#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:25:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179411 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/08/4330819.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_4330819
loop_
_publ_author_name
'Weiting Yang'
'Hong-Yue Wu'
'Run-Xue Wang'
'Qing-Jiang Pan'
'Zhong-Ming Sun'
'Hongjie Zhang'
_publ_contact_author_address
;
 State Key Laboratory of Rare Earth Resource Utilization,
 Changchun Institute of Applied Chemistry, Chinese Academy of Sciences,
 5625 Renmin Street, Changchun, Jilin 130022, P.R. China.
;
_publ_contact_author_email       szm@ciac.jl.cn
_publ_contact_author_name
;
Prof Z. M. Sun
;
_publ_section_title
;
 From 1D Chain to 3D Framework Uranyl Diphosphonates: Syntheses, Crystal
 Structures, and Selective Ion Exchange
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11458
_journal_page_last               11465
_journal_paper_doi               10.1021/ic301183h
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C17 H18 N2 O11 P2 U'
_chemical_formula_weight         726.30
_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                 96.6810(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.1749(4)
_cell_length_b                   11.4055(6)
_cell_length_c                   27.2222(15)
_cell_measurement_temperature    273(2)
_cell_volume                     2212.6(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            11954
_diffrn_reflns_theta_full        26.07
_diffrn_reflns_theta_max         26.07
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    7.543
_exptl_absorpt_correction_T_max  0.46
_exptl_absorpt_correction_T_min  0.24
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    2.180
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.882
_refine_diff_density_min         -1.360
_refine_diff_density_rms         0.319
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.300
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         4358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.300
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0430P)²+12.3006P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1157
_reflns_number_gt                3668
_reflns_number_total             4358
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301183h_si_002_02.cif
_cod_data_source_block           UP-1
_cod_database_code               4330819
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 1.11423(4) 0.50455(2) 0.255447(11) 0.01273(12) Uani 1 1 d .
P1 P 0.7545(3) 0.70884(18) 0.19958(8) 0.0124(4) Uani 1 1 d .
P2 P 0.8573(3) 0.27846(18) 0.31466(8) 0.0124(4) Uani 1 1 d .
O1 O 1.2038(7) 0.6853(5) 0.2238(2) 0.0127(12) Uani 1 1 d .
O2 O 1.1790(8) 0.5669(5) 0.3142(2) 0.0175(13) Uani 1 1 d .
O3 O 1.0492(8) 0.4403(5) 0.1961(2) 0.0183(13) Uani 1 1 d .
O4 O 0.8402(8) 0.6192(5) 0.2377(2) 0.0142(12) Uani 1 1 d .
O5 O 1.4409(9) 0.5052(5) 0.2367(2) 0.0226(14) Uani 1 1 d .
O6 O 1.2629(8) 0.3298(5) 0.2770(2) 0.0168(13) Uani 1 1 d .
O7 O 0.8874(8) 0.3982(5) 0.2927(2) 0.0167(13) Uani 1 1 d .
O8 O 0.7111(8) 0.2872(5) 0.3521(2) 0.0147(12) Uani 1 1 d .
H8A H 0.6169 0.2501 0.3417 0.022 Uiso 1 1 calc R
O9 O 0.5690(8) 0.6642(5) 0.1741(2) 0.0153(12) Uani 1 1 d .
O10 O 0.9420(10) 0.6227(6) 0.1246(2) 0.0297(16) Uani 1 1 d .
H10A H 0.9647 0.6389 0.0966 0.045 Uiso 1 1 calc R
N1 N 0.3258(11) 0.2383(7) 0.1052(3) 0.0197(16) Uani 1 1 d .
N2 N 0.3059(11) 0.1191(7) 0.1651(3) 0.0282(19) Uani 1 1 d .
H2 H 0.2862 0.0911 0.1934 0.034 Uiso 1 1 calc R
C1 C 0.9175(11) 0.7307(7) 0.1520(3) 0.0152(17) Uani 1 1 d .
