# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               Org.Biomol.Chem.
_journal_coden_cambridge         0177
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_name        'Choong Eui Song'
_publ_contact_author_email       oh.joongsuk@gmail.com
loop_
_publ_author_name
'Joong Suk Oh'
'Kyung Il Kim'
'Choong Eui Song'

data_2
_database_code_depnum_ccdc_archive 'CCDC 837463'
#TrackingRef 'BQn-SQ.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H48 N6 O4, 2(H2 O)'
_chemical_formula_sum            'C44 H52 N6 O6'
_chemical_formula_weight         760.92

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) '
_symmetry_space_group_name_Hall  'P 2yb'

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

_cell_length_a                   10.2837(2)
_cell_length_b                   16.8731(3)
_cell_length_c                   12.5611(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.1920(10)
_cell_angle_gamma                90.00
_cell_volume                     2058.44(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9923
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      27.27

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.40
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             812
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9552
_exptl_absorpt_correction_T_max  0.9677
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         '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            28370
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_sigmaI/netI    0.0481
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.10
_diffrn_reflns_theta_max         28.29
_reflns_number_total             9930
_reflns_number_gt                6598
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0591P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0025(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.2(7)
_refine_ls_number_reflns         9930
_refine_ls_number_parameters     522
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0432
_refine_ls_wR_factor_ref         0.1060
_refine_ls_wR_factor_gt          0.0963
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_restrained_S_all      0.935
_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 0.22006(15) -0.45042(8) 0.01591(12) 0.0711(4) Uani 1 1 d . . .
O2 O -0.28470(17) -0.48523(9) -0.0851(2) 0.1029(7) Uani 1 1 d . . .
O3 O 0.52495(15) -0.42073(8) 0.20424(12) 0.0684(4) Uani 1 1 d . . .
O4 O 0.97451(18) -0.47045(9) 0.26030(17) 0.0896(5) Uani 1 1 d . . .
O5 O 0.37001(16) -0.11314(9) -0.03643(15) 0.0663(4) Uani 1 1 d . . .
O6 O 0.53325(17) -0.58671(10) 0.20573(14) 0.0671(4) Uani 1 1 d . . .
N1 N 0.21256(13) -0.26286(8) -0.05545(11) 0.0431(3) Uani 1 1 d . . .
H1 H 0.2269 -0.2126 -0.0484 0.052 Uiso 1 1 calc R . .
N2 N -0.27653(17) -0.16332(9) -0.15388(13) 0.0549(4) Uani 1 1 d . . .
N3 N 0.23719(16) -0.33021(11) -0.25829(14) 0.0627(4) Uani 1 1 d . . .
N4 N 0.51138(14) -0.23663(8) 0.12010(11) 0.0432(3) Uani 1 1 d . . .
H4 H 0.4943 -0.1977 0.0733 0.052 Uiso 1 1 calc R . .
N5 N 0.99057(18) -0.15753(10) 0.14488(15) 0.0629(4) Uani 1 1 d . . .
N6 N 0.46402(16) -0.19196(10) 0.32049(14) 0.0611(4) Uani 1 1 d . . .
C1 C 0.30035(16) -0.31167(9) 0.01469(13) 0.0395(4) Uani 1 1 d . . .
C2 C 0.29968(19) -0.39488(10) 0.04576(15) 0.0504(4) Uani 1 1 d . . .
C3 C 0.43971(18) -0.38134(10) 0.13228(15) 0.0479(4) Uani 1 1 d . . .
C4 C 0.43043(16) -0.29941(10) 0.09488(13) 0.0398(4) Uani 1 1 d . . .
C5 C 0.09129(15) -0.29240(10) -0.14499(13) 0.0415(4) Uani 1 1 d . . .
H5 H 0.0799 -0.3488 -0.1314 0.050 Uiso 1 1 calc R . .
C6 C -0.03781(16) -0.24857(10) -0.14453(13) 0.0423(4) Uani 1 1 d . . .
C7 C -0.0473(2) -0.16837(12) -0.15854(17) 0.0551(5) Uani 1 1 d . . .
H7 H 0.0271 -0.1402 -0.1657 0.066 Uiso 1 1 calc R . .
