# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_974597
_audit_block_doi                 10.5517/cc11q4mj
_database_code_depnum_ccdc_archive 'CCDC 974597'
_audit_update_record             
;
2014-11-17 deposited with the CCDC.
2014-11-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H43 Eu N8 O15'
_chemical_formula_weight         1075.82

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'
Eu Eu -0.1578 3.6682 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P c c n'

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

_cell_length_a                   13.166(3)
_cell_length_b                   34.112(7)
_cell_length_c                   10.078(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4526.2(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    11803
_cell_measurement_theta_min      2.6143
_cell_measurement_theta_max      28.9186

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2184
_exptl_absorpt_coefficient_mu    1.465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6845
_exptl_absorpt_correction_T_max  0.7582
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 2007)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      193(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10771
_diffrn_reflns_av_R_equivalents  0.0878
_diffrn_reflns_av_sigmaI/netI    0.1296
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.32
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3787
_reflns_number_gt                1980
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.1076P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0020(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3787
_refine_ls_number_parameters     301
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.1498
_refine_ls_R_factor_gt           0.0764
_refine_ls_wR_factor_ref         0.2236
_refine_ls_wR_factor_gt          0.1858
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.002
_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
Eu1 Eu 0.2500 0.7500 0.03590(7) 0.0397(4) Uani 1 2 d S . 2
O1 O 0.1853(7) 0.79177(19) 0.1952(7) 0.045(2) Uani 1 1 d . A 2
O5 O 0.1026(8) 0.7738(2) -0.0862(7) 0.052(2) Uani 1 1 d D B 2
H5A H 0.0495 0.7681 -0.0443 0.063 Uiso 1 1 calc R B 2
O4 O -0.0962(7) 1.2178(2) 0.3665(7) 0.055(2) Uani 1 1 d D . 2
O3 O 0.0282(8) 1.2176(3) 0.5106(9) 0.080(3) Uani 1 1 d D . 2
O2 O 0.2073(7) 0.8056(2) 0.4063(7) 0.045(2) Uani 1 1 d . . 2
N3 N 0.1375(8) 0.9794(2) 0.1871(9) 0.045(3) Uani 1 1 d . A 2
H3A H 0.1335 0.9930 0.2589 0.054 Uiso 1 1 d R A 2
N1 N 0.1303(8) 0.9856(3) -0.0441(9) 0.046(3) Uani 1 1 d . A 2
N2 N 0.1091(9) 1.0666(3) -0.0081(12) 0.062(3) Uani 1 1 d . A 2
H2A H 0.1037 1.0921 0.0027 0.074 Uiso 1 1 calc R A 2
N4A N 0.133(2) 1.0561(8) 0.219(3) 0.059(4) Uani 0.50 1 d PU A 2
H4A H 0.1732 1.0428 0.2730 0.070 Uiso 0.50 1 calc PR A 2
C21 C 0.1909(10) 0.8146(3) 0.2886(10) 0.035(3) Uani 1 1 d . . .
C18 C 0.1713(8) 0.8579(3) 0.2600(10) 0.033(3) Uani 1 1 d . A .
C6 C 0.1208(10) 1.0109(3) -0.1499(13) 0.050(3) Uani 1 1 d . . .
C17 C 0.1651(9) 0.8719(3) 0.1323(11) 0.043(3) Uani 1 1 d . . .
H17 H 0.1678 0.8538 0.0608 0.051 Uiso 1 1 calc R A .
C15 C 0.1497(8) 0.9378(3) 0.2078(11) 0.036(3) Uani 1 1 d U . .
C20 C 0.1553(10) 0.9242(3) 0.3369(10) 0.046(3) Uani 1 1 d . A .
H20 H 0.1517 0.9424 0.4082 0.055 Uiso 1 1 calc R . .
C16 C 0.1549(8) 0.9114(3) 0.1042(11) 0.038(3) Uani 1 1 d . A .
H16 H 0.1516 0.9203 0.0149 0.046 Uiso 1 1 calc R . .
C5 C 0.1096(9) 1.0507(3) -0.1355(13) 0.043(3) Uani 1 1 d . A .
C7 C 0.1307(9) 1.0005(3) 0.0737(13) 0.044(3) Uani 1 1 d . . .
C10 C -0.0113(12) 1.1060(3) 0.2347(13) 0.058(4) Uani 1 1 d . A .
H10 H -0.0549 1.0903 0.1814 0.070 Uiso 1 1 calc R . .
C11 C -0.0459(10) 1.1413(3) 0.2798(11) 0.045(3) Uani 1 1 d . . .
H11 H -0.1120 1.1503 0.2569 0.054 Uiso 1 1 calc R . .
C2 C 0.1114(12) 1.0205(4) -0.3874(13) 0.071(4) Uani 1 1 d . . .
H2 H 0.1124 1.0103 -0.4750 0.085 Uiso 1 1 calc R A .
C19 C 0.1660(9) 0.8855(3) 0.3639(10) 0.037(3) Uani 1 1 d . . .
H19 H 0.1698 0.8768 0.4534 0.045 Uiso 1 1 calc R A .
C12 C 0.0178(11) 1.1642(3) 0.3605(11) 0.051(3) Uani 1 1 d . . .
