weight         649.65
_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_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.075(2)
_cell_angle_beta                 95.036(2)
_cell_angle_gamma                116.486(2)
_cell_formula_units_Z            1
_cell_length_a                   6.7769(13)
_cell_length_b                   6.8215(13)
_cell_length_c                   7.6799(14)
_cell_measurement_reflns_used    2082
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.76
_cell_measurement_theta_min      4.52
_cell_volume                     310.05(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       '0.3 deg w/exposures'
_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  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5377
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         33.76
_diffrn_reflns_theta_min         4.52
_exptl_absorpt_coefficient_mu    25.954
_exptl_absorpt_correction_T_max  0.1811
_exptl_absorpt_correction_T_min  0.1811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.479
_exptl_crystal_description       prism
_exptl_crystal_F_000             278
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.606
_refine_diff_density_min         -2.715
_refine_diff_density_rms         0.316
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     52
_refine_ls_number_reflns         2288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0265
_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)+(0.0381P)²+0.5897P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0715
_reflns_number_gt                2082
_reflns_number_total             2288
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201265s_si_001_2.cif
_cod_data_source_block           p1ammonium
_cod_database_code               4326617
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
U1 U 0.0000 0.5000 0.0000 0.00810(7) Uani 1 2 d S
Br1 Br 0.39814(7) 0.68329(7) -0.14312(6) 0.01239(10) Uani 1 1 d .
Br2 Br 0.23119(8) 0.73768(7) 0.34545(6) 0.01289(10) Uani 1 1 d .
O1 O -0.0465(6) 0.7287(5) -0.0339(5) 0.0123(6) Uani 1 1 d .
O2 O 0.2349(6) 0.2661(6) 0.4337(5) 0.0154(6) Uani 1 1 d .
N1 N 0.2121(7) 0.0633(7) 0.7371(5) 0.0139(7) Uani 1 1 d .
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
U1 0.00889(10) 0.00895(10) 0.00717(10) 0.00206(7) 0.00197(7) 0.00452(7)
Br1 0.0106(2) 0.0153(2) 0.0116(2) 0.00380(15) 0.00393(15) 0.00561(16)
Br2 0.0141(2) 0.0138(2) 0.00893(19) -0.00013(15) 0.00019(16) 0.00593(16)
O1 0.0139(15) 0.0112(14) 0.0139(15) 0.0041(11) 0.0027(12) 0.0070(12)
O2 0.0188(17) 0.0148(15) 0.0133(15) 0.0052(12) 0.0039(13) 0.0077(13)
N1 0.0151(18) 0.0175(18) 0.0115(17) 0.0047(14) 0.0017(14) 0.0094(15)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Br Br -0.2901 2.4595 '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
O1 U1 O1 180.000(1) 2_565 .
O1 U1 Br2 89.19(11) 2_565 2_565
O1 U1 Br2 90.81(11) . 2_565
O1 U1 Br2 90.81(11) 2_565 .
O1 U1 Br2 89.19(11) . .
Br2 U1 Br2 180.000(11) 2_565 .
O1 U1 Br1 90.03(11) 2_565 .
O1 U1 Br1 89.97(11) . .
Br2 U1 Br1 88.707(17) 2_565 .
Br2 U1 Br1 91.293(17) . .
O1 U1 Br1 89.97(11) 2_565 2_565
O1 U1 Br1 90.03(11) . 2_565
Br2 U1 Br1 91.293(17) 2_565 2_565
Br2 U1 Br1 88.707(17) . 2_565
Br1 U1 Br1 180.0 . 2_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.772(3) 2_565
U1 O1 1.772(3) .
U1 Br2 2.8139(6) 2_565
U1 Br2 2.8139(6) .
U1 Br1 2.8194(6) .
U1 Br1 2.8194(6) 2_565
