# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Wenhao Hu'
_publ_contact_author_email       WHU@CHEM.ECNU.EDU.CN

_publ_section_title              
;
One-pot Three-component Tandem Reaction of Diazo
Compounds with Anilines and Unsaturated Ketoesters: a Novel
Synthesis of 2,3-Dihydropyrrole Derivatives
;
loop_
_publ_author_name
'Wenhao Hu.'
'Liping Yang.'
'Yongli Yue.'
'Changwei Zhai.'
'Yingguang Zhu.'

# Attachment 'crystal_structure_data_for_compound_4a.cif'

data_z
_database_code_depnum_ccdc_archive 'CCDC 714098'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H25 N O5'
_chemical_formula_weight         431.47

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                   9.0431(2)
_cell_length_b                   9.1987(2)
_cell_length_c                   14.3311(2)
_cell_angle_alpha                104.7420(10)
_cell_angle_beta                 98.0810(10)
_cell_angle_gamma                101.1600(10)
_cell_volume                     1108.22(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9982
_cell_measurement_theta_min      2.06
_cell_measurement_theta_max      27.14

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.628
_exptl_crystal_size_mid          0.624
_exptl_crystal_size_min          0.516
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             456
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.897856
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15997
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0158
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.50
_diffrn_reflns_theta_max         25.01
_reflns_number_total             3889
_reflns_number_gt                3515
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+0.3245P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.034(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         3889
_refine_ls_number_parameters     290
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0375
_refine_ls_wR_factor_ref         0.1062
_refine_ls_wR_factor_gt          0.1014
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_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 -0.06397(12) 0.07091(13) 0.27324(8) 0.0553(3) Uani 1 1 d . . .
O2 O -0.11204(12) 0.13671(13) 0.13572(8) 0.0531(3) Uani 1 1 d . . .
O3 O 0.40702(15) 0.19031(17) 0.53443(8) 0.0719(4) Uani 1 1 d . . .
O4 O 0.18128(13) 0.04256(14) 0.44408(8) 0.0580(3) Uani 1 1 d . . .
O5 O 0.44786(12) 0.35621(13) 0.41252(8) 0.0550(3) Uani 1 1 d . . .
H5A H 0.4611 0.4295 0.4619 0.083 Uiso 1 1 calc R . .
C1 C 0.3167(2) 0.36968(19) -0.00371(12) 0.0561(4) Uani 1 1 d . . .
H1A H 0.3543 0.3933 -0.0566 0.067 Uiso 1 1 calc R . .
C2 C 0.40942(19) 0.33251(18) 0.06630(13) 0.0553(4) Uani 1 1 d . . .
H2A H 0.5115 0.3347 0.0621 0.066 Uiso 1 1 calc R . .
C3 C 0.35253(16) 0.29178(17) 0.14318(11) 0.0447(3) Uani 1 1 d . . .
H3A H 0.4173 0.2679 0.1905 0.054 Uiso 1 1 calc R . .
C4 C 0.20059(15) 0.28601(14) 0.15078(9) 0.0354(3) Uani 1 1 d . . .
C5 C 0.11026(17) 0.33172(18) 0.08201(11) 0.0464(3) Uani 1 1 d . . .
H5B H 0.0098 0.3355 0.0878 0.056 Uiso 1 1 calc R . .
C6 C 0.1677(2) 0.37169(19) 0.00495(11) 0.0552(4) Uani 1 1 d . . .
H6A H 0.1051 0.4000 -0.0412 0.066 Uiso 1 1 calc R . .
C7 C 0.01685(16) 0.47751(16) 0.30681(9) 0.0399(3) Uani 1 1 d . . .
C8 C 0.0393(2) 0.60978(19) 0.27612(12) 0.0567(4) Uani 1 1 d . . .
H8A H 0.1346 0.6491 0.2633 0.068 Uiso 1 1 calc R . .
C9 C -0.0776(3) 0.6841(2) 0.26422(15) 0.0765(6) Uani 1 1 d . . .
H9A H -0.0605 0.7731 0.2438 0.092 Uiso 1 1 calc R . .
C10 C -0.2181(3) 0.6275(3) 0.28227(14) 0.0766(6) Uani 1 1 d . . .
H10A H -0.2970 0.6773 0.2736 0.092 Uiso 1 1 calc R . .
C11 C -0.2432(2) 0.4967(2) 0.31329(13) 0.0650(5) Uani 1 1 d . . .
H11A H -0.3391 0.4580 0.3255 0.078 Uiso 1 1 calc R . .
C12 C -0.12611(18) 0.42280(19) 0.32631(11) 0.0499(4) Uani 1 1 d . . .
H12A H -0.1433 0.3354 0.3484 0.060 Uiso 1 1 calc R . .
C13 C 0.29018(15) 0.04284(15) 0.24872(9) 0.0364(3) Uani 1 1 d . . .
C14 C 0.21138(16) -0.05629(16) 0.15701(10) 0.0412(3) Uani 1 1 d . . .
H14A H 0.1282 -0.0325 0.1232 0.049 Uiso 1 1 calc R . .
