# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2017

####################################################################### 
# 
# 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_szg242
_database_code_depnum_ccdc_archive 'CCDC 1503581'
_audit_update_record             
;
2016-09-09 deposited with the CCDC.
2017-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H30 La2 N2 O20 P2'
_chemical_formula_weight         934.20

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

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.3565(16)
_cell_length_b                   13.069(3)
_cell_length_c                   17.040(4)
_cell_angle_alpha                90.315(3)
_cell_angle_beta                 97.970(3)
_cell_angle_gamma                93.548(3)
_cell_volume                     1399.1(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2918
_cell_measurement_theta_min      3.12
_cell_measurement_theta_max      28.63

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.218
_exptl_crystal_F_000             912
_exptl_transmission_factor_min   0.359
_exptl_transmission_factor_max   0.938
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    3.221
_shelx_estimated_absorpt_T_min   0.359
_shelx_estimated_absorpt_T_max   0.938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7711
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.960
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measured_fraction_theta_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_point_group_measured_fraction_full 0.977
_reflns_number_total             5587
_reflns_number_gt                3789
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0625P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5587
_refine_ls_number_parameters     397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0433
_refine_ls_wR_factor_ref         0.1237
_refine_ls_wR_factor_gt          0.1087
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.21815(5) -0.05822(2) 0.42485(2) 0.01321(12) Uani 1 1 d . . . . .
La2 La 0.22111(5) 0.44060(2) 0.42714(2) 0.01290(12) Uani 1 1 d . . . . .
P1 P -0.2611(3) -0.00573(12) 0.35457(11) 0.0177(4) Uani 1 1 d . . . . .
P2 P 0.6545(3) 0.48592(12) 0.35270(10) 0.0159(4) Uani 1 1 d . . . . .
O1 O -0.1118(7) -0.0736(3) 0.3187(3) 0.0214(10) Uani 1 1 d . . . . .
O2 O -0.1498(6) 0.0231(3) 0.4376(3) 0.0225(10) Uani 1 1 d . . . . .
O3 O -0.4872(7) -0.0474(3) 0.3476(3) 0.0216(10) Uani 1 1 d . . . . .
O4 O -0.7993(11) 0.1351(6) -0.0648(4) 0.0643(19) Uani 1 1 d . . . . .
H4D H -0.7276 0.1911 -0.0714 0.097 Uiso 1 1 d R U . . .
O5 O -1.0355(10) 0.1259(5) 0.0194(4) 0.0554(17) Uani 1 1 d . . . . .
O6 O 0.4545(6) 0.4268(3) 0.3124(3) 0.0197(10) Uani 1 1 d . . . . .
O7 O 0.6164(6) 0.5109(3) 0.4371(3) 0.0192(10) Uani 1 1 d . . . . .
O8 O 0.8616(6) 0.4370(3) 0.3470(3) 0.0192(10) Uani 1 1 d . . . . .
O9 O 0.2213(10) 0.6366(5) -0.0764(3) 0.0555(17) Uani 1 1 d . . . . .
H9E H 0.2915 0.5836 -0.0807 0.083 Uiso 1 1 d R U . . .
O10 O -0.0201(10) 0.6310(5) 0.0068(4) 0.0540(17) Uani 1 1 d . . . . .
O11 O 0.0444(6) -0.3958(3) 0.4753(3) 0.0182(9) Uani 1 1 d . . . . .
O12 O 0.2268(7) -0.3937(3) 0.3430(3) 0.0222(10) Uani 1 1 d . . . . .
O13 O 0.0652(7) -0.2248(3) 0.4787(3) 0.0259(11) Uani 1 1 d . . . . .
O14 O 0.2334(7) -0.2244(3) 0.3430(3) 0.0266(11) Uani 1 1 d . . . . .
O15 O 0.2020(7) 0.1065(3) 0.3421(3) 0.0208(10) Uani 1 1 d . . . . .
O16 O 0.4505(7) 0.1135(3) 0.4833(3) 0.0215(10) Uani 1 1 d . . . . .
O17 O 0.1452(7) 0.2716(3) 0.3547(3) 0.0233(11) Uani 1 1 d . . . . .
O18 O 0.4245(7) 0.2839(3) 0.4892(3) 0.0262(11) Uani 1 1 d . . . . .
O1W O 0.9619(10) 0.5933(5) 0.7916(4) 0.063(2) Uani 1 1 d . . . . .
H1WA H 1.0892 0.5805 0.8105 0.094 Uiso 1 1 d R U . . .
H1WB H 0.9644 0.6469 0.7634 0.094 Uiso 1 1 d R U . . .
O2W O 0.0645(12) 0.8837(6) 0.1984(4) 0.085(3) Uani 1 1 d . . . . .
H2WC H 0.0769 0.8702 0.1504 0.102 Uiso 1 1 d R U . . .
H2WA H -0.0599 0.9038 0.2013 0.128 Uiso 1 1 d R U . . .
N1 N -0.4645(8) 0.1113(4) 0.2340(3) 0.0196(12) Uani 1 1 d . . . . .
H1C H -0.5826 0.0860 0.2531 0.024 Uiso 1 1 d R U . . .
N2 N 0.5156(8) 0.6130(4) 0.2286(3) 0.0217(12) Uani 1 1 d . . . . .
H2C H 0.3870 0.5934 0.2425 0.026 Uiso 1 1 d R U . . .
C1 C -0.2800(10) 0.1163(5) 0.3010(4) 0.0232(15) Uani 1 1 d . . . . .
H1A H -0.2986 0.1713 0.3377 0.028 Uiso 1 1 d R U . . .
H1B H -0.1477 0.1323 0.2795 0.028 Uiso 1 1 d R U . . .
C2 C -0.5069(12) 0.2171(5) 0.2031(4) 0.0297(17) Uani 1 1 d . . . . .
H2A H -0.3800 0.2460 0.1831 0.036 Uiso 1 1 d R U . . .
H2B H -0.5347 0.2609 0.2464 0.036 Uiso 1 1 d R U . . .
C3 C -0.4271(13) 0.0414(6) 0.1684(5) 0.0359(19) Uani 1 1 d . . . . .
H3A H -0.4046 -0.0272 0.1888 0.043 Uiso 1 1 d R U . . .
H3B H -0.2983 0.0667 0.1479 0.043 Uiso 1 1 d R U . . .
C4 C -0.6953(12) 0.2137(6) 0.1386(5) 0.038(2) Uani 1 1 d . . . . .
H4A H -0.7168 0.2828 0.1189 0.046 Uiso 1 1 d R U . . .
H4B H -0.8238 0.1888 0.1595 0.046 Uiso 1 1 d R U . . .
C5 C -0.6158(14) 0.0371(6) 0.1039(5) 0.043(2) Uani 1 1 d . . . . .
H5A H -0.7422 0.0074 0.1238 0.052 Uiso 1 1 d R U . . .
H5B H -0.5854 -0.0071 0.0613 0.052 Uiso 1 1 d R U . . .
C6 C -0.6620(13) 0.1438(6) 0.0708(5) 0.0367(19) Uani 1 1 d . . . . .
H6 H -0.5371 0.1718 0.0478 0.044 Uiso 1 1 d R U . . .
C7 C -0.8543(14) 0.1343(6) 0.0075(5) 0.038(2) Uani 1 1 d . . . . .
C8 C 0.6773(10) 0.6098(5) 0.3016(4) 0.0213(14) Uani 1 1 d . . . . .
H8A H 0.6586 0.6657 0.3375 0.026 Uiso 1 1 d R U . . .
H8B H 0.8194 0.6197 0.2863 0.026 Uiso 1 1 d R U . . .
C9 C 0.5010(12) 0.7203(5) 0.1945(5) 0.0312(17) Uani 1 1 d . . . . .
H9A H 0.6359 0.7425 0.1770 0.037 Uiso 1 1 d R U . . .
H9B H 0.4737 0.7681 0.2354 0.037 Uiso 1 1 d R U . . .
C10 C 0.5603(12) 0.5401(6) 0.1652(4) 0.0308(17) Uani 1 1 d . . . . .
H10A H 0.5744 0.4716 0.1868 0.037 Uiso 1 1 d R U . . .
H10B H 0.6938 0.5620 0.1465 0.037 Uiso 1 1 d R U . . .
C11 C 0.3216(13) 0.7189(6) 0.1263(5) 0.0377(19) Uani 1 1 d . . . . .
H11A H 0.3141 0.7877 0.1046 0.045 Uiso 1 1 d R U . . .
H11B H 0.1863 0.7005 0.1450 0.045 Uiso 1 1 d R U . . .
C12 C 0.3762(13) 0.5379(6) 0.0963(5) 0.0390(19) Uani 1 1 d . . . . .
H12A H 0.4037 0.4892 0.0561 0.047 Uiso 1 1 d R U . . .
H12B H 0.2434 0.5149 0.1151 0.047 Uiso 1 1 d R U . . .
C13 C 0.3509(13) 0.6442(6) 0.0612(5) 0.0373(19) Uani 1 1 d . . . . .
H13 H 0.4811 0.6657 0.0388 0.045 Uiso 1 1 d R U . . .
C14 C 0.1620(14) 0.6364(7) -0.0041(5) 0.042(2) Uani 1 1 d . . . . .
C15 C 0.0948(9) -0.3086(5) 0.4485(4) 0.0170(13) Uani 1 1 d . . . . .
C16 C 0.1967(9) -0.3088(5) 0.3726(4) 0.0169(14) Uani 1 1 d . . . . .
C17 C 0.2256(9) 0.1916(4) 0.3783(4) 0.0173(14) Uani 1 1 d . . . . .
C18 C 0.3801(9) 0.1982(4) 0.4576(4) 0.0167(13) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La1 O3 2.432(4) 1_655 ?
La1 O2 2.487(4) 2_556 ?
La1 O13 2.556(4) . ?
La1 O15 2.579(4) . ?
La1 O1 2.570(5) . ?
La1 O14 2.588(4) . ?
La1 O16 2.587(4) 2_656 ?
La1 O2 2.663(4) . ?
La1 O16 2.714(4) . ?
La2 O7 2.462(4) 2_666 ?
La2 O8 2.492(4) 1_455 ?
La2 O17 2.512(4) . ?
La2 O11 2.573(4) 2_556 ?
La2 O12 2.605(4) 1_565 ?
La2 O7 2.604(4) . ?
La2 O6 2.625(4) . ?
La2 O18 2.637(4) . ?
La2 O11 2.654(4) 1_565 ?
La2 La2 4.2405(10) 2_666 ?
P1 O3 1.494(4) . ?
P1 O2 1.526(5) . ?
P1 O1 1.523(4) . ?
P1 C1 1.844(7) . ?
P2 O8 1.513(4) . ?
P2 O7 1.529(5) . ?
P2 O6 1.522(4) . ?
P2 C8 1.850(7) . ?
O2 La1 2.487(4) 2_556 ?
O3 La1 2.432(4) 1_455 ?
O4 C7 1.327(10) . ?
O4 H4D 0.8544 . ?
O5 C7 1.195(10) . ?
O7 La2 2.461(4) 2_666 ?
O8 La2 2.492(4) 1_655 ?
O9 C14 1.336(10) . ?
O9 H9E 0.8553 . ?
O10 C14 1.196(10) . ?
O11 C15 1.269(7) . ?
O11 La2 2.573(4) 2_556 ?
O11 La2 2.654(4) 1_545 ?
O12 C16 1.252(7) . ?
O12 La2 2.605(4) 1_545 ?
O13 C15 1.243(7) . ?
O14 C16 1.238(7) . ?
O15 C17 1.260(7) . ?
O16 C18 1.277(7) . ?
O16 La1 2.587(4) 2_656 ?
O17 C17 1.236(7) . ?
O18 C18 1.239(7) . ?
O1W H1WA 0.8553 . ?
O1W H1WB 0.8531 . ?
O2W H2WC 0.8511 . ?
O2W H2WA 0.8556 . ?
N1 C3 1.493(8) . ?
N1 C2 1.509(8) . ?
N1 C1 1.517(8) . ?
N1 H1C 0.9042 . ?
N2 C8 1.502(8) . ?
N2 C9 1.524(9) . ?
N2 C10 1.505(8) . ?
N2 H2C 0.9045 . ?
C1 H1A 0.9741 . ?
C1 H1B 0.9745 . ?
C2 C4 1.508(10) . ?
C2 H2A 0.9742 . ?
C2 H2B 0.9733 . ?
C3 C5 1.509(11) . ?
C3 H3A 0.9748 . ?
C3 H3B 0.9744 . ?
C4 C6 1.515(11) . ?
C4 H4A 0.9747 . ?
C4 H4B 0.9744 . ?
C5 C6 1.536(11) . ?
C5 H5A 0.9744 . ?
C5 H5B 0.9734 . ?
C6 C7 1.512(11) . ?
C6 H6 0.9841 . ?
C8 H8A 0.9744 . ?
C8 H8B 0.9752 . ?
C9 C11 1.510(11) . ?
C9 H9A 0.9747 . ?
C9 H9B 0.9738 . ?
C10 C12 1.536(10) . ?
C10 H10A 0.9744 . ?
C10 H10B 0.9747 . ?
C11 C13 1.512(10) . ?
C11 H11A 0.9744 . ?
C11 H11B 0.9748 . ?
C12 C13 1.524(11) . ?
C12 H12A 0.9739 . ?
C12 H12B 0.9746 . ?
C13 C14 1.518(11) . ?
C13 H13 0.9843 . ?
C15 C16 1.525(9) . ?
C17 C18 1.555(9) . ?

