#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:07:42 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179468 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/65/4336532.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_4336532
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            'C24 H18 N2 O6 U'
_chemical_formula_weight         668.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.123(3)
_cell_angle_beta                 80.122(3)
_cell_angle_gamma                74.356(3)
_cell_formula_units_Z            2
_cell_length_a                   8.8559(14)
_cell_length_b                   9.0269(14)
_cell_length_c                   14.430(2)
_cell_measurement_temperature    173(2)
_cell_volume                     1094.2(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 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0770
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6076
_diffrn_reflns_theta_full        26.10
_diffrn_reflns_theta_max         26.10
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    7.461
_exptl_absorpt_correction_T_max  0.327
_exptl_absorpt_correction_T_min  0.123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sasabs
_exptl_crystal_density_diffrn    2.029
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.821
_refine_diff_density_min         -2.402
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0431
_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)+(0.0423P)²+1.8539P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0989
_reflns_number_gt                3509
_reflns_number_total             4257
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4012444_si_002_6.cif
_cod_data_source_block           6
_cod_original_cell_volume        1094.3(3)
_cod_database_code               4336532
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.24307(4) 0.83179(3) 0.72498(2) 0.02746(12) Uani 1 1 d .
O1 O 0.3888(7) 0.6811(6) 0.6597(4) 0.0329(14) Uani 1 1 d .
O2 O 0.0982(7) 0.9832(6) 0.7899(4) 0.0354(15) Uani 1 1 d .
O3 O 0.0189(7) 0.7349(6) 0.7020(4) 0.0360(15) Uani 1 1 d .
O4 O 0.1441(7) 0.6354(7) 0.8181(4) 0.0393(16) Uani 1 1 d .
O5 O 0.3616(7) 0.7606(6) 0.8657(4) 0.0360(15) Uani 1 1 d .
O6 O 0.4704(7) 0.9058(6) 0.7668(4) 0.0339(14) Uani 1 1 d .
N1 N 0.2951(8) 1.0767(7) 0.6344(5) 0.0310(17) Uani 1 1 d .
N2 N 0.1897(8) 0.8796(7) 0.5487(5) 0.0311(17) Uani 1 1 d .
C1 C 0.0318(11) 0.6445(8) 0.7725(6) 0.031(2) Uani 1 1 d .
C2 C -0.0836(10) 0.5517(8) 0.7986(6) 0.0280(19) Uani 1 1 d .
C3 C -0.2003(11) 0.5585(9) 0.7447(6) 0.037(2) Uani 1 1 d .
H3 H -0.2057 0.6200 0.6917 0.044 Uiso 1 1 calc R
C4 C -0.3098(11) 0.4724(10) 0.7705(7) 0.043(2) Uani 1 1 d .
H4 H -0.3907 0.4786 0.7360 0.051 Uiso 1 1 calc R
C5 C -0.2976(13) 0.3786(10) 0.8472(8) 0.050(3) Uani 1 1 d .
H5 H -0.3680 0.3181 0.8624 0.060 Uiso 1 1 calc R
C6 C -0.1819(12) 0.3722(10) 0.9024(8) 0.048(3) Uani 1 1 d .
H6 H -0.1766 0.3107 0.9553 0.058 Uiso 1 1 calc R
C7 C -0.0753(11) 0.4590(9) 0.8771(7) 0.039(2) Uani 1 1 d .
H7 H 0.0031 0.4554 0.9132 0.046 Uiso 1 1 calc R
C8 C 0.5802(9) 0.8341(8) 0.9073(6) 0.029(2) Uani 1 1 d .
C9 C 0.5928(10) 0.7340(9) 0.9831(6) 0.030(2) Uani 1 1 d .
H9 H 0.5303 0.6652 0.9928 0.036 Uiso 1 1 calc R
C10 C 0.6965(11) 0.7357(10) 1.0434(7) 0.038(2) Uani 1 1 d .
H10 H 0.7042 0.6689 1.0939 0.045 Uiso 1 1 calc R
C11 C 0.7894(11) 0.8383(10) 1.0279(7) 0.040(2) Uani 1 1 d .
H11 H 0.8589 0.8403 1.0692 0.048 Uiso 1 1 calc R
C12 C 0.7819(11) 0.9360(9) 0.9543(6) 0.036(2) Uani 1 1 d .
H12 H 0.8462 1.0032 0.9451 0.044 Uiso 1 1 calc R
C13 C 0.6770(11) 0.9350(9) 0.8925(6) 0.038(2) Uani 1 1 d .
H13 H 0.6715 1.0011 0.8417 0.046 Uiso 1 1 calc R
C14 C 0.4657(10) 0.8329(8) 0.8444(6) 0.030(2) Uani 1 1 d .
C15 C 0.1299(11) 0.7782(11) 0.4110(7) 0.045(2) Uani 1 1 d .
H15 H 0.0870 0.7083 0.3859 0.054 Uiso 1 1 calc R
C16 C 0.1915(12) 0.8786(10) 0.3539(7) 0.046(3) Uani 1 1 d .
H16 H 0.1919 0.8786 0.2894 0.056 Uiso 1 1 calc R
C17 C 0.2533(11) 0.9801(10) 0.3950(7) 0.043(3) Uani 1 1 d .
H17 H 0.2986 1.0480 0.3576 0.051 Uiso 1 1 calc R
C18 C 0.2481(10) 0.9814(8) 0.4916(6) 0.034(2) Uani 1 1 d .
