 
data_dq0702a

# start Validation Reply Form
_vrf_PLAT430_dq0702a
;
PROBLEM: Short Inter D...A Contact O36      ..O42       .       1.97 Ang.  
RESPONSE: disordered water molecules
;
_vrf_PLAT043_dq0702a
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      74.59 Check 
RESPONSE: hydrogen atoms not modeled for ammonia or water
molecules
;
_vrf_PLAT112_dq0702a
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         I         96 %Fit  
RESPONSE: two independent molecules per cell with approximate body
centering.
;
_vrf_PLAT306_dq0702a
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O27 Check 
RESPONSE: hydrogen atoms not modeled on water molecules
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H42.50 La N9 O23.25 P4'
_chemical_formula_weight         947.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   11.7674(10)
_cell_length_b                   12.1610(10)
_cell_length_c                   28.605(3)
_cell_angle_alpha                83.764(2)
_cell_angle_beta                 80.941(2)
_cell_angle_gamma                78.3598(17)
_cell_volume                     3946.8(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    9780
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      34.28

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_F_000             1922
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.331
_shelx_estimated_absorpt_T_min   0.777
_shelx_estimated_absorpt_T_max   0.924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.29
_exptl_absorpt_correction_T_max  0.36
_exptl_absorpt_process_details   'SADABS v. 2014/3 (Bruker AXS, 2013)'
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Quest with CMOS detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            88909
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         2.170
_diffrn_reflns_theta_max         34.896
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             32144
_reflns_number_gt                24090
_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 V.2014.7-1 (Bruker AXS, 2014)'
_computing_cell_refinement       'APEX2 V.2014.7-1 (Bruker AXS, 2014)'
_computing_data_reduction        'SAINT, v. 8.34A (Bruker AXS, 2013)'
_computing_structure_solution    'SHELXS 2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL, v. 2014/7, (Bruker AXS, 2014)'
_computing_publication_material  'SHELXTL, v. 2014/7, (Bruker AXS, 2014)'
_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)+(0.0612P)²] 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         32144
_refine_ls_number_parameters     937
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0471
_refine_ls_wR_factor_ref         0.1314
_refine_ls_wR_factor_gt          0.1221
_refine_ls_goodness_of_fit_ref   1.243
_refine_ls_restrained_S_all      1.243
_refine_ls_shift/su_max          0.002
_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_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 0.65072(2) 0.66628(2) 0.14664(2) 0.00532(4) Uani 1 1 d . . . . .
La2 La 0.86392(2) 0.85130(2) 0.35114(2) 0.00482(4) Uani 1 1 d . . . . .
P1 P 0.41215(6) 0.90151(6) 0.15850(2) 0.00682(12) Uani 1 1 d . . . . .
P2 P 0.42528(6) 0.49355(6) 0.16543(2) 0.00739(12) Uani 1 1 d . . . . .
P3 P 0.86885(6) 0.41809(6) 0.17084(3) 0.00782(12) Uani 1 1 d . . . . .
P4 P 0.86582(6) 0.84093(6) 0.15371(2) 0.00669(12) Uani 1 1 d . . . . .
P5 P 0.64788(6) 0.67575(5) 0.34593(2) 0.00601(12) Uani 1 1 d . . . . .
P6 P 0.64674(6) 1.09970(5) 0.32384(2) 0.00704(12) Uani 1 1 d . . . . .
P7 P 1.08804(6) 1.02759(5) 0.33108(2) 0.00640(12) Uani 1 1 d . . . . .
P8 P 1.09858(6) 0.61053(5) 0.34383(2) 0.00656(12) Uani 1 1 d . . . . .
N1 N 0.51851(19) 0.79149(19) 0.07807(8) 0.0084(4) Uani 1 1 d . . . . .
N2 N 0.57381(19) 0.53776(18) 0.08384(8) 0.0084(4) Uani 1 1 d . . . . .
N3 N 0.82732(19) 0.54057(18) 0.08500(8) 0.0083(4) Uani 1 1 d . . . . .
N4 N 0.77639(19) 0.79536(19) 0.07589(8) 0.0081(4) Uani 1 1 d . . . . .
N5 N 0.73434(19) 0.72684(18) 0.42332(8) 0.0074(4) Uani 1 1 d . . . . .
N6 N 0.68485(19) 0.98250(18) 0.41157(8) 0.0079(4) Uani 1 1 d . . . . .
