# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2011

data_global
_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
loop_
_publ_author_name
K.Kutlescha
G.T.Venkanna
R.Kempe
_publ_contact_author_name        'Rhett Kempe'
_publ_contact_author_email       kempe@uni-bayreuth.de

data_k479m
_database_code_depnum_ccdc_archive 'CCDC 782978'
#TrackingRef 'k479m.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H23 N'
_chemical_formula_weight         397.49

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   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                   11.4870(8)
_cell_length_b                   10.7950(5)
_cell_length_c                   17.4210(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.575(5)
_cell_angle_gamma                90.00
_cell_volume                     2116.3(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    all
_cell_measurement_2theta_min     3.77
_cell_measurement_2theta_max     52.02

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.35
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             840
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  STOE-IPDSII
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27225
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         25.82
_reflns_number_total             3993
_reflns_number_gt                2986
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       X-AREA-STOE
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    SIR-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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^)+(0.0451P)^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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3993
_refine_ls_number_parameters     373
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0330
_refine_ls_wR_factor_ref         0.0746
_refine_ls_wR_factor_gt          0.0703
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_restrained_S_all      0.912
_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
C1 C 0.82935(11) 0.54125(11) 0.34451(7) 0.0246(3) Uani 1 1 d . . .
C2 C 0.94590(10) 0.50407(11) 0.35441(7) 0.0242(3) Uani 1 1 d . . .
C3 C 0.98203(11) 0.38971(11) 0.32251(7) 0.0249(3) Uani 1 1 d . . .
C4 C 1.10170(10) 0.37710(11) 0.34327(7) 0.0242(3) Uani 1 1 d . . .
C5 C 1.14648(11) 0.48539(11) 0.38898(7) 0.0243(3) Uani 1 1 d . . .
C6 C 1.05596(10) 0.56317(11) 0.39546(7) 0.0237(3) Uani 1 1 d . . .
C7 C 1.07356(10) 0.68148(10) 0.43945(7) 0.0237(3) Uani 1 1 d . . .
C8 C 1.00519(11) 0.71484(11) 0.49381(7) 0.0255(3) Uani 1 1 d . . .
C9 C 1.02601(12) 0.82479(12) 0.53529(8) 0.0296(3) Uani 1 1 d . . .
C10 C 1.11612(12) 0.90284(12) 0.52372(8) 0.0318(3) Uani 1 1 d . . .
C11 C 1.18547(11) 0.87116(12) 0.47061(8) 0.0315(3) Uani 1 1 d . . .
C12 C 1.16475(11) 0.76132(11) 0.42867(7) 0.0282(3) Uani 1 1 d . . .
C13 C 1.17291(11) 0.27056(11) 0.32751(7) 0.0249(3) Uani 1 1 d . . .
C14 C 1.28006(12) 0.24235(12) 0.37681(8) 0.0327(3) Uani 1 1 d . . .
C15 C 1.34445(13) 0.13861(13) 0.36438(8) 0.0383(3) Uani 1 1 d . . .
C16 C 1.30352(12) 0.06058(13) 0.30209(8) 0.0353(3) Uani 1 1 d . . .
C17 C 1.19743(12) 0.08768(13) 0.25249(8) 0.0347(3) Uani 1 1 d . . .
C18 C 1.13256(12) 0.19104(12) 0.26462(8) 0.0302(3) Uani 1 1 d . . .
C19 C 0.69670(11) 0.70158(11) 0.38526(7) 0.0259(3) Uani 1 1 d . . .
C20 C 0.62143(12) 0.62465(13) 0.41699(7) 0.0309(3) Uani 1 1 d . . .
C21 C 0.52372(12) 0.67449(14) 0.44102(8) 0.0374(3) Uani 1 1 d . . .
C22 C 0.50089(13) 0.79986(15) 0.43564(9) 0.0423(4) Uani 1 1 d . . .
C23 C 0.57697(13) 0.87634(14) 0.40557(9) 0.0409(4) Uani 1 1 d . . .
C24 C 0.67326(12) 0.82794(12) 0.38004(8) 0.0319(3) Uani 1 1 d . . .
C25 C 0.73003(10) 0.45682(11) 0.31148(7) 0.0252(3) Uani 1 1 d . . .
C26 C 0.64222(11) 0.49471(12) 0.24893(7) 0.0286(3) Uani 1 1 d . . .
C27 C 0.54743(12) 0.41775(13) 0.21953(8) 0.0336(3) Uani 1 1 d . . .
C28 C 0.53777(12) 0.30341(13) 0.25356(8) 0.0356(3) Uani 1 1 d . . .
C29 C 0.62514(12) 0.26501(13) 0.31550(8) 0.0351(3) Uani 1 1 d . . .
C30 C 0.72090(12) 0.34034(12) 0.34448(8) 0.0298(3) Uani 1 1 d . . .
N1 N 0.79849(9) 0.65952(10) 0.35998(6) 0.0268(2) Uani 1 1 d . . .
H1N H 0.8534(13) 0.7149(13) 0.3626(8) 0.032(4) Uiso 1 1 d . . .
