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

#######################################################################
#
#                 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_dyida_0m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'Dysprosium iminodiacetato nitrate hydrate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H10 Dy N3 O12'
_chemical_formula_sum            'C4 H10 Dy N3 O12'
_chemical_formula_weight         454.65

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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.9728(17)
_cell_length_b                   8.7556(19)
_cell_length_c                   9.748(2)
_cell_angle_alpha                66.953(2)
_cell_angle_beta                 88.290(2)
_cell_angle_gamma                73.131(2)
_cell_volume                     596.5(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5149
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      29.36

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             434
_exptl_absorpt_coefficient_mu    6.337
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.5168
_exptl_absorpt_correction_T_max  0.7023
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD'
_diffrn_measurement_method       'Omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4671
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.65
_diffrn_reflns_theta_max         26.00
_reflns_number_total             2265
_reflns_number_gt                2224
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_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)+(0.0654P)²+10.9246P] 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         2265
_refine_ls_number_parameters     187
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0456
_refine_ls_wR_factor_ref         0.1223
_refine_ls_wR_factor_gt          0.1219
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.772
_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
Dy1 Dy -0.07833(8) -0.98091(7) 0.24364(6) 0.0144(3) Uani 1 1 d . . .
O2 O -0.1310(15) -0.7630(14) 0.3267(13) 0.026(2) Uani 1 1 d . . .
N1 N -0.2831(16) -0.4196(15) 0.2194(14) 0.017(2) Uani 1 1 d . . .
H1A H -0.3579 -0.3162 0.2103 0.021 Uiso 1 1 calc R . .
H1B H -0.3477 -0.4856 0.2122 0.021 Uiso 1 1 calc R . .
O1 O -0.1521(15) -0.1572(14) 0.1579(13) 0.028(2) Uani 1 1 d D . .
O4 O 0.0060(16) -0.2169(16) -0.0432(14) 0.032(3) Uani 1 1 d D . .
O5 O 0.2111(16) -1.1522(16) 0.1945(15) 0.031(3) Uani 1 1 d . . .
O6 O 0.2240(16) -0.9881(17) 0.3098(15) 0.034(3) Uani 1 1 d . . .
O7 O -0.3421(16) -0.7981(16) 0.0868(13) 0.032(3) Uani 1 1 d D . .
H7A H -0.42(2) -0.72(2) 0.12(3) 0.048 Uiso 1 1 d D . .
H7B H -0.34(3) -0.74(3) -0.012(6) 0.048 Uiso 1 1 d D . .
O8 O 0.0188(17) -1.2175(16) 0.4593(14) 0.036(3) Uani 1 1 d . . .
O11 O -0.3258(16) -1.0178(18) 0.3847(14) 0.038(3) Uani 1 1 d D . .
H11A H -0.2953 -1.1322 0.4387 0.058 Uiso 1 1 d D . .
H11B H -0.4011 -1.0473 0.3401 0.058 Uiso 1 1 d D . .
C12 C -0.106(2) -0.7003(18) 0.4152(17) 0.019(3) Uani 1 1 d . . .
