# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2014

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#                                CCDC 
# 
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#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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#  fide research purposes only. It may contain copyright material
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data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H30 La N5 O13, 2(C6 H2 N3 O7), H2 O, O'
_chemical_formula_sum            'C28 H38 La N11 O29'
_chemical_formula_weight         1131.60

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'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.8370(4)
_cell_length_b                   17.2880(5)
_cell_length_c                   16.7480(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.6600(10)
_cell_angle_gamma                90.00
_cell_volume                     4287.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9352
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      31.12

_exptl_crystal_description       Needle
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2288
_exptl_absorpt_coefficient_mu    1.111
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6418
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_process_details   
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            55503
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.69
_diffrn_reflns_theta_max         31.65
_reflns_number_total             14413
_reflns_number_gt                10755
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Sir-92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 This complex is highly
 disordered due to vibrations in oxygen atoms of nitro groups. In the 
presence of heavy metal atoms, protons of highly disordered lattice water 
could not be located from difference Fourier map.The disorder has been applied
on oxygen atoms of nitro groups and on lattice water molecules. 
  
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0411P)²+7.2930P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14413
_refine_ls_number_parameters     655
_refine_ls_number_restraints     35
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0443
_refine_ls_wR_factor_ref         0.1171
_refine_ls_wR_factor_gt          0.1047
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.001

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
C1 C 0.6687(3) -0.0245(3) 0.3786(3) 0.0590(11) Uani 1 1 d . . .
H1A H 0.6445 -0.0714 0.3536 0.071 Uiso 1 1 calc R . .
H1B H 0.6311 -0.0103 0.4216 0.071 Uiso 1 1 calc R . .
C2 C 0.7642(3) -0.0377(3) 0.4110(2) 0.0553(10) Uani 1 1 d . . .
H2A H 0.7831 0.0055 0.4451 0.066 Uiso 1 1 calc R . .
H2B H 0.7664 -0.0841 0.4436 0.066 Uiso 1 1 calc R . .
C3 C 0.9533(3) 0.0344(3) 0.4056(2) 0.0535(10) Uani 1 1 d . . .
H3A H 0.9178 0.0553 0.4471 0.064 Uiso 1 1 calc R . .
H3B H 1.0161 0.0329 0.4257 0.064 Uiso 1 1 calc R . .
C4 C 0.9217(2) -0.0450(3) 0.3841(2) 0.0515(9) Uani 1 1 d . . .
H4A H 0.9621 -0.0676 0.3472 0.062 Uiso 1 1 calc R . .
H4B H 0.9242 -0.0767 0.4319 0.062 Uiso 1 1 calc R . .
C5 C 0.8122(3) -0.1207(2) 0.3052(2) 0.0503(9) Uani 1 1 d . . .
H5A H 0.7477 -0.1286 0.2957 0.060 Uiso 1 1 calc R . .
H5B H 0.8358 -0.1623 0.3393 0.060 Uiso 1 1 calc R . .
C6 C 0.8561(3) -0.1238(2) 0.2265(2) 0.0510(9) Uani 1 1 d . . .
H6A H 0.9203 -0.1143 0.2360 0.061 Uiso 1 1 calc R . .
H6B H 0.8487 -0.1754 0.2043 0.061 Uiso 1 1 calc R . .
C7 C 0.6744(3) -0.0338(3) 0.0921(2) 0.0545(10) Uani 1 1 d . . .
H7A H 0.7038 -0.0148 0.0459 0.065 Uiso 1 1 calc R . .
H7B H 0.6156 -0.0539 0.0741 0.065 Uiso 1 1 calc R . .
C8 C 0.7301(3) -0.0961(2) 0.1326(2) 0.0489(9) Uani 1 1 d . . .
H8A H 0.6968 -0.1185 0.1749 0.059 Uiso 1 1 calc R . .
H8B H 0.7406 -0.1366 0.0943 0.059 Uiso 1 1 calc R . .
C9 C 0.9685(2) -0.0220(2) 0.1276(2) 0.0482(9) Uani 1 1 d . . .
H9A H 1.0044 -0.0574 0.1615 0.058 Uiso 1 1 calc R . .
H9B H 1.0020 -0.0096 0.0814 0.058 Uiso 1 1 calc R . .
C10 C 0.8796(3) -0.0587(2) 0.1013(2) 0.0465(8) Uani 1 1 d . . .
H10A H 0.8500 -0.0275 0.0592 0.056 Uiso 1 1 calc R . .
H10B H 0.8908 -0.1094 0.0791 0.056 Uiso 1 1 calc R . .
C11 C 0.9272(2) 0.22516(18) 0.1594(2) 0.0370(7) Uani 1 1 d . . .
C12 C 0.9282(2) 0.20298(19) 0.0775(2) 0.0374(7) Uani 1 1 d . . .
C13 C 0.9925(2) 0.2287(2) 0.0271(2) 0.0398(7) Uani 1 1 d . . .
H15 H 0.9921 0.2112 -0.0254 0.048 Uiso 1 1 calc R . .
C14 C 1.0570(2) 0.2807(2) 0.0561(2) 0.0424(7) Uani 1 1 d . . .
C15 C 1.0580(2) 0.3085(2) 0.1336(2) 0.0451(8) Uani 1 1 d . . .
H13 H 1.1012 0.3443 0.1522 0.054 Uiso 1 1 calc R . .
C16 C 0.9944(2) 0.28224(19) 0.1817(2) 0.0394(7) Uani 1 1 d . A .
C17 C 0.1699(2) 0.15050(19) 0.26104(19) 0.0354(6) Uani 1 1 d . . .
C18 C 0.2247(2) 0.15385(19) 0.19233(19) 0.0360(6) Uani 1 1 d . B .
C19 C 0.3086(2) 0.1867(2) 0.1925(2) 0.0420(7) Uani 1 1 d . . .
H19 H 0.3405 0.1864 0.1465 0.050 Uiso 1 1 calc R . .
C20 C 0.3453(2) 0.2206(2) 0.2621(2) 0.0430(8) Uani 1 1 d . . .
C21 C 0.2986(2) 0.2221(2) 0.3303(2) 0.0430(7) Uani 1 1 d . . .
H21 H 0.3235 0.2459 0.3763 0.052 Uiso 1 1 calc R . .
C22 C 0.2152(2) 0.1882(2) 0.3301(2) 0.0404(7) Uani 1 1 d . C .
C23 C 0.4304(2) 0.0269(2) 0.2626(3) 0.0539(10) Uani 1 1 d . . .
C24 C 0.3907(2) 0.0352(2) 0.3391(3) 0.0506(9) Uani 1 1 d . D .
C25 C 0.3088(2) 0.0063(2) 0.3564(3) 0.0529(9) Uani 1 1 d . . .
H25 H 0.2876 0.0131 0.4070 0.063 Uiso 1 1 calc R . .
C26 C 0.2582(2) -0.0328(2) 0.2987(3) 0.0549(10) Uani 1 1 d . . .
C27 C 0.2881(3) -0.0432(3) 0.2235(3) 0.0609(11) Uani 1 1 d . . .
H27 H 0.2530 -0.0702 0.1849 0.073 Uiso 1 1 calc R . .
C28 C 0.3705(3) -0.0133(3) 0.2059(3) 0.0557(10) Uani 1 1 d . . .
N1 N 0.82836(18) -0.04609(18) 0.34680(16) 0.0384(6) Uani 1 1 d . . .
N2 N 0.81831(18) -0.06708(16) 0.16721(16) 0.0368(6) Uani 1 1 d . . .
N3 N 0.8622(2) 0.14910(18) 0.04281(19) 0.0447(7) Uani 1 1 d . . .
N4 N 1.1262(2) 0.3056(2) 0.0050(2) 0.0527(8) Uani 1 1 d . . .
N5 N 0.9974(2) 0.3113(2) 0.2630(2) 0.0539(8) Uani 1 1 d D . .
N6 N 0.1915(2) 0.1183(2) 0.11799(18) 0.0504(8) Uani 1 1 d D . .