C8 C -0.1672(2) -0.12805(12) -0.16223(17) 0.0609(5) Uani 1 1 d . . .
H8 H -0.1694 -0.0733 -0.1711 0.073 Uiso 1 1 calc R . .
C9 C -0.27124(17) -0.24338(10) -0.13754(14) 0.0460(4) Uani 1 1 d . . .
C10 C -0.38720(18) -0.28156(12) -0.12552(17) 0.0582(5) Uani 1 1 d . . .
H10 H -0.4646 -0.2517 -0.1290 0.070 Uiso 1 1 calc R . .
C11 C -0.3886(2) -0.36046(13) -0.1090(2) 0.0697(6) Uani 1 1 d . . .
H11 H -0.4668 -0.3847 -0.1023 0.084 Uiso 1 1 calc R . .
C12 C -0.2718(2) -0.40602(12) -0.1020(2) 0.0653(6) Uani 1 1 d . . .
C13 C -0.15688(19) -0.37190(11) -0.11247(17) 0.0535(5) Uani 1 1 d . . .
H13 H -0.0805 -0.4031 -0.1074 0.064 Uiso 1 1 calc R . .
C14 C -0.15242(16) -0.28894(10) -0.13109(13) 0.0408(4) Uani 1 1 d . . .
C15 C -0.1765(3) -0.53589(15) -0.0945(4) 0.1193(12) Uani 1 1 d . . .
H15A H -0.1974 -0.5900 -0.0826 0.179 Uiso 1 1 calc R . .
H15B H -0.0909 -0.5210 -0.0388 0.179 Uiso 1 1 calc R . .
H15C H -0.1690 -0.5305 -0.1683 0.179 Uiso 1 1 calc R . .
C16 C 0.11652(17) -0.28409(12) -0.25775(14) 0.0479(4) Uani 1 1 d . . .
H16 H 0.1375 -0.2282 -0.2658 0.058 Uiso 1 1 calc R . .
C17 C -0.0107(2) -0.30558(14) -0.36001(15) 0.0638(5) Uani 1 1 d . . .
H17A H -0.0720 -0.3401 -0.3368 0.077 Uiso 1 1 calc R . .
H17B H -0.0609 -0.2580 -0.3930 0.077 Uiso 1 1 calc R . .
C18 C 0.0427(3) -0.34808(17) -0.44594(19) 0.0823(7) Uani 1 1 d . . .
H18 H -0.0323 -0.3550 -0.5175 0.099 Uiso 1 1 calc R . .
C19 C 0.1594(3) -0.30068(17) -0.46442(17) 0.0790(7) Uani 1 1 d . . .
H19 H 0.1904 -0.3300 -0.5190 0.095 Uiso 1 1 calc R . .
C20 C 0.2808(2) -0.29999(18) -0.35125(17) 0.0767(7) Uani 1 1 d . . .
H20A H 0.3552 -0.3326 -0.3584 0.092 Uiso 1 1 calc R . .
H20B H 0.3150 -0.2463 -0.3343 0.092 Uiso 1 1 calc R . .
C21 C 0.2022(3) -0.41431(15) -0.2793(2) 0.0864(7) Uani 1 1 d . . .
H21A H 0.1643 -0.4338 -0.2230 0.104 Uiso 1 1 calc R . .
H21B H 0.2851 -0.4442 -0.2723 0.104 Uiso 1 1 calc R . .
C22 C 0.0975(3) -0.42743(19) -0.3970(3) 0.1038(9) Uani 1 1 d . . .
H22A H 0.1413 -0.4538 -0.4449 0.125 Uiso 1 1 calc R . .
H22B H 0.0227 -0.4606 -0.3920 0.125 Uiso 1 1 calc R . .
C23 C 0.1131(3) -0.2214(2) -0.5139(2) 0.0922(9) Uani 1 1 d . . .
H23 H 0.0364 -0.2224 -0.5788 0.111 Uiso 1 1 calc R . .
C24 C 0.1602(4) -0.1522(2) -0.4829(3) 0.1100(10) Uani 1 1 d . . .
H24A H 0.2369 -0.1457 -0.4187 0.132 Uiso 1 1 calc R . .
