# Electronic Supplementary Material (ESI) for RSC Advances
# This journal is © The Royal Society of Chemistry 2012


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#                                CCDC 
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#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
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#  fide research purposes only. It may contain copyright material 
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data_safin21
_database_code_depnum_ccdc_archive 'CCDC 828843'
#TrackingRef 'web_deposit_cif_file_0_DamirSafin_1336409175.2a.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H16 N2 O2'
_chemical_formula_sum            'C20 H16 N2 O2'
_chemical_formula_weight         316.35

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   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   7.3048(4)
_cell_length_b                   6.2025(3)
_cell_length_c                   35.783(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.732(5)
_cell_angle_gamma                90.00
_cell_volume                     1613.17(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    297(2)
_cell_measurement_reflns_used    3684
_cell_measurement_theta_min      2.2835
_cell_measurement_theta_max      25.3978

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             664
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_min  0.96751
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      297(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'RU200 rotating anode'
_diffrn_radiation_monochromator  'Zr filter'
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method       '250 images, \D\F 0.75\%'
_diffrn_detector_area_resol_mean 6.66
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2997
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         2.92
_diffrn_reflns_theta_max         25.50
_reflns_number_total             2989
_reflns_number_gt                2258
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    PLATON
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0751P)^2^+0.0696P] 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       0.017(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         2989
_refine_ls_number_parameters     221
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0491
_refine_ls_wR_factor_ref         0.1314
_refine_ls_wR_factor_gt          0.1170
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7767(3) 0.7869(4) 0.08898(6) 0.0451(5) Uani 1 1 d . . .
H1 H 0.7283 0.9253 0.0897 0.054 Uiso 1 1 calc R . .
C2 C 0.8250(3) 0.6758(4) 0.12240(6) 0.0462(6) Uani 1 1 d . . .
C3 C 0.9032(4) 0.4690(4) 0.12101(7) 0.0525(6) Uani 1 1 d . . .
H3 H 0.9365 0.3933 0.1431 0.063 Uiso 1 1 calc R . .
C4 C 0.9303(4) 0.3788(4) 0.08666(7) 0.0523(6) Uani 1 1 d . . .
H4 H 0.9826 0.2424 0.0859 0.063 Uiso 1 1 calc R . .
C5 C 0.8813(4) 0.4872(4) 0.05355(7) 0.0482(6) Uani 1 1 d . . .
H5 H 0.9017 0.4247 0.0307 0.058 Uiso 1 1 calc R . .
C6 C 0.8004(3) 0.6923(4) 0.05443(6) 0.0450(6) Uani 1 1 d . . .
N7 N 0.7527(3) 0.8129(3) 0.02103(5) 0.0475(5) Uani 1 1 d . . .
C8 C 0.6865(3) 0.7162(4) -0.00920(7) 0.0477(6) Uani 1 1 d . . .
H8 H 0.6537 0.5718 -0.0077 0.057 Uiso 1 1 calc R . .
C9 C 0.6607(3) 0.8216(4) -0.04548(7) 0.0443(6) Uani 1 1 d . . .
C10 C 0.5872(4) 0.7076(4) -0.07747(7) 0.0507(6) Uani 1 1 d . . .
H10 H 0.5425 0.5688 -0.0746 0.061 Uiso 1 1 calc R . .
C11 C 0.5796(4) 0.7956(4) -0.11285(7) 0.0570(7) Uani 1 1 d . . .
H11 H 0.5300 0.7180 -0.1337 0.068 Uiso 1 1 calc R . .
C12 C 0.6479(4) 1.0038(4) -0.11696(7) 0.0583(7) Uani 1 1 d . . .
H12 H 0.6451 1.0637 -0.1408 0.070 Uiso 1 1 calc R . .
C13 C 0.7193(4) 1.1221(4) -0.08624(7) 0.0543(6) Uani 1 1 d . . .
H13 H 0.7651 1.2600 -0.0895 0.065 Uiso 1 1 calc R . .
C14 C 0.7228(3) 1.0350(4) -0.05039(7) 0.0463(6) Uani 1 1 d . . .
O15 O 0.7893(3) 1.1564(3) -0.02052(5) 0.0645(6) Uani 1 1 d . . .
H15 H 0.7981 1.0819 -0.0015 0.097 Uiso 1 1 calc R . .
N16 N 0.7962(3) 0.7863(3) 0.15659(5) 0.0500(5) Uani 1 1 d . . .
