# Electronic Supplementary Material (ESI) for Chemical Communications.
# 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_1op
_database_code_depnum_ccdc_archive 'CCDC 1040381'
_audit_update_record             
;
2014-12-19 deposited with the CCDC.
2015-04-17 downloaded from the CCDC.
;

#=============================================================================
_audit_creation_method           'SHELXL-2014/6, manual editing plus enCIFer'
_audit_creation_date             '19 december 2014'
#=============================================================================

#============================================================================
# start Validation Reply Form

# Alerts level A
_vrf_RINTA01_1op                 
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: The only available crystal for study was not single being instead
a small agglomerate of crystals. In this context, diffraction was very poor,
especially at high angles, for a resolution above ca. 1 A, even for very long
exposure times. In this context, the Rint value is significantly high, even
though the structural model refined to good agreement factors. 
;

_vrf_PLAT020_1op                 
;
PROBLEM: The value of Rint is greater than 0.12
RESPONSE: Please see our response to _vrf_RINTA01. 
;


# Alerts level B
_vrf_PLAT043_1op                 
;
PROBLEM: Calculated and Reported Mol. Weight Differ
RESPONSE: The hydrogen atoms associated with the water molecules could not
be located from difference Fourier maps. They have been, nevertheless, 
added to the empirical formula of the compound, hence the Alert. 
;

_vrf_PLAT306_1op                 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?)
RESPONSE: Please see our response to _vrf_PLAT043 and _vrf_PLAT430.
;

_vrf_PLAT430_1op                 
;
PROBLEM: Short Inter D...A Contact
RESPONSE: The absence of hydrogen atoms associated with the water molecules
of crystallization and coordinated led to the presence of a series of this
type of alert. These correspond to hydrogen bonds between water molecules
and between water molecules and the 1D polymer present in the crystal 
structure.
;


# Alerts level C
_vrf_CHEMW03_1op                 
;
PROBLEM: The ratio of given/expected molecular weight 
RESPONSE: Please see our response to _vrf_PLAT043 and _vrf_PLAT430.
;

_vrf_PLAT041_1op                 
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ
RESPONSE: Please see our response to _vrf_PLAT043 and _vrf_PLAT430.
;

_vrf_PLAT044_1op                 
;
PROBLEM: Calculated and Reported Density Dx  Differ
RESPONSE: Please see our response to _vrf_PLAT043 and _vrf_PLAT430.
;

_vrf_PLAT068_1op                 
;
PROBLEM: Reported F000 Differs from Calcd (or Missing)
RESPONSE: Please see our response to _vrf_PLAT043 and _vrf_PLAT430.
;

_vrf_PLAT202_1op                 
;
PROBLEM: Isotropic non-H Atoms in Anion/Solvent 
RESPONSE: All water molecules of crystallization have been refined using
isotropic displacement parameters (independent for each location).
;

# end Validation Reply Form
#=============================================================================


#=============================================================================
# GENERAL AND CHEMICAL DATA
#=============================================================================

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C6 H18 La2 O22 P6), 9(H2 O)'
_chemical_formula_sum            'C12 H78 La4 N4 O53 P12'
_chemical_formula_weight         2054.06

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'
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'
P P 0.1023 0.0942 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


#=============================================================================
# CRYSTAL DATA
#=============================================================================

_space_group_crystal_system      Monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   14.274(4)
_cell_length_b                   18.624(5)
_cell_length_c                   12.530(4)
_cell_angle_alpha                90
_cell_angle_beta                 115.140(12)
_cell_angle_gamma                90
_cell_volume                     3015.3(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    7502
_cell_measurement_theta_min      2.84
_cell_measurement_theta_max      27.43

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.262
_exptl_crystal_F_000             2020
_exptl_transmission_factor_min   0.4192
_exptl_transmission_factor_max   0.7456
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    3.217
_shelx_estimated_absorpt_T_min   0.783
_shelx_estimated_absorpt_T_max   0.969
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
; 
 SADABS V2012/1 (Bruker AXS Inc.) 
;

#=============================================================================
# EXPERIMENTAL DATA
#============================================================================= 

