# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1003764'
_audit_update_record             
;
2015-07-23 deposited with the CCDC.
2015-11-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H9 O6 La1, (H2 O), (C3 H8 N O), (H2 O)'
_chemical_formula_sum            'C24 H20 N O9 La'
_chemical_formula_weight         605.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -1.4094 9.0376 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   Cc

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'

_cell_length_a                   18.4394(5)
_cell_length_b                   13.7828(3)
_cell_length_c                   8.1160(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.319(2)
_cell_angle_gamma                90.00
_cell_volume                     2060.96(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1000
_exptl_absorpt_coefficient_mu    16.366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2441
_exptl_absorpt_correction_T_max  0.3543
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5354
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         4.01
_diffrn_reflns_theta_max         66.84
_reflns_number_total             2453
_reflns_number_gt                2350
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0634P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.021(7)
_refine_ls_number_reflns         2453
_refine_ls_number_parameters     256
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0356
_refine_ls_wR_factor_ref         0.0917
_refine_ls_wR_factor_gt          0.0903
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.073
_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 0.6300(4) 0.5571(5) 0.4824(9) 0.0114(14) Uani 1 1 d . . .
La1 La 0.50125(3) 0.51709(2) 0.25533(4) 0.01050(14) Uani 1 1 d . . .
O1 O 0.5901(3) 0.4829(4) 0.5137(8) 0.0151(12) Uani 1 1 d . . .
O1W O 0.3636(3) 0.5503(5) 0.2506(7) 0.0204(12) Uani 1 1 d D . .
H1W H 0.3492 0.5426 0.3454 0.031 Uiso 1 1 d RD . .
H2W H 0.3317 0.5349 0.1803 0.031 Uiso 1 1 d RD . .
C2 C 0.6985(4) 0.5724(6) 0.5863(9) 0.0146(15) Uani 1 1 d . . .
O2 O 0.6136(3) 0.6134(4) 0.3671(6) 0.0156(11) Uani 1 1 d . . .
C3 C 0.7356(4) 0.4930(6) 0.6502(10) 0.0130(15) Uani 1 1 d . . .
H3 H 0.7172 0.4311 0.6298 0.016 Uiso 1 1 calc R . .
O3 O 0.9427(3) 0.0895(4) 0.9624(7) 0.0168(11) Uani 1 1 d . . .
C4 C 0.8009(4) 0.5038(6) 0.7458(11) 0.0162(16) Uani 1 1 d . . .
O4 O 0.9924(3) 0.1877(4) 1.1499(7) 0.0173(12) Uani 1 1 d . . .
C5 C 0.8412(4) 0.4202(6) 0.8083(10) 0.0141(15) Uani 1 1 d . . .
O5 O 1.0419(3) 0.8334(4) 1.2080(6) 0.0144(11) Uani 1 1 d . . .
C6 C 0.8210(4) 0.3254(6) 0.7693(10) 0.0160(16) Uani 1 1 d . . .
H6 H 0.7810 0.3164 0.6972 0.019 Uiso 1 1 calc R . .
O6 O 0.9630(3) 0.8930(4) 1.0206(6) 0.0130(11) Uani 1 1 d . . .
C7 C 0.8560(4) 0.2445(6) 0.8302(10) 0.0183(16) Uani 1 1 d . . .
H7 H 0.8408 0.1825 0.7998 0.022 Uiso 1 1 calc R . .
C8 C 0.9163(4) 0.2589(5) 0.9410(9) 0.0123(14) Uani 1 1 d . . .
C9 C 0.9528(4) 0.1737(5) 1.0208(9) 0.0128(15) Uani 1 1 d . . .
C10 C 0.9388(4) 0.3505(6) 0.9802(9) 0.0149(16) Uani 1 1 d . . .
H10 H 0.9785 0.3586 1.0535 0.018 Uiso 1 1 calc R . .
C11 C 0.9039(4) 0.4334(5) 0.9131(9) 0.0094(10) Uani 1 1 d U . .
C12 C 0.9313(4) 0.5315(5) 0.9492(11) 0.0138(16) Uani 1 1 d . . .
C13 C 0.9938(4) 0.5482(6) 1.0495(11) 0.0176(16) Uani 1 1 d . . .
H13 H 1.0206 0.4953 1.0887 0.021 Uiso 1 1 calc R . .
C14 C 1.0165(4) 0.6390(6) 1.0911(10) 0.0167(16) Uani 1 1 d . . .
H14 H 1.0581 0.6473 1.1582 0.020 Uiso 1 1 calc R . .
C15 C 0.9773(4) 0.7203(5) 1.0333(9) 0.0129(14) Uani 1 1 d . . .
C16 C 0.9960(4) 0.8204(5) 1.0914(9) 0.0127(15) Uani 1 1 d . . .
C17 C 0.9177(4) 0.7075(6) 0.9299(10) 0.0182(17) Uani 1 1 d . . .
H17 H 0.8930 0.7614 0.8876 0.022 Uiso 1 1 calc R . .
C18 C 0.8932(4) 0.6130(6) 0.8865(9) 0.0141(15) Uani 1 1 d . . .
C19 C 0.8273(4) 0.6016(5) 0.7812(9) 0.0094(10) Uani 1 1 d U . .
C20 C 0.7892(5) 0.6789(6) 0.7094(10) 0.0203(17) Uani 1 1 d . . .
H20 H 0.8068 0.7415 0.7260 0.024 Uiso 1 1 calc R . .
C21 C 0.7254(4) 0.6658(6) 0.6131(10) 0.0164(16) Uani 1 1 d . . .
H21 H 0.7010 0.7191 0.5674 0.020 Uiso 1 1 calc R . .


