# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_L
_database_code_depnum_ccdc_archive 'CCDC 1442097'
_audit_update_record             
;
2015-12-13 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C28 H26 O3 P2, 0.5(C6 H6)'
_chemical_formula_sum            'C31 H29 O3 P2'
_chemical_formula_weight         511.48
_chemical_melting_point          ?
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   9.8274(12)
_cell_length_b                   11.8989(15)
_cell_length_c                   13.0901(16)
_cell_angle_alpha                70.615(2)
_cell_angle_beta                 68.839(2)
_cell_angle_gamma                87.156(2)
_cell_volume                     1342.3(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    148(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_exptl_absorpt_coefficient_mu    0.193
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             538
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16085
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.77
_diffrn_ambient_temperature      148(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Apex 2 CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                5432
_reflns_number_total             7124
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    ?
_computing_publication_material  ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         7124
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0474
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0630P)²+0.1541P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1251
_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. 
;
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H2A(0.031) H3A(0.037) H4A(0.033) H5A(0.032) H6A(0.029) H8A(0.033)
 H9A(0.045) H10A(0.05) H11A(0.046) H12A(0.033) H13A(0.02) H15A(0.029)
 H16A(0.037) H17A(0.04) H18A(0.039) H19A(0.031) H21A(0.028) H22A(0.033)
 H23A(0.031) H24A(0.031) H25A(0.028) H26A(0.026) H26B(0.026) H28A(0.081)
 H28B(0.081) H28C(0.081) H1SA(0.065) H2SA(0.065) H3SA(0.067)
 Fixed X: H2A(1.0481) H3A(1.1605) H4A(1.0451) H5A(0.8125) H6A(0.696)
 H8A(0.7999) H9A(0.6698) H10A(0.4704) H11A(0.4002) H12A(0.5306) H13A(0.6073)
 H15A(0.4811) H16A(0.3001) H17A(0.1217) H18A(0.1237) H19A(0.3019) H21A(0.4911)
 H22A(0.5946) H23A(0.7924) H24A(0.8877) H25A(0.785) H26A(0.8557) H26B(0.7878)
 H28A(0.6935) H28B(0.7013) H28C(0.8426) H1SA(0.769) H2SA(0.8986) H3SA(1.1303)
 Fixed Y: H2A(0.1136) H3A(-0.0665) H4A(-0.2311) H5A(-0.2205) H6A(-0.0434)
 H8A(0.3319) H9A(0.3291) H10A(0.1903) H11A(0.0523) H12A(0.0521) H13A(0.1287)
 H15A(0.4584) H16A(0.4381) H17A(0.2785) H18A(0.1363) H19A(0.1565) H21A(0.5263)
 H22A(0.7226) H23A(0.7856) H24A(0.6526) H25A(0.4558) H26A(0.1735) H26B(0.2936)
 H28A(0.1319) H28B(0.2666) H28C(0.192) H1SA(0.5681) H2SA(0.5198) H3SA(0.4523)
 Fixed Z: H2A(0.0736) H3A(0.1047) H4A(0.2694) H5A(0.3997) H6A(0.3671) H8A(-
 0.0426) H9A(-0.1608) H10A(-0.089) H11A(0.0986) H12A(0.2173) H13A(0.3656)
 H15A(0.1301) H16A(0.0592) H17A(0.1603) H18A(0.3336) H19A(0.4067) H21A(0.4033)
 H22A(0.3264) H23A(0.1492) H24A(0.0493) H25A(0.1252) H26A(0.3645) H26B(0.3824)
 H28A(0.6822) H28B(0.5986) H28C(0.5762) H1SA(0.5257) H2SA(0.3601) H3SA(0.3351)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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
P1 P 0.78627(4) 0.19727(4) 0.18234(4) 0.01766(11) Uani 1 1 d . . .
P2 P 0.53692(4) 0.32129(4) 0.34194(4) 0.01715(11) Uani 1 1 d . . .
O1 O 0.90639(12) 0.29401(11) 0.11536(10) 0.0245(3) Uani 1 1 d . . .
O2 O 0.46130(13) 0.29517(11) 0.46974(10) 0.0235(3) Uani 1 1 d . . .
O3 O 0.60145(15) 0.05742(12) 0.56096(11) 0.0317(3) Uani 1 1 d . . .
C1 C 0.86045(17) 0.05301(15) 0.21756(15) 0.0199(3) Uani 1 1 d . . .
C2 C 0.99966(19) 0.04572(16) 0.13950(16) 0.0261(4) Uani 1 1 d . . .
H2A H 1.0481 0.1136 0.0736 0.031 Uiso 1 1 calc R . .
C3 C 1.0670(2) -0.06102(17) 0.15851(17) 0.0306(4) Uani 1 1 d . . .
H3A H 1.1605 -0.0665 0.1047 0.037 Uiso 1 1 calc R . .
C4 C 0.9978(2) -0.15897(16) 0.25567(17) 0.0277(4) Uani 1 1 d . . .
H4A H 1.0451 -0.2311 0.2694 0.033 Uiso 1 1 calc R . .
C5 C 0.8598(2) -0.15264(16) 0.33337(16) 0.0271(4) Uani 1 1 d . . .
H5A H 0.8125 -0.2205 0.3997 0.032 Uiso 1 1 calc R . .
C6 C 0.79095(19) -0.04729(16) 0.31423(15) 0.0246(4) Uani 1 1 d . . .
H6A H 0.6960 -0.0434 0.3671 0.029 Uiso 1 1 calc R . .
C7 C 0.67775(18) 0.19230(15) 0.09851(14) 0.0204(3) Uani 1 1 d . . .
C8 C 0.7190(2) 0.27483(17) -0.01393(15) 0.0274(4) Uani 1 1 d . . .
H8A H 0.7999 0.3319 -0.0426 0.033 Uiso 1 1 calc R . .
C9 C 0.6416(2) 0.2735(2) -0.08397(18) 0.0374(5) Uani 1 1 d . . .
H9A H 0.6698 0.3291 -0.1608 0.045 Uiso 1 1 calc R . .
C10 C 0.5235(3) 0.1908(2) -0.04128(19) 0.0416(5) Uani 1 1 d . . .
H10A H 0.4704 0.1903 -0.0890 0.050 Uiso 1 1 calc R . .
C11 C 0.4817(2) 0.1087(2) 0.07027(19) 0.0380(5) Uani 1 1 d . . .
H11A H 0.4002 0.0523 0.0986 0.046 Uiso 1 1 calc R . .
C12 C 0.5587(2) 0.10863(17) 0.14081(16) 0.0274(4) Uani 1 1 d . . .
H12A H 0.5306 0.0521 0.2173 0.033 Uiso 1 1 calc R . .
C13 C 0.66771(17) 0.20688(14) 0.32326(13) 0.0167(3) Uani 1 1 d . . .
H13A H 0.6073 0.1287 0.3656 0.020 Uiso 1 1 calc R . .
C14 C 0.40961(17) 0.30991(15) 0.27521(14) 0.0193(3) Uani 1 1 d . . .
C15 C 0.40850(19) 0.39317(16) 0.17189(15) 0.0241(4) Uani 1 1 d . . .
H15A H 0.4811 0.4584 0.1301 0.029 Uiso 1 1 calc R . .
C16 C 0.3008(2) 0.38086(19) 0.12970(17) 0.0312(4) Uani 1 1 d . . .
H16A H 0.3001 0.4381 0.0592 0.037 Uiso 1 1 calc R . .
C17 C 0.1950(2) 0.28616(19) 0.18952(18) 0.0335(5) Uani 1 1 d . . .
H17A H 0.1217 0.2785 0.1603 0.040 Uiso 1 1 calc R . .
C18 C 0.1959(2) 0.20188(18) 0.29275(18) 0.0324(4) Uani 1 1 d . . .
H18A H 0.1237 0.1363 0.3336 0.039 Uiso 1 1 calc R . .
C19 C 0.30197(19) 0.21366(16) 0.33594(16) 0.0255(4) Uani 1 1 d . . .
H19A H 0.3019 0.1565 0.4067 0.031 Uiso 1 1 calc R . .
C20 C 0.62756(17) 0.47009(15) 0.27246(14) 0.0188(3) Uani 1 1 d . . .
C21 C 0.57176(19) 0.55151(16) 0.33136(15) 0.0236(4) Uani 1 1 d . . .
H21A H 0.4911 0.5263 0.4033 0.028 Uiso 1 1 calc R . .
C22 C 0.6330(2) 0.66827(17) 0.28574(16) 0.0277(4) Uani 1 1 d . . .
H22A H 0.5946 0.7226 0.3264 0.033 Uiso 1 1 calc R . .
C23 C 0.7505(2) 0.70551(17) 0.18063(15) 0.0260(4) Uani 1 1 d . . .
H23A H 0.7924 0.7856 0.1492 0.031 Uiso 1 1 calc R . .
C24 C 0.80703(19) 0.62662(16) 0.12122(15) 0.0261(4) Uani 1 1 d . . .
H24A H 0.8877 0.6526 0.0493 0.031 Uiso 1 1 calc R . .
C25 C 0.74598(19) 0.50947(16) 0.16650(15) 0.0235(4) Uani 1 1 d . . .
H25A H 0.7850 0.4558 0.1252 0.028 Uiso 1 1 calc R . .
C26 C 0.76302(18) 0.20940(16) 0.39433(14) 0.0213(3) Uani 1 1 d . . .
H26A H 0.8557 0.1735 0.3645 0.026 Uiso 1 1 calc R . .
H26B H 0.7878 0.2936 0.3824 0.026 Uiso 1 1 calc R . .
C27 C 0.6886(2) 0.14282(17) 0.52387(15) 0.0256(4) Uani 1 1 d . . .
C28 C 0.7356(3) 0.1872(2) 0.60204(19) 0.0540(7) Uani 1 1 d . . .
H28A H 0.6935 0.1319 0.6822 0.081 Uiso 1 1 calc R . .
H28B H 0.7013 0.2666 0.5986 0.081 Uiso 1 1 calc R . .
H28C H 0.8426 0.1920 0.5762 0.081 Uiso 1 1 calc R . .
C1S C 0.8637(2) 0.5401(2) 0.5151(3) 0.0542(7) Uani 1 1 d . . .
H1SA H 0.7690 0.5681 0.5257 0.065 Uiso 1 1 calc R . .
C2S C 0.9400(3) 0.5118(2) 0.4172(2) 0.0544(7) Uani 1 1 d . . .
H2SA H 0.8986 0.5198 0.3601 0.065 Uiso 1 1 calc R . .
C3S C 1.0767(3) 0.4718(2) 0.4027(2) 0.0558(7) Uani 1 1 d . . .
H3SA H 1.1303 0.4523 0.3351 0.067 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
P1 O1 1.4849(12) . ?
P1 C1 1.8121(17) . ?
P1 C7 1.7998(17) . ?
P1 C13 1.8297(16) . ?
P2 O2 1.4925(12) . ?
P2 C13 1.8400(16) . ?
P2 C14 1.7975(17) . ?
P2 C20 1.8050(17) . ?
O3 C27 1.208(2) . ?
C1 C2 1.400(2) . ?
C1 C6 1.395(2) . ?
C2 H2A 0.9500 . ?
C2 C3 1.392(3) . ?
C3 H3A 0.9500 . ?
C3 C4 1.381(3) . ?
C4 H4A 0.9500 . ?
C4 C5 1.387(3) . ?
C5 H5A 0.9500 . ?
C5 C6 1.386(2) . ?
C6 H6A 0.9500 . ?
C7 C8 1.394(2) . ?
C7 C12 1.396(2) . ?
C8 H8A 0.9500 . ?
C8 C9 1.391(3) . ?
C9 H9A 0.9500 . ?
C9 C10 1.381(3) . ?
C10 H10A 0.9500 . ?
C10 C11 1.384(3) . ?
C11 H11A 0.9500 . ?
C11 C12 1.389(3) . ?
C12 H12A 0.9500 . ?
C13 H13A 1.0000 . ?
C13 C26 1.547(2) . ?
C14 C15 1.390(2) . ?
C14 C19 1.404(2) . ?
C15 H15A 0.9500 . ?
C15 C16 1.392(2) . ?
C16 H16A 0.9500 . ?
C16 C17 1.381(3) . ?
C17 H17A 0.9500 . ?
C17 C18 1.393(3) . ?
C18 H18A 0.9500 . ?
C18 C19 1.385(2) . ?
C19 H19A 0.9500 . ?
C20 C21 1.404(2) . ?
C20 C25 1.398(2) . ?
C21 H21A 0.9500 . ?
C21 C22 1.386(2) . ?
C22 H22A 0.9500 . ?
C22 C23 1.386(3) . ?
C23 H23A 0.9500 . ?
C23 C24 1.384(3) . ?
C24 H24A 0.9500 . ?
C24 C25 1.390(2) . ?
C25 H25A 0.9500 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.519(2) . ?
C27 C28 1.504(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C1S H1SA 0.9500 . ?
C1S C2S 1.373(4) . ?
C1S C3S 1.366(4) 2_766 ?
C2S H2SA 0.9500 . ?
C2S C3S 1.370(4) . ?
C3S C1S 1.366(4) 2_766 ?
C3S H3SA 0.9500 . ?

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 P1 C1 110.38(7) . . ?
O1 P1 C7 111.08(8) . . ?
O1 P1 C13 113.76(7) . . ?
C1 P1 C13 104.56(8) . . ?
C7 P1 C1 106.81(8) . . ?
C7 P1 C13 109.84(7) . . ?
O2 P2 C13 106.93(7) . . ?
O2 P2 C14 111.23(7) . . ?
O2 P2 C20 110.73(7) . . ?
C14 P2 C13 108.03(7) . . ?
C14 P2 C20 108.29(8) . . ?
C20 P2 C13 111.62(7) . . ?
C2 C1 P1 115.27(13) . . ?
C6 C1 P1 125.41(13) . . ?
C6 C1 C2 119.32(16) . . ?
C1 C2 H2A 120.0 . . ?
C3 C2 C1 119.99(17) . . ?
C3 C2 H2A 120.0 . . ?
C2 C3 H3A 120.0 . . ?
C4 C3 C2 120.00(17) . . ?
C4 C3 H3A 120.0 . . ?
C3 C4 H4A 119.8 . . ?
C3 C4 C5 120.39(17) . . ?
C5 C4 H4A 119.8 . . ?
C4 C5 H5A 120.0 . . ?
C6 C5 C4 120.01(17) . . ?
C6 C5 H5A 120.0 . . ?
C1 C6 H6A 119.9 . . ?
C5 C6 C1 120.26(16) . . ?
C5 C6 H6A 119.9 . . ?
C8 C7 P1 117.24(14) . . ?
C8 C7 C12 120.05(16) . . ?
C12 C7 P1 122.69(13) . . ?
C7 C8 H8A 120.1 . . ?
C9 C8 C7 119.89(19) . . ?
C9 C8 H8A 120.1 . . ?
C8 C9 H9A 120.1 . . ?
C10 C9 C8 119.71(19) . . ?
C10 C9 H9A 120.1 . . ?
C9 C10 H10A 119.6 . . ?
C9 C10 C11 120.77(19) . . ?
C11 C10 H10A 119.6 . . ?
C10 C11 H11A 120.0 . . ?
C10 C11 C12 120.1(2) . . ?
C12 C11 H11A 120.0 . . ?
C7 C12 H12A 120.2 . . ?
C11 C12 C7 119.50(18) . . ?
C11 C12 H12A 120.2 . . ?
P1 C13 P2 124.40(9) . . ?
P1 C13 H13A 105.2 . . ?
P2 C13 H13A 105.2 . . ?
C26 C13 P1 108.92(11) . . ?
C26 C13 P2 106.33(11) . . ?
C26 C13 H13A 105.2 . . ?
C15 C14 P2 123.74(13) . . ?
C15 C14 C19 119.50(15) . . ?
C19 C14 P2 116.68(13) . . ?
C14 C15 H15A 120.0 . . ?
C14 C15 C16 119.91(17) . . ?
C16 C15 H15A 120.0 . . ?
C15 C16 H16A 119.7 . . ?
C17 C16 C15 120.52(18) . . ?
C17 C16 H16A 119.7 . . ?
C16 C17 H17A 120.0 . . ?
C16 C17 C18 119.94(17) . . ?
C18 C17 H17A 120.0 . . ?
C17 C18 H18A 120.0 . . ?
C19 C18 C17 120.03(18) . . ?
C19 C18 H18A 120.0 . . ?
C14 C19 H19A 120.0 . . ?
C18 C19 C14 120.09(17) . . ?
C18 C19 H19A 120.0 . . ?
C21 C20 P2 115.95(12) . . ?
C25 C20 P2 125.51(13) . . ?
C25 C20 C21 118.54(16) . . ?
C20 C21 H21A 119.6 . . ?
C22 C21 C20 120.77(16) . . ?
C22 C21 H21A 119.6 . . ?
C21 C22 H22A 120.1 . . ?
C21 C22 C23 119.80(17) . . ?
C23 C22 H22A 120.1 . . ?
C22 C23 H23A 119.8 . . ?
C24 C23 C22 120.30(17) . . ?
C24 C23 H23A 119.8 . . ?
C23 C24 H24A 119.9 . . ?
C23 C24 C25 120.15(16) . . ?
C25 C24 H24A 119.9 . . ?
C20 C25 H25A 119.8 . . ?
C24 C25 C20 120.44(16) . . ?
C24 C25 H25A 119.8 . . ?
C13 C26 H26A 108.9 . . ?
C13 C26 H26B 108.9 . . ?
H26A C26 H26B 107.7 . . ?
C27 C26 C13 113.33(14) . . ?
C27 C26 H26A 108.9 . . ?
C27 C26 H26B 108.9 . . ?
O3 C27 C26 122.01(16) . . ?
O3 C27 C28 122.48(17) . . ?
C28 C27 C26 115.46(17) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C2S C1S H1SA 119.9 . . ?
C3S C1S H1SA 119.9 2_766 . ?
C3S C1S C2S 120.2(2) 2_766 . ?
C1S C2S H2SA 120.3 . . ?
C3S C2S C1S 119.3(3) . . ?
C3S C2S H2SA 120.3 . . ?
C1S C3S C2S 120.4(2) 2_766 . ?
C1S C3S H3SA 119.8 2_766 . ?
C2S C3S H3SA 119.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 C1 C2 C3 179.83(14) . . . . ?
P1 C1 C6 C5 -178.81(14) . . . . ?
P1 C7 C8 C9 178.41(14) . . . . ?
P1 C7 C12 C11 -178.76(14) . . . . ?
P1 C13 C26 C27 -143.98(13) . . . . ?
P2 C13 C26 C27 79.73(15) . . . . ?
P2 C14 C15 C16 -176.44(14) . . . . ?
P2 C14 C19 C18 177.08(14) . . . . ?
P2 C20 C21 C22 -179.92(14) . . . . ?
P2 C20 C25 C24 179.94(13) . . . . ?
O1 P1 C1 C2 -27.78(15) . . . . ?
O1 P1 C1 C6 151.75(15) . . . . ?
O1 P1 C7 C8 0.76(16) . . . . ?
O1 P1 C7 C12 179.29(13) . . . . ?
O1 P1 C13 P2 71.00(12) . . . . ?
O1 P1 C13 C26 -55.51(13) . . . . ?
O2 P2 C13 P1 178.91(9) . . . . ?
O2 P2 C13 C26 -53.50(12) . . . . ?
O2 P2 C14 C15 134.95(14) . . . . ?
O2 P2 C14 C19 -41.80(15) . . . . ?
O2 P2 C20 C21 -23.69(15) . . . . ?
O2 P2 C20 C25 156.66(14) . . . . ?
C1 P1 C7 C8 -119.66(14) . . . . ?
C1 P1 C7 C12 58.87(16) . . . . ?
C1 P1 C13 P2 -168.51(10) . . . . ?
C1 P1 C13 C26 64.99(12) . . . . ?
C1 C2 C3 C4 -1.4(3) . . . . ?
C2 C1 C6 C5 0.7(3) . . . . ?
C2 C3 C4 C5 1.5(3) . . . . ?
C3 C4 C5 C6 -0.5(3) . . . . ?
C4 C5 C6 C1 -0.6(3) . . . . ?
C6 C1 C2 C3 0.3(3) . . . . ?
C7 P1 C1 C2 93.09(14) . . . . ?
C7 P1 C1 C6 -87.38(16) . . . . ?
C7 P1 C13 P2 -54.22(12) . . . . ?
C7 P1 C13 C26 179.28(11) . . . . ?
C7 C8 C9 C10 0.5(3) . . . . ?
C8 C7 C12 C11 -0.3(3) . . . . ?
C8 C9 C10 C11 -0.4(3) . . . . ?
C9 C10 C11 C12 0.0(3) . . . . ?
C10 C11 C12 C7 0.4(3) . . . . ?
C12 C7 C8 C9 -0.2(3) . . . . ?
C13 P1 C1 C2 -150.50(13) . . . . ?
C13 P1 C1 C6 29.03(17) . . . . ?
C13 P1 C7 C8 127.50(13) . . . . ?
C13 P1 C7 C12 -53.98(16) . . . . ?
C13 P2 C14 C15 -107.99(15) . . . . ?
C13 P2 C14 C19 75.26(14) . . . . ?
C13 P2 C20 C21 -142.69(13) . . . . ?
C13 P2 C20 C25 37.65(17) . . . . ?
C13 C26 C27 O3 30.5(2) . . . . ?
C13 C26 C27 C28 -151.98(18) . . . . ?
C14 P2 C13 P1 59.10(12) . . . . ?
C14 P2 C13 C26 -173.31(10) . . . . ?
C14 P2 C20 C21 98.52(14) . . . . ?
C14 P2 C20 C25 -81.14(16) . . . . ?
C14 C15 C16 C17 -0.2(3) . . . . ?
C15 C14 C19 C18 0.2(3) . . . . ?
C15 C16 C17 C18 -0.2(3) . . . . ?
C16 C17 C18 C19 0.6(3) . . . . ?
C17 C18 C19 C14 -0.6(3) . . . . ?
C19 C14 C15 C16 0.2(3) . . . . ?
C20 P2 C13 P1 -59.85(12) . . . . ?
C20 P2 C13 C26 67.75(12) . . . . ?
C20 P2 C14 C15 13.05(17) . . . . ?
C20 P2 C14 C19 -163.70(13) . . . . ?
C20 C21 C22 C23 0.2(3) . . . . ?
C21 C20 C25 C24 0.3(2) . . . . ?
C21 C22 C23 C24 -0.1(3) . . . . ?
C22 C23 C24 C25 0.2(3) . . . . ?
C23 C24 C25 C20 -0.3(3) . . . . ?
C25 C20 C21 C22 -0.2(3) . . . . ?
C1S C2S C3S C1S 0.2(4) . . . 2_766 ?
C3S C1S C2S C3S -0.2(4) 2_766 . . . ?

#==
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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 1442098'
_audit_update_record             
;
2015-12-13 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;
_audit_creation_date             2015-02-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C28 H26 N2 O11 P2 U'
_chemical_formula_sum            'C28 H26 N2 O11 P2 U'
_chemical_formula_weight         866.48
_chemical_melting_point          ?
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'
U U -9.6767 9.6646 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   11.3280(7)
_cell_length_b                   13.8253(9)
_cell_length_c                   19.7227(13)
_cell_angle_alpha                90
_cell_angle_beta                 104.445(1)
_cell_angle_gamma                90
_cell_volume                     2991.2(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9645
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.77
_cell_measurement_theta_min      2.37
_shelx_estimated_absorpt_T_max   0.604
_shelx_estimated_absorpt_T_min   0.359
_exptl_absorpt_coefficient_mu    5.597
_exptl_absorpt_correction_T_max  0.605
_exptl_absorpt_correction_T_min  0.359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
"'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was"
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.924
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34749
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.000
_diffrn_reflns_theta_min         2.454
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6105
_reflns_number_total             7917
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.547
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.142
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         7917
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0275
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0223P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0571
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
U1 U 0.76352(2) 0.02692(2) 0.52320(2) 0.01078(4) Uani 1 1 d . . . . .
