# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2015

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#                                CCDC 
# 
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# 
#  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.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
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#  except for the purpose of generating routine backup copies
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data_1_[(N,N)Me2]3TAPB

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H33 N3'
_chemical_formula_weight         435.59

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   13.508(9)
_cell_length_b                   24.193(16)
_cell_length_c                   7.507(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.8640(10)
_cell_angle_gamma                90.00
_cell_volume                     2444(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3446
_cell_measurement_theta_min      2.9
_cell_measurement_theta_max      29.1

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.614
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18213
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_sigmaI/netI    0.0666
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         2.85
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4282
_reflns_number_gt                3331
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0'

_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.

Comments on restraints

Four carbon atoms have been found to have thermal parameters which become npd
during the anisotropic refinement of structure, and hence ISOR restraints were applied.

ISOR     0.010 C23A C23B
ISOR     0.010 C26A C26B

Apart from above restraints, one of the benzene rings C23-C28 has also been 
split into two parts, due to higher thermal parameters for these carbon atoms
 and  were treated with command flat.

;

_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)+(0.0484P)²+3.1463P] 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         4282
_refine_ls_number_parameters     329
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1581
_refine_ls_R_factor_gt           0.1283
_refine_ls_wR_factor_ref         0.2450
_refine_ls_wR_factor_gt          0.2274
_refine_ls_goodness_of_fit_ref   1.303
_refine_ls_restrained_S_all      1.299
_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
N1 N 1.0093(3) 0.31570(15) 0.0526(5) 0.0533(10) Uani 1 1 d . . .
N2 N 0.2118(3) 0.07702(14) 0.2492(5) 0.0591(11) Uani 1 1 d . . .
N3 N 0.2607(3) 0.58206(13) 0.3268(5) 0.0461(9) Uani 1 1 d . . .
C1 C 0.6056(3) 0.31988(15) 0.2234(5) 0.0367(9) Uani 1 1 d . . .
C2 C 0.5486(3) 0.27172(15) 0.2269(5) 0.0390(10) Uani 1 1 d . . .
H2 H 0.5795 0.2369 0.2116 0.047 Uiso 1 1 calc R . .
C3 C 0.4479(3) 0.27352(15) 0.2522(5) 0.0408(10) Uani 1 1 d . . .
C4 C 0.4041(3) 0.32495(16) 0.2757(6) 0.0470(11) Uani 1 1 d . A .
H4 H 0.3357 0.3265 0.2958 0.056 Uiso 1 1 calc R . .
C5 C 0.4575(3) 0.37425(15) 0.2707(5) 0.0419(10) Uani 1 1 d . . .
C6 C 0.5589(3) 0.37055(15) 0.2458(5) 0.0377(10) Uani 1 1 d . A .
H6 H 0.5970 0.4035 0.2441 0.045 Uiso 1 1 calc R . .
C7 C 0.7118(3) 0.31782(15) 0.1888(5) 0.0372(9) Uani 1 1 d . . .
C8 C 0.7814(3) 0.35567(16) 0.2619(6) 0.0430(10) Uani 1 1 d . . .
H8 H 0.7612 0.3829 0.3425 0.052 Uiso 1 1 calc R . .
C9 C 0.8796(3) 0.35468(16) 0.2199(5) 0.0437(10) Uani 1 1 d . . .
H9 H 0.9253 0.3809 0.2734 0.052 Uiso 1 1 calc R . .
C10 C 0.9125(3) 0.31555(16) 0.0999(5) 0.0391(10) Uani 1 1 d . . .
C11 C 0.8436(3) 0.27670(16) 0.0277(5) 0.0414(10) Uani 1 1 d . . .
H11 H 0.8635 0.2491 -0.0520 0.050 Uiso 1 1 calc R . .
C12 C 0.7464(3) 0.27849(15) 0.0727(5) 0.0377(10) Uani 1 1 d . . .
H12 H 0.7009 0.2517 0.0221 0.045 Uiso 1 1 calc R . .
C13 C 1.0810(3) 0.3547(2) 0.1270(7) 0.0678(15) Uani 1 1 d . . .
H13A H 1.1445 0.3486 0.0757 0.102 Uiso 1 1 calc R . .
H13B H 1.0901 0.3499 0.2570 0.102 Uiso 1 1 calc R . .
H13C H 1.0576 0.3923 0.0992 0.102 Uiso 1 1 calc R . .
C14 C 1.0391(3) 0.27457(19) -0.0715(6) 0.0565(13) Uani 1 1 d . . .
H14A H 1.1089 0.2804 -0.0933 0.085 Uiso 1 1 calc R . .
H14B H 0.9975 0.2777 -0.1844 0.085 Uiso 1 1 calc R . .
H14C H 1.0313 0.2376 -0.0209 0.085 Uiso 1 1 calc R . .
C15 C 0.3876(3) 0.22212(16) 0.2496(5) 0.0410(10) Uani 1 1 d . . .