H3 H 0.9290(11) 0.3310(11) 0.2923(7) 0.024(3) Uiso 1 1 d . . .
H5 H 1.2299(11) 0.4987(11) 0.4127(7) 0.023(3) Uiso 1 1 d . . .
H8 H 0.9427(11) 0.6597(11) 0.5032(7) 0.022(3) Uiso 1 1 d . . .
H9 H 0.9756(12) 0.8434(12) 0.5711(8) 0.034(4) Uiso 1 1 d . . .
H10 H 1.1297(12) 0.9821(13) 0.5525(8) 0.036(4) Uiso 1 1 d . . .
H11 H 1.2485(12) 0.9245(13) 0.4627(7) 0.032(3) Uiso 1 1 d . . .
H12 H 1.2131(12) 0.7403(12) 0.3909(8) 0.031(3) Uiso 1 1 d . . .
H14 H 1.3095(13) 0.2943(13) 0.4224(8) 0.040(4) Uiso 1 1 d . . .
H15 H 1.4200(14) 0.1210(14) 0.3998(9) 0.049(4) Uiso 1 1 d . . .
H16 H 1.3478(13) -0.0136(13) 0.2925(8) 0.040(4) Uiso 1 1 d . . .
H17 H 1.1646(13) 0.0327(14) 0.2085(9) 0.046(4) Uiso 1 1 d . . .
H18 H 1.0569(13) 0.2079(12) 0.2294(8) 0.036(4) Uiso 1 1 d . . .
H20 H 0.6387(12) 0.5378(14) 0.4223(8) 0.038(4) Uiso 1 1 d . . .
H21 H 0.4692(13) 0.6203(13) 0.4622(8) 0.038(4) Uiso 1 1 d . . .
H22 H 0.4331(13) 0.8340(13) 0.4515(8) 0.041(4) Uiso 1 1 d . . .
H23 H 0.5628(13) 0.9664(14) 0.4006(8) 0.044(4) Uiso 1 1 d . . .
H24 H 0.7264(12) 0.8798(13) 0.3578(8) 0.037(4) Uiso 1 1 d . . .
H26 H 0.6496(12) 0.5768(14) 0.2256(8) 0.036(4) Uiso 1 1 d . . .
H27 H 0.4876(13) 0.4445(12) 0.1749(8) 0.037(4) Uiso 1 1 d . . .
H28 H 0.4697(13) 0.2488(12) 0.2345(8) 0.035(4) Uiso 1 1 d . . .
H29 H 0.6169(12) 0.1854(14) 0.3397(8) 0.039(4) Uiso 1 1 d . . .
H30 H 0.7810(12) 0.3154(11) 0.3880(8) 0.026(3) 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
C1 0.0272(7) 0.0231(6) 0.0233(6) 0.0025(5) 0.0048(5) 0.0013(5)
C2 0.0258(6) 0.0220(6) 0.0249(6) 0.0020(5) 0.0049(5) 0.0011(5)
C3 0.0271(7) 0.0235(7) 0.0235(6) -0.0003(5) 0.0038(5) -0.0007(5)
C4 0.0256(6) 0.0251(6) 0.0226(6) 0.0018(5) 0.0062(5) 0.0006(5)
C5 0.0212(7) 0.0268(7) 0.0248(6) 0.0009(5) 0.0042(5) -0.0013(5)
C6 0.0240(6) 0.0228(6) 0.0250(6) 0.0032(5) 0.0064(5) -0.0002(5)
C7 0.0234(6) 0.0210(6) 0.0250(6) 0.0021(5) 0.0007(5) 0.0030(5)
C8 0.0257(7) 0.0226(6) 0.0274(6) 0.0037(5) 0.0030(5) 0.0013(5)
C9 0.0316(7) 0.0264(7) 0.0304(7) 0.0008(5) 0.0050(6) 0.0062(5)
C10 0.0322(8) 0.0204(7) 0.0389(7) -0.0028(6) -0.0021(6) 0.0037(6)
C11 0.0247(7) 0.0239(7) 0.0439(8) 0.0030(6) 0.0021(6) -0.0026(6)
C12 0.0238(7) 0.0271(7) 0.0332(7) 0.0013(5) 0.0045(6) 0.0011(5)
C13 0.0254(6) 0.0245(6) 0.0264(6) 0.0012(5) 0.0092(5) 0.0001(5)
C14 0.0300(7) 0.0350(8) 0.0318(7) -0.0083(6) 0.0033(6) 0.0056(6)
C15 0.0331(8) 0.0428(8) 0.0373(8) -0.0043(6) 0.0027(6) 0.0137(6)
C16 0.0376(8) 0.0310(7) 0.0397(8) -0.0031(6) 0.0134(6) 0.0102(6)
C17 0.0384(8) 0.0320(7) 0.0351(7) -0.0097(6) 0.0106(6) 0.0000(6)
C18 0.0264(7) 0.0331(7) 0.0309(7) -0.0023(6) 0.0053(6) 0.0015(6)
C19 0.0221(6) 0.0291(7) 0.0244(6) -0.0041(5) -0.0005(5) 0.0028(5)
C20 0.0315(7) 0.0320(8) 0.0286(7) -0.0021(5) 0.0045(5) 0.0012(6)
C21 0.0273(7) 0.0523(9) 0.0330(7) -0.0053(6) 0.0071(6) -0.0020(7)
C22 0.0268(8) 0.0565(10) 0.0425(8) -0.0138(7) 0.0040(6) 0.0123(7)
C23 0.0355(8) 0.0361(8) 0.0475(9) -0.0075(7) 0.0000(7) 0.0120(7)
C24 0.0288(7) 0.0287(7) 0.0360(7) -0.0040(6) 0.0013(6) 0.0029(6)
C25 0.0227(6) 0.0245(6) 0.0289(6) -0.0031(5) 0.0065(5) 0.0028(5)
C26 0.0283(7) 0.0272(7) 0.0303(7) -0.0016(5) 0.0059(5) 0.0047(5)
C27 0.0284(7) 0.0373(8) 0.0328(7) -0.0061(6) 0.0004(6) 0.0029(6)
C28 0.0302(8) 0.0350(8) 0.0409(8) -0.0109(6) 0.0055(6) -0.0054(6)
C29 0.0351(8) 0.0258(7) 0.0446(8) -0.0011(6) 0.0084(6) -0.0029(6)
C30 0.0266(7) 0.0277(7) 0.0339(7) 0.0009(6) 0.0033(6) 0.0020(6)
N1 0.0220(6) 0.0217(6) 0.0367(6) -0.0006(4) 0.0062(5) -0.0005(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
C1 N1 1.3662(15) . ?
C1 C2 1.3751(16) . ?
C1 C25 1.4833(17) . ?
C2 C3 1.4483(17) . ?
C2 C6 1.4676(17) . ?
C3 C4 1.3563(17) . ?
C4 C5 1.4496(17) . ?
C4 C13 1.4687(16) . ?
C5 C6 1.3587(17) . ?
C6 C7 1.4824(16) . ?
C7 C8 1.3935(17) . ?
C7 C12 1.3979(17) . ?
C8 C9 1.3852(18) . ?
C9 C10 1.3805(19) . ?
C10 C11 1.3796(19) . ?
C11 C12 1.3880(18) . ?
C13 C14 1.3860(18) . ?
C13 C18 1.3958(17) . ?
C14 C15 1.3830(19) . ?
C15 C16 1.380(2) . ?
C16 C17 1.377(2) . ?
C17 C18 1.3813(18) . ?
C19 C24 1.3898(18) . ?
C19 C20 1.3909(18) . ?
C19 N1 1.4050(16) . ?
C20 C21 1.3831(19) . ?
C21 C22 1.378(2) . ?
C22 C23 1.380(2) . ?
C23 C24 1.3754(19) . ?
C25 C26 1.3897(18) . ?
C25 C30 1.3952(17) . ?
C26 C27 1.3836(19) . ?
C27 C28 1.383(2) . ?
C28 C29 1.382(2) . ?
C29 C30 1.3795(19) . ?

