# Supplementary Material (ESI) for ChemComm
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 182/1759

data_s91
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C26 H31 N2 O3'
_chemical_formula_weight          419.53
 
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                    9.4057(6)
_cell_length_b                    13.8445(11)
_cell_length_c                    18.9676(14)
_cell_angle_alpha                 92.243(4)
_cell_angle_beta                  99.513(4)
_cell_angle_gamma                 103.536(4)
_cell_volume                      2360.5(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used     na
_cell_measurement_theta_min       na
_cell_measurement_theta_max       na
 
_exptl_crystal_description        ?
_exptl_crystal_colour             ?
_exptl_crystal_size_max           0.10
_exptl_crystal_size_mid           0.10
_exptl_crystal_size_min           0.05
_exptl_crystal_density_meas       'not measured'
_exptl_crystal_density_diffrn     1.181
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              900
_exptl_absorpt_coefficient_mu     0.077
_exptl_absorpt_correction_type    'Empirical, SORTAV'
_exptl_absorpt_correction_T_min   0.9923
_exptl_absorpt_correction_T_max   0.9962
_exptl_absorpt_process_details    ?
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Nonius FR591 Rotating Anode'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Enraf Nonius KappaCCD area detector'
_diffrn_measurement_method        'Phi and Omega scans to fill Ewald sphere'
_diffrn_detector_area_resol_mean  '9.091 pixels/mm'
_diffrn_standards_number          'not measured'
_diffrn_standards_interval_count  na
_diffrn_standards_interval_time   na
_diffrn_standards_decay_%         na
_diffrn_reflns_number             12951
_diffrn_reflns_av_R_equivalents   0.0629
_diffrn_reflns_av_sigmaI/netI     0.0950
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          3.02
_diffrn_reflns_theta_max          21.97
_reflns_number_total              5590
_reflns_number_gt                 3391
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection
;
DENZO and COLLECT
;
_computing_cell_refinement        'DENZO and COLLECT'
_computing_data_reduction         'DENZO and COLLECT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ORTEP
_computing_publication_material   CIFTAB
 
_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^)+(0.0906P)^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        0.0085(17)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          5590
_refine_ls_number_parameters      564
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1129
_refine_ls_R_factor_gt            0.0621
_refine_ls_wR_factor_ref          0.1803
_refine_ls_wR_factor_gt           0.1511
_refine_ls_goodness_of_fit_ref    1.011
_refine_ls_restrained_S_all       1.011
_refine_ls_shift/su_max           0.009
_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
O2B O 0.4740(3) 0.63958(19) 0.06531(12) 0.0386(7) Uani 1 1 d . . .
O1B O 0.5690(3) 0.5288(2) 0.12936(13) 0.0461(7) Uani 1 1 d . . .
N1B N 0.7595(3) 0.4369(2) 0.04800(14) 0.0339(8) Uani 1 1 d . . .
N2B N 0.9346(3) 0.5646(2) 0.09959(15) 0.0368(8) Uani 1 1 d . . .
C19B C 0.5723(4) 0.5940(3) 0.07714(18) 0.0348(10) Uani 1 1 d . . .
O3B O 0.8577(3) 0.6703(2) -0.03088(14) 0.0522(8) Uani 1 1 d . . .
C20B C 0.6986(4) 0.6010(3) 0.04413(17) 0.0325(9) Uani 1 1 d . . .
C9B C 0.7957(4) 0.5353(3) 0.06448(17) 0.0339(10) Uani 1 1 d . . .
C22B C 0.6454(4) 0.7365(3) -0.03775(18) 0.0380(10) Uani 1 1 d . . .
H22A H 0.6362 0.7819 0.0020 0.046 Uiso 1 1 calc R . .
H22B H 0.5444 0.6960 -0.0585 0.046 Uiso 1 1 calc R . .
C10B C 1.0127(4) 0.6664(3) 0.12578(19) 0.0421(10) Uani 1 1 d . . .
H10A H 0.9404 0.7082 0.1253 0.051 Uiso 1 1 calc R . .
H10B H 1.0829 0.6939 0.0939 0.051 Uiso 1 1 calc R . .
C7B C 0.8784(4) 0.3900(3) 0.07817(18) 0.0360(10) Uani 1 1 d . . .
H7B H 0.9011 0.3476 0.0397 0.043 Uiso 1 1 calc R . .
C21B C 0.7397(4) 0.6682(3) -0.00808(18) 0.0365(10) Uani 1 1 d . . .
C6B C 0.8429(4) 0.3288(3) 0.13970(19) 0.0359(10) Uani 1 1 d . . .
C8B C 1.0094(4) 0.4835(3) 0.10086(19) 0.0360(10) Uani 1 1 d . . .
H8B1 H 1.0646 0.4797 0.1495 0.043 Uiso 1 1 calc R . .
H8B2 H 1.0792 0.4914 0.0665 0.043 Uiso 1 1 calc R . .
C24B C 0.6298(4) 0.8795(3) -0.11768(19) 0.0465(11) Uani 1 1 d . . .
H24A H 0.6579 0.9029 -0.1633 0.056 Uiso 1 1 calc R . .
H24B H 0.5211 0.8505 -0.1269 0.056 Uiso 1 1 calc R . .
C1B C 0.9088(4) 0.2508(3) 0.1535(2) 0.0508(12) Uani 1 1 d . . .
H1B H 0.9696 0.2335 0.1222 0.061 Uiso 1 1 calc R . .
C3B C 0.8008(5) 0.2230(4) 0.2588(2) 0.0578(13) Uani 1 1 d . . .
H3B H 0.7885 0.1879 0.3003 0.069 Uiso 1 1 calc R . .
C5B C 0.7537(4) 0.3527(3) 0.1857(2) 0.0471(11) Uani 1 1 d . . .
H5B H 0.7070 0.4059 0.1767 0.057 Uiso 1 1 calc R . .