C1 C 0.1237(10) 0.9952(4) -0.2803(11) 0.053(4) Uani 1 1 d . A .
H1 H 0.1337 0.9679 -0.2942 0.063 Uiso 1 1 calc R . .
C22 C -0.0189(7) 1.2031(3) 0.4161(10) 0.052(3) Uani 1 1 d D . .
C8 C 0.1170(11) 1.0431(3) 0.0980(17) 0.066(4) Uani 1 1 d . A .
C4 C 0.0961(11) 1.0761(4) -0.2394(13) 0.059(4) Uani 1 1 d . . .
H44 H 0.0859 1.1033 -0.2243 0.071 Uiso 1 1 calc R A .
C3 C 0.0978(10) 1.0609(4) -0.3682(16) 0.062(4) Uani 1 1 d . A .
H3 H 0.0897 1.0779 -0.4423 0.075 Uiso 1 1 calc R . .
C9 C 0.0858(12) 1.0920(3) 0.2643(11) 0.055(4) Uani 1 1 d . . .
C14 C 0.1511(12) 1.1158(3) 0.3451(12) 0.060(4) Uani 1 1 d . . .
H14 H 0.2186 1.1076 0.3637 0.072 Uiso 1 1 calc R . .
C13 C 0.1149(9) 1.1506(3) 0.3953(10) 0.055(3) Uani 1 1 d . . .
H13 H 0.1558 1.1655 0.4542 0.066 Uiso 1 1 calc R . .
O6 O 0.5563(9) 0.7044(3) 0.1971(10) 0.072(6) Uani 0.50 1 d PR . .
H5B H 0.082(11) 0.783(4) -0.157(7) 0.086 Uiso 1 1 d D . .
N4B N 0.098(2) 1.0532(8) 0.234(3) 0.059(4) Uani 0.50 1 d PU A 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O1 2.309(7) 2_565 ?
Eu1 O1 2.309(7) . ?
Eu1 O2 2.372(7) 8_575 ?
Eu1 O2 2.372(7) 7_655 ?
Eu1 O5 2.436(9) . ?
Eu1 O5 2.436(9) 2_565 ?
Eu1 O4 2.505(8) 3_575 ?
Eu1 O4 2.505(8) 4_545 ?
O1 C21 1.224(11) . ?
O5 H5A 0.8400 . ?
O5 H5B 0.823(10) . ?
O4 C22 1.241(2) . ?
O4 Eu1 2.505(8) 3_475 ?
O3 C22 1.240(2) . ?
O2 C21 1.243(11) . ?
O2 Eu1 2.372(7) 7_656 ?
N3 C7 1.352(13) . ?
N3 C15 1.446(13) . ?
N3 H3A 0.8601 . ?
N1 C7 1.291(13) . ?
N1 C6 1.377(14) . ?
N2 C8 1.341(16) . ?
N2 C5 1.394(15) . ?
N2 H2A 0.8800 . ?
N4A C8 1.32(3) . ?
N4A C9 1.45(3) . ?
N4A H4A 0.8800 . ?
C21 C18 1.527(14) . ?
C18 C17 1.375(13) . ?
C18 C19 1.408(13) . ?
C6 C5 1.372(15) . ?
C6 C1 1.420(16) . ?
C17 C16 1.383(13) . ?
C17 H17 0.9500 . ?
C15 C16 1.379(13) . ?
C15 C20 1.383(14) . ?
C20 C19 1.357(13) . ?
C20 H20 0.9500 . ?
C16 H16 0.9500 . ?
C5 C4 1.372(15) . ?
C7 C8 1.483(15) . ?
C10 C11 1.367(16) . ?
C10 C9 1.396(19) . ?
C10 H10 0.9500 . ?
C11 C12 1.406(16) . ?
C11 H11 0.9500 . ?
C2 C3 1.404(17) . ?
C2 C1 1.391(16) . ?
C2 H2 0.9500 . ?
C19 H19 0.9500 . ?
C12 C13 1.405(17) . ?
C12 C22 1.517(15) . ?
C1 H1 0.9500 . ?
C8 N4B 1.44(3) . ?
C4 C3 1.397(18) . ?
C4 H44 0.9500 . ?
C3 H3 0.9500 . ?
C9 N4B 1.37(3) . ?
C9 C14 1.436(18) . ?
C14 C13 1.375(15) . ?
C14 H14 0.9500 . ?
C13 H13 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Eu1 O1 91.9(4) 2_565 . ?
O1 Eu1 O2 88.7(2) 2_565 8_575 ?
O1 Eu1 O2 142.1(3) . 8_575 ?
O1 Eu1 O2 142.1(3) 2_565 7_655 ?
O1 Eu1 O2 88.7(2) . 7_655 ?
O2 Eu1 O2 113.2(4) 8_575 7_655 ?
O1 Eu1 O5 148.2(3) 2_565 . ?
O1 Eu1 O5 81.5(3) . . ?
O2 Eu1 O5 78.4(3) 8_575 . ?
O2 Eu1 O5 69.2(3) 7_655 . ?
O1 Eu1 O5 81.5(3) 2_565 2_565 ?
O1 Eu1 O5 148.2(3) . 2_565 ?
O2 Eu1 O5 69.2(3) 8_575 2_565 ?
O2 Eu1 O5 78.4(3) 7_655 2_565 ?
O5 Eu1 O5 119.3(4) . 2_565 ?
O1 Eu1 O4 72.5(3) 2_565 3_575 ?
O1 Eu1 O4 75.8(3) . 3_575 ?
O2 Eu1 O4 139.3(3) 8_575 3_575 ?
O2 Eu1 O4 71.0(3) 7_655 3_575 ?
O5 Eu1 O4 134.1(3) . 3_575 ?
O5 Eu1 O4 72.6(3) 2_565 3_575 ?
O1 Eu1 O4 75.8(3) 2_565 4_545 ?
O1 Eu1 O4 72.5(3) . 4_545 ?
O2 Eu1 O4 71.0(3) 8_575 4_545 ?
O2 Eu1 O4 139.3(3) 7_655 4_545 ?
O5 Eu1 O4 72.6(3) . 4_545 ?
O5 Eu1 O4 134.1(3) 2_565 4_545 ?
O4 Eu1 O4 133.8(3) 3_575 4_545 ?
C21 O1 Eu1 154.9(9) . . ?
Eu1 O5 H5A 109.5 . . ?
Eu1 O5 H5B 145(10) . . ?
H5A O5 H5B 104.4 . . ?
C22 O4 Eu1 133.1(7) . 3_475 ?
C21 O2 Eu1 139.8(7) . 7_656 ?
C7 N3 C15 130.7(9) . . ?
C7 N3 H3A 115.0 . . ?
C15 N3 H3A 114.4 . . ?
C7 N1 C6 117.8(10) . . ?
C8 N2 C5 120.2(11) . . ?
C8 N2 H2A 119.9 . . ?
C5 N2 H2A 119.9 . . ?
C8 N4A C9 120(2) . . ?
C8 N4A H4A 119.8 . . ?
C9 N4A H4A 119.8 . . ?
O1 C21 O2 125.9(10) . . ?
O1 C21 C18 117.4(9) . . ?
O2 C21 C18 116.6(10) . . ?
C17 C18 C19 117.5(9) . . ?
C17 C18 C21 121.5(10) . . ?
C19 C18 C21 120.9(9) . . ?
C5 C6 N1 123.2(12) . . ?
C5 C6 C1 118.3(12) . . ?
N1 C6 C1 118.5(10) . . ?
C18 C17 C16 122.4(11) . . ?
C18 C17 H17 118.8 . . ?
C16 C17 H17 118.8 . . ?
C16 C15 C20 119.5(9) . . ?
C16 C15 N3 122.5(9) . . ?
C20 C15 N3 118.0(9) . . ?
C19 C20 C15 121.3(10) . . ?
C19 C20 H20 119.4 . . ?
C15 C20 H20 119.4 . . ?
C15 C16 C17 119.0(10) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 H16 120.5 . . ?
C6 C5 C4 124.0(12) . . ?
