 
data_lb016 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C40 H38 N2 O6' 
_chemical_formula_weight          642.72 
  
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)/n 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
  
_cell_length_a                    22.9943(4) 
_cell_length_b                    6.72840(10) 
_cell_length_c                    23.2627(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  112.8790(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      3315.94(9) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     296(2) 
_cell_measurement_reflns_used     3888 
_cell_measurement_theta_min       2.66 
_cell_measurement_theta_max       19.74 
  
_exptl_crystal_description        needle 
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.23 
_exptl_crystal_size_mid           0.09 
_exptl_crystal_size_min           0.07 
_exptl_crystal_density_meas       n/a 
_exptl_crystal_density_diffrn     1.287 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1360 
_exptl_absorpt_coefficient_mu     0.087 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.9804 
_exptl_absorpt_correction_T_max   0.9940 
_exptl_absorpt_process_details    'SADABS, Bruker (2003)' 
  
_exptl_special_details 
; 
 Data collection is performed with three batch runs at phi = 0.00 deg 
 (650 frames), at phi = 120.00 deg (650 frames), and at phi = 240.00 deg 
 (650 frames). 
 Frame width = 0.30 deg in omega. 
 Data is merged, corrected for decay (if any), and treated with multi-scan 
 absorption corrections (if required). All symmetry-equivalent reflections 
 are merged for centrosymmetric data. 
 Friedel pairs are not merged for noncentrosymmetric data. 
; 
  
_diffrn_ambient_temperature       296(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   'Bruker APEX-II CCD' 
_diffrn_measurement_method        'φ and ω scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_reflns_number             28901 
_diffrn_reflns_av_R_equivalents   0.0679 
_diffrn_reflns_av_sigmaI/netI     0.0344 
_diffrn_reflns_limit_h_min        -24 
_diffrn_reflns_limit_h_max        24 
_diffrn_reflns_limit_k_min        -7 
_diffrn_reflns_limit_k_max        7 
_diffrn_reflns_limit_l_min        -24 
_diffrn_reflns_limit_l_max        22 
_diffrn_reflns_theta_min          1.90 
_diffrn_reflns_theta_max          22.01 
_reflns_number_total              4012 
_reflns_number_gt                 2863 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'APEX II, Bruker (2009)' 
_computing_cell_refinement        'APEX II, Bruker (2009)' 
_computing_data_reduction         'XPREP, Bruker (2009)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     'SHELXTL, Bruker (2004)' 
_computing_publication_material   'SHELXTL, Bruker (2004)' 
  
_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)+(0.0539P)²+0.5324P] 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      SHELXL 
_refine_ls_extinction_coef        0.0054(5) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          4012 
_refine_ls_number_parameters      434 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0701 
_refine_ls_R_factor_gt            0.0423 
_refine_ls_wR_factor_ref          0.1064 
_refine_ls_wR_factor_gt           0.0946 
_refine_ls_goodness_of_fit_ref    1.014 
_refine_ls_restrained_S_all       1.014 
_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 
N1 N 0.84234(9) 0.3307(3) 0.76929(10) 0.0503(6) Uani 1 1 d . . . 
O1 O 0.90575(9) 0.0647(3) 0.77144(9) 0.0747(6) Uani 1 1 d . . . 
O2 O 0.77725(10) 0.5504(4) 0.79103(9) 0.0822(7) Uani 1 1 d . . . 
O3 O 0.92919(10) 0.0730(3) 1.01193(10) 0.0904(7) Uani 1 1 d . . . 
C1 C 0.87345(12) 0.1538(4) 0.79327(13) 0.0554(7) Uani 1 1 d . . . 
C2 C 0.86299(12) 0.1042(4) 0.85170(12) 0.0531(7) Uani 1 1 d . . . 
H2A H 0.8503 -0.0353 0.8501 0.064 Uiso 1 1 calc R . . 
C3 C 0.92522(12) 0.1360(4) 0.90946(13) 0.0579(7) Uani 1 1 d . . . 