C2B C 0.8873(5) 0.1977(3) 0.2124(2) 0.0601(13) Uani 1 1 d . . .
H2B H 0.9321 0.1435 0.2211 0.072 Uiso 1 1 calc R . .
C23B C 0.7084(4) 0.7982(3) -0.09493(19) 0.0453(11) Uani 1 1 d . . .
H23A H 0.7024 0.7531 -0.1377 0.054 Uiso 1 1 calc R . .
H23B H 0.8148 0.8295 -0.0767 0.054 Uiso 1 1 calc R . .
C26B C 0.6100(4) 1.0572(3) -0.0871(2) 0.0502(11) Uani 1 1 d . . .
H26A H 0.5000 1.0389 -0.0957 0.060 Uiso 1 1 calc R . .
H26B H 0.6415 1.0746 -0.1332 0.060 Uiso 1 1 calc R . .
C11B C 1.0963(4) 0.6690(3) 0.2007(2) 0.0425(11) Uani 1 1 d . . .
C4B C 0.7329(5) 0.2989(4) 0.2447(2) 0.0542(12) Uani 1 1 d . . .
H4B H 0.6707 0.3150 0.2757 0.065 Uiso 1 1 calc R . .
C25B C 0.6657(4) 0.9681(3) -0.06285(19) 0.0422(10) Uani 1 1 d . . .
H25A H 0.6234 0.9460 -0.0201 0.051 Uiso 1 1 calc R . .
H25B H 0.7750 0.9895 -0.0479 0.051 Uiso 1 1 calc R . .
C17B C 0.4420(4) 0.5122(4) 0.1638(2) 0.0564(12) Uani 1 1 d . . .
H17A H 0.4387 0.5748 0.1888 0.085 Uiso 1 1 calc R . .
H17B H 0.4490 0.4621 0.1985 0.085 Uiso 1 1 calc R . .
H17C H 0.3514 0.4884 0.1278 0.085 Uiso 1 1 calc R . .
C12B C 1.0241(5) 0.6284(3) 0.2543(2) 0.0540(12) Uani 1 1 d . . .
H12B H 0.9198 0.6007 0.2442 0.065 Uiso 1 1 calc R . .
C27B C 0.6661(5) 1.1480(3) -0.0336(2) 0.0633(13) Uani 1 1 d . . .
H27A H 0.6336 1.1319 0.0120 0.095 Uiso 1 1 calc R . .
H27B H 0.6259 1.2030 -0.0523 0.095 Uiso 1 1 calc R . .
H27C H 0.7749 1.1678 -0.0258 0.095 Uiso 1 1 calc R . .
C14B C 1.2553(8) 0.6688(4) 0.3367(3) 0.0838(18) Uani 1 1 d . . .
H14B H 1.3105 0.6678 0.3833 0.101 Uiso 1 1 calc R . .
C13B C 1.1033(7) 0.6278(4) 0.3232(2) 0.0733(15) Uani 1 1 d . . .
H13B H 1.0540 0.5998 0.3601 0.088 Uiso 1 1 calc R . .
C16B C 1.2475(5) 0.7104(3) 0.2173(2) 0.0575(13) Uani 1 1 d . . .
H16B H 1.2983 0.7398 0.1812 0.069 Uiso 1 1 calc R . .
C15B C 1.3261(6) 0.7100(4) 0.2851(3) 0.0791(17) Uani 1 1 d . . .
H15B H 1.4301 0.7388 0.2955 0.095 Uiso 1 1 calc R . .
O2A O 0.5355(3) 0.8806(2) 0.41699(12) 0.0417(7) Uani 1 1 d . . .
O1A O 0.4260(3) 0.9884(2) 0.35697(13) 0.0458(7) Uani 1 1 d . . .
N2A N 0.0823(3) 0.9577(2) 0.38991(15) 0.0398(8) Uani 1 1 d . . .
N1A N 0.2451(3) 1.0728(2) 0.46254(15) 0.0385(8) Uani 1 1 d . . .
C20A C 0.3128(4) 0.9137(3) 0.44621(18) 0.0345(10) Uani 1 1 d . . .
O3A O 0.1637(3) 0.8448(2) 0.52564(15) 0.0586(8) Uani 1 1 d . . .
C19A C 0.4333(4) 0.9230(3) 0.40926(19) 0.0365(10) Uani 1 1 d . . .
C7A C 0.1260(4) 1.1233(3) 0.43893(18) 0.0370(10) Uani 1 1 d . . .
H7A H 0.0902 1.1468 0.4818 0.044 Uiso 1 1 calc R . .
C9A C 0.2141(4) 0.9803(3) 0.43210(18) 0.0348(10) Uani 1 1 d . . .
C21A C 0.2757(4) 0.8449(3) 0.49842(19) 0.0394(10) Uani 1 1 d . . .
C8A C 0.0032(4) 1.0357(3) 0.39581(19) 0.0393(10) Uani 1 1 d . . .
H8A1 H -0.0802 1.0144 0.4220 0.047 Uiso 1 1 calc R . .
H8A2 H -0.0357 1.0546 0.3479 0.047 Uiso 1 1 calc R . .
C11A C -0.0437(4) 0.8773(3) 0.2715(2) 0.0430(11) Uani 1 1 d . . .
C6A C 0.1734(4) 1.2100(3) 0.39553(19) 0.0385(10) Uani 1 1 d . . .
C22A C 0.3666(4) 0.7724(3) 0.5221(2) 0.0443(11) Uani 1 1 d . . .
H22C H 0.4437 0.8035 0.5640 0.053 Uiso 1 1 calc R . .
H22D H 0.4177 0.7573 0.4829 0.053 Uiso 1 1 calc R . .
C10A C 0.0098(4) 0.8627(3) 0.34984(19) 0.0478(11) Uani 1 1 d . . .
H10C H -0.0759 0.8292 0.3713 0.057 Uiso 1 1 calc R . .
