# Supplementary Material (ESI) for Photochemical & Photobiological Sciences
# This journal is © The Royal Society of Chemistry 2002

data_global                                                                     
#============================================================================== 
# 1. SUBMISSION DETAILS

_journal_coden_Cambridge	568

loop_                                                                           
_publ_author_name                                                              
'Kisch, Horst'
'Heinemann, Frank W.'
'Hopfner, M.'
'Meissner, H.'
'Weiss, H.'

_publ_contact_author_name     	'Prof Horst Kisch'  
_publ_contact_author_address 
;
Anorganische Chemie
University of Erlangen-Nurnberg
Egerlandstr.1
Erlangen
D-91058
GERMANY
;

_publ_contact_author_phone        '049 9131 852-7363'                            
_publ_contact_author_fax          '049 9131 852-7367'                            
_publ_contact_author_email        'KISCH@ANORGANIK.CHEMIE.UNI-ERLANGEN.DE'      
_publ_requested_journal           'Photochem. Photobiol. Sci.'
_publ_requested_coeditor_name     ?                                             

_publ_contact_letter                                                            
;                                                                               
Please consider this CIF submission for data deposition.                      
;                                                                               

#============================================================================== 
# 2. TITLE AND AUTHOR LIST                                                      

_publ_section_title                                                             
;                                                                               
Semiconductor Photocatalysis Type B - Synthesis of Unsaturated \a-Amino Esters
from Imines and Olefines Photocatalyzed by Silica Supported Cadmium Sulfide
;                                                                               



_publ_section_experimental                                                      
;                                                                               
source of material: see actual publication                                     
;                                                                               


data_mh9801 

_database_code_CSD	185614


_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C25 H29 N O2' 
_chemical_formula_weight          375.49 
_chemical_melting_point           ? 
_chemical_compound_source         ? 

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) 

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

_cell_length_a                    8.464(2) 
_cell_length_b                    25.375(4) 
_cell_length_c                    10.154(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.42(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      2180.8(8) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     295(2) 
_cell_measurement_reflns_used     42
_cell_measurement_theta_min       3.20
_cell_measurement_theta_max       13.00

_exptl_crystal_description        prism
_exptl_crystal_colour             colorless
_exptl_crystal_size_max           0.70
_exptl_crystal_size_mid           0.55
_exptl_crystal_size_min           0.40
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.144 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              808 
_exptl_absorpt_coefficient_mu     0.072 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       295(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        'Siemens P4'
_diffrn_measurement_method        'profile data from \w-scans'
_diffrn_standards_number          3 
_diffrn_standards_interval_count  100
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         2.89
_diffrn_reflns_number             6088 
_diffrn_reflns_av_R_equivalents   0.0168 
_diffrn_reflns_av_sigmaI/netI     0.0408 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        1 
_diffrn_reflns_limit_k_min        -1 
_diffrn_reflns_limit_k_max        32 
_diffrn_reflns_limit_l_min        -12 
_diffrn_reflns_limit_l_max        12 
_diffrn_reflns_theta_min          2.01 
_diffrn_reflns_theta_max          27.00 
_reflns_number_total              5072 
_reflns_number_observed           3638 
_reflns_observed_criterion        >2sigma(I) 

_computing_data_collection        
'XSCAnS 2.20 (Siemens An. X-Ray Instr., 1996)'
_computing_cell_refinement        
'XSCAnS 2.20 (Siemens An. X-Ray Instr., 1996)'
_computing_data_reduction         
'XSCAnS 2.20 (Siemens An. X-Ray Instr., 1996)'
_computing_structure_solution     
'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)'
_computing_structure_refinement   
'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)'
_computing_molecular_graphics     
'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)'
_computing_publication_material   
'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)'

_refine_special_details 
; 
Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ 
or flagged by the user for potential systematic errors.  Weighted R-factors 
wR and all goodnesses 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 observed criterion 
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. 

The asymmetric unit contains two crystallographically independent
molecules of the same enantiomer. The absolute structure could not
be determined reliably.
; 

