#------------------------------------------------------------------------------
#$Date: 2016-03-26 20:54:12 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180454 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/23/7212327.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_7212327
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 H44 N4 O17 U'
_chemical_formula_weight         826.60
_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                 97.853(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.3207(11)
_cell_length_b                   16.6570(9)
_cell_length_c                   10.1919(4)
_cell_measurement_reflns_used    45059
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      3.17
_cell_volume                     3585.6(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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and five ω scans with 2° steps (487 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  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            45059
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.17
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.592
_exptl_absorpt_correction_T_max  0.759
_exptl_absorpt_correction_T_min  0.479
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.301
_refine_diff_density_min         -3.536
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3400
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0391
_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)+(0.0590P)²+18.5474P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1062
_reflns_number_gt                3069
_reflns_number_total             3400
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b924966d.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7212327
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
U U 0.5000 0.148902(17) 0.2500 0.01996(13) Uani 1 2 d S
O1 O 0.5480(2) 0.1517(2) 0.1221(4) 0.0272(9) Uani 1 1 d .
O2 O 0.4174(2) 0.1917(3) 0.0849(4) 0.0327(10) Uani 1 1 d .
O3 O 0.3189(2) 0.2052(3) -0.0142(4) 0.0421(12) Uani 1 1 d .
O4 O 0.44608(19) -0.0328(3) 0.6562(4) 0.0295(10) Uani 1 1 d .
O5 O 0.3495(2) -0.0454(3) 0.7194(4) 0.0332(10) Uani 1 1 d .
O6 O 0.5000 0.2943(4) 0.2500 0.062(2) Uani 1 2 d S
H6 H 0.4908 0.3258 0.3122 0.074 Uiso 1 1 d R
N1 N 0.2821(2) 0.2818(3) 0.2057(5) 0.0316(12) Uani 1 1 d .
H1 H 0.2620 0.2941 0.1267 0.038 Uiso 0.50 1 d PR
N2 N 0.2981(2) 0.0760(3) 0.5711(5) 0.0285(12) Uani 1 1 d .
H2 H 0.2807 0.0302 0.6009 0.034 Uiso 0.50 1 d PR
C1 C 0.2598(3) 0.2023(4) 0.2551(6) 0.0288(14) Uani 1 1 d .
H1A H 0.2666 0.1604 0.1925 0.035 Uiso 1 1 calc R
H1B H 0.2146 0.2054 0.2593 0.035 Uiso 1 1 calc R
C2 C 0.2941(3) 0.1799(4) 0.3919(6) 0.0311(14) Uani 1 1 d .
H2A H 0.3388 0.1716 0.3872 0.037 Uiso 1 1 calc R
H2B H 0.2901 0.2231 0.4541 0.037 Uiso 1 1 calc R
C3 C 0.2652(3) 0.1037(4) 0.4382(6) 0.0307(14) Uani 1 1 d .
H3A H 0.2678 0.0617 0.3733 0.037 Uiso 1 1 calc R
H3B H 0.2208 0.1131 0.4444 0.037 Uiso 1 1 calc R
C4 C 0.2951(3) 0.1351(4) 0.6840(6) 0.0293(14) Uani 1 1 d .
H4A H 0.3132 0.1860 0.6625 0.035 Uiso 1 1 calc R
H4B H 0.3198 0.1147 0.7641 0.035 Uiso 1 1 calc R
C5 C 0.2267(4) 0.1476(4) 0.7078(7) 0.0351(16) Uani 1 1 d .
H5A H 0.2005 0.1550 0.6230 0.042 Uiso 1 1 calc R
H5B H 0.2121 0.0997 0.7483 0.042 Uiso 1 1 calc R
C6 C 0.3503(3) 0.2776(4) 0.1860(6) 0.0326(15) Uani 1 1 d .
H6A H 0.3753 0.2610 0.2683 0.039 Uiso 1 1 calc R
H6B H 0.3645 0.3306 0.1640 0.039 Uiso 1 1 calc R
C7 C 0.3615(3) 0.2190(4) 0.0766(6) 0.0317(14) Uani 1 1 d .
C8 C 0.3667(3) 0.0545(4) 0.5633(6) 0.0278(13) Uani 1 1 d .
H8A H 0.3713 0.0389 0.4734 0.033 Uiso 1 1 calc R
H8B H 0.3934 0.1010 0.5864 0.033 Uiso 1 1 calc R
C9 C 0.3878(3) -0.0139(4) 0.6568(5) 0.0242(12) Uani 1 1 d .
O7 O 0.4445(3) 0.0974(5) -0.1381(7) 0.083(2) Uani 1 1 d U
O8 O 0.1874(3) -0.0580(3) 0.5413(7) 0.053(2) Uani 0.576(17) 1 d PU
O9 O 0.2206(6) -0.0737(6) 0.4790(10) 0.047(3) Uani 0.424(17) 1 d PU
O10 O 0.1134(5) 0.1872(7) 0.4002(12) 0.127(4) 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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 U O1 177.0(3) 2_655 .