H10D H 0.0804 0.8194 0.3526 0.057 Uiso 1 1 calc R . .
C5A C 0.2637(4) 1.2057(3) 0.3451(2) 0.0502(12) Uani 1 1 d . . .
H5A H 0.3018 1.1486 0.3396 0.060 Uiso 1 1 calc R . .
C4A C 0.2982(5) 1.2836(4) 0.3032(2) 0.0631(14) Uani 1 1 d . . .
H4A H 0.3596 1.2799 0.2686 0.076 Uiso 1 1 calc R . .
C12A C -0.1899(4) 0.8379(3) 0.2400(2) 0.0525(12) Uani 1 1 d . . .
H12A H -0.2577 0.8017 0.2672 0.063 Uiso 1 1 calc R . .
C1A C 0.1189(5) 1.2929(3) 0.4029(2) 0.0547(12) Uani 1 1 d . . .
H1A H 0.0569 1.2965 0.4372 0.066 Uiso 1 1 calc R . .
C17A C 0.5467(4) 1.0073(4) 0.3187(2) 0.0600(13) Uani 1 1 d . . .
H17D H 0.6405 1.0312 0.3526 0.090 Uiso 1 1 calc R . .
H17E H 0.5343 1.0580 0.2851 0.090 Uiso 1 1 calc R . .
H17F H 0.5483 0.9456 0.2920 0.090 Uiso 1 1 calc R . .
C13A C -0.2388(5) 0.8510(4) 0.1681(2) 0.0625(14) Uani 1 1 d . . .
H13A H -0.3398 0.8238 0.1466 0.075 Uiso 1 1 calc R . .
C16A C 0.0524(5) 0.9294(3) 0.2314(2) 0.0569(13) Uani 1 1 d . . .
H16A H 0.1536 0.9567 0.2525 0.068 Uiso 1 1 calc R . .
C14A C -0.1420(6) 0.9028(4) 0.1290(2) 0.0697(15) Uani 1 1 d . . .
H14A H -0.1748 0.9113 0.0800 0.084 Uiso 1 1 calc R . .
C23A C 0.2722(5) 0.6750(4) 0.5422(2) 0.0647(13) Uani 1 1 d . . .
H23C H 0.2360 0.6889 0.5867 0.078 Uiso 1 1 calc R . .
H23D H 0.1842 0.6510 0.5037 0.078 Uiso 1 1 calc R . .
C15A C 0.0025(5) 0.9423(4) 0.1605(2) 0.0714(15) Uani 1 1 d . . .
H15A H 0.0698 0.9792 0.1334 0.086 Uiso 1 1 calc R . .
C3A C 0.2443(6) 1.3665(4) 0.3110(3) 0.0726(15) Uani 1 1 d . . .
H3A H 0.2695 1.4206 0.2823 0.087 Uiso 1 1 calc R . .
C25A C 0.2620(9) 0.5013(4) 0.5760(3) 0.124(3) Uani 1 1 d . . .
H25C H 0.1693 0.4757 0.5406 0.148 Uiso 1 1 calc R . .
H25D H 0.2352 0.5142 0.6232 0.148 Uiso 1 1 calc R . .
C2A C 0.1536(5) 1.3714(4) 0.3605(3) 0.0745(15) Uani 1 1 d . . .
H2A H 0.1151 1.4284 0.3656 0.089 Uiso 1 1 calc R . .
C24A C 0.3521(6) 0.5945(4) 0.5534(3) 0.0896(17) Uani 1 1 d . . .
H24C H 0.4425 0.6195 0.5903 0.107 Uiso 1 1 calc R . .
H24D H 0.3844 0.5784 0.5081 0.107 Uiso 1 1 calc R . .
C27A C 0.2931(8) 0.3389(7) 0.6082(4) 0.161(4) Uani 1 1 d . . .
H27D H 0.2876 0.3548 0.6583 0.241 Uiso 1 1 calc R . .
H27E H 0.3484 0.2874 0.6056 0.241 Uiso 1 1 calc R . .
H27F H 0.1925 0.3145 0.5804 0.241 Uiso 1 1 calc R . .
C26A C 0.3633(9) 0.4215(7) 0.5810(4) 0.143(3) Uani 1 1 d . . .
H26C H 0.3813 0.4041 0.5327 0.171 Uiso 1 1 calc R . .
H26D H 0.4606 0.4508 0.6122 0.171 Uiso 1 1 calc R . .