_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 O2 1.243(9) . ?
C1 O1 1.291(10) . ?
C1 C2 1.505(10) . ?
C1 La1 2.997(7) . ?
La1 O4 2.506(5) 3_454 ?
La1 O3 2.509(5) 4_454 ?
La1 O1W 2.578(5) . ?
La1 O2 2.594(5) . ?
La1 O1 2.606(6) 2_564 ?
La1 O6 2.606(5) 4_464 ?
La1 O6 2.635(5) 3_444 ?
La1 O1 2.651(6) . ?
La1 O5 2.672(5) 3_444 ?
La1 O3 2.758(6) 3_454 ?
La1 C9 2.991(8) 3_454 ?
O1 La1 2.606(6) 2_565 ?
O1W H1W 0.8308 . ?
O1W H2W 0.8300 . ?
C2 C3 1.380(11) . ?
C2 C21 1.393(11) . ?
C3 C4 1.413(12) . ?
C3 H3 0.9300 . ?
O3 C9 1.265(10) . ?
O3 La1 2.509(5) 4 ?
O3 La1 2.758(6) 3_546 ?
C4 C5 1.452(11) . ?
C4 C19 1.459(11) . ?
O4 C9 1.267(9) . ?
O4 La1 2.506(5) 3_546 ?
C5 C6 1.391(11) . ?
C5 C11 1.419(11) . ?
O5 C16 1.257(9) . ?
O5 La1 2.672(5) 3_556 ?
C6 C7 1.371(11) . ?
C6 H6 0.9300 . ?
O6 C16 1.293(9) . ?
O6 La1 2.606(5) 4_565 ?
O6 La1 2.635(5) 3_556 ?
C7 C8 1.415(12) . ?
C7 H7 0.9300 . ?
C8 C10 1.363(12) . ?
C8 C9 1.488(10) . ?
C9 La1 2.991(8) 3_546 ?
C10 C11 1.410(11) . ?
C10 H10 0.9300 . ?
C11 C12 1.468(11) . ?
C12 C13 1.402(12) . ?
C12 C18 1.410(11) . ?
C13 C14 1.358(12) . ?
C13 H13 0.9300 . ?
C14 C15 1.404(11) . ?
C14 H14 0.9300 . ?
C15 C17 1.367(11) . ?
C15 C16 1.493(11) . ?
C16 La1 3.020(8) 3_556 ?
C17 C18 1.419(11) . ?
C17 H17 0.9300 . ?
C18 C19 1.465(10) . ?
C19 C20 1.390(11) . ?
C20 C21 1.398(11) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?