N7 N 0.4368(2) 0.2508(2) 0.2645(2) 0.0528(8) Uani 1 1 d . . .
N8 N 0.1730(2) 0.1905(2) 0.40615(19) 0.0566(9) Uani 1 1 d D . .
N9 N 0.4372(3) 0.0779(2) 0.4044(3) 0.0690(11) Uani 1 1 d D . .
N10 N 0.1710(3) -0.0645(3) 0.3182(4) 0.0791(14) Uani 1 1 d . . .
N11 N 0.3972(4) -0.0235(4) 0.1238(3) 0.0900(15) Uani 1 1 d . . .
O1 O 0.66926(16) 0.03576(19) 0.32169(17) 0.0587(8) Uani 1 1 d D . .
H1 H 0.6169(14) 0.0390(14) 0.3070(15) 0.070 Uiso 1 1 d D . .
O2 O 0.94397(16) 0.08223(18) 0.33607(15) 0.0501(6) Uani 1 1 d D . .
H2 H 0.987(2) 0.108(2) 0.327(3) 0.060 Uiso 1 1 d D . .
O3 O 0.66476(18) 0.02739(19) 0.1481(2) 0.0598(7) Uani 1 1 d D . .
H3 H 0.6124(17) 0.034(3) 0.161(3) 0.072 Uiso 1 1 d D . .
O4 O 0.95053(15) 0.04665(15) 0.17073(15) 0.0406(5) Uani 1 1 d D . .
H4 H 0.9983(16) 0.0602(12) 0.192(2) 0.049 Uiso 1 1 d D . .
O5 O 0.87562(17) 0.19946(14) 0.21031(15) 0.0475(6) Uani 1 1 d . . .
O6 O 0.80132(17) 0.12427(18) 0.08356(16) 0.0535(7) Uani 1 1 d . . .
O7 O 0.8670(2) 0.1290(2) -0.02638(19) 0.0754(10) Uani 1 1 d . . .
O8 O 1.1312(2) 0.27440(19) -0.05985(18) 0.0634(8) Uani 1 1 d . . .
O9 O 1.1771(2) 0.3573(2) 0.0286(2) 0.0846(11) Uani 1 1 d . . .
O10 O 0.9599(5) 0.3759(5) 0.2720(4) 0.0781(6) Uani 0.529(6) 1 d PD A 1
O10' O 0.9338(5) 0.3253(5) 0.2954(4) 0.0781(6) Uani 0.471(6) 1 d PD A 2
O11 O 1.0754(4) 0.3102(4) 0.2998(3) 0.0781(6) Uani 0.611(5) 1 d PD A 1
O11' O 1.0116(6) 0.2734(6) 0.3207(5) 0.0781(6) Uani 0.389(5) 1 d PD A 2
O12 O 0.09362(16) 0.11998(17) 0.25981(15) 0.0488(6) Uani 1 1 d . . .
O13 O 0.1143(6) 0.0995(8) 0.1039(5) 0.0781(6) Uani 0.522(14) 1 d PD B 1
O13' O 0.1417(8) 0.0657(8) 0.1173(5) 0.0781(6) Uani 0.478(14) 1 d PD B 2
O14 O 0.2181(4) 0.1522(4) 0.0563(3) 0.0781(6) Uani 0.588(6) 1 d PD B 1
O14' O 0.2484(6) 0.0912(6) 0.0722(5) 0.0781(6) Uani 0.412(6) 1 d PD B 2
O15 O 0.4762(2) 0.2501(2) 0.2028(2) 0.0789(11) Uani 1 1 d . . .
O16 O 0.4694(2) 0.2758(3) 0.3276(2) 0.0884(12) Uani 1 1 d . . .
O17 O 0.1978(12) 0.2442(15) 0.4509(11) 0.0781(6) Uani 0.42(4) 1 d PD C 1
O17' O 0.2113(8) 0.2205(12) 0.4655(7) 0.0781(6) Uani 0.58(4) 1 d PD C 2
O18 O 0.0953(9) 0.1685(11) 0.4140(6) 0.0781(6) Uani 0.43(2) 1 d PD C 1
O18' O 0.1201(8) 0.1397(8) 0.4178(4) 0.0781(6) Uani 0.57(2) 1 d PD C 2
O19 O 0.5062(2) 0.0524(2) 0.2475(2) 0.0796(11) Uani 1 1 d . . .
O20 O 0.3914(3) 0.1072(3) 0.4584(3) 0.0781(6) Uani 0.782(6) 1 d PD D 1
O20' O 0.4540(11) 0.0515(10) 0.4666(8) 0.0781(6) Uani 0.218(6) 1 d PD D 2
O21 O 0.5163(5) 0.0779(6) 0.4196(5) 0.0781(6) Uani 0.492(8) 1 d PD D 1
O21' O 0.5093(5) 0.1100(6) 0.3815(5) 0.0781(6) Uani 0.508(8) 1 d PD D 2
O22 O 0.1485(3) -0.0561(3) 0.3872(3) 0.1102(16) Uani 1 1 d . . .
O23 O 0.1260(3) -0.0960(3) 0.2643(4) 0.1148(17) Uani 1 1 d . . .
O24 O 0.3612(5) -0.0754(4) 0.0836(3) 0.156(3) Uani 1 1 d . . .
O25 O 0.4527(4) 0.0155(5) 0.0972(3) 0.167(3) Uani 1 1 d . . .
O1W O 0.6665(2) 0.1738(2) 0.2156(2) 0.0673(9) Uani 1 1 d D . .
H11W H 0.653(3) 0.184(3) 0.1693(12) 0.081 Uiso 1 1 d D . .
H12W H 0.637(3) 0.181(3) 0.2535(18) 0.081 Uiso 1 1 d D . .
O2W O 0.7876(2) 0.1617(2) 0.3652(2) 0.0762(11) Uani 1 1 d D . .
H21W H 0.830(2) 0.187(3) 0.396(3) 0.091 Uiso 1 1 d D . .
H22W H 0.7366(14) 0.171(3) 0.377(3) 0.091 Uiso 1 1 d D . .
O3W O 0.5838(5) 0.1803(4) 0.0589(4) 0.167(3) Uani 1 1 d D . .
H31W H 0.536(4) 0.197(4) 0.030(6) 0.201 Uiso 1 1 d D . .
H32W H 0.574(6) 0.134(2) 0.077(4) 0.201 Uiso 1 1 d D . .
O4W O 0.4056(9) 0.2762(9) 0.0047(9) 0.169(4) Uani 0.618(13) 1 d P E 1
O4W' O 0.4055(16) 0.2533(16) -0.0521(15) 0.169(4) Uani 0.382(13) 1 d P E 2
La1 La 0.800356(11) 0.078122(10) 0.240044(10) 0.03007(5) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
C1 O1 1.412(5) . ?
C1 C2 1.502(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N1 1.487(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 O2 1.427(5) . ?
C3 C4 1.488(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N1 1.482(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N1 1.478(5) . ?
C5 C6 1.508(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N2 1.480(5) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 O3 1.427(5) . ?
C7 C8 1.493(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N2 1.484(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 O4 1.423(4) . ?
C9 C10 1.505(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.482(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 O5 1.262(4) . ?
C11 C12 1.426(5) . ?
C11 C16 1.436(5) . ?
C12 C13 1.387(4) . ?
C12 N3 1.446(4) . ?
C13 C14 1.379(5) . ?
C13 H15 0.9300 . ?
C14 C15 1.382(5) . ?
C14 N4 1.444(4) . ?
C15 C16 1.357(5) . ?
C15 H13 0.9300 . ?
C16 N5 1.450(5) . ?
C17 O12 1.248(4) . ?
C17 C18 1.452(4) . ?
C17 C22 1.455(5) . ?
C18 C19 1.368(4) . ?
C18 N6 1.446(4) . ?
C19 C20 1.385(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.373(5) . ?
C20 N7 1.452(4) . ?
C21 C22 1.368(5) . ?
C21 H21 0.9300 . ?
C22 N8 1.456(5) . ?
C23 O19 1.249(4) . ?
C23 C28 1.438(6) . ?
C23 C24 1.452(6) . ?
C24 C25 1.361(5) . ?
C24 N9 1.457(6) . ?
C25 C26 1.364(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.373(6) . ?
C26 N10 1.460(5) . ?
C27 C28 1.377(6) . ?
C27 H27 0.9300 . ?
C28 N11 1.465(7) . ?
N1 La1 2.808(3) . ?
N2 La1 2.811(3) . ?
N3 O7 1.216(4) . ?
N3 O6 1.242(4) . ?
N4 O8 1.219(4) . ?
N4 O9 1.220(4) . ?
N5 O10' 1.144(7) . ?
N5 O11' 1.175(9) . ?
N5 O10 1.261(8) . ?
N5 O11 1.276(6) . ?
N6 O13' 1.172(9) . ?
N6 O13 1.200(8) . ?
N6 O14' 1.265(8) . ?
N6 O14 1.273(7) . ?
N7 O16 1.214(5) . ?
N7 O15 1.220(5) . ?
N8 O18' 1.201(8) . ?
N8 O18 1.227(10) . ?
N8 O17' 1.229(8) . ?
N8 O17 1.235(11) . ?
N9 O20' 1.149(14) . ?
N9 O21 1.186(8) . ?
N9 O20 1.271(6) . ?
N9 O21' 1.285(8) . ?
N10 O23 1.216(7) . ?
N10 O22 1.231(7) . ?
N11 O25 1.174(8) . ?
N11 O24 1.223(8) . ?
O1 La1 2.555(2) . ?
O1 H1 0.802(19) . ?
O2 La1 2.587(2) . ?
O2 H2 0.801(19) . ?
O3 La1 2.606(3) . ?
O3 H3 0.826(19) . ?
O4 La1 2.634(2) . ?
O4 H4 0.807(18) . ?
O5 La1 2.443(2) . ?
O6 La1 2.740(3) . ?
O10' O11' 1.502(13) . ?
O1W La1 2.597(3) . ?
O1W H11W 0.807(18) . ?
O1W H12W 0.80(4) . ?
O2W La1 2.563(3) . ?
O2W H21W 0.90(4) . ?
O2W H22W 0.810(19) . ?
O3W H31W 0.88(7) . ?
O3W H32W 0.87(2) . ?

