#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:18:24 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179240 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/60/4316095.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_4316095
loop_
_publ_author_name
'Clare E. Rowland'
'Christopher L. Cahill'
_publ_contact_author_address
;Department of Chemistry
George Washington University
725 21st Street, NW
Washington, DC 20052
;
_publ_contact_author_email       cahill@gwu.edu
_publ_contact_author_fax         202-994-5873
_publ_contact_author_name        'Christopher L. Cahill'
_publ_contact_author_phone       202-994-6959
_publ_section_title
;
 Hydrothermal Synthesis of Uranyl Squarates and Squarate-Oxalates:
 Hydrolysis Trends and in Situ Oxalate Formation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6716
_journal_page_last               6724
_journal_paper_doi               10.1021/ic100887c
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C6 H O13 U2, H2O, NH4'
_chemical_formula_sum            'C6 H7 N O14 U2'
_chemical_formula_weight         793.176
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.6960(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.4469(6)
_cell_length_b                   7.7589(5)
_cell_length_c                   10.5257(7)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.214
_cell_measurement_theta_min      2.504
_cell_volume                     664.12(8)
_computing_cell_refinement       'ApexII software suite (Bruker AXS)'
_computing_data_collection       'SMART v5.05 (Bruker AXS)'
_computing_data_reduction        'ApexII software suite (Bruker AXS)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker Smart APEXII CCD'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2017
_diffrn_reflns_theta_full        30.42
_diffrn_reflns_theta_max         30.42
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    24.448
_exptl_absorpt_correction_T_max  0.163
_exptl_absorpt_correction_T_min  0.141
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.927
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         11.339
_refine_diff_density_min         -6.112
_refine_diff_density_rms         0.459
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2017
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0382
_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)+(0.0540P)²+1.5504P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.0991
_reflns_number_gt                1787
_reflns_number_total             2017
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100887c_si_002_1.cif
_cod_data_source_block           4
_cod_database_code               4316095
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.27158(5) 0.2500 0.06539(4) 0.00653(13) Uani 1 2 d S . .
U2 U 0.24674(6) 0.2500 0.46412(4) 0.00789(13) Uani 1 2 d S . .
O10 O 0.4787(11) 0.2500 0.1704(8) 0.0097(15) Uani 1 2 d S . .
O11 O 0.0652(12) 0.2500 -0.0379(8) 0.0144(17) Uani 1 2 d S . .
O12 O 0.1576(12) 0.2500 0.2399(8) 0.0110(16) Uani 1 2 d S . .
O13 O 0.2617(8) -0.0474(8) 0.1099(6) 0.0112(12) Uani 1 1 d . . .
O14 O 0.3334(7) 0.0791(8) -0.1136(6) 0.0104(12) Uani 1 1 d . . .
O20 O 0.4545(11) 0.2500 0.4563(9) 0.0128(18) Uani 1 2 d S . .
O21 O 0.0378(12) 0.2500 0.4717(9) 0.0153(19) Uani 1 2 d S . .
O22 O 0.3183(9) 0.0786(8) -0.3313(5) 0.0133(12) Uani 1 1 d . . .
O23 O 0.2285(8) -0.0493(8) 0.4173(5) 0.0122(11) Uani 1 1 d . . .
C1 C 0.2513(9) -0.1559(11) 0.1946(8) 0.0078(15) Uani 1 1 d . . .
C2 C 0.2377(10) -0.1573(11) 0.3304(7) 0.0100(16) Uani 1 1 d . . .
C3 C 0.3288(11) 0.1505(10) -0.2205(7) 0.0096(14) Uani 1 1 d . . .
N1 N -0.1710(12) 0.2500 0.1749(10) 0.0092(19) Uani 1 2 d S . .
OW1 O -0.2804(11) 0.2500 0.3698(8) 0.012 Uiso 1 2 d S . .
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'
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
O11 U1 O10 179.6(4) . . ?
O11 U1 O12 86.3(4) . . ?
O10 U1 O12 93.3(4) . . ?