H3A H 0.9501 0.0135 0.9170 0.069 Uiso 1 1 calc R . . 
C4 C 0.96655(12) 0.3094(4) 0.90486(13) 0.0646(8) Uani 1 1 d . . . 
H4A H 1.0089 0.2929 0.9363 0.077 Uiso 1 1 calc R . . 
H4B H 0.9692 0.3065 0.8643 0.077 Uiso 1 1 calc R . . 
C5 C 0.94138(13) 0.5054(4) 0.91373(13) 0.0627(8) Uani 1 1 d . . . 
H5A H 0.9565 0.6186 0.9012 0.075 Uiso 1 1 calc R . . 
C6 C 0.89868(14) 0.5284(4) 0.93837(12) 0.0600(8) Uani 1 1 d . . . 
H6A H 0.8861 0.6568 0.9430 0.072 Uiso 1 1 calc R . . 
C7 C 0.86951(12) 0.3585(4) 0.95918(11) 0.0519(7) Uani 1 1 d . . . 
C8 C 0.80476(12) 0.3082(4) 0.90831(12) 0.0602(8) Uani 1 1 d . . . 
H8A H 0.7849 0.2063 0.9240 0.072 Uiso 1 1 calc R . . 
H8B H 0.7783 0.4256 0.8998 0.072 Uiso 1 1 calc R . . 
C9 C 0.80777(11) 0.2365(4) 0.84803(12) 0.0538(7) Uani 1 1 d . . . 
H9A H 0.7697 0.1565 0.8275 0.065 Uiso 1 1 calc R . . 
C10 C 0.80632(13) 0.3957(5) 0.80178(12) 0.0579(7) Uani 1 1 d . . . 
C11 C 0.84521(11) 0.4294(4) 0.71569(12) 0.0498(7) Uani 1 1 d . . . 
C12 C 0.82003(13) 0.3374(5) 0.65846(14) 0.0653(8) Uani 1 1 d . . . 
H12A H 0.8016 0.2123 0.6545 0.078 Uiso 1 1 calc R . . 
C13 C 0.82249(14) 0.4336(6) 0.60692(15) 0.0760(9) Uani 1 1 d . . . 
H13A H 0.8061 0.3723 0.5680 0.091 Uiso 1 1 calc R . . 
C14 C 0.84893(14) 0.6183(6) 0.61282(15) 0.0730(9) Uani 1 1 d . . . 
H14A H 0.8506 0.6825 0.5781 0.088 Uiso 1 1 calc R . . 
C15 C 0.87303(14) 0.7086(5) 0.67009(17) 0.0742(9) Uani 1 1 d . . . 
H15A H 0.8908 0.8346 0.6742 0.089 Uiso 1 1 calc R . . 
C16 C 0.87100(13) 0.6135(5) 0.72147(14) 0.0638(8) Uani 1 1 d . . . 
H16A H 0.8873 0.6753 0.7603 0.077 Uiso 1 1 calc R . . 
C17 C 0.91007(12) 0.1773(4) 0.96568(14) 0.0587(8) Uani 1 1 d . . . 
C18 C 0.86271(15) 0.4044(5) 1.02118(13) 0.0759(9) Uani 1 1 d . . . 
H18A H 0.8503 0.2836 1.0361 0.091 Uiso 1 1 calc R . . 
H18B H 0.9036 0.4436 1.0518 0.091 Uiso 1 1 calc R . . 
C19 C 0.8151(2) 0.5669(7) 1.01723(18) 0.1116(15) Uani 1 1 d . . . 
H19A H 0.7728 0.5312 0.9979 0.134 Uiso 1 1 calc R . . 
C20 C 0.8249(2) 0.7329(9) 1.03555(19) 0.1386(18) Uani 1 1 d . . . 
H20A H 0.8662 0.7779 1.0553 0.166 Uiso 1 1 calc R . . 
H20B H 0.7914 0.8181 1.0302 0.166 Uiso 1 1 calc R . . 
N2 N 0.74238(10) 1.0089(3) 0.15070(9) 0.0493(6) Uani 1 1 d . . . 
