#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:34:18 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180343 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/12/7201282.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_7201282
loop_
_publ_author_name
'Thuéry, Pierre'
_publ_section_title
;
 Structural variability in uranyl--lanthanide heterometallic complexes
 with DOTA and oxalato ligands
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              2319
_journal_paper_doi               10.1039/b907392b
_journal_volume                  11
_journal_year                    2009
_chemical_formula_sum            'C18 H27 Gd N4 O18 U2'
_chemical_formula_weight         1220.75
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 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                 111.391(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.4846(13)
_cell_length_b                   6.6387(11)
_cell_length_c                   16.759(2)
_cell_measurement_reflns_used    61943
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      3.07
_cell_volume                     1396.9(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, 1999)'
_computing_publication_material
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(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 nine ω scans with 2° steps (543 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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            61943
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.001
_exptl_absorpt_correction_T_max  0.326
_exptl_absorpt_correction_T_min  0.097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    2.902
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1110
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.709
_refine_diff_density_min         -5.085
_refine_diff_density_rms         0.378
_refine_ls_extinction_coef       0.0041(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         2637
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0802
_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)+(0.1317P)²+43.3490P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2183
_refine_ls_wR_factor_ref         0.2252
_reflns_number_gt                2243
_reflns_number_total             2637
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b907392b.txt
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               7201282
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
U U 0.74492(5) 0.48406(12) 0.61674(4) 0.0426(4) Uani 1 1 d . . .
Gd Gd 0.7500 0.7781(3) 0.2500 0.0508(5) Uani 1 2 d S . .
N1 N 0.7620(14) 1.002(3) 0.3776(9) 0.051(5) Uani 1 1 d . . .
N2 N 0.9150(14) 0.999(2) 0.2902(10) 0.048(4) Uani 1 1 d . . .
O1 O 0.8318(12) 0.618(3) 0.3841(8) 0.057(4) Uani 1 1 d . . .
O2 O 0.8260(12) 0.559(3) 0.5136(9) 0.069(5) Uani 1 1 d . . .
O3 O 0.8987(10) 0.616(2) 0.2377(8) 0.051(3) Uani 1 1 d . . .
O4 O 1.0688(13) 0.535(3) 0.3081(8) 0.061(4) Uani 1 1 d . . .
O5 O 0.7414(11) 0.219(3) 0.5912(9) 0.069(5) Uani 1 1 d . . .
O6 O 0.7453(12) 0.750(3) 0.6405(10) 0.068(5) Uani 1 1 d . . .
O7 O 0.6100(11) 0.532(2) 0.4732(9) 0.055(4) Uani 1 1 d . . .
O8 O 0.5610(11) 0.458(3) 0.6087(8) 0.060(4) Uani 1 1 d . . .
O9 O 0.7500 0.392(4) 0.7500 0.057(5) Uani 1 2 d S . .
O10 O 0.670(3) 1.012(4) 0.7253(18) 0.055(8) Uani 0.50 1 d P . .
C1 C 0.8698(16) 1.096(4) 0.4164(12) 0.051(5) Uani 1 1 d . . .
H1A H 0.9195 0.9978 0.4525 0.061 Uiso 1 1 calc R . .
H1B H 0.8664 1.2083 0.4521 0.061 Uiso 1 1 calc R . .
C2 C 0.9093(18) 1.168(4) 0.3481(13) 0.060(5) Uani 1 1 d . . .
H2A H 0.8618 1.2718 0.3142 0.072 Uiso 1 1 calc R . .
H2B H 0.9794 1.2272 0.3750 0.072 Uiso 1 1 calc R . .
C3 C 0.9246(16) 1.084(4) 0.2110(12) 0.056(5) Uani 1 1 d . . .
H3A H 0.9513 0.9801 0.1834 0.067 Uiso 1 1 calc R . .
H3B H 0.9768 1.1920 0.2273 0.067 Uiso 1 1 calc R . .
C4 C 0.8206(17) 1.167(4) 0.1462(13) 0.060(6) Uani 1 1 d . . .