H24B H 0.1180 -0.1081 -0.5244 0.132 Uiso 1 1 calc R . .
C25 C 0.62838(15) -0.23024(10) 0.22367(13) 0.0396(4) Uani 1 1 d . . .
H25 H 0.6445 -0.2825 0.2597 0.048 Uiso 1 1 calc R . .
C26 C 0.75552(16) -0.20730(9) 0.19549(13) 0.0397(4) Uani 1 1 d . . .
C27 C 0.7691(2) -0.13215(11) 0.16071(18) 0.0579(5) Uani 1 1 d . . .
H27 H 0.6996 -0.0952 0.1534 0.069 Uiso 1 1 calc R . .
C28 C 0.8870(2) -0.11036(13) 0.1359(2) 0.0694(6) Uani 1 1 d . . .
H28 H 0.8921 -0.0588 0.1114 0.083 Uiso 1 1 calc R . .
C29 C 0.97911(18) -0.23294(11) 0.17621(14) 0.0478(4) Uani 1 1 d . . .
C30 C 1.0905(2) -0.28479(13) 0.18635(17) 0.0617(5) Uani 1 1 d . . .
H30 H 1.1684 -0.2657 0.1727 0.074 Uiso 1 1 calc R . .
C31 C 1.0862(2) -0.36116(14) 0.2153(2) 0.0717(6) Uani 1 1 d . . .
H31 H 1.1613 -0.3940 0.2229 0.086 Uiso 1 1 calc R . .
C32 C 0.9680(2) -0.39171(12) 0.23430(17) 0.0599(5) Uani 1 1 d . . .
C33 C 0.85813(19) -0.34395(10) 0.22764(15) 0.0480(4) Uani 1 1 d . . .
H33 H 0.7812 -0.3647 0.2412 0.058 Uiso 1 1 calc R . .
C34 C 0.86207(16) -0.26231(9) 0.19986(13) 0.0394(4) Uani 1 1 d . . .
C35 C 0.8622(3) -0.50423(13) 0.2838(3) 0.0908(8) Uani 1 1 d . . .
H35A H 0.8797 -0.5595 0.3006 0.136 Uiso 1 1 calc R . .
H35B H 0.7806 -0.4985 0.2193 0.136 Uiso 1 1 calc R . .
H35C H 0.8495 -0.4779 0.3473 0.136 Uiso 1 1 calc R . .
C36 C 0.59503(18) -0.17214(11) 0.30442(14) 0.0487(4) Uani 1 1 d . . .
H36 H 0.5839 -0.1198 0.2688 0.058 Uiso 1 1 calc R . .
C37 C 0.7120(2) -0.16536(16) 0.41781(17) 0.0717(6) Uani 1 1 d . . .
H37A H 0.7766 -0.2087 0.4261 0.086 Uiso 1 1 calc R . .
H37B H 0.7612 -0.1159 0.4212 0.086 Uiso 1 1 calc R . .
C38 C 0.6487(3) -0.16836(17) 0.51187(19) 0.0819(7) Uani 1 1 d . . .
H38 H 0.7200 -0.1596 0.5850 0.098 Uiso 1 1 calc R . .
C39 C 0.5365(3) -0.10668(15) 0.4925(2) 0.0935(9) Uani 1 1 d . . .
H39 H 0.4938 -0.1137 0.5511 0.112 Uiso 1 1 calc R . .
C40 C 0.4261(3) -0.12391(17) 0.3781(2) 0.0935(8) Uani 1 1 d . . .
H40A H 0.3392 -0.1350 0.3898 0.112 Uiso 1 1 calc R . .
H40B H 0.4137 -0.0774 0.3305 0.112 Uiso 1 1 calc R . .
C41 C 0.4772(2) -0.26068(14) 0.3928(2) 0.0738(6) Uani 1 1 d . . .
H41A H 0.5023 -0.3063 0.3568 0.089 Uiso 1 1 calc R . .
H41B H 0.3888 -0.2716 0.4018 0.089 Uiso 1 1 calc R . .
C42 C 0.5853(3) -0.24909(17) 0.5093(2) 0.0921(8) Uani 1 1 d . . .