P1 P 0.88031(8) 0.27142(6) 0.58635(5) 0.01043(18) Uani 1 1 d . . . . .
P2 P 0.77836(8) 0.16162(6) 0.68835(5) 0.01087(18) Uani 1 1 d . . . . .
O1 O 0.6227(2) 0.08673(18) 0.49409(13) 0.0157(5) Uani 1 1 d . . . . .
O2 O 0.9029(2) -0.03489(19) 0.55170(13) 0.0188(5) Uani 1 1 d . . . . .
O3 O 0.8704(2) 0.17713(17) 0.54774(12) 0.0125(5) Uani 1 1 d . . . . .
O4 O 0.7709(2) 0.07552(17) 0.64090(12) 0.0133(5) Uani 1 1 d . . . . .
O5 O 0.6685(2) -0.08787(18) 0.59323(13) 0.0170(5) Uani 1 1 d . . . . .
O6 O 0.6603(2) -0.13413(19) 0.48804(14) 0.0206(6) Uani 1 1 d . . . . .
O7 O 0.7447(3) -0.03389(19) 0.40125(13) 0.0221(6) Uani 1 1 d . . . . .
O8 O 0.8204(2) 0.10834(18) 0.42035(13) 0.0186(6) Uani 1 1 d . . . . .
O9 O 0.6516(2) 0.44916(19) 0.63740(15) 0.0260(7) Uani 1 1 d . . . . .
O10 O 0.5864(2) -0.22749(18) 0.55629(14) 0.0199(6) Uani 1 1 d . . . . .
O11 O 0.7912(3) 0.04548(19) 0.31594(13) 0.0243(6) Uani 1 1 d . . . . .
N1 N 0.6361(3) -0.1527(2) 0.54654(16) 0.0159(7) Uani 1 1 d . . . . .
N2 N 0.7862(3) 0.0401(2) 0.37658(16) 0.0170(7) Uani 1 1 d . . . . .
C1 C 0.7686(3) 0.2739(2) 0.63883(18) 0.0115(7) Uani 1 1 d . . . . .
H1 H 0.7886 0.3290 0.6726 0.014 Uiso 1 1 calc R . . . .
C2 C 0.6385(3) 0.2893(3) 0.59171(18) 0.0131(7) Uani 1 1 d . . . . .
H2A H 0.6396 0.2791 0.5422 0.016 Uiso 1 1 calc R . . . .
H2B H 0.5830 0.2406 0.6038 0.016 Uiso 1 1 calc R . . . .
C3 C 0.5902(3) 0.3890(3) 0.5997(2) 0.0192(8) Uani 1 1 d . . . . .
C4 C 0.4614(4) 0.4083(4) 0.5594(3) 0.0473(15) Uani 1 1 d . . . . .
H4A H 0.4550 0.4009 0.5092 0.071 Uiso 1 1 calc GR . . . .
H4B H 0.4385 0.4744 0.5689 0.071 Uiso 1 1 calc GR . . . .
H4C H 0.4066 0.3623 0.5738 0.071 Uiso 1 1 calc GR . . . .
C5 C 0.8503(3) 0.3707(2) 0.52676(18) 0.0116(7) Uani 1 1 d . . . . .
C6 C 0.8154(3) 0.3513(3) 0.45540(19) 0.0164(8) Uani 1 1 d . . . . .
H6 H 0.8023 0.2865 0.4393 0.020 Uiso 1 1 calc R . . . .
C7 C 0.7997(3) 0.4269(3) 0.40771(19) 0.0173(8) Uani 1 1 d . . . . .
H7 H 0.7756 0.4139 0.3589 0.021 Uiso 1 1 calc R . . . .
C8 C 0.8191(3) 0.5208(3) 0.43112(19) 0.0155(7) Uani 1 1 d . . . . .
H8 H 0.8095 0.5723 0.3983 0.019 Uiso 1 1 calc R . . . .
C9 C 0.8526(3) 0.5409(3) 0.50255(19) 0.0156(8) Uani 1 1 d . . . . .
H9 H 0.8647 0.6059 0.5184 0.019 Uiso 1 1 calc R . . . .
C10 C 0.8681(3) 0.4661(3) 0.55021(18) 0.0136(7) Uani 1 1 d . . . . .
H10 H 0.8910 0.4795 0.5990 0.016 Uiso 1 1 calc R . . . .
C11 C 1.0299(3) 0.2891(2) 0.64179(18) 0.0120(7) Uani 1 1 d . . . . .
C12 C 1.0533(3) 0.3561(3) 0.69685(18) 0.0141(7) Uani 1 1 d . . . . .
H12 H 0.9881 0.3912 0.7075 0.017 Uiso 1 1 calc R . . . .
C13 C 1.1722(3) 0.3712(3) 0.73590(19) 0.0169(8) Uani 1 1 d . . . . .
H13 H 1.1887 0.4171 0.7729 0.020 Uiso 1 1 calc R . . . .
C14 C 1.2664(3) 0.3187(3) 0.7205(2) 0.0200(8) Uani 1 1 d . . . . .
H14 H 1.3476 0.3288 0.7474 0.024 Uiso 1 1 calc R . . . .
C15 C 1.2442(3) 0.2518(3) 0.6666(2) 0.0183(8) Uani 1 1 d . . . . .
H15 H 1.3097 0.2162 0.6568 0.022 Uiso 1 1 calc R . . . .
C16 C 1.1255(3) 0.2369(3) 0.62690(19) 0.0156(8) Uani 1 1 d . . . . .
H16 H 1.1098 0.1913 0.5897 0.019 Uiso 1 1 calc R . . . .
C17 C 0.6553(3) 0.1608(3) 0.73083(18) 0.0127(7) Uani 1 1 d . . . . .
C18 C 0.5849(3) 0.0771(3) 0.72502(18) 0.0157(7) Uani 1 1 d . . . . .
H18 H 0.5957 0.0264 0.6946 0.019 Uiso 1 1 calc R . . . .
C19 C 0.4989(3) 0.0684(3) 0.7638(2) 0.0217(8) Uani 1 1 d . . . . .
H19 H 0.4506 0.0116 0.7600 0.026 Uiso 1 1 calc R . . . .
C20 C 0.4833(3) 0.1424(3) 0.8080(2) 0.0208(8) Uani 1 1 d . . . . .
H20 H 0.4258 0.1354 0.8355 0.025 Uiso 1 1 calc R . . . .
C21 C 0.5512(3) 0.2267(3) 0.8123(2) 0.0187(8) Uani 1 1 d . . . . .
H21 H 0.5397 0.2775 0.8424 0.022 Uiso 1 1 calc R . . . .
C22 C 0.6357(3) 0.2367(3) 0.77262(19) 0.0157(8) Uani 1 1 d . . . . .
H22 H 0.6801 0.2953 0.7741 0.019 Uiso 1 1 calc R . . . .
C23 C 0.9200(3) 0.1628(2) 0.75379(17) 0.0116(7) Uani 1 1 d . . . . .
C24 C 1.0131(3) 0.1026(2) 0.74442(18) 0.0132(7) Uani 1 1 d . . . . .
H24 H 0.9984 0.0584 0.7064 0.016 Uiso 1 1 calc R . . . .
C25 C 1.1277(3) 0.1073(3) 0.79102(18) 0.0158(8) Uani 1 1 d . . . . .
H25 H 1.1917 0.0666 0.7846 0.019 Uiso 1 1 calc R . . . .
C26 C 1.1482(3) 0.1709(3) 0.84650(19) 0.0168(8) Uani 1 1 d . . . . .
H26 H 1.2264 0.1736 0.8783 0.020 Uiso 1 1 calc R . . . .
C27 C 1.0562(3) 0.2311(3) 0.85653(18) 0.0166(8) Uani 1 1 d . . . . .
H27 H 1.0716 0.2748 0.8949 0.020 Uiso 1 1 calc R . . . .
C28 C 0.9423(3) 0.2273(3) 0.81067(18) 0.0150(7) Uani 1 1 d . . . . .
H28 H 0.8789 0.2682 0.8176 0.018 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
U1 O1 1.761(2) . ?
U1 O2 1.760(2) . ?
U1 O3 2.392(2) . ?
U1 O4 2.398(2) . ?
U1 O5 2.515(2) . ?
U1 O6 2.530(3) . ?
U1 O7 2.506(3) . ?
U1 O8 2.540(3) . ?
U1 N1 2.965(3) . ?
U1 N2 2.972(3) . ?
P1 O3 1.500(2) . ?
P1 C1 1.824(3) . ?
P1 C5 1.783(4) . ?
P1 C11 1.790(3) . ?
P2 O4 1.503(2) . ?
P2 C1 1.823(3) . ?
P2 C17 1.796(4) . ?
P2 C23 1.791(3) . ?
O5 N1 1.272(4) . ?
O6 N1 1.277(4) . ?
O7 N2 1.272(4) . ?
O8 N2 1.272(4) . ?
O9 C3 1.213(4) . ?
O10 N1 1.215(4) . ?
O11 N2 1.213(4) . ?
C1 H1 1.0000 . ?
C1 C2 1.548(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.506(5) . ?
C3 C4 1.501(5) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.390(5) . ?
C5 C10 1.396(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.388(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.377(5) . ?
C8 H8 0.9500 . ?
C8 C9 1.392(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.379(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.402(5) . ?
C11 C16 1.392(5) . ?
C12 H12 0.9500 . ?
C12 C13 1.390(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.385(5) . ?
C14 H14 0.9500 . ?
C14 C15 1.384(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.392(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.394(5) . ?
C17 C22 1.386(5) . ?
C18 H18 0.9500 . ?
C18 C19 1.385(5) . ?
C19 H19 0.9500 . ?
C19 C20 1.383(6) . ?
C20 H20 0.9500 . ?
C20 C21 1.387(6) . ?
C21 H21 0.9500 . ?
C21 C22 1.386(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.392(5) . ?
C23 C28 1.405(5) . ?
C24 H24 0.9500 . ?
C24 C25 1.393(5) . ?
C25 H25 0.9500 . ?
C25 C26 1.378(5) . ?
C26 H26 0.9500 . ?
C26 C27 1.385(5) . ?
C27 H27 0.9500 . ?
C27 C28 1.380(5) . ?
C28 H28 0.9500 . ?

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 U1 O3 91.71(10) . . ?
O1 U1 O4 89.66(10) . . ?
O1 U1 O5 89.91(10) . . ?
O1 U1 O6 90.26(10) . . ?
O1 U1 O7 89.51(10) . . ?
O1 U1 O8 85.49(10) . . ?
O1 U1 N1 90.41(10) . . ?
O1 U1 N2 86.86(10) . . ?
O2 U1 O1 178.93(12) . . ?
O2 U1 O3 89.34(10) . . ?
O2 U1 O4 90.86(10) . . ?
O2 U1 O5 89.48(10) . . ?
O2 U1 O6 88.68(11) . . ?
O2 U1 O7 89.91(11) . . ?
O2 U1 O8 94.82(10) . . ?
O2 U1 N1 88.66(10) . . ?
O2 U1 N2 92.99(10) . . ?
O3 U1 O4 70.55(8) . . ?
O3 U1 O5 134.51(8) . . ?
O3 U1 O6 174.64(8) . . ?
O3 U1 O7 113.77(8) . . ?
O3 U1 O8 63.91(8) . . ?
O3 U1 N1 159.57(8) . . ?
O3 U1 N2 88.93(8) . . ?
O4 U1 O5 64.00(8) . . ?
O4 U1 O6 114.45(8) . . ?
O4 U1 O7 175.62(8) . . ?
O4 U1 O8 133.98(8) . . ?
O4 U1 N1 89.15(8) . . ?
O4 U1 N2 159.08(8) . . ?
O5 U1 O6 50.46(8) . . ?
O5 U1 O8 161.25(8) . . ?
O5 U1 N1 25.15(8) . . ?
O5 U1 N2 136.54(8) . . ?
O6 U1 O8 111.30(8) . . ?
O6 U1 N1 25.31(8) . . ?
O6 U1 N2 86.20(8) . . ?
O7 U1 O5 111.70(8) . . ?
O7 U1 O6 61.25(8) . . ?
O7 U1 O8 50.20(8) . . ?
O7 U1 N1 86.56(9) . . ?
O7 U1 N2 25.06(8) . . ?
O8 U1 N1 136.52(8) . . ?
O8 U1 N2 25.15(8) . . ?
N1 U1 N2 111.48(8) . . ?
O3 P1 C1 109.26(15) . . ?
O3 P1 C5 110.88(15) . . ?
O3 P1 C11 111.62(15) . . ?
C5 P1 C1 108.31(16) . . ?
C5 P1 C11 107.08(16) . . ?
C11 P1 C1 109.63(16) . . ?
O4 P2 C1 110.75(15) . . ?
O4 P2 C17 110.82(16) . . ?
O4 P2 C23 110.92(15) . . ?
C17 P2 C1 107.76(16) . . ?
C23 P2 C1 107.57(16) . . ?
C23 P2 C17 108.89(16) . . ?
P1 O3 U1 145.85(14) . . ?
P2 O4 U1 143.84(15) . . ?
N1 O5 U1 97.6(2) . . ?
N1 O6 U1 96.8(2) . . ?
N2 O7 U1 98.4(2) . . ?
N2 O8 U1 96.80(19) . . ?
O5 N1 U1 57.22(17) . . ?
O5 N1 O6 115.1(3) . . ?
O6 N1 U1 57.93(17) . . ?
O10 N1 U1 178.4(2) . . ?
O10 N1 O5 123.1(3) . . ?
O10 N1 O6 121.7(3) . . ?
O7 N2 U1 56.54(17) . . ?
O8 N2 U1 58.05(16) . . ?
O8 N2 O7 114.6(3) . . ?
O11 N2 U1 177.8(3) . . ?
O11 N2 O7 122.6(3) . . ?
O11 N2 O8 122.8(3) . . ?
P1 C1 H1 108.6 . . ?
P2 C1 P1 109.27(18) . . ?
P2 C1 H1 108.6 . . ?
C2 C1 P1 110.7(2) . . ?
C2 C1 P2 111.1(2) . . ?
C2 C1 H1 108.6 . . ?
C1 C2 H2A 109.2 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
C3 C2 C1 112.3(3) . . ?
C3 C2 H2A 109.2 . . ?
C3 C2 H2B 109.2 . . ?
O9 C3 C2 121.6(3) . . ?
O9 C3 C4 122.4(4) . . ?
C4 C3 C2 116.0(3) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 P1 118.6(3) . . ?
C6 C5 C10 119.9(3) . . ?
C10 C5 P1 121.4(3) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 C5 119.8(3) . . ?
C7 C6 H6 120.1 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 C6 120.0(3) . . ?
C8 C7 H7 120.0 . . ?
C7 C8 H8 119.7 . . ?
C7 C8 C9 120.5(3) . . ?
C9 C8 H8 119.7 . . ?
C8 C9 H9 120.1 . . ?
C10 C9 C8 119.8(3) . . ?
C10 C9 H9 120.1 . . ?
C5 C10 H10 120.0 . . ?
C9 C10 C5 120.0(3) . . ?
C9 C10 H10 120.0 . . ?
C12 C11 P1 122.1(3) . . ?
C16 C11 P1 117.9(3) . . ?
C16 C11 C12 119.9(3) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 C11 119.9(3) . . ?
C13 C12 H12 120.1 . . ?
C12 C13 H13 120.2 . . ?
C14 C13 C12 119.5(4) . . ?
C14 C13 H13 120.2 . . ?
C13 C14 H14 119.5 . . ?
C15 C14 C13 121.0(3) . . ?
C15 C14 H14 119.5 . . ?
C14 C15 H15 120.1 . . ?
C14 C15 C16 119.8(4) . . ?
C16 C15 H15 120.1 . . ?
C11 C16 H16 120.1 . . ?
C15 C16 C11 119.9(4) . . ?
C15 C16 H16 120.1 . . ?
C18 C17 P2 117.5(3) . . ?
C22 C17 P2 122.0(3) . . ?
C22 C17 C18 120.3(3) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 C17 119.6(4) . . ?
C19 C18 H18 120.2 . . ?
C18 C19 H19 119.9 . . ?
C20 C19 C18 120.1(4) . . ?
C20 C19 H19 119.9 . . ?
C19 C20 H20 119.9 . . ?
C19 C20 C21 120.2(4) . . ?
C21 C20 H20 119.9 . . ?
C20 C21 H21 120.0 . . ?
C22 C21 C20 120.0(4) . . ?
C22 C21 H21 120.0 . . ?
C17 C22 H22 120.2 . . ?
C21 C22 C17 119.7(4) . . ?
C21 C22 H22 120.2 . . ?
C24 C23 P2 118.1(3) . . ?
C24 C23 C28 119.6(3) . . ?
C28 C23 P2 122.1(3) . . ?
C23 C24 H24 120.1 . . ?
C23 C24 C25 119.8(3) . . ?
C25 C24 H24 120.1 . . ?
C24 C25 H25 120.1 . . ?
C26 C25 C24 119.9(3) . . ?
C26 C25 H25 120.1 . . ?
C25 C26 H26 119.6 . . ?
C25 C26 C27 120.9(3) . . ?
C27 C26 H26 119.6 . . ?
C26 C27 H27 120.1 . . ?
C28 C27 C26 119.8(3) . . ?
C28 C27 H27 120.1 . . ?
C23 C28 H28 120.0 . . ?
C27 C28 C23 120.0(3) . . ?
C27 C28 H28 120.0 . . ?

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
U1 O5 N1 O6 -1.3(3) . . . . ?
U1 O5 N1 O10 178.2(3) . . . . ?
U1 O6 N1 O5 1.3(3) . . . . ?
U1 O6 N1 O10 -178.2(3) . . . . ?
U1 O7 N2 O8 1.5(3) . . . . ?
U1 O7 N2 O11 -177.6(3) . . . . ?
U1 O8 N2 O7 -1.5(3) . . . . ?
U1 O8 N2 O11 177.6(3) . . . . ?
P1 C1 C2 C3 -107.8(3) . . . . ?
P1 C5 C6 C7 -175.5(3) . . . . ?
P1 C5 C10 C9 175.3(3) . . . . ?
P1 C11 C12 C13 -176.3(3) . . . . ?
P1 C11 C16 C15 177.0(3) . . . . ?
P2 C1 C2 C3 130.6(3) . . . . ?
P2 C17 C18 C19 172.1(3) . . . . ?
P2 C17 C22 C21 -170.6(3) . . . . ?
P2 C23 C24 C25 174.7(3) . . . . ?
P2 C23 C28 C27 -174.6(3) . . . . ?
O3 P1 C1 P2 48.5(2) . . . . ?
O3 P1 C1 C2 -74.1(3) . . . . ?
O3 P1 C5 C6 3.8(3) . . . . ?
O3 P1 C5 C10 -172.3(3) . . . . ?
O3 P1 C11 C12 -161.8(3) . . . . ?
O3 P1 C11 C16 21.1(3) . . . . ?
O4 P2 C1 P1 -51.8(2) . . . . ?
O4 P2 C1 C2 70.6(3) . . . . ?
O4 P2 C17 C18 10.6(3) . . . . ?
O4 P2 C17 C22 -174.4(3) . . . . ?
O4 P2 C23 C24 14.4(3) . . . . ?
O4 P2 C23 C28 -170.4(3) . . . . ?
C1 P1 O3 U1 2.6(3) . . . . ?
C1 P1 C5 C6 -116.0(3) . . . . ?
C1 P1 C5 C10 67.8(3) . . . . ?
C1 P1 C11 C12 -40.6(3) . . . . ?
C1 P1 C11 C16 142.3(3) . . . . ?
C1 P2 O4 U1 5.8(3) . . . . ?
C1 P2 C17 C18 132.0(3) . . . . ?
C1 P2 C17 C22 -53.0(3) . . . . ?
C1 P2 C23 C24 -106.8(3) . . . . ?
C1 P2 C23 C28 68.4(3) . . . . ?
C1 C2 C3 O9 2.7(5) . . . . ?
C1 C2 C3 C4 -176.2(4) . . . . ?
C5 P1 O3 U1 -116.7(3) . . . . ?
C5 P1 C1 P2 169.39(17) . . . . ?
C5 P1 C1 C2 46.8(3) . . . . ?
C5 P1 C11 C12 76.7(3) . . . . ?
C5 P1 C11 C16 -100.4(3) . . . . ?
C5 C6 C7 C8 0.2(6) . . . . ?
C6 C5 C10 C9 -0.8(5) . . . . ?
C6 C7 C8 C9 -1.0(6) . . . . ?
C7 C8 C9 C10 0.9(5) . . . . ?
C8 C9 C10 C5 0.0(5) . . . . ?
C10 C5 C6 C7 0.7(5) . . . . ?
C11 P1 O3 U1 124.0(3) . . . . ?
C11 P1 C1 P2 -74.1(2) . . . . ?
C11 P1 C1 C2 163.3(2) . . . . ?
C11 P1 C5 C6 125.8(3) . . . . ?
C11 P1 C5 C10 -50.3(3) . . . . ?
C11 C12 C13 C14 -0.8(5) . . . . ?
C12 C11 C16 C15 -0.2(5) . . . . ?
C12 C13 C14 C15 0.3(5) . . . . ?
C13 C14 C15 C16 0.2(6) . . . . ?
C14 C15 C16 C11 -0.3(5) . . . . ?
C16 C11 C12 C13 0.7(5) . . . . ?
C17 P2 O4 U1 125.3(2) . . . . ?
C17 P2 C1 P1 -173.17(17) . . . . ?
C17 P2 C1 C2 -50.8(3) . . . . ?
C17 P2 C23 C24 136.7(3) . . . . ?
C17 P2 C23 C28 -48.2(3) . . . . ?
C17 C18 C19 C20 0.0(6) . . . . ?
C18 C17 C22 C21 4.2(5) . . . . ?
C18 C19 C20 C21 1.7(6) . . . . ?
C19 C20 C21 C22 -0.5(6) . . . . ?
C20 C21 C22 C17 -2.5(5) . . . . ?
C22 C17 C18 C19 -3.0(5) . . . . ?
C23 P2 O4 U1 -113.6(2) . . . . ?
C23 P2 C1 P1 69.6(2) . . . . ?
C23 P2 C1 C2 -168.0(2) . . . . ?
C23 P2 C17 C18 -111.6(3) . . . . ?
C23 P2 C17 C22 63.4(3) . . . . ?
C23 C24 C25 C26 0.5(5) . . . . ?
C24 C23 C28 C27 0.5(5) . . . . ?
C24 C25 C26 C27 -0.3(5) . . . . ?
C25 C26 C27 C28 0.2(5) . . . . ?
C26 C27 C28 C23 -0.3(5) . . . . ?
C28 C23 C24 C25 -0.6(5) . . . . ?

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1442099'
_audit_update_record             
;
2015-12-13 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;
_audit_creation_date             2015-02-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C56 H52 N2 O18 P4 U2, C2 H6 O'
_chemical_formula_sum            'C58 H58 N2 O19 P4 U2'
_chemical_formula_weight         1687.00
_chemical_melting_point          ?
