#------------------------------------------------------------------------------
#$Date: 2016-03-22 22:43:21 +0100 (Tue 22 de Mar de 2016) $
#$Revision: 179074 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/36/4303684.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_4303684
loop_
_publ_author_name
'Margaret-Jane Crawford'
'Arkady Ellern'
'Konstantin Karaghiosoff'
'Peter Mayer'
_publ_contact_author_address
;
Department Chemie
Ludwig-Maximilians Universität
Butenandtstraße 5-13 (Haus D)
D-81377 München
Bundesrepublik Deutschland
;
_publ_contact_author_email       mjc@cup.uni-muenchen.de
_publ_contact_author_fax         +49-89-2180-77492
_publ_contact_author_name        'M.-J. Crawford'
_publ_contact_author_phone       +49-89-2180-77491
_publ_section_title
;
Nitrate and Perchlorate Complexes of Uranium(IV)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10877
_journal_page_last               10879
_journal_paper_doi               10.1021/ic901386y
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C10 H15 Cl4 N5 O16 U'
_chemical_formula_weight         841.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           104
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4 -2n'
_symmetry_space_group_name_H-M   'P 4 n c'
_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            2
_cell_length_a                   10.65500(10)
_cell_length_b                   10.65500(10)
_cell_length_c                   11.1445(2)
_cell_measurement_reflns_used    20186
_cell_measurement_temperature    200
_cell_measurement_theta_max      29.9988
_cell_measurement_theta_min      3.6534
_cell_volume                     1265.22(3)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Oxford XCalibur'
_diffrn_measurement_method       'phi and omega 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  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0117
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            33325
_diffrn_reflns_theta_full        30.17
_diffrn_reflns_theta_max         30.17
_diffrn_reflns_theta_min         3.66
_exptl_absorpt_coefficient_mu    6.916
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    2.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.516
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.038(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1868
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0156
_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)+(0.0157P)²+1.7115P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0356
_refine_ls_wR_factor_ref         0.0429
_reflns_number_gt                1483
_reflns_number_total             1868
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901386y_si_001_4.cif
_cod_data_source_block           dx079
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4303684
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
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
U1 U 0.0000 1.0000 0.64553(5) 0.01972(5) Uani 1 4 d S . .
Cl3 Cl 0.16095(9) 0.69615(8) 0.57651(10) 0.03857(19) Uani 1 1 d . . .
O4 O 0.0921(2) 0.8176(2) 0.5689(3) 0.0322(5) Uani 1 1 d . . .
O1 O 0.2799(4) 0.7217(4) 0.6220(6) 0.098(2) Uani 1 1 d . . .
O2 O 0.0877(5) 0.6141(3) 0.6454(5) 0.1025(19) Uani 1 1 d . . .
O3 O 0.1723(3) 0.6505(3) 0.4591(3) 0.0542(9) Uani 1 1 d . . .
N3 N -0.0600(3) 0.8256(3) 0.7826(3) 0.0319(7) Uani 1 1 d . . .
N4 N 0.0000 1.0000 0.4109(6) 0.0302(12) Uani 1 4 d S . .
C3 C 0.0000 1.0000 0.3089(6) 0.0282(13) Uani 1 4 d S . .
C6 C -0.0943(4) 0.7346(4) 0.8215(3) 0.0321(8) Uani 1 1 d . . .
C7 C 0.0000 1.0000 0.1773(7) 0.043(2) Uani 1 4 d S . .
C8 C -0.1388(5) 0.6144(4) 0.8681(4) 0.0437(11) Uani 1 1 d . . .
H8A H -0.1159 0.5485 0.8136 0.052 Uiso 1 1 calc R . .
H8B H -0.2285 0.6169 0.8763 0.052 Uiso 1 1 calc R . .
