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

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

data_prdtpaaq
_database_code_depnum_ccdc_archive 'CCDC 1033642'
_audit_update_record             
;
2015-05-22 deposited with the CCDC.
2015-12-02 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C32 H34 N7 O9 Pr'
_chemical_formula_sum            'C32 H34 N7 O9 Pr'

_chemical_formula_weight         801.57

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.085(5)
_cell_length_b                   11.118(5)
_cell_length_c                   18.036(5)
_cell_angle_alpha                98.989(5)
_cell_angle_beta                 93.383(5)
_cell_angle_gamma                96.356(5)
_cell_volume                     1979.2(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             812
_exptl_absorpt_coefficient_mu    1.285
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7831
_exptl_absorpt_correction_T_max  0.8610
_exptl_absorpt_process_details   SADABS(Sheldrick,1997)

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 0.5
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7688
_diffrn_reflns_av_R_equivalents  0.0917
_diffrn_reflns_av_sigmaI/netI    0.1731
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5998
_reflns_number_gt                4293
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX II V2012.4-3'
_computing_cell_refinement       'Bruker APEX II V2012.4-3'
_computing_data_reduction        'Bruker APEX II V2012.4-3'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1711P)²+6.1209P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5998
_refine_ls_number_parameters     440
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1469
_refine_ls_R_factor_gt           0.1091
_refine_ls_wR_factor_ref         0.2886
_refine_ls_wR_factor_gt          0.2624
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.74863(7) 0.84225(7) 0.26943(4) 0.0315(3) Uani 1 1 d . . .
C1 C 1.0204(13) 0.7149(15) 0.2158(8) 0.043(4) Uani 1 1 d . . .
C2 C 1.0554(15) 0.7371(19) 0.3004(9) 0.057(5) Uani 1 1 d . . .
H2A H 1.1122 0.6771 0.3130 0.069 Uiso 1 1 calc R . .
H2B H 1.1052 0.8180 0.3154 0.069 Uiso 1 1 calc R . .
C3 C 0.9537(16) 0.7948(18) 0.4206(8) 0.056(5) Uani 1 1 d . . .
H3A H 1.0122 0.7535 0.4501 0.067 Uiso 1 1 calc R . .
H3B H 0.9969 0.8774 0.4211 0.067 Uiso 1 1 calc R . .
C4 C 0.8288(17) 0.8014(17) 0.4552(8) 0.058(5) Uani 1 1 d . . .
H4B H 0.8478 0.8399 0.5074 0.069 Uiso 1 1 calc R . .
H4A H 0.7864 0.7185 0.4548 0.069 Uiso 1 1 calc R . .
C5 C 0.754(2) 1.0008(18) 0.4514(9) 0.069(6) Uani 1 1 d . . .
H5A H 0.7272 1.0097 0.5025 0.083 Uiso 1 1 calc R . .
H5B H 0.8491 1.0292 0.4542 0.083 Uiso 1 1 calc R . .
C6 C 0.6822(18) 1.0818(17) 0.4107(7) 0.057(5) Uani 1 1 d . . .
H6A H 0.6973 1.1643 0.4391 0.069 Uiso 1 1 calc R . .
H6B H 0.5870 1.0546 0.4080 0.069 Uiso 1 1 calc R . .
C7 C 0.6195(18) 1.1259(16) 0.2863(9) 0.053(4) Uani 1 1 d . . .
H7A H 0.6222 1.2144 0.2978 0.063 Uiso 1 1 calc R . .
H7B H 0.5322 1.0888 0.2964 0.063 Uiso 1 1 calc R . .
C8 C 0.6451(14) 1.0870(13) 0.2042(8) 0.037(3) Uani 1 1 d . . .
C9 C 0.8866(19) 0.5984(15) 0.3386(10) 0.064(5) Uani 1 1 d . . .
H9A H 0.8971 0.5786 0.3889 0.076 Uiso 1 1 calc R . .
H9B H 0.9421 0.5493 0.3072 0.076 Uiso 1 1 calc R . .
C10 C 0.7397(17) 0.5613(17) 0.3081(9) 0.052(4) Uani 1 1 d . . .
C11 C 0.5886(17) 0.826(2) 0.4317(8) 0.068(6) Uani 1 1 d . . .
H11B H 0.5802 0.7385 0.4340 0.082 Uiso 1 1 calc R . .
H11A H 0.5673 0.8677 0.4800 0.082 Uiso 1 1 calc R . .
C12 C 0.4873(15) 0.8478(19) 0.3710(10) 0.059(5) Uani 1 1 d . . .
C13 C 0.8479(18) 1.1624(17) 0.3322(10) 0.062(5) Uani 1 1 d . . .
H13B H 0.8594 1.2216 0.3784 0.074 Uiso 1 1 calc R . .
H13A H 0.8419 1.2076 0.2906 0.074 Uiso 1 1 calc R . .
C14 C 0.9695(18) 1.096(2) 0.3264(10) 0.062(5) Uani 1 1 d . . .
C15 C 0.6266(14) 1.1312(12) 0.0761(8) 0.039(3) Uani 1 1 d . . .
C16 C 0.7273(13) 1.0737(13) 0.0466(8) 0.037(3) Uani 1 1 d . . .
H16 H 0.7893 1.0460 0.0781 0.045 Uiso 1 1 calc R . .
C17 C 0.7388(14) 1.0552(13) -0.0324(8) 0.038(3) Uani 1 1 d . . .
C18 C 0.836(2) 0.9955(17) -0.0682(9) 0.062(5) Uani 1 1 d . . .
H18 H 0.8985 0.9611 -0.0404 0.075 Uiso 1 1 calc R . .
C19 C 0.842(2) 0.987(2) -0.1447(10) 0.080(6) Uani 1 1 d . . .
H19 H 0.9109 0.9503 -0.1675 0.097 Uiso 1 1 calc R . .
C20 C 0.748(3) 1.0311(19) -0.1888(10) 0.080(6) Uani 1 1 d . . .
H20 H 0.7517 1.0225 -0.2408 0.096 Uiso 1 1 calc R . .
C21 C 0.6531(16) 1.0867(17) -0.1542(8) 0.051(4) Uani 1 1 d . . .
H21 H 0.5883 1.1150 -0.1837 0.061 Uiso 1 1 calc R . .
C22 C 0.6448(14) 1.1048(13) -0.0762(8) 0.043(4) Uani 1 1 d . . .
C23 C 0.5336(14) 1.1741(15) 0.0277(8) 0.043(3) Uani 1 1 d . . .
H23 H 0.4641 1.2128 0.0487 0.052 Uiso 1 1 calc R . .
C24 C 1.0942(14) 0.6602(13) 0.0914(9) 0.042(3) Uani 1 1 d . . .
C25 C 0.9849(16) 0.6808(13) 0.0501(8) 0.045(4) Uani 1 1 d . . .
H25 H 0.9104 0.7060 0.0732 0.054 Uiso 1 1 calc R . .
C26 C 0.9875(17) 0.6625(15) -0.0300(9) 0.050(4) Uani 1 1 d . . .
C27 C 0.8850(19) 0.6856(17) -0.0782(10) 0.061(5) Uani 1 1 d . . .
H27 H 0.8088 0.7126 -0.0579 0.074 Uiso 1 1 calc R . .
C28 C 0.891(2) 0.6710(14) -0.1514(10) 0.068(5) Uani 1 1 d . . .
H28 H 0.8174 0.6822 -0.1820 0.081 Uiso 1 1 calc R . .
C29 C 1.012(3) 0.6373(19) -0.1853(11) 0.083(7) Uani 1 1 d . . .
H29 H 1.0170 0.6293 -0.2371 0.100 Uiso 1 1 calc R . .
C30 C 1.113(2) 0.6185(19) -0.1427(12) 0.071(6) Uani 1 1 d . . .
H30 H 1.1912 0.5978 -0.1640 0.085 Uiso 1 1 calc R . .
C31 C 1.1052(16) 0.6299(15) -0.0614(8) 0.051(4) Uani 1 1 d . . .
C32 C 1.2069(14) 0.6191(14) 0.0551(9) 0.047(4) Uani 1 1 d . . .
H32 H 1.2792 0.6025 0.0847 0.057 Uiso 1 1 calc R . .
N1 N 0.9361(13) 0.7285(12) 0.3415(6) 0.044(3) Uani 1 1 d . . .
N2 N 0.7343(11) 0.8690(13) 0.4191(5) 0.043(3) Uani 1 1 d . . .
N3 N 0.7240(12) 1.0848(10) 0.3317(6) 0.039(3) Uani 1 1 d . . .
N4 N 0.6046(11) 1.1543(11) 0.1542(6) 0.039(3) Uani 1 1 d . . .
H4 H 0.5627 1.2154 0.1699 0.047 Uiso 1 1 calc R . .
N5 N 1.1076(12) 0.6724(11) 0.1711(6) 0.041(3) Uani 1 1 d . . .
H5 H 1.1783 0.6502 0.1914 0.049 Uiso 1 1 calc R . .
N6 N 0.5408(12) 1.1619(12) -0.0457(7) 0.049(3) Uani 1 1 d . . .
N7 N 1.2132(12) 0.6036(13) -0.0180(8) 0.055(4) Uani 1 1 d . . .
O1 O 0.9137(11) 0.7427(9) 0.1935(6) 0.052(3) Uani 1 1 d . . .
O4 O 0.5274(18) 0.8523(17) 0.3059(10) 0.107(5) Uani 1 1 d . . .
O5 O 0.9509(11) 0.9816(11) 0.3047(6) 0.057(3) Uani 1 1 d . . .
O6 O 0.6294(11) 0.7407(10) 0.1450(6) 0.051(3) Uani 1 1 d . . .
O7 O 0.7029(17) 0.4513(12) 0.3033(11) 0.100(5) Uani 1 1 d . . .
O8 O 1.0802(13) 1.1557(16) 0.3379(11) 0.103(6) Uani 1 1 d . . .
O9 O 0.3694(14) 0.840(2) 0.3868(7) 0.106(6) Uani 1 1 d . . .
O2 O 0.7117(16) 0.9919(15) 0.1905(9) 0.050(4) Uiso 0.70 1 d P . .
O2A O 0.752(4) 0.977(4) 0.220(2) 0.050(9) Uiso 0.30 1 d P . .
O3 O 0.7366(16) 0.7063(15) 0.3135(8) 0.050(4) Uiso 0.70 1 d P . .
O3A O 0.676(4) 0.644(4) 0.287(2) 0.050(8) Uiso 0.30 1 d P . .


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

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 1.810(16) . ?
Pr1 O2A 1.85(4) . ?
Pr1 O3A 2.32(4) . ?
Pr1 O4 2.372(19) . ?
Pr1 O2 2.397(18) . ?
Pr1 O5 2.409(12) . ?
Pr1 O1 2.464(9) . ?
Pr1 O6 2.520(10) . ?
Pr1 N2 2.683(9) . ?
Pr1 N1 2.760(12) . ?
Pr1 N3 2.798(11) . ?
C1 O1 1.215(17) . ?
C1 N5 1.304(17) . ?
C1 C2 1.52(2) . ?
C2 N1 1.45(2) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.44(2) . ?
C3 N1 1.490(17) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N2 1.46(2) . ?
C4 H4B 0.9700 . ?
C4 H4A 0.9700 . ?
C5 C6 1.47(2) . ?
C5 N2 1.48(2) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N3 1.514(19) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N3 1.454(19) . ?
C7 C8 1.52(2) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 O2 1.31(2) . ?
C8 N4 1.332(17) . ?
C8 O2A 1.76(4) . ?
C9 N1 1.47(2) . ?
C9 C10 1.54(2) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 O7 1.23(2) . ?
C10 O3A 1.27(4) . ?
C10 O3 1.60(2) . ?
C11 C12 1.52(2) . ?
C11 N2 1.54(2) . ?
C11 H11B 0.9700 . ?
C11 H11A 0.9700 . ?
C12 O9 1.24(2) . ?
C12 O4 1.27(2) . ?
C13 N3 1.44(2) . ?
C13 C14 1.50(3) . ?
C13 H13B 0.9700 . ?
C13 H13A 0.9700 . ?
C14 O8 1.22(2) . ?
C14 O5 1.27(2) . ?
C15 C16 1.35(2) . ?
C15 C23 1.42(2) . ?
C15 N4 1.426(19) . ?
C16 C17 1.421(19) . ?
C16 H16 0.9300 . ?
C17 C18 1.38(2) . ?
C17 C22 1.411(19) . ?
C18 C19 1.37(2) . ?
C18 H18 0.9300 . ?
C19 C20 1.38(3) . ?
C19 H19 0.9300 . ?
C20 C21 1.33(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.40(2) . ?
C21 H21 0.9300 . ?
C22 N6 1.38(2) . ?
C23 N6 1.317(19) . ?
C23 H23 0.9300 . ?
C24 C25 1.35(2) . ?
C24 N5 1.420(19) . ?
C24 C32 1.428(19) . ?
C25 C26 1.43(2) . ?
C25 H25 0.9300 . ?
C26 C27 1.38(2) . ?
C26 C31 1.40(2) . ?
C27 C28 1.31(2) . ?
C27 H27 0.9300 . ?
C28 C29 1.46(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.29(3) . ?
C29 H29 0.9300 . ?
C30 C31 1.46(3) . ?
C30 H30 0.9300 . ?
C31 N7 1.39(2) . ?
C32 N7 1.31(2) . ?
C32 H32 0.9300 . ?
N4 H4 0.8600 . ?
N5 H5 0.8600 . ?
O2 O2A 0.71(4) . ?
O3 O3A 0.92(4) . ?
# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.017 0.500 0.483 485.5 -6.0
_platon_squeeze_details          
; ?
;

