#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:34:18 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180343 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/12/7201281.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_7201281
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            'C38 H64 Gd2 N8 O44 U4'
_chemical_formula_weight         2603.59
_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                 115.999(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   43.698(2)
_cell_length_b                   8.3956(3)
_cell_length_c                   19.4670(8)
_cell_measurement_reflns_used    150622
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.94
_cell_volume                     6419.1(5)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and eight ω scans with 2° steps (540 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  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            150622
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.94
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.205
_exptl_absorpt_correction_T_max  0.614
_exptl_absorpt_correction_T_min  0.408
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    2.694
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             4784
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.565
_refine_diff_density_min         -2.393
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         6060
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0644P)²+131.1216P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1222
_reflns_number_gt                5057
_reflns_number_total             6060
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b907392b.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7201281
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
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.811815(9) 0.41852(4) 0.485203(19) 0.02741(13) Uani 1 1 d . . .
U2A U 1.03680(2) 0.17798(11) 0.40930(4) 0.0313(3) Uani 0.5297(19) 1 d P . .
U2B U 1.02976(2) 0.93848(11) 0.39231(6) 0.0314(3) Uani 0.4703(19) 1 d P . .
Gd Gd 0.873309(11) 0.15924(5) 0.29910(2) 0.02198(13) Uani 1 1 d . . .
O1 O 0.84183(16) 0.2872(9) 0.3550(3) 0.0311(15) Uani 1 1 d . . .
O2 O 0.79656(18) 0.4125(9) 0.3508(4) 0.0331(16) Uani 1 1 d . . .
O3 O 0.86030(18) 0.3970(8) 0.2209(4) 0.0325(16) Uani 1 1 d . . .
O4 O 0.84902(19) 0.5171(9) 0.1110(4) 0.0374(17) Uani 1 1 d . . .
O5 O 0.92663(17) 0.1585(9) 0.2955(4) 0.0347(16) Uani 1 1 d . . .
O6 O 0.9782(3) 0.0560(16) 0.3415(7) 0.050(3) Uani 1 1 d . . .
O7 O 0.90434(19) 0.0555(10) 0.4227(4) 0.041(2) Uani 1 1 d . . .
O8 O 0.9094(3) -0.0703(17) 0.5265(7) 0.067(3) Uani 1 1 d . . .
O9 O 0.79355(18) 0.6107(9) 0.4714(4) 0.0343(16) Uani 1 1 d . . .
O10 O 0.82830(18) 0.2226(8) 0.4969(4) 0.0315(15) Uani 1 1 d . . .
O11A O 1.0331(3) 0.2136(18) 0.4943(8) 0.040(3) Uani 0.5297(19) 1 d P . .
O12A O 1.0430(4) 0.151(2) 0.3275(8) 0.051(4) Uani 0.5297(19) 1 d P . .
O11B O 1.0220(4) 0.929(2) 0.4741(10) 0.043(4) Uani 0.4703(19) 1 d P . .
O12B O 1.0367(4) 0.952(2) 0.3112(10) 0.050(5) Uani 0.4703(19) 1 d P . .
O13 O 0.9086(3) 0.3736(12) 0.3792(5) 0.065(3) Uani 1 1 d . . .
O14 O 0.75586(18) 0.2938(9) 0.4198(4) 0.0351(16) Uani 1 1 d . . .
O15 O 0.78528(18) 0.3429(9) 0.5695(4) 0.0354(17) Uani 1 1 d . . .
O16 O 0.8648(3) 0.5249(9) 0.4764(5) 0.051(2) Uani 1 1 d . . .
H16A H 0.8884 0.4879 0.5055 0.061 Uiso 1 1 d R . .
H16B H 0.8666 0.6243 0.4982 0.061 Uiso 1 1 d R . .
O17 O 1.0709(4) 0.4352(17) 0.4358(9) 0.064(4) Uani 1 1 d . . .
O18 O 1.0683(4) 0.7004(18) 0.4321(9) 0.074(4) Uani 1 1 d . . .
O19 O 1.0038(4) 0.4195(18) 0.3565(10) 0.075(4) Uani 1 1 d . . .
O20 O 1.0018(4) 0.6794(16) 0.3477(9) 0.069(4) Uani 1 1 d . . .