C17 C 0.8171(3) 0.6912(4) 0.18846(7) 0.0480(6) Uani 1 1 d . . .
H17 H 0.8543 0.5478 0.1894 0.058 Uiso 1 1 calc R . .
C18 C 0.7850(3) 0.7992(4) 0.22315(6) 0.0442(6) Uani 1 1 d . . .
C19 C 0.8152(4) 0.6897(4) 0.25738(7) 0.0545(7) Uani 1 1 d . . .
H19 H 0.8611 0.5498 0.2576 0.065 Uiso 1 1 calc R . .
C20 C 0.7785(4) 0.7841(5) 0.29085(7) 0.0633(8) Uani 1 1 d . . .
H20 H 0.8007 0.7094 0.3134 0.076 Uiso 1 1 calc R . .
C21 C 0.7077(4) 0.9927(5) 0.29028(8) 0.0650(8) Uani 1 1 d . . .
H21 H 0.6803 1.0564 0.3126 0.078 Uiso 1 1 calc R . .
C22 C 0.6777(4) 1.1063(4) 0.25704(7) 0.0560(7) Uani 1 1 d . . .
H22 H 0.6308 1.2457 0.2571 0.067 Uiso 1 1 calc R . .
C23 C 0.7172(4) 1.0131(4) 0.22347(7) 0.0477(6) Uani 1 1 d . . .
O24 O 0.6904(3) 1.1309(3) 0.19144(5) 0.0652(6) Uani 1 1 d . . .
H24 H 0.7169 1.0580 0.1736 0.098 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
C1 0.0466(13) 0.0412(12) 0.0487(14) -0.0008(11) 0.0103(11) 0.0006(11)
C2 0.0438(13) 0.0492(13) 0.0466(14) -0.0016(11) 0.0087(12) 0.0006(11)
C3 0.0566(16) 0.0498(14) 0.0514(15) 0.0018(11) 0.0067(12) 0.0064(12)
C4 0.0511(15) 0.0451(12) 0.0616(16) -0.0052(12) 0.0110(13) 0.0071(12)
C5 0.0491(14) 0.0481(13) 0.0487(14) -0.0083(11) 0.0119(12) -0.0019(12)
C6 0.0460(14) 0.0458(13) 0.0441(14) -0.0023(11) 0.0099(11) -0.0018(11)
N7 0.0511(12) 0.0505(11) 0.0421(12) -0.0040(9) 0.0104(9) 0.0015(10)
C8 0.0461(14) 0.0471(12) 0.0515(15) -0.0030(12) 0.0126(11) -0.0029(11)
C9 0.0404(13) 0.0484(13) 0.0450(14) -0.0054(11) 0.0083(11) 0.0037(11)
C10 0.0474(14) 0.0491(13) 0.0554(16) -0.0080(12) 0.0046(12) -0.0033(12)
C11 0.0571(16) 0.0667(17) 0.0456(15) -0.0109(13) -0.0021(12) 0.0085(14)
C12 0.0585(17) 0.0663(17) 0.0504(16) 0.0045(13) 0.0078(13) 0.0119(15)
C13 0.0575(16) 0.0505(13) 0.0560(16) 0.0028(12) 0.0110(13) 0.0029(13)
C14 0.0430(14) 0.0458(13) 0.0510(14) -0.0063(11) 0.0088(11) -0.0006(11)
O15 0.0878(15) 0.0488(9) 0.0560(11) -0.0081(8) 0.0030(11) -0.0099(10)
N16 0.0549(13) 0.0524(11) 0.0435(12) -0.0029(10) 0.0079(9) 0.0034(10)
C17 0.0487(15) 0.0485(13) 0.0474(14) 0.0003(11) 0.0074(11) 0.0025(11)
C18 0.0425(14) 0.0483(13) 0.0416(13) 0.0029(11) 0.0030(10) -0.0015(11)
C19 0.0578(16) 0.0544(15) 0.0506(16) 0.0066(12) 0.0031(12) 0.0005(13)
C20 0.0680(18) 0.0785(19) 0.0427(15) 0.0101(13) 0.0031(14) -0.0094(16)
C21 0.0675(19) 0.079(2) 0.0488(16) -0.0139(14) 0.0073(13) -0.0121(16)
C22 0.0562(16) 0.0588(15) 0.0534(16) -0.0065(13) 0.0071(13) 0.0000(13)
C23 0.0477(15) 0.0522(13) 0.0427(13) 0.0006(11) 0.0026(11) -0.0026(12)
O24 0.0903(15) 0.0542(9) 0.0506(11) 0.0041(9) 0.0054(11) 0.0151(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
C1 C6 1.395(3) . ?