C6 C5 N2 118.8(11) . . ?
C4 C5 N2 117.2(11) . . ?
N1 C7 N3 124.6(10) . . ?
N1 C7 C8 122.4(12) . . ?
N3 C7 C8 112.9(11) . . ?
C11 C10 C9 122.3(12) . . ?
C11 C10 H10 118.9 . . ?
C9 C10 H10 118.9 . . ?
C10 C11 C12 118.9(13) . . ?
C10 C11 H11 120.5 . . ?
C12 C11 H11 120.5 . . ?
C3 C2 C1 121.2(13) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
C20 C19 C18 120.4(10) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C13 C12 C11 120.2(11) . . ?
C13 C12 C22 119.1(11) . . ?
C11 C12 C22 120.6(11) . . ?
C2 C1 C6 118.7(12) . . ?
C2 C1 H1 120.6 . . ?
C6 C1 H1 120.6 . . ?
O3 C22 O4 123.8(11) . . ?
O3 C22 C12 118.4(9) . . ?
O4 C22 C12 117.8(9) . . ?
N4A C8 N2 123.4(16) . . ?
N2 C8 N4B 127.2(15) . . ?
N4A C8 C7 117.6(18) . . ?
N2 C8 C7 117.6(13) . . ?
N4B C8 C7 114.4(16) . . ?
C5 C4 C3 118.2(13) . . ?
C5 C4 H44 120.9 . . ?
C3 C4 H44 120.9 . . ?
C2 C3 C4 119.6(13) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
N4B C9 C10 112.8(16) . . ?
N4B C9 C14 127.2(17) . . ?
C10 C9 C14 118.5(12) . . ?
C10 C9 N4A 128.0(16) . . ?
C14 C9 N4A 113.4(17) . . ?
C13 C14 C9 119.2(13) . . ?
C13 C14 H14 120.4 . . ?
C9 C14 H14 120.4 . . ?
C14 C13 C12 120.7(11) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C9 N4B C8 118(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Eu1 O1 C21 62.8(14) 2_565 . . . ?
O2 Eu1 O1 C21 153.1(14) 8_575 . . . ?
O2 Eu1 O1 C21 -79.3(15) 7_655 . . . ?
O5 Eu1 O1 C21 -148.4(15) . . . . ?
O5 Eu1 O1 C21 -14.0(17) 2_565 . . . ?
O4 Eu1 O1 C21 -8.6(14) 3_575 . . . ?
O4 Eu1 O1 C21 137.3(15) 4_545 . . . ?
Eu1 O1 C21 O2 -76(2) . . . . ?
Eu1 O1 C21 C18 107.1(16) . . . . ?
Eu1 O2 C21 O1 6(2) 7_656 . . . ?
Eu1 O2 C21 C18 -176.5(7) 7_656 . . . ?
O1 C21 C18 C17 -10.9(17) . . . . ?
O2 C21 C18 C17 171.7(11) . . . . ?
O1 C21 C18 C19 173.4(11) . . . . ?
O2 C21 C18 C19 -4.0(17) . . . . ?
C7 N1 C6 C5 -1.5(18) . . . . ?
C7 N1 C6 C1 177.9(12) . . . . ?
C19 C18 C17 C16 0.7(17) . . . . ?
C21 C18 C17 C16 -175.1(10) . . . . ?
C7 N3 C15 C16 -1.1(19) . . . . ?
C7 N3 C15 C20 179.4(12) . . . . ?
C16 C15 C20 C19 0.0(19) . . . . ?
N3 C15 C20 C19 179.5(11) . . . . ?
C20 C15 C16 C17 0.4(16) . . . . ?
N3 C15 C16 C17 -179.0(10) . . . . ?
C18 C17 C16 C15 -0.8(17) . . . . ?
N1 C6 C5 C4 -177.4(12) . . . . ?
C1 C6 C5 C4 3.1(19) . . . . ?
N1 C6 C5 N2 1.0(19) . . . . ?
C1 C6 C5 N2 -178.5(11) . . . . ?
C8 N2 C5 C6 -1.7(18) . . . . ?
C8 N2 C5 C4 176.8(13) . . . . ?
C6 N1 C7 N3 178.7(11) . . . . ?
C6 N1 C7 C8 2.7(18) . . . . ?
C15 N3 C7 N1 3(2) . . . . ?
C15 N3 C7 C8 179.1(11) . . . . ?
C9 C10 C11 C12 -1.0(19) . . . . ?
C15 C20 C19 C18 -0.1(19) . . . . ?
C17 C18 C19 C20 -0.2(17) . . . . ?
C21 C18 C19 C20 175.6(11) . . . . ?
C10 C11 C12 C13 -0.8(18) . . . . ?
C10 C11 C12 C22 -178.1(11) . . . . ?
C3 C2 C1 C6 1(2) . . . . ?
C5 C6 C1 C2 -2.2(19) . . . . ?
N1 C6 C1 C2 178.4(12) . . . . ?
Eu1 O4 C22 O3 -41.6(19) 3_475 . . . ?
Eu1 O4 C22 C12 136.2(9) 3_475 . . . ?
C13 C12 C22 O3 -14.5(17) . . . . ?
C11 C12 C22 O3 162.8(11) . . . . ?
C13 C12 C22 O4 167.6(11) . . . . ?
C11 C12 C22 O4 -15.1(17) . . . . ?
C9 N4A C8 N2 38(3) . . . . ?
C9 N4A C8 N4B -70(6) . . . . ?
C9 N4A C8 C7 -156.0(17) . . . . ?
C5 N2 C8 N4A 168.8(18) . . . . ?
C5 N2 C8 N4B -166.5(18) . . . . ?
C5 N2 C8 C7 2.8(19) . . . . ?
N1 C7 C8 N4A -170.3(17) . . . . ?
N3 C7 C8 N4A 13(2) . . . . ?
N1 C7 C8 N2 -3(2) . . . . ?
N3 C7 C8 N2 -179.8(12) . . . . ?
N1 C7 C8 N4B 167.2(16) . . . . ?
N3 C7 C8 N4B -9(2) . . . . ?
C6 C5 C4 C3 -3(2) . . . . ?
N2 C5 C4 C3 179.1(12) . . . . ?
C1 C2 C3 C4 0(2) . . . . ?
C5 C4 C3 C2 1(2) . . . . ?
C11 C10 C9 N4B 167.0(17) . . . . ?
C11 C10 C9 C14 0.1(19) . . . . ?
C11 C10 C9 N4A -177.4(17) . . . . ?
C8 N4A C9 N4B 83(6) . . . . ?
C8 N4A C9 C10 37(3) . . . . ?
C8 N4A C9 C14 -140.7(18) . . . . ?
N4B C9 C14 C13 -162.0(18) . . . . ?
C10 C9 C14 C13 2.8(18) . . . . ?
N4A C9 C14 C13 -179.4(15) . . . . ?
C9 C14 C13 C12 -4.6(17) . . . . ?
C11 C12 C13 C14 3.7(17) . . . . ?
C22 C12 C13 C14 -179.0(10) . . . . ?
C10 C9 N4B C8 80(2) . . . . ?
C14 C9 N4B C8 -114(2) . . . . ?
N4A C9 N4B C8 -62(5) . . . . ?
N4A C8 N4B C9 75(6) . . . . ?
N2 C8 N4B C9 -11(3) . . . . ?
C7 C8 N4B C9 179.0(16) . . . . ?