C16 C 0.2902(3) 0.22091(17) 0.1723(6) 0.0490(11) Uani 1 1 d . . .
H16 H 0.2625 0.2538 0.1198 0.059 Uiso 1 1 calc R . .
C17 C 0.2321(3) 0.17369(17) 0.1689(6) 0.0500(11) Uani 1 1 d . . .
H17 H 0.1660 0.1747 0.1146 0.060 Uiso 1 1 calc R . .
C18 C 0.2702(3) 0.12454(17) 0.2451(6) 0.0470(11) Uani 1 1 d . . .
C19 C 0.3687(3) 0.12475(18) 0.3196(6) 0.0496(11) Uani 1 1 d . . .
H19 H 0.3973 0.0918 0.3699 0.060 Uiso 1 1 calc R . .
C20 C 0.4245(3) 0.17263(16) 0.3206(6) 0.0449(11) Uani 1 1 d . . .
H20 H 0.4912 0.1716 0.3721 0.054 Uiso 1 1 calc R . .
C21 C 0.1108(4) 0.0777(2) 0.1666(9) 0.0866(19) Uani 1 1 d . . .
H21A H 0.0805 0.0413 0.1796 0.130 Uiso 1 1 calc R . .
H21B H 0.1115 0.0866 0.0394 0.130 Uiso 1 1 calc R . .
H21C H 0.0722 0.1057 0.2250 0.130 Uiso 1 1 calc R . .
C22 C 0.2587(5) 0.0251(2) 0.2992(9) 0.103(2) Uani 1 1 d . . .
H22A H 0.2085 -0.0042 0.2950 0.154 Uiso 1 1 calc R . .
H22B H 0.2911 0.0280 0.4207 0.154 Uiso 1 1 calc R . .
H22C H 0.3085 0.0164 0.2159 0.154 Uiso 1 1 calc R . .
C23A C 0.4076(4) 0.43071(16) 0.3006(7) 0.041(3) Uani 0.517(5) 1 d PGDU A 1
C24A C 0.3053(4) 0.43375(19) 0.2612(8) 0.048(3) Uani 0.517(5) 1 d PGD A 1
H24A H 0.2684 0.4012 0.2305 0.057 Uiso 0.517(5) 1 calc PR A 1
C25A C 0.2571(3) 0.4844(2) 0.2667(9) 0.050(3) Uani 0.517(5) 1 d PGD A 1
H25A H 0.1872 0.4865 0.2397 0.061 Uiso 0.517(5) 1 calc PR A 1
C26A C 0.3112(4) 0.53202(19) 0.3116(7) 0.020(2) Uani 0.517(5) 1 d PGDU A 1
C27A C 0.4134(4) 0.52898(17) 0.3510(8) 0.049(2) Uani 0.517(5) 1 d PGD A 1
H27A H 0.4504 0.5615 0.3817 0.059 Uiso 0.517(5) 1 calc PR A 1
C28A C 0.4617(3) 0.47833(19) 0.3455(8) 0.044(2) Uani 0.517(5) 1 d PGD A 1
H28A H 0.5316 0.4763 0.3725 0.053 Uiso 0.517(5) 1 calc PR A 1
C23B C 0.4055(4) 0.42889(19) 0.2698(8) 0.034(3) Uani 0.483(5) 1 d PGDU A 2
C24B C 0.3158(5) 0.4311(2) 0.3474(9) 0.046(3) Uani 0.483(5) 1 d PGD A 2
H24B H 0.2880 0.3983 0.3920 0.056 Uiso 0.483(5) 1 calc PR A 2
C25B C 0.2666(4) 0.4812(3) 0.3599(10) 0.046(3) Uani 0.483(5) 1 d PGD A 2
H25B H 0.2053 0.4827 0.4130 0.055 Uiso 0.483(5) 1 calc PR A 2
C26B C 0.3072(5) 0.5292(2) 0.2948(9) 0.063(5) Uani 0.483(5) 1 d PGDU A 2
C27B C 0.3970(5) 0.52701(19) 0.2171(9) 0.051(3) Uani 0.483(5) 1 d PGD A 2
H27B H 0.4247 0.5598 0.1726 0.061 Uiso 0.483(5) 1 calc PR A 2
C28B C 0.4461(4) 0.4769(2) 0.2046(9) 0.043(2) Uani 0.483(5) 1 d PGD A 2
H28B H 0.5074 0.4754 0.1515 0.051 Uiso 0.483(5) 1 calc PR A 2
C29 C 0.3143(4) 0.63201(17) 0.2873(6) 0.0581(13) Uani 1 1 d . A .
H29A H 0.2731 0.6644 0.3073 0.087 Uiso 1 1 calc R . .
H29B H 0.3301 0.6313 0.1622 0.087 Uiso 1 1 calc R . .
H29C H 0.3761 0.6340 0.3657 0.087 Uiso 1 1 calc R . .
C30 C 0.1549(3) 0.5854(2) 0.2783(7) 0.0668(15) Uani 1 1 d . A .
H30A H 0.1316 0.6229 0.3001 0.100 Uiso 1 1 calc R . .
H30B H 0.1202 0.5591 0.3505 0.100 Uiso 1 1 calc R . .
H30C H 0.1412 0.5763 0.1513 0.100 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
N1 C10 1.383(5) . ?
N1 C13 1.432(5) . ?
N1 C14 1.443(5) . ?
N2 C18 1.396(5) . ?
N2 C22 1.442(6) . ?
N2 C21 1.449(6) . ?
N3 C26A 1.399(5) . ?
N3 C30 1.446(5) . ?
N3 C29 1.453(5) . ?
N3 C26B 1.454(6) . ?
C1 C6 1.395(5) . ?
C1 C2 1.398(5) . ?
C1 C7 1.480(5) . ?
C2 C3 1.391(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.395(5) . ?
C3 C15 1.486(5) . ?
C4 C5 1.396(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.401(5) . ?
C5 C23B 1.497(6) . ?
C5 C23A 1.548(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.391(5) . ?
C7 C12 1.397(5) . ?
C8 C9 1.390(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.405(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.399(5) . ?
C11 C12 1.385(5) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C20 1.386(5) . ?
C15 C16 1.393(6) . ?
C16 C17 1.385(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.399(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.398(6) . ?
C19 C20 1.382(5) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23A C24A 1.3900 . ?
C23A C28A 1.3900 . ?
C24A C25A 1.3900 . ?
C24A H24A 0.9500 . ?
C25A C26A 1.3900 . ?
C25A H25A 0.9500 . ?
C26A C27A 1.3900 . ?
C27A C28A 1.3900 . ?
C27A H27A 0.9500 . ?
C28A H28A 0.9500 . ?
C23B C24B 1.3900 . ?
C23B C28B 1.3900 . ?
C24B C25B 1.3900 . ?
C24B H24B 0.9500 . ?
C25B C26B 1.3900 . ?
C25B H25B 0.9500 . ?
C26B C27B 1.3900 . ?
C27B C28B 1.3900 . ?
C27B H27B 0.9500 . ?
C28B H28B 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?

