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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_b016

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'Trimer 4'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H22 N2 O7'
_chemical_formula_weight         450.44

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/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                   14.0883(19)
_cell_length_b                   9.8136(14)
_cell_length_c                   16.084(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.581(4)
_cell_angle_gamma                90.00
_cell_volume                     2053.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    835
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      27.15

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             944
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9378
_exptl_absorpt_correction_T_max  0.9786
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2001)'

_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14175
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.57
_diffrn_reflns_theta_max         27.48
_reflns_number_total             4705
_reflns_number_gt                3997
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0825P)²+0.4225P] 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         4705
_refine_ls_number_parameters     310
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0492
_refine_ls_wR_factor_ref         0.1412
_refine_ls_wR_factor_gt          0.1270
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.093
_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 -0.25962(9) 1.10261(12) -0.11106(8) 0.0200(3) Uani 1 1 d . . .
O2 O -0.21849(8) 1.04537(12) 0.15590(7) 0.0177(3) Uani 1 1 d . . .
O3 O -0.07775(9) 0.86347(12) -0.04946(7) 0.0175(3) Uani 1 1 d . . .
H3 H -0.0518 0.8131 -0.0774 0.026 Uiso 1 1 calc R . .
O4 O 0.03469(9) 0.67541(13) -0.07022(7) 0.0204(3) Uani 1 1 d . . .
O5 O 0.29386(9) 0.41305(12) 0.15819(7) 0.0168(3) Uani 1 1 d . . .
O6 O 0.47972(9) 0.26647(13) 0.16800(8) 0.0233(3) Uani 1 1 d . . .
O7 O 0.42610(8) 0.09950(12) 0.06499(8) 0.0192(3) Uani 1 1 d . . .
N1 N -0.15028(10) 1.00367(14) 0.05096(9) 0.0152(3) Uani 1 1 d . . .
H1N H -0.1598(15) 1.018(2) -0.0041(15) 0.020(5) Uiso 1 1 d . . .
N2 N 0.14407(10) 0.55602(14) 0.04913(9) 0.0146(3) Uani 1 1 d . . .
H2N H 0.1665(15) 0.542(2) 0.1065(15) 0.020(5) Uiso 1 1 d . . .
C1 C -0.30978(11) 1.18684(16) -0.07327(11) 0.0150(3) Uani 1 1 d . . .
C2 C -0.38141(12) 1.28338(17) -0.12386(11) 0.0174(3) Uani 1 1 d . . .
H2 H -0.3962 1.2932 -0.1864 0.021 Uiso 1 1 calc R . .
C3 C -0.43103(12) 1.36498(17) -0.08274(12) 0.0197(4) Uani 1 1 d . . .
H3A H -0.4798 1.4305 -0.1174 0.024 Uiso 1 1 calc R . .
C4 C -0.41015(12) 1.35191(17) 0.00837(12) 0.0187(3) Uani 1 1 d . . .
H4 H -0.4443 1.4079 0.0364 0.022 Uiso 1 1 calc R . .
C5 C -0.33869(12) 1.25592(17) 0.05813(11) 0.0161(3) Uani 1 1 d . . .
H5 H -0.3240 1.2476 0.1207 0.019 Uiso 1 1 calc R . .
C6 C -0.28772(11) 1.17121(16) 0.01925(10) 0.0137(3) Uani 1 1 d . . .
C7 C -0.28382(14) 1.11132(19) -0.20564(11) 0.0232(4) Uani 1 1 d . . .
H7A H -0.3561 1.0868 -0.2385 0.035 Uiso 1 1 calc R . .
H7B H -0.2399 1.0485 -0.2221 0.035 Uiso 1 1 calc R . .
H7C H -0.2721 1.2046 -0.2212 0.035 Uiso 1 1 calc R . .
C8 C -0.21629(11) 1.06692(16) 0.08151(10) 0.0134(3) Uani 1 1 d . . .
C9 C -0.03984(11) 0.82848(16) 0.03871(10) 0.0139(3) Uani 1 1 d . . .
C10 C -0.07763(11) 0.90279(16) 0.09495(11) 0.0143(3) Uani 1 1 d . . .
C11 C -0.04068(12) 0.87395(17) 0.18648(11) 0.0166(3) Uani 1 1 d . . .
H11 H -0.0643 0.9249 0.2250 0.020 Uiso 1 1 calc R . .
C12 C 0.03123(12) 0.76980(17) 0.22176(11) 0.0171(3) Uani 1 1 d . . .
H12 H 0.0556 0.7494 0.2842 0.021 Uiso 1 1 calc R . .
C13 C 0.06711(12) 0.69633(16) 0.16676(11) 0.0157(3) Uani 1 1 d . . .
H13 H 0.1155 0.6252 0.1918 0.019 Uiso 1 1 calc R . .
C14 C 0.03330(11) 0.72498(16) 0.07445(10) 0.0141(3) Uani 1 1 d . . .
C15 C 0.07018(11) 0.65051(16) 0.01184(10) 0.0141(3) Uani 1 1 d . . .
