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#$Date: 2016-03-23 21:11:09 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179443 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/40/4334078.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_4334078
loop_
_publ_author_name
'Weiting Yang'
'Tao Tian'
'Hong-Yue Wu'
'Qing-Jiang Pan'
'Song Dang'
'Zhong-Ming Sun'
_publ_section_title
;
 Syntheses and Structures of a Series of Uranyl Phosphonates and
 Sulfonates: An Insight into Their Correlations and Discrepancies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2736
_journal_page_last               2743
_journal_paper_doi               10.1021/ic302847g
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C24 H20 N4 O10 P2 U Zn'
_chemical_formula_weight         889.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.9990(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1880(11)
_cell_length_b                   10.4948(9)
_cell_length_c                   21.5361(18)
_cell_measurement_temperature    106(2)
_cell_volume                     2964.4(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      106(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15864
_diffrn_reflns_theta_full        26.13
_diffrn_reflns_theta_max         26.13
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    6.433
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6789
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.994
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.098
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.891
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5871
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.891
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0308
_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)+(0.0402P)²+2.9102P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0681
_refine_ls_wR_factor_ref         0.0752
_reflns_number_gt                4566
_reflns_number_total             5871
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302847g_si_002_3.cif
_cod_data_source_block           UPhP-3
_cod_database_code               4334078
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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 0.778002(14) 0.049482(18) 0.225548(9) 0.01729(7) Uani 1 1 d .
Zn1 Zn 0.45758(4) 0.05065(6) 0.29267(3) 0.01754(13) Uani 1 1 d .
P1 P 0.56928(10) -0.17032(12) 0.22538(6) 0.0188(3) Uani 1 1 d .
P2 P 0.93175(10) -0.22043(13) 0.28358(7) 0.0210(3) Uani 1 1 d .
O1 O 0.7460(3) 0.0441(4) 0.30384(18) 0.0300(9) Uani 1 1 d .
O2 O 0.8069(3) 0.0536(3) 0.14711(17) 0.0274(9) Uani 1 1 d .
O3 O 0.6585(3) -0.1040(4) 0.19836(17) 0.0242(9) Uani 1 1 d .
O4 O 0.6612(3) 0.2041(4) 0.20035(19) 0.0327(10) Uani 1 1 d .
O5 O 0.9004(3) -0.1034(3) 0.24468(17) 0.0260(9) Uani 1 1 d .
O6 O 0.9039(3) 0.1932(3) 0.25647(18) 0.0263(9) Uani 1 1 d .
O7 O 0.5332(3) -0.1007(3) 0.28027(17) 0.0238(8) Uani 1 1 d .
O8 O 0.4937(3) 0.1984(3) 0.24772(17) 0.0278(9) Uani 1 1 d .
C1 C 0.3834(4) 0.0459(5) 0.4212(2) 0.0260(12) Uani 1 1 d .
H1 H 0.3315 -0.0148 0.4094 0.031 Uiso 1 1 calc R
C2 C 0.3997(4) 0.1011(6) 0.4777(3) 0.0276(13) Uani 1 1 d .
H2 H 0.3624 0.0873 0.5125 0.033 Uiso 1 1 calc R
C3 C 0.5112(4) 0.1712(5) 0.4168(2) 0.0248(12) Uani 1 1 d .
H3 H 0.5667 0.2163 0.4025 0.030 Uiso 1 1 calc R
C4 C 0.5321(4) 0.2541(5) 0.5251(2) 0.0249(12) Uani 1 1 d .
C5 C 0.4804(4) 0.2827(6) 0.5763(3) 0.0352(15) Uani 1 1 d .
H5 H 0.4104 0.2616 0.5762 0.042 Uiso 1 1 calc R
C6 C 0.6328(4) 0.2896(6) 0.5242(3) 0.0315(14) Uani 1 1 d .
H6 H 0.6679 0.2703 0.4891 0.038 Uiso 1 1 calc R
C7 C 0.2268(4) -0.0357(5) 0.2678(2) 0.0242(12) Uani 1 1 d .
H7 H 0.2238 -0.0891 0.3032 0.029 Uiso 1 1 calc R
C8 C 0.2837(4) 0.0919(5) 0.2026(3) 0.0216(12) Uani 1 1 d .
H8 H 0.3272 0.1463 0.1820 0.026 Uiso 1 1 calc R
C9 C 0.1487(4) -0.0159(5) 0.2229(2) 0.0259(13) Uani 1 1 d .
H9 H 0.0823 -0.0517 0.2208 0.031 Uiso 1 1 calc R
C10 C 0.1320(4) 0.1231(5) 0.1267(2) 0.0216(12) Uani 1 1 d .