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
O3 La1 O2 139.08(14) 1_655 2_556 ?
O3 La1 O13 124.35(14) 1_655 . ?
O2 La1 O13 72.26(14) 2_556 . ?
O3 La1 O15 70.59(14) 1_655 . ?
O2 La1 O15 110.87(14) 2_556 . ?
O13 La1 O15 154.87(14) . . ?
O3 La1 O1 103.36(14) 1_655 . ?
O2 La1 O1 115.85(13) 2_556 . ?
O13 La1 O1 85.42(14) . . ?
O15 La1 O1 70.65(13) . . ?
O3 La1 O14 68.31(14) 1_655 . ?
O2 La1 O14 133.76(15) 2_556 . ?
O13 La1 O14 62.73(14) . . ?
O15 La1 O14 114.29(15) . . ?
O1 La1 O14 71.86(14) . . ?
O3 La1 O16 73.19(15) 1_655 2_656 ?
O2 La1 O16 74.18(14) 2_556 2_656 ?
O13 La1 O16 79.86(14) . 2_656 ?
O15 La1 O16 125.26(13) . 2_656 ?
O1 La1 O16 158.67(13) . 2_656 ?
O14 La1 O16 87.62(14) . 2_656 ?
O3 La1 O2 141.88(15) 1_655 . ?
O2 La1 O2 64.33(17) 2_556 . ?
O13 La1 O2 88.03(14) . . ?
O15 La1 O2 72.29(14) . . ?
O1 La1 O2 55.33(13) . . ?
O14 La1 O2 121.50(13) . . ?
O16 La1 O2 138.51(14) 2_656 . ?
O3 La1 O16 76.66(14) 1_655 . ?
O2 La1 O16 70.15(14) 2_556 . ?
O13 La1 O16 137.64(15) . . ?
O15 La1 O16 60.95(14) . . ?
O1 La1 O16 128.66(13) . . ?
O14 La1 O16 143.32(13) . . ?
O16 La1 O16 71.78(14) 2_656 . ?
O2 La1 O16 92.81(12) . . ?
O7 La2 O8 137.51(13) 2_666 1_455 ?
O7 La2 O17 133.14(14) 2_666 . ?
O8 La2 O17 70.61(14) 1_455 . ?
O7 La2 O11 70.25(13) 2_666 2_556 ?
O8 La2 O11 74.37(14) 1_455 2_556 ?
O17 La2 O11 93.12(14) . 2_556 ?
O7 La2 O12 107.00(14) 2_666 1_565 ?
O8 La2 O12 75.28(14) 1_455 1_565 ?
O17 La2 O12 117.85(15) . 1_565 ?
O11 La2 O12 125.09(13) 2_556 1_565 ?
O7 La2 O7 66.35(16) 2_666 . ?
O8 La2 O7 145.41(14) 1_455 . ?
O17 La2 O7 113.74(13) . . ?
O11 La2 O7 136.44(14) 2_556 . ?
O12 La2 O7 72.82(14) 1_565 . ?
O7 La2 O6 121.10(13) 2_666 . ?
O8 La2 O6 99.44(14) 1_455 . ?
O17 La2 O6 68.74(14) . . ?
O11 La2 O6 161.83(13) 2_556 . ?
O12 La2 O6 67.72(13) 1_565 . ?
O7 La2 O6 55.93(13) . . ?
O7 La2 O18 71.86(14) 2_666 . ?
O8 La2 O18 127.75(13) 1_455 . ?
O17 La2 O18 63.05(14) . . ?
O11 La2 O18 85.09(14) 2_556 . ?
O12 La2 O18 148.38(14) 1_565 . ?
O7 La2 O18 78.34(13) . . ?
O6 La2 O18 85.57(14) . . ?
O7 La2 O11 70.21(13) 2_666 1_565 ?
O8 La2 O11 75.01(13) 1_455 1_565 ?
O17 La2 O11 144.06(13) . 1_565 ?
O11 La2 O11 67.40(14) 2_556 1_565 ?
O12 La2 O11 61.09(13) 1_565 1_565 ?
O7 La2 O11 100.43(12) . 1_565 ?
O6 La2 O11 128.28(13) . 1_565 ?
O18 La2 O11 138.77(14) . 1_565 ?
O7 La2 La2 34.23(9) 2_666 2_666 ?
O8 La2 La2 159.00(9) 1_455 2_666 ?
O17 La2 La2 130.10(10) . 2_666 ?
O11 La2 La2 104.41(10) 2_556 2_666 ?
O12 La2 La2 89.33(10) 1_565 2_666 ?
O7 La2 La2 32.12(10) . 2_666 ?
O6 La2 La2 87.47(9) . 2_666 ?
O18 La2 La2 72.26(9) . 2_666 ?
O11 La2 La2 85.11(9) 1_565 2_666 ?
O3 P1 O2 117.0(3) . . ?
O3 P1 O1 115.1(2) . . ?
O2 P1 O1 105.7(2) . . ?
O3 P1 C1 103.3(3) . . ?
O2 P1 C1 105.3(3) . . ?
O1 P1 C1 110.0(3) . . ?
O8 P2 O7 114.7(3) . . ?
O8 P2 O6 115.6(2) . . ?
O7 P2 O6 107.0(2) . . ?
O8 P2 C8 105.0(3) . . ?
O7 P2 C8 106.6(3) . . ?
O6 P2 C8 107.4(3) . . ?
P1 O1 La1 101.2(2) . . ?
P1 O2 La1 142.7(2) . 2_556 ?
P1 O2 La1 97.2(2) . . ?
La1 O2 La1 115.67(17) 2_556 . ?
P1 O3 La1 139.7(3) . 1_455 ?
C7 O4 H4D 109.4 . . ?
P2 O6 La2 98.1(2) . . ?
P2 O7 La2 146.4(2) . 2_666 ?
P2 O7 La2 98.74(19) . . ?
La2 O7 La2 113.65(16) 2_666 . ?
P2 O8 La2 136.1(3) . 1_655 ?
C14 O9 H9E 107.8 . . ?
C15 O11 La2 128.4(4) . 2_556 ?
C15 O11 La2 119.0(4) . 1_545 ?
La2 O11 La2 112.59(14) 2_556 1_545 ?
C16 O12 La2 120.6(4) . 1_545 ?
C15 O13 La1 120.1(4) . . ?
C16 O14 La1 119.8(4) . . ?
C17 O15 La1 118.2(4) . . ?
C18 O16 La1 136.1(4) . 2_656 ?
C18 O16 La1 115.6(4) . . ?
La1 O16 La1 108.22(14) 2_656 . ?
C17 O17 La2 123.6(4) . . ?
C18 O18 La2 118.3(4) . . ?
H1WA O1W H1WB 109.4 . . ?
H2WC O2W H2WA 109.8 . . ?
C3 N1 C2 110.7(5) . . ?
C3 N1 C1 111.8(5) . . ?
C2 N1 C1 110.6(5) . . ?
C3 N1 H1C 107.5 . . ?
C2 N1 H1C 107.6 . . ?
C1 N1 H1C 108.5 . . ?
C8 N2 C9 112.5(5) . . ?
C8 N2 C10 111.8(5) . . ?
C9 N2 C10 109.1(5) . . ?
C8 N2 H2C 107.6 . . ?
C9 N2 H2C 107.6 . . ?
C10 N2 H2C 108.0 . . ?
N1 C1 P1 111.8(4) . . ?
N1 C1 H1A 109.1 . . ?
P1 C1 H1A 109.6 . . ?
N1 C1 H1B 109.3 . . ?
P1 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
N1 C2 C4 111.2(6) . . ?
N1 C2 H2A 108.7 . . ?
C4 C2 H2A 110.3 . . ?
N1 C2 H2B 109.4 . . ?
C4 C2 H2B 109.2 . . ?
H2A C2 H2B 108.0 . . ?
N1 C3 C5 110.0(6) . . ?
N1 C3 H3A 109.8 . . ?
C5 C3 H3A 109.7 . . ?
N1 C3 H3B 108.6 . . ?
C5 C3 H3B 110.7 . . ?
H3A C3 H3B 108.0 . . ?
C2 C4 C6 111.1(6) . . ?
C2 C4 H4A 109.4 . . ?
C6 C4 H4A 109.6 . . ?
C2 C4 H4B 110.2 . . ?
C6 C4 H4B 108.6 . . ?
H4A C4 H4B 107.9 . . ?
C3 C5 C6 112.0(6) . . ?
C3 C5 H5A 110.4 . . ?
C6 C5 H5A 109.0 . . ?
C3 C5 H5B 108.3 . . ?
C6 C5 H5B 109.2 . . ?
H5A C5 H5B 107.9 . . ?
C7 C6 C4 112.1(6) . . ?
C7 C6 C5 109.2(6) . . ?
C4 C6 C5 108.6(7) . . ?
C7 C6 H6 109.9 . . ?
C4 C6 H6 108.2 . . ?
C5 C6 H6 108.8 . . ?
O5 C7 O4 122.7(8) . . ?
O5 C7 C6 125.5(8) . . ?
O4 C7 C6 111.8(7) . . ?
N2 C8 P2 111.5(4) . . ?
N2 C8 H8A 109.6 . . ?
P2 C8 H8A 109.7 . . ?
N2 C8 H8B 108.9 . . ?
P2 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
N2 C9 C11 109.2(6) . . ?
N2 C9 H9A 109.5 . . ?
C11 C9 H9A 110.8 . . ?
N2 C9 H9B 109.6 . . ?
C11 C9 H9B 109.6 . . ?
H9A C9 H9B 108.2 . . ?
N2 C10 C12 109.1(5) . . ?
N2 C10 H10A 109.8 . . ?
C12 C10 H10A 109.8 . . ?
N2 C10 H10B 109.8 . . ?
C12 C10 H10B 110.2 . . ?
H10A C10 H10B 108.0 . . ?
C9 C11 C13 112.5(6) . . ?
C9 C11 H11A 108.6 . . ?
C13 C11 H11A 109.2 . . ?
C9 C11 H11B 110.1 . . ?
C13 C11 H11B 108.5 . . ?
H11A C11 H11B 107.8 . . ?
C10 C12 C13 110.9(6) . . ?
C10 C12 H12A 108.9 . . ?
C13 C12 H12A 110.6 . . ?
C10 C12 H12B 110.0 . . ?
C13 C12 H12B 108.4 . . ?
H12A C12 H12B 107.9 . . ?
C14 C13 C12 107.7(7) . . ?
C14 C13 C11 112.4(7) . . ?
C12 C13 C11 109.1(7) . . ?
C14 C13 H13 109.8 . . ?
C12 C13 H13 108.7 . . ?
C11 C13 H13 109.1 . . ?
O10 C14 O9 123.1(8) . . ?
O10 C14 C13 124.5(8) . . ?
O9 C14 C13 112.4(7) . . ?
O13 C15 O11 125.2(6) . . ?
O13 C15 C16 118.6(6) . . ?
O11 C15 C16 116.2(5) . . ?
O14 C16 O12 125.2(6) . . ?
O14 C16 C15 116.7(5) . . ?
O12 C16 C15 118.0(6) . . ?
O17 C17 O15 126.0(6) . . ?
O17 C17 C18 117.0(5) . . ?
O15 C17 C18 116.9(5) . . ?
O18 C18 O16 126.4(6) . . ?
O18 C18 C17 117.7(5) . . ?
O16 C18 C17 115.9(5) . . ?

_refine_diff_density_max         1.784
_refine_diff_density_min         -1.947
_refine_diff_density_rms         0.200

####################################################################### 
# 
# 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_szg245
_database_code_depnum_ccdc_archive 'CCDC 1503584'
_audit_update_record             
;
2016-09-09 deposited with the CCDC.
2017-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H26 Eu2 N O23 P'
_chemical_formula_weight         899.24

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'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   11.5659(4)
_cell_length_b                   14.4845(5)
_cell_length_c                   15.8549(5)
_cell_angle_alpha                90
_cell_angle_beta                 109.4150(10)
_cell_angle_gamma                90
_cell_volume                     2505.07(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    6980
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      30.55

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.384
_exptl_crystal_F_000             1744
_exptl_transmission_factor_min   0.748
_exptl_transmission_factor_max   0.821
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    5.132
_shelx_estimated_absorpt_T_min   0.748
_shelx_estimated_absorpt_T_max   0.821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13865
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.910
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             5149
_reflns_number_gt                4494
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0243P)²+2.9737P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5149
_refine_ls_number_parameters     379
_refine_ls_number_restraints     319
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0217
_refine_ls_wR_factor_ref         0.0525
_refine_ls_wR_factor_gt          0.0499
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.054
_refine_ls_shift/su_mean         0.003