C1 C2 1.395(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.407(3) . ?
C2 N16 1.436(3) . ?
C3 C4 1.383(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.378(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.404(3) . ?
C5 H5 0.9300 . ?
C6 N7 1.423(3) . ?
N7 C8 1.288(3) . ?
C8 C9 1.449(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.406(3) . ?
C9 C14 1.416(3) . ?
C10 C11 1.375(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.397(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.380(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.390(3) . ?
C13 H13 0.9300 . ?
C14 O15 1.357(3) . ?
O15 H15 0.8200 . ?
N16 C17 1.280(3) . ?
C17 C18 1.450(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.399(3) . ?
C18 C23 1.416(3) . ?
C19 C20 1.383(3) . ?
C19 H19 0.9300 . ?
C20 C21 1.393(4) . ?
C20 H20 0.9300 . ?
C21 C22 1.381(4) . ?
C21 H21 0.9300 . ?
C22 C23 1.389(3) . ?
C22 H22 0.9300 . ?
C23 O24 1.357(3) . ?
O24 H24 0.8200 . ?

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
C6 C1 C2 120.6(2) . . ?
C6 C1 H1 119.7 . . ?
C2 C1 H1 119.7 . . ?
C1 C2 C3 119.3(2) . . ?
C1 C2 N16 116.7(2) . . ?
C3 C2 N16 124.0(2) . . ?
C4 C3 C2 119.6(2) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C5 C4 C3 121.3(2) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C4 C5 C6 119.8(2) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C1 C6 C5 119.4(2) . . ?
C1 C6 N7 118.8(2) . . ?
C5 C6 N7 121.7(2) . . ?
C8 N7 C6 120.0(2) . . ?
N7 C8 C9 123.1(2) . . ?
N7 C8 H8 118.4 . . ?
C9 C8 H8 118.4 . . ?
C10 C9 C14 118.1(2) . . ?
C10 C9 C8 120.5(2) . . ?
C14 C9 C8 121.2(2) . . ?
C11 C10 C9 121.8(2) . . ?
C11 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
C10 C11 C12 118.8(2) . . ?
C10 C11 H11 120.6 . . ?
C12 C11 H11 120.6 . . ?
C13 C12 C11 121.2(2) . . ?
C13 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
C12 C13 C14 119.9(2) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
O15 C14 C13 118.9(2) . . ?
O15 C14 C9 121.0(2) . . ?
C13 C14 C9 120.1(2) . . ?
C14 O15 H15 109.5 . . ?
C17 N16 C2 121.64(19) . . ?
N16 C17 C18 122.3(2) . . ?
N16 C17 H17 118.8 . . ?
C18 C17 H17 118.8 . . ?
C19 C18 C23 118.2(2) . . ?
C19 C18 C17 120.0(2) . . ?
C23 C18 C17 121.7(2) . . ?
C20 C19 C18 121.7(2) . . ?
C20 C19 H19 119.2 . . ?
C18 C19 H19 119.2 . . ?
C19 C20 C21 119.0(2) . . ?
C19 C20 H20 120.5 . . ?
C21 C20 H20 120.5 . . ?
C22 C21 C20 120.9(3) . . ?
C22 C21 H21 119.6 . . ?
C20 C21 H21 119.6 . . ?
C21 C22 C23 120.2(3) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
O24 C23 C22 118.7(2) . . ?
O24 C23 C18 121.3(2) . . ?
C22 C23 C18 120.0(2) . . ?
C23 O24 H24 109.5 . . ?

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 1.8(4) . . . . ?
C6 C1 C2 N16 179.8(2) . . . . ?
C1 C2 C3 C4 -0.2(4) . . . . ?
N16 C2 C3 C4 -178.1(2) . . . . ?
C2 C3 C4 C5 -0.3(4) . . . . ?
C3 C4 C5 C6 -0.7(4) . . . . ?
C2 C1 C6 C5 -2.8(4) . . . . ?
C2 C1 C6 N7 -178.8(2) . . . . ?
C4 C5 C6 C1 2.3(4) . . . . ?
C4 C5 C6 N7 178.1(2) . . . . ?