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 O2A 176.5(13) . . ?
O3 Pr1 O3A 21.5(9) . . ?
O2A Pr1 O3A 155.1(15) . . ?
O3 Pr1 O4 83.3(7) . . ?
O2A Pr1 O4 94.9(13) . . ?
O3A Pr1 O4 75.6(10) . . ?
O3 Pr1 O2 164.2(6) . . ?
O2A Pr1 O2 12.3(12) . . ?
O3A Pr1 O2 142.8(10) . . ?
O4 Pr1 O2 88.2(6) . . ?
O3 Pr1 O5 115.2(6) . . ?
O2A Pr1 O5 68.2(13) . . ?
O3A Pr1 O5 135.0(9) . . ?
O4 Pr1 O5 131.2(5) . . ?
O2 Pr1 O5 80.4(5) . . ?
O3 Pr1 O1 85.2(5) . . ?
O2A Pr1 O1 95.1(12) . . ?
O3A Pr1 O1 84.2(9) . . ?
O4 Pr1 O1 151.5(5) . . ?
O2 Pr1 O1 96.3(5) . . ?
O5 Pr1 O1 77.2(4) . . ?
O3 Pr1 O6 96.3(6) . . ?
O2A Pr1 O6 80.6(12) . . ?
O3A Pr1 O6 75.4(9) . . ?
O4 Pr1 O6 83.0(5) . . ?
O2 Pr1 O6 69.4(5) . . ?
O5 Pr1 O6 133.7(4) . . ?
O1 Pr1 O6 72.4(4) . . ?
O3 Pr1 N2 61.5(6) . . ?
O2A Pr1 N2 120.5(12) . . ?
O3A Pr1 N2 77.5(9) . . ?
O4 Pr1 N2 67.0(5) . . ?
O2 Pr1 N2 126.7(5) . . ?
O5 Pr1 N2 82.6(4) . . ?
O1 Pr1 N2 128.1(4) . . ?
O6 Pr1 N2 143.7(4) . . ?
O3 Pr1 N1 47.1(6) . . ?
O2A Pr1 N1 135.9(12) . . ?
O3A Pr1 N1 65.0(9) . . ?
O4 Pr1 N1 123.7(5) . . ?
O2 Pr1 N1 146.1(5) . . ?
O5 Pr1 N1 70.1(4) . . ?
O1 Pr1 N1 61.8(4) . . ?
O6 Pr1 N1 120.9(3) . . ?
N2 Pr1 N1 66.4(3) . . ?
O3 Pr1 N3 129.3(5) . . ?
O2A Pr1 N3 52.4(11) . . ?
O3A Pr1 N3 139.4(9) . . ?
O4 Pr1 N3 71.4(5) . . ?
O2 Pr1 N3 59.1(4) . . ?
O5 Pr1 N3 62.1(4) . . ?
O1 Pr1 N3 134.4(3) . . ?
O6 Pr1 N3 122.1(3) . . ?
N2 Pr1 N3 68.3(4) . . ?
N1 Pr1 N3 116.5(3) . . ?
O1 C1 N5 123.6(13) . . ?
O1 C1 C2 117.4(12) . . ?
N5 C1 C2 118.9(12) . . ?
N1 C2 C1 111.4(12) . . ?
N1 C2 H2A 109.3 . . ?
C1 C2 H2A 109.3 . . ?
N1 C2 H2B 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
C4 C3 N1 112.8(13) . . ?
C4 C3 H3A 109.0 . . ?
N1 C3 H3A 109.0 . . ?
C4 C3 H3B 109.0 . . ?
N1 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
C3 C4 N2 114.7(14) . . ?
C3 C4 H4B 108.6 . . ?
N2 C4 H4B 108.6 . . ?
C3 C4 H4A 108.6 . . ?
N2 C4 H4A 108.6 . . ?
H4B C4 H4A 107.6 . . ?
C6 C5 N2 116.3(13) . . ?
C6 C5 H5A 108.2 . . ?
N2 C5 H5A 108.2 . . ?
C6 C5 H5B 108.2 . . ?
N2 C5 H5B 108.2 . . ?
H5A C5 H5B 107.4 . . ?
C5 C6 N3 113.6(13) . . ?
C5 C6 H6A 108.8 . . ?
N3 C6 H6A 108.8 . . ?
C5 C6 H6B 108.8 . . ?
N3 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
N3 C7 C8 107.1(12) . . ?
N3 C7 H7A 110.3 . . ?
C8 C7 H7A 110.3 . . ?
N3 C7 H7B 110.3 . . ?
C8 C7 H7B 110.3 . . ?
H7A C7 H7B 108.5 . . ?
O2 C8 N4 126.2(14) . . ?
O2 C8 C7 115.5(13) . . ?
N4 C8 C7 118.2(11) . . ?
O2 C8 O2A 20.7(13) . . ?
N4 C8 O2A 144.1(17) . . ?
C7 C8 O2A 96.2(15) . . ?
N1 C9 C10 115.1(12) . . ?
N1 C9 H9A 108.5 . . ?
C10 C9 H9A 108.5 . . ?
N1 C9 H9B 108.5 . . ?
C10 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
O7 C10 O3A 129(2) . . ?
O7 C10 C9 113.6(15) . . ?
O3A C10 C9 118(2) . . ?
O7 C10 O3 161.5(17) . . ?
O3A C10 O3 35.1(18) . . ?
C9 C10 O3 84.0(12) . . ?
C12 C11 N2 113.8(13) . . ?
C12 C11 H11B 108.8 . . ?
N2 C11 H11B 108.8 . . ?
C12 C11 H11A 108.8 . . ?
N2 C11 H11A 108.8 . . ?
H11B C11 H11A 107.7 . . ?
O9 C12 O4 125.8(17) . . ?
O9 C12 C11 115.7(17) . . ?
O4 C12 C11 117.4(14) . . ?
N3 C13 C14 114.9(16) . . ?
N3 C13 H13B 108.5 . . ?
C14 C13 H13B 108.5 . . ?
N3 C13 H13A 108.5 . . ?
C14 C13 H13A 108.5 . . ?
H13B C13 H13A 107.5 . . ?
O8 C14 O5 123.5(18) . . ?
O8 C14 C13 119.2(19) . . ?
O5 C14 C13 117.2(16) . . ?
C16 C15 C23 119.3(13) . . ?
C16 C15 N4 125.3(12) . . ?
C23 C15 N4 115.3(12) . . ?
C15 C16 C17 120.4(13) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C18 C17 C22 118.7(14) . . ?
C18 C17 C16 124.7(13) . . ?
C22 C17 C16 116.5(13) . . ?
C19 C18 C17 120.0(17) . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C19 C20 122(2) . . ?
C18 C19 H19 118.9 . . ?
C20 C19 H19 118.9 . . ?
C21 C20 C19 117.5(16) . . ?
C21 C20 H20 121.2 . . ?
C19 C20 H20 121.2 . . ?
C20 C21 C22 123.8(15) . . ?
C20 C21 H21 118.1 . . ?
C22 C21 H21 118.1 . . ?
N6 C22 C21 119.5(13) . . ?
N6 C22 C17 122.7(14) . . ?
C21 C22 C17 117.6(14) . . ?
N6 C23 C15 123.0(12) . . ?
N6 C23 H23 118.5 . . ?
C15 C23 H23 118.5 . . ?
C25 C24 N5 125.3(12) . . ?
C25 C24 C32 120.3(14) . . ?
N5 C24 C32 114.3(13) . . ?
C24 C25 C26 118.1(13) . . ?
C24 C25 H25 121.0 . . ?
C26 C25 H25 121.0 . . ?
C27 C26 C31 117.7(15) . . ?
C27 C26 C25 123.7(14) . . ?
C31 C26 C25 118.3(15) . . ?
C28 C27 C26 122.7(18) . . ?
C28 C27 H27 118.7 . . ?
C26 C27 H27 118.7 . . ?
C27 C28 C29 120.5(19) . . ?
C27 C28 H28 119.8 . . ?
C29 C28 H28 119.8 . . ?
C30 C29 C28 119.6(17) . . ?
C30 C29 H29 120.2 . . ?
C28 C29 H29 120.2 . . ?
C29 C30 C31 120.1(18) . . ?
C29 C30 H30 120.0 . . ?
C31 C30 H30 120.0 . . ?
N7 C31 C26 122.1(14) . . ?
N7 C31 C30 118.4(14) . . ?
C26 C31 C30 119.4(16) . . ?
N7 C32 C24 123.0(14) . . ?
N7 C32 H32 118.5 . . ?
C24 C32 H32 118.5 . . ?
C2 N1 C9 108.8(13) . . ?
C2 N1 C3 114.7(13) . . ?
C9 N1 C3 111.2(13) . . ?
C2 N1 Pr1 106.8(9) . . ?
C9 N1 Pr1 109.8(9) . . ?
C3 N1 Pr1 105.3(9) . . ?
C4 N2 C5 111.4(12) . . ?
C4 N2 C11 111.9(13) . . ?
C5 N2 C11 104.8(14) . . ?
C4 N2 Pr1 112.4(8) . . ?
C5 N2 Pr1 109.5(10) . . ?
C11 N2 Pr1 106.3(8) . . ?
C13 N3 C7 110.3(13) . . ?
C13 N3 C6 111.5(12) . . ?
C7 N3 C6 110.1(12) . . ?
C13 N3 Pr1 111.0(9) . . ?
C7 N3 Pr1 107.5(9) . . ?
C6 N3 Pr1 106.3(9) . . ?
C8 N4 C15 124.1(11) . . ?
C8 N4 H4 118.0 . . ?
C15 N4 H4 118.0 . . ?
C1 N5 C24 124.7(12) . . ?
C1 N5 H5 117.6 . . ?
C24 N5 H5 117.6 . . ?
C23 N6 C22 117.9(12) . . ?
C32 N7 C31 117.8(12) . . ?
C1 O1 Pr1 127.5(10) . . ?
C12 O4 Pr1 127.1(13) . . ?
C14 O5 Pr1 131.4(11) . . ?
O2A O2 C8 118(4) . . ?
O2A O2 Pr1 34(4) . . ?
C8 O2 Pr1 128.1(12) . . ?
O2 O2A C8 41(3) . . ?
O2 O2A Pr1 134(4) . . ?
C8 O2A Pr1 137(2) . . ?
O3A O3 C10 52(2) . . ?
O3A O3 Pr1 112(3) . . ?
C10 O3 Pr1 150.0(11) . . ?
O3 O3A C10 93(3) . . ?
O3 O3A Pr1 46(2) . . ?
C10 O3A Pr1 131(3) . . ?

_diffrn_measured_fraction_theta_max 0.863
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.863
_refine_diff_density_max         3.716
_refine_diff_density_min         -2.168
_refine_diff_density_rms         0.211
####################################################################### 
# 
# 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_eudtpaaq
_database_code_depnum_ccdc_archive 'CCDC 1033643'
_audit_update_record             
;
2015-05-22 deposited with the CCDC.
2015-12-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C35 H41 Eu N8 O13'
_chemical_formula_sum            'C35 H41 Eu N8 O13'
_chemical_formula_weight         933.72

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/n

loop_
_symmetry_equiv_pos_as_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                   11.132(2)
_cell_length_b                   23.789(5)
_cell_length_c                   17.045(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.57(3)
_cell_angle_gamma                90.00
_cell_volume                     4279.0(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1896
_exptl_absorpt_coefficient_mu    1.534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7290
_exptl_absorpt_correction_T_max  0.7698
_exptl_absorpt_process_details   SADABS(Sheldrick,1997)