_exptl_special_details           
;
 ?
;
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Sealed tube'
_diffrn_radiation_monochromator  'Multi-layer X-ray mirror'
_diffrn_measurement_device_type  'Bruker D8 QUEST '
_diffrn_measurement_method       'ω / φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            42667
_diffrn_reflns_av_unetI/netI     0.1986
_diffrn_reflns_av_R_equivalents  0.2947
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.592
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             5510
_reflns_number_gt                2925
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX2 2012.4 (Bruker AXS Inc., 2012)'
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_structure_solution    'SHELXS (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2014)'


#=============================================================================
# REFINEMENT DATA
#=============================================================================

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0381P)²+21.7999P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5510
_refine_ls_number_parameters     371
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1757
_refine_ls_R_factor_gt           0.0754
_refine_ls_wR_factor_ref         0.1464
_refine_ls_wR_factor_gt          0.1177
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


#=============================================================================
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
#=============================================================================

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.38277(6) 0.57044(5) 0.49526(7) 0.0197(2) Uani 1 1 d . . . . .
O1W O 0.2443(7) 0.6483(6) 0.3169(9) 0.038(3) Uani 1 1 d . . . . .
O2W O 0.4261(8) 0.7122(5) 0.5180(9) 0.033(3) Uani 1 1 d . . . . .
La2 La 0.07485(6) 0.47916(5) 0.38855(7) 0.0221(2) Uani 1 1 d . . . . .
O3W O 0.0743(7) 0.5690(7) 0.2209(8) 0.045(3) Uani 1 1 d . . . . .
O4W O -0.0336(7) 0.4296(7) 0.1775(8) 0.048(3) Uani 1 1 d . . . . .
P1 P 0.4750(3) 0.6312(2) 0.8201(3) 0.0246(10) Uani 1 1 d . . . . .
P2 P 0.1587(3) 0.6065(2) 0.5866(3) 0.0228(9) Uani 1 1 d . . . . .
P3 P 0.1761(3) 0.4181(2) 0.7100(3) 0.0233(9) Uani 1 1 d . . . . .
P4 P 0.4729(3) 0.4052(2) 0.6887(3) 0.0226(9) Uani 1 1 d . . . . .
P5 P 0.3209(3) 0.4150(2) 0.3551(3) 0.0237(10) Uani 1 1 d . . . . .
P6 P 0.0985(3) 0.2730(2) 0.4128(4) 0.0323(11) Uani 1 1 d . . . . .
O1 O 0.4313(7) 0.6216(5) 0.6873(8) 0.028(2) Uani 1 1 d . . . . .
O2 O 0.4481(7) 0.7020(5) 0.8587(8) 0.029(2) Uani 1 1 d . . . . .
O3 O 0.5942(7) 0.6173(7) 0.8841(9) 0.042(3) Uani 1 1 d . . . . .
H3 H 0.6161 0.6046 0.8345 0.063 Uiso 1 1 calc R U . . .
O4 O 0.2148(6) 0.5775(5) 0.5174(8) 0.022(2) Uani 1 1 d . . . . .
O5 O 0.0595(7) 0.5633(5) 0.5506(8) 0.026(2) Uani 1 1 d . . . . .