O11 U1 O13 92.27(16) . 4_565 ?
O10 U1 O13 87.64(16) . 4_565 ?
O12 U1 O13 78.22(14) . 4_565 ?
O11 U1 O13 92.27(16) . . ?
O10 U1 O13 87.64(16) . . ?
O12 U1 O13 78.22(14) . . ?
O13 U1 O13 155.7(3) 4_565 . ?
O11 U1 O14 84.8(3) . 4_565 ?
O10 U1 O14 95.6(3) . 4_565 ?
O12 U1 O14 146.25(15) . 4_565 ?
O13 U1 O14 69.7(2) 4_565 4_565 ?
O13 U1 O14 134.6(2) . 4_565 ?
O11 U1 O14 84.8(3) . . ?
O10 U1 O14 95.6(3) . . ?
O12 U1 O14 146.25(15) . . ?
O13 U1 O14 134.6(2) 4_565 . ?
O13 U1 O14 69.7(2) . . ?
O14 U1 O14 64.9(3) 4_565 . ?
O20 U2 O21 179.9(4) . . ?
O20 U2 O12 90.3(4) . . ?
O21 U2 O12 89.6(4) . . ?
O20 U2 O23 89.99(17) . . ?
O21 U2 O23 89.99(17) . . ?
O12 U2 O23 78.43(13) . . ?
O20 U2 O23 89.99(17) . 4_565 ?
O21 U2 O23 89.99(17) . 4_565 ?
O12 U2 O23 78.43(13) . 4_565 ?
O23 U2 O23 156.9(3) . 4_565 ?
O20 U2 O22 91.7(3) . 1_556 ?
O21 U2 O22 88.4(3) . 1_556 ?
O12 U2 O22 147.26(14) . 1_556 ?
O23 U2 O22 68.89(19) . 1_556 ?
O23 U2 O22 134.23(19) 4_565 1_556 ?
O20 U2 O22 91.7(3) . 4_566 ?
O21 U2 O22 88.4(3) . 4_566 ?
O12 U2 O22 147.26(14) . 4_566 ?
O23 U2 O22 134.23(19) . 4_566 ?
O23 U2 O22 68.89(19) 4_565 4_566 ?
O22 U2 O22 65.3(3) 1_556 4_566 ?
U2 O12 U1 137.6(4) . . ?
C1 O13 U1 144.6(5) . . ?
C3 O14 U1 119.2(5) . . ?
C3 O22 U2 120.2(5) . 1_554 ?
C2 O23 U2 142.2(5) . . ?
O13 C1 C1 132.5(5) . 4 ?
O13 C1 C2 137.9(7) . . ?
C1 C1 C2 89.6(4) 4 . ?
O23 C2 C2 131.8(5) . 4 ?
O23 C2 C1 137.8(7) . . ?
C2 C2 C1 90.4(4) 4 . ?
O14 C3 O22 127.6(8) . . ?
O14 C3 C3 116.4(5) . 4_565 ?
O22 C3 C3 116.0(4) . 4_565 ?
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 O11 1.787(9) . ?
U1 O10 1.799(8) . ?
U1 O12 2.293(8) . ?
U1 O13 2.361(6) 4_565 ?
U1 O13 2.361(6) . ?
U1 O14 2.472(6) 4_565 ?
U1 O14 2.472(6) . ?
U2 O20 1.779(9) . ?
U2 O21 1.788(9) . ?
U2 O12 2.275(8) . ?
U2 O23 2.370(6) . ?
U2 O23 2.370(6) 4_565 ?
U2 O22 2.463(5) 1_556 ?
U2 O22 2.463(5) 4_566 ?
O13 C1 1.246(10) . ?
O14 C3 1.245(9) . ?
O22 C3 1.274(9) . ?
O22 U2 2.463(5) 1_554 ?
O23 C2 1.258(10) . ?
C1 C1 1.460(17) 4 ?
C1 C2 1.464(11) . ?
C2 C2 1.439(17) 4 ?
C3 C3 1.543(16) 4_565 ?