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
C10 N1 C13 121.7(4) . . ?
C10 N1 C14 119.1(3) . . ?
C13 N1 C14 119.3(4) . . ?
C18 N2 C22 119.0(4) . . ?
C18 N2 C21 119.6(4) . . ?
C22 N2 C21 119.9(4) . . ?
C26A N3 C30 120.4(4) . . ?
C26A N3 C29 116.6(4) . . ?
C30 N3 C29 113.7(3) . . ?
C26A N3 C26B 5.6(4) . . ?
C30 N3 C26B 116.0(4) . . ?
C29 N3 C26B 117.9(4) . . ?
C6 C1 C2 118.4(3) . . ?
C6 C1 C7 120.3(3) . . ?
C2 C1 C7 121.2(3) . . ?
C3 C2 C1 121.5(3) . . ?
C3 C2 H2 119.2 . . ?
C1 C2 H2 119.2 . . ?
C2 C3 C4 118.4(3) . . ?
C2 C3 C15 120.9(3) . . ?
C4 C3 C15 120.7(4) . . ?
C3 C4 C5 122.2(4) . . ?
C3 C4 H4 118.9 . . ?
C5 C4 H4 118.9 . . ?
C4 C5 C6 117.5(3) . . ?
C4 C5 C23B 120.8(4) . . ?
C6 C5 C23B 121.3(4) . . ?
C4 C5 C23A 121.2(4) . . ?
C6 C5 C23A 121.2(4) . . ?
C23B C5 C23A 8.6(3) . . ?
C1 C6 C5 121.9(3) . . ?
C1 C6 H6 119.0 . . ?
C5 C6 H6 119.0 . . ?
C8 C7 C12 116.4(4) . . ?
C8 C7 C1 122.7(3) . . ?
C12 C7 C1 120.8(3) . . ?
C9 C8 C7 121.7(4) . . ?
C9 C8 H8 119.2 . . ?
C7 C8 H8 119.2 . . ?
C8 C9 C10 121.1(4) . . ?
C8 C9 H9 119.4 . . ?
C10 C9 H9 119.4 . . ?
N1 C10 C11 121.0(4) . . ?
N1 C10 C9 121.3(4) . . ?
C11 C10 C9 117.7(4) . . ?
C12 C11 C10 119.9(4) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C11 C12 C7 123.2(4) . . ?
C11 C12 H12 118.4 . . ?
C7 C12 H12 118.4 . . ?
N1 C13 H13A 109.5 . . ?
N1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N1 C14 H14A 109.5 . . ?
N1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C20 C15 C16 116.0(4) . . ?
C20 C15 C3 122.6(4) . . ?
C16 C15 C3 121.4(4) . . ?
C17 C16 C15 122.6(4) . . ?
C17 C16 H16 118.7 . . ?
C15 C16 H16 118.7 . . ?
C16 C17 C18 120.3(4) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
N2 C18 C19 121.0(4) . . ?
N2 C18 C17 121.3(4) . . ?
C19 C18 C17 117.7(4) . . ?
C20 C19 C18 120.3(4) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C19 C20 C15 122.9(4) . . ?
C19 C20 H20 118.5 . . ?
C15 C20 H20 118.5 . . ?
N2 C21 H21A 109.5 . . ?
N2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N2 C22 H22A 109.5 . . ?
N2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24A C23A C28A 120.0 . . ?
C24A C23A C5 116.9(3) . . ?
C28A C23A C5 122.7(3) . . ?
C25A C24A C23A 120.0 . . ?
C25A C24A H24A 120.0 . . ?
C23A C24A H24A 120.0 . . ?
C24A C25A C26A 120.0 . . ?
C24A C25A H25A 120.0 . . ?
C26A C25A H25A 120.0 . . ?
C25A C26A C27A 120.0 . . ?
C25A C26A N3 119.2(4) . . ?
C27A C26A N3 120.7(4) . . ?
C28A C27A C26A 120.0 . . ?
C28A C27A H27A 120.0 . . ?
C26A C27A H27A 120.0 . . ?
C27A C28A C23A 120.0 . . ?
C27A C28A H28A 120.0 . . ?
C23A C28A H28A 120.0 . . ?
C24B C23B C28B 120.0 . . ?
C24B C23B C5 117.2(4) . . ?
C28B C23B C5 122.7(4) . . ?
C23B C24B C25B 120.0 . . ?
C23B C24B H24B 120.0 . . ?
C25B C24B H24B 120.0 . . ?
C26B C25B C24B 120.0 . . ?
C26B C25B H25B 120.0 . . ?
C24B C25B H25B 120.0 . . ?
C25B C26B C27B 120.0 . . ?
C25B C26B N3 119.1(4) . . ?
C27B C26B N3 120.5(4) . . ?
C28B C27B C26B 120.0 . . ?
C28B C27B H27B 120.0 . . ?
C26B C27B H27B 120.0 . . ?
C27B C28B C23B 120.0 . . ?
C27B C28B H28B 120.0 . . ?
C23B C28B H28B 120.0 . . ?
N3 C29 H29A 109.5 . . ?
N3 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
N3 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C30 H30A 109.5 . . ?
N3 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
N3 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?