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 0.5
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            31403
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         25.49
_reflns_number_total             7968
_reflns_number_gt                6030
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX II V2012.4-3'
_computing_cell_refinement       'Bruker APEX II V2012.4-3'
_computing_data_reduction        'Bruker APEX II V2012.4-3'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1321P)²+1.7078P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7968
_refine_ls_number_parameters     514
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0548
_refine_ls_wR_factor_ref         0.1961
_refine_ls_wR_factor_gt          0.1746
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.033
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1106(6) 0.1579(3) -0.1155(4) 0.0515(16) Uani 1 1 d . . .
C2 C 0.0931(7) 0.2093(3) -0.1697(4) 0.0591(18) Uani 1 1 d . . .
H2A H 0.1547 0.2093 -0.1991 0.071 Uiso 1 1 calc R . .
H2B H 0.0089 0.2093 -0.2100 0.071 Uiso 1 1 calc R . .
C3 C 0.1382(7) 0.3096(3) -0.1583(4) 0.0570(17) Uani 1 1 d . . .
H3A H 0.0641 0.3196 -0.2044 0.068 Uiso 1 1 calc R . .
H3B H 0.2070 0.3014 -0.1800 0.068 Uiso 1 1 calc R . .
C4 C 0.1747(7) 0.3582(3) -0.0985(4) 0.0615(19) Uani 1 1 d . . .
H4A H 0.1859 0.3916 -0.1282 0.074 Uiso 1 1 calc R . .
H4B H 0.1061 0.3656 -0.0763 0.074 Uiso 1 1 calc R . .
C5 C 0.4012(7) 0.3641(3) -0.0558(5) 0.073(2) Uani 1 1 d . . .
H5A H 0.3985 0.4044 -0.0649 0.087 Uiso 1 1 calc R . .
H5B H 0.3930 0.3459 -0.1081 0.087 Uiso 1 1 calc R . .
C6 C 0.5289(7) 0.3485(3) 0.0067(6) 0.078(2) Uani 1 1 d . . .
H6A H 0.5968 0.3650 -0.0098 0.093 Uiso 1 1 calc R . .
H6B H 0.5343 0.3632 0.0608 0.093 Uiso 1 1 calc R . .
C7 C 0.6384(7) 0.2693(3) 0.0866(6) 0.064(2) Uani 1 1 d . . .
H7A H 0.6283 0.2897 0.1334 0.077 Uiso 1 1 calc R . .
H7B H 0.7224 0.2768 0.0835 0.077 Uiso 1 1 calc R . .
C8 C 0.6199(7) 0.2061(3) 0.0962(5) 0.0559(17) Uani 1 1 d . . .
C9 C -0.0053(7) 0.2662(3) -0.0906(5) 0.0584(18) Uani 1 1 d . . .
H9A H -0.0602 0.2341 -0.1103 0.070 Uiso 1 1 calc R . .
H9B H -0.0509 0.2995 -0.1171 0.070 Uiso 1 1 calc R . .
C10 C 0.0225(7) 0.2713(3) 0.0007(5) 0.0549(17) Uani 1 1 d . . .
C11 C 0.2918(8) 0.3803(3) 0.0459(4) 0.068(2) Uani 1 1 d . . .
H11A H 0.2044 0.3854 0.0438 0.082 Uiso 1 1 calc R . .
H11B H 0.3271 0.4173 0.0434 0.082 Uiso 1 1 calc R . .
C12 C 0.3629(7) 0.3540(4) 0.1265(5) 0.070(2) Uani 1 1 d . . .
C13 C 0.5743(10) 0.2639(4) -0.0620(6) 0.083(3) Uani 1 1 d . . .
H13A H 0.5927 0.2953 -0.0926 0.099 Uiso 1 1 calc R . .
H13B H 0.6507 0.2414 -0.0421 0.099 Uiso 1 1 calc R . .
C14 C 0.4740(9) 0.2294(4) -0.1190(5) 0.071(2) Uani 1 1 d . . .
C15 C 0.2643(7) 0.1803(3) 0.1816(4) 0.0598(17) Uani 1 1 d . . .
H15 H 0.2139 0.2108 0.1849 0.072 Uiso 1 1 calc R . .
C16 C 0.2036(9) 0.1412(5) 0.2911(5) 0.097(3) Uani 1 1 d . . .
H16A H 0.2201 0.1079 0.3247 0.145 Uiso 1 1 calc R . .
H16B H 0.1145 0.1438 0.2616 0.145 Uiso 1 1 calc R . .
H16C H 0.2298 0.1737 0.3259 0.145 Uiso 1 1 calc R . .
C17 C 0.3445(9) 0.0878(4) 0.2251(6) 0.091(3) Uani 1 1 d . . .
H17A H 0.3431 0.0613 0.2674 0.137 Uiso 1 1 calc R . .
H17B H 0.4306 0.0977 0.2313 0.137 Uiso 1 1 calc R . .
H17C H 0.3060 0.0711 0.1717 0.137 Uiso 1 1 calc R . .
C18 C 0.0534(6) 0.0583(3) -0.1153(4) 0.0481(14) Uani 1 1 d . . .
C19 C 0.1421(6) 0.0401(3) -0.0458(4) 0.0519(15) Uani 1 1 d . . .
H19 H 0.2017 0.0650 -0.0133 0.062 Uiso 1 1 calc R . .
C20 C 0.1441(7) -0.0165(3) -0.0229(4) 0.0560(16) Uani 1 1 d . . .
C21 C 0.2365(8) -0.0395(3) 0.0484(5) 0.070(2) Uani 1 1 d . . .
H21 H 0.2969 -0.0160 0.0835 0.084 Uiso 1 1 calc R . .
C22 C 0.2371(8) -0.0958(3) 0.0658(5) 0.076(2) Uani 1 1 d . . .
H22 H 0.2973 -0.1101 0.1128 0.091 Uiso 1 1 calc R . .
C23 C 0.1480(8) -0.1318(3) 0.0133(6) 0.074(2) Uani 1 1 d . . .
H23 H 0.1518 -0.1702 0.0246 0.089 Uiso 1 1 calc R . .
C24 C 0.0556(7) -0.1117(3) -0.0542(5) 0.068(2) Uani 1 1 d . . .
H24 H -0.0053 -0.1358 -0.0873 0.081 Uiso 1 1 calc R . .
C25 C 0.0528(6) -0.0536(3) -0.0735(4) 0.0517(16) Uani 1 1 d . . .
C26 C -0.0381(7) 0.0193(3) -0.1620(5) 0.0630(18) Uani 1 1 d . . .
H26 H -0.1018 0.0324 -0.2083 0.076 Uiso 1 1 calc R . .
C27 C 0.7292(7) 0.1205(3) 0.1641(4) 0.0573(17) Uani 1 1 d . . .
C28 C 0.6416(7) 0.0811(3) 0.1283(5) 0.068(2) Uani 1 1 d . . .
H28 H 0.5689 0.0909 0.0855 0.082 Uiso 1 1 calc R . .
C29 C 0.6606(8) 0.0249(4) 0.1558(6) 0.074(2) Uani 1 1 d . . .
C30 C 0.5777(10) -0.0183(4) 0.1186(7) 0.097(3) Uani 1 1 d . . .
H30 H 0.5057 -0.0112 0.0738 0.116 Uiso 1 1 calc R . .
C31 C 0.6045(13) -0.0718(5) 0.1496(10) 0.117(4) Uani 1 1 d . . .
H31 H 0.5503 -0.1009 0.1238 0.141 Uiso 1 1 calc R . .
C32 C 0.7057(14) -0.0841(5) 0.2157(10) 0.114(4) Uani 1 1 d . . .
H32 H 0.7185 -0.1210 0.2346 0.137 Uiso 1 1 calc R . .
C33 C 0.7901(11) -0.0434(5) 0.2556(7) 0.102(3) Uani 1 1 d . . .
H33 H 0.8591 -0.0520 0.3017 0.122 Uiso 1 1 calc R . .
C34 C 0.7687(9) 0.0133(4) 0.2241(6) 0.075(2) Uani 1 1 d . . .
C35 C 0.8348(8) 0.1047(3) 0.2279(5) 0.069(2) Uani 1 1 d . . .
H35 H 0.8950 0.1324 0.2506 0.083 Uiso 1 1 calc R . .
Eu1 Eu 0.31703(3) 0.241012(14) 0.015641(19) 0.04489(17) Uani 1 1 d . . .
N1 N 0.1105(6) 0.2596(2) -0.1161(4) 0.0521(14) Uani 1 1 d . . .
N2 N 0.2938(5) 0.3477(2) -0.0283(3) 0.0559(14) Uani 1 1 d . . .
N3 N 0.5428(5) 0.2863(3) 0.0109(4) 0.0620(15) Uani 1 1 d . . .
N4 N 0.0418(5) 0.1128(2) -0.1489(3) 0.0542(13) Uani 1 1 d . . .
H4 H -0.0157 0.1177 -0.1960 0.065 Uiso 1 1 calc R . .
N5 N 0.7227(5) 0.1776(3) 0.1413(3) 0.0582(14) Uani 1 1 d . . .
H5 H 0.7924 0.1962 0.1580 0.070 Uiso 1 1 calc R . .
N6 N -0.0376(6) -0.0352(3) -0.1429(4) 0.0676(17) Uani 1 1 d . . .
N7 N 0.8582(7) 0.0538(3) 0.2597(4) 0.082(2) Uani 1 1 d . . .
N8 N 0.2732(6) 0.1387(3) 0.2328(4) 0.0639(16) Uani 1 1 d . . .
O1 O 0.1888(4) 0.15854(19) -0.0451(3) 0.0592(12) Uani 1 1 d . . .
O2 O 0.5152(4) 0.1850(2) 0.0673(3) 0.0677(13) Uani 1 1 d . . .
O3 O 0.1368(5) 0.2695(2) 0.0483(3) 0.0573(12) Uani 1 1 d . . .
O4 O 0.3989(4) 0.3039(2) 0.1275(3) 0.0575(12) Uani 1 1 d . . .
O5 O 0.3671(5) 0.2251(2) -0.1058(3) 0.0672(13) Uani 1 1 d . . .
O6 O 0.3189(5) 0.1815(2) 0.1293(3) 0.0678(14) Uani 1 1 d . . .
O7 O -0.0694(5) 0.2750(3) 0.0262(4) 0.0822(16) Uani 1 1 d . . .
O8 O 0.3833(8) 0.3841(3) 0.1882(4) 0.123(3) Uani 1 1 d . . .
O9 O 0.4982(7) 0.2069(3) -0.1789(4) 0.101(2) Uani 1 1 d . . .
O1W O 0.0907(9) 0.0217(7) 0.3851(8) 0.224(6) Uani 1 1 d . . .
O2W O 0.7389(11) 0.2024(7) 0.7904(8) 0.214(6) Uani 1 1 d . . .
O3W O 0.9529(6) 0.2326(3) 0.1776(5) 0.0886(19) Uani 1 1 d . . .
O4W O -0.001(3) 0.4341(11) 0.1339(16) 0.423(17) 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
C1 O1 1.238(7) . ?
C1 N4 1.335(8) . ?
C1 C2 1.507(9) . ?
C2 N1 1.480(9) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N1 1.474(8) . ?
C3 C4 1.509(10) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N2 1.498(8) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N2 1.469(10) . ?
C5 C6 1.526(10) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N3 1.487(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N3 1.445(10) . ?
C7 C8 1.534(11) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 O2 1.219(8) . ?
C8 N5 1.342(8) . ?
C9 N1 1.494(10) . ?
C9 C10 1.492(11) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 O7 1.235(9) . ?
C10 O3 1.273(9) . ?
C11 N2 1.490(9) . ?