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
N1 C1 C2 122.19(11) . . ?
N1 C1 C25 116.17(10) . . ?
C2 C1 C25 121.53(10) . . ?
C1 C2 C3 123.19(11) . . ?
C1 C2 C6 131.00(11) . . ?
C3 C2 C6 105.81(10) . . ?
C4 C3 C2 109.66(11) . . ?
C3 C4 C5 107.13(10) . . ?
C3 C4 C13 126.98(11) . . ?
C5 C4 C13 125.77(11) . . ?
C6 C5 C4 110.54(11) . . ?
C5 C6 C2 106.84(10) . . ?
C5 C6 C7 123.23(11) . . ?
C2 C6 C7 129.89(10) . . ?
C8 C7 C12 118.15(11) . . ?
C8 C7 C6 122.48(11) . . ?
C12 C7 C6 119.33(10) . . ?
C9 C8 C7 120.93(12) . . ?
C10 C9 C8 120.19(12) . . ?
C11 C10 C9 119.82(12) . . ?
C10 C11 C12 120.25(12) . . ?
C11 C12 C7 120.65(12) . . ?
C14 C13 C18 117.71(12) . . ?
C14 C13 C4 120.99(11) . . ?
C18 C13 C4 121.24(12) . . ?
C15 C14 C13 121.15(13) . . ?
C16 C15 C14 120.60(14) . . ?
C17 C16 C15 118.89(12) . . ?
C16 C17 C18 120.82(13) . . ?
C17 C18 C13 120.83(13) . . ?
C24 C19 C20 118.97(12) . . ?
C24 C19 N1 117.33(11) . . ?
C20 C19 N1 123.67(11) . . ?
C21 C20 C19 119.67(13) . . ?
C22 C21 C20 121.09(14) . . ?
C21 C22 C23 119.15(13) . . ?
C24 C23 C22 120.48(14) . . ?
C23 C24 C19 120.62(14) . . ?
C26 C25 C30 119.05(12) . . ?
C26 C25 C1 120.27(11) . . ?
C30 C25 C1 120.63(11) . . ?
C27 C26 C25 120.47(13) . . ?
C26 C27 C28 120.13(13) . . ?
C29 C28 C27 119.62(13) . . ?
C30 C29 C28 120.65(13) . . ?
C29 C30 C25 120.05(13) . . ?
C1 N1 C19 128.98(11) . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        25.82
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         0.172
_refine_diff_density_min         -0.139
_refine_diff_density_rms         0.032


# Attachment 'k575a.cif'

data_k575a
_database_code_depnum_ccdc_archive 'CCDC 782979'
#TrackingRef 'k575a.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H30 K N O'
_chemical_formula_weight         507.69

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'
K K 0.2009 0.2494 '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                   9.2950(11)
_cell_length_b                   11.2290(15)
_cell_length_c                   13.2300(16)
_cell_angle_alpha                102.247(10)
_cell_angle_beta                 90.466(10)
_cell_angle_gamma                90.952(10)
_cell_volume                     1349.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    all
_cell_measurement_2theta_min     3.15
_cell_measurement_2theta_max     52.06

_exptl_crystal_description       needle-like
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             536
_exptl_absorpt_coefficient_mu    0.224
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
Alert Level C: The crystal is very weakly diffracting.
;