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
Eu1 Eu 0.47774(2) 0.08744(2) 0.17027(2) 0.01582(5) Uani 1 1 d . . . . .
Eu2 Eu 0.45389(2) 0.52977(2) 0.17669(2) 0.01621(5) Uani 1 1 d . . . . .
P1 P 0.34655(8) 0.20169(6) -0.05239(6) 0.01814(19) Uani 1 1 d . . . . .
O1 O 0.3638(2) 0.30416(17) -0.01813(17) 0.0231(6) Uani 1 1 d . U . . .
H1C H 0.4399 0.3161 0.0038 0.035 Uiso 1 1 d R U . . .
O2 O 0.3905(2) 0.14024(19) 0.02681(18) 0.0278(6) Uani 1 1 d . U . . .
O3 O 0.3991(3) 0.18829(19) -0.12542(19) 0.0277(6) Uani 1 1 d . U . . .
O4 O 0.4126(3) -0.0431(2) 0.0633(2) 0.0306(7) Uani 1 1 d . U . . .
H4D H 0.4270 -0.0938 0.0920 0.046 Uiso 1 1 d R U . . .
O5 O 0.6627(2) 0.04733(18) 0.13584(17) 0.0217(5) Uani 1 1 d . U . . .
O6 O 0.6639(2) 0.11193(19) 0.29674(18) 0.0241(6) Uani 1 1 d . U . . .
O7 O 0.8646(2) 0.02395(18) 0.19347(17) 0.0232(6) Uani 1 1 d . U . . .
O8 O 0.8648(2) 0.08686(18) 0.35155(17) 0.0216(5) Uani 1 1 d . U . . .
O9 O 0.5456(3) -0.0688(2) 0.2384(2) 0.0370(7) Uani 1 1 d . U . . .
H9A H 0.6003 -0.0900 0.2187 0.055 Uiso 1 1 d R U . . .
H9B H 0.5750 -0.0635 0.2949 0.055 Uiso 1 1 d R U . . .
O10 O 0.4203(2) 0.0615(2) 0.30489(18) 0.0269(6) Uani 1 1 d . U . . .
O11 O 0.2561(2) 0.0694(2) 0.13807(17) 0.0245(6) Uani 1 1 d . U . . .
O12 O 0.1045(2) 0.0580(2) 0.19503(18) 0.0259(6) Uani 1 1 d . U . . .
O13 O 0.2662(2) 0.0541(2) 0.36026(18) 0.0261(6) Uani 1 1 d . U . . .
O14 O 0.3945(3) 0.23093(19) 0.2102(2) 0.0323(6) Uani 1 1 d . U . . .
O15 O 0.5832(2) 0.24258(18) 0.15006(19) 0.0259(6) Uani 1 1 d . U . . .
O16 O 0.3735(3) 0.38362(19) 0.2014(2) 0.0294(6) Uani 1 1 d . U . . .
O17 O 0.5603(2) 0.39662(18) 0.14034(19) 0.0265(6) Uani 1 1 d . U . . .
O18 O 0.4443(3) 0.6934(2) 0.1721(3) 0.0478(9) Uani 1 1 d . U . . .
H18B H 0.3758 0.7105 0.1352 0.072 Uiso 1 1 d R U . . .
H18C H 0.4513 0.7135 0.2239 0.072 Uiso 1 1 d R U . . .
O19 O 0.3784(3) 0.5409(2) 0.0164(2) 0.0368(7) Uani 1 1 d . U . . .
H19A H 0.3805 0.5969 0.0011 0.055 Uiso 1 1 d R U . . .
O20 O -0.2784(4) 0.2266(3) 0.0463(3) 0.0646(11) Uani 1 1 d . U . . .
H20A H -0.3144 0.2347 0.0845 0.097 Uiso 1 1 d R U . A .
C7 C -0.1727(5) 0.2548(5) 0.0767(4) 0.0585(17) Uani 0.288(9) 1 d D . P A 1
O21 O -0.1759(10) 0.3473(9) 0.1006(9) 0.053(4) Uani 0.288(9) 1 d D U P A 1
C7' C -0.1727(5) 0.2548(5) 0.0767(4) 0.0585(17) Uani 0.712(9) 1 d D . P A 2
O21' O -0.1281(6) 0.2605(6) 0.1613(4) 0.084(3) Uani 0.712(9) 1 d D U P A 2
O1W O 0.3022(4) 0.8286(3) 0.2098(3) 0.0697(12) Uani 1 1 d . U . . .
H1WC H 0.3295 0.8459 0.2641 0.084 Uiso 1 1 d R U . . .
H1WA H 0.3381 0.8586 0.1795 0.105 Uiso 1 1 d R U . . .
O2W O 0.1340(5) 0.5151(5) 0.9481(4) 0.126(2) Uani 1 1 d . . . . .
H2WA H 0.1322 0.5700 0.9665 0.188 Uiso 1 1 d R U . . .
H2WB H 0.0637 0.4906 0.9366 0.188 Uiso 1 1 d R U . . .
N1 N 0.1184(3) 0.1816(2) -0.0297(2) 0.0214(7) Uani 1 1 d . . . . .
H1D H 0.1624 0.1476 0.0176 0.026 Uiso 1 1 d R U . . .
C1 C 0.1825(3) 0.1803(3) -0.0983(3) 0.0237(8) Uani 1 1 d . . . . .
H1A H 0.1455 0.2268 -0.1431 0.028 Uiso 1 1 d R U . . .
H1B H 0.1692 0.1207 -0.1279 0.028 Uiso 1 1 d R U . . .
C2 C -0.0069(4) 0.1382(3) -0.0689(3) 0.0291(9) Uani 1 1 d . . . . .
H2A H 0.0025 0.0738 -0.0821 0.035 Uiso 1 1 d R U . . .
H2B H -0.0504 0.1690 -0.1247 0.035 Uiso 1 1 d R U . . .
C3 C 0.1093(4) 0.2781(3) 0.0020(3) 0.0370(11) Uani 1 1 d . . . . .
H3A H 0.0711 0.3172 -0.0495 0.044 Uiso 1 1 d R U . . .
H3B H 0.1908 0.3021 0.0326 0.044 Uiso 1 1 d R U . . .
C4 C 0.0348(4) 0.2817(3) 0.0645(3) 0.0400(11) Uani 1 1 d . . . . .
H4A H 0.0297 0.3450 0.0828 0.048 Uiso 1 1 d R U . . .
H4B H 0.0748 0.2454 0.1176 0.048 Uiso 1 1 d R U . . .
C5 C -0.0826(4) 0.1440(3) -0.0070(3) 0.0306(9) Uani 1 1 d . . . . .
H5A H -0.1636 0.1185 -0.0364 0.037 Uiso 1 1 d R U . . .
H5B H -0.0436 0.1083 0.0468 0.037 Uiso 1 1 d R U . . .
C6 C -0.0940(4) 0.2441(3) 0.0178(3) 0.0329(10) Uani 1 1 d . . . . .
H6 H -0.1321 0.2794 -0.0372 0.039 Uiso 1 1 d R U . A .
C8 C 0.5332(3) 0.3162(2) 0.1573(2) 0.0190(7) Uani 1 1 d . . . . .
C9 C 0.4240(4) 0.3091(3) 0.1925(3) 0.0228(8) Uani 1 1 d . . . . .
C10 C 0.7629(3) 0.0491(2) 0.1980(2) 0.0178(7) Uani 1 1 d . . . . .
C11 C 0.7623(3) 0.0857(2) 0.2895(2) 0.0178(7) Uani 1 1 d . . . . .
C12 C 0.2153(3) 0.0629(3) 0.2018(2) 0.0192(7) Uani 1 1 d . . . . .
C13 C 0.3094(3) 0.0596(3) 0.2978(2) 0.0184(7) Uani 1 1 d . . . . .
H4C H 0.389(5) -0.038(4) 0.014(4) 0.06(2) Uiso 1 1 d . . . . .
H19C H 0.372(11) 0.536(8) -0.041(8) 0.20(5) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O2 2.291(3) . ?
Eu1 O6 2.431(3) . ?
Eu1 O5 2.447(2) . ?
Eu1 O11 2.455(2) . ?
Eu1 O14 2.460(3) . ?
Eu1 O10 2.466(3) . ?
Eu1 O4 2.484(3) . ?
Eu1 O9 2.518(3) . ?
Eu1 O15 2.626(3) . ?
Eu1 C11 3.205(4) . ?
Eu1 C10 3.227(3) . ?
Eu1 C12 3.256(4) . ?
Eu2 O18 2.373(3) . ?
Eu2 O12 2.382(3) 2 ?
Eu2 O16 2.396(3) . ?
Eu2 O19 2.403(3) . ?
Eu2 O7 2.404(3) 2_655 ?
Eu2 O8 2.431(2) 2_655 ?
Eu2 O13 2.440(3) 2 ?
Eu2 O17 2.457(3) . ?
Eu2 C12 3.206(4) 2 ?
Eu2 C10 3.229(3) 2_655 ?
Eu2 C13 3.232(4) 2 ?
Eu2 C11 3.248(3) 2_655 ?
Eu2 H18B 2.7762 . ?
Eu2 H18C 2.7681 . ?
Eu2 H19A 2.8017 . ?
P1 O2 1.484(3) . ?
P1 O3 1.489(3) . ?
P1 O1 1.570(3) . ?
P1 C1 1.819(4) . ?
O1 H1C 0.8500 . ?
O4 H4D 0.8499 . ?
O4 H4C 0.74(6) . ?
O5 C10 1.248(4) . ?
O6 C11 1.241(4) . ?
O7 C10 1.256(4) . ?
O7 Eu2 2.404(3) 2_645 ?
O8 C11 1.264(4) . ?
O8 Eu2 2.431(2) 2_645 ?
O9 H9A 0.8500 . ?
O9 H9B 0.8500 . ?
O10 C13 1.249(4) . ?
O11 C12 1.253(4) . ?
O12 C12 1.252(4) . ?
O12 Eu2 2.382(3) 2_545 ?
O13 C13 1.252(4) . ?
O13 Eu2 2.440(3) 2_545 ?
O14 C9 1.241(5) . ?
O15 C8 1.236(4) . ?
O16 C9 1.258(5) . ?
O17 C8 1.259(4) . ?
O18 H18B 0.8501 . ?
O18 H18C 0.8500 . ?
O19 H19A 0.8502 . ?
O19 H19C 0.89(12) . ?
O20 C7' 1.225(6) . ?
O20 C7 1.225(6) . ?
O20 H20A 0.8500 . ?
C7 O21 1.397(12) . ?
C7 C6 1.514(6) . ?
C7' O21' 1.270(7) . ?
C7' C6 1.514(6) . ?
O1W H1WC 0.8500 . ?
O1W H1WA 0.8497 . ?
O2W H2WA 0.8500 . ?
O2W H2WB 0.8499 . ?
N1 C3 1.502(5) . ?
N1 C1 1.506(5) . ?
N1 C2 1.510(5) . ?
N1 H1D 0.8999 . ?
C1 H1A 0.9698 . ?
C1 H1B 0.9700 . ?
C2 C5 1.519(5) . ?
C2 H2A 0.9699 . ?
C2 H2B 0.9699 . ?
C3 C4 1.515(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C6 1.527(6) . ?
C4 H4A 0.9704 . ?
C4 H4B 0.9698 . ?
C5 C6 1.519(6) . ?
C5 H5A 0.9703 . ?
C5 H5B 0.9703 . ?
C6 H6 0.9799 . ?
C8 C9 1.544(5) . ?
C10 C11 1.546(5) . ?
C10 Eu2 3.229(3) 2_645 ?
C11 Eu2 3.248(3) 2_645 ?
C12 C13 1.550(5) . ?
C12 Eu2 3.206(4) 2_545 ?
C13 Eu2 3.232(3) 2_545 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Eu1 O6 138.34(9) . . ?
O2 Eu1 O5 89.27(9) . . ?
O6 Eu1 O5 67.57(8) . . ?
O2 Eu1 O11 75.18(9) . . ?
O6 Eu1 O11 139.81(9) . . ?
O5 Eu1 O11 149.08(9) . . ?
O2 Eu1 O14 83.83(10) . . ?
O6 Eu1 O14 88.82(9) . . ?
O5 Eu1 O14 134.74(9) . . ?
O11 Eu1 O14 70.90(9) . . ?
O2 Eu1 O10 138.88(9) . . ?
O6 Eu1 O10 74.22(9) . . ?
O5 Eu1 O10 131.61(9) . . ?
O11 Eu1 O10 66.46(9) . . ?
O14 Eu1 O10 70.43(10) . . ?
O2 Eu1 O4 69.08(10) . . ?
O6 Eu1 O4 131.19(9) . . ?
O5 Eu1 O4 75.89(9) . . ?
O11 Eu1 O4 73.64(10) . . ?
O14 Eu1 O4 139.74(10) . . ?
O10 Eu1 O4 111.53(10) . . ?
O2 Eu1 O9 134.22(10) . . ?
O6 Eu1 O9 73.32(10) . . ?
O5 Eu1 O9 73.22(9) . . ?
O11 Eu1 O9 98.54(10) . . ?
O14 Eu1 O9 137.88(10) . . ?
O10 Eu1 O9 68.10(10) . . ?
O4 Eu1 O9 65.74(10) . . ?
O2 Eu1 O15 70.28(9) . . ?
O6 Eu1 O15 69.89(9) . . ?
O5 Eu1 O15 72.56(8) . . ?
O11 Eu1 O15 124.09(9) . . ?
O14 Eu1 O15 62.98(8) . . ?
O10 Eu1 O15 120.37(9) . . ?
O4 Eu1 O15 128.01(10) . . ?
O9 Eu1 O15 136.89(9) . . ?
O2 Eu1 C11 127.97(9) . . ?
O6 Eu1 C11 20.03(9) . . ?
O5 Eu1 C11 47.71(9) . . ?
O11 Eu1 C11 156.68(9) . . ?
O14 Eu1 C11 105.53(9) . . ?
O10 Eu1 C11 90.45(9) . . ?
O4 Eu1 C11 114.56(9) . . ?
O9 Eu1 C11 68.12(10) . . ?
O15 Eu1 C11 69.58(8) . . ?
O2 Eu1 C10 106.61(9) . . ?
O6 Eu1 C10 47.77(9) . . ?
O5 Eu1 C10 19.96(9) . . ?
O11 Eu1 C10 163.54(9) . . ?
O14 Eu1 C10 125.43(9) . . ?
O10 Eu1 C10 114.39(9) . . ?
O4 Eu1 C10 91.52(10) . . ?
O9 Eu1 C10 68.18(10) . . ?
O15 Eu1 C10 70.66(8) . . ?
C11 Eu1 C10 27.81(9) . . ?
O2 Eu1 C12 93.62(9) . . ?
O6 Eu1 C12 120.30(9) . . ?
O5 Eu1 C12 159.59(9) . . ?
O11 Eu1 C12 19.63(9) . . ?
O14 Eu1 C12 65.67(9) . . ?
O10 Eu1 C12 46.94(9) . . ?
O4 Eu1 C12 86.28(10) . . ?
O9 Eu1 C12 90.56(10) . . ?
O15 Eu1 C12 127.32(8) . . ?
C11 Eu1 C12 137.38(9) . . ?
C10 Eu1 C12 157.39(9) . . ?
O18 Eu2 O12 80.27(11) . 2 ?
O18 Eu2 O16 150.55(10) . . ?
O12 Eu2 O16 77.08(10) 2 . ?
O18 Eu2 O19 84.49(13) . . ?
O12 Eu2 O19 141.77(10) 2 . ?
O16 Eu2 O19 102.00(11) . . ?
O18 Eu2 O7 94.58(12) . 2_655 ?
O12 Eu2 O7 71.91(9) 2 2_655 ?
O16 Eu2 O7 96.01(10) . 2_655 ?
O19 Eu2 O7 144.58(10) . 2_655 ?
O18 Eu2 O8 71.88(10) . 2_655 ?
O12 Eu2 O8 127.29(9) 2 2_655 ?
O16 Eu2 O8 137.40(9) . 2_655 ?
O19 Eu2 O8 79.31(10) . 2_655 ?
O7 Eu2 O8 66.94(8) 2_655 2_655 ?
O18 Eu2 O13 79.27(11) . 2 ?
O12 Eu2 O13 67.12(9) 2 2 ?
O16 Eu2 O13 74.73(9) . 2 ?
O19 Eu2 O13 75.71(10) . 2 ?
O7 Eu2 O13 139.02(9) 2_655 2 ?
O8 Eu2 O13 143.28(9) 2_655 2 ?
O18 Eu2 O17 143.02(9) . . ?
O12 Eu2 O17 129.88(10) 2 . ?
O16 Eu2 O17 66.22(9) . . ?
O19 Eu2 O17 80.70(10) . . ?
O7 Eu2 O17 79.07(9) 2_655 . ?
O8 Eu2 O17 72.16(9) 2_655 . ?
O13 Eu2 O17 128.38(9) 2 . ?
O18 Eu2 C12 80.62(10) . 2 ?
O12 Eu2 C12 19.64(9) 2 2 ?
O16 Eu2 C12 71.74(9) . 2 ?
O19 Eu2 C12 123.10(10) . 2 ?
O7 Eu2 C12 91.40(9) 2_655 2 ?
O8 Eu2 C12 142.77(9) 2_655 2 ?
O13 Eu2 C12 47.65(9) 2 2 ?
O17 Eu2 C12 135.39(9) . 2 ?
O18 Eu2 C10 87.68(11) . 2_655 ?
O12 Eu2 C10 88.70(9) 2 2_655 ?
O16 Eu2 C10 110.21(9) . 2_655 ?
O19 Eu2 C10 125.62(10) . 2_655 ?
O7 Eu2 C10 19.58(9) 2_655 2_655 ?
O8 Eu2 C10 47.37(9) 2_655 2_655 ?
O13 Eu2 C10 154.02(9) 2 2_655 ?
O17 Eu2 C10 74.20(9) . 2_655 ?
C12 Eu2 C10 108.32(9) 2 2_655 ?
O18 Eu2 C13 80.44(10) . 2 ?
O12 Eu2 C13 47.44(9) 2 2 ?
O16 Eu2 C13 70.41(9) . 2 ?
O19 Eu2 C13 95.60(10) . 2 ?
O7 Eu2 C13 119.23(9) 2_655 2 ?
O8 Eu2 C13 152.17(9) 2_655 2 ?
O13 Eu2 C13 19.89(9) 2 2 ?
O17 Eu2 C13 134.48(9) . 2 ?
C12 Eu2 C13 27.85(9) 2 2 ?
C10 Eu2 C13 135.78(9) 2_655 2 ?
O18 Eu2 C11 77.89(10) . 2_655 ?
O12 Eu2 C11 111.96(9) 2 2_655 ?
O16 Eu2 C11 128.25(9) . 2_655 ?
O19 Eu2 C11 98.61(10) . 2_655 ?
O7 Eu2 C11 47.19(9) 2_655 2_655 ?
O8 Eu2 C11 19.76(9) 2_655 2_655 ?
O13 Eu2 C11 156.89(9) 2 2_655 ?
O17 Eu2 C11 71.16(9) . 2_655 ?
C12 Eu2 C11 130.43(9) 2 2_655 ?
C10 Eu2 C11 27.61(9) 2_655 2_655 ?
C13 Eu2 C11 152.70(9) 2 2_655 ?
O18 Eu2 H18B 16.8 . . ?
O12 Eu2 H18B 83.0 2 . ?
O16 Eu2 H18B 139.3 . . ?
O19 Eu2 H18B 73.2 . . ?
O7 Eu2 H18B 111.0 2_655 . ?
O8 Eu2 H18B 82.4 2_655 . ?
O13 Eu2 H18B 64.9 2 . ?
O17 Eu2 H18B 146.4 . . ?
C12 Eu2 H18B 77.6 2 . ?
C10 Eu2 H18B 104.3 2_655 . ?
C13 Eu2 H18B 70.0 2 . ?
C11 Eu2 H18B 92.0 2_655 . ?
O18 Eu2 H18C 16.9 . . ?
O12 Eu2 H18C 64.7 2 . ?
O16 Eu2 H18C 140.0 . . ?
O19 Eu2 H18C 100.9 . . ?
O7 Eu2 H18C 83.5 2_655 . ?
O8 Eu2 H18C 79.1 2_655 . ?
O13 Eu2 H18C 79.7 2 . ?
O17 Eu2 H18C 150.4 . . ?
C12 Eu2 H18C 68.3 2 . ?
C10 Eu2 H18C 81.4 2_655 . ?
C13 Eu2 H18C 75.0 2 . ?
C11 Eu2 H18C 79.4 2_655 . ?
H18B Eu2 H18C 29.0 . . ?
O18 Eu2 H19A 68.1 . . ?
O12 Eu2 H19A 135.3 2 . ?
O16 Eu2 H19A 117.6 . . ?
O19 Eu2 H19A 16.6 . . ?
O7 Eu2 H19A 138.9 2_655 . ?
O8 Eu2 H19A 72.2 2_655 . ?
O13 Eu2 H19A 76.3 2 . ?
O17 Eu2 H19A 92.8 . . ?
C12 Eu2 H19A 120.1 2 . ?
C10 Eu2 H19A 119.4 2_655 . ?
C13 Eu2 H19A 95.2 2 . ?
C11 Eu2 H19A 91.9 2_655 . ?
H18B Eu2 H19A 58.0 . . ?
H18C Eu2 H19A 84.7 . . ?
O2 P1 O3 117.81(16) . . ?
O2 P1 O1 107.80(15) . . ?
O3 P1 O1 110.78(15) . . ?
O2 P1 C1 104.72(17) . . ?
O3 P1 C1 107.95(17) . . ?
O1 P1 C1 107.17(17) . . ?
P1 O1 H1C 109.2 . . ?
P1 O2 Eu1 162.53(18) . . ?
Eu1 O4 H4D 109.3 . . ?
Eu1 O4 H4C 124(5) . . ?
H4D O4 H4C 126.1 . . ?
C10 O5 Eu1 118.1(2) . . ?
C11 O6 Eu1 117.8(2) . . ?
C10 O7 Eu2 120.5(2) . 2_645 ?
C11 O8 Eu2 119.7(2) . 2_645 ?
Eu1 O9 H9A 109.3 . . ?
Eu1 O9 H9B 109.3 . . ?
H9A O9 H9B 109.5 . . ?
C13 O10 Eu1 119.3(2) . . ?
C12 O11 Eu1 119.2(2) . . ?
C12 O12 Eu2 120.6(2) . 2_545 ?
C13 O13 Eu2 118.6(2) . 2_545 ?
C9 O14 Eu1 123.5(2) . . ?
C8 O15 Eu1 118.4(2) . . ?
C9 O16 Eu2 121.3(2) . . ?
C8 O17 Eu2 119.8(2) . . ?
Eu2 O18 H18B 109.6 . . ?
Eu2 O18 H18C 108.9 . . ?
H18B O18 H18C 109.5 . . ?
Eu2 O19 H19A 109.3 . . ?
Eu2 O19 H19C 162(8) . . ?
H19A O19 H19C 77.7 . . ?
C7' O20 H20A 109.5 . . ?
C7 O20 H20A 109.5 . . ?
O20 C7 O21 108.3(6) . . ?
O20 C7 C6 116.7(4) . . ?
O21 C7 C6 109.9(6) . . ?
O20 C7' O21' 116.1(6) . . ?
O20 C7' C6 116.7(4) . . ?
O21' C7' C6 122.8(5) . . ?
H1WC O1W H1WA 109.5 . . ?
H2WA O2W H2WB 109.5 . . ?
C3 N1 C1 111.1(3) . . ?
C3 N1 C2 111.2(3) . . ?
C1 N1 C2 109.5(3) . . ?
C3 N1 H1D 108.2 . . ?
C1 N1 H1D 108.4 . . ?
C2 N1 H1D 108.4 . . ?
N1 C1 P1 114.1(3) . . ?
N1 C1 H1A 108.5 . . ?
P1 C1 H1A 108.8 . . ?
N1 C1 H1B 108.8 . . ?
P1 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
N1 C2 C5 113.0(3) . . ?
N1 C2 H2A 109.2 . . ?
C5 C2 H2A 108.8 . . ?
N1 C2 H2B 108.7 . . ?
C5 C2 H2B 109.2 . . ?
H2A C2 H2B 107.8 . . ?
N1 C3 C4 111.7(4) . . ?
N1 C3 H3A 108.9 . . ?
C4 C3 H3A 109.4 . . ?
N1 C3 H3B 109.6 . . ?
C4 C3 H3B 109.3 . . ?
H3A C3 H3B 107.9 . . ?
C3 C4 C6 110.2(4) . . ?
C3 C4 H4A 109.4 . . ?
C6 C4 H4A 109.7 . . ?
C3 C4 H4B 109.8 . . ?
C6 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
C6 C5 C2 109.8(4) . . ?
C6 C5 H5A 109.5 . . ?
C2 C5 H5A 109.9 . . ?
C6 C5 H5B 109.6 . . ?
C2 C5 H5B 109.8 . . ?
H5A C5 H5B 108.2 . . ?
C7' C6 C5 112.3(4) . . ?
C7 C6 C5 112.3(4) . . ?
C7' C6 C4 110.7(4) . . ?
C7 C6 C4 110.7(4) . . ?
C5 C6 C4 108.1(3) . . ?
C7' C6 H6 108.1 . . ?
C7 C6 H6 108.1 . . ?
C5 C6 H6 108.7 . . ?
C4 C6 H6 108.8 . . ?
O15 C8 O17 128.4(3) . . ?
O15 C8 C9 116.1(3) . . ?
O17 C8 C9 115.5(3) . . ?
O14 C9 O16 125.7(4) . . ?
O14 C9 C8 117.5(3) . . ?
O16 C9 C8 116.7(3) . . ?
O5 C10 O7 126.2(3) . . ?
O5 C10 C11 117.1(3) . . ?
O7 C10 C11 116.7(3) . . ?
O5 C10 Eu2 166.0(3) . 2_645 ?
O7 C10 Eu2 39.88(17) . 2_645 ?
C11 C10 Eu2 76.88(19) . 2_645 ?
O5 C10 Eu1 41.99(17) . . ?
O7 C10 Eu1 167.4(3) . . ?
C11 C10 Eu1 75.28(19) . . ?
Eu2 C10 Eu1 151.71(13) 2_645 . ?
O6 C11 O8 125.1(3) . . ?
O6 C11 C10 118.8(3) . . ?
O8 C11 C10 116.1(3) . . ?
O6 C11 Eu1 42.14(17) . . ?
O8 C11 Eu1 166.5(2) . . ?
C10 C11 Eu1 76.92(19) . . ?
O6 C11 Eu2 165.6(3) . 2_645 ?
O8 C11 Eu2 40.57(16) . 2_645 ?
C10 C11 Eu2 75.51(18) . 2_645 ?
Eu1 C11 Eu2 151.98(12) . 2_645 ?
O12 C12 O11 125.8(4) . . ?
O12 C12 C13 116.6(3) . . ?
O11 C12 C13 117.6(3) . . ?
O12 C12 Eu2 39.74(18) . 2_545 ?
O11 C12 Eu2 164.8(3) . 2_545 ?
C13 C12 Eu2 77.00(19) . 2_545 ?
O12 C12 Eu1 166.7(3) . . ?
O11 C12 Eu1 41.18(17) . . ?
C13 C12 Eu1 76.56(19) . . ?
Eu2 C12 Eu1 153.52(13) 2_545 . ?
O10 C13 O13 126.7(4) . . ?
O10 C13 C12 116.9(3) . . ?
O13 C13 C12 116.4(3) . . ?
O10 C13 Eu2 166.6(3) . 2_545 ?
O13 C13 Eu2 41.53(17) . 2_545 ?
C12 C13 Eu2 75.14(18) . 2_545 ?
O10 C13 Eu1 41.23(18) . . ?
O13 C13 Eu1 167.2(3) . . ?
C12 C13 Eu1 75.94(19) . . ?
Eu2 C13 Eu1 151.04(12) 2_545 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1C O15 0.85 2.59 3.138(4) 123.3 .
O1 H1C O17 0.85 2.45 3.078(4) 131.8 .
O4 H4D O3 0.85 2.34 2.951(4) 128.7 3_655
O4 H4D O9 0.85 2.30 2.715(5) 110.4 .
O9 H9A O3 0.85 2.06 2.716(4) 134.0 3_655
O9 H9B O2W 0.85 2.40 3.232(7) 166.8 4_665
O20 H20A O15 0.85 1.82 2.660(4) 169.0 1_455
O1W H1WA O9 0.85 2.50 3.080(5) 126.3 1_565
O2W H2WB O10 0.85 2.32 2.961(6) 132.6 4_566
N1 H1D O2 0.90 2.59 3.031(4) 110.7 .
N1 H1D O11 0.90 2.18 3.072(4) 174.4 .
C1 H1A O6 0.97 2.56 3.412(5) 146.8 4_565
C1 H1B O7 0.97 2.31 3.283(5) 177.6 3_655
C2 H2A O12 0.97 2.63 3.442(5) 141.7 3
C3 H3B O1 0.97 2.39 3.087(5) 128.2 .
C5 H5B O12 0.97 2.51 3.447(5) 161.7 .
O4 H4C O5 0.74(6) 2.25(6) 2.984(4) 169(6) 3_655
O19 H19C O8 0.89(12) 2.44(12) 3.162(4) 138(10) 4_565
O19 H19C O17 0.89(12) 2.20(12) 2.944(4) 140(10) 3_665