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
O1 C1 C2 108.0(3) . . ?
O1 C1 H1A 110.1 . . ?
C2 C1 H1A 110.1 . . ?
O1 C1 H1B 110.1 . . ?
C2 C1 H1B 110.1 . . ?
H1A C1 H1B 108.4 . . ?
N1 C2 C1 112.7(3) . . ?
N1 C2 H2A 109.0 . . ?
C1 C2 H2A 109.0 . . ?
N1 C2 H2B 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
O2 C3 C4 109.0(3) . . ?
O2 C3 H3A 109.9 . . ?
C4 C3 H3A 109.9 . . ?
O2 C3 H3B 109.9 . . ?
C4 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?
N1 C4 C3 112.7(3) . . ?
N1 C4 H4A 109.1 . . ?
C3 C4 H4A 109.1 . . ?
N1 C4 H4B 109.1 . . ?
C3 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
N1 C5 C6 112.2(3) . . ?
N1 C5 H5A 109.2 . . ?
C6 C5 H5A 109.2 . . ?
N1 C5 H5B 109.2 . . ?
C6 C5 H5B 109.2 . . ?
H5A C5 H5B 107.9 . . ?
N2 C6 C5 113.4(3) . . ?
N2 C6 H6A 108.9 . . ?
C5 C6 H6A 108.9 . . ?
N2 C6 H6B 108.9 . . ?
C5 C6 H6B 108.9 . . ?
H6A C6 H6B 107.7 . . ?
O3 C7 C8 108.2(3) . . ?
O3 C7 H7A 110.1 . . ?
C8 C7 H7A 110.1 . . ?
O3 C7 H7B 110.1 . . ?
C8 C7 H7B 110.1 . . ?
H7A C7 H7B 108.4 . . ?
N2 C8 C7 112.5(3) . . ?
N2 C8 H8A 109.1 . . ?
C7 C8 H8A 109.1 . . ?
N2 C8 H8B 109.1 . . ?
C7 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
O4 C9 C10 108.2(3) . . ?
O4 C9 H9A 110.1 . . ?
C10 C9 H9A 110.1 . . ?
O4 C9 H9B 110.1 . . ?
C10 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
N2 C10 C9 113.0(3) . . ?
N2 C10 H10A 109.0 . . ?
C9 C10 H10A 109.0 . . ?
N2 C10 H10B 109.0 . . ?
C9 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
O5 C11 C12 126.8(3) . . ?
O5 C11 C16 120.6(3) . . ?
C12 C11 C16 112.6(3) . . ?
C13 C12 C11 123.3(3) . . ?
C13 C12 N3 115.9(3) . . ?
C11 C12 N3 120.8(3) . . ?
C14 C13 C12 118.9(3) . . ?
C14 C13 H15 120.5 . . ?
C12 C13 H15 120.5 . . ?
C13 C14 C15 121.6(3) . . ?
C13 C14 N4 119.2(3) . . ?
C15 C14 N4 119.2(3) . . ?
C16 C15 C14 118.3(3) . . ?
C16 C15 H13 120.8 . . ?
C14 C15 H13 120.8 . . ?
C15 C16 C11 125.0(3) . . ?
C15 C16 N5 117.5(3) . . ?
C11 C16 N5 117.4(3) . . ?
O12 C17 C18 123.8(3) . . ?
O12 C17 C22 125.1(3) . . ?
C18 C17 C22 111.0(3) . . ?
C19 C18 N6 116.0(3) . . ?
C19 C18 C17 124.8(3) . . ?
N6 C18 C17 119.2(3) . . ?
C18 C19 C20 119.1(3) . . ?
C18 C19 H19 120.5 . . ?
C20 C19 H19 120.5 . . ?
C21 C20 C19 121.0(3) . . ?
C21 C20 N7 119.4(3) . . ?
C19 C20 N7 119.5(3) . . ?
C22 C21 C20 119.7(3) . . ?
C22 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
C21 C22 C17 124.4(3) . . ?
C21 C22 N8 115.3(3) . . ?
C17 C22 N8 120.3(3) . . ?
O19 C23 C28 124.4(4) . . ?
O19 C23 C24 124.4(4) . . ?
C28 C23 C24 111.2(3) . . ?
C25 C24 C23 124.7(4) . . ?
C25 C24 N9 114.4(4) . . ?
C23 C24 N9 120.9(3) . . ?
C24 C25 C26 119.3(4) . . ?
C24 C25 H25 120.4 . . ?
C26 C25 H25 120.4 . . ?
C25 C26 C27 121.2(4) . . ?
C25 C26 N10 118.9(5) . . ?
C27 C26 N10 119.9(4) . . ?
C26 C27 C28 119.5(4) . . ?
C26 C27 H27 120.3 . . ?
C28 C27 H27 120.3 . . ?
C27 C28 C23 124.0(4) . . ?
C27 C28 N11 117.0(5) . . ?
C23 C28 N11 119.0(4) . . ?
C5 N1 C4 109.2(3) . . ?
C5 N1 C2 109.5(3) . . ?
C4 N1 C2 108.6(3) . . ?
C5 N1 La1 110.7(2) . . ?
C4 N1 La1 110.8(2) . . ?
C2 N1 La1 108.1(2) . . ?
C6 N2 C10 109.9(3) . . ?
C6 N2 C8 108.9(3) . . ?
C10 N2 C8 108.0(3) . . ?
C6 N2 La1 110.1(2) . . ?
C10 N2 La1 108.4(2) . . ?
C8 N2 La1 111.4(2) . . ?
O7 N3 O6 120.9(3) . . ?
O7 N3 C12 119.1(3) . . ?
O6 N3 C12 119.9(3) . . ?
O8 N4 O9 122.8(3) . . ?
O8 N4 C14 118.9(3) . . ?
O9 N4 C14 118.3(4) . . ?
O10' N5 O11' 80.7(7) . . ?
O10' N5 O10 51.1(5) . . ?
O11' N5 O10 116.9(6) . . ?
O10' N5 O11 121.6(5) . . ?
O11' N5 O11 59.0(5) . . ?
O10 N5 O11 110.4(5) . . ?
O10' N5 C16 122.8(5) . . ?
O11' N5 C16 125.0(5) . . ?
O10 N5 C16 115.5(4) . . ?
O11 N5 C16 114.9(4) . . ?
O13' N6 O14' 98.7(7) . . ?
O13 N6 O14' 116.5(6) . . ?
O13' N6 O14 125.3(6) . . ?
O13 N6 O14 107.8(6) . . ?
O14' N6 O14 54.8(5) . . ?
O13' N6 C18 121.2(5) . . ?
O13 N6 C18 123.5(4) . . ?
O14' N6 C18 118.4(5) . . ?
O14 N6 C18 113.4(4) . . ?
O16 N7 O15 123.6(3) . . ?
O16 N7 C20 118.2(3) . . ?
O15 N7 C20 118.1(3) . . ?
O18' N8 O17' 116.8(8) . . ?
O18 N8 O17' 115.7(6) . . ?
O18' N8 O17 128.6(9) . . ?
O18 N8 O17 114.5(9) . . ?
O18' N8 C22 116.4(5) . . ?
O18 N8 C22 123.0(5) . . ?
O17' N8 C22 121.1(5) . . ?
O17 N8 C22 115.0(8) . . ?
O20' N9 O21 69.6(9) . . ?
O20' N9 O20 66.9(9) . . ?
O21 N9 O20 114.5(5) . . ?
O20' N9 O21' 107.8(10) . . ?
O20 N9 O21' 122.2(5) . . ?
O20' N9 C24 123.1(9) . . ?
O21 N9 C24 125.2(5) . . ?
O20 N9 C24 119.1(4) . . ?
O21' N9 C24 111.0(5) . . ?
O23 N10 O22 125.4(5) . . ?
O23 N10 C26 117.0(5) . . ?
O22 N10 C26 117.6(5) . . ?
O25 N11 O24 120.3(7) . . ?
O25 N11 C28 121.7(6) . . ?
O24 N11 C28 118.0(6) . . ?
C1 O1 La1 127.6(2) . . ?
C1 O1 H1 102.2(13) . . ?
La1 O1 H1 124.8(15) . . ?
C3 O2 La1 121.6(2) . . ?
C3 O2 H2 117(3) . . ?
La1 O2 H2 121(3) . . ?
C7 O3 La1 122.1(2) . . ?
C7 O3 H3 114(4) . . ?
La1 O3 H3 120(4) . . ?
C9 O4 La1 125.94(19) . . ?
C9 O4 H4 106.1(17) . . ?
La1 O4 H4 119(3) . . ?
C11 O5 La1 138.2(2) . . ?
N3 O6 La1 132.4(2) . . ?
N5 O10' O11' 50.6(5) . . ?
N5 O11' O10' 48.8(5) . . ?
La1 O1W H11W 115(4) . . ?
La1 O1W H12W 115(4) . . ?
H11W O1W H12W 128(4) . . ?
La1 O2W H21W 131(3) . . ?
La1 O2W H22W 115(3) . . ?
H21W O2W H22W 113(3) . . ?
H31W O3W H32W 110(7) . . ?
O5 La1 O1 136.78(10) . . ?
O5 La1 O2W 74.98(10) . . ?
O1 La1 O2W 68.02(11) . . ?
O5 La1 O2 74.58(9) . . ?
O1 La1 O2 107.46(8) . . ?
O2W La1 O2 64.97(10) . . ?
O5 La1 O1W 77.05(10) . . ?
O1 La1 O1W 70.50(10) . . ?
O2W La1 O1W 70.99(13) . . ?
O2 La1 O1W 132.21(11) . . ?
O5 La1 O3 120.94(10) . . ?
O1 La1 O3 68.56(10) . . ?
O2W La1 O3 125.36(10) . . ?
O2 La1 O3 161.91(10) . . ?
O1W La1 O3 64.36(11) . . ?
O5 La1 O4 71.15(8) . . ?
O1 La1 O4 150.56(10) . . ?
O2W La1 O4 125.83(9) . . ?
O2 La1 O4 66.01(8) . . ?
O1W La1 O4 136.22(10) . . ?
O3 La1 O4 108.23(9) . . ?
O5 La1 O6 61.62(9) . . ?
O1 La1 O6 130.23(8) . . ?
O2W La1 O6 128.54(12) . . ?
O2 La1 O6 122.15(7) . . ?
O1W La1 O6 73.41(10) . . ?
O3 La1 O6 65.40(9) . . ?
O4 La1 O6 65.32(8) . . ?
O5 La1 N1 137.35(9) . . ?
O1 La1 N1 61.76(8) . . ?
O2W La1 N1 85.77(12) . . ?
O2 La1 N1 62.79(8) . . ?
O1W La1 N1 131.91(9) . . ?
O3 La1 N1 101.32(10) . . ?
O4 La1 N1 91.59(8) . . ?
O6 La1 N1 145.28(9) . . ?
O5 La1 N2 128.41(8) . . ?
O1 La1 N2 94.17(10) . . ?
O2W La1 N2 150.75(12) . . ?
O2 La1 N2 101.37(9) . . ?
O1W La1 N2 126.37(10) . . ?
O3 La1 N2 62.23(9) . . ?
O4 La1 N2 61.19(8) . . ?
O6 La1 N2 80.71(9) . . ?
N1 La1 N2 65.11(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 N1 -49.7(5) . . . . ?
O2 C3 C4 N1 -55.0(4) . . . . ?
N1 C5 C6 N2 -64.3(4) . . . . ?
O3 C7 C8 N2 -55.1(4) . . . . ?
O4 C9 C10 N2 -50.0(4) . . . . ?
O5 C11 C12 C13 -173.9(3) . . . . ?
C16 C11 C12 C13 5.5(5) . . . . ?
O5 C11 C12 N3 4.0(5) . . . . ?
C16 C11 C12 N3 -176.7(3) . . . . ?
C11 C12 C13 C14 -2.6(5) . . . . ?
N3 C12 C13 C14 179.4(3) . . . . ?
C12 C13 C14 C15 -1.0(5) . . . . ?
C12 C13 C14 N4 177.7(3) . . . . ?
C13 C14 C15 C16 1.2(6) . . . . ?
N4 C14 C15 C16 -177.6(3) . . . . ?
C14 C15 C16 C11 2.3(6) . . . . ?
C14 C15 C16 N5 179.2(3) . . . . ?
O5 C11 C16 C15 174.0(3) . . . . ?
C12 C11 C16 C15 -5.4(5) . . . . ?
O5 C11 C16 N5 -2.9(5) . . . . ?
C12 C11 C16 N5 177.8(3) . . . . ?
O12 C17 C18 C19 -179.7(4) . . . . ?
C22 C17 C18 C19 1.1(5) . . . . ?
O12 C17 C18 N6 -1.8(5) . . . . ?
C22 C17 C18 N6 179.1(3) . . . . ?
N6 C18 C19 C20 -178.8(3) . . . . ?
C17 C18 C19 C20 -0.8(5) . . . . ?
C18 C19 C20 C21 -0.5(6) . . . . ?
C18 C19 C20 N7 175.7(3) . . . . ?
C19 C20 C21 C22 1.3(6) . . . . ?
N7 C20 C21 C22 -174.8(3) . . . . ?
C20 C21 C22 C17 -0.9(6) . . . . ?
C20 C21 C22 N8 177.8(3) . . . . ?
O12 C17 C22 C21 -179.4(4) . . . . ?
C18 C17 C22 C21 -0.3(5) . . . . ?
O12 C17 C22 N8 2.0(6) . . . . ?
C18 C17 C22 N8 -178.9(3) . . . . ?
O19 C23 C24 C25 -178.7(4) . . . . ?
C28 C23 C24 C25 2.3(6) . . . . ?
O19 C23 C24 N9 2.3(6) . . . . ?
C28 C23 C24 N9 -176.6(4) . . . . ?
C23 C24 C25 C26 -0.9(6) . . . . ?
N9 C24 C25 C26 178.1(4) . . . . ?
C24 C25 C26 C27 -0.3(6) . . . . ?