C15 C 0.25618(19) -0.18984(17) 0.11606(11) 0.0491(4) Uani 1 1 d . . .
H15A H 0.2031 -0.2544 0.0545 0.059 Uiso 1 1 calc R . .
C16 C 0.3778(2) -0.22897(19) 0.16462(12) 0.0548(4) Uani 1 1 d . . .
H16A H 0.4057 -0.3202 0.1372 0.066 Uiso 1 1 calc R . .
C17 C 0.4571(2) -0.1309(2) 0.25425(12) 0.0579(4) Uani 1 1 d . . .
H17A H 0.5397 -0.1561 0.2878 0.070 Uiso 1 1 calc R . .
C18 C 0.41650(18) 0.00430(19) 0.29541(11) 0.0496(4) Uani 1 1 d . . .
H18A H 0.4741 0.0708 0.3552 0.060 Uiso 1 1 calc R . .
C19 C 0.14204(15) 0.24577(15) 0.23900(9) 0.0342(3) Uani 1 1 d . . .
C20 C 0.14881(16) 0.40112(15) 0.31962(9) 0.0382(3) Uani 1 1 d . . .
H20A H 0.2418 0.4755 0.3187 0.046 Uiso 1 1 calc R . .
C21 C 0.17993(17) 0.35807(17) 0.41495(10) 0.0448(3) Uani 1 1 d . . .
H21A H 0.0870 0.2986 0.4266 0.054 Uiso 1 1 calc R . .
H21B H 0.2223 0.4494 0.4708 0.054 Uiso 1 1 calc R . .
C22 C 0.29695(16) 0.26073(17) 0.39567(10) 0.0422(3) Uani 1 1 d . . .
C23 C -0.02215(15) 0.13977(15) 0.21769(9) 0.0369(3) Uani 1 1 d . . .
C24 C -0.2702(2) 0.0507(3) 0.11841(16) 0.0744(6) Uani 1 1 d . . .
H24A H -0.3254 0.0559 0.0575 0.112 Uiso 1 1 calc R . .
H24B H -0.3173 0.0947 0.1714 0.112 Uiso 1 1 calc R . .
H24C H -0.2730 -0.0554 0.1149 0.112 Uiso 1 1 calc R . .
C25 C 0.30251(18) 0.15865(19) 0.46532(10) 0.0486(4) Uani 1 1 d . . .
C26 C 0.1810(3) -0.0591(3) 0.50659(16) 0.0802(6) Uani 1 1 d . . .
H26A H 0.0880 -0.1398 0.4848 0.120 Uiso 1 1 calc R . .
H26B H 0.1867 -0.0007 0.5734 0.120 Uiso 1 1 calc R . .
H26C H 0.2681 -0.1042 0.5030 0.120 Uiso 1 1 calc R . .
N1 N 0.24692(13) 0.17808(13) 0.29261(7) 0.0375(3) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0511(6) 0.0622(7) 0.0596(7) 0.0348(6) 0.0110(5) 0.0070(5)
O2 0.0422(6) 0.0624(7) 0.0483(6) 0.0236(5) -0.0041(4) -0.0031(5)
O3 0.0745(8) 0.0961(10) 0.0433(6) 0.0246(6) -0.0089(6) 0.0254(7)
O4 0.0603(7) 0.0746(8) 0.0497(6) 0.0342(6) 0.0095(5) 0.0203(6)
O5 0.0471(6) 0.0577(6) 0.0482(6) 0.0032(5) 0.0010(5) 0.0068(5)
C1 0.0726(11) 0.0507(9) 0.0495(9) 0.0200(7) 0.0269(8) 0.0071(8)
C2 0.0522(9) 0.0516(9) 0.0698(10) 0.0225(8) 0.0293(8) 0.0114(7)
C3 0.0411(7) 0.0453(8) 0.0500(8) 0.0175(6) 0.0106(6) 0.0096(6)
C4 0.0393(7) 0.0329(6) 0.0328(6) 0.0083(5) 0.0076(5) 0.0072(5)
C5 0.0447(8) 0.0543(9) 0.0437(8) 0.0218(7) 0.0077(6) 0.0108(7)
C6 0.0650(10) 0.0581(9) 0.0436(8) 0.0244(7) 0.0070(7) 0.0068(8)
C7 0.0478(8) 0.0411(7) 0.0335(7) 0.0091(5) 0.0113(6) 0.0172(6)
C8 0.0737(11) 0.0498(9) 0.0583(9) 0.0224(7) 0.0246(8) 0.0246(8)
C9 0.1145(17) 0.0680(12) 0.0727(12) 0.0345(10) 0.0297(12) 0.0547(12)
C10 0.0951(15) 0.0957(15) 0.0580(11) 0.0205(10) 0.0164(10) 0.0686(13)
C11 0.0541(10) 0.0914(14) 0.0530(9) 0.0111(9) 0.0154(8) 0.0351(9)
C12 0.0508(9) 0.0567(9) 0.0480(8) 0.0162(7) 0.0162(7) 0.0206(7)
C13 0.0385(7) 0.0414(7) 0.0336(6) 0.0140(5) 0.0089(5) 0.0140(6)