C1 C6 N7 C8 -146.1(2) . . . . ?
C5 C6 N7 C8 38.0(4) . . . . ?
C6 N7 C8 C9 -170.4(2) . . . . ?
N7 C8 C9 C10 -179.8(2) . . . . ?
N7 C8 C9 C14 5.7(4) . . . . ?
C14 C9 C10 C11 1.9(4) . . . . ?
C8 C9 C10 C11 -172.8(2) . . . . ?
C9 C10 C11 C12 0.3(4) . . . . ?
C10 C11 C12 C13 -1.0(4) . . . . ?
C11 C12 C13 C14 -0.5(4) . . . . ?
C12 C13 C14 O15 -178.3(2) . . . . ?
C12 C13 C14 C9 2.8(4) . . . . ?
C10 C9 C14 O15 177.7(2) . . . . ?
C8 C9 C14 O15 -7.6(3) . . . . ?
C10 C9 C14 C13 -3.5(3) . . . . ?
C8 C9 C14 C13 171.2(2) . . . . ?
C1 C2 N16 C17 172.4(2) . . . . ?
C3 C2 N16 C17 -9.7(4) . . . . ?
C2 N16 C17 C18 -178.7(2) . . . . ?
N16 C17 C18 C19 -178.1(2) . . . . ?
N16 C17 C18 C23 4.1(4) . . . . ?
C23 C18 C19 C20 0.8(4) . . . . ?
C17 C18 C19 C20 -177.1(2) . . . . ?
C18 C19 C20 C21 0.7(4) . . . . ?
C19 C20 C21 C22 -1.3(4) . . . . ?
C20 C21 C22 C23 0.3(4) . . . . ?
C21 C22 C23 O24 -178.4(3) . . . . ?
C21 C22 C23 C18 1.3(4) . . . . ?
C19 C18 C23 O24 177.9(3) . . . . ?
C17 C18 C23 O24 -4.3(4) . . . . ?
C19 C18 C23 C22 -1.8(4) . . . . ?
C17 C18 C23 C22 176.1(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.060


data_safin17
_database_code_depnum_ccdc_archive 'CCDC 828844'
#TrackingRef 'web_deposit_cif_file_2_DamirSafin_1336409175.7a.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H20 N2 O2 S'
_chemical_formula_sum            'C26 H20 N2 O2 S'
_chemical_formula_weight         424.50

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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                   5.5937(3)
_cell_length_b                   42.721(3)
_cell_length_c                   8.7533(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.129(6)
_cell_angle_gamma                90.00
_cell_volume                     2079.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    297(2)
_cell_measurement_reflns_used    6280
_cell_measurement_theta_min      1.9029
_cell_measurement_theta_max      25.2090

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             888
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_T_min  0.94293
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      297(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'RU200 rotating anode'
_diffrn_radiation_monochromator  'Zr filter'
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method       '150 images, \D\F 1.5\%'
_diffrn_detector_area_resol_mean 6.66
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16858
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.39
_diffrn_reflns_theta_max         25.26
_reflns_number_total             3776
_reflns_number_gt                2959
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    PLATON
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.7038P] 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         3776
_refine_ls_number_parameters     282
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.1316
_refine_ls_wR_factor_gt          0.1208
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_restrained_S_all      0.997
_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
S1 S 1.32565(10) 0.236374(13) 0.56011(8) 0.0557(2) Uani 1 1 d . . .
C2 C 1.1512(3) 0.20551(5) 0.6256(2) 0.0420(5) Uani 1 1 d . . .
C3 C 0.9579(4) 0.20921(5) 0.7110(3) 0.0484(5) Uani 1 1 d . . .
H3 H 0.9106 0.2291 0.7384 0.058 Uiso 1 1 calc R . .
C4 C 0.8358(4) 0.18306(5) 0.7553(3) 0.0485(5) Uani 1 1 d . . .
H4 H 0.7071 0.1857 0.8130 0.058 Uiso 1 1 calc R . .
C5 C 0.9007(3) 0.15308(4) 0.7156(2) 0.0414(5) Uani 1 1 d . . .
C6 C 1.0969(4) 0.14969(5) 0.6319(2) 0.0478(5) Uani 1 1 d . . .
H6 H 1.1455 0.1298 0.6053 0.057 Uiso 1 1 calc R . .
C7 C 1.2200(4) 0.17550(5) 0.5880(2) 0.0482(5) Uani 1 1 d . . .