C16 C 0.19452(11) 0.47171(16) 0.00827(10) 0.0133(3) Uani 1 1 d . . .
C17 C 0.27377(12) 0.39090(16) 0.06879(10) 0.0139(3) Uani 1 1 d . . .
C18 C 0.32758(12) 0.29954(16) 0.03595(10) 0.0145(3) Uani 1 1 d . . .
C19 C 0.30037(12) 0.28884(16) -0.05720(11) 0.0159(3) Uani 1 1 d . . .
H19 H 0.3345 0.2250 -0.0805 0.019 Uiso 1 1 calc R . .
C20 C 0.22385(12) 0.37110(17) -0.11538(11) 0.0171(3) Uani 1 1 d . . .
H20 H 0.2072 0.3645 -0.1783 0.021 Uiso 1 1 calc R . .
C21 C 0.17079(12) 0.46320(16) -0.08350(11) 0.0151(3) Uani 1 1 d . . .
H21 H 0.1189 0.5196 -0.1242 0.018 Uiso 1 1 calc R . .
C22 C 0.29160(14) 0.29793(18) 0.21317(11) 0.0230(4) Uani 1 1 d . . .
H22A H 0.2501 0.2249 0.1747 0.034 Uiso 1 1 calc R . .
H22B H 0.2613 0.3256 0.2562 0.034 Uiso 1 1 calc R . .
H22C H 0.3618 0.2650 0.2460 0.034 Uiso 1 1 calc R . .
C23 C 0.41855(12) 0.22288(16) 0.09803(11) 0.0155(3) Uani 1 1 d . . .
C24 C 0.51297(12) 0.01737(17) 0.12084(12) 0.0210(4) Uani 1 1 d . . .
H24A H 0.5771 0.0647 0.1288 0.031 Uiso 1 1 calc R . .
H24B H 0.5112 -0.0708 0.0917 0.031 Uiso 1 1 calc R . .
H24C H 0.5092 0.0028 0.1798 0.031 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.3718(19) . ?
O1 C7 1.4281(19) . ?
O2 C8 1.2272(19) . ?
O3 C9 1.3538(18) . ?
O4 C15 1.2430(19) . ?
O5 C17 1.3721(18) . ?
O5 C22 1.443(2) . ?
O6 C23 1.203(2) . ?
O7 C23 1.343(2) . ?
O7 C24 1.4526(19) . ?
N1 C8 1.357(2) . ?
N1 C10 1.404(2) . ?
N2 C15 1.351(2) . ?
N2 C16 1.407(2) . ?
C1 C2 1.396(2) . ?
C1 C6 1.407(2) . ?
C2 C3 1.387(2) . ?
C3 C4 1.385(2) . ?
C4 C5 1.387(2) . ?
C5 C6 1.394(2) . ?
C6 C8 1.513(2) . ?
C9 C14 1.403(2) . ?
C9 C10 1.415(2) . ?
C10 C11 1.389(2) . ?
C11 C12 1.397(2) . ?
C12 C13 1.379(2) . ?
C13 C14 1.403(2) . ?
C14 C15 1.490(2) . ?
C16 C21 1.385(2) . ?
C16 C17 1.410(2) . ?
C17 C18 1.402(2) . ?
C18 C19 1.401(2) . ?
C18 C23 1.491(2) . ?
C19 C20 1.384(2) . ?
C20 C21 1.390(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 C7 118.88(13) . . ?
C17 O5 C22 118.30(12) . . ?
C23 O7 C24 115.57(13) . . ?
C8 N1 C10 127.45(14) . . ?
C15 N2 C16 129.63(14) . . ?
O1 C1 C2 122.07(14) . . ?
O1 C1 C6 117.44(14) . . ?
C2 C1 C6 120.48(14) . . ?
C3 C2 C1 119.88(15) . . ?
C4 C3 C2 120.66(15) . . ?
C3 C4 C5 119.05(15) . . ?
C4 C5 C6 122.09(15) . . ?
C5 C6 C1 117.83(14) . . ?
C5 C6 C8 115.65(14) . . ?
C1 C6 C8 126.47(14) . . ?
O2 C8 N1 123.47(14) . . ?
O2 C8 C6 120.17(14) . . ?
N1 C8 C6 116.35(13) . . ?
O3 C9 C14 123.03(14) . . ?
O3 C9 C10 116.42(13) . . ?
C14 C9 C10 120.55(14) . . ?
C11 C10 N1 125.56(14) . . ?
C11 C10 C9 119.51(14) . . ?
N1 C10 C9 114.93(14) . . ?
C10 C11 C12 119.85(14) . . ?
C13 C12 C11 120.62(15) . . ?
C12 C13 C14 121.01(14) . . ?
C13 C14 C9 118.44(14) . . ?
C13 C14 C15 123.52(14) . . ?
C9 C14 C15 118.03(14) . . ?
O4 C15 N2 122.25(14) . . ?
O4 C15 C14 121.25(14) . . ?