C14 0.0420(7) 0.0442(7) 0.0382(7) 0.0122(6) 0.0045(6) 0.0146(6)
C15 0.0546(9) 0.0445(8) 0.0444(8) 0.0056(6) 0.0077(7) 0.0140(7)
C16 0.0635(10) 0.0519(9) 0.0570(9) 0.0138(7) 0.0188(8) 0.0302(8)
C17 0.0602(10) 0.0738(11) 0.0515(9) 0.0199(8) 0.0105(7) 0.0416(9)
C18 0.0491(8) 0.0627(9) 0.0375(7) 0.0089(7) 0.0027(6) 0.0260(7)
C19 0.0365(7) 0.0369(7) 0.0313(6) 0.0108(5) 0.0060(5) 0.0129(5)
C20 0.0406(7) 0.0379(7) 0.0359(7) 0.0085(5) 0.0094(5) 0.0106(6)
C21 0.0516(8) 0.0502(8) 0.0326(7) 0.0072(6) 0.0074(6) 0.0193(7)
C22 0.0426(7) 0.0505(8) 0.0315(7) 0.0079(6) 0.0033(5) 0.0146(6)
C23 0.0405(7) 0.0359(7) 0.0373(7) 0.0125(5) 0.0086(6) 0.0131(6)
C24 0.0458(9) 0.0855(13) 0.0774(12) 0.0300(11) -0.0086(9) -0.0116(9)
C25 0.0536(9) 0.0645(10) 0.0326(7) 0.0139(7) 0.0077(6) 0.0269(8)
C26 0.0942(15) 0.0948(15) 0.0718(12) 0.0549(12) 0.0183(11) 0.0277(12)
N1 0.0416(6) 0.0436(6) 0.0285(5) 0.0090(5) 0.0038(4) 0.0174(5)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C23 1.1943(16) . ?
O2 C23 1.3219(16) . ?
O2 C24 1.4478(19) . ?
O3 C25 1.2010(18) . ?
O4 C25 1.312(2) . ?
O4 C26 1.450(2) . ?
O5 C22 1.4239(18) . ?
C1 C2 1.369(2) . ?
C1 C6 1.373(3) . ?
C2 C3 1.383(2) . ?
C3 C4 1.3854(19) . ?
C4 C5 1.3902(19) . ?
C4 C19 1.5383(17) . ?
C5 C6 1.385(2) . ?
C7 C8 1.384(2) . ?
C7 C12 1.387(2) . ?
C7 C20 1.5100(19) . ?
C8 C9 1.379(3) . ?
C9 C10 1.362(3) . ?
C10 C11 1.376(3) . ?
C11 C12 1.380(2) . ?
C13 C18 1.3932(19) . ?
C13 C14 1.3936(19) . ?
C13 N1 1.3984(17) . ?
C14 C15 1.382(2) . ?
C15 C16 1.374(2) . ?
C16 C17 1.371(2) . ?
C17 C18 1.376(2) . ?
C19 N1 1.4645(16) . ?
C19 C23 1.5521(18) . ?
C19 C20 1.5769(18) . ?
C20 C21 1.5208(19) . ?
C21 C22 1.5235(19) . ?
C22 N1 1.4393(17) . ?
C22 C25 1.537(2) . ?

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
C23 O2 C24 116.09(12) . . ?
C25 O4 C26 116.15(14) . . ?
C2 C1 C6 119.36(14) . . ?
C1 C2 C3 120.56(15) . . ?
C2 C3 C4 121.02(14) . . ?
C3 C4 C5 117.64(13) . . ?
C3 C4 C19 119.84(12) . . ?
C5 C4 C19 122.24(12) . . ?
C6 C5 C4 120.93(15) . . ?
C1 C6 C5 120.33(15) . . ?
C8 C7 C12 118.07(14) . . ?
C8 C7 C20 119.02(13) . . ?
C12 C7 C20 122.89(13) . . ?
C9 C8 C7 121.01(18) . . ?
C10 C9 C8 120.14(18) . . ?
C9 C10 C11 120.02(16) . . ?
C10 C11 C12 120.04(18) . . ?
C11 C12 C7 120.69(16) . . ?
C18 C13 C14 117.71(12) . . ?
C18 C13 N1 120.48(12) . . ?
C14 C13 N1 121.80(12) . . ?
C15 C14 C13 120.37(13) . . ?
C16 C15 C14 121.20(14) . . ?
C17 C16 C15 118.72(14) . . ?
C16 C17 C18 121.03(14) . . ?
C17 C18 C13 120.90(14) . . ?
N1 C19 C4 112.58(10) . . ?
N1 C19 C23 107.73(10) . . ?
C4 C19 C23 116.92(10) . . ?
N1 C19 C20 101.39(10) . . ?
C4 C19 C20 108.61(10) . . ?
C23 C19 C20 108.42(10) . . ?
C7 C20 C21 116.40(11) . . ?
C7 C20 C19 117.41(11) . . ?
C21 C20 C19 102.49(10) . . ?
C20 C21 C22 102.36(11) . . ?
O5 C22 N1 109.63(11) . . ?
O5 C22 C21 111.12(12) . . ?