H7 H 1.3511 0.1728 0.5323 0.058 Uiso 1 1 calc R . .
N8 N 0.7599(3) 0.12810(4) 0.7654(2) 0.0459(4) Uani 1 1 d . . .
C9 C 0.7933(4) 0.09964(5) 0.7291(2) 0.0486(5) Uani 1 1 d . . .
H9 H 0.9171 0.0949 0.6699 0.058 Uiso 1 1 calc R . .
C10 C 0.6446(4) 0.07453(5) 0.7770(2) 0.0452(5) Uani 1 1 d . . .
C11 C 0.6917(4) 0.04360(5) 0.7383(3) 0.0579(6) Uani 1 1 d . . .
H11 H 0.8213 0.0394 0.6831 0.069 Uiso 1 1 calc R . .
C12 C 0.5512(5) 0.01909(6) 0.7796(3) 0.0649(7) Uani 1 1 d . . .
H12 H 0.5855 -0.0014 0.7528 0.078 Uiso 1 1 calc R . .
C13 C 0.3590(5) 0.02543(6) 0.8613(3) 0.0635(6) Uani 1 1 d . . .
H13 H 0.2631 0.0091 0.8895 0.076 Uiso 1 1 calc R . .
C14 C 0.3072(4) 0.05566(6) 0.9017(3) 0.0584(6) Uani 1 1 d . . .
H14 H 0.1774 0.0595 0.9571 0.070 Uiso 1 1 calc R . .
C15 C 0.4479(4) 0.08034(5) 0.8602(2) 0.0485(5) Uani 1 1 d . . .
O16 O 0.3921(3) 0.10960(4) 0.9010(2) 0.0627(4) Uani 1 1 d . . .
H16 H 0.4903 0.1219 0.8723 0.094 Uiso 1 1 calc R . .
C17 C 1.1826(4) 0.27101(5) 0.6165(2) 0.0462(5) Uani 1 1 d . . .
C18 C 0.9666(4) 0.28132(5) 0.5397(3) 0.0543(5) Uani 1 1 d . . .
H18 H 0.8900 0.2693 0.4604 0.065 Uiso 1 1 calc R . .
C19 C 0.8649(4) 0.30900(5) 0.5795(3) 0.0548(6) Uani 1 1 d . . .
H19 H 0.7201 0.3156 0.5272 0.066 Uiso 1 1 calc R . .
C20 C 0.9780(4) 0.32730(5) 0.6981(2) 0.0438(5) Uani 1 1 d . . .
C21 C 1.1937(4) 0.31697(5) 0.7740(3) 0.0519(5) Uani 1 1 d . . .
H21 H 1.2712 0.3290 0.8530 0.062 Uiso 1 1 calc R . .
C22 C 1.2953(4) 0.28909(5) 0.7338(3) 0.0523(5) Uani 1 1 d . . .
H22 H 1.4401 0.2825 0.7858 0.063 Uiso 1 1 calc R . .
N23 N 0.8899(3) 0.35591(4) 0.7505(2) 0.0483(4) Uani 1 1 d . . .
C24 C 0.6936(4) 0.36849(5) 0.6920(3) 0.0507(5) Uani 1 1 d . . .
H24 H 0.6018 0.3584 0.6120 0.061 Uiso 1 1 calc R . .
C25 C 0.6109(4) 0.39801(5) 0.7471(2) 0.0482(5) Uani 1 1 d . . .
C26 C 0.3969(4) 0.41108(6) 0.6798(3) 0.0624(6) Uani 1 1 d . . .
H26 H 0.3047 0.4001 0.6028 0.075 Uiso 1 1 calc R . .
C27 C 0.3189(5) 0.43990(6) 0.7251(3) 0.0699(7) Uani 1 1 d . . .
H27 H 0.1776 0.4485 0.6774 0.084 Uiso 1 1 calc R . .
C28 C 0.4532(5) 0.45577(6) 0.8420(3) 0.0715(7) Uani 1 1 d . . .
H28 H 0.4006 0.4751 0.8734 0.086 Uiso 1 1 calc R . .
C29 C 0.6631(5) 0.44341(6) 0.9126(3) 0.0667(7) Uani 1 1 d . . .
H29 H 0.7511 0.4543 0.9915 0.080 Uiso 1 1 calc R . .
C30 C 0.7438(4) 0.41461(5) 0.8661(3) 0.0530(5) Uani 1 1 d . . .