N7 N 0.93783(19) 0.98329(18) 0.41273(8) 0.0072(4) Uani 1 1 d . . . . .
N8 N 0.99162(19) 0.72850(18) 0.42218(8) 0.0070(4) Uani 1 1 d . . . . .
N9 N 0.5157(2) 0.16373(19) 0.19427(9) 0.0119(4) Uani 1 1 d . . . . .
N10 N 0.3305(2) 0.8120(2) 0.29556(9) 0.0125(4) Uani 1 1 d . . . . .
N11 N 0.1822(2) 0.7000(2) 0.20991(9) 0.0134(5) Uani 1 1 d . . . . .
N12 N 0.63189(19) 0.90134(19) 0.24582(8) 0.0093(4) Uani 1 1 d . . . . .
N13 N 0.88124(19) 0.61485(18) 0.25323(8) 0.0088(4) Uani 1 1 d . . . . .
N14 N 0.9991(2) 0.35481(19) 0.30305(9) 0.0125(4) Uani 1 1 d . . . . .
N15 N 0.3236(2) 0.1845(2) 0.32557(9) 0.0135(5) Uani 1 1 d . . . . .
N16 N 0.1879(2) 0.3471(2) 0.16522(9) 0.0153(5) Uani 1 1 d . . . . .
N17 N 0.5893(2) 0.3995(2) 0.26367(9) 0.0132(5) Uani 1 1 d . . . . .
N18 N 0.9253(2) 0.1180(2) 0.23196(9) 0.0136(5) Uani 1 1 d . . . . .
O1 O 0.57887(17) 0.66890(16) 0.24021(7) 0.0113(4) Uani 1 1 d . . . . .
O2 O 0.53344(16) 0.84380(15) 0.17073(7) 0.0094(4) Uani 1 1 d . . . . .
O3 O 0.40156(17) 1.02869(15) 0.15008(7) 0.0109(4) Uani 1 1 d . . . . .
O4 O 0.31211(17) 0.87154(17) 0.19560(7) 0.0128(4) Uani 1 1 d . . . . .
O5 O 0.47158(16) 0.59167(15) 0.17998(7) 0.0089(3) Uani 1 1 d . . . . .
O6 O 0.30155(16) 0.53006(16) 0.15268(7) 0.0112(4) Uani 1 1 d . . . . .
O7 O 0.43160(16) 0.39283(16) 0.20232(7) 0.0105(4) Uani 1 1 d . . . . .
O8 O 0.74715(16) 0.48694(15) 0.18610(7) 0.0108(4) Uani 1 1 d . . . . .
O9 O 0.86673(18) 0.29678(16) 0.16284(8) 0.0144(4) Uani 1 1 d . . . . .
O10 O 0.95655(16) 0.42230(15) 0.20442(7) 0.0096(4) Uani 1 1 d . . . . .
O11 O 0.80246(16) 0.74372(15) 0.17500(7) 0.0084(3) Uani 1 1 d . . . . .
O12 O 0.82991(16) 0.94263(15) 0.18370(7) 0.0087(3) Uani 1 1 d . . . . .
O13 O 0.99838(16) 0.80366(16) 0.14626(7) 0.0114(4) Uani 1 1 d . . . . .
O14 O 0.93898(17) 0.84560(16) 0.25832(7) 0.0109(4) Uani 1 1 d . . . . .
O15 O 0.71099(16) 0.77278(15) 0.32442(7) 0.0079(3) Uani 1 1 d . . . . .
O16 O 0.68459(16) 0.57330(15) 0.31619(7) 0.0085(3) Uani 1 1 d . . . . .
O17 O 0.51493(16) 0.71216(16) 0.35358(7) 0.0103(4) Uani 1 1 d . . . . .
O18 O 0.76514(16) 1.02481(16) 0.30866(7) 0.0108(4) Uani 1 1 d . . . . .
O19 O 0.55546(16) 1.09787(16) 0.29148(7) 0.0094(4) Uani 1 1 d . . . . .
O20 O 0.65717(18) 1.21962(16) 0.32941(8) 0.0148(4) Uani 1 1 d . . . . .
O21 O 1.04533(16) 0.92606(15) 0.31778(7) 0.0093(4) Uani 1 1 d . . . . .