_refine_diff_density_max         1.607
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.111

####################################################################### 
# 
# 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_szg243
_database_code_depnum_ccdc_archive 'CCDC 1503582'
_audit_update_record             
;
2016-09-09 deposited with the CCDC.
2017-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H30 Ce2 N2 O20 P2'
_chemical_formula_weight         936.62

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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.3158(7)
_cell_length_b                   12.9942(13)
_cell_length_c                   17.0265(18)
_cell_angle_alpha                90.4050(10)
_cell_angle_beta                 98.0440(10)
_cell_angle_gamma                93.4940(10)
_cell_volume                     1380.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2685
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      28.57

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.253
_exptl_crystal_F_000             916
_exptl_transmission_factor_min   0.681
_exptl_transmission_factor_max   0.903
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    3.467
_shelx_estimated_absorpt_T_min   0.681
_shelx_estimated_absorpt_T_max   0.903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7796
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.966
_diffrn_reflns_theta_max         26.494
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             5539
_reflns_number_gt                3870
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0605P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5539
_refine_ls_number_parameters     397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0354
_refine_ls_wR_factor_ref         0.1075
_refine_ls_wR_factor_gt          0.0954
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Ce1 Ce 0.21835(4) -0.05800(2) 0.42548(2) 0.01207(10) Uani 1 1 d . . . . .
Ce2 Ce 0.22131(4) 0.44097(2) 0.42757(2) 0.01180(10) Uani 1 1 d . . . . .
P1 P -0.2623(2) -0.00560(12) 0.35550(8) 0.0182(3) Uani 1 1 d . . . . .
P2 P 0.6553(2) 0.48600(11) 0.35366(8) 0.0163(3) Uani 1 1 d . . . . .
O1 O -0.1122(6) -0.0745(3) 0.3199(2) 0.0258(10) Uani 1 1 d . . . . .
O2 O -0.1510(6) 0.0226(3) 0.4387(2) 0.0222(9) Uani 1 1 d . . . . .
O3 O -0.4889(6) -0.0481(3) 0.3482(2) 0.0208(9) Uani 1 1 d . . . . .
O4 O -0.7967(9) 0.1345(5) -0.0657(3) 0.0604(16) Uani 1 1 d . . . . .
H4D H -0.7250 0.1905 -0.0722 0.091 Uiso 1 1 d R U . . .
O5 O -1.0369(9) 0.1259(5) 0.0187(3) 0.0541(15) Uani 1 1 d . . . . .
O6 O 0.4526(6) 0.4265(3) 0.3130(2) 0.0226(9) Uani 1 1 d . . . . .
O7 O 0.6148(6) 0.5102(3) 0.4380(2) 0.0204(9) Uani 1 1 d . . . . .
O8 O 0.8633(6) 0.4370(3) 0.3484(2) 0.0210(9) Uani 1 1 d . . . . .
O9 O 0.2195(9) 0.6363(5) -0.0756(3) 0.0534(15) Uani 1 1 d . . . . .
H9E H 0.2897 0.5833 -0.0799 0.080 Uiso 1 1 d R U . . .
O10 O -0.0215(9) 0.6316(5) 0.0071(3) 0.0547(15) Uani 1 1 d . . . . .
O11 O 0.0425(6) -0.3957(3) 0.4762(2) 0.0206(9) Uani 1 1 d . . . . .
O12 O 0.2259(6) -0.3949(3) 0.3441(2) 0.0193(8) Uani 1 1 d . . . . .
O13 O 0.0643(6) -0.2228(3) 0.4792(2) 0.0256(9) Uani 1 1 d . . . . .
O14 O 0.2363(7) -0.2230(3) 0.3440(2) 0.0275(10) Uani 1 1 d . . . . .
O15 O 0.2006(6) 0.1062(3) 0.3438(2) 0.0201(9) Uani 1 1 d . . . . .
O16 O 0.4509(6) 0.1137(3) 0.4831(2) 0.0219(9) Uani 1 1 d . . . . .
O17 O 0.1432(6) 0.2727(3) 0.3551(2) 0.0243(9) Uani 1 1 d . . . . .
O18 O 0.4244(6) 0.2853(3) 0.4888(2) 0.0260(10) Uani 1 1 d . . . . .
O1W O 0.9612(9) 0.5937(5) 0.7911(3) 0.0610(18) Uani 1 1 d . . . . .
H1WA H 1.0885 0.5809 0.8099 0.092 Uiso 1 1 d R U . . .
H1WB H 0.9637 0.6474 0.7628 0.092 Uiso 1 1 d R U . . .
O2W O 0.0657(11) 0.8857(6) 0.1994(3) 0.094(3) Uani 1 1 d . . . . .
H2WC H 0.0781 0.8722 0.1514 0.113 Uiso 1 1 d R U . . .
H2WA H -0.0587 0.9058 0.2022 0.141 Uiso 1 1 d R U . . .
N1 N -0.4680(8) 0.1108(4) 0.2341(3) 0.0232(11) Uani 1 1 d . . . . .
H1C H -0.5861 0.0855 0.2533 0.028 Uiso 1 1 d R U . . .
N2 N 0.5151(8) 0.6140(4) 0.2295(3) 0.0210(11) Uani 1 1 d . . . . .
H2C H 0.3865 0.5944 0.2435 0.025 Uiso 1 1 d R U . . .
C1 C -0.2815(9) 0.1161(5) 0.3022(3) 0.0227(13) Uani 1 1 d . . . . .
H1A H -0.3000 0.1711 0.3389 0.027 Uiso 1 1 d R U . . .
H1B H -0.1492 0.1321 0.2807 0.027 Uiso 1 1 d R U . . .
C2 C -0.5076(11) 0.2174(5) 0.2047(4) 0.0325(16) Uani 1 1 d . . . . .
H2A H -0.3808 0.2463 0.1847 0.039 Uiso 1 1 d R U . . .
H2B H -0.5355 0.2612 0.2480 0.039 Uiso 1 1 d R U . . .
C3 C -0.4274(12) 0.0405(5) 0.1691(4) 0.0372(17) Uani 1 1 d . . . . .
H3A H -0.4049 -0.0281 0.1895 0.045 Uiso 1 1 d R U . . .
H3B H -0.2986 0.0658 0.1486 0.045 Uiso 1 1 d R U . . .
C4 C -0.6975(12) 0.2142(6) 0.1387(4) 0.0392(17) Uani 1 1 d . . . . .
H4A H -0.7190 0.2832 0.1191 0.047 Uiso 1 1 d R U . . .
H4B H -0.8260 0.1892 0.1597 0.047 Uiso 1 1 d R U . . .
C5 C -0.6145(13) 0.0359(6) 0.1027(4) 0.045(2) Uani 1 1 d . . . . .
H5A H -0.7408 0.0061 0.1227 0.054 Uiso 1 1 d R U . . .
H5B H -0.5841 -0.0084 0.0601 0.054 Uiso 1 1 d R U . . .
C6 C -0.6599(12) 0.1433(6) 0.0706(4) 0.0370(16) Uani 1 1 d . . . . .
H6 H -0.5351 0.1713 0.0476 0.044 Uiso 1 1 d R U . . .
C7 C -0.8536(13) 0.1348(6) 0.0064(4) 0.0422(19) Uani 1 1 d . . . . .
C8 C 0.6775(9) 0.6103(5) 0.3021(3) 0.0209(13) Uani 1 1 d . . . . .
H8A H 0.6589 0.6662 0.3380 0.025 Uiso 1 1 d R U . . .
H8B H 0.8196 0.6202 0.2868 0.025 Uiso 1 1 d R U . . .
C9 C 0.5011(11) 0.7207(5) 0.1967(4) 0.0309(15) Uani 1 1 d . . . . .
H9A H 0.6360 0.7429 0.1792 0.037 Uiso 1 1 d R U . . .
H9B H 0.4738 0.7685 0.2376 0.037 Uiso 1 1 d R U . . .
C10 C 0.5585(11) 0.5398(5) 0.1656(4) 0.0312(15) Uani 1 1 d . . . . .
H10A H 0.5726 0.4713 0.1872 0.037 Uiso 1 1 d R U . . .
H10B H 0.6920 0.5618 0.1469 0.037 Uiso 1 1 d R U . . .
C11 C 0.3203(11) 0.7203(6) 0.1268(4) 0.0375(17) Uani 1 1 d . . . . .
H11A H 0.3128 0.7891 0.1052 0.045 Uiso 1 1 d R U . . .
H11B H 0.1850 0.7019 0.1455 0.045 Uiso 1 1 d R U . . .
C12 C 0.3772(11) 0.5373(5) 0.0968(4) 0.0343(16) Uani 1 1 d . . . . .
H12A H 0.4047 0.4886 0.0565 0.041 Uiso 1 1 d R U . . .
H12B H 0.2444 0.5143 0.1155 0.041 Uiso 1 1 d R U . . .
C13 C 0.3535(11) 0.6434(5) 0.0606(4) 0.0324(16) Uani 1 1 d . . . . .
H13 H 0.4836 0.6649 0.0382 0.039 Uiso 1 1 d R U . . .
C14 C 0.1619(13) 0.6375(6) -0.0045(4) 0.0408(18) Uani 1 1 d . . . . .
C15 C 0.0947(8) -0.3072(4) 0.4500(3) 0.0150(11) Uani 1 1 d . . . . .
C16 C 0.1978(8) -0.3084(4) 0.3734(3) 0.0150(11) Uani 1 1 d . . . . .
C17 C 0.2237(8) 0.1920(4) 0.3791(3) 0.0163(12) Uani 1 1 d . . . . .
C18 C 0.3805(8) 0.1982(4) 0.4587(3) 0.0178(12) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ce1 O3 2.412(4) 1_655 ?
Ce1 O2 2.455(4) 2_556 ?
Ce1 O13 2.528(4) . ?
Ce1 O15 2.555(4) . ?
Ce1 O1 2.555(4) . ?
Ce1 O14 2.562(4) . ?
Ce1 O16 2.570(4) 2_656 ?
Ce1 O2 2.652(4) . ?
Ce1 O16 2.695(4) . ?
Ce2 O7 2.440(4) 2_666 ?
Ce2 O8 2.463(4) 1_455 ?
Ce2 O17 2.492(4) . ?
Ce2 O11 2.542(4) 2_556 ?
Ce2 O12 2.572(4) 1_565 ?
Ce2 O7 2.573(4) . ?
Ce2 O18 2.607(4) . ?
Ce2 O6 2.608(4) . ?
Ce2 O11 2.645(4) 1_565 ?
P1 O3 1.490(4) . ?
P1 O2 1.522(4) . ?
P1 O1 1.525(4) . ?
P1 C1 1.830(6) . ?
P2 O8 1.508(4) . ?
P2 O7 1.527(4) . ?
P2 O6 1.530(4) . ?
P2 C8 1.851(6) . ?
O2 Ce1 2.455(4) 2_556 ?
O3 Ce1 2.412(4) 1_455 ?
O4 C7 1.326(9) . ?
O4 H4D 0.8500 . ?
O5 C7 1.204(9) . ?
O7 Ce2 2.440(4) 2_666 ?
O8 Ce2 2.463(4) 1_655 ?
O9 C14 1.312(9) . ?
O9 H9E 0.8499 . ?
O10 C14 1.200(9) . ?
O11 C15 1.278(6) . ?
O11 Ce2 2.542(4) 2_556 ?
O11 Ce2 2.645(4) 1_545 ?
O12 C16 1.259(6) . ?
O12 Ce2 2.572(4) 1_545 ?
O13 C15 1.237(6) . ?
O14 C16 1.244(6) . ?
O15 C17 1.254(7) . ?
O16 C18 1.260(6) . ?
O16 Ce1 2.570(4) 2_656 ?
O17 C17 1.240(6) . ?
O18 C18 1.239(6) . ?
O1W H1WA 0.8499 . ?
O1W H1WB 0.8502 . ?
O2W H2WC 0.8500 . ?
O2W H2WA 0.8500 . ?
N1 C3 1.489(8) . ?
N1 C2 1.500(7) . ?
N1 C1 1.531(7) . ?
N1 H1C 0.9001 . ?
N2 C8 1.494(7) . ?
N2 C9 1.502(7) . ?
N2 C10 1.514(7) . ?
N2 H2C 0.8999 . ?
C1 H1A 0.9698 . ?
C1 H1B 0.9700 . ?
C2 C4 1.522(9) . ?
C2 H2A 0.9698 . ?
C2 H2B 0.9699 . ?
C3 C5 1.515(9) . ?
C3 H3A 0.9701 . ?
C3 H3B 0.9700 . ?
C4 C6 1.529(10) . ?
C4 H4A 0.9699 . ?
C4 H4B 0.9700 . ?
C5 C6 1.532(9) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9699 . ?
C6 C7 1.520(9) . ?
C6 H6 0.9799 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C11 1.529(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C12 1.518(9) . ?
C10 H10A 0.9699 . ?
C10 H10B 0.9700 . ?
C11 C13 1.547(9) . ?
C11 H11A 0.9699 . ?
C11 H11B 0.9700 . ?
C12 C13 1.520(9) . ?
C12 H12A 0.9701 . ?
C12 H12B 0.9700 . ?
C13 C14 1.520(9) . ?
C13 H13 0.9799 . ?
C15 C16 1.538(7) . ?
C17 C18 1.561(7) . ?