N2 C15 C14 116.49(13) . . ?
C21 C16 N2 125.07(14) . . ?
C21 C16 C17 120.32(14) . . ?
N2 C16 C17 114.60(14) . . ?
O5 C17 C18 124.92(14) . . ?
O5 C17 C16 115.11(13) . . ?
C18 C17 C16 119.94(14) . . ?
C19 C18 C17 119.05(14) . . ?
C19 C18 C23 119.36(14) . . ?
C17 C18 C23 121.37(14) . . ?
C20 C19 C18 120.12(15) . . ?
C19 C20 C21 121.30(15) . . ?
C16 C21 C20 119.22(14) . . ?
O6 C23 O7 123.62(15) . . ?
O6 C23 C18 124.74(15) . . ?
O7 C23 C18 111.61(13) . . ?

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
N2 H2N O5 0.86(2) 2.09(2) 2.5798(17) 115.2(16) .
N1 H1N O1 0.85(2) 1.94(2) 2.6503(18) 139.4(18) .
O3 H3 O4 0.84 1.79 2.5364(16) 146.4 .

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.087
_database_code_depnum_ccdc_archive 'CCDC 1017708'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_8429

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'Trimer 5'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25.13 H25.88 N3 Na O11'
_chemical_formula_weight         568.85

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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   15.2734(12)
_cell_length_b                   15.273
_cell_length_c                   23.031(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5372.6(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    2952
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      21.13

_exptl_crystal_description       Rod
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2373
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_type   'Sadabs, (Sheldrick 2001)'
_exptl_absorpt_correction_T_min  0.9659
_exptl_absorpt_correction_T_max  0.9950
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      223(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            31686
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_sigmaI/netI    0.0742
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.60
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9464
_reflns_number_gt                6457
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0658P)²+0.9184P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(7)
_refine_ls_number_reflns         9464
_refine_ls_number_parameters     762
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.1212
_refine_ls_R_factor_gt           0.0818
_refine_ls_wR_factor_ref         0.1703
_refine_ls_wR_factor_gt          0.1553
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.122
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Na1 Na 0.65659(8) 0.23657(9) 0.52387(6) 0.0513(4) Uani 1 1 d . . .
Na2 Na 0.71905(8) 0.26211(9) 0.02225(6) 0.0458(4) Uani 1 1 d . . .
N1 N 0.70213(16) 0.1291(2) 0.38990(11) 0.0460(8) Uani 1 1 d D . .
H1N H 0.6765(16) 0.122(2) 0.4241(7) 0.055 Uiso 1 1 d D . .
N2 N 0.41436(15) 0.16366(18) 0.49365(12) 0.0404(8) Uani 1 1 d D . .
H2N H 0.4627(11) 0.1737(19) 0.5141(10) 0.048 Uiso 1 1 d D . .
N3 N 0.4585(3) 0.1120(3) 0.71957(14) 0.0967(16) Uani 1 1 d . . .
N4 N 0.76443(16) 0.3734(2) -0.10657(12) 0.0445(8) Uani 1 1 d D . .
H4N H 0.7436(17) 0.375(2) -0.0698(7) 0.053 Uiso 1 1 d D . .
N5 N 0.47501(15) 0.33985(18) -0.00438(10) 0.0355(7) Uani 1 1 d D . .
H5N H 0.5194(11) 0.3521(18) 0.0202(9) 0.043 Uiso 1 1 d D . .
N6 N 0.5215(2) 0.3893(3) 0.22262(14) 0.0785(13) Uani 1 1 d . . .
O1 O 0.93902(14) 0.09486(16) 0.54607(10) 0.0519(7) Uani 1 1 d . . .
O2 O 1.05266(14) 0.15737(17) 0.50312(11) 0.0562(8) Uani 1 1 d . . .
O3 O 0.78355(13) 0.12273(15) 0.49114(9) 0.0410(6) Uani 1 1 d . . .
O4 O 0.66572(16) 0.1440(2) 0.29532(11) 0.0805(10) Uani 1 1 d . . .
O5 O 0.57759(12) 0.14252(15) 0.46762(9) 0.0397(6) Uani 1 1 d . . .
O6 O 0.26559(14) 0.16630(17) 0.49084(11) 0.0555(8) Uani 1 1 d . . .
O7 O 0.48444(13) 0.12797(15) 0.59886(9) 0.0421(6) Uani 1 1 d . A .
O8 O 0.5258(3) 0.1555(4) 0.71478(19) 0.1108(18) Uani 0.761(4) 1 d P A 1
O9 O 0.4500(4) 0.0542(4) 0.7583(2) 0.127(2) Uani 0.761(4) 1 d P A 1
O8A O 0.5166(18) 0.0704(17) 0.7073(11) 0.189(10) Uiso 0.239(4) 1 d P A 2
O9A O 0.4411(12) 0.1188(14) 0.7608(9) 0.130(7) Uiso 0.239(4) 1 d P A 2
O10 O 0.6591(2) 0.2154(2) 0.62082(13) 0.0842(11) Uani 1 1 d D . .