C19 C 0.1318(10) 0.7813(9) 0.5059(6) 0.038(2) Uani 1 1 d .
H19 H 0.0903 0.7108 0.5432 0.045 Uiso 1 1 calc R
C20 C 0.3333(11) 1.2235(9) 0.4962(7) 0.043(3) Uani 1 1 d .
H20 H 0.3377 1.2342 0.4316 0.052 Uiso 1 1 calc R
C21 C 0.3618(11) 1.3360(10) 0.5507(8) 0.051(3) Uani 1 1 d .
H21 H 0.3886 1.4215 0.5222 0.062 Uiso 1 1 calc R
C22 C 0.3501(11) 1.3191(9) 0.6457(8) 0.047(3) Uani 1 1 d .
H22 H 0.3618 1.3963 0.6828 0.057 Uiso 1 1 calc R
C23 C 0.3205(11) 1.1862(8) 0.6867(7) 0.042(3) Uani 1 1 d .
H23 H 0.3181 1.1725 0.7511 0.051 Uiso 1 1 calc R
C24 C 0.2984(10) 1.0957(8) 0.5419(6) 0.033(2) 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'
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
O2 U1 O1 179.6(2)
O2 U1 O5 88.9(3)
O1 U1 O5 91.1(2)
O2 U1 O4 92.4(2)
O1 U1 O4 88.0(2)
O5 U1 O4 66.4(2)
O2 U1 O3 85.7(2)
O1 U1 O3 94.6(2)
O5 U1 O3 119.13(18)
O4 U1 O3 53.4(2)
O2 U1 O6 94.7(2)
O1 U1 O6 85.0(2)
O5 U1 O6 53.06(17)
O4 U1 O6 118.7(2)
O3 U1 O6 172.13(18)
O2 U1 N1 77.8(2)
O1 U1 N1 101.8(2)
O5 U1 N1 117.3(2)
O4 U1 N1 169.2(2)
O3 U1 N1 120.5(2)
O6 U1 N1 67.2(2)
O2 U1 N2 103.9(3)
O1 U1 N2 76.1(2)
O5 U1 N2 165.28(19)
O4 U1 N2 119.4(2)
O3 U1 N2 69.89(19)
O6 U1 N2 117.50(19)
N1 U1 N2 59.9(2)
C1 O3 U1 93.4(5)
C1 O4 U1 93.8(5)
C14 O5 U1 94.9(5)
C14 O6 U1 93.3(5)
C24 N1 C23 119.9(6)
C24 N1 U1 123.7(5)
C23 N1 U1 116.4(5)
C19 N2 C18 115.8(8)
C19 N2 U1 120.4(5)
C18 N2 U1 122.4(6)
O4 C1 O3 119.2(7)
O4 C1 C2 121.1(7)
O3 C1 C2 119.6(9)
C3 C2 C7 120.1(7)
C3 C2 C1 119.8(7)
C7 C2 C1 120.1(9)
C2 C3 C4 119.4(9)
C5 C4 C3 119.7(10)
C4 C5 C6 121.3(8)
C7 C6 C5 118.7(9)
C6 C7 C2 120.8(10)
C9 C8 C13 119.0(9)
C9 C8 C14 120.0(7)
C13 C8 C14 121.0(8)
C10 C9 C8 120.8(7)
C9 C10 C11 119.0(8)
C12 C11 C10 121.9(10)
C11 C12 C13 119.5(8)
C12 C13 C8 119.8(8)
O5 C14 O6 118.7(9)
O5 C14 C8 120.9(7)
O6 C14 C8 120.4(7)
C16 C15 C19 119.4(9)
C15 C16 C17 117.9(10)
C16 C17 C18 120.5(8)
N2 C18 C17 122.0(8)
N2 C18 C24 114.3(8)
C17 C18 C24 123.7(7)
N2 C19 C15 124.5(7)
C24 C20 C21 118.0(9)
C22 C21 C20 119.6(7)
C21 C22 C23 119.7(9)
N1 C23 C22 120.8(9)
N1 C24 C20 121.9(8)
N1 C24 C18 116.7(6)
C20 C24 C18 121.2(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
U1 O2 1.766(5)
U1 O1 1.767(5)
U1 O5 2.434(7)
U1 O4 2.448(5)
U1 O3 2.449(6)
U1 O6 2.456(6)
U1 N1 2.638(6)
U1 N2 2.666(8)
O3 C1 1.283(10)
O4 C1 1.268(11)
O5 C14 1.258(9)
O6 C14 1.280(10)
N1 C24 1.337(11)
N1 C23 1.351(11)
N2 C19 1.350(11)
N2 C18 1.362(9)
C1 C2 1.482(10)
C2 C3 1.384(13)
C2 C7 1.387(12)
C3 C4 1.395(11)
C4 C5 1.372(14)
C5 C6 1.390(16)
C6 C7 1.379(11)
C8 C9 1.396(11)
C8 C13 1.398(11)
C8 C14 1.474(13)
C9 C10 1.373(13)
C10 C11 1.386(11)
C11 C12 1.358(13)
C12 C13 1.396(14)
C15 C16 1.364(12)
C15 C19 1.374(14)
C16 C17 1.381(14)
C17 C18 1.388(13)
C18 C24 1.482(12)
C20 C24 1.391(10)
C20 C21 1.404(14)
C21 C22 1.363(15)
C22 C23 1.389(11)