_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
'calc w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+0.2129P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    difmap 
_refine_ls_hydrogen_treatment     noref
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0136(11) 
_refine_ls_extinction_expression 
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_abs_structure_details 
'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    -0.64(142) 
_refine_ls_number_reflns          5072 
_refine_ls_number_parameters      506 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.0743 
_refine_ls_R_factor_obs           0.0459 
_refine_ls_wR_factor_all          0.1069 
_refine_ls_wR_factor_obs          0.0930 
_refine_ls_goodness_of_fit_all    1.013 
_refine_ls_goodness_of_fit_obs    1.062 
_refine_ls_restrained_S_all       1.013 
_refine_ls_restrained_S_obs       1.061 
_refine_ls_shift/esd_max          0.001 
_refine_ls_shift/esd_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_thermal_displace_type 
_atom_site_occupancy 
_atom_site_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_group 
N1 N 0.6131(3) 0.18822(10) 0.2215(2) 0.0428(6) Uani 1 d . . 
O1 O 0.3191(3) 0.15946(9) 0.3275(2) 0.0532(6) Uani 1 d . . 
O2 O 0.2114(2) 0.22315(10) 0.2066(2) 0.0525(6) Uani 1 d . . 
C1 C 0.4933(3) 0.22787(12) 0.2511(3) 0.0403(7) Uani 1 d . . 
C2 C 0.5319(4) 0.24671(11) 0.3958(3) 0.0408(7) Uani 1 d . . 
C3 C 0.4067(4) 0.28071(12) 0.4577(3) 0.0459(7) Uani 1 d . . 
C4 C 0.4482(4) 0.32159(14) 0.5322(3) 0.0547(9) Uani 1 d . . 
C5 C 0.6223(5) 0.33458(14) 0.5406(4) 0.0634(10) Uani 1 d . . 
C6 C 0.7217(4) 0.2843(2) 0.5641(4) 0.0603(9) Uani 1 d . . 
C7 C 0.6927(4) 0.27328(14) 0.4140(3) 0.0526(8) Uani 1 d . . 
C8 C 0.6809(5) 0.3339(2) 0.3961(4) 0.0692(11) Uani 1 d . . 
C9 C 0.3346(5) 0.3553(2) 0.6077(4) 0.0820(13) Uani 1 d . . 
C10 C 0.8951(5) 0.2967(2) 0.5928(5) 0.094(2) Uani 1 d . . 
C11 C 0.6667(5) 0.2444(2) 0.6650(4) 0.0724(11) Uani 1 d . . 
C12 C 0.6021(3) 0.15304(12) 0.1155(3) 0.0422(7) Uani 1 d . . 
C13 C 0.7088(4) 0.11118(13) 0.1116(3) 0.0490(8) Uani 1 d . . 
C14 C 0.7075(4) 0.07619(14) 0.0084(3) 0.0587(9) Uani 1 d . . 
C15 C 0.5999(5) 0.0812(2) -0.0928(3) 0.0655(10) Uani 1 d . . 
C16 C 0.4934(5) 0.1223(2) -0.0899(3) 0.0637(10) Uani 1 d . . 
C17 C 0.4930(4) 0.15863(15) 0.0124(3) 0.0533(8) Uani 1 d . . 
C18 C 0.5012(4) 0.27426(13) 0.1543(3) 0.0464(7) Uani 1 d . . 
C19 C 0.3872(5) 0.31360(15) 0.1501(4) 0.0631(10) Uani 1 d . . 
C20 C 0.4056(6) 0.3572(2) 0.0697(4) 0.0826(14) Uani 1 d . . 
C21 C 0.5383(7) 0.3627(2) -0.0057(5) 0.092(2) Uani 1 d . . 
C22 C 0.6514(6) 0.3244(2) -0.0025(4) 0.0795(13) Uani 1 d . . 
C23 C 0.6357(4) 0.28016(15) 0.0766(3) 0.0599(9) Uani 1 d . . 
C24 C 0.3324(4) 0.19936(13) 0.2645(3) 0.0402(7) Uani 1 d . . 
C25 C 0.0579(4) 0.1997(2) 0.2277(4) 0.0711(12) Uani 1 d . . 
N2 N 1.1116(3) 0.10479(10) 0.5550(2) 0.0440(6) Uani 1 d . . 
O3 O 0.8192(3) 0.13322(9) 0.4430(2) 0.0529(6) Uani 1 d . . 
O4 O 0.7123(2) 0.07006(9) 0.5645(2) 0.0529(6) Uani 1 d . . 
C26 C 0.9935(3) 0.06526(12) 0.5214(3) 0.0397(7) Uani 1 d . . 
C27 C 1.0366(3) 0.04707(12) 0.3773(3) 0.0402(7) Uani 1 d . . 
C28 C 0.9210(4) 0.01051(13) 0.3104(3) 0.0478(8) Uani 1 d . . 
C29 C 0.9733(4) -0.02986(14) 0.2404(3) 0.0556(9) Uani 1 d . . 
C30 C 1.1494(4) -0.04041(14) 0.2428(4) 0.0635(10) Uani 1 d . . 
C31 C 1.2396(4) 0.01225(14) 0.2167(4) 0.0597(9) Uani 1 d . . 
C32 C 1.2029(4) 0.02413(13) 0.3654(3) 0.0501(8) Uani 1 d . . 
C33 C 1.2025(4) -0.03635(15) 0.3874(4) 0.0650(10) Uani 1 d . . 
C34 C 0.8681(5) -0.0637(2) 0.1544(4) 0.0784(13) Uani 1 d . . 
C35 C 1.4174(5) 0.0040(2) 0.1972(5) 0.0881(14) Uani 1 d . . 
C36 C 1.1796(5) 0.0496(2) 0.1117(4) 0.0732(12) Uani 1 d . . 
C37 C 1.0978(4) 0.14067(12) 0.6598(3) 0.0426(7) Uani 1 d . . 
C38 C 1.2031(4) 0.18269(14) 0.6642(3) 0.0490(8) Uani 1 d . . 
C39 C 1.2003(4) 0.21834(15) 0.7667(3) 0.0585(9) Uani 1 d . . 
C40 C 1.0923(5) 0.2129(2) 0.8669(3) 0.0659(10) Uani 1 d . . 
C41 C 0.9881(5) 0.1716(2) 0.8633(3) 0.0642(10) Uani 1 d . . 
C42 C 0.9894(4) 0.13474(14) 0.7615(3) 0.0519(8) Uani 1 d . . 
C43 C 0.9986(4) 0.01847(13) 0.6179(3) 0.0486(8) Uani 1 d . . 
C44 C 0.8860(5) -0.02156(15) 0.6140(4) 0.0646(10) Uani 1 d . . 
C45 C 0.9036(7) -0.0660(2) 0.6919(5) 0.0862(15) Uani 1 d . . 
C46 C 1.0300(9) -0.0718(2) 0.7742(5) 0.104(2) Uani 1 d . . 
C47 C 1.1425(7) -0.0330(2) 0.7788(4) 0.090(2) Uani 1 d . . 
C48 C 1.1278(5) 0.0123(2) 0.7011(3) 0.0654(10) Uani 1 d . . 
C49 C 0.8328(4) 0.09346(13) 0.5057(3) 0.0406(7) Uani 1 d . . 
C50 C 0.5595(4) 0.0948(2) 0.5472(4) 0.0671(10) Uani 1 d . . 
H1 H 0.6696 0.1750 0.2965 0.080 Uiso 1 d . . 
H2A H 0.5326 0.2116 0.4434 0.080 Uiso 1 d . . 
H2B H 1.1580 0.1179 0.4852 0.080 Uiso 1 d . . 
H3 H 0.2939 0.2708 0.4467 0.080 Uiso 1 d . . 
H5 H 0.6447 0.3635 0.5904 0.080 Uiso 1 d . . 
H7 H 0.7851 0.2536 0.3642 0.080 Uiso 1 d . . 
H8A H 0.6019 0.3468 0.3230 0.080 Uiso 1 d . . 
H8B H 0.7790 0.3498 0.3866 0.080 Uiso 1 d . . 
H9A H 0.2236 0.3466 0.5935 0.080 Uiso 1 d . . 
H9B H 0.3775 0.3553 0.7059 0.080 Uiso 1 d . . 
H9C H 0.3607 0.3943 0.5828 0.080 Uiso 1 d . . 
H10A H 0.9503 0.3224 0.5214 0.080 Uiso 1 d . . 
H10B H 0.9697 0.2698 0.5832 0.080 Uiso 1 d . . 
H10C H 0.9162 0.3115 0.6735 0.080 Uiso 1 d . . 
H11A H 0.6875 0.2639 0.7444 0.080 Uiso 1 d . . 
H11B H 0.5435 0.2365 0.6614 0.080 Uiso 1 d . . 
H11C H 0.7112 0.2100 0.6550 0.080 Uiso 1 d . . 
H13 H 0.7846 0.1091 0.1820 0.080 Uiso 1 d . . 
H14 H 0.7826 0.0498 0.0150 0.080 Uiso 1 d . . 
H15 H 0.5985 0.0567 -0.1574 0.080 Uiso 1 d . . 
H16 H 0.4132 0.1293 -0.1619 0.080 Uiso 1 d . . 
H17 H 0.4171 0.1921 0.0059 0.080 Uiso 1 d . . 
H19 H 0.2940 0.3117 0.2057 0.080 Uiso 1 d . . 
H20 H 0.3227 0.3835 0.0604 0.080 Uiso 1 d . . 
H21 H 0.5483 0.3953 -0.0594 0.080 Uiso 1 d . . 
H22 H 0.7568 0.3290 -0.0442 0.080 Uiso 1 d . . 
H23 H 0.7107 0.2534 0.0810 0.080 Uiso 1 d . . 
H25A H -0.0185 0.2233 0.1931 0.080 Uiso 1 d . . 
H25B H 0.0482 0.1901 0.3251 0.080 Uiso 1 d . . 
H25C H 0.0613 0.1663 0.1782 0.080 Uiso 1 d . . 
H27 H 1.0301 0.0818 0.3288 0.080 Uiso 1 d . . 
H28 H 0.8046 0.0177 0.3165 0.080 Uiso 1 d . . 
H30 H 1.1881 -0.0740 0.1970 0.080 Uiso 1 d . . 
H32 H 1.2821 0.0454 0.4180 0.080 Uiso 1 d . . 
H33A H 1.1334 -0.0526 0.4507 0.080 Uiso 1 d . . 
H33B H 1.3175 -0.0462 0.4126 0.080 Uiso 1 d . . 
H34A H 0.8868 -0.1011 0.1741 0.080 Uiso 1 d . . 
H34B H 0.9087 -0.0582 0.0715 0.080 Uiso 1 d . . 
H34C H 0.7458 -0.0560 0.1623 0.080 Uiso 1 d . . 
H35A H 1.4775 0.0416 0.2113 0.080 Uiso 1 d . . 
H35B H 1.4403 -0.0117 0.1223 0.080 Uiso 1 d . . 
H35C H 1.4640 -0.0217 0.2630 0.080 Uiso 1 d . . 
H36A H 1.2003 0.0377 0.0308 0.080 Uiso 1 d . . 
H36B H 1.0546 0.0532 0.1130 0.080 Uiso 1 d . . 
H36C H 1.2340 0.0831 0.1254 0.080 Uiso 1 d . . 
H38 H 1.2840 0.1851 0.5942 0.080 Uiso 1 d . . 
H39 H 1.2851 0.2470 0.7694 0.080 Uiso 1 d . . 
H40 H 1.0891 0.2417 0.9378 0.080 Uiso 1 d . . 
H41 H 0.9032 0.1671 0.9335 0.080 Uiso 1 d . . 
H42 H 0.9133 0.1078 0.7625 0.080 Uiso 1 d . . 
H44 H 0.7887 -0.0205 0.5562 0.080 Uiso 1 d . . 
H45 H 0.8105 -0.0924 0.6878 0.080 Uiso 1 d . . 
H46 H 1.0260 -0.1012 0.8152 0.080 Uiso 1 d . . 
H47 H 1.2294 -0.0327 0.8300 0.080 Uiso 1 d . . 
H48 H 1.2028 0.0390 0.6953 0.080 Uiso 1 d . . 
H50A H 0.5342 0.1003 0.4515 0.080 Uiso 1 d . . 
H50B H 0.4913 0.0713 0.5870 0.080 Uiso 1 d . . 
H50C H 0.5600 0.1329 0.5817 0.080 Uiso 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 
N1 0.0426(14) 0.0466(15) 0.0392(13) -0.0007(12) -0.0007(11) 0.0065(12) 
O1 0.0551(14) 0.0501(13) 0.0544(13) 0.0117(11) -0.0025(10) -0.0069(12) 
O2 0.0390(12) 0.0636(15) 0.0548(13) 0.0101(12) -0.0023(10) 0.0002(11) 
C1 0.038(2) 0.039(2) 0.043(2) 0.0047(13) 0.0010(13) 0.0010(14) 
C2 0.043(2) 0.036(2) 0.044(2) 0.0013(13) 0.0001(13) -0.0021(14) 
C3 0.047(2) 0.042(2) 0.049(2) -0.0017(15) 0.0021(14) 0.003(2) 
C4 0.058(2) 0.047(2) 0.059(2) -0.005(2) -0.001(2) 0.007(2) 
C5 0.069(2) 0.040(2) 0.081(3) -0.018(2) -0.003(2) -0.007(2) 
C6 0.053(2) 0.058(2) 0.070(2) -0.018(2) -0.012(2) -0.002(2) 
C7 0.039(2) 0.056(2) 0.062(2) -0.005(2) -0.0001(15) -0.005(2) 
C8 0.063(2) 0.058(2) 0.087(3) 0.001(2) 0.004(2) -0.022(2) 
C9 0.082(3) 0.072(3) 0.092(3) -0.030(2) -0.006(2) 0.015(2) 
C10 0.059(2) 0.113(4) 0.109(3) -0.040(3) -0.025(2) -0.001(3) 
C11 0.097(3) 0.063(2) 0.057(2) -0.009(2) -0.023(2) 0.005(2) 
C12 0.044(2) 0.045(2) 0.0374(15) 0.0033(13) 0.0081(13) 0.0013(15) 
C13 0.050(2) 0.047(2) 0.050(2) 0.0035(15) 0.0035(14) 0.002(2) 
C14 0.067(2) 0.052(2) 0.058(2) -0.001(2) 0.007(2) 0.005(2) 
C15 0.085(3) 0.063(2) 0.049(2) -0.012(2) 0.005(2) 0.003(2) 
C16 0.071(2) 0.077(3) 0.043(2) -0.004(2) -0.004(2) 0.006(2) 
C17 0.057(2) 0.062(2) 0.041(2) 0.001(2) -0.0012(15) 0.007(2) 
C18 0.051(2) 0.046(2) 0.042(2) 0.0099(14) 0.0010(14) -0.001(2) 
C19 0.067(2) 0.060(2) 0.063(2) 0.019(2) 0.000(2) 0.008(2) 
C20 0.103(4) 0.065(3) 0.080(3) 0.028(2) -0.004(3) 0.018(3) 
C21 0.136(5) 0.063(3) 0.076(3) 0.033(2) 0.004(3) -0.005(3) 
C22 0.099(3) 0.072(3) 0.069(3) 0.015(2) 0.028(2) -0.021(3) 
C23 0.067(2) 0.060(2) 0.053(2) 0.005(2) 0.013(2) -0.001(2) 
C24 0.040(2) 0.050(2) 0.0309(14) 0.0009(14) -0.0011(12) 0.0028(15) 
C25 0.034(2) 0.097(3) 0.083(3) 0.015(2) 0.001(2) -0.003(2) 
N2 0.0428(14) 0.047(2) 0.0419(13) -0.0023(12) 0.0020(11) -0.0054(13) 
O3 0.0525(13) 0.0508(14) 0.0555(13) 0.0120(12) 0.0060(10) 0.0089(12) 
O4 0.0395(12) 0.0615(15) 0.0579(13) 0.0096(12) 0.0035(10) 0.0003(11) 
C26 0.039(2) 0.041(2) 0.039(2) 0.0006(13) 0.0024(12) -0.0013(14) 
C27 0.045(2) 0.035(2) 0.0406(15) -0.0019(13) 0.0053(13) -0.0018(14) 
C28 0.049(2) 0.052(2) 0.042(2) 0.0003(15) 0.0041(14) -0.006(2) 
C29 0.061(2) 0.051(2) 0.055(2) -0.009(2) 0.013(2) -0.014(2) 
C30 0.070(2) 0.042(2) 0.079(3) -0.020(2) 0.023(2) -0.007(2) 
C31 0.058(2) 0.049(2) 0.073(2) -0.020(2) 0.022(2) -0.008(2) 
C32 0.045(2) 0.045(2) 0.061(2) -0.008(2) 0.005(2) -0.001(2) 
C33 0.062(2) 0.048(2) 0.084(3) -0.003(2) 0.006(2) 0.008(2) 
C34 0.091(3) 0.074(3) 0.071(3) -0.026(2) 0.017(2) -0.033(2) 
C35 0.069(3) 0.077(3) 0.119(4) -0.031(3) 0.041(2) -0.006(2) 
C36 0.100(3) 0.064(2) 0.055(2) -0.014(2) 0.027(2) -0.021(2) 
C37 0.047(2) 0.045(2) 0.0358(15) 0.0015(13) -0.0057(13) 0.0018(15) 
C38 0.050(2) 0.051(2) 0.046(2) 0.000(2) 0.0023(14) -0.004(2) 
C39 0.070(2) 0.051(2) 0.054(2) -0.002(2) -0.007(2) -0.008(2) 
C40 0.087(3) 0.064(2) 0.046(2) -0.012(2) 0.000(2) -0.007(2) 
C41 0.075(2) 0.076(3) 0.041(2) -0.006(2) 0.010(2) -0.002(2) 
C42 0.058(2) 0.056(2) 0.041(2) -0.001(2) 0.0064(15) -0.011(2) 
C43 0.061(2) 0.044(2) 0.040(2) 0.0037(14) 0.0047(15) 0.008(2) 
C44 0.081(3) 0.051(2) 0.061(2) 0.010(2) 0.016(2) -0.004(2) 
C45 0.124(4) 0.053(2) 0.082(3) 0.021(2) 0.035(3) 0.004(3) 
C46 0.187(6) 0.061(3) 0.065(3) 0.027(2) 0.028(4) 0.029(4) 
C47 0.130(4) 0.086(3) 0.052(2) 0.006(2) -0.018(2) 0.045(3) 
C48 0.084(3) 0.061(2) 0.052(2) 0.006(2) -0.007(2) 0.018(2) 
C49 0.046(2) 0.042(2) 0.0340(14) -0.0033(14) 0.0058(12) -0.0011(14) 
C50 0.041(2) 0.086(3) 0.074(2) 0.013(2) 0.001(2) -0.001(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 
N1 C12 1.401(4) . ? 
N1 C1 1.461(4) . ? 
N1 H1 0.957(2) . ? 
O1 C24 1.203(4) . ? 
O2 C24 1.322(4) . ? 
O2 C25 1.447(4) . ? 
C1 C18 1.535(4) . ? 
C1 C24 1.549(4) . ? 
C1 C2 1.578(4) . ? 
C2 C3 1.507(4) . ? 
C2 C7 1.529(4) . ? 
C2 H2A 1.012(3) . ? 
C3 C4 1.329(4) . ? 
C3 H3 0.993(3) . ? 
C4 C9 1.501(5) . ? 
C4 C5 1.511(5) . ? 
C5 C6 1.546(5) . ? 
C5 C8 1.553(5) . ? 
C5 H5 0.911(3) . ? 
C6 C11 1.515(6) . ? 
C6 C10 1.527(5) . ? 
C6 C7 1.567(5) . ? 
C7 C8 1.553(5) . ? 
C7 H7 1.060(3) . ? 
C8 H8A 1.048(4) . ? 
C8 H8B 0.929(4) . ? 
C9 H9A 0.974(5) . ? 
C9 H9B 1.059(4) . ? 
C9 H9C 1.046(5) . ? 
C10 H10A 1.083(6) . ? 
C10 H10B 0.936(5) . ? 
C10 H10C 0.918(4) . ? 
C11 H11A 0.961(4) . ? 
C11 H11B 1.063(4) . ? 
C11 H11C 0.957(4) . ? 
C12 C13 1.395(4) . ? 
C12 C17 1.398(4) . ? 
C13 C14 1.374(5) . ? 
C13 H13 0.959(3) . ? 
C14 C15 1.374(5) . ? 
C14 H14 0.925(4) . ? 
C15 C16 1.378(5) . ? 
C15 H15 0.905(4) . ? 
C16 C17 1.389(5) . ? 
C16 H16 1.009(4) . ? 
C17 H17 1.066(3) . ? 
C18 C19 1.389(5) . ? 
C18 C23 1.398(4) . ? 
C19 C20 1.385(5) . ? 
C19 H19 0.975(4) . ? 
C20 C21 1.371(7) . ? 
C20 H20 0.973(4) . ? 
C21 C22 1.364(7) . ? 
C21 H21 0.995(4) . ? 
C22 C23 1.387(5) . ? 
C22 H22 0.997(4) . ? 
C23 H23 0.931(4) . ? 
C25 H25A 0.948(4) . ? 
C25 H25B 1.023(4) . ? 
C25 H25C 0.985(5) . ? 
N2 C37 1.406(4) . ? 
N2 C26 1.455(4) . ? 
N2 H2B 0.879(2) . ? 
O3 C49 1.198(4) . ? 
O4 C49 1.326(4) . ? 
O4 C50 1.447(4) . ? 
C26 C43 1.540(4) . ? 
C26 C49 1.544(4) . ? 
C26 C27 1.580(4) . ? 
C27 C28 1.506(4) . ? 
C27 C32 1.529(4) . ? 
C27 H27 1.010(3) . ? 
C28 C29 1.325(4) . ? 
C28 H28 1.005(3) . ? 
C29 C34 1.510(5) . ? 
C29 C30 1.515(5) . ? 
C30 C33 1.535(6) . ? 
C30 C31 1.562(5) . ? 
C30 H30 1.027(3) . ? 
C31 C36 1.512(6) . ? 
C31 C35 1.534(5) . ? 
C31 C32 1.573(5) . ? 
C32 C33 1.551(5) . ? 
C32 H32 1.010(3) . ? 
C33 H33A 0.965(4) . ? 
C33 H33B 1.036(4) . ? 
C34 H34A 0.983(5) . ? 
C34 H34B 0.923(4) . ? 
C34 H34C 1.056(5) . ? 
C35 H35A 1.090(5) . ? 
C35 H35B 0.881(4) . ? 
C35 H35C 1.011(5) . ? 
C36 H36A 0.893(3) . ? 
C36 H36B 1.062(4) . ? 
C36 H36C 0.977(4) . ? 
C37 C38 1.390(4) . ? 
C37 C42 1.395(4) . ? 
C38 C39 1.379(5) . ? 
C38 H38 0.993(3) . ? 
C39 C40 1.380(5) . ? 
C39 H39 1.023(4) . ? 
C40 C41 1.370(5) . ? 
C40 H40 1.027(4) . ? 
C41 C42 1.393(5) . ? 
C41 H41 1.022(3) . ? 
C42 H42 0.940(3) . ? 
C43 C48 1.386(5) . ? 
C43 C44 1.393(5) . ? 
C44 C45 1.385(6) . ? 
C44 H44 1.008(4) . ? 
C45 C46 1.360(8) . ? 
C45 H45 1.034(5) . ? 
C46 C47 1.369(8) . ? 
C46 H46 0.856(4) . ? 
C47 C48 1.399(6) . ? 
C47 H47 0.898(5) . ? 
C48 H48 0.931(4) . ? 
C50 H50A 1.003(4) . ? 
C50 H50B 0.926(4) . ? 
C50 H50C 1.029(5) . ? 