_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  STOE-IPDSII
_diffrn_measurement_method       Omega-Scan
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17692
_diffrn_reflns_av_R_equivalents  0.1965
_diffrn_reflns_av_sigmaI/netI    0.3229
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.58
_diffrn_reflns_theta_max         25.74
_reflns_number_total             5098
_reflns_number_gt                1784
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       X-AREA-STOE
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    SIR-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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^)+(0.0000P)^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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5098
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1970
_refine_ls_R_factor_gt           0.0561
_refine_ls_wR_factor_ref         0.0989
_refine_ls_wR_factor_gt          0.0706
_refine_ls_goodness_of_fit_ref   0.684
_refine_ls_restrained_S_all      0.684
_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
C1 C 0.2932(4) 0.9653(4) 0.6852(3) 0.0203(11) Uani 1 1 d . . .
H1 H 0.2995 0.9043 0.7250 0.024 Uiso 1 1 calc R . .
C2 C -0.3113(5) 0.9087(4) 0.2771(4) 0.0212(12) Uani 1 1 d . . .
C3 C -0.2908(5) 0.8527(4) 0.3618(3) 0.0213(12) Uani 1 1 d . . .
H3 H -0.2961 0.7674 0.3582 0.026 Uiso 1 1 calc R . .
C4 C 0.2620(5) 1.0600(4) 0.5490(4) 0.0196(11) Uani 1 1 d . . .
C5 C -0.3454(5) 0.8470(4) 0.1695(4) 0.0231(12) Uani 1 1 d . . .
C6 C -0.3727(5) 0.9107(4) 0.0928(3) 0.0235(12) Uani 1 1 d . . .
H6 H -0.3668 0.9972 0.1095 0.028 Uiso 1 1 calc R . .
C7 C -0.4083(5) 0.8525(4) -0.0074(4) 0.0302(13) Uani 1 1 d . . .
H7 H -0.4274 0.8990 -0.0580 0.036 Uiso 1 1 calc R . .
C8 C -0.4160(5) 0.7263(5) -0.0338(4) 0.0325(14) Uani 1 1 d . . .
H8 H -0.4398 0.6857 -0.1026 0.039 Uiso 1 1 calc R . .
C9 C -0.3888(5) 0.6603(4) 0.0407(4) 0.0357(14) Uani 1 1 d . . .
H9 H -0.3935 0.5737 0.0230 0.043 Uiso 1 1 calc R . .
C10 C -0.3547(5) 0.7191(4) 0.1415(4) 0.0290(13) Uani 1 1 d . . .
H10 H -0.3375 0.6723 0.1922 0.035 Uiso 1 1 calc R . .
C11 C 0.2515(5) 1.0893(4) 0.4454(3) 0.0176(11) Uani 1 1 d . . .
C12 C 0.3331(5) 1.0299(4) 0.3638(4) 0.0193(12) Uani 1 1 d . . .
H12 H 0.3951 0.9666 0.3733 0.023 Uiso 1 1 calc R . .
C13 C 0.3254(5) 1.0616(4) 0.2684(4) 0.0242(12) Uani 1 1 d . . .
H13 H 0.3801 1.0186 0.2125 0.029 Uiso 1 1 calc R . .
C14 C 0.2396(5) 1.1545(4) 0.2544(4) 0.0302(13) Uani 1 1 d . . .
H14 H 0.2351 1.1766 0.1890 0.036 Uiso 1 1 calc R . .
C15 C 0.1599(5) 1.2155(4) 0.3352(4) 0.0284(13) Uani 1 1 d . . .
H15 H 0.1009 1.2807 0.3259 0.034 Uiso 1 1 calc R . .
C16 C 0.1650(5) 1.1830(4) 0.4297(4) 0.0238(12) Uani 1 1 d . . .
H16 H 0.1084 1.2254 0.4849 0.029 Uiso 1 1 calc R . .
C17 C 0.0438(5) 0.6609(4) 0.2960(4) 0.0257(12) Uani 1 1 d . . .
H17 H -0.0451 0.6962 0.3201 0.031 Uiso 1 1 calc R . .
C18 C 0.0445(6) 0.5623(4) 0.2133(4) 0.0367(15) Uani 1 1 d . . .
H18 H -0.0437 0.5301 0.1812 0.044 Uiso 1 1 calc R . .
C19 C 0.1720(5) 0.5108(4) 0.1774(4) 0.0359(15) Uani 1 1 d . . .
H19 H 0.1725 0.4420 0.1214 0.043 Uiso 1 1 calc R . .
C20 C 0.2993(6) 0.5595(4) 0.2232(4) 0.0347(14) Uani 1 1 d . . .
H20 H 0.3881 0.5254 0.1977 0.042 Uiso 1 1 calc R . .
C21 C 0.2989(5) 0.6576(4) 0.3060(4) 0.0260(13) Uani 1 1 d . . .
H21 H 0.3876 0.6902 0.3369 0.031 Uiso 1 1 calc R . .
C22 C 0.1718(5) 0.7090(4) 0.3446(3) 0.0213(12) Uani 1 1 d . . .
C23 C 0.2355(5) 0.8252(4) 0.5110(4) 0.0227(12) Uani 1 1 d . . .
C24 C 0.2640(5) 0.9446(4) 0.5775(4) 0.0223(12) Uani 1 1 d . . .
C25 C 0.2848(5) 0.7160(4) 0.5488(4) 0.0189(12) Uani 1 1 d . . .
C26 C 0.1889(5) 0.6213(4) 0.5512(4) 0.0277(13) Uani 1 1 d . . .
H26 H 0.0930 0.6247 0.5267 0.033 Uiso 1 1 calc R . .
C27 C 0.2320(6) 0.5217(4) 0.5889(4) 0.0373(15) Uani 1 1 d . . .
H27 H 0.1649 0.4577 0.5914 0.045 Uiso 1 1 calc R . .
C28 C 0.3700(6) 0.5144(4) 0.6226(4) 0.0373(15) Uani 1 1 d . . .
H28 H 0.3991 0.4451 0.6475 0.045 Uiso 1 1 calc R . .
C29 C 0.4671(5) 0.6079(4) 0.6202(4) 0.0323(14) Uani 1 1 d . . .
H29 H 0.5633 0.6035 0.6437 0.039 Uiso 1 1 calc R . .
C30 C 0.4237(5) 0.7076(4) 0.5837(4) 0.0246(12) Uani 1 1 d . . .
H30 H 0.4907 0.7720 0.5825 0.030 Uiso 1 1 calc R . .
C31 C 0.2117(6) 0.8068(5) 0.0677(4) 0.0549(18) Uani 1 1 d . . .
H31A H 0.2442 0.7620 0.1204 0.066 Uiso 1 1 calc R . .
H31B H 0.2859 0.8689 0.0614 0.066 Uiso 1 1 calc R . .
C32 C 0.1856(7) 0.7198(5) -0.0356(5) 0.066(2) Uani 1 1 d . . .
H32A H 0.2729 0.7119 -0.0786 0.079 Uiso 1 1 calc R . .
H32B H 0.1546 0.6381 -0.0262 0.079 Uiso 1 1 calc R . .
C33 C 0.0695(6) 0.7793(5) -0.0818(4) 0.0442(16) Uani 1 1 d . . .
H33A H 0.1082 0.8437 -0.1154 0.053 Uiso 1 1 calc R . .
H33B H 0.0128 0.7195 -0.1332 0.053 Uiso 1 1 calc R . .
C34 C -0.0177(6) 0.8315(6) 0.0089(4) 0.0578(19) Uani 1 1 d . . .
H34A H -0.0673 0.9049 -0.0025 0.069 Uiso 1 1 calc R . .
H34B H -0.0912 0.7713 0.0208 0.069 Uiso 1 1 calc R . .
N1 N 0.1666(4) 0.8163(3) 0.4234(3) 0.0223(10) Uani 1 1 d . . .
K1 K 0.01143(12) 0.94570(10) 0.29959(9) 0.0248(3) Uani 1 1 d . . .
O1 O 0.0772(4) 0.8624(3) 0.0954(3) 0.0414(10) Uani 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
C1 0.023(3) 0.016(3) 0.023(3) 0.006(2) 0.002(2) 0.004(2)
C2 0.027(3) 0.015(3) 0.021(3) 0.003(2) -0.003(2) -0.002(2)
C3 0.027(3) 0.008(2) 0.027(3) 0.000(2) -0.001(2) 0.002(2)
C4 0.019(3) 0.017(3) 0.024(3) 0.007(2) 0.003(2) 0.006(2)
C5 0.021(3) 0.023(3) 0.025(3) 0.006(2) -0.001(2) -0.001(2)
C6 0.025(3) 0.022(3) 0.021(3) 0.000(2) 0.001(2) 0.009(2)
C7 0.032(3) 0.039(3) 0.021(3) 0.009(3) -0.001(3) 0.006(3)
C8 0.030(3) 0.044(3) 0.020(3) -0.001(3) 0.000(3) 0.001(3)
C9 0.042(4) 0.029(3) 0.032(4) 0.000(3) -0.001(3) 0.000(3)
C10 0.042(4) 0.028(3) 0.020(3) 0.011(2) 0.001(3) -0.004(3)
C11 0.012(3) 0.019(3) 0.019(3) -0.001(2) 0.001(2) -0.005(2)
C12 0.020(3) 0.019(3) 0.016(3) -0.002(2) -0.003(2) -0.006(2)
C13 0.023(3) 0.026(3) 0.019(3) -0.005(2) 0.005(2) -0.008(2)
C14 0.034(3) 0.035(3) 0.023(3) 0.009(3) 0.003(3) -0.003(3)
C15 0.028(3) 0.032(3) 0.025(3) 0.006(3) 0.002(3) 0.008(2)
C16 0.026(3) 0.024(3) 0.020(3) 0.001(2) 0.002(2) 0.000(2)
C17 0.028(3) 0.023(3) 0.025(3) 0.003(2) 0.000(2) 0.004(2)
C18 0.037(4) 0.031(3) 0.037(4) -0.004(3) -0.003(3) -0.008(3)
C19 0.039(4) 0.027(3) 0.033(4) -0.013(3) 0.013(3) -0.003(3)
C20 0.033(3) 0.035(3) 0.031(3) -0.006(3) 0.005(3) 0.010(3)
C21 0.024(3) 0.023(3) 0.030(3) 0.002(2) 0.000(2) 0.004(2)
C22 0.029(3) 0.015(3) 0.019(3) 0.000(2) -0.001(2) 0.005(2)
C23 0.023(3) 0.021(3) 0.024(3) 0.005(2) 0.002(2) -0.005(2)
C24 0.029(3) 0.016(3) 0.022(3) 0.003(2) -0.006(2) 0.003(2)
C25 0.020(3) 0.017(3) 0.018(3) 0.001(2) 0.004(2) 0.006(2)
C26 0.020(3) 0.028(3) 0.036(4) 0.012(3) -0.004(3) -0.001(2)
C27 0.041(4) 0.026(3) 0.045(4) 0.010(3) 0.000(3) -0.011(3)
C28 0.038(4) 0.027(3) 0.051(4) 0.015(3) -0.001(3) 0.006(3)
C29 0.028(3) 0.021(3) 0.050(4) 0.011(3) -0.007(3) 0.004(2)
C30 0.025(3) 0.021(3) 0.027(3) 0.004(2) -0.002(2) -0.002(2)
C31 0.046(4) 0.063(4) 0.048(4) -0.007(3) -0.016(3) 0.013(3)
C32 0.065(5) 0.065(4) 0.054(5) -0.017(3) -0.020(4) 0.025(4)
C33 0.043(4) 0.048(4) 0.037(4) 0.000(3) -0.002(3) -0.008(3)
C34 0.031(4) 0.085(5) 0.047(4) -0.009(4) 0.000(3) 0.000(3)
N1 0.026(3) 0.021(2) 0.020(2) 0.0043(19) -0.003(2) -0.0031(18)
K1 0.0226(7) 0.0260(7) 0.0252(7) 0.0041(6) -0.0012(5) -0.0012(5)
O1 0.033(2) 0.055(2) 0.031(2) -0.0037(18) 0.0020(19) -0.003(2)