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.2266(7)
_cell_length_b                   17.8372(7)
_cell_length_c                   19.0939(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6207.6(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    100
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.387
_exptl_absorpt_correction_T_max  0.400
_exptl_absorpt_correction_T_min  0.172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            62107
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         2.133
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  apex
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4803
_reflns_number_total             6743
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         2.163
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.180
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6743
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0650
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0700P)²+28.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1463
_refine_ls_wR_factor_ref         0.1578
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Others
 Fixed Sof: O6'(0.5) O7(0.5) O1(0.5) O2(0.5) O1A(0.5) O2A(0.5) O11(0.5)
 H11(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5) C2S(0.5) H2SA(0.5) H2SB(0.5) H2SC(0.5)
 Fixed Uiso: H1(0.064) H2A(0.07) H2B(0.07) H4A(0.107) H4B(0.107) H4C(0.107)
 H6(0.079) H7(0.09) H8(0.098) H9(0.1) H10(0.087) H12(0.075) H13(0.086)
 H14(0.097) H15(0.087) H16(0.076) H18(0.079) H19(0.086) H20(0.078) H21(0.082)
 H22(0.08) H24(0.09) H25(0.104) H26(0.102) H27(0.081) H28(0.074) H11(0.059)
 H1SA(0.111) H1SB(0.111) H2SA(0.115) H2SB(0.115) H2SC(0.115)
 Fixed X: H1(0.3028) H2A(0.4463) H2B(0.3856) H4A(0.4303) H4B(0.4679)
 H4C(0.4881) H6(0.303) H7(0.2289) H8(0.1295) H9(0.1078) H10(0.1823) H12(0.3035)
 H13(0.234) H14(0.1377) H15(0.1076) H16(0.1777) H18(0.3968) H19(0.4867)
 H20(0.5978) H21(0.6226) H22(0.5354) H24(0.3496) H25(0.2601) H26(0.186)
 H27(0.194) H28(0.2814) H11(0.5168) H1SA(0.4885) H1SB(0.4353) H2SA(0.399)
 H2SB(0.4312) H2SC(0.3643)
 Fixed Y: H1(0.2193) H2A(0.2683) H2B(0.3228) H4A(0.207) H4B(0.2736)
 H4C(0.1883) H6(0.4827) H7(0.5447) H8(0.4833) H9(0.3586) H10(0.2931)
 H12(0.3932) H13(0.3705) H14(0.2846) H15(0.2245) H16(0.2439) H18(0.0955)
 H19(0.0077) H20(0.0026) H21(0.0838) H22(0.1698) H24(0.1945) H25(0.1253)
 H26(0.0425) H27(0.0292) H28(0.0976) H11(0.4144) H1SA(0.5082) H1SB(0.4826)
 H2SA(0.4891) H2SB(0.409) H2SC(0.4272)
 Fixed Z: H1(0.0837) H2A(0.1117) H2B(0.1444) H4A(0.2881) H4B(0.2448)
 H4C(0.2275) H6(0.0983) H7(0.1764) H8(0.2282) H9(0.2051) H10(0.1251) H12(-
 0.1039) H13(-0.2053) H14(-0.2013) H15(-0.0991) H16(0.0028) H18(0.1031)
 H19(0.1356) H20(0.0807) H21(-0.0114) H22(-0.0475) H24(-0.1494) H25(-0.2111)
 H26(-0.1511) H27(-0.0303) H28(0.0317) H11(0.147) H1SA(0.2294) H1SB(0.1677)
 H2SA(0.2861) H2SB(0.2868) H2SC(0.2395)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
U1 U 0.48371(2) 0.38988(2) -0.03909(2) 0.06338(15) Uani 1 1 d D . . . .
P1 P 0.30430(11) 0.34030(12) 0.03358(12) 0.0520(5) Uani 1 1 d . . . . .
P2 P 0.39128(12) 0.20820(12) -0.00717(12) 0.0539(5) Uani 1 1 d . . . . .
O5 O 0.6098(3) 0.4090(4) -0.0902(4) 0.0677(17) Uani 1 1 d . . . . .
O6 O 0.5623(4) 0.3034(3) -0.1143(4) 0.080(2) Uani 1 1 d . . . . .
O6' O 0.6530(8) 0.3381(8) -0.1725(8) 0.072(4) Uiso 0.5 1 d . U P A 1
O7 O 0.6797(7) 0.3339(7) -0.1436(7) 0.056(3) Uiso 0.5 1 d . U P A 2
O8 O 0.4260(3) 0.2659(3) -0.0526(3) 0.0586(14) Uani 1 1 d . . . . .
O9 O 0.3649(3) 0.3931(3) 0.0147(3) 0.0561(13) Uani 1 1 d . . . . .
O10 O 0.3341(4) 0.1788(5) 0.1951(4) 0.093(2) Uani 1 1 d . . . . .
N1 N 0.6142(5) 0.3489(4) -0.1216(5) 0.074(2) Uani 1 1 d . . . . .
C1 C 0.3432(5) 0.2528(5) 0.0671(4) 0.0536(18) Uani 1 1 d . . . . .
H1 H 0.3028 0.2193 0.0837 0.064 Uiso 1 1 calc R . . . .
C2 C 0.3950(5) 0.2708(5) 0.1285(5) 0.059(2) Uani 1 1 d . . . . .
H2A H 0.4463 0.2683 0.1117 0.070 Uiso 1 1 calc R . . . .
H2B H 0.3856 0.3228 0.1444 0.070 Uiso 1 1 calc R . . . .
C3 C 0.3864(6) 0.2193(7) 0.1887(5) 0.071(3) Uani 1 1 d . . . . .
C4 C 0.4488(7) 0.2223(8) 0.2421(6) 0.090(3) Uani 1 1 d . . . . .
H4A H 0.4303 0.2070 0.2881 0.107 Uiso 1 1 calc GR . . . .
H4B H 0.4679 0.2736 0.2448 0.107 Uiso 1 1 calc GR . . . .
H4C H 0.4881 0.1883 0.2275 0.107 Uiso 1 1 calc GR . . . .
C5 C 0.2494(5) 0.3814(5) 0.1013(5) 0.059(2) Uani 1 1 d . . . . .
C6 C 0.2628(5) 0.4571(5) 0.1191(5) 0.066(2) Uani 1 1 d . . . . .
H6 H 0.3030 0.4827 0.0983 0.079 Uiso 1 1 calc R . . . .
C7 C 0.2193(6) 0.4937(6) 0.1653(5) 0.075(3) Uani 1 1 d . . . . .
H7 H 0.2289 0.5447 0.1764 0.090 Uiso 1 1 calc R . . . .
C8 C 0.1605(6) 0.4569(8) 0.1967(6) 0.082(3) Uani 1 1 d . . . . .
H8 H 0.1295 0.4833 0.2282 0.098 Uiso 1 1 calc R . . . .
C9 C 0.1473(6) 0.3837(8) 0.1825(6) 0.083(3) Uani 1 1 d . . . . .
H9 H 0.1078 0.3586 0.2051 0.100 Uiso 1 1 calc R . . . .
C10 C 0.1916(5) 0.3445(6) 0.1347(5) 0.073(3) Uani 1 1 d . . . . .
H10 H 0.1823 0.2931 0.1251 0.087 Uiso 1 1 calc R . . . .
C11 C 0.2477(5) 0.3212(5) -0.0410(5) 0.0555(19) Uani 1 1 d . . . . .
C12 C 0.2641(5) 0.3584(5) -0.1026(5) 0.063(2) Uani 1 1 d . . . . .
H12 H 0.3035 0.3932 -0.1039 0.075 Uiso 1 1 calc R . . . .
C13 C 0.2229(6) 0.3451(6) -0.1629(5) 0.071(2) Uani 1 1 d . . . . .
H13 H 0.2340 0.3705 -0.2053 0.086 Uiso 1 1 calc R . . . .
C14 C 0.1654(6) 0.2943(7) -0.1601(6) 0.081(3) Uani 1 1 d . . . . .
H14 H 0.1377 0.2846 -0.2013 0.097 Uiso 1 1 calc R . . . .
C15 C 0.1480(5) 0.2581(6) -0.1000(6) 0.073(3) Uani 1 1 d . . . . .
H15 H 0.1076 0.2245 -0.0991 0.087 Uiso 1 1 calc R . . . .
C16 C 0.1892(5) 0.2700(5) -0.0391(5) 0.064(2) Uani 1 1 d . . . . .
H16 H 0.1777 0.2439 0.0028 0.076 Uiso 1 1 calc R . . . .
C17 C 0.4577(5) 0.1429(5) 0.0263(5) 0.061(2) Uani 1 1 d . . . . .
C18 C 0.4427(5) 0.0941(5) 0.0795(5) 0.066(2) Uani 1 1 d . . . . .
H18 H 0.3968 0.0955 0.1031 0.079 Uiso 1 1 calc R . . . .
C19 C 0.4967(5) 0.0417(5) 0.0985(6) 0.071(3) Uani 1 1 d . . . . .
H19 H 0.4867 0.0077 0.1356 0.086 Uiso 1 1 calc R . . . .
C20 C 0.5620(5) 0.0381(5) 0.0661(6) 0.065(2) Uani 1 1 d . . . . .
H20 H 0.5978 0.0026 0.0807 0.078 Uiso 1 1 calc R . . . .
C21 C 0.5766(5) 0.0862(5) 0.0119(6) 0.068(2) Uani 1 1 d . . . . .
H21 H 0.6226 0.0838 -0.0114 0.082 Uiso 1 1 calc R . . . .
C22 C 0.5253(5) 0.1376(6) -0.0091(6) 0.066(2) Uani 1 1 d . . . . .
H22 H 0.5354 0.1698 -0.0475 0.080 Uiso 1 1 calc R . . . .
C23 C 0.3237(5) 0.1533(5) -0.0536(5) 0.060(2) Uani 1 1 d . . . . .
C24 C 0.3179(6) 0.1611(6) -0.1251(5) 0.075(3) Uani 1 1 d . . . . .
H24 H 0.3496 0.1945 -0.1494 0.090 Uiso 1 1 calc R . . . .
C25 C 0.2651(7) 0.1197(6) -0.1618(6) 0.087(3) Uani 1 1 d . . . . .
H25 H 0.2601 0.1253 -0.2111 0.104 Uiso 1 1 calc R . . . .
C26 C 0.2211(7) 0.0713(6) -0.1260(6) 0.085(3) Uani 1 1 d . . . . .
H26 H 0.1860 0.0425 -0.1511 0.102 Uiso 1 1 calc R . . . .
C27 C 0.2259(6) 0.0627(5) -0.0541(5) 0.068(3) Uani 1 1 d . . . . .
H27 H 0.1940 0.0292 -0.0303 0.081 Uiso 1 1 calc R . . . .
C28 C 0.2772(5) 0.1032(4) -0.0176(5) 0.062(2) Uani 1 1 d . . . . .
H28 H 0.2814 0.0976 0.0317 0.074 Uiso 1 1 calc R . . . .
O1 O 0.5233(6) 0.3329(7) 0.0344(5) 0.055(3) Uiso 0.5 1 d D U P B 1
O2 O 0.4456(7) 0.4408(7) -0.1020(6) 0.061(3) Uiso 0.5 1 d D U P B 1
O3 O 0.4799(6) 0.4817(6) 0.0532(7) 0.065(5) Uani 0.53(3) 1 d . . . B 1
O4 O 0.5519(6) 0.4855(7) 0.0163(8) 0.057(5) Uani 0.45(2) 1 d . . . B 1
O1A O 0.5248(6) 0.3775(7) 0.0385(5) 0.057(3) Uiso 0.5 1 d D U P B 2
O2A O 0.4430(6) 0.4084(7) -0.1270(6) 0.052(3) Uiso 0.5 1 d D U P B 2
O11 O 0.5101(6) 0.4116(6) 0.1910(5) 0.049(2) Uani 0.5 1 d . . P . .
H11 H 0.5168 0.4144 0.1470 0.059 Uiso 0.5 1 d R . P . .
C1S C 0.4607(14) 0.4650(15) 0.2105(14) 0.093(7) Uani 0.5 1 d . U P . .
H1SA H 0.4885 0.5082 0.2294 0.111 Uiso 0.5 1 calc R . P . .
H1SB H 0.4353 0.4826 0.1677 0.111 Uiso 0.5 1 calc R . P . .
C2S C 0.4099(15) 0.4466(14) 0.2571(12) 0.096(8) Uani 0.5 1 d . . P . .
H2SA H 0.3990 0.4891 0.2861 0.115 Uiso 0.5 1 d R . P . .
H2SB H 0.4312 0.4090 0.2868 0.115 Uiso 0.5 1 d R . P . .
H2SC H 0.3643 0.4272 0.2395 0.115 Uiso 0.5 1 d R . 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.
;
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
U1 O5 2.520(6) . ?
U1 O6 2.549(7) . ?
U1 O8 2.463(6) . ?
U1 O9 2.397(6) . ?
U1 O1 1.877(10) . ?
U1 O2 1.658(10) . ?
U1 O3 2.399(11) 5_665 ?
U1 O3 2.407(12) . ?
U1 O4 2.355(12) 5_665 ?
U1 O4 2.361(12) . ?
U1 O1A 1.674(10) . ?
U1 O2A 1.864(10) . ?
P1 O9 1.495(6) . ?
P1 C1 1.829(8) . ?
P1 C5 1.792(9) . ?
P1 C11 1.791(9) . ?
P2 O8 1.487(6) . ?
P2 C1 1.847(9) . ?
P2 C17 1.797(9) . ?
P2 C23 1.806(9) . ?
O5 N1 1.231(9) . ?
O6 N1 1.253(10) . ?
O6' N1 1.217(15) . ?
O7 N1 1.294(14) . ?
O10 C3 1.202(12) . ?
C1 H1 1.0000 . ?
C1 C2 1.539(11) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.480(14) . ?
C3 C4 1.528(15) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.413(13) . ?
C5 C10 1.396(13) . ?
C6 H6 0.9500 . ?
C6 C7 1.354(13) . ?
C7 H7 0.9500 . ?
C7 C8 1.392(16) . ?
C8 H8 0.9500 . ?
C8 C9 1.356(16) . ?
C9 H9 0.9500 . ?
C9 C10 1.405(15) . ?
C10 H10 0.9500 . ?
C11 C12 1.385(12) . ?
C11 C16 1.403(12) . ?
C12 H12 0.9500 . ?
C12 C13 1.395(14) . ?
C13 H13 0.9500 . ?
C13 C14 1.386(15) . ?
C14 H14 0.9500 . ?
C14 C15 1.355(15) . ?
C15 H15 0.9500 . ?
C15 C16 1.399(13) . ?
C16 H16 0.9500 . ?
C17 C18 1.366(13) . ?
C17 C22 1.408(13) . ?
C18 H18 0.9500 . ?
C18 C19 1.405(13) . ?
C19 H19 0.9500 . ?
C19 C20 1.344(13) . ?
C20 H20 0.9500 . ?
C20 C21 1.371(14) . ?
C21 H21 0.9500 . ?
C21 C22 1.369(13) . ?
C22 H22 0.9500 . ?
C23 C24 1.375(13) . ?
C23 C28 1.412(13) . ?
C24 H24 0.9500 . ?
C24 C25 1.401(14) . ?
C25 H25 0.9500 . ?
C25 C26 1.364(16) . ?
C26 H26 0.9500 . ?
C26 C27 1.383(15) . ?
C27 H27 0.9500 . ?
C27 C28 1.373(12) . ?
C28 H28 0.9500 . ?
O3 U1 2.399(11) 5_665 ?
O3 O4 1.561(19) 5_665 ?
O3 O4 1.491(16) . ?
O4 U1 2.355(12) 5_665 ?
O4 O3 1.561(19) 5_665 ?
O11 H11 0.8503 . ?
O11 C1S 1.36(3) . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
C1S C2S 1.33(3) . ?
C2S H2SA 0.9600 . ?
C2S H2SB 0.9601 . ?
C2S H2SC 0.9602 . ?

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
O5 U1 O6 49.5(2) . . ?
O8 U1 O5 118.08(19) . . ?
O8 U1 O6 68.8(2) . . ?
O9 U1 O5 170.55(19) . . ?
O9 U1 O6 139.8(2) . . ?
O9 U1 O8 71.36(19) . . ?
O9 U1 O3 106.0(3) . 5_665 ?
O9 U1 O3 69.1(3) . . ?
O1 U1 O5 90.7(4) . . ?
O1 U1 O6 83.0(4) . . ?
O1 U1 O8 75.9(4) . . ?
O1 U1 O9 92.3(4) . . ?
O1 U1 O3 119.6(5) . 5_665 ?
O1 U1 O3 80.4(5) . . ?
O1 U1 O4 81.6(5) . . ?
O1 U1 O4 118.6(5) . 5_665 ?
O2 U1 O5 91.5(5) . . ?
O2 U1 O6 99.1(5) . . ?
O2 U1 O8 103.7(5) . . ?
O2 U1 O9 85.4(5) . . ?
O2 U1 O1 177.7(6) . . ?
O2 U1 O3 98.4(6) . . ?
O2 U1 O3 60.8(6) . 5_665 ?
O2 U1 O4 60.1(6) . 5_665 ?
O2 U1 O4 98.6(6) . . ?
O3 U1 O5 64.8(3) 5_665 . ?
O3 U1 O5 102.6(3) . . ?
O3 U1 O6 147.2(3) . . ?
O3 U1 O6 111.0(3) 5_665 . ?
O3 U1 O8 132.5(3) . . ?
O3 U1 O8 164.5(4) 5_665 . ?
O3 U1 O3 56.0(5) 5_665 . ?
O4 U1 O5 101.2(3) 5_665 . ?
O4 U1 O5 66.1(3) . . ?
O4 U1 O6 146.1(3) 5_665 . ?
O4 U1 O6 113.2(3) . . ?
O4 U1 O8 138.5(3) 5_665 . ?
O4 U1 O8 157.1(4) . . ?
O4 U1 O9 105.4(3) . . ?
O4 U1 O9 69.5(3) 5_665 . ?
O4 U1 O3 36.5(4) 5_665 5_665 ?
O4 U1 O3 38.3(4) . 5_665 ?
O4 U1 O3 36.4(4) . . ?
O4 U1 O3 38.2(5) 5_665 . ?
O4 U1 O4 51.7(5) 5_665 . ?
O1A U1 O5 87.3(4) . . ?
O1A U1 O6 99.6(5) . . ?
O1A U1 O8 99.5(5) . . ?
O1A U1 O9 91.6(4) . . ?
O1A U1 O2A 176.1(5) . . ?
O2A U1 O5 89.5(4) . . ?
O2A U1 O6 79.8(4) . . ?
O2A U1 O8 83.9(4) . . ?
O2A U1 O9 91.3(4) . . ?
O9 P1 C1 109.5(4) . . ?
O9 P1 C5 109.2(4) . . ?
O9 P1 C11 110.8(4) . . ?
C5 P1 C1 108.3(4) . . ?
C11 P1 C1 109.8(4) . . ?
C11 P1 C5 109.2(4) . . ?
O8 P2 C1 110.6(4) . . ?
O8 P2 C17 111.7(4) . . ?
O8 P2 C23 112.2(4) . . ?
C17 P2 C1 109.0(4) . . ?
C17 P2 C23 106.4(4) . . ?
C23 P2 C1 106.7(4) . . ?
N1 O5 U1 97.4(5) . . ?
N1 O6 U1 95.4(5) . . ?
P2 O8 U1 137.9(3) . . ?
P1 O9 U1 139.1(3) . . ?
O5 N1 U1 58.1(4) . . ?
O5 N1 O6 117.5(7) . . ?
O5 N1 O7 113.4(9) . . ?
O6 N1 U1 59.5(4) . . ?
O6 N1 O7 126.7(9) . . ?
O6' N1 U1 159.3(10) . . ?
O6' N1 O5 124.4(10) . . ?
O6' N1 O6 115.0(10) . . ?
O7 N1 U1 166.0(9) . . ?
P1 C1 P2 106.5(4) . . ?
P1 C1 H1 109.5 . . ?
P2 C1 H1 109.5 . . ?
C2 C1 P1 109.1(6) . . ?
C2 C1 P2 112.6(6) . . ?
C2 C1 H1 109.5 . . ?
C1 C2 H2A 108.9 . . ?
C1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
C3 C2 C1 113.4(8) . . ?
C3 C2 H2A 108.9 . . ?
C3 C2 H2B 108.9 . . ?
O10 C3 C2 122.5(9) . . ?
O10 C3 C4 122.8(10) . . ?
C2 C3 C4 114.7(9) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 P1 117.9(7) . . ?
C10 C5 P1 123.9(8) . . ?
C10 C5 C6 118.1(9) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 C5 121.0(10) . . ?
C7 C6 H6 119.5 . . ?
C6 C7 H7 119.9 . . ?
C6 C7 C8 120.3(10) . . ?
C8 C7 H7 119.9 . . ?
C7 C8 H8 119.8 . . ?
C9 C8 C7 120.4(10) . . ?
C9 C8 H8 119.8 . . ?
C8 C9 H9 119.8 . . ?
C8 C9 C10 120.4(11) . . ?
C10 C9 H9 119.8 . . ?
C5 C10 C9 119.8(11) . . ?
C5 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C12 C11 P1 117.4(7) . . ?
C12 C11 C16 119.8(8) . . ?
C16 C11 P1 122.8(7) . . ?
C11 C12 H12 119.9 . . ?
C11 C12 C13 120.2(9) . . ?
C13 C12 H12 119.9 . . ?
C12 C13 H13 120.4 . . ?
C14 C13 C12 119.1(10) . . ?
C14 C13 H13 120.4 . . ?
C13 C14 H14 119.3 . . ?
C15 C14 C13 121.4(10) . . ?
C15 C14 H14 119.3 . . ?
C14 C15 H15 119.8 . . ?
C14 C15 C16 120.4(9) . . ?
C16 C15 H15 119.8 . . ?
C11 C16 H16 120.5 . . ?
C15 C16 C11 119.0(9) . . ?
C15 C16 H16 120.5 . . ?
C18 C17 P2 122.9(7) . . ?
C18 C17 C22 119.3(9) . . ?
C22 C17 P2 117.5(7) . . ?
C17 C18 H18 120.8 . . ?
C17 C18 C19 118.4(9) . . ?
C19 C18 H18 120.8 . . ?
C18 C19 H19 118.8 . . ?
C20 C19 C18 122.3(10) . . ?
C20 C19 H19 118.8 . . ?
C19 C20 H20 120.4 . . ?
C19 C20 C21 119.3(9) . . ?
C21 C20 H20 120.4 . . ?
C20 C21 H21 119.7 . . ?
C22 C21 C20 120.6(9) . . ?
C22 C21 H21 119.7 . . ?
C17 C22 H22 119.9 . . ?
C21 C22 C17 120.1(10) . . ?
C21 C22 H22 119.9 . . ?
C24 C23 P2 119.0(7) . . ?
C24 C23 C28 120.1(8) . . ?
C28 C23 P2 120.9(7) . . ?
C23 C24 H24 120.1 . . ?
C23 C24 C25 119.8(10) . . ?
C25 C24 H24 120.1 . . ?
C24 C25 H25 120.4 . . ?
C26 C25 C24 119.1(10) . . ?
C26 C25 H25 120.4 . . ?
C25 C26 H26 119.0 . . ?
C25 C26 C27 122.0(10) . . ?
C27 C26 H26 119.0 . . ?
C26 C27 H27 120.3 . . ?
C28 C27 C26 119.3(9) . . ?
C28 C27 H27 120.3 . . ?
C23 C28 H28 120.2 . . ?
C27 C28 C23 119.6(9) . . ?
C27 C28 H28 120.2 . . ?
U1 O3 U1 124.0(5) 5_665 . ?
O4 O3 U1 70.1(6) . . ?
O4 O3 U1 69.5(6) 5_665 5_665 ?
O4 O3 U1 70.1(6) . 5_665 ?
O4 O3 U1 69.1(6) 5_665 . ?
O4 O3 O4 84.7(10) . 5_665 ?
U1 O4 U1 128.3(5) 5_665 . ?
O3 O4 U1 72.2(6) 5_665 . ?
O3 O4 U1 73.5(6) . . ?
O3 O4 U1 73.3(6) . 5_665 ?
O3 O4 U1 72.7(7) 5_665 5_665 ?
