#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:26:43 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179412 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/09/4330976.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_4330976
loop_
_publ_author_name
'Pius O. Adelani'
'Laurent J. Jouffret'
'Jennifer E. S. Szymanowski'
'Peter C. Burns'
_publ_section_title
;
 Correlations and Differences between Uranium(VI) Arsonates and
 Phosphonates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12032
_journal_page_last               12040
_journal_paper_doi               10.1021/ic301942t
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C12 H12 As2 O8 U'
_chemical_formula_sum            'C12 H12 As2 O8 U'
_chemical_formula_weight         672.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 103.727(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.917(8)
_cell_length_b                   7.018(3)
_cell_length_c                   12.667(6)
_cell_measurement_reflns_used    6238
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      2.34
_cell_volume                     1547.3(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16977
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.17
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.774
_exptl_absorpt_correction_T_max  0.4422
_exptl_absorpt_correction_T_min  0.1855
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SHELXPREP
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.885
_exptl_crystal_description       'rectangular tablet'
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.160
_refine_diff_density_min         -1.073
_refine_diff_density_rms         0.170
_refine_ls_extinction_coef       0.00019(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0102P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0431
_refine_ls_wR_factor_ref         0.0452
_reflns_number_gt                3045
_reflns_number_total             3515
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301942t_si_002_1.cif
_cod_data_source_block           p21c
_cod_original_cell_volume        1547.2(12)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4330976
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-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
U1 U 0.743309(9) 0.21672(2) 0.324221(12) 0.00703(5) Uani 1 1 d .
As1 As 0.71976(2) 0.52739(6) 0.55111(3) 0.00771(10) Uani 1 1 d .
As2 As 0.78240(2) 0.78827(6) 0.75502(3) 0.00743(9) Uani 1 1 d .
O1 O 0.64381(17) 0.2198(4) 0.3199(2) 0.0125(6) Uani 1 1 d .
O2 O 0.84333(16) 0.2096(4) 0.3324(2) 0.0111(6) Uani 1 1 d .
O3 O 0.7689(2) 0.0764(5) 0.5109(2) 0.0159(7) Uani 1 1 d .
H3C H 0.764(2) -0.023(6) 0.528(3) 0.006(13) Uiso 1 1 d .
H3B H 0.751(3) 0.125(7) 0.559(4) 0.022(15) Uiso 1 1 d .
O4 O 0.76204(16) 0.4662(4) 0.4533(2) 0.0102(6) Uani 1 1 d .
O5 O 0.71832(17) 0.3480(4) 0.6365(2) 0.0108(6) Uani 1 1 d .
O6 O 0.78181(16) 0.7037(4) 0.6219(2) 0.0097(6) Uani 1 1 d .
O7 O 0.73366(16) 0.9909(4) 0.7287(2) 0.0089(6) Uani 1 1 d .
O8 O 0.73984(16) 0.6226(4) 0.8135(2) 0.0103(6) Uani 1 1 d .
C1 C 0.6214(2) 0.6387(6) 0.5014(3) 0.0108(9) Uani 1 1 d .
C2 C 0.5946(3) 0.6840(6) 0.3921(3) 0.0147(10) Uani 1 1 d .
H2A H 0.6252 0.6634 0.3434 0.018 Uiso 1 1 calc R
C3 C 0.5215(3) 0.7602(6) 0.3568(4) 0.0191(10) Uani 1 1 d .
H3A H 0.5029 0.7910 0.2839 0.023 Uiso 1 1 calc R
C4 C 0.4760(3) 0.7907(6) 0.4295(4) 0.0165(10) Uani 1 1 d .
H4A H 0.4270 0.8415 0.4050 0.020 Uiso 1 1 calc R
C5 C 0.5031(3) 0.7458(6) 0.5395(4) 0.0172(10) Uani 1 1 d .
H5A H 0.4723 0.7678 0.5879 0.021 Uiso 1 1 calc R
C6 C 0.5756(3) 0.6688(6) 0.5762(3) 0.0140(10) Uani 1 1 d .
H6A H 0.5939 0.6374 0.6491 0.017 Uiso 1 1 calc R
C7 C 0.8889(2) 0.8138(5) 0.8186(3) 0.0103(9) Uani 1 1 d .
C8 C 0.9344(3) 0.9089(6) 0.7600(4) 0.0171(10) Uani 1 1 d .
H8A H 0.9126 0.9627 0.6926 0.020 Uiso 1 1 calc R
C9 C 1.0132(3) 0.9213(7) 0.8047(4) 0.0199(10) Uani 1 1 d .
H9A H 1.0446 0.9824 0.7665 0.024 Uiso 1 1 calc R
C10 C 1.0447(3) 0.8427(7) 0.9058(4) 0.0214(11) Uani 1 1 d .
H10A H 1.0973 0.8525 0.9354 0.026 Uiso 1 1 calc R
C11 C 0.9985(3) 0.7494(6) 0.9634(4) 0.0206(11) Uani 1 1 d .
H11A H 1.0202 0.6972 1.0312 0.025 Uiso 1 1 calc R
C12 C 0.9203(3) 0.7339(6) 0.9200(4) 0.0149(10) Uani 1 1 d .
