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#$Date: 2016-03-23 22:07:42 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179468 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/65/4336533.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_4336533
loop_
_publ_author_name
'Weiting Yang'
'Song Dang'
'Hao Wang'
'Tao Tian'
'Qing-Jiang Pan'
'Zhong-Ming Sun'
_publ_section_title
;
 Synthesis, Structures, and Properties of Uranyl Hybrids Constructed by a
 Variety of Mono- and Polycarboxylic Acids
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12394
_journal_page_last               12402
_journal_paper_doi               10.1021/ic4012444
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C54 H34 N6 O16 U2 Zn'
_chemical_formula_weight         1564.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 123.5640(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.0976(9)
_cell_length_b                   11.7435(4)
_cell_length_c                   20.7722(8)
_cell_measurement_temperature    173(2)
_cell_volume                     5101.5(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13893
_diffrn_reflns_theta_full        26.12
_diffrn_reflns_theta_max         26.12
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    6.880
_exptl_absorpt_correction_T_max  0.52
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    2.037
_exptl_crystal_F_000             2968
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.145
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         5072
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0234
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0242P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0491
_refine_ls_wR_factor_ref         0.0513
_reflns_number_gt                4399
_reflns_number_total             5072
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4012444_si_002_7.cif
_cod_data_source_block           7
_cod_database_code               4336533
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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 0.215480(6) 0.960859(10) 0.270698(8) 0.01878(5) Uani 1 1 d .
Zn1 Zn 1.0000 0.41740(5) 0.2500 0.02117(13) Uani 1 2 d S
O1 O 0.15151(13) 0.9509(2) 0.17177(15) 0.0279(6) Uani 1 1 d .
O2 O 0.28042(14) 0.9730(2) 0.36776(16) 0.0329(7) Uani 1 1 d .
O3 O 0.14755(13) 0.9609(2) 0.30687(16) 0.0310(6) Uani 1 1 d .
O4 O 0.12141(14) 1.0936(2) 0.36048(16) 0.0379(7) Uani 1 1 d .
O5 O 0.27377(12) 1.0804(2) 0.23291(15) 0.0272(6) Uani 1 1 d .
O6 O 0.19424(11) 1.1625(2) 0.26783(14) 0.0225(6) Uani 1 1 d .
O7 O 0.28079(12) 0.8396(2) 0.24556(16) 0.0304(6) Uani 1 1 d .
O8 O 0.20288(12) 0.7583(2) 0.28276(15) 0.0265(6) Uani 1 1 d .
C1 C 0.85017(18) 0.4588(3) 0.1572(2) 0.0284(9) Uani 1 1 d .
H1 H 0.8576 0.4966 0.2008 0.034 Uiso 1 1 calc R
C2 C 0.78778(19) 0.4565(3) 0.0914(2) 0.0313(9) Uani 1 1 d .
H2 H 0.7546 0.4913 0.0916 0.038 Uiso 1 1 calc R
C3 C 0.77640(18) 0.4021(3) 0.0267(2) 0.0289(9) Uani 1 1 d .
H3 H 0.7353 0.4004 -0.0178 0.035 Uiso 1 1 calc R
C4 C 0.82708(17) 0.3486(3) 0.0276(2) 0.0238(8) Uani 1 1 d .
C5 C 0.81918(19) 0.2874(3) -0.0361(2) 0.0275(9) Uani 1 1 d .
H5 H 0.7793 0.2864 -0.0825 0.033 Uiso 1 1 calc R
C6 C 0.86821(19) 0.2307(3) -0.0308(2) 0.0303(9) Uani 1 1 d .
H6 H 0.8617 0.1913 -0.0734 0.036 Uiso 1 1 calc R
C7 C 0.93045(18) 0.2306(3) 0.0401(2) 0.0244(8) Uani 1 1 d .
C8 C 0.94067(17) 0.2938(3) 0.1029(2) 0.0195(8) Uani 1 1 d .
C9 C 0.88782(16) 0.3535(3) 0.09712(19) 0.0187(8) Uani 1 1 d .
C10 C 0.9828(2) 0.1669(3) 0.0521(2) 0.0310(9) Uani 1 1 d .
H10 H 0.9789 0.1245 0.0118 0.037 Uiso 1 1 calc R
C11 C 1.0389(2) 0.1673(3) 0.1223(2) 0.0346(10) Uani 1 1 d .
H11 H 1.0728 0.1225 0.1310 0.042 Uiso 1 1 calc R
C12 C 1.04547(18) 0.2352(3) 0.1816(2) 0.0283(9) Uani 1 1 d .
H12 H 1.0844 0.2362 0.2292 0.034 Uiso 1 1 calc R
C13 C 0.9670(2) 0.5626(4) 0.3527(2) 0.0417(11) Uani 1 1 d .