_diffrn_measured_fraction_theta_max 0.950
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.950
_refine_diff_density_max         0.946
_refine_diff_density_min         -1.261
_refine_diff_density_rms         0.144

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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
_platon_squeeze_void_content
1 0.250 0.250 -0.026 258 85 ' '
2 0.750 0.750 -0.030 258 86 ' '
_platon_squeeze_details          
;
The highly disoeder solvent region in each molecule of MOF which has been removed 
by SQUEEZE contains four water molecules. the four water molecules contain (4*10=40) 
electrons. In per unit cell, 160 electrons (40*4)is reasonable agreement with the 
171 electrons calculated from SQUEEZE.
;
####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_974598
_audit_block_doi                 10.5517/cc11q4nk
_database_code_depnum_ccdc_archive 'CCDC 974598'
_audit_update_record             
;
2014-11-17 deposited with the CCDC.
2014-11-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H43 Er N8 O15'
_chemical_formula_weight         1091.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
Er Er -0.2590 4.9580 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P c c n'

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

_cell_length_a                   13.138(3)
_cell_length_b                   33.947(7)
_cell_length_c                   10.013(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4465.8(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    9638
_cell_measurement_theta_min      3.5084
_cell_measurement_theta_max      28.7517

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2204
_exptl_absorpt_coefficient_mu    1.960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6298
_exptl_absorpt_correction_T_max  0.6953
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 2007)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       dtintegrate.ref
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13058
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.51
_diffrn_reflns_theta_max         26.01
_reflns_number_total             4268
_reflns_number_gt                2921
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku, 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku, 2007)'
_computing_data_reduction        'CrystalClear (Rigaku, 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0720P)²+0.0000P] 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         4268
_refine_ls_number_parameters     292
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0466
_refine_ls_wR_factor_ref         0.1367
_refine_ls_wR_factor_gt          0.1221
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_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
Er1 Er 0.2500 0.2500 0.03191(3) 0.02734(16) Uani 1 2 d S . .
O1 O 0.1841(3) 0.29039(11) 0.1882(4) 0.0363(9) Uani 1 1 d . . .
O2 O 0.2091(3) 0.30406(10) 0.4011(4) 0.0342(9) Uani 1 1 d . . .
O3 O 0.0257(3) 0.71693(15) 0.5140(4) 0.0590(13) Uani 1 1 d . A .
O4 O -0.1035(3) 0.71638(12) 0.3692(3) 0.0418(10) Uani 1 1 d . . .
O5 O 0.1026(3) 0.27308(12) -0.0866(4) 0.0394(9) Uani 1 1 d . . .
H5A H 0.1069 0.2794 -0.1675 0.009(12) Uiso 1 1 d R . .
H5B H 0.0601 0.2547 -0.0796 0.06(2) Uiso 1 1 d R . .
N1 N 0.1329(3) 0.48493(14) -0.0465(5) 0.0339(11) Uani 1 1 d . . .
N2 N 0.1094(4) 0.56651(14) -0.0055(5) 0.0392(12) Uani 1 1 d . A .
H2 H 0.1033 0.5921 0.0071 0.047 Uiso 1 1 calc R . .
N3 N 0.1393(3) 0.47812(13) 0.1858(5) 0.0304(11) Uani 1 1 d . . .
H3 H 0.1285 0.4943 0.2556 0.026(15) Uiso 1 1 d R . .
N4B N 0.1041(13) 0.5532(11) 0.231(4) 0.036(4) Uani 0.50 1 d P A 2
C1 C 0.1215(5) 0.4956(2) -0.2834(6) 0.0442(17) Uani 1 1 d . . .
H1 H 0.1312 0.4682 -0.2976 0.053 Uiso 1 1 calc R . .
C2 C 0.1075(5) 0.5205(2) -0.3907(7) 0.0506(17) Uani 1 1 d . . .
H2A H 0.1066 0.5100 -0.4786 0.061 Uiso 1 1 calc R . .
C3 C 0.0948(5) 0.5605(2) -0.3721(7) 0.0510(18) Uani 1 1 d . . .
H3A H 0.0866 0.5773 -0.4472 0.061 Uiso 1 1 calc R . .
C4 C 0.0941(5) 0.5763(2) -0.2445(7) 0.0432(16) Uani 1 1 d . . .
H4 H 0.0841 0.6037 -0.2315 0.052 Uiso 1 1 calc R . .
C5 C 0.1081(4) 0.55144(17) -0.1356(6) 0.0353(14) Uani 1 1 d . . .
C6 C 0.1212(4) 0.51104(17) -0.1525(6) 0.0369(14) Uani 1 1 d . . .
C7 C 0.1315(4) 0.50006(17) 0.0725(6) 0.0334(13) Uani 1 1 d . A .
C8 C 0.1199(4) 0.54264(17) 0.1003(7) 0.0439(16) Uani 1 1 d . . .
C9 C 0.0881(5) 0.59217(18) 0.2639(6) 0.0413(15) Uani 1 1 d . . .
C10 C -0.0099(5) 0.6052(2) 0.2329(6) 0.0480(16) Uani 1 1 d . A .
H10 H -0.0528 0.5895 0.1781 0.058 Uiso 1 1 calc R . .