O21 O 1.0393(6) -0.109(3) 0.4307(16) 0.068(6) Uani 0.5297(19) 1 d PU . .
O22 O 1.0252(11) 1.238(6) 0.384(2) 0.084(12) Uani 0.4703(19) 1 d PU . .
O23 O 0.9718(6) 0.392(3) 0.4721(14) 0.087(7) Uani 0.50 1 d PU . .
H23A H 0.9769 0.2930 0.4791 0.104 Uiso 0.50 1 d PR . .
H23B H 0.9768 0.4240 0.4286 0.104 Uiso 0.50 1 d PR . .
O24 O 0.9352(8) 0.491(3) 0.2618(18) 0.043(7) Uani 0.50 1 d PU . .
N1 N 0.8062(2) 0.1640(15) 0.2115(5) 0.049(3) Uani 1 1 d . . .
N2 N 0.8597(2) 0.1027(10) 0.1572(5) 0.0287(18) Uani 1 1 d . . .
N3 N 0.8945(3) -0.1247(11) 0.2842(6) 0.056(3) Uani 1 1 d . . .
N4 N 0.8409(3) -0.0656(11) 0.3369(5) 0.046(3) Uani 1 1 d . . .
C1 C 0.7995(3) 0.175(2) 0.1286(6) 0.053(4) Uani 1 1 d . . .
H1A H 0.8034 0.2839 0.1171 0.064 Uiso 1 1 calc R . .
H1B H 0.7760 0.1484 0.0960 0.064 Uiso 1 1 calc R . .
C2 C 0.8230(3) 0.0624(17) 0.1124(6) 0.045(3) Uani 1 1 d . . .
H2A H 0.8191 -0.0455 0.1246 0.054 Uiso 1 1 calc R . .
H2B H 0.8173 0.0662 0.0583 0.054 Uiso 1 1 calc R . .
C3 C 0.8812(3) -0.0314(12) 0.1529(6) 0.035(2) Uani 1 1 d . . .
H3A H 0.9043 0.0062 0.1686 0.042 Uiso 1 1 calc R . .
H3B H 0.8725 -0.0676 0.1004 0.042 Uiso 1 1 calc R . .
C4 C 0.8815(4) -0.1680(14) 0.2027(7) 0.052(3) Uani 1 1 d . . .
H4A H 0.8586 -0.2090 0.1847 0.062 Uiso 1 1 calc R . .
H4B H 0.8956 -0.2525 0.1977 0.062 Uiso 1 1 calc R . .
C5 C 0.8822(5) -0.2491(17) 0.3230(9) 0.070(4) Uani 1 1 d . . .
H5A H 0.8844 -0.3539 0.3047 0.084 Uiso 1 1 calc R . .
H5B H 0.8966 -0.2461 0.3777 0.084 Uiso 1 1 calc R . .
C6 C 0.8470(5) -0.2239(18) 0.3088(9) 0.068(4) Uani 1 1 d . . .
H6A H 0.8403 -0.3081 0.3335 0.082 Uiso 1 1 calc R . .
H6B H 0.8326 -0.2314 0.2542 0.082 Uiso 1 1 calc R . .
C7 C 0.8033(3) -0.0310(19) 0.3047(8) 0.058(3) Uani 1 1 d . . .
H7A H 0.7914 -0.1254 0.3087 0.070 Uiso 1 1 calc R . .
H7B H 0.7994 0.0532 0.3342 0.070 Uiso 1 1 calc R . .
C8 C 0.7895(3) 0.019(2) 0.2227(7) 0.059(3) Uani 1 1 d . . .
H8A H 0.7927 -0.0679 0.1934 0.071 Uiso 1 1 calc R . .
H8B H 0.7653 0.0380 0.2030 0.071 Uiso 1 1 calc R . .
C9 C 0.7935(3) 0.3109(18) 0.2342(6) 0.050(3) Uani 1 1 d . . .
H9A H 0.7693 0.3007 0.2190 0.061 Uiso 1 1 calc R . .
H9B H 0.7969 0.4022 0.2078 0.061 Uiso 1 1 calc R . .