 
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
O2B 0.0361(15) 0.0384(17) 0.0408(15) 0.0016(12) -0.0018(11) 0.0146(13)
O1B 0.0457(16) 0.055(2) 0.0475(16) 0.0207(15) 0.0161(13) 0.0243(14)
N1B 0.0355(18) 0.030(2) 0.0379(17) 0.0044(15) 0.0042(13) 0.0125(15)
N2B 0.0347(18) 0.031(2) 0.0425(18) 0.0038(15) -0.0005(14) 0.0097(16)
C19B 0.033(2) 0.035(3) 0.032(2) 0.0002(19) -0.0037(18) 0.009(2)
O3B 0.0542(18) 0.057(2) 0.0586(18) 0.0249(14) 0.0210(14) 0.0286(15)
C20B 0.034(2) 0.034(2) 0.031(2) 0.0044(18) 0.0031(17) 0.0146(18)
C9B 0.037(2) 0.042(3) 0.025(2) 0.0083(18) 0.0058(17) 0.015(2)
C22B 0.042(2) 0.032(2) 0.040(2) 0.0061(18) 0.0007(17) 0.0117(19)
C10B 0.046(2) 0.030(3) 0.048(2) 0.0078(19) 0.0019(18) 0.0084(19)
C7B 0.037(2) 0.034(3) 0.038(2) 0.0052(18) 0.0027(17) 0.0147(19)
C21B 0.037(2) 0.035(3) 0.038(2) 0.0023(19) 0.0054(18) 0.0128(19)
C6B 0.032(2) 0.033(3) 0.041(2) 0.0046(19) -0.0007(18) 0.0100(19)
C8B 0.032(2) 0.039(3) 0.038(2) 0.0076(18) 0.0031(16) 0.0132(19)
C24B 0.060(3) 0.044(3) 0.039(2) 0.014(2) 0.0078(19) 0.018(2)
C1B 0.053(3) 0.052(3) 0.051(3) 0.013(2) 0.009(2) 0.019(2)
C3B 0.054(3) 0.060(3) 0.055(3) 0.029(2) 0.005(2) 0.003(3)
C5B 0.045(2) 0.048(3) 0.051(3) 0.016(2) 0.007(2) 0.016(2)
C2B 0.072(3) 0.050(3) 0.065(3) 0.025(3) 0.010(3) 0.026(3)
C23B 0.066(3) 0.039(3) 0.037(2) 0.0107(19) 0.0112(19) 0.022(2)
C26B 0.056(3) 0.042(3) 0.059(3) 0.013(2) 0.013(2) 0.021(2)
C11B 0.043(2) 0.032(3) 0.046(2) -0.0018(19) -0.006(2) 0.008(2)
C4B 0.055(3) 0.061(3) 0.051(3) 0.022(2) 0.012(2) 0.017(2)
C25B 0.044(2) 0.042(3) 0.045(2) 0.008(2) 0.0095(18) 0.016(2)
C17B 0.059(3) 0.065(3) 0.062(3) 0.023(2) 0.031(2) 0.031(2)
C12B 0.078(3) 0.036(3) 0.050(3) 0.003(2) 0.012(2) 0.018(2)
C27B 0.074(3) 0.041(3) 0.082(3) 0.011(2) 0.022(3) 0.021(2)
C14B 0.125(5) 0.066(4) 0.059(4) -0.020(3) -0.028(4) 0.055(4)
C13B 0.133(5) 0.050(3) 0.044(3) 0.003(2) 0.016(3) 0.036(3)
C16B 0.058(3) 0.043(3) 0.063(3) -0.009(2) -0.012(2) 0.013(2)
C15B 0.078(4) 0.072(4) 0.075(4) -0.022(3) -0.026(3) 0.025(3)
O2A 0.0359(15) 0.0471(19) 0.0413(15) -0.0013(13) -0.0029(12) 0.0159(14)
O1A 0.0440(16) 0.050(2) 0.0458(16) 0.0146(14) 0.0056(13) 0.0159(14)
N2A 0.0394(19) 0.034(2) 0.0425(19) -0.0005(15) -0.0056(15) 0.0112(16)
N1A 0.0413(19) 0.033(2) 0.0419(18) 0.0035(16) 0.0024(14) 0.0140(16)
C20A 0.032(2) 0.034(3) 0.037(2) 0.0016(19) -0.0015(17) 0.0116(18)
O3A 0.0563(19) 0.059(2) 0.073(2) 0.0275(16) 0.0240(16) 0.0262(16)
C19A 0.034(2) 0.037(3) 0.034(2) -0.005(2) -0.0089(18) 0.010(2)
C7A 0.044(2) 0.032(2) 0.037(2) 0.0057(18) 0.0057(17) 0.0130(19)
C9A 0.035(2) 0.038(3) 0.030(2) 0.0068(18) -0.0005(17) 0.0103(19)
C21A 0.036(2) 0.040(3) 0.041(2) -0.001(2) 0.0022(18) 0.010(2)
C8A 0.035(2) 0.037(3) 0.045(2) 0.0059(18) -0.0007(17) 0.0131(19)
C11A 0.040(2) 0.036(3) 0.048(2) -0.008(2) -0.008(2) 0.013(2)
C6A 0.039(2) 0.035(3) 0.039(2) 0.0043(19) -0.0011(18) 0.0085(19)
C22A 0.051(2) 0.037(3) 0.046(2) 0.003(2) -0.0028(19) 0.021(2)
C10A 0.051(3) 0.030(3) 0.054(3) -0.001(2) -0.0105(19) 0.008(2)
C5A 0.049(3) 0.056(3) 0.045(2) 0.009(2) 0.001(2) 0.014(2)
C4A 0.055(3) 0.080(4) 0.052(3) 0.027(3) 0.008(2) 0.008(3)
C12A 0.049(3) 0.044(3) 0.061(3) 0.003(2) -0.003(2) 0.012(2)
C1A 0.058(3) 0.045(3) 0.064(3) 0.014(2) 0.014(2) 0.015(2)
C17A 0.051(3) 0.072(4) 0.063(3) 0.019(2) 0.020(2) 0.017(2)
C13A 0.054(3) 0.060(3) 0.063(3) -0.007(3) -0.020(2) 0.016(2)
C16A 0.048(3) 0.061(3) 0.053(3) -0.004(2) 0.001(2) 0.005(2)
C14A 0.087(4) 0.065(4) 0.048(3) -0.002(3) -0.004(3) 0.013(3)
C23A 0.086(3) 0.065(4) 0.063(3) 0.032(3) 0.033(3) 0.041(3)
C15A 0.080(4) 0.076(4) 0.052(3) -0.001(3) 0.014(3) 0.006(3)
C3A 0.066(3) 0.058(4) 0.088(4) 0.041(3) 0.004(3) 0.004(3)
C25A 0.242(8) 0.039(4) 0.095(4) 0.023(3) 0.048(5) 0.029(5)
C2A 0.075(4) 0.048(4) 0.100(4) 0.025(3) 0.012(3) 0.014(3)
C24A 0.120(5) 0.067(4) 0.078(4) 0.004(3) -0.012(3) 0.038(3)
C27A 0.123(6) 0.171(9) 0.173(8) 0.044(7) 0.039(5) -0.009(6)
C26A 0.160(7) 0.103(7) 0.144(7) 0.018(5) 0.012(5) 0.002(6)
 
_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
O2B C19B 1.232(4) . ?