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
O3 Ce1 O2 139.33(13) 1_655 2_556 ?
O3 Ce1 O13 124.61(13) 1_655 . ?
O2 Ce1 O13 72.02(13) 2_556 . ?
O3 Ce1 O15 70.89(13) 1_655 . ?
O2 Ce1 O15 110.60(13) 2_556 . ?
O13 Ce1 O15 154.50(13) . . ?
O3 Ce1 O1 103.15(13) 1_655 . ?
O2 Ce1 O1 115.90(12) 2_556 . ?
O13 Ce1 O1 85.05(13) . . ?
O15 Ce1 O1 70.87(13) . . ?
O3 Ce1 O14 67.56(13) 1_655 . ?
O2 Ce1 O14 134.15(13) 2_556 . ?
O13 Ce1 O14 63.50(13) . . ?
O15 Ce1 O14 114.23(13) . . ?
O1 Ce1 O14 71.84(13) . . ?
O3 Ce1 O16 73.49(12) 1_655 2_656 ?
O2 Ce1 O16 74.13(12) 2_556 2_656 ?
O13 Ce1 O16 79.86(12) . 2_656 ?
O15 Ce1 O16 125.60(12) . 2_656 ?
O1 Ce1 O16 158.24(13) . 2_656 ?
O14 Ce1 O16 87.35(13) . 2_656 ?
O3 Ce1 O2 142.18(13) 1_655 . ?
O2 Ce1 O2 64.16(13) 2_556 . ?
O13 Ce1 O2 87.29(12) . . ?
O15 Ce1 O2 72.39(12) . . ?
O1 Ce1 O2 55.51(12) . . ?
O14 Ce1 O2 121.76(13) . . ?
O16 Ce1 O2 138.28(12) 2_656 . ?
O3 Ce1 O16 76.79(13) 1_655 . ?
O2 Ce1 O16 70.29(12) 2_556 . ?
O13 Ce1 O16 137.71(12) . . ?
O15 Ce1 O16 60.76(12) . . ?
O1 Ce1 O16 128.85(12) . . ?
O14 Ce1 O16 142.73(12) . . ?
O16 Ce1 O16 72.05(14) 2_656 . ?
O2 Ce1 O16 93.07(12) . . ?
O7 Ce2 O8 137.70(12) 2_666 1_455 ?
O7 Ce2 O17 133.54(12) 2_666 . ?
O8 Ce2 O17 70.14(13) 1_455 . ?
O7 Ce2 O11 70.68(12) 2_666 2_556 ?
O8 Ce2 O11 74.23(12) 1_455 2_556 ?
O17 Ce2 O11 92.78(13) . 2_556 ?
O7 Ce2 O12 107.04(13) 2_666 1_565 ?
O8 Ce2 O12 75.28(13) 1_455 1_565 ?
O17 Ce2 O12 117.44(13) . 1_565 ?
O11 Ce2 O12 125.34(12) 2_556 1_565 ?
O7 Ce2 O7 65.94(14) 2_666 . ?
O8 Ce2 O7 145.77(12) 1_455 . ?
O17 Ce2 O7 113.94(13) . . ?
O11 Ce2 O7 136.42(11) 2_556 . ?
O12 Ce2 O7 73.17(12) 1_565 . ?
O7 Ce2 O18 71.91(12) 2_666 . ?
O8 Ce2 O18 127.66(13) 1_455 . ?
O17 Ce2 O18 63.40(12) . . ?
O11 Ce2 O18 85.01(12) 2_556 . ?
O12 Ce2 O18 148.32(13) 1_565 . ?
O7 Ce2 O18 78.04(12) . . ?
O7 Ce2 O6 121.15(12) 2_666 . ?
O8 Ce2 O6 99.21(12) 1_455 . ?
O17 Ce2 O6 68.57(13) . . ?
O11 Ce2 O6 161.32(13) 2_556 . ?
O12 Ce2 O6 67.66(12) 1_565 . ?
O7 Ce2 O6 56.34(11) . . ?
O18 Ce2 O6 85.54(13) . . ?
O7 Ce2 O11 70.19(12) 2_666 1_565 ?
O8 Ce2 O11 75.01(12) 1_455 1_565 ?
O17 Ce2 O11 143.54(12) . 1_565 ?
O11 Ce2 O11 67.29(14) 2_556 1_565 ?
O12 Ce2 O11 61.56(12) 1_565 1_565 ?
O7 Ce2 O11 100.82(12) . 1_565 ?
O18 Ce2 O11 138.60(12) . 1_565 ?
O6 Ce2 O11 128.73(12) . 1_565 ?
O3 P1 O2 116.9(2) . . ?
O3 P1 O1 114.5(2) . . ?
O2 P1 O1 105.5(2) . . ?
O3 P1 C1 103.6(2) . . ?
O2 P1 C1 105.8(3) . . ?
O1 P1 C1 110.3(3) . . ?
O8 P2 O7 114.7(2) . . ?
O8 P2 O6 115.9(2) . . ?
O7 P2 O6 106.3(2) . . ?
O8 P2 C8 105.1(3) . . ?
O7 P2 C8 107.3(2) . . ?
O6 P2 C8 107.0(2) . . ?
P1 O1 Ce1 101.07(19) . . ?
P1 O2 Ce1 142.9(2) . 2_556 ?
P1 O2 Ce1 97.14(18) . . ?
Ce1 O2 Ce1 115.84(13) 2_556 . ?
P1 O3 Ce1 139.1(2) . 1_455 ?
C7 O4 H4D 109.2 . . ?
P2 O6 Ce2 97.76(18) . . ?
P2 O7 Ce2 145.6(2) . 2_666 ?
P2 O7 Ce2 99.31(18) . . ?
Ce2 O7 Ce2 114.06(14) 2_666 . ?
P2 O8 Ce2 136.3(2) . 1_655 ?
C14 O9 H9E 108.3 . . ?
C15 O11 Ce2 128.5(3) . 2_556 ?
C15 O11 Ce2 118.8(3) . 1_545 ?
Ce2 O11 Ce2 112.71(14) 2_556 1_545 ?
C16 O12 Ce2 121.1(3) . 1_545 ?
C15 O13 Ce1 120.2(3) . . ?
C16 O14 Ce1 119.6(3) . . ?
C17 O15 Ce1 119.0(3) . . ?
C18 O16 Ce1 135.9(3) . 2_656 ?
C18 O16 Ce1 116.1(3) . . ?
Ce1 O16 Ce1 107.95(13) 2_656 . ?
C17 O17 Ce2 123.1(3) . . ?
C18 O18 Ce2 119.5(3) . . ?
H1WA O1W H1WB 109.5 . . ?
H2WC O2W H2WA 109.8 . . ?
C3 N1 C2 111.6(5) . . ?
C3 N1 C1 111.4(5) . . ?
C2 N1 C1 109.5(5) . . ?
C3 N1 H1C 108.1 . . ?
C2 N1 H1C 108.1 . . ?
C1 N1 H1C 108.1 . . ?
C8 N2 C9 112.3(5) . . ?
C8 N2 C10 111.8(4) . . ?
C9 N2 C10 109.7(5) . . ?
C8 N2 H2C 107.6 . . ?
C9 N2 H2C 107.7 . . ?
C10 N2 H2C 107.6 . . ?
N1 C1 P1 111.8(4) . . ?
N1 C1 H1A 109.5 . . ?
P1 C1 H1A 109.4 . . ?
N1 C1 H1B 108.8 . . ?
P1 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
N1 C2 C4 110.3(5) . . ?
N1 C2 H2A 109.1 . . ?
C4 C2 H2A 109.5 . . ?
N1 C2 H2B 109.9 . . ?
C4 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
N1 C3 C5 110.5(5) . . ?
N1 C3 H3A 109.9 . . ?
C5 C3 H3A 109.8 . . ?
N1 C3 H3B 109.2 . . ?
C5 C3 H3B 109.3 . . ?
H3A C3 H3B 108.2 . . ?
C2 C4 C6 110.8(6) . . ?
C2 C4 H4A 109.6 . . ?
C6 C4 H4A 109.5 . . ?
C2 C4 H4B 109.4 . . ?
C6 C4 H4B 109.4 . . ?
H4A C4 H4B 108.1 . . ?
C3 C5 C6 111.4(6) . . ?
C3 C5 H5A 109.0 . . ?
C6 C5 H5A 109.1 . . ?
C3 C5 H5B 109.6 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.0 . . ?
C7 C6 C5 109.3(6) . . ?
C7 C6 C4 111.3(6) . . ?
C5 C6 C4 109.3(6) . . ?
C7 C6 H6 109.1 . . ?
C5 C6 H6 108.8 . . ?
C4 C6 H6 108.9 . . ?
O5 C7 O4 123.5(7) . . ?
O5 C7 C6 124.7(7) . . ?
O4 C7 C6 111.8(7) . . ?
N2 C8 P2 111.9(4) . . ?
N2 C8 H8A 109.4 . . ?
P2 C8 H8A 109.3 . . ?
N2 C8 H8B 108.9 . . ?
P2 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
N2 C9 C11 109.4(5) . . ?
N2 C9 H9A 109.5 . . ?
C11 C9 H9A 109.8 . . ?
N2 C9 H9B 109.9 . . ?
C11 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
N2 C10 C12 110.1(5) . . ?
N2 C10 H10A 109.8 . . ?
C12 C10 H10A 109.9 . . ?
N2 C10 H10B 109.4 . . ?
C12 C10 H10B 109.5 . . ?
H10A C10 H10B 108.2 . . ?
C9 C11 C13 112.0(5) . . ?
C9 C11 H11A 109.3 . . ?
C13 C11 H11A 109.2 . . ?
C9 C11 H11B 109.2 . . ?
C13 C11 H11B 109.1 . . ?
H11A C11 H11B 107.9 . . ?
C13 C12 C10 111.2(6) . . ?
C13 C12 H12A 109.5 . . ?
C10 C12 H12A 109.6 . . ?
C13 C12 H12B 109.2 . . ?
C10 C12 H12B 109.2 . . ?
H12A C12 H12B 108.1 . . ?
C12 C13 C14 108.8(6) . . ?
C12 C13 C11 108.4(5) . . ?
C14 C13 C11 110.7(5) . . ?
C12 C13 H13 109.5 . . ?
C14 C13 H13 109.8 . . ?
C11 C13 H13 109.6 . . ?
O10 C14 O9 123.3(7) . . ?
O10 C14 C13 124.4(7) . . ?
O9 C14 C13 112.2(7) . . ?
O13 C15 O11 126.1(5) . . ?
O13 C15 C16 118.4(5) . . ?
O11 C15 C16 115.5(5) . . ?
O14 C16 O12 126.0(5) . . ?
O14 C16 C15 116.4(5) . . ?
O12 C16 C15 117.6(5) . . ?
O17 C17 O15 126.4(5) . . ?
O17 C17 C18 117.4(5) . . ?
O15 C17 C18 116.1(5) . . ?
O18 C18 O16 128.2(5) . . ?
O18 C18 C17 116.3(5) . . ?
O16 C18 C17 115.5(5) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C12 H12B O1W 0.97 2.56 3.444(10) 150.9 2_666
C10 H10A O6 0.97 2.43 3.053(8) 121.4 .
C9 H9B O14 0.97 2.51 3.304(8) 138.5 1_565
C8 H8B O12 0.97 2.63 3.442(7) 141.0 1_665
C5 H5A O2W 0.97 2.43 3.331(12) 154.7 1_445
C2 H2B O6 0.97 2.42 3.314(8) 153.3 1_455
C1 H1B O15 0.97 2.36 3.038(7) 126.4 .
C12 H12B O1W 0.97 2.56 3.444(10) 150.9 2_666
C10 H10A O6 0.97 2.43 3.053(8) 121.4 .
C9 H9B O14 0.97 2.51 3.304(8) 138.5 1_565
C8 H8B O12 0.97 2.63 3.442(7) 141.0 1_665
C5 H5A O2W 0.97 2.43 3.331(12) 154.7 1_445
C2 H2B O6 0.97 2.42 3.314(8) 153.3 1_455
C1 H1B O15 0.97 2.36 3.038(7) 126.4 .
N2 H2C O12 0.90 2.12 2.851(6) 138.0 1_565
N1 H1C O15 0.90 2.21 2.992(6) 145.0 1_455
O2W H2WA O1 0.85 2.09 2.537(7) 111.9 1_565
O1W H1WB O17 0.85 2.30 3.063(6) 149.0 2_666
O1W H1WA O9 0.85 2.11 2.638(7) 119.7 1_656
C1 H1B O15 0.97 2.36 3.038(7) 126.4 .
C2 H2B O6 0.97 2.42 3.314(8) 153.3 1_455
C5 H5A O2W 0.97 2.43 3.331(12) 154.7 1_445
C8 H8B O12 0.97 2.63 3.442(7) 141.0 1_665
C9 H9B O14 0.97 2.51 3.304(8) 138.5 1_565
C10 H10A O6 0.97 2.43 3.053(8) 121.4 .
C12 H12B O1W 0.97 2.56 3.444(10) 150.9 2_666
O2W H2WA O1 0.85 2.09 2.537(7) 111.9 1_565
N1 H1C O15 0.90 2.21 2.992(6) 145.0 1_455
N2 H2C O12 0.90 2.12 2.851(6) 138.0 1_565
C1 H1B O15 0.97 2.36 3.038(7) 126.4 .
C2 H2B O6 0.97 2.42 3.314(8) 153.3 1_455
C5 H5A O2W 0.97 2.43 3.331(12) 154.7 1_445
C8 H8B O12 0.97 2.63 3.442(7) 141.0 1_665
C9 H9B O14 0.97 2.51 3.304(8) 138.5 1_565
C10 H10A O6 0.97 2.43 3.053(8) 121.4 .