O6 O 0.1415(7) 0.6875(5) 0.5770(8) 0.028(2) Uani 1 1 d . . . . .
O7 O 0.1855(6) 0.4274(5) 0.5945(7) 0.023(2) Uani 1 1 d . . . . .
O8 O 0.0811(7) 0.4443(5) 0.7143(8) 0.026(2) Uani 1 1 d . . . . .
O9 O 0.2001(7) 0.3385(5) 0.7528(9) 0.028(2) Uani 1 1 d . . . . .
H9 H 0.1652 0.3271 0.7899 0.042 Uiso 1 1 calc R U . . .
O10 O 0.4018(6) 0.4688(5) 0.6375(7) 0.022(2) Uani 1 1 d . . . . .
O11 O 0.5592(7) 0.3954(5) 0.6539(8) 0.027(2) Uani 1 1 d . . . . .
O12 O 0.5139(7) 0.4046(6) 0.8275(7) 0.027(2) Uani 1 1 d . . . . .
H12 H 0.5789 0.4044 0.8588 0.040 Uiso 1 1 calc R U . . .
O13 O 0.2447(7) 0.4657(5) 0.3733(7) 0.025(2) Uani 1 1 d . . . . .
O14 O 0.4265(6) 0.4491(5) 0.4171(8) 0.022(2) Uani 1 1 d . . . . .
O15 O 0.2935(7) 0.3947(5) 0.2277(8) 0.032(3) Uani 1 1 d . . . . .
O16 O 0.0896(7) 0.3486(6) 0.3715(8) 0.035(3) Uani 1 1 d . . . . .
O17 O 0.0340(8) 0.2581(6) 0.4843(10) 0.044(3) Uani 1 1 d . . . . .
H17 H 0.0731 0.2420 0.5511 0.066 Uiso 1 1 calc R U . . .
O18 O 0.0736(8) 0.2142(6) 0.3183(9) 0.047(3) Uani 1 1 d . . . . .
N1 N 0.3164(8) 0.5332(6) 0.7810(9) 0.024(3) Uani 1 1 d . . . . .
H1 H 0.3267 0.5201 0.7094 0.028 Uiso 1 1 calc R U . . .
N2 N 0.2991(8) 0.3265(6) 0.5331(9) 0.024(3) Uani 1 1 d . . . . .
H2 H 0.2589 0.3706 0.5322 0.029 Uiso 1 1 calc R U . . .
C1 C 0.4216(10) 0.5587(8) 0.8749(11) 0.022(3) Uani 1 1 d . U . . .
H1A H 0.4706 0.5179 0.8991 0.026 Uiso 1 1 calc R U . . .
H1B H 0.4132 0.5755 0.9453 0.026 Uiso 1 1 calc R U . . .
C2 C 0.2400(10) 0.5921(7) 0.7468(11) 0.018(3) Uani 1 1 d . U . . .
H2A H 0.2776 0.6373 0.7798 0.022 Uiso 1 1 calc R U . . .
H2B H 0.1930 0.5834 0.7852 0.022 Uiso 1 1 calc R U . . .
C3 C 0.2855(11) 0.4663(8) 0.8234(12) 0.031(4) Uani 1 1 d . U . . .
H3A H 0.2671 0.4789 0.8889 0.037 Uiso 1 1 calc R U . . .
H3B H 0.3459 0.4337 0.8553 0.037 Uiso 1 1 calc R U . . .
C4 C 0.3931(10) 0.3242(8) 0.6499(12) 0.030(4) Uani 1 1 d . U . . .
H4A H 0.4368 0.2832 0.6491 0.036 Uiso 1 1 calc R U . . .
H4B H 0.3697 0.3150 0.7126 0.036 Uiso 1 1 calc R U . . .
C5 C 0.3205(11) 0.3286(8) 0.4268(12) 0.027(4) Uani 1 1 d . U . . .
H5A H 0.2688 0.2974 0.3665 0.032 Uiso 1 1 calc R U . . .
H5B H 0.3890 0.3061 0.4485 0.032 Uiso 1 1 calc R U . . .
C6 C 0.2307(11) 0.2620(8) 0.5235(13) 0.033(4) Uani 1 1 d . U . . .
H6A H 0.2298 0.2535 0.6010 0.040 Uiso 1 1 calc R U . . .
H6B H 0.2611 0.2190 0.5038 0.040 Uiso 1 1 calc R U . . .
O5W O 0.2884(7) 0.5941(6) 0.0433(8) 0.038(3) Uiso 1 1 d . . . . .
O6W O 0.6912(8) 0.2755(6) 0.8364(9) 0.042(3) Uiso 1 1 d . . . . .
O7W O 0.8718(9) 0.2537(7) 0.6371(10) 0.060(4) Uiso 1 1 d . . . . .
O8W O 0.1502(15) 0.4967(11) 0.0569(16) 0.055(6) Uiso 0.667 1 d . . P . .
O9W O 0.113(2) 0.5253(19) 0.039(3) 0.031(8) Uiso 0.333 1 d . . P . .
O10W O 0.0900(15) 0.3755(12) 0.0818(18) 0.042(6) Uiso 0.5 1 d . . P . .