H42A H 0.5424 -0.2529 0.5673 0.111 Uiso 1 1 calc R . .
H42B H 0.6555 -0.2898 0.5231 0.111 Uiso 1 1 calc R . .
C43 C 0.5882(6) -0.0238(3) 0.5005(5) 0.188(2) Uani 1 1 d . . .
H43A H 0.6419 -0.0163 0.4544 0.226 Uiso 1 1 calc R . .
C44 C 0.5809(8) 0.0319(3) 0.5458(8) 0.271(5) Uani 1 1 d . . .
H44A H 0.5301 0.0328 0.5949 0.326 Uiso 1 1 calc R . .
H44B H 0.6257 0.0774 0.5346 0.326 Uiso 1 1 calc R . .
H51 H 0.376(2) -0.0672(16) -0.010(2) 0.074(7) Uiso 1 1 d . . .
H52 H 0.414(4) -0.102(2) -0.095(3) 0.137(11) Uiso 1 1 d . . .
H61 H 0.523(2) -0.5326(15) 0.2101(17) 0.067(6) Uiso 1 1 d . . .
H62 H 0.452(3) -0.6066(17) 0.184(2) 0.104(10) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0667(9) 0.0546(8) 0.0797(9) -0.0051(7) 0.0073(7) -0.0227(7)
O2 0.0876(12) 0.0542(9) 0.208(2) 0.0243(10) 0.1041(14) 0.0127(8)
O3 0.0621(8) 0.0444(7) 0.0794(9) 0.0087(7) -0.0029(7) 0.0000(6)
O4 0.0936(12) 0.0497(9) 0.1430(15) 0.0121(9) 0.0623(11) 0.0183(8)
O5 0.0760(10) 0.0468(9) 0.0836(10) 0.0112(8) 0.0366(8) 0.0069(7)
O6 0.0583(9) 0.0491(9) 0.1005(11) -0.0089(8) 0.0349(8) -0.0082(7)
N1 0.0357(7) 0.0424(8) 0.0470(8) -0.0048(6) 0.0079(6) -0.0045(6)
N2 0.0521(10) 0.0527(10) 0.0616(10) -0.0027(7) 0.0208(8) 0.0090(7)
N3 0.0466(9) 0.0851(12) 0.0603(10) -0.0025(9) 0.0229(8) 0.0113(8)
N4 0.0385(7) 0.0407(7) 0.0440(7) 0.0054(6) 0.0048(6) -0.0055(6)
N5 0.0541(10) 0.0647(11) 0.0772(11) 0.0194(8) 0.0313(9) 0.0014(8)
N6 0.0422(9) 0.0802(12) 0.0651(10) -0.0047(9) 0.0233(8) -0.0001(8)
C1 0.0331(8) 0.0452(10) 0.0403(8) -0.0051(7) 0.0121(7) -0.0018(7)
C2 0.0499(11) 0.0448(10) 0.0543(10) -0.0071(8) 0.0143(9) -0.0096(9)
C3 0.0440(10) 0.0408(9) 0.0555(11) -0.0030(8) 0.0116(9) -0.0012(8)
C4 0.0331(8) 0.0434(9) 0.0418(8) -0.0043(7) 0.0111(7) -0.0030(7)
C5 0.0298(8) 0.0479(9) 0.0440(8) -0.0064(7) 0.0083(7) -0.0044(7)
C6 0.0385(9) 0.0494(10) 0.0361(8) -0.0059(7) 0.0084(7) -0.0007(8)
C7 0.0496(11) 0.0526(11) 0.0665(12) -0.0042(9) 0.0235(9) -0.0048(9)
C8 0.0645(13) 0.0473(11) 0.0744(14) 0.0006(9) 0.0275(11) 0.0053(10)
C9 0.0403(10) 0.0483(11) 0.0484(10) -0.0055(8) 0.0132(8) 0.0055(8)
C10 0.0396(10) 0.0611(13) 0.0775(13) -0.0020(10) 0.0239(10) 0.0122(9)
C11 0.0471(11) 0.0620(13) 0.1153(19) 0.0014(12) 0.0476(12) 0.0010(9)
C12 0.0593(12) 0.0493(12) 0.1023(16) 0.0085(10) 0.0470(12) 0.0057(9)