loop_ 
_geom_angle_atom_site_label_1 
_geom_angle_atom_site_label_2 
_geom_angle_atom_site_label_3 
_geom_angle 
_geom_angle_site_symmetry_1 
_geom_angle_site_symmetry_3 
_geom_angle_publ_flag 
C12 N1 C1 123.7(2) . . ? 
C12 N1 H1 114.8(3) . . ? 
C1 N1 H1 114.9(2) . . ? 
C24 O2 C25 116.1(3) . . ? 
N1 C1 C18 111.3(2) . . ? 
N1 C1 C24 108.0(2) . . ? 
C18 C1 C24 117.2(2) . . ? 
N1 C1 C2 105.1(2) . . ? 
C18 C1 C2 110.7(2) . . ? 
C24 C1 C2 103.6(2) . . ? 
C3 C2 C7 109.0(2) . . ? 
C3 C2 C1 114.9(2) . . ? 
C7 C2 C1 115.1(2) . . ? 
C3 C2 H2A 107.8(3) . . ? 
C7 C2 H2A 109.1(3) . . ? 
C1 C2 H2A 100.3(2) . . ? 
C4 C3 C2 120.0(3) . . ? 
C4 C3 H3 120.7(3) . . ? 
C2 C3 H3 119.1(3) . . ? 
C3 C4 C9 124.6(3) . . ? 
C3 C4 C5 117.1(3) . . ? 
C9 C4 C5 118.3(3) . . ? 
C4 C5 C6 111.0(3) . . ? 
C4 C5 C8 105.2(3) . . ? 
C6 C5 C8 87.7(3) . . ? 
C4 C5 H5 114.0(3) . . ? 
C6 C5 H5 118.0(4) . . ? 
C8 C5 H5 117.8(4) . . ? 
C11 C6 C10 107.9(3) . . ? 
C11 C6 C5 119.1(3) . . ? 
C10 C6 C5 112.4(3) . . ? 
C11 C6 C7 119.4(3) . . ? 
C10 C6 C7 111.4(3) . . ? 
C5 C6 C7 85.2(3) . . ? 
C2 C7 C8 111.5(3) . . ? 
C2 C7 C6 109.2(3) . . ? 
C8 C7 C6 87.0(3) . . ? 
C2 C7 H7 113.2(3) . . ? 
C8 C7 H7 117.3(3) . . ? 
C6 C7 H7 116.0(3) . . ? 
C7 C8 C5 85.4(3) . . ? 
C7 C8 H8A 115.6(3) . . ? 
C5 C8 H8A 117.3(4) . . ? 
C7 C8 H8B 112.7(4) . . ? 
C5 C8 H8B 112.6(4) . . ? 
H8A C8 H8B 111.0(4) . . ? 
C4 C9 H9A 114.7(4) . . ? 
C4 C9 H9B 105.3(4) . . ? 
H9A C9 H9B 117.6(5) . . ? 
C4 C9 H9C 106.1(4) . . ? 
H9A C9 H9C 112.4(4) . . ? 
H9B C9 H9C 99.0(4) . . ? 
C6 C10 H10A 114.5(4) . . ? 
C6 C10 H10B 118.6(4) . . ? 
H10A C10 H10B 94.3(4) . . ? 
C6 C10 H10C 115.8(4) . . ? 
H10A C10 H10C 105.6(5) . . ? 
H10B C10 H10C 105.2(4) . . ? 
C6 C11 H11A 99.7(4) . . ? 
C6 C11 H11B 114.2(3) . . ? 
H11A C11 H11B 107.4(4) . . ? 
C6 C11 H11C 114.5(4) . . ? 
H11A C11 H11C 119.2(4) . . ? 
H11B C11 H11C 102.1(4) . . ? 
C13 C12 C17 118.7(3) . . ? 
C13 C12 N1 117.9(3) . . ? 
C17 C12 N1 123.4(3) . . ? 
C14 C13 C12 120.8(3) . . ? 
C14 C13 H13 122.4(3) . . ? 
C12 C13 H13 116.8(3) . . ? 
C13 C14 C15 120.8(3) . . ? 
C13 C14 H14 114.2(4) . . ? 
C15 C14 H14 125.0(4) . . ? 
C14 C15 C16 119.0(3) . . ? 
C14 C15 H15 118.9(4) . . ? 
C16 C15 H15 122.0(4) . . ? 
C15 C16 C17 121.5(3) . . ? 
C15 C16 H16 123.7(4) . . ? 
C17 C16 H16 114.7(4) . . ? 
C16 C17 C12 119.2(3) . . ? 
C16 C17 H17 119.2(3) . . ? 
C12 C17 H17 121.4(3) . . ? 
C19 C18 C23 118.3(3) . . ? 
C19 C18 C1 122.5(3) . . ? 
C23 C18 C1 118.9(3) . . ? 
C20 C19 C18 120.7(4) . . ? 
C20 C19 H19 118.5(4) . . ? 
C18 C19 H19 120.8(3) . . ? 
C21 C20 C19 120.4(4) . . ? 
C21 C20 H20 118.0(4) . . ? 
C19 C20 H20 121.5(5) . . ? 
C22 C21 C20 119.5(4) . . ? 
C22 C21 H21 122.9(5) . . ? 
C20 C21 H21 117.6(5) . . ? 
C21 C22 C23 121.3(4) . . ? 
C21 C22 H22 122.4(4) . . ? 
C23 C22 H22 115.6(5) . . ? 
C22 C23 C18 119.7(4) . . ? 
C22 C23 H23 123.4(4) . . ? 
C18 C23 H23 116.8(3) . . ? 
O1 C24 O2 123.0(3) . . ? 
O1 C24 C1 121.7(3) . . ? 
O2 C24 C1 115.2(3) . . ? 
O2 C25 H25A 107.3(4) . . ? 
O2 C25 H25B 108.6(3) . . ? 
H25A C25 H25B 116.7(4) . . ? 
O2 C25 H25C 104.4(3) . . ? 
H25A C25 H25C 112.1(4) . . ? 
H25B C25 H25C 107.0(4) . . ? 
C37 N2 C26 124.3(2) . . ? 
C37 N2 H2B 113.9(3) . . ? 
C26 N2 H2B 112.5(2) . . ? 
C49 O4 C50 116.1(3) . . ? 
N2 C26 C43 111.5(2) . . ? 
N2 C26 C49 108.0(2) . . ? 
C43 C26 C49 116.3(2) . . ? 
N2 C26 C27 104.8(2) . . ? 
C43 C26 C27 111.0(2) . . ? 
C49 C26 C27 104.4(2) . . ? 
C28 C27 C32 109.0(2) . . ? 
C28 C27 C26 116.4(2) . . ? 
C32 C27 C26 113.8(2) . . ? 
C28 C27 H27 106.5(3) . . ? 
C32 C27 H27 109.9(3) . . ? 
C26 C27 H27 100.7(2) . . ? 
C29 C28 C27 120.0(3) . . ? 
C29 C28 H28 120.3(3) . . ? 
C27 C28 H28 119.6(3) . . ? 
C28 C29 C34 123.5(3) . . ? 
C28 C29 C30 117.4(3) . . ? 
C34 C29 C30 119.0(3) . . ? 
C29 C30 C33 106.5(3) . . ? 
C29 C30 C31 109.2(3) . . ? 
C33 C30 C31 88.0(3) . . ? 
C29 C30 H30 117.2(3) . . ? 
C33 C30 H30 113.4(4) . . ? 
C31 C30 H30 118.4(3) . . ? 
C36 C31 C35 108.6(3) . . ? 
C36 C31 C30 119.6(3) . . ? 
C35 C31 C30 112.7(3) . . ? 
C36 C31 C32 119.3(3) . . ? 
C35 C31 C32 110.5(3) . . ? 
C30 C31 C32 84.3(3) . . ? 
C27 C32 C33 111.2(3) . . ? 
C27 C32 C31 109.7(3) . . ? 
C33 C32 C31 87.1(3) . . ? 
C27 C32 H32 111.3(3) . . ? 
C33 C32 H32 117.0(3) . . ? 
C31 C32 H32 118.4(3) . . ? 
C30 C33 C32 86.0(3) . . ? 
C30 C33 H33A 115.8(4) . . ? 
C32 C33 H33A 121.3(3) . . ? 
C30 C33 H33B 119.2(3) . . ? 
C32 C33 H33B 105.7(3) . . ? 
H33A C33 H33B 107.8(4) . . ? 
C29 C34 H34A 109.8(4) . . ? 
C29 C34 H34B 102.7(3) . . ? 
H34A C34 H34B 105.7(4) . . ? 
C29 C34 H34C 115.2(3) . . ? 
H34A C34 H34C 108.6(4) . . ? 
H34B C34 H34C 114.4(5) . . ? 
C31 C35 H35A 108.7(3) . . ? 
C31 C35 H35B 113.3(4) . . ? 
H35A C35 H35B 113.9(4) . . ? 
C31 C35 H35C 112.4(4) . . ? 
H35A C35 H35C 107.4(4) . . ? 
H35B C35 H35C 101.0(4) . . ? 
C31 C36 H36A 111.7(4) . . ? 
C31 C36 H36B 112.0(3) . . ? 
H36A C36 H36B 104.0(4) . . ? 
C31 C36 H36C 106.9(4) . . ? 
H36A C36 H36C 109.3(4) . . ? 
H36B C36 H36C 113.1(4) . . ? 
C38 C37 C42 119.0(3) . . ? 
C38 C37 N2 117.7(3) . . ? 
C42 C37 N2 123.3(3) . . ? 
C39 C38 C37 120.9(3) . . ? 
C39 C38 H38 121.1(3) . . ? 
C37 C38 H38 118.0(3) . . ? 
C38 C39 C40 120.4(3) . . ? 
C38 C39 H39 118.1(3) . . ? 
C40 C39 H39 121.3(3) . . ? 
C41 C40 C39 119.1(3) . . ? 
C41 C40 H40 122.9(4) . . ? 
C39 C40 H40 117.8(4) . . ? 
C40 C41 C42 121.6(3) . . ? 
C40 C41 H41 121.4(4) . . ? 
C42 C41 H41 116.9(4) . . ? 
C41 C42 C37 119.1(3) . . ? 
C41 C42 H42 118.1(3) . . ? 
C37 C42 H42 122.8(3) . . ? 
C48 C43 C44 118.1(3) . . ? 
C48 C43 C26 119.6(3) . . ? 
C44 C43 C26 121.9(3) . . ? 
C45 C44 C43 120.5(4) . . ? 
C45 C44 H44 116.0(4) . . ? 
C43 C44 H44 123.5(3) . . ? 
C46 C45 C44 121.2(5) . . ? 
C46 C45 H45 123.5(5) . . ? 
C44 C45 H45 115.1(5) . . ? 
C45 C46 C47 119.2(4) . . ? 
C45 C46 H46 111.0(8) . . ? 
C47 C46 H46 129.8(8) . . ? 
C46 C47 C48 120.8(4) . . ? 
C46 C47 H47 126.3(6) . . ? 
C48 C47 H47 112.9(6) . . ? 
C43 C48 C47 120.2(4) . . ? 
C43 C48 H48 114.4(3) . . ? 
C47 C48 H48 125.2(4) . . ? 
O3 C49 O4 123.1(3) . . ? 
O3 C49 C26 121.7(3) . . ? 
O4 C49 C26 115.2(3) . . ? 
O4 C50 H50A 111.2(3) . . ? 
O4 C50 H50B 103.1(4) . . ? 
H50A C50 H50B 112.4(4) . . ? 
O4 C50 H50C 111.5(3) . . ? 
H50A C50 H50C 101.5(4) . . ? 
H50B C50 H50C 117.3(4) . . ? 