_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.
;

#=============================================================================
# GEOMETRY
#============================================================================= 

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 O1 2.400(9) . ?
La1 O11 2.429(9) 3_666 ?
La1 O14 2.492(8) 3_666 ?
La1 O4 2.532(8) . ?
La1 O10 2.534(9) . ?
La1 O14 2.642(9) . ?
La1 O1W 2.693(9) . ?
La1 O2W 2.699(10) . ?
La1 O13 2.733(9) . ?
La1 P5 3.306(4) . ?
La1 La1 4.2144(18) 3_666 ?
La2 O16 2.458(11) . ?
La2 O5 2.475(8) 3_566 ?
La2 O8 2.493(9) 3_566 ?
La2 O13 2.524(9) . ?
La2 O7 2.573(8) . ?
La2 O4W 2.601(10) . ?
La2 O5 2.647(9) . ?
La2 O3W 2.682(10) . ?
La2 O4 2.685(9) . ?
La2 P2 3.269(4) . ?
P1 O2 1.510(10) . ?
P1 O1 1.520(9) . ?
P1 O3 1.564(10) . ?
P1 C1 1.822(14) . ?
P2 O4 1.508(9) . ?
P2 O5 1.520(10) . ?
P2 O6 1.525(10) . ?
P2 C2 1.863(13) . ?
P3 O8 1.463(9) . ?
P3 O7 1.518(9) . ?
P3 O9 1.565(10) . ?
P3 C3 1.838(15) . ?
P4 O11 1.482(9) . ?
P4 O10 1.515(10) . ?
P4 O12 1.582(9) . ?
P4 C4 1.826(15) . ?
P5 O14 1.511(9) . ?
P5 O15 1.520(9) . ?
P5 O13 1.529(10) . ?
P5 C5 1.843(15) . ?
P6 O16 1.485(11) . ?
P6 O18 1.540(11) . ?
P6 O17 1.557(10) . ?
P6 C6 1.818(15) . ?
O3 H3 0.8400 . ?
O5 La2 2.475(8) 3_566 ?
O8 La2 2.493(9) 3_566 ?
O9 H9 0.8400 . ?
O11 La1 2.429(9) 3_666 ?
O12 H12 0.8400 . ?
O14 La1 2.492(8) 3_666 ?
O17 H17 0.8400 . ?
N1 C2 1.476(16) . ?
N1 C3 1.492(18) . ?
N1 C1 1.537(16) . ?
N1 H1 1.0000 . ?
N2 C5 1.488(16) . ?
N2 C4 1.508(17) . ?
N2 C6 1.520(17) . ?
N2 H2 1.0000 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
O8W O9W 0.72(3) . ?