C10 C 0.8119(3) 0.3381(15) 0.3198(6) 0.037(3) Uani 1 1 d . . .
C11 C 0.8680(3) 0.2456(12) 0.1263(5) 0.031(2) Uani 1 1 d . . .
H11A H 0.8564 0.2424 0.0710 0.038 Uiso 1 1 calc R . .
H11B H 0.8923 0.2480 0.1414 0.038 Uiso 1 1 calc R . .
C12 C 0.8578(2) 0.3953(13) 0.1546(6) 0.032(2) Uani 1 1 d . . .
C13 C 0.9325(4) -0.1177(17) 0.3217(8) 0.061(4) Uani 1 1 d . . .
H13A H 0.9411 -0.1955 0.2977 0.073 Uiso 1 1 calc R . .
H13B H 0.9407 -0.1473 0.3750 0.073 Uiso 1 1 calc R . .
C14 C 0.9467(3) 0.0443(17) 0.3174(7) 0.051(3) Uani 1 1 d . . .
C15 C 0.8560(4) -0.0706(14) 0.4226(7) 0.049(3) Uani 1 1 d . . .
H15A H 0.8436 0.0025 0.4399 0.059 Uiso 1 1 calc R . .
H15B H 0.8533 -0.1769 0.4386 0.059 Uiso 1 1 calc R . .
C16 C 0.8922(3) -0.0281(16) 0.4590(7) 0.048(3) Uani 1 1 d . . .
C17 C 0.7414(3) 0.2348(12) 0.4567(5) 0.028(2) Uani 1 1 d . . .
C18 C 1.0552(5) 0.565(2) 0.4150(12) 0.056(5) Uani 1 1 d . . .
C19 C 1.0163(5) 0.557(3) 0.3681(12) 0.054(5) 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
O9 U1 O10 177.5(3) . . ?
O9 U1 O4 90.5(3) . 6_566 ?
O10 U1 O4 91.3(3) . 6_566 ?
O9 U1 O2 87.8(3) . . ?
O10 U1 O2 91.3(3) . . ?
O4 U1 O2 151.9(3) 6_566 . ?
O9 U1 O14 91.7(3) . . ?
O10 U1 O14 85.8(3) . . ?
O4 U1 O14 136.4(2) 6_566 . ?
O2 U1 O14 71.7(2) . . ?
O9 U1 O15 91.4(3) . . ?
O10 U1 O15 87.7(3) . . ?
O4 U1 O15 71.1(2) 6_566 . ?
O2 U1 O15 137.0(2) . . ?
O14 U1 O15 65.3(2) . . ?
O9 U1 O16 91.9(3) . . ?
O10 U1 O16 90.2(3) . . ?
O4 U1 O16 75.8(3) 6_566 . ?
O2 U1 O16 76.2(3) . . ?
O14 U1 O16 147.5(2) . . ?
O15 U1 O16 146.8(2) . . ?
O12A U2A O11A 176.0(7) . . ?
O12A U2A O8 85.0(6) . 5_756 ?
O11A U2A O8 92.8(5) . 5_756 ?
O12A U2A O21 90.7(9) . . ?
O11A U2A O21 91.3(8) . . ?
O8 U2A O21 64.0(6) 5_756 . ?
O12A U2A O19 91.4(7) . . ?
O11A U2A O19 88.5(6) . . ?
O8 U2A O19 145.8(5) 5_756 . ?
O21 U2A O19 150.1(7) . . ?
O12A U2A O6 89.9(6) . . ?
O11A U2A O6 94.1(5) . . ?
O8 U2A O6 133.0(5) 5_756 . ?
O21 U2A O6 69.4(6) . . ?
O19 U2A O6 80.8(5) . . ?
O12A U2A O17 89.1(7) . . ?
O11A U2A O17 87.3(6) . . ?
O8 U2A O17 81.7(5) 5_756 . ?
O21 U2A O17 145.6(6) . . ?
O19 U2A O17 64.2(5) . . ?
O6 U2A O17 145.0(4) . . ?
O12B U2B O6 96.4(6) . 1_565 ?
O11B U2B O6 82.2(6) . 1_565 ?
O12B U2B O20 89.7(8) . . ?
O11B U2B O20 90.9(7) . . ?