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
C6 C1 C2 C3 -0.1(6) . . . . ?
C7 C1 C2 C3 -177.4(4) . . . . ?
C1 C2 C3 C4 -0.5(6) . . . . ?
C1 C2 C3 C15 178.0(4) . . . . ?
C2 C3 C4 C5 1.4(6) . . . . ?
C15 C3 C4 C5 -177.0(4) . . . . ?
C3 C4 C5 C6 -1.7(6) . . . . ?
C3 C4 C5 C23B 171.0(4) . . . . ?
C3 C4 C5 C23A -178.9(4) . . . . ?
C2 C1 C6 C5 -0.2(6) . . . . ?
C7 C1 C6 C5 177.1(4) . . . . ?
C4 C5 C6 C1 1.1(6) . . . . ?
C23B C5 C6 C1 -171.6(4) . . . . ?
C23A C5 C6 C1 178.3(4) . . . . ?
C6 C1 C7 C8 33.9(6) . . . . ?
C2 C1 C7 C8 -148.8(4) . . . . ?
C6 C1 C7 C12 -143.1(4) . . . . ?
C2 C1 C7 C12 34.1(6) . . . . ?
C12 C7 C8 C9 0.7(6) . . . . ?
C1 C7 C8 C9 -176.5(4) . . . . ?
C7 C8 C9 C10 0.7(6) . . . . ?
C13 N1 C10 C11 -179.1(4) . . . . ?
C14 N1 C10 C11 -0.8(6) . . . . ?
C13 N1 C10 C9 1.7(6) . . . . ?
C14 N1 C10 C9 -180.0(4) . . . . ?
C8 C9 C10 N1 177.5(4) . . . . ?
C8 C9 C10 C11 -1.7(6) . . . . ?
N1 C10 C11 C12 -177.9(4) . . . . ?
C9 C10 C11 C12 1.3(6) . . . . ?
C10 C11 C12 C7 0.1(6) . . . . ?
C8 C7 C12 C11 -1.0(6) . . . . ?
C1 C7 C12 C11 176.2(4) . . . . ?
C2 C3 C15 C20 37.2(6) . . . . ?
C4 C3 C15 C20 -144.4(4) . . . . ?
C2 C3 C15 C16 -141.9(4) . . . . ?
C4 C3 C15 C16 36.6(6) . . . . ?
C20 C15 C16 C17 1.3(6) . . . . ?
C3 C15 C16 C17 -179.6(4) . . . . ?
C15 C16 C17 C18 0.1(7) . . . . ?
C22 N2 C18 C19 -12.0(7) . . . . ?
C21 N2 C18 C19 -178.4(5) . . . . ?
C22 N2 C18 C17 168.9(5) . . . . ?
C21 N2 C18 C17 2.6(7) . . . . ?
C16 C17 C18 N2 177.6(4) . . . . ?
C16 C17 C18 C19 -1.5(6) . . . . ?
N2 C18 C19 C20 -177.6(4) . . . . ?
C17 C18 C19 C20 1.5(6) . . . . ?
C18 C19 C20 C15 0.0(7) . . . . ?
C16 C15 C20 C19 -1.4(6) . . . . ?
C3 C15 C20 C19 179.6(4) . . . . ?
C4 C5 C23A C24A -25.2(6) . . . . ?
C6 C5 C23A C24A 157.7(4) . . . . ?
C23B C5 C23A C24A 65(2) . . . . ?
C4 C5 C23A C28A 161.8(4) . . . . ?
C6 C5 C23A C28A -15.3(6) . . . . ?
C23B C5 C23A C28A -108(2) . . . . ?
C28A C23A C24A C25A 0.0 . . . . ?
C5 C23A C24A C25A -173.2(4) . . . . ?
C23A C24A C25A C26A 0.0 . . . . ?
C24A C25A C26A C27A 0.0 . . . . ?
C24A C25A C26A N3 -176.2(4) . . . . ?
C30 N3 C26A C25A -6.4(6) . . . . ?
C29 N3 C26A C25A -151.0(4) . . . . ?
C26B N3 C26A C25A -46(4) . . . . ?
C30 N3 C26A C27A 177.4(4) . . . . ?
C29 N3 C26A C27A 32.8(5) . . . . ?
C26B N3 C26A C27A 137(4) . . . . ?
C25A C26A C27A C28A 0.0 . . . . ?
N3 C26A C27A C28A 176.2(4) . . . . ?
C26A C27A C28A C23A 0.0 . . . . ?
C24A C23A C28A C27A 0.0 . . . . ?
C5 C23A C28A C27A 172.8(4) . . . . ?
C4 C5 C23B C24B 26.6(6) . . . . ?
C6 C5 C23B C24B -160.9(4) . . . . ?
C23A C5 C23B C24B -69(2) . . . . ?
C4 C5 C23B C28B -157.2(4) . . . . ?
C6 C5 C23B C28B 15.3(6) . . . . ?
C23A C5 C23B C28B 107(2) . . . . ?
C28B C23B C24B C25B 0.0 . . . . ?
C5 C23B C24B C25B 176.3(5) . . . . ?
C23B C24B C25B C26B 0.0 . . . . ?
C24B C25B C26B C27B 0.0 . . . . ?
C24B C25B C26B N3 -173.2(6) . . . . ?
C26A N3 C26B C25B 90(4) . . . . ?
C30 N3 C26B C25B -51.4(6) . . . . ?
C29 N3 C26B C25B 168.8(4) . . . . ?
C26A N3 C26B C27B -83(4) . . . . ?
C30 N3 C26B C27B 135.4(4) . . . . ?
C29 N3 C26B C27B -4.4(6) . . . . ?
C25B C26B C27B C28B 0.0 . . . . ?
N3 C26B C27B C28B 173.1(6) . . . . ?
C26B C27B C28B C23B 0.0 . . . . ?
C24B C23B C28B C27B 0.0 . . . . ?
C5 C23B C28B C27B -176.1(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.051
_database_code_depnum_ccdc_archive 'CCDC 1010527'
#######################################################################
#
#                 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_2_[(N,N)Me2]3TAPB-PA

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H42 N12 O21'
_chemical_formula_weight         1122.94

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           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.766(3)
_cell_length_b                   13.960(5)
_cell_length_c                   17.294(6)
_cell_angle_alpha                102.357(5)
_cell_angle_beta                 98.189(5)
_cell_angle_gamma                100.935(4)
_cell_volume                     2447.0(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3237
_cell_measurement_theta_min      2.7
_cell_measurement_theta_max      25.3