N1 C22 C21 103.17(10) . . ?
O5 C22 C25 106.84(11) . . ?
N1 C22 C25 115.26(12) . . ?
C21 C22 C25 110.87(12) . . ?
O1 C23 O2 123.30(13) . . ?
O1 C23 C19 121.95(12) . . ?
O2 C23 C19 114.72(11) . . ?
O3 C25 O4 125.11(15) . . ?
O3 C25 C22 121.15(15) . . ?
O4 C25 C22 113.66(12) . . ?
C13 N1 C22 123.08(11) . . ?
C13 N1 C19 123.26(10) . . ?
C22 N1 C19 113.63(10) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 2.4(2) . . . . ?
C1 C2 C3 C4 0.7(2) . . . . ?
C2 C3 C4 C5 -3.9(2) . . . . ?
C2 C3 C4 C19 -177.91(13) . . . . ?
C3 C4 C5 C6 4.2(2) . . . . ?
C19 C4 C5 C6 178.06(13) . . . . ?
C2 C1 C6 C5 -2.0(3) . . . . ?
C4 C5 C6 C1 -1.3(2) . . . . ?
C12 C7 C8 C9 -0.7(2) . . . . ?
C20 C7 C8 C9 -179.46(16) . . . . ?
C7 C8 C9 C10 -0.3(3) . . . . ?
C8 C9 C10 C11 0.6(3) . . . . ?
C9 C10 C11 C12 0.1(3) . . . . ?
C10 C11 C12 C7 -1.1(3) . . . . ?
C8 C7 C12 C11 1.4(2) . . . . ?
C20 C7 C12 C11 -179.91(14) . . . . ?
C18 C13 C14 C15 1.6(2) . . . . ?
N1 C13 C14 C15 -179.39(13) . . . . ?
C13 C14 C15 C16 0.6(2) . . . . ?
C14 C15 C16 C17 -1.5(3) . . . . ?
C15 C16 C17 C18 0.1(3) . . . . ?
C16 C17 C18 C13 2.2(3) . . . . ?
C14 C13 C18 C17 -3.0(2) . . . . ?
N1 C13 C18 C17 178.00(14) . . . . ?
C3 C4 C19 N1 -15.13(17) . . . . ?
C5 C4 C19 N1 171.11(12) . . . . ?
C3 C4 C19 C23 -140.66(13) . . . . ?
C5 C4 C19 C23 45.59(17) . . . . ?
C3 C4 C19 C20 96.32(14) . . . . ?
C5 C4 C19 C20 -77.43(15) . . . . ?
C8 C7 C20 C21 132.35(14) . . . . ?
C12 C7 C20 C21 -46.35(19) . . . . ?
C8 C7 C20 C19 -105.68(15) . . . . ?
C12 C7 C20 C19 75.62(17) . . . . ?
N1 C19 C20 C7 -158.89(11) . . . . ?
C4 C19 C20 C7 82.35(14) . . . . ?
C23 C19 C20 C7 -45.65(15) . . . . ?
N1 C19 C20 C21 -30.00(13) . . . . ?
C4 C19 C20 C21 -148.76(11) . . . . ?
C23 C19 C20 C21 83.24(12) . . . . ?
C7 C20 C21 C22 170.38(12) . . . . ?
C19 C20 C21 C22 40.85(13) . . . . ?
C20 C21 C22 O5 81.36(13) . . . . ?
C20 C21 C22 N1 -36.05(14) . . . . ?
C20 C21 C22 C25 -159.98(12) . . . . ?
C24 O2 C23 O1 3.4(2) . . . . ?
C24 O2 C23 C19 -174.34(14) . . . . ?
N1 C19 C23 O1 33.08(17) . . . . ?
C4 C19 C23 O1 160.99(13) . . . . ?
C20 C19 C23 O1 -75.89(16) . . . . ?
N1 C19 C23 O2 -149.18(11) . . . . ?
C4 C19 C23 O2 -21.27(16) . . . . ?
C20 C19 C23 O2 101.85(13) . . . . ?
C26 O4 C25 O3 -4.0(2) . . . . ?
C26 O4 C25 C22 179.22(14) . . . . ?
O5 C22 C25 O3 16.64(19) . . . . ?
N1 C22 C25 O3 138.72(15) . . . . ?
C21 C22 C25 O3 -104.57(17) . . . . ?
O5 C22 C25 O4 -166.43(12) . . . . ?
N1 C22 C25 O4 -44.36(17) . . . . ?
C21 C22 C25 O4 72.35(16) . . . . ?
C18 C13 N1 C22 -17.9(2) . . . . ?
C14 C13 N1 C22 163.11(13) . . . . ?
C18 C13 N1 C19 164.41(13) . . . . ?
C14 C13 N1 C19 -14.53(19) . . . . ?
O5 C22 N1 C13 81.18(15) . . . . ?
C21 C22 N1 C13 -160.37(12) . . . . ?
C25 C22 N1 C13 -39.38(18) . . . . ?
O5 C22 N1 C19 -100.97(13) . . . . ?
C21 C22 N1 C19 17.47(15) . . . . ?