_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
C1 C2 1.404(5) 2_576 ?
C1 C24 1.416(6) . ?
C1 K1 3.013(4) 2_576 ?
C2 C1 1.404(5) 2_576 ?
C2 C3 1.409(6) . ?
C2 C5 1.475(6) . ?
C2 K1 3.025(5) . ?
C3 C4 1.386(6) 2_576 ?
C3 K1 3.157(5) . ?
C4 C3 1.386(6) 2_576 ?
C4 C24 1.425(6) . ?
C4 C11 1.479(6) . ?
C4 K1 3.257(5) 2_576 ?
C5 C6 1.384(6) . ?
C5 C10 1.406(5) . ?
C6 C7 1.382(6) . ?
C7 C8 1.387(6) . ?
C8 C9 1.378(6) . ?
C9 C10 1.388(6) . ?
C11 C12 1.383(6) . ?
C11 C16 1.383(6) . ?
C11 K1 3.129(4) . ?
C12 C13 1.383(6) . ?
C12 K1 3.175(4) . ?
C13 C14 1.366(6) . ?
C13 K1 3.241(5) . ?
C14 C15 1.371(6) . ?
C14 K1 3.286(5) . ?
C15 C16 1.376(6) . ?
C15 K1 3.249(5) . ?
C16 K1 3.161(4) . ?
C17 C18 1.382(6) . ?
C17 C22 1.393(6) . ?
C17 K1 3.208(4) . ?
C18 C19 1.371(6) . ?
C19 C20 1.376(6) . ?
C20 C21 1.378(6) . ?
C21 C22 1.377(6) . ?
C22 N1 1.418(5) . ?
C22 K1 3.229(4) . ?
C23 N1 1.304(5) . ?
C23 C24 1.458(6) . ?
C23 C25 1.496(6) . ?
C24 K1 3.168(5) 2_576 ?
C25 C30 1.378(5) . ?
C25 C26 1.382(6) . ?
C26 C27 1.381(6) . ?
C27 C28 1.364(6) . ?
C28 C29 1.379(6) . ?
C29 C30 1.375(6) . ?
C31 O1 1.423(6) . ?
C31 C32 1.517(7) . ?
C32 C33 1.474(7) . ?
C33 C34 1.474(7) . ?
C34 O1 1.419(6) . ?
N1 K1 2.814(4) . ?
K1 O1 2.742(4) . ?
K1 C1 3.013(4) 2_576 ?
K1 C24 3.168(5) 2_576 ?