C1 C -0.183(2) -0.506(2) 0.3693(17) 0.025(3) Uani 1 1 d . . .
H11 H -0.2609 -0.4841 0.4425 0.029 Uiso 1 1 calc R . .
H12 H -0.0890 -0.4559 0.3681 0.029 Uiso 1 1 calc R . .
C2 C -0.167(2) -0.3906(19) 0.0929(16) 0.026(4) Uani 1 1 d D . .
H21 H -0.0683 -0.4948 0.1154 0.031 Uiso 1 1 calc R . .
H22 H -0.2338 -0.3696 0.0021 0.031 Uiso 1 1 calc R . .
O14 O -0.5600(18) -0.5416(17) 0.1625(14) 0.035(3) Uani 1 1 d . . .
N3 N 0.3044(18) -1.0925(18) 0.2514(17) 0.029(3) Uani 1 1 d . . .
O13 O 0.4639(17) -1.129(2) 0.248(2) 0.052(4) Uani 1 1 d . . .
N4 N -0.627(2) -0.590(2) 0.2869(18) 0.034(3) Uani 1 1 d . . .
O15 O -0.545(2) -0.602(3) 0.3970(19) 0.060(5) Uani 1 1 d . . .
O16 O -0.764(3) -0.623(3) 0.297(3) 0.087(7) Uani 1 1 d . . .
C3 C -0.1013(19) -0.2413(17) 0.0673(15) 0.015(3) Uani 1 1 d 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
Dy1 O8 2.251(12) . ?
Dy1 O1 2.235(11) 1_545 ?
Dy1 O2 2.279(11) . ?
Dy1 O4 2.239(11) 2_545 ?
Dy1 O7 2.376(11) . ?
Dy1 O11 2.397(12) . ?
Dy1 O6 2.491(12) . ?
Dy1 O5 2.508(12) . ?
Dy1 N3 2.915(14) . ?
O2 C12 1.24(2) . ?
N1 C1 1.482(19) . ?
N1 C2 1.503(19) . ?
O1 C3 1.342(18) . ?
O1 Dy1 2.235(11) 1_565 ?
O4 C3 1.345(18) . ?
O4 Dy1 2.239(11) 2_545 ?
O5 N3 1.269(19) . ?
O6 N3 1.272(18) . ?
O8 C12 1.25(2) 2_536 ?
C12 O8 1.25(2) 2_536 ?
C12 C1 1.51(2) . ?
C2 C3 1.478(18) . ?
O14 N4 1.27(2) . ?
N3 O13 1.220(19) . ?
N4 O16 1.20(2) . ?
N4 O15 1.23(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
O8 Dy1 O1 86.1(5) . 1_545 ?
O8 Dy1 O2 101.1(5) . . ?
O1 Dy1 O2 155.3(4) 1_545 . ?
O8 Dy1 O4 146.6(5) . 2_545 ?
O1 Dy1 O4 105.0(4) 1_545 2_545 ?
O2 Dy1 O4 81.9(4) . 2_545 ?
O8 Dy1 O7 140.8(5) . . ?
O1 Dy1 O7 77.0(4) 1_545 . ?
O2 Dy1 O7 82.9(4) . . ?
O4 Dy1 O7 72.6(4) 2_545 . ?
O8 Dy1 O11 71.9(5) . . ?
O1 Dy1 O11 82.0(4) 1_545 . ?
O2 Dy1 O11 78.0(4) . . ?
O4 Dy1 O11 140.0(5) 2_545 . ?
O7 Dy1 O11 70.9(4) . . ?
O8 Dy1 O6 74.7(5) . . ?
O1 Dy1 O6 127.3(4) 1_545 . ?
O2 Dy1 O6 77.3(4) . . ?
O4 Dy1 O6 73.6(5) 2_545 . ?
O7 Dy1 O6 142.7(5) . . ?
O11 Dy1 O6 133.3(4) . . ?
O8 Dy1 O5 75.1(5) . . ?
O1 Dy1 O5 76.5(4) 1_545 . ?
O2 Dy1 O5 128.1(4) . . ?
O4 Dy1 O5 77.1(4) 2_545 . ?
O7 Dy1 O5 132.3(4) . . ?
O11 Dy1 O5 141.5(4) . . ?
O6 Dy1 O5 51.4(4) . . ?
O8 Dy1 N3 73.9(5) . . ?
O1 Dy1 N3 102.0(4) 1_545 . ?
O2 Dy1 N3 102.7(4) . . ?
O4 Dy1 N3 73.0(4) 2_545 . ?
O7 Dy1 N3 143.9(4) . . ?
O11 Dy1 N3 145.3(4) . . ?
O6 Dy1 N3 25.7(4) . . ?
O5 Dy1 N3 25.7(4) . . ?
C12 O2 Dy1 153.3(10) . . ?
C1 N1 C2 113.4(12) . . ?
C3 O1 Dy1 141.9(10) . 1_565 ?
C3 O4 Dy1 145.2(10) . 2_545 ?
N3 O5 Dy1 95.4(9) . . ?
N3 O6 Dy1 96.2(9) . . ?
C12 O8 Dy1 152.9(11) 2_536 . ?
O2 C12 O8 126.1(14) . 2_536 ?
O2 C12 C1 118.3(13) . . ?
O8 C12 C1 115.6(14) 2_536 . ?
N1 C1 C12 111.8(12) . . ?
C3 C2 N1 112.0(11) . . ?
O13 N3 O5 122.5(15) . . ?
O13 N3 O6 120.5(16) . . ?
O5 N3 O6 117.0(13) . . ?
O13 N3 Dy1 176.0(13) . . ?
O5 N3 Dy1 58.9(8) . . ?
O6 N3 Dy1 58.1(8) . . ?
O16 N4 O15 121.2(19) . . ?
O16 N4 O14 121.5(19) . . ?
O15 N4 O14 117.3(16) . . ?
O4 C3 O1 131.0(13) . . ?
O4 C3 C2 112.5(12) . . ?
O1 C3 C2 116.5(12) . . ?