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 C1 O1 121.3(7) . . ?
O2 C1 C2 120.4(7) . . ?
O1 C1 C2 118.2(7) . . ?
O2 C1 La1 59.4(4) . . ?
O1 C1 La1 62.1(4) . . ?
C2 C1 La1 175.1(5) . . ?
O4 La1 O3 138.97(18) 3_454 4_454 ?
O4 La1 O1W 77.14(19) 3_454 . ?
O3 La1 O1W 70.36(19) 4_454 . ?
O4 La1 O2 71.29(17) 3_454 . ?
O3 La1 O2 115.14(17) 4_454 . ?
O1W La1 O2 133.35(18) . . ?
O4 La1 O1 77.13(17) 3_454 2_564 ?
O3 La1 O1 143.60(17) 4_454 2_564 ?
O1W La1 O1 129.59(18) . 2_564 ?
O2 La1 O1 75.25(17) . 2_564 ?
O4 La1 O6 79.59(17) 3_454 4_464 ?
O3 La1 O6 65.62(17) 4_454 4_464 ?
O1W La1 O6 68.21(17) . 4_464 ?
O2 La1 O6 72.93(16) . 4_464 ?
O1 La1 O6 145.17(16) 2_564 4_464 ?
O4 La1 O6 110.54(17) 3_454 3_444 ?
O3 La1 O6 89.66(17) 4_454 3_444 ?
O1W La1 O6 82.54(17) . 3_444 ?
O2 La1 O6 140.51(16) . 3_444 ?
O1 La1 O6 67.30(17) 2_564 3_444 ?
O6 La1 O6 146.4(2) 4_464 3_444 ?
O4 La1 O1 117.83(16) 3_454 . ?
O3 La1 O1 68.59(18) 4_454 . ?
O1W La1 O1 128.33(19) . . ?
O2 La1 O1 49.82(16) . . ?
O1 La1 O1 102.01(19) 2_564 . ?
O6 La1 O1 67.07(17) 4_464 . ?
O6 La1 O1 126.51(16) 3_444 . ?
O4 La1 O5 148.77(17) 3_454 3_444 ?
O3 La1 O5 70.85(17) 4_454 3_444 ?
O1W La1 O5 116.59(18) . 3_444 ?
O2 La1 O5 108.10(16) . 3_444 ?
O1 La1 O5 72.77(16) 2_564 3_444 ?
O6 La1 O5 131.00(16) 4_464 3_444 ?
O6 La1 O5 49.41(16) 3_444 3_444 ?
O1 La1 O5 77.13(16) . 3_444 ?
O4 La1 O3 49.32(17) 3_454 3_454 ?
O3 La1 O3 128.7(2) 4_454 3_454 ?
O1W La1 O3 64.65(18) . 3_454 ?
O2 La1 O3 113.31(16) . 3_454 ?
O1 La1 O3 65.63(17) 2_564 3_454 ?
O6 La1 O3 115.49(16) 4_464 3_454 ?
O6 La1 O3 61.83(16) 3_444 3_454 ?
O1 La1 O3 162.60(17) . 3_454 ?
O5 La1 O3 108.74(16) 3_444 3_454 ?
O4 La1 C9 24.69(19) 3_454 3_454 ?
O3 La1 C9 136.34(18) 4_454 3_454 ?
O1W La1 C9 66.0(2) . 3_454 ?
O2 La1 C9 93.83(18) . 3_454 ?
O1 La1 C9 72.64(18) 2_564 3_454 ?
O6 La1 C9 95.65(17) 4_464 3_454 ?
O6 La1 C9 86.82(19) 3_444 3_454 ?
O1 La1 C9 142.28(18) . 3_454 ?
O5 La1 C9 132.13(18) 3_444 3_454 ?
O3 La1 C9 25.00(19) 3_454 3_454 ?
O4 La1 C1 94.37(19) 3_454 . ?
O3 La1 C1 92.73(19) 4_454 . ?
O1W La1 C1 137.00(19) . . ?
O2 La1 C1 24.35(19) . . ?
O1 La1 C1 87.50(18) 2_564 . ?
O6 La1 C1 68.79(18) 4_464 . ?
O6 La1 C1 138.26(18) 3_444 . ?
O1 La1 C1 25.5(2) . . ?