C11 C12 1.487(10) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 O8 1.232(9) . ?
C12 O4 1.255(9) . ?
C12 Eu1 3.231(8) . ?
C13 C14 1.475(14) . ?
C13 N3 1.493(11) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 O9 1.255(10) . ?
C14 O5 1.284(10) . ?
C15 O6 1.230(8) . ?
C15 N8 1.301(9) . ?
C15 H15 0.9300 . ?
C16 N8 1.444(10) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 N8 1.477(11) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.349(9) . ?
C18 N4 1.408(8) . ?
C18 C26 1.419(9) . ?
C19 C20 1.401(10) . ?
C19 H19 0.9300 . ?
C20 C25 1.412(9) . ?
C20 C21 1.428(10) . ?
C21 C22 1.372(11) . ?
C21 H21 0.9300 . ?
C22 C23 1.398(12) . ?
C22 H22 0.9300 . ?
C23 C24 1.363(11) . ?
C23 H23 0.9300 . ?
C24 C25 1.418(10) . ?
C24 H24 0.9300 . ?
C25 N6 1.359(9) . ?
C26 N6 1.337(10) . ?
C26 H26 0.9300 . ?
C27 C28 1.352(10) . ?
C27 C35 1.376(10) . ?
C27 N5 1.407(9) . ?
C28 C29 1.410(11) . ?
C28 H28 0.9300 . ?
C29 C30 1.393(12) . ?
C29 C34 1.409(12) . ?
C30 C31 1.373(15) . ?
C30 H30 0.9300 . ?
C31 C32 1.348(17) . ?
C31 H31 0.9300 . ?
C32 C33 1.371(16) . ?
C32 H32 0.9300 . ?
C33 C34 1.443(13) . ?
C33 H33 0.9300 . ?
C34 N7 1.380(11) . ?
C35 N7 1.319(10) . ?
C35 H35 0.9300 . ?
Eu1 O5 2.339(5) . ?
Eu1 O3 2.348(5) . ?
Eu1 O4 2.366(4) . ?
Eu1 O6 2.394(5) . ?
Eu1 O1 2.453(4) . ?
Eu1 O2 2.486(5) . ?
Eu1 N2 2.636(5) . ?
Eu1 N1 2.689(6) . ?
Eu1 N3 2.759(6) . ?
N4 H4 0.8600 . ?
N5 H5 0.8600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 N4 123.7(6) . . ?
O1 C1 C2 119.9(6) . . ?
N4 C1 C2 116.4(5) . . ?
N1 C2 C1 108.1(6) . . ?
N1 C2 H2A 110.1 . . ?
C1 C2 H2A 110.1 . . ?
N1 C2 H2B 110.1 . . ?
C1 C2 H2B 110.1 . . ?
H2A C2 H2B 108.4 . . ?
N1 C3 C4 110.0(6) . . ?
N1 C3 H3A 109.7 . . ?
C4 C3 H3A 109.7 . . ?
N1 C3 H3B 109.7 . . ?
C4 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
N2 C4 C3 113.0(6) . . ?
N2 C4 H4A 109.0 . . ?
C3 C4 H4A 109.0 . . ?
N2 C4 H4B 109.0 . . ?
C3 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
N2 C5 C6 112.6(6) . . ?
N2 C5 H5A 109.1 . . ?
C6 C5 H5A 109.1 . . ?
N2 C5 H5B 109.1 . . ?
C6 C5 H5B 109.1 . . ?
H5A C5 H5B 107.8 . . ?
N3 C6 C5 109.6(6) . . ?
N3 C6 H6A 109.8 . . ?
C5 C6 H6A 109.8 . . ?
N3 C6 H6B 109.8 . . ?
C5 C6 H6B 109.8 . . ?
H6A C6 H6B 108.2 . . ?
N3 C7 C8 106.4(6) . . ?
N3 C7 H7A 110.4 . . ?
C8 C7 H7A 110.4 . . ?
N3 C7 H7B 110.4 . . ?
C8 C7 H7B 110.4 . . ?
H7A C7 H7B 108.6 . . ?
O2 C8 N5 123.7(7) . . ?
O2 C8 C7 120.3(6) . . ?
N5 C8 C7 116.0(6) . . ?
N1 C9 C10 113.6(6) . . ?
N1 C9 H9A 108.9 . . ?
C10 C9 H9A 108.9 . . ?
N1 C9 H9B 108.9 . . ?
C10 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
O7 C10 O3 123.3(7) . . ?
O7 C10 C9 116.9(7) . . ?
O3 C10 C9 119.7(7) . . ?
N2 C11 C12 114.7(6) . . ?
N2 C11 H11A 108.6 . . ?
C12 C11 H11A 108.6 . . ?
N2 C11 H11B 108.6 . . ?
C12 C11 H11B 108.6 . . ?
H11A C11 H11B 107.6 . . ?
O8 C12 O4 124.7(7) . . ?
O8 C12 C11 116.2(7) . . ?
O4 C12 C11 119.0(7) . . ?
O8 C12 Eu1 159.2(7) . . ?
O4 C12 Eu1 37.7(3) . . ?
C11 C12 Eu1 82.6(4) . . ?
C14 C13 N3 114.7(7) . . ?
C14 C13 H13A 108.6 . . ?
N3 C13 H13A 108.6 . . ?
C14 C13 H13B 108.6 . . ?
N3 C13 H13B 108.6 . . ?
H13A C13 H13B 107.6 . . ?
O9 C14 O5 124.1(9) . . ?
O9 C14 C13 117.3(8) . . ?
O5 C14 C13 118.6(8) . . ?
O6 C15 N8 123.6(8) . . ?
O6 C15 H15 118.2 . . ?
N8 C15 H15 118.2 . . ?
N8 C16 H16A 109.5 . . ?
N8 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N8 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N8 C17 H17A 109.5 . . ?
N8 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N8 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 N4 126.8(6) . . ?
C19 C18 C26 118.5(6) . . ?
N4 C18 C26 114.7(6) . . ?
C18 C19 C20 119.6(6) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 H19 120.2 . . ?
C19 C20 C25 119.1(7) . . ?
C19 C20 C21 123.2(7) . . ?
C25 C20 C21 117.7(7) . . ?
C22 C21 C20 120.7(8) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C21 C22 C23 120.5(8) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 H22 119.8 . . ?
C24 C23 C22 121.0(7) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C23 C24 C25 119.6(7) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
N6 C25 C20 121.3(6) . . ?
N6 C25 C24 118.1(7) . . ?
C20 C25 C24 120.5(7) . . ?
N6 C26 C18 123.4(7) . . ?
N6 C26 H26 118.3 . . ?
C18 C26 H26 118.3 . . ?
C28 C27 C35 118.7(7) . . ?
C28 C27 N5 125.4(7) . . ?
C35 C27 N5 116.0(7) . . ?
C27 C28 C29 119.8(8) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 H28 120.1 . . ?
C30 C29 C34 120.0(9) . . ?
C30 C29 C28 122.7(9) . . ?
C34 C29 C28 117.3(8) . . ?
C31 C30 C29 118.5(11) . . ?
C31 C30 H30 120.7 . . ?
C29 C30 H30 120.7 . . ?
C32 C31 C30 122.9(12) . . ?
C32 C31 H31 118.5 . . ?
C30 C31 H31 118.5 . . ?
C31 C32 C33 121.4(11) . . ?
C31 C32 H32 119.3 . . ?
C33 C32 H32 119.3 . . ?
C32 C33 C34 118.0(11) . . ?
C32 C33 H33 121.0 . . ?
C34 C33 H33 121.0 . . ?
N7 C34 C29 122.2(8) . . ?
N7 C34 C33 118.6(9) . . ?
C29 C34 C33 119.1(10) . . ?
N7 C35 C27 125.6(8) . . ?
N7 C35 H35 117.2 . . ?
C27 C35 H35 117.2 . . ?
O5 Eu1 O3 136.00(18) . . ?
O5 Eu1 O4 132.53(18) . . ?
O3 Eu1 O4 76.40(17) . . ?
O5 Eu1 O6 132.62(19) . . ?
O3 Eu1 O6 76.50(18) . . ?
O4 Eu1 O6 79.66(18) . . ?
O5 Eu1 O1 76.59(18) . . ?
O3 Eu1 O1 84.53(18) . . ?
O4 Eu1 O1 150.33(17) . . ?
O6 Eu1 O1 73.86(17) . . ?
O5 Eu1 O2 77.98(19) . . ?
O3 Eu1 O2 143.16(17) . . ?
O4 Eu1 O2 89.04(17) . . ?
O6 Eu1 O2 67.59(18) . . ?
O1 Eu1 O2 93.00(16) . . ?
O5 Eu1 N2 86.21(19) . . ?
O3 Eu1 N2 77.00(18) . . ?
O4 Eu1 N2 66.26(16) . . ?
O6 Eu1 N2 140.73(19) . . ?
O1 Eu1 N2 131.24(15) . . ?
O2 Eu1 N2 127.76(17) . . ?
O5 Eu1 N1 70.7(2) . . ?
O3 Eu1 N1 65.32(18) . . ?
O4 Eu1 N1 125.18(16) . . ?
O6 Eu1 N1 123.86(18) . . ?
O1 Eu1 N1 63.34(15) . . ?
O2 Eu1 N1 144.08(18) . . ?
N2 Eu1 N1 67.93(16) . . ?
O5 Eu1 N3 63.99(19) . . ?
O3 Eu1 N3 138.5(2) . . ?
O4 Eu1 N3 69.87(18) . . ?
O6 Eu1 N3 118.78(18) . . ?
O1 Eu1 N3 135.50(19) . . ?
O2 Eu1 N3 60.38(17) . . ?
N2 Eu1 N3 67.88(18) . . ?
N1 Eu1 N3 117.13(18) . . ?
O5 Eu1 C12 127.9(2) . . ?
O3 Eu1 C12 67.0(2) . . ?
O4 Eu1 C12 18.92(17) . . ?
O6 Eu1 C12 93.4(2) . . ?
O1 Eu1 C12 151.0(2) . . ?
O2 Eu1 C12 106.35(18) . . ?
N2 Eu1 C12 49.31(19) . . ?
N1 Eu1 C12 106.59(17) . . ?
N3 Eu1 C12 73.5(2) . . ?
C3 N1 C2 111.0(6) . . ?
C3 N1 C9 113.0(6) . . ?
C2 N1 C9 108.0(6) . . ?
C3 N1 Eu1 106.5(4) . . ?
C2 N1 Eu1 106.9(4) . . ?
C9 N1 Eu1 111.3(4) . . ?
C5 N2 C11 111.5(6) . . ?
C5 N2 C4 107.7(6) . . ?
C11 N2 C4 110.0(6) . . ?
C5 N2 Eu1 109.3(4) . . ?
C11 N2 Eu1 106.7(4) . . ?
C4 N2 Eu1 111.7(4) . . ?
C7 N3 C6 110.9(6) . . ?
C7 N3 C13 110.0(7) . . ?
C6 N3 C13 111.3(7) . . ?
C7 N3 Eu1 106.5(4) . . ?
C6 N3 Eu1 108.0(4) . . ?
C13 N3 Eu1 110.0(5) . . ?
C1 N4 C18 126.9(5) . . ?
C1 N4 H4 116.5 . . ?
C18 N4 H4 116.5 . . ?
C8 N5 C27 127.3(6) . . ?
C8 N5 H5 116.4 . . ?
C27 N5 H5 116.4 . . ?
C26 N6 C25 118.0(6) . . ?
C35 N7 C34 116.2(7) . . ?
C15 N8 C16 119.1(8) . . ?
C15 N8 C17 119.6(7) . . ?
C16 N8 C17 121.1(7) . . ?
C1 O1 Eu1 123.6(4) . . ?
C8 O2 Eu1 123.3(5) . . ?
C10 O3 Eu1 127.9(5) . . ?
C12 O4 Eu1 123.4(4) . . ?
C14 O5 Eu1 129.6(5) . . ?
C15 O6 Eu1 136.2(5) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.49
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.919
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.165
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_PrDTPAAQ_DMF
_database_code_depnum_ccdc_archive 'CCDC 1402443'
_audit_update_record             
;
2015-08-04 deposited with the CCDC.
2015-12-02 downloaded from the CCDC.
;