C11 C -0.0447(4) 0.64082(19) 0.2814(5) 0.0386(15) Uani 1 1 d . . .
H11 H -0.1117 0.6493 0.2601 0.046 Uiso 1 1 calc R A .
C12 C 0.0167(4) 0.66437(16) 0.3605(5) 0.0324(13) Uani 1 1 d . A .
C13 C 0.1144(4) 0.65148(19) 0.3906(6) 0.0399(14) Uani 1 1 d . . .
H13 H 0.1568 0.6673 0.4458 0.048 Uiso 1 1 calc R A .
C14 C 0.1512(5) 0.61623(19) 0.3419(6) 0.0450(15) Uani 1 1 d . A .
H14 H 0.2190 0.6083 0.3611 0.054 Uiso 1 1 calc R . .
C15 C 0.1507(4) 0.43718(15) 0.2041(5) 0.0248(12) Uani 1 1 d . . .
C16 C 0.1540(4) 0.41055(16) 0.0999(5) 0.0318(12) Uani 1 1 d . . .
H16 H 0.1497 0.4196 0.0104 0.038 Uiso 1 1 calc R . .
C17 C 0.1638(4) 0.37040(16) 0.1258(5) 0.0289(12) Uani 1 1 d . . .
H17 H 0.1652 0.3522 0.0536 0.035 Uiso 1 1 calc R . .
C18 C 0.1713(4) 0.35669(15) 0.2558(5) 0.0248(11) Uani 1 1 d . . .
C19 C 0.1674(4) 0.38392(15) 0.3617(5) 0.0277(12) Uani 1 1 d . . .
H19 H 0.1717 0.3750 0.4514 0.033 Uiso 1 1 calc R . .
C20 C 0.1575(4) 0.42346(15) 0.3352(5) 0.0304(12) Uani 1 1 d . . .
H20 H 0.1552 0.4417 0.4071 0.037 Uiso 1 1 calc R . .
C21 C 0.1897(4) 0.31405(16) 0.2849(5) 0.0276(12) Uani 1 1 d . . .
C22 C -0.0221(5) 0.70221(18) 0.4189(6) 0.0402(14) Uani 1 1 d . . .
N4A N 0.1394(14) 0.5557(11) 0.220(4) 0.036(4) Uani 0.50 1 d P A 1
H4A H 0.1811 0.5406 0.2695 0.043 Uiso 0.50 1 d PR A 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O1 2.253(4) . ?
Er1 O1 2.253(4) 2 ?
Er1 O2 2.317(4) 8_565 ?
Er1 O2 2.317(4) 7_655 ?
Er1 O5 2.403(4) . ?
Er1 O5 2.403(4) 2 ?
Er1 O4 2.447(4) 3_565 ?
Er1 O4 2.447(4) 4_545 ?
O1 C21 1.260(6) . ?
O2 C21 1.239(6) . ?
O2 Er1 2.317(4) 7_656 ?
O3 C22 1.245(7) . ?
O4 C22 1.273(7) . ?
O4 Er1 2.447(4) 3_465 ?
N1 C7 1.298(7) . ?
N1 C6 1.391(7) . ?
N2 C8 1.341(8) . ?
N2 C5 1.401(7) . ?
N3 C7 1.361(7) . ?
N3 C15 1.410(6) . ?
N4B C8 1.37(4) . ?
N4B C9 1.38(4) . ?
C1 C2 1.379(9) . ?
C1 C6 1.411(9) . ?
C2 C3 1.380(9) . ?
C3 C4 1.385(10) . ?
C4 C5 1.390(8) . ?
C5 C6 1.392(8) . ?
C7 C8 1.480(8) . ?
C8 N4A 1.30(4) . ?
C9 C10 1.397(9) . ?
C9 C14 1.401(9) . ?
C9 N4A 1.48(4) . ?
C10 C11 1.381(9) . ?
C11 C12 1.385(8) . ?
C12 C13 1.390(8) . ?
C12 C22 1.501(8) . ?
C13 C14 1.380(8) . ?
C15 C16 1.381(7) . ?
C15 C20 1.395(7) . ?
C16 C17 1.393(7) . ?
C17 C18 1.386(7) . ?
C18 C19 1.408(7) . ?
C18 C21 1.496(7) . ?
C19 C20 1.375(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
O1 Er1 O1 92.05(19) . 2 ?
O1 Er1 O2 141.73(14) . 8_565 ?
O1 Er1 O2 89.98(13) 2 8_565 ?
O1 Er1 O2 89.98(13) . 7_655 ?
O1 Er1 O2 141.73(14) 2 7_655 ?
O2 Er1 O2 111.19(18) 8_565 7_655 ?
O1 Er1 O5 80.48(14) . . ?
O1 Er1 O5 148.33(14) 2 . ?
O2 Er1 O5 78.03(14) 8_565 . ?
O2 Er1 O5 69.48(14) 7_655 . ?
O1 Er1 O5 148.33(14) . 2 ?
O1 Er1 O5 80.48(14) 2 2 ?
O2 Er1 O5 69.48(14) 8_565 2 ?
O2 Er1 O5 78.03(14) 7_655 2 ?
O5 Er1 O5 120.83(18) . 2 ?
O1 Er1 O4 74.80(13) . 3_565 ?
O1 Er1 O4 72.58(13) 2 3_565 ?
O2 Er1 O4 141.27(14) 8_565 3_565 ?
O2 Er1 O4 71.15(13) 7_655 3_565 ?
O5 Er1 O4 132.98(14) . 3_565 ?
O5 Er1 O4 73.60(14) 2 3_565 ?
O1 Er1 O4 72.58(13) . 4_545 ?
O1 Er1 O4 74.80(13) 2 4_545 ?
O2 Er1 O4 71.15(13) 8_565 4_545 ?
O2 Er1 O4 141.27(14) 7_655 4_545 ?
O5 Er1 O4 73.60(14) . 4_545 ?
O5 Er1 O4 132.98(14) 2 4_545 ?
O4 Er1 O4 132.29(17) 3_565 4_545 ?
C21 O1 Er1 154.0(4) . . ?
C21 O2 Er1 142.7(4) . 7_656 ?
C22 O4 Er1 132.7(3) . 3_465 ?
C7 N1 C6 116.5(5) . . ?
C8 N2 C5 121.1(5) . . ?
C7 N3 C15 131.0(5) . . ?
C8 N4B C9 120(3) . . ?
C2 C1 C6 119.7(7) . . ?
C1 C2 C3 120.9(7) . . ?
C4 C3 C2 120.3(6) . . ?
C3 C4 C5 119.2(7) . . ?
C4 C5 C6 121.2(6) . . ?
C4 C5 N2 120.7(6) . . ?
C6 C5 N2 118.1(5) . . ?
N1 C6 C5 123.3(6) . . ?
N1 C6 C1 118.2(6) . . ?
C5 C6 C1 118.5(6) . . ?
N1 C7 N3 123.2(5) . . ?
N1 C7 C8 124.1(6) . . ?
N3 C7 C8 112.6(6) . . ?
N4A C8 N2 122.7(17) . . ?
N2 C8 N4B 125.4(16) . . ?
N4A C8 C7 119.1(17) . . ?
N2 C8 C7 116.9(6) . . ?
N4B C8 C7 116.8(17) . . ?
N4B C9 C10 113.0(11) . . ?
N4B C9 C14 127.0(13) . . ?
C10 C9 C14 119.0(6) . . ?
C10 C9 N4A 128.3(13) . . ?
C14 C9 N4A 112.6(12) . . ?
C11 C10 C9 120.3(6) . . ?
C12 C11 C10 120.9(5) . . ?
C11 C12 C13 118.7(5) . . ?
C11 C12 C22 121.3(5) . . ?
C13 C12 C22 119.9(5) . . ?
C14 C13 C12 121.3(6) . . ?
C13 C14 C9 119.7(6) . . ?
C16 C15 C20 119.3(5) . . ?
C16 C15 N3 123.4(5) . . ?
C20 C15 N3 117.3(5) . . ?
C15 C16 C17 120.2(5) . . ?
C18 C17 C16 120.6(5) . . ?
C17 C18 C19 119.0(5) . . ?
C17 C18 C21 121.3(5) . . ?
C19 C18 C21 119.6(5) . . ?
C20 C19 C18 120.0(5) . . ?
C19 C20 C15 120.9(5) . . ?
O2 C21 O1 124.0(5) . . ?
O2 C21 C18 118.8(5) . . ?
O1 C21 C18 117.2(5) . . ?
O3 C22 O4 124.8(6) . . ?
O3 C22 C12 118.1(5) . . ?
O4 C22 C12 117.1(5) . . ?
C8 N4A C9 118(2) . . ?