_diffrn_measured_fraction_theta_max 0.966
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.966
_refine_diff_density_max         3.959
_refine_diff_density_min         -2.801
_refine_diff_density_rms         0.288
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_database_code_depnum_ccdc_archive 'CCDC 1018502'
#######################################################################
#
#                 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_laidac

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'lanthanum iminodiacetato nitrate iminodiacetate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H38 La2 N6 O31'
_chemical_formula_sum            'C12 H38 La2 N6 O31'
_chemical_formula_weight         1040.30

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

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Cmcm

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

_cell_length_a                   18.835(8)
_cell_length_b                   9.133(4)
_cell_length_c                   19.034(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3274(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2814
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      27.01

_exptl_crystal_description       needle
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2056
_exptl_absorpt_coefficient_mu    2.698
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6144
_exptl_absorpt_correction_T_max  0.8336
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART Apex-2 CCD'
_diffrn_measurement_method       'Omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12628
_diffrn_reflns_av_R_equivalents  0.0860
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.48
_diffrn_reflns_theta_max         26.00
_reflns_number_total             1675
_reflns_number_gt                1107
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_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)+(0.0338P)²+1.6184P] 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         1675
_refine_ls_number_parameters     166
_refine_ls_number_restraints     109
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0321
_refine_ls_wR_factor_ref         0.0740
_refine_ls_wR_factor_gt          0.0679
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.026
_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
La1 La 0.264693(18) 0.5000 0.5000 0.02023(13) Uani 1 2 d SDU . .
O1 O 0.15366(19) 0.4337(4) 0.42952(19) 0.0353(8) Uani 1 1 d DU . .
H102 H 0.169(2) 0.387(5) 0.392(2) 0.042 Uiso 1 1 d D . .
H101 H 0.112(2) 0.479(5) 0.443(2) 0.042 Uiso 1 1 d D . .
O2 O 0.22363(17) 0.2702(3) 0.56499(17) 0.0270(8) Uani 1 1 d U . .