_refine_diff_density_max         1.347
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.171

####################################################################### 
# 
# 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_szg248
_database_code_depnum_ccdc_archive 'CCDC 1503587'
_audit_update_record             
;
2016-09-09 deposited with the CCDC.
2017-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H26 Dy2 N O23 P'
_chemical_formula_weight         920.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   11.4663(4)
_cell_length_b                   14.3926(5)
_cell_length_c                   15.8262(6)
_cell_angle_alpha                90
_cell_angle_beta                 109.4280(10)
_cell_angle_gamma                90
_cell_volume                     2463.08(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    6676
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      30.39

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.482
_exptl_crystal_F_000             1768
_exptl_transmission_factor_min   0.437
_exptl_transmission_factor_max   0.790
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    6.194
_shelx_estimated_absorpt_T_min   0.437
_shelx_estimated_absorpt_T_max   0.790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13646
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.923
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5085
_reflns_number_gt                4378
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0228P)²+8.7319P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5085
_refine_ls_number_parameters     379
_refine_ls_number_restraints     319
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0243
_refine_ls_wR_factor_ref         0.0567
_refine_ls_wR_factor_gt          0.0538
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      0.996
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.001

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
Dy1 Dy 0.47738(2) 0.08762(2) 0.17140(2) 0.01565(6) Uani 1 1 d . . . . .
Dy2 Dy 0.45597(2) 0.52865(2) 0.17970(2) 0.01591(6) Uani 1 1 d . . . . .
P1 P 0.35104(10) 0.20226(8) -0.04999(8) 0.0179(2) Uani 1 1 d . . . . .
O1 O 0.3684(3) 0.3059(2) -0.0167(2) 0.0226(7) Uani 1 1 d . U . . .
H1C H 0.4445 0.3179 0.0052 0.034 Uiso 1 1 d R U . . .
O2 O 0.3950(3) 0.1407(2) 0.0302(2) 0.0263(7) Uani 1 1 d . U . . .
O3 O 0.4042(3) 0.1880(2) -0.1234(2) 0.0272(8) Uani 1 1 d . U . . .
O4 O 0.4110(3) -0.0418(3) 0.0647(2) 0.0278(8) Uani 1 1 d . U . . .
H4D H 0.4253 -0.0924 0.0933 0.042 Uiso 1 1 d R U . . .
O5 O 0.6599(3) 0.0474(2) 0.1352(2) 0.0205(7) Uani 1 1 d . U . . .
O6 O 0.6623(3) 0.1103(2) 0.2970(2) 0.0232(7) Uani 1 1 d . U . . .
O7 O 0.8643(3) 0.0241(2) 0.1927(2) 0.0222(7) Uani 1 1 d . U . . .
O8 O 0.8658(3) 0.0860(2) 0.3512(2) 0.0197(7) Uani 1 1 d . U . . .
O9 O 0.5429(3) -0.0678(3) 0.2382(2) 0.0329(8) Uani 1 1 d . U . . .
H9A H 0.5976 -0.0890 0.2186 0.049 Uiso 1 1 d R U . . .
H9B H 0.5723 -0.0625 0.2947 0.049 Uiso 1 1 d R U . . .
O10 O 0.4202(3) 0.0628(3) 0.3048(2) 0.0253(7) Uani 1 1 d . U . . .
O11 O 0.2571(3) 0.0691(2) 0.1379(2) 0.0238(7) Uani 1 1 d . U . . .
O12 O 0.1028(3) 0.0564(2) 0.1938(2) 0.0241(7) Uani 1 1 d . U . . .
O13 O 0.2639(3) 0.0531(3) 0.3598(2) 0.0258(7) Uani 1 1 d . U . . .
O14 O 0.3928(3) 0.2301(2) 0.2094(2) 0.0302(7) Uani 1 1 d . U . . .
O15 O 0.5870(3) 0.2424(2) 0.1541(2) 0.0261(7) Uani 1 1 d . U . . .
O16 O 0.3738(3) 0.3844(2) 0.2029(2) 0.0284(8) Uani 1 1 d . U . . .
O17 O 0.5639(3) 0.3976(2) 0.1446(2) 0.0286(8) Uani 1 1 d . U . . .
O18 O 0.4450(4) 0.6902(3) 0.1745(3) 0.0438(10) Uani 1 1 d . U . . .
H18B H 0.3765 0.7072 0.1376 0.066 Uiso 1 1 d R U . . .
H18C H 0.4520 0.7103 0.2263 0.066 Uiso 1 1 d R U . . .
O19 O 0.3843(4) 0.5386(3) 0.0214(3) 0.0347(9) Uani 1 1 d . U . . .
H19A H 0.3864 0.5947 0.0061 0.052 Uiso 1 1 d R U . . .
O20 O -0.2785(5) 0.2281(4) 0.0479(4) 0.0700(15) Uani 1 1 d . U . . .
H20A H -0.3145 0.2362 0.0862 0.105 Uiso 1 1 d R U . A .
C7 C -0.1757(6) 0.2589(6) 0.0747(5) 0.067(2) Uani 0.394(10) 1 d D . P A 1
O21 O -0.1818(10) 0.3541(8) 0.0946(8) 0.054(3) Uani 0.394(10) 1 d D U P A 1
C7' C -0.1757(6) 0.2589(6) 0.0747(5) 0.067(2) Uani 0.606(10) 1 d D . P A 2
O21' O -0.1283(8) 0.2597(6) 0.1622(5) 0.065(3) Uani 0.606(10) 1 d D U P A 2
O1W O 0.3018(4) 0.8264(4) 0.2087(3) 0.0686(15) Uani 1 1 d . U . . .
H1WC H 0.3291 0.8437 0.2629 0.082 Uiso 1 1 d R U . . .
H1WA H 0.3376 0.8564 0.1784 0.103 Uiso 1 1 d R U . . .
O2W O 0.1397(8) 0.5152(6) 0.9488(6) 0.153(4) Uani 1 1 d . . . . .
H2WA H 0.1379 0.5701 0.9671 0.230 Uiso 1 1 d R U . . .
H2WB H 0.0694 0.4907 0.9372 0.230 Uiso 1 1 d R U . . .
N1 N 0.1201(3) 0.1824(3) -0.0286(3) 0.0209(8) Uani 1 1 d . . . . .
H1D H 0.1642 0.1485 0.0187 0.025 Uiso 1 1 d R U . . .
C1 C 0.1865(4) 0.1803(3) -0.0958(3) 0.0217(10) Uani 1 1 d . . . . .
H1A H 0.1495 0.2268 -0.1407 0.026 Uiso 1 1 d R U . . .
H1B H 0.1731 0.1207 -0.1254 0.026 Uiso 1 1 d R U . . .
C2 C -0.0067(4) 0.1391(4) -0.0687(3) 0.0281(11) Uani 1 1 d . . . . .
H2A H 0.0027 0.0747 -0.0819 0.034 Uiso 1 1 d R U . . .
H2B H -0.0503 0.1699 -0.1246 0.034 Uiso 1 1 d R U . . .
C3 C 0.1114(5) 0.2794(4) 0.0034(4) 0.0349(13) Uani 1 1 d . . . . .
H3A H 0.0732 0.3184 -0.0481 0.042 Uiso 1 1 d R U . . .
H3B H 0.1930 0.3033 0.0340 0.042 Uiso 1 1 d R U . . .
C4 C 0.0357(5) 0.2839(4) 0.0657(4) 0.0393(14) Uani 1 1 d . . . . .
H4A H 0.0306 0.3473 0.0840 0.047 Uiso 1 1 d R U . . .
H4B H 0.0757 0.2477 0.1188 0.047 Uiso 1 1 d R U . . .
C5 C -0.0836(5) 0.1458(4) -0.0069(3) 0.0315(12) Uani 1 1 d . . . . .
H5A H -0.1646 0.1203 -0.0363 0.038 Uiso 1 1 d R U . . .
H5B H -0.0446 0.1101 0.0469 0.038 Uiso 1 1 d R U . . .
C6 C -0.0947(5) 0.2470(4) 0.0176(4) 0.0332(12) Uani 1 1 d . . . . .
H6 H -0.1328 0.2823 -0.0374 0.040 Uiso 1 1 d R U . A .
C8 C 0.5365(4) 0.3165(3) 0.1609(3) 0.0190(9) Uani 1 1 d . . . . .
C9 C 0.4246(4) 0.3093(3) 0.1933(3) 0.0217(10) Uani 1 1 d . . . . .
C10 C 0.7613(4) 0.0488(3) 0.1973(3) 0.0173(9) Uani 1 1 d . . . . .
C11 C 0.7619(4) 0.0853(3) 0.2894(3) 0.0169(9) Uani 1 1 d . . . . .
C12 C 0.2144(4) 0.0619(3) 0.2008(3) 0.0174(9) Uani 1 1 d . . . . .
C13 C 0.3084(4) 0.0597(3) 0.2975(3) 0.0180(9) Uani 1 1 d . . . . .
H4C H 0.377(6) -0.031(5) 0.010(4) 0.05(2) Uiso 1 1 d . . . . .
H19C H 0.328(8) 0.523(7) -0.010(6) 0.10(4) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O2 2.251(3) . ?
Dy1 O6 2.398(3) . ?
Dy1 O5 2.416(3) . ?
Dy1 O11 2.416(3) . ?
Dy1 O14 2.428(3) . ?
Dy1 O10 2.436(3) . ?
Dy1 O4 2.459(4) . ?
Dy1 O9 2.481(4) . ?
Dy1 O15 2.617(3) . ?
Dy2 O18 2.328(4) . ?
Dy2 O12 2.349(3) 2 ?
Dy2 O16 2.359(3) . ?
Dy2 O7 2.358(3) 2_655 ?
Dy2 O19 2.367(4) . ?
Dy2 O8 2.400(3) 2_655 ?
Dy2 O13 2.413(3) 2 ?
Dy2 O17 2.419(3) . ?
P1 O2 1.491(3) . ?
P1 O3 1.495(3) . ?
P1 O1 1.573(3) . ?
P1 C1 1.810(5) . ?
O1 H1C 0.8428 . ?
O4 H4D 0.8454 . ?
O4 H4C 0.83(7) . ?
O5 C10 1.248(5) . ?
O6 C11 1.242(5) . ?
O7 C10 1.259(5) . ?
O7 Dy2 2.358(3) 2_645 ?
O8 C11 1.265(5) . ?
O8 Dy2 2.400(3) 2_645 ?
O9 H9A 0.8443 . ?
O9 H9B 0.8482 . ?
O10 C13 1.249(5) . ?
O11 C12 1.251(5) . ?
O12 C12 1.249(5) . ?
O12 Dy2 2.349(3) 2_545 ?
O13 C13 1.255(5) . ?
O13 Dy2 2.413(3) 2_545 ?
O14 C9 1.248(6) . ?
O15 C8 1.234(5) . ?
O16 C9 1.261(6) . ?
O17 C8 1.258(6) . ?
O18 H18B 0.8443 . ?
O18 H18C 0.8481 . ?
O19 H19A 0.8451 . ?
O19 H19C 0.71(9) . ?
O20 C7' 1.197(8) . ?
O20 C7 1.197(8) . ?
O20 H20A 0.8464 . ?
C7 O21 1.412(12) . ?
C7 C6 1.506(7) . ?
C7' O21' 1.309(9) . ?
C7' C6 1.506(7) . ?
O1W H1WC 0.8480 . ?
O1W H1WA 0.8453 . ?
O2W H2WA 0.8451 . ?
O2W H2WB 0.8428 . ?
N1 C3 1.499(6) . ?
N1 C2 1.514(6) . ?
N1 C1 1.501(5) . ?
N1 H1D 0.8960 . ?
C1 H1A 0.9653 . ?
C1 H1B 0.9648 . ?
C2 C5 1.523(6) . ?
C2 H2A 0.9640 . ?
C2 H2B 0.9664 . ?
C3 C4 1.516(7) . ?
C3 H3A 0.9662 . ?
C3 H3B 0.9624 . ?
C4 C6 1.530(7) . ?
C4 H4A 0.9647 . ?
C4 H4B 0.9661 . ?
C5 C6 1.523(8) . ?
C5 H5A 0.9626 . ?
C5 H5B 0.9667 . ?
C6 H6 0.9763 . ?
C8 C9 1.535(6) . ?
C10 C11 1.546(6) . ?
C12 C13 1.552(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy1 O6 137.76(12) . . ?
O2 Dy1 O5 87.52(11) . . ?
O6 Dy1 O5 68.44(10) . . ?
O2 Dy1 O11 75.91(11) . . ?
O6 Dy1 O11 140.20(10) . . ?
O5 Dy1 O11 147.75(11) . . ?
O2 Dy1 O14 83.63(12) . . ?
O6 Dy1 O14 89.72(12) . . ?
O5 Dy1 O14 135.19(11) . . ?
O11 Dy1 O14 70.95(12) . . ?
O2 Dy1 O10 139.93(11) . . ?
O6 Dy1 O10 73.73(10) . . ?
O5 Dy1 O10 132.37(10) . . ?
O11 Dy1 O10 67.13(10) . . ?
O14 Dy1 O10 70.40(12) . . ?
O2 Dy1 O4 69.11(13) . . ?
O6 Dy1 O4 131.23(11) . . ?
O5 Dy1 O4 75.56(11) . . ?
O11 Dy1 O4 72.74(11) . . ?
O14 Dy1 O4 138.78(12) . . ?
O10 Dy1 O4 111.90(12) . . ?
O2 Dy1 O9 134.17(12) . . ?
O6 Dy1 O9 73.18(12) . . ?
O5 Dy1 O9 73.85(11) . . ?
O11 Dy1 O9 98.06(12) . . ?
O14 Dy1 O9 138.16(12) . . ?
O10 Dy1 O9 68.22(11) . . ?
O4 Dy1 O9 65.83(12) . . ?
O2 Dy1 O15 70.41(11) . . ?
O6 Dy1 O15 69.37(11) . . ?
O5 Dy1 O15 72.26(10) . . ?
O11 Dy1 O15 125.05(11) . . ?
O14 Dy1 O15 63.37(10) . . ?
O10 Dy1 O15 119.50(11) . . ?
O4 Dy1 O15 128.54(11) . . ?
O9 Dy1 O15 136.40(11) . . ?
O18 Dy2 O12 80.36(13) . 2 ?
O18 Dy2 O16 149.87(12) . . ?
O12 Dy2 O16 76.97(12) 2 . ?
O18 Dy2 O7 94.56(14) . 2_655 ?
O12 Dy2 O7 72.04(10) 2 2_655 ?
O16 Dy2 O7 97.03(12) . 2_655 ?
O18 Dy2 O19 84.63(16) . . ?
O12 Dy2 O19 142.61(12) 2 . ?
O16 Dy2 O19 101.67(14) . . ?
O7 Dy2 O19 143.61(12) 2_655 . ?
O18 Dy2 O8 71.91(12) . 2_655 ?
O12 Dy2 O8 128.33(11) 2 2_655 ?
O16 Dy2 O8 138.19(11) . 2_655 ?
O7 Dy2 O8 67.87(10) 2_655 2_655 ?
O19 Dy2 O8 77.47(12) . 2_655 ?
O18 Dy2 O13 78.80(13) . 2 ?
O12 Dy2 O13 67.94(10) 2 2 ?
O16 Dy2 O13 74.45(12) . 2 ?
O7 Dy2 O13 139.98(10) 2_655 2 ?
O19 Dy2 O13 75.65(12) . 2 ?
O8 Dy2 O13 141.66(11) 2_655 2 ?
O18 Dy2 O17 142.75(12) . . ?
O12 Dy2 O17 129.95(12) 2 . ?
O16 Dy2 O17 67.10(11) . . ?
O7 Dy2 O17 78.88(12) 2_655 . ?
O19 Dy2 O17 80.11(13) . . ?
O8 Dy2 O17 71.69(11) 2_655 . ?
O13 Dy2 O17 128.64(12) 2 . ?
O2 P1 O3 118.0(2) . . ?
O2 P1 O1 108.00(19) . . ?
O3 P1 O1 110.62(19) . . ?
O2 P1 C1 104.4(2) . . ?
O3 P1 C1 107.7(2) . . ?
O1 P1 C1 107.4(2) . . ?
P1 O1 H1C 109.2 . . ?
P1 O2 Dy1 163.4(2) . . ?
Dy1 O4 H4D 108.9 . . ?
Dy1 O4 H4C 120(5) . . ?
H4D O4 H4C 131.0 . . ?
C10 O5 Dy1 117.6(3) . . ?
C11 O6 Dy1 117.9(3) . . ?
C10 O7 Dy2 120.8(3) . 2_645 ?
C11 O8 Dy2 119.1(3) . 2_645 ?
Dy1 O9 H9A 109.0 . . ?
Dy1 O9 H9B 109.1 . . ?
H9A O9 H9B 109.7 . . ?
C13 O10 Dy1 119.2(3) . . ?
C12 O11 Dy1 119.5(3) . . ?
C12 O12 Dy2 120.8(3) . 2_545 ?
C13 O13 Dy2 118.1(3) . 2_545 ?
C9 O14 Dy1 123.5(3) . . ?
C8 O15 Dy1 118.1(3) . . ?
C9 O16 Dy2 120.7(3) . . ?
C8 O17 Dy2 119.7(3) . . ?
Dy2 O18 H18B 110.0 . . ?
Dy2 O18 H18C 108.7 . . ?
H18B O18 H18C 109.7 . . ?
Dy2 O19 H19A 109.2 . . ?
Dy2 O19 H19C 129(8) . . ?
H19A O19 H19C 102.5 . . ?
C7' O20 H20A 110.7 . . ?
C7 O20 H20A 110.7 . . ?
O20 C7 O21 108.8(8) . . ?
O20 C7 C6 118.5(6) . . ?
O21 C7 C6 109.3(8) . . ?
O20 C7' O21' 113.0(7) . . ?
O20 C7' C6 118.5(6) . . ?
O21' C7' C6 120.9(6) . . ?
H1WC O1W H1WA 109.8 . . ?
H2WA O2W H2WB 109.5 . . ?
C3 N1 C2 111.3(4) . . ?
C3 N1 C1 111.4(4) . . ?
C2 N1 C1 109.7(3) . . ?
C3 N1 H1D 107.9 . . ?
C2 N1 H1D 108.8 . . ?
C1 N1 H1D 107.7 . . ?
N1 C1 P1 114.8(3) . . ?
N1 C1 H1A 107.7 . . ?
P1 C1 H1A 108.5 . . ?
N1 C1 H1B 109.1 . . ?
P1 C1 H1B 109.0 . . ?
H1A C1 H1B 107.4 . . ?
N1 C2 C5 112.6(4) . . ?
N1 C2 H2A 109.0 . . ?
C5 C2 H2A 109.3 . . ?
N1 C2 H2B 109.1 . . ?
C5 C2 H2B 109.0 . . ?
H2A C2 H2B 107.7 . . ?
N1 C3 C4 112.1(5) . . ?
N1 C3 H3A 108.6 . . ?
C4 C3 H3A 109.0 . . ?
N1 C3 H3B 109.9 . . ?
C4 C3 H3B 109.1 . . ?
H3A C3 H3B 107.9 . . ?
C3 C4 C6 109.8(4) . . ?
C3 C4 H4A 110.0 . . ?
C6 C4 H4A 109.3 . . ?
C3 C4 H4B 109.4 . . ?
C6 C4 H4B 110.4 . . ?
H4A C4 H4B 107.9 . . ?
C6 C5 C2 109.8(4) . . ?
C6 C5 H5A 109.7 . . ?
C2 C5 H5A 109.7 . . ?
C6 C5 H5B 109.7 . . ?
C2 C5 H5B 109.6 . . ?
H5A C5 H5B 108.2 . . ?
C7' C6 C5 112.5(5) . . ?
C7 C6 C5 112.5(5) . . ?
C7' C6 C4 110.9(5) . . ?
C7 C6 C4 110.9(5) . . ?
C5 C6 C4 107.9(4) . . ?
C7' C6 H6 107.0 . . ?
C7 C6 H6 107.0 . . ?
C5 C6 H6 108.8 . . ?
C4 C6 H6 109.6 . . ?
O15 C8 O17 128.9(4) . . ?
O15 C8 C9 116.0(4) . . ?
O17 C8 C9 115.0(4) . . ?
O14 C9 O16 125.4(4) . . ?
O14 C9 C8 117.6(4) . . ?
O16 C9 C8 117.0(4) . . ?
O5 C10 O7 126.6(4) . . ?
O5 C10 C11 117.3(4) . . ?
O7 C10 C11 116.1(4) . . ?
O6 C11 O8 125.6(4) . . ?
O6 C11 C10 118.3(4) . . ?
O8 C11 C10 116.1(4) . . ?
O12 C12 O11 126.6(4) . . ?
O12 C12 C13 116.1(4) . . ?
O11 C12 C13 117.3(4) . . ?
O10 C13 O13 127.1(4) . . ?
O10 C13 C12 116.4(4) . . ?
O13 C13 C12 116.5(4) . . ?