_refine_diff_density_max    0.156 
_refine_diff_density_min   -0.130 
_refine_diff_density_rms    0.030 


#===END OF DATA FOR 2




data_mh9903 

_database_code_CSD	185615


_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C22 H25 N O2' 
_chemical_formula_weight          335.43 

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                    14.560(4) 
_cell_length_b                    6.584(2) 
_cell_length_c                    20.801(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  109.42(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      1880.6(9) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     298(2) 
_cell_measurement_reflns_used     58 
_cell_measurement_theta_min       3.40
_cell_measurement_theta_max       11.70

_exptl_crystal_description        platelet 
_exptl_crystal_colour             colorless
_exptl_crystal_size_max           0.55
_exptl_crystal_size_mid           0.45
_exptl_crystal_size_min           0.10
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.185 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              720 
_exptl_absorpt_coefficient_mu     0.075 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       298(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   'Nicolet R3m/V'
_diffrn_measurement_method        'profile data from \w-scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  100 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         8.66 
_diffrn_reflns_number             5235 
_diffrn_reflns_av_R_equivalents   0.0555 
_diffrn_reflns_av_sigmaI/netI     0.1967 
_diffrn_reflns_limit_h_min        -18 
_diffrn_reflns_limit_h_max        17 
_diffrn_reflns_limit_k_min        -1 
_diffrn_reflns_limit_k_max        8 
_diffrn_reflns_limit_l_min        -1 
_diffrn_reflns_limit_l_max        26 
_diffrn_reflns_theta_min          2.07 
_diffrn_reflns_theta_max          27.00 
_reflns_number_total              4114 
_reflns_number_gt                 1176 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        
'P3/PC (Siemens Analytical X-Ray Instr., 1989)'
_computing_cell_refinement        
'P3/PC (Siemens Analytical X-Ray Instr., 1989)'
_computing_data_reduction         
'XDISK (Siemens Analytical X-Ray Instr. , 1989)'
_computing_structure_solution     'SHELXTL 5.1 (Bruker AXS, 1998)'
_computing_structure_refinement   'SHELXTL 5.1 (Bruker AXS, 1998)'
_computing_molecular_graphics     'SHELXTL 5.1 (Bruker AXS, 1998)'
_computing_publication_material   'SHELXTL 5.1 (Bruker AXS, 1998)'


_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^)+(0.0365P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    difmap 
_refine_ls_hydrogen_treatment     noref
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          4114 
_refine_ls_number_parameters      226 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.2126 
_refine_ls_R_factor_gt            0.0531 
_refine_ls_wR_factor_ref          0.1176 
_refine_ls_wR_factor_gt           0.0856 
_refine_ls_goodness_of_fit_ref    0.706 
_refine_ls_restrained_S_all       0.706 
_refine_ls_shift/su_max           0.016 
_refine_ls_shift/su_mean          0.001 