_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C38 H54 N9 O13 Pr'
_chemical_formula_sum            'C38 H54 N9 O13 Pr'
_chemical_formula_weight         985.81

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   11.343(5)
_cell_length_b                   23.530(5)
_cell_length_c                   16.714(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 109.356(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     4209(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2032
_exptl_absorpt_coefficient_mu    1.233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7906
_exptl_absorpt_correction_T_max  0.8272
_exptl_absorpt_process_details   SADABS(Sheldrick,1997)

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 0.5
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            39462
_diffrn_reflns_av_R_equivalents  0.1328
_diffrn_reflns_av_sigmaI/netI    0.0864
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         26.00
_reflns_number_total             8264
_reflns_number_gt                5852
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX II V2012.4-3'
_computing_cell_refinement       'Bruker APEX II V2012.4-3'
_computing_data_reduction        'Bruker APEX II V2012.4-3'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0650P)²+9.4794P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8264
_refine_ls_number_parameters     559
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0497
_refine_ls_wR_factor_ref         0.1381
_refine_ls_wR_factor_gt          0.1219
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.059
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.19035(3) 0.257877(12) 0.009218(18) 0.01925(11) Uani 1 1 d . . .
C1 C 0.2768(6) 0.3438(2) -0.1221(3) 0.0230(13) Uani 1 1 d . . .
C2 C 0.2349(6) 0.2928(2) -0.1798(3) 0.0280(14) Uani 1 1 d . . .
H2A H 0.1456 0.2950 -0.2094 0.034 Uiso 1 1 calc R . .
H2B H 0.2771 0.2926 -0.2217 0.034 Uiso 1 1 calc R . .
C3 C 0.1885(6) 0.1926(2) -0.1763(3) 0.0290(15) Uani 1 1 d . . .
H3A H 0.2141 0.1836 -0.2248 0.035 Uiso 1 1 calc R . .
H3B H 0.1013 0.2038 -0.1973 0.035 Uiso 1 1 calc R . .
C4 C 0.2032(6) 0.1408(2) -0.1209(3) 0.0285(15) Uani 1 1 d . . .
H4A H 0.1580 0.1094 -0.1550 0.034 Uiso 1 1 calc R . .
H4B H 0.2908 0.1304 -0.0990 0.034 Uiso 1 1 calc R . .
C5 C 0.0216(6) 0.1357(3) -0.0742(4) 0.0344(16) Uani 1 1 d . . .
H5A H 0.0117 0.0953 -0.0856 0.041 Uiso 1 1 calc R . .
H5B H -0.0210 0.1555 -0.1268 0.041 Uiso 1 1 calc R . .
C6 C -0.0406(6) 0.1507(3) -0.0105(4) 0.0357(16) Uani 1 1 d . . .
H6A H -0.1248 0.1354 -0.0286 0.043 Uiso 1 1 calc R . .
H6B H 0.0055 0.1340 0.0440 0.043 Uiso 1 1 calc R . .
C7 C -0.0642(6) 0.2292(3) 0.0782(4) 0.0309(15) Uani 1 1 d . . .
H7A H -0.0090 0.2074 0.1250 0.037 Uiso 1 1 calc R . .
H7B H -0.1498 0.2218 0.0750 0.037 Uiso 1 1 calc R . .
C8 C -0.0353(6) 0.2924(2) 0.0917(4) 0.0253(13) Uani 1 1 d . . .
C27 C -0.0807(5) 0.3795(3) 0.1540(4) 0.0256(13) Uani 1 1 d . . .
C28 C -0.0208(6) 0.4183(3) 0.1207(4) 0.0298(15) Uani 1 1 d . . .
H28 H 0.0126 0.4077 0.0790 0.036 Uiso 1 1 calc R . .
C29 C -0.0101(6) 0.4746(3) 0.1503(4) 0.0286(14) Uani 1 1 d . . .
C30 C 0.0444(7) 0.5177(3) 0.1168(5) 0.048(2) Uani 1 1 d . . .
H30 H 0.0765 0.5091 0.0738 0.058 Uiso 1 1 calc R . .
C31 C 0.0515(7) 0.5716(3) 0.1460(5) 0.048(2) Uani 1 1 d . . .
H31 H 0.0868 0.5997 0.1219 0.058 Uiso 1 1 calc R . .
C32 C 0.0066(7) 0.5857(3) 0.2117(5) 0.0422(18) Uani 1 1 d . . .
H32 H 0.0133 0.6228 0.2317 0.051 Uiso 1 1 calc R . .
C33 C -0.0472(6) 0.5452(3) 0.2467(4) 0.0329(15) Uani 1 1 d . . .
H33 H -0.0762 0.5547 0.2910 0.039 Uiso 1 1 calc R . .
C34 C -0.0589(6) 0.4883(3) 0.2155(4) 0.0263(14) Uani 1 1 d . . .
C35 C -0.1303(6) 0.3981(3) 0.2172(3) 0.0274(14) Uani 1 1 d . . .
H35 H -0.1737 0.3717 0.2381 0.033 Uiso 1 1 calc R . .
C18 C 0.3382(5) 0.4438(2) -0.1180(3) 0.0217(13) Uani 1 1 d . . .
C19 C 0.3159(5) 0.4615(2) -0.0466(3) 0.0225(13) Uani 1 1 d . . .
H19 H 0.2865 0.4361 -0.0150 0.027 Uiso 1 1 calc R . .
C20 C 0.3380(5) 0.5189(2) -0.0215(3) 0.0221(13) Uani 1 1 d . . .
C21 C 0.3133(6) 0.5413(2) 0.0509(4) 0.0296(14) Uani 1 1 d . . .
H21 H 0.2848 0.5174 0.0848 0.035 Uiso 1 1 calc R . .
C22 C 0.3315(6) 0.5979(3) 0.0707(4) 0.0315(15) Uani 1 1 d . . .
H22 H 0.3134 0.6124 0.1171 0.038 Uiso 1 1 calc R . .
C23 C 0.3772(6) 0.6339(3) 0.0209(4) 0.0295(14) Uani 1 1 d . . .
H23 H 0.3902 0.6722 0.0352 0.035 Uiso 1 1 calc R . .
C24 C 0.4029(6) 0.6139(2) -0.0478(4) 0.0274(14) Uani 1 1 d . . .
H24 H 0.4324 0.6385 -0.0805 0.033 Uiso 1 1 calc R . .
C25 C 0.3849(5) 0.5557(2) -0.0698(3) 0.0200(12) Uani 1 1 d . . .
C26 C 0.3887(5) 0.4835(2) -0.1610(4) 0.0256(14) Uani 1 1 d . . .
H26 H 0.4079 0.4709 -0.2079 0.031 Uiso 1 1 calc R . .
C9 C 0.3996(6) 0.2282(2) -0.1026(4) 0.0267(14) Uani 1 1 d . . .
H9A H 0.4388 0.2569 -0.1270 0.032 Uiso 1 1 calc R . .
H9B H 0.4109 0.1918 -0.1264 0.032 Uiso 1 1 calc R . .
C10 C 0.4671(6) 0.2264(2) -0.0081(4) 0.0250(14) Uani 1 1 d . . .
C11 C 0.2277(6) 0.1130(2) 0.0239(3) 0.0278(15) Uani 1 1 d . . .
H11A H 0.3107 0.1075 0.0206 0.033 Uiso 1 1 calc R . .
H11B H 0.1875 0.0761 0.0171 0.033 Uiso 1 1 calc R . .
C12 C 0.2403(6) 0.1357(2) 0.1112(4) 0.0262(14) Uani 1 1 d . . .
C13 C -0.1449(7) 0.2391(3) -0.0736(4) 0.0421(17) Uani 1 1 d . . .
H13B H -0.1972 0.2622 -0.0508 0.051 Uiso 1 1 calc R . .
H13A H -0.1968 0.2090 -0.1068 0.051 Uiso 1 1 calc R . .
C14 C -0.0997(7) 0.2758(3) -0.1324(4) 0.0385(17) Uani 1 1 d . . .
C15 C 0.4142(6) 0.3194(2) 0.1808(3) 0.0232(13) Uani 1 1 d . . .
H15 H 0.4682 0.2899 0.1801 0.028 Uiso 1 1 calc R . .
C16 C 0.5868(6) 0.3612(3) 0.2889(4) 0.0369(16) Uani 1 1 d . . .
H16A H 0.6032 0.3950 0.3230 0.055 Uiso 1 1 calc R . .
H16B H 0.6413 0.3600 0.2556 0.055 Uiso 1 1 calc R . .
H16C H 0.6012 0.3285 0.3251 0.055 Uiso 1 1 calc R . .
C17 C 0.3821(6) 0.4106(2) 0.2349(4) 0.0294(14) Uani 1 1 d . . .
H17A H 0.4298 0.4369 0.2772 0.044 Uiso 1 1 calc R . .
H17B H 0.3097 0.3988 0.2481 0.044 Uiso 1 1 calc R . .
H17C H 0.3564 0.4288 0.1804 0.044 Uiso 1 1 calc R . .
C36 C 0.5785(9) 0.0625(4) -0.0078(6) 0.068(3) Uani 1 1 d . . .
C37 C 0.5927(11) 0.0937(5) 0.1367(6) 0.092(3) Uani 1 1 d . . .
C38 C 0.7438(12) 0.0253(7) 0.1096(8) 0.155(7) Uani 1 1 d . . .
N1 N 0.2646(5) 0.24034(18) -0.1288(3) 0.0233(11) Uani 1 1 d . . .
N2 N 0.1559(5) 0.14980(19) -0.0476(3) 0.0254(12) Uani 1 1 d . . .
N3 N -0.0455(5) 0.2130(2) -0.0018(3) 0.0294(12) Uani 1 1 d . . .
N4 N 0.3129(5) 0.38923(19) -0.1543(3) 0.0248(11) Uani 1 1 d . . .
H4 H 0.3220 0.3850 -0.2030 0.030 Uiso 1 1 calc R . .
N5 N -0.0996(4) 0.3215(2) 0.1314(3) 0.0244(11) Uani 1 1 d . . .
H5 H -0.1570 0.3038 0.1444 0.029 Uiso 1 1 calc R . .
N6 N 0.4106(5) 0.5373(2) -0.1393(3) 0.0257(11) Uani 1 1 d . . .
N7 N -0.1196(5) 0.4497(2) 0.2482(3) 0.0288(12) Uani 1 1 d . . .
N8 N 0.4581(4) 0.3615(2) 0.2333(3) 0.0227(11) Uani 1 1 d . . .
N9 N 0.6396(7) 0.0627(3) 0.0759(5) 0.072(2) Uani 1 1 d . . .
O1 O 0.2720(4) 0.34188(15) -0.0486(2) 0.0267(10) Uani 1 1 d . . .
O2 O 0.0454(4) 0.31340(17) 0.0660(3) 0.0338(11) Uani 1 1 d . . .
O3 O 0.4020(4) 0.22557(16) 0.0412(2) 0.0241(9) Uani 1 1 d . . .
O4 O 0.2143(4) 0.18705(16) 0.1187(2) 0.0251(9) Uani 1 1 d . . .
O5 O 0.0174(4) 0.27882(18) -0.1183(3) 0.0336(10) Uani 1 1 d . . .
O6 O 0.3046(4) 0.31645(16) 0.1318(2) 0.0252(9) Uani 1 1 d . . .
O7 O 0.5837(4) 0.2247(2) 0.0168(3) 0.0387(11) Uani 1 1 d . . .
O8 O 0.2794(5) 0.10129(18) 0.1704(3) 0.0390(12) Uani 1 1 d . . .
O9 O -0.1803(5) 0.2990(2) -0.1924(3) 0.0563(15) Uani 1 1 d . . .
O10 O 0.4761(7) 0.0872(3) -0.0431(4) 0.088(2) Uani 1 1 d . . .
OW2 O 0.7110(4) 0.26699(18) 0.1700(3) 0.0336(10) Uani 1 1 d . . .
OW4 O 0.2156(5) 0.98487(19) 0.1219(3) 0.0421(12) Uani 1 1 d . . .
OW3 O 0.9569(13) 0.0214(5) 0.0353(8) 0.204(5) Uani 1 1 d . . .
OW1 O 0.5406(13) 0.3060(5) 0.7712(9) 0.210(6) 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 2.404(4) . ?
Pr1 O5 2.421(4) . ?
Pr1 O4 2.422(4) . ?
Pr1 O6 2.453(4) . ?
Pr1 O1 2.508(4) . ?
Pr1 O2 2.519(4) . ?
Pr1 N2 2.697(4) . ?
Pr1 N1 2.737(4) . ?
Pr1 N3 2.824(5) . ?
C1 O1 1.249(6) . ?
C1 N4 1.323(7) . ?
C1 C2 1.513(8) . ?
C2 N1 1.475(7) . ?
C3 N1 1.477(7) . ?
C3 C4 1.509(8) . ?
C4 N2 1.506(7) . ?
C5 N2 1.476(8) . ?
C5 C6 1.502(8) . ?
C6 N3 1.475(8) . ?
C7 N3 1.473(7) . ?
C7 C8 1.523(8) . ?
C8 O2 1.236(7) . ?
C8 N5 1.328(7) . ?
C27 C28 1.363(8) . ?
C27 N5 1.411(7) . ?
C27 C35 1.421(8) . ?
C28 C29 1.405(8) . ?
C29 C30 1.397(9) . ?
C29 C34 1.414(8) . ?
C30 C31 1.352(10) . ?
C31 C32 1.396(9) . ?
C32 C33 1.363(9) . ?
C33 C34 1.427(8) . ?
C34 N7 1.359(8) . ?
C35 N7 1.310(7) . ?
C18 C19 1.365(7) . ?
C18 N4 1.408(7) . ?
C18 C26 1.411(8) . ?
C19 C20 1.414(8) . ?
C20 C25 1.404(8) . ?
C20 C21 1.430(8) . ?
C21 C22 1.371(8) . ?
C22 C23 1.400(8) . ?
C23 C24 1.361(8) . ?
C24 C25 1.414(8) . ?
C25 N6 1.358(7) . ?
C26 N6 1.316(7) . ?
C9 N1 1.474(8) . ?
C9 C10 1.510(8) . ?
C10 O7 1.249(7) . ?
C10 O3 1.275(7) . ?
C11 N2 1.481(7) . ?
C11 C12 1.516(7) . ?
C12 O8 1.241(7) . ?
C12 O4 1.259(7) . ?
C13 N3 1.480(8) . ?
C13 C14 1.520(10) . ?
C14 O9 1.238(8) . ?
C14 O5 1.273(8) . ?
C15 O6 1.243(7) . ?
C15 N8 1.308(7) . ?
C16 N8 1.448(8) . ?
C17 N8 1.446(7) . ?
C36 O10 1.258(10) . ?
C36 N9 1.339(11) . ?
C37 N9 1.485(12) . ?
C38 N9 1.431(12) . ?