C13 0.0410(10) 0.0540(11) 0.0742(12) 0.0070(9) 0.0308(9) 0.0104(8)
C14 0.0341(8) 0.0472(10) 0.0391(8) -0.0038(7) 0.0094(7) 0.0041(7)
C15 0.111(2) 0.0583(14) 0.238(4) 0.0362(18) 0.124(3) 0.0253(13)
C16 0.0342(9) 0.0663(11) 0.0432(9) -0.0032(8) 0.0126(7) 0.0020(8)
C17 0.0463(11) 0.0978(16) 0.0440(10) -0.0117(10) 0.0102(9) -0.0030(10)
C18 0.0728(15) 0.119(2) 0.0533(13) -0.0307(13) 0.0185(11) -0.0172(15)
C19 0.0727(15) 0.119(2) 0.0497(11) -0.0140(13) 0.0261(11) 0.0029(14)
C20 0.0501(12) 0.124(2) 0.0638(13) -0.0015(13) 0.0290(10) 0.0116(12)
C21 0.0979(19) 0.0803(17) 0.0916(18) -0.0115(14) 0.0454(15) 0.0204(14)
C22 0.124(2) 0.097(2) 0.102(2) -0.0324(17) 0.0514(19) -0.0090(19)
C23 0.0711(17) 0.152(3) 0.0519(14) 0.0045(17) 0.0182(12) 0.0024(18)
C24 0.107(2) 0.138(3) 0.096(2) 0.014(2) 0.0465(19) 0.018(2)
C25 0.0286(8) 0.0423(9) 0.0430(9) 0.0054(7) 0.0052(7) -0.0022(7)
C26 0.0316(8) 0.0458(9) 0.0387(8) 0.0030(7) 0.0076(7) -0.0042(7)
C27 0.0459(11) 0.0517(11) 0.0773(13) 0.0169(10) 0.0220(10) 0.0077(8)
C28 0.0600(13) 0.0563(12) 0.0974(16) 0.0272(11) 0.0332(12) -0.0013(10)
C29 0.0463(10) 0.0575(11) 0.0423(9) 0.0029(8) 0.0183(8) -0.0007(8)
C30 0.0526(11) 0.0740(14) 0.0712(13) 0.0058(11) 0.0375(10) 0.0072(10)
C31 0.0660(13) 0.0724(15) 0.0894(16) 0.0078(12) 0.0428(12) 0.0190(11)
C32 0.0643(13) 0.0504(11) 0.0700(13) 0.0010(9) 0.0291(11) 0.0091(10)
C33 0.0487(10) 0.0463(10) 0.0520(10) -0.0030(8) 0.0205(8) -0.0022(8)
C34 0.0378(8) 0.0451(9) 0.0335(8) -0.0026(7) 0.0095(7) -0.0013(7)
C35 0.113(2) 0.0445(12) 0.131(2) 0.0049(13) 0.0625(18) 0.0000(13)
C36 0.0403(9) 0.0532(10) 0.0507(10) -0.0020(8) 0.0124(8) -0.0044(8)
C37 0.0572(13) 0.0992(17) 0.0557(12) -0.0192(11) 0.0145(10) -0.0206(11)
C38 0.0864(17) 0.1034(19) 0.0567(13) -0.0215(12) 0.0244(12) -0.0216(15)
C39 0.133(2) 0.0808(18) 0.0938(19) -0.0295(14) 0.0746(19) -0.0277(17)
C40 0.0962(18) 0.0987(19) 0.106(2) 0.0078(16) 0.0609(17) 0.0278(16)
C41 0.0673(13) 0.0840(16) 0.0827(15) -0.0100(12) 0.0416(12) -0.0208(11)
C42 0.1021(19) 0.101(2) 0.0758(16) 0.0126(14) 0.0328(15) -0.0046(16)
C43 0.265(6) 0.099(3) 0.279(6) -0.070(3) 0.196(5) -0.046(3)
C44 0.358(10) 0.117(4) 0.468(13) -0.105(5) 0.311(10) -0.081(5)

_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 C2 1.220(2) . ?