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 0.45658(16) 0.5938(4) 0.21808(13) 0.0420(7) Uani 1 1 d . . . 
O1 O 0.41546(18) 1.1196(4) 0.17935(13) 0.0730(8) Uani 1 1 d . . . 
O2 O 0.33623(14) 0.8931(3) 0.21999(11) 0.0529(6) Uani 1 1 d . . . 
C1 C 0.4499(2) 0.7597(4) 0.17035(16) 0.0385(8) Uani 1 1 d . . . 
C2 C 0.3808(2) 0.6888(5) 0.09708(15) 0.0413(8) Uani 1 1 d . . . 
C3 C 0.4288(2) 0.5224(5) 0.06724(16) 0.0527(9) Uani 1 1 d . . . 
C4 C 0.3564(3) 0.4220(5) 0.00511(17) 0.0662(11) Uani 1 1 d . . . 
C5 C 0.2741(2) 0.3235(5) 0.02238(17) 0.0628(10) Uani 1 1 d . . . 
C6 C 0.2338(2) 0.4611(6) 0.06426(16) 0.0527(10) Uani 1 1 d . . . 
C7 C 0.2814(2) 0.6213(5) 0.09728(16) 0.0503(9) Uani 1 1 d . . . 
C8 C 0.1352(2) 0.4017(6) 0.06753(18) 0.0867(13) Uani 1 1 d . . . 
C12 C 0.4991(2) 0.6093(5) 0.28869(17) 0.0439(8) Uani 1 1 d . . . 
C13 C 0.4926(2) 0.4418(6) 0.32820(18) 0.0566(10) Uani 1 1 d . . . 
C14 C 0.5337(3) 0.4507(7) 0.3990(2) 0.0740(12) Uani 1 1 d . . . 
C15 C 0.5813(3) 0.6214(8) 0.43145(19) 0.0834(14) Uani 1 1 d . . . 
C16 C 0.5892(2) 0.7830(6) 0.3925(2) 0.0702(12) Uani 1 1 d . . . 
C17 C 0.5484(2) 0.7822(5) 0.32102(17) 0.0539(10) Uani 1 1 d . . . 
C18 C 0.5505(2) 0.8155(5) 0.16514(17) 0.0468(9) Uani 1 1 d . . . 
C19 C 0.5604(3) 0.9805(6) 0.1260(2) 0.0712(12) Uani 1 1 d . . . 
C20 C 0.6514(4) 1.0218(7) 0.1193(2) 0.0918(15) Uani 1 1 d . . . 
C21 C 0.7292(3) 0.9013(9) 0.1494(2) 0.0954(18) Uani 1 1 d . . . 
C22 C 0.7194(3) 0.7337(8) 0.1861(2) 0.0858(15) Uani 1 1 d . . . 
C23 C 0.6299(2) 0.6896(6) 0.19352(17) 0.0631(11) Uani 1 1 d . . . 
C24 C 0.4011(2) 0.9457(5) 0.19027(16) 0.0447(8) Uani 1 1 d . . . 
C25 C 0.2784(2) 1.0568(5) 0.23318(18) 0.0713(11) Uani 1 1 d . . . 
H1 H 0.4340 0.4900 0.2040 0.080 Uiso 1 1 d . . . 
H2 H 0.3718 0.8164 0.0630 0.080 Uiso 1 1 d . . . 
H3A H 0.4810 0.5888 0.0548 0.080 Uiso 1 1 d . . . 
H3B H 0.4558 0.4083 0.1025 0.080 Uiso 1 1 d . . . 
H4A H 0.3901 0.3138 -0.0141 0.080 Uiso 1 1 d . . . 
H4B H 0.3281 0.5403 -0.0308 0.080 Uiso 1 1 d . . . 
H5A H 0.2207 0.2838 -0.0203 0.080 Uiso 1 1 d . . . 
H5B H 0.2946 0.2022 0.0496 0.080 Uiso 1 1 d . . . 
H7 H 0.2497 0.7093 0.1224 0.080 Uiso 1 1 d . . . 
H8A H 0.1127 0.4894 0.0988 0.080 Uiso 1 1 d . . . 
H8B H 0.0839 0.4165 0.0201 0.080 Uiso 1 1 d . . . 
H8C H 0.1306 0.2456 0.0850 0.080 Uiso 1 1 d . . . 
H13 H 0.4622 0.3133 0.3058 0.080 Uiso 1 1 d . . . 
H14 H 0.5296 0.3406 0.4227 0.080 Uiso 1 1 d . . . 
H15 H 0.6081 0.6226 0.4820 0.080 Uiso 1 1 d . . . 
H16 H 0.6216 0.9098 0.4143 0.080 Uiso 1 1 d . . . 
H17 H 0.5597 0.8932 0.2956 0.080 Uiso 1 1 d . . . 
H19 H 0.4980 1.0752 0.1027 0.080 Uiso 1 1 d . . . 
H20 H 0.6520 1.1472 0.0915 0.080 Uiso 1 1 d . . . 
H21 H 0.7912 0.9306 0.1457 0.080 Uiso 1 1 d . . . 
H22 H 0.7758 0.6319 0.2083 0.080 Uiso 1 1 d . . . 
H23 H 0.6247 0.5704 0.2213 0.080 Uiso 1 1 d . . . 
H25A H 0.2569 1.1426 0.1974 0.080 Uiso 1 1 d . . . 
H25B H 0.2340 0.9971 0.2511 0.080 Uiso 1 1 d . . . 
H25C H 0.3167 1.1258 0.2697 0.080 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 
N1 0.0455(15) 0.0319(16) 0.0474(17) 0.0009(15) 0.0139(13) 0.0001(14) 
O1 0.101(2) 0.0389(14) 0.102(2) 0.0069(16) 0.0636(17) 0.0018(15) 
O2 0.0529(14) 0.0421(14) 0.0749(17) -0.0052(14) 0.0362(13) 0.0006(13) 
C1 0.0412(18) 0.0296(19) 0.049(2) 0.0013(18) 0.0200(17) -0.0039(17) 
C2 0.0445(19) 0.038(2) 0.041(2) -0.0018(18) 0.0139(16) -0.0045(17) 
C3 0.048(2) 0.056(2) 0.061(2) -0.016(2) 0.0270(18) -0.0115(19) 
C4 0.068(2) 0.069(3) 0.069(3) -0.025(2) 0.032(2) -0.014(2) 
C5 0.058(2) 0.067(3) 0.057(2) -0.007(2) 0.0105(19) -0.014(2) 
C6 0.041(2) 0.073(3) 0.041(2) 0.005(2) 0.0105(17) -0.005(2) 
C7 0.045(2) 0.064(3) 0.043(2) -0.006(2) 0.0162(17) -0.002(2) 
C8 0.061(2) 0.132(4) 0.070(3) -0.016(3) 0.025(2) -0.033(3) 
C12 0.0323(17) 0.052(2) 0.049(2) 0.000(2) 0.0150(16) 0.0018(18) 
C13 0.048(2) 0.063(3) 0.060(3) 0.020(2) 0.0187(19) 0.005(2) 
C14 0.065(3) 0.093(3) 0.065(3) 0.029(3) 0.022(2) 0.018(3) 
C15 0.068(3) 0.132(4) 0.045(3) 0.008(3) 0.013(2) 0.023(3) 
C16 0.056(2) 0.090(3) 0.057(3) -0.021(3) 0.010(2) 0.009(3) 
C17 0.054(2) 0.055(2) 0.052(2) -0.006(2) 0.0177(19) -0.004(2) 
C18 0.047(2) 0.047(2) 0.051(2) -0.005(2) 0.0223(18) -0.0092(19) 
C19 0.073(3) 0.058(3) 0.101(3) -0.001(3) 0.054(2) -0.011(2) 
C20 0.102(3) 0.077(3) 0.121(4) -0.016(3) 0.070(3) -0.037(3) 
C21 0.064(3) 0.146(5) 0.092(4) -0.048(4) 0.046(3) -0.044(3) 
C22 0.051(3) 0.140(4) 0.069(3) -0.011(3) 0.024(2) -0.002(3) 
C23 0.045(2) 0.088(3) 0.061(3) -0.005(2) 0.0245(19) -0.002(2) 
C24 0.048(2) 0.042(2) 0.047(2) -0.003(2) 0.0195(17) -0.007(2) 
C25 0.080(3) 0.055(2) 0.093(3) -0.009(2) 0.049(2) 0.012(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 
N1 C12 1.395(3) . ? 
N1 C1 1.457(3) . ? 
N1 H1 0.7723 . ? 
O1 C24 1.199(3) . ? 
O2 C24 1.336(3) . ? 
O2 C25 1.449(3) . ? 
C1 C24 1.540(4) . ? 
C1 C18 1.548(4) . ? 
C1 C2 1.592(4) . ? 
C2 C7 1.516(4) . ? 
C2 C3 1.537(4) . ? 
C2 H2 1.0792 . ? 
C3 C4 1.520(4) . ? 
C3 H3A 0.9828 . ? 
C3 H3B 1.0319 . ? 
C4 C5 1.508(4) . ? 
C4 H4A 1.0188 . ? 
C4 H4B 1.0626 . ? 
C5 C6 1.504(4) . ? 
C5 H5A 0.9999 . ? 
C5 H5B 0.9673 . ? 
C6 C7 1.322(4) . ? 
C6 C8 1.511(4) . ? 
C7 H7 0.9911 . ? 
C8 H8A 1.0034 . ? 
C8 H8B 1.0245 . ? 
C8 H8C 1.0994 . ? 
C12 C17 1.393(4) . ? 
C12 C13 1.397(4) . ? 
C13 C14 1.395(5) . ? 
C13 H13 0.9959 . ? 
C14 C15 1.374(5) . ? 
C14 H14 0.8898 . ? 
C15 C16 1.366(5) . ? 
C15 H15 0.9922 . ? 
C16 C17 1.406(4) . ? 
C16 H16 0.9906 . ? 
C17 H17 0.9487 . ? 
C18 C23 1.386(4) . ? 
C18 C19 1.393(4) . ? 
C19 C20 1.405(5) . ? 
C19 H19 1.0756 . ? 
C20 C21 1.353(6) . ? 
C20 H20 1.0107 . ? 
C21 C22 1.376(6) . ? 
C21 H21 0.9519 . ? 
C22 C23 1.392(4) . ? 
C22 H22 1.0420 . ? 
C23 H23 0.9930 . ? 
C25 H25A 0.9031 . ? 
C25 H25B 0.9343 . ? 
C25 H25C 0.9021 . ? 

loop_ 
_geom_angle_atom_site_label_1 
_geom_angle_atom_site_label_2 
_geom_angle_atom_site_label_3 
_geom_angle 
_geom_angle_site_symmetry_1 
_geom_angle_site_symmetry_3 
_geom_angle_publ_flag 
C12 N1 C1 124.6(3) . . ? 
C12 N1 H1 116.6 . . ? 
C1 N1 H1 118.7 . . ? 
C24 O2 C25 116.1(3) . . ? 
N1 C1 C24 110.2(2) . . ? 
N1 C1 C18 112.0(3) . . ? 
C24 C1 C18 111.2(3) . . ? 
N1 C1 C2 108.1(2) . . ? 
C24 C1 C2 106.9(2) . . ? 
C18 C1 C2 108.3(2) . . ? 
C7 C2 C3 110.8(3) . . ? 
C7 C2 C1 112.5(2) . . ? 
C3 C2 C1 111.6(2) . . ? 
C7 C2 H2 108.8 . . ? 
C3 C2 H2 105.2 . . ? 
C1 C2 H2 107.5 . . ? 
C4 C3 C2 111.9(3) . . ? 
C4 C3 H3A 110.4 . . ? 
C2 C3 H3A 106.5 . . ? 
C4 C3 H3B 106.3 . . ? 
C2 C3 H3B 110.4 . . ? 
H3A C3 H3B 111.4 . . ? 
C5 C4 C3 111.4(3) . . ? 
C5 C4 H4A 108.5 . . ? 
C3 C4 H4A 110.5 . . ? 
C5 C4 H4B 109.2 . . ? 
C3 C4 H4B 106.0 . . ? 
H4A C4 H4B 111.2 . . ? 
C6 C5 C4 111.9(3) . . ? 
C6 C5 H5A 109.5 . . ? 
C4 C5 H5A 110.2 . . ? 
C6 C5 H5B 105.2 . . ? 
C4 C5 H5B 112.3 . . ? 
H5A C5 H5B 107.5 . . ? 
C7 C6 C5 122.9(3) . . ? 
C7 C6 C8 121.6(3) . . ? 
C5 C6 C8 115.4(3) . . ? 
C6 C7 C2 124.6(3) . . ? 
C6 C7 H7 119.0 . . ? 
C2 C7 H7 116.3 . . ? 
C6 C8 H8A 113.6 . . ? 
C6 C8 H8B 109.4 . . ? 
H8A C8 H8B 106.1 . . ? 
C6 C8 H8C 114.9 . . ? 
H8A C8 H8C 104.7 . . ? 
H8B C8 H8C 107.6 . . ? 
C17 C12 C13 119.1(3) . . ? 
C17 C12 N1 123.0(3) . . ? 
C13 C12 N1 117.9(3) . . ? 
C14 C13 C12 119.9(4) . . ? 
C14 C13 H13 119.9 . . ? 
C12 C13 H13 120.1 . . ? 
C15 C14 C13 121.5(4) . . ? 
C15 C14 H14 120.7 . . ? 
C13 C14 H14 117.8 . . ? 
C16 C15 C14 118.3(4) . . ? 
C16 C15 H15 122.8 . . ? 
C14 C15 H15 118.9 . . ? 
C15 C16 C17 122.3(4) . . ? 
C15 C16 H16 120.4 . . ? 
C17 C16 H16 117.2 . . ? 
C12 C17 C16 118.9(3) . . ? 
C12 C17 H17 121.2 . . ? 
C16 C17 H17 119.7 . . ? 
C23 C18 C19 118.8(3) . . ? 
C23 C18 C1 120.2(3) . . ? 
C19 C18 C1 120.6(3) . . ? 
C18 C19 C20 119.5(4) . . ? 
C18 C19 H19 118.7 . . ? 
C20 C19 H19 121.7 . . ? 
C21 C20 C19 120.9(4) . . ? 
C21 C20 H20 125.4 . . ? 
C19 C20 H20 113.7 . . ? 
C20 C21 C22 120.1(4) . . ? 
C20 C21 H21 121.0 . . ? 
C22 C21 H21 118.9 . . ? 
C21 C22 C23 120.2(4) . . ? 
C21 C22 H22 123.4 . . ? 
C23 C22 H22 116.4 . . ? 
C18 C23 C22 120.5(4) . . ? 
C18 C23 H23 120.4 . . ? 
C22 C23 H23 119.1 . . ? 
O1 C24 O2 122.0(3) . . ? 
O1 C24 C1 125.7(3) . . ? 
O2 C24 C1 112.3(3) . . ? 
O2 C25 H25A 112.0 . . ? 
O2 C25 H25B 106.6 . . ? 
H25A C25 H25B 119.7 . . ? 
O2 C25 H25C 107.4 . . ? 
H25A C25 H25C 109.1 . . ? 
H25B C25 H25C 101.0 . . ? 