C24 C25 C26 N10 179.2(4) . . . . ?
C25 C26 C27 C28 -0.3(6) . . . . ?
N10 C26 C27 C28 -179.8(4) . . . . ?
C26 C27 C28 C23 2.1(6) . . . . ?
C26 C27 C28 N11 -177.6(4) . . . . ?
O19 C23 C28 C27 178.1(4) . . . . ?
C24 C23 C28 C27 -2.9(6) . . . . ?
O19 C23 C28 N11 -2.2(7) . . . . ?
C24 C23 C28 N11 176.7(4) . . . . ?
C6 C5 N1 C4 -76.9(4) . . . . ?
C6 C5 N1 C2 164.4(3) . . . . ?
C6 C5 N1 La1 45.4(4) . . . . ?
C3 C4 N1 C5 162.6(3) . . . . ?
C3 C4 N1 C2 -78.1(4) . . . . ?
C3 C4 N1 La1 40.4(4) . . . . ?
C1 C2 N1 C5 -70.7(4) . . . . ?
C1 C2 N1 C4 170.2(4) . . . . ?
C1 C2 N1 La1 50.0(4) . . . . ?
C5 C6 N2 C10 164.7(3) . . . . ?
C5 C6 N2 C8 -77.1(4) . . . . ?
C5 C6 N2 La1 45.4(4) . . . . ?
C9 C10 N2 C6 -67.1(4) . . . . ?
C9 C10 N2 C8 174.2(3) . . . . ?
C9 C10 N2 La1 53.3(4) . . . . ?
C7 C8 N2 C6 162.4(3) . . . . ?
C7 C8 N2 C10 -78.2(4) . . . . ?
C7 C8 N2 La1 40.8(4) . . . . ?
C13 C12 N3 O7 0.9(5) . . . . ?
C11 C12 N3 O7 -177.1(4) . . . . ?
C13 C12 N3 O6 -178.8(3) . . . . ?
C11 C12 N3 O6 3.2(5) . . . . ?
C13 C14 N4 O8 -7.2(5) . . . . ?
C15 C14 N4 O8 171.6(4) . . . . ?
C13 C14 N4 O9 172.8(4) . . . . ?
C15 C14 N4 O9 -8.4(6) . . . . ?
C15 C16 N5 O10' 141.8(7) . . . . ?
C11 C16 N5 O10' -41.1(8) . . . . ?
C15 C16 N5 O11' -115.8(7) . . . . ?
C11 C16 N5 O11' 61.3(7) . . . . ?
C15 C16 N5 O10 83.1(5) . . . . ?
C11 C16 N5 O10 -99.8(5) . . . . ?
C15 C16 N5 O11 -47.3(6) . . . . ?
C11 C16 N5 O11 129.8(5) . . . . ?
C19 C18 N6 O13' 150.5(9) . . . . ?
C17 C18 N6 O13' -27.7(10) . . . . ?
C19 C18 N6 O13 -166.3(9) . . . . ?
C17 C18 N6 O13 15.6(10) . . . . ?
C19 C18 N6 O14' 28.5(7) . . . . ?
C17 C18 N6 O14' -149.6(6) . . . . ?
C19 C18 N6 O14 -32.9(6) . . . . ?
C17 C18 N6 O14 149.0(5) . . . . ?
C21 C20 N7 O16 0.7(6) . . . . ?
C19 C20 N7 O16 -175.5(4) . . . . ?
C21 C20 N7 O15 -178.6(4) . . . . ?
C19 C20 N7 O15 5.1(5) . . . . ?
C21 C22 N8 O18' -153.0(9) . . . . ?
C17 C22 N8 O18' 25.7(10) . . . . ?
C21 C22 N8 O18 173.7(12) . . . . ?
C17 C22 N8 O18 -7.6(13) . . . . ?
C21 C22 N8 O17' -0.6(14) . . . . ?
C17 C22 N8 O17' 178.2(13) . . . . ?
C21 C22 N8 O17 25.8(16) . . . . ?
C17 C22 N8 O17 -155.5(16) . . . . ?
C25 C24 N9 O20' 56.8(12) . . . . ?
C23 C24 N9 O20' -124.2(11) . . . . ?
C25 C24 N9 O21 143.9(8) . . . . ?
C23 C24 N9 O21 -37.0(9) . . . . ?
C25 C24 N9 O20 -23.3(6) . . . . ?
C23 C24 N9 O20 155.8(5) . . . . ?
C25 C24 N9 O21' -173.5(6) . . . . ?
C23 C24 N9 O21' 5.6(7) . . . . ?
C25 C26 N10 O23 176.9(4) . . . . ?
C27 C26 N10 O23 -3.6(6) . . . . ?
C25 C26 N10 O22 -2.1(6) . . . . ?
C27 C26 N10 O22 177.4(5) . . . . ?
C27 C28 N11 O25 160.1(6) . . . . ?
C23 C28 N11 O25 -19.6(8) . . . . ?
C27 C28 N11 O24 -21.5(7) . . . . ?
C23 C28 N11 O24 158.8(5) . . . . ?
C2 C1 O1 La1 24.6(5) . . . . ?
C4 C3 O2 La1 43.9(4) . . . . ?
C8 C7 O3 La1 44.4(4) . . . . ?
C10 C9 O4 La1 21.3(4) . . . . ?
C12 C11 O5 La1 32.9(6) . . . . ?
C16 C11 O5 La1 -146.3(3) . . . . ?
O7 N3 O6 La1 140.1(3) . . . . ?
C12 N3 O6 La1 -40.3(5) . . . . ?
O10 N5 O10' O11' -136.2(7) . . . . ?
O11 N5 O10' O11' -44.5(7) . . . . ?
C16 N5 O10' O11' 125.8(7) . . . . ?
O10 N5 O11' O10' 37.2(6) . . . . ?
O11 N5 O11' O10' 135.9(6) . . . . ?
C16 N5 O11' O10' -123.8(7) . . . . ?
C11 O5 La1 O1 -162.0(3) . . . . ?
C11 O5 La1 O2W 166.4(4) . . . . ?
C11 O5 La1 O2 98.7(4) . . . . ?
C11 O5 La1 O1W -120.2(4) . . . . ?
C11 O5 La1 O3 -71.1(4) . . . . ?
C11 O5 La1 O4 29.3(3) . . . . ?
C11 O5 La1 O6 -42.2(3) . . . . ?
C11 O5 La1 N1 100.2(4) . . . . ?
C11 O5 La1 N2 6.3(4) . . . . ?
C1 O1 La1 O5 -130.0(3) . . . . ?
C1 O1 La1 O2W -96.9(4) . . . . ?
C1 O1 La1 O2 -44.2(4) . . . . ?
C1 O1 La1 O1W -173.6(4) . . . . ?
C1 O1 La1 O3 117.1(4) . . . . ?
C1 O1 La1 O4 27.8(5) . . . . ?
C1 O1 La1 O6 140.5(3) . . . . ?
C1 O1 La1 N1 0.3(3) . . . . ?
C1 O1 La1 N2 59.1(4) . . . . ?
C3 O2 La1 O5 162.2(3) . . . . ?
C3 O2 La1 O1 27.3(3) . . . . ?
C3 O2 La1 O2W 81.8(3) . . . . ?
C3 O2 La1 O1W 106.5(3) . . . . ?
C3 O2 La1 O3 -47.0(4) . . . . ?
C3 O2 La1 O4 -122.0(3) . . . . ?
C3 O2 La1 O6 -156.9(3) . . . . ?
C3 O2 La1 N1 -16.7(3) . . . . ?
C3 O2 La1 N2 -70.8(3) . . . . ?
C7 O3 La1 O5 103.0(3) . . . . ?
C7 O3 La1 O1 -124.4(3) . . . . ?
C7 O3 La1 O2W -163.9(3) . . . . ?
C7 O3 La1 O2 -43.8(5) . . . . ?
C7 O3 La1 O1W 157.7(3) . . . . ?
C7 O3 La1 O4 24.4(3) . . . . ?
C7 O3 La1 O6 75.1(3) . . . . ?
C7 O3 La1 N1 -71.0(3) . . . . ?
C7 O3 La1 N2 -17.2(3) . . . . ?
C9 O4 La1 O5 -155.9(3) . . . . ?
C9 O4 La1 O1 40.0(4) . . . . ?
C9 O4 La1 O2W 149.8(3) . . . . ?
C9 O4 La1 O2 123.0(3) . . . . ?
C9 O4 La1 O1W -110.2(3) . . . . ?
C9 O4 La1 O3 -38.6(3) . . . . ?
C9 O4 La1 O6 -89.2(3) . . . . ?
C9 O4 La1 N1 63.9(3) . . . . ?
C9 O4 La1 N2 3.6(3) . . . . ?
N3 O6 La1 O5 46.7(3) . . . . ?
N3 O6 La1 O1 175.6(3) . . . . ?
N3 O6 La1 O2W 82.9(3) . . . . ?
N3 O6 La1 O2 0.8(4) . . . . ?
N3 O6 La1 O1W 130.7(3) . . . . ?
N3 O6 La1 O3 -160.5(4) . . . . ?
N3 O6 La1 O4 -34.4(3) . . . . ?
N3 O6 La1 N1 -86.8(4) . . . . ?
N3 O6 La1 N2 -96.8(3) . . . . ?
C5 N1 La1 O5 -135.9(2) . . . . ?
C4 N1 La1 O5 -14.6(3) . . . . ?
C2 N1 La1 O5 104.2(2) . . . . ?
C5 N1 La1 O1 94.4(2) . . . . ?
C4 N1 La1 O1 -144.3(3) . . . . ?
C2 N1 La1 O1 -25.5(2) . . . . ?
C5 N1 La1 O2W 161.7(2) . . . . ?
C4 N1 La1 O2W -77.0(2) . . . . ?
C2 N1 La1 O2W 41.8(2) . . . . ?
C5 N1 La1 O2 -134.3(2) . . . . ?
C4 N1 La1 O2 -13.1(2) . . . . ?
C2 N1 La1 O2 105.8(3) . . . . ?
C5 N1 La1 O1W 102.1(2) . . . . ?
C4 N1 La1 O1W -136.7(2) . . . . ?
C2 N1 La1 O1W -17.9(3) . . . . ?
C5 N1 La1 O3 36.5(2) . . . . ?
C4 N1 La1 O3 157.8(2) . . . . ?
C2 N1 La1 O3 -83.4(2) . . . . ?
C5 N1 La1 O4 -72.5(2) . . . . ?
C4 N1 La1 O4 48.8(2) . . . . ?
C2 N1 La1 O4 167.6(2) . . . . ?
C5 N1 La1 O6 -26.4(3) . . . . ?
C4 N1 La1 O6 94.9(3) . . . . ?
C2 N1 La1 O6 -146.3(2) . . . . ?
C5 N1 La1 N2 -15.4(2) . . . . ?
C4 N1 La1 N2 105.8(2) . . . . ?
C2 N1 La1 N2 -135.4(3) . . . . ?
C6 N2 La1 O5 117.0(2) . . . . ?
C10 N2 La1 O5 -3.2(3) . . . . ?
C8 N2 La1 O5 -122.0(2) . . . . ?
C6 N2 La1 O1 -71.0(2) . . . . ?
C10 N2 La1 O1 168.8(2) . . . . ?
C8 N2 La1 O1 50.0(2) . . . . ?
C6 N2 La1 O2W -20.6(3) . . . . ?
C10 N2 La1 O2W -140.9(2) . . . . ?
C8 N2 La1 O2W 100.4(3) . . . . ?
C6 N2 La1 O2 37.8(2) . . . . ?
C10 N2 La1 O2 -82.5(2) . . . . ?
C8 N2 La1 O2 158.7(2) . . . . ?
C6 N2 La1 O1W -139.8(2) . . . . ?
C10 N2 La1 O1W 100.0(2) . . . . ?
C8 N2 La1 O1W -18.8(3) . . . . ?
C6 N2 La1 O3 -134.1(2) . . . . ?
C10 N2 La1 O3 105.7(2) . . . . ?
C8 N2 La1 O3 -13.1(2) . . . . ?
C6 N2 La1 O4 92.0(2) . . . . ?
C10 N2 La1 O4 -28.2(2) . . . . ?
C8 N2 La1 O4 -147.0(2) . . . . ?
C6 N2 La1 O6 158.9(2) . . . . ?
C10 N2 La1 O6 38.7(2) . . . . ?
C8 N2 La1 O6 -80.1(2) . . . . ?
C6 N2 La1 N1 -14.8(2) . . . . ?
C10 N2 La1 N1 -135.1(2) . . . . ?
C8 N2 La1 N1 106.2(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        31.65
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.042
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.089
# start Validation Reply Form
_vrf_PLAT430_shelxl              
;
RESPONSE: This alerts is because of possibly missed Hydrogen
bonds as indicated by short Donor - Acceptor distances 
due to presence of disorder in the structure.
;
_vrf_PLAT041_shelxl              
;
RESPONSE: This Alert is due to missing of protons of disordered oxygen
atom of water molecule. 
;
_vrf_PLAT417_shelxl              
;
RESPONSE: This alerts is because of short non-bonding inter D-H..H-D contacts 
related to the disorder in the structure.
;
_vrf_PLAT420_shelxl              
;
RESPONSE: This alerts is because of unexpected positioning of donor-acceptor 
bond (O1W-H12W) due to disorder in the structure.
;
#
_database_code_depnum_ccdc_archive 'CCDC 881488'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'Department of ChemistryUniversity of AnywhereSometownSomewhere, UK'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H34 La N2 O8, 3(C6 H2 N3 O7)'
_chemical_formula_sum            'C30 H40 La N11 O29'
_chemical_formula_weight         1157.64