O22 O 1.07940(16) 1.12701(15) 0.29311(7) 0.0097(4) Uani 1 1 d . . . . .
O23 O 1.21176(16) 0.99650(16) 0.34442(7) 0.0104(4) Uani 1 1 d . . . . .
O24 O 0.98231(16) 0.67312(15) 0.32861(7) 0.0088(3) Uani 1 1 d . . . . .
O25 O 1.20483(17) 0.63227(18) 0.30784(7) 0.0140(4) Uani 1 1 d . . . . .
O26 O 1.10142(18) 0.48522(16) 0.35385(7) 0.0135(4) Uani 1 1 d . . . . .
O27 O 0.74145(17) 0.14920(16) 0.14578(7) 0.0134(4) Uani 1 1 d . . . . .
O28 O 0.77447(17) 0.36616(16) 0.35315(7) 0.0127(4) Uani 1 1 d . . . . .
O29 O 0.09457(18) 0.97655(18) 0.16962(8) 0.0179(4) Uani 1 1 d . . . . .
O30 O 0.24258(18) 0.38577(18) 0.27051(8) 0.0183(4) Uani 1 1 d . . . . .
O31 O 0.2933(2) 0.9979(2) 0.43082(9) 0.0291(6) Uani 1 1 d . . . . .
O32 O 0.0869(2) 0.3393(2) 0.43104(9) 0.0305(6) Uani 1 1 d . . . . .
O33 O 0.2052(2) 0.2996(2) 0.06871(8) 0.0250(5) Uani 1 1 d . . . . .
O34 O 0.3074(2) 0.2238(2) 0.42497(8) 0.0236(5) Uani 1 1 d . . . . .
O35 O 0.26553(18) 0.15027(18) 0.22298(8) 0.0180(4) Uani 1 1 d . . . . .
O36 O 0.0440(4) 0.1634(4) 0.10396(17) 0.0233(10) Uani 0.5 1 d . . P . .
O37 O 0.4693(4) 0.3455(4) 0.38893(17) 0.0215(10) Uani 0.5 1 d . . P . .
O38 O 0.6154(4) 0.3815(4) 0.48981(17) 0.0281(11) Uani 0.5 1 d . . P . .
O39 O 0.1453(7) 0.8353(8) 0.0034(3) 0.065(2) Uani 0.5 1 d . . P . .
O40 O 0.6804(5) 0.4115(5) 0.51526(18) 0.0315(12) Uani 0.5 1 d . . P . .
O41 O 0.0193(5) 0.0466(5) 0.0264(2) 0.0410(14) Uani 0.5 1 d . . P . .
O42 O 0.1561(6) 0.0393(7) 0.0743(2) 0.0569(19) Uani 0.5 1 d . . P . .
O43 O 0.4767(5) 0.4118(4) 0.47699(18) 0.0295(11) Uani 0.5 1 d . . P . .
O44 O -0.0207(6) 0.2185(5) 0.0671(2) 0.0529(18) Uani 0.5 1 d . . P . .
O45 O 0.1745(6) 0.8625(6) 0.0216(2) 0.0354(15) Uani 0.5 1 d . . P . .
O46 O 0.4332(5) 0.3998(4) 0.43291(18) 0.0324(12) Uani 0.5 1 d . . P . .
O47 O 0.8484(2) 0.3346(2) 0.44242(8) 0.0245(5) Uani 1 1 d . . . . .
O48 O 0.6557(2) 0.1826(2) 0.05850(9) 0.0298(6) Uani 1 1 d . . . . .
O49 O 0.42549(19) 0.5300(2) 0.33359(10) 0.0279(6) Uani 1 1 d . . . . .
O50 O 0.3429(2) 0.7667(2) 0.42780(10) 0.0324(6) Uani 1 1 d . . . . .
O51 O 0.4186(2) 0.1730(3) 0.07172(11) 0.0472(9) Uani 1 1 d . . . . .
O52 O 0.1655(2) 0.6800(3) 0.08711(10) 0.0374(7) Uani 1 1 d . . . . .
C1 C 0.5010(2) 0.7235(2) 0.04042(9) 0.0105(5) Uani 1 1 d . . . . .
H1A H 0.5722 0.7136 0.0165 0.013 Uiso 1 1 calc R U . . .
H1B H 0.4348 0.7647 0.0242 0.013 Uiso 1 1 calc R U . . .