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
C2 C1 C24 108.3(4) 2_576 . ?
C2 C1 K1 77.1(3) 2_576 2_576 ?
C24 C1 K1 83.0(3) . 2_576 ?
C1 C2 C3 106.8(4) 2_576 . ?
C1 C2 C5 126.5(4) 2_576 . ?
C3 C2 C5 126.7(4) . . ?
C1 C2 K1 76.0(3) 2_576 . ?
C3 C2 K1 82.1(3) . . ?
C5 C2 K1 108.5(3) . . ?
C4 C3 C2 110.3(4) 2_576 . ?
C4 C3 K1 81.6(3) 2_576 . ?
C2 C3 K1 71.7(3) . . ?
C3 C4 C24 106.8(4) 2_576 . ?
C3 C4 C11 122.9(4) 2_576 . ?
C24 C4 C11 129.9(4) . . ?
C3 C4 K1 73.5(3) 2_576 2_576 ?
C24 C4 K1 73.7(3) . 2_576 ?
C11 C4 K1 123.9(3) . 2_576 ?
C6 C5 C10 117.2(4) . . ?
C6 C5 C2 122.3(4) . . ?
C10 C5 C2 120.4(4) . . ?
C7 C6 C5 122.1(4) . . ?
C6 C7 C8 119.9(5) . . ?
C9 C8 C7 119.3(5) . . ?
C8 C9 C10 120.6(5) . . ?
C9 C10 C5 120.9(5) . . ?
C12 C11 C16 118.2(4) . . ?
C12 C11 C4 121.5(4) . . ?
C16 C11 C4 120.1(4) . . ?
C12 C11 K1 79.2(2) . . ?
C16 C11 K1 78.6(2) . . ?
C4 C11 K1 115.3(3) . . ?
C11 C12 C13 120.7(4) . . ?
C11 C12 K1 75.5(2) . . ?
C13 C12 K1 80.2(3) . . ?
C14 C13 C12 120.3(5) . . ?
C14 C13 K1 79.8(3) . . ?
C12 C13 K1 74.9(3) . . ?
C13 C14 C15 119.6(5) . . ?
C13 C14 K1 76.1(3) . . ?
C15 C14 K1 76.3(3) . . ?
C14 C15 C16 120.4(5) . . ?
C14 C15 K1 79.4(3) . . ?
C16 C15 K1 74.1(3) . . ?
C15 C16 C11 120.8(5) . . ?
C15 C16 K1 81.2(3) . . ?
C11 C16 K1 76.0(2) . . ?
C18 C17 C22 120.8(5) . . ?
C18 C17 K1 130.0(4) . . ?
C22 C17 K1 78.4(3) . . ?
C19 C18 C17 120.2(5) . . ?
C18 C19 C20 119.4(5) . . ?
C19 C20 C21 120.4(5) . . ?
C22 C21 C20 121.0(4) . . ?
C21 C22 C17 118.1(4) . . ?
C21 C22 N1 122.9(4) . . ?
C17 C22 N1 118.6(4) . . ?
C21 C22 K1 129.8(3) . . ?
C17 C22 K1 76.7(3) . . ?
N1 C22 K1 60.4(2) . . ?
N1 C23 C24 120.1(4) . . ?
N1 C23 C25 122.5(4) . . ?
C24 C23 C25 117.4(4) . . ?
C1 C24 C4 107.8(4) . . ?
C1 C24 C23 124.7(4) . . ?
C4 C24 C23 127.4(4) . . ?
C1 C24 K1 70.7(3) . 2_576 ?
C4 C24 K1 80.7(3) . 2_576 ?
C23 C24 K1 112.7(3) . 2_576 ?
C30 C25 C26 118.4(4) . . ?
C30 C25 C23 121.9(4) . . ?
C26 C25 C23 119.7(4) . . ?
C27 C26 C25 120.3(4) . . ?
C28 C27 C26 120.6(5) . . ?
C27 C28 C29 119.8(5) . . ?
C30 C29 C28 119.5(5) . . ?
C29 C30 C25 121.4(5) . . ?
O1 C31 C32 105.6(4) . . ?
C33 C32 C31 102.5(5) . . ?
C34 C33 C32 102.3(5) . . ?
O1 C34 C33 107.4(4) . . ?
C23 N1 C22 121.4(4) . . ?
C23 N1 K1 144.6(3) . . ?
C22 N1 K1 93.6(3) . . ?
O1 K1 N1 109.93(12) . . ?
O1 K1 C1 109.19(12) . 2_576 ?
N1 K1 C1 130.89(13) . 2_576 ?
O1 K1 C2 97.24(12) . . ?
N1 K1 C2 119.38(12) . . ?
C1 K1 C2 26.89(10) 2_576 . ?
O1 K1 C11 117.73(12) . . ?
N1 K1 C11 62.75(11) . . ?
C1 K1 C11 120.01(11) 2_576 . ?
C2 K1 C11 142.57(12) . . ?
O1 K1 C3 113.82(11) . . ?
N1 K1 C3 93.79(11) . . ?
C1 K1 C3 42.88(11) 2_576 . ?
C2 K1 C3 26.23(11) . . ?
C11 K1 C3 127.96(12) . . ?
O1 K1 C16 120.39(12) . . ?
N1 K1 C16 86.50(11) . . ?
C1 K1 C16 98.28(11) 2_576 . ?
C2 K1 C16 124.34(12) . . ?
C11 K1 C16 25.40(10) . . ?
C3 K1 C16 121.96(12) . . ?
O1 K1 C24 135.50(11) . 2_576 ?
N1 K1 C24 108.47(12) . 2_576 ?
C1 K1 C24 26.34(11) 2_576 2_576 ?
C2 K1 C24 43.24(12) . 2_576 ?
C11 K1 C24 99.37(12) . 2_576 ?
C3 K1 C24 41.80(11) . 2_576 ?
C16 K1 C24 83.34(12) . 2_576 ?
O1 K1 C12 93.57(11) . . ?
N1 K1 C12 61.50(12) . . ?
C1 K1 C12 142.24(11) 2_576 . ?
C2 K1 C12 167.72(12) . . ?
C11 K1 C12 25.33(10) . . ?
C3 K1 C12 148.78(12) . . ?
C16 K1 C12 44.01(11) . . ?
C24 K1 C12 124.52(12) 2_576 . ?
O1 K1 C17 80.15(12) . . ?
N1 K1 C17 46.77(11) . . ?
C1 K1 C17 114.90(12) 2_576 . ?
C2 K1 C17 89.54(12) . . ?
C11 K1 C17 108.27(12) . . ?
C3 K1 C17 73.62(12) . . ?
C16 K1 C17 133.05(12) . . ?
C24 K1 C17 112.07(12) 2_576 . ?
C12 K1 C17 98.05(12) . . ?
O1 K1 C22 86.99(11) . . ?
N1 K1 C22 25.99(10) . . ?
C1 K1 C22 135.25(13) 2_576 . ?
C2 K1 C22 112.66(12) . . ?
C11 K1 C22 83.77(11) . . ?
C3 K1 C22 92.38(12) . . ?
C16 K1 C22 109.02(11) . . ?
C24 K1 C22 122.61(12) 2_576 . ?
C12 K1 C22 73.61(11) . . ?
C17 K1 C22 24.99(10) . . ?
O1 K1 C13 74.05(11) . . ?
N1 K1 C13 83.26(12) . . ?
C1 K1 C13 135.94(12) 2_576 . ?
C2 K1 C13 157.32(13) . . ?
C11 K1 C13 44.29(12) . . ?
C3 K1 C13 172.12(12) . . ?
C16 K1 C13 50.71(12) . . ?
C24 K1 C13 132.46(12) 2_576 . ?
C12 K1 C13 24.87(11) . . ?
C17 K1 C13 108.98(13) . . ?
C22 K1 C13 88.15(12) . . ?
C34 O1 C31 108.4(4) . . ?
C34 O1 K1 128.6(3) . . ?
C31 O1 K1 120.2(3) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        25.74
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.050

# Attachment 'k754m.cif'

data_k754m
_database_code_depnum_ccdc_archive 'CCDC 782980'
#TrackingRef 'k754m.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H25 N O'
_chemical_formula_weight         427.52

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                   10.0630(8)
_cell_length_b                   15.9800(13)
_cell_length_c                   13.9950(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.129(7)
_cell_angle_gamma                90.00
_cell_volume                     2247.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    all
_cell_measurement_2theta_min     2.92
_cell_measurement_2theta_max     51.96