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'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
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'

_cell_length_a                   11.481(3)
_cell_length_b                   27.028(8)
_cell_length_c                   14.742(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.433(13)
_cell_angle_gamma                90.00
_cell_volume                     4258(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7574
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      38.03

_exptl_crystal_description       rectangular
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2344
_exptl_absorpt_coefficient_mu    1.121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5951
_exptl_absorpt_correction_T_max  0.7482
_exptl_absorpt_process_details   
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'

_exptl_special_details           
;
Department of Chemistry
University of Anywhere
Sometown
Somewhere, UK
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            59913
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.05
_diffrn_reflns_theta_max         42.38
_reflns_number_total             14972
_reflns_number_gt                12548
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Sir-92 (altomare, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'


_refine_special_details          
;
Ninteen restraints were used in the refinment of structure.
DFIX, OMIT, BUMP and LIST commands are the restraints used during 
structure refinement. DFIX command used to fix distance of protons
of water molecules to their O atoms. OMIT command is used to suppresses
all unnecessary reflections those who are truncated by beam stop. BUMP
is used for solvent water to suppress unnecessary weak interactions.
  
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0435P)²+1.3997P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14972
_refine_ls_number_parameters     338
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0313
_refine_ls_wR_factor_ref         0.0839
_refine_ls_wR_factor_gt          0.0761
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.588
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
C1 C 0.27024(18) 0.46507(8) 0.26985(19) 0.0394(4) Uani 1 1 d . . .
H1A H 0.2571 0.4451 0.3199 0.047 Uiso 1 1 calc R . .
H1B H 0.2385 0.4470 0.2088 0.047 Uiso 1 1 calc R . .
C2 C 0.2025(2) 0.51356(8) 0.25992(19) 0.0398(4) Uani 1 1 d . . .
H2A H 0.1132 0.5074 0.2375 0.048 Uiso 1 1 calc R . .
H2B H 0.2275 0.5293 0.3233 0.048 Uiso 1 1 calc R . .
C3 C 0.2343(2) 0.63502(8) 0.15348(19) 0.0410(4) Uani 1 1 d . . .
H3A H 0.1929 0.6321 0.0834 0.049 Uiso 1 1 calc R . .
H3B H 0.2192 0.6680 0.1729 0.049 Uiso 1 1 calc R . .
C4 C 0.1845(2) 0.59687(8) 0.2037(2) 0.0403(4) Uani 1 1 d . . .
H4A H 0.2116 0.6047 0.2726 0.048 Uiso 1 1 calc R . .
H4B H 0.0938 0.5975 0.1769 0.048 Uiso 1 1 calc R . .
C5 C 0.2488(2) 0.53422(9) 0.03225(15) 0.0411(4) Uani 1 1 d . . .
H5A H 0.2093 0.5185 -0.0307 0.049 Uiso 1 1 calc R . .
H5B H 0.2609 0.5689 0.0214 0.049 Uiso 1 1 calc R . .
C6 C 0.16631(18) 0.52953(8) 0.08981(16) 0.0391(4) Uani 1 1 d . . .
H6A H 0.0906 0.5486 0.0584 0.047 Uiso 1 1 calc R . .
H6B H 0.1426 0.4951 0.0906 0.047 Uiso 1 1 calc R . .
C7 C 0.59432(17) 0.36966(7) 0.41581(13) 0.0303(3) Uani 1 1 d . . .
C8 C 0.50876(16) 0.32895(8) 0.38376(13) 0.0317(3) Uani 1 1 d . . .
C9 C 0.54281(18) 0.28207(8) 0.36799(13) 0.0330(3) Uani 1 1 d . . .
H9 H 0.4832 0.2571 0.3464 0.040 Uiso 1 1 calc R . .
C10 C 0.66729(18) 0.27241(7) 0.38475(13) 0.0316(3) Uani 1 1 d . . .
C11 C 0.75792(17) 0.30866(7) 0.41991(13) 0.0313(3) Uani 1 1 d . . .
H11 H 0.8414 0.3018 0.4312 0.038 Uiso 1 1 calc R . .
C12 C 0.72224(16) 0.35481(7) 0.43767(13) 0.0296(3) Uani 1 1 d . . .
C13 C 0.5000 0.74889(9) 0.2500 0.0300(4) Uani 1 2 d S . .
C14 C 0.46008(15) 0.77869(6) 0.16212(12) 0.0261(2) Uani 1 1 d . . .
C15 C 0.46098(15) 0.82917(6) 0.16167(13) 0.0277(3) Uani 1 1 d . . .
H15 H 0.4359 0.8466 0.1033 0.033 Uiso 1 1 calc R . .
C16 C 0.5000 0.85388(8) 0.2500 0.0270(4) Uani 1 2 d S . .
N1 N 0.22856(15) 0.54719(5) 0.19171(13) 0.0292(3) Uani 1 1 d . . .
N2 N 0.37625(17) 0.33698(9) 0.36501(14) 0.0421(4) Uani 1 1 d . . .
N3 N 0.7037(2) 0.22353(7) 0.36557(13) 0.0400(4) Uani 1 1 d . . .
N4 N 0.82177(17) 0.39039(7) 0.48161(14) 0.0365(3) Uani 1 1 d . . .
N5 N 0.41830(16) 0.75441(7) 0.06841(12) 0.0341(3) Uani 1 1 d . . .
N6 N 0.5000 0.90688(8) 0.2500 0.0325(4) Uani 1 2 d S . .
O1 O 0.40032(13) 0.47497(6) 0.29544(13) 0.0408(3) Uani 1 1 d D . .
H1 H 0.440(2) 0.4535(10) 0.331(2) 0.049 Uiso 1 1 d D . .
O2 O 0.36549(14) 0.62672(5) 0.18089(14) 0.0412(3) Uani 1 1 d D . .
H2 H 0.401(2) 0.6538(9) 0.186(2) 0.049 Uiso 1 1 d D . .
O3 O 0.36797(15) 0.51134(7) 0.08330(11) 0.0400(3) Uani 1 1 d D . .
H3 H 0.363(3) 0.4820(9) 0.074(2) 0.048 Uiso 1 1 d D . .
O4 O 0.56182(15) 0.41379(6) 0.42237(13) 0.0399(3) Uani 1 1 d . . .
O5 O 0.34775(19) 0.36846(8) 0.41255(19) 0.0568(5) Uani 1 1 d . . .
O6 O 0.30078(18) 0.30999(13) 0.30514(17) 0.0789(9) Uani 1 1 d . . .
O7 O 0.6230(2) 0.19157(8) 0.33941(19) 0.0650(6) Uani 1 1 d . . .
O8 O 0.8133(2) 0.21585(8) 0.37852(17) 0.0551(5) Uani 1 1 d . . .
O9 O 0.9159(2) 0.38692(11) 0.4650(3) 0.0838(10) Uani 1 1 d . . .
O10 O 0.8083(2) 0.42244(9) 0.53383(18) 0.0631(6) Uani 1 1 d . . .
O11 O 0.5000 0.70312(8) 0.2500 0.0493(6) Uani 1 2 d S . .
O12 O 0.3710(3) 0.71360(8) 0.05902(15) 0.0623(6) Uani 1 1 d . . .
O13 O 0.4324(2) 0.77682(8) 0.00123(12) 0.0472(4) Uani 1 1 d . . .
O14 O 0.53588(18) 0.92874(6) 0.32879(14) 0.0462(4) Uani 1 1 d . . .
O1W O 0.4463(2) 0.59128(9) 0.38675(14) 0.0527(5) Uani 1 1 d D . .
H11W H 0.463(4) 0.5788(14) 0.439(2) 0.063 Uiso 1 1 d D . .
H12W H 0.454(4) 0.6200(9) 0.385(3) 0.063 Uiso 1 1 d D . .
La1 La 0.5000 0.550051(4) 0.2500 0.02219(4) Uani 1 2 d S . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1 O1 1.426(2) . ?
C1 C2 1.503(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N1 1.465(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 O2 1.428(3) . ?
C3 C4 1.499(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N1 1.468(2) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O3 1.438(3) . ?
C5 C6 1.490(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N1 1.487(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 O4 1.264(2) . ?
C7 C8 1.435(3) . ?
C7 C12 1.441(3) . ?
C8 C9 1.371(3) . ?
C8 N2 1.460(3) . ?
C9 C10 1.383(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.385(3) . ?
C10 N3 1.444(3) . ?
C11 C12 1.368(3) . ?
C11 H11 0.9300 . ?
C12 N4 1.452(3) . ?
C13 O11 1.237(3) . ?
C13 C14 1.450(2) . ?
C13 C14 1.450(2) 2_655 ?
C14 C15 1.364(2) . ?
C14 N5 1.444(2) . ?
C15 C16 1.384(2) . ?
C15 H15 0.9300 . ?
C16 C15 1.384(2) 2_655 ?
C16 N6 1.432(3) . ?
N1 La1 2.9153(18) . ?
N2 O5 1.221(3) . ?
N2 O6 1.226(3) . ?
N3 O8 1.219(3) . ?
N3 O7 1.221(3) . ?
N4 O9 1.195(3) . ?
N4 O10 1.206(3) . ?
N5 O12 1.215(3) . ?
N5 O13 1.221(2) . ?
N6 O14 1.232(2) 2_655 ?
N6 O14 1.232(2) . ?
O1 La1 2.5370(15) . ?
O1 H1 0.80(2) . ?
O2 La1 2.5625(15) . ?
O2 H2 0.83(2) . ?
O3 La1 2.5902(16) . ?
O3 H3 0.80(2) . ?
O1W La1 2.5680(18) . ?
O1W H11W 0.80(2) . ?
O1W H12W 0.78(2) . ?
La1 O1 2.5370(15) 2_655 ?
La1 O2 2.5626(15) 2_655 ?
La1 O1W 2.5679(18) 2_655 ?
La1 O3 2.5901(16) 2_655 ?
La1 N1 2.9153(18) 2_655 ?