H10A H 0.665(3) 0.2662(7) 0.6367(12) 0.101 Uiso 1 1 d D . .
O11 O 0.99943(14) 0.40276(16) 0.05136(10) 0.0500(7) Uani 1 1 d . . .
O12 O 1.11369(13) 0.34053(16) 0.00834(10) 0.0501(7) Uani 1 1 d . . .
O13 O 0.84534(13) 0.37523(14) -0.00488(9) 0.0380(6) Uani 1 1 d . . .
O14 O 0.73316(15) 0.3527(2) -0.20189(10) 0.0679(9) Uani 1 1 d . . .
O15 O 0.64053(12) 0.36081(15) -0.03063(9) 0.0384(6) Uani 1 1 d . . .
O16 O 0.32746(12) 0.33441(17) -0.00642(10) 0.0474(7) Uani 1 1 d . . .
O17 O 0.54751(14) 0.37482(15) 0.10002(10) 0.0444(7) Uani 1 1 d . . .
O18 O 0.5889(2) 0.3505(3) 0.21331(14) 0.1294(16) Uani 1 1 d . . .
O19 O 0.5113(3) 0.4316(3) 0.26414(16) 0.1365(17) Uani 1 1 d . . .
O20 O 0.7171(2) 0.2811(2) 0.11905(13) 0.0889(11) Uani 1 1 d D . .
H20A H 0.720(2) 0.2446(11) 0.1490(9) 0.107 Uiso 1 1 d D . .
H20B H 0.7549(14) 0.3184(13) 0.1352(13) 0.107 Uiso 1 1 d D . .
C1 C 0.8357(2) 0.1231(2) 0.44211(14) 0.0384(9) Uani 1 1 d . . .
C2 C 0.9267(2) 0.1262(2) 0.44617(15) 0.0422(10) Uani 1 1 d . . .
C3 C 0.9751(2) 0.1325(2) 0.39418(17) 0.0530(11) Uani 1 1 d . . .
H3 H 1.0365 0.1362 0.3957 0.064 Uiso 1 1 calc R . .
C4 C 0.9339(2) 0.1333(3) 0.34174(15) 0.0599(12) Uani 1 1 d . . .
H4 H 0.9667 0.1363 0.3073 0.072 Uiso 1 1 calc R . .
C5 C 0.8438(2) 0.1297(3) 0.33951(16) 0.0601(12) Uani 1 1 d . . .
H5 H 0.8158 0.1294 0.3032 0.072 Uiso 1 1 calc R . .
C6 C 0.7942(2) 0.1267(2) 0.38879(15) 0.0417(10) Uani 1 1 d . . .
C7 C 0.9786(2) 0.1284(2) 0.50088(15) 0.0388(9) Uani 1 1 d . . .
C8 C 0.9848(3) 0.0966(3) 0.60055(17) 0.0596(12) Uani 1 1 d . . .
H8A H 1.0388 0.0635 0.5971 0.089 Uiso 1 1 calc R . .
H8B H 0.9484 0.0707 0.6305 0.089 Uiso 1 1 calc R . .
H8C H 0.9982 0.1567 0.6108 0.089 Uiso 1 1 calc R . .
C9 C 0.7582(2) 0.0363(2) 0.50982(17) 0.0577(12) Uani 1 1 d . . .
H9A H 0.7170 0.0117 0.4822 0.087 Uiso 1 1 calc R . .
H9B H 0.7308 0.0399 0.5478 0.087 Uiso 1 1 calc R . .
H9C H 0.8096 -0.0008 0.5121 0.087 Uiso 1 1 calc R . .
C10 C 0.6457(2) 0.1422(3) 0.34610(15) 0.0522(11) Uani 1 1 d . . .
C11 C 0.52574(18) 0.1566(2) 0.42369(13) 0.0337(9) Uani 1 1 d . . .
C12 C 0.5534(2) 0.1574(3) 0.36564(14) 0.0463(10) Uani 1 1 d . . .
C13 C 0.4924(2) 0.1738(3) 0.32035(16) 0.0566(12) Uani 1 1 d . . .
H13 H 0.5111 0.1737 0.2815 0.068 Uiso 1 1 calc R . .
C14 C 0.4058(2) 0.1897(3) 0.33332(16) 0.0643(13) Uani 1 1 d . . .
H14 H 0.3659 0.2018 0.3033 0.077 Uiso 1 1 calc R . .
C15 C 0.3772(2) 0.1881(3) 0.39076(16) 0.0526(11) Uani 1 1 d . . .
H15 H 0.3179 0.1986 0.3992 0.063 Uiso 1 1 calc R . .
C16 C 0.4338(2) 0.1715(2) 0.43428(13) 0.0355(9) Uani 1 1 d . . .
C17 C 0.3341(2) 0.1599(2) 0.51881(16) 0.0406(10) Uani 1 1 d . . .
C18 C 0.4006(2) 0.1317(2) 0.61970(16) 0.0507(11) Uani 1 1 d . . .