O3 O 0.3035(2) 0.4259(3) 0.37301(15) 0.0321(8) Uani 1 1 d U . .
O4 O 0.3784(2) 0.3628(4) 0.5347(2) 0.0486(10) Uani 1 1 d DU . .
H4A H 0.375(2) 0.275(4) 0.523(3) 0.058 Uiso 1 1 d D . .
H4B H 0.414(2) 0.428(5) 0.550(3) 0.058 Uiso 1 1 d D . .
N1 N 0.1974(3) 0.2152(5) 0.7500 0.0224(11) Uani 1 2 d SU . .
H1A H 0.1606 0.1523 0.7500 0.027 Uiso 1 2 calc SR . .
H1B H 0.2377 0.1623 0.7500 0.027 Uiso 1 2 calc SR . .
C1 C 0.2051(3) 0.2082(5) 0.6222(2) 0.0237(9) Uani 1 1 d U . .
C2 C 0.1946(3) 0.3047(5) 0.6856(2) 0.0276(11) Uani 1 1 d U . .
H2A H 0.2315 0.3788 0.6870 0.033 Uiso 1 1 calc R . .
H2B H 0.1491 0.3538 0.6825 0.033 Uiso 1 1 calc R . .
O8 O 0.0000 0.3177(12) 0.7500 0.113(5) Uani 1 4 d SU . .
O11 O 0.5000 0.4870(9) 0.5970(5) 0.094(3) Uani 1 2 d SD . .
H11A H 0.517(5) 0.565(6) 0.575(4) 0.113 Uiso 1 1 d D . .
O5 O 0.0000 0.4911(9) 0.4165(6) 0.106(3) Uani 1 2 d SU . .
N3 N 0.0000 0.6252(10) 0.4213(4) 0.0522(18) Uani 1 2 d SU . .
O7 O 0.0559(4) 0.1198(9) 0.7500 0.097(3) Uani 1 2 d SU . .
O6 O -0.0569(2) 0.6865(7) 0.4238(3) 0.0859(16) Uani 1 1 d U . .
N2 N 0.0000 0.1919(14) 0.7500 0.066(3) Uani 1 4 d SU . .
O9 O 0.3768(6) 0.2414(16) 0.6908(7) 0.108(5) Uani 0.50 1 d PU . 1
O10 O 0.3337(4) 0.1391(8) 0.7850(4) 0.0419(18) Uani 0.50 1 d PU . 1
C3 C 0.4471(8) 0.2480(18) 0.7883(9) 0.084(5) Uani 0.50 1 d PDU . 1
H3B H 0.465(4) 0.144(4) 0.790(6) 0.100 Uiso 0.50 1 d PD A 1
H3C H 0.415(9) 0.308(16) 0.838(9) 0.100 Uiso 0.50 1 d P B 1
C4 C 0.3805(4) 0.2077(9) 0.7500 0.0381(17) Uani 1 2 d SU . 1
N4 N 0.5000 0.3203(10) 0.7500 0.051(3) Uani 1 4 d SDU . 1
H4C H 0.5000 0.417(2) 0.7500 0.061 Uiso 1 4 d SD C 1


_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
La1 O2 2.556(3) . ?
La1 O2 2.556(3) 4_566 ?
La1 O1 2.557(3) . ?
La1 O1 2.557(3) 4_566 ?
La1 O4 2.567(4) 4_566 ?
La1 O4 2.567(4) . ?
La1 O3 2.614(3) 4_566 ?
La1 O3 2.614(3) . ?
La1 O2 2.769(3) 16 ?
La1 O2 2.769(3) 13_556 ?
La1 C1 3.057(4) 16 ?
La1 C1 3.057(4) 13_556 ?
O2 C1 1.276(5) . ?
O2 La1 2.769(3) 13_556 ?
O3 C1 1.239(5) 13_556 ?
N1 C2 1.475(5) 10_557 ?
N1 C2 1.475(5) . ?
C1 O3 1.239(5) 13_556 ?
C1 C2 1.507(6) . ?
C1 La1 3.057(4) 13_556 ?
O8 N2 1.149(15) . ?
O5 N3 1.228(9) . ?
N3 O6 1.210(6) 12 ?
N3 O6 1.210(6) . ?
O7 N2 1.242(9) . ?
N2 O7 1.242(9) 3_556 ?
O9 C4 1.170(11) . ?
O9 O10 1.321(12) 10_557 ?
O9 C3 1.384(18) 10_557 ?
O10 C4 1.271(9) . ?
O10 O9 1.321(13) 10_557 ?
O10 O10 1.333(14) 10_557 ?
C3 O9 1.384(18) 10_557 ?
C3 N4 1.400(13) . ?
C3 C3 1.46(3) 10_557 ?
C3 C4 1.496(16) . ?
C3 C3 1.99(3) 12_655 ?
C4 O9 1.170(11) 10_557 ?
C4 O10 1.271(9) 10_557 ?
C4 C3 1.496(16) 10_557 ?
N4 C3 1.400(13) 12_655 ?
N4 C3 1.400(13) 10_557 ?
N4 C3 1.400(13) 3_656 ?