O1B C19B 1.366(5) . ?
O1B C17B 1.431(4) . ?
N1B C9B 1.336(5) . ?
N1B C7B 1.469(5) . ?
N2B C9B 1.325(4) . ?
N2B C10B 1.453(4) . ?
N2B C8B 1.458(5) . ?
C19B C20B 1.418(5) . ?
O3B C21B 1.251(4) . ?
C20B C21B 1.423(5) . ?
C20B C9B 1.453(5) . ?
C22B C21B 1.506(5) . ?
C22B C23B 1.518(5) . ?
C10B C11B 1.500(5) . ?
C7B C6B 1.505(5) . ?
C7B C8B 1.554(5) . ?
C6B C1B 1.379(6) . ?
C6B C5B 1.387(5) . ?
C24B C25B 1.513(5) . ?
C24B C23B 1.524(5) . ?
C1B C2B 1.377(6) . ?
C3B C4B 1.364(6) . ?
C3B C2B 1.381(6) . ?
C5B C4B 1.383(6) . ?
C26B C25B 1.508(6) . ?
C26B C27B 1.518(5) . ?
C11B C12B 1.380(5) . ?
C11B C16B 1.381(5) . ?
C12B C13B 1.395(6) . ?
C14B C15B 1.344(7) . ?
C14B C13B 1.385(7) . ?
C16B C15B 1.374(6) . ?
O2A C19A 1.230(4) . ?
O1A C19A 1.373(5) . ?
O1A C17A 1.426(4) . ?
N2A C9A 1.321(4) . ?
N2A C10A 1.450(4) . ?
N2A C8A 1.458(5) . ?
N1A C9A 1.330(5) . ?
N1A C7A 1.472(5) . ?
C20A C19A 1.412(5) . ?
C20A C21A 1.429(5) . ?
C20A C9A 1.457(5) . ?
O3A C21A 1.247(4) . ?
C7A C6A 1.505(5) . ?
C7A C8A 1.558(5) . ?
C21A C22A 1.500(5) . ?
C11A C16A 1.371(5) . ?
C11A C12A 1.378(5) . ?
C11A C10A 1.525(5) . ?
C6A C1A 1.374(6) . ?
C6A C5A 1.388(5) . ?
C22A C23A 1.531(6) . ?
C5A C4A 1.375(6) . ?
C4A C3A 1.372(7) . ?
C12A C13A 1.398(6) . ?
C1A C2A 1.386(6) . ?
C13A C14A 1.362(6) . ?
C16A C15A 1.382(6) . ?
C14A C15A 1.365(6) . ?
C23A C24A 1.487(7) . ?
C3A C2A 1.379(6) . ?
C25A C24A 1.490(8) . ?
C25A C26A 1.615(10) . ?
C27A C26A 1.347(9) . ?
 
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
C19B O1B C17B 116.4(3) . . ?
C9B N1B C7B 112.2(3) . . ?
C9B N2B C10B 125.8(3) . . ?
C9B N2B C8B 111.3(3) . . ?
C10B N2B C8B 122.3(3) . . ?
O2B C19B O1B 119.8(3) . . ?
O2B C19B C20B 128.5(4) . . ?
O1B C19B C20B 111.7(3) . . ?
C19B C20B C21B 125.2(4) . . ?
C19B C20B C9B 118.5(3) . . ?
C21B C20B C9B 116.3(3) . . ?
N2B C9B N1B 110.2(3) . . ?
N2B C9B C20B 125.1(3) . . ?
N1B C9B C20B 124.7(3) . . ?
C21B C22B C23B 113.0(3) . . ?
N2B C10B C11B 110.2(3) . . ?
N1B C7B C6B 113.4(3) . . ?
N1B C7B C8B 100.5(3) . . ?
C6B C7B C8B 113.1(3) . . ?
O3B C21B C20B 119.1(4) . . ?
O3B C21B C22B 118.5(3) . . ?
C20B C21B C22B 122.4(3) . . ?
C1B C6B C5B 119.0(4) . . ?
C1B C6B C7B 119.0(3) . . ?
C5B C6B C7B 121.9(4) . . ?
N2B C8B C7B 102.8(3) . . ?
C25B C24B C23B 113.8(3) . . ?
C2B C1B C6B 120.5(4) . . ?
C4B C3B C2B 119.5(4) . . ?
C4B C5B C6B 120.0(4) . . ?
C1B C2B C3B 120.2(5) . . ?
C22B C23B C24B 114.4(3) . . ?
C25B C26B C27B 113.4(4) . . ?
C12B C11B C16B 118.4(4) . . ?
C12B C11B C10B 120.7(3) . . ?
C16B C11B C10B 120.9(4) . . ?
C3B C4B C5B 120.7(4) . . ?
C26B C25B C24B 115.9(3) . . ?
C11B C12B C13B 120.4(4) . . ?
C15B C14B C13B 121.1(5) . . ?
C14B C13B C12B 118.8(5) . . ?
C15B C16B C11B 121.3(5) . . ?
C14B C15B C16B 119.8(5) . . ?
C19A O1A C17A 115.9(3) . . ?
C9A N2A C10A 126.4(3) . . ?
C9A N2A C8A 111.7(3) . . ?
C10A N2A C8A 121.3(3) . . ?
C9A N1A C7A 111.9(3) . . ?
C19A C20A C21A 126.7(4) . . ?
C19A C20A C9A 118.9(4) . . ?
C21A C20A C9A 114.4(3) . . ?
O2A C19A O1A 119.2(3) . . ?
O2A C19A C20A 129.5(4) . . ?
O1A C19A C20A 111.2(4) . . ?
N1A C7A C6A 113.2(3) . . ?
N1A C7A C8A 101.3(3) . . ?
C6A C7A C8A 113.7(3) . . ?
N2A C9A N1A 110.9(3) . . ?