H4A H 0.7961 1.2793 0.1709 0.072 Uiso 1 1 calc R . .
H4B H 0.8321 1.2135 0.0954 0.072 Uiso 1 1 calc R . .
C5 C 0.7426(16) 0.867(4) 0.4408(13) 0.055(5) Uani 1 1 d . . .
H5A H 0.6670 0.8384 0.4231 0.066 Uiso 1 1 calc R . .
H5B H 0.7655 0.9321 0.4964 0.066 Uiso 1 1 calc R . .
C6 C 0.8045(16) 0.669(4) 0.4474(12) 0.060(6) Uani 1 1 d . . .
C7 C 1.0094(18) 0.868(4) 0.3315(13) 0.062(6) Uani 1 1 d . . .
H7A H 1.0215 0.8529 0.3919 0.074 Uiso 1 1 calc R . .
H7B H 1.0721 0.9302 0.3266 0.074 Uiso 1 1 calc R . .
C8 C 0.9904(16) 0.663(3) 0.2881(11) 0.050(5) Uani 1 1 d . . .
C9 C 0.513(2) 0.520(3) 0.4606(14) 0.056(6) 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'
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'
Gd Gd -0.1653 3.9035 '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'
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
_geom_angle_publ_flag
O6 U O5 178.7(7) . . ?
O6 U O9 92.8(8) . . ?
O5 U O9 87.7(8) . . ?
O6 U O4 91.1(7) . 3_766 ?
O5 U O4 90.2(6) . 3_766 ?
O9 U O4 79.5(3) . 3_766 ?
O6 U O2 89.5(7) . . ?
O5 U O2 90.6(7) . . ?
O9 U O2 153.3(4) . . ?
O4 U O2 73.9(5) 3_766 . ?
O6 U O8 90.1(7) . . ?
O5 U O8 88.8(6) . . ?
O9 U O8 72.8(3) . . ?
O4 U O8 152.3(5) 3_766 . ?
O2 U O8 133.8(5) . . ?
O6 U O7 91.8(6) . . ?
O5 U O7 87.0(6) . . ?
O9 U O7 137.6(3) . . ?
O4 U O7 142.5(5) 3_766 . ?
O2 U O7 68.8(5) . . ?
O8 U O7 65.1(5) . . ?
O3 Gd O3 125.5(7) . 2_655 ?
O3 Gd O1 76.1(5) . . ?
O3 Gd O1 80.1(5) 2_655 . ?
O3 Gd O1 80.1(5) . 2_655 ?
O3 Gd O1 76.1(5) 2_655 2_655 ?
O1 Gd O1 126.6(8) . 2_655 ?
O3 Gd N2 159.0(5) . 2_655 ?
O3 Gd N2 66.1(5) 2_655 2_655 ?
O1 Gd N2 124.8(5) . 2_655 ?
O1 Gd N2 87.0(5) 2_655 2_655 ?
O3 Gd N2 66.1(5) . . ?
O3 Gd N2 159.0(5) 2_655 . ?
O1 Gd N2 87.0(5) . . ?
O1 Gd N2 124.8(5) 2_655 . ?
N2 Gd N2 109.6(8) 2_655 . ?
O3 Gd N1 122.9(5) . . ?
O3 Gd N1 89.3(5) 2_655 . ?
O1 Gd N1 66.5(5) . . ?
O1 Gd N1 157.0(5) 2_655 . ?
N2 Gd N1 70.7(5) 2_655 . ?
N2 Gd N1 70.3(5) . . ?
O3 Gd N1 89.3(5) . 2_655 ?
O3 Gd N1 122.9(5) 2_655 2_655 ?
O1 Gd N1 157.0(5) . 2_655 ?
O1 Gd N1 66.5(5) 2_655 2_655 ?
N2 Gd N1 70.3(5) 2_655 2_655 ?
N2 Gd N1 70.7(5) . 2_655 ?
N1 Gd N1 109.1(8) . 2_655 ?
C5 N1 C1 109.8(15) . . ?
C5 N1 C4 108.8(16) . 2_655 ?