O4 O 0.71679(9) 1.1198(3) 0.05010(9) 0.0719(6) Uani 1 1 d . . . 
O5 O 0.73633(8) 0.9045(3) 0.24274(8) 0.0582(5) Uani 1 1 d . . . 
O6 O 0.49577(9) 0.7786(3) 0.02724(9) 0.0790(6) Uani 1 1 d . . . 
C21 C 0.70046(13) 1.0670(4) 0.09114(13) 0.0542(7) Uani 1 1 d . . . 
C22 C 0.63443(12) 1.0417(4) 0.08803(12) 0.0520(7) Uani 1 1 d . . . 
H22A H 0.6100 1.1613 0.0695 0.062 Uiso 1 1 calc R . . 
C23 C 0.60272(12) 0.8591(4) 0.04645(11) 0.0540(7) Uani 1 1 d . . . 
H23A H 0.5848 0.9017 0.0027 0.065 Uiso 1 1 calc R . . 
C24 C 0.64656(13) 0.6804(4) 0.05250(13) 0.0614(8) Uani 1 1 d . . . 
H24A H 0.6265 0.5904 0.0178 0.074 Uiso 1 1 calc R . . 
H24B H 0.6855 0.7270 0.0501 0.074 Uiso 1 1 calc R . . 
C25 C 0.66158(12) 0.5709(4) 0.11211(13) 0.0538(7) Uani 1 1 d . . . 
H25A H 0.6964 0.4866 0.1257 0.065 Uiso 1 1 calc R . . 
C26 C 0.62808(12) 0.5876(4) 0.14636(12) 0.0513(7) Uani 1 1 d . . . 
H26A H 0.6400 0.5115 0.1825 0.062 Uiso 1 1 calc R . . 
C27 C 0.57189(11) 0.7210(4) 0.13120(12) 0.0492(7) Uani 1 1 d . . . 
C28 C 0.59455(12) 0.9100(4) 0.17145(13) 0.0563(7) Uani 1 1 d . . . 
H28A H 0.5583 0.9940 0.1654 0.068 Uiso 1 1 calc R . . 
H28B H 0.6128 0.8718 0.2151 0.068 Uiso 1 1 calc R . . 
C29 C 0.64305(12) 1.0294(4) 0.15645(12) 0.0496(7) Uani 1 1 d . . . 
H29A H 0.6401 1.1661 0.1696 0.059 Uiso 1 1 calc R . . 
C30 C 0.71097(12) 0.9676(4) 0.19041(13) 0.0485(7) Uani 1 1 d . . . 
C31 C 0.80887(13) 0.9849(5) 0.16737(12) 0.0547(7) Uani 1 1 d . . . 
C32 C 0.83672(14) 0.8050(5) 0.18940(12) 0.0681(8) Uani 1 1 d . . . 
H32A H 0.8130 0.7007 0.1951 0.082 Uiso 1 1 calc R . . 
C33 C 0.90014(17) 0.7800(6) 0.20293(14) 0.0880(11) Uani 1 1 d . . . 
H33A H 0.9195 0.6591 0.2184 0.106 Uiso 1 1 calc R . . 
C34 C 0.93472(17) 0.9333(8) 0.19356(16) 0.0982(13) Uani 1 1 d . . . 
H34A H 0.9774 0.9153 0.2020 0.118 Uiso 1 1 calc R . . 
C35 C 0.90674(17) 1.1128(7) 0.17186(15) 0.0939(12) Uani 1 1 d . . . 
H35A H 0.9305 1.2165 0.1659 0.113 Uiso 1 1 calc R . . 
C36 C 0.84317(15) 1.1404(5) 0.15876(13) 0.0741(9) Uani 1 1 d . . . 
H36A H 0.8241 1.2625 0.1444 0.089 Uiso 1 1 calc R . . 
C37 C 0.55030(13) 0.7858(4) 0.06400(13) 0.0550(7) Uani 1 1 d . . . 