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 La1 O11 128.3(3) . 3_666 ?
O1 La1 O14 79.6(3) . 3_666 ?
O11 La1 O14 73.2(3) 3_666 3_666 ?
O1 La1 O4 75.7(3) . . ?
O11 La1 O4 136.0(3) 3_666 . ?
O14 La1 O4 150.2(3) 3_666 . ?
O1 La1 O10 72.1(3) . . ?
O11 La1 O10 140.1(3) 3_666 . ?
O14 La1 O10 79.1(3) 3_666 . ?
O4 La1 O10 77.6(3) . . ?
O1 La1 O14 134.3(3) . . ?
O11 La1 O14 74.2(3) 3_666 . ?
O14 La1 O14 69.7(3) 3_666 . ?
O4 La1 O14 118.0(3) . . ?
O10 La1 O14 69.5(3) . . ?
O1 La1 O1W 114.6(3) . . ?
O11 La1 O1W 65.8(3) 3_666 . ?
O14 La1 O1W 136.3(3) 3_666 . ?
O4 La1 O1W 70.6(3) . . ?
O10 La1 O1W 143.9(3) . . ?
O14 La1 O1W 111.0(3) . . ?
O1 La1 O2W 63.2(3) . . ?
O11 La1 O2W 71.8(3) 3_666 . ?
O14 La1 O2W 86.4(3) 3_666 . ?
O4 La1 O2W 97.1(3) . . ?
O10 La1 O2W 134.8(3) . . ?
O14 La1 O2W 142.8(3) . . ?
O1W La1 O2W 67.4(3) . . ?
O1 La1 O13 132.6(3) . . ?
O11 La1 O13 99.0(3) 3_666 . ?
O14 La1 O13 122.4(3) 3_666 . ?
O4 La1 O13 66.8(3) . . ?
O10 La1 O13 72.3(3) . . ?
O14 La1 O13 53.8(3) . . ?
O1W La1 O13 79.6(3) . . ?
O2W La1 O13 146.7(3) . . ?
O1 La1 P5 141.1(2) . . ?
O11 La1 P5 85.5(2) 3_666 . ?
O14 La1 P5 95.8(2) 3_666 . ?
O4 La1 P5 93.0(2) . . ?
O10 La1 P5 69.2(2) . . ?
O14 La1 P5 26.54(19) . . ?
O1W La1 P5 95.4(2) . . ?
O2W La1 P5 155.6(2) . . ?
O13 La1 P5 27.3(2) . . ?
O1 La1 La1 109.4(2) . 3_666 ?
O11 La1 La1 70.0(2) 3_666 3_666 ?
O14 La1 La1 36.0(2) 3_666 3_666 ?
O4 La1 La1 143.8(2) . 3_666 ?
O10 La1 La1 70.66(19) . 3_666 ?
O14 La1 La1 33.68(18) . 3_666 ?
O1W La1 La1 130.7(2) . 3_666 ?
O2W La1 La1 117.6(2) . 3_666 ?
O13 La1 La1 86.9(2) . 3_666 ?
P5 La1 La1 59.96(6) . 3_666 ?
O16 La2 O5 79.4(3) . 3_566 ?
O16 La2 O8 127.7(3) . 3_566 ?
O5 La2 O8 72.7(3) 3_566 3_566 ?
O16 La2 O13 77.0(3) . . ?
O5 La2 O13 152.4(3) 3_566 . ?
O8 La2 O13 133.9(3) 3_566 . ?
O16 La2 O7 71.2(3) . . ?
O5 La2 O7 78.3(3) 3_566 . ?
O8 La2 O7 140.0(3) 3_566 . ?
O13 La2 O7 80.7(3) . . ?
O16 La2 O4W 66.2(3) . . ?
O5 La2 O4W 89.7(3) 3_566 . ?
O8 La2 O4W 70.2(3) 3_566 . ?
O13 La2 O4W 93.7(3) . . ?
O7 La2 O4W 137.2(3) . . ?
O16 La2 O5 133.7(3) . . ?
O5 La2 O5 68.0(4) 3_566 . ?
O8 La2 O5 73.2(3) 3_566 . ?
O13 La2 O5 120.8(3) . . ?
O7 La2 O5 70.6(3) . . ?
O4W La2 O5 141.5(3) . . ?
O16 La2 O3W 121.4(3) . . ?
O5 La2 O3W 134.1(3) 3_566 . ?
O8 La2 O3W 62.2(3) 3_566 . ?
O13 La2 O3W 71.7(3) . . ?
O7 La2 O3W 144.6(3) . . ?
O4W La2 O3W 67.8(4) . . ?
O5 La2 O3W 104.9(3) . . ?
O16 La2 O4 131.1(3) . . ?
O5 La2 O4 120.6(3) 3_566 . ?
O8 La2 O4 101.2(3) 3_566 . ?
O13 La2 O4 67.7(3) . . ?
O7 La2 O4 70.7(3) . . ?
O4W La2 O4 145.4(3) . . ?
O5 La2 O4 54.4(3) . . ?
O3W La2 O4 78.4(3) . . ?
O16 La2 P2 140.0(2) . . ?
O5 La2 P2 94.6(2) 3_566 . ?
O8 La2 P2 86.3(2) 3_566 . ?
O13 La2 P2 94.4(2) . . ?
O7 La2 P2 68.9(2) . . ?
O4W La2 P2 153.8(3) . . ?
O5 La2 P2 27.3(2) . . ?
O3W La2 P2 91.2(3) . . ?