O5 La1 C1 92.48(18) 3_444 . ?
O3 La1 C1 137.41(19) 3_454 . ?
C9 La1 C1 117.8(2) 3_454 . ?
C1 O1 La1 121.9(5) . 2_565 ?
C1 O1 La1 92.4(4) . . ?
La1 O1 La1 102.00(19) 2_565 . ?
La1 O1W H1W 108.2 . . ?
La1 O1W H2W 129.4 . . ?
H1W O1W H2W 111.1 . . ?
C3 C2 C21 120.4(7) . . ?
C3 C2 C1 119.4(7) . . ?
C21 C2 C1 120.1(7) . . ?
C1 O2 La1 96.3(4) . . ?
C2 C3 C4 121.4(7) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C9 O3 La1 136.7(5) . 4 ?
C9 O3 La1 87.8(4) . 3_546 ?
La1 O3 La1 101.60(18) 4 3_546 ?
C3 C4 C5 121.4(8) . . ?
C3 C4 C19 118.4(7) . . ?
C5 C4 C19 120.2(7) . . ?
C9 O4 La1 99.6(4) . 3_546 ?
C6 C5 C11 117.5(7) . . ?
C6 C5 C4 122.5(7) . . ?
C11 C5 C4 120.0(7) . . ?
C16 O5 La1 93.4(4) . 3_556 ?
C7 C6 C5 124.3(7) . . ?
C7 C6 H6 117.9 . . ?
C5 C6 H6 117.9 . . ?
C16 O6 La1 126.7(4) . 4_565 ?
C16 O6 La1 94.2(4) . 3_556 ?
La1 O6 La1 102.41(17) 4_565 3_556 ?
C6 C7 C8 117.5(7) . . ?
C6 C7 H7 121.2 . . ?
C8 C7 H7 121.2 . . ?
C10 C8 C7 120.1(7) . . ?
C10 C8 C9 120.1(7) . . ?
C7 C8 C9 119.7(7) . . ?
O3 C9 O4 121.4(7) . . ?
O3 C9 C8 120.2(7) . . ?
O4 C9 C8 118.4(6) . . ?
O3 C9 La1 67.2(4) . 3_546 ?
O4 C9 La1 55.7(4) . 3_546 ?
C8 C9 La1 164.7(5) . 3_546 ?
C8 C10 C11 122.1(7) . . ?
C8 C10 H10 119.0 . . ?
C11 C10 H10 119.0 . . ?
C10 C11 C5 118.4(7) . . ?
C10 C11 C12 121.4(7) . . ?
C5 C11 C12 120.2(7) . . ?
C13 C12 C18 117.7(7) . . ?
C13 C12 C11 122.3(7) . . ?
C18 C12 C11 119.9(7) . . ?
C14 C13 C12 122.2(7) . . ?
C14 C13 H13 118.9 . . ?
C12 C13 H13 118.9 . . ?
C13 C14 C15 120.2(7) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C17 C15 C14 119.5(7) . . ?
C17 C15 C16 118.8(7) . . ?
C14 C15 C16 121.5(7) . . ?
O5 C16 O6 120.9(7) . . ?
O5 C16 C15 120.6(7) . . ?
O6 C16 C15 118.4(6) . . ?
O5 C16 La1 62.0(4) . 3_556 ?
O6 C16 La1 60.5(4) . 3_556 ?
C15 C16 La1 166.2(5) . 3_556 ?
C15 C17 C18 120.7(7) . . ?
C15 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C12 C18 C17 119.5(7) . . ?
C12 C18 C19 121.0(7) . . ?
C17 C18 C19 119.5(7) . . ?
C20 C19 C4 117.8(7) . . ?
C20 C19 C18 123.7(7) . . ?
C4 C19 C18 118.5(7) . . ?
C19 C20 C21 122.4(7) . . ?
C19 C20 H20 118.8 . . ?
C21 C20 H20 118.8 . . ?
C2 C21 C20 119.5(7) . . ?
C2 C21 H21 120.3 . . ?
C20 C21 H21 120.3 . . ?