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1164
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       "'profile data from ω-scans'"
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18789
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.52
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8546
_reflns_number_gt                6702
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0'

_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)+(0.0663P)²+1.5798P] 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         8546
_refine_ls_number_parameters     730
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0662
_refine_ls_wR_factor_ref         0.1631
_refine_ls_wR_factor_gt          0.1486
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_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 0.3269(2) 0.49937(15) -0.44357(12) 0.0352(5) Uani 1 1 d . . .
O2 O 0.2008(2) 0.64823(16) -0.45552(13) 0.0435(6) Uani 1 1 d . . .
O3 O 0.0253(2) 0.59180(17) -0.54567(14) 0.0424(6) Uani 1 1 d . . .
O4 O 0.0740(2) 0.42038(18) -0.80591(14) 0.0480(6) Uani 1 1 d . . .
O5 O 0.1539(2) 0.28841(18) -0.81160(14) 0.0497(6) Uani 1 1 d . . .
O6 O 0.4643(2) 0.36372(19) -0.46714(13) 0.0461(6) Uani 1 1 d . . .
O7 O 0.4725(2) 0.29181(18) -0.58859(14) 0.0470(6) Uani 1 1 d . . .
O8 O 1.2193(2) 0.04659(16) -0.00484(13) 0.0358(5) Uani 1 1 d . . .
O9 O 1.2379(2) -0.08810(18) -0.14320(13) 0.0439(6) Uani 1 1 d . . .
O10 O 1.2206(2) -0.23261(17) -0.11350(14) 0.0440(6) Uani 1 1 d . . .
O11 O 1.5810(3) -0.2234(2) 0.0967(2) 0.0787(10) Uani 1 1 d . . .
O12 O 1.6108(2) -0.1109(2) 0.20938(17) 0.0574(7) Uani 1 1 d . . .
O13 O 1.3591(2) 0.14859(19) 0.22429(14) 0.0500(6) Uani 1 1 d . . .
O14 O 1.3624(3) 0.20858(18) 0.11814(17) 0.0558(7) Uani 1 1 d . . .
O15 O 1.1825(2) 0.78847(17) 0.42933(13) 0.0389(5) Uani 1 1 d . . .
O16 O 1.3096(2) 0.6989(2) 0.32527(16) 0.0571(8) Uani 1 1 d . . .
O17 O 1.5028(3) 0.7798(2) 0.33087(17) 0.0653(8) Uani 1 1 d . . .
O18 O 1.7648(3) 0.9544(2) 0.5835(2) 0.0749(9) Uani 1 1 d . . .
O19 O 1.6792(3) 1.0302(2) 0.67808(18) 0.0719(9) Uani 1 1 d . . .
O20 O 1.2276(3) 0.9114(2) 0.66843(15) 0.0605(7) Uani 1 1 d . . .
O21 O 1.1010(2) 0.88993(18) 0.55438(14) 0.0451(6) Uani 1 1 d . . .
N1 N 1.0380(2) 0.04986(17) -0.13084(14) 0.0252(5) Uani 1 1 d . . .
N2 N 0.9258(2) 0.78046(17) 0.39434(14) 0.0252(5) Uani 1 1 d . . .
N3 N 0.3204(2) 0.61081(17) -0.29678(14) 0.0249(5) Uani 1 1 d . . .
N4 N 0.1367(2) 0.58904(18) -0.51805(15) 0.0326(6) Uani 1 1 d . . .
N5 N 0.1353(2) 0.3681(2) -0.77430(15) 0.0345(6) Uani 1 1 d . . .
N6 N 0.4275(2) 0.34701(18) -0.54018(15) 0.0307(6) Uani 1 1 d . . .
N7 N 1.2569(2) -0.1396(2) -0.09507(16) 0.0331(6) Uani 1 1 d . . .
N8 N 1.5616(3) -0.1470(2) 0.1375(2) 0.0487(8) Uani 1 1 d . . .
N9 N 1.3641(2) 0.1403(2) 0.15183(18) 0.0386(7) Uani 1 1 d . . .
N10 N 1.4057(3) 0.7634(2) 0.35999(17) 0.0379(7) Uani 1 1 d . . .
N11 N 1.6702(3) 0.9724(2) 0.6120(2) 0.0558(9) Uani 1 1 d . . .
N12 N 1.2076(3) 0.89686(19) 0.59413(16) 0.0373(6) Uani 1 1 d . . .
C1 C 0.8152(3) 0.3902(2) -0.03307(17) 0.0238(6) Uani 1 1 d . . .
C2 C 0.8496(3) 0.4522(2) 0.04565(17) 0.0245(6) Uani 1 1 d . . .
H2 H 0.9068 0.4354 0.0851 0.029 Uiso 1 1 calc R . .
C3 C 0.8012(3) 0.5379(2) 0.06689(17) 0.0238(6) Uani 1 1 d . . .
C4 C 0.7162(3) 0.5612(2) 0.00889(17) 0.0253(6) Uani 1 1 d . . .
H4 H 0.6835 0.6199 0.0231 0.030 Uiso 1 1 calc R . .
C5 C 0.6779(3) 0.5003(2) -0.06956(17) 0.0250(6) Uani 1 1 d . . .
C6 C 0.7288(3) 0.4155(2) -0.08953(17) 0.0249(6) Uani 1 1 d . . .
H6 H 0.7042 0.3739 -0.1429 0.030 Uiso 1 1 calc R . .
C7 C 0.8694(3) 0.2991(2) -0.05608(16) 0.0226(6) Uani 1 1 d . . .
C8 C 0.9803(3) 0.2881(2) -0.00987(17) 0.0260(6) Uani 1 1 d . . .
H8 H 1.0201 0.3380 0.0384 0.031 Uiso 1 1 calc R . .
C9 C 1.0345(3) 0.2060(2) -0.03255(17) 0.0268(6) Uani 1 1 d . . .
H9 H 1.1103 0.1999 -0.0003 0.032 Uiso 1 1 calc R . .
C10 C 0.9763(3) 0.1335(2) -0.10273(17) 0.0232(6) Uani 1 1 d . . .
C11 C 0.8645(3) 0.1410(2) -0.14907(17) 0.0276(6) Uani 1 1 d . . .
H11 H 0.8241 0.0901 -0.1967 0.033 Uiso 1 1 calc R . .
C12 C 0.8117(3) 0.2231(2) -0.12569(17) 0.0275(6) Uani 1 1 d . . .
H12 H 0.7347 0.2278 -0.1576 0.033 Uiso 1 1 calc R . .
C13 C 0.9506(3) -0.0522(2) -0.1468(2) 0.0391(8) Uani 1 1 d . . .
H13A H 0.9975 -0.1040 -0.1647 0.059 Uiso 1 1 calc R . .
H13B H 0.8762 -0.0583 -0.1889 0.059 Uiso 1 1 calc R . .
H13C H 0.9209 -0.0611 -0.0972 0.059 Uiso 1 1 calc R . .
C14 C 1.0895(3) 0.0626(3) -0.2051(2) 0.0425(8) Uani 1 1 d . . .
H14A H 1.1307 0.0073 -0.2235 0.064 Uiso 1 1 calc R . .
H14B H 1.1529 0.1269 -0.1926 0.064 Uiso 1 1 calc R . .
H14C H 1.0185 0.0619 -0.2476 0.064 Uiso 1 1 calc R . .
C15 C 0.8353(3) 0.6020(2) 0.15112(17) 0.0245(6) Uani 1 1 d . . .
C16 C 0.9595(3) 0.6222(2) 0.19689(17) 0.0242(6) Uani 1 1 d . . .
H16 H 1.0244 0.5955 0.1737 0.029 Uiso 1 1 calc R . .
C17 C 0.9895(3) 0.6808(2) 0.27588(17) 0.0246(6) Uani 1 1 d . . .
H17 H 1.0742 0.6942 0.3065 0.029 Uiso 1 1 calc R . .
C18 C 0.8943(3) 0.7192(2) 0.30933(17) 0.0246(6) Uani 1 1 d . . .
C19 C 0.7710(3) 0.7012(2) 0.26499(17) 0.0267(6) Uani 1 1 d . . .
H19 H 0.7066 0.7284 0.2883 0.032 Uiso 1 1 calc R . .
C20 C 0.7424(3) 0.6432(2) 0.18659(18) 0.0263(6) Uani 1 1 d . . .
H20 H 0.6578 0.6311 0.1561 0.032 Uiso 1 1 calc R . .
C21 C 0.9210(3) 0.8879(2) 0.3992(2) 0.0376(8) Uani 1 1 d . . .
H21A H 0.9423 0.9260 0.4559 0.056 Uiso 1 1 calc R . .
H21B H 0.8342 0.8912 0.3754 0.056 Uiso 1 1 calc R . .
H21C H 0.9834 0.9170 0.3697 0.056 Uiso 1 1 calc R . .
