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

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

data_cd15340
_database_code_depnum_ccdc_archive 'CCDC 1484784'
_audit_update_record             
;
2016-06-13 deposited with the CCDC.
2016-08-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H24 N18 O21'
_chemical_formula_weight         732.47

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'

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

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

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

_cell_length_a                   6.8808(18)
_cell_length_b                   13.354(3)
_cell_length_c                   15.942(4)
_cell_angle_alpha                89.832(6)
_cell_angle_beta                 81.391(6)
_cell_angle_gamma                75.199(6)
_cell_volume                     1399.3(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1054
_cell_measurement_theta_min      5.172
_cell_measurement_theta_max      43.396

_exptl_crystal_description       prismatic
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_F_000             756
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.167
_shelx_estimated_absorpt_T_min   0.964
_shelx_estimated_absorpt_T_max   0.988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5611
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7773
_diffrn_reflns_av_unetI/netI     0.0740
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.578
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.976
_reflns_number_total             4926
_reflns_number_gt                3137
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0837P)²+0.1099P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4926
_refine_ls_number_parameters     466
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_gt           0.0693
_refine_ls_wR_factor_ref         0.1805
_refine_ls_wR_factor_gt          0.1579
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.7423(5) 0.62815(19) 0.68378(17) 0.0570(9) Uani 1 1 d . . . . .
O2 O 0.7871(4) 0.41410(18) 0.49408(17) 0.0473(7) Uani 1 1 d . . . . .
O3 O 0.8252(4) 0.29627(18) 0.58991(18) 0.0496(8) Uani 1 1 d . . . . .
O4 O 0.9602(5) 0.3750(2) 0.7294(2) 0.0672(9) Uani 1 1 d . . . . .
O5 O 0.6467(5) 0.4477(3) 0.7687(2) 0.0657(9) Uani 1 1 d . . . . .
O6 O 0.6701(5) 0.5822(2) 0.38961(17) 0.0581(9) Uani 1 1 d . . . . .
O7 O 0.5883(4) 0.7085(2) 0.30852(18) 0.0516(8) Uani 1 1 d . . . . .
O8 O 0.7597(5) 0.8506(2) 0.33031(18) 0.0524(8) Uani 1 1 d . . . . .
O9 O 0.7034(5) 0.9058(2) 0.45931(18) 0.0590(9) Uani 1 1 d . . . . .
O10 O 0.2325(4) 0.74176(18) 0.05378(16) 0.0454(7) Uani 1 1 d . . . . .