C38 C 0.51810(13) 0.6266(4) 0.14467(14) 0.0680(8) Uani 1 1 d . . . 
H38A H 0.5319 0.6091 0.1894 0.082 Uiso 1 1 calc R . . 
H38B H 0.4827 0.7180 0.1314 0.082 Uiso 1 1 calc R . . 
C39 C 0.49574(13) 0.4301(5) 0.11358(14) 0.0710(9) Uani 1 1 d . . . 
H39A H 0.5021 0.4038 0.0772 0.085 Uiso 1 1 calc R . . 
C40 C 0.46858(14) 0.2955(5) 0.13327(16) 0.0865(10) Uani 1 1 d . . . 
H40A H 0.4614 0.3163 0.1695 0.104 Uiso 1 1 calc R . . 
H40B H 0.4560 0.1770 0.1113 0.104 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 C1 1.389(3) . ? 
N1 C10 1.391(3) . ? 
N1 C11 1.437(3) . ? 
O1 C1 1.209(3) . ? 
O2 C10 1.210(3) . ? 
O3 C17 1.215(3) . ? 
C1 C2 1.507(4) . ? 
C2 C9 1.526(3) . ? 
C2 C3 1.550(3) . ? 
C3 C17 1.505(4) . ? 
C3 C4 1.534(4) . ? 
C4 C5 1.486(4) . ? 
C5 C6 1.325(4) . ? 
C6 C7 1.498(4) . ? 
C7 C17 1.506(4) . ? 
C7 C8 1.537(3) . ? 
C7 C18 1.541(4) . ? 
C8 C9 1.510(3) . ? 
C9 C10 1.510(4) . ? 
C11 C16 1.358(4) . ? 
C11 C12 1.375(4) . ? 
C12 C13 1.383(4) . ? 
C13 C14 1.367(4) . ? 
C14 C15 1.370(4) . ? 
C15 C16 1.372(4) . ? 
C18 C19 1.525(5) . ? 
C19 C20 1.185(5) . ? 
N2 C21 1.401(3) . ? 
N2 C30 1.404(3) . ? 
N2 C31 1.433(3) . ? 
O4 C21 1.207(3) . ? 
O5 C30 1.204(3) . ? 
O6 C37 1.213(3) . ? 
C21 C22 1.501(4) . ? 
C22 C29 1.528(3) . ? 
C22 C23 1.559(3) . ? 
C23 C37 1.498(4) . ? 
C23 C24 1.540(3) . ? 
C24 C25 1.488(4) . ? 
C25 C26 1.311(3) . ? 
C26 C27 1.498(3) . ? 
C27 C37 1.509(4) . ? 
C27 C38 1.527(4) . ? 
C27 C28 1.545(3) . ? 
C28 C29 1.521(3) . ? 
C29 C30 1.509(3) . ? 
C31 C32 1.373(4) . ? 
C31 C36 1.371(4) . ? 
C32 C33 1.377(4) . ? 
C33 C34 1.370(5) . ? 
C34 C35 1.369(5) . ? 
C35 C36 1.385(4) . ? 
C38 C39 1.499(4) . ? 
C39 C40 1.282(4) . ? 
  
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 N1 C10 111.9(2) . . ? 
C1 N1 C11 123.7(2) . . ? 
C10 N1 C11 124.3(2) . . ? 
O1 C1 N1 124.1(3) . . ? 
O1 C1 C2 127.5(3) . . ? 
N1 C1 C2 108.3(2) . . ? 
C1 C2 C9 104.0(2) . . ? 
C1 C2 C3 109.5(2) . . ? 
C9 C2 C3 115.8(2) . . ? 
C17 C3 C4 106.2(2) . . ? 
C17 C3 C2 109.3(2) . . ? 
C4 C3 C2 115.6(2) . . ? 
C5 C4 C3 112.3(2) . . ? 
C6 C5 C4 123.9(3) . . ? 
C5 C6 C7 123.4(3) . . ? 
C6 C7 C17 108.2(2) . . ? 
C6 C7 C8 109.9(2) . . ? 