C11 C 0.1818(4) 0.1469(6) 0.0746(3) 0.0304(13) Uani 1 1 d .
H11 H 0.2502 0.1193 0.0735 0.037 Uiso 1 1 calc R
C12 C 0.0317(4) 0.1581(6) 0.1273(3) 0.0301(14) Uani 1 1 d .
H12 H -0.0025 0.1413 0.1631 0.036 Uiso 1 1 calc R
C13 C 0.3707(4) -0.2154(5) 0.1742(3) 0.0270(13) Uani 1 1 d .
H13 H 0.3601 -0.2484 0.2141 0.032 Uiso 1 1 calc R
C14 C 0.4666(4) -0.1722(5) 0.1628(2) 0.0191(11) Uani 1 1 d .
C15 C 0.4791(4) -0.1257(6) 0.1040(3) 0.0327(14) Uani 1 1 d .
H15 H 0.5442 -0.0957 0.0954 0.039 Uiso 1 1 calc R
C16 C 0.3981(5) -0.1221(6) 0.0574(3) 0.0435(17) Uani 1 1 d .
H16 H 0.4077 -0.0903 0.0172 0.052 Uiso 1 1 calc R
C17 C 0.3047(5) -0.1643(6) 0.0697(3) 0.0426(17) Uani 1 1 d .
H17 H 0.2490 -0.1616 0.0380 0.051 Uiso 1 1 calc R
C18 C 0.2908(4) -0.2105(6) 0.1274(3) 0.0405(16) Uani 1 1 d .
H18 H 0.2253 -0.2396 0.1355 0.049 Uiso 1 1 calc R
C19 C 0.9974(4) -0.1667(5) 0.3563(2) 0.0219(12) Uani 1 1 d .
C20 C 1.0223(4) -0.0398(6) 0.3677(3) 0.0310(14) Uani 1 1 d .
H20 H 1.0029 0.0223 0.3366 0.037 Uiso 1 1 calc R
C21 C 1.0748(5) -0.0027(6) 0.4234(3) 0.0388(16) Uani 1 1 d .
H21 H 1.0904 0.0848 0.4306 0.047 Uiso 1 1 calc R
C22 C 1.1046(5) -0.0911(7) 0.4685(3) 0.0422(17) Uani 1 1 d .
H22 H 1.1414 -0.0651 0.5067 0.051 Uiso 1 1 calc R
C23 C 1.0812(5) -0.2159(7) 0.4585(3) 0.0409(17) Uani 1 1 d .
H23 H 1.1011 -0.2770 0.4900 0.049 Uiso 1 1 calc R
C24 C 1.0284(4) -0.2546(6) 0.4027(3) 0.0338(14) Uani 1 1 d .
H24 H 1.0132 -0.3423 0.3961 0.041 Uiso 1 1 calc R
N1 N 0.4528(3) 0.0901(4) 0.3827(2) 0.0217(10) Uani 1 1 d .
N2 N 0.3113(3) 0.0327(4) 0.2548(2) 0.0194(10) Uani 1 1 d .
N3 N 0.4817(3) 0.1818(4) 0.47483(19) 0.0236(10) Uani 1 1 d .
N4 N 0.1855(3) 0.0668(4) 0.1810(2) 0.0206(10) Uani 1 1 d .
O1W O 0.7496(3) 0.2443(4) 0.39833(19) 0.0448(11) Uani 1 1 d .
O2W O 0.7467(4) 0.8673(5) 0.4097(2) 0.0637(15) 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'
Zn Zn 0.2839 1.4301 '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 O1 178.66(16) . .
O2 U1 O4 87.84(15) . .
O1 U1 O4 91.55(16) . .
O2 U1 O5 88.34(15) . .
O1 U1 O5 92.29(16) . .
O4 U1 O5 176.05(13) . .
O2 U1 O3 89.11(15) . .
O1 U1 O3 89.71(15) . .
O4 U1 O3 90.58(14) . .
O5 U1 O3 90.37(13) . .
O2 U1 O6 92.26(15) . .
O1 U1 O6 88.97(15) . .
O4 U1 O6 92.98(13) . .
O5 U1 O6 86.15(13) . .
O3 U1 O6 176.22(13) . .
O7 Zn1 O8 116.21(16) . .
O7 Zn1 N1 112.32(16) . .
O8 Zn1 N1 111.03(17) . .
O7 Zn1 N2 110.88(17) . .
O8 Zn1 N2 98.56(16) . .
N1 Zn1 N2 106.64(17) . .
O7 P1 O6 109.8(2) . 2_645
O7 P1 O3 113.2(2) . .
O6 P1 O3 111.1(2) 2_645 .
O7 P1 C14 108.4(2) . .
O6 P1 C14 108.5(2) 2_645 .