O11 O 0.3976(6) 0.6949(3) -0.1123(2) 0.0801(11) Uani 1 1 d . . . . .
O12 O 0.1611(6) 0.7917(2) -0.1701(2) 0.0786(11) Uani 1 1 d . . . . .
O13 O 0.2435(5) 0.9720(2) -0.16095(17) 0.0590(9) Uani 1 1 d . . . . .
O14 O 0.2151(5) 1.0283(2) -0.03182(17) 0.0573(8) Uani 1 1 d . . . . .
O15 O 0.1810(6) 0.9011(2) 0.35327(17) 0.0626(9) Uani 1 1 d . . . . .
O16 O 0.3472(5) 1.0151(2) 0.35554(19) 0.0660(10) Uani 1 1 d . . . . .
O17 O 0.2434(6) 1.1478(2) 0.24606(19) 0.0654(9) Uani 1 1 d . . . . .
O18 O 0.3140(5) 1.0811(2) 0.11986(18) 0.0571(8) Uani 1 1 d . . . . .
O19 O 0.7679(6) 0.4296(3) 0.2463(3) 0.0977(13) Uani 1 1 d D . . . .
H19A H 0.6791 0.4031 0.2170 0.117 Uiso 1 1 d DR U . . .
H19B H 0.6909 0.4592 0.3074 0.117 Uiso 1 1 d DR U . . .
O20 O 0.8577(7) 0.6040(3) 0.8603(3) 0.0747(10) Uani 1 1 d D . . . .
O21 O 0.7191(8) 0.4793(3) 0.9868(3) 0.0927(13) Uani 1 1 d D . . . .
N1 N 0.7196(5) 0.7772(2) 0.5778(2) 0.0432(9) Uani 1 1 d . . . . .
H1A H 0.7325 0.7577 0.6286 0.052 Uiso 1 1 calc R U . . .
H1B H 0.7126 0.8406 0.5654 0.052 Uiso 1 1 calc R U . . .
N2 N 0.7227(5) 0.6117(2) 0.5428(2) 0.0346(8) Uani 1 1 d . . . . .
N3 N 0.7975(5) 0.3894(2) 0.5704(2) 0.0370(8) Uani 1 1 d . . . . .
N4 N 0.7978(6) 0.4260(2) 0.7153(2) 0.0443(9) Uani 1 1 d . . . . .
N5 N 0.6499(5) 0.6742(2) 0.3738(2) 0.0388(8) Uani 1 1 d . . . . .
N6 N 0.7174(5) 0.8366(2) 0.4056(2) 0.0403(8) Uani 1 1 d . . . . .
N7 N 0.2136(5) 0.8070(2) 0.20973(19) 0.0437(9) Uani 1 1 d . . . . .
H7A H 0.2046 0.7576 0.1772 0.052 Uiso 1 1 calc R U . . .
H7B H 0.2035 0.7999 0.2637 0.052 Uiso 1 1 calc R U . . .
N8 N 0.2578(5) 0.9017(2) 0.09201(19) 0.0340(8) Uani 1 1 d . . . . .
N9 N 0.2737(6) 0.7766(2) -0.1170(2) 0.0435(8) Uani 1 1 d . . . . .
N10 N 0.2360(5) 0.9545(2) -0.08389(19) 0.0411(8) Uani 1 1 d . . . . .
N11 N 0.2607(5) 0.9653(2) 0.3172(2) 0.0398(8) Uani 1 1 d . . . . .
N12 N 0.2749(5) 1.0736(2) 0.1979(2) 0.0404(8) Uani 1 1 d . . . . .
N13 N 0.7947(5) 0.2514(2) 0.3674(2) 0.0488(9) Uani 1 1 d . . . . .
H13A H 0.8025 0.2952 0.4054 0.059 Uiso 1 1 calc R U . . .
H13B H 0.7905 0.2696 0.3157 0.059 Uiso 1 1 calc R U . . .
N14 N 0.7764(5) 0.0894(2) 0.3307(2) 0.0476(9) Uani 1 1 d . . . . .
H14A H 0.7723 0.0277 0.3449 0.057 Uiso 1 1 calc R U . . .
H14B H 0.7721 0.1068 0.2789 0.057 Uiso 1 1 calc R U . . .
N15 N 0.7955(6) 0.1291(3) 0.4667(2) 0.0557(10) Uani 1 1 d . . . . .
H15A H 0.8033 0.1728 0.5048 0.067 Uiso 1 1 calc R U . . .
H15B H 0.7919 0.0672 0.4802 0.067 Uiso 1 1 calc R U . . .
N16 N 0.7432(5) 0.7939(2) 0.1464(2) 0.0503(9) Uani 1 1 d . . . . .
H16A H 0.7402 0.8562 0.1317 0.060 Uiso 1 1 calc R U . . .
H16B H 0.7378 0.7788 0.1991 0.060 Uiso 1 1 calc R U . . .
N17 N 0.7644(6) 0.7444(3) 0.0080(2) 0.0547(10) Uani 1 1 d . . . . .
