#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:51:50 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179458 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/55/4335586.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_4335586
loop_
_publ_author_name
'Tao Tian'
'Weiting Yang'
'Hao Wang'
'Song Dang'
'Zhong-Ming Sun'
_publ_section_title
;
 Flexible Diphosphonic Acids for the Isolation of Uranyl Hybrids with
 Heterometallic UVI=O-ZnII Cation-Cation Interactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8288
_journal_page_last               8290
_journal_paper_doi               10.1021/ic4009834
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C12 H12 N2 O8 P2 U Zn'
_chemical_formula_weight         677.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_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                 100.074(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3814(9)
_cell_length_b                   21.4752(18)
_cell_length_c                   8.0597(7)
_cell_measurement_temperature    273(2)
_cell_volume                     1769.1(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0495
_diffrn_reflns_av_sigmaI/netI    0.0608
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9575
_diffrn_reflns_theta_full        26.04
_diffrn_reflns_theta_max         26.04
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    10.723
_exptl_absorpt_correction_T_max  0.65
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    2.544
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.733
_refine_diff_density_min         -0.944
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3484
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0369
_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)+(0.0306P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0784
_reflns_number_gt                2829
_reflns_number_total             3484
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4009834_si_002_1.cif
_cod_data_source_block           1
_cod_database_code               4335586
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 0.23734(2) 0.465972(13) -0.01439(3) 0.01193(10) Uani 1 1 d .
Zn1 Zn 0.26958(8) 0.63057(4) 0.13717(11) 0.0156(2) Uani 1 1 d .
P1 P 0.08454(18) 0.53709(9) 0.2863(2) 0.0122(4) Uani 1 1 d .
P2 P 0.50414(18) 0.53984(9) 0.2468(2) 0.0121(4) Uani 1 1 d .
C1 C 0.2589(8) 0.7665(4) 0.1274(10) 0.0206(18) Uani 1 1 d .
C2 C 0.2938(9) 0.8293(4) 0.1528(11) 0.030(2) Uani 1 1 d .
H2 H 0.2435 0.8607 0.0941 0.036 Uiso 1 1 calc R
C3 C 0.4049(9) 0.8432(4) 0.2674(11) 0.032(2) Uani 1 1 d .
H3 H 0.4304 0.8845 0.2863 0.038 Uiso 1 1 calc R
C4 C 0.4774(8) 0.7970(4) 0.3527(11) 0.029(2) Uani 1 1 d .
H4 H 0.5517 0.8060 0.4316 0.035 Uiso 1 1 calc R
C5 C 0.4373(8) 0.7360(4) 0.3186(11) 0.026(2) Uani 1 1 d .
H5 H 0.4876 0.7040 0.3742 0.031 Uiso 1 1 calc R
C6 C 0.1428(8) 0.7460(4) 0.0051(10) 0.0185(18) Uani 1 1 d .
C7 C 0.0260(7) 0.6620(4) -0.1172(10) 0.0207(18) Uani 1 1 d .
H7 H 0.0166 0.6191 -0.1288 0.025 Uiso 1 1 calc R
C8 C -0.0699(8) 0.6998(5) -0.2080(11) 0.031(2) Uani 1 1 d .
H8 H -0.1415 0.6826 -0.2787 0.037 Uiso 1 1 calc R
C9 C -0.0565(9) 0.7623(5) -0.1911(11) 0.032(2) Uani 1 1 d .
H9 H -0.1187 0.7888 -0.2513 0.039 Uiso 1 1 calc R
C10 C 0.0508(8) 0.7868(4) -0.0831(11) 0.028(2) Uani 1 1 d .
H10 H 0.0611 0.8296 -0.0699 0.033 Uiso 1 1 calc R
C11 C 0.0575(7) 0.5230(3) 0.4960(8) 0.0139(17) Uani 1 1 d .
H11A H 0.1369 0.5061 0.5622 0.017 Uiso 1 1 calc R
H11B H 0.0390 0.5622 0.5464 0.017 Uiso 1 1 calc R
C12 C 0.4894(7) 0.5330(3) 0.4647(9) 0.0185(17) Uani 1 1 d .
H12A H 0.5525 0.5605 0.5307 0.022 Uiso 1 1 calc R
H12B H 0.4028 0.5469 0.4779 0.022 Uiso 1 1 calc R
N1 N 0.1304(6) 0.6839(3) -0.0147(7) 0.0191(15) Uani 1 1 d .
N2 N 0.3310(6) 0.7216(3) 0.2110(8) 0.0169(15) Uani 1 1 d .
O1 O 0.4266(5) 0.4846(2) 0.1581(6) 0.0135(11) Uani 1 1 d .
O2 O 0.2618(5) 0.3846(3) 0.0231(6) 0.0205(12) Uani 1 1 d .
O3 O 0.1845(4) 0.5889(2) 0.3035(6) 0.0133(11) Uani 1 1 d .
O4 O 0.0459(5) 0.4424(3) -0.1819(6) 0.0174(12) Uani 1 1 d .