H13 H 0.9623 0.4931 0.3705 0.050 Uiso 1 1 calc R
C14 C 0.9558(2) 0.6619(5) 0.3798(3) 0.0534(14) Uani 1 1 d .
H14 H 0.9432 0.6582 0.4143 0.064 Uiso 1 1 calc R
C15 C 0.9633(2) 0.7648(5) 0.3553(3) 0.0560(15) Uani 1 1 d .
H15 H 0.9561 0.8317 0.3733 0.067 Uiso 1 1 calc R
C16 C 0.98183(19) 0.7693(4) 0.3034(3) 0.0417(11) Uani 1 1 d .
C17 C 0.99102(17) 0.6651(3) 0.2775(2) 0.0327(10) Uani 1 1 d .
C18 C 0.9918(2) 0.8731(4) 0.2751(3) 0.0546(15) Uani 1 1 d .
H18 H 0.9864 0.9422 0.2927 0.065 Uiso 1 1 calc R
C19 C 0.26867(17) 1.1862(3) 0.2322(2) 0.0199(8) Uani 1 1 d .
C20 C 0.22316(17) 1.2345(3) 0.2528(2) 0.0204(8) Uani 1 1 d .
C21 C 0.13576(17) 0.9961(3) 0.3574(2) 0.0230(8) Uani 1 1 d .
C22 C 0.14000(16) 0.9067(3) 0.4124(2) 0.0228(8) Uani 1 1 d .
C23 C 0.1567(2) 0.7958(3) 0.4117(2) 0.0367(10) Uani 1 1 d .
H23 H 0.1669 0.7730 0.3769 0.044 Uiso 1 1 calc R
C24 C 0.1584(2) 0.7171(4) 0.4630(3) 0.0509(13) Uani 1 1 d .
H24 H 0.1685 0.6415 0.4614 0.061 Uiso 1 1 calc R
C25 C 0.1450(2) 0.7511(4) 0.5161(3) 0.0441(12) Uani 1 1 d .
H25 H 0.1464 0.6987 0.5506 0.053 Uiso 1 1 calc R
C26 C 0.1296(2) 0.8628(4) 0.5180(2) 0.0399(11) Uani 1 1 d .
H26 H 0.1214 0.8866 0.5545 0.048 Uiso 1 1 calc R
C27 C 0.1263(2) 0.9392(3) 0.4658(2) 0.0315(9) Uani 1 1 d .
H27 H 0.1146 1.0141 0.4663 0.038 Uiso 1 1 calc R
N1 N 0.99793(14) 0.2980(2) 0.17173(17) 0.0219(7) Uani 1 1 d .
N2 N 0.89904(14) 0.4100(3) 0.16069(16) 0.0215(7) Uani 1 1 d .
N3 N 0.98409(15) 0.5624(3) 0.30282(19) 0.0302(8) 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'
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 178.08(12) . .
O2 U1 O3 90.59(12) . .
O1 U1 O3 91.12(11) . .
O2 U1 O6 90.04(10) . .
O1 U1 O6 89.44(9) . .
O3 U1 O6 78.89(8) . .
O2 U1 O8 92.98(10) . .
O1 U1 O8 88.21(10) . .
O3 U1 O8 78.27(8) . .
O6 U1 O8 156.98(8) . .
O2 U1 O7 89.21(11) . .
O1 U1 O7 89.91(10) . .
O3 U1 O7 144.09(8) . .
O6 U1 O7 137.02(8) . .
O8 U1 O7 65.89(8) . .
O2 U1 O5 88.96(11) . .
O1 U1 O5 89.14(10) . .
O3 U1 O5 144.92(8) . .
O6 U1 O5 66.04(8) . .
O8 U1 O5 136.78(8) . .
O7 U1 O5 70.98(8) . .
N1 Zn1 N1 97.44(16) . 2_755
N1 Zn1 N2 78.22(11) . .
N1 Zn1 N2 98.70(11) 2_755 .
N1 Zn1 N2 98.71(11) . 2_755
N1 Zn1 N2 78.21(11) 2_755 2_755
N2 Zn1 N2 175.41(16) . 2_755
N1 Zn1 N3 93.68(12) . 2_755
N1 Zn1 N3 165.22(12) 2_755 2_755
N2 Zn1 N3 93.05(11) . 2_755
N2 Zn1 N3 90.54(12) 2_755 2_755
N1 Zn1 N3 165.22(11) . .
N1 Zn1 N3 93.68(12) 2_755 .
N2 Zn1 N3 90.53(11) . .
N2 Zn1 N3 93.05(11) 2_755 .
N3 Zn1 N3 77.20(18) 2_755 .
C21 O3 U1 146.5(2) . .
C19 O5 U1 119.9(2) . .