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
O1 C1 C2 108.45(17) . . ?
O1 C1 H1A 110.0 . . ?
C2 C1 H1A 110.0 . . ?
O1 C1 H1B 110.0 . . ?
C2 C1 H1B 110.0 . . ?
H1A C1 H1B 108.4 . . ?
N1 C2 C1 112.33(17) . . ?
N1 C2 H2A 109.1 . . ?
C1 C2 H2A 109.1 . . ?
N1 C2 H2B 109.1 . . ?
C1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.9 . . ?
O2 C3 C4 107.78(16) . . ?
O2 C3 H3A 110.2 . . ?
C4 C3 H3A 110.2 . . ?
O2 C3 H3B 110.2 . . ?
C4 C3 H3B 110.2 . . ?
H3A C3 H3B 108.5 . . ?
N1 C4 C3 111.04(18) . . ?
N1 C4 H4A 109.4 . . ?
C3 C4 H4A 109.4 . . ?
N1 C4 H4B 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
O3 C5 C6 110.28(18) . . ?
O3 C5 H5A 109.6 . . ?
C6 C5 H5A 109.6 . . ?
O3 C5 H5B 109.6 . . ?
C6 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
N1 C6 C5 112.16(16) . . ?
N1 C6 H6A 109.2 . . ?
C5 C6 H6A 109.2 . . ?
N1 C6 H6B 109.2 . . ?
C5 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
O4 C7 C8 124.26(17) . . ?
O4 C7 C12 123.43(19) . . ?
C8 C7 C12 112.29(17) . . ?
C9 C8 C7 124.14(17) . . ?
C9 C8 N2 116.57(19) . . ?
C7 C8 N2 119.28(19) . . ?
C8 C9 C10 118.96(18) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
C9 C10 C11 121.28(18) . . ?
C9 C10 N3 119.44(18) . . ?
C11 C10 N3 119.28(18) . . ?
C12 C11 C10 118.72(17) . . ?
C12 C11 H11 120.6 . . ?
C10 C11 H11 120.6 . . ?
C11 C12 C7 124.28(17) . . ?
C11 C12 N4 116.58(16) . . ?
C7 C12 N4 119.14(17) . . ?
O11 C13 C14 123.74(10) . . ?
O11 C13 C14 123.74(10) . 2_655 ?
C14 C13 C14 112.5(2) . 2_655 ?
C15 C14 C13 124.00(16) . . ?
C15 C14 N5 116.77(16) . . ?
C13 C14 N5 119.22(16) . . ?
C14 C15 C16 118.58(16) . . ?
C14 C15 H15 120.7 . . ?
C16 C15 H15 120.7 . . ?
C15 C16 C15 122.3(2) . 2_655 ?
C15 C16 N6 118.85(11) . . ?
C15 C16 N6 118.85(11) 2_655 . ?
C2 N1 C4 108.60(17) . . ?
C2 N1 C6 110.56(17) . . ?
C4 N1 C6 110.85(17) . . ?
C2 N1 La1 106.16(12) . . ?
C4 N1 La1 108.56(12) . . ?
C6 N1 La1 111.95(12) . . ?
O5 N2 O6 124.1(2) . . ?
O5 N2 C8 118.3(2) . . ?
O6 N2 C8 117.5(2) . . ?
O8 N3 O7 123.3(2) . . ?
O8 N3 C10 118.7(2) . . ?
O7 N3 C10 117.9(2) . . ?
O9 N4 O10 121.5(2) . . ?
O9 N4 C12 118.6(2) . . ?
O10 N4 C12 119.80(19) . . ?
O12 N5 O13 122.96(19) . . ?
O12 N5 C14 120.01(18) . . ?
O13 N5 C14 117.02(17) . . ?
O14 N6 O14 122.7(2) 2_655 . ?
O14 N6 C16 118.65(12) 2_655 . ?
O14 N6 C16 118.66(12) . . ?
C1 O1 La1 127.61(12) . . ?
C1 O1 H1 108.8(18) . . ?
La1 O1 H1 123.4(18) . . ?
C3 O2 La1 131.29(12) . . ?
C3 O2 H2 108.8(17) . . ?
La1 O2 H2 118.1(18) . . ?
C5 O3 La1 115.97(13) . . ?
C5 O3 H3 110(2) . . ?
La1 O3 H3 123(2) . . ?
La1 O1W H11W 122(3) . . ?
La1 O1W H12W 110(3) . . ?
H11W O1W H12W 118(4) . . ?
O1 La1 O1 73.77(9) . 2_655 ?
O1 La1 O2 119.16(5) . . ?
O1 La1 O2 143.73(6) 2_655 . ?
O1 La1 O2 143.73(6) . 2_655 ?
O1 La1 O2 119.17(5) 2_655 2_655 ?
O2 La1 O2 72.08(7) . 2_655 ?
O1 La1 O1W 144.61(7) . 2_655 ?
O1 La1 O1W 83.05(7) 2_655 2_655 ?
O2 La1 O1W 67.64(7) . 2_655 ?
O2 La1 O1W 71.25(7) 2_655 2_655 ?
O1 La1 O1W 83.05(7) . . ?
O1 La1 O1W 144.61(7) 2_655 . ?
O2 La1 O1W 71.25(7) . . ?
O2 La1 O1W 67.64(7) 2_655 . ?
O1W La1 O1W 128.56(11) 2_655 . ?
O1 La1 O3 65.83(5) . 2_655 ?
O1 La1 O3 76.31(6) 2_655 2_655 ?
O2 La1 O3 139.69(6) . 2_655 ?
O2 La1 O3 83.72(6) 2_655 2_655 ?
O1W La1 O3 134.02(7) 2_655 2_655 ?
O1W La1 O3 69.85(7) . 2_655 ?
O1 La1 O3 76.31(6) . . ?
O1 La1 O3 65.83(5) 2_655 . ?
O2 La1 O3 83.72(6) . . ?
O2 La1 O3 139.69(6) 2_655 . ?
O1W La1 O3 69.85(7) 2_655 . ?
O1W La1 O3 134.03(7) . . ?
O3 La1 O3 132.36(8) 2_655 . ?
O1 La1 N1 115.96(5) . 2_655 ?
O1 La1 N1 61.31(4) 2_655 2_655 ?
O2 La1 N1 124.24(5) . 2_655 ?
O2 La1 N1 58.69(5) 2_655 2_655 ?
O1W La1 N1 72.87(7) 2_655 2_655 ?
O1W La1 N1 108.51(7) . 2_655 ?
O3 La1 N1 61.16(5) 2_655 2_655 ?
O3 La1 N1 117.44(5) . 2_655 ?
O1 La1 N1 61.30(4) . . ?
O1 La1 N1 115.95(5) 2_655 . ?
O2 La1 N1 58.69(5) . . ?
O2 La1 N1 124.24(5) 2_655 . ?
O1W La1 N1 108.51(7) 2_655 . ?
O1W La1 N1 72.87(7) . . ?
O3 La1 N1 117.44(5) 2_655 . ?
O3 La1 N1 61.16(5) . . ?
N1 La1 N1 176.96(6) 2_655 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 N1 54.3(3) . . . . ?
O2 C3 C4 N1 -48.1(3) . . . . ?
O3 C5 C6 N1 51.9(2) . . . . ?
O4 C7 C8 C9 173.63(18) . . . . ?
C12 C7 C8 C9 -5.0(2) . . . . ?
O4 C7 C8 N2 -5.6(3) . . . . ?
C12 C7 C8 N2 175.84(16) . . . . ?
C7 C8 C9 C10 0.8(3) . . . . ?
N2 C8 C9 C10 -179.93(17) . . . . ?
C8 C9 C10 C11 2.1(3) . . . . ?
C8 C9 C10 N3 -178.14(17) . . . . ?
C9 C10 C11 C12 -0.3(3) . . . . ?
N3 C10 C11 C12 179.92(17) . . . . ?
C10 C11 C12 C7 -4.6(3) . . . . ?
C10 C11 C12 N4 175.33(17) . . . . ?
O4 C7 C12 C11 -171.73(19) . . . . ?
C8 C7 C12 C11 6.9(3) . . . . ?
O4 C7 C12 N4 8.4(3) . . . . ?
C8 C7 C12 N4 -173.00(16) . . . . ?
O11 C13 C14 C15 -179.36(12) . . . . ?
C14 C13 C14 C15 0.64(12) 2_655 . . . ?
O11 C13 C14 N5 -0.42(17) . . . . ?
C14 C13 C14 N5 179.59(17) 2_655 . . . ?
C13 C14 C15 C16 -1.2(2) . . . . ?
N5 C14 C15 C16 179.79(13) . . . . ?
C14 C15 C16 C15 0.60(11) . . . 2_655 ?
C14 C15 C16 N6 -179.40(11) . . . . ?
C1 C2 N1 C4 -166.64(19) . . . . ?
C1 C2 N1 C6 71.5(2) . . . . ?
C1 C2 N1 La1 -50.1(2) . . . . ?
C3 C4 N1 C2 166.88(19) . . . . ?
C3 C4 N1 C6 -71.5(2) . . . . ?
C3 C4 N1 La1 51.9(2) . . . . ?
C5 C6 N1 C2 -137.82(18) . . . . ?
C5 C6 N1 C4 101.7(2) . . . . ?
C5 C6 N1 La1 -19.7(2) . . . . ?
C9 C8 N2 O5 150.1(2) . . . . ?
C7 C8 N2 O5 -30.6(3) . . . . ?
C9 C8 N2 O6 -26.8(3) . . . . ?
C7 C8 N2 O6 152.5(2) . . . . ?
C9 C10 N3 O8 178.3(2) . . . . ?
C11 C10 N3 O8 -1.9(3) . . . . ?
C9 C10 N3 O7 -3.5(3) . . . . ?
C11 C10 N3 O7 176.3(2) . . . . ?
C11 C12 N4 O9 29.7(3) . . . . ?
C7 C12 N4 O9 -150.4(3) . . . . ?
C11 C12 N4 O10 -150.0(2) . . . . ?
C7 C12 N4 O10 29.9(3) . . . . ?
C15 C14 N5 O12 -152.5(2) . . . . ?
C13 C14 N5 O12 28.5(3) . . . . ?
C15 C14 N5 O13 27.1(3) . . . . ?
C13 C14 N5 O13 -151.93(17) . . . . ?
C15 C16 N6 O14 0.65(13) . . . 2_655 ?
C15 C16 N6 O14 -179.35(13) 2_655 . . 2_655 ?
C15 C16 N6 O14 -179.35(13) . . . . ?
C15 C16 N6 O14 0.65(13) 2_655 . . . ?
C2 C1 O1 La1 -30.3(3) . . . . ?
C4 C3 O2 La1 20.3(3) . . . . ?
C6 C5 O3 La1 -62.9(2) . . . . ?
C1 O1 La1 O1 -129.2(2) . . . 2_655 ?
C1 O1 La1 O2 13.9(2) . . . . ?
C1 O1 La1 O2 113.35(19) . . . 2_655 ?
C1 O1 La1 O1W -78.1(2) . . . 2_655 ?
C1 O1 La1 O1W 77.8(2) . . . . ?
C1 O1 La1 O3 148.8(2) . . . 2_655 ?
C1 O1 La1 O3 -60.8(2) . . . . ?
C1 O1 La1 N1 -174.92(18) . . . 2_655 ?
C1 O1 La1 N1 3.58(18) . . . . ?
C3 O2 La1 O1 -6.2(2) . . . . ?
C3 O2 La1 O1 96.5(2) . . . 2_655 ?
C3 O2 La1 O2 -148.4(2) . . . 2_655 ?
C3 O2 La1 O1W 135.1(2) . . . 2_655 ?
C3 O2 La1 O1W -76.6(2) . . . . ?
C3 O2 La1 O3 -92.4(2) . . . 2_655 ?
C3 O2 La1 O3 64.3(2) . . . . ?
C3 O2 La1 N1 -176.64(19) . . . 2_655 ?
C3 O2 La1 N1 4.36(19) . . . . ?
C5 O3 La1 O1 99.95(17) . . . . ?
C5 O3 La1 O1 178.06(18) . . . 2_655 ?
C5 O3 La1 O2 -22.15(16) . . . . ?
C5 O3 La1 O2 -74.69(18) . . . 2_655 ?
C5 O3 La1 O1W -90.60(18) . . . 2_655 ?
C5 O3 La1 O1W 34.1(2) . . . . ?
C5 O3 La1 O3 137.54(17) . . . 2_655 ?
C5 O3 La1 N1 -147.65(15) . . . 2_655 ?
C5 O3 La1 N1 35.42(15) . . . . ?
C2 N1 La1 O1 24.17(13) . . . . ?
C4 N1 La1 O1 140.75(16) . . . . ?
C6 N1 La1 O1 -96.56(13) . . . . ?
C2 N1 La1 O1 75.79(14) . . . 2_655 ?
C4 N1 La1 O1 -167.62(14) . . . 2_655 ?
C6 N1 La1 O1 -44.94(14) . . . 2_655 ?
C2 N1 La1 O2 -145.32(15) . . . . ?
C4 N1 La1 O2 -28.73(14) . . . . ?
C6 N1 La1 O2 93.95(13) . . . . ?
C2 N1 La1 O2 -113.50(13) . . . 2_655 ?
C4 N1 La1 O2 3.09(16) . . . 2_655 ?
C6 N1 La1 O2 125.77(12) . . . 2_655 ?
C2 N1 La1 O1W 167.00(14) . . . 2_655 ?
C4 N1 La1 O1W -76.42(15) . . . 2_655 ?
C6 N1 La1 O1W 46.27(13) . . . 2_655 ?
C2 N1 La1 O1W -67.22(14) . . . . ?
C4 N1 La1 O1W 49.36(15) . . . . ?
C6 N1 La1 O1W 172.05(14) . . . . ?
C2 N1 La1 O3 -11.70(15) . . . 2_655 ?
C4 N1 La1 O3 104.88(14) . . . 2_655 ?
C6 N1 La1 O3 -132.43(12) . . . 2_655 ?
C2 N1 La1 O3 113.80(14) . . . . ?
C4 N1 La1 O3 -129.62(15) . . . . ?
C6 N1 La1 O3 -6.93(12) . . . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        42.38
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         2.271
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.090
# start Validation Reply Form
_vrf_PLAT094_shelxl              
;
RESPONSE: This Alert is due to the presence of heavy
metal atom like lanthanum in the complex.
;
_vrf_PLAT973_shelxl              
;
RESPONSE: This Alert is due to the presence of large
expected residual density on heavy metal atom location.
;
# end Validation Reply Form

_database_code_depnum_ccdc_archive 'CCDC 902457'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_I

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'Department of ChemistryUniversity of AnywhereSometownSomewhere, UK'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H26 N2 O4, 2(C6 H2 N3 O7)'
_chemical_formula_sum            'C22 H30 N8 O18'
_chemical_formula_weight         694.54

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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'

_cell_length_a                   23.9300(5)
_cell_length_b                   8.4550(2)
_cell_length_c                   14.1050(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.3190(9)
_cell_angle_gamma                90.00
_cell_volume                     2823.81(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9908
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      34.32

_exptl_crystal_description       Needles
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1448
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6791
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_process_details   
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'