O6 U2B O20 89.2(5) 1_565 . ?
O12B U2B O18 88.4(7) . . ?
O11B U2B O18 93.1(7) . . ?
O6 U2B O18 153.1(5) 1_565 . ?
O20 U2B O18 64.3(5) . . ?
O12B U2B O22 85.4(12) . . ?
O11B U2B O22 93.4(11) . . ?
O6 U2B O22 59.9(10) 1_565 . ?
O20 U2B O22 147.8(10) . . ?
O18 U2B O22 147.0(10) . . ?
O12B U2B O8 89.2(6) . 5_766 ?
O11B U2B O8 91.2(6) . 5_766 ?
O6 U2B O8 128.6(5) 1_565 5_766 ?
O20 U2B O8 142.1(4) . 5_766 ?
O18 U2B O8 77.7(4) . 5_766 ?
O22 U2B O8 69.8(10) . 5_766 ?
O7 Gd O1 83.6(2) . . ?
O7 Gd O5 84.0(2) . . ?
O1 Gd O5 143.0(3) . . ?
O7 Gd O3 145.1(3) . . ?
O1 Gd O3 83.7(2) . . ?
O5 Gd O3 86.9(2) . . ?
O7 Gd O13 72.5(3) . . ?
O1 Gd O13 72.6(3) . . ?
O5 Gd O13 70.4(3) . . ?
O3 Gd O13 72.7(3) . . ?
O7 Gd N2 141.3(3) . . ?
O1 Gd N2 131.8(2) . . ?
O5 Gd N2 74.8(2) . . ?
O3 Gd N2 66.5(2) . . ?
O13 Gd N2 126.9(3) . . ?
O7 Gd N3 72.7(3) . . ?
O1 Gd N3 140.7(3) . . ?
O5 Gd N3 65.9(3) . . ?
O3 Gd N3 132.6(3) . . ?
O13 Gd N3 126.0(4) . . ?
N2 Gd N3 69.1(3) . . ?
O7 Gd N4 65.8(3) . . ?
O1 Gd N4 72.8(3) . . ?
O5 Gd N4 131.4(3) . . ?
O3 Gd N4 139.0(3) . . ?
O13 Gd N4 127.8(3) . . ?
N2 Gd N4 105.3(3) . . ?
N3 Gd N4 69.0(3) . . ?
O7 Gd N1 129.7(3) . . ?
O1 Gd N1 65.6(3) . . ?
O5 Gd N1 143.4(2) . . ?
O3 Gd N1 72.4(3) . . ?
O13 Gd N1 127.4(4) . . ?
N2 Gd N1 69.5(3) . . ?
N3 Gd N1 106.6(4) . . ?
N4 Gd N1 67.5(4) . . ?
C10 O1 Gd 125.6(6) . . ?
C10 O2 U1 125.9(6) . . ?
C12 O3 Gd 122.1(6) . . ?
C12 O4 U1 138.7(7) . 6_565 ?
C14 O5 Gd 123.4(8) . . ?
C14 O5 O24 132.2(10) . . ?
Gd O5 O24 103.2(7) . . ?
C14 O6 U2B 148.9(11) . 1_545 ?
C14 O6 U2A 157.9(11) . . ?
C16 O7 Gd 125.6(7) . . ?
C16 O8 U2A 133.2(9) . 5_756 ?
C16 O8 U2B 119.5(10) . 5_766 ?
Gd O13 O23 133.0(7) . . ?
Gd O13 O24 95.7(6) . . ?
O23 O13 O24 82.3(8) . . ?
C17 O14 U1 120.8(6) . . ?
C17 O15 U1 119.7(6) 7_656 . ?
U1 O16 H16A 127.0 . . ?
U1 O16 H16B 100.4 . . ?
H16A O16 H16B 99.5 . . ?
C18 O17 U2A 118.7(13) . . ?
C18 O18 U2B 118.4(13) . . ?
C19 O19 U2A 124.0(14) . . ?
C19 O20 U2B 122.8(14) . . ?
O13 O23 H23A 100.1 . . ?
O13 O23 H23B 89.2 . . ?
H23A O23 H23B 104.8 . . ?