_refine_diff_density_max         2.190
_refine_diff_density_min         -1.149
_refine_diff_density_rms         0.133

####################################################################### 
# 
# 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_szg244
_database_code_depnum_ccdc_archive 'CCDC 1503583'
_audit_update_record             
;
2016-09-09 deposited with the CCDC.
2017-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H30 N2 O20 P2 Pr2'
_chemical_formula_weight         938.20

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'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.2863(6)
_cell_length_b                   12.9372(12)
_cell_length_c                   17.0220(15)
_cell_angle_alpha                90.3480(10)
_cell_angle_beta                 98.0560(10)
_cell_angle_gamma                93.4980(10)
_cell_volume                     1368.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2321
_cell_measurement_theta_min      4.834
_cell_measurement_theta_max      57.626

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.278
_exptl_crystal_F_000             920
_exptl_transmission_factor_min   0.663
_exptl_transmission_factor_max   0.896
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    3.733
_shelx_estimated_absorpt_T_min   0.663
_shelx_estimated_absorpt_T_max   0.896
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7748
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.973
_diffrn_reflns_theta_max         26.498
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             5505
_reflns_number_gt                3526
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0325P)²+0.4482P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5505
_refine_ls_number_parameters     397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0332
_refine_ls_wR_factor_ref         0.0820
_refine_ls_wR_factor_gt          0.0706
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Pr1 Pr 0.21816(5) -0.05783(3) 0.42583(2) 0.01078(9) Uani 1 1 d . . . . .
Pr2 Pr 0.22176(5) 0.44143(3) 0.42781(2) 0.01068(9) Uani 1 1 d . . . . .
P1 P -0.2648(3) -0.00575(14) 0.35593(9) 0.0191(4) Uani 1 1 d . . . . .
P2 P 0.6576(3) 0.48590(13) 0.35436(9) 0.0167(4) Uani 1 1 d . . . . .
O1 O -0.1116(7) -0.0749(4) 0.3211(3) 0.0245(11) Uani 1 1 d . . . . .
O2 O -0.1511(7) 0.0226(3) 0.4391(2) 0.0224(10) Uani 1 1 d . . . . .
O3 O -0.4920(6) -0.0487(3) 0.3483(2) 0.0216(10) Uani 1 1 d . . . . .
O4 O -0.7981(9) 0.1340(5) -0.0658(3) 0.0571(18) Uani 1 1 d . . . . .
H4D H -0.7264 0.1900 -0.0723 0.086 Uiso 1 1 d R U . . .
O5 O -1.0377(9) 0.1270(5) 0.0175(3) 0.0469(15) Uani 1 1 d . . . . .
O6 O 0.4545(7) 0.4270(3) 0.3149(2) 0.0218(10) Uani 1 1 d . . . . .
O7 O 0.6144(6) 0.5104(3) 0.4383(2) 0.0189(9) Uani 1 1 d . . . . .
O8 O 0.8646(6) 0.4361(3) 0.3481(2) 0.0213(10) Uani 1 1 d . . . . .
O9 O 0.2203(9) 0.6362(5) -0.0750(3) 0.0470(15) Uani 1 1 d . . . . .
H9E H 0.2905 0.5832 -0.0793 0.071 Uiso 1 1 d R U . . .
O10 O -0.0226(9) 0.6305(5) 0.0076(3) 0.0466(15) Uani 1 1 d . . . . .
O11 O 0.0406(7) -0.3960(3) 0.4768(2) 0.0202(10) Uani 1 1 d . . . . .
O12 O 0.2249(6) -0.3953(3) 0.3448(2) 0.0171(10) Uani 1 1 d . . . . .
O13 O 0.0636(7) -0.2214(3) 0.4799(3) 0.0266(11) Uani 1 1 d . . . . .
O14 O 0.2348(7) -0.2214(3) 0.3449(2) 0.0244(11) Uani 1 1 d . . . . .
O15 O 0.2017(7) 0.1062(3) 0.3447(2) 0.0190(10) Uani 1 1 d . . . . .
O16 O 0.4542(7) 0.1133(3) 0.4842(2) 0.0226(10) Uani 1 1 d . . . . .
O17 O 0.1461(7) 0.2740(3) 0.3556(2) 0.0225(10) Uani 1 1 d . . . . .
O18 O 0.4269(7) 0.2867(4) 0.4900(3) 0.0288(11) Uani 1 1 d . . . . .
O1W O 0.9585(9) 0.5931(5) 0.7909(3) 0.0549(18) Uani 1 1 d . . . . .
H1WA H 1.0858 0.5803 0.8098 0.082 Uiso 1 1 d R U . . .
H1WB H 0.9611 0.6468 0.7627 0.082 Uiso 1 1 d R U . . .
O2W O 0.0639(10) 0.8863(6) 0.2002(3) 0.084(3) Uani 1 1 d . . . . .
H2WC H 0.0763 0.8727 0.1522 0.101 Uiso 1 1 d R U . . .
H2WA H -0.0605 0.9064 0.2030 0.126 Uiso 1 1 d R U . . .
N1 N -0.4678(8) 0.1125(4) 0.2351(3) 0.0190(12) Uani 1 1 d . . . . .
H1C H -0.5859 0.0872 0.2542 0.023 Uiso 1 1 d R U . . .
N2 N 0.5169(8) 0.6135(4) 0.2304(3) 0.0173(12) Uani 1 1 d . . . . .
H2C H 0.3883 0.5939 0.2443 0.021 Uiso 1 1 d R U . . .
C1 C -0.2831(10) 0.1164(5) 0.3017(4) 0.0209(15) Uani 1 1 d . . . . .
H1A H -0.3016 0.1715 0.3384 0.025 Uiso 1 1 d R U . . .
H1B H -0.1508 0.1325 0.2802 0.025 Uiso 1 1 d R U . . .
C2 C -0.5108(11) 0.2182(5) 0.2040(4) 0.0294(18) Uani 1 1 d . . . . .
H2A H -0.3839 0.2471 0.1840 0.035 Uiso 1 1 d R U . . .
H2B H -0.5386 0.2620 0.2473 0.035 Uiso 1 1 d R U . . .
C3 C -0.4247(12) 0.0412(6) 0.1695(4) 0.035(2) Uani 1 1 d . . . . .
H3A H -0.4022 -0.0274 0.1899 0.042 Uiso 1 1 d R U . . .
H3B H -0.2959 0.0665 0.1489 0.042 Uiso 1 1 d R U . . .
C4 C -0.6964(12) 0.2147(6) 0.1378(4) 0.037(2) Uani 1 1 d . . . . .
H4A H -0.7179 0.2837 0.1181 0.044 Uiso 1 1 d R U . . .
H4B H -0.8249 0.1898 0.1587 0.044 Uiso 1 1 d R U . . .
C5 C -0.6134(13) 0.0365(6) 0.1033(4) 0.0359(19) Uani 1 1 d . . . . .
H5A H -0.7398 0.0068 0.1232 0.043 Uiso 1 1 d R U . . .
H5B H -0.5831 -0.0078 0.0606 0.043 Uiso 1 1 d R U . . .
C6 C -0.6584(11) 0.1445(6) 0.0704(4) 0.0272(16) Uani 1 1 d . . . . .
H6 H -0.5335 0.1725 0.0474 0.033 Uiso 1 1 d R U . . .
C7 C -0.8519(14) 0.1346(6) 0.0055(4) 0.038(2) Uani 1 1 d . . . . .
C8 C 0.6800(10) 0.6103(5) 0.3027(3) 0.0199(15) Uani 1 1 d . . . . .
H8A H 0.6613 0.6662 0.3387 0.024 Uiso 1 1 d R U . . .
H8B H 0.8221 0.6203 0.2875 0.024 Uiso 1 1 d R U . . .
C9 C 0.5019(11) 0.7211(5) 0.1968(4) 0.0281(17) Uani 1 1 d . . . . .
H9A H 0.6369 0.7433 0.1793 0.034 Uiso 1 1 d R U . . .
H9B H 0.4747 0.7689 0.2377 0.034 Uiso 1 1 d R U . . .
C10 C 0.5613(11) 0.5408(5) 0.1664(4) 0.0234(16) Uani 1 1 d . . . . .
H10A H 0.5754 0.4723 0.1880 0.028 Uiso 1 1 d R U . . .
H10B H 0.6949 0.5628 0.1477 0.028 Uiso 1 1 d R U . . .
C11 C 0.3214(11) 0.7197(6) 0.1271(4) 0.0306(17) Uani 1 1 d . . . . .
H11A H 0.3140 0.7884 0.1054 0.037 Uiso 1 1 d R U . . .
H11B H 0.1861 0.7013 0.1458 0.037 Uiso 1 1 d R U . . .
C12 C 0.3822(12) 0.5369(6) 0.0965(4) 0.0333(19) Uani 1 1 d . . . . .
H12A H 0.4097 0.4881 0.0563 0.040 Uiso 1 1 d R U . . .
H12B H 0.2494 0.5139 0.1152 0.040 Uiso 1 1 d R U . . .
C13 C 0.3501(11) 0.6454(6) 0.0605(4) 0.0283(17) Uani 1 1 d . . . . .
H13 H 0.4802 0.6669 0.0381 0.034 Uiso 1 1 d R U . . .
C14 C 0.1618(13) 0.6368(6) -0.0035(4) 0.0333(18) Uani 1 1 d . . . . .
C15 C 0.0941(10) -0.3075(5) 0.4510(3) 0.0189(14) Uani 1 1 d . . . . .
C16 C 0.2008(9) -0.3083(5) 0.3736(4) 0.0171(14) Uani 1 1 d . . . . .
C17 C 0.2236(9) 0.1926(5) 0.3797(3) 0.0115(13) Uani 1 1 d . . . . .
C18 C 0.3816(9) 0.1983(5) 0.4593(4) 0.0177(14) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pr1 O3 2.393(4) 1_655 ?
Pr1 O2 2.440(4) 2_556 ?
Pr1 O13 2.509(5) . ?
Pr1 O15 2.538(4) . ?
Pr1 O1 2.535(4) . ?
Pr1 O14 2.534(5) . ?
Pr1 O16 2.532(4) 2_656 ?
Pr1 O2 2.638(4) . ?
Pr1 O16 2.693(5) . ?
Pr1 P1 3.2145(17) . ?
Pr2 O7 2.427(4) 2_666 ?
Pr2 O8 2.452(4) 1_455 ?
Pr2 O17 2.471(4) . ?
Pr2 O11 2.519(4) 2_556 ?
Pr2 O7 2.555(4) . ?
Pr2 O12 2.549(4) 1_565 ?
Pr2 O18 2.598(4) . ?
Pr2 O6 2.585(4) . ?
Pr2 O11 2.637(4) 1_565 ?
Pr2 P2 3.1900(17) . ?
P1 O3 1.489(4) . ?
P1 O1 1.529(4) . ?
P1 O2 1.526(4) . ?
P1 C1 1.837(6) . ?
P2 O8 1.504(4) . ?
P2 O6 1.515(5) . ?
P2 O7 1.526(4) . ?
P2 C8 1.846(6) . ?
O2 Pr1 2.440(4) 2_556 ?
O3 Pr1 2.393(4) 1_455 ?
O4 C7 1.304(8) . ?
O4 H4D 0.8462 . ?
O5 C7 1.212(9) . ?
O7 Pr2 2.427(4) 2_666 ?
O8 Pr2 2.452(4) 1_655 ?
O9 C14 1.319(8) . ?
O9 H9E 0.8463 . ?
O10 C14 1.199(9) . ?
O11 C15 1.272(7) . ?
O11 Pr2 2.519(4) 2_556 ?
O11 Pr2 2.637(4) 1_545 ?
O12 C16 1.252(8) . ?
O12 Pr2 2.549(4) 1_545 ?
O13 C15 1.251(8) . ?
O14 C16 1.247(7) . ?
O15 C17 1.255(7) . ?
O16 C18 1.268(7) . ?
O16 Pr1 2.532(4) 2_656 ?
O17 C17 1.236(6) . ?
O18 C18 1.254(8) . ?
O1W H1WA 0.8462 . ?
O1W H1WB 0.8472 . ?
O2W H2WC 0.8497 . ?
O2W H2WA 0.8462 . ?
N1 C3 1.508(8) . ?
N1 C2 1.496(8) . ?
N1 C1 1.503(7) . ?
N1 H1C 0.8965 . ?
N2 C8 1.490(7) . ?
N2 C9 1.512(8) . ?
N2 C10 1.502(7) . ?
N2 H2C 0.8961 . ?
C1 H1A 0.9677 . ?
C1 H1B 0.9662 . ?
C2 C4 1.503(9) . ?
C2 H2A 0.9659 . ?
C2 H2B 0.9685 . ?
C3 C5 1.516(9) . ?
C3 H3A 0.9660 . ?
C3 H3B 0.9662 . ?
C4 C6 1.512(9) . ?
C4 H4A 0.9658 . ?
C4 H4B 0.9662 . ?
C5 C6 1.536(9) . ?
C5 H5A 0.9661 . ?
C5 H5B 0.9684 . ?
C6 C7 1.523(9) . ?
C6 H6 0.9762 . ?
C8 H8A 0.9678 . ?
C8 H8B 0.9659 . ?
C9 C11 1.522(9) . ?
C9 H9A 0.9660 . ?
C9 H9B 0.9684 . ?
C10 C12 1.517(9) . ?
C10 H10A 0.9659 . ?
C10 H10B 0.9661 . ?
C11 C13 1.518(9) . ?
C11 H11A 0.9659 . ?
C11 H11B 0.9661 . ?
C12 C13 1.549(9) . ?
C12 H12A 0.9683 . ?
C12 H12B 0.9661 . ?
C13 C14 1.490(9) . ?
C13 H13 0.9762 . ?
C15 C16 1.560(8) . ?
C17 C18 1.562(8) . ?