O31 O 0.9496(3) 0.40269(4) 0.9383(2) 0.0709(5) Uani 1 1 d . . .
H31 H 0.9879 0.3870 0.8926 0.106 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
S1 0.0486(3) 0.0446(3) 0.0761(4) 0.0036(3) 0.0168(3) 0.0002(2)
C2 0.0393(10) 0.0421(11) 0.0430(11) 0.0008(8) -0.0034(8) 0.0017(8)
C3 0.0457(11) 0.0393(11) 0.0609(14) -0.0042(9) 0.0094(10) 0.0033(9)
C4 0.0440(11) 0.0440(11) 0.0586(13) -0.0045(9) 0.0108(10) 0.0034(9)
C5 0.0418(10) 0.0399(10) 0.0412(11) 0.0004(8) -0.0019(8) 0.0005(8)
C6 0.0550(12) 0.0361(10) 0.0529(13) -0.0034(9) 0.0083(10) 0.0049(9)
C7 0.0472(11) 0.0476(12) 0.0505(12) -0.0029(9) 0.0091(9) 0.0042(9)
N8 0.0471(9) 0.0409(9) 0.0489(10) 0.0004(7) 0.0006(8) -0.0010(7)
C9 0.0478(12) 0.0479(12) 0.0496(12) -0.0005(9) 0.0035(9) 0.0005(9)
C10 0.0453(11) 0.0441(11) 0.0446(11) 0.0023(9) -0.0030(9) -0.0014(9)
C11 0.0620(14) 0.0446(12) 0.0677(15) -0.0032(11) 0.0093(12) 0.0011(10)
C12 0.0736(16) 0.0407(12) 0.0798(17) 0.0003(11) 0.0051(14) -0.0039(11)
C13 0.0649(15) 0.0547(14) 0.0692(16) 0.0110(12) -0.0003(13) -0.0142(12)
C14 0.0525(13) 0.0595(14) 0.0632(15) 0.0068(11) 0.0067(11) -0.0030(11)
C15 0.0492(12) 0.0456(12) 0.0490(12) 0.0050(9) -0.0017(10) 0.0030(9)
O16 0.0641(10) 0.0494(9) 0.0774(12) 0.0004(8) 0.0198(9) 0.0029(8)
C17 0.0442(11) 0.0425(11) 0.0520(12) 0.0078(9) 0.0058(9) -0.0035(9)
C18 0.0548(13) 0.0471(12) 0.0581(14) -0.0077(10) -0.0070(11) -0.0013(10)
C19 0.0499(12) 0.0534(13) 0.0576(14) -0.0033(11) -0.0105(10) 0.0059(10)
C20 0.0481(11) 0.0389(11) 0.0440(11) 0.0057(8) 0.0032(9) -0.0031(9)
C21 0.0520(12) 0.0501(12) 0.0509(13) -0.0011(10) -0.0068(10) -0.0051(10)
C22 0.0455(11) 0.0509(12) 0.0580(14) 0.0071(10) -0.0055(10) 0.0006(10)
N23 0.0532(10) 0.0447(10) 0.0461(10) 0.0039(8) 0.0006(8) 0.0007(8)
C24 0.0561(13) 0.0488(12) 0.0465(12) 0.0022(10) 0.0018(10) -0.0027(10)
C25 0.0558(13) 0.0427(11) 0.0464(12) 0.0066(9) 0.0067(10) -0.0014(9)
C26 0.0620(14) 0.0619(15) 0.0613(15) 0.0006(12) -0.0030(12) 0.0057(12)
C27 0.0713(16) 0.0619(15) 0.0757(18) 0.0050(13) 0.0035(14) 0.0187(13)
C28 0.092(2) 0.0529(14) 0.0708(17) 0.0009(12) 0.0149(15) 0.0148(14)
C29 0.0880(19) 0.0509(14) 0.0602(16) -0.0046(11) 0.0038(14) -0.0013(12)
C30 0.0608(14) 0.0505(13) 0.0474(12) 0.0071(10) 0.0037(11) 0.0001(10)
O31 0.0741(12) 0.0639(11) 0.0695(12) -0.0094(9) -0.0162(9) 0.0055(9)

_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
S1 C2 1.772(2) . ?
S1 C17 1.777(2) . ?
C2 C3 1.388(3) . ?
C2 C7 1.388(3) . ?