O3 P1 C14 105.5(2) . .
O8 P2 O5 111.2(2) 2_645 .
O8 P2 O4 112.5(2) 2_645 2_645
O5 P2 O4 111.4(2) . 2_645
O8 P2 C19 106.8(2) 2_645 .
O5 P2 C19 107.8(2) . .
O4 P2 C19 106.8(2) 2_645 .
P1 O3 U1 139.3(2) . .
P2 O4 U1 149.1(2) 2_655 .
P2 O5 U1 144.5(2) . .
P1 O6 U1 147.0(2) 2_655 .
P1 O7 Zn1 136.4(2) . .
P2 O8 Zn1 152.9(2) 2_655 .
C2 C1 N1 110.3(5) . .
C1 C2 N3 106.0(5) . .
N1 C3 N3 111.1(5) . .
C6 C4 C5 120.3(5) . .
C6 C4 N3 120.4(5) . .
C5 C4 N3 119.3(5) . .
C12 C5 C4 119.4(5) 4_666 .
C11 C6 C4 119.6(5) 4_666 .
C9 C7 N2 110.2(5) . .
N2 C8 N4 111.9(5) . .
C7 C9 N4 105.7(5) . .
C12 C10 C11 120.0(5) . .
C12 C10 N4 119.7(5) . .
C11 C10 N4 120.3(5) . .
C6 C11 C10 120.3(5) 4_565 .
C10 C12 C5 120.4(5) . 4_565
C14 C13 C18 119.9(6) . .
C15 C14 C13 118.4(5) . .
C15 C14 P1 121.7(4) . .
C13 C14 P1 119.8(4) . .
C14 C15 C16 121.0(6) . .
C17 C16 C15 119.7(6) . .
C16 C17 C18 120.2(6) . .
C17 C18 C13 120.9(6) . .
C20 C19 C24 117.7(5) . .
C20 C19 P2 122.5(4) . .
C24 C19 P2 119.8(4) . .
C21 C20 C19 120.9(6) . .
C20 C21 C22 120.5(6) . .
C23 C22 C21 119.8(6) . .
C22 C23 C24 120.4(6) . .
C19 C24 C23 120.8(6) . .
C3 N1 C1 105.6(5) . .
C3 N1 Zn1 126.9(4) . .
C1 N1 Zn1 127.3(4) . .
C8 N2 C7 105.4(4) . .
C8 N2 Zn1 118.2(3) . .
C7 N2 Zn1 136.3(3) . .
C3 N3 C2 107.1(4) . .
C3 N3 C4 126.0(5) . .
C2 N3 C4 126.7(4) . .
C8 N4 C9 106.8(4) . .
C8 N4 C10 124.9(4) . .
C9 N4 C10 128.3(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O2 1.771(4) .
U1 O1 1.781(4) .
U1 O4 2.264(4) .
U1 O5 2.283(3) .
U1 O3 2.287(3) .
U1 O6 2.290(3) .
Zn1 O7 1.909(4) .
Zn1 O8 1.915(4) .
Zn1 N1 1.990(4) .
Zn1 N2 2.024(4) .
P1 O7 1.508(4) .
P1 O6 1.517(4) 2_645
P1 O3 1.533(4) .
P1 C14 1.808(5) .
P2 O8 1.511(4) 2_645
P2 O5 1.519(4) .
P2 O4 1.529(4) 2_645
P2 C19 1.799(5) .
O4 P2 1.529(4) 2_655
O6 P1 1.517(4) 2_655
O8 P2 1.511(4) 2_655
C1 C2 1.345(7) .
C1 N1 1.378(7) .
C2 N3 1.381(7) .
C3 N1 1.319(7) .
C3 N3 1.352(6) .
C4 C6 1.381(7) .
C4 C5 1.389(7) .
C4 N3 1.427(7) .
C5 C12 1.376(7) 4_666
C6 C11 1.375(7) 4_666
C7 C9 1.352(7) .
C7 N2 1.379(6) .
C8 N2 1.303(7) .
C8 N4 1.355(6) .
C9 N4 1.376(6) .
C10 C12 1.374(7) .
C10 C11 1.381(7) .
C10 N4 1.430(6) .
C11 C6 1.375(7) 4_565
C12 C5 1.376(7) 4_565
C13 C14 1.389(7) .
C13 C18 1.380(8) .
C14 C15 1.383(7) .
C15 C16 1.388(8) .
C16 C17 1.360(9) .
C17 C18 1.364(9) .
C19 C20 1.387(7) .
C19 C24 1.389(8) .
C20 C21 1.377(8) .
C21 C22 1.371(9) .
C22 C23 1.358(9) .
C23 C24 1.385(8) .