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             904
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  STOE-IPDSII
_diffrn_measurement_method       Omega-Scan
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27913
_diffrn_reflns_av_R_equivalents  0.1170
_diffrn_reflns_av_sigmaI/netI    0.0972
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         25.70
_reflns_number_total             4256
_reflns_number_gt                2494
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       X-AREA-STOE
_computing_cell_refinement       X-AREA-STOE
_computing_data_reduction        X-AREA-STOE
_computing_structure_solution    SIR-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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^)+(0.0298P)^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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4256
_refine_ls_number_parameters     303
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0534
_refine_ls_wR_factor_ref         0.0880
_refine_ls_wR_factor_gt          0.0751
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_restrained_S_all      0.908
_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
C1 C 0.1692(2) 0.27216(14) 0.91388(15) 0.0249(5) Uani 1 1 d . . .
C2 C 0.2651(2) 0.21050(13) 0.91606(14) 0.0242(5) Uani 1 1 d . . .
C3 C 0.3778(2) 0.20640(13) 0.98427(15) 0.0249(5) Uani 1 1 d . . .
H3 H 0.3889 0.2388 1.0411 0.030 Uiso 1 1 calc R . .
C4 C 0.4656(2) 0.14869(13) 0.95410(15) 0.0238(5) Uani 1 1 d . . .
C5 C 0.4069(2) 0.11110(14) 0.86730(15) 0.0263(5) Uani 1 1 d . . .
H5 H 0.4461 0.0673 0.8326 0.032 Uiso 1 1 calc R . .
C6 C 0.2877(2) 0.14769(14) 0.84283(15) 0.0247(5) Uani 1 1 d . . .
C7 C 0.1933(2) 0.12184(14) 0.76433(15) 0.0257(5) Uani 1 1 d . . .
C8 C 0.0584(2) 0.11079(14) 0.77926(17) 0.0320(6) Uani 1 1 d . . .
H8 H 0.0273 0.1192 0.8414 0.038 Uiso 1 1 calc R . .
C9 C -0.0302(2) 0.08788(15) 0.70553(18) 0.0385(6) Uani 1 1 d . . .
H9 H -0.1218 0.0814 0.7171 0.046 Uiso 1 1 calc R . .
C10 C 0.0129(3) 0.07421(15) 0.61491(19) 0.0395(6) Uani 1 1 d . . .
H10 H -0.0488 0.0591 0.5640 0.047 Uiso 1 1 calc R . .
C11 C 0.1464(3) 0.08270(15) 0.59870(17) 0.0352(6) Uani 1 1 d . . .
H11 H 0.1769 0.0726 0.5367 0.042 Uiso 1 1 calc R . .
C12 C 0.2357(2) 0.10591(13) 0.67259(15) 0.0290(6) Uani 1 1 d . . .
H12 H 0.3274 0.1111 0.6608 0.035 Uiso 1 1 calc R . .
C13 C 0.5983(2) 0.12805(14) 0.99712(14) 0.0242(5) Uani 1 1 d . . .
C14 C 0.6619(2) 0.05359(15) 0.97574(16) 0.0330(6) Uani 1 1 d . . .
H14 H 0.6182 0.0148 0.9332 0.040 Uiso 1 1 calc R . .
C15 C 0.7879(2) 0.03489(17) 1.01539(17) 0.0391(7) Uani 1 1 d . . .
H15 H 0.8293 -0.0166 1.0004 0.047 Uiso 1 1 calc R . .
C16 C 0.8530(2) 0.09074(16) 1.07635(17) 0.0372(6) Uani 1 1 d . . .
H16 H 0.9397 0.0784 1.1029 0.045 Uiso 1 1 calc R . .
C17 C 0.7918(2) 0.16462(15) 1.09868(16) 0.0327(6) Uani 1 1 d . . .
H17 H 0.8364 0.2031 1.1411 0.039 Uiso 1 1 calc R . .
C18 C 0.6664(2) 0.18325(14) 1.06006(15) 0.0266(5) Uani 1 1 d . . .
H18 H 0.6254 0.2345 1.0765 0.032 Uiso 1 1 calc R . .
C19 C -0.0342(2) 0.31906(14) 0.81917(15) 0.0249(5) Uani 1 1 d . . .
C20 C -0.0742(2) 0.36527(13) 0.73898(15) 0.0264(5) Uani 1 1 d . . .
H20 H -0.0104 0.3829 0.6956 0.032 Uiso 1 1 calc R . .
C21 C -0.2060(2) 0.38563(13) 0.72196(15) 0.0270(5) Uani 1 1 d . . .
H21 H -0.2328 0.4170 0.6665 0.032 Uiso 1 1 calc R . .
C22 C -0.3005(2) 0.36085(13) 0.78500(15) 0.0249(5) Uani 1 1 d . . .
C23 C -0.2609(2) 0.31505(13) 0.86524(15) 0.0260(5) Uani 1 1 d . . .
H23 H -0.3245 0.2984 0.9092 0.031 Uiso 1 1 calc R . .
C24 C -0.1281(2) 0.29333(14) 0.88163(15) 0.0266(5) Uani 1 1 d . . .
H24 H -0.1015 0.2606 0.9360 0.032 Uiso 1 1 calc R . .
C25 C -0.5285(2) 0.36155(16) 0.82439(16) 0.0351(6) Uani 1 1 d . . .
H25A H -0.5350 0.3005 0.8281 0.053 Uiso 1 1 calc R . .
H25B H -0.6144 0.3847 0.8009 0.053 Uiso 1 1 calc R . .
H25C H -0.5047 0.3842 0.8881 0.053 Uiso 1 1 calc R . .
C26 C 0.1455(2) 0.32347(13) 1.00008(15) 0.0238(5) Uani 1 1 d . . .
C27 C 0.1416(2) 0.40990(14) 0.99366(16) 0.0285(5) Uani 1 1 d . . .
H27 H 0.1487 0.4362 0.9333 0.034 Uiso 1 1 calc R . .
C28 C 0.1275(2) 0.45821(14) 1.07431(17) 0.0299(6) Uani 1 1 d . . .
H28 H 0.1270 0.5175 1.0698 0.036 Uiso 1 1 calc R . .
C29 C 0.1141(2) 0.41957(15) 1.16164(17) 0.0300(6) Uani 1 1 d . . .
H29 H 0.1039 0.4525 1.2173 0.036 Uiso 1 1 calc R . .
C30 C 0.1155(2) 0.33400(15) 1.16844(16) 0.0296(6) Uani 1 1 d . . .
H30 H 0.1048 0.3079 1.2285 0.036 Uiso 1 1 calc R . .
C31 C 0.1322(2) 0.28553(14) 1.08827(15) 0.0283(5) Uani 1 1 d . . .
H31 H 0.1346 0.2263 1.0935 0.034 Uiso 1 1 calc R . .
N1 N 0.10157(19) 0.29449(13) 0.83084(14) 0.0278(5) Uani 1 1 d . . .
O1 O -0.42841(14) 0.38384(10) 0.76029(11) 0.0335(4) Uani 1 1 d . . .
H1N H 0.130(2) 0.2720(13) 0.7792(16) 0.028(7) 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
C1 0.0224(12) 0.0274(13) 0.0250(12) 0.0023(10) 0.0027(10) -0.0023(10)
C2 0.0229(12) 0.0263(12) 0.0237(12) 0.0012(10) 0.0033(10) 0.0014(11)
C3 0.0256(12) 0.0274(13) 0.0217(11) 0.0005(10) 0.0028(10) -0.0006(11)
C4 0.0232(12) 0.0246(13) 0.0237(11) 0.0013(10) 0.0020(10) -0.0002(10)
C5 0.0238(12) 0.0297(14) 0.0259(12) -0.0010(10) 0.0061(10) 0.0038(11)
C6 0.0250(13) 0.0252(13) 0.0243(12) -0.0001(9) 0.0046(10) -0.0002(10)
C7 0.0253(12) 0.0238(12) 0.0277(12) -0.0018(10) -0.0020(10) 0.0046(11)
C8 0.0236(13) 0.0352(15) 0.0375(14) -0.0054(11) 0.0041(11) 0.0000(11)
C9 0.0220(13) 0.0394(15) 0.0535(17) -0.0056(13) -0.0047(12) -0.0017(12)
C10 0.0402(16) 0.0346(15) 0.0418(16) -0.0055(12) -0.0150(13) 0.0019(13)
C11 0.0413(16) 0.0342(14) 0.0296(14) -0.0018(11) -0.0026(12) 0.0034(12)
C12 0.0261(13) 0.0282(14) 0.0324(13) -0.0035(10) 0.0001(11) 0.0034(11)
C13 0.0259(12) 0.0274(13) 0.0195(11) 0.0035(10) 0.0041(9) -0.0016(11)
C14 0.0309(14) 0.0352(15) 0.0324(14) -0.0041(11) -0.0022(11) 0.0046(12)
C15 0.0297(15) 0.0445(16) 0.0426(16) -0.0019(13) -0.0021(13) 0.0129(12)
C16 0.0229(13) 0.0497(17) 0.0385(15) 0.0025(13) -0.0039(11) 0.0041(12)
C17 0.0308(14) 0.0403(15) 0.0266(13) -0.0004(11) -0.0019(11) -0.0055(12)
C18 0.0254(13) 0.0291(13) 0.0255(12) 0.0029(10) 0.0036(10) -0.0001(10)
C19 0.0232(13) 0.0277(13) 0.0237(12) -0.0032(10) -0.0005(10) 0.0027(10)
C20 0.0262(13) 0.0273(13) 0.0259(12) 0.0009(10) 0.0022(10) -0.0008(11)
C21 0.0304(13) 0.0268(13) 0.0235(12) 0.0036(10) -0.0006(10) 0.0009(11)
C22 0.0233(12) 0.0259(13) 0.0251(12) -0.0010(10) -0.0028(10) 0.0005(10)
C23 0.0258(13) 0.0278(13) 0.0247(12) 0.0016(10) 0.0031(10) -0.0023(10)
C24 0.0283(13) 0.0287(13) 0.0225(12) 0.0039(10) -0.0006(10) 0.0027(11)
C25 0.0239(13) 0.0466(16) 0.0351(14) 0.0015(12) 0.0034(11) 0.0021(12)
C26 0.0161(12) 0.0267(13) 0.0284(13) 0.0013(10) -0.0003(10) 0.0026(10)
C27 0.0233(13) 0.0315(13) 0.0306(13) 0.0013(11) 0.0006(10) 0.0006(11)
C28 0.0229(13) 0.0257(13) 0.0407(15) -0.0027(11) -0.0025(11) 0.0017(11)
C29 0.0216(13) 0.0359(15) 0.0327(14) -0.0089(12) 0.0030(11) 0.0019(11)
C30 0.0272(13) 0.0344(15) 0.0275(13) 0.0009(11) 0.0037(10) 0.0025(11)
C31 0.0273(13) 0.0261(13) 0.0316(13) 0.0004(11) 0.0024(10) 0.0036(11)
N1 0.0248(11) 0.0363(12) 0.0227(11) -0.0012(9) 0.0033(9) 0.0061(9)
O1 0.0243(9) 0.0422(10) 0.0338(9) 0.0066(8) -0.0001(7) 0.0017(8)