_exptl_special_details           
;
Department of Chemistry
University of Anywhere
Sometown
Somewhere, UK
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22404
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.72
_diffrn_reflns_theta_max         34.39
_reflns_number_total             5858
_reflns_number_gt                4478
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Sir-92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0975P)²+1.5702P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5858
_refine_ls_number_parameters     219
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0554
_refine_ls_wR_factor_ref         0.1789
_refine_ls_wR_factor_gt          0.1638
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
C1 C 0.75025(5) 0.32948(13) 0.63523(9) 0.0275(2) Uani 1 1 d . . .
H1A H 0.7895 0.3160 0.6266 0.033 Uiso 1 1 calc R . .
H1B H 0.7475 0.3100 0.7022 0.033 Uiso 1 1 calc R . .
C2 C 0.73245(6) 0.49828(13) 0.61059(8) 0.0294(2) Uani 1 1 d . . .
H2A H 0.7589 0.5706 0.6467 0.035 Uiso 1 1 calc R . .
H2B H 0.6954 0.5173 0.6287 0.035 Uiso 1 1 calc R . .
C3 C 0.66491(7) 0.54118(17) 0.34655(10) 0.0390(3) Uani 1 1 d . . .
H3A H 0.6947 0.4823 0.3223 0.047 Uiso 1 1 calc R . .
H3B H 0.6289 0.4992 0.3169 0.047 Uiso 1 1 calc R . .
C4 C 0.67039(5) 0.52232(15) 0.45374(9) 0.0315(2) Uani 1 1 d . . .
H4A H 0.6541 0.4215 0.4680 0.038 Uiso 1 1 calc R . .
H4B H 0.6486 0.6048 0.4791 0.038 Uiso 1 1 calc R . .
C5 C 0.76318(4) 0.67469(12) 0.48400(8) 0.0252(2) Uani 1 1 d . . .
H5A H 0.7648 0.6807 0.4158 0.030 Uiso 1 1 calc R . .
H5B H 0.8016 0.6658 0.5168 0.030 Uiso 1 1 calc R . .
C6 C 0.57139(5) 0.16576(15) 0.63534(8) 0.0274(2) Uani 1 1 d . . .
C7 C 0.51608(5) 0.23724(14) 0.62378(9) 0.0297(2) Uani 1 1 d . . .
C8 C 0.46655(5) 0.15369(15) 0.61253(9) 0.0309(2) Uani 1 1 d . . .
H8 H 0.4320 0.2061 0.6022 0.037 Uiso 1 1 calc R . .
C9 C 0.46855(5) -0.00984(15) 0.61679(9) 0.0291(2) Uani 1 1 d . . .
C10 C 0.51924(5) -0.09165(15) 0.63068(9) 0.0305(2) Uani 1 1 d . . .
H10 H 0.5200 -0.2015 0.6340 0.037 Uiso 1 1 calc R . .
C11 C 0.56865(5) -0.00480(15) 0.63942(9) 0.0287(2) Uani 1 1 d . . .
N1 N 0.73048(4) 0.52974(10) 0.50435(7) 0.02437(18) Uani 1 1 d . . .
H1C H 0.7487 0.4468 0.4813 0.029 Uiso 1 1 calc R . .
N2 N 0.51064(6) 0.40973(15) 0.62434(11) 0.0449(3) Uani 1 1 d . . .
N3 N 0.41587(5) -0.09604(15) 0.60689(10) 0.0399(3) Uani 1 1 d . . .
N4 N 0.62097(5) -0.09434(15) 0.65222(10) 0.0382(3) Uani 1 1 d . . .
O1 O 0.71675(4) 0.21651(10) 0.57801(7) 0.03002(19) Uani 1 1 d . . .
H1 H 0.6861 0.2077 0.5970 0.045 Uiso 1 1 calc R . .
O2 O 0.66879(6) 0.70313(14) 0.32295(8) 0.0487(3) Uani 1 1 d . . .
H2 H 0.6520 0.7186 0.2689 0.073 Uiso 1 1 calc R . .
O3 O 0.61620(4) 0.24499(13) 0.63820(8) 0.0381(2) Uani 1 1 d . . .
O4 O 0.54686(7) 0.48736(17) 0.67154(16) 0.0782(5) Uani 1 1 d . . .
O5 O 0.46797(7) 0.46774(18) 0.57915(16) 0.0743(5) Uani 1 1 d . . .
O6 O 0.37311(5) -0.03061(17) 0.56733(13) 0.0618(4) Uani 1 1 d . . .
O7 O 0.41593(6) -0.22973(16) 0.63910(16) 0.0763(5) Uani 1 1 d . . .
O8 O 0.62049(6) -0.22650(16) 0.61635(13) 0.0635(4) Uani 1 1 d . . .
O9 O 0.66342(5) -0.03397(19) 0.69638(12) 0.0625(4) Uani 1 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1 O1 1.4210(14) . ?
C1 C2 1.5153(16) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N1 1.5160(15) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 O2 1.4154(18) . ?
C3 C4 1.5071(19) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N1 1.5113(15) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N1 1.5040(14) . ?
C5 C5 1.519(2) 7_666 ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 O3 1.2602(14) . ?
C6 C7 1.4426(16) . ?
C6 C11 1.4451(17) . ?
C7 C8 1.3693(16) . ?
C7 N2 1.4643(17) . ?
C8 C9 1.3845(17) . ?
C8 H8 0.9300 . ?
C9 C10 1.3854(16) . ?
C9 N3 1.4453(15) . ?
C10 C11 1.3821(16) . ?
C10 H10 0.9300 . ?
C11 N4 1.4519(16) . ?
N1 H1C 0.9100 . ?
N2 O4 1.208(2) . ?
N2 O5 1.225(2) . ?
N3 O7 1.2182(19) . ?
N3 O6 1.2243(18) . ?
N4 O9 1.2236(18) . ?
N4 O8 1.2260(19) . ?
O1 H1 0.8200 . ?
O2 H2 0.8200 . ?

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
O1 C1 C2 112.71(9) . . ?
O1 C1 H1A 109.0 . . ?
C2 C1 H1A 109.0 . . ?
O1 C1 H1B 109.0 . . ?
C2 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
C1 C2 N1 111.07(9) . . ?
C1 C2 H2A 109.4 . . ?
N1 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
N1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
O2 C3 C4 109.82(11) . . ?
O2 C3 H3A 109.7 . . ?
C4 C3 H3A 109.7 . . ?
O2 C3 H3B 109.7 . . ?
C4 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
C3 C4 N1 114.09(11) . . ?
C3 C4 H4A 108.7 . . ?
N1 C4 H4A 108.7 . . ?
C3 C4 H4B 108.7 . . ?
N1 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
N1 C5 C5 112.12(11) . 7_666 ?
N1 C5 H5A 109.2 . . ?
C5 C5 H5A 109.2 7_666 . ?
N1 C5 H5B 109.2 . . ?
C5 C5 H5B 109.2 7_666 . ?
H5A C5 H5B 107.9 . . ?
O3 C6 C7 122.92(12) . . ?
O3 C6 C11 124.93(11) . . ?
C7 C6 C11 112.11(10) . . ?
C8 C7 C6 124.17(11) . . ?
C8 C7 N2 116.00(11) . . ?
C6 C7 N2 119.83(11) . . ?
C7 C8 C9 119.10(11) . . ?
C7 C8 H8 120.5 . . ?
C9 C8 H8 120.5 . . ?
C8 C9 C10 121.93(11) . . ?
C8 C9 N3 118.37(11) . . ?
C10 C9 N3 119.70(11) . . ?
C11 C10 C9 117.87(11) . . ?
C11 C10 H10 121.1 . . ?
C9 C10 H10 121.1 . . ?
C10 C11 C6 124.74(10) . . ?
C10 C11 N4 116.44(11) . . ?
C6 C11 N4 118.81(10) . . ?
C5 N1 C4 115.44(8) . . ?
C5 N1 C2 112.89(8) . . ?
C4 N1 C2 110.55(9) . . ?
C5 N1 H1C 105.7 . . ?
C4 N1 H1C 105.7 . . ?
C2 N1 H1C 105.7 . . ?
O4 N2 O5 123.15(15) . . ?
O4 N2 C7 119.15(14) . . ?
O5 N2 C7 117.64(13) . . ?
O7 N3 O6 123.03(13) . . ?
O7 N3 C9 118.55(13) . . ?
O6 N3 C9 118.42(13) . . ?
O9 N4 O8 123.21(13) . . ?
O9 N4 C11 118.90(13) . . ?
O8 N4 C11 117.87(12) . . ?
C1 O1 H1 109.5 . . ?
C3 O2 H2 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 N1 -53.12(13) . . . . ?
O2 C3 C4 N1 -79.42(15) . . . . ?
O3 C6 C7 C8 174.39(13) . . . . ?
C11 C6 C7 C8 -3.45(17) . . . . ?
O3 C6 C7 N2 -6.06(19) . . . . ?
C11 C6 C7 N2 176.10(12) . . . . ?
C6 C7 C8 C9 3.2(2) . . . . ?
N2 C7 C8 C9 -176.35(12) . . . . ?
C7 C8 C9 C10 -1.0(2) . . . . ?
C7 C8 C9 N3 178.66(12) . . . . ?
C8 C9 C10 C11 -0.63(19) . . . . ?
N3 C9 C10 C11 179.74(12) . . . . ?
C9 C10 C11 C6 0.14(19) . . . . ?
C9 C10 C11 N4 -178.95(11) . . . . ?
O3 C6 C11 C10 -176.05(12) . . . . ?
C7 C6 C11 C10 1.74(17) . . . . ?
O3 C6 C11 N4 3.02(19) . . . . ?
C7 C6 C11 N4 -179.19(11) . . . . ?
C5 C5 N1 C4 61.87(15) 7_666 . . . ?
C5 C5 N1 C2 -66.64(14) 7_666 . . . ?
C3 C4 N1 C5 54.32(14) . . . . ?
C3 C4 N1 C2 -176.02(10) . . . . ?
C1 C2 N1 C5 -128.46(10) . . . . ?
C1 C2 N1 C4 100.53(11) . . . . ?
C8 C7 N2 O4 148.74(17) . . . . ?
C6 C7 N2 O4 -30.8(2) . . . . ?
C8 C7 N2 O5 -28.6(2) . . . . ?
C6 C7 N2 O5 151.86(16) . . . . ?
C8 C9 N3 O7 -157.47(17) . . . . ?
C10 C9 N3 O7 22.2(2) . . . . ?
C8 C9 N3 O6 21.8(2) . . . . ?
C10 C9 N3 O6 -158.56(15) . . . . ?
C10 C11 N4 O9 -151.41(14) . . . . ?
C6 C11 N4 O9 29.44(19) . . . . ?
C10 C11 N4 O8 29.91(19) . . . . ?
C6 C11 N4 O8 -149.24(14) . . . . ?