C25 C22 N1 C19 138.47(12) . . . . ?
C4 C19 N1 C13 -58.43(16) . . . . ?
C23 C19 N1 C13 71.94(14) . . . . ?
C20 C19 N1 C13 -174.30(11) . . . . ?
C4 C19 N1 C22 123.73(12) . . . . ?
C23 C19 N1 C22 -105.90(12) . . . . ?
C20 C19 N1 C22 7.85(14) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.031

# Attachment 'crystal_structure_data_for_compound_4c.cif'

data_za
_database_code_depnum_ccdc_archive 'CCDC 714099'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H25 N O5'
_chemical_formula_weight         431.47

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                   13.6991(6)
_cell_length_b                   9.8616(5)
_cell_length_c                   17.5991(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.5260(10)
_cell_angle_gamma                90.00
_cell_volume                     2290.79(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9953
_cell_measurement_theta_min      2.08
_cell_measurement_theta_max      27.16

_exptl_crystal_description       Block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.255
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             912
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.839748
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26067
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0135
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         25.01
_reflns_number_total             4025
_reflns_number_gt                3408
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0632P)^2^+0.8354P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4025
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_ref         0.1257
_refine_ls_wR_factor_gt          0.1168
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.76749(9) 0.90702(13) 0.02988(7) 0.0377(3) Uani 1 1 d . . .
O1 O 0.92660(8) 1.01146(13) 0.08233(7) 0.0521(3) Uani 1 1 d . . .
H1A H 0.9409 0.9308 0.0889 0.078 Uiso 1 1 calc R . .
O2 O 0.88672(10) 0.68511(13) 0.05596(8) 0.0595(4) Uani 1 1 d . . .
O3 O 0.77143(14) 0.56691(14) -0.03137(9) 0.0800(5) Uani 1 1 d . . .
O4 O 0.83644(10) 1.24510(13) 0.08785(8) 0.0609(4) Uani 1 1 d . . .
O5 O 0.68590(9) 1.17042(12) 0.01715(8) 0.0532(3) Uani 1 1 d . . .
C1 C 0.73406(12) 0.86846(17) 0.09541(9) 0.0415(4) Uani 1 1 d . . .
C2 C 0.66637(14) 0.7613(2) 0.09014(11) 0.0536(5) Uani 1 1 d . . .
H2A H 0.6438 0.7141 0.0430 0.064 Uiso 1 1 calc R . .
C3 C 0.63240(16) 0.7245(2) 0.15471(14) 0.0678(6) Uani 1 1 d . . .
H3A H 0.5873 0.6527 0.1504 0.081 Uiso 1 1 calc R . .
C4 C 0.66444(17) 0.7925(3) 0.22473(13) 0.0710(6) Uani 1 1 d . . .
H4A H 0.6414 0.7673 0.2678 0.085 Uiso 1 1 calc R . .
C5 C 0.73078(16) 0.8982(2) 0.23053(11) 0.0627(5) Uani 1 1 d . . .
H5A H 0.7523 0.9452 0.2779 0.075 Uiso 1 1 calc R . .
C6 C 0.76636(13) 0.93630(19) 0.16727(10) 0.0493(4) Uani 1 1 d . . .
H6A H 0.8121 1.0076 0.1727 0.059 Uiso 1 1 calc R . .
C7 C 0.84606(12) 0.83984(16) -0.15527(9) 0.0415(4) Uani 1 1 d . . .
C8 C 0.90620(14) 0.7329(2) -0.16589(12) 0.0545(5) Uani 1 1 d . . .
H8A H 0.9446 0.6869 -0.1218 0.065 Uiso 1 1 calc R . .
C9 C 0.91100(18) 0.6924(3) -0.23933(14) 0.0720(6) Uani 1 1 d . . .
H9A H 0.9513 0.6191 -0.2448 0.086 Uiso 1 1 calc R . .
C10 C 0.8565(2) 0.7600(3) -0.30378(14) 0.0786(7) Uani 1 1 d . . .
H10A H 0.8608 0.7342 -0.3536 0.094 Uiso 1 1 calc R . .
C11 C 0.7947(2) 0.8668(3) -0.29606(12) 0.0819(8) Uani 1 1 d . . .
H11A H 0.7565 0.9116 -0.3406 0.098 Uiso 1 1 calc R . .
C12 C 0.78974(18) 0.9071(2) -0.22132(11) 0.0649(6) Uani 1 1 d . . .
H12A H 0.7485 0.9793 -0.2159 0.078 Uiso 1 1 calc R . .
C13 C 0.65955(12) 0.80798(17) -0.09504(10) 0.0425(4) Uani 1 1 d . . .
C14 C 0.63665(15) 0.7152(2) -0.15673(12) 0.0598(5) Uani 1 1 d . . .
H14A H 0.6852 0.6526 -0.1621 0.072 Uiso 1 1 calc R . .
C15 C 0.54144(18) 0.7154(3) -0.21059(13) 0.0748(6) Uani 1 1 d . . .
H15A H 0.5266 0.6525 -0.2515 0.090 Uiso 1 1 calc R . .