_diffrn_measured_fraction_theta_max 0.968
_diffrn_reflns_theta_full        26.01
_diffrn_measured_fraction_theta_full 0.968
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.106

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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
_platon_squeeze_void_content
1 0.750 0.250 -0.009 411 70 ' '
2 0.250 0.750 -0.026 411 70 ' '
_platon_squeeze_details          
;
The highly disoeder solvent region in each molecule of MOF which has been removed 
by SQUEEZE contains five water molecules.
;

####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_974661
_database_code_depnum_ccdc_archive 'CCDC 974661'
_audit_update_record             
;
2014-09-19 deposited with the CCDC.
2014-11-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H25 N5 O6 '
_chemical_formula_weight         491.50

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'

_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                   9.826(2)
_cell_length_b                   11.358(2)
_cell_length_c                   11.609(2)
_cell_angle_alpha                66.07(3)
_cell_angle_beta                 84.95(3)
_cell_angle_gamma                78.63(3)
_cell_volume                     1161.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    4492
_cell_measurement_theta_min      2.6365
_cell_measurement_theta_max      28.6795

_exptl_crystal_description       prism
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             516
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8581
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 2007)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       dtintegrate.ref
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            8826
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.15
_diffrn_reflns_theta_max         25.36
_reflns_number_total             4152
_reflns_number_gt                3413
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku, 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku, 2007)'
_computing_data_reduction        'CrystalClear (Rigaku, 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0612P)²+0.1258P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4152
_refine_ls_number_parameters     339
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0442
_refine_ls_wR_factor_ref         0.1176
_refine_ls_wR_factor_gt          0.1092
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_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
O1 O -0.34545(13) 1.57573(13) -0.31734(12) 0.0365(3) Uani 1 1 d . . .
H1 H -0.404(2) 1.657(2) -0.347(2) 0.055 Uiso 1 1 d . . .
O2 O -0.24258(13) 1.67638(12) -0.22875(12) 0.0384(3) Uani 1 1 d . . .
O3 O 0.86026(12) 0.48564(12) 0.44040(11) 0.0336(3) Uani 1 1 d . . .
O4 O 0.89524(12) 0.66014(12) 0.47116(11) 0.0327(3) Uani 1 1 d . . .
H4 H 0.9704 0.6135 0.4973 0.049 Uiso 1 1 calc R . .
N1 N 0.12155(14) 0.98138(13) -0.12713(12) 0.0248(3) Uani 1 1 d . . .
N2 N 0.35323(14) 0.80083(13) 0.00143(13) 0.0263(3) Uani 1 1 d . . .
N3 N 0.16027(14) 1.12283(13) -0.03938(12) 0.0240(3) Uani 1 1 d . . .
H3 H 0.2110 1.1311 0.0127 0.029 Uiso 1 1 calc R . .
N4 N 0.37320(14) 0.92787(13) 0.11055(13) 0.0256(3) Uani 1 1 d . . .
H4A H 0.3459 1.0024 0.1156 0.031 Uiso 1 1 calc R . .
C1 C 0.08646(19) 0.83394(18) -0.21926(16) 0.0309(4) Uani 1 1 d . . .
H1A H 0.0085 0.8923 -0.2609 0.037 Uiso 1 1 calc R . .
C2 C 0.1268(2) 0.71886(18) -0.23461(17) 0.0348(4) Uani 1 1 d . . .
H2 H 0.0758 0.6991 -0.2861 0.042 Uiso 1 1 calc R . .
C3 C 0.2447(2) 0.63064(19) -0.17315(17) 0.0361(5) Uani 1 1 d . . .
H3A H 0.2715 0.5525 -0.1839 0.043 Uiso 1 1 calc R . .
C4 C 0.32065(19) 0.65883(18) -0.09740(17) 0.0332(4) Uani 1 1 d . . .
H4B H 0.3996 0.6004 -0.0579 0.040 Uiso 1 1 calc R . .
C5 C 0.16192(17) 0.86477(16) -0.14113(15) 0.0251(4) Uani 1 1 d . . .
C6 C 0.27991(17) 0.77558(16) -0.07915(15) 0.0248(4) Uani 1 1 d . . .
C7 C 0.19177(17) 1.00450(16) -0.05080(15) 0.0224(4) Uani 1 1 d . . .
C8 C 0.30887(17) 0.90717(16) 0.02129(15) 0.0229(4) Uani 1 1 d . . .
