#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:54:12 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180454 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/23/7212326.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_7212326
loop_
_publ_author_name
'Thuéry, Pierre'
_publ_section_title
;
 Uranyl--organic assemblies with the macrocyclic ligand
 1,4,8,11-tetraazacyclotetradecane-1,4,8,11-tetraacetate (TETA)
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              1905
_journal_paper_doi               10.1039/b924966d
_journal_volume                  12
_journal_year                    2010
_chemical_formula_sum            'C18 H34 Cl N5 O14 U'
_chemical_formula_weight         817.98
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 103.303(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.3512(13)
_cell_length_b                   12.8168(6)
_cell_length_c                   10.9421(6)
_cell_measurement_reflns_used    42985
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.67
_cell_measurement_theta_min      2.47
_cell_volume                     2777.5(3)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and four ω scans with 2° steps (412 frames)'
_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    0.0472
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            42985
_diffrn_reflns_theta_full        25.67
_diffrn_reflns_theta_max         25.67
_diffrn_reflns_theta_min         2.47
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.014
_exptl_absorpt_correction_T_max  0.835
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    1.956
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.804
_refine_diff_density_min         -1.098
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2763
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0326
_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)+(0.0360P)²+10.8841P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0738
_reflns_number_gt                2456
_reflns_number_total             2763
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b924966d.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7212326
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
U U 0.119529(13) 0.0000 0.42113(3) 0.01820(10) Uani 1 2 d S
Cl Cl 0.26483(12) 0.5000 0.0576(2) 0.0414(5) Uani 1 2 d S
O1 O 0.1166(3) 0.0000 0.5815(5) 0.0223(11) Uani 1 2 d S
O2 O 0.1244(3) 0.0000 0.2608(5) 0.0261(12) Uani 1 2 d S
O3 O 0.16124(19) 0.1733(3) 0.4369(4) 0.0264(8) Uani 1 1 d .
O4 O 0.1777(2) 0.3319(3) 0.5176(4) 0.0351(10) Uani 1 1 d .
O5 O 0.52519(18) 0.3907(3) 0.3697(4) 0.0338(10) Uani 1 1 d .
O6 O 0.52795(18) 0.3098(3) 0.1884(4) 0.0315(9) Uani 1 1 d .
O7 O 0.2442(3) 0.0000 0.4833(5) 0.0291(13) Uani 1 2 d S
H7 H 0.2680 0.0523 0.4697 0.035 Uiso 1 1 d R
O8 O 0.5066(2) 0.0848(4) 0.2018(7) 0.0704(18) Uani 1 1 d .
O9 O 0.4248(4) 0.0000 0.0853(7) 0.0511(18) Uani 1 2 d S
N1 N 0.1574(2) 0.2400(3) 0.1954(4) 0.0194(9) Uani 1 1 d .
H1 H 0.1191 0.1896 0.2045 0.023 Uiso 1 1 d R
N2 N 0.4001(2) 0.2318(3) 0.1615(4) 0.0209(9) Uani 1 1 d .
H2 H 0.4404 0.1923 0.1706 0.025 Uiso 1 1 d R
N3 N 0.4791(4) 0.0000 0.1624(9) 0.042(2) Uani 1 2 d S
C1 C 0.2211(2) 0.1773(4) 0.2047(5) 0.0216(11) Uani 1 1 d .
H1A H 0.2128 0.1233 0.1408 0.026 Uiso 1 1 calc R
H1B H 0.2327 0.1433 0.2860 0.026 Uiso 1 1 calc R
C2 C 0.2804(3) 0.2438(5) 0.1883(6) 0.0323(13) Uani 1 1 d .
H2A H 0.2922 0.2935 0.2567 0.039 Uiso 1 1 calc R
H2B H 0.2682 0.2822 0.1100 0.039 Uiso 1 1 calc R
C3 C 0.3402(2) 0.1725(4) 0.1875(5) 0.0206(11) Uani 1 1 d .
H3A H 0.3537 0.1379 0.2682 0.025 Uiso 1 1 calc R
H3B H 0.3265 0.1193 0.1237 0.025 Uiso 1 1 calc R
C4 C 0.3849(3) 0.2845(4) 0.0354(5) 0.0226(11) Uani 1 1 d .
H4A H 0.4240 0.3247 0.0265 0.027 Uiso 1 1 calc R
H4B H 0.3475 0.3325 0.0302 0.027 Uiso 1 1 calc R
C5 C 0.3670(3) 0.2050(4) -0.0719(5) 0.0220(11) Uani 1 1 d .
H5A H 0.4065 0.1634 -0.0746 0.026 Uiso 1 1 calc R
H5B H 0.3321 0.1584 -0.0571 0.026 Uiso 1 1 calc R
C6 C 0.1628(3) 0.3189(4) 0.3001(5) 0.0231(11) Uani 1 1 d .
H6A H 0.1234 0.3639 0.2812 0.028 Uiso 1 1 calc R
H6B H 0.2023 0.3621 0.3032 0.028 Uiso 1 1 calc R
C7 C 0.1680(2) 0.2698(4) 0.4283(5) 0.0238(12) Uani 1 1 d .
C8 C 0.4265(3) 0.3085(5) 0.2645(5) 0.0273(12) Uani 1 1 d .