H12A H 0.8891 0.6710 0.9579 0.018 Uiso 1 1 calc R
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'
As As 0.0499 2.0058 '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 O2 178.23(12) . .
O1 U1 O5 91.26(12) . 4_565
O2 U1 O5 90.05(11) . 4_565
O1 U1 O4 89.37(11) . .
O2 U1 O4 90.28(11) . .
O5 U1 O4 143.34(10) 4_565 .
O1 U1 O7 91.30(11) . 4_575
O2 U1 O7 90.25(11) . 4_575
O5 U1 O7 71.21(9) 4_565 4_575
O4 U1 O7 72.13(10) . 4_575
O1 U1 O8 89.89(11) . 4_565
O2 U1 O8 89.28(11) . 4_565
O5 U1 O8 75.76(9) 4_565 4_565
O4 U1 O8 140.90(9) . 4_565
O7 U1 O8 146.97(9) 4_575 4_565
O1 U1 O3 89.51(12) . .
O2 U1 O3 88.73(12) . .
O5 U1 O3 145.70(11) 4_565 .
O4 U1 O3 70.96(11) . .
O7 U1 O3 143.06(10) 4_575 .
O8 U1 O3 69.95(10) 4_565 .
O4 As1 O5 111.77(14) . .
O4 As1 O6 102.59(13) . .
O5 As1 O6 107.80(13) . .
O4 As1 C1 114.41(16) . .
O5 As1 C1 111.81(16) . .
O6 As1 C1 107.76(16) . .
O8 As2 O7 114.51(14) . .
O8 As2 O6 106.77(13) . .
O7 As2 O6 102.12(13) . .
O8 As2 C7 113.57(16) . .
O7 As2 C7 115.63(15) . .
O6 As2 C7 102.26(16) . .
U1 O3 H3C 130(3) . .
U1 O3 H3B 121(3) . .
H3C O3 H3B 94(5) . .
As1 O4 U1 134.01(15) . .
As1 O5 U1 140.64(15) . 4_566
As1 O6 As2 125.20(16) . .
As2 O7 U1 131.94(14) . 4_576
As2 O8 U1 135.81(15) . 4_566
C2 C1 C6 121.1(4) . .
C2 C1 As1 120.0(3) . .
C6 C1 As1 118.8(3) . .
C3 C2 C1 119.1(4) . .
C3 C2 H2A 120.5 . .
C1 C2 H2A 120.5 . .
C4 C3 C2 120.3(4) . .
C4 C3 H3A 119.8 . .
C2 C3 H3A 119.8 . .
C3 C4 C5 120.6(4) . .
C3 C4 H4A 119.7 . .
C5 C4 H4A 119.7 . .
C6 C5 C4 119.9(4) . .
C6 C5 H5A 120.0 . .
C4 C5 H5A 120.0 . .
C5 C6 C1 118.9(4) . .
C5 C6 H6A 120.6 . .
C1 C6 H6A 120.6 . .
C12 C7 C8 121.7(4) . .
C12 C7 As2 119.9(3) . .
C8 C7 As2 118.4(3) . .
C9 C8 C7 118.5(4) . .
C9 C8 H8A 120.8 . .
C7 C8 H8A 120.8 . .
C10 C9 C8 120.2(4) . .
C10 C9 H9A 119.9 . .
C8 C9 H9A 119.9 . .
C9 C10 C11 120.6(4) . .
C9 C10 H10A 119.7 . .
C11 C10 H10A 119.7 . .
C12 C11 C10 120.2(4) . .
C12 C11 H11A 119.9 . .
C10 C11 H11A 119.9 . .
C11 C12 C7 119.0(4) . .
C11 C12 H12A 120.5 . .
C7 C12 H12A 120.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.771(3) .
U1 O2 1.771(3) .
U1 O5 2.357(3) 4_565
U1 O4 2.365(3) .
U1 O7 2.367(3) 4_575
U1 O8 2.385(3) 4_565
U1 O3 2.502(3) .
As1 O4 1.655(3) .
As1 O5 1.664(3) .
As1 O6 1.760(3) .
As1 C1 1.894(4) .
As2 O8 1.659(3) .
As2 O7 1.661(3) .
As2 O6 1.785(3) .
As2 C7 1.896(4) .
O3 H3C 0.74(4) .
O3 H3B 0.83(5) .
O5 U1 2.357(3) 4_566
O7 U1 2.367(3) 4_576
O8 U1 2.385(3) 4_566
C1 C2 1.390(6) .
C1 C6 1.408(6) .
C2 C3 1.387(6) .
C2 H2A 0.9300 .
C3 C4 1.382(6) .
C3 H3A 0.9300 .
C4 C5 1.398(6) .
C4 H4A 0.9300 .
C5 C6 1.383(6) .
C5 H5A 0.9300 .
C6 H6A 0.9300 .
C7 C12 1.392(6) .
C7 C8 1.395(6) .
C8 C9 1.393(6) .
C8 H8A 0.9300 .
C9 C10 1.386(6) .
C9 H9A 0.9300 .
C10 C11 1.391(7) .
C10 H10A 0.9300 .
C11 C12 1.382(6) .
C11 H11A 0.9300 .
C12 H12A 0.9300 .