H8C H -0.1014 0.5990 0.9451 0.052 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
U1 0.01676(6) 0.01676(6) 0.02566(9) 0.000 0.000 0.000
Cl3 0.0406(5) 0.0291(4) 0.0461(5) -0.0069(4) -0.0006(5) 0.0120(3)
O4 0.0320(13) 0.0242(11) 0.0406(14) -0.0010(13) 0.0021(13) 0.0081(10)
O1 0.069(2) 0.094(3) 0.129(6) -0.063(3) -0.056(3) 0.055(2)
O2 0.158(5) 0.0376(17) 0.111(3) 0.029(3) 0.077(4) 0.031(2)
O3 0.057(2) 0.051(2) 0.0549(19) -0.0235(17) 0.0068(18) 0.0087(17)
N3 0.0249(15) 0.0298(16) 0.0411(17) 0.0026(15) 0.0017(14) 0.0002(13)
N4 0.0295(17) 0.0295(17) 0.032(3) 0.000 0.000 0.000
C3 0.0252(19) 0.0252(19) 0.034(4) 0.000 0.000 0.000
C6 0.0280(19) 0.032(2) 0.0357(19) 0.0043(15) 0.0040(14) 0.0001(15)
C7 0.049(3) 0.049(3) 0.032(4) 0.000 0.000 0.000
C8 0.041(2) 0.032(2) 0.058(3) 0.010(2) 0.006(2) -0.0047(18)
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
N N 0.0061 0.0033 '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
O4 U1 O4 137.19(15) 4_465 3_665 ?
O4 U1 O4 82.34(5) 4_465 . ?
O4 U1 O4 82.34(5) 3_665 . ?
O4 U1 O4 82.34(5) 4_465 2_575 ?
O4 U1 O4 82.34(5) 3_665 2_575 ?
O4 U1 O4 137.19(15) . 2_575 ?
O4 U1 N3 138.66(9) 4_465 2_575 ?
O4 U1 N3 72.37(12) 3_665 2_575 ?
O4 U1 N3 137.45(10) . 2_575 ?
O4 U1 N3 73.22(10) 2_575 2_575 ?
O4 U1 N3 137.45(10) 4_465 3_665 ?
O4 U1 N3 73.22(11) 3_665 3_665 ?
O4 U1 N3 72.37(12) . 3_665 ?
O4 U1 N3 138.66(9) 2_575 3_665 ?
N3 U1 N3 67.88(9) 2_575 3_665 ?
O4 U1 N3 72.37(12) 4_465 . ?
O4 U1 N3 138.66(9) 3_665 . ?
O4 U1 N3 73.22(10) . . ?
O4 U1 N3 137.45(10) 2_575 . ?
N3 U1 N3 104.30(17) 2_575 . ?
N3 U1 N3 67.88(9) 3_665 . ?
O4 U1 N3 73.22(11) 4_465 4_465 ?
O4 U1 N3 137.45(10) 3_665 4_465 ?
O4 U1 N3 138.66(9) . 4_465 ?
O4 U1 N3 72.37(12) 2_575 4_465 ?
N3 U1 N3 67.88(9) 2_575 4_465 ?
N3 U1 N3 104.30(17) 3_665 4_465 ?
N3 U1 N3 67.88(9) . 4_465 ?
O4 U1 N4 68.59(7) 4_465 . ?
O4 U1 N4 68.59(7) 3_665 . ?
O4 U1 N4 68.59(7) . . ?
O4 U1 N4 68.59(7) 2_575 . ?
N3 U1 N4 127.85(8) 2_575 . ?
N3 U1 N4 127.85(8) 3_665 . ?
N3 U1 N4 127.85(8) . . ?
N3 U1 N4 127.85(8) 4_465 . ?
O1 Cl3 O2 115.5(4) . . ?
O1 Cl3 O3 109.2(3) . . ?
O2 Cl3 O3 110.1(3) . . ?
O1 Cl3 O4 107.4(2) . . ?
O2 Cl3 O4 107.4(2) . . ?
O3 Cl3 O4 106.9(2) . . ?
Cl3 O4 U1 155.2(2) . . ?
C6 N3 U1 164.8(3) . . ?
C3 N4 U1 180.000(2) . . ?
N4 C3 C7 180.000(3) . . ?
N3 C6 C8 178.1(4) . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
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
U1 O4 2.339(2) 4_465 ?
U1 O4 2.339(2) 3_665 ?
U1 O4 2.339(2) . ?
U1 O4 2.339(2) 2_575 ?
U1 N3 2.489(3) 2_575 ?
U1 N3 2.489(3) 3_665 ?
U1 N3 2.489(3) . ?
U1 N3 2.489(3) 4_465 ?
U1 N4 2.615(6) . ?
Cl3 O1 1.392(4) . ?
Cl3 O2 1.401(4) . ?
Cl3 O3 1.401(3) . ?
Cl3 O4 1.489(2) . ?
N3 C6 1.123(5) . ?
N4 C3 1.137(10) . ?
C3 C7 1.467(10) . ?
C6 C8 1.461(6) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