C20 O6 U1 120.9(2) . .
C20 O7 U1 120.2(2) 4_545 .
C19 O8 U1 120.8(2) 4_545 .
N2 C1 C2 123.4(4) . .
C3 C2 C1 118.8(4) . .
C2 C3 C4 119.9(4) . .
C9 C4 C3 117.0(3) . .
C9 C4 C5 119.4(3) . .
C3 C4 C5 123.6(4) . .
C6 C5 C4 121.5(4) . .
C5 C6 C7 120.6(4) . .
C8 C7 C10 116.5(4) . .
C8 C7 C6 119.4(3) . .
C10 C7 C6 124.1(3) . .
N1 C8 C7 123.0(3) . .
N1 C8 C9 117.3(3) . .
C7 C8 C9 119.6(3) . .
N2 C9 C4 122.8(3) . .
N2 C9 C8 117.9(3) . .
C4 C9 C8 119.3(3) . .
C11 C10 C7 120.0(4) . .
C10 C11 C12 119.8(4) . .
N1 C12 C11 121.7(4) . .
N3 C13 C14 123.0(5) . .
C15 C14 C13 119.5(5) . .
C14 C15 C16 119.8(4) . .
C15 C16 C17 117.3(4) . .
C15 C16 C18 124.0(4) . .
C17 C16 C18 118.7(4) . .
N3 C17 C16 122.6(4) . .
N3 C17 C17 117.9(2) . 2_755
C16 C17 C17 119.5(3) . 2_755
C18 C18 C16 121.8(3) 2_755 .
O5 C19 O8 127.4(3) . 4
O5 C19 C20 116.9(3) . .
O8 C19 C20 115.7(3) 4 .
O7 C20 O6 126.5(3) 4 .
O7 C20 C19 117.3(3) 4 .
O6 C20 C19 116.2(3) . .
O4 C21 O3 123.1(3) . .
O4 C21 C22 121.1(3) . .
O3 C21 C22 115.8(3) . .
C23 C22 C27 118.9(4) . .
C23 C22 C21 123.2(3) . .
C27 C22 C21 118.0(3) . .
C22 C23 C24 120.2(4) . .
C25 C24 C23 120.2(4) . .
C26 C25 C24 119.8(4) . .
C25 C26 C27 119.7(4) . .
C26 C27 C22 121.3(4) . .
C12 N1 C8 119.0(3) . .
C12 N1 Zn1 127.8(3) . .
C8 N1 Zn1 113.2(2) . .
C1 N2 C9 118.1(3) . .
C1 N2 Zn1 130.0(3) . .
C9 N2 Zn1 111.6(2) . .
C13 N3 C17 117.8(4) . .
C13 N3 Zn1 128.7(3) . .
C17 N3 Zn1 113.5(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O2 1.763(3) .
U1 O1 1.779(3) .
U1 O3 2.211(2) .
U1 O6 2.421(2) .
U1 O8 2.431(2) .
U1 O7 2.436(2) .
U1 O5 2.449(2) .
Zn1 N1 2.126(3) .
Zn1 N1 2.126(3) 2_755
Zn1 N2 2.161(3) .
Zn1 N2 2.161(3) 2_755
Zn1 N3 2.179(3) 2_755
Zn1 N3 2.179(3) .
O3 C21 1.306(4) .
O4 C21 1.212(4) .
O5 C19 1.248(4) .
O6 C20 1.260(4) .
O7 C20 1.241(4) 4_545
O8 C19 1.252(4) 4_545
C1 N2 1.319(4) .
C1 C2 1.398(5) .
C2 C3 1.368(5) .
C3 C4 1.409(5) .
C4 C9 1.406(5) .
C4 C5 1.420(5) .
C5 C6 1.349(5) .
C6 C7 1.437(5) .
C7 C8 1.396(5) .
C7 C10 1.409(5) .
C8 N1 1.357(4) .
C8 C9 1.445(5) .
C9 N2 1.361(4) .
C10 C11 1.356(6) .
C11 C12 1.398(5) .
C12 N1 1.318(4) .
C13 N3 1.322(5) .
C13 C14 1.389(6) .
C14 C15 1.364(7) .
C15 C16 1.391(6) .
C16 C17 1.406(6) .
C16 C18 1.433(6) .
C17 N3 1.365(5) .
C17 C17 1.441(8) 2_755
C18 C18 1.317(9) 2_755
C19 O8 1.252(4) 4
C19 C20 1.534(5) .
C20 O7 1.241(4) 4
C21 C22 1.511(5) .
C22 C23 1.370(5) .
C22 C27 1.384(5) .
C23 C24 1.392(6) .
C24 C25 1.379(6) .
C25 C26 1.374(6) .
C26 C27 1.375(5) .