O3 O4 O3 95.3(10) . 5_665 ?
C1S O11 H11 108.9 . . ?
O11 C1S H1SA 107.8 . . ?
O11 C1S H1SB 107.8 . . ?
H1SA C1S H1SB 107.1 . . ?
C2S C1S O11 118(2) . . ?
C2S C1S H1SA 107.8 . . ?
C2S C1S H1SB 107.8 . . ?
C1S C2S H2SA 109.6 . . ?
C1S C2S H2SB 106.6 . . ?
C1S C2S H2SC 117.3 . . ?
H2SA C2S H2SB 107.1 . . ?
H2SA C2S H2SC 107.9 . . ?
H2SB C2S H2SC 107.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
U1 O5 N1 O6 -3.6(10) . . . . ?
U1 O5 N1 O6' 155.4(12) . . . . ?
U1 O5 N1 O7 -167.5(8) . . . . ?
U1 O6 N1 O5 3.5(10) . . . . ?
U1 O6 N1 O6' -157.4(10) . . . . ?
U1 O6 N1 O7 165.0(11) . . . . ?
U1 O3 O4 U1 139.8(5) . . . 5_665 ?
U1 O3 O4 U1 -139.8(5) 5_665 . . . ?
U1 O3 O4 O3 -70.1(6) 5_665 . . 5_665 ?
U1 O3 O4 O3 69.6(6) . . . 5_665 ?
P1 C1 C2 C3 136.6(7) . . . . ?
P1 C5 C6 C7 174.2(7) . . . . ?
P1 C5 C10 C9 -174.1(7) . . . . ?
P1 C11 C12 C13 178.9(7) . . . . ?
P1 C11 C16 C15 -179.6(8) . . . . ?
P2 C1 C2 C3 -105.5(8) . . . . ?
P2 C17 C18 C19 175.6(8) . . . . ?
P2 C17 C22 C21 -176.7(8) . . . . ?
P2 C23 C24 C25 -179.2(9) . . . . ?
P2 C23 C28 C27 179.4(7) . . . . ?
O8 P2 C1 P1 35.7(5) . . . . ?
O8 P2 C1 C2 -83.7(7) . . . . ?
O8 P2 C17 C18 166.8(8) . . . . ?
O8 P2 C17 C22 -19.5(9) . . . . ?
O8 P2 C23 C24 9.0(10) . . . . ?
O8 P2 C23 C28 -170.7(7) . . . . ?
O9 P1 C1 P2 -66.6(5) . . . . ?
O9 P1 C1 C2 55.1(7) . . . . ?
O9 P1 C5 C6 8.8(8) . . . . ?
O9 P1 C5 C10 -174.8(7) . . . . ?
O9 P1 C11 C12 -2.9(8) . . . . ?
O9 P1 C11 C16 176.3(7) . . . . ?
C1 P1 O9 U1 40.0(7) . . . . ?
C1 P1 C5 C6 128.0(7) . . . . ?
C1 P1 C5 C10 -55.6(9) . . . . ?
C1 P1 C11 C12 -124.0(7) . . . . ?
C1 P1 C11 C16 55.2(9) . . . . ?
C1 P2 O8 U1 33.2(6) . . . . ?
C1 P2 C17 C18 44.3(9) . . . . ?
C1 P2 C17 C22 -142.0(7) . . . . ?
C1 P2 C23 C24 130.3(8) . . . . ?
C1 P2 C23 C28 -49.5(8) . . . . ?
C1 C2 C3 O10 -15.3(14) . . . . ?
C1 C2 C3 C4 165.1(8) . . . . ?
C5 P1 O9 U1 158.4(5) . . . . ?
C5 P1 C1 P2 174.4(4) . . . . ?
C5 P1 C1 C2 -63.9(7) . . . . ?
C5 P1 C11 C12 117.4(7) . . . . ?
C5 P1 C11 C16 -63.4(9) . . . . ?
C5 C6 C7 C8 0.5(14) . . . . ?
C6 C5 C10 C9 2.3(13) . . . . ?
C6 C7 C8 C9 1.6(15) . . . . ?
C7 C8 C9 C10 -1.6(15) . . . . ?
C8 C9 C10 C5 -0.4(15) . . . . ?
C10 C5 C6 C7 -2.4(14) . . . . ?
C11 P1 O9 U1 -81.3(6) . . . . ?
C11 P1 C1 P2 55.2(5) . . . . ?
C11 P1 C1 C2 176.9(6) . . . . ?
C11 P1 C5 C6 -112.5(7) . . . . ?
C11 P1 C5 C10 63.9(9) . . . . ?
C11 C12 C13 C14 0.1(15) . . . . ?
C12 C11 C16 C15 -0.5(14) . . . . ?
C12 C13 C14 C15 0.8(17) . . . . ?
C13 C14 C15 C16 -1.6(17) . . . . ?
C14 C15 C16 C11 1.4(16) . . . . ?
C16 C11 C12 C13 -0.3(14) . . . . ?
C17 P2 O8 U1 -88.4(6) . . . . ?
C17 P2 C1 P1 158.9(4) . . . . ?
C17 P2 C1 C2 39.5(7) . . . . ?
C17 P2 C23 C24 -113.4(9) . . . . ?
C17 P2 C23 C28 66.8(8) . . . . ?
C17 C18 C19 C20 -0.2(16) . . . . ?
C18 C17 C22 C21 -2.8(15) . . . . ?
C18 C19 C20 C21 -1.0(16) . . . . ?
C19 C20 C21 C22 0.2(15) . . . . ?
C20 C21 C22 C17 1.7(15) . . . . ?
C22 C17 C18 C19 2.0(15) . . . . ?
C23 P2 O8 U1 152.2(5) . . . . ?
C23 P2 C1 P1 -86.5(5) . . . . ?
C23 P2 C1 C2 154.0(6) . . . . ?
C23 P2 C17 C18 -70.5(9) . . . . ?
C23 P2 C17 C22 103.2(8) . . . . ?
C23 C24 C25 C26 -1.0(19) . . . . ?
C24 C23 C28 C27 -0.3(14) . . . . ?
C24 C25 C26 C27 1(2) . . . . ?
C25 C26 C27 C28 -1.0(18) . . . . ?
C26 C27 C28 C23 0.5(15) . . . . ?
C28 C23 C24 C25 0.6(16) . . . . ?
O4 O3 O4 U1 70.1(6) 5_665 . . 5_665 ?
O4 O3 O4 U1 -69.7(6) 5_665 . . . ?
O4 O3 O4 O3 -0.005(0) 5_665 . . 5_665 ?

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1442100'
_audit_update_record             
;
2015-12-13 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;
_audit_creation_date             2014-04-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.03.12 svn.r2899 for OlexSys, GUI svn.r4796)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C56 H52 La N3 O15 P4, 2.33(C2 H3 N)'
_chemical_formula_sum            'C60.67 H59 La N5.33 O15 P4'
_chemical_formula_weight         1365.59
_chemical_melting_point          ?
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'
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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   13.444(8)
_cell_length_b                   17.849(9)
_cell_length_c                   26.571(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.709(14)
_cell_angle_gamma                90.00
_cell_volume                     6375(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2078
_cell_measurement_temperature    120
_cell_measurement_theta_max      22.95
_cell_measurement_theta_min      2.41
_exptl_absorpt_coefficient_mu    0.839
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   "SADABS (Sheldrick, 1998)'"
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2789
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.2178
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8845
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.69
_diffrn_reflns_theta_min         1.53
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_special_details          ?
_reflns_number_gt                4827
_reflns_number_total             8846
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.207
_refine_diff_density_min         -4.243
_refine_diff_density_rms         0.247
_refine_ls_extinction_coef       0.00155(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         8846
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.1823
_refine_ls_R_factor_gt           0.0985
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0600P)²+110.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2071
_refine_ls_wR_factor_ref         0.2451
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4S-C3S
 1.5 with sigma of 0.02
 C4S-N2S
 1 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C3S) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C8) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.008
Uanis(N2S) = Uanis(C4S) = Uanis(C3S)
4. Others
 Fixed Sof: C3S(0.16667) H3SA(0.16667) H3SB(0.16667) H3SC(0.16667)
 N2S(0.16667) C4S(0.16667)
5.a Ternary CH refined with riding coordinates:
 C1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
5.c Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC)
5.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
La1 La 0.5000 1.15924(4) 1.2500 0.0143(2) Uani 1 d . . 2 S T P
P1 P 0.41718(19) 1.13415(13) 1.10954(10) 0.0182(5) Uani 1 d . . 1 . . .
P2 P 0.5154(2) 1.00061(13) 1.15515(9) 0.0209(6) Uani 1 d . . 1 . . .
O1 O 0.4181(5) 1.1581(4) 1.1633(2) 0.0242(14) Uani 1 d . . 1 . . .
O2 O 0.5446(5) 1.0443(4) 1.2014(2) 0.0199(15) Uani 1 d . . 1 . . .
O3 O 0.5679(6) 1.0756(4) 1.0002(3) 0.0334(19) Uani 1 d . . 1 . . .
O4 O 0.5552(6) 1.2925(4) 1.2803(3) 0.0310(18) Uani 1 d . . 1 . . .
O5 O 0.5000 1.3979(5) 1.2500 0.046(3) Uani 1 d . . 2 S T P
O6 O 0.3715(6) 1.2063(4) 1.3151(3) 0.0254(16) Uani 1 d . . 1 . . .
O7 O 0.2135(6) 1.1809(6) 1.3146(4) 0.052(3) Uani 1 d . . 1 . . .
O8 O 0.3030(5) 1.1504(4) 1.2500(3) 0.0252(15) Uani 1 d . . 1 . . .
N1 N 0.5000 1.3293(5) 1.2500 0.018(2) Uani 1 d . . 2 S T P
N2 N 0.2917(7) 1.1796(5) 1.2941(3) 0.029(2) Uani 1 d . . 1 . . .
C1 C 0.5095(8) 1.0606(5) 1.0987(4) 0.022(2) Uani 1 d . . 1 . . .
H1 H 0.4862 1.0293 1.0696 0.026 Uiso 1 calc . . 1 R . .
C2 C 0.6102(8) 1.0931(6) 1.0860(4) 0.023(2) Uani 1 d . . 1 . . .
H2A H 0.6198 1.1408 1.1045 0.028 Uiso 1 calc . . 1 R . .
H2B H 0.6630 1.0580 1.0972 0.028 Uiso 1 calc . . 1 R . .
C3 C 0.6198(9) 1.1072(6) 1.0307(4) 0.030(2) Uani 1 d . . 1 . . .
C4 C 0.7024(9) 1.1620(8) 1.0155(5) 0.044(3) Uani 1 d . . 1 . . .
H4A H 0.7082 1.1624 0.9787 0.066 Uiso 1 calc . . 1 R . .
H4B H 0.7657 1.1461 1.0307 0.066 Uiso 1 calc . . 1 R . .
H4C H 0.6859 1.2124 1.0273 0.066 Uiso 1 calc . . 1 R . .
C5 C 0.4496(8) 1.2110(6) 1.0692(4) 0.026(2) Uani 1 d . . 1 . . .
C6 C 0.4994(8) 1.2711(5) 1.0909(4) 0.024(2) Uani 1 d . . 1 . . .
H6 H 0.5116 1.2723 1.1262 0.028 Uiso 1 calc . . 1 R . .
C7 C 0.5308(9) 1.3283(7) 1.0611(5) 0.045(3) Uani 1 d . . 1 . . .
H7 H 0.5695 1.3673 1.0758 0.054 Uiso 1 calc . . 1 R . .
C8 C 0.5081(10) 1.3316(6) 1.0099(4) 0.036(3) Uani 1 d . . 1 . U .
H8 H 0.5292 1.3726 0.9900 0.043 Uiso 1 calc . . 1 R . .
C9 C 0.4534(10) 1.2727(7) 0.9886(5) 0.042(3) Uani 1 d . . 1 . . .
H9 H 0.4363 1.2735 0.9538 0.050 Uiso 1 calc . . 1 R . .
C10 C 0.4242(9) 1.2131(6) 1.0186(4) 0.032(3) Uani 1 d . . 1 . . .
H10 H 0.3864 1.1734 1.0042 0.039 Uiso 1 calc . . 1 R . .
C11 C 0.3002(8) 1.0983(5) 1.0896(4) 0.024(2) Uani 1 d . . 1 . . .
C12 C 0.2172(8) 1.1123(6) 1.1194(5) 0.035(3) Uani 1 d . . 1 . . .
H12 H 0.2239 1.1422 1.1488 0.042 Uiso 1 calc . . 1 R . .
C13 C 0.1257(10) 1.0830(7) 1.1062(6) 0.047(4) Uani 1 d . . 1 . . .
H13 H 0.0696 1.0928 1.1265 0.057 Uiso 1 calc . . 1 R . .
C14 C 0.1153(10) 1.0395(7) 1.0636(6) 0.049(4) Uani 1 d . . 1 . . .
H14 H 0.0520 1.0192 1.0549 0.059 Uiso 1 calc . . 1 R . .
C15 C 0.1944(10) 1.0254(7) 1.0340(6) 0.049(4) Uani 1 d . . 1 . . .
H15 H 0.1860 0.9959 1.0045 0.058 Uiso 1 calc . . 1 R . .
C16 C 0.2890(8) 1.0541(6) 1.0464(5) 0.031(3) Uani 1 d . . 1 . . .
H16 H 0.3445 1.0437 1.0257 0.038 Uiso 1 calc . . 1 R . .
C17 C 0.3989(8) 0.9536(5) 1.1597(4) 0.022(2) Uani 1 d . . 1 . . .
C18 C 0.3263(8) 0.9815(7) 1.1904(4) 0.029(2) Uani 1 d . . 1 . . .
H18 H 0.3385 1.0261 1.2089 0.035 Uiso 1 calc . . 1 R . .
C19 C 0.2366(9) 0.9458(6) 1.1946(5) 0.035(3) Uani 1 d . . 1 . . .
H19 H 0.1867 0.9663 1.2156 0.042 Uiso 1 calc . . 1 R . .
C20 C 0.2179(9) 0.8784(7) 1.1676(5) 0.037(3) Uani 1 d . . 1 . . .
H20 H 0.1561 0.8530 1.1705 0.044 Uiso 1 calc . . 1 R . .
C21 C 0.2907(11) 0.8511(7) 1.1377(5) 0.046(3) Uani 1 d . . 1 . . .
H21 H 0.2786 0.8058 1.1199 0.055 Uiso 1 calc . . 1 R . .
C22 C 0.3827(9) 0.8868(6) 1.1316(5) 0.035(3) Uani 1 d . . 1 . . .
H22 H 0.4318 0.8673 1.1099 0.042 Uiso 1 calc . . 1 R . .
C23 C 0.6081(7) 0.9294(5) 1.1445(4) 0.022(2) Uani 1 d . . 1 . . .
C24 C 0.6424(8) 0.9078(6) 1.0984(4) 0.030(2) Uani 1 d . . 1 . . .
H24 H 0.6152 0.9294 1.0685 0.036 Uiso 1 calc . . 1 R . .
C25 C 0.7185(9) 0.8534(7) 1.0952(5) 0.037(3) Uani 1 d . . 1 . . .
H25 H 0.7465 0.8409 1.0637 0.045 Uiso 1 calc . . 1 R . .
C26 C 0.7519(9) 0.8181(7) 1.1393(5) 0.038(3) Uani 1 d . . 1 . . .
H26 H 0.7995 0.7790 1.1373 0.046 Uiso 1 calc . . 1 R . .
C27 C 0.7174(10) 0.8391(8) 1.1841(5) 0.048(3) Uani 1 d . . 1 . . .
H27 H 0.7424 0.8158 1.2138 0.058 Uiso 1 calc . . 1 R . .
C28 C 0.6461(9) 0.8941(7) 1.1877(5) 0.037(3) Uani 1 d . . 1 . . .
H28 H 0.6223 0.9082 1.2198 0.045 Uiso 1 calc . . 1 R . .
N3S N 0.8671(8) 1.0487(8) 1.0841(5) 0.058(4) Uani 1 d . . 1 . . .
C1S C 0.8684(10) 1.0307(8) 1.1254(6) 0.054(4) Uani 1 d . . 1 . . .
C2S C 0.8695(15) 1.0068(11) 1.1787(7) 0.086(7) Uani 1 d . . 1 . . .
H2SA H 0.9140 0.9637 1.1829 0.129 Uiso 1 calc . . 1 R . .
H2SB H 0.8020 0.9926 1.1886 0.129 Uiso 1 calc . . 1 R . .
H2SC H 0.8930 1.0481 1.2000 0.129 Uiso 1 calc . . 1 R . .
C3S C 0.5000 0.750(3) 1.2500 0.079(11) Uani 0.33 d . . 2 DS TU P
H3SA H 0.4438 0.7687 1.2697 0.119 Uiso 0.17 calc A -1 1 R . .
H3SB H 0.4938 0.7687 1.2153 0.119 Uiso 0.17 calc A -1 1 R . .
H3SC H 0.5624 0.7687 1.2650 0.119 Uiso 0.17 calc A -1 1 R . .
N2S N 0.5000 0.614(3) 1.2500 0.079(11) Uani 0.33 d . . 2 DS T P
C4S C 0.5000 0.669(3) 1.2500 0.079(11) Uani 0.33 d . . 2 DS T 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. 
;
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 2.541(6) . ?
La1 O1 2.541(6) 2_657 ?
La1 O2 2.501(7) 2_657 ?
La1 O2 2.501(7) . ?
La1 O4 2.615(7) 2_657 ?
La1 O4 2.615(7) . ?
La1 O6 2.599(7) . ?
La1 O6 2.599(8) 2_657 ?
La1 O8 2.653(6) 2_657 ?
La1 O8 2.653(6) . ?
La1 N1 3.035(9) . ?
P1 O1 1.491(7) . ?
P1 C1 1.832(10) . ?
P1 C5 1.798(11) . ?
P1 C11 1.773(10) . ?
P2 O2 1.504(7) . ?
P2 C1 1.843(10) . ?
P2 C17 1.783(10) . ?
P2 C23 1.805(11) . ?
O3 C3 1.202(13) . ?
O4 N1 1.271(8) . ?
O5 N1 1.224(13) . ?
O6 N2 1.293(11) . ?
O7 N2 1.191(12) . ?
O8 N2 1.293(11) . ?
N1 O4 1.271(8) 2_657 ?
C1 H1 1.0000 . ?
C1 C2 1.515(15) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.498(15) . ?
C3 C4 1.538(16) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.386(14) . ?
C5 C10 1.383(15) . ?
C6 H6 0.9500 . ?
C6 C7 1.363(15) . ?
C7 H7 0.9500 . ?
C7 C8 1.391(17) . ?
C8 H8 0.9500 . ?
C8 C9 1.398(17) . ?
C9 H9 0.9500 . ?
C9 C10 1.388(16) . ?
C10 H10 0.9500 . ?
C11 C12 1.398(16) . ?
C11 C16 1.399(15) . ?
C12 H12 0.9500 . ?
C12 C13 1.378(17) . ?
C13 H13 0.9500 . ?
C13 C14 1.38(2) . ?
C14 H14 0.9500 . ?
C14 C15 1.35(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.406(16) . ?
C16 H16 0.9500 . ?
C17 C18 1.372(15) . ?
C17 C22 1.422(15) . ?
C18 H18 0.9500 . ?
C18 C19 1.369(16) . ?
C19 H19 0.9500 . ?
C19 C20 1.422(17) . ?
C20 H20 0.9500 . ?
C20 C21 1.360(19) . ?
C21 H21 0.9500 . ?
C21 C22 1.401(18) . ?
C22 H22 0.9500 . ?
C23 C24 1.370(15) . ?
C23 C28 1.400(14) . ?
C24 H24 0.9500 . ?
C24 C25 1.415(15) . ?
C25 H25 0.9500 . ?
C25 C26 1.397(17) . ?
C26 H26 0.9500 . ?
C26 C27 1.337(18) . ?
C27 H27 0.9500 . ?
C27 C28 1.376(16) . ?
C28 H28 0.9500 . ?
N3S C1S 1.144(18) . ?
C1S C2S 1.48(2) . ?
C2S H2SA 0.9800 . ?
C2S H2SB 0.9800 . ?
C2S H2SC 0.9800 . ?
C3S H3SA 0.9800 . ?
C3S H3SB 0.9800 . ?
C3S H3SC 0.9800 . ?
C3S C4S 1.46(2) . ?
N2S C4S 0.98(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 La1 O1 179.1(3) . 2_657 ?
O1 La1 O4 113.9(2) 2_657 2_657 ?
O1 La1 O4 113.8(2) . . ?
O1 La1 O4 67.0(2) . 2_657 ?
O1 La1 O4 67.0(2) 2_657 . ?
O1 La1 O6 71.6(2) . 2_657 ?
O1 La1 O6 71.6(2) 2_657 . ?
O1 La1 O6 108.7(2) 2_657 2_657 ?
O1 La1 O6 108.7(2) . . ?
O1 La1 O8 65.1(2) 2_657 2_657 ?
O1 La1 O8 65.1(2) . . ?
O1 La1 O8 114.9(2) 2_657 . ?
O1 La1 O8 114.9(2) . 2_657 ?
O1 La1 N1 90.45(16) . . ?
O1 La1 N1 90.45(16) 2_657 . ?
O2 La1 O1 110.9(2) . 2_657 ?
O2 La1 O1 68.3(2) 2_657 2_657 ?
O2 La1 O1 110.9(2) 2_657 . ?
O2 La1 O1 68.3(2) . . ?
O2 La1 O2 69.7(3) . 2_657 ?
O2 La1 O4 146.7(2) . . ?
O2 La1 O4 131.0(2) . 2_657 ?
O2 La1 O4 146.7(2) 2_657 2_657 ?
O2 La1 O4 131.0(2) 2_657 . ?
O2 La1 O6 140.7(2) 2_657 2_657 ?
O2 La1 O6 75.9(2) . 2_657 ?
O2 La1 O6 75.9(2) 2_657 . ?
O2 La1 O6 140.7(2) . . ?
O2 La1 O8 101.4(2) 2_657 2_657 ?
O2 La1 O8 101.4(2) . . ?
O2 La1 O8 72.9(2) 2_657 . ?
O2 La1 O8 72.9(2) . 2_657 ?
O2 La1 N1 145.13(16) 2_657 . ?
O2 La1 N1 145.13(16) . . ?
O4 La1 O4 49.2(3) . 2_657 ?
O4 La1 O8 77.0(2) 2_657 . ?
O4 La1 O8 109.5(2) 2_657 2_657 ?
O4 La1 O8 77.0(2) . 2_657 ?
O4 La1 O8 109.5(2) . . ?
O4 La1 N1 24.59(15) 2_657 . ?
O4 La1 N1 24.59(15) . . ?
O6 La1 O4 73.9(2) 2_657 . ?
O6 La1 O4 71.9(2) 2_657 2_657 ?
O6 La1 O4 71.9(2) . . ?
O6 La1 O4 73.9(2) . 2_657 ?
O6 La1 O6 142.3(3) 2_657 . ?
O6 La1 O8 133.8(2) . 2_657 ?
O6 La1 O8 133.8(2) 2_657 . ?
O6 La1 O8 49.2(2) . . ?
O6 La1 O8 49.2(2) 2_657 2_657 ?
O6 La1 N1 71.15(16) 2_657 . ?
O6 La1 N1 71.15(16) . . ?
O8 La1 O8 173.2(3) 2_657 . ?
O8 La1 N1 93.41(14) 2_657 . ?
O8 La1 N1 93.41(14) . . ?
O1 P1 C1 111.0(4) . . ?
O1 P1 C5 110.7(5) . . ?
O1 P1 C11 112.7(5) . . ?
C5 P1 C1 106.5(5) . . ?
C11 P1 C1 107.1(5) . . ?
C11 P1 C5 108.5(5) . . ?