C19 C 0.3302(2) 0.1464(2) 0.58359(15) 0.0438(10) Uani 1 1 d . A .
C20 C 0.2458(3) 0.1472(3) 0.60665(19) 0.0721(14) Uani 1 1 d . . .
H20 H 0.1979 0.1548 0.5815 0.087 Uiso 1 1 calc R A .
C21 C 0.2310(3) 0.1374(4) 0.6645(2) 0.0991(19) Uani 1 1 d . A .
H21 H 0.1736 0.1391 0.6792 0.119 Uiso 1 1 calc R . .
C22 C 0.2996(3) 0.1250(4) 0.7006(2) 0.0956(18) Uani 1 1 d . . .
H22 H 0.2894 0.1185 0.7406 0.115 Uiso 1 1 calc R A .
C23 C 0.3861(3) 0.1216(3) 0.67952(17) 0.0699(14) Uani 1 1 d . A .
C24 C 0.5169(3) 0.0403(3) 0.5922(2) 0.0752(15) Uani 1 1 d . . .
H24A H 0.5360 0.0182 0.6296 0.113 Uiso 1 1 calc R A .
H24B H 0.5659 0.0404 0.5654 0.113 Uiso 1 1 calc R . .
H24C H 0.4707 0.0031 0.5770 0.113 Uiso 1 1 calc R . .
C25 C 0.89787(18) 0.3767(2) -0.05307(13) 0.0320(8) Uani 1 1 d . . .
C26 C 0.9891(2) 0.3713(2) -0.04921(14) 0.0390(9) Uani 1 1 d . . .
C27 C 1.0370(2) 0.3685(2) -0.09976(14) 0.0466(10) Uani 1 1 d . . .
H27 H 1.0983 0.3641 -0.0976 0.056 Uiso 1 1 calc R . .
C28 C 0.9979(2) 0.3718(3) -0.15261(16) 0.0579(12) Uani 1 1 d . . .
H28 H 1.0327 0.3714 -0.1863 0.069 Uiso 1 1 calc R . .
C29 C 0.9083(2) 0.3757(3) -0.15772(16) 0.0512(11) Uani 1 1 d . . .
H29 H 0.8818 0.3787 -0.1945 0.061 Uiso 1 1 calc R . .
C30 C 0.85724(19) 0.3753(2) -0.10716(15) 0.0415(10) Uani 1 1 d . . .
C31 C 1.0402(2) 0.3695(2) 0.00590(15) 0.0400(9) Uani 1 1 d . . .
C32 C 1.0461(3) 0.4001(3) 0.10616(16) 0.0609(13) Uani 1 1 d . . .
H32A H 1.0634 0.3403 0.1145 0.091 Uiso 1 1 calc R . .
H32B H 1.0083 0.4214 0.1369 0.091 Uiso 1 1 calc R . .
H32C H 1.0978 0.4368 0.1037 0.091 Uiso 1 1 calc R . .
C33 C 0.8210(3) 0.4602(2) 0.01592(17) 0.0595(12) Uani 1 1 d . . .
H33A H 0.8733 0.4949 0.0225 0.089 Uiso 1 1 calc R . .
H33B H 0.7888 0.4542 0.0520 0.089 Uiso 1 1 calc R . .
H33C H 0.7844 0.4890 -0.0127 0.089 Uiso 1 1 calc R . .
C34 C 0.7082(2) 0.3575(2) -0.15131(14) 0.0416(10) Uani 1 1 d . . .
C35 C 0.5891(2) 0.3468(2) -0.07421(14) 0.0370(9) Uani 1 1 d . . .
C36 C 0.6152(2) 0.3453(2) -0.13325(13) 0.0399(9) Uani 1 1 d . . .
C37 C 0.5550(2) 0.3315(3) -0.17657(15) 0.0546(12) Uani 1 1 d . . .
H37 H 0.5738 0.3315 -0.2154 0.065 Uiso 1 1 calc R . .
C38 C 0.4668(2) 0.3175(3) -0.16442(16) 0.0561(12) Uani 1 1 d . . .
H38 H 0.4269 0.3066 -0.1946 0.067 Uiso 1 1 calc R . .
C39 C 0.4392(2) 0.3197(3) -0.10870(16) 0.0523(11) Uani 1 1 d . . .
H39 H 0.3796 0.3114 -0.1004 0.063 Uiso 1 1 calc R . .
C40 C 0.4973(2) 0.3339(2) -0.06394(14) 0.0367(9) Uani 1 1 d . . .
C41 C 0.3963(2) 0.3427(2) 0.02031(15) 0.0370(9) Uani 1 1 d . . .
C42 C 0.4640(2) 0.3690(2) 0.12241(14) 0.0390(9) Uani 1 1 d . . .
C43 C 0.3930(2) 0.3550(2) 0.08511(16) 0.0421(10) Uani 1 1 d . . .
C44 C 0.3090(2) 0.3507(3) 0.11090(17) 0.0575(12) Uani 1 1 d . . .