H17A H 0.7695 0.6977 -0.0299 0.066 Uiso 1 1 calc R U . . .
H17B H 0.7647 0.8064 -0.0066 0.066 Uiso 1 1 calc R U . . .
N18 N 0.7557(7) 0.6271(3) 0.1114(2) 0.0697(12) Uani 1 1 d . . . . .
H18A H 0.7608 0.5798 0.0740 0.084 Uiso 1 1 calc R U . . .
H18B H 0.7503 0.6126 0.1641 0.084 Uiso 1 1 calc R U . . .
C1 C 0.7109(5) 0.7111(2) 0.5201(2) 0.0307(8) Uani 1 1 d . . . . .
C2 C 0.6901(6) 0.7400(3) 0.4345(2) 0.0352(9) Uani 1 1 d . . . . .
C3 C 0.7452(6) 0.5731(3) 0.6228(2) 0.0373(9) Uani 1 1 d . . . . .
C4 C 0.7783(6) 0.4631(3) 0.6298(2) 0.0369(9) Uani 1 1 d . . . . .
C5 C 0.2424(5) 0.8923(3) 0.1773(2) 0.0295(8) Uani 1 1 d . . . . .
C6 C 0.2585(5) 0.9762(3) 0.2285(2) 0.0307(8) Uani 1 1 d . . . . .
C7 C 0.2463(5) 0.8276(3) 0.0334(2) 0.0325(8) Uani 1 1 d . . . . .
C8 C 0.2554(6) 0.8573(3) -0.0543(2) 0.0338(9) Uani 1 1 d . . . . .
C9 C 0.7892(6) 0.1570(3) 0.3882(2) 0.0353(9) Uani 1 1 d . . . . .
C10 C 0.7562(6) 0.7211(3) 0.0880(3) 0.0428(10) Uani 1 1 d . . . . .
H2 H 0.731(5) 0.568(3) 0.504(2) 0.031(10) Uiso 1 1 d . . . . .
H8 H 0.265(5) 0.959(2) 0.075(2) 0.015(8) Uiso 1 1 d . . . . .
H20A H 0.814(14) 0.641(6) 0.822(4) 0.19(4) Uiso 1 1 d D . . . .
H20B H 0.979(5) 0.575(8) 0.851(7) 0.26(6) Uiso 1 1 d D . . . .
H21A H 0.749(11) 0.517(5) 0.949(3) 0.14(3) Uiso 1 1 d D . . . .
H21B H 0.75(2) 0.419(4) 1.001(8) 0.34(8) Uiso 1 1 d 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 C3 1.216(4) . ?
O2 N3 1.268(4) . ?
O3 N3 1.254(4) . ?
O4 N4 1.204(4) . ?
O5 N4 1.213(5) . ?
O6 N5 1.231(4) . ?
O7 N5 1.226(4) . ?
O8 N6 1.217(4) . ?
O9 N6 1.237(4) . ?
O10 C7 1.213(4) . ?
O11 N9 1.211(4) . ?
O12 N9 1.214(4) . ?
O13 N10 1.246(4) . ?
O14 N10 1.255(4) . ?
O15 N11 1.229(4) . ?
O16 N11 1.219(4) . ?
O17 N12 1.210(4) . ?
O18 N12 1.243(4) . ?
O19 H19A 0.9554 . ?
O19 H19B 1.0617 . ?
O20 H20A 0.83(2) . ?
O20 H20B 0.82(2) . ?
O21 H21A 0.82(2) . ?
O21 H21B 0.82(2) . ?
N1 C1 1.295(4) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N2 C1 1.361(4) . ?
N2 C3 1.388(5) . ?
N2 H2 0.83(3) . ?
N3 C4 1.335(4) . ?
N4 C4 1.462(5) . ?
N5 C2 1.412(5) . ?
N6 C2 1.416(5) . ?
N7 C5 1.298(4) . ?
N7 H7A 0.8600 . ?
N7 H7B 0.8600 . ?
N8 C5 1.356(4) . ?
N8 C7 1.388(4) . ?
N8 H8 0.83(3) . ?
N9 C8 1.441(4) . ?
N10 C8 1.361(5) . ?
N11 C6 1.423(4) . ?
N12 C6 1.413(4) . ?
N13 C9 1.311(4) . ?
N13 H13A 0.8600 . ?
N13 H13B 0.8600 . ?
N14 C9 1.316(4) . ?
N14 H14A 0.8600 . ?
N14 H14B 0.8600 . ?
N15 C9 1.309(5) . ?
N15 H15A 0.8600 . ?
N15 H15B 0.8600 . ?
N16 C10 1.326(5) . ?
N16 H16A 0.8600 . ?
N16 H16B 0.8600 . ?
N17 C10 1.307(5) . ?
N17 H17A 0.8600 . ?
N17 H17B 0.8600 . ?
N18 C10 1.310(5) . ?
N18 H18A 0.8600 . ?
N18 H18B 0.8600 . ?
C1 C2 1.436(5) . ?
C3 C4 1.435(5) . ?
C5 C6 1.424(4) . ?
C7 C8 1.448(5) . ?