C22 C 0.8381(3) 0.7369(2) 0.44489(19) 0.0338(7) Uani 1 1 d . . .
H22A H 0.8614 0.7788 0.5003 0.051 Uiso 1 1 calc R . .
H22B H 0.8472 0.6683 0.4447 0.051 Uiso 1 1 calc R . .
H22C H 0.7486 0.7352 0.4225 0.051 Uiso 1 1 calc R . .
C23 C 0.5838(3) 0.5257(2) -0.12919(17) 0.0242(6) Uani 1 1 d . . .
C24 C 0.4952(3) 0.5813(2) -0.10357(17) 0.0264(6) Uani 1 1 d . . .
H24 H 0.4940 0.6011 -0.0476 0.032 Uiso 1 1 calc R . .
C25 C 0.4097(3) 0.6080(2) -0.15780(17) 0.0258(6) Uani 1 1 d . . .
H25 H 0.3505 0.6460 -0.1393 0.031 Uiso 1 1 calc R . .
C26 C 0.4104(3) 0.5793(2) -0.23933(17) 0.0240(6) Uani 1 1 d . . .
C27 C 0.4923(3) 0.5216(2) -0.26773(17) 0.0264(6) Uani 1 1 d . . .
H27 H 0.4898 0.4999 -0.3240 0.032 Uiso 1 1 calc R . .
C28 C 0.5789(3) 0.4954(2) -0.21267(17) 0.0257(6) Uani 1 1 d . . .
H28 H 0.6362 0.4560 -0.2320 0.031 Uiso 1 1 calc R . .
C29 C 0.1826(3) 0.5708(2) -0.29341(19) 0.0330(7) Uani 1 1 d . . .
H29A H 0.1263 0.5930 -0.3323 0.050 Uiso 1 1 calc R . .
H29B H 0.1675 0.5962 -0.2390 0.050 Uiso 1 1 calc R . .
H29C H 0.1638 0.4970 -0.3067 0.050 Uiso 1 1 calc R . .
C30 C 0.3482(3) 0.7229(2) -0.28388(18) 0.0305(7) Uani 1 1 d . . .
H30A H 0.2872 0.7408 -0.3230 0.046 Uiso 1 1 calc R . .
H30B H 0.4363 0.7473 -0.2911 0.046 Uiso 1 1 calc R . .
H30C H 0.3393 0.7539 -0.2291 0.046 Uiso 1 1 calc R . .
C31 C 0.2873(3) 0.4718(2) -0.51851(17) 0.0267(6) Uani 1 1 d . . .
C32 C 0.1929(3) 0.5126(2) -0.56207(17) 0.0263(6) Uani 1 1 d . . .
C33 C 0.1461(3) 0.4811(2) -0.64352(17) 0.0278(6) Uani 1 1 d . . .
H33 H 0.0862 0.5123 -0.6687 0.033 Uiso 1 1 calc R . .
C34 C 0.1878(3) 0.4027(2) -0.68836(17) 0.0286(7) Uani 1 1 d . . .
C35 C 0.2776(3) 0.3589(2) -0.65338(17) 0.0269(6) Uani 1 1 d . . .
H35 H 0.3052 0.3053 -0.6851 0.032 Uiso 1 1 calc R . .
C36 C 0.3271(3) 0.3933(2) -0.57198(17) 0.0246(6) Uani 1 1 d . . .
C37 C 1.3013(3) 0.0050(2) 0.02440(18) 0.0293(7) Uani 1 1 d . . .
C38 C 1.3260(3) -0.0899(2) -0.01428(18) 0.0297(7) Uani 1 1 d . . .
C39 C 1.4082(3) -0.1391(2) 0.02166(19) 0.0337(7) Uani 1 1 d . . .
H39 H 1.4192 -0.2022 -0.0067 0.040 Uiso 1 1 calc R . .
C40 C 1.4749(3) -0.0949(2) 0.1001(2) 0.0357(7) Uani 1 1 d . . .
C41 C 1.4586(3) -0.0044(2) 0.14232(19) 0.0349(7) Uani 1 1 d . . .
H41 H 1.5033 0.0244 0.1963 0.042 Uiso 1 1 calc R . .
C42 C 1.3772(3) 0.0435(2) 0.10563(18) 0.0310(7) Uani 1 1 d . . .
C43 C 1.2921(3) 0.8290(2) 0.47067(18) 0.0290(7) Uani 1 1 d . . .
C44 C 1.4104(3) 0.8228(2) 0.44172(18) 0.0298(7) Uani 1 1 d . . .
C45 C 1.5306(3) 0.8691(2) 0.4862(2) 0.0360(7) Uani 1 1 d . . .
H45 H 1.6049 0.8633 0.4634 0.043 Uiso 1 1 calc R . .
C46 C 1.5430(3) 0.9244(2) 0.5646(2) 0.0387(8) Uani 1 1 d . . .
C47 C 1.4364(3) 0.9331(2) 0.59900(19) 0.0378(8) Uani 1 1 d . . .
H47 H 1.4462 0.9704 0.6532 0.045 Uiso 1 1 calc R . .
C48 C 1.3161(3) 0.8873(2) 0.55393(18) 0.0306(7) Uani 1 1 d . . .
H3W H 0.3330 0.5774 -0.3515 0.080 Uiso 1 1 d . . .
H2W H 1.0210 0.7848 0.4199 0.080 Uiso 1 1 d . . .
H1W H 1.1095 0.0443 -0.0882 0.080 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 O1 0.000(7) 1 ?
O1 C31 1.256(3) . ?
O2 N4 1.232(3) . ?
O3 N4 1.238(3) . ?
O4 N5 1.232(3) . ?
O5 N5 1.228(3) . ?
O6 N6 1.226(3) . ?
O7 N6 1.230(3) . ?
O8 O8 0.000(7) 1 ?
O8 C37 1.251(4) . ?
O9 O9 0.0000 1 ?
O9 N7 1.231(3) . ?
O10 N7 1.239(3) . ?
O11 N8 1.218(4) . ?
O12 N8 1.234(4) . ?
O13 N9 1.243(4) . ?
O14 N9 1.220(4) . ?
O15 O15 0.000(5) 1 ?
O15 C43 1.247(4) . ?
O16 N10 1.217(3) . ?
O17 N10 1.228(3) . ?
O18 N11 1.236(4) . ?
O19 N11 1.230(4) . ?
O20 N12 1.238(3) . ?
O21 O21 0.000(8) 1 ?
O21 N12 1.226(3) . ?
N1 C10 1.479(3) . ?
N1 C13 1.497(4) . ?
N1 C14 1.500(4) . ?
N1 H1W 1.014(2) . ?
N2 C18 1.489(3) . ?
N2 C21 1.495(4) . ?
N2 C22 1.507(4) . ?
N2 H2W 1.042(2) . ?
N3 C26 1.481(3) . ?
N3 C29 1.497(4) . ?
N3 C30 1.497(4) . ?
N3 H3W 1.002(2) . ?
N4 C32 1.453(4) . ?
N5 C34 1.453(4) . ?
N6 C36 1.460(4) . ?
N7 O9 1.231(3) 1 ?
N7 C38 1.442(4) . ?
N8 C40 1.451(4) . ?
N9 C42 1.459(4) . ?
N10 C44 1.466(4) . ?
N11 C46 1.447(4) . ?
N12 O21 1.226(3) 1 ?
N12 C48 1.455(4) . ?
C1 C6 1.399(4) . ?
C1 C2 1.403(4) . ?
C1 C7 1.499(4) . ?
C2 C3 1.394(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.393(4) . ?
C3 C15 1.491(4) . ?
C4 C5 1.396(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.395(4) . ?
C5 C23 1.487(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.393(4) . ?
C7 C12 1.397(4) . ?
C8 C9 1.390(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.381(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.382(4) . ?
C11 C12 1.383(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C20 1.396(4) . ?
C15 C16 1.397(4) . ?
C16 C17 1.391(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.384(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.384(4) . ?
C19 C20 1.380(4) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.401(4) . ?
C23 C28 1.405(4) . ?
C24 C25 1.378(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.383(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.375(4) . ?
C27 C28 1.391(4) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 O1 1.256(3) 1 ?
C31 C36 1.449(4) . ?
C31 C32 1.453(4) . ?
C32 C33 1.371(4) . ?
C33 C34 1.386(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.376(4) . ?
C35 C36 1.377(4) . ?
C35 H35 0.9500 . ?
C37 O8 1.251(4) 1 ?
C37 C38 1.442(4) . ?
C37 C42 1.454(4) . ?
C38 C39 1.377(4) . ?
C39 C40 1.390(4) . ?
C39 H39 0.9500 . ?
C40 C41 1.373(4) . ?
C41 C42 1.365(4) . ?
C41 H41 0.9500 . ?
C43 O15 1.247(3) 1 ?
C43 C44 1.444(4) . ?
C43 C48 1.454(4) . ?
C44 C45 1.367(4) . ?
C45 C46 1.383(5) . ?
C45 H45 0.9500 . ?
C46 C47 1.380(5) . ?
C47 C48 1.370(4) . ?