N2A C9A C20A 125.7(3) . . ?
N1A C9A C20A 123.3(3) . . ?
O3A C21A C20A 119.1(4) . . ?
O3A C21A C22A 118.4(4) . . ?
C20A C21A C22A 122.5(3) . . ?
N2A C8A C7A 102.7(3) . . ?
C16A C11A C12A 119.0(4) . . ?
C16A C11A C10A 120.7(3) . . ?
C12A C11A C10A 120.2(4) . . ?
C1A C6A C5A 119.2(4) . . ?
C1A C6A C7A 119.2(4) . . ?
C5A C6A C7A 121.5(4) . . ?
C21A C22A C23A 112.5(3) . . ?
N2A C10A C11A 110.7(3) . . ?
C4A C5A C6A 120.3(5) . . ?
C3A C4A C5A 120.3(4) . . ?
C11A C12A C13A 120.2(4) . . ?
C6A C1A C2A 120.5(4) . . ?
C14A C13A C12A 120.1(4) . . ?
C11A C16A C15A 120.2(4) . . ?
C13A C14A C15A 119.6(4) . . ?
C24A C23A C22A 114.2(4) . . ?
C14A C15A C16A 120.9(4) . . ?
C4A C3A C2A 119.9(5) . . ?
C24A C25A C26A 106.8(7) . . ?
C3A C2A C1A 119.8(5) . . ?
C23A C24A C25A 114.1(6) . . ?
C27A C26A C25A 109.4(8) . . ?
 
_diffrn_measured_fraction_theta_max    0.970
_diffrn_reflns_theta_full              21.97
_diffrn_measured_fraction_theta_full   0.970
_refine_diff_density_max    0.545
_refine_diff_density_min   -0.325
_refine_diff_density_rms    0.046
 
data_s92 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C25 H30 N2 O3' 
_chemical_formula_weight          406.51 
 
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    C2/c 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1/2, z-1/2' 
 
_cell_length_a                    26.9087(10) 
_cell_length_b                    6.8778(4) 
_cell_length_c                    24.9780(10) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  106.211(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      4438.9(4) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        needle 
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.12 
_exptl_crystal_size_mid           0.02 
_exptl_crystal_size_min           0.02 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.217 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1744 
_exptl_absorpt_coefficient_mu     0.080 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   0.9905 
_exptl_absorpt_correction_T_max   0.9984 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       150(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   ? 
_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             8729 
_diffrn_reflns_av_R_equivalents   0.1029 
_diffrn_reflns_av_sigmaI/netI     0.1849 
_diffrn_reflns_limit_h_min        -30 
_diffrn_reflns_limit_h_max        22 
_diffrn_reflns_limit_k_min        -6 
_diffrn_reflns_limit_k_max        7 
_diffrn_reflns_limit_l_min        -28 
_diffrn_reflns_limit_l_max        27 
_diffrn_reflns_theta_min          3.06 
_diffrn_reflns_theta_max          24.00 
_reflns_number_total              3468 
_reflns_number_gt                 1505 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_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^)+(0.0025P)^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        0.00099(14) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          3468 
_refine_ls_number_parameters      301 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1882 
_refine_ls_R_factor_gt            0.0662 
_refine_ls_wR_factor_ref          0.1059 
_refine_ls_wR_factor_gt           0.0909 
_refine_ls_goodness_of_fit_ref    1.007 
_refine_ls_restrained_S_all       1.007 
_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 0.22411(9) 0.6826(4) 0.04372(8) 0.0412(7) Uani 1 1 d . . . 
O2 O 0.11678(10) 0.2784(4) 0.08141(11) 0.0700(10) Uani 1 1 d . . . 
O3 O 0.07957(10) 0.3151(4) -0.01062(11) 0.0494(8) Uani 1 1 d . . . 
N1 N 0.16624(10) 0.2058(5) -0.05682(11) 0.0327(8) Uani 1 1 d . . . 
N2 N 0.20930(10) 0.4790(4) -0.04721(11) 0.0371(9) Uani 1 1 d . . . 
H2 H 0.2205 0.5943 -0.0339 0.050 Uiso 1 1 calc . . . 
C1 C 0.17879(13) 0.3691(6) -0.02591(14) 0.0321(10) Uani 1 1 d . . . 
C2 C 0.19145(15) 0.1992(6) -0.10153(15) 0.0416(11) Uani 1 1 d . . . 
H2A H 0.1656 0.1932 -0.1385 0.055(12) Uiso 1 1 calc R . . 
H2B H 0.2148 0.0854 -0.0973 0.055(13) Uiso 1 1 calc R . . 
C3 C 0.22232(14) 0.3910(5) -0.09444(14) 0.0339(10) Uani 1 1 d . . . 
H3 H 0.2602 0.3617 -0.0842 0.024(9) Uiso 1 1 calc R . . 
C4 C 0.14698(14) 0.0251(5) -0.04039(14) 0.0377(10) Uani 1 1 d . . . 
H4A H 0.1417 0.0426 -0.0030 0.034(9) Uiso 1 1 calc R . . 
H4B H 0.1737 -0.0766 -0.0372 0.072(14) Uiso 1 1 calc R . . 
C5 C 0.09698(14) -0.0450(6) -0.08003(15) 0.0344(10) Uani 1 1 d . . . 
C6 C 0.07970(16) -0.2293(6) -0.07254(17) 0.0407(11) Uani 1 1 d . . . 
H6 H 0.0987 -0.3077 -0.0424 0.059(13) Uiso 1 1 calc R . . 
C7 C 0.03496(18) -0.2992(7) -0.10871(19) 0.0575(13) Uani 1 1 d . . . 
H7 H 0.0234 -0.4262 -0.1031 0.047(12) Uiso 1 1 calc R . . 
C8 C 0.00659(18) -0.1905(8) -0.1525(2) 0.0705(15) Uani 1 1 d . . . 