O4 La2 P2 27.14(19) . . ?
O2 P1 O1 114.3(6) . . ?
O2 P1 O3 110.5(6) . . ?
O1 P1 O3 113.1(5) . . ?
O2 P1 C1 108.8(6) . . ?
O1 P1 C1 106.4(6) . . ?
O3 P1 C1 102.9(6) . . ?
O4 P2 O5 107.2(5) . . ?
O4 P2 O6 114.5(5) . . ?
O5 P2 O6 113.7(5) . . ?
O4 P2 C2 109.1(5) . . ?
O5 P2 C2 108.6(6) . . ?
O6 P2 C2 103.5(6) . . ?
O4 P2 La2 54.3(4) . . ?
O5 P2 La2 52.9(3) . . ?
O6 P2 La2 131.5(4) . . ?
C2 P2 La2 125.0(4) . . ?
O8 P3 O7 117.1(5) . . ?
O8 P3 O9 112.0(5) . . ?
O7 P3 O9 109.8(6) . . ?
O8 P3 C3 107.7(6) . . ?
O7 P3 C3 107.0(6) . . ?
O9 P3 C3 102.0(6) . . ?
O11 P4 O10 117.6(5) . . ?
O11 P4 O12 110.9(5) . . ?
O10 P4 O12 109.8(5) . . ?
O11 P4 C4 108.8(6) . . ?
O10 P4 C4 107.7(6) . . ?
O12 P4 C4 100.6(6) . . ?
O14 P5 O15 113.6(5) . . ?
O14 P5 O13 106.3(5) . . ?
O15 P5 O13 115.3(5) . . ?
O14 P5 C5 109.0(6) . . ?
O15 P5 C5 104.0(6) . . ?
O13 P5 C5 108.5(6) . . ?
O14 P5 La1 51.4(3) . . ?
O15 P5 La1 131.8(4) . . ?
O13 P5 La1 55.0(4) . . ?
C5 P5 La1 124.1(5) . . ?
O16 P6 O18 116.7(6) . . ?
O16 P6 O17 112.7(6) . . ?
O18 P6 O17 108.4(7) . . ?
O16 P6 C6 106.3(6) . . ?
O18 P6 C6 109.3(7) . . ?
O17 P6 C6 102.5(7) . . ?
P1 O1 La1 162.5(6) . . ?
P1 O3 H3 109.5 . . ?
P2 O4 La1 147.2(5) . . ?
P2 O4 La2 98.5(4) . . ?
La1 O4 La2 113.3(3) . . ?
P2 O5 La2 145.4(5) . 3_566 ?
P2 O5 La2 99.8(4) . . ?
La2 O5 La2 112.0(4) 3_566 . ?
P3 O7 La2 137.1(5) . . ?
P3 O8 La2 144.0(5) . 3_566 ?
P3 O9 H9 109.5 . . ?
P4 O10 La1 137.3(5) . . ?
P4 O11 La1 142.4(6) . 3_666 ?
P4 O12 H12 109.5 . . ?
P5 O13 La2 147.1(6) . . ?
P5 O13 La1 97.7(4) . . ?
La2 O13 La1 112.0(3) . . ?
P5 O14 La1 146.0(5) . 3_666 ?
P5 O14 La1 102.1(4) . . ?
La1 O14 La1 110.3(3) 3_666 . ?
P6 O16 La2 154.8(6) . . ?
P6 O17 H17 109.5 . . ?
C2 N1 C3 115.5(10) . . ?
C2 N1 C1 110.7(10) . . ?
C3 N1 C1 109.0(10) . . ?
C2 N1 H1 107.1 . . ?
C3 N1 H1 107.1 . . ?
C1 N1 H1 107.1 . . ?
C5 N2 C4 115.7(11) . . ?
C5 N2 C6 108.6(11) . . ?
C4 N2 C6 109.3(11) . . ?
C5 N2 H2 107.6 . . ?
C4 N2 H2 107.6 . . ?
C6 N2 H2 107.6 . . ?
N1 C1 P1 111.7(9) . . ?
N1 C1 H1A 109.3 . . ?
P1 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
P1 C1 H1B 109.3 . . ?
H1A C1 H1B 107.9 . . ?
N1 C2 P2 117.7(9) . . ?
N1 C2 H2A 107.9 . . ?
P2 C2 H2A 107.9 . . ?
N1 C2 H2B 107.9 . . ?
P2 C2 H2B 107.9 . . ?
H2A C2 H2B 107.2 . . ?
N1 C3 P3 114.5(9) . . ?
N1 C3 H3A 108.6 . . ?
P3 C3 H3A 108.6 . . ?
N1 C3 H3B 108.6 . . ?
P3 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
N2 C4 P4 115.6(10) . . ?
N2 C4 H4A 108.4 . . ?
P4 C4 H4A 108.4 . . ?
N2 C4 H4B 108.4 . . ?
P4 C4 H4B 108.4 . . ?
H4A C4 H4B 107.4 . . ?
N2 C5 P5 120.3(10) . . ?
N2 C5 H5A 107.3 . . ?
P5 C5 H5A 107.3 . . ?
N2 C5 H5B 107.3 . . ?
P5 C5 H5B 107.3 . . ?
H5A C5 H5B 106.9 . . ?
N2 C6 P6 113.2(10) . . ?
N2 C6 H6A 108.9 . . ?
P6 C6 H6A 108.9 . . ?
N2 C6 H6B 108.9 . . ?
P6 C6 H6B 108.9 . . ?
H6A C6 H6B 107.7 . . ?