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
O3 Pr1 O2 139.81(15) 1_655 2_556 ?
O3 Pr1 O13 124.79(14) 1_655 . ?
O2 Pr1 O13 71.64(15) 2_556 . ?
O3 Pr1 O15 70.75(14) 1_655 . ?
O2 Pr1 O15 110.64(14) 2_556 . ?
O13 Pr1 O15 154.62(14) . . ?
O3 Pr1 O1 102.76(14) 1_655 . ?
O2 Pr1 O1 115.90(14) 2_556 . ?
O13 Pr1 O1 84.91(15) . . ?
O15 Pr1 O1 71.25(14) . . ?
O3 Pr1 O14 67.21(15) 1_655 . ?
O2 Pr1 O14 134.25(14) 2_556 . ?
O13 Pr1 O14 63.96(14) . . ?
O15 Pr1 O14 114.09(13) . . ?
O1 Pr1 O14 71.47(14) . . ?
O3 Pr1 O16 73.77(14) 1_655 2_656 ?
O2 Pr1 O16 74.19(13) 2_556 2_656 ?
O13 Pr1 O16 79.87(14) . 2_656 ?
O15 Pr1 O16 125.44(14) . 2_656 ?
O1 Pr1 O16 157.95(15) . 2_656 ?
O14 Pr1 O16 87.47(14) . 2_656 ?
O3 Pr1 O2 142.10(13) 1_655 . ?
O2 Pr1 O2 64.13(15) 2_556 . ?
O13 Pr1 O2 86.97(14) . . ?
O15 Pr1 O2 72.60(13) . . ?
O1 Pr1 O2 55.62(13) . . ?
O14 Pr1 O2 121.60(14) . . ?
O16 Pr1 O2 138.32(13) 2_656 . ?
O3 Pr1 O16 77.13(14) 1_655 . ?
O2 Pr1 O16 70.17(14) 2_556 . ?
O13 Pr1 O16 137.08(13) . . ?
O15 Pr1 O16 61.11(13) . . ?
O1 Pr1 O16 129.60(13) . . ?
O14 Pr1 O16 142.58(13) . . ?
O16 Pr1 O16 71.59(15) 2_656 . ?
O2 Pr1 O16 93.46(13) . . ?
O3 Pr1 P1 122.97(10) 1_655 . ?
O2 Pr1 P1 91.06(10) 2_556 . ?
O13 Pr1 P1 87.95(11) . . ?
O15 Pr1 P1 66.91(10) . . ?
O1 Pr1 P1 27.76(10) . . ?
O14 Pr1 P1 97.61(10) . . ?
O16 Pr1 P1 163.19(10) 2_656 . ?
O2 Pr1 P1 28.07(9) . . ?
O16 Pr1 P1 111.44(9) . . ?
O7 Pr2 O8 138.26(14) 2_666 1_455 ?
O7 Pr2 O17 133.43(13) 2_666 . ?
O8 Pr2 O17 69.81(14) 1_455 . ?
O7 Pr2 O11 70.61(13) 2_666 2_556 ?
O8 Pr2 O11 74.57(13) 1_455 2_556 ?
O17 Pr2 O11 93.06(14) . 2_556 ?
O7 Pr2 O7 65.93(15) 2_666 . ?
O8 Pr2 O7 145.77(13) 1_455 . ?
O17 Pr2 O7 113.61(14) . . ?
O11 Pr2 O7 136.33(13) 2_556 . ?
O7 Pr2 O12 107.35(14) 2_666 1_565 ?
O8 Pr2 O12 75.22(14) 1_455 1_565 ?
O17 Pr2 O12 117.17(13) . 1_565 ?
O11 Pr2 O12 125.33(12) 2_556 1_565 ?
O7 Pr2 O12 73.45(13) . 1_565 ?
O7 Pr2 O18 71.23(14) 2_666 . ?
O8 Pr2 O18 127.75(15) 1_455 . ?
O17 Pr2 O18 63.89(14) . . ?
O11 Pr2 O18 84.84(13) 2_556 . ?
O7 Pr2 O18 77.69(14) . . ?
O12 Pr2 O18 148.41(14) 1_565 . ?
O7 Pr2 O6 120.80(14) 2_666 . ?
O8 Pr2 O6 99.17(13) 1_455 . ?
O17 Pr2 O6 68.37(14) . . ?
O11 Pr2 O6 161.36(15) 2_556 . ?
O7 Pr2 O6 56.06(13) . . ?
O12 Pr2 O6 67.89(13) 1_565 . ?
O18 Pr2 O6 85.50(13) . . ?
O7 Pr2 O11 70.27(13) 2_666 1_565 ?
O8 Pr2 O11 75.43(14) 1_455 1_565 ?
O17 Pr2 O11 143.56(14) . 1_565 ?
O11 Pr2 O11 66.95(15) 2_556 1_565 ?
O7 Pr2 O11 101.18(13) . 1_565 ?
O12 Pr2 O11 61.91(13) 1_565 1_565 ?
O18 Pr2 O11 137.94(13) . 1_565 ?
O6 Pr2 O11 129.26(13) . 1_565 ?
O7 Pr2 P2 93.75(10) 2_666 . ?
O8 Pr2 P2 123.08(10) 1_455 . ?
O17 Pr2 P2 91.87(11) . . ?
O11 Pr2 P2 162.24(10) 2_556 . ?
O7 Pr2 P2 28.14(9) . . ?
O12 Pr2 P2 66.45(9) 1_565 . ?
O18 Pr2 P2 82.04(11) . . ?
O6 Pr2 P2 28.00(10) . . ?
O11 Pr2 P2 116.63(10) 1_565 . ?
O3 P1 O1 114.7(3) . . ?
O3 P1 O2 117.6(2) . . ?
O1 P1 O2 104.5(2) . . ?
O3 P1 C1 103.7(3) . . ?
O1 P1 C1 110.0(3) . . ?
O2 P1 C1 106.0(3) . . ?
O3 P1 Pr1 142.10(19) . . ?
O1 P1 Pr1 50.57(17) . . ?
O2 P1 Pr1 54.48(16) . . ?
C1 P1 Pr1 114.1(2) . . ?
O8 P2 O6 115.7(3) . . ?
O8 P2 O7 116.0(2) . . ?
O6 P2 O7 105.1(2) . . ?
O8 P2 C8 105.1(3) . . ?
O6 P2 C8 107.2(3) . . ?
O7 P2 C8 107.2(3) . . ?
O8 P2 Pr2 139.66(19) . . ?
O6 P2 Pr2 53.22(16) . . ?
O7 P2 Pr2 52.12(16) . . ?
C8 P2 Pr2 115.3(2) . . ?
P1 O1 Pr1 101.7(2) . . ?
P1 O2 Pr1 142.5(2) . 2_556 ?
P1 O2 Pr1 97.45(19) . . ?
Pr1 O2 Pr1 115.87(15) 2_556 . ?
P1 O3 Pr1 138.3(3) . 1_455 ?
C7 O4 H4D 108.7 . . ?
P2 O6 Pr2 98.8(2) . . ?
P2 O7 Pr2 145.0(2) . 2_666 ?
P2 O7 Pr2 99.7(2) . . ?
Pr2 O7 Pr2 114.07(15) 2_666 . ?
P2 O8 Pr2 135.0(3) . 1_655 ?
C14 O9 H9E 108.1 . . ?
C15 O11 Pr2 128.7(4) . 2_556 ?
C15 O11 Pr2 118.2(4) . 1_545 ?
Pr2 O11 Pr2 113.04(15) 2_556 1_545 ?
C16 O12 Pr2 121.6(4) . 1_545 ?
C15 O13 Pr1 120.3(4) . . ?
C16 O14 Pr1 120.7(4) . . ?
C17 O15 Pr1 119.3(4) . . ?
C18 O16 Pr1 136.4(4) . 2_656 ?
C18 O16 Pr1 115.1(4) . . ?
Pr1 O16 Pr1 108.41(15) 2_656 . ?
C17 O17 Pr2 123.5(4) . . ?
C18 O18 Pr2 118.6(4) . . ?
H1WA O1W H1WB 109.5 . . ?
H2WC O2W H2WA 109.8 . . ?
C3 N1 C2 110.7(5) . . ?
C3 N1 C1 110.4(5) . . ?
C2 N1 C1 111.4(5) . . ?
C3 N1 H1C 108.5 . . ?
C2 N1 H1C 107.8 . . ?
C1 N1 H1C 108.0 . . ?
C8 N2 C9 112.3(5) . . ?
C8 N2 C10 112.1(5) . . ?
C9 N2 C10 108.6(5) . . ?
C8 N2 H2C 107.7 . . ?
C9 N2 H2C 107.6 . . ?
C10 N2 H2C 108.3 . . ?
N1 C1 P1 112.4(4) . . ?
N1 C1 H1A 108.9 . . ?
P1 C1 H1A 108.8 . . ?
N1 C1 H1B 108.9 . . ?
P1 C1 H1B 109.7 . . ?
H1A C1 H1B 108.1 . . ?
N1 C2 C4 111.6(6) . . ?
N1 C2 H2A 108.8 . . ?
C4 C2 H2A 108.6 . . ?
N1 C2 H2B 108.8 . . ?
C4 C2 H2B 110.7 . . ?
H2A C2 H2B 108.3 . . ?
N1 C3 C5 109.9(5) . . ?
N1 C3 H3A 109.9 . . ?
C5 C3 H3A 109.8 . . ?
N1 C3 H3B 109.6 . . ?
C5 C3 H3B 109.4 . . ?
H3A C3 H3B 108.2 . . ?
C2 C4 C6 111.5(6) . . ?
C2 C4 H4A 109.6 . . ?
C6 C4 H4A 109.5 . . ?
C2 C4 H4B 108.4 . . ?
C6 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
C3 C5 C6 111.5(6) . . ?
C3 C5 H5A 109.2 . . ?
C6 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C6 C5 H5B 109.0 . . ?
H5A C5 H5B 108.1 . . ?
C7 C6 C5 108.8(6) . . ?
C7 C6 C4 112.0(6) . . ?
C5 C6 C4 108.9(6) . . ?
C7 C6 H6 108.8 . . ?
C5 C6 H6 109.2 . . ?
C4 C6 H6 109.2 . . ?
O5 C7 O4 122.5(7) . . ?
O5 C7 C6 124.5(7) . . ?
O4 C7 C6 113.0(7) . . ?
N2 C8 P2 111.6(4) . . ?
N2 C8 H8A 109.7 . . ?
P2 C8 H8A 109.1 . . ?
N2 C8 H8B 109.0 . . ?
P2 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
N2 C9 C11 109.3(6) . . ?
N2 C9 H9A 109.5 . . ?
C11 C9 H9A 109.8 . . ?
N2 C9 H9B 109.5 . . ?
C11 C9 H9B 110.4 . . ?
H9A C9 H9B 108.4 . . ?
N2 C10 C12 111.5(5) . . ?
N2 C10 H10A 109.0 . . ?
C12 C10 H10A 109.4 . . ?
N2 C10 H10B 110.1 . . ?
C12 C10 H10B 108.6 . . ?
H10A C10 H10B 108.3 . . ?
C9 C11 C13 113.9(6) . . ?
C9 C11 H11A 108.9 . . ?
C13 C11 H11A 107.9 . . ?
C9 C11 H11B 109.1 . . ?
C13 C11 H11B 108.9 . . ?
H11A C11 H11B 108.0 . . ?
C10 C12 C13 111.5(6) . . ?
C10 C12 H12A 111.0 . . ?
C13 C12 H12A 110.5 . . ?
C10 C12 H12B 108.4 . . ?
C13 C12 H12B 107.3 . . ?
H12A C12 H12B 108.1 . . ?
C12 C13 C14 108.4(6) . . ?
C12 C13 C11 108.0(5) . . ?
C14 C13 C11 113.2(6) . . ?
C12 C13 H13 107.6 . . ?
C14 C13 H13 109.9 . . ?
C11 C13 H13 109.6 . . ?
O10 C14 O9 123.1(7) . . ?
O10 C14 C13 124.6(7) . . ?
O9 C14 C13 112.3(7) . . ?
O13 C15 O11 126.6(6) . . ?
O13 C15 C16 117.7(6) . . ?
O11 C15 C16 115.6(6) . . ?
O14 C16 O12 128.1(6) . . ?
O14 C16 C15 115.1(6) . . ?
O12 C16 C15 116.5(6) . . ?
O17 C17 O15 127.2(6) . . ?
O17 C17 C18 117.2(5) . . ?
O15 C17 C18 115.4(5) . . ?
O18 C18 O16 127.5(6) . . ?
O18 C18 C17 116.3(5) . . ?
O16 C18 C17 116.2(6) . . ?

_refine_diff_density_max         0.996
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.151