C2 C 0.4763(2) 0.6093(2) 0.06037(10) 0.0111(5) Uani 1 1 d . . . . .
H2A H 0.4042 0.6197 0.0838 0.013 Uiso 1 1 calc R U . . .
H2B H 0.4613 0.5691 0.0343 0.013 Uiso 1 1 calc R U . . .
C3 C 0.6698(2) 0.4897(2) 0.04701(10) 0.0112(5) Uani 1 1 d . . . . .
H3A H 0.6807 0.5478 0.0205 0.013 Uiso 1 1 calc R U . . .
H3B H 0.6473 0.4260 0.0342 0.013 Uiso 1 1 calc R U . . .
C4 C 0.7846(2) 0.4487(2) 0.06702(10) 0.0106(5) Uani 1 1 d . . . . .
H4A H 0.7736 0.3899 0.0932 0.013 Uiso 1 1 calc R U . . .
H4B H 0.8447 0.4140 0.0419 0.013 Uiso 1 1 calc R U . . .
C5 C 0.8753(2) 0.6118(2) 0.04362(9) 0.0112(5) Uani 1 1 d . . . . .
H5A H 0.8226 0.6231 0.0191 0.013 Uiso 1 1 calc R U . . .
H5B H 0.9527 0.5709 0.0298 0.013 Uiso 1 1 calc R U . . .
C6 C 0.8890(2) 0.7250(2) 0.05600(10) 0.0103(5) Uani 1 1 d . . . . .
H6A H 0.9445 0.7139 0.0795 0.012 Uiso 1 1 calc R U . . .
H6B H 0.9232 0.7660 0.0271 0.012 Uiso 1 1 calc R U . . .
C7 C 0.7068(2) 0.8442(2) 0.03698(9) 0.0109(5) Uani 1 1 d . . . . .
H7A H 0.7134 0.7867 0.0142 0.013 Uiso 1 1 calc R U . . .
H7B H 0.7398 0.9083 0.0197 0.013 Uiso 1 1 calc R U . . .
C8 C 0.5788(2) 0.8845(2) 0.05519(10) 0.0097(5) Uani 1 1 d . . . . .
H8A H 0.5726 0.9406 0.0785 0.012 Uiso 1 1 calc R U . . .
H8B H 0.5382 0.9225 0.0284 0.012 Uiso 1 1 calc R U . . .
C9 C 0.4020(2) 0.8407(2) 0.10352(9) 0.0094(5) Uani 1 1 d . . . . .
H9A H 0.3541 0.7812 0.1113 0.011 Uiso 1 1 calc R U . . .
H9B H 0.3614 0.9001 0.0822 0.011 Uiso 1 1 calc R U . . .
C10 C 0.5283(2) 0.4446(2) 0.11416(9) 0.0100(5) Uani 1 1 d . . . . .
H10A H 0.5949 0.3899 0.1253 0.012 Uiso 1 1 calc R U . . .
H10B H 0.4889 0.4049 0.0949 0.012 Uiso 1 1 calc R U . . .
C11 C 0.9207(2) 0.4915(2) 0.11468(10) 0.0102(5) Uani 1 1 d . . . . .
H11A H 0.9583 0.5526 0.1216 0.012 Uiso 1 1 calc R U . . .
H11B H 0.9813 0.4379 0.0962 0.012 Uiso 1 1 calc R U . . .
C12 C 0.8049(2) 0.8883(2) 0.09877(9) 0.0097(5) Uani 1 1 d . . . . .
H12A H 0.7328 0.9455 0.1056 0.012 Uiso 1 1 calc R U . . .
H12B H 0.8618 0.9248 0.0764 0.012 Uiso 1 1 calc R U . . .
C13 C 0.6213(2) 0.7996(2) 0.44131(9) 0.0092(5) Uani 1 1 d . . . . .
H13A H 0.5845 0.7607 0.4702 0.011 Uiso 1 1 calc R U . . .
H13B H 0.5678 0.8097 0.4171 0.011 Uiso 1 1 calc R U . . .
C14 C 0.6350(2) 0.9142(2) 0.45289(9) 0.0093(5) Uani 1 1 d . . . . .
H14A H 0.5573 0.9561 0.4659 0.011 Uiso 1 1 calc R U . . .
H14B H 0.6864 0.9040 0.4779 0.011 Uiso 1 1 calc R U . . .