C16 C 0.46946(16) 0.8077(3) -0.20378(14) 0.0736(6) Uani 1 1 d . . .
H16A H 0.4058 0.8071 -0.2397 0.088 Uiso 1 1 calc R . .
C17 C 0.49162(14) 0.9004(2) -0.14410(13) 0.0640(5) Uani 1 1 d . . .
H17A H 0.4431 0.9638 -0.1398 0.077 Uiso 1 1 calc R . .
C18 C 0.58576(13) 0.90068(19) -0.08993(11) 0.0489(4) Uani 1 1 d . . .
H18A H 0.5997 0.9642 -0.0494 0.059 Uiso 1 1 calc R . .
C19 C 0.76457(11) 0.81410(15) -0.03605(9) 0.0381(4) Uani 1 1 d . . .
C20 C 0.84732(11) 0.87972(16) -0.07217(9) 0.0385(4) Uani 1 1 d . . .
H20A H 0.9133 0.8517 -0.0383 0.046 Uiso 1 1 calc R . .
C21 C 0.83586(12) 1.02888(16) -0.05585(10) 0.0417(4) Uani 1 1 d . . .
H21A H 0.7750 1.0666 -0.0910 0.050 Uiso 1 1 calc R . .
H21B H 0.8941 1.0807 -0.0605 0.050 Uiso 1 1 calc R . .
C22 C 0.82881(11) 1.02511(16) 0.02930(9) 0.0394(4) Uani 1 1 d . . .
C23 C 0.80540(13) 0.67304(17) -0.00450(10) 0.0460(4) Uani 1 1 d . . .
C24 C 0.9338(2) 0.5612(2) 0.09037(14) 0.0843(8) Uani 1 1 d . . .
H24A H 0.9920 0.5820 0.1331 0.126 Uiso 1 1 calc R . .
H24B H 0.9547 0.5097 0.0511 0.126 Uiso 1 1 calc R . .
H24C H 0.8864 0.5092 0.1098 0.126 Uiso 1 1 calc R . .
C25 C 0.78401(13) 1.15865(17) 0.04961(10) 0.0427(4) Uani 1 1 d . . .
C26 C 0.64005(17) 1.2977(2) 0.02979(14) 0.0668(6) Uani 1 1 d . . .
H26A H 0.5689 1.2954 0.0037 0.100 Uiso 1 1 calc R . .
H26B H 0.6713 1.3706 0.0087 0.100 Uiso 1 1 calc R . .
H26C H 0.6496 1.3115 0.0853 0.100 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
N1 0.0394(7) 0.0392(7) 0.0366(7) -0.0006(5) 0.0138(5) -0.0023(5)
O1 0.0384(6) 0.0600(7) 0.0551(7) -0.0067(6) 0.0076(5) -0.0005(5)
O2 0.0601(8) 0.0465(7) 0.0629(8) 0.0075(6) 0.0011(6) 0.0107(6)
O3 0.1191(13) 0.0398(7) 0.0671(9) 0.0006(6) 0.0005(9) -0.0071(8)
O4 0.0672(8) 0.0491(7) 0.0631(8) -0.0156(6) 0.0115(7) -0.0081(6)
O5 0.0488(7) 0.0471(7) 0.0637(8) -0.0087(6) 0.0149(6) 0.0047(5)
C1 0.0384(8) 0.0479(9) 0.0399(9) 0.0091(7) 0.0135(7) 0.0087(7)
C2 0.0536(10) 0.0583(11) 0.0522(11) 0.0092(9) 0.0200(8) -0.0030(9)
C3 0.0636(12) 0.0743(14) 0.0729(15) 0.0258(12) 0.0308(11) 0.0001(10)
C4 0.0701(13) 0.0983(17) 0.0531(12) 0.0305(12) 0.0311(11) 0.0194(13)
C5 0.0643(12) 0.0861(15) 0.0396(10) 0.0123(10) 0.0172(9) 0.0194(11)
C6 0.0478(9) 0.0596(11) 0.0408(9) 0.0058(8) 0.0125(7) 0.0098(8)
C7 0.0449(9) 0.0422(9) 0.0402(9) -0.0015(7) 0.0163(7) -0.0062(7)
C8 0.0498(10) 0.0598(11) 0.0569(11) -0.0125(9) 0.0192(9) 0.0001(8)
C9 0.0724(14) 0.0833(15) 0.0687(14) -0.0254(12) 0.0332(12) -0.0063(12)
C10 0.1093(19) 0.0790(16) 0.0623(14) -0.0292(12) 0.0486(14) -0.0394(15)
C11 0.127(2) 0.0710(15) 0.0411(11) 0.0071(10) 0.0119(12) -0.0232(15)
C12 0.0958(16) 0.0516(11) 0.0450(11) 0.0033(9) 0.0148(10) 0.0039(10)
C13 0.0400(8) 0.0441(9) 0.0425(9) 0.0034(7) 0.0094(7) -0.0084(7)
C14 0.0565(11) 0.0620(12) 0.0575(12) -0.0107(9) 0.0093(9) -0.0083(9)
C15 0.0710(14) 0.0833(16) 0.0596(13) -0.0123(11) -0.0006(11) -0.0242(13)
C16 0.0466(11) 0.0946(17) 0.0681(14) 0.0123(13) -0.0047(10) -0.0147(11)
C17 0.0421(10) 0.0726(13) 0.0724(13) 0.0146(11) 0.0068(9) -0.0016(9)
C18 0.0429(9) 0.0504(10) 0.0526(10) 0.0066(8) 0.0110(8) -0.0035(8)
C19 0.0396(8) 0.0379(8) 0.0373(8) -0.0008(6) 0.0112(7) -0.0012(6)
C20 0.0368(8) 0.0411(8) 0.0385(8) -0.0005(7) 0.0117(6) 0.0005(6)
C21 0.0439(9) 0.0410(9) 0.0438(9) -0.0008(7) 0.0178(7) -0.0051(7)
C22 0.0357(8) 0.0426(9) 0.0404(9) -0.0030(7) 0.0108(6) -0.0034(6)
C23 0.0559(10) 0.0406(9) 0.0430(9) 0.0010(7) 0.0156(8) -0.0005(8)
C24 0.1057(19) 0.0639(14) 0.0733(15) 0.0184(12) 0.0067(13) 0.0340(13)
C25 0.0493(9) 0.0432(9) 0.0385(9) -0.0012(7) 0.0165(7) -0.0048(7)
C26 0.0689(13) 0.0536(11) 0.0825(15) -0.0037(10) 0.0280(11) 0.0145(10)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.402(2) . ?