C47 H47 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 O1 C31 0(10) 1 . ?
O8 O8 C37 0(10) 1 . ?
O9 O9 N7 0(10) 1 . ?
O15 O15 C43 0(10) 1 . ?
O21 O21 N12 0(10) 1 . ?
C10 N1 C13 113.6(2) . . ?
C10 N1 C14 109.6(2) . . ?
C13 N1 C14 110.1(2) . . ?
C10 N1 H1W 112.9(2) . . ?
C13 N1 H1W 100.4(2) . . ?
C14 N1 H1W 110.0(2) . . ?
C18 N2 C21 111.6(2) . . ?
C18 N2 C22 111.6(2) . . ?
C21 N2 C22 110.2(2) . . ?
C18 N2 H2W 110.5(2) . . ?
C21 N2 H2W 103.7(2) . . ?
C22 N2 H2W 109.0(2) . . ?
C26 N3 C29 112.0(2) . . ?
C26 N3 C30 111.8(2) . . ?
C29 N3 C30 110.4(2) . . ?
C26 N3 H3W 105.0(2) . . ?
C29 N3 H3W 106.3(2) . . ?
C30 N3 H3W 111.1(2) . . ?
O2 N4 O3 122.7(2) . . ?
O2 N4 C32 119.4(2) . . ?
O3 N4 C32 117.9(2) . . ?
O5 N5 O4 123.4(3) . . ?
O5 N5 C34 118.5(3) . . ?
O4 N5 C34 118.0(3) . . ?
O6 N6 O7 122.0(3) . . ?
O6 N6 C36 120.0(2) . . ?
O7 N6 C36 118.0(2) . . ?
O9 N7 O9 0.00(18) 1 . ?
O9 N7 O10 122.7(3) 1 . ?
O9 N7 O10 122.7(3) . . ?
O9 N7 C38 118.8(3) 1 . ?
O9 N7 C38 118.8(3) . . ?
O10 N7 C38 118.6(3) . . ?
O11 N8 O12 124.0(3) . . ?
O11 N8 C40 118.6(3) . . ?
O12 N8 C40 117.5(3) . . ?
O14 N9 O13 124.1(3) . . ?
O14 N9 C42 118.6(3) . . ?
O13 N9 C42 117.3(3) . . ?
O16 N10 O17 123.0(3) . . ?
O16 N10 C44 119.7(3) . . ?
O17 N10 C44 117.2(3) . . ?
O19 N11 O18 123.1(3) . . ?
O19 N11 C46 118.5(4) . . ?
O18 N11 C46 118.4(3) . . ?
O21 N12 O21 0.00(12) 1 . ?
O21 N12 O20 122.5(3) 1 . ?
O21 N12 O20 122.5(3) . . ?
O21 N12 C48 120.0(3) 1 . ?
O21 N12 C48 120.0(3) . . ?
O20 N12 C48 117.6(3) . . ?
C6 C1 C2 118.3(3) . . ?
C6 C1 C7 120.8(2) . . ?
C2 C1 C7 120.9(2) . . ?
C3 C2 C1 121.1(3) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C4 C3 C2 119.0(3) . . ?
C4 C3 C15 120.1(2) . . ?
C2 C3 C15 120.8(3) . . ?
C3 C4 C5 121.5(3) . . ?
C3 C4 H4 119.2 . . ?
C5 C4 H4 119.2 . . ?
C6 C5 C4 118.3(3) . . ?
C6 C5 C23 121.6(2) . . ?
C4 C5 C23 120.0(2) . . ?
C5 C6 C1 121.8(3) . . ?
C5 C6 H6 119.1 . . ?
C1 C6 H6 119.1 . . ?
C8 C7 C12 117.6(2) . . ?
C8 C7 C1 121.3(2) . . ?
C12 C7 C1 121.1(2) . . ?
C9 C8 C7 121.8(3) . . ?
C9 C8 H8 119.1 . . ?
C7 C8 H8 119.1 . . ?
C10 C9 C8 118.9(3) . . ?
C10 C9 H9 120.5 . . ?
C8 C9 H9 120.5 . . ?
C9 C10 C11 120.8(3) . . ?
C9 C10 N1 119.6(2) . . ?
C11 C10 N1 119.6(2) . . ?
C10 C11 C12 119.6(3) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
C11 C12 C7 121.3(3) . . ?
C11 C12 H12 119.3 . . ?
C7 C12 H12 119.3 . . ?
N1 C13 H13A 109.5 . . ?
N1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N1 C14 H14A 109.5 . . ?
N1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C20 C15 C16 118.1(3) . . ?
C20 C15 C3 120.2(2) . . ?
C16 C15 C3 121.6(2) . . ?
C17 C16 C15 121.0(3) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C18 C17 C16 119.2(3) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
C19 C18 C17 120.9(3) . . ?
C19 C18 N2 119.9(2) . . ?
C17 C18 N2 119.2(2) . . ?
C20 C19 C18 119.4(3) . . ?
C20 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
C19 C20 C15 121.3(3) . . ?
C19 C20 H20 119.3 . . ?
C15 C20 H20 119.3 . . ?
N2 C21 H21A 109.5 . . ?
N2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N2 C22 H22A 109.5 . . ?
N2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C28 117.2(3) . . ?
C24 C23 C5 120.6(2) . . ?
C28 C23 C5 122.2(2) . . ?
C25 C24 C23 121.4(3) . . ?
C25 C24 H24 119.3 . . ?
C23 C24 H24 119.3 . . ?
C24 C25 C26 119.7(3) . . ?
C24 C25 H25 120.2 . . ?
C26 C25 H25 120.2 . . ?
C27 C26 C25 121.2(3) . . ?
C27 C26 N3 119.7(2) . . ?
C25 C26 N3 119.1(2) . . ?
C26 C27 C28 118.9(3) . . ?
C26 C27 H27 120.6 . . ?
C28 C27 H27 120.6 . . ?
C27 C28 C23 121.7(3) . . ?
C27 C28 H28 119.2 . . ?
C23 C28 H28 119.2 . . ?
N3 C29 H29A 109.5 . . ?
N3 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
N3 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C30 H30A 109.5 . . ?
N3 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
N3 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O1 C31 O1 0.0(3) 1 . ?
O1 C31 C36 124.2(3) 1 . ?
O1 C31 C36 124.2(3) . . ?
O1 C31 C32 124.2(3) 1 . ?
O1 C31 C32 124.2(3) . . ?
C36 C31 C32 111.6(2) . . ?
C33 C32 C31 124.7(3) . . ?
C33 C32 N4 115.6(3) . . ?
C31 C32 N4 119.6(2) . . ?
C32 C33 C34 118.7(3) . . ?
C32 C33 H33 120.7 . . ?
C34 C33 H33 120.7 . . ?
C35 C34 C33 121.5(3) . . ?
C35 C34 N5 120.2(3) . . ?
C33 C34 N5 118.3(3) . . ?
C34 C35 C36 119.4(3) . . ?
C34 C35 H35 120.3 . . ?
C36 C35 H35 120.3 . . ?
C35 C36 C31 124.1(3) . . ?
C35 C36 N6 116.2(2) . . ?
C31 C36 N6 119.8(2) . . ?
O8 C37 O8 0.0(2) 1 . ?
O8 C37 C38 125.3(3) 1 . ?
O8 C37 C38 125.3(3) . . ?
O8 C37 C42 123.4(3) 1 . ?
O8 C37 C42 123.4(3) . . ?
C38 C37 C42 111.1(3) . . ?
C39 C38 N7 117.0(3) . . ?
C39 C38 C37 124.5(3) . . ?
N7 C38 C37 118.4(3) . . ?
C38 C39 C40 119.0(3) . . ?
C38 C39 H39 120.5 . . ?
C40 C39 H39 120.5 . . ?
C41 C40 C39 121.2(3) . . ?
C41 C40 N8 120.1(3) . . ?
C39 C40 N8 118.7(3) . . ?
C42 C41 C40 119.0(3) . . ?
C42 C41 H41 120.5 . . ?
C40 C41 H41 120.5 . . ?
C41 C42 C37 125.1(3) . . ?
C41 C42 N9 117.5(3) . . ?
C37 C42 N9 117.4(3) . . ?
O15 C43 O15 0.0(3) 1 . ?
O15 C43 C44 124.0(3) 1 . ?
O15 C43 C44 124.0(3) . . ?
O15 C43 C48 124.1(3) 1 . ?
O15 C43 C48 124.1(3) . . ?
C44 C43 C48 111.9(3) . . ?
C45 C44 C43 124.2(3) . . ?
C45 C44 N10 116.0(3) . . ?
C43 C44 N10 119.8(3) . . ?
C44 C45 C46 119.4(3) . . ?
C44 C45 H45 120.3 . . ?
C46 C45 H45 120.3 . . ?
C47 C46 C45 121.2(3) . . ?
C47 C46 N11 119.3(3) . . ?
C45 C46 N11 119.5(3) . . ?
C48 C47 C46 119.1(3) . . ?
C48 C47 H47 120.5 . . ?
C46 C47 H47 120.5 . . ?
C47 C48 C43 124.2(3) . . ?
C47 C48 N12 116.6(3) . . ?
C43 C48 N12 119.2(3) . . ?