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 O5 135.88(13) . . ?
O3 Pr1 O4 76.18(13) . . ?
O5 Pr1 O4 131.31(14) . . ?
O3 Pr1 O6 77.27(13) . . ?
O5 Pr1 O6 132.11(14) . . ?
O4 Pr1 O6 81.96(13) . . ?
O3 Pr1 O1 82.27(13) . . ?
O5 Pr1 O1 78.20(15) . . ?
O4 Pr1 O1 150.42(14) . . ?
O6 Pr1 O1 73.63(13) . . ?
O3 Pr1 O2 144.01(13) . . ?
O5 Pr1 O2 77.67(15) . . ?
O4 Pr1 O2 89.78(14) . . ?
O6 Pr1 O2 67.94(14) . . ?
O1 Pr1 O2 96.13(13) . . ?
O3 Pr1 N2 78.32(15) . . ?
O5 Pr1 N2 84.34(14) . . ?
O4 Pr1 N2 65.42(13) . . ?
O6 Pr1 N2 143.00(14) . . ?
O1 Pr1 N2 129.53(13) . . ?
O2 Pr1 N2 125.80(14) . . ?
O3 Pr1 N1 64.89(13) . . ?
O5 Pr1 N1 71.00(15) . . ?
O4 Pr1 N1 122.96(13) . . ?
O6 Pr1 N1 124.29(14) . . ?
O1 Pr1 N1 62.49(12) . . ?
O2 Pr1 N1 144.82(14) . . ?
N2 Pr1 N1 67.07(13) . . ?
O3 Pr1 N3 138.67(14) . . ?
O5 Pr1 N3 62.95(15) . . ?
O4 Pr1 N3 70.05(14) . . ?
O6 Pr1 N3 119.46(13) . . ?
O1 Pr1 N3 137.07(14) . . ?
O2 Pr1 N3 59.75(14) . . ?
N2 Pr1 N3 66.46(15) . . ?
N1 Pr1 N3 115.97(14) . . ?
O1 C1 N4 123.4(5) . . ?
O1 C1 C2 119.5(5) . . ?
N4 C1 C2 117.1(5) . . ?
N1 C2 C1 109.4(4) . . ?
N1 C3 C4 111.0(5) . . ?
N2 C4 C3 112.9(5) . . ?
N2 C5 C6 114.4(5) . . ?
N3 C6 C5 110.1(5) . . ?
N3 C7 C8 107.3(5) . . ?
O2 C8 N5 124.0(6) . . ?
O2 C8 C7 119.2(5) . . ?
N5 C8 C7 116.8(5) . . ?
C28 C27 N5 126.2(5) . . ?
C28 C27 C35 118.0(6) . . ?
N5 C27 C35 115.8(5) . . ?
C27 C28 C29 119.1(5) . . ?
C30 C29 C28 122.8(6) . . ?
C30 C29 C34 118.8(6) . . ?
C28 C29 C34 118.4(5) . . ?
C31 C30 C29 121.2(6) . . ?
C30 C31 C32 120.9(7) . . ?
C33 C32 C31 120.3(6) . . ?
C32 C33 C34 119.9(6) . . ?
N7 C34 C29 122.5(5) . . ?
N7 C34 C33 118.6(5) . . ?
C29 C34 C33 118.9(6) . . ?
N7 C35 C27 125.0(6) . . ?
C19 C18 N4 125.7(5) . . ?
C19 C18 C26 117.8(5) . . ?
N4 C18 C26 116.4(5) . . ?
C18 C19 C20 119.0(5) . . ?
C25 C20 C19 118.8(5) . . ?
C25 C20 C21 118.6(5) . . ?
C19 C20 C21 122.6(5) . . ?
C22 C21 C20 120.4(6) . . ?
C21 C22 C23 120.0(6) . . ?
C24 C23 C22 121.1(6) . . ?
C23 C24 C25 120.1(5) . . ?
N6 C25 C20 121.6(5) . . ?
N6 C25 C24 118.6(5) . . ?
C20 C25 C24 119.8(5) . . ?
N6 C26 C18 124.6(5) . . ?
N1 C9 C10 115.7(5) . . ?
O7 C10 O3 124.1(5) . . ?
O7 C10 C9 117.6(5) . . ?
O3 C10 C9 118.3(6) . . ?
N2 C11 C12 115.0(5) . . ?
O8 C12 O4 125.5(5) . . ?
O8 C12 C11 115.6(5) . . ?
O4 C12 C11 118.8(5) . . ?
N3 C13 C14 115.4(6) . . ?
O9 C14 O5 124.8(7) . . ?
O9 C14 C13 117.3(7) . . ?
O5 C14 C13 117.9(6) . . ?
O6 C15 N8 124.1(6) . . ?
O10 C36 N9 124.5(9) . . ?
C9 N1 C2 110.5(5) . . ?
C9 N1 C3 112.1(4) . . ?
C2 N1 C3 110.1(5) . . ?
C9 N1 Pr1 111.0(3) . . ?
C2 N1 Pr1 106.6(3) . . ?
C3 N1 Pr1 106.2(3) . . ?
C5 N2 C11 110.4(5) . . ?
C5 N2 C4 109.5(5) . . ?
C11 N2 C4 108.9(4) . . ?
C5 N2 Pr1 109.4(3) . . ?
C11 N2 Pr1 106.8(3) . . ?
C4 N2 Pr1 111.7(3) . . ?
C7 N3 C6 111.6(5) . . ?
C7 N3 C13 109.1(5) . . ?
C6 N3 C13 112.1(5) . . ?
C7 N3 Pr1 105.2(3) . . ?
C6 N3 Pr1 108.2(4) . . ?
C13 N3 Pr1 110.4(4) . . ?
C1 N4 C18 127.5(5) . . ?
C8 N5 C27 124.9(5) . . ?
C26 N6 C25 118.0(5) . . ?
C35 N7 C34 117.0(5) . . ?
C15 N8 C16 120.4(5) . . ?
C15 N8 C17 121.3(5) . . ?
C16 N8 C17 118.2(5) . . ?
C36 N9 C38 118.9(9) . . ?
C36 N9 C37 122.5(8) . . ?
C38 N9 C37 118.0(9) . . ?
C1 O1 Pr1 123.3(3) . . ?
C8 O2 Pr1 125.1(4) . . ?
C10 O3 Pr1 127.0(4) . . ?
C12 O4 Pr1 123.8(3) . . ?
C14 O5 Pr1 130.0(4) . . ?
C15 O6 Pr1 135.9(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 N1 -33.4(8) . . . . ?
N4 C1 C2 N1 148.9(5) . . . . ?
N1 C3 C4 N2 63.6(7) . . . . ?
N2 C5 C6 N3 67.5(7) . . . . ?
N3 C7 C8 O2 -32.4(7) . . . . ?
N3 C7 C8 N5 147.9(5) . . . . ?
N5 C27 C28 C29 179.9(6) . . . . ?
C35 C27 C28 C29 0.3(9) . . . . ?
C27 C28 C29 C30 -176.9(6) . . . . ?
C27 C28 C29 C34 1.9(9) . . . . ?
C28 C29 C30 C31 179.0(7) . . . . ?
C34 C29 C30 C31 0.3(11) . . . . ?
C29 C30 C31 C32 1.3(12) . . . . ?
C30 C31 C32 C33 -1.0(12) . . . . ?
C31 C32 C33 C34 -0.7(10) . . . . ?
C30 C29 C34 N7 176.3(6) . . . . ?
C28 C29 C34 N7 -2.5(9) . . . . ?
C30 C29 C34 C33 -2.0(9) . . . . ?
C28 C29 C34 C33 179.2(6) . . . . ?
C32 C33 C34 N7 -176.1(6) . . . . ?
C32 C33 C34 C29 2.2(9) . . . . ?
C28 C27 C35 N7 -2.2(9) . . . . ?
N5 C27 C35 N7 178.1(5) . . . . ?
N4 C18 C19 C20 -175.4(5) . . . . ?
C26 C18 C19 C20 3.2(8) . . . . ?
C18 C19 C20 C25 -1.4(8) . . . . ?
C18 C19 C20 C21 178.0(6) . . . . ?
C25 C20 C21 C22 2.1(9) . . . . ?
C19 C20 C21 C22 -177.3(6) . . . . ?
C20 C21 C22 C23 -1.5(10) . . . . ?
C21 C22 C23 C24 0.8(10) . . . . ?
C22 C23 C24 C25 -0.7(9) . . . . ?
C19 C20 C25 N6 -0.7(9) . . . . ?
C21 C20 C25 N6 179.9(5) . . . . ?
C19 C20 C25 C24 177.4(5) . . . . ?
C21 C20 C25 C24 -2.0(8) . . . . ?
C23 C24 C25 N6 179.5(6) . . . . ?
C23 C24 C25 C20 1.3(9) . . . . ?
C19 C18 C26 N6 -3.3(9) . . . . ?
N4 C18 C26 N6 175.5(5) . . . . ?
N1 C9 C10 O7 -169.6(5) . . . . ?
N1 C9 C10 O3 11.8(7) . . . . ?
N2 C11 C12 O8 167.2(6) . . . . ?
N2 C11 C12 O4 -14.6(8) . . . . ?
N3 C13 C14 O9 -179.0(5) . . . . ?
N3 C13 C14 O5 3.5(8) . . . . ?
C10 C9 N1 C2 119.5(5) . . . . ?
C10 C9 N1 C3 -117.2(5) . . . . ?
C10 C9 N1 Pr1 1.4(6) . . . . ?
C1 C2 N1 C9 -75.1(6) . . . . ?
C1 C2 N1 C3 160.5(5) . . . . ?
C1 C2 N1 Pr1 45.6(5) . . . . ?
C4 C3 N1 C9 64.9(6) . . . . ?
C4 C3 N1 C2 -171.6(5) . . . . ?
C4 C3 N1 Pr1 -56.5(5) . . . . ?
O3 Pr1 N1 C9 -7.6(3) . . . . ?
O5 Pr1 N1 C9 173.1(4) . . . . ?
O4 Pr1 N1 C9 -59.4(4) . . . . ?
O6 Pr1 N1 C9 44.5(4) . . . . ?
O1 Pr1 N1 C9 86.8(4) . . . . ?
O2 Pr1 N1 C9 144.8(3) . . . . ?
N2 Pr1 N1 C9 -95.1(4) . . . . ?
N3 Pr1 N1 C9 -141.6(3) . . . . ?
O3 Pr1 N1 C2 -128.0(4) . . . . ?
O5 Pr1 N1 C2 52.6(4) . . . . ?
O4 Pr1 N1 C2 -179.8(3) . . . . ?
O6 Pr1 N1 C2 -75.9(4) . . . . ?
O1 Pr1 N1 C2 -33.6(4) . . . . ?
O2 Pr1 N1 C2 24.4(5) . . . . ?
N2 Pr1 N1 C2 144.5(4) . . . . ?
N3 Pr1 N1 C2 98.0(4) . . . . ?
O3 Pr1 N1 C3 114.5(4) . . . . ?
O5 Pr1 N1 C3 -64.8(3) . . . . ?
O4 Pr1 N1 C3 62.7(4) . . . . ?
O6 Pr1 N1 C3 166.6(3) . . . . ?
O1 Pr1 N1 C3 -151.1(4) . . . . ?
O2 Pr1 N1 C3 -93.1(4) . . . . ?
N2 Pr1 N1 C3 27.0(3) . . . . ?
N3 Pr1 N1 C3 -19.5(4) . . . . ?
C6 C5 N2 C11 68.2(6) . . . . ?
C6 C5 N2 C4 -171.9(5) . . . . ?
C6 C5 N2 Pr1 -49.1(6) . . . . ?
C12 C11 N2 C5 -88.7(6) . . . . ?
C12 C11 N2 C4 151.1(5) . . . . ?
C12 C11 N2 Pr1 30.2(6) . . . . ?
C3 C4 N2 C5 88.3(6) . . . . ?
C3 C4 N2 C11 -150.9(5) . . . . ?
C3 C4 N2 Pr1 -33.1(6) . . . . ?
O3 Pr1 N2 C5 173.9(4) . . . . ?
O5 Pr1 N2 C5 -46.9(4) . . . . ?
O4 Pr1 N2 C5 93.9(4) . . . . ?
O6 Pr1 N2 C5 124.3(4) . . . . ?
O1 Pr1 N2 C5 -116.5(3) . . . . ?
O2 Pr1 N2 C5 23.4(4) . . . . ?
N1 Pr1 N2 C5 -118.7(4) . . . . ?
N3 Pr1 N2 C5 16.0(3) . . . . ?
O3 Pr1 N2 C11 54.3(3) . . . . ?
O5 Pr1 N2 C11 -166.5(4) . . . . ?
O4 Pr1 N2 C11 -25.7(3) . . . . ?
O6 Pr1 N2 C11 4.7(5) . . . . ?
O1 Pr1 N2 C11 123.9(3) . . . . ?
O2 Pr1 N2 C11 -96.1(4) . . . . ?
N1 Pr1 N2 C11 121.8(4) . . . . ?
N3 Pr1 N2 C11 -103.6(4) . . . . ?
O3 Pr1 N2 C4 -64.8(4) . . . . ?
O5 Pr1 N2 C4 74.5(4) . . . . ?
O4 Pr1 N2 C4 -144.8(4) . . . . ?
O6 Pr1 N2 C4 -114.4(4) . . . . ?
O1 Pr1 N2 C4 4.8(5) . . . . ?
O2 Pr1 N2 C4 144.8(4) . . . . ?
N1 Pr1 N2 C4 2.7(4) . . . . ?
N3 Pr1 N2 C4 137.4(4) . . . . ?
C8 C7 N3 C6 166.0(5) . . . . ?
C8 C7 N3 C13 -69.6(6) . . . . ?
C8 C7 N3 Pr1 48.9(5) . . . . ?
C5 C6 N3 C7 -160.3(5) . . . . ?
C5 C6 N3 C13 77.0(7) . . . . ?
C5 C6 N3 Pr1 -45.0(6) . . . . ?
C14 C13 N3 C7 124.3(6) . . . . ?
C14 C13 N3 C6 -111.6(6) . . . . ?
C14 C13 N3 Pr1 9.1(6) . . . . ?
O3 Pr1 N3 C7 100.6(4) . . . . ?
O5 Pr1 N3 C7 -129.6(4) . . . . ?
O4 Pr1 N3 C7 63.5(4) . . . . ?
O6 Pr1 N3 C7 -4.4(4) . . . . ?
O1 Pr1 N3 C7 -102.0(4) . . . . ?
O2 Pr1 N3 C7 -38.4(3) . . . . ?
N2 Pr1 N3 C7 134.6(4) . . . . ?
N1 Pr1 N3 C7 -178.6(3) . . . . ?
O3 Pr1 N3 C6 -18.8(5) . . . . ?
O5 Pr1 N3 C6 111.0(4) . . . . ?
O4 Pr1 N3 C6 -55.9(4) . . . . ?
O6 Pr1 N3 C6 -123.8(4) . . . . ?
O1 Pr1 N3 C6 138.6(3) . . . . ?
O2 Pr1 N3 C6 -157.8(4) . . . . ?
N2 Pr1 N3 C6 15.2(4) . . . . ?
N1 Pr1 N3 C6 62.0(4) . . . . ?
O3 Pr1 N3 C13 -141.8(3) . . . . ?
O5 Pr1 N3 C13 -12.0(4) . . . . ?
O4 Pr1 N3 C13 -178.9(4) . . . . ?
O6 Pr1 N3 C13 113.2(4) . . . . ?
O1 Pr1 N3 C13 15.6(5) . . . . ?
O2 Pr1 N3 C13 79.2(4) . . . . ?
N2 Pr1 N3 C13 -107.8(4) . . . . ?
N1 Pr1 N3 C13 -61.0(4) . . . . ?
O1 C1 N4 C18 -7.6(10) . . . . ?
C2 C1 N4 C18 170.0(5) . . . . ?
C19 C18 N4 C1 -8.1(10) . . . . ?
C26 C18 N4 C1 173.2(6) . . . . ?
O2 C8 N5 C27 -3.6(9) . . . . ?
C7 C8 N5 C27 176.1(5) . . . . ?
C28 C27 N5 C8 18.8(9) . . . . ?
C35 C27 N5 C8 -161.6(5) . . . . ?
C18 C26 N6 C25 1.2(9) . . . . ?
C20 C25 N6 C26 0.8(8) . . . . ?
C24 C25 N6 C26 -177.3(5) . . . . ?
C27 C35 N7 C34 1.7(9) . . . . ?
C29 C34 N7 C35 0.8(9) . . . . ?
C33 C34 N7 C35 179.0(5) . . . . ?
O6 C15 N8 C16 179.3(5) . . . . ?
O6 C15 N8 C17 -3.5(8) . . . . ?
O10 C36 N9 C38 169.6(12) . . . . ?
O10 C36 N9 C37 -1.2(16) . . . . ?
N4 C1 O1 Pr1 175.9(4) . . . . ?
C2 C1 O1 Pr1 -1.7(7) . . . . ?
O3 Pr1 O1 C1 85.7(4) . . . . ?
O5 Pr1 O1 C1 -54.5(4) . . . . ?
O4 Pr1 O1 C1 129.0(4) . . . . ?
O6 Pr1 O1 C1 164.6(5) . . . . ?
O2 Pr1 O1 C1 -130.5(4) . . . . ?
N2 Pr1 O1 C1 17.8(5) . . . . ?
N1 Pr1 O1 C1 20.0(4) . . . . ?
N3 Pr1 O1 C1 -79.5(5) . . . . ?
N5 C8 O2 Pr1 170.9(4) . . . . ?
C7 C8 O2 Pr1 -8.8(8) . . . . ?
O3 Pr1 O2 C8 -105.9(5) . . . . ?
O5 Pr1 O2 C8 92.4(5) . . . . ?
O4 Pr1 O2 C8 -40.2(5) . . . . ?
O6 Pr1 O2 C8 -121.6(5) . . . . ?
O1 Pr1 O2 C8 168.8(5) . . . . ?
N2 Pr1 O2 C8 18.8(5) . . . . ?
N1 Pr1 O2 C8 119.7(5) . . . . ?
N3 Pr1 O2 C8 26.7(4) . . . . ?
O7 C10 O3 Pr1 158.8(4) . . . . ?
C9 C10 O3 Pr1 -22.7(7) . . . . ?
O5 Pr1 O3 C10 17.7(5) . . . . ?
O4 Pr1 O3 C10 154.0(5) . . . . ?
O6 Pr1 O3 C10 -121.2(4) . . . . ?
O1 Pr1 O3 C10 -46.4(4) . . . . ?
O2 Pr1 O3 C10 -136.2(4) . . . . ?
N2 Pr1 O3 C10 86.8(4) . . . . ?
N1 Pr1 O3 C10 16.8(4) . . . . ?
N3 Pr1 O3 C10 118.3(4) . . . . ?
O8 C12 O4 Pr1 163.5(5) . . . . ?
C11 C12 O4 Pr1 -14.5(8) . . . . ?
O3 Pr1 O4 C12 -60.4(5) . . . . ?
O5 Pr1 O4 C12 79.7(5) . . . . ?
O6 Pr1 O4 C12 -139.2(5) . . . . ?
O1 Pr1 O4 C12 -104.9(5) . . . . ?
O2 Pr1 O4 C12 153.0(5) . . . . ?
N2 Pr1 O4 C12 22.9(5) . . . . ?
N1 Pr1 O4 C12 -13.3(5) . . . . ?
N3 Pr1 O4 C12 95.3(5) . . . . ?
O9 C14 O5 Pr1 163.1(4) . . . . ?
C13 C14 O5 Pr1 -19.6(8) . . . . ?
O3 Pr1 O5 C14 151.1(4) . . . . ?
O4 Pr1 O5 C14 34.4(5) . . . . ?
O6 Pr1 O5 C14 -88.6(5) . . . . ?
O1 Pr1 O5 C14 -143.3(5) . . . . ?
O2 Pr1 O5 C14 -44.3(5) . . . . ?
N2 Pr1 O5 C14 84.3(5) . . . . ?
N1 Pr1 O5 C14 152.0(5) . . . . ?
N3 Pr1 O5 C14 17.9(5) . . . . ?
N8 C15 O6 Pr1 167.3(4) . . . . ?
O3 Pr1 O6 C15 -4.1(5) . . . . ?
O5 Pr1 O6 C15 -146.1(5) . . . . ?
O4 Pr1 O6 C15 73.5(5) . . . . ?
O1 Pr1 O6 C15 -89.6(5) . . . . ?
O2 Pr1 O6 C15 166.5(5) . . . . ?
N2 Pr1 O6 C15 45.8(6) . . . . ?
N1 Pr1 O6 C15 -51.2(5) . . . . ?
N3 Pr1 O6 C15 135.1(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.255
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.140
####################################################################### 
# 
# 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_TbDTPAAQ
_database_code_depnum_ccdc_archive 'CCDC 1402444'
_audit_update_record             
;
2015-08-04 deposited with the CCDC.
2015-12-02 downloaded from the CCDC.
;