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
O1 H1 O3 0.82 1.87 2.6756(13) 165.1 .
O2 H2 O3 0.82 1.94 2.7601(15) 176.8 6_565
N1 H1C O1 0.91 1.87 2.7755(13) 174.5 7_656

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        34.39
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.064
_database_code_depnum_ccdc_archive 'CCDC 936271'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_II

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'Department of ChemistryUniversity of AnywhereSometownSomewhere, UK'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H16 N O3, C6 H2 N3 O7'
_chemical_formula_sum            'C12 H18 N4 O10'
_chemical_formula_weight         378.30

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.4430(4)
_cell_length_b                   8.3890(2)
_cell_length_c                   14.8400(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.8460(14)
_cell_angle_gamma                90.00
_cell_volume                     1667.57(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6138
_cell_measurement_theta_min      2.76
_cell_measurement_theta_max      26.71

_exptl_crystal_description       Rectangular
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             792
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6530
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_process_details   
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'

_exptl_special_details           
;
Department of Chemistry
University of Anywhere
Sometown
Somewhere, UK
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15966
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         32.33
_reflns_number_total             5059
_reflns_number_gt                3207
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Sir-92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0658P)²+0.4799P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5059
_refine_ls_number_parameters     241
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0527
_refine_ls_wR_factor_ref         0.1499
_refine_ls_wR_factor_gt          0.1295
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
C1 C 0.39810(13) 0.7538(3) 0.17370(12) 0.0545(5) Uani 1 1 d . . .
H1A H 0.3405 0.6944 0.1483 0.065 Uiso 1 1 calc R . .
H1B H 0.4087 0.8426 0.1337 0.065 Uiso 1 1 calc R . .
C2 C 0.37799(13) 0.8165(2) 0.26599(12) 0.0480(4) Uani 1 1 d . . .
H2A H 0.4294 0.8923 0.2869 0.058 Uiso 1 1 calc R . .
H2B H 0.3140 0.8708 0.2625 0.058 Uiso 1 1 calc R . .
C3 C 0.51560(12) 0.7693(2) 0.44161(12) 0.0497(4) Uani 1 1 d . . .
H3A H 0.5283 0.8632 0.4061 0.060 Uiso 1 1 calc R . .
H3B H 0.5332 0.7934 0.5049 0.060 Uiso 1 1 calc R . .
C4 C 0.40760(11) 0.7232(2) 0.42726(11) 0.0452(4) Uani 1 1 d . . .
H4A H 0.3953 0.6332 0.4659 0.054 Uiso 1 1 calc R . .
H4B H 0.3668 0.8114 0.4448 0.054 Uiso 1 1 calc R . .
C5 C 0.29006(13) 0.4228(2) 0.34835(12) 0.0488(4) Uani 1 1 d . . .
H5A H 0.3202 0.4140 0.4099 0.059 Uiso 1 1 calc R . .
H5B H 0.2250 0.3722 0.3456 0.059 Uiso 1 1 calc R . .
C6 C 0.27815(11) 0.5948(2) 0.32338(11) 0.0428(4) Uani 1 1 d . . .
H6A H 0.2339 0.6456 0.3630 0.051 Uiso 1 1 calc R . .
H6B H 0.2479 0.6033 0.2619 0.051 Uiso 1 1 calc R . .
C7 C 0.16481(10) 0.2730(2) 0.08329(10) 0.0383(3) Uani 1 1 d . . .
C8 C 0.13830(10) 0.34905(19) -0.00283(10) 0.0366(3) Uani 1 1 d . . .
C9 C 0.04704(11) 0.3388(2) -0.05086(10) 0.0392(3) Uani 1 1 d . . .
H9 H 0.0337 0.3949 -0.1046 0.047 Uiso 1 1 calc R . .
C10 C -0.02499(10) 0.2426(2) -0.01729(11) 0.0403(4) Uani 1 1 d . . .
C11 C -0.00783(11) 0.1659(2) 0.06441(11) 0.0424(4) Uani 1 1 d . . .
H11 H -0.0571 0.1022 0.0861 0.051 Uiso 1 1 calc R . .
C12 C 0.08235(11) 0.1839(2) 0.11370(10) 0.0407(4) Uani 1 1 d . . .
N1 N 0.37728(9) 0.67966(16) 0.33081(8) 0.0339(3) Uani 1 1 d D . .
H1C H 0.4210(12) 0.616(2) 0.3148(11) 0.041 Uiso 1 1 d D . .
N2 N 0.21213(10) 0.44927(18) -0.04193(9) 0.0430(3) Uani 1 1 d . . .
N3 N -0.12183(10) 0.2275(2) -0.06712(11) 0.0549(4) Uani 1 1 d . . .
N4 N 0.09319(13) 0.1041(2) 0.20117(11) 0.0600(4) Uani 1 1 d . . .
O1 O 0.48314(9) 0.65376(16) 0.17943(8) 0.0517(3) Uani 1 1 d . . .
H1 H 0.5338 0.7086 0.1838 0.062 Uiso 1 1 calc R . .
O2 O 0.57279(8) 0.63967(17) 0.41428(9) 0.0550(3) Uani 1 1 d . . .
H2 H 0.6287 0.6710 0.4045 0.066 Uiso 1 1 calc R . .
O3 O 0.35059(8) 0.34405(16) 0.28909(8) 0.0512(3) Uani 1 1 d . . .
H3 H 0.3169 0.3205 0.2424 0.061 Uiso 1 1 calc R . .
O4 O 0.24931(8) 0.28664(19) 0.12461(8) 0.0570(4) Uani 1 1 d . . .
O5 O 0.29830(9) 0.40475(19) -0.03877(12) 0.0711(4) Uani 1 1 d . . .
O6 O 0.18344(10) 0.57331(16) -0.07899(9) 0.0574(3) Uani 1 1 d . . .
O7 O -0.14001(11) 0.3163(2) -0.13207(12) 0.0878(6) Uani 1 1 d . . .
O8 O -0.18121(9) 0.12893(19) -0.04179(11) 0.0688(4) Uani 1 1 d . . .
O9 O 0.03334(15) 0.0024(3) 0.21693(12) 0.1019(7) Uani 1 1 d . . .
O10 O 0.16027(16) 0.1419(3) 0.25606(12) 0.1097(8) Uani 1 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1 O1 1.415(2) . ?
C1 C2 1.513(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N1 1.498(2) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 O2 1.411(2) . ?
C3 C4 1.500(2) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N1 1.4999(19) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O3 1.411(2) . ?
C5 C6 1.495(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N1 1.5068(19) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 O4 1.2498(18) . ?
C7 C12 1.441(2) . ?
C7 C8 1.446(2) . ?
C8 C9 1.368(2) . ?
C8 N2 1.458(2) . ?
C9 C10 1.385(2) . ?
C9 H9 0.9300 . ?
C10 C11 1.375(2) . ?
C10 N3 1.4474(19) . ?
C11 C12 1.370(2) . ?
C11 H11 0.9300 . ?
C12 N4 1.457(2) . ?
N1 H1C 0.845(14) . ?
N2 O5 1.2142(18) . ?
N2 O6 1.2239(19) . ?
N3 O7 1.226(2) . ?
N3 O8 1.230(2) . ?
N4 O10 1.206(2) . ?
N4 O9 1.209(2) . ?
O1 H1 0.8200 . ?
O2 H2 0.8200 . ?
O3 H3 0.8200 . ?

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
O1 C1 C2 110.93(14) . . ?
O1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.0 . . ?
N1 C2 C1 109.03(15) . . ?
N1 C2 H2A 109.9 . . ?
C1 C2 H2A 109.9 . . ?
N1 C2 H2B 109.9 . . ?
C1 C2 H2B 109.9 . . ?
H2A C2 H2B 108.3 . . ?
O2 C3 C4 107.74(14) . . ?
O2 C3 H3A 110.2 . . ?
C4 C3 H3A 110.2 . . ?
O2 C3 H3B 110.2 . . ?
C4 C3 H3B 110.2 . . ?
H3A C3 H3B 108.5 . . ?
N1 C4 C3 112.33(13) . . ?
N1 C4 H4A 109.1 . . ?
C3 C4 H4A 109.1 . . ?
N1 C4 H4B 109.1 . . ?
C3 C4 H4B 109.1 . . ?
H4A C4 H4B 107.9 . . ?
O3 C5 C6 110.63(14) . . ?
O3 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
O3 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
C5 C6 N1 111.26(13) . . ?
C5 C6 H6A 109.4 . . ?
N1 C6 H6A 109.4 . . ?
C5 C6 H6B 109.4 . . ?
N1 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
O4 C7 C12 125.83(15) . . ?
O4 C7 C8 122.62(15) . . ?
C12 C7 C8 111.54(12) . . ?
C9 C8 C7 125.16(14) . . ?
C9 C8 N2 116.06(14) . . ?
C7 C8 N2 118.75(13) . . ?
C8 C9 C10 118.19(15) . . ?
C8 C9 H9 120.9 . . ?
C10 C9 H9 120.9 . . ?
C11 C10 C9 121.31(13) . . ?
C11 C10 N3 119.11(15) . . ?
C9 C10 N3 119.53(15) . . ?
C12 C11 C10 119.62(15) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C11 C12 C7 124.01(15) . . ?
C11 C12 N4 116.26(15) . . ?
C7 C12 N4 119.72(14) . . ?
C2 N1 C4 114.21(13) . . ?
C2 N1 C6 111.64(12) . . ?
C4 N1 C6 110.63(12) . . ?
C2 N1 H1C 105.4(12) . . ?
C4 N1 H1C 106.4(12) . . ?
C6 N1 H1C 108.1(12) . . ?
O5 N2 O6 122.83(15) . . ?
O5 N2 C8 119.11(14) . . ?
O6 N2 C8 118.02(13) . . ?
O7 N3 O8 123.86(15) . . ?
O7 N3 C10 117.37(17) . . ?
O8 N3 C10 118.77(17) . . ?
O10 N4 O9 121.80(18) . . ?
O10 N4 C12 119.60(17) . . ?
O9 N4 C12 118.59(16) . . ?
C1 O1 H1 109.5 . . ?
C3 O2 H2 109.5 . . ?
C5 O3 H3 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 N1 -50.58(19) . . . . ?
O2 C3 C4 N1 -58.0(2) . . . . ?
O3 C5 C6 N1 -61.67(18) . . . . ?
O4 C7 C8 C9 -179.73(16) . . . . ?
C12 C7 C8 C9 -0.3(2) . . . . ?
O4 C7 C8 N2 -1.7(2) . . . . ?
C12 C7 C8 N2 177.71(13) . . . . ?
C7 C8 C9 C10 -3.1(2) . . . . ?
N2 C8 C9 C10 178.81(14) . . . . ?
C8 C9 C10 C11 3.5(2) . . . . ?
C8 C9 C10 N3 -179.17(14) . . . . ?
C9 C10 C11 C12 -0.3(2) . . . . ?
N3 C10 C11 C12 -177.68(15) . . . . ?
C10 C11 C12 C7 -3.5(3) . . . . ?
C10 C11 C12 N4 177.56(15) . . . . ?
O4 C7 C12 C11 -176.91(16) . . . . ?
C8 C7 C12 C11 3.7(2) . . . . ?
O4 C7 C12 N4 2.0(3) . . . . ?
C8 C7 C12 N4 -177.42(15) . . . . ?
C1 C2 N1 C4 151.83(13) . . . . ?
C1 C2 N1 C6 -81.74(16) . . . . ?
C3 C4 N1 C2 -67.65(19) . . . . ?
C3 C4 N1 C6 165.39(15) . . . . ?
C5 C6 N1 C2 151.14(14) . . . . ?
C5 C6 N1 C4 -80.50(16) . . . . ?
C9 C8 N2 O5 -139.57(17) . . . . ?
C7 C8 N2 O5 42.2(2) . . . . ?
C9 C8 N2 O6 38.4(2) . . . . ?
C7 C8 N2 O6 -139.80(15) . . . . ?
C11 C10 N3 O7 168.87(18) . . . . ?
C9 C10 N3 O7 -8.5(2) . . . . ?
C11 C10 N3 O8 -10.3(2) . . . . ?
C9 C10 N3 O8 172.29(16) . . . . ?
C11 C12 N4 O10 -163.8(2) . . . . ?
C7 C12 N4 O10 17.2(3) . . . . ?
C11 C12 N4 O9 15.4(3) . . . . ?
C7 C12 N4 O9 -163.6(2) . . . . ?

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
O1 H1 O3 0.82 1.94 2.7542(17) 172.2 2_655
O2 H2 O4 0.82 1.98 2.7938(17) 168.9 2_655
O3 H3 O4 0.82 1.92 2.7354(16) 171.9 .

_diffrn_measured_fraction_theta_max 0.849
_diffrn_reflns_theta_full        32.33
_diffrn_measured_fraction_theta_full 0.849
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.047
_database_code_depnum_ccdc_archive 'CCDC 877861'