C17 C7 C8 106.0(2) . . ? 
C6 C7 C18 111.7(2) . . ? 
C17 C7 C18 110.6(2) . . ? 
C8 C7 C18 110.1(2) . . ? 
C9 C8 C7 113.9(2) . . ? 
C8 C9 C10 116.0(2) . . ? 
C8 C9 C2 118.2(2) . . ? 
C10 C9 C2 103.9(2) . . ? 
O2 C10 N1 123.8(3) . . ? 
O2 C10 C9 128.0(3) . . ? 
N1 C10 C9 108.1(2) . . ? 
C16 C11 C12 120.7(3) . . ? 
C16 C11 N1 120.1(2) . . ? 
C12 C11 N1 119.2(3) . . ? 
C11 C12 C13 119.0(3) . . ? 
C14 C13 C12 120.3(3) . . ? 
C13 C14 C15 119.8(3) . . ? 
C14 C15 C16 120.2(3) . . ? 
C11 C16 C15 120.0(3) . . ? 
O3 C17 C3 122.5(3) . . ? 
O3 C17 C7 123.6(3) . . ? 
C3 C17 C7 113.9(2) . . ? 
C19 C18 C7 114.8(3) . . ? 
C20 C19 C18 128.4(5) . . ? 
C21 N2 C30 111.9(2) . . ? 
C21 N2 C31 123.4(2) . . ? 
C30 N2 C31 124.6(2) . . ? 
O4 C21 N2 123.9(3) . . ? 
O4 C21 C22 127.9(2) . . ? 
N2 C21 C22 108.1(2) . . ? 
C21 C22 C29 103.7(2) . . ? 
C21 C22 C23 109.8(2) . . ? 
C29 C22 C23 116.3(2) . . ? 
C37 C23 C24 106.6(2) . . ? 
C37 C23 C22 108.8(2) . . ? 
C24 C23 C22 115.3(2) . . ? 
C25 C24 C23 112.2(2) . . ? 
C26 C25 C24 123.1(2) . . ? 
C25 C26 C27 124.4(3) . . ? 
C26 C27 C37 108.9(2) . . ? 
C26 C27 C38 113.3(2) . . ? 
C37 C27 C38 111.5(2) . . ? 
C26 C27 C28 107.1(2) . . ? 
C37 C27 C28 106.7(2) . . ? 
C38 C27 C28 109.1(2) . . ? 
C29 C28 C27 113.6(2) . . ? 
C30 C29 C28 115.9(2) . . ? 
C30 C29 C22 104.4(2) . . ? 
C28 C29 C22 117.3(2) . . ? 
O5 C30 N2 124.3(2) . . ? 
O5 C30 C29 128.5(3) . . ? 
N2 C30 C29 107.1(2) . . ? 
C32 C31 C36 121.1(3) . . ? 
C32 C31 N2 119.6(3) . . ? 
C36 C31 N2 119.3(3) . . ? 
C31 C32 C33 119.4(3) . . ? 
C34 C33 C32 120.0(4) . . ? 
C35 C34 C33 120.2(3) . . ? 
C34 C35 C36 120.3(4) . . ? 
C31 C36 C35 118.9(3) . . ? 
O6 C37 C23 122.8(3) . . ? 
O6 C37 C27 123.5(3) . . ? 
C23 C37 C27 113.7(2) . . ? 
C39 C38 C27 114.9(2) . . ? 
C40 C39 C38 125.1(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 
C10 N1 C1 O1 177.3(2) . . . . ? 
C11 N1 C1 O1 -0.3(4) . . . . ? 
C10 N1 C1 C2 -6.3(3) . . . . ? 
C11 N1 C1 C2 176.1(2) . . . . ? 
O1 C1 C2 C9 -167.7(3) . . . . ? 
N1 C1 C2 C9 16.0(3) . . . . ? 
O1 C1 C2 C3 67.9(3) . . . . ? 
N1 C1 C2 C3 -108.4(2) . . . . ? 