H8A H 0.4230 0.2785 0.3442 0.033 Uiso 1 1 calc R
H8B H 0.3988 0.3708 0.2507 0.033 Uiso 1 1 calc R
C9 C 0.4995(3) 0.3383(4) 0.2717(5) 0.0254(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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 U O2 178.8(2) . .
O1 U O5 91.46(16) . 3_445
O2 U O5 89.53(16) . 3_445
O1 U O5 91.46(16) . 8_455
O2 U O5 89.53(16) . 8_455
O5 U O5 73.6(2) 3_445 8_455
O1 U O3 91.20(11) . .
O2 U O3 88.37(11) . .
O5 U O3 147.10(14) 3_445 .
O5 U O3 73.53(14) 8_455 .
O1 U O3 91.20(11) . 6
O2 U O3 88.37(11) . 6
O5 U O3 73.53(14) 3_445 6
O5 U O3 147.10(14) 8_455 6
O3 U O3 139.17(18) . 6
O1 U O7 89.7(2) . .
O2 U O7 89.1(2) . .
O5 U O7 143.16(11) 3_445 .
O5 U O7 143.16(11) 8_455 .
O3 U O7 69.63(9) . .
O3 U O7 69.63(9) 6 .
C7 O3 U 164.9(4) . .
C9 O5 U 132.4(4) . 3
U O7 H7 122.4 . .
C5 N1 C1 114.3(4) 7 .
C5 N1 C6 108.6(4) 7 .
C1 N1 C6 113.2(4) . .
C5 N1 H1 106.2 7 .
C1 N1 H1 108.3 . .
C6 N1 H1 105.6 . .
C8 N2 C4 110.9(4) . .
C8 N2 C3 110.6(4) . .
C4 N2 C3 113.2(4) . .
C8 N2 H2 96.8 . .
C4 N2 H2 109.0 . .
C3 N2 H2 115.2 . .
O9 N3 O8 119.8(4) . 6
O9 N3 O8 119.8(4) . .
O8 N3 O8 120.4(8) 6 .
N1 C1 C2 112.7(4) . .
N1 C1 H1A 109.1 . .
C2 C1 H1A 109.1 . .
N1 C1 H1B 109.1 . .
C2 C1 H1B 109.1 . .
H1A C1 H1B 107.8 . .
C1 C2 C3 108.8(4) . .
C1 C2 H2A 109.9 . .
C3 C2 H2A 109.9 . .
C1 C2 H2B 109.9 . .
C3 C2 H2B 109.9 . .
H2A C2 H2B 108.3 . .
N2 C3 C2 112.3(4) . .
N2 C3 H3A 109.1 . .
C2 C3 H3A 109.1 . .
N2 C3 H3B 109.1 . .
C2 C3 H3B 109.1 . .
H3A C3 H3B 107.9 . .
N2 C4 C5 111.4(4) . .
N2 C4 H4A 109.3 . .
C5 C4 H4A 109.3 . .
N2 C4 H4B 109.3 . .
C5 C4 H4B 109.3 . .
H4A C4 H4B 108.0 . .
N1 C5 C4 110.3(4) 7 .
N1 C5 H5A 109.6 7 .
C4 C5 H5A 109.6 . .
N1 C5 H5B 109.6 7 .
C4 C5 H5B 109.6 . .
H5A C5 H5B 108.1 . .
N1 C6 C7 113.6(4) . .
N1 C6 H6A 108.8 . .
C7 C6 H6A 108.8 . .
N1 C6 H6B 108.8 . .
C7 C6 H6B 108.8 . .
H6A C6 H6B 107.7 . .
O4 C7 O3 125.1(5) . .
O4 C7 C6 115.3(5) . .
O3 C7 C6 119.6(5) . .
N2 C8 C9 112.5(4) . .
N2 C8 H8A 109.1 . .
C9 C8 H8A 109.1 . .
N2 C8 H8B 109.1 . .
C9 C8 H8B 109.1 . .
H8A C8 H8B 107.8 . .
O6 C9 O5 127.2(5) . .
O6 C9 C8 120.2(5) . .
O5 C9 C8 112.6(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U O1 1.770(5) .
U O2 1.780(5) .
U O5 2.339(4) 3_445
U O5 2.339(4) 8_455
U O3 2.369(4) .
U O3 2.369(4) 6
U O7 2.471(5) .
O3 C7 1.251(6) .
O4 C7 1.241(7) .
O5 C9 1.271(6) .
O5 U 2.339(4) 3
O6 C9 1.242(7) .
O7 H7 0.8592 .
O8 N3 1.253(6) .
O9 N3 1.226(10) .
N1 C5 1.503(6) 7
N1 C1 1.509(6) .
N1 C6 1.513(6) .
N1 H1 1.0341 .
N2 C8 1.499(7) .
N2 C4 1.504(7) .
N2 C3 1.516(6) .
N2 H2 0.9487 .
N3 O8 1.253(6) 6
C1 C2 1.521(7) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 C3 1.524(7) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 C5 1.535(7) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 N1 1.503(6) 7
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 C7 1.518(7) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C8 C9 1.519(7) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O6 1.03 1.82 2.694(5) 139.4 8_455
N2 H2 O8 0.95 1.90 2.829(7) 164.6 .
O7 H7 O4 0.86 1.84 2.678(5) 165.9 7_556