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
O2 La1 O2 144.77(15) . 4_566 ?
O2 La1 O1 79.16(11) . . ?
O2 La1 O1 72.13(11) 4_566 . ?
O2 La1 O1 72.13(11) . 4_566 ?
O2 La1 O1 79.16(11) 4_566 4_566 ?
O1 La1 O1 70.28(18) . 4_566 ?
O2 La1 O4 141.06(12) . 4_566 ?
O2 La1 O4 74.16(12) 4_566 4_566 ?
O1 La1 O4 131.50(14) . 4_566 ?
O1 La1 O4 134.53(12) 4_566 4_566 ?
O2 La1 O4 74.16(12) . . ?
O2 La1 O4 141.06(12) 4_566 . ?
O1 La1 O4 134.53(12) . . ?
O1 La1 O4 131.50(14) 4_566 . ?
O4 La1 O4 66.99(19) 4_566 . ?
O2 La1 O3 81.34(11) . 4_566 ?
O2 La1 O3 108.64(10) 4_566 4_566 ?
O1 La1 O3 140.79(12) . 4_566 ?
O1 La1 O3 71.48(12) 4_566 4_566 ?
O4 La1 O3 83.02(13) 4_566 4_566 ?
O4 La1 O3 69.83(13) . 4_566 ?
O2 La1 O3 108.64(10) . . ?
O2 La1 O3 81.34(11) 4_566 . ?
O1 La1 O3 71.47(12) . . ?
O1 La1 O3 140.79(12) 4_566 . ?
O4 La1 O3 69.83(13) 4_566 . ?
O4 La1 O3 83.02(13) . . ?
O3 La1 O3 147.54(16) 4_566 . ?
O2 La1 O2 122.65(12) . 16 ?
O2 La1 O2 60.56(12) 4_566 16 ?
O1 La1 O2 120.69(10) . 16 ?
O1 La1 O2 67.64(11) 4_566 16 ?
O4 La1 O2 67.27(12) 4_566 16 ?
O4 La1 O2 104.71(11) . 16 ?
O3 La1 O2 48.26(10) 4_566 16 ?
O3 La1 O2 128.42(10) . 16 ?
O2 La1 O2 60.56(12) . 13_556 ?
O2 La1 O2 122.65(12) 4_566 13_556 ?
O1 La1 O2 67.64(11) . 13_556 ?
O1 La1 O2 120.69(10) 4_566 13_556 ?
O4 La1 O2 104.71(11) 4_566 13_556 ?
O4 La1 O2 67.27(12) . 13_556 ?
O3 La1 O2 128.42(10) 4_566 13_556 ?
O3 La1 O2 48.26(10) . 13_556 ?
O2 La1 O2 170.89(13) 16 13_556 ?
O2 La1 C1 101.47(11) . 16 ?
O2 La1 C1 85.05(11) 4_566 16 ?
O1 La1 C1 134.30(13) . 16 ?
O1 La1 C1 66.79(13) 4_566 16 ?
O4 La1 C1 74.75(13) 4_566 16 ?
O4 La1 C1 87.29(13) . 16 ?
O3 La1 C1 23.62(10) 4_566 16 ?
O3 La1 C1 144.31(11) . 16 ?
O2 La1 C1 24.66(10) 16 16 ?
O2 La1 C1 151.55(11) 13_556 16 ?
O2 La1 C1 85.05(11) . 13_556 ?
O2 La1 C1 101.47(11) 4_566 13_556 ?
O1 La1 C1 66.79(12) . 13_556 ?
O1 La1 C1 134.30(13) 4_566 13_556 ?
O4 La1 C1 87.29(13) 4_566 13_556 ?
O4 La1 C1 74.75(13) . 13_556 ?