C1 N1 C4 108.6(17) . 2_655 ?
C5 N1 Gd 105.9(12) . . ?
C1 N1 Gd 111.1(12) . . ?
C4 N1 Gd 112.6(11) 2_655 . ?
C7 N2 C3 107.4(17) . . ?
C7 N2 C2 111.8(16) . . ?
C3 N2 C2 109.3(17) . . ?
C7 N2 Gd 107.8(13) . . ?
C3 N2 Gd 109.6(12) . . ?
C2 N2 Gd 110.8(13) . . ?
C6 O1 Gd 119.4(14) . . ?
C6 O2 U 136.6(14) . . ?
C8 O3 Gd 119.3(13) . . ?
C8 O4 U 141.2(15) . 3_766 ?
C9 O7 U 121.0(13) . . ?
C9 O8 U 120.2(14) 3_666 . ?
U O9 U 149.1(12) . 2_656 ?
N1 C1 C2 111.1(16) . . ?
N1 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
N2 C2 C1 111.5(19) . . ?
N2 C2 H2A 109.3 . . ?
C1 C2 H2A 109.3 . . ?
N2 C2 H2B 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
N2 C3 C4 114.4(17) . . ?
N2 C3 H3A 108.7 . . ?
C4 C3 H3A 108.7 . . ?
N2 C3 H3B 108.7 . . ?
C4 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
N1 C4 C3 109(2) 2_655 . ?
N1 C4 H4A 109.9 2_655 . ?
C3 C4 H4A 109.9 . . ?
N1 C4 H4B 109.9 2_655 . ?
C3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
N1 C5 C6 109.5(16) . . ?
N1 C5 H5A 109.8 . . ?
C6 C5 H5A 109.8 . . ?
N1 C5 H5B 109.8 . . ?
C6 C5 H5B 109.8 . . ?
H5A C5 H5B 108.2 . . ?
O2 C6 O1 122(2) . . ?
O2 C6 C5 119.9(18) . . ?
O1 C6 C5 118(2) . . ?
N2 C7 C8 109.4(17) . . ?
N2 C7 H7A 109.8 . . ?
C8 C7 H7A 109.8 . . ?
N2 C7 H7B 109.8 . . ?
C8 C7 H7B 109.8 . . ?
H7A C7 H7B 108.2 . . ?
O3 C8 O4 121(2) . . ?
O3 C8 C7 119.8(19) . . ?
O4 C8 C7 118.7(19) . . ?
O8 C9 O7 126(2) 3_666 . ?
O8 C9 C9 118(3) 3_666 3_666 ?
O7 C9 C9 115(3) . 3_666 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U O6 1.808(19) . ?
U O5 1.81(2) . ?
U O9 2.292(7) . ?
U O4 2.367(16) 3_766 ?
U O2 2.409(15) . ?
U O8 2.441(14) . ?
U O7 2.451(13) . ?
Gd O3 2.351(14) . ?
Gd O3 2.351(14) 2_655 ?
Gd O1 2.364(14) . ?
Gd O1 2.364(14) 2_655 ?
Gd N2 2.541(17) 2_655 ?
Gd N2 2.541(17) . ?
Gd N1 2.559(16) . ?
Gd N1 2.559(16) 2_655 ?
N1 C5 1.48(3) . ?
N1 C1 1.50(3) . ?
N1 C4 1.51(3) 2_655 ?
N2 C7 1.48(3) . ?
N2 C3 1.49(3) . ?
N2 C2 1.51(3) . ?
O1 C6 1.29(2) . ?
O2 C6 1.27(3) . ?
O3 C8 1.26(2) . ?
O4 C8 1.30(3) . ?
O4 U 2.367(16) 3_766 ?
O7 C9 1.25(3) . ?
O8 C9 1.23(3) 3_666 ?
O9 U 2.292(7) 2_656 ?
C1 C2 1.51(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.53(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N1 1.51(3) 2_655 ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.54(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C7 C8 1.52(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C9 O8 1.23(3) 3_666 ?
C9 C9 1.51(4) 3_666 ?