H44 H 0.2602 0.3398 0.0872 0.069 Uiso 1 1 calc R . .
C45 C 0.2967(3) 0.3619(4) 0.1689(2) 0.0836(17) Uani 1 1 d . . .
H45 H 0.2399 0.3616 0.1846 0.100 Uiso 1 1 calc R . .
C46 C 0.3680(3) 0.3737(4) 0.2044(2) 0.0849(17) Uani 1 1 d . . .
H46 H 0.3609 0.3791 0.2448 0.102 Uiso 1 1 calc R . .
C47 C 0.4496(3) 0.3775(3) 0.18005(17) 0.0602(13) Uani 1 1 d . . .
C48 C 0.5787(3) 0.4639(3) 0.0948(2) 0.0815(16) Uani 1 1 d . . .
H48A H 0.5485 0.4927 0.0631 0.122 Uiso 1 1 calc R . .
H48B H 0.6412 0.4635 0.0872 0.122 Uiso 1 1 calc R . .
H48C H 0.5673 0.4951 0.1307 0.122 Uiso 1 1 calc R . .
C1S C 0.7527(4) 0.0540(5) 0.1795(3) 0.140(3) Uani 1 1 d . . .
H1S1 H 0.7934 0.0313 0.2081 0.210 Uiso 1 1 calc R . .
H1S2 H 0.7778 0.0478 0.1410 0.210 Uiso 1 1 calc R . .
H1S3 H 0.6983 0.0215 0.1815 0.210 Uiso 1 1 calc R . .
C2S C 0.7011(4) 0.4427(4) 0.6689(3) 0.108(2) Uani 1 1 d . . .
H2S1 H 0.7549 0.4606 0.6878 0.163 Uiso 1 1 calc R . .
H2S2 H 0.6551 0.4843 0.6780 0.163 Uiso 1 1 calc R . .
H2S3 H 0.7101 0.4410 0.6272 0.163 Uiso 1 1 calc R . .
O1S O 0.7366(3) 0.1418(3) 0.19065(15) 0.1312(16) Uani 1 1 d . . .
H1S H 0.7055 0.1463 0.2200 0.197 Uiso 1 1 calc R . .
O2S O 0.6772(2) 0.3604(2) 0.68840(12) 0.0948(12) Uani 1 1 d . . .
H2S H 0.6939 0.3539 0.7224 0.142 Uiso 1 1 calc R . .
C1X C 0.7200(6) 0.1614(2) 0.6581(3) 0.073(5) Uiso 0.239(4) 1 d PRD A 2
H10B H 0.6814 0.1852 0.6493 0.100 Uiso 0.761(4) 1 d PRD 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
Na1 O6 2.256(3) 4_556 ?
Na1 O10 2.256(3) . ?
Na1 O5 2.280(3) . ?
Na1 O2 2.352(3) 4_456 ?
Na1 O3 2.711(2) . ?
Na2 O16 2.247(3) 4 ?
Na2 O20 2.249(3) . ?
Na2 O15 2.279(2) . ?
Na2 O12 2.354(3) 4_455 ?
Na2 O13 2.664(2) . ?
N1 C10 1.342(4) . ?
N1 C6 1.407(4) . ?
N2 C17 1.356(4) . ?
N2 C16 1.405(4) . ?
N3 O9A 0.99(2) . ?
N3 O8A 1.13(3) . ?
N3 O8 1.229(6) . ?
N3 O9 1.262(6) . ?
N3 C23 1.448(6) . ?
N4 C34 1.363(4) . ?
N4 C30 1.418(4) . ?
N5 C41 1.330(4) . ?
N5 C40 1.416(4) . ?
N6 O19 1.165(5) . ?
N6 O18 1.207(5) . ?
N6 C47 1.484(5) . ?
O1 C7 1.308(4) . ?
O1 C8 1.437(4) . ?
O2 C7 1.216(4) . ?
O2 Na1 2.352(3) 4_556 ?
O3 C1 1.382(4) . ?
O3 C9 1.441(4) . ?
O4 C10 1.209(4) . ?
O5 C11 1.303(3) . ?
O6 C17 1.233(4) . ?
O6 Na1 2.256(3) 4_456 ?
O7 C18 1.369(4) . ?
O7 C24 1.436(4) . ?
O10 C1X 1.511(9) . ?
O11 C31 1.320(4) . ?
O11 C32 1.450(4) . ?
O12 C31 1.208(4) . ?
O12 Na2 2.354(3) 4 ?
O13 C25 1.370(4) . ?
O13 C33 1.432(4) . ?
O14 C34 1.228(4) . ?
O15 C35 1.292(4) . ?
O16 C41 1.225(4) . ?
O16 Na2 2.247(3) 4_455 ?
O17 C42 1.379(4) . ?
O17 C48 1.446(5) . ?
C1 C6 1.383(5) . ?
C1 C2 1.394(4) . ?
C2 C3 1.411(5) . ?
C2 C7 1.489(5) . ?
C3 C4 1.362(5) . ?