O2 C12 1.366(2) . ?
O2 C15 1.438(3) . ?
O3 C3 1.227(2) . ?
O4 C32 1.365(2) . ?
O4 C35 1.403(3) . ?
O5 H51 0.84(3) . ?
O5 H52 1.00(4) . ?
O6 H61 0.92(3) . ?
O6 H62 0.86(3) . ?
N1 C1 1.322(2) . ?
N1 C5 1.465(2) . ?
N1 H1 0.8600 . ?
N2 C8 1.306(2) . ?
N2 C9 1.365(2) . ?
N3 C21 1.466(3) . ?
N3 C16 1.467(2) . ?
N3 C20 1.473(3) . ?
N4 C4 1.320(2) . ?
N4 C25 1.457(2) . ?
N4 H4 0.8600 . ?
N5 C28 1.304(3) . ?
N5 C29 1.349(2) . ?
N6 C41 1.451(3) . ?
N6 C36 1.465(2) . ?
N6 C40 1.477(3) . ?
C1 C4 1.400(2) . ?
C1 C2 1.458(2) . ?
C2 C3 1.509(3) . ?
C3 C4 1.453(2) . ?
C5 C6 1.521(2) . ?
C5 C16 1.528(2) . ?
C5 H5 0.9800 . ?
C6 C7 1.364(3) . ?
C6 C14 1.419(2) . ?
C7 C8 1.396(3) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C10 1.406(3) . ?
C9 C14 1.423(2) . ?
C10 C11 1.348(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.404(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.360(3) . ?
C13 C14 1.422(3) . ?
C13 H13 0.9300 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.545(3) . ?
C16 H16 0.9800 . ?
C17 C18 1.540(3) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C22 1.504(4) . ?
C18 C19 1.522(4) . ?
C18 H18 0.9800 . ?
C19 C23 1.486(4) . ?
C19 C20 1.553(3) . ?
C19 H19 0.9800 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.532(4) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.276(4) . ?
C23 H23 0.9300 . ?
C24 H24A 0.9300 . ?
C24 H24B 0.9300 . ?
C25 C26 1.513(2) . ?
C25 C36 1.529(2) . ?
C25 H25 0.9800 . ?
C26 C27 1.363(2) . ?
C26 C34 1.423(2) . ?
C27 C28 1.397(3) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 C30 1.414(3) . ?
C29 C34 1.420(2) . ?
C30 C31 1.344(3) . ?
C30 H30 0.9300 . ?
C31 C32 1.411(3) . ?
C31 H31 0.9300 . ?
C32 C33 1.368(3) . ?
C33 C34 1.425(2) . ?
C33 H33 0.9300 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 C37 1.537(3) . ?
C36 H36 0.9800 . ?
C37 C38 1.526(3) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 C42 1.506(4) . ?
C38 C39 1.513(4) . ?
C38 H38 0.9800 . ?
C39 C43 1.488(5) . ?
C39 C40 1.538(4) . ?
C39 H39 0.9800 . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 C42 1.531(4) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.114(5) . ?
C43 H43A 0.9300 . ?
C44 H44A 0.9300 . ?
C44 H44B 0.9300 . ?

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
C12 O2 C15 116.82(16) . . ?
C32 O4 C35 117.82(17) . . ?
H51 O5 H52 97(3) . . ?
H61 O6 H62 107(2) . . ?
C1 N1 C5 121.49(14) . . ?
C1 N1 H1 119.3 . . ?
C5 N1 H1 119.3 . . ?
C8 N2 C9 118.05(16) . . ?
C21 N3 C16 110.88(17) . . ?
C21 N3 C20 108.23(18) . . ?
C16 N3 C20 107.37(16) . . ?
C4 N4 C25 122.97(13) . . ?
C4 N4 H4 118.5 . . ?
C25 N4 H4 118.5 . . ?
C28 N5 C29 116.99(16) . . ?
C41 N6 C36 111.56(15) . . ?
C41 N6 C40 107.44(17) . . ?
C36 N6 C40 107.06(17) . . ?
N1 C1 C4 132.00(15) . . ?