O2 P2 C1 111.8(4) . . ?
O2 P2 C17 114.2(5) . . ?
O2 P2 C23 108.6(4) . . ?
C17 P2 C1 107.5(5) . . ?
C17 P2 C23 106.8(5) . . ?
C23 P2 C1 107.7(5) . . ?
P1 O1 La1 150.3(4) . . ?
P2 O2 La1 141.7(4) . . ?
N1 O4 La1 96.5(5) . . ?
N2 O6 La1 98.6(6) . . ?
N2 O8 La1 96.0(5) . . ?
O4 N1 La1 58.9(5) 2_657 . ?
O4 N1 La1 58.9(5) . . ?
O4 N1 O4 117.8(9) . 2_657 ?
O5 N1 La1 180.000(5) . . ?
O5 N1 O4 121.1(5) . 2_657 ?
O5 N1 O4 121.1(5) . . ?
O7 N2 O6 121.9(10) . . ?
O7 N2 O8 122.5(9) . . ?
O8 N2 O6 115.6(9) . . ?
P1 C1 P2 108.1(5) . . ?
P1 C1 H1 108.3 . . ?
P2 C1 H1 108.3 . . ?
C2 C1 P1 111.7(6) . . ?
C2 C1 P2 112.0(7) . . ?
C2 C1 H1 108.3 . . ?
C1 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 107.9 . . ?
C3 C2 C1 111.7(9) . . ?
C3 C2 H2A 109.3 . . ?
C3 C2 H2B 109.3 . . ?
O3 C3 C2 121.7(10) . . ?
O3 C3 C4 122.4(11) . . ?
C2 C3 C4 115.8(10) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 P1 117.5(8) . . ?
C10 C5 P1 122.8(9) . . ?
C10 C5 C6 119.7(10) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 C5 119.3(10) . . ?
C7 C6 H6 120.3 . . ?
C6 C7 H7 118.9 . . ?
C6 C7 C8 122.2(12) . . ?
C8 C7 H7 118.9 . . ?
C7 C8 H8 120.9 . . ?
C7 C8 C9 118.2(11) . . ?
C9 C8 H8 120.9 . . ?
C8 C9 H9 120.2 . . ?
C10 C9 C8 119.7(11) . . ?
C10 C9 H9 120.2 . . ?
C5 C10 C9 120.7(11) . . ?
C5 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C12 C11 P1 118.5(8) . . ?
C12 C11 C16 119.1(10) . . ?
C16 C11 P1 122.3(9) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.3(13) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 119.9 . . ?
C12 C13 C14 120.2(14) . . ?
C14 C13 H13 119.9 . . ?
C13 C14 H14 119.7 . . ?
C15 C14 C13 120.6(13) . . ?
C15 C14 H14 119.7 . . ?
C14 C15 H15 119.7 . . ?
C14 C15 C16 120.7(13) . . ?
C16 C15 H15 119.7 . . ?
C11 C16 C15 119.0(12) . . ?
C11 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
C18 C17 P2 120.1(8) . . ?
C18 C17 C22 120.7(10) . . ?
C22 C17 P2 119.2(9) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 C17 120.9(11) . . ?
C19 C18 H18 119.6 . . ?
C18 C19 H19 119.9 . . ?
C18 C19 C20 120.2(12) . . ?
C20 C19 H19 119.9 . . ?
C19 C20 H20 120.9 . . ?
C21 C20 C19 118.3(12) . . ?
C21 C20 H20 120.9 . . ?
C20 C21 H21 118.4 . . ?
C20 C21 C22 123.2(12) . . ?
C22 C21 H21 118.4 . . ?
C17 C22 H22 121.6 . . ?
C21 C22 C17 116.8(12) . . ?
C21 C22 H22 121.6 . . ?
C24 C23 P2 125.4(8) . . ?
C24 C23 C28 118.9(10) . . ?
C28 C23 P2 115.7(8) . . ?
C23 C24 H24 120.1 . . ?
C23 C24 C25 119.8(10) . . ?
C25 C24 H24 120.1 . . ?
C24 C25 H25 120.5 . . ?
C26 C25 C24 119.0(11) . . ?
C26 C25 H25 120.5 . . ?
C25 C26 H26 119.7 . . ?
C27 C26 C25 120.6(11) . . ?
C27 C26 H26 119.7 . . ?
C26 C27 H27 119.7 . . ?
C26 C27 C28 120.7(12) . . ?
C28 C27 H27 119.7 . . ?
C23 C28 H28 119.6 . . ?
C27 C28 C23 120.8(11) . . ?
C27 C28 H28 119.6 . . ?
N3S C1S C2S 179.3(18) . . ?
C1S C2S H2SA 109.5 . . ?
C1S C2S H2SB 109.5 . . ?
C1S C2S H2SC 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
H3SA C3S H3SB 109.5 . . ?
H3SA C3S H3SC 109.5 . . ?
H3SB C3S H3SC 109.5 . . ?
C4S C3S H3SA 109.5 . . ?
C4S C3S H3SB 109.5 . . ?
C4S C3S H3SC 109.5 . . ?
N2S C4S C3S 180.00(2) . . ?

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
La1 O4 N1 O4 -0.002(6) . . . 2_657 ?
La1 O4 N1 O5 180.000(5) . . . . ?
La1 O6 N2 O7 171.4(10) . . . . ?
La1 O6 N2 O8 -7.4(8) . . . . ?
La1 O8 N2 O6 7.2(8) . . . . ?
La1 O8 N2 O7 -171.6(10) . . . . ?
P1 C1 C2 C3 -87.6(9) . . . . ?
P1 C5 C6 C7 175.9(9) . . . . ?
P1 C5 C10 C9 -178.1(10) . . . . ?
P1 C11 C12 C13 -177.5(9) . . . . ?
P1 C11 C16 C15 177.7(9) . . . . ?
P2 C1 C2 C3 151.0(7) . . . . ?
P2 C17 C18 C19 -179.6(9) . . . . ?
P2 C17 C22 C21 178.4(9) . . . . ?
P2 C23 C24 C25 177.4(9) . . . . ?
P2 C23 C28 C27 -179.8(11) . . . . ?
O1 La1 O1 P1 -55.5(10) 2_657 . . . ?
O1 La1 O2 P2 -13.0(6) . . . . ?
O1 La1 O2 P2 166.5(6) 2_657 . . . ?
O1 La1 O4 N1 19.0(5) . . . . ?
O1 La1 O4 N1 -161.2(5) 2_657 . . . ?
O1 La1 O6 N2 32.6(6) . . . . ?
O1 La1 O6 N2 -146.5(6) 2_657 . . . ?
O1 La1 O8 N2 26.4(6) 2_657 . . . ?
O1 La1 O8 N2 -154.6(6) . . . . ?
O1 La1 N1 O4 17.3(5) . . . 2_657 ?
O1 La1 N1 O4 17.3(5) 2_657 . . . ?
O1 La1 N1 O4 -162.7(5) . . . . ?
O1 La1 N1 O4 -162.7(5) 2_657 . . 2_657 ?
O1 La1 N1 O5 65(100) . . . . ?
O1 La1 N1 O5 -115(100) 2_657 . . . ?
O1 P1 C1 P2 35.4(6) . . . . ?
O1 P1 C1 C2 -88.3(8) . . . . ?
O1 P1 C5 C6 19.6(10) . . . . ?
O1 P1 C5 C10 -158.3(9) . . . . ?
O1 P1 C11 C12 15.5(10) . . . . ?
O1 P1 C11 C16 -161.9(8) . . . . ?
O2 La1 O1 P1 -83.7(9) 2_657 . . . ?
O2 La1 O1 P1 -27.2(8) . . . . ?
O2 La1 O2 P2 110.8(7) 2_657 . . . ?
O2 La1 O4 N1 105.3(5) . . . . ?
O2 La1 O4 N1 -135.5(4) 2_657 . . . ?
O2 La1 O6 N2 -75.1(6) 2_657 . . . ?
O2 La1 O6 N2 -45.7(7) . . . . ?
O2 La1 O8 N2 81.7(5) 2_657 . . . ?
O2 La1 O8 N2 146.1(5) . . . . ?
O2 La1 N1 O4 -112.2(5) 2_657 . . 2_657 ?
O2 La1 N1 O4 -112.2(5) . . . . ?
O2 La1 N1 O4 67.8(5) . . . 2_657 ?
O2 La1 N1 O4 67.8(5) 2_657 . . . ?
O2 La1 N1 O5 115(100) . . . . ?
O2 La1 N1 O5 -65(100) 2_657 . . . ?
O2 P2 C1 P1 -59.8(6) . . . . ?
O2 P2 C1 C2 63.7(8) . . . . ?
O2 P2 C17 C18 27.8(10) . . . . ?
O2 P2 C17 C22 -151.6(8) . . . . ?
O2 P2 C23 C24 -141.5(9) . . . . ?
O2 P2 C23 C28 39.0(10) . . . . ?
O4 La1 O1 P1 132.2(9) 2_657 . . . ?
O4 La1 O1 P1 116.7(8) . . . . ?
O4 La1 O2 P2 -113.7(6) . . . . ?
O4 La1 O2 P2 -38.5(8) 2_657 . . . ?
O4 La1 O4 N1 0.001(4) 2_657 . . . ?
O4 La1 O6 N2 90.8(6) 2_657 . . . ?
O4 La1 O6 N2 142.4(6) . . . . ?
O4 La1 O8 N2 -84.1(5) 2_657 . . . ?
O4 La1 O8 N2 -46.6(6) . . . . ?
O4 La1 N1 O4 179.998(6) . . . 2_657 ?
O4 La1 N1 O4 180.002(6) 2_657 . . . ?
O4 La1 N1 O5 48(100) 2_657 . . . ?
O4 La1 N1 O5 -132(100) . . . . ?
O6 La1 O1 P1 54.6(8) 2_657 . . . ?
O6 La1 O1 P1 -165.3(8) . . . . ?
O6 La1 O2 P2 80.3(7) . . . . ?
O6 La1 O2 P2 -88.5(7) 2_657 . . . ?
O6 La1 O4 N1 79.8(4) 2_657 . . . ?
O6 La1 O4 N1 -84.0(4) . . . . ?
O6 La1 O6 N2 116.5(5) 2_657 . . . ?
O6 La1 O8 N2 -4.3(5) . . . . ?
O6 La1 O8 N2 -132.6(5) 2_657 . . . ?
O6 La1 N1 O4 87.6(5) 2_657 . . 2_657 ?
O6 La1 N1 O4 -92.4(5) . . . 2_657 ?
O6 La1 N1 O4 87.6(5) . . . . ?
O6 La1 N1 O4 -92.4(5) 2_657 . . . ?
O6 La1 N1 O5 135(100) 2_657 . . . ?
O6 La1 N1 O5 -45(100) . . . . ?
O8 La1 O1 P1 -142.0(9) . . . . ?
O8 La1 O1 P1 30.5(9) 2_657 . . . ?
O8 La1 O2 P2 -139.7(7) 2_657 . . . ?
O8 La1 O2 P2 44.1(7) . . . . ?
O8 La1 O4 N1 -51.6(5) . . . . ?
O8 La1 O4 N1 130.7(4) 2_657 . . . ?
O8 La1 O6 N2 4.3(5) . . . . ?
O8 La1 O6 N2 -167.4(5) 2_657 . . . ?
O8 La1 O8 N2 114.3(5) 2_657 . . . ?
O8 La1 N1 O4 -47.7(5) . . . 2_657 ?
O8 La1 N1 O4 -47.7(5) 2_657 . . . ?
O8 La1 N1 O4 132.3(5) . . . . ?
O8 La1 N1 O4 132.3(5) 2_657 . . 2_657 ?
O8 La1 N1 O5 0(100) . . . . ?
O8 La1 N1 O5 180(100) 2_657 . . . ?
N1 La1 O1 P1 124.5(9) . . . . ?
N1 La1 O2 P2 -69.2(7) . . . . ?
N1 La1 O6 N2 116.5(5) . . . . ?
N1 La1 O8 N2 -65.7(5) . . . . ?
C1 P1 O1 La1 12.7(10) . . . . ?
C1 P1 C5 C6 -101.1(9) . . . . ?
C1 P1 C5 C10 81.0(10) . . . . ?
C1 P1 C11 C12 137.9(8) . . . . ?
C1 P1 C11 C16 -39.4(10) . . . . ?
C1 P2 O2 La1 51.6(8) . . . . ?
C1 P2 C17 C18 -96.8(9) . . . . ?
C1 P2 C17 C22 83.7(9) . . . . ?
C1 P2 C23 C24 -20.2(11) . . . . ?
C1 P2 C23 C28 160.2(9) . . . . ?
C1 C2 C3 O3 -21.1(15) . . . . ?
C1 C2 C3 C4 161.1(9) . . . . ?
C5 P1 O1 La1 -105.3(9) . . . . ?
C5 P1 C1 P2 155.9(5) . . . . ?
C5 P1 C1 C2 32.3(8) . . . . ?
C5 P1 C11 C12 -107.5(9) . . . . ?
C5 P1 C11 C16 75.2(9) . . . . ?
C5 C6 C7 C8 5.0(19) . . . . ?
C6 C5 C10 C9 4.0(18) . . . . ?
C6 C7 C8 C9 -2(2) . . . . ?
C7 C8 C9 C10 0(2) . . . . ?
C8 C9 C10 C5 -0.7(19) . . . . ?
C10 C5 C6 C7 -6.0(17) . . . . ?
C11 P1 O1 La1 132.9(8) . . . . ?
C11 P1 C1 P2 -88.1(6) . . . . ?
C11 P1 C1 C2 148.2(7) . . . . ?
C11 P1 C5 C6 143.9(9) . . . . ?
C11 P1 C5 C10 -34.1(11) . . . . ?
C11 C12 C13 C14 0.1(18) . . . . ?
C12 C11 C16 C15 0.4(15) . . . . ?
C12 C13 C14 C15 -0.5(19) . . . . ?
C13 C14 C15 C16 1(2) . . . . ?
C14 C15 C16 C11 -0.7(18) . . . . ?
C16 C11 C12 C13 -0.1(16) . . . . ?
C17 P2 O2 La1 -70.7(7) . . . . ?
C17 P2 C1 P1 66.3(6) . . . . ?
C17 P2 C1 C2 -170.2(7) . . . . ?
C17 P2 C23 C24 95.0(10) . . . . ?
C17 P2 C23 C28 -84.6(10) . . . . ?
C17 C18 C19 C20 0.9(17) . . . . ?
C18 C17 C22 C21 -1.0(16) . . . . ?
C18 C19 C20 C21 -0.5(17) . . . . ?
C19 C20 C21 C22 -0.7(19) . . . . ?
C20 C21 C22 C17 1.5(19) . . . . ?
C22 C17 C18 C19 -0.1(16) . . . . ?
C23 P2 O2 La1 170.3(6) . . . . ?
C23 P2 C1 P1 -179.0(5) . . . . ?
C23 P2 C1 C2 -55.5(8) . . . . ?
C23 P2 C17 C18 147.9(9) . . . . ?
C23 P2 C17 C22 -31.6(10) . . . . ?
C23 C24 C25 C26 5.0(18) . . . . ?
C24 C23 C28 C27 0.7(19) . . . . ?
C24 C25 C26 C27 -4.5(19) . . . . ?
C25 C26 C27 C28 2(2) . . . . ?
C26 C27 C28 C23 0(2) . . . . ?
C28 C23 C24 C25 -3.1(17) . . . . ?

_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_vrf_REFLT01_3                   
;
PROBLEM: Reflection count > 10% excess reflns - sys abs data present?
RESPONSE: The crystal was twinned with slightly disoriented domains. 
The indexing with  Cell_Now program (Bruker (2005)[Bruker (2005). APEX2 software package, 
Bruker AXS Inc., 5465, East Cheryl Parkway, Madison, WI 5317]) allowed one to decribe 
the twinning as superposition of two components. The refining of structure 
was carried out using HKLF5 instruction 
and additional scale factor (BASF instruction).   
;
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1442101'
_audit_update_record             
;
2015-12-13 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;
_audit_creation_date             2015-05-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C56 H52 N3 Nd O15 P4, 3(C2 H3 N)'
_chemical_formula_sum            'C62 H61 N6 Nd O15 P4'
_chemical_formula_weight         1398.28
_chemical_melting_point          ?
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'
Nd Nd -0.1943 3.0179 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   13.4706(8)
_cell_length_b                   17.8919(10)
_cell_length_c                   26.4711(15)
_cell_angle_alpha                90
_cell_angle_beta                 91.3780(10)
_cell_angle_gamma                90
_cell_volume                     6378.1(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    120
_cell_measurement_theta_max      31.62
_cell_measurement_theta_min      2.40
_shelx_estimated_absorpt_T_max   0.925
_shelx_estimated_absorpt_T_min   0.763
_exptl_absorpt_coefficient_mu    0.984
_exptl_absorpt_correction_T_max  0.3380
_exptl_absorpt_correction_T_min  0.2324
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1131 before and 0.0381 after correction.
The Ratio of minimum to maximum transmission is 0.6876.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2860
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            44834
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.673
_diffrn_reflns_theta_min         1.539
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10078
_reflns_number_total             10755
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         10755
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0233
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0300P)²+5.7460P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0598
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2S-C3S
 1.1 with sigma of 0.005
 C3S-C4S
 1.5 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(N2S) = Uanis(C3S) = Uanis(C4S)
4. Others
 Fixed Sof: C4S(0.5) H4SA(0.5) H4SB(0.5) H4SC(0.5) C3S(0.5) N2S(0.5)
5.a Ternary CH refined with riding coordinates:
 C0AA(H0AA)
5.b Secondary CH2 refined with riding coordinates:
 C1AA(H1AA,H1AB)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28)
5.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C2S(H2SA,H2SB,H2SC), C4S(H4SA,H4SB,H4SC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Nd1 Nd 0.5000 1.15669(2) 1.2500 0.01043(3) Uani 1 2 d S T P . .
P1 P 0.41767(2) 1.13362(2) 1.10990(2) 0.01109(6) Uani 1 1 d . . . . .
P2 P 0.51764(2) 1.00040(2) 1.15550(2) 0.01124(6) Uani 1 1 d . . . . .
O1 O 0.41860(7) 1.15752(5) 1.16406(3) 0.01432(16) Uani 1 1 d . . . . .
O2 O 0.54429(7) 1.04425(5) 1.20223(3) 0.01367(16) Uani 1 1 d . . . . .
O3 O 0.56768(9) 1.07592(6) 0.99960(4) 0.0276(2) Uani 1 1 d . . . . .
O4 O 0.55790(7) 1.28701(5) 1.27895(4) 0.01951(18) Uani 1 1 d . . . . .
O5 O 0.5000 1.39243(9) 1.2500 0.0385(4) Uani 1 2 d S T P . .
O6 O 0.37521(7) 1.20350(5) 1.31393(4) 0.01856(18) Uani 1 1 d . . . . .
O7 O 0.21674(9) 1.18056(8) 1.31328(5) 0.0382(3) Uani 1 1 d . . . . .
O8 O 0.30675(7) 1.14724(6) 1.24978(4) 0.02025(19) Uani 1 1 d . . . . .
N1 N 0.5000 1.32421(9) 1.2500 0.0174(3) Uani 1 2 d S T P . .
N2 N 0.29676(8) 1.17716(7) 1.29275(4) 0.0189(2) Uani 1 1 d . . . . .
C0AA C 0.51027(9) 1.05986(7) 1.09939(4) 0.01208(19) Uani 1 1 d . . . . .
H0AA H 0.4870 1.0287 1.0701 0.014 Uiso 1 1 calc R . . . .
C1AA C 0.61162(9) 1.09417(7) 1.08677(5) 0.0156(2) Uani 1 1 d . . . . .
H1AA H 0.6198 1.1422 1.1049 0.019 Uiso 1 1 calc R . . . .
H1AB H 0.6652 1.0601 1.0986 0.019 Uiso 1 1 calc R . . . .
C2AA C 0.62114(10) 1.10751(8) 1.03040(5) 0.0197(2) Uani 1 1 d . . . . .
C4 C 0.70073(13) 1.16131(10) 1.01554(7) 0.0312(3) Uani 1 1 d . . . . .
H4A H 0.7163 1.1536 0.9799 0.047 Uiso 1 1 calc GR . . . .
H4B H 0.7605 1.1528 1.0366 0.047 Uiso 1 1 calc GR . . . .
H4C H 0.6774 1.2126 1.0204 0.047 Uiso 1 1 calc GR . . . .
C5 C 0.44836(9) 1.21118(7) 1.06966(5) 0.0153(2) Uani 1 1 d . . . . .
C6 C 0.50065(11) 1.27098(8) 1.09134(6) 0.0224(3) Uani 1 1 d . . . . .
H6 H 0.5159 1.2711 1.1266 0.027 Uiso 1 1 calc R . . . .
C7 C 0.53032(13) 1.33026(9) 1.06129(7) 0.0311(3) Uani 1 1 d . . . . .
H7 H 0.5662 1.3708 1.0760 0.037 Uiso 1 1 calc R . . . .
C8 C 0.50770(14) 1.33045(10) 1.00983(7) 0.0341(4) Uani 1 1 d . . . . .
H8 H 0.5296 1.3705 0.9893 0.041 Uiso 1 1 calc R . . . .
C9 C 0.45343(16) 1.27255(10) 0.98842(7) 0.0363(4) Uani 1 1 d . . . . .
H9 H 0.4365 1.2735 0.9534 0.044 Uiso 1 1 calc R . . . .
C10 C 0.42357(13) 1.21275(9) 1.01819(5) 0.0261(3) Uani 1 1 d . . . . .
H10 H 0.3863 1.1730 1.0034 0.031 Uiso 1 1 calc R . . . .
C11 C 0.29917(9) 1.09710(7) 1.08983(5) 0.0158(2) Uani 1 1 d . . . . .
C12 C 0.21757(10) 1.11264(9) 1.11959(6) 0.0242(3) Uani 1 1 d . . . . .
H12 H 0.2250 1.1430 1.1489 0.029 Uiso 1 1 calc R . . . .
C13 C 0.12494(11) 1.08305(10) 1.10578(8) 0.0364(4) Uani 1 1 d . . . . .
H13 H 0.0691 1.0931 1.1259 0.044 Uiso 1 1 calc R . . . .
C14 C 0.11403(12) 1.03929(10) 1.06307(9) 0.0397(5) Uani 1 1 d . . . . .
H14 H 0.0507 1.0192 1.0541 0.048 Uiso 1 1 calc R . . . .
C15 C 0.19439(13) 1.02444(9) 1.03321(8) 0.0368(4) Uani 1 1 d . . . . .
H15 H 0.1862 0.9947 1.0037 0.044 Uiso 1 1 calc R . . . .
C16 C 0.28759(11) 1.05325(8) 1.04657(6) 0.0247(3) Uani 1 1 d . . . . .
H16 H 0.3431 1.0430 1.0262 0.030 Uiso 1 1 calc R . . . .
C17 C 0.40123(9) 0.95166(7) 1.15961(5) 0.0146(2) Uani 1 1 d . . . . .
C18 C 0.32644(10) 0.98009(8) 1.18944(5) 0.0201(2) Uani 1 1 d . . . . .
H18 H 0.3368 1.0253 1.2076 0.024 Uiso 1 1 calc R . . . .
C19 C 0.23634(11) 0.94223(10) 1.19263(6) 0.0268(3) Uani 1 1 d . . . . .
H19 H 0.1849 0.9621 1.2126 0.032 Uiso 1 1 calc R . . . .
C20 C 0.22179(12) 0.87594(9) 1.16681(6) 0.0277(3) Uani 1 1 d . . . . .
H20 H 0.1608 0.8498 1.1696 0.033 Uiso 1 1 calc R . . . .
C21 C 0.29549(14) 0.84738(9) 1.13691(7) 0.0318(3) Uani 1 1 d . . . . .