O3 La1 C1 144.31(11) 4_566 13_556 ?
O3 La1 C1 23.62(10) . 13_556 ?
O2 La1 C1 151.55(11) 16 13_556 ?
O2 La1 C1 24.66(10) 13_556 13_556 ?
C1 La1 C1 158.56(18) 16 13_556 ?
C1 O2 La1 149.4(3) . . ?
C1 O2 La1 90.4(3) . 13_556 ?
La1 O2 La1 119.44(12) . 13_556 ?
C1 O3 La1 98.7(3) 13_556 . ?
C2 N1 C2 112.5(5) 10_557 . ?
O3 C1 O2 122.6(4) 13_556 . ?
O3 C1 C2 120.1(4) 13_556 . ?
O2 C1 C2 117.3(4) . . ?
O3 C1 La1 57.7(2) 13_556 13_556 ?
O2 C1 La1 64.9(2) . 13_556 ?
C2 C1 La1 175.6(3) . 13_556 ?
N1 C2 C1 109.7(4) . . ?
O6 N3 O6 124.7(10) 12 . ?
O6 N3 O5 117.7(5) 12 . ?
O6 N3 O5 117.7(5) . . ?
O8 N2 O7 122.0(6) . 3_556 ?
O8 N2 O7 122.0(6) . . ?
O7 N2 O7 115.9(13) 3_556 . ?
C4 O9 O10 61.0(7) . 10_557 ?
C4 O9 C3 71.2(10) . 10_557 ?
O10 O9 C3 121.3(11) 10_557 10_557 ?
C4 O10 O9 53.6(6) . 10_557 ?
C4 O10 O10 58.4(4) . 10_557 ?
O9 O10 O10 110.4(7) 10_557 10_557 ?
O9 C3 N4 148.4(15) 10_557 . ?
O9 C3 C3 106.7(9) 10_557 10_557 ?
N4 C3 C3 58.7(7) . 10_557 ?
O9 C3 C4 47.7(7) 10_557 . ?
N4 C3 C4 117.4(11) . . ?
C3 C3 C4 60.9(6) 10_557 . ?
O9 C3 C3 163.1(9) 10_557 12_655 ?
N4 C3 C3 44.6(7) . 12_655 ?
C3 C3 C3 90.000(10) 10_557 12_655 ?
C4 C3 C3 146.9(7) . 12_655 ?
O9 C4 O9 148.7(18) 10_557 . ?
O9 C4 O10 65.4(7) 10_557 . ?
O9 C4 O10 126.4(10) . . ?
O9 C4 O10 126.4(10) 10_557 10_557 ?
O9 C4 O10 65.4(7) . 10_557 ?
O10 C4 O10 63.3(8) . 10_557 ?
O9 C4 C3 61.1(9) 10_557 . ?
O9 C4 C3 117.0(10) . . ?
O10 C4 C3 116.6(7) . . ?
O10 C4 C3 163.4(10) 10_557 . ?
O9 C4 C3 117.0(10) 10_557 10_557 ?
O9 C4 C3 61.1(9) . 10_557 ?
O10 C4 C3 163.4(10) . 10_557 ?
O10 C4 C3 116.6(7) 10_557 10_557 ?
C3 C4 C3 58.2(12) . 10_557 ?
C3 N4 C3 90.8(15) . 12_655 ?
C3 N4 C3 62.7(13) . 10_557 ?
C3 N4 C3 123.7(16) 12_655 10_557 ?
C3 N4 C3 123.7(16) . 3_656 ?
C3 N4 C3 62.7(13) 12_655 3_656 ?
C3 N4 C3 90.8(15) 10_557 3_656 ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.106
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_database_code_depnum_ccdc_archive 'CCDC 1018503'