_diffrn_measured_fraction_theta_max    1.000 
_diffrn_reflns_theta_full              27.00 
_diffrn_measured_fraction_theta_full   1.000 
_refine_diff_density_max    0.164 
_refine_diff_density_min   -0.163 
_refine_diff_density_rms    0.035 

#===END OF DATA FOR 5


data_mh9902 

_database_code_CSD	185616


_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum             'C20 H23 N O2' 
_chemical_formula_weight          309.39 

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                    9.8010(10) 
_cell_length_b                    17.753(3) 
_cell_length_c                    10.0680(10) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  91.020(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      1751.5(4) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     295(2) 
_cell_measurement_reflns_used     36
_cell_measurement_theta_min       4.10 
_cell_measurement_theta_max       11.60

_exptl_crystal_description        fragment
_exptl_crystal_colour             colorless
_exptl_crystal_size_max           0.42
_exptl_crystal_size_mid           0.35
_exptl_crystal_size_min           0.25
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.173 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              664 
_exptl_absorpt_coefficient_mu     0.075 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       295(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   'Siemens P4' 
_diffrn_measurement_method        'profile data from \w-scans'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  100 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         2.73
_diffrn_reflns_number             4325 
_diffrn_reflns_av_R_equivalents   0.0230 
_diffrn_reflns_av_sigmaI/netI     0.0708 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        1 
_diffrn_reflns_limit_k_min        -1 
_diffrn_reflns_limit_k_max        21 
_diffrn_reflns_limit_l_min        -12 
_diffrn_reflns_limit_l_max        12 
_diffrn_reflns_theta_min          2.29 
_diffrn_reflns_theta_max          25.99 
_reflns_number_total              3426 
_reflns_number_gt                 1750 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        'XSCAnS 2.20 (Siemens An. X-Ray Instr., 1996)'
_computing_cell_refinement        'XSCAnS 2.20 (Siemens An. X-Ray Instr., 1996)'
_computing_data_reduction         'XSCAnS 2.20 (Siemens An. X-Ray Instr., 1996)'
_computing_structure_solution     'SHELXTL 5.1 (Bruker AXS, 1998)'
_computing_structure_refinement   'SHELXTL 5.1 (Bruker AXS, 1998)'
_computing_molecular_graphics     'SHELXTL 5.1 (Bruker AXS, 1998)'
_computing_publication_material   'SHELXTL 5.1 (Bruker AXS, 1998)'


_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^)+(0.0614P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    difmap
_refine_ls_hydrogen_treatment     noref
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3426 
_refine_ls_number_parameters      208 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1424 
_refine_ls_R_factor_gt            0.0627 
_refine_ls_wR_factor_ref          0.1508 
_refine_ls_wR_factor_gt           0.1196 
_refine_ls_goodness_of_fit_ref    1.012 
_refine_ls_restrained_S_all       1.012 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 

loop_ 
_atom_site_label 
_atom_site_type_symbol 
_atom_site_fract_x 
_atom_site_fract_y 
_atom_site_fract_z 
_atom_site_U_iso_or_equiv 
_atom_site_adp_type 
_atom_site_occupancy 
_atom_site_symmetry_multiplicity 
_atom_site_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_assembly 
_atom_site_disorder_group 
N1 N 0.0666(2) 0.11498(12) 0.4296(2) 0.0476(6) Uani 1 1 d . . . 
O1 O 0.1722(2) 0.00489(12) 0.6142(2) 0.0739(7) Uani 1 1 d . . . 
O2 O 0.33057(18) 0.09154(11) 0.6481(2) 0.0622(6) Uani 1 1 d . . . 
C1 C 0.1080(3) 0.13344(14) 0.5662(2) 0.0428(6) Uani 1 1 d . . . 
C2 C -0.0228(3) 0.12378(15) 0.6520(2) 0.0462(7) Uani 1 1 d . . . 
C3 C -0.1356(3) 0.17620(16) 0.6120(3) 0.0549(8) Uani 1 1 d . . . 
C4 C -0.2595(3) 0.15646(17) 0.5795(3) 0.0635(9) Uani 1 1 d . . . 
C5 C -0.3749(3) 0.2092(2) 0.5513(4) 0.0886(11) Uani 1 1 d . . . 
C6 C 0.0066(3) 0.13109(18) 0.8008(3) 0.0653(9) Uani 1 1 d . . . 
C12 C 0.1584(3) 0.10274(14) 0.3270(2) 0.0434(6) Uani 1 1 d . . . 
C13 C 0.1110(3) 0.06544(15) 0.2131(3) 0.0533(7) Uani 1 1 d . . . 
C14 C 0.1953(4) 0.05393(18) 0.1070(3) 0.0683(9) Uani 1 1 d . . . 
C15 C 0.3285(4) 0.07907(19) 0.1102(3) 0.0706(9) Uani 1 1 d . . . 
C16 C 0.3762(3) 0.11601(17) 0.2219(3) 0.0624(8) Uani 1 1 d . . . 
C17 C 0.2938(3) 0.12767(16) 0.3297(3) 0.0518(7) Uani 1 1 d . . . 
C18 C 0.1621(3) 0.21428(15) 0.5766(3) 0.0451(7) Uani 1 1 d . . . 
C19 C 0.2367(3) 0.23985(16) 0.6872(3) 0.0527(7) Uani 1 1 d . . . 
C20 C 0.2765(3) 0.31449(18) 0.6961(3) 0.0663(9) Uani 1 1 d . . . 
C21 C 0.2442(3) 0.36437(17) 0.5974(4) 0.0687(9) Uani 1 1 d . . . 
C22 C 0.1712(3) 0.34043(16) 0.4882(3) 0.0633(9) Uani 1 1 d . . . 
C23 C 0.1297(3) 0.26622(15) 0.4775(3) 0.0526(7) Uani 1 1 d . . . 
C24 C 0.2059(3) 0.06988(16) 0.6121(3) 0.0473(7) Uani 1 1 d . . . 
C25 C 0.4241(3) 0.03278(19) 0.6898(4) 0.0819(11) Uani 1 1 d . . . 
H1 H -0.0007 0.0856 0.4272 0.080 Uiso 1 1 d . . . 
H2 H -0.0541 0.0727 0.6319 0.080 Uiso 1 1 d . . . 
H3 H -0.1177 0.2280 0.6215 0.080 Uiso 1 1 d . . . 
H4 H -0.2841 0.1007 0.5702 0.080 Uiso 1 1 d . . . 
H5A H -0.4536 0.1977 0.6072 0.080 Uiso 1 1 d . . . 
H5B H -0.4169 0.1974 0.4689 0.080 Uiso 1 1 d . . . 
H5C H -0.3437 0.2626 0.5607 0.080 Uiso 1 1 d . . . 
H6A H -0.0706 0.1166 0.8505 0.080 Uiso 1 1 d . . . 
H6B H 0.0201 0.1852 0.8217 0.080 Uiso 1 1 d . . . 
H6C H 0.0901 0.1012 0.8290 0.080 Uiso 1 1 d . . . 
H13 H 0.0190 0.0465 0.2101 0.080 Uiso 1 1 d . . . 
H14 H 0.1535 0.0282 0.0305 0.080 Uiso 1 1 d . . . 
H15 H 0.3899 0.0715 0.0347 0.080 Uiso 1 1 d . . . 
H16 H 0.4743 0.1364 0.2277 0.080 Uiso 1 1 d . . . 
H17 H 0.3265 0.1545 0.4033 0.080 Uiso 1 1 d . . . 
H19 H 0.2624 0.2039 0.7552 0.080 Uiso 1 1 d . . . 
H20 H 0.3278 0.3278 0.7712 0.080 Uiso 1 1 d . . . 
H21 H 0.2713 0.4144 0.6043 0.080 Uiso 1 1 d . . . 
H22 H 0.1392 0.3738 0.4193 0.080 Uiso 1 1 d . . . 
H23 H 0.0797 0.2496 0.4026 0.080 Uiso 1 1 d . . . 
H25A H 0.3837 0.0051 0.7598 0.080 Uiso 1 1 d . . . 
H25B H 0.5118 0.0517 0.6994 0.080 Uiso 1 1 d . . . 
H25C H 0.4366 -0.0021 0.6233 0.080 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 
N1 0.0382(12) 0.0600(15) 0.0447(12) -0.0074(11) 0.0012(10) -0.0076(11) 
O1 0.0567(14) 0.0474(13) 0.1172(19) 0.0006(12) -0.0102(12) -0.0033(11) 
O2 0.0411(11) 0.0591(12) 0.0859(15) 0.0154(11) -0.0135(10) -0.0004(10) 
C1 0.0384(15) 0.0445(15) 0.0453(16) -0.0012(13) -0.0020(12) -0.0027(13) 
C2 0.0410(15) 0.0493(16) 0.0484(15) 0.0006(13) 0.0042(13) 0.0003(13) 
C3 0.0450(17) 0.0559(18) 0.0639(19) -0.0036(15) 0.0084(15) -0.0020(15) 
C4 0.0474(18) 0.069(2) 0.074(2) -0.0012(17) 0.0045(16) 0.0020(17) 
C5 0.050(2) 0.107(3) 0.109(3) 0.009(2) 0.000(2) 0.011(2) 
C6 0.064(2) 0.082(2) 0.0500(17) 0.0012(16) 0.0122(15) -0.0104(18) 
C12 0.0474(16) 0.0403(15) 0.0425(15) 0.0015(12) -0.0005(13) 0.0041(13) 
C13 0.0614(18) 0.0507(17) 0.0476(16) 0.0010(14) -0.0015(15) 0.0036(15) 
C14 0.092(3) 0.065(2) 0.0484(19) -0.0070(15) -0.0002(19) 0.007(2) 
C15 0.086(3) 0.071(2) 0.056(2) 0.0041(18) 0.0220(19) 0.017(2) 
C16 0.0550(19) 0.064(2) 0.069(2) 0.0083(17) 0.0139(17) 0.0089(16) 
C17 0.0489(17) 0.0553(17) 0.0513(17) -0.0003(14) 0.0027(14) 0.0036(15) 
C18 0.0361(15) 0.0511(16) 0.0482(16) -0.0010(14) 0.0038(13) -0.0008(13) 
C19 0.0513(17) 0.0541(18) 0.0527(17) -0.0024(14) -0.0008(15) -0.0084(15) 
C20 0.065(2) 0.067(2) 0.067(2) -0.0102(18) 0.0026(17) -0.0154(18) 
C21 0.068(2) 0.054(2) 0.085(2) -0.0063(19) 0.020(2) -0.0131(17) 
C22 0.065(2) 0.0535(19) 0.072(2) 0.0135(17) 0.0122(18) 0.0014(17) 
C23 0.0496(17) 0.0521(18) 0.0564(17) 0.0037(15) 0.0075(14) -0.0013(15) 
C24 0.0403(16) 0.0497(18) 0.0518(17) -0.0013(14) 0.0004(13) -0.0039(14) 
C25 0.050(2) 0.078(2) 0.117(3) 0.022(2) -0.011(2) 0.0099(18) 

_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 C12 1.400(3) . ? 
N1 C1 1.464(3) . ? 
N1 H1 0.8410 . ? 
O1 C24 1.200(3) . ? 
O2 C24 1.325(3) . ? 
O2 C25 1.446(3) . ? 
C1 C18 1.533(3) . ? 
C1 C24 1.546(4) . ? 
C1 C2 1.567(3) . ? 
C2 C3 1.495(4) . ? 
C2 C6 1.526(4) . ? 
C2 H2 0.9775 . ? 
C3 C4 1.300(4) . ? 
C3 H3 0.9411 . ? 
C4 C5 1.492(4) . ? 
C4 H4 1.0235 . ? 
C5 H5A 0.9841 . ? 
C5 H5B 0.9426 . ? 
C5 H5C 1.0004 . ? 
C6 H6A 0.9500 . ? 
C6 H6B 0.9919 . ? 
C6 H6C 1.0117 . ? 
C12 C13 1.396(4) . ? 
C12 C17 1.398(4) . ? 
C13 C14 1.377(4) . ? 
C13 H13 0.9623 . ? 
C14 C15 1.380(4) . ? 
C14 H14 0.9791 . ? 
C15 C16 1.377(4) . ? 
C15 H15 0.9876 . ? 
C16 C17 1.380(4) . ? 
C16 H16 1.0275 . ? 
C17 H17 0.9333 . ? 
C18 C23 1.391(3) . ? 
C18 C19 1.396(3) . ? 
C19 C20 1.384(4) . ? 
C19 H19 0.9671 . ? 
C20 C21 1.364(4) . ? 
C20 H20 0.9318 . ? 
C21 C22 1.369(4) . ? 
C21 H21 0.9297 . ? 
C22 C23 1.382(4) . ? 
C22 H22 0.9603 . ? 
C23 H23 0.9400 . ? 
C25 H25A 0.9508 . ? 
C25 H25B 0.9257 . ? 
C25 H25C 0.9213 . ? 