_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C38 H52 N9 O13 Tb'
_chemical_formula_sum            'C38 H52 N9 O13 Tb'
_chemical_formula_weight         1001
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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/n

loop_
_symmetry_equiv_pos_as_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                   10.9299(4)
_cell_length_b                   23.1611(10)
_cell_length_c                   17.1891(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.1320(10)
_cell_angle_gamma                90.00
_cell_volume                     4135.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2048
_exptl_absorpt_coefficient_mu    1.786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6946
_exptl_absorpt_correction_T_max  0.7631
_exptl_absorpt_process_details   SADABS(Sheldrick,1997)

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 0.5
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            36308
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0560
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         28.28
_reflns_number_total             10258
_reflns_number_gt                7689
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX II V2012.4-3'
_computing_cell_refinement       'Bruker APEX II V2012.4-3'
_computing_data_reduction        'Bruker APEX II V2012.4-3'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0551P)²+13.1271P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10258
_refine_ls_number_parameters     550
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0454
_refine_ls_wR_factor_ref         0.1231
_refine_ls_wR_factor_gt          0.1105
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.175368(19) 0.245773(8) 0.987076(12) 0.01418(7) Uani 1 1 d . . .
C1 C 0.3834(4) 0.16143(19) 1.1146(3) 0.0177(9) Uani 1 1 d . . .
C2 C 0.4026(5) 0.2154(2) 1.1678(3) 0.0211(10) Uani 1 1 d . . .
H2A H 0.3403 0.2163 1.1975 0.025 Uiso 1 1 calc R . .
H2B H 0.4883 0.2157 1.2072 0.025 Uiso 1 1 calc R . .
C3 C 0.3583(5) 0.31848(19) 1.1535(3) 0.0199(9) Uani 1 1 d . . .
H3A H 0.4334 0.3287 1.1990 0.024 Uiso 1 1 calc R . .
H3B H 0.2872 0.3115 1.1748 0.024 Uiso 1 1 calc R . .
C4 C 0.3246(5) 0.3679(2) 1.0919(3) 0.0238(10) Uani 1 1 d . . .
H4A H 0.3126 0.4030 1.1196 0.029 Uiso 1 1 calc R . .
H4B H 0.3958 0.3743 1.0705 0.029 Uiso 1 1 calc R . .
C5 C 0.0931(5) 0.3774(2) 1.0456(4) 0.0342(13) Uani 1 1 d . . .
H5A H 0.0963 0.4193 1.0482 0.041 Uiso 1 1 calc R . .
H5B H 0.0996 0.3632 1.0998 0.041 Uiso 1 1 calc R . .
C6 C -0.0350(5) 0.3592(2) 0.9867(4) 0.0324(13) Uani 1 1 d . . .
H6A H -0.1041 0.3777 1.0017 0.039 Uiso 1 1 calc R . .
H6B H -0.0406 0.3715 0.9318 0.039 Uiso 1 1 calc R . .
C7 C -0.1458(4) 0.2751(2) 0.9136(3) 0.0215(10) Uani 1 1 d . . .
H7A H -0.1349 0.2947 0.8663 0.026 Uiso 1 1 calc R . .
H7B H -0.2318 0.2833 0.9157 0.026 Uiso 1 1 calc R . .
C8 C -0.1283(4) 0.2106(2) 0.9067(3) 0.0181(9) Uani 1 1 d . . .
C27 C -0.2356(4) 0.1236(2) 0.8360(3) 0.0195(9) Uani 1 1 d . . .
C35 C -0.3436(5) 0.1081(2) 0.7691(3) 0.0256(10) Uani 1 1 d . . .
H35 H -0.4032 0.1368 0.7458 0.031 Uiso 1 1 calc R . .
C34 C -0.2792(5) 0.0140(2) 0.7736(3) 0.0288(12) Uani 1 1 d . . .
C33 C -0.3032(7) -0.0429(2) 0.7408(4) 0.0412(15) Uani 1 1 d . . .
H33 H -0.3736 -0.0504 0.6950 0.049 Uiso 1 1 calc R . .
C32 C -0.2208(7) -0.0864(2) 0.7779(5) 0.0461(17) Uani 1 1 d . . .
H32 H -0.2356 -0.1236 0.7566 0.055 Uiso 1 1 calc R . .
C31 C -0.1159(7) -0.0763(3) 0.8463(5) 0.0468(17) Uani 1 1 d . . .
H31 H -0.0625 -0.1068 0.8711 0.056 Uiso 1 1 calc R . .
C30 C -0.0897(6) -0.0210(2) 0.8783(4) 0.0389(14) Uani 1 1 d . . .
H30 H -0.0183 -0.0145 0.9238 0.047 Uiso 1 1 calc R . .
C29 C -0.1707(5) 0.0251(2) 0.8421(3) 0.0278(11) Uani 1 1 d . . .
C28 C -0.1489(5) 0.0823(2) 0.8731(3) 0.0241(10) Uani 1 1 d . . .
H28 H -0.0774 0.0912 0.9175 0.029 Uiso 1 1 calc R . .
C18 C 0.4456(4) 0.05972(19) 1.1142(3) 0.0182(9) Uani 1 1 d . . .
C19 C 0.3562(4) 0.04148(19) 1.0442(3) 0.0187(9) Uani 1 1 d . . .
H19 H 0.2976 0.0673 1.0111 0.022 Uiso 1 1 calc R . .
C20 C 0.3542(4) -0.01800(19) 1.0224(3) 0.0173(9) Uani 1 1 d . . .
C21 C 0.2610(5) -0.0416(2) 0.9532(3) 0.0222(10) Uani 1 1 d . . .
H21 H 0.2007 -0.0174 0.9182 0.027 Uiso 1 1 calc R . .
C22 C 0.2579(5) -0.0990(2) 0.9368(3) 0.0272(11) Uani 1 1 d . . .
H22 H 0.1949 -0.1138 0.8915 0.033 Uiso 1 1 calc R . .
C23 C 0.3507(5) -0.1362(2) 0.9887(3) 0.0258(11) Uani 1 1 d . . .
H23 H 0.3476 -0.1756 0.9777 0.031 Uiso 1 1 calc R . .
C24 C 0.4447(5) -0.1149(2) 1.0548(3) 0.0236(10) Uani 1 1 d . . .
H24 H 0.5069 -0.1395 1.0875 0.028 Uiso 1 1 calc R . .
C25 C 0.4476(4) -0.05544(19) 1.0737(3) 0.0197(9) Uani 1 1 d . . .
C26 C 0.5373(4) 0.0195(2) 1.1608(3) 0.0212(10) Uani 1 1 d . . .
H26 H 0.5995 0.0329 1.2075 0.025 Uiso 1 1 calc R . .
C9 C 0.5005(4) 0.2720(2) 1.0858(3) 0.0207(9) Uani 1 1 d . . .
H9A H 0.5563 0.2390 1.1049 0.025 Uiso 1 1 calc R . .
H9B H 0.5475 0.3062 1.1113 0.025 Uiso 1 1 calc R . .
C10 C 0.4713(4) 0.27693(18) 0.9946(3) 0.0192(9) Uani 1 1 d . . .
C11 C 0.2110(5) 0.3852(2) 0.9470(3) 0.0267(11) Uani 1 1 d . . .
H11A H 0.3004 0.3887 0.9493 0.032 Uiso 1 1 calc R . .
H11B H 0.1766 0.4239 0.9458 0.032 Uiso 1 1 calc R . .
C12 C 0.1377(5) 0.3546(2) 0.8679(3) 0.0278(11) Uani 1 1 d . . .
C13 C -0.0837(5) 0.2769(3) 1.0602(3) 0.0317(12) Uani 1 1 d . . .
H13A H -0.1668 0.2579 1.0419 0.038 Uiso 1 1 calc R . .
H13B H -0.0923 0.3107 1.0913 0.038 Uiso 1 1 calc R . .
C14 C 0.0135(5) 0.2358(2) 1.1168(3) 0.0254(11) Uani 1 1 d . . .
C15 C 0.2245(4) 0.18207(19) 0.8252(3) 0.0201(9) Uani 1 1 d . . .
H15 H 0.2737 0.2139 0.8206 0.024 Uiso 1 1 calc R . .
C16 C 0.1474(5) 0.0864(2) 0.7822(3) 0.0258(11) Uani 1 1 d . . .
H16A H 0.1510 0.0593 0.7407 0.039 Uiso 1 1 calc R . .
H16B H 0.0592 0.0958 0.7757 0.039 Uiso 1 1 calc R . .
H16C H 0.1862 0.0697 0.8353 0.039 Uiso 1 1 calc R . .
C17 C 0.2885(5) 0.1377(2) 0.7158(3) 0.0264(11) Uani 1 1 d . . .
H17A H 0.2703 0.1027 0.6846 0.040 Uiso 1 1 calc R . .
H17B H 0.3790 0.1399 0.7447 0.040 Uiso 1 1 calc R . .
H17C H 0.2635 0.1702 0.6796 0.040 Uiso 1 1 calc R . .
N1 N 0.3851(4) 0.26563(16) 1.1134(2) 0.0172(8) Uani 1 1 d . . .
N2 N 0.2056(4) 0.35615(17) 1.0226(3) 0.0220(8) Uani 1 1 d . . .
N3 N -0.0500(4) 0.29579(18) 0.9883(3) 0.0239(9) Uani 1 1 d . . .
N5 N -0.2301(4) 0.18228(16) 0.8592(2) 0.0202(8) Uani 1 1 d . . .