C8 N1 C9 111.5(10) . . ?
C8 N1 C1 109.4(10) . . ?
C9 N1 C1 109.9(10) . . ?
C8 N1 Gd 111.4(8) . . ?
C9 N1 Gd 105.6(7) . . ?
C1 N1 Gd 109.0(6) . . ?
C11 N2 C2 110.2(9) . . ?
C11 N2 C3 108.7(7) . . ?
C2 N2 C3 109.8(8) . . ?
C11 N2 Gd 107.8(6) . . ?
C2 N2 Gd 110.4(6) . . ?
C3 N2 Gd 109.9(6) . . ?
C4 N3 C13 110.9(10) . . ?
C4 N3 C5 108.2(11) . . ?
C13 N3 C5 110.2(11) . . ?
C4 N3 Gd 110.7(8) . . ?
C13 N3 Gd 106.4(8) . . ?
C5 N3 Gd 110.5(8) . . ?
C15 N4 C6 108.6(10) . . ?
C15 N4 C7 109.5(9) . . ?
C6 N4 C7 110.7(11) . . ?
C15 N4 Gd 107.5(7) . . ?
C6 N4 Gd 109.0(7) . . ?
C7 N4 Gd 111.4(8) . . ?
N1 C1 C2 110.4(11) . . ?
N1 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N1 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N2 C2 C1 112.7(9) . . ?
N2 C2 H2A 109.1 . . ?
C1 C2 H2A 109.1 . . ?
N2 C2 H2B 109.1 . . ?
C1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
N2 C3 C4 111.7(9) . . ?
N2 C3 H3A 109.3 . . ?
C4 C3 H3A 109.3 . . ?
N2 C3 H3B 109.3 . . ?
C4 C3 H3B 109.3 . . ?
H3A C3 H3B 107.9 . . ?
N3 C4 C3 113.4(10) . . ?
N3 C4 H4A 108.9 . . ?
C3 C4 H4A 108.9 . . ?
N3 C4 H4B 108.9 . . ?
C3 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
C6 C5 N3 112.4(13) . . ?
C6 C5 H5A 109.1 . . ?
N3 C5 H5A 109.1 . . ?
C6 C5 H5B 109.1 . . ?
N3 C5 H5B 109.1 . . ?
H5A C5 H5B 107.8 . . ?
C5 C6 N4 113.6(12) . . ?
C5 C6 H6A 108.8 . . ?
N4 C6 H6A 108.8 . . ?
C5 C6 H6B 108.8 . . ?
N4 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
C8 C7 N4 110.5(10) . . ?
C8 C7 H7A 109.5 . . ?
N4 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
N1 C8 C7 113.1(10) . . ?
N1 C8 H8A 109.0 . . ?
C7 C8 H8A 109.0 . . ?
N1 C8 H8B 109.0 . . ?
C7 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
N1 C9 C10 111.2(10) . . ?
N1 C9 H9A 109.4 . . ?
C10 C9 H9A 109.4 . . ?
N1 C9 H9B 109.4 . . ?
C10 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
O2 C10 O1 123.9(9) . . ?
O2 C10 C9 117.8(9) . . ?
O1 C10 C9 118.3(9) . . ?
N2 C11 C12 111.4(8) . . ?
N2 C11 H11A 109.3 . . ?
C12 C11 H11A 109.3 . . ?
N2 C11 H11B 109.3 . . ?
C12 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
O3 C12 O4 122.9(10) . . ?
O3 C12 C11 118.6(9) . . ?
O4 C12 C11 118.3(9) . . ?
N3 C13 C14 113.8(10) . . ?
N3 C13 H13A 108.8 . . ?
C14 C13 H13A 108.8 . . ?
N3 C13 H13B 108.8 . . ?
C14 C13 H13B 108.8 . . ?
H13A C13 H13B 107.7 . . ?
O5 C14 O6 124.5(14) . . ?
O5 C14 C13 117.8(11) . . ?
O6 C14 C13 117.5(12) . . ?
C16 C15 N4 112.6(9) . . ?
C16 C15 H15A 109.1 . . ?
N4 C15 H15A 109.1 . . ?
C16 C15 H15B 109.1 . . ?