C9 C 0.50348(18) 0.70511(17) 0.23161(16) 0.0287(4) Uani 1 1 d . . .
H9 H 0.4470 0.6661 0.2029 0.034 Uiso 1 1 calc R . .
C10 C 0.55889(17) 0.89559(17) 0.24628(15) 0.0253(4) Uani 1 1 d . . .
H10 H 0.5385 0.9848 0.2278 0.030 Uiso 1 1 calc R . .
C11 C 0.66869(17) 0.81818(17) 0.32479(15) 0.0267(4) Uani 1 1 d . . .
H11 H 0.7225 0.8561 0.3574 0.032 Uiso 1 1 calc R . .
C12 C 0.61254(18) 0.62954(17) 0.31103(15) 0.0285(4) Uani 1 1 d . . .
H12 H 0.6284 0.5392 0.3356 0.034 Uiso 1 1 calc R . .
C13 C 0.69900(17) 0.68448(16) 0.35524(15) 0.0252(4) Uani 1 1 d . . .
C14 C -0.04110(17) 1.23931(16) -0.18204(15) 0.0235(4) Uani 1 1 d . . .
H14 H -0.0415 1.1687 -0.2032 0.028 Uiso 1 1 calc R . .
C15 C 0.05773(18) 1.34103(16) -0.07173(16) 0.0272(4) Uani 1 1 d . . .
H15 H 0.1245 1.3380 -0.0181 0.033 Uiso 1 1 calc R . .
C16 C 0.05794(16) 1.23215(15) -0.09974(15) 0.0219(4) Uani 1 1 d . . .
C17 C -0.13935(17) 1.35262(16) -0.23239(15) 0.0250(4) Uani 1 1 d . . .
H17 H -0.2055 1.3568 -0.2871 0.030 Uiso 1 1 calc R . .
C18 C -0.04014(18) 1.45212(16) -0.12266(16) 0.0277(4) Uani 1 1 d . . .
H18 H -0.0387 1.5235 -0.1030 0.033 Uiso 1 1 calc R . .
C19 C -0.14120(17) 1.45980(16) -0.20297(14) 0.0233(4) Uani 1 1 d . . .
C20 C -0.24695(18) 1.58048(17) -0.25065(15) 0.0281(4) Uani 1 1 d . . .
C21 C 0.82479(18) 0.60041(17) 0.42684(15) 0.0275(4) Uani 1 1 d . . .
C22 C 0.47858(16) 0.84117(16) 0.19462(15) 0.0233(4) Uani 1 1 d . . .
C23 C 0.8240(2) 0.1533(2) 0.5822(2) 0.0443(5) Uani 1 1 d . . .
H23A H 0.8084 0.2453 0.5636 0.066 Uiso 1 1 calc R . .
H23B H 0.9121 0.1287 0.5478 0.066 Uiso 1 1 calc R . .
H23C H 0.8238 0.1049 0.6719 0.066 Uiso 1 1 calc R . .
C24 C 0.7250(2) -0.0081(2) 0.5388(2) 0.0518(6) Uani 1 1 d . . .
H24A H 0.6394 -0.0179 0.5127 0.078 Uiso 1 1 calc R . .
H24B H 0.7425 -0.0672 0.6250 0.078 Uiso 1 1 calc R . .
H24C H 0.7996 -0.0275 0.4865 0.078 Uiso 1 1 calc R . .
C25 C 0.6124(2) 0.21872(19) 0.46504(17) 0.0352(4) Uani 1 1 d . . .
H25 H 0.6121 0.3022 0.4611 0.042 Uiso 1 1 calc R . .
O5 O 0.51788(14) 0.20487(13) 0.41259(13) 0.0431(4) Uani 1 1 d . . .
N5 N 0.71534(15) 0.12467(14) 0.52718(13) 0.0310(4) Uani 1 1 d . . .
O6 O 0.36089(14) 0.19333(13) 0.08382(13) 0.0341(3) Uani 1 1 d . . .
H6A H 0.333(3) 0.234(2) 0.134(2) 0.064(8) Uiso 1 1 d . . .
H6B H 0.446(3) 0.216(3) 0.045(2) 0.085(9) 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
O1 C20 1.314(2) . ?
O1 H1 0.93(2) . ?
O2 C20 1.224(2) . ?
O3 C21 1.229(2) . ?
O4 C21 1.317(2) . ?
O4 H4 0.8200 . ?
N1 C7 1.303(2) . ?
N1 C5 1.376(2) . ?
N2 C8 1.305(2) . ?
N2 C6 1.376(2) . ?
N3 C7 1.376(2) . ?
N3 C16 1.404(2) . ?
N3 H3 0.8600 . ?
N4 C8 1.378(2) . ?
N4 C22 1.411(2) . ?
N4 H4A 0.8600 . ?
C1 C2 1.367(2) . ?
C1 C5 1.405(2) . ?
C1 H1A 0.9300 . ?
C2 C3 1.401(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.368(3) . ?
C3 H3A 0.9300 . ?
C4 C6 1.403(2) . ?
C4 H4B 0.9300 . ?
C5 C6 1.407(2) . ?
C7 C8 1.471(2) . ?
C9 C12 1.380(2) . ?
C9 C22 1.401(2) . ?
C9 H9 0.9300 . ?
C10 C11 1.384(2) . ?
C10 C22 1.393(2) . ?
C10 H10 0.9300 . ?
C11 C13 1.387(2) . ?
C11 H11 0.9300 . ?
C12 C13 1.386(2) . ?
C12 H12 0.9300 . ?
C13 C21 1.484(2) . ?
C14 C17 1.389(2) . ?
C14 C16 1.391(2) . ?
C14 H14 0.9300 . ?
C15 C18 1.372(2) . ?
C15 C16 1.400(2) . ?
C15 H15 0.9300 . ?
C17 C19 1.388(2) . ?
C17 H17 0.9300 . ?
C18 C19 1.388(2) . ?
C18 H18 0.9300 . ?
C19 C20 1.480(2) . ?
C23 N5 1.442(2) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 N5 1.443(2) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 O5 1.222(2) . ?
C25 N5 1.328(2) . ?
C25 H25 0.9300 . ?
O6 H6A 0.88(3) . ?
O6 H6B 0.95(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C20 O1 H1 108.4(14) . . ?
C21 O4 H4 109.5 . . ?
C7 N1 C5 118.29(14) . . ?
C8 N2 C6 118.56(14) . . ?
C7 N3 C16 129.84(14) . . ?
C7 N3 H3 115.1 . . ?
C16 N3 H3 115.1 . . ?
C8 N4 C22 127.63(14) . . ?
C8 N4 H4A 116.2 . . ?
C22 N4 H4A 116.2 . . ?
C2 C1 C5 120.51(17) . . ?
C2 C1 H1A 119.7 . . ?
C5 C1 H1A 119.7 . . ?
C1 C2 C3 120.27(17) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
C4 C3 C2 120.36(17) . . ?
C4 C3 H3A 119.8 . . ?
C2 C3 H3A 119.8 . . ?
C3 C4 C6 120.21(17) . . ?
C3 C4 H4B 119.9 . . ?
C6 C4 H4B 119.9 . . ?