O1 U O2 85.27(18) 2_655 2_655
O1 U O2 93.82(18) . 2_655
O1 U O2 93.82(18) 2_655 .
O1 U O2 85.27(18) . .
O2 U O2 145.0(2) 2_655 .
O1 U O4 91.19(17) 2_655 6
O1 U O4 91.27(17) . 6
O2 U O4 143.06(16) 2_655 6
O2 U O4 71.89(16) . 6
O1 U O4 91.27(17) 2_655 5_656
O1 U O4 91.19(17) . 5_656
O2 U O4 71.89(16) 2_655 5_656
O2 U O4 143.06(16) . 5_656
O4 U O4 71.4(2) 6 5_656
O1 U O6 88.49(13) 2_655 .
O1 U O6 88.49(13) . .
O2 U O6 72.49(12) 2_655 .
O2 U O6 72.49(12) . .
O4 U O6 144.28(10) 6 .
O4 U O6 144.28(11) 5_656 .
C7 O2 U 139.0(4) . .
C9 O4 U 127.7(4) . 5_656
U O6 H6 127.3 . .
C6 N1 C5 108.5(5) . 7_556
C6 N1 C1 111.0(5) . .
C5 N1 C1 114.8(5) 7_556 .
C6 N1 H1 104.4 . .
C5 N1 H1 105.7 7_556 .
C1 N1 H1 111.7 . .
C3 N2 C8 111.0(4) . .
C3 N2 C4 114.7(5) . .
C8 N2 C4 109.4(5) . .
C3 N2 H2 113.0 . .
C8 N2 H2 104.9 . .
C4 N2 H2 103.1 . .
N1 C1 C2 112.5(5) . .
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 . .
C3 C2 C1 108.9(6) . .
C3 C2 H2A 109.9 . .
C1 C2 H2A 109.9 . .
C3 C2 H2B 109.9 . .
C1 C2 H2B 109.9 . .
H2A C2 H2B 108.3 . .
C2 C3 N2 112.1(5) . .
C2 C3 H3A 109.2 . .
N2 C3 H3A 109.2 . .
C2 C3 H3B 109.2 . .
N2 C3 H3B 109.2 . .
H3A C3 H3B 107.9 . .
N2 C4 C5 110.4(6) . .
N2 C4 H4A 109.6 . .
C5 C4 H4A 109.6 . .
N2 C4 H4B 109.6 . .
C5 C4 H4B 109.6 . .
H4A C4 H4B 108.1 . .
N1 C5 C4 113.6(6) 7_556 .
N1 C5 H5A 108.8 7_556 .
C4 C5 H5A 108.8 . .
N1 C5 H5B 108.8 7_556 .
C4 C5 H5B 108.8 . .
H5A C5 H5B 107.7 . .
N1 C6 C7 112.3(6) . .
N1 C6 H6A 109.1 . .
C7 C6 H6A 109.1 . .
N1 C6 H6B 109.1 . .
C7 C6 H6B 109.1 . .
H6A C6 H6B 107.9 . .
O3 C7 O2 125.2(6) . .
O3 C7 C6 119.9(6) . .
O2 C7 C6 114.8(6) . .
C9 C8 N2 110.5(5) . .
C9 C8 H8A 109.6 . .
N2 C8 H8A 109.6 . .
C9 C8 H8B 109.6 . .
N2 C8 H8B 109.6 . .
H8A C8 H8B 108.1 . .
O5 C9 O4 127.9(6) . .
O5 C9 C8 119.4(5) . .
O4 C9 C8 112.7(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U O1 1.765(4) 2_655
U O1 1.765(4) .
U O2 2.372(4) 2_655
U O2 2.372(4) .
U O4 2.382(4) 6
U O4 2.382(4) 5_656
U O6 2.422(7) .
O2 C7 1.269(7) .
O3 C7 1.226(8) .
O4 C9 1.283(7) .
O4 U 2.382(4) 5_656
O5 C9 1.220(7) .
O6 H6 0.8656 .
N1 C6 1.496(8) .
N1 C5 1.496(8) 7_556
N1 C1 1.516(8) .
N1 H1 0.8830 .
N2 C3 1.511(7) .
N2 C8 1.518(7) .
N2 C4 1.522(8) .
N2 H2 0.9174 .
C1 C2 1.530(8) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 C3 1.514(10) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 C5 1.526(9) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 N1 1.496(8) 7_556
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 C7 1.524(9) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C8 C9 1.513(8) .
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 O3 0.88 1.94 2.710(7) 145.4 7
N2 H2 O5 0.92 2.17 2.668(6) 113.1 .