H8 H -0.0242 -0.2406 -0.1774 0.068(14) Uiso 1 1 calc R . . 
C9 C 0.02393(17) -0.0061(8) -0.15962(19) 0.0640(14) Uani 1 1 d . . . 
H9 H 0.0049 0.0717 -0.1898 0.066(13) Uiso 1 1 calc R . . 
C10 C 0.06838(16) 0.0666(6) -0.12354(17) 0.0479(12) Uani 1 1 d . . . 
H10 H 0.0794 0.1947 -0.1287 0.033(10) Uiso 1 1 calc R . . 
C11 C 0.20766(14) 0.5141(5) -0.14686(14) 0.0317(9) Uani 1 1 d . . . 
C12 C 0.16921(14) 0.6523(6) -0.15682(15) 0.0405(11) Uani 1 1 d . . . 
H12 H 0.1520 0.6782 -0.1292 0.029(9) Uiso 1 1 calc R . . 
C13 C 0.15527(15) 0.7542(6) -0.20645(16) 0.0507(12) Uani 1 1 d . . . 
H13 H 0.1291 0.8511 -0.2126 0.024(10) Uiso 1 1 calc R . . 
C14 C 0.17979(16) 0.7139(6) -0.24722(16) 0.0494(12) Uani 1 1 d . . . 
H14 H 0.1699 0.7813 -0.2818 0.061(13) Uiso 1 1 calc R . . 
C15 C 0.21814(15) 0.5771(6) -0.23762(15) 0.0445(11) Uani 1 1 d . . . 
H15 H 0.2351 0.5497 -0.2654 0.041(11) Uiso 1 1 calc R . . 
C16 C 0.23212(14) 0.4790(6) -0.18745(15) 0.0400(11) Uani 1 1 d . . . 
H16 H 0.2591 0.3855 -0.1808 0.034(11) Uiso 1 1 calc R . . 
C17 C 0.16498(13) 0.4211(5) 0.02329(13) 0.0320(10) Uani 1 1 d . . . 
C18 C 0.12032(17) 0.3301(5) 0.03603(18) 0.0451(11) Uani 1 1 d . . . 
C19 C 0.03410(18) 0.2185(8) -0.0035(2) 0.0730(15) Uani 1 1 d . . . 
H19A H 0.0071 0.2158 -0.0392 0.14(2) Uiso 1 1 calc R . . 
H19B H 0.0213 0.2892 0.0241 0.127(19) Uiso 1 1 calc R . . 
H19C H 0.0430 0.0852 0.0095 0.12(2) Uiso 1 1 calc R . . 
C20 C 0.19200(14) 0.5759(6) 0.05787(13) 0.0327(10) Uani 1 1 d . . . 
C21 C 0.18106(14) 0.6223(5) 0.11244(13) 0.0394(10) Uani 1 1 d . . . 
H21A H 0.2133 0.6681 0.1395 0.025(9) Uiso 1 1 calc R . . 
H21B H 0.1697 0.5026 0.1276 0.044(11) Uiso 1 1 calc R . . 
C22 C 0.13950(16) 0.7773(6) 0.10559(14) 0.0464(11) Uani 1 1 d . . . 
H22A H 0.1079 0.7338 0.0771 0.041(11) Uiso 1 1 calc R . . 
H22B H 0.1516 0.8984 0.0919 0.064(13) Uiso 1 1 calc R . . 
C23 C 0.12583(16) 0.8208(6) 0.15984(15) 0.0474(11) Uani 1 1 d . . . 
H23A H 0.1583 0.8315 0.1904 0.048(12) Uiso 1 1 calc R . . 
H23B H 0.1082 0.9485 0.1562 0.073(14) Uiso 1 1 calc R . . 
C24 C 0.09160(16) 0.6706(6) 0.17577(14) 0.0483(11) Uani 1 1 d . . . 
H24A H 0.1056 0.5395 0.1723 0.038(11) Uiso 1 1 calc R . . 
H24B H 0.0566 0.6783 0.1493 0.063(13) Uiso 1 1 calc R . . 
C25 C 0.08733(16) 0.6967(7) 0.23509(14) 0.0560(12) Uani 1 1 d . . . 
H25A H 0.0652 0.5945 0.2433 0.018(9) Uiso 1 1 calc R . . 
H25B H 0.0722 0.8242 0.2384 0.077(16) Uiso 1 1 calc R . . 
H25C H 0.1219 0.6882 0.2616 0.073(14) Uiso 1 1 calc R . . 