C15 C 0.7280(2) 1.0752(2) 0.42915(9) 0.0093(5) Uani 1 1 d . . . . .
H15A H 0.6683 1.1104 0.4543 0.011 Uiso 1 1 calc R U . . .
H15B H 0.7391 1.1335 0.4028 0.011 Uiso 1 1 calc R U . . .
C16 C 0.8429(2) 1.0334(2) 0.44893(9) 0.0083(5) Uani 1 1 d . . . . .
H16A H 0.8666 1.0971 0.4613 0.010 Uiso 1 1 calc R U . . .
H16B H 0.8313 0.9763 0.4758 0.010 Uiso 1 1 calc R U . . .
C17 C 1.0351(2) 0.9135(2) 0.43592(9) 0.0088(5) Uani 1 1 d . . . . .
H17A H 1.0522 0.9556 0.4609 0.011 Uiso 1 1 calc R U . . .
H17B H 1.1062 0.9006 0.4121 0.011 Uiso 1 1 calc R U . . .
C18 C 1.0092(2) 0.8007(2) 0.45798(9) 0.0090(5) Uani 1 1 d . . . . .
H18A H 1.0751 0.7612 0.4748 0.011 Uiso 1 1 calc R U . . .
H18B H 0.9379 0.8133 0.4817 0.011 Uiso 1 1 calc R U . . .
C19 C 0.9295(2) 0.6380(2) 0.44636(9) 0.0085(5) Uani 1 1 d . . . . .
H19A H 0.9684 0.6025 0.4740 0.010 Uiso 1 1 calc R U . . .
H19B H 0.9360 0.5794 0.4241 0.010 Uiso 1 1 calc R U . . .
C20 C 0.8013(2) 0.6812(2) 0.46317(9) 0.0087(5) Uani 1 1 d . . . . .
H20A H 0.7667 0.6190 0.4813 0.010 Uiso 1 1 calc R U . . .
H20B H 0.7946 0.7410 0.4849 0.010 Uiso 1 1 calc R U . . .
C21 C 0.7072(2) 0.6316(2) 0.40153(9) 0.0088(5) Uani 1 1 d . . . . .
H21A H 0.6498 0.5960 0.4241 0.011 Uiso 1 1 calc R U . . .
H21B H 0.7796 0.5743 0.3955 0.011 Uiso 1 1 calc R U . . .
C22 C 0.5927(2) 1.0326(2) 0.38104(9) 0.0090(5) Uani 1 1 d . . . . .
H22A H 0.5340 1.0892 0.3987 0.011 Uiso 1 1 calc R U . . .
H22B H 0.5523 0.9725 0.3752 0.011 Uiso 1 1 calc R U . . .
C23 C 0.9837(2) 1.0765(2) 0.38184(9) 0.0092(5) Uani 1 1 d . . . . .
H23A H 1.0220 1.1173 0.4011 0.011 Uiso 1 1 calc R U . . .
H23B H 0.9171 1.1303 0.3703 0.011 Uiso 1 1 calc R U . . .
C24 C 1.1077(2) 0.6749(2) 0.39772(9) 0.0092(5) Uani 1 1 d . . . . .
H24A H 1.1461 0.6164 0.4200 0.011 Uiso 1 1 calc R U . . .
H24B H 1.1576 0.7326 0.3893 0.011 Uiso 1 1 calc R U . . .


_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 2.4209(18) . ?
La1 O11 2.4565(18) . ?
La1 O5 2.4753(18) . ?
La1 O8 2.4876(18) . ?
La1 O1 2.6785(19) . ?
La1 N3 2.813(2) . ?
La1 N1 2.818(2) . ?
La1 N4 2.837(2) . ?
La1 N2 2.860(2) . ?
La2 O24 2.4194(18) . ?
La2 O15 2.4535(18) . ?
La2 O18 2.4856(18) . ?
La2 O21 2.4995(18) . ?
La2 O14 2.6667(19) . ?
La2 N8 2.831(2) . ?
La2 N6 2.841(2) . ?
La2 N7 2.845(2) . ?
La2 N5 2.853(2) . ?
P1 O3 1.5220(19) . ?
P1 O4 1.530(2) . ?
P1 O2 1.5335(19) . ?
P1 C9 1.839(3) . ?
P2 O6 1.5235(19) . ?
P2 O7 1.525(2) . ?