C4 C5 1.378(5) . ?
C5 C6 1.365(5) . ?
C10 C12 1.497(5) . ?
C11 C12 1.402(4) . ?
C11 C16 1.443(4) . ?
C12 C13 1.422(5) . ?
C13 C14 1.377(5) . ?
C14 C15 1.393(5) . ?
C15 C16 1.348(5) . ?
C17 C19 1.508(5) . ?
C18 C19 1.378(5) . ?
C18 C23 1.404(5) . ?
C19 C20 1.393(5) . ?
C20 C21 1.359(6) . ?
C21 C22 1.352(6) . ?
C22 C23 1.408(6) . ?
C25 C30 1.392(4) . ?
C25 C26 1.398(4) . ?
C26 C27 1.376(4) . ?
C26 C31 1.490(5) . ?
C27 C28 1.356(5) . ?
C28 C29 1.375(5) . ?
C29 C30 1.401(5) . ?
C34 C36 1.491(5) . ?
C35 C36 1.417(4) . ?
C35 C40 1.435(4) . ?
C36 C37 1.373(5) . ?
C37 C38 1.393(5) . ?
C38 C39 1.351(5) . ?
C39 C40 1.377(5) . ?
C41 C43 1.505(5) . ?
C42 C47 1.352(5) . ?
C42 C43 1.400(5) . ?
C43 C44 1.415(5) . ?
C44 C45 1.360(6) . ?
C45 C46 1.375(6) . ?
C46 C47 1.367(6) . ?
C1S O1S 1.387(8) . ?
C2S O2S 1.384(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Na1 O10 103.34(11) 4_556 . ?
O6 Na1 O5 136.02(10) 4_556 . ?
O10 Na1 O5 118.74(11) . . ?
O6 Na1 O2 90.31(10) 4_556 4_456 ?
O10 Na1 O2 111.83(12) . 4_456 ?
O5 Na1 O2 85.79(9) . 4_456 ?
O6 Na1 O3 81.49(9) 4_556 . ?
O10 Na1 O3 99.85(11) . . ?
O5 Na1 O3 79.43(8) . . ?
O2 Na1 O3 148.31(10) 4_456 . ?
O16 Na2 O20 104.80(11) 4 . ?
O16 Na2 O15 137.32(10) 4 . ?
O20 Na2 O15 115.93(12) . . ?
O16 Na2 O12 91.05(9) 4 4_455 ?
O20 Na2 O12 111.93(11) . 4_455 ?
O15 Na2 O12 85.46(9) . 4_455 ?
O16 Na2 O13 81.60(8) 4 . ?
O20 Na2 O13 99.12(11) . . ?
O15 Na2 O13 80.02(8) . . ?
O12 Na2 O13 148.94(9) 4_455 . ?
C10 N1 C6 129.2(3) . . ?
C17 N2 C16 127.6(3) . . ?
O9A N3 O8A 120.7(18) . . ?
O9A N3 O8 104.7(12) . . ?
O8A N3 O8 67.9(14) . . ?
O9A N3 O9 50.8(12) . . ?
O8A N3 O9 82.2(14) . . ?
O8 N3 O9 121.9(5) . . ?
O9A N3 C23 113.2(12) . . ?
O8A N3 C23 120.0(14) . . ?
O8 N3 C23 121.8(4) . . ?
O9 N3 C23 116.3(5) . . ?
C34 N4 C30 128.8(3) . . ?
C41 N5 C40 129.3(3) . . ?
O19 N6 O18 122.2(4) . . ?
O19 N6 C47 120.7(4) . . ?
O18 N6 C47 117.0(3) . . ?
C7 O1 C8 117.6(3) . . ?
C7 O2 Na1 150.2(2) . 4_556 ?
C1 O3 C9 113.8(3) . . ?
C1 O3 Na1 129.53(19) . . ?
C9 O3 Na1 108.18(18) . . ?
C11 O5 Na1 131.2(2) . . ?
C17 O6 Na1 139.2(2) . 4_456 ?
C18 O7 C24 113.6(3) . . ?
C1X O10 Na1 130.7(2) . . ?
C31 O11 C32 116.6(3) . . ?
C31 O12 Na2 149.9(2) . 4 ?
C25 O13 C33 114.1(3) . . ?
C25 O13 Na2 128.67(18) . . ?
C33 O13 Na2 108.73(19) . . ?
C35 O15 Na2 128.7(2) . . ?
C41 O16 Na2 141.4(2) . 4_455 ?
C42 O17 C48 113.3(3) . . ?
O3 C1 C6 117.5(3) . . ?
O3 C1 C2 121.3(3) . . ?
C6 C1 C2 121.0(3) . . ?
C1 C2 C3 117.9(3) . . ?
C1 C2 C7 126.1(3) . . ?
C3 C2 C7 115.9(3) . . ?
C4 C3 C2 120.7(3) . . ?
C3 C4 C5 119.6(3) . . ?
C6 C5 C4 121.6(3) . . ?
C5 C6 C1 119.1(3) . . ?