C2 C 0.8377(13) 0.8218(9) 0.1154(4) 0.029(2) Uani 1 1 d .
H2A H 0.9238 0.8354 0.0916 0.044 Uiso 1 1 calc R
H2B H 0.8181 0.8935 0.1326 0.044 Uiso 1 1 calc R
H2C H 0.7202 0.7945 0.0989 0.044 Uiso 1 1 calc R
C3 C 0.3773(13) 0.4472(8) 0.0975(3) 0.023(2) Uani 1 1 d .
H3 H 0.4341 0.4490 0.1300 0.028 Uiso 1 1 calc R
C4 C 0.3127(12) 0.3436(7) 0.0760(3) 0.0176(18) Uani 1 1 d .
C5 C 0.2391(13) 0.3393(9) 0.0266(3) 0.026(2) Uani 1 1 d .
H5 H 0.2030 0.2680 0.0120 0.031 Uiso 1 1 calc R
C6 C 0.2197(13) 0.4415(9) -0.0007(3) 0.024(2) Uani 1 1 d .
H6 H 0.1681 0.4388 -0.0336 0.028 Uiso 1 1 calc R
C7 C 0.2764(12) 0.5483(9) 0.0205(3) 0.023(2) Uani 1 1 d .
C8 C 0.3554(14) 0.5501(8) 0.0691(3) 0.025(2) Uani 1 1 d .
H8 H 0.3951 0.6212 0.0835 0.030 Uiso 1 1 calc R
C9 C 0.3836(14) 0.1280(8) 0.0906(3) 0.026(2) Uani 1 1 d .
H9 H 0.4243 0.1083 0.0605 0.031 Uiso 1 1 calc R
C10 C 0.3688(15) 0.0577(10) 0.1283(4) 0.034(2) Uani 1 1 d .
H10 H 0.3972 -0.0219 0.1292 0.041 Uiso 1 1 calc R
C11 C 0.2788(14) 0.2314(9) 0.1508(4) 0.029(2) Uani 1 1 d .
H11 H 0.2356 0.2922 0.1693 0.035 Uiso 1 1 calc R
C12 C 0.2243(14) 0.7671(9) 0.0166(4) 0.030(2) Uani 1 1 d .
H12 H 0.2448 0.7700 0.0510 0.037 Uiso 1 1 calc R
C13 C 0.2403(13) 0.6601(9) -0.0077(3) 0.024(2) Uani 1 1 d .
C14 C 0.2127(14) 0.6600(10) -0.0595(3) 0.029(2) Uani 1 1 d .
H14 H 0.2243 0.5907 -0.0769 0.035 Uiso 1 1 calc R
C15 C 0.1678(15) 0.7639(10) -0.0849(4) 0.034(3) Uani 1 1 d .
H15 H 0.1495 0.7630 -0.1193 0.041 Uiso 1 1 calc R
C16 C 0.1498(15) 0.8673(11) -0.0605(4) 0.040(3) Uani 1 1 d .
H16 H 0.1187 0.9361 -0.0779 0.048 Uiso 1 1 calc R
C17 C 0.1788(15) 0.8676(9) -0.0096(4) 0.036(3) Uani 1 1 d .
H17 H 0.1672 0.9375 0.0074 0.044 Uiso 1 1 calc R
O1W O 0.6419(10) 0.3326(7) 0.1960(3) 0.0399(19) Uani 1 1 d .
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'
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'
P P 0.1023 0.0942 '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
O2 U1 O3 179.6(3) . .
O2 U1 O6 93.0(2) . .
O3 U1 O6 86.6(2) . .
O2 U1 O7 86.5(2) . .
O3 U1 O7 93.3(2) . .
O6 U1 O7 76.53(19) . .
O2 U1 O1 85.7(2) . .
O3 U1 O1 94.7(2) . .
O6 U1 O1 135.50(19) . .
O7 U1 O1 147.36(19) . .
O2 U1 O4 95.0(2) . .
O3 U1 O4 85.3(2) . .
O6 U1 O4 151.6(2) . .