N4 C15 H15B 109.1 . . ?
H15A C15 H15B 107.8 . . ?
O8 C16 O7 122.6(13) . . ?
O8 C16 C15 117.8(12) . . ?
O7 C16 C15 119.6(10) . . ?
O15 C17 O14 126.6(9) 7_656 . ?
O15 C17 C17 117.3(10) 7_656 7_656 ?
O14 C17 C17 116.1(11) . 7_656 ?
O18 C18 O17 125(2) . . ?
O18 C18 C19 117.1(18) . . ?
O17 C18 C19 117.4(17) . . ?
O20 C19 O19 127.9(19) . . ?
O20 C19 C18 116.7(19) . . ?
O19 C19 C18 115.4(18) . . ?
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
U1 O9 1.767(7) . ?
U1 O10 1.770(7) . ?
U1 O4 2.333(7) 6_566 ?
U1 O2 2.402(6) . ?
U1 O14 2.443(7) . ?
U1 O15 2.471(7) . ?
U1 O16 2.558(9) . ?
U2A O12A 1.744(14) . ?
U2A O11A 1.756(14) . ?
U2A O8 2.307(12) 5_756 ?
U2A O21 2.44(2) . ?
U2A O19 2.439(15) . ?
U2A O6 2.526(13) . ?
U2A O17 2.546(15) . ?
U2B O12B 1.737(17) . ?
U2B O11B 1.770(16) . ?
U2B O6 2.252(11) 1_565 ?
U2B O20 2.459(14) . ?
U2B O18 2.508(15) . ?
U2B O22 2.52(5) . ?
U2B O8 2.664(14) 5_766 ?
Gd O7 2.350(7) . ?
Gd O1 2.355(6) . ?
Gd O5 2.362(7) . ?
Gd O3 2.422(7) . ?
Gd O13 2.437(8) . ?
Gd N2 2.601(8) . ?
Gd N3 2.620(10) . ?
Gd N4 2.650(9) . ?
Gd N1 2.671(9) . ?
O1 C10 1.255(12) . ?
O2 C10 1.249(12) . ?
O3 C12 1.247(12) . ?
O4 C12 1.275(12) . ?
O4 U1 2.333(7) 6_565 ?
O5 C14 1.243(14) . ?
O5 O24 2.93(3) . ?
O6 C14 1.247(17) . ?
O6 U2B 2.252(11) 1_545 ?
O7 C16 1.266(14) . ?
O8 C16 1.247(16) . ?
O8 U2A 2.307(12) 5_756 ?
O8 U2B 2.664(14) 5_766 ?
O13 O23 2.56(3) . ?
O13 O24 3.14(3) . ?
O14 C17 1.248(11) . ?
O15 C17 1.236(12) 7_656 ?
O16 H16A 0.9829 . ?
O16 H16B 0.9243 . ?
O17 C18 1.25(2) . ?
O18 C18 1.25(2) . ?
O19 C19 1.25(2) . ?
O19 O24 2.81(4) . ?
O20 C19 1.18(2) . ?
O20 O24 3.08(3) . ?
O23 H23A 0.8591 . ?
O23 H23B 0.9984 . ?
N1 C8 1.484(18) . ?
N1 C9 1.496(17) . ?
N1 C1 1.513(13) . ?
N2 C11 1.458(13) . ?
N2 C2 1.491(13) . ?
N2 C3 1.492(13) . ?
N3 C4 1.478(16) . ?
N3 C13 1.49(2) . ?
N3 C5 1.519(17) . ?
N4 C15 1.502(15) . ?
N4 C6 1.505(17) . ?
N4 C7 1.509(18) . ?
C1 C2 1.527(18) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.497(15) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.45(2) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.498(19) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.515(14) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C11 C12 1.516(15) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C13 C14 1.51(2) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C15 C16 1.465(19) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C17 O15 1.236(12) 7_656 ?
C17 C17 1.536(18) 7_656 ?
C18 C19 1.54(3) . ?
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
O16 H16A O17 0.98 1.76 2.591(17) 139.7 5_766
O23 H23A O11B 0.86 2.07 2.86(3) 154.4 5_766
O23 H23B O19 1.00 2.19 3.14(3) 156.4 .