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
O2 C1 La1 O4 -18.3(4) . . . 3_454 ?
O1 C1 La1 O4 158.0(4) . . . 3_454 ?
C2 C1 La1 O4 -107(6) . . . 3_454 ?
O2 C1 La1 O3 -157.9(4) . . . 4_454 ?
O1 C1 La1 O3 18.4(4) . . . 4_454 ?
C2 C1 La1 O3 113(6) . . . 4_454 ?
O2 C1 La1 O1W -94.1(5) . . . . ?
O1 C1 La1 O1W 82.2(5) . . . . ?
C2 C1 La1 O1W 177(6) . . . . ?
O1 C1 La1 O2 176.3(7) . . . . ?
C2 C1 La1 O2 -89(6) . . . . ?
O2 C1 La1 O1 58.6(4) . . . 2_564 ?
O1 C1 La1 O1 -125.1(4) . . . 2_564 ?
C2 C1 La1 O1 -30(6) . . . 2_564 ?
O2 C1 La1 O6 -95.4(4) . . . 4_464 ?
O1 C1 La1 O6 80.9(4) . . . 4_464 ?
C2 C1 La1 O6 176(6) . . . 4_464 ?
O2 C1 La1 O6 109.6(4) . . . 3_444 ?
O1 C1 La1 O6 -74.1(5) . . . 3_444 ?
C2 C1 La1 O6 21(6) . . . 3_444 ?
O2 C1 La1 O1 -176.3(7) . . . . ?
C2 C1 La1 O1 95(6) . . . . ?
O2 C1 La1 O5 131.2(4) . . . 3_444 ?
O1 C1 La1 O5 -52.5(4) . . . 3_444 ?
C2 C1 La1 O5 42(6) . . . 3_444 ?
O2 C1 La1 O3 9.7(6) . . . 3_454 ?
O1 C1 La1 O3 -174.0(4) . . . 3_454 ?
C2 C1 La1 O3 -79(6) . . . 3_454 ?
O2 C1 La1 C9 -10.3(5) . . . 3_454 ?
O1 C1 La1 C9 166.0(4) . . . 3_454 ?
C2 C1 La1 C9 -99(6) . . . 3_454 ?
O2 C1 O1 La1 -102.0(7) . . . 2_565 ?
C2 C1 O1 La1 79.9(7) . . . 2_565 ?
La1 C1 O1 La1 -105.7(4) . . . 2_565 ?
O2 C1 O1 La1 3.7(7) . . . . ?
C2 C1 O1 La1 -174.4(6) . . . . ?
O4 La1 O1 C1 -25.0(5) 3_454 . . . ?
O3 La1 O1 C1 -160.2(5) 4_454 . . . ?
O1W La1 O1 C1 -120.5(4) . . . . ?
O2 La1 O1 C1 -2.0(4) . . . . ?
O1 La1 O1 C1 56.7(4) 2_564 . . . ?
O6 La1 O1 C1 -88.5(4) 4_464 . . . ?
O6 La1 O1 C1 127.2(4) 3_444 . . . ?
O5 La1 O1 C1 125.6(5) 3_444 . . . ?
O3 La1 O1 C1 13.7(8) 3_454 . . . ?
C9 La1 O1 C1 -20.4(6) 3_454 . . . ?
O4 La1 O1 La1 98.3(2) 3_454 . . 2_565 ?
O3 La1 O1 La1 -36.86(17) 4_454 . . 2_565 ?
O1W La1 O1 La1 2.8(3) . . . 2_565 ?
O2 La1 O1 La1 121.3(3) . . . 2_565 ?
O1 La1 O1 La1 180.0(2) 2_564 . . 2_565 ?
O6 La1 O1 La1 34.75(16) 4_464 . . 2_565 ?
O6 La1 O1 La1 -109.51(19) 3_444 . . 2_565 ?
O5 La1 O1 La1 -111.09(19) 3_444 . . 2_565 ?
O3 La1 O1 La1 137.0(5) 3_454 . . 2_565 ?
C9 La1 O1 La1 102.9(3) 3_454 . . 2_565 ?
C1 La1 O1 La1 123.3(5) . . . 2_565 ?
O2 C1 C2 C3 -147.0(7) . . . . ?
O1 C1 C2 C3 31.1(10) . . . . ?