C5 C6 N1 124.7(3) . . ?
C1 C6 N1 116.3(3) . . ?
O2 C7 O1 122.6(3) . . ?
O2 C7 C2 122.7(3) . . ?
O1 C7 C2 114.7(3) . . ?
O4 C10 N1 124.6(3) . . ?
O4 C10 C12 121.7(3) . . ?
N1 C10 C12 113.7(3) . . ?
O5 C11 C12 124.0(3) . . ?
O5 C11 C16 119.1(3) . . ?
C12 C11 C16 117.0(3) . . ?
C11 C12 C13 120.2(3) . . ?
C11 C12 C10 124.7(3) . . ?
C13 C12 C10 115.1(3) . . ?
C14 C13 C12 120.1(3) . . ?
C13 C14 C15 120.3(3) . . ?
C16 C15 C14 120.5(3) . . ?
C15 C16 N2 127.1(3) . . ?
C15 C16 C11 121.9(3) . . ?
N2 C16 C11 110.9(3) . . ?
O6 C17 N2 122.7(3) . . ?
O6 C17 C19 119.6(3) . . ?
N2 C17 C19 117.7(3) . . ?
O7 C18 C19 121.7(3) . . ?
O7 C18 C23 119.1(3) . . ?
C19 C18 C23 119.2(3) . . ?
C18 C19 C20 119.5(3) . . ?
C18 C19 C17 126.0(3) . . ?
C20 C19 C17 114.4(3) . . ?
C21 C20 C19 121.8(4) . . ?
C22 C21 C20 119.3(4) . . ?
C21 C22 C23 121.4(4) . . ?
C18 C23 C22 118.8(4) . . ?
C18 C23 N3 121.1(4) . . ?
C22 C23 N3 120.1(4) . . ?
O13 C25 C30 117.6(3) . . ?
O13 C25 C26 122.1(3) . . ?
C30 C25 C26 120.0(3) . . ?
C27 C26 C25 118.6(3) . . ?
C27 C26 C31 116.2(3) . . ?
C25 C26 C31 125.2(3) . . ?
C28 C27 C26 121.6(3) . . ?
C27 C28 C29 121.1(3) . . ?
C28 C29 C30 118.9(3) . . ?
C25 C30 C29 119.7(3) . . ?
C25 C30 N4 115.9(3) . . ?
C29 C30 N4 124.4(3) . . ?
O12 C31 O11 122.8(3) . . ?
O12 C31 C26 122.2(3) . . ?
O11 C31 C26 114.9(3) . . ?
O14 C34 N4 122.1(3) . . ?
O14 C34 C36 123.6(3) . . ?
N4 C34 C36 114.3(3) . . ?
O15 C35 C36 125.2(3) . . ?
O15 C35 C40 119.2(3) . . ?
C36 C35 C40 115.5(3) . . ?
C37 C36 C35 120.7(3) . . ?
C37 C36 C34 117.0(3) . . ?
C35 C36 C34 122.3(3) . . ?
C36 C37 C38 121.7(3) . . ?
C39 C38 C37 119.2(3) . . ?
C38 C39 C40 121.0(3) . . ?
C39 C40 N5 125.5(3) . . ?
C39 C40 C35 121.8(3) . . ?
N5 C40 C35 112.7(3) . . ?
O16 C41 N5 123.9(3) . . ?
O16 C41 C43 118.8(3) . . ?
N5 C41 C43 117.3(3) . . ?
C47 C42 O17 120.8(3) . . ?
C47 C42 C43 119.4(3) . . ?
O17 C42 C43 119.8(3) . . ?
C42 C43 C44 116.8(3) . . ?
C42 C43 C41 127.0(3) . . ?
C44 C43 C41 116.2(3) . . ?
C45 C44 C43 122.2(4) . . ?
C44 C45 C46 119.5(4) . . ?
C47 C46 C45 118.8(4) . . ?
C42 C47 C46 123.2(4) . . ?
C42 C47 N6 122.7(3) . . ?
C46 C47 N6 114.1(4) . . ?

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
N1 H1N O5 0.887(15) 1.84(2) 2.620(3) 145(3) .
N2 H2N O7 0.890(15) 2.10(2) 2.704(3) 124(2) .
N2 H2N O5 0.890(15) 2.11(2) 2.584(3) 112.5(19) .
N4 H4N O15 0.904(15) 1.83(2) 2.584(3) 140(2) .
N4 H4N O13 0.904(15) 2.16(2) 2.648(3) 113(2) .
N5 H5N O17 0.903(15) 1.919(19) 2.701(3) 144(2) .
O10 H10A O2S 0.862(15) 1.878(18) 2.722(5) 166(2) .
O20 H20A O1S 0.887(15) 1.858(16) 2.709(6) 160(2) .
O1S H1S O4 0.83 1.84 2.643(4) 163.2 .
O2S H2S O14 0.83 1.84 2.670(4) 173.7 1_556

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.220
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.050
_database_code_depnum_ccdc_archive 'CCDC 1017709'