N1 C5 C1 120.20(15) . . ?
N1 C5 C6 120.79(15) . . ?
C1 C5 C6 119.00(16) . . ?
N2 C6 C4 119.96(15) . . ?
N2 C6 C5 120.39(15) . . ?
C4 C6 C5 119.62(16) . . ?
N1 C7 N3 120.31(15) . . ?
N1 C7 C8 120.98(15) . . ?
N3 C7 C8 118.68(14) . . ?
N2 C8 N4 119.30(15) . . ?
N2 C8 C7 120.60(15) . . ?
N4 C8 C7 120.10(14) . . ?
C12 C9 C22 119.41(16) . . ?
C12 C9 H9 120.3 . . ?
C22 C9 H9 120.3 . . ?
C11 C10 C22 120.68(16) . . ?
C11 C10 H10 119.7 . . ?
C22 C10 H10 119.7 . . ?
C10 C11 C13 120.47(16) . . ?
C10 C11 H11 119.8 . . ?
C13 C11 H11 119.8 . . ?
C9 C12 C13 121.81(16) . . ?
C9 C12 H12 119.1 . . ?
C13 C12 H12 119.1 . . ?
C12 C13 C11 118.52(15) . . ?
C12 C13 C21 119.18(15) . . ?
C11 C13 C21 122.21(16) . . ?
C17 C14 C16 119.56(16) . . ?
C17 C14 H14 120.2 . . ?
C16 C14 H14 120.2 . . ?
C18 C15 C16 120.59(16) . . ?
C18 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
C14 C16 C15 118.90(15) . . ?
C14 C16 N3 125.53(15) . . ?
C15 C16 N3 115.56(15) . . ?
C19 C17 C14 121.59(16) . . ?
C19 C17 H17 119.2 . . ?
C14 C17 H17 119.2 . . ?
C15 C18 C19 121.16(16) . . ?
C15 C18 H18 119.4 . . ?
C19 C18 H18 119.4 . . ?
C18 C19 C17 118.18(15) . . ?
C18 C19 C20 118.42(15) . . ?
C17 C19 C20 123.39(16) . . ?
O2 C20 O1 123.08(17) . . ?
O2 C20 C19 122.30(16) . . ?
O1 C20 C19 114.62(15) . . ?
O3 C21 O4 123.64(16) . . ?
O3 C21 C13 121.97(16) . . ?
O4 C21 C13 114.37(15) . . ?
C10 C22 C9 118.81(15) . . ?
C10 C22 N4 117.06(15) . . ?
C9 C22 N4 124.09(15) . . ?
N5 C23 H23A 109.5 . . ?
N5 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N5 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N5 C24 H24A 109.5 . . ?
N5 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N5 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O5 C25 N5 125.50(19) . . ?
O5 C25 H25 117.2 . . ?
N5 C25 H25 117.2 . . ?
C25 N5 C23 120.68(16) . . ?
C25 N5 C24 121.54(17) . . ?
C23 N5 C24 117.75(16) . . ?
H6A O6 H6B 110(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 C1 C2 C3 -0.5(3) . . . . ?
C1 C2 C3 C4 -0.1(3) . . . . ?
C2 C3 C4 C6 0.9(3) . . . . ?
C7 N1 C5 C1 177.91(14) . . . . ?
C7 N1 C5 C6 -2.9(2) . . . . ?
C2 C1 C5 N1 179.33(15) . . . . ?
C2 C1 C5 C6 0.2(2) . . . . ?
C8 N2 C6 C4 -176.67(15) . . . . ?
C8 N2 C6 C5 1.7(2) . . . . ?
C3 C4 C6 N2 177.19(15) . . . . ?
C3 C4 C6 C5 -1.2(2) . . . . ?
N1 C5 C6 N2 3.1(2) . . . . ?
C1 C5 C6 N2 -177.74(14) . . . . ?
N1 C5 C6 C4 -178.50(14) . . . . ?
C1 C5 C6 C4 0.7(2) . . . . ?
C5 N1 C7 N3 176.21(13) . . . . ?
C5 N1 C7 C8 -1.6(2) . . . . ?
C16 N3 C7 N1 0.1(2) . . . . ?
C16 N3 C7 C8 177.94(14) . . . . ?
C6 N2 C8 N4 173.92(14) . . . . ?
C6 N2 C8 C7 -6.3(2) . . . . ?
C22 N4 C8 N2 -5.7(2) . . . . ?
C22 N4 C8 C7 174.50(14) . . . . ?
N1 C7 C8 N2 6.5(2) . . . . ?
N3 C7 C8 N2 -171.35(14) . . . . ?
N1 C7 C8 N4 -173.67(14) . . . . ?
N3 C7 C8 N4 8.5(2) . . . . ?
C22 C10 C11 C13 -1.2(2) . . . . ?
C22 C9 C12 C13 -0.2(2) . . . . ?
C9 C12 C13 C11 4.2(2) . . . . ?
C9 C12 C13 C21 -172.26(15) . . . . ?
C10 C11 C13 C12 -3.5(2) . . . . ?
C10 C11 C13 C21 172.88(14) . . . . ?
C17 C14 C16 C15 -1.3(2) . . . . ?
C17 C14 C16 N3 178.04(14) . . . . ?
C18 C15 C16 C14 1.2(2) . . . . ?
C18 C15 C16 N3 -178.19(14) . . . . ?
C7 N3 C16 C14 3.8(3) . . . . ?
C7 N3 C16 C15 -176.81(15) . . . . ?
C16 C14 C17 C19 0.2(2) . . . . ?
C16 C15 C18 C19 0.0(2) . . . . ?
C15 C18 C19 C17 -1.1(2) . . . . ?
C15 C18 C19 C20 177.64(15) . . . . ?
C14 C17 C19 C18 1.0(2) . . . . ?
C14 C17 C19 C20 -177.67(15) . . . . ?
C18 C19 C20 O2 5.1(2) . . . . ?
C17 C19 C20 O2 -176.20(16) . . . . ?
C18 C19 C20 O1 -174.53(14) . . . . ?
C17 C19 C20 O1 4.1(2) . . . . ?
C12 C13 C21 O3 5.4(2) . . . . ?
C11 C13 C21 O3 -170.95(16) . . . . ?
C12 C13 C21 O4 -176.08(14) . . . . ?
C11 C13 C21 O4 7.6(2) . . . . ?
C11 C10 C22 C9 5.2(2) . . . . ?
C11 C10 C22 N4 -176.86(14) . . . . ?
C12 C9 C22 C10 -4.5(2) . . . . ?
C12 C9 C22 N4 177.74(15) . . . . ?
C8 N4 C22 C10 159.44(15) . . . . ?
C8 N4 C22 C9 -22.7(2) . . . . ?
O5 C25 N5 C23 178.04(17) . . . . ?
O5 C25 N5 C24 -0.1(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        25.36
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.042