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
O9 O9 N7 O10 0.00(16) 1 . . . ?
O9 O9 N7 C38 0.00(7) 1 . . . ?
O21 O21 N12 O20 0.0(5) 1 . . . ?
O21 O21 N12 C48 0.0(5) 1 . . . ?
C6 C1 C2 C3 -1.3(4) . . . . ?
C7 C1 C2 C3 178.9(2) . . . . ?
C1 C2 C3 C4 0.8(4) . . . . ?
C1 C2 C3 C15 178.4(2) . . . . ?
C2 C3 C4 C5 0.5(4) . . . . ?
C15 C3 C4 C5 -177.1(2) . . . . ?
C3 C4 C5 C6 -1.2(4) . . . . ?
C3 C4 C5 C23 178.1(2) . . . . ?
C4 C5 C6 C1 0.7(4) . . . . ?
C23 C5 C6 C1 -178.6(3) . . . . ?
C2 C1 C6 C5 0.5(4) . . . . ?
C7 C1 C6 C5 -179.6(2) . . . . ?
C6 C1 C7 C8 161.4(3) . . . . ?
C2 C1 C7 C8 -18.7(4) . . . . ?
C6 C1 C7 C12 -17.3(4) . . . . ?
C2 C1 C7 C12 162.6(3) . . . . ?
C12 C7 C8 C9 1.5(4) . . . . ?
C1 C7 C8 C9 -177.2(3) . . . . ?
C7 C8 C9 C10 -0.1(4) . . . . ?
C8 C9 C10 C11 -1.3(4) . . . . ?
C8 C9 C10 N1 175.4(2) . . . . ?
C13 N1 C10 C9 127.0(3) . . . . ?
C14 N1 C10 C9 -109.5(3) . . . . ?
C13 N1 C10 C11 -56.3(3) . . . . ?
C14 N1 C10 C11 67.3(3) . . . . ?
C9 C10 C11 C12 1.3(4) . . . . ?
N1 C10 C11 C12 -175.5(2) . . . . ?
C10 C11 C12 C7 0.2(4) . . . . ?
C8 C7 C12 C11 -1.6(4) . . . . ?
C1 C7 C12 C11 177.1(3) . . . . ?
C4 C3 C15 C20 37.2(4) . . . . ?
C2 C3 C15 C20 -140.4(3) . . . . ?
C4 C3 C15 C16 -143.2(3) . . . . ?
C2 C3 C15 C16 39.2(4) . . . . ?
C20 C15 C16 C17 0.7(4) . . . . ?
C3 C15 C16 C17 -178.9(3) . . . . ?
C15 C16 C17 C18 0.1(4) . . . . ?
C16 C17 C18 C19 -0.8(4) . . . . ?
C16 C17 C18 N2 179.0(2) . . . . ?
C21 N2 C18 C19 -67.4(3) . . . . ?
C22 N2 C18 C19 56.4(3) . . . . ?
C21 N2 C18 C17 112.9(3) . . . . ?
C22 N2 C18 C17 -123.3(3) . . . . ?
C17 C18 C19 C20 0.6(4) . . . . ?
N2 C18 C19 C20 -179.2(2) . . . . ?
C18 C19 C20 C15 0.3(4) . . . . ?
C16 C15 C20 C19 -0.9(4) . . . . ?
C3 C15 C20 C19 178.7(3) . . . . ?
C6 C5 C23 C24 153.4(3) . . . . ?
C4 C5 C23 C24 -25.9(4) . . . . ?
C6 C5 C23 C28 -26.4(4) . . . . ?
C4 C5 C23 C28 154.4(3) . . . . ?
C28 C23 C24 C25 -2.1(4) . . . . ?
C5 C23 C24 C25 178.2(3) . . . . ?
C23 C24 C25 C26 0.2(4) . . . . ?
C24 C25 C26 C27 2.2(4) . . . . ?
C24 C25 C26 N3 -178.4(2) . . . . ?
C29 N3 C26 C27 118.7(3) . . . . ?
C30 N3 C26 C27 -116.8(3) . . . . ?
C29 N3 C26 C25 -60.7(3) . . . . ?
C30 N3 C26 C25 63.8(3) . . . . ?
C25 C26 C27 C28 -2.5(4) . . . . ?
N3 C26 C27 C28 178.0(2) . . . . ?
C26 C27 C28 C23 0.6(4) . . . . ?
C24 C23 C28 C27 1.7(4) . . . . ?
C5 C23 C28 C27 -178.6(3) . . . . ?
O1 O1 C31 C36 0.0(2) 1 . . . ?
O1 O1 C31 C32 0.00(14) 1 . . . ?
O1 C31 C32 C33 -178.0(3) 1 . . . ?
O1 C31 C32 C33 -178.0(3) . . . . ?
C36 C31 C32 C33 0.4(4) . . . . ?
O1 C31 C32 N4 -1.2(4) 1 . . . ?
O1 C31 C32 N4 -1.2(4) . . . . ?
C36 C31 C32 N4 177.1(2) . . . . ?
O2 N4 C32 C33 -152.2(3) . . . . ?
O3 N4 C32 C33 27.6(4) . . . . ?
O2 N4 C32 C31 30.8(4) . . . . ?
O3 N4 C32 C31 -149.4(3) . . . . ?
C31 C32 C33 C34 1.9(4) . . . . ?
N4 C32 C33 C34 -175.0(2) . . . . ?
C32 C33 C34 C35 -2.2(4) . . . . ?
C32 C33 C34 N5 178.5(3) . . . . ?
O5 N5 C34 C35 13.2(4) . . . . ?
O4 N5 C34 C35 -167.0(3) . . . . ?
O5 N5 C34 C33 -167.5(3) . . . . ?
O4 N5 C34 C33 12.4(4) . . . . ?
C33 C34 C35 C36 0.1(4) . . . . ?
N5 C34 C35 C36 179.4(3) . . . . ?
C34 C35 C36 C31 2.4(4) . . . . ?
C34 C35 C36 N6 -176.5(2) . . . . ?
O1 C31 C36 C35 175.8(3) 1 . . . ?
O1 C31 C36 C35 175.8(3) . . . . ?
C32 C31 C36 C35 -2.5(4) . . . . ?
O1 C31 C36 N6 -5.3(4) 1 . . . ?
O1 C31 C36 N6 -5.3(4) . . . . ?
C32 C31 C36 N6 176.3(2) . . . . ?
O6 N6 C36 C35 -170.4(3) . . . . ?
O7 N6 C36 C35 9.6(4) . . . . ?
O6 N6 C36 C31 10.6(4) . . . . ?
O7 N6 C36 C31 -169.4(3) . . . . ?
O8 O8 C37 C38 0.00(7) 1 . . . ?
O8 O8 C37 C42 0.00(6) 1 . . . ?
O9 N7 C38 C39 -143.4(3) 1 . . . ?
O9 N7 C38 C39 -143.4(3) . . . . ?
O10 N7 C38 C39 35.6(4) . . . . ?
O9 N7 C38 C37 38.9(4) 1 . . . ?
O9 N7 C38 C37 38.9(4) . . . . ?
O10 N7 C38 C37 -142.1(3) . . . . ?
O8 C37 C38 C39 -173.8(3) 1 . . . ?
O8 C37 C38 C39 -173.8(3) . . . . ?
C42 C37 C38 C39 1.5(4) . . . . ?
O8 C37 C38 N7 3.7(4) 1 . . . ?
O8 C37 C38 N7 3.7(4) . . . . ?
C42 C37 C38 N7 179.0(2) . . . . ?
N7 C38 C39 C40 -178.7(3) . . . . ?
C37 C38 C39 C40 -1.2(5) . . . . ?
C38 C39 C40 C41 1.0(5) . . . . ?
C38 C39 C40 N8 -179.9(3) . . . . ?
O11 N8 C40 C41 -174.9(3) . . . . ?
O12 N8 C40 C41 5.4(5) . . . . ?
O11 N8 C40 C39 6.0(5) . . . . ?
O12 N8 C40 C39 -173.7(3) . . . . ?
C39 C40 C41 C42 -1.3(5) . . . . ?
N8 C40 C41 C42 179.6(3) . . . . ?
C40 C41 C42 C37 1.8(5) . . . . ?
C40 C41 C42 N9 -178.9(3) . . . . ?
O8 C37 C42 C41 173.5(3) 1 . . . ?
O8 C37 C42 C41 173.5(3) . . . . ?
C38 C37 C42 C41 -1.9(4) . . . . ?
O8 C37 C42 N9 -5.7(4) 1 . . . ?
O8 C37 C42 N9 -5.7(4) . . . . ?
C38 C37 C42 N9 178.9(2) . . . . ?
O14 N9 C42 C41 137.3(3) . . . . ?
O13 N9 C42 C41 -40.6(4) . . . . ?
O14 N9 C42 C37 -43.3(4) . . . . ?
O13 N9 C42 C37 138.7(3) . . . . ?
O15 O15 C43 C44 0.0(3) 1 . . . ?
O15 O15 C43 C48 0.0(2) 1 . . . ?
O15 C43 C44 C45 178.4(3) 1 . . . ?
O15 C43 C44 C45 178.4(3) . . . . ?
C48 C43 C44 C45 -2.1(4) . . . . ?
O15 C43 C44 N10 -2.0(5) 1 . . . ?
O15 C43 C44 N10 -2.0(5) . . . . ?
C48 C43 C44 N10 177.5(3) . . . . ?
O16 N10 C44 C45 159.6(3) . . . . ?
O17 N10 C44 C45 -18.0(4) . . . . ?
O16 N10 C44 C43 -20.0(4) . . . . ?
O17 N10 C44 C43 162.4(3) . . . . ?
C43 C44 C45 C46 1.2(5) . . . . ?
N10 C44 C45 C46 -178.4(3) . . . . ?
C44 C45 C46 C47 0.5(5) . . . . ?
C44 C45 C46 N11 179.3(3) . . . . ?
O19 N11 C46 C47 -9.1(5) . . . . ?
O18 N11 C46 C47 171.8(3) . . . . ?
O19 N11 C46 C45 172.0(3) . . . . ?
O18 N11 C46 C45 -7.0(5) . . . . ?
C45 C46 C47 C48 -1.0(5) . . . . ?
N11 C46 C47 C48 -179.9(3) . . . . ?
C46 C47 C48 C43 -0.1(5) . . . . ?
C46 C47 C48 N12 178.4(3) . . . . ?
O15 C43 C48 C47 -179.0(3) 1 . . . ?
O15 C43 C48 C47 -179.0(3) . . . . ?
C44 C43 C48 C47 1.5(4) . . . . ?
O15 C43 C48 N12 2.6(5) 1 . . . ?
O15 C43 C48 N12 2.6(5) . . . . ?
C44 C43 C48 N12 -176.9(3) . . . . ?
O21 N12 C48 C47 155.1(3) 1 . . . ?
O21 N12 C48 C47 155.1(3) . . . . ?
O20 N12 C48 C47 -25.3(4) . . . . ?
O21 N12 C48 C43 -26.4(4) 1 . . . ?
O21 N12 C48 C43 -26.4(4) . . . . ?
O20 N12 C48 C43 153.2(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
N3 H3W O1 1.002(2) 1.711(2) 2.697(3) 167.15(15) 1
N2 H2W O15 1.042(2) 1.713(2) 2.719(3) 160.97(14) 1
N2 H2W O21 1.042(2) 2.407(2) 3.027(3) 117.08(13) 1
N1 H1W O8 1.014(2) 1.719(2) 2.724(3) 170.60(14) 1
N1 H1W O9 1.014(2) 2.612(2) 3.149(3) 112.91(14) 1

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.057


_database_code_depnum_ccdc_archive 'CCDC 1010528'