loop_ 
_geom_angle_atom_site_label_1 
_geom_angle_atom_site_label_2 
_geom_angle_atom_site_label_3 
_geom_angle 
_geom_angle_site_symmetry_1 
_geom_angle_site_symmetry_3 
_geom_angle_publ_flag 
C12 N1 C1 123.9(2) . . ? 
C12 N1 H1 113.4 . . ? 
C1 N1 H1 111.7 . . ? 
C24 O2 C25 116.5(2) . . ? 
N1 C1 C18 111.3(2) . . ? 
N1 C1 C24 106.1(2) . . ? 
C18 C1 C24 116.8(2) . . ? 
N1 C1 C2 106.08(19) . . ? 
C18 C1 C2 110.5(2) . . ? 
C24 C1 C2 105.3(2) . . ? 
C3 C2 C6 109.7(2) . . ? 
C3 C2 C1 113.1(2) . . ? 
C6 C2 C1 113.0(2) . . ? 
C3 C2 H2 107.1 . . ? 
C6 C2 H2 109.6 . . ? 
C1 C2 H2 104.2 . . ? 
C4 C3 C2 125.7(3) . . ? 
C4 C3 H3 117.4 . . ? 
C2 C3 H3 116.5 . . ? 
C3 C4 C5 125.5(3) . . ? 
C3 C4 H4 120.0 . . ? 
C5 C4 H4 114.5 . . ? 
C4 C5 H5A 111.0 . . ? 
C4 C5 H5B 110.2 . . ? 
H5A C5 H5B 97.1 . . ? 
C4 C5 H5C 110.3 . . ? 
H5A C5 H5C 112.6 . . ? 
H5B C5 H5C 115.0 . . ? 
C2 C6 H6A 110.9 . . ? 
C2 C6 H6B 108.2 . . ? 
H6A C6 H6B 104.8 . . ? 
C2 C6 H6C 111.6 . . ? 
H6A C6 H6C 110.9 . . ? 
H6B C6 H6C 110.1 . . ? 
C13 C12 C17 118.0(2) . . ? 
C13 C12 N1 118.1(2) . . ? 
C17 C12 N1 124.0(2) . . ? 
C14 C13 C12 120.8(3) . . ? 
C14 C13 H13 119.9 . . ? 
C12 C13 H13 119.4 . . ? 
C13 C14 C15 121.0(3) . . ? 
C13 C14 H14 115.6 . . ? 
C15 C14 H14 123.4 . . ? 
C16 C15 C14 118.7(3) . . ? 
C16 C15 H15 119.4 . . ? 
C14 C15 H15 121.9 . . ? 
C15 C16 C17 121.3(3) . . ? 
C15 C16 H16 121.2 . . ? 
C17 C16 H16 117.5 . . ? 
C16 C17 C12 120.3(3) . . ? 
C16 C17 H17 120.3 . . ? 
C12 C17 H17 119.3 . . ? 
C23 C18 C19 117.7(3) . . ? 
C23 C18 C1 119.8(2) . . ? 
C19 C18 C1 122.3(2) . . ? 
C20 C19 C18 120.4(3) . . ? 
C20 C19 H19 121.1 . . ? 
C18 C19 H19 118.4 . . ? 
C21 C20 C19 120.9(3) . . ? 
C21 C20 H20 122.8 . . ? 
C19 C20 H20 116.3 . . ? 
C20 C21 C22 119.6(3) . . ? 
C20 C21 H21 120.2 . . ? 
C22 C21 H21 120.1 . . ? 
C21 C22 C23 120.5(3) . . ? 
C21 C22 H22 123.3 . . ? 
C23 C22 H22 116.1 . . ? 
C22 C23 C18 120.9(3) . . ? 
C22 C23 H23 120.7 . . ? 
C18 C23 H23 118.5 . . ? 
O1 C24 O2 121.8(3) . . ? 
O1 C24 C1 122.5(2) . . ? 
O2 C24 C1 115.7(2) . . ? 
O2 C25 H25A 108.5 . . ? 
O2 C25 H25B 110.5 . . ? 
H25A C25 H25B 120.6 . . ? 
O2 C25 H25C 111.4 . . ? 
H25A C25 H25C 104.7 . . ? 
H25B C25 H25C 100.6 . . ? 

_diffrn_measured_fraction_theta_max    1.000 
_diffrn_reflns_theta_full              25.99 
_diffrn_measured_fraction_theta_full   1.000 
_refine_diff_density_max    0.136 
_refine_diff_density_min   -0.208 
_refine_diff_density_rms    0.040 

#===END OF DATA FOR 6


data_mh9901 

_database_code_CSD	185617


_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C23 H25 N O2' 
_chemical_formula_weight          347.44 
_chemical_melting_point           ? 
_chemical_compound_source         ? 

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            orthorhombic
_symmetry_space_group_name_H-M    Pbca

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

_cell_length_a                    17.470(2) 
_cell_length_b                    11.704(2) 
_cell_length_c                    18.731(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      3829.9(11) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     295(2) 
_cell_measurement_reflns_used     36
_cell_measurement_theta_min       2.17
_cell_measurement_theta_max       14.06

_exptl_crystal_description        block
_exptl_crystal_colour             colorless
_exptl_crystal_size_max           0.50
_exptl_crystal_size_mid           0.50
_exptl_crystal_size_min           0.30
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.205 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1488 
_exptl_absorpt_coefficient_mu     0.076 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       295(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        'Siemens P4'
_diffrn_measurement_method        'profile data from \w-scans'
_diffrn_standards_number          3 
_diffrn_standards_interval_count  100
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         2.28
_diffrn_reflns_number             4682 
_diffrn_reflns_av_R_equivalents   0.0307 
_diffrn_reflns_av_sigmaI/netI     0.0646 
_diffrn_reflns_limit_h_min        -1 
_diffrn_reflns_limit_h_max        23 
_diffrn_reflns_limit_k_min        -1 
_diffrn_reflns_limit_k_max        15 
_diffrn_reflns_limit_l_min        -1 
_diffrn_reflns_limit_l_max        24 
_diffrn_reflns_theta_min          2.17 
_diffrn_reflns_theta_max          26.00 
_reflns_number_total              3759 
_reflns_number_observed           1744 
_reflns_observed_criterion        >2sigma(I) 

_computing_data_collection        
'XSCAnS 2.20 (Siemens An. X-Ray Instr., 1996)'
_computing_cell_refinement        
'XSCAnS 2.20 (Siemens An. X-Ray Instr., 1996)'
_computing_data_reduction         
'XSCAnS 2.20 (Siemens An. X-Ray Instr., 1996)'
_computing_structure_solution     
'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)'
_computing_structure_refinement   
'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)'
_computing_molecular_graphics     
'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)'
_computing_publication_material   
'SHELXTL 5.03 (Siemens An. X-Ray Instr., 1995)'

_refine_special_details 
; 
Refinement on F^2^ for ALL reflections except for 45 with very negative F^2^ 
or flagged by the user for potential systematic errors.  Weighted R-factors 
wR and all goodnesses 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 observed criterion 
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. 

The COD moiety is disordered. Two different orientations could be refined
with s.o.f.'s of 0.603(4) for site A and 0.397(4) for site B.
; 

_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
'calc w=1/[\s^2^(Fo^2^)+(0.0593P)^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     'riding on preceding C or N atom' 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0044(6) 
_refine_ls_extinction_expression 
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          3714 
_refine_ls_number_parameters      273 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1533 
_refine_ls_R_factor_obs           0.0656 
_refine_ls_wR_factor_all          0.1715 
_refine_ls_wR_factor_obs          0.1350 
_refine_ls_goodness_of_fit_all    1.082 
_refine_ls_goodness_of_fit_obs    1.324 
_refine_ls_restrained_S_all       1.100 
_refine_ls_restrained_S_obs       1.324 
_refine_ls_shift/esd_max          0.000 
_refine_ls_shift/esd_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_thermal_displace_type 
_atom_site_occupancy 
_atom_site_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_group 
N1 N -0.03850(13) 0.2597(2) 0.67516(12) 0.0493(6) Uani 1 d . . 
H1A H -0.05013(13) 0.3266(2) 0.69081(12) 0.059 Uiso 1 calc R . 
O1 O -0.00385(13) -0.0072(2) 0.76366(13) 0.0771(8) Uani 1 d . . 
O2 O 0.06545(12) 0.1485(2) 0.74765(11) 0.0639(6) Uani 1 d . . 
C1 C -0.0657(2) 0.1620(2) 0.71432(15) 0.0439(7) Uani 1 d . . 
C2 C -0.1094(2) 0.2052(2) 0.7831(2) 0.0470(7) Uani 1 d . . 
H2A H -0.1300(2) 0.1367(2) 0.8062(2) 0.056 Uiso 0.603(4) calc PR 1 
H2B H -0.1458(2) 0.2633(2) 0.7669(2) 0.056 Uiso 0.397(4) calc PR 2 
C3A C -0.1762(3) 0.2766(4) 0.7647(3) 0.0522(15) Uani 0.603(4) d P 1 
H3AA H -0.1740(3) 0.3147(4) 0.7212(3) 0.063 Uiso 0.603(4) calc PR 1 
C4A C -0.2389(4) 0.2924(6) 0.8033(4) 0.083(2) Uani 0.603(4) d P 1 
H4AA H -0.2717(4) 0.3476(6) 0.7847(4) 0.100 Uiso 0.603(4) calc PR 1 
C6A C -0.2152(5) 0.1735(7) 0.9173(4) 0.094(2) Uani 0.603(4) d P 1 
H6AA H -0.2359(5) 0.1066(7) 0.9360(4) 0.113 Uiso 0.603(4) calc PR 1 
C7A C -0.1463(4) 0.1985(7) 0.9366(3) 0.090(2) Uani 0.603(4) d P 1 
H7AA H -0.1218(4) 0.1525(7) 0.9700(3) 0.108 Uiso 0.603(4) calc PR 1 
C5 C -0.2660(3) 0.2418(6) 0.8673(3) 0.137(2) Uani 1 d . . 
H5A H -0.3080(3) 0.1919(6) 0.8539(3) 0.164 Uiso 0.603(4) calc PR 1 
H5B H -0.2880(3) 0.3029(6) 0.8955(3) 0.164 Uiso 0.603(4) calc PR 1 
H5C H -0.2849(3) 0.2364(6) 0.9159(3) 0.164 Uiso 0.397(4) calc PR 2 
H5D H -0.3107(3) 0.2397(6) 0.8366(3) 0.164 Uiso 0.397(4) calc PR 2 
C8 C -0.1022(2) 0.3057(4) 0.9048(2) 0.1032(15) Uani 1 d . . 
H8A H -0.1381(2) 0.3652(4) 0.8916(2) 0.124 Uiso 0.603(4) calc PR 1 
H8B H -0.0668(2) 0.3363(4) 0.9398(2) 0.124 Uiso 0.603(4) calc PR 1 
H8C H -0.0671(2) 0.3450(4) 0.9365(2) 0.124 Uiso 0.397(4) calc PR 2 
H8D H -0.1235(2) 0.2410(4) 0.9304(2) 0.124 Uiso 0.397(4) calc PR 2 
C9 C -0.0586(2) 0.2631(3) 0.8388(2) 0.0680(10) Uani 1 d . . 
H9A H -0.0329(2) 0.3274(3) 0.8166(2) 0.082 Uiso 1 calc R . 
H9B H -0.0196(2) 0.2094(3) 0.8540(2) 0.082 Uiso 1 calc R . 
C12 C 0.0059(2) 0.2522(3) 0.6129(2) 0.0483(7) Uani 1 d . . 
C13 C 0.0296(2) 0.3533(3) 0.5807(2) 0.0639(9) Uani 1 d . . 
H13A H 0.0170(2) 0.4232(3) 0.6011(2) 0.077 Uiso 1 calc R . 
C14 C 0.0721(2) 0.3499(4) 0.5181(2) 0.0777(11) Uani 1 d . . 
H14A H 0.0876(2) 0.4179(4) 0.4969(2) 0.093 Uiso 1 calc R . 
C15 C 0.0913(2) 0.2491(4) 0.4874(2) 0.0777(11) Uani 1 d . . 
H15A H 0.1198(2) 0.2480(4) 0.4454(2) 0.093 Uiso 1 calc R . 
C16 C 0.0685(2) 0.1497(3) 0.5182(2) 0.0660(9) Uani 1 d . . 
H16A H 0.0818(2) 0.0806(3) 0.4971(2) 0.079 Uiso 1 calc R . 
C17 C 0.0258(2) 0.1491(3) 0.5807(2) 0.0547(8) Uani 1 d . . 
H17A H 0.0105(2) 0.0802(3) 0.6010(2) 0.066 Uiso 1 calc R . 
C18 C -0.1238(2) 0.0934(2) 0.6695(2) 0.0467(7) Uani 1 d . . 
C19 C -0.1441(2) -0.0178(3) 0.6837(2) 0.0722(10) Uani 1 d . . 
H19A H -0.1197(2) -0.0567(3) 0.7205(2) 0.087 Uiso 1 calc R . 
C20 C -0.1999(2) -0.0727(3) 0.6444(3) 0.0916(13) Uani 1 d . . 
H20A H -0.2119(2) -0.1483(3) 0.6549(3) 0.110 Uiso 1 calc R . 
C21 C -0.2376(2) -0.0183(4) 0.5907(2) 0.0865(13) Uani 1 d . . 
H21A H -0.2757(2) -0.0558(4) 0.5650(2) 0.104 Uiso 1 calc R . 
C22 C -0.2187(2) 0.0921(4) 0.5751(2) 0.0811(12) Uani 1 d . . 
H22A H -0.2438(2) 0.1306(4) 0.5385(2) 0.097 Uiso 1 calc R . 
C23 C -0.1620(2) 0.1466(3) 0.6141(2) 0.0662(10) Uani 1 d . . 
H23A H -0.1492(2) 0.2215(3) 0.6025(2) 0.079 Uiso 1 calc R . 
C24 C 0.0009(2) 0.0892(3) 0.7430(2) 0.0504(7) Uani 1 d . . 
C25 C 0.1286(2) 0.0919(3) 0.7831(2) 0.0909(13) Uani 1 d . . 
H25A H 0.1723(2) 0.1416(3) 0.7836(2) 0.136 Uiso 1 calc R . 
H25B H 0.1411(2) 0.0229(3) 0.7579(2) 0.136 Uiso 1 calc R . 
H25C H 0.1142(2) 0.0736(3) 0.8312(2) 0.136 Uiso 1 calc R . 
C3B C -0.1556(5) 0.1159(7) 0.8212(4) 0.067(3) Uani 0.397(4) d P 2 
H3BA H -0.1363(5) 0.0418(7) 0.8228(4) 0.080 Uiso 0.397(4) calc PR 2 
C4B C -0.2252(9) 0.1370(12) 0.8541(7) 0.116(5) Uani 0.397(4) d P 2 
H4BA H -0.2500(9) 0.0718(12) 0.8705(7) 0.139 Uiso 0.397(4) calc PR 2 
C6B C -0.2325(6) 0.3619(10) 0.8599(6) 0.086(3) Uani 0.397(4) d P 2 
H6BA H -0.2618(6) 0.4178(10) 0.8374(6) 0.104 Uiso 0.397(4) calc PR 2 
C7B C -0.1679(6) 0.3884(9) 0.8826(5) 0.082(3) Uani 0.397(4) d P 2 
H7BA H -0.1577(6) 0.4661(9) 0.8868(5) 0.098 Uiso 0.397(4) calc PR 2 