La1 C1 C2 C3 -61(6) . . . . ?
O2 C1 C2 C21 30.9(10) . . . . ?
O1 C1 C2 C21 -150.9(7) . . . . ?
La1 C1 C2 C21 117(6) . . . . ?
O1 C1 O2 La1 -3.8(8) . . . . ?
C2 C1 O2 La1 174.3(6) . . . . ?
O4 La1 O2 C1 160.7(5) 3_454 . . . ?
O3 La1 O2 C1 24.6(5) 4_454 . . . ?
O1W La1 O2 C1 110.7(5) . . . . ?
O1 La1 O2 C1 -118.2(5) 2_564 . . . ?
O6 La1 O2 C1 76.2(4) 4_464 . . . ?
O6 La1 O2 C1 -99.4(5) 3_444 . . . ?
O1 La1 O2 C1 2.1(4) . . . . ?
O5 La1 O2 C1 -52.3(5) 3_444 . . . ?
O3 La1 O2 C1 -172.9(4) 3_454 . . . ?
C9 La1 O2 C1 170.9(4) 3_454 . . . ?
C21 C2 C3 C4 0.9(12) . . . . ?
C1 C2 C3 C4 178.8(7) . . . . ?
C2 C3 C4 C5 -177.9(7) . . . . ?
C2 C3 C4 C19 2.2(12) . . . . ?
C3 C4 C5 C6 4.4(12) . . . . ?
C19 C4 C5 C6 -175.7(7) . . . . ?
C3 C4 C5 C11 -175.8(7) . . . . ?
C19 C4 C5 C11 4.1(11) . . . . ?
C11 C5 C6 C7 2.5(12) . . . . ?
C4 C5 C6 C7 -177.7(8) . . . . ?
C5 C6 C7 C8 0.6(12) . . . . ?
C6 C7 C8 C10 -1.8(11) . . . . ?
C6 C7 C8 C9 175.3(7) . . . . ?
La1 O3 C9 O4 -91.4(9) 4 . . . ?
La1 O3 C9 O4 13.2(7) 3_546 . . . ?
La1 O3 C9 C8 90.4(8) 4 . . . ?
La1 O3 C9 C8 -165.0(6) 3_546 . . . ?
La1 O3 C9 La1 -104.7(6) 4 . . 3_546 ?
La1 O4 C9 O3 -14.8(8) 3_546 . . . ?
La1 O4 C9 C8 163.4(6) 3_546 . . . ?
C10 C8 C9 O3 -165.6(7) . . . . ?
C7 C8 C9 O3 17.2(11) . . . . ?
C10 C8 C9 O4 16.1(10) . . . . ?
C7 C8 C9 O4 -161.0(7) . . . . ?
C10 C8 C9 La1 79(2) . . . 3_546 ?
C7 C8 C9 La1 -97.9(19) . . . 3_546 ?
C7 C8 C10 C11 -0.1(12) . . . . ?
C9 C8 C10 C11 -177.3(7) . . . . ?
C8 C10 C11 C5 3.3(11) . . . . ?
C8 C10 C11 C12 -176.5(7) . . . . ?
C6 C5 C11 C10 -4.3(10) . . . . ?
C4 C5 C11 C10 175.8(7) . . . . ?
C6 C5 C11 C12 175.5(7) . . . . ?
C4 C5 C11 C12 -4.3(10) . . . . ?
C10 C11 C12 C13 1.0(11) . . . . ?
C5 C11 C12 C13 -178.8(7) . . . . ?
C10 C11 C12 C18 -177.0(7) . . . . ?
C5 C11 C12 C18 3.2(11) . . . . ?
C18 C12 C13 C14 2.3(13) . . . . ?
C11 C12 C13 C14 -175.8(8) . . . . ?
C12 C13 C14 C15 -0.2(13) . . . . ?
C13 C14 C15 C17 -2.4(12) . . . . ?
C13 C14 C15 C16 173.2(8) . . . . ?
La1 O5 C16 O6 14.5(7) 3_556 . . . ?
La1 O5 C16 C15 -164.5(6) 3_556 . . . ?
La1 O6 C16 O5 94.2(7) 4_565 . . . ?
La1 O6 C16 O5 -14.7(7) 3_556 . . . ?
La1 O6 C16 C15 -86.8(7) 4_565 . . . ?