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
H19A O19 H19B 109.5 . . ?
H20A O20 H20B 115(10) . . ?
H21A O21 H21B 141(10) . . ?
C1 N1 H1A 120.0 . . ?
C1 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
C1 N2 C3 126.1(3) . . ?
C1 N2 H2 117(2) . . ?
C3 N2 H2 116(2) . . ?
O3 N3 O2 120.1(3) . . ?
O3 N3 C4 120.4(3) . . ?
O2 N3 C4 119.6(3) . . ?
O4 N4 O5 123.2(4) . . ?
O4 N4 C4 119.1(4) . . ?
O5 N4 C4 117.7(4) . . ?
O7 N5 O6 120.6(3) . . ?
O7 N5 C2 121.0(3) . . ?
O6 N5 C2 118.4(3) . . ?
O8 N6 O9 120.6(3) . . ?
O8 N6 C2 121.3(3) . . ?
O9 N6 C2 118.1(3) . . ?
C5 N7 H7A 120.0 . . ?
C5 N7 H7B 120.0 . . ?
H7A N7 H7B 120.0 . . ?
C5 N8 C7 126.3(3) . . ?
C5 N8 H8 115(2) . . ?
C7 N8 H8 119(2) . . ?
O11 N9 O12 122.9(3) . . ?
O11 N9 C8 117.9(3) . . ?
O12 N9 C8 119.2(3) . . ?
O13 N10 O14 119.2(3) . . ?
O13 N10 C8 122.1(3) . . ?
O14 N10 C8 118.7(3) . . ?
O16 N11 O15 120.8(3) . . ?
O16 N11 C6 120.8(3) . . ?
O15 N11 C6 118.3(3) . . ?
O17 N12 O18 121.4(3) . . ?
O17 N12 C6 120.9(3) . . ?
O18 N12 C6 117.7(3) . . ?
C9 N13 H13A 120.0 . . ?
C9 N13 H13B 120.0 . . ?
H13A N13 H13B 120.0 . . ?
C9 N14 H14A 120.0 . . ?
C9 N14 H14B 120.0 . . ?
H14A N14 H14B 120.0 . . ?
C9 N15 H15A 120.0 . . ?
C9 N15 H15B 120.0 . . ?
H15A N15 H15B 120.0 . . ?
C10 N16 H16A 120.0 . . ?
C10 N16 H16B 120.0 . . ?
H16A N16 H16B 120.0 . . ?
C10 N17 H17A 120.0 . . ?
C10 N17 H17B 120.0 . . ?
H17A N17 H17B 120.0 . . ?
C10 N18 H18A 120.0 . . ?
C10 N18 H18B 120.0 . . ?
H18A N18 H18B 120.0 . . ?
N1 C1 N2 117.9(3) . . ?
N1 C1 C2 122.0(3) . . ?
N2 C1 C2 120.1(3) . . ?
N5 C2 N6 116.2(3) . . ?
N5 C2 C1 123.0(3) . . ?
N6 C2 C1 120.7(3) . . ?
O1 C3 N2 122.6(3) . . ?
O1 C3 C4 121.0(3) . . ?
N2 C3 C4 116.4(3) . . ?
N3 C4 C3 130.2(3) . . ?
N3 C4 N4 115.2(3) . . ?
C3 C4 N4 114.6(3) . . ?
N7 C5 N8 118.8(3) . . ?
N7 C5 C6 122.1(3) . . ?
N8 C5 C6 119.1(3) . . ?
N12 C6 N11 114.9(3) . . ?
N12 C6 C5 124.8(3) . . ?
N11 C6 C5 120.3(3) . . ?
O10 C7 N8 122.2(3) . . ?
O10 C7 C8 121.4(3) . . ?