H21 H 0.2848 0.8019 1.1191 0.038 Uiso 1 1 calc R . . . .
C22 C 0.38510(12) 0.88509(8) 1.13282(6) 0.0252(3) Uani 1 1 d . . . . .
H22 H 0.4353 0.8658 1.1119 0.030 Uiso 1 1 calc R . . . .
C23 C 0.60977(9) 0.92963(7) 1.14518(5) 0.0155(2) Uani 1 1 d . . . . .
C24 C 0.64536(11) 0.90825(8) 1.09841(5) 0.0225(3) Uani 1 1 d . . . . .
H24 H 0.6197 0.9309 1.0684 0.027 Uiso 1 1 calc R . . . .
C25 C 0.71873(12) 0.85355(9) 1.09569(6) 0.0281(3) Uani 1 1 d . . . . .
H25 H 0.7443 0.8399 1.0639 0.034 Uiso 1 1 calc R . . . .
C26 C 0.75435(12) 0.81912(10) 1.13940(7) 0.0308(3) Uani 1 1 d . . . . .
H26 H 0.8045 0.7820 1.1374 0.037 Uiso 1 1 calc R . . . .
C27 C 0.71721(15) 0.83859(11) 1.18581(7) 0.0377(4) Uani 1 1 d . . . . .
H27 H 0.7408 0.8141 1.2156 0.045 Uiso 1 1 calc R . . . .
C28 C 0.64542(12) 0.89399(9) 1.18889(6) 0.0276(3) Uani 1 1 d . . . . .
H28 H 0.6205 0.9077 1.2209 0.033 Uiso 1 1 calc R . . . .
N1S N 0.86625(12) 1.04857(12) 1.08695(7) 0.0486(4) Uani 1 1 d . . . . .
C1S C 0.86874(13) 1.03139(13) 1.12787(9) 0.0426(5) Uani 1 1 d . . . . .
C2S C 0.8688(2) 1.00995(17) 1.18102(10) 0.0701(8) Uani 1 1 d . . . . .
H2SA H 0.8980 0.9600 1.1850 0.105 Uiso 1 1 calc GR . . . .
H2SB H 0.8005 1.0094 1.1929 0.105 Uiso 1 1 calc GR . . . .
H2SC H 0.9081 1.0460 1.2009 0.105 Uiso 1 1 calc GR . . . .
C4S C -0.0149(6) 1.2431(4) 1.2597(3) 0.0903(12) Uani 0.5 1 d D . . A -1
H4SA H -0.0743 1.2629 1.2423 0.136 Uiso 0.5 1 calc GR . . A -1
H4SB H 0.0375 1.2811 1.2600 0.136 Uiso 0.5 1 calc GR . . A -1
H4SC H -0.0310 1.2301 1.2946 0.136 Uiso 0.5 1 calc GR . . A -1
C3S C 0.0198(6) 1.1756(4) 1.2331(3) 0.0903(12) Uani 0.5 1 d D . . A -1
N2S N 0.0447(4) 1.1229(4) 1.2157(2) 0.0903(12) Uani 0.5 1 d D . . A -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
Nd1 O1 2.5015(9) 2_657 ?
Nd1 O1 2.5016(9) . ?
Nd1 O2 2.4573(9) . ?
Nd1 O2 2.4572(9) 2_657 ?
Nd1 O4 2.5698(10) 2_657 ?
Nd1 O4 2.5697(10) . ?
Nd1 O6 2.5551(10) 2_657 ?
Nd1 O6 2.5550(10) . ?
Nd1 O8 2.6085(10) 2_657 ?
Nd1 O8 2.6085(10) . ?
Nd1 N1 2.9973(16) . ?
Nd1 N2 3.0099(12) . ?
P1 O1 1.4957(9) . ?
P1 C0AA 1.8417(12) . ?
P1 C5 1.8035(13) . ?
P1 C11 1.7934(13) . ?
P2 O2 1.5010(9) . ?
P2 C0AA 1.8278(12) . ?
P2 C17 1.7999(13) . ?
P2 C23 1.7984(13) . ?
O3 C2AA 1.2143(18) . ?
O4 N1 1.2688(12) . ?
O5 N1 1.221(2) . ?
O6 N2 1.2746(15) . ?
O7 N2 1.2202(16) . ?
O8 N2 1.2672(15) . ?
N1 O4 1.2688(12) 2_657 ?
C0AA H0AA 1.0000 . ?
C0AA C1AA 1.5409(17) . ?
C1AA H1AA 0.9900 . ?
C1AA H1AB 0.9900 . ?
C1AA C2AA 1.5196(18) . ?
C2AA C4 1.500(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.3968(19) . ?
C5 C10 1.3951(19) . ?
C6 H6 0.9500 . ?
C6 C7 1.390(2) . ?
C7 H7 0.9500 . ?
C7 C8 1.389(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.382(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.394(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.3956(19) . ?
C11 C16 1.3939(19) . ?
C12 H12 0.9500 . ?
C12 C13 1.396(2) . ?
C13 H13 0.9500 . ?
C13 C14 1.380(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.381(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.395(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.3911(18) . ?
C17 C22 1.4005(19) . ?
C18 H18 0.9500 . ?
C18 C19 1.3942(19) . ?
C19 H19 0.9500 . ?
C19 C20 1.381(2) . ?
C20 H20 0.9500 . ?
C20 C21 1.382(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.389(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.3920(18) . ?
C23 C28 1.3963(19) . ?
C24 H24 0.9500 . ?
C24 C25 1.394(2) . ?
C25 H25 0.9500 . ?
C25 C26 1.386(2) . ?
C26 H26 0.9500 . ?
C26 C27 1.382(2) . ?
C27 H27 0.9500 . ?
C27 C28 1.389(2) . ?
C28 H28 0.9500 . ?
N1S C1S 1.126(3) . ?
C1S C2S 1.458(3) . ?
C2S H2SA 0.9800 . ?
C2S H2SB 0.9800 . ?
C2S H2SC 0.9800 . ?
C4S H4SA 0.9800 . ?
C4S H4SB 0.9800 . ?
C4S H4SC 0.9800 . ?
C4S C3S 1.481(4) . ?
C3S N2S 1.104(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
O1 Nd1 O1 179.32(4) 2_657 . ?
O1 Nd1 O4 66.43(3) . 2_657 ?
O1 Nd1 O4 112.89(3) . . ?
O1 Nd1 O4 112.90(3) 2_657 2_657 ?
O1 Nd1 O4 66.43(3) 2_657 . ?
O1 Nd1 O6 108.63(3) 2_657 2_657 ?
O1 Nd1 O6 71.14(3) . 2_657 ?
O1 Nd1 O6 108.63(3) . . ?
O1 Nd1 O6 71.14(3) 2_657 . ?
O1 Nd1 O8 114.71(3) . 2_657 ?
O1 Nd1 O8 114.71(3) 2_657 . ?
O1 Nd1 O8 65.34(3) . . ?
O1 Nd1 O8 65.34(3) 2_657 2_657 ?
O1 Nd1 N1 89.66(2) . . ?
O1 Nd1 N1 89.66(2) 2_657 . ?
O1 Nd1 N2 87.62(3) . . ?
O1 Nd1 N2 92.30(3) 2_657 . ?
O2 Nd1 O1 69.11(3) . . ?
O2 Nd1 O1 111.49(3) . 2_657 ?
O2 Nd1 O1 69.11(3) 2_657 2_657 ?
O2 Nd1 O1 111.49(3) 2_657 . ?
O2 Nd1 O2 70.10(4) 2_657 . ?
O2 Nd1 O4 145.15(3) 2_657 2_657 ?
O2 Nd1 O4 131.69(3) 2_657 . ?
O2 Nd1 O4 145.14(3) . . ?
O2 Nd1 O4 131.69(3) . 2_657 ?
O2 Nd1 O6 141.35(3) 2_657 2_657 ?
O2 Nd1 O6 141.35(3) . . ?
O2 Nd1 O6 75.87(3) 2_657 . ?
O2 Nd1 O6 75.86(3) . 2_657 ?
O2 Nd1 O8 72.15(3) 2_657 . ?
O2 Nd1 O8 72.15(3) . 2_657 ?
O2 Nd1 O8 101.56(3) . . ?
O2 Nd1 O8 101.56(3) 2_657 2_657 ?
O2 Nd1 N1 144.95(2) . . ?
O2 Nd1 N1 144.95(2) 2_657 . ?
O2 Nd1 N2 121.83(3) . . ?
O2 Nd1 N2 70.84(3) 2_657 . ?
O4 Nd1 O4 49.71(4) . 2_657 ?
O4 Nd1 O8 76.26(3) . 2_657 ?
O4 Nd1 O8 110.80(3) 2_657 2_657 ?
O4 Nd1 O8 110.80(3) . . ?
O4 Nd1 O8 76.26(3) 2_657 . ?
O4 Nd1 N1 24.86(2) . . ?
O4 Nd1 N1 24.86(2) 2_657 . ?
O4 Nd1 N2 74.30(3) 2_657 . ?
O4 Nd1 N2 92.85(3) . . ?
O6 Nd1 O4 72.83(3) 2_657 2_657 ?
O6 Nd1 O4 72.56(3) 2_657 . ?
O6 Nd1 O4 72.83(3) . . ?
O6 Nd1 O4 72.56(3) . 2_657 ?
O6 Nd1 O6 141.73(5) . 2_657 ?
O6 Nd1 O8 49.48(3) . . ?
O6 Nd1 O8 133.81(3) 2_657 . ?
O6 Nd1 O8 49.48(3) 2_657 2_657 ?
O6 Nd1 O8 133.81(3) . 2_657 ?
O6 Nd1 N1 70.86(2) . . ?
O6 Nd1 N1 70.86(2) 2_657 . ?
O6 Nd1 N2 24.79(3) . . ?
O6 Nd1 N2 145.90(3) 2_657 . ?
O8 Nd1 O8 172.57(5) 2_657 . ?
O8 Nd1 N1 93.71(2) 2_657 . ?
O8 Nd1 N1 93.71(2) . . ?
O8 Nd1 N2 157.48(3) 2_657 . ?
O8 Nd1 N2 24.77(3) . . ?
N1 Nd1 N2 83.01(2) . . ?
O1 P1 C0AA 111.08(5) . . ?
O1 P1 C5 110.46(6) . . ?
O1 P1 C11 112.02(6) . . ?
C5 P1 C0AA 107.24(6) . . ?
C11 P1 C0AA 107.18(6) . . ?
C11 P1 C5 108.68(6) . . ?
O2 P2 C0AA 111.88(5) . . ?
O2 P2 C17 113.26(6) . . ?
O2 P2 C23 109.94(6) . . ?
C17 P2 C0AA 107.51(6) . . ?
C23 P2 C0AA 108.09(6) . . ?
C23 P2 C17 105.87(6) . . ?
P1 O1 Nd1 149.69(5) . . ?
P2 O2 Nd1 142.73(5) . . ?
N1 O4 Nd1 96.79(8) . . ?
N2 O6 Nd1 98.00(7) . . ?
N2 O8 Nd1 95.63(7) . . ?
O4 N1 Nd1 58.36(7) 2_657 . ?
O4 N1 Nd1 58.36(7) . . ?
O4 N1 O4 116.71(15) . 2_657 ?
O5 N1 Nd1 180.0 . . ?
O5 N1 O4 121.64(7) . . ?
O5 N1 O4 121.64(7) . 2_657 ?
O6 N2 Nd1 57.20(6) . . ?
O7 N2 Nd1 174.11(11) . . ?
O7 N2 O6 121.17(12) . . ?
O7 N2 O8 122.33(13) . . ?
O8 N2 Nd1 59.59(6) . . ?
O8 N2 O6 116.50(11) . . ?
P1 C0AA H0AA 108.4 . . ?
P2 C0AA P1 108.54(6) . . ?
P2 C0AA H0AA 108.4 . . ?
C1AA C0AA P1 110.74(8) . . ?
C1AA C0AA P2 112.15(8) . . ?
C1AA C0AA H0AA 108.4 . . ?
C0AA C1AA H1AA 109.3 . . ?
C0AA C1AA H1AB 109.3 . . ?
H1AA C1AA H1AB 107.9 . . ?
C2AA C1AA C0AA 111.81(11) . . ?
C2AA C1AA H1AA 109.3 . . ?
C2AA C1AA H1AB 109.3 . . ?
O3 C2AA C1AA 121.56(12) . . ?
O3 C2AA C4 122.59(13) . . ?
C4 C2AA C1AA 115.84(13) . . ?
C2AA C4 H4A 109.5 . . ?
C2AA C4 H4B 109.5 . . ?
C2AA C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 P1 117.84(10) . . ?
C10 C5 P1 122.65(10) . . ?
C10 C5 C6 119.50(12) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 C5 119.88(14) . . ?
C7 C6 H6 120.1 . . ?
C6 C7 H7 119.9 . . ?
C8 C7 C6 120.26(15) . . ?
C8 C7 H7 119.9 . . ?
C7 C8 H8 119.9 . . ?
C9 C8 C7 120.13(14) . . ?
C9 C8 H8 119.9 . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C10 120.04(15) . . ?
C10 C9 H9 120.0 . . ?
C5 C10 H10 119.9 . . ?
C9 C10 C5 120.14(15) . . ?
C9 C10 H10 119.9 . . ?
C12 C11 P1 117.89(11) . . ?
C16 C11 P1 121.99(11) . . ?
C16 C11 C12 120.11(13) . . ?
C11 C12 H12 120.4 . . ?
C11 C12 C13 119.20(16) . . ?
C13 C12 H12 120.4 . . ?
C12 C13 H13 119.8 . . ?
C14 C13 C12 120.44(17) . . ?
C14 C13 H13 119.8 . . ?
C13 C14 H14 119.7 . . ?
C13 C14 C15 120.56(15) . . ?
C15 C14 H14 119.7 . . ?
C14 C15 H15 120.1 . . ?
C14 C15 C16 119.78(17) . . ?
C16 C15 H15 120.1 . . ?
C11 C16 C15 119.91(16) . . ?
C11 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C18 C17 P2 120.07(10) . . ?
C18 C17 C22 119.52(12) . . ?
C22 C17 P2 120.41(10) . . ?
C17 C18 H18 120.0 . . ?
C17 C18 C19 120.00(13) . . ?
C19 C18 H18 120.0 . . ?
C18 C19 H19 120.0 . . ?
C20 C19 C18 120.06(15) . . ?
C20 C19 H19 120.0 . . ?
C19 C20 H20 119.8 . . ?
C19 C20 C21 120.37(14) . . ?
C21 C20 H20 119.8 . . ?
C20 C21 H21 119.9 . . ?
C20 C21 C22 120.16(15) . . ?
C22 C21 H21 119.9 . . ?
C17 C22 H22 120.1 . . ?
C21 C22 C17 119.87(14) . . ?
C21 C22 H22 120.1 . . ?
C24 C23 P2 125.62(10) . . ?
C24 C23 C28 119.51(12) . . ?
C28 C23 P2 114.87(10) . . ?
C23 C24 H24 120.0 . . ?
C23 C24 C25 119.91(14) . . ?
C25 C24 H24 120.0 . . ?
C24 C25 H25 120.0 . . ?
C26 C25 C24 120.04(14) . . ?
C26 C25 H25 120.0 . . ?
C25 C26 H26 119.9 . . ?
C27 C26 C25 120.29(14) . . ?
C27 C26 H26 119.9 . . ?
C26 C27 H27 120.0 . . ?
C26 C27 C28 119.97(15) . . ?
C28 C27 H27 120.0 . . ?
C23 C28 H28 119.9 . . ?
C27 C28 C23 120.24(14) . . ?
C27 C28 H28 119.9 . . ?
N1S C1S C2S 178.2(2) . . ?
C1S C2S H2SA 109.5 . . ?
C1S C2S H2SB 109.5 . . ?
C1S C2S H2SC 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
H4SA C4S H4SB 109.5 . . ?
H4SA C4S H4SC 109.5 . . ?
H4SB C4S H4SC 109.5 . . ?
C3S C4S H4SA 109.5 . . ?
C3S C4S H4SB 109.5 . . ?
C3S C4S H4SC 109.5 . . ?
N2S C3S C4S 175.9(9) . . ?

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
Nd1 O4 N1 O4 -0.004(5) . . . 2_657 ?
Nd1 O4 N1 O5 180.000(1) . . . . ?
Nd1 O6 N2 O7 173.32(13) . . . . ?
Nd1 O6 N2 O8 -6.31(12) . . . . ?
Nd1 O8 N2 O6 6.15(12) . . . . ?
Nd1 O8 N2 O7 -173.47(13) . . . . ?
P1 C0AA C1AA C2AA -88.53(11) . . . . ?
P1 C5 C6 C7 176.76(13) . . . . ?
P1 C5 C10 C9 -176.87(14) . . . . ?
P1 C11 C12 C13 -178.04(12) . . . . ?
P1 C11 C16 C15 178.29(12) . . . . ?
P2 C0AA C1AA C2AA 150.06(9) . . . . ?
P2 C17 C18 C19 -179.94(11) . . . . ?
P2 C17 C22 C21 179.01(13) . . . . ?
P2 C23 C24 C25 178.58(12) . . . . ?
P2 C23 C28 C27 -179.65(15) . . . . ?
O1 P1 C0AA P2 34.86(8) . . . . ?
O1 P1 C0AA C1AA -88.66(9) . . . . ?
O1 P1 C5 C6 21.91(13) . . . . ?
O1 P1 C5 C10 -159.28(12) . . . . ?
O1 P1 C11 C12 16.72(12) . . . . ?
O1 P1 C11 C16 -162.03(11) . . . . ?
O2 P2 C0AA P1 -57.85(7) . . . . ?
O2 P2 C0AA C1AA 64.82(10) . . . . ?
O2 P2 C17 C18 29.12(12) . . . . ?
O2 P2 C17 C22 -151.02(11) . . . . ?
O2 P2 C23 C24 -141.41(12) . . . . ?
O2 P2 C23 C28 39.49(13) . . . . ?
C0AA P1 O1 Nd1 11.85(13) . . . . ?
C0AA P1 C5 C6 -99.26(11) . . . . ?
C0AA P1 C5 C10 79.55(13) . . . . ?
C0AA P1 C11 C12 138.80(11) . . . . ?
C0AA P1 C11 C16 -39.95(13) . . . . ?
C0AA P2 O2 Nd1 49.64(10) . . . . ?
C0AA P2 C17 C18 -94.99(11) . . . . ?
C0AA P2 C17 C22 84.87(12) . . . . ?
C0AA P2 C23 C24 -19.04(14) . . . . ?
C0AA P2 C23 C28 161.87(11) . . . . ?
C0AA C1AA C2AA O3 -18.84(18) . . . . ?
C0AA C1AA C2AA C4 161.62(12) . . . . ?
C5 P1 O1 Nd1 -107.01(11) . . . . ?
C5 P1 C0AA P2 155.64(6) . . . . ?
C5 P1 C0AA C1AA 32.12(10) . . . . ?
C5 P1 C11 C12 -105.60(11) . . . . ?
C5 P1 C11 C16 75.65(12) . . . . ?
C5 C6 C7 C8 0.3(3) . . . . ?
C6 C5 C10 C9 1.9(2) . . . . ?
C6 C7 C8 C9 1.6(3) . . . . ?
C7 C8 C9 C10 -1.8(3) . . . . ?
C8 C9 C10 C5 0.0(3) . . . . ?
C10 C5 C6 C7 -2.1(2) . . . . ?
C11 P1 O1 Nd1 131.68(10) . . . . ?
C11 P1 C0AA P2 -87.81(7) . . . . ?
C11 P1 C0AA C1AA 148.68(8) . . . . ?
C11 P1 C5 C6 145.18(11) . . . . ?
C11 P1 C5 C10 -36.01(14) . . . . ?
C11 C12 C13 C14 -0.3(2) . . . . ?
C12 C11 C16 C15 -0.4(2) . . . . ?
C12 C13 C14 C15 -0.4(3) . . . . ?
C13 C14 C15 C16 0.7(3) . . . . ?
C14 C15 C16 C11 -0.3(2) . . . . ?
C16 C11 C12 C13 0.7(2) . . . . ?
C17 P2 O2 Nd1 -72.06(10) . . . . ?
C17 P2 C0AA P1 67.10(7) . . . . ?
C17 P2 C0AA C1AA -170.23(8) . . . . ?
C17 P2 C23 C24 95.91(13) . . . . ?
C17 P2 C23 C28 -83.18(12) . . . . ?
C17 C18 C19 C20 1.0(2) . . . . ?
C18 C17 C22 C21 -1.1(2) . . . . ?
C18 C19 C20 C21 -1.3(2) . . . . ?
C19 C20 C21 C22 0.3(3) . . . . ?
C20 C21 C22 C17 0.9(3) . . . . ?
C22 C17 C18 C19 0.2(2) . . . . ?
C23 P2 O2 Nd1 169.74(8) . . . . ?
C23 P2 C0AA P1 -179.03(6) . . . . ?
C23 P2 C0AA C1AA -56.36(10) . . . . ?
C23 P2 C17 C18 149.66(11) . . . . ?
C23 P2 C17 C22 -30.48(13) . . . . ?
C23 C24 C25 C26 1.7(2) . . . . ?
C24 C23 C28 C27 1.2(3) . . . . ?
C24 C25 C26 C27 0.2(3) . . . . ?
C25 C26 C27 C28 -1.4(3) . . . . ?
C26 C27 C28 C23 0.7(3) . . . . ?
C28 C23 C24 C25 -2.4(2) . . . . ?

####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1442102'
_audit_update_record             
;
2015-12-13 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;
_audit_creation_date             2015-04-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C56 H52 N2 Nd O12 P4, N O3, C2 H6 O'
_chemical_formula_sum            'C58 H58 N3 Nd O16 P4'
_chemical_formula_weight         1321.19
_chemical_melting_point          ?
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'
Nd Nd -0.1943 3.0179 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.590(7)
_cell_length_b                   13.510(10)
_cell_length_c                   19.148(15)
_cell_angle_alpha                90.574(16)
_cell_angle_beta                 96.836(16)
_cell_angle_gamma                111.923(17)
_cell_volume                     2994(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1994
_cell_measurement_temperature    120
_cell_measurement_theta_max      21.70
_cell_measurement_theta_min      2.25
_shelx_estimated_absorpt_T_max   0.894
_shelx_estimated_absorpt_T_min   0.795
_exptl_absorpt_coefficient_mu    1.043
_exptl_absorpt_correction_T_max  0.493
_exptl_absorpt_correction_T_min  0.250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1350
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1446
_diffrn_reflns_av_unetI/netI     0.2429
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            38088
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         29.906
_diffrn_reflns_theta_min         1.628
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8453
_reflns_number_total             17037
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         2.962
_refine_diff_density_min         -2.742
_refine_diff_density_rms         0.188
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         17037
_refine_ls_number_restraints     41
_refine_ls_R_factor_all          0.1646
_refine_ls_R_factor_gt           0.0780
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0200P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1516
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C2S-C1S
 1.5 with sigma of 0.02
 O1S-C1S
 1.4 with sigma of 0.02
 C3S-C4S
 1.5 with sigma of 0.02
 O2S-C3S
 1.4 with sigma of 0.02
 C2S-C1S
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C2S) \\sim Ueq, Uanis(C1S) \\sim Ueq, Uanis(C3S) \\sim Ueq, Uanis(C4S)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(O1S) \\sim Ueq, Uanis(O2S) \\sim Ueq: with sigma of 0.008 and sigma for
terminal atoms of 0.008
Uanis(O1S) = Uanis(O2S)
Uanis(C3S) = Uanis(C1S)
Uanis(C2S) = Uanis(C4S)
4. Others
 Fixed Sof: O1S(0.5) H1A(0.5) O2S(0.5) H10(0.5) C1S(0.5) H2A(0.5) H2B(0.5)
 C2S(0.5) H4A(0.5) H4B(0.5) H4C(0.5) C4S(0.5) H10A(0.5) H10B(0.5) H10C(0.5)
 C3S(0.5) H15A(0.5) H15B(0.5)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C29(H29)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2C,H2D), C30(H30A,H30B), C1S(H2A,H2B), C3S(H15A,H15B)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10D), C12(H12), C13(H13), C14(H14),
 C1AA(H1AA), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
 C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C34(H34), C35(H35), C36(H36),
  C37(H37), C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44),
 C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54),
  C55(H55), C56(H56)
5.d Tetrahedral OH refined with riding coordinates:
 O1S(H1A), O2S(H10)
5.e Idealised Me refined as rotating group:
 C4(H4D,H4E,H4F), C32(H32A,H32B,H32C), C2S(H4A,H4B,H4C), C4S(H10A,H10B,H10C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Nd1 Nd 0.26079(3) 0.62063(3) 0.34463(2) 0.01786(10) Uani 1 1 d . . . . .