C3 C4 1.386(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.385(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.391(3) . ?
C5 N8 1.422(3) . ?
C6 C7 1.376(3) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
N8 C9 1.276(3) . ?
C9 C10 1.447(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.397(3) . ?
C10 C15 1.405(3) . ?
C11 C12 1.380(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.381(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.378(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.387(3) . ?
C14 H14 0.9300 . ?
C15 O16 1.346(3) . ?
O16 H16 0.8200 . ?
C17 C22 1.382(3) . ?
C17 C18 1.390(3) . ?
C18 C19 1.373(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.396(3) . ?
C19 H19 0.9300 . ?
C20 C21 1.386(3) . ?
C20 N23 1.412(3) . ?
C21 C22 1.381(3) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
N23 C24 1.279(3) . ?
C24 C25 1.444(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.393(3) . ?
C25 C30 1.406(3) . ?
C26 C27 1.378(3) . ?
C26 H26 0.9300 . ?
C27 C28 1.381(4) . ?
C27 H27 0.9300 . ?
C28 C29 1.372(4) . ?
C28 H28 0.9300 . ?
C29 C30 1.387(3) . ?
C29 H29 0.9300 . ?
C30 O31 1.352(3) . ?
O31 H31 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 S1 C17 104.48(10) . . ?
C3 C2 C7 118.98(18) . . ?
C3 C2 S1 125.24(15) . . ?
C7 C2 S1 115.78(15) . . ?
C4 C3 C2 119.61(19) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C5 C4 C3 121.68(19) . . ?
C5 C4 H4 119.2 . . ?
C3 C4 H4 119.2 . . ?
C4 C5 C6 118.09(18) . . ?
C4 C5 N8 116.65(18) . . ?
C6 C5 N8 125.25(18) . . ?
C7 C6 C5 120.65(19) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C7 C2 120.97(19) . . ?
C6 C7 H7 119.5 . . ?
C2 C7 H7 119.5 . . ?
C9 N8 C5 122.55(18) . . ?
N8 C9 C10 122.0(2) . . ?
N8 C9 H9 119.0 . . ?
C10 C9 H9 119.0 . . ?
C11 C10 C15 118.14(19) . . ?
C11 C10 C9 120.1(2) . . ?
C15 C10 C9 121.72(19) . . ?
C12 C11 C10 121.8(2) . . ?
C12 C11 H11 119.1 . . ?
C10 C11 H11 119.1 . . ?
C13 C12 C11 118.9(2) . . ?
C13 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
C14 C13 C12 120.9(2) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C13 C14 C15 120.3(2) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
O16 C15 C14 118.8(2) . . ?
O16 C15 C10 121.23(19) . . ?
C14 C15 C10 119.9(2) . . ?
C15 O16 H16 109.5 . . ?
C22 C17 C18 119.1(2) . . ?
C22 C17 S1 119.25(16) . . ?
C18 C17 S1 121.55(17) . . ?
C19 C18 C17 120.8(2) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C18 C19 C20 120.2(2) . . ?
C18 C19 H19 119.9 . . ?
C20 C19 H19 119.9 . . ?
C21 C20 C19 118.71(19) . . ?
C21 C20 N23 115.86(18) . . ?
C19 C20 N23 125.43(19) . . ?
C22 C21 C20 120.9(2) . . ?
C22 C21 H21 119.6 . . ?
C20 C21 H21 119.6 . . ?
C21 C22 C17 120.3(2) . . ?
C21 C22 H22 119.9 . . ?
C17 C22 H22 119.9 . . ?
C24 N23 C20 123.23(19) . . ?
N23 C24 C25 121.7(2) . . ?
N23 C24 H24 119.1 . . ?
C25 C24 H24 119.1 . . ?
C26 C25 C30 118.3(2) . . ?
C26 C25 C24 120.1(2) . . ?
C30 C25 C24 121.7(2) . . ?
C27 C26 C25 121.4(2) . . ?
C27 C26 H26 119.3 . . ?
C25 C26 H26 119.3 . . ?
C28 C27 C26 119.2(2) . . ?
C28 C27 H27 120.4 . . ?
C26 C27 H27 120.4 . . ?
C29 C28 C27 121.1(2) . . ?
C29 C28 H28 119.5 . . ?
C27 C28 H28 119.5 . . ?
C28 C29 C30 119.9(2) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
O31 C30 C29 119.0(2) . . ?
O31 