C1 C2 C3 C17 154.8(2) . . . . ? 
C9 C2 C3 C17 37.6(3) . . . . ? 
C1 C2 C3 C4 35.0(3) . . . . ? 
C9 C2 C3 C4 -82.1(3) . . . . ? 
C17 C3 C4 C5 -45.3(3) . . . . ? 
C2 C3 C4 C5 76.2(3) . . . . ? 
C3 C4 C5 C6 16.4(4) . . . . ? 
C4 C5 C6 C7 -1.3(4) . . . . ? 
C5 C6 C7 C17 17.1(4) . . . . ? 
C5 C6 C7 C8 -98.2(3) . . . . ? 
C5 C6 C7 C18 139.1(3) . . . . ? 
C6 C7 C8 C9 63.6(3) . . . . ? 
C17 C7 C8 C9 -53.1(3) . . . . ? 
C18 C7 C8 C9 -172.9(2) . . . . ? 
C7 C8 C9 C10 -87.3(3) . . . . ? 
C7 C8 C9 C2 37.2(3) . . . . ? 
C1 C2 C9 C8 -149.1(2) . . . . ? 
C3 C2 C9 C8 -28.9(3) . . . . ? 
C1 C2 C9 C10 -18.8(3) . . . . ? 
C3 C2 C9 C10 101.4(3) . . . . ? 
C1 N1 C10 O2 176.7(3) . . . . ? 
C11 N1 C10 O2 -5.7(4) . . . . ? 
C1 N1 C10 C9 -6.4(3) . . . . ? 
C11 N1 C10 C9 171.2(2) . . . . ? 
C8 C9 C10 O2 -35.8(4) . . . . ? 
C2 C9 C10 O2 -167.3(3) . . . . ? 
C8 C9 C10 N1 147.5(2) . . . . ? 
C2 C9 C10 N1 16.0(3) . . . . ? 
C1 N1 C11 C16 -117.0(3) . . . . ? 
C10 N1 C11 C16 65.7(3) . . . . ? 
C1 N1 C11 C12 64.7(3) . . . . ? 
C10 N1 C11 C12 -112.6(3) . . . . ? 
C16 C11 C12 C13 1.3(4) . . . . ? 
N1 C11 C12 C13 179.5(2) . . . . ? 
C11 C12 C13 C14 -0.7(4) . . . . ? 
C12 C13 C14 C15 -0.1(4) . . . . ? 
C13 C14 C15 C16 0.4(4) . . . . ? 
C12 C11 C16 C15 -1.0(4) . . . . ? 
N1 C11 C16 C15 -179.2(2) . . . . ? 
C14 C15 C16 C11 0.2(4) . . . . ? 
C4 C3 C17 O3 -114.1(3) . . . . ? 
C2 C3 C17 O3 120.5(3) . . . . ? 
C4 C3 C17 C7 65.8(3) . . . . ? 
C2 C3 C17 C7 -59.6(3) . . . . ? 
C6 C7 C17 O3 129.3(3) . . . . ? 
C8 C7 C17 O3 -112.8(3) . . . . ? 
C18 C7 C17 O3 6.6(4) . . . . ? 
C6 C7 C17 C3 -50.6(3) . . . . ? 
C8 C7 C17 C3 67.3(3) . . . . ? 
C18 C7 C17 C3 -173.3(2) . . . . ? 
C6 C7 C18 C19 67.6(4) . . . . ? 
C17 C7 C18 C19 -171.7(3) . . . . ? 
C8 C7 C18 C19 -54.8(4) . . . . ? 
C7 C18 C19 C20 -105.5(5) . . . . ? 
C30 N2 C21 O4 176.0(3) . . . . ? 
C31 N2 C21 O4 -7.1(4) . . . . ? 
C30 N2 C21 C22 -6.6(3) . . . . ? 
C31 N2 C21 C22 170.3(2) . . . . ? 
O4 C21 C22 C29 -164.9(3) . . . . ? 
N2 C21 C22 C29 17.8(3) . . . . ? 