N8 C7 C8 116.5(3) . . ?
N10 C8 N9 115.9(3) . . ?
N10 C8 C7 127.2(3) . . ?
N9 C8 C7 116.8(3) . . ?
N15 C9 N13 120.1(3) . . ?
N15 C9 N14 119.2(3) . . ?
N13 C9 N14 120.6(4) . . ?
N17 C10 N18 120.8(4) . . ?
N17 C10 N16 119.8(4) . . ?
N18 C10 N16 119.4(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
C3 N2 C1 N1 -0.6(6) . . . . ?
C3 N2 C1 C2 179.2(3) . . . . ?
O7 N5 C2 N6 -19.0(5) . . . . ?
O6 N5 C2 N6 164.0(3) . . . . ?
O7 N5 C2 C1 163.4(3) . . . . ?
O6 N5 C2 C1 -13.7(5) . . . . ?
O8 N6 C2 N5 -19.5(5) . . . . ?
O9 N6 C2 N5 162.7(3) . . . . ?
O8 N6 C2 C1 158.2(3) . . . . ?
O9 N6 C2 C1 -19.6(5) . . . . ?
N1 C1 C2 N5 -170.3(3) . . . . ?
N2 C1 C2 N5 10.0(5) . . . . ?
N1 C1 C2 N6 12.2(6) . . . . ?
N2 C1 C2 N6 -167.6(3) . . . . ?
C1 N2 C3 O1 5.4(6) . . . . ?
C1 N2 C3 C4 -172.9(3) . . . . ?
O3 N3 C4 C3 -179.7(4) . . . . ?
O2 N3 C4 C3 0.2(6) . . . . ?
O3 N3 C4 N4 1.6(5) . . . . ?
O2 N3 C4 N4 -178.5(3) . . . . ?
O1 C3 C4 N3 -176.1(4) . . . . ?
N2 C3 C4 N3 2.3(6) . . . . ?
O1 C3 C4 N4 2.6(6) . . . . ?
N2 C3 C4 N4 -179.0(3) . . . . ?
O4 N4 C4 N3 67.7(4) . . . . ?
O5 N4 C4 N3 -111.5(4) . . . . ?
O4 N4 C4 C3 -111.2(4) . . . . ?
O5 N4 C4 C3 69.6(5) . . . . ?
C7 N8 C5 N7 -0.2(5) . . . . ?
C7 N8 C5 C6 179.7(3) . . . . ?
O17 N12 C6 N11 -16.9(5) . . . . ?
O18 N12 C6 N11 166.1(3) . . . . ?
O17 N12 C6 C5 163.6(4) . . . . ?
O18 N12 C6 C5 -13.4(6) . . . . ?
O16 N11 C6 N12 -27.4(5) . . . . ?
O15 N11 C6 N12 155.8(3) . . . . ?
O16 N11 C6 C5 152.1(4) . . . . ?
O15 N11 C6 C5 -24.7(5) . . . . ?
N7 C5 C6 N12 -175.1(4) . . . . ?
N8 C5 C6 N12 4.9(5) . . . . ?
N7 C5 C6 N11 5.4(5) . . . . ?
N8 C5 C6 N11 -174.5(3) . . . . ?
C5 N8 C7 O10 -4.5(6) . . . . ?
C5 N8 C7 C8 176.5(3) . . . . ?
O13 N10 C8 N9 -3.3(6) . . . . ?
O14 N10 C8 N9 178.5(3) . . . . ?
O13 N10 C8 C7 -179.0(4) . . . . ?
O14 N10 C8 C7 2.8(6) . . . . ?
O11 N9 C8 N10 137.6(4) . . . . ?
O12 N9 C8 N10 -44.8(5) . . . . ?
O11 N9 C8 C7 -46.2(5) . . . . ?
O12 N9 C8 C7 131.4(4) . . . . ?
O10 C7 C8 N10 167.9(4) . . . . ?