P2 O5 1.5283(19) . ?
P2 C10 1.820(3) . ?
P3 O9 1.523(2) . ?
P3 O10 1.528(2) . ?
P3 O8 1.5301(19) . ?
P3 C11 1.830(3) . ?
P4 O13 1.522(2) . ?
P4 O12 1.5329(19) . ?
P4 O11 1.5429(19) . ?
P4 C12 1.819(3) . ?
P5 O17 1.5249(19) . ?
P5 O16 1.5362(19) . ?
P5 O15 1.5409(19) . ?
P5 C21 1.821(3) . ?
P6 O20 1.515(2) . ?
P6 O19 1.5294(19) . ?
P6 O18 1.5305(19) . ?
P6 C22 1.827(3) . ?
P7 O23 1.5262(19) . ?
P7 O21 1.5280(19) . ?
P7 O22 1.5335(19) . ?
P7 C23 1.817(3) . ?
P8 O26 1.514(2) . ?
P8 O24 1.5286(19) . ?
P8 O25 1.537(2) . ?
P8 C24 1.830(3) . ?
N1 C1 1.489(3) . ?
N1 C9 1.489(3) . ?
N1 C8 1.492(3) . ?
N2 C10 1.486(3) . ?
N2 C3 1.490(3) . ?
N2 C2 1.496(3) . ?
N3 C4 1.483(3) . ?
N3 C11 1.485(3) . ?
N3 C5 1.494(3) . ?
N4 C12 1.484(3) . ?
N4 C7 1.486(3) . ?
N4 C6 1.490(3) . ?
N5 C20 1.483(3) . ?
N5 C21 1.484(3) . ?
N5 C13 1.492(3) . ?
N6 C14 1.482(3) . ?
N6 C15 1.489(3) . ?
N6 C22 1.491(3) . ?
N7 C16 1.479(3) . ?
N7 C17 1.482(3) . ?
N7 C23 1.495(3) . ?
N8 C18 1.483(3) . ?
N8 C24 1.489(3) . ?
N8 C19 1.491(3) . ?
O36 O44 1.427(8) . ?
O37 O46 1.448(7) . ?
O38 O40 1.263(7) . ?
O38 O43 1.688(7) . ?
O39 O45 0.800(8) . ?
O43 O46 1.465(7) . ?
C1 C2 1.510(4) . ?
C3 C4 1.520(4) . ?
C5 C6 1.504(4) . ?
C7 C8 1.514(4) . ?
C13 C14 1.512(4) . ?
C15 C16 1.519(4) . ?
C17 C18 1.514(3) . ?
C19 C20 1.512(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 La1 O11 81.09(6) . . ?
O2 La1 O5 83.66(6) . . ?
O11 La1 O5 138.53(6) . . ?
O2 La1 O8 137.16(6) . . ?
O11 La1 O8 83.39(6) . . ?
O5 La1 O8 82.14(6) . . ?
O2 La1 O1 65.79(6) . . ?
O11 La1 O1 77.15(6) . . ?
O5 La1 O1 61.43(6) . . ?
O8 La1 O1 71.91(6) . . ?
O2 La1 N3 151.25(6) . . ?
O11 La1 N3 88.85(6) . . ?
O5 La1 N3 120.10(6) . . ?
O8 La1 N3 67.11(6) . . ?
O1 La1 N3 137.90(6) . . ?
O2 La1 N1 64.92(6) . . ?
O11 La1 N1 120.36(6) . . ?
O5 La1 N1 86.44(6) . . ?
O8 La1 N1 152.93(7) . . ?
O1 La1 N1 123.03(6) . . ?
N3 La1 N1 98.41(6) . . ?
O2 La1 N4 86.63(6) . . ?
O11 La1 N4 65.64(6) . . ?
O5 La1 N4 151.19(6) . . ?
O8 La1 N4 122.07(6) . . ?
O1 La1 N4 136.72(6) . . ?
N3 La1 N4 64.73(6) . . ?
N1 La1 N4 64.91(6) . . ?
O2 La1 N2 121.01(6) . . ?
O11 La1 N2 152.32(6) . . ?
O5 La1 N2 65.66(6) . . ?
O8 La1 N2 88.82(6) . . ?
O1 La1 N2 125.37(6) . . ?
N3 La1 N2 63.73(6) . . ?