La1 O6 C16 C15 164.3(6) 3_556 . . . ?
La1 O6 C16 La1 108.9(4) 4_565 . . 3_556 ?
C17 C15 C16 O5 167.3(7) . . . . ?
C14 C15 C16 O5 -8.3(11) . . . . ?
C17 C15 C16 O6 -11.7(10) . . . . ?
C14 C15 C16 O6 172.7(7) . . . . ?
C17 C15 C16 La1 70(2) . . . 3_556 ?
C14 C15 C16 La1 -106(2) . . . 3_556 ?
C14 C15 C17 C18 2.9(11) . . . . ?
C16 C15 C17 C18 -172.8(7) . . . . ?
C13 C12 C18 C17 -1.8(11) . . . . ?
C11 C12 C18 C17 176.4(7) . . . . ?
C13 C12 C18 C19 -179.9(7) . . . . ?
C11 C12 C18 C19 -1.8(11) . . . . ?
C15 C17 C18 C12 -0.8(11) . . . . ?
C15 C17 C18 C19 177.4(7) . . . . ?
C3 C4 C19 C20 -4.2(11) . . . . ?
C5 C4 C19 C20 175.9(7) . . . . ?
C3 C4 C19 C18 177.3(7) . . . . ?
C5 C4 C19 C18 -2.6(11) . . . . ?
C12 C18 C19 C20 -176.9(8) . . . . ?
C17 C18 C19 C20 5.0(11) . . . . ?
C12 C18 C19 C4 1.5(10) . . . . ?
C17 C18 C19 C4 -176.6(7) . . . . ?
C4 C19 C20 C21 3.4(12) . . . . ?
C18 C19 C20 C21 -178.2(7) . . . . ?
C3 C2 C21 C20 -1.8(11) . . . . ?
C1 C2 C21 C20 -179.8(7) . . . . ?
C19 C20 C21 C2 -0.4(12) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        66.84
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.965
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.130

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.682 0.000 -0.026 273 128 ' '
2 0.182 0.500 -0.020 273 128 ' '
_platon_squeeze_details          
;
One DMF and one water molecules are highly disordered. 
Therefore, the SQUEEZE routine of PLATON was applied.
The final formula was calculated from the TGA combined 
with elemental analysis data.

;
# start Validation Reply Form



_vrf_CHEMW03_I                   
;

PROBLEM: The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.90 <> 1.10 
RESPONSE: This is a consequence of the use of SQUEEZE. 
The solvent is included in formula, but is not in the model. 
;


_vrf_DENSD01_I                   
;

PROBLEM: The ratio of the submitted crystal density and that
         calculated from the formula is outside 
         the range 0.90 <> 1.10 
RESPONSE: See SQUEEZE above.

;

_vrf_PLAT046_I                   
;

PROBLEM: Reported Z, MW and D(calc) are Inconsistent
RESPONSE: See SQUEEZE above.
;


# end Validation Reply Form