 
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 0.0457(18) 0.0472(19) 0.0330(16) -0.0039(13) 0.0146(13) -0.0134(15) 
O2 0.109(3) 0.070(2) 0.0463(18) -0.0112(16) 0.0466(17) -0.0428(18) 
O3 0.0416(19) 0.049(2) 0.063(2) -0.0051(15) 0.0226(16) -0.0105(15) 
N1 0.042(2) 0.027(2) 0.0325(19) 0.0001(17) 0.0154(16) -0.0032(17) 
N2 0.049(2) 0.039(2) 0.0290(19) -0.0090(16) 0.0208(16) -0.0146(18) 
C1 0.031(3) 0.032(3) 0.031(2) 0.003(2) 0.005(2) -0.001(2) 
C2 0.051(3) 0.041(3) 0.039(3) -0.004(2) 0.022(2) -0.001(3) 
C3 0.028(3) 0.040(3) 0.035(3) -0.002(2) 0.0099(19) 0.002(2) 
C4 0.051(3) 0.034(3) 0.027(2) -0.001(2) 0.010(2) 0.001(3) 
C5 0.044(3) 0.035(3) 0.026(2) 0.001(2) 0.013(2) 0.002(2) 
C6 0.039(3) 0.041(3) 0.045(3) 0.003(3) 0.016(2) -0.005(3) 
C7 0.053(4) 0.053(4) 0.069(4) -0.006(3) 0.022(3) -0.016(3) 
C8 0.034(3) 0.099(5) 0.072(4) -0.009(3) 0.003(3) -0.020(3) 
C9 0.039(3) 0.085(4) 0.057(3) 0.010(3) -0.004(3) -0.001(3) 
C10 0.043(3) 0.046(4) 0.056(3) 0.005(3) 0.015(2) -0.003(3) 
C11 0.028(2) 0.033(3) 0.035(3) -0.008(2) 0.0110(19) -0.008(2) 
C12 0.036(3) 0.047(3) 0.041(3) -0.006(2) 0.016(2) 0.003(2) 
C13 0.051(3) 0.040(3) 0.055(3) 0.007(2) 0.003(2) 0.015(3) 
C14 0.063(3) 0.045(3) 0.039(3) 0.007(2) 0.011(2) -0.003(3) 
C15 0.051(3) 0.045(3) 0.040(3) -0.002(2) 0.017(2) -0.005(2) 
C16 0.040(3) 0.043(3) 0.039(3) -0.003(2) 0.015(2) 0.001(3) 
C17 0.041(3) 0.030(3) 0.029(2) 0.0022(19) 0.016(2) -0.007(2) 
C18 0.066(3) 0.028(3) 0.049(3) -0.005(2) 0.028(3) -0.007(2) 
C19 0.055(3) 0.081(5) 0.100(4) -0.022(3) 0.049(4) -0.034(3) 
C20 0.033(3) 0.039(3) 0.026(2) 0.002(2) 0.008(2) 0.006(2) 
C21 0.048(3) 0.042(3) 0.026(2) 0.001(2) 0.004(2) -0.002(2) 
C22 0.062(3) 0.046(3) 0.033(2) -0.001(2) 0.017(2) -0.001(3) 
C23 0.058(3) 0.043(3) 0.043(3) -0.005(2) 0.017(3) 0.002(3) 
C24 0.046(3) 0.055(4) 0.044(3) -0.002(2) 0.014(3) 0.009(3) 
C25 0.051(3) 0.072(4) 0.046(3) 0.006(2) 0.016(3) 0.013(3) 
 
_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 C20 1.257(3) . ? 
O2 C18 1.217(4) . ? 
O3 C18 1.363(4) . ? 
O3 C19 1.446(4) . ? 
N1 C1 1.351(4) . ? 
N1 C4 1.449(4) . ? 
N1 C2 1.460(3) . ? 
N2 C1 1.331(3) . ? 
N2 C3 1.453(4) . ? 
C1 C17 1.425(4) . ? 
C2 C3 1.543(4) . ? 
C3 C11 1.516(4) . ? 
C4 C5 1.510(4) . ? 
C5 C10 1.377(4) . ? 
C5 C6 1.381(4) . ? 
C6 C7 1.375(5) . ? 
C7 C8 1.369(5) . ? 
C8 C9 1.379(5) . ? 
C9 C10 1.375(5) . ? 
C11 C16 1.376(4) . ? 
C11 C12 1.376(4) . ? 
C12 C13 1.382(4) . ? 
C13 C14 1.387(4) . ? 
C14 C15 1.367(4) . ? 
C15 C16 1.380(4) . ? 
C17 C20 1.435(4) . ? 
C17 C18 1.467(4) . ? 
C20 C21 1.507(4) . ? 
C21 C22 1.520(4) . ? 
C22 C23 1.529(4) . ? 
C23 C24 1.510(4) . ? 
C24 C25 1.528(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 
C18 O3 C19 115.8(4) . . ? 
C1 N1 C4 127.1(3) . . ? 
C1 N1 C2 111.6(3) . . ? 
C4 N1 C2 118.0(3) . . ? 
C1 N2 C3 113.8(3) . . ? 
N2 C1 N1 109.1(3) . . ? 
N2 C1 C17 122.7(3) . . ? 
N1 C1 C17 128.1(3) . . ? 
N1 C2 C3 103.6(3) . . ? 
N2 C3 C11 113.9(3) . . ? 
N2 C3 C2 101.8(3) . . ? 
C11 C3 C2 112.1(3) . . ? 
N1 C4 C5 114.3(3) . . ? 
C10 C5 C6 118.9(4) . . ? 
C10 C5 C4 122.6(4) . . ? 
C6 C5 C4 118.5(4) . . ? 
C7 C6 C5 119.9(4) . . ? 
C8 C7 C6 121.7(5) . . ? 
C7 C8 C9 118.1(5) . . ? 
C10 C9 C8 120.9(5) . . ? 
C9 C10 C5 120.4(4) . . ? 
C16 C11 C12 118.6(4) . . ? 
C16 C11 C3 118.4(4) . . ? 
C12 C11 C3 122.9(3) . . ? 
C11 C12 C13 121.0(3) . . ? 
C12 C13 C14 119.4(4) . . ? 
C15 C14 C13 119.9(4) . . ? 
C14 C15 C16 119.8(4) . . ? 
C11 C16 C15 121.2(4) . . ? 
C1 C17 C20 119.7(3) . . ? 
C1 C17 C18 120.5(3) . . ? 
C20 C17 C18 119.6(3) . . ? 
O2 C18 O3 121.4(4) . . ? 
O2 C18 C17 127.5(4) . . ? 
O3 C18 C17 111.0(3) . . ? 
O1 C20 C17 122.5(3) . . ? 
O1 C20 C21 117.0(3) . . ? 
C17 C20 C21 120.5(3) . . ? 
C20 C21 C22 111.7(3) . . ? 
C21 C22 C23 112.9(3) . . ? 
C24 C23 C22 114.5(3) . . ? 
C23 C24 C25 113.1(3) . . ? 
 
_diffrn_measured_fraction_theta_max    0.996 
_diffrn_reflns_theta_full              24.00 
_diffrn_measured_fraction_theta_full   0.996 
_refine_diff_density_max    0.453 
_refine_diff_density_min   -0.221 
_refine_diff_density_rms    0.049