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 P1 O1 La1 -172.6(17) . . . . ?
O3 P1 O1 La1 60(2) . . . . ?
C1 P1 O1 La1 -52(2) . . . . ?
O5 P2 O4 La1 -164.2(9) . . . . ?
O6 P2 O4 La1 68.7(11) . . . . ?
C2 P2 O4 La1 -46.8(11) . . . . ?
La2 P2 O4 La1 -166.6(11) . . . . ?
O5 P2 O4 La2 2.4(5) . . . . ?
O6 P2 O4 La2 -124.7(5) . . . . ?
C2 P2 O4 La2 119.8(5) . . . . ?
O4 P2 O5 La2 154.6(9) . . . 3_566 ?
O6 P2 O5 La2 -77.8(11) . . . 3_566 ?
C2 P2 O5 La2 36.8(12) . . . 3_566 ?
La2 P2 O5 La2 157.0(12) . . . 3_566 ?
O4 P2 O5 La2 -2.5(5) . . . . ?
O6 P2 O5 La2 125.1(5) . . . . ?
C2 P2 O5 La2 -120.3(5) . . . . ?
O8 P3 O7 La2 -0.2(11) . . . . ?
O9 P3 O7 La2 128.9(8) . . . . ?
C3 P3 O7 La2 -121.1(8) . . . . ?
O7 P3 O8 La2 -14.7(13) . . . 3_566 ?
O9 P3 O8 La2 -142.8(9) . . . 3_566 ?
C3 P3 O8 La2 105.8(10) . . . 3_566 ?
O11 P4 O10 La1 1.7(10) . . . . ?
O12 P4 O10 La1 129.8(7) . . . . ?
C4 P4 O10 La1 -121.5(8) . . . . ?
O10 P4 O11 La1 -19.3(12) . . . 3_666 ?
O12 P4 O11 La1 -146.8(9) . . . 3_666 ?
C4 P4 O11 La1 103.4(10) . . . 3_666 ?
O14 P5 O13 La2 -152.8(8) . . . . ?
O15 P5 O13 La2 80.4(10) . . . . ?
C5 P5 O13 La2 -35.8(11) . . . . ?
La1 P5 O13 La2 -155.0(11) . . . . ?
O14 P5 O13 La1 2.1(5) . . . . ?
O15 P5 O13 La1 -124.7(5) . . . . ?
C5 P5 O13 La1 119.2(5) . . . . ?
O15 P5 O14 La1 -71.9(11) . . . 3_666 ?
O13 P5 O14 La1 160.3(8) . . . 3_666 ?
C5 P5 O14 La1 43.5(11) . . . 3_666 ?
La1 P5 O14 La1 162.5(11) . . . 3_666 ?
O15 P5 O14 La1 125.6(5) . . . . ?
O13 P5 O14 La1 -2.2(5) . . . . ?
C5 P5 O14 La1 -119.0(5) . . . . ?
O18 P6 O16 La2 163.1(12) . . . . ?
O17 P6 O16 La2 36.8(16) . . . . ?
C6 P6 O16 La2 -74.8(15) . . . . ?
C2 N1 C1 P1 -61.5(12) . . . . ?
C3 N1 C1 P1 170.4(9) . . . . ?
O2 P1 C1 N1 96.3(10) . . . . ?
O1 P1 C1 N1 -27.3(11) . . . . ?
O3 P1 C1 N1 -146.5(9) . . . . ?
C3 N1 C2 P2 -101.6(12) . . . . ?
C1 N1 C2 P2 133.9(9) . . . . ?
O4 P2 C2 N1 -24.8(12) . . . . ?
O5 P2 C2 N1 91.7(10) . . . . ?
O6 P2 C2 N1 -147.2(10) . . . . ?
La2 P2 C2 N1 34.5(12) . . . . ?
C2 N1 C3 P3 67.0(13) . . . . ?
C1 N1 C3 P3 -167.6(9) . . . . ?
O8 P3 C3 N1 -91.8(10) . . . . ?
O7 P3 C3 N1 34.9(12) . . . . ?
O9 P3 C3 N1 150.2(9) . . . . ?
C5 N2 C4 P4 67.3(14) . . . . ?
C6 N2 C4 P4 -169.7(10) . . . . ?
O11 P4 C4 N2 -95.7(11) . . . . ?
O10 P4 C4 N2 32.7(12) . . . . ?
O12 P4 C4 N2 147.7(10) . . . . ?
C4 N2 C5 P5 -96.9(13) . . . . ?
C6 N2 C5 P5 139.8(10) . . . . ?
O14 P5 C5 N2 84.8(11) . . . . ?
O15 P5 C5 N2 -153.7(10) . . . . ?
O13 P5 C5 N2 -30.5(12) . . . . ?
La1 P5 C5 N2 29.2(13) . . . . ?
C5 N2 C6 P6 -71.9(13) . . . . ?
C4 N2 C6 P6 161.0(10) . . . . ?
O16 P6 C6 N2 -7.5(12) . . . . ?
O18 P6 C6 N2 119.2(11) . . . . ?
O17 P6 C6 N2 -125.9(10) . . . . ?