N1 La1 N2 64.11(6) . . ?
N4 La1 N2 97.09(6) . . ?
O24 La2 O15 81.92(6) . . ?
O24 La2 O18 135.88(6) . . ?
O15 La2 O18 81.52(6) . . ?
O24 La2 O21 83.58(6) . . ?
O15 La2 O21 139.81(6) . . ?
O18 La2 O21 83.35(6) . . ?
O24 La2 O14 65.81(6) . . ?
O15 La2 O14 78.64(6) . . ?
O18 La2 O14 70.95(6) . . ?
O21 La2 O14 61.23(6) . . ?
O24 La2 N8 65.30(6) . . ?
O15 La2 N8 119.52(6) . . ?
O18 La2 N8 154.93(6) . . ?
O21 La2 N8 87.12(6) . . ?
O14 La2 N8 123.64(6) . . ?
O24 La2 N6 151.90(6) . . ?
O15 La2 N6 88.14(6) . . ?
O18 La2 N6 67.37(6) . . ?
O21 La2 N6 119.48(6) . . ?
O14 La2 N6 137.66(6) . . ?
N8 La2 N6 97.95(6) . . ?
O24 La2 N7 121.14(6) . . ?
O15 La2 N7 151.14(6) . . ?
O18 La2 N7 90.55(6) . . ?
O21 La2 N7 65.46(6) . . ?
O14 La2 N7 124.90(6) . . ?
N8 La2 N7 64.42(6) . . ?
N6 La2 N7 63.31(6) . . ?
O24 La2 N5 87.56(6) . . ?
O15 La2 N5 64.94(6) . . ?
O18 La2 N5 120.86(6) . . ?
O21 La2 N5 151.21(6) . . ?
O14 La2 N5 137.69(6) . . ?
N8 La2 N5 64.35(6) . . ?
N6 La2 N5 64.47(6) . . ?
N7 La2 N5 96.70(6) . . ?
O3 P1 O4 110.59(11) . . ?
O3 P1 O2 111.84(11) . . ?
O4 P1 O2 112.88(11) . . ?
O3 P1 C9 110.47(12) . . ?
O4 P1 C9 107.06(12) . . ?
O2 P1 C9 103.67(11) . . ?
O6 P2 O7 110.59(11) . . ?
O6 P2 O5 111.96(11) . . ?
O7 P2 O5 113.29(11) . . ?
O6 P2 C10 110.94(12) . . ?
O7 P2 C10 105.16(12) . . ?
O5 P2 C10 104.53(11) . . ?
O9 P3 O10 110.76(11) . . ?
O9 P3 O8 113.20(11) . . ?
O10 P3 O8 112.97(11) . . ?
O9 P3 C11 109.51(12) . . ?
O10 P3 C11 105.77(11) . . ?
O8 P3 C11 104.11(11) . . ?
O13 P4 O12 110.60(11) . . ?
O13 P4 O11 112.25(11) . . ?
O12 P4 O11 111.82(11) . . ?
O13 P4 C12 113.34(12) . . ?
O12 P4 C12 104.76(11) . . ?
O11 P4 C12 103.68(11) . . ?
O17 P5 O16 110.69(11) . . ?
O17 P5 O15 112.64(11) . . ?
O16 P5 O15 111.74(11) . . ?
O17 P5 C21 112.31(12) . . ?
O16 P5 C21 105.66(11) . . ?
O15 P5 C21 103.40(11) . . ?
O20 P6 O19 110.73(11) . . ?
O20 P6 O18 112.76(12) . . ?
O19 P6 O18 113.14(11) . . ?
O20 P6 C22 110.16(12) . . ?
O19 P6 C22 105.37(11) . . ?
O18 P6 C22 104.20(11) . . ?
O23 P7 O21 112.36(11) . . ?
O23 P7 O22 110.43(11) . . ?
O21 P7 O22 113.60(11) . . ?
O23 P7 C23 110.38(12) . . ?
O21 P7 C23 104.27(11) . . ?
O22 P7 C23 105.37(11) . . ?
O26 P8 O24 112.15(11) . . ?
O26 P8 O25 110.34(12) . . ?
O24 P8 O25 112.62(11) . . ?
O26 P8 C24 111.01(12) . . ?
O24 P8 C24 103.86(11) . . ?
O25 P8 C24 106.54(12) . . ?