O5 O 0.4498(4) 0.6022(2) 0.1790(6) 0.0168(12) Uani 1 1 d .
O6 O 0.1337(5) 0.4769(2) 0.2148(6) 0.0135(11) Uani 1 1 d .
O7 O 0.3511(5) 0.4661(2) -0.2337(6) 0.0158(11) Uani 1 1 d .
O8 O 0.2130(5) 0.5487(2) -0.0466(6) 0.0143(12) 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 O8 178.5(2) . .
O2 U1 O1 89.2(2) . .
O8 U1 O1 90.0(2) . .
O2 U1 O4 88.1(2) . .
O8 U1 O4 92.8(2) . .
O1 U1 O4 177.05(18) . .
O2 U1 O7 93.1(2) . .
O8 U1 O7 88.0(2) . .
O1 U1 O7 87.93(17) . .
O4 U1 O7 93.31(17) . .
O2 U1 O6 92.1(2) . .
O8 U1 O6 86.70(19) . .
O1 U1 O6 88.04(17) . .
O4 U1 O6 90.95(17) . .
O7 U1 O6 173.38(17) . .
O5 Zn1 O3 106.0(2) . .
O5 Zn1 N1 146.0(2) . .
O3 Zn1 N1 107.9(2) . .
O5 Zn1 N2 90.4(2) . .
O3 Zn1 N2 112.5(2) . .
N1 Zn1 N2 78.4(2) . .
O5 Zn1 O8 90.1(2) . .
O3 Zn1 O8 89.81(18) . .
N1 Zn1 O8 88.2(2) . .
N2 Zn1 O8 156.6(2) . .
O3 P1 O4 111.5(3) . 3_565
O3 P1 O6 112.7(3) . .
O4 P1 O6 110.8(3) 3_565 .
O3 P1 C11 104.9(3) . .
O4 P1 C11 107.4(3) 3_565 .
O6 P1 C11 109.2(3) . .
O5 P2 O7 110.9(3) . 3_665
O5 P2 O1 112.5(3) . .
O7 P2 O1 110.1(3) 3_665 .
O5 P2 C12 109.6(3) . .
O7 P2 C12 108.3(3) 3_665 .
O1 P2 C12 105.3(3) . .
N2 C1 C2 121.1(8) . .
N2 C1 C6 116.1(7) . .
C2 C1 C6 122.8(8) . .
C3 C2 C1 118.0(8) . .
C4 C3 C2 120.5(8) . .
C3 C4 C5 118.0(8) . .
N2 C5 C4 122.8(8) . .
N1 C6 C10 121.2(7) . .
N1 C6 C1 115.0(7) . .
C10 C6 C1 123.7(7) . .
N1 C7 C8 123.5(8) . .
C9 C8 C7 118.3(8) . .
C8 C9 C10 119.6(8) . .
C6 C10 C9 118.9(8) . .
C11 C11 P1 113.3(6) 3_566 .
C12 C12 P2 114.1(7) 3_666 .
C7 N1 C6 118.4(7) . .
C7 N1 Zn1 125.6(5) . .
C6 N1 Zn1 115.8(5) . .
C5 N2 C1 119.7(7) . .
C5 N2 Zn1 125.6(6) . .
C1 N2 Zn1 114.5(5) . .
P2 O1 U1 139.3(3) . .
P1 O3 Zn1 131.5(3) . .
P1 O4 U1 150.2(3) 3_565 .
P2 O5 Zn1 128.8(3) . .
P1 O6 U1 128.1(3) . .
P2 O7 U1 134.3(3) 3_665 .
U1 O8 Zn1 130.0(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O2 1.784(5) .
U1 O8 1.806(5) .
U1 O1 2.235(5) .
U1 O4 2.256(5) .
U1 O7 2.291(5) .
U1 O6 2.306(5) .
Zn1 O5 1.941(5) .
Zn1 O3 1.947(5) .
Zn1 N1 2.068(6) .
Zn1 N2 2.109(6) .
Zn1 O8 2.308(5) .
P1 O3 1.512(5) .
P1 O4 1.529(5) 3_565
P1 O6 1.540(5) .
P1 C11 1.787(7) .
P2 O5 1.517(5) .
P2 O7 1.530(5) 3_665
P2 O1 1.538(5) .
P2 C12 1.796(7) .
C1 N2 1.330(10) .
C1 C2 1.402(11) .
C1 C6 1.485(11) .
C2 C3 1.378(12) .
C3 C4 1.357(12) .
C4 C5 1.388(11) .
C5 N2 1.316(10) .
C6 N1 1.347(9) .
C6 C10 1.396(11) .
C7 N1 1.328(9) .
C7 C8 1.390(11) .
C8 C9 1.355(12) .
C9 C10 1.391(12) .
C11 C11 1.558(14) 3_566
C12 C12 1.528(14) 3_666
O4 P1 1.529(5) 3_565
O7 P2 1.530(5) 3_665