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
O3 H3 O15 0.84 1.77 2.548(13) 153.4 3_666
O9 H9 O18 0.84 1.68 2.480(14) 158.4 4_566
O12 H12 O5W 0.84 1.77 2.589(13) 166.0 3_666
O17 H17 O10W 0.84 2.22 2.74(2) 120.1 4_566
N1 H1 O4 1.00 2.49 3.102(14) 118.9 .
N1 H1 O10 1.00 1.92 2.832(13) 150.1 .
N2 H2 O7 1.00 1.88 2.796(15) 151.4 .
N2 H2 O13 1.00 2.61 3.164(15) 115.2 .
C1 H1A O12 0.99 2.47 3.315(17) 143.0 .
C1 H1B O12 0.99 2.61 3.507(15) 150.9 3_667
C1 H1B O5W 0.99 2.58 3.451(16) 146.7 1_556
C2 H2A O2 0.99 2.51 3.384(16) 146.7 .
C2 H2B O4W 0.99 2.52 3.480(16) 162.9 3_566
C3 H3B O12 0.99 2.62 3.437(17) 139.5 .
C4 H4A O2 0.99 2.26 3.247(17) 171.2 2_646
C5 H5B O2W 0.99 2.51 3.466(16) 161.4 3_666
C6 H6A O9 0.99 2.64 3.398(18) 133.1 .

_refine_diff_density_max         1.318
_refine_diff_density_min         -1.071
_refine_diff_density_rms         0.246
_shelxl_version_number           2014/6

#=============================================================================
#   SHELXL Ins File
#=============================================================================