C1 N1 C9 108.9(2) . . ?
C1 N1 C8 108.7(2) . . ?
C9 N1 C8 109.2(2) . . ?
C1 N1 La1 113.83(15) . . ?
C9 N1 La1 107.26(15) . . ?
C8 N1 La1 108.82(15) . . ?
C10 N2 C3 109.4(2) . . ?
C10 N2 C2 108.9(2) . . ?
C3 N2 C2 109.7(2) . . ?
C10 N2 La1 106.05(15) . . ?
C3 N2 La1 112.90(15) . . ?
C2 N2 La1 109.86(15) . . ?
C4 N3 C11 109.5(2) . . ?
C4 N3 C5 108.8(2) . . ?
C11 N3 C5 109.7(2) . . ?
C4 N3 La1 111.49(15) . . ?
C11 N3 La1 104.65(15) . . ?
C5 N3 La1 112.55(15) . . ?
C12 N4 C7 108.9(2) . . ?
C12 N4 C6 107.8(2) . . ?
C7 N4 C6 109.8(2) . . ?
C12 N4 La1 107.95(15) . . ?
C7 N4 La1 111.91(15) . . ?
C6 N4 La1 110.32(15) . . ?
C20 N5 C21 108.78(19) . . ?
C20 N5 C13 110.1(2) . . ?
C21 N5 C13 108.1(2) . . ?
C20 N5 La2 112.11(15) . . ?
C21 N5 La2 107.83(15) . . ?
C13 N5 La2 109.83(15) . . ?
C14 N6 C15 108.8(2) . . ?
C14 N6 C22 110.0(2) . . ?
C15 N6 C22 108.8(2) . . ?
C14 N6 La2 112.55(15) . . ?
C15 N6 La2 111.52(15) . . ?
C22 N6 La2 105.00(15) . . ?
C16 N7 C17 110.2(2) . . ?
C16 N7 C23 108.56(19) . . ?
C17 N7 C23 108.4(2) . . ?
C16 N7 La2 113.90(14) . . ?
C17 N7 La2 109.19(14) . . ?
C23 N7 La2 106.34(15) . . ?
C18 N8 C24 109.4(2) . . ?
C18 N8 C19 109.5(2) . . ?
C24 N8 C19 108.6(2) . . ?
C18 N8 La2 112.70(15) . . ?
C24 N8 La2 107.03(15) . . ?
C19 N8 La2 109.52(14) . . ?
P1 O2 La1 128.64(10) . . ?
P2 O5 La1 129.67(11) . . ?
P3 O8 La1 127.44(11) . . ?
P4 O11 La1 130.95(10) . . ?
P5 O15 La2 131.67(10) . . ?
P6 O18 La2 128.59(11) . . ?
P7 O21 La2 129.29(11) . . ?
P8 O24 La2 129.86(10) . . ?
O40 O38 O43 141.2(5) . . ?
O46 O43 O38 129.2(4) . . ?
O37 O46 O43 141.0(5) . . ?
N1 C1 C2 112.0(2) . . ?
N2 C2 C1 113.6(2) . . ?
N2 C3 C4 111.8(2) . . ?
N3 C4 C3 112.6(2) . . ?
N3 C5 C6 113.8(2) . . ?
N4 C6 C5 113.3(2) . . ?
N4 C7 C8 112.3(2) . . ?
N1 C8 C7 113.1(2) . . ?
N1 C9 P1 112.95(17) . . ?
N2 C10 P2 112.75(18) . . ?
N3 C11 P3 114.14(18) . . ?
N4 C12 P4 112.92(18) . . ?
N5 C13 C14 113.4(2) . . ?
N6 C14 C13 113.8(2) . . ?
N6 C15 C16 112.0(2) . . ?
N7 C16 C15 112.3(2) . . ?
N7 C17 C18 113.5(2) . . ?
N8 C18 C17 112.4(2) . . ?
N8 C19 C20 112.9(2) . . ?
N5 C20 C19 112.4(2) . . ?
N5 C21 P5 112.46(17) . . ?
N6 C22 P6 114.80(17) . . ?
N7 C23 P7 113.26(17) . . ?
N8 C24 P8 113.58(17) . . ?

_refine_diff_density_max         2.629
_refine_diff_density_min         -1.050
_refine_diff_density_rms         0.202


_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'Bruker Triumph curved graphite'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0