P1 P 0.41369(14) 0.86533(13) 0.24851(10) 0.0195(4) Uani 1 1 d . . . . .
P2 P 0.53138(14) 0.70882(13) 0.26168(9) 0.0173(4) Uani 1 1 d . . . . .
P3 P 0.17800(14) 0.33292(13) 0.30637(9) 0.0193(4) Uani 1 1 d . . . . .
P4 P 0.04737(14) 0.43704(13) 0.20787(9) 0.0188(4) Uani 1 1 d . . . . .
O1 O 0.3170(3) 0.7893(3) 0.2845(3) 0.0256(11) Uani 1 1 d . . . . .
O2 O 0.4192(3) 0.6336(3) 0.2811(2) 0.0204(10) Uani 1 1 d . . . . .
O4 O 0.2558(3) 0.4423(3) 0.3361(2) 0.0224(11) Uani 1 1 d . . . . .
O5 O 0.1396(3) 0.5425(3) 0.2358(2) 0.0216(10) Uani 1 1 d . . . . .
O3 O 0.7516(5) 1.0248(4) 0.3370(3) 0.0432(14) Uani 1 1 d . . . . .
O6 O 0.0633(4) 0.4836(4) 0.3800(3) 0.0280(11) Uani 1 1 d . . . . .
O7 O 0.1079(4) 0.7007(3) 0.3519(3) 0.0295(12) Uani 1 1 d . . . . .
O8 O 0.2605(4) 0.7662(4) 0.4291(3) 0.0392(14) Uani 1 1 d . . . . .
O9 O 0.1293(5) 0.8372(4) 0.4206(3) 0.0567(18) Uani 1 1 d . . . . .
O10 O 0.4443(4) 0.6788(4) 0.4321(2) 0.0320(12) Uani 1 1 d . . . . .
O11 O 0.2913(4) 0.5707(4) 0.4711(3) 0.0339(12) Uani 1 1 d . . . . .
O12 O 0.4587(5) 0.6263(4) 0.5387(3) 0.0545(17) Uani 1 1 d . . . . .
N1 N 0.1646(5) 0.7690(5) 0.4011(3) 0.0353(16) Uani 1 1 d . . . . .
N2 N 0.3986(5) 0.6244(5) 0.4824(4) 0.0313(15) Uani 1 1 d . . . . .
C1 C 0.5491(5) 0.8490(5) 0.2786(3) 0.0164(14) Uani 1 1 d . . . . .
H1 H 0.6114 0.8966 0.2526 0.020 Uiso 1 1 calc R . . . .
C2 C 0.5788(5) 0.8834(5) 0.3575(4) 0.0240(16) Uani 1 1 d . . . . .
H2C H 0.5085 0.8837 0.3757 0.029 Uiso 1 1 calc R . . . .
H2D H 0.6027 0.8301 0.3828 0.029 Uiso 1 1 calc R . . . .
C3 C 0.6742(7) 0.9929(6) 0.3735(4) 0.0330(18) Uani 1 1 d . . . . .
C4 C 0.6700(7) 1.0549(6) 0.4372(5) 0.054(3) Uani 1 1 d . . . . .
H4D H 0.7470 1.1089 0.4529 0.082 Uiso 1 1 calc GR . . . .
H4E H 0.6447 1.0064 0.4749 0.082 Uiso 1 1 calc GR . . . .
H4F H 0.6155 1.0904 0.4256 0.082 Uiso 1 1 calc GR . . . .
C5 C 0.4416(6) 1.0010(5) 0.2743(4) 0.0231(15) Uani 1 1 d . . . . .
C6 C 0.5289(6) 1.0859(5) 0.2504(4) 0.0280(17) Uani 1 1 d . . . . .
H6 H 0.5738 1.0716 0.2180 0.034 Uiso 1 1 calc R . . . .
C7 C 0.5527(7) 1.1908(6) 0.2723(5) 0.041(2) Uani 1 1 d . . . . .
H7 H 0.6114 1.2480 0.2542 0.050 Uiso 1 1 calc R . . . .
C8 C 0.4883(8) 1.2113(6) 0.3218(4) 0.045(2) Uani 1 1 d . . . . .
H8 H 0.5044 1.2827 0.3382 0.054 Uiso 1 1 calc R . . . .
C9 C 0.4021(7) 1.1281(6) 0.3463(4) 0.040(2) Uani 1 1 d . . . . .
H9 H 0.3584 1.1425 0.3794 0.048 Uiso 1 1 calc R . . . .
C10 C 0.3778(6) 1.0224(5) 0.3234(4) 0.0335(19) Uani 1 1 d . . . . .
H10D H 0.3184 0.9654 0.3411 0.040 Uiso 1 1 calc R . . . .
C11 C 0.3820(6) 0.8463(5) 0.1547(4) 0.0230(15) Uani 1 1 d . . . . .
C12 C 0.4698(6) 0.8880(5) 0.1109(4) 0.0265(16) Uani 1 1 d . . . . .
H12 H 0.5477 0.9254 0.1310 0.032 Uiso 1 1 calc R . . . .
C13 C 0.4405(7) 0.8735(6) 0.0376(4) 0.0363(19) Uani 1 1 d . . . . .
H13 H 0.4988 0.8992 0.0077 0.044 Uiso 1 1 calc R . . . .
C14 C 0.3272(8) 0.8219(7) 0.0093(5) 0.053(2) Uani 1 1 d . . . . .
H14 H 0.3070 0.8148 -0.0404 0.063 Uiso 1 1 calc R . . . .
C1AA C 0.2406(7) 0.7793(7) 0.0531(5) 0.055(3) Uani 1 1 d . . . . .
H1AA H 0.1624 0.7425 0.0331 0.066 Uiso 1 1 calc R . . . .
C16 C 0.2707(6) 0.7917(6) 0.1259(5) 0.039(2) Uani 1 1 d . . . . .
H16 H 0.2129 0.7617 0.1557 0.047 Uiso 1 1 calc R . . . .
C17 C 0.6514(5) 0.6917(5) 0.3119(3) 0.0196(14) Uani 1 1 d . . . . .
C18 C 0.6335(6) 0.5988(5) 0.3472(4) 0.0278(17) Uani 1 1 d . . . . .
H18 H 0.5573 0.5473 0.3464 0.033 Uiso 1 1 calc R . . . .
C19 C 0.7253(6) 0.5804(6) 0.3834(4) 0.0336(19) Uani 1 1 d . . . . .
H19 H 0.7122 0.5169 0.4078 0.040 Uiso 1 1 calc R . . . .
C20 C 0.8358(6) 0.6546(6) 0.3840(4) 0.0366(19) Uani 1 1 d . . . . .
H20 H 0.8990 0.6404 0.4075 0.044 Uiso 1 1 calc R . . . .
C21 C 0.8569(6) 0.7504(5) 0.3507(4) 0.0285(17) Uani 1 1 d . . . . .
H21 H 0.9330 0.8023 0.3524 0.034 Uiso 1 1 calc R . . . .
C22 C 0.7638(6) 0.7673(5) 0.3152(4) 0.0268(16) Uani 1 1 d . . . . .
H22 H 0.7765 0.8321 0.2925 0.032 Uiso 1 1 calc R . . . .
C23 C 0.5371(5) 0.6844(5) 0.1701(4) 0.0198(15) Uani 1 1 d . . . . .
C24 C 0.4376(6) 0.6194(5) 0.1279(4) 0.0317(18) Uani 1 1 d . . . . .
H24 H 0.3673 0.5901 0.1476 0.038 Uiso 1 1 calc R . . . .
C25 C 0.4391(8) 0.5966(6) 0.0579(4) 0.045(2) Uani 1 1 d . . . . .
H25 H 0.3705 0.5507 0.0298 0.054 Uiso 1 1 calc R . . . .
C26 C 0.5406(8) 0.6407(6) 0.0285(4) 0.045(2) Uani 1 1 d . . . . .
H26 H 0.5410 0.6255 -0.0200 0.054 Uiso 1 1 calc R . . . .
C27 C 0.6409(7) 0.7061(6) 0.0685(4) 0.037(2) Uani 1 1 d . . . . .
H27 H 0.7106 0.7365 0.0483 0.044 Uiso 1 1 calc R . . . .
C28 C 0.6380(6) 0.7270(5) 0.1403(4) 0.0259(16) Uani 1 1 d . . . . .
H28 H 0.7069 0.7713 0.1688 0.031 Uiso 1 1 calc R . . . .
C29 C 0.0356(5) 0.3279(5) 0.2659(3) 0.0171(14) Uani 1 1 d . . . . .
H29 H 0.0028 0.2614 0.2341 0.020 Uiso 1 1 calc R . . . .
C30 C -0.0525(5) 0.3127(5) 0.3199(4) 0.0245(16) Uani 1 1 d . . . . .
H30A H -0.1280 0.3049 0.2933 0.029 Uiso 1 1 calc R . . . .
H30B H -0.0631 0.2449 0.3427 0.029 Uiso 1 1 calc R . . . .
C31 C -0.0214(6) 0.4003(6) 0.3769(4) 0.0245(16) Uani 1 1 d . . . . .
C32 C -0.1017(7) 0.3815(6) 0.4317(5) 0.049(2) Uani 1 1 d . . . . .
H32A H -0.0926 0.3269 0.4625 0.073 Uiso 1 1 calc GR . . . .
H32B H -0.1816 0.3570 0.4085 0.073 Uiso 1 1 calc GR . . . .
H32C H -0.0832 0.4482 0.4597 0.073 Uiso 1 1 calc GR . . . .
C33 C 0.1568(5) 0.2380(5) 0.3732(4) 0.0214(15) Uani 1 1 d . . . . .
C34 C 0.2337(6) 0.2706(5) 0.4354(4) 0.0243(16) Uani 1 1 d . . . . .
H34 H 0.2881 0.3422 0.4425 0.029 Uiso 1 1 calc R . . . .
C35 C 0.2306(7) 0.1991(6) 0.4863(4) 0.0351(19) Uani 1 1 d . . . . .
H35 H 0.2838 0.2215 0.5283 0.042 Uiso 1 1 calc R . . . .
C36 C 0.1509(7) 0.0949(7) 0.4774(5) 0.045(2) Uani 1 1 d . . . . .
H36 H 0.1492 0.0464 0.5132 0.054 Uiso 1 1 calc R . . . .
C37 C 0.0732(6) 0.0615(6) 0.4157(4) 0.0328(18) Uani 1 1 d . . . . .
H37 H 0.0190 -0.0101 0.4086 0.039 Uiso 1 1 calc R . . . .
C38 C 0.0763(6) 0.1348(5) 0.3646(4) 0.0294(17) Uani 1 1 d . . . . .
H38 H 0.0219 0.1132 0.3231 0.035 Uiso 1 1 calc R . . . .
C39 C 0.2405(5) 0.2907(5) 0.2377(4) 0.0211(15) Uani 1 1 d . . . . .
C40 C 0.3336(6) 0.3686(6) 0.2118(4) 0.0318(18) Uani 1 1 d . . . . .
H40 H 0.3621 0.4404 0.2306 0.038 Uiso 1 1 calc R . . . .
C41 C 0.3844(6) 0.3399(6) 0.1582(4) 0.038(2) Uani 1 1 d . . . . .
H41 H 0.4455 0.3933 0.1392 0.046 Uiso 1 1 calc R . . . .
C42 C 0.3477(6) 0.2361(6) 0.1326(4) 0.0366(19) Uani 1 1 d . . . . .
H42 H 0.3827 0.2170 0.0960 0.044 Uiso 1 1 calc R . . . .
C43 C 0.2594(7) 0.1600(6) 0.1606(4) 0.039(2) Uani 1 1 d . . . . .
H43 H 0.2359 0.0874 0.1443 0.046 Uiso 1 1 calc R . . . .
C44 C 0.2043(6) 0.1848(5) 0.2111(4) 0.0332(19) Uani 1 1 d . . . . .
H44 H 0.1416 0.1305 0.2282 0.040 Uiso 1 1 calc R . . . .
C45 C -0.0892(5) 0.4512(5) 0.1941(4) 0.0173(14) Uani 1 1 d . . . . .
C46 C -0.0968(6) 0.5451(6) 0.2189(4) 0.041(2) Uani 1 1 d . . . . .
H46 H -0.0324 0.5973 0.2469 0.049 Uiso 1 1 calc R . . . .
C47 C -0.1985(7) 0.5625(7) 0.2028(5) 0.056(3) Uani 1 1 d . . . . .
H47 H -0.2026 0.6275 0.2190 0.068 Uiso 1 1 calc R . . . .
C48 C -0.2935(6) 0.4870(6) 0.1639(5) 0.042(2) Uani 1 1 d . . . . .
H48 H -0.3626 0.4999 0.1531 0.050 Uiso 1 1 calc R . . . .
C49 C -0.2880(6) 0.3912(5) 0.1401(4) 0.0308(18) Uani 1 1 d . . . . .
H49 H -0.3540 0.3380 0.1142 0.037 Uiso 1 1 calc R . . . .
C50 C -0.1849(5) 0.3735(5) 0.1546(4) 0.0285(17) Uani 1 1 d . . . . .
H50 H -0.1802 0.3091 0.1377 0.034 Uiso 1 1 calc R . . . .
C51 C 0.0724(5) 0.3987(6) 0.1230(4) 0.0253(16) Uani 1 1 d . . . . .
C52 C 0.1155(6) 0.4839(7) 0.0794(4) 0.043(2) Uani 1 1 d . . . . .
H52 H 0.1329 0.5553 0.0962 0.051 Uiso 1 1 calc R . . . .
C53 C 0.1324(7) 0.4619(9) 0.0109(5) 0.058(3) Uani 1 1 d . . . . .
H53 H 0.1620 0.5187 -0.0190 0.070 Uiso 1 1 calc R . . . .
C54 C 0.1062(7) 0.3583(9) -0.0130(5) 0.058(3) Uani 1 1 d . . . . .
H54 H 0.1173 0.3440 -0.0597 0.070 Uiso 1 1 calc R . . . .
C55 C 0.0645(7) 0.2759(7) 0.0290(5) 0.050(2) Uani 1 1 d . . . . .
H55 H 0.0481 0.2046 0.0122 0.059 Uiso 1 1 calc R . . . .
C56 C 0.0464(6) 0.2963(6) 0.0959(4) 0.0363(19) Uani 1 1 d . . . . .
H56 H 0.0149 0.2380 0.1244 0.044 Uiso 1 1 calc R . . . .
O13 O 0.7474(4) 0.9692(4) 0.1725(3) 0.0463(15) Uani 1 1 d . . . . .
O14 O 0.7861(5) 1.1399(4) 0.1828(3) 0.0489(16) Uani 1 1 d . . . . .
O15 O 0.9238(4) 1.0802(4) 0.2001(3) 0.0385(14) Uani 1 1 d . . . . .
N3 N 0.8171(5) 1.0632(5) 0.1853(3) 0.0329(15) Uani 1 1 d . . . . .
O1S O 0.0749(11) 0.8928(10) 0.2304(8) 0.076(3) Uani 0.5 1 d D U P A 2
H1A H 0.1209 0.8608 0.2362 0.113 Uiso 0.5 1 calc R . P A 2
O2S O 0.0231(12) 0.9867(12) -0.0049(10) 0.076(3) Uani 0.5 1 d D U P B -1
H10 H 0.0376 0.9474 0.0254 0.113 Uiso 0.5 1 calc R . P B -1
C1S C 0.0132(16) 0.8632(15) 0.1702(10) 0.072(4) Uani 0.5 1 d D U P A 2
H2A H -0.0367 0.7885 0.1774 0.086 Uiso 0.5 1 calc R . P A 2
H2B H 0.0695 0.8568 0.1404 0.086 Uiso 0.5 1 calc R . P A 2
C2S C -0.0567(17) 0.8933(17) 0.1243(12) 0.091(5) Uani 0.5 1 d D U P A 2
H4A H -0.0476 0.8759 0.0761 0.136 Uiso 0.5 1 calc GR . P A 2
H4B H -0.0363 0.9706 0.1310 0.136 Uiso 0.5 1 calc GR . P A 2
H4C H -0.1371 0.8555 0.1322 0.136 Uiso 0.5 1 calc GR . P A 2
C4S C 0.2118(17) 1.0127(16) -0.0037(13) 0.091(5) Uani 0.5 1 d D U P B -1
H10A H 0.2754 1.0592 0.0307 0.136 Uiso 0.5 1 calc GR . P B -1
H10B H 0.2421 1.0026 -0.0469 0.136 Uiso 0.5 1 calc GR . P B -1
H10C H 0.1748 0.9433 0.0159 0.136 Uiso 0.5 1 calc GR . P B -1
C3S C 0.1255(13) 1.0630(14) -0.0202(12) 0.072(4) Uani 0.5 1 d D U P B -1
H15A H 0.1466 1.1298 0.0094 0.086 Uiso 0.5 1 calc R . P B -1
H15B H 0.1194 1.0794 -0.0704 0.086 Uiso 0.5 1 calc R . P B -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
Nd1 O1 2.462(5) . ?
Nd1 O2 2.410(4) . ?
Nd1 O4 2.389(4) . ?
Nd1 O5 2.405(5) . ?
Nd1 O6 2.657(5) . ?
Nd1 O7 2.551(4) . ?
Nd1 O8 2.536(5) . ?
Nd1 O10 2.540(5) . ?
Nd1 O11 2.543(5) . ?
P1 O1 1.514(5) . ?
P1 C1 1.826(6) . ?
P1 C5 1.785(7) . ?
P1 C11 1.787(7) . ?
P2 O2 1.492(4) . ?
P2 C1 1.842(6) . ?
P2 C17 1.783(6) . ?
P2 C23 1.796(7) . ?
P3 O4 1.496(4) . ?
P3 C29 1.843(6) . ?
P3 C33 1.791(7) . ?
P3 C39 1.800(7) . ?
P4 O5 1.505(5) . ?
P4 C29 1.827(6) . ?
P4 C45 1.789(6) . ?
P4 C51 1.798(8) . ?
O3 C3 1.217(9) . ?
O6 C31 1.222(7) . ?
O7 N1 1.257(7) . ?
O8 N1 1.275(7) . ?
O9 N1 1.235(7) . ?
O10 N2 1.278(7) . ?
O11 N2 1.262(7) . ?
O12 N2 1.236(7) . ?
C1 H1 1.0000 . ?
C1 C2 1.537(9) . ?
C2 H2C 0.9900 . ?
C2 H2D 0.9900 . ?
C2 C3 1.517(9) . ?
C3 C4 1.488(10) . ?
C4 H4D 0.9800 . ?
C4 H4E 0.9800 . ?
C4 H4F 0.9800 . ?
C5 C6 1.387(9) . ?
C5 C10 1.400(10) . ?
C6 H6 0.9500 . ?
C6 C7 1.385(9) . ?
C7 H7 0.9500 . ?
C7 C8 1.407(11) . ?
C8 H8 0.9500 . ?
C8 C9 1.372(10) . ?
C9 H9 0.9500 . ?
C9 C10 1.398(9) . ?
C10 H10D 0.9500 . ?
C11 C12 1.418(9) . ?
C11 C16 1.360(9) . ?
C12 H12 0.9500 . ?
C12 C13 1.400(10) . ?
C13 H13 0.9500 . ?
C13 C14 1.370(10) . ?
C14 H14 0.9500 . ?
C14 C1AA 1.408(11) . ?
C1AA H1AA 0.9500 . ?
C1AA C16 1.392(11) . ?
C16 H16 0.9500 . ?
C17 C18 1.387(9) . ?
C17 C22 1.395(8) . ?
C18 H18 0.9500 . ?
C18 C19 1.380(9) . ?
C19 H19 0.9500 . ?
C19 C20 1.377(9) . ?
C20 H20 0.9500 . ?
C20 C21 1.397(9) . ?
C21 H21 0.9500 . ?
C21 C22 1.378(9) . ?
C22 H22 0.9500 . ?
C23 C24 1.383(9) . ?
C23 C28 1.380(8) . ?
C24 H24 0.9500 . ?
C24 C25 1.377(10) . ?
C25 H25 0.9500 . ?
C25 C26 1.384(11) . ?
C26 H26 0.9500 . ?
C26 C27 1.373(11) . ?
C27 H27 0.9500 . ?
C27 C28 1.407(10) . ?
C28 H28 0.9500 . ?
C29 H29 1.0000 . ?
C29 C30 1.566(9) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.507(9) . ?
C31 C32 1.501(9) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.395(9) . ?
C33 C38 1.378(9) . ?
C34 H34 0.9500 . ?
C34 C35 1.374(9) . ?
C35 H35 0.9500 . ?
C35 C36 1.384(10) . ?
C36 H36 0.9500 . ?
C36 C37 1.393(11) . ?
C37 H37 0.9500 . ?
C37 C38 1.392(9) . ?
C38 H38 0.9500 . ?
C39 C40 1.398(9) . ?
C39 C44 1.399(9) . ?
C40 H40 0.9500 . ?
C40 C41 1.396(10) . ?
C41 H41 0.9500 . ?
C41 C42 1.367(9) . ?
C42 H42 0.9500 . ?
C42 C43 1.372(9) . ?
C43 H43 0.9500 . ?
C43 C44 1.362(10) . ?
C44 H44 0.9500 . ?
C45 C46 1.391(9) . ?
C45 C50 1.395(8) . ?
C46 H46 0.9500 . ?
C46 C47 1.387(9) . ?
C47 H47 0.9500 . ?
C47 C48 1.374(10) . ?
C48 H48 0.9500 . ?
C48 C49 1.396(10) . ?
C49 H49 0.9500 . ?
C49 C50 1.402(9) . ?
C50 H50 0.9500 . ?
C51 C52 1.406(10) . ?
C51 C56 1.378(9) . ?
C52 H52 0.9500 . ?
C52 C53 1.400(12) . ?
C53 H53 0.9500 . ?
C53 C54 1.372(12) . ?
C54 H54 0.9500 . ?
C54 C55 1.359(12) . ?
C55 H55 0.9500 . ?
C55 C56 1.369(11) . ?
C56 H56 0.9500 . ?
O13 N3 1.246(7) . ?
O14 N3 1.236(7) . ?
O15 N3 1.271(7) . ?
O1S H1A 0.8400 . ?
O1S C1S 1.279(15) . ?
O2S H10 0.8400 . ?
O2S C3S 1.384(15) . ?
C1S H2A 0.9900 . ?
C1S H2B 0.9900 . ?
C1S C2S 1.343(12) . ?
C2S H4A 0.9800 . ?
C2S H4B 0.9800 . ?
C2S H4C 0.9800 . ?
C4S H10A 0.9800 . ?
C4S H10B 0.9800 . ?
C4S H10C 0.9800 . ?
C4S C3S 1.488(15) . ?
C3S H15A 0.9900 . ?
C3S H15B 0.9900 . ?