_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
C1 N1 1.362(3) . ?
C1 C2 1.378(3) . ?
C1 C26 1.489(3) . ?
C2 C3 1.444(3) . ?
C2 C6 1.461(3) . ?
C3 C4 1.360(3) . ?
C4 C5 1.451(3) . ?
C4 C13 1.472(3) . ?
C5 C6 1.362(3) . ?
C6 C7 1.472(3) . ?
C7 C8 1.395(3) . ?
C7 C12 1.398(3) . ?
C8 C9 1.376(3) . ?
C9 C10 1.380(3) . ?
C10 C11 1.381(4) . ?
C11 C12 1.383(3) . ?
C13 C14 1.391(3) . ?
C13 C18 1.399(3) . ?
C14 C15 1.389(3) . ?
C15 C16 1.376(3) . ?
C16 C17 1.375(3) . ?
C17 C18 1.378(3) . ?
C19 C24 1.385(3) . ?
C19 C20 1.385(3) . ?
C19 N1 1.422(3) . ?
C20 C21 1.373(3) . ?
C21 C22 1.390(3) . ?
C22 O1 1.365(3) . ?
C22 C23 1.381(3) . ?
C23 C24 1.388(3) . ?
C25 O1 1.430(3) . ?
C26 C27 1.384(3) . ?
C26 C31 1.388(3) . ?
C27 C28 1.381(3) . ?
C28 C29 1.382(3) . ?
C29 C30 1.371(3) . ?
C30 C31 1.381(3) . ?

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
N1 C1 C2 121.5(2) . . ?
N1 C1 C26 116.89(19) . . ?
C2 C1 C26 121.26(19) . . ?
C1 C2 C3 124.81(19) . . ?
C1 C2 C6 127.67(19) . . ?
C3 C2 C6 106.62(18) . . ?
C4 C3 C2 109.01(19) . . ?
C3 C4 C5 107.41(18) . . ?
C3 C4 C13 128.0(2) . . ?
C5 C4 C13 124.61(19) . . ?
C6 C5 C4 110.20(19) . . ?
C5 C6 C2 106.69(19) . . ?
C5 C6 C7 126.2(2) . . ?
C2 C6 C7 126.71(19) . . ?
C8 C7 C12 117.56(19) . . ?
C8 C7 C6 121.13(19) . . ?
C12 C7 C6 121.3(2) . . ?
C9 C8 C7 121.1(2) . . ?
C8 C9 C10 120.5(2) . . ?
C9 C10 C11 119.5(2) . . ?
C10 C11 C12 120.1(2) . . ?
C11 C12 C7 121.1(2) . . ?
C14 C13 C18 117.3(2) . . ?
C14 C13 C4 121.42(19) . . ?
C18 C13 C4 121.2(2) . . ?
C15 C14 C13 121.2(2) . . ?
C16 C15 C14 120.1(2) . . ?
C17 C16 C15 119.6(2) . . ?
C16 C17 C18 120.5(2) . . ?
C17 C18 C13 121.2(2) . . ?
C24 C19 C20 119.4(2) . . ?
C24 C19 N1 122.01(19) . . ?
C20 C19 N1 118.4(2) . . ?
C21 C20 C19 120.2(2) . . ?
C20 C21 C22 120.7(2) . . ?
O1 C22 C23 125.1(2) . . ?
O1 C22 C21 115.54(18) . . ?
C23 C22 C21 119.4(2) . . ?
C22 C23 C24 120.0(2) . . ?
C19 C24 C23 120.4(2) . . ?
C27 C26 C31 119.3(2) . . ?
C27 C26 C1 120.1(2) . . ?
C31 C26 C1 120.5(2) . . ?
C28 C27 C26 120.6(2) . . ?
C27 C28 C29 119.5(2) . . ?
C30 C29 C28 120.4(2) . . ?
C29 C30 C31 120.3(2) . . ?
C30 C31 C26 120.0(2) . . ?
C1 N1 C19 127.1(2) . . ?
C22 O1 C25 117.45(17) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.70
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.170
_refine_diff_density_min         -0.134
_refine_diff_density_rms         0.036