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 
N1 0.0538(15) 0.0396(13) 0.054(2) 0.0029(12) 0.0093(13) 0.0034(12) 
O1 0.074(2) 0.0495(13) 0.107(2) 0.0212(13) -0.0127(15) 0.0059(13) 
O2 0.0483(12) 0.0645(14) 0.079(2) 0.0081(13) -0.0094(12) 0.0019(12) 
C1 0.046(2) 0.042(2) 0.044(2) 0.0023(14) 0.0002(15) 0.0009(14) 
C2 0.046(2) 0.050(2) 0.045(2) -0.0009(15) 0.0020(15) -0.0011(15) 
C3A 0.050(3) 0.061(3) 0.045(3) 0.001(2) 0.006(3) 0.009(3) 
C4A 0.077(5) 0.118(6) 0.055(4) 0.001(4) 0.000(4) 0.030(4) 
C6A 0.090(6) 0.125(6) 0.068(5) 0.023(5) 0.000(5) -0.020(5) 
C7A 0.093(5) 0.130(6) 0.048(4) 0.019(4) 0.006(4) 0.000(5) 
C5 0.080(3) 0.224(7) 0.106(4) -0.031(5) 0.019(3) -0.011(4) 
C8 0.080(3) 0.149(4) 0.081(3) -0.047(3) -0.014(3) -0.005(3) 
C9 0.063(2) 0.079(2) 0.063(2) -0.010(2) 0.000(2) 0.001(2) 
C12 0.044(2) 0.056(2) 0.046(2) 0.002(2) -0.0033(15) -0.004(2) 
C13 0.064(2) 0.061(2) 0.067(2) 0.011(2) 0.006(2) -0.009(2) 
C14 0.081(3) 0.087(3) 0.065(2) 0.020(2) 0.017(2) -0.018(2) 
C15 0.067(2) 0.109(3) 0.057(2) -0.004(3) 0.014(2) -0.008(3) 
C16 0.056(2) 0.085(3) 0.057(2) -0.013(2) 0.004(2) 0.003(2) 
C17 0.051(2) 0.059(2) 0.054(2) -0.003(2) 0.005(2) 0.000(2) 
C18 0.047(2) 0.047(2) 0.046(2) -0.0022(15) 0.0057(15) 0.0021(15) 
C19 0.065(2) 0.056(2) 0.096(3) 0.004(2) -0.009(2) -0.012(2) 
C20 0.083(3) 0.065(2) 0.127(4) -0.014(3) -0.008(3) -0.020(2) 
C21 0.061(3) 0.117(4) 0.082(3) -0.040(3) 0.005(2) -0.020(3) 
C22 0.060(2) 0.119(3) 0.064(2) -0.001(3) -0.010(2) -0.008(2) 
C23 0.059(2) 0.075(2) 0.064(2) 0.007(2) -0.009(2) -0.005(2) 
C24 0.051(2) 0.051(2) 0.049(2) 0.000(2) 0.005(2) 0.001(2) 
C25 0.058(2) 0.108(3) 0.106(3) 0.008(3) -0.022(2) 0.013(2) 
C3B 0.086(7) 0.057(5) 0.057(5) -0.001(4) 0.018(5) -0.013(5) 
C4B 0.142(12) 0.113(10) 0.091(10) -0.019(8) 0.063(9) -0.048(9) 
C6B 0.070(7) 0.083(8) 0.106(10) -0.002(7) -0.012(7) 0.001(6) 
C7B 0.070(7) 0.081(7) 0.095(8) -0.025(6) 0.006(6) 0.012(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 
N1 C12 1.403(3) . ? 
N1 C1 1.439(3) . ? 
O1 C24 1.196(3) . ? 
O2 C24 1.328(3) . ? 
O2 C25 1.448(4) . ? 
C1 C24 1.539(4) . ? 
C1 C18 1.542(4) . ? 
C1 C2 1.581(4) . ? 
C2 C3A 1.476(5) . ? 
C2 C3B 1.500(8) . ? 
C2 C9 1.527(4) . ? 
C3A C4A 1.326(7) . ? 
C4A C5 1.419(8) . ? 
C6A C7A 1.290(9) . ? 
C6A C5 1.517(9) . ? 
C7A C8 1.588(8) . ? 
C5 C4B 1.440(13) . ? 
C5 C6B 1.530(11) . ? 
C8 C9 1.536(4) . ? 
C8 C7B 1.559(10) . ? 
C12 C13 1.392(4) . ? 
C12 C17 1.393(4) . ? 
C13 C14 1.387(4) . ? 
C14 C15 1.354(5) . ? 
C15 C16 1.360(4) . ? 
C16 C17 1.389(4) . ? 
C18 C19 1.375(4) . ? 
C18 C23 1.383(4) . ? 
C19 C20 1.380(5) . ? 
C20 C21 1.361(5) . ? 
C21 C22 1.366(5) . ? 
C22 C23 1.386(4) . ? 
C3B C4B 1.385(14) . ? 
C6B C7B 1.246(12) . ? 

loop_ 
_geom_angle_atom_site_label_1 
_geom_angle_atom_site_label_2 
_geom_angle_atom_site_label_3 
_geom_angle 
_geom_angle_site_symmetry_1 
_geom_angle_site_symmetry_3 
_geom_angle_publ_flag 
C12 N1 C1 123.8(2) . . ? 
C24 O2 C25 116.0(3) . . ? 
N1 C1 C24 111.6(2) . . ? 
N1 C1 C18 110.7(2) . . ? 
C24 C1 C18 113.5(2) . . ? 
N1 C1 C2 108.7(2) . . ? 
C24 C1 C2 104.9(2) . . ? 
C18 C1 C2 107.0(2) . . ? 
C3A C2 C9 111.6(3) . . ? 
C3B C2 C9 107.3(4) . . ? 
C3A C2 C1 111.8(3) . . ? 
C3B C2 C1 115.1(4) . . ? 
C9 C2 C1 114.7(2) . . ? 
C4A C3A C2 127.2(5) . . ? 
C3A C4A C5 132.7(6) . . ? 
C7A C6A C5 126.7(7) . . ? 
C6A C7A C8 121.9(6) . . ? 
C4A C5 C6A 123.2(5) . . ? 
C4B C5 C6B 125.3(7) . . ? 
C9 C8 C7B 110.6(5) . . ? 
C9 C8 C7A 106.6(4) . . ? 
C2 C9 C8 113.9(3) . . ? 
C13 C12 C17 118.3(3) . . ? 
C13 C12 N1 118.2(3) . . ? 
C17 C12 N1 123.5(3) . . ? 
C14 C13 C12 120.1(3) . . ? 
C15 C14 C13 121.1(3) . . ? 
C14 C15 C16 119.5(3) . . ? 
C15 C16 C17 121.3(3) . . ? 
C16 C17 C12 119.6(3) . . ? 
C19 C18 C23 116.5(3) . . ? 
C19 C18 C1 123.9(3) . . ? 
C23 C18 C1 119.5(3) . . ? 
C18 C19 C20 121.4(4) . . ? 
C21 C20 C19 121.2(4) . . ? 
C20 C21 C22 118.9(4) . . ? 
C21 C22 C23 119.8(4) . . ? 
C18 C23 C22 122.2(3) . . ? 
O1 C24 O2 122.1(3) . . ? 
O1 C24 C1 125.7(3) . . ? 
O2 C24 C1 112.0(3) . . ? 
C4B C3B C2 123.9(9) . . ? 
C3B C4B C5 131.6(9) . . ? 
C7B C6B C5 122.9(10) . . ? 
C6B C7B C8 127.2(9) . . ? 

_refine_diff_density_max    0.197 
_refine_diff_density_min   -0.186 
_refine_diff_density_rms    0.035 

#===END OF ALL DATA