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 Nd1 O6 134.54(14) . . ?
O1 Nd1 O7 71.15(14) . . ?
O1 Nd1 O8 71.83(17) . . ?
O1 Nd1 O10 94.86(15) . . ?
O1 Nd1 O11 134.86(16) . . ?
O2 Nd1 O1 71.61(14) . . ?
O2 Nd1 O6 142.94(14) . . ?
O2 Nd1 O7 141.27(15) . . ?
O2 Nd1 O8 124.48(15) . . ?
O2 Nd1 O10 71.75(16) . . ?
O2 Nd1 O11 112.53(16) . . ?
O4 Nd1 O1 142.62(15) . . ?
O4 Nd1 O2 75.42(14) . . ?
O4 Nd1 O5 75.03(14) . . ?
O4 Nd1 O6 69.75(14) . . ?
O4 Nd1 O7 134.11(14) . . ?
O4 Nd1 O8 144.03(16) . . ?
O4 Nd1 O10 91.10(15) . . ?
O4 Nd1 O11 74.55(16) . . ?
O5 Nd1 O1 85.20(15) . . ?
O5 Nd1 O2 85.48(15) . . ?
O5 Nd1 O6 73.85(15) . . ?
O5 Nd1 O7 81.22(15) . . ?
O5 Nd1 O8 130.65(15) . . ?
O5 Nd1 O10 155.85(14) . . ?
O5 Nd1 O11 138.87(15) . . ?
O7 Nd1 O6 66.14(15) . . ?
O8 Nd1 O6 91.85(16) . . ?
O8 Nd1 O7 50.40(14) . . ?
O8 Nd1 O10 71.35(16) . . ?
O8 Nd1 O11 70.09(17) . . ?
O10 Nd1 O6 120.29(16) . . ?
O10 Nd1 O7 121.71(16) . . ?
O10 Nd1 O11 50.27(15) . . ?
O11 Nd1 O6 70.04(15) . . ?
O11 Nd1 O7 101.12(16) . . ?
O1 P1 C1 110.0(3) . . ?
O1 P1 C5 111.0(3) . . ?
O1 P1 C11 111.7(3) . . ?
C5 P1 C1 104.1(3) . . ?
C5 P1 C11 109.4(3) . . ?
C11 P1 C1 110.4(3) . . ?
O2 P2 C1 111.2(3) . . ?
O2 P2 C17 111.7(3) . . ?
O2 P2 C23 109.2(3) . . ?
C17 P2 C1 106.6(3) . . ?
C17 P2 C23 108.2(3) . . ?
C23 P2 C1 109.8(3) . . ?
O4 P3 C29 112.6(3) . . ?
O4 P3 C33 110.9(3) . . ?
O4 P3 C39 110.1(3) . . ?
C33 P3 C29 108.6(3) . . ?
C33 P3 C39 108.3(3) . . ?
C39 P3 C29 106.2(3) . . ?
O5 P4 C29 113.9(3) . . ?
O5 P4 C45 109.2(3) . . ?
O5 P4 C51 110.6(3) . . ?
C45 P4 C29 108.6(3) . . ?
C45 P4 C51 106.0(3) . . ?
C51 P4 C29 108.3(3) . . ?
P1 O1 Nd1 142.1(2) . . ?
P2 O2 Nd1 143.8(2) . . ?
P3 O4 Nd1 140.6(2) . . ?
P4 O5 Nd1 138.2(2) . . ?
C31 O6 Nd1 156.9(4) . . ?
N1 O7 Nd1 95.8(4) . . ?
N1 O8 Nd1 96.0(4) . . ?
N2 O10 Nd1 96.5(4) . . ?
N2 O11 Nd1 96.8(4) . . ?
O7 N1 O8 117.5(5) . . ?
O9 N1 O7 121.0(6) . . ?
O9 N1 O8 121.5(6) . . ?
O11 N2 O10 116.5(6) . . ?
O12 N2 O10 120.2(6) . . ?
O12 N2 O11 123.3(6) . . ?
P1 C1 P2 109.6(3) . . ?
P1 C1 H1 109.4 . . ?
P2 C1 H1 109.4 . . ?
C2 C1 P1 106.8(4) . . ?
C2 C1 P2 112.1(4) . . ?
C2 C1 H1 109.4 . . ?
C1 C2 H2C 108.8 . . ?
C1 C2 H2D 108.8 . . ?
H2C C2 H2D 107.7 . . ?
C3 C2 C1 113.6(6) . . ?
C3 C2 H2C 108.8 . . ?
C3 C2 H2D 108.8 . . ?
O3 C3 C2 120.4(7) . . ?
O3 C3 C4 122.9(7) . . ?
C4 C3 C2 116.6(7) . . ?
C3 C4 H4D 109.5 . . ?
C3 C4 H4E 109.5 . . ?
C3 C4 H4F 109.5 . . ?
H4D C4 H4E 109.5 . . ?
H4D C4 H4F 109.5 . . ?
H4E C4 H4F 109.5 . . ?
C6 C5 P1 122.1(5) . . ?
C6 C5 C10 118.8(6) . . ?
C10 C5 P1 119.0(5) . . ?
C5 C6 H6 119.0 . . ?
C7 C6 C5 121.9(7) . . ?
C7 C6 H6 119.0 . . ?
C6 C7 H7 120.6 . . ?
C6 C7 C8 118.8(7) . . ?
C8 C7 H7 120.6 . . ?
C7 C8 H8 120.0 . . ?
C9 C8 C7 119.9(7) . . ?
C9 C8 H8 120.0 . . ?
C8 C9 H9 119.5 . . ?
C8 C9 C10 121.0(8) . . ?
C10 C9 H9 119.5 . . ?
C5 C10 H10D 120.2 . . ?
C9 C10 C5 119.6(7) . . ?
C9 C10 H10D 120.2 . . ?
C12 C11 P1 121.3(5) . . ?
C16 C11 P1 118.4(6) . . ?
C16 C11 C12 120.3(7) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 C11 119.3(7) . . ?
C13 C12 H12 120.3 . . ?
C12 C13 H13 120.2 . . ?
C14 C13 C12 119.7(8) . . ?
C14 C13 H13 120.2 . . ?
C13 C14 H14 119.6 . . ?
C13 C14 C1AA 120.8(8) . . ?
C1AA C14 H14 119.6 . . ?
C14 C1AA H1AA 120.4 . . ?
C16 C1AA C14 119.3(7) . . ?
C16 C1AA H1AA 120.4 . . ?
C11 C16 C1AA 120.6(8) . . ?
C11 C16 H16 119.7 . . ?
C1AA C16 H16 119.7 . . ?
C18 C17 P2 119.2(5) . . ?
C18 C17 C22 118.5(6) . . ?
C22 C17 P2 122.3(5) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 C17 120.7(7) . . ?
C19 C18 H18 119.6 . . ?
C18 C19 H19 120.2 . . ?
C20 C19 C18 119.7(7) . . ?
C20 C19 H19 120.2 . . ?
C19 C20 H20 119.4 . . ?
C19 C20 C21 121.2(7) . . ?
C21 C20 H20 119.4 . . ?
C20 C21 H21 121.0 . . ?
C22 C21 C20 118.0(6) . . ?
C22 C21 H21 121.0 . . ?
C17 C22 H22 119.1 . . ?
C21 C22 C17 121.8(6) . . ?
C21 C22 H22 119.1 . . ?
C24 C23 P2 119.2(5) . . ?
C28 C23 P2 122.2(5) . . ?
C28 C23 C24 118.5(7) . . ?
C23 C24 H24 119.5 . . ?
C25 C24 C23 121.0(7) . . ?
C25 C24 H24 119.5 . . ?
C24 C25 H25 120.1 . . ?
C24 C25 C26 119.9(8) . . ?
C26 C25 H25 120.1 . . ?
C25 C26 H26 119.5 . . ?
C27 C26 C25 120.9(8) . . ?
C27 C26 H26 119.5 . . ?
C26 C27 H27 120.8 . . ?
C26 C27 C28 118.3(7) . . ?
C28 C27 H27 120.8 . . ?
C23 C28 C27 121.4(7) . . ?
C23 C28 H28 119.3 . . ?
C27 C28 H28 119.3 . . ?
P3 C29 H29 105.2 . . ?
P4 C29 P3 112.2(3) . . ?
P4 C29 H29 105.2 . . ?
C30 C29 P3 113.6(5) . . ?
C30 C29 P4 114.2(4) . . ?
C30 C29 H29 105.2 . . ?
C29 C30 H30A 108.1 . . ?
C29 C30 H30B 108.1 . . ?
H30A C30 H30B 107.3 . . ?
C31 C30 C29 116.6(5) . . ?
C31 C30 H30A 108.1 . . ?
C31 C30 H30B 108.1 . . ?
O6 C31 C30 123.8(6) . . ?
O6 C31 C32 119.8(7) . . ?
C32 C31 C30 116.3(6) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 P3 116.3(5) . . ?
C38 C33 P3 124.3(6) . . ?
C38 C33 C34 119.3(6) . . ?
C33 C34 H34 120.1 . . ?
C35 C34 C33 119.9(7) . . ?
C35 C34 H34 120.1 . . ?
C34 C35 H35 119.5 . . ?
C34 C35 C36 120.9(7) . . ?
C36 C35 H35 119.5 . . ?
C35 C36 H36 120.1 . . ?
C35 C36 C37 119.7(7) . . ?
C37 C36 H36 120.1 . . ?
C36 C37 H37 120.5 . . ?
C38 C37 C36 118.9(7) . . ?
C38 C37 H37 120.5 . . ?
C33 C38 C37 121.2(7) . . ?
C33 C38 H38 119.4 . . ?
C37 C38 H38 119.4 . . ?
C40 C39 P3 117.4(5) . . ?
C40 C39 C44 118.7(6) . . ?
C44 C39 P3 123.9(5) . . ?
C39 C40 H40 120.3 . . ?
C41 C40 C39 119.4(7) . . ?
C41 C40 H40 120.3 . . ?
C40 C41 H41 119.4 . . ?
C42 C41 C40 121.1(7) . . ?
C42 C41 H41 119.4 . . ?
C41 C42 H42 120.7 . . ?
C41 C42 C43 118.6(7) . . ?
C43 C42 H42 120.7 . . ?
C42 C43 H43 118.8 . . ?
C44 C43 C42 122.4(7) . . ?
C44 C43 H43 118.8 . . ?
C39 C44 H44 120.2 . . ?
C43 C44 C39 119.7(7) . . ?
C43 C44 H44 120.2 . . ?
C46 C45 P4 118.8(5) . . ?
C46 C45 C50 119.9(6) . . ?
C50 C45 P4 121.1(5) . . ?
C45 C46 H46 120.1 . . ?
C47 C46 C45 119.9(7) . . ?
C47 C46 H46 120.1 . . ?
C46 C47 H47 119.5 . . ?
C48 C47 C46 121.0(7) . . ?
C48 C47 H47 119.5 . . ?
C47 C48 H48 120.1 . . ?
C47 C48 C49 119.8(7) . . ?
C49 C48 H48 120.1 . . ?
C48 C49 H49 120.0 . . ?
C48 C49 C50 119.9(6) . . ?
C50 C49 H49 120.0 . . ?
C45 C50 C49 119.6(6) . . ?
C45 C50 H50 120.2 . . ?
C49 C50 H50 120.2 . . ?
C52 C51 P4 114.6(6) . . ?
C56 C51 P4 127.0(6) . . ?
C56 C51 C52 118.3(7) . . ?
C51 C52 H52 120.5 . . ?
C53 C52 C51 119.1(8) . . ?
C53 C52 H52 120.5 . . ?
C52 C53 H53 120.0 . . ?
C54 C53 C52 120.0(9) . . ?
C54 C53 H53 120.0 . . ?
C53 C54 H54 119.5 . . ?
C55 C54 C53 121.0(9) . . ?
C55 C54 H54 119.5 . . ?
C54 C55 H55 120.3 . . ?
C54 C55 C56 119.5(9) . . ?
C56 C55 H55 120.3 . . ?
C51 C56 H56 119.0 . . ?
C55 C56 C51 122.1(8) . . ?
C55 C56 H56 119.0 . . ?
O13 N3 O15 118.6(6) . . ?
O14 N3 O13 122.2(6) . . ?
O14 N3 O15 119.3(6) . . ?
C1S O1S H1A 109.5 . . ?
C3S O2S H10 109.5 . . ?
O1S C1S H2A 102.0 . . ?
O1S C1S H2B 102.0 . . ?
O1S C1S C2S 140(2) . . ?
H2A C1S H2B 104.8 . . ?
C2S C1S H2A 102.0 . . ?
C2S C1S H2B 102.0 . . ?
C1S C2S H4A 109.5 . . ?
C1S C2S H4B 109.5 . . ?
C1S C2S H4C 109.5 . . ?
H4A C2S H4B 109.5 . . ?
H4A C2S H4C 109.5 . . ?
H4B C2S H4C 109.5 . . ?
H10A C4S H10B 109.5 . . ?
H10A C4S H10C 109.5 . . ?
H10B C4S H10C 109.5 . . ?
C3S C4S H10A 109.5 . . ?
C3S C4S H10B 109.5 . . ?
C3S C4S H10C 109.5 . . ?
O2S C3S C4S 104.1(15) . . ?
O2S C3S H15A 110.9 . . ?
O2S C3S H15B 110.9 . . ?
C4S C3S H15A 110.9 . . ?
C4S C3S H15B 110.9 . . ?
H15A C3S H15B 109.0 . . ?

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
Nd1 O6 C31 C30 -7.0(16) . . . . ?
Nd1 O6 C31 C32 173.5(8) . . . . ?
Nd1 O7 N1 O8 -5.3(7) . . . . ?
Nd1 O7 N1 O9 173.5(6) . . . . ?
Nd1 O8 N1 O7 5.3(7) . . . . ?
Nd1 O8 N1 O9 -173.5(6) . . . . ?
Nd1 O10 N2 O11 -1.4(6) . . . . ?
Nd1 O10 N2 O12 178.7(6) . . . . ?
Nd1 O11 N2 O10 1.4(6) . . . . ?
Nd1 O11 N2 O12 -178.7(6) . . . . ?
P1 C1 C2 C3 -103.8(5) . . . . ?
P1 C5 C6 C7 -177.9(6) . . . . ?
P1 C5 C10 C9 177.3(6) . . . . ?
P1 C11 C12 C13 -178.4(5) . . . . ?
P1 C11 C16 C1AA 176.8(6) . . . . ?
P2 C1 C2 C3 136.1(5) . . . . ?
P2 C17 C18 C19 176.5(5) . . . . ?
P2 C17 C22 C21 -176.0(5) . . . . ?
P2 C23 C24 C25 -178.4(6) . . . . ?
P2 C23 C28 C27 179.4(5) . . . . ?
P3 C29 C30 C31 62.6(7) . . . . ?
P3 C33 C34 C35 -173.6(5) . . . . ?
P3 C33 C38 C37 172.6(5) . . . . ?
P3 C39 C40 C41 -179.5(6) . . . . ?
P3 C39 C44 C43 -177.8(6) . . . . ?
P4 C29 C30 C31 -67.9(7) . . . . ?
P4 C45 C46 C47 173.6(7) . . . . ?
P4 C45 C50 C49 -174.9(5) . . . . ?
P4 C51 C52 C53 -176.8(6) . . . . ?
P4 C51 C56 C55 177.0(6) . . . . ?
O1 P1 C1 P2 56.9(4) . . . . ?
O1 P1 C1 C2 -64.8(5) . . . . ?
O1 P1 C5 C6 177.8(5) . . . . ?
O1 P1 C5 C10 1.6(7) . . . . ?
O1 P1 C11 C12 -163.7(5) . . . . ?
O1 P1 C11 C16 17.1(6) . . . . ?
O2 P2 C1 P1 -43.3(4) . . . . ?
O2 P2 C1 C2 75.0(5) . . . . ?
O2 P2 C17 C18 17.0(6) . . . . ?
O2 P2 C17 C22 -165.1(5) . . . . ?
O2 P2 C23 C24 11.6(6) . . . . ?
O2 P2 C23 C28 -167.4(5) . . . . ?
O4 P3 C29 P4 46.9(4) . . . . ?
O4 P3 C29 C30 -84.6(5) . . . . ?
O4 P3 C33 C34 -15.2(6) . . . . ?
O4 P3 C33 C38 169.6(5) . . . . ?
O4 P3 C39 C40 -13.2(6) . . . . ?
O4 P3 C39 C44 164.2(6) . . . . ?
O5 P4 C29 P3 -39.9(4) . . . . ?
O5 P4 C29 C30 91.2(5) . . . . ?
O5 P4 C45 C46 -9.2(7) . . . . ?
O5 P4 C45 C50 166.0(5) . . . . ?
O5 P4 C51 C52 -37.3(6) . . . . ?
O5 P4 C51 C56 147.5(6) . . . . ?
C1 P1 O1 Nd1 -22.5(5) . . . . ?
C1 P1 C5 C6 59.5(6) . . . . ?
C1 P1 C5 C10 -116.7(6) . . . . ?
C1 P1 C11 C12 -40.9(6) . . . . ?
C1 P1 C11 C16 139.9(5) . . . . ?
C1 P2 O2 Nd1 -14.7(5) . . . . ?
C1 P2 C17 C18 138.7(5) . . . . ?
C1 P2 C17 C22 -43.4(6) . . . . ?
C1 P2 C23 C24 -110.5(5) . . . . ?
C1 P2 C23 C28 70.5(6) . . . . ?
C1 C2 C3 O3 -32.4(9) . . . . ?
C1 C2 C3 C4 150.4(6) . . . . ?
C5 P1 O1 Nd1 -137.1(4) . . . . ?
C5 P1 C1 P2 175.8(3) . . . . ?
C5 P1 C1 C2 54.2(5) . . . . ?
C5 P1 C11 C12 73.1(6) . . . . ?
C5 P1 C11 C16 -106.1(6) . . . . ?
C5 C6 C7 C8 1.8(11) . . . . ?
C6 C5 C10 C9 1.0(11) . . . . ?
C6 C7 C8 C9 -1.3(12) . . . . ?
C7 C8 C9 C10 0.7(12) . . . . ?
C8 C9 C10 C5 -0.5(11) . . . . ?
C10 C5 C6 C7 -1.6(11) . . . . ?
C11 P1 O1 Nd1 100.5(5) . . . . ?
C11 P1 C1 P2 -66.9(4) . . . . ?
C11 P1 C1 C2 171.4(4) . . . . ?
C11 P1 C5 C6 -58.4(6) . . . . ?
C11 P1 C5 C10 125.3(6) . . . . ?
C11 C12 C13 C14 1.8(10) . . . . ?
C12 C11 C16 C1AA -2.4(11) . . . . ?
C12 C13 C14 C1AA -2.7(12) . . . . ?
C13 C14 C1AA C16 1.1(14) . . . . ?
C14 C1AA C16 C11 1.5(13) . . . . ?
C16 C11 C12 C13 0.8(10) . . . . ?
C17 P2 O2 Nd1 104.3(4) . . . . ?
C17 P2 C1 P1 -165.3(3) . . . . ?
C17 P2 C1 C2 -46.9(5) . . . . ?
C17 P2 C23 C24 133.4(5) . . . . ?
C17 P2 C23 C28 -45.6(6) . . . . ?
C17 C18 C19 C20 -0.6(11) . . . . ?
C18 C17 C22 C21 2.0(10) . . . . ?
C18 C19 C20 C21 2.4(11) . . . . ?
C19 C20 C21 C22 -1.9(11) . . . . ?
C20 C21 C22 C17 -0.3(10) . . . . ?
C22 C17 C18 C19 -1.5(10) . . . . ?
C23 P2 O2 Nd1 -136.0(4) . . . . ?
C23 P2 C1 P1 77.6(4) . . . . ?
C23 P2 C1 C2 -164.0(4) . . . . ?
C23 P2 C17 C18 -103.2(6) . . . . ?
C23 P2 C17 C22 74.7(6) . . . . ?
C23 C24 C25 C26 -1.3(12) . . . . ?
C24 C23 C28 C27 0.4(10) . . . . ?
C24 C25 C26 C27 0.8(12) . . . . ?
C25 C26 C27 C28 0.2(11) . . . . ?
C26 C27 C28 C23 -0.8(10) . . . . ?
C28 C23 C24 C25 0.6(10) . . . . ?
C29 P3 O4 Nd1 -3.8(5) . . . . ?
C29 P3 C33 C34 -139.4(5) . . . . ?
C29 P3 C33 C38 45.4(6) . . . . ?
C29 P3 C39 C40 109.0(5) . . . . ?
C29 P3 C39 C44 -73.7(6) . . . . ?
C29 P4 O5 Nd1 -12.6(5) . . . . ?
C29 P4 C45 C46 115.5(6) . . . . ?
C29 P4 C45 C50 -69.3(6) . . . . ?
C29 P4 C51 C52 -162.8(5) . . . . ?
C29 P4 C51 C56 22.1(7) . . . . ?
C29 C30 C31 O6 5.0(10) . . . . ?
C29 C30 C31 C32 -175.5(6) . . . . ?
C33 P3 O4 Nd1 -125.7(4) . . . . ?
C33 P3 C29 P4 170.1(3) . . . . ?
C33 P3 C29 C30 38.6(5) . . . . ?
C33 P3 C39 C40 -134.5(5) . . . . ?
C33 P3 C39 C44 42.8(7) . . . . ?
C33 C34 C35 C36 -0.9(11) . . . . ?
C34 C33 C38 C37 -2.5(10) . . . . ?
C34 C35 C36 C37 0.5(12) . . . . ?
C35 C36 C37 C38 -1.1(11) . . . . ?
C36 C37 C38 C33 2.1(11) . . . . ?
C38 C33 C34 C35 1.9(10) . . . . ?
C39 P3 O4 Nd1 114.5(4) . . . . ?
C39 P3 C29 P4 -73.6(4) . . . . ?
C39 P3 C29 C30 154.9(4) . . . . ?
C39 P3 C33 C34 105.7(5) . . . . ?
C39 P3 C33 C38 -69.5(6) . . . . ?
C39 C40 C41 C42 -2.8(12) . . . . ?
C40 C39 C44 C43 -0.5(11) . . . . ?
C40 C41 C42 C43 0.0(12) . . . . ?
C41 C42 C43 C44 2.6(12) . . . . ?
C42 C43 C44 C39 -2.3(12) . . . . ?
C44 C39 C40 C41 3.0(11) . . . . ?
C45 P4 O5 Nd1 108.9(4) . . . . ?
C45 P4 C29 P3 -161.7(3) . . . . ?
C45 P4 C29 C30 -30.6(5) . . . . ?
C45 P4 C51 C52 80.9(5) . . . . ?
C45 P4 C51 C56 -94.2(6) . . . . ?
C45 C46 C47 C48 1.5(14) . . . . ?
C46 C45 C50 C49 0.3(11) . . . . ?
C46 C47 C48 C49 0.1(14) . . . . ?
C47 C48 C49 C50 -1.6(13) . . . . ?
C48 C49 C50 C45 1.4(11) . . . . ?
C50 C45 C46 C47 -1.7(12) . . . . ?
C51 P4 O5 Nd1 -134.8(4) . . . . ?
C51 P4 C29 P3 83.6(4) . . . . ?
C51 P4 C29 C30 -145.3(5) . . . . ?
C51 P4 C45 C46 -128.4(6) . . . . ?
C51 P4 C45 C50 46.8(6) . . . . ?
C51 C52 C53 C54 0.5(12) . . . . ?
C52 C51 C56 C55 2.0(11) . . . . ?
C52 C53 C54 C55 -0.5(13) . . . . ?
C53 C54 C55 C56 1.2(13) . . . . ?
C54 C55 C56 C51 -2.0(12) . . . . ?
C56 C51 C52 C53 -1.2(10) . . . . ?

#==