O4 C21 C22 C23 70.1(3) . . . . ? 
N2 C21 C22 C23 -107.2(2) . . . . ? 
C21 C22 C23 C37 157.1(2) . . . . ? 
C29 C22 C23 C37 39.8(3) . . . . ? 
C21 C22 C23 C24 37.4(3) . . . . ? 
C29 C22 C23 C24 -79.9(3) . . . . ? 
C37 C23 C24 C25 -47.0(3) . . . . ? 
C22 C23 C24 C25 73.9(3) . . . . ? 
C23 C24 C25 C26 18.3(4) . . . . ? 
C24 C25 C26 C27 -1.6(4) . . . . ? 
C25 C26 C27 C37 15.3(3) . . . . ? 
C25 C26 C27 C38 139.9(3) . . . . ? 
C25 C26 C27 C28 -99.7(3) . . . . ? 
C26 C27 C28 C29 63.6(3) . . . . ? 
C37 C27 C28 C29 -52.8(3) . . . . ? 
C38 C27 C28 C29 -173.4(2) . . . . ? 
C27 C28 C29 C30 -86.7(3) . . . . ? 
C27 C28 C29 C22 37.4(3) . . . . ? 
C21 C22 C29 C30 -21.7(3) . . . . ? 
C23 C22 C29 C30 99.0(2) . . . . ? 
C21 C22 C29 C28 -151.4(2) . . . . ? 
C23 C22 C29 C28 -30.7(3) . . . . ? 
C21 N2 C30 O5 175.7(2) . . . . ? 
C31 N2 C30 O5 -1.2(4) . . . . ? 
C21 N2 C30 C29 -7.8(3) . . . . ? 
C31 N2 C30 C29 175.3(2) . . . . ? 
C28 C29 C30 O5 -34.6(4) . . . . ? 
C22 C29 C30 O5 -165.2(2) . . . . ? 
C28 C29 C30 N2 149.1(2) . . . . ? 
C22 C29 C30 N2 18.5(3) . . . . ? 
C21 N2 C31 C32 -122.0(3) . . . . ? 
C30 N2 C31 C32 54.5(3) . . . . ? 
C21 N2 C31 C36 55.5(4) . . . . ? 
C30 N2 C31 C36 -128.0(3) . . . . ? 
C36 C31 C32 C33 -0.2(4) . . . . ? 
N2 C31 C32 C33 177.3(2) . . . . ? 
C31 C32 C33 C34 -0.9(5) . . . . ? 
C32 C33 C34 C35 1.2(5) . . . . ? 
C33 C34 C35 C36 -0.5(5) . . . . ? 
C32 C31 C36 C35 0.9(4) . . . . ? 
N2 C31 C36 C35 -176.6(2) . . . . ? 
C34 C35 C36 C31 -0.6(5) . . . . ? 
C24 C23 C37 O6 -114.9(3) . . . . ? 
C22 C23 C37 O6 120.2(3) . . . . ? 
C24 C23 C37 C27 64.7(3) . . . . ? 
C22 C23 C37 C27 -60.2(3) . . . . ? 
C26 C27 C37 O6 131.6(3) . . . . ? 
C38 C27 C37 O6 5.9(4) . . . . ? 
C28 C27 C37 O6 -113.1(3) . . . . ? 
C26 C27 C37 C23 -48.0(3) . . . . ? 
C38 C27 C37 C23 -173.7(2) . . . . ? 
C28 C27 C37 C23 67.3(3) . . . . ? 
C26 C27 C38 C39 -54.9(3) . . . . ? 
C37 C27 C38 C39 68.3(3) . . . . ? 
C28 C27 C38 C39 -174.1(2) . . . . ? 
C27 C38 C39 C40 154.7(3) . . . . ? 
  
_diffrn_measured_fraction_theta_max    0.986 
_diffrn_reflns_theta_full              22.01 
_diffrn_measured_fraction_theta_full   0.986 
_refine_diff_density_max    0.348 
_refine_diff_density_min   -0.163 
_refine_diff_density_rms    0.030 