O7 U1 O4 76.87(19) . .
O1 U1 O4 72.33(19) . .
O2 U1 O5 91.7(2) . .
O3 U1 O5 88.2(2) . .
O6 U1 O5 68.3(2) . .
O7 U1 O5 144.68(19) . .
O1 U1 O5 67.26(19) . .
O4 U1 O5 138.32(19) . .
O9 P1 O4 110.3(3) . .
O9 P1 O6 112.6(3) . 2_755
O4 P1 O6 111.4(3) . 2_755
O9 P1 C1 108.4(4) . .
O4 P1 C1 109.0(3) . .
O6 P1 C1 104.9(4) 2_755 .
O7 P2 O1 113.6(3) . 2_745
O7 P2 O8 109.9(3) . .
O1 P2 O8 109.6(3) 2_745 .
O7 P2 C1 107.7(4) . 2_745
O1 P2 C1 107.4(3) 2_745 2_745
O8 P2 C1 108.5(4) . 2_745
P2 O1 U1 142.8(3) 2_755 .
P1 O4 U1 140.0(3) . .
P1 O6 U1 145.9(3) 2_745 .
P2 O7 U1 140.6(3) . .
C11 N1 C9 109.2(8) . .
C11 N1 C4 124.1(8) . .
C9 N1 C4 126.8(7) . .
C10 N2 C11 109.3(8) . .
O10 C1 C2 107.7(8) . .
O10 C1 P2 110.5(6) . 2_755
C2 C1 P2 111.5(6) . 2_755
O10 C1 P1 111.4(5) . .
C2 C1 P1 109.3(6) . .
P2 C1 P1 106.4(4) 2_755 .
C4 C3 C8 118.3(8) . .
C3 C4 C5 121.0(8) . .
C3 C4 N1 119.0(8) . .
C5 C4 N1 120.0(8) . .
C6 C5 C4 119.7(9) . .
C5 C6 C7 120.6(9) . .
C8 C7 C6 118.8(9) . .
C8 C7 C13 120.5(9) . .
C6 C7 C13 120.6(8) . .
C7 C8 C3 121.5(9) . .
C10 C9 N1 106.0(8) . .
C9 C10 N2 109.1(9) . .
N1 C11 N2 106.4(9) . .
C17 C12 C13 120.7(10) . .
C14 C13 C12 117.9(9) . .
C14 C13 C7 120.8(9) . .
C12 C13 C7 121.2(9) . .
C15 C14 C13 119.8(10) . .
C16 C15 C14 121.7(10) . .
C15 C16 C17 118.5(10) . .
C12 C17 C16 121.4(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O2 1.764(6) .
U1 O3 1.786(6) .
U1 O6 2.304(6) .
U1 O7 2.351(6) .
U1 O1 2.352(5) .
U1 O4 2.364(6) .
U1 O5 2.456(6) .
P1 O9 1.516(6) .
P1 O4 1.533(6) .
P1 O6 1.531(6) 2_755
P1 C1 1.861(9) .
P2 O7 1.517(6) .
P2 O1 1.520(5) 2_745
P2 O8 1.548(6) .
P2 C1 1.842(8) 2_745
O1 P2 1.520(5) 2_755
O6 P1 1.531(6) 2_745
O10 C1 1.460(10) .
N1 C11 1.327(12) .
N1 C9 1.396(12) .
N1 C4 1.437(11) .
N2 C10 1.344(13) .
N2 C11 1.346(12) .
C1 C2 1.504(11) .
C1 P2 1.842(8) 2_755
C3 C4 1.375(13) .
C3 C8 1.403(13) .
C4 C5 1.385(12) .
C5 C6 1.381(13) .
C6 C7 1.388(14) .
C7 C8 1.378(12) .
C7 C13 1.497(13) .
C9 C10 1.315(14) .
C12 C17 1.368(14) .
C12 C13 1.400(14) .
C13 C14 1.401(13) .
C14 C15 1.389(14) .
C15 C16 1.367(16) .
C16 C17 1.379(15) .