N1 C1 C2 135.75(15) . . ?
C4 C1 C2 92.13(13) . . ?
O1 C2 C1 136.02(17) . . ?
O1 C2 C3 136.29(17) . . ?
C1 C2 C3 87.69(13) . . ?
O3 C3 C4 135.11(16) . . ?
O3 C3 C2 136.87(16) . . ?
C4 C3 C2 88.02(13) . . ?
N4 C4 C1 132.01(15) . . ?
N4 C4 C3 135.79(15) . . ?
C1 C4 C3 92.16(13) . . ?
N1 C5 C6 110.82(12) . . ?
N1 C5 C16 108.62(13) . . ?
C6 C5 C16 111.91(13) . . ?
N1 C5 H5 108.5 . . ?
C6 C5 H5 108.5 . . ?
C16 C5 H5 108.5 . . ?
C7 C6 C14 117.70(16) . . ?
C7 C6 C5 120.48(15) . . ?
C14 C6 C5 121.82(14) . . ?
C6 C7 C8 120.84(18) . . ?
C6 C7 H7 119.6 . . ?
C8 C7 H7 119.6 . . ?
N2 C8 C7 123.34(19) . . ?
N2 C8 H8 118.3 . . ?
C7 C8 H8 118.3 . . ?
N2 C9 C10 118.43(16) . . ?
N2 C9 C14 122.29(16) . . ?
C10 C9 C14 119.27(16) . . ?
C11 C10 C9 121.41(17) . . ?
C11 C10 H10 119.3 . . ?
C9 C10 H10 119.3 . . ?
C10 C11 C12 119.87(17) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C13 C12 O2 124.13(16) . . ?
C13 C12 C11 121.00(17) . . ?
O2 C12 C11 114.87(16) . . ?
C12 C13 C14 120.58(16) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
C6 C14 C13 124.41(15) . . ?
C6 C14 C9 117.72(15) . . ?
C13 C14 C9 117.87(15) . . ?
O2 C15 H15A 109.5 . . ?
O2 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O2 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N3 C16 C5 110.94(14) . . ?
N3 C16 C17 110.99(15) . . ?
C5 C16 C17 113.17(14) . . ?
N3 C16 H16 107.1 . . ?
C5 C16 H16 107.1 . . ?
C17 C16 H16 107.1 . . ?
C18 C17 C16 106.99(16) . . ?
C18 C17 H17A 110.3 . . ?
C16 C17 H17A 110.3 . . ?
C18 C17 H17B 110.3 . . ?
C16 C17 H17B 110.3 . . ?
H17A C17 H17B 108.6 . . ?
C22 C18 C19 108.8(2) . . ?
C22 C18 C17 107.5(2) . . ?
C19 C18 C17 110.1(2) . . ?
C22 C18 H18 110.2 . . ?
C19 C18 H18 110.2 . . ?
C17 C18 H18 110.2 . . ?
C23 C19 C18 112.1(2) . . ?
C23 C19 C20 115.2(2) . . ?
C18 C19 C20 107.53(19) . . ?
C23 C19 H19 107.2 . . ?
C18 C19 H19 107.2 . . ?
C20 C19 H19 107.2 . . ?
N3 C20 C19 111.13(18) . . ?
N3 C20 H20A 109.4 . . ?
C19 C20 H20A 109.4 . . ?
N3 C20 H20B 109.4 . . ?
C19 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
N3 C21 C22 111.5(2) . . ?
N3 C21 H21A 109.3 . . ?
C22 C21 H21A 109.3 . . ?
N3 C21 H21B 109.3 . . ?
C22 C21 H21B 109.3 . . ?
H21A C21 H21B 108.0 . . ?
C18 C22 C21 108.4(2) . . ?
C18 C22 H22A 110.0 . . ?
C21 C22 H22A 110.0 . . ?
C18 C22 H22B 110.0 . . ?
C21 C22 H22B 110.0 . . ?
H22A C22 H22B 108.4 . . ?
C24 C23 C19 131.3(3) . . ?
C24 C23 H23 114.4 . . ?
C19 C23 H23 114.4 . . ?
C23 C24 H24A 120.0 . . ?