H4 H -0.3002 0.2018 0.8407 0.024 Uiso 1 1 calc R . .
N4 N 0.4563(4) 0.11607(16) 1.1472(2) 0.0185(8) Uani 1 1 d . . .
H5 H 0.5159 0.1216 1.1929 0.022 Uiso 1 1 calc R . .
N7 N -0.3655(4) 0.05624(18) 0.7376(3) 0.0292(10) Uani 1 1 d . . .
N6 N 0.5402(4) -0.03560(18) 1.1424(3) 0.0235(9) Uani 1 1 d . . .
N8 N 0.2162(4) 0.13840(16) 0.7746(2) 0.0190(8) Uani 1 1 d . . .
O1 O 0.3015(3) 0.16174(13) 1.0462(2) 0.0206(7) Uani 1 1 d . . .
O2 O -0.0233(3) 0.18785(13) 0.9425(2) 0.0216(7) Uani 1 1 d . . .
O3 O 0.3553(3) 0.27212(14) 0.9495(2) 0.0196(7) Uani 1 1 d . . .
O4 O 0.0951(3) 0.30455(13) 0.87186(19) 0.0197(7) Uani 1 1 d . . .
O5 O 0.1237(3) 0.23249(15) 1.1073(2) 0.0249(7) Uani 1 1 d . . .
O6 O 0.1701(3) 0.18286(14) 0.8782(2) 0.0216(7) Uani 1 1 d . . .
O7 O 0.5648(3) 0.28478(15) 0.9684(2) 0.0270(8) Uani 1 1 d . . .
O8 O 0.1287(5) 0.38102(19) 0.8029(3) 0.0602(15) Uani 1 1 d . . .
O9 O -0.0206(4) 0.20916(16) 1.1697(2) 0.0352(9) Uani 1 1 d . . .
O10 O 0.3592(8) 0.5165(3) 0.8844(5) 0.113(3) Uani 1 1 d . . .
N9 N 0.4885(7) 0.4455(3) 0.8702(5) 0.072(2) Uani 1 1 d . . .
C38 C 0.418(2) 0.4856(6) 0.8848(13) 0.254(14) Uani 1 1 d . . .
C36 C 0.4453(9) 0.3971(5) 0.8156(6) 0.080(3) Uani 1 1 d . . .
C37 C 0.6268(11) 0.4409(8) 0.9209(9) 0.167(8) Uani 1 1 d . . .
OW1 O 0.5366(3) 0.23765(15) 0.8181(2) 0.0283(8) Uani 1 1 d . . .
OW3 O 0.8952(4) 0.4675(2) 0.1024(3) 0.0522(12) Uani 1 1 d . . .
OW2 O 0.7415(6) 0.2072(3) 0.2032(5) 0.101(2) 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
Tb1 O5 2.327(3) . ?
Tb1 O3 2.334(3) . ?
Tb1 O4 2.338(3) . ?
Tb1 O6 2.358(3) . ?
Tb1 O1 2.419(3) . ?
Tb1 O2 2.463(3) . ?
Tb1 N2 2.625(4) . ?
Tb1 N1 2.662(4) . ?
Tb1 N3 2.728(4) . ?
C1 O1 1.237(5) . ?
C1 N4 1.332(6) . ?
C1 C2 1.524(6) . ?
C2 N1 1.467(6) . ?
C3 N1 1.478(5) . ?
C3 C4 1.526(7) . ?
C4 N2 1.490(6) . ?
C5 N2 1.488(6) . ?
C5 C6 1.510(7) . ?
C6 N3 1.479(6) . ?
C7 N3 1.461(6) . ?
C7 C8 1.517(6) . ?
C8 O2 1.238(5) . ?
C8 N5 1.331(6) . ?
C27 C28 1.357(7) . ?
C27 C35 1.413(7) . ?
C27 N5 1.413(6) . ?
C35 N7 1.309(6) . ?
C34 N7 1.366(7) . ?
C34 C29 1.410(8) . ?
C34 C33 1.426(7) . ?
C33 C32 1.369(9) . ?
C32 C31 1.383(10) . ?
C31 C30 1.388(8) . ?
C30 C29 1.402(8) . ?
C29 C28 1.421(7) . ?
C18 C19 1.360(7) . ?
C18 N4 1.413(6) . ?
C18 C26 1.419(6) . ?
C19 C20 1.426(6) . ?
C20 C21 1.414(6) . ?
C20 C25 1.418(6) . ?
C21 C22 1.356(7) . ?
C22 C23 1.416(7) . ?
C23 C24 1.365(7) . ?
C24 C25 1.412(6) . ?
C25 N6 1.374(6) . ?
C26 N6 1.316(6) . ?
C9 N1 1.486(6) . ?
C9 C10 1.504(7) . ?
C10 O7 1.252(5) . ?
C10 O3 1.268(5) . ?
C11 N2 1.480(7) . ?
C11 C12 1.522(7) . ?
C12 O8 1.250(6) . ?
C12 O4 1.259(6) . ?
C13 N3 1.462(7) . ?
C13 C14 1.529(8) . ?
C14 O9 1.249(6) . ?
C14 O5 1.267(6) . ?
C15 O6 1.234(6) . ?
C15 N8 1.319(6) . ?
C16 N8 1.447(6) . ?
C17 N8 1.463(6) . ?
O10 C38 0.963(10) . ?
N9 C38 1.277(11) . ?
N9 C36 1.444(12) . ?
N9 C37 1.495(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Tb1 O3 137.63(12) . . ?
O5 Tb1 O4 134.33(12) . . ?
O3 Tb1 O4 74.91(11) . . ?
O5 Tb1 O6 132.12(12) . . ?
O3 Tb1 O6 75.90(11) . . ?
O4 Tb1 O6 77.15(11) . . ?
O5 Tb1 O1 77.55(12) . . ?
O3 Tb1 O1 84.69(11) . . ?
O4 Tb1 O1 147.07(11) . . ?
O6 Tb1 O1 72.92(11) . . ?
O5 Tb1 O2 76.70(11) . . ?
O3 Tb1 O2 142.52(11) . . ?
O4 Tb1 O2 89.52(11) . . ?
O6 Tb1 O2 67.38(11) . . ?
O1 Tb1 O2 91.40(10) . . ?
O5 Tb1 N2 88.28(13) . . ?
O3 Tb1 N2 75.74(12) . . ?
O4 Tb1 N2 67.47(12) . . ?
O6 Tb1 N2 139.15(12) . . ?
O1 Tb1 N2 132.20(11) . . ?
O2 Tb1 N2 129.63(11) . . ?
O5 Tb1 N1 71.56(12) . . ?
O3 Tb1 N1 66.08(11) . . ?
O4 Tb1 N1 126.26(11) . . ?
O6 Tb1 N1 123.79(11) . . ?
O1 Tb1 N1 64.05(11) . . ?
O2 Tb1 N1 143.13(11) . . ?
N2 Tb1 N1 68.15(12) . . ?
O5 Tb1 N3 65.17(13) . . ?
O3 Tb1 N3 137.02(12) . . ?
O4 Tb1 N3 69.96(12) . . ?
O6 Tb1 N3 117.99(12) . . ?
O1 Tb1 N3 137.43(12) . . ?
O2 Tb1 N3 61.50(11) . . ?
N2 Tb1 N3 68.50(12) . . ?
N1 Tb1 N3 118.11(12) . . ?
O1 C1 N4 124.4(4) . . ?
O1 C1 C2 119.3(4) . . ?
N4 C1 C2 116.3(4) . . ?
N1 C2 C1 107.6(4) . . ?
N1 C3 C4 109.8(4) . . ?
N2 C4 C3 112.3(4) . . ?
N2 C5 C6 113.6(4) . . ?
N3 C6 C5 110.5(4) . . ?
N3 C7 C8 108.5(4) . . ?
O2 C8 N5 124.4(4) . . ?
O2 C8 C7 120.0(4) . . ?
N5 C8 C7 115.6(4) . . ?
C28 C27 C35 119.2(5) . . ?
C28 C27 N5 125.6(4) . . ?
C35 C27 N5 115.1(4) . . ?
N7 C35 C27 124.6(5) . . ?
N7 C34 C29 122.1(5) . . ?
N7 C34 C33 117.8(5) . . ?
C29 C34 C33 120.1(5) . . ?
C32 C33 C34 118.8(6) . . ?
C33 C32 C31 121.5(6) . . ?
C32 C31 C30 120.5(6) . . ?
C31 C30 C29 120.2(6) . . ?
C30 C29 C34 118.9(5) . . ?
C30 C29 C28 122.3(5) . . ?
C34 C29 C28 118.8(5) . . ?
C27 C28 C29 118.0(5) . . ?
C19 C18 N4 126.1(4) . . ?
C19 C18 C26 118.8(4) . . ?
N4 C18 C26 115.1(4) . . ?
C18 C19 C20 118.7(4) . . ?
C21 C20 C25 118.5(4) . . ?
C21 C20 C19 122.9(4) . . ?
C25 C20 C19 118.6(4) . . ?
C22 C21 C20 121.3(4) . . ?
C21 C22 C23 119.9(5) . . ?
C24 C23 C22 120.6(5) . . ?
C23 C24 C25 120.1(4) . . ?
N6 C25 C24 118.8(4) . . ?
N6 C25 C20 121.7(4) . . ?
C24 C25 C20 119.6(5) . . ?
N6 C26 C18 124.5(5) . . ?
N1 C9 C10 114.4(4) . . ?
O7 C10 O3 124.4(5) . . ?
O7 C10 C9 117.0(4) . . ?
O3 C10 C9 118.6(4) . . ?
N2 C11 C12 114.8(4) . . ?
O8 C12 O4 124.9(5) . . ?
O8 C12 C11 116.4(4) . . ?
O4 C12 C11 118.7(4) . . ?
N3 C13 C14 114.6(4) . . ?
O9 C14 O5 125.1(5) . . ?
O9 C14 C13 117.8(5) . . ?
O5 C14 C13 117.1(4) . . ?
O6 C15 N8 123.3(4) . . ?
C2 N1 C3 111.4(4) . . ?
C2 N1 C9 109.1(4) . . ?
C3 N1 C9 112.2(4) . . ?
C2 N1 Tb1 106.9(3) . . ?
C3 N1 Tb1 106.1(3) . . ?
C9 N1 Tb1 111.0(3) . . ?
C11 N2 C5 110.1(4) . . ?
C11 N2 C4 110.8(4) . . ?
C5 N2 C4 108.4(4) . . ?
C11 N2 Tb1 106.0(3) . . ?
C5 N2 Tb1 109.3(3) . . ?
C4 N2 Tb1 112.3(3) . . ?
C7 N3 C13 110.1(4) . . ?
C7 N3 C6 111.2(4) . . ?
C13 N3 C6 111.8(4) . . ?
C7 N3 Tb1 104.9(3) . . ?
C13 N3 Tb1 110.2(3) . . ?
C6 N3 Tb1 108.4(3) . . ?
C8 N5 C27 127.0(4) . . ?
C1 N4 C18 126.6(4) . . ?
C35 N7 C34 117.2(5) . . ?
C26 N6 C25 117.6(4) . . ?
C15 N8 C16 120.6(4) . . ?
C15 N8 C17 121.5(4) . . ?
C16 N8 C17 117.5(4) . . ?
C1 O1 Tb1 123.6(3) . . ?
C8 O2 Tb1 120.9(3) . . ?
C10 O3 Tb1 128.4(3) . . ?
C12 O4 Tb1 122.3(3) . . ?
C14 O5 Tb1 127.5(3) . . ?
C15 O6 Tb1 134.2(3) . . ?
C38 N9 C36 126.7(14) . . ?
C38 N9 C37 119.8(15) . . ?
C36 N9 C37 113.0(8) . . ?
O10 C38 N9 169(2) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.417
_refine_diff_density_min         -1.531
_refine_diff_density_rms         0.154