N1 C22 1.438(2) . ?
N1 C19 1.4706(19) . ?
O1 C22 1.4192(19) . ?
O2 C23 1.324(2) . ?
O2 C24 1.438(2) . ?
O3 C23 1.191(2) . ?
O4 C25 1.199(2) . ?
O5 C25 1.317(2) . ?
O5 C26 1.447(2) . ?
C1 C2 1.392(2) . ?
C1 C6 1.394(2) . ?
C2 C3 1.387(3) . ?
C3 C4 1.368(3) . ?
C4 C5 1.368(3) . ?
C5 C6 1.381(3) . ?
C7 C12 1.381(3) . ?
C7 C8 1.382(2) . ?
C7 C20 1.510(2) . ?
C8 C9 1.371(3) . ?
C9 C10 1.354(4) . ?
C10 C11 1.381(4) . ?
C11 C12 1.393(3) . ?
C13 C18 1.384(2) . ?
C13 C14 1.390(3) . ?
C13 C19 1.534(2) . ?
C14 C15 1.392(3) . ?
C15 C16 1.371(3) . ?
C16 C17 1.364(3) . ?
C17 C18 1.383(3) . ?
C19 C23 1.546(2) . ?
C19 C20 1.579(2) . ?
C20 C21 1.515(2) . ?
C21 C22 1.528(2) . ?
C22 C25 1.535(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C22 123.06(13) . . ?
C1 N1 C19 122.27(13) . . ?
C22 N1 C19 113.06(12) . . ?
C23 O2 C24 116.65(16) . . ?
C25 O5 C26 116.37(14) . . ?
C2 C1 C6 117.94(15) . . ?
C2 C1 N1 120.61(15) . . ?
C6 C1 N1 121.44(15) . . ?
C3 C2 C1 120.51(19) . . ?
C4 C3 C2 120.8(2) . . ?
C3 C4 C5 119.16(18) . . ?
C4 C5 C6 121.2(2) . . ?
C5 C6 C1 120.38(19) . . ?
C12 C7 C8 118.16(17) . . ?
C12 C7 C20 123.32(16) . . ?
C8 C7 C20 118.50(15) . . ?
C9 C8 C7 122.0(2) . . ?
C10 C9 C8 119.4(2) . . ?
C9 C10 C11 120.5(2) . . ?
C10 C11 C12 119.8(2) . . ?
C7 C12 C11 120.0(2) . . ?
C18 C13 C14 118.01(16) . . ?
C18 C13 C19 119.96(15) . . ?
C14 C13 C19 121.96(16) . . ?
C13 C14 C15 120.3(2) . . ?
C16 C15 C14 120.4(2) . . ?
C17 C16 C15 119.69(19) . . ?
C16 C17 C18 120.4(2) . . ?
C17 C18 C13 121.08(18) . . ?
N1 C19 C13 112.40(13) . . ?
N1 C19 C23 110.27(12) . . ?
C13 C19 C23 113.04(13) . . ?
N1 C19 C20 101.04(11) . . ?
C13 C19 C20 112.83(12) . . ?
C23 C19 C20 106.48(12) . . ?
C7 C20 C21 117.50(13) . . ?
C7 C20 C19 117.37(13) . . ?
C21 C20 C19 101.51(12) . . ?
C20 C21 C22 101.50(13) . . ?
O1 C22 N1 111.65(13) . . ?
O1 C22 C21 110.54(12) . . ?
N1 C22 C21 102.54(12) . . ?
O1 C22 C25 107.11(13) . . ?
N1 C22 C25 115.00(12) . . ?
C21 C22 C25 109.98(13) . . ?
O3 C23 O2 123.61(16) . . ?
O3 C23 C19 125.66(16) . . ?