C23 C24 H24B 120.0 . . ?
H24A C24 H24B 120.0 . . ?
N4 C25 C26 109.48(12) . . ?
N4 C25 C36 109.90(13) . . ?
C26 C25 C36 113.01(13) . . ?
N4 C25 H25 108.1 . . ?
C26 C25 H25 108.1 . . ?
C36 C25 H25 108.1 . . ?
C27 C26 C34 117.39(15) . . ?
C27 C26 C25 120.04(15) . . ?
C34 C26 C25 122.53(14) . . ?
C26 C27 C28 120.29(17) . . ?
C26 C27 H27 119.9 . . ?
C28 C27 H27 119.9 . . ?
N5 C28 C27 124.34(18) . . ?
N5 C28 H28 117.8 . . ?
C27 C28 H28 117.8 . . ?
N5 C29 C30 117.66(16) . . ?
N5 C29 C34 123.47(16) . . ?
C30 C29 C34 118.86(17) . . ?
C31 C30 C29 121.32(19) . . ?
C31 C30 H30 119.3 . . ?
C29 C30 H30 119.3 . . ?
C30 C31 C32 120.21(19) . . ?
C30 C31 H31 119.9 . . ?
C32 C31 H31 119.9 . . ?
O4 C32 C33 124.26(18) . . ?
O4 C32 C31 114.76(18) . . ?
C33 C32 C31 120.97(19) . . ?
C32 C33 C34 119.68(17) . . ?
C32 C33 H33 120.2 . . ?
C34 C33 H33 120.2 . . ?
C29 C34 C26 117.33(15) . . ?
C29 C34 C33 118.86(15) . . ?
C26 C34 C33 123.81(15) . . ?
O4 C35 H35A 109.5 . . ?
O4 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
O4 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N6 C36 C25 111.23(14) . . ?
N6 C36 C37 111.37(15) . . ?
C25 C36 C37 112.62(15) . . ?
N6 C36 H36 107.1 . . ?
C25 C36 H36 107.1 . . ?
C37 C36 H36 107.1 . . ?
C38 C37 C36 108.17(17) . . ?
C38 C37 H37A 110.1 . . ?
C36 C37 H37A 110.1 . . ?
C38 C37 H37B 110.1 . . ?
C36 C37 H37B 110.1 . . ?
H37A C37 H37B 108.4 . . ?
C42 C38 C39 108.5(2) . . ?
C42 C38 C37 107.8(2) . . ?
C39 C38 C37 110.5(2) . . ?
C42 C38 H38 110.0 . . ?
C39 C38 H38 110.0 . . ?
C37 C38 H38 110.0 . . ?
C43 C39 C38 113.5(3) . . ?
C43 C39 C40 112.2(3) . . ?
C38 C39 C40 108.06(18) . . ?
C43 C39 H39 107.6 . . ?
C38 C39 H39 107.6 . . ?
C40 C39 H39 107.6 . . ?
N6 C40 C39 111.8(2) . . ?
N6 C40 H40A 109.3 . . ?
C39 C40 H40A 109.3 . . ?
N6 C40 H40B 109.3 . . ?
C39 C40 H40B 109.3 . . ?
H40A C40 H40B 107.9 . . ?
N6 C41 C42 112.67(18) . . ?
N6 C41 H41A 109.1 . . ?
C42 C41 H41A 109.1 . . ?
N6 C41 H41B 109.1 . . ?
C42 C41 H41B 109.1 . . ?
H41A C41 H41B 107.8 . . ?
C38 C42 C41 108.0(2) . . ?
C38 C42 H42A 110.1 . . ?
C41 C42 H42A 110.1 . . ?
C38 C42 H42B 110.1 . . ?
C41 C42 H42B 110.1 . . ?
H42A C42 H42B 108.4 . . ?
C44 C43 C39 138.1(5) . . ?
C44 C43 H43A 110.9 . . ?
C39 C43 H43A 110.9 . . ?
C43 C44 H44A 120.0 . . ?
C43 C44 H44B 120.0 . . ?
H44A C44 H44B 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        28.29
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.152
_refine_diff_density_min         -0.153
_refine_diff_density_rms         0.029