N8 C7 C8 N10 -13.2(6) . . . . ?
O10 C7 C8 N9 -7.8(5) . . . . ?
N8 C7 C8 N9 171.2(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O19 H19A O11 0.96 2.33 3.215(5) 154.7 2_665
O19 H19A O12 0.96 2.62 3.091(5) 111.1 2_665
O19 H19B O6 1.06 2.07 2.948(4) 138.7 .
N1 H1A O1 0.86 1.93 2.596(4) 133.4 .
N1 H1A O17 0.86 2.41 3.051(4) 131.2 2_676
N1 H1B O9 0.86 1.90 2.545(4) 130.4 .
N1 H1B O16 0.86 2.22 2.872(4) 132.7 2_676
N7 H7A O10 0.86 1.96 2.611(4) 132.1 .
N7 H7B O15 0.86 1.93 2.566(4) 129.6 .
N13 H13A O2 0.86 2.10 2.956(4) 172.7 .
N13 H13B O12 0.86 2.41 3.154(5) 145.0 2_665
N13 H13B O19 0.86 2.38 3.045(5) 134.1 .
N14 H14A O8 0.86 2.40 3.219(4) 159.1 1_545
N14 H14A O9 0.86 2.51 3.280(4) 148.9 1_545
N14 H14B O12 0.86 2.26 3.042(5) 150.8 2_665
N14 H14B O13 0.86 2.19 2.862(4) 135.2 2_665
N15 H15A O3 0.86 2.19 3.043(4) 173.4 .
N15 H15A O15 0.86 2.47 2.920(4) 113.2 2_666
N15 H15B O9 0.86 2.42 3.210(4) 152.7 1_545
N16 H16A O13 0.86 2.38 3.161(4) 152.0 2_675
N16 H16A O14 0.86 2.26 3.038(4) 151.0 2_675
N16 H16A N10 0.86 2.68 3.533(4) 175.3 2_675
N16 H16B O7 0.86 2.22 2.982(4) 147.5 .
N16 H16B O8 0.86 2.35 3.056(4) 140.1 .
N17 H17A O20 0.86 2.08 2.904(5) 161.6 1_554
N17 H17B O14 0.86 2.34 3.102(4) 148.3 2_675
N17 H17B O18 0.86 2.38 3.088(4) 139.8 2_675
N18 H18A O21 0.86 2.04 2.886(6) 169.9 1_554
N18 H18B O7 0.86 2.59 3.269(5) 136.8 .
N2 H2 O2 0.83(3) 2.00(3) 2.659(4) 136(3) .
N2 H2 O6 0.83(3) 1.93(4) 2.568(4) 132(3) .
N8 H8 O14 0.83(3) 1.97(3) 2.597(4) 132(3) .
N8 H8 O18 0.83(3) 1.90(3) 2.573(4) 138(3) .
N8 H8 N12 0.83(3) 2.50(3) 2.890(4) 110(2) .
O20 H20A O1 0.83(2) 2.34(6) 3.031(5) 141(8) .
O20 H20B O19 0.82(2) 2.14(8) 2.798(6) 138(10) 2_766
O21 H21A O20 0.82(2) 2.01(2) 2.822(6) 173(8) .
O21 H21B O10 0.82(2) 2.29(9) 2.947(5) 138(12) 2_666
O21 H21B O11 0.82(2) 2.59(10) 3.241(6) 137(12) 2_666

_refine_diff_density_max         0.454
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.062

_shelxl_version_number           2013-4