O2 C23 C19 110.70(14) . . ?
O4 C25 O5 124.70(16) . . ?
O4 C25 C22 121.61(15) . . ?
O5 C25 C22 113.56(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C22 N1 C1 C2 173.36(15) . . . . ?
C19 N1 C1 C2 -22.1(2) . . . . ?
C22 N1 C1 C6 -6.0(2) . . . . ?
C19 N1 C1 C6 158.53(15) . . . . ?
C6 C1 C2 C3 0.2(3) . . . . ?
N1 C1 C2 C3 -179.16(17) . . . . ?
C1 C2 C3 C4 0.1(3) . . . . ?
C2 C3 C4 C5 0.1(3) . . . . ?
C3 C4 C5 C6 -0.5(3) . . . . ?
C4 C5 C6 C1 0.9(3) . . . . ?
C2 C1 C6 C5 -0.7(2) . . . . ?
N1 C1 C6 C5 178.68(16) . . . . ?
C12 C7 C8 C9 -0.2(3) . . . . ?
C20 C7 C8 C9 -178.53(17) . . . . ?
C7 C8 C9 C10 1.0(3) . . . . ?
C8 C9 C10 C11 -1.5(3) . . . . ?
C9 C10 C11 C12 1.2(4) . . . . ?
C8 C7 C12 C11 -0.1(3) . . . . ?
C20 C7 C12 C11 178.14(18) . . . . ?
C10 C11 C12 C7 -0.4(3) . . . . ?
C18 C13 C14 C15 -1.0(3) . . . . ?
C19 C13 C14 C15 -178.00(18) . . . . ?
C13 C14 C15 C16 0.5(3) . . . . ?
C14 C15 C16 C17 0.4(4) . . . . ?
C15 C16 C17 C18 -0.8(3) . . . . ?
C16 C17 C18 C13 0.3(3) . . . . ?
C14 C13 C18 C17 0.6(3) . . . . ?
C19 C13 C18 C17 177.68(16) . . . . ?
C1 N1 C19 C13 81.83(17) . . . . ?
C22 N1 C19 C13 -112.23(14) . . . . ?
C1 N1 C19 C23 -45.30(18) . . . . ?
C22 N1 C19 C23 120.64(14) . . . . ?
C1 N1 C19 C20 -157.64(13) . . . . ?
C22 N1 C19 C20 8.30(15) . . . . ?
C18 C13 C19 N1 10.6(2) . . . . ?
C14 C13 C19 N1 -172.40(15) . . . . ?
C18 C13 C19 C23 136.26(16) . . . . ?
C14 C13 C19 C23 -46.8(2) . . . . ?
C18 C13 C19 C20 -102.84(17) . . . . ?
C14 C13 C19 C20 74.1(2) . . . . ?
C12 C7 C20 C21 -32.8(2) . . . . ?
C8 C7 C20 C21 145.51(16) . . . . ?
C12 C7 C20 C19 88.7(2) . . . . ?
C8 C7 C20 C19 -92.98(18) . . . . ?
N1 C19 C20 C7 -162.06(13) . . . . ?
C13 C19 C20 C7 -41.84(19) . . . . ?
C23 C19 C20 C7 82.74(16) . . . . ?
N1 C19 C20 C21 -32.57(14) . . . . ?
C13 C19 C20 C21 87.66(15) . . . . ?
C23 C19 C20 C21 -147.77(13) . . . . ?
C7 C20 C21 C22 173.88(13) . . . . ?
C19 C20 C21 C22 44.46(14) . . . . ?
C1 N1 C22 O1 66.62(18) . . . . ?
C19 N1 C22 O1 -99.20(15) . . . . ?
C1 N1 C22 C21 -175.02(13) . . . . ?
C19 N1 C22 C21 19.17(16) . . . . ?
C1 N1 C22 C25 -55.68(19) . . . . ?
C19 N1 C22 C25 138.51(13) . . . . ?
C20 C21 C22 O1 79.65(15) . . . . ?
C20 C21 C22 N1 -39.50(15) . . . . ?
C20 C21 C22 C25 -162.29(13) . . . . ?
C24 O2 C23 O3 -0.9(3) . . . . ?
C24 O2 C23 C19 -178.92(17) . . . . ?
N1 C19 C23 O3 140.05(19) . . . . ?
C13 C19 C23 O3 13.3(3) . . . . ?
C20 C19 C23 O3 -111.2(2) . . . . ?
N1 C19 C23 O2 -42.02(18) . . . . ?
C13 C19 C23 O2 -168.79(14) . . . . ?
C20 C19 C23 O2 66.77(17) . . . . ?
C26 O5 C25 O4 -0.3(3) . . . . ?
C26 O5 C25 C22 -176.17(15) . . . . ?
O1 C22 C25 O4 18.0(2) . . . . ?
N1 C22 C25 O4 142.71(16) . . . . ?
C21 C22 C25 O4 -102.17(18) . . . . ?
O1 C22 C25 O5 -165.94(13) . . . . ?
N1 C22 C25 O5 -41.23(19) . . . . ?
C21 C22 C25 O5 73.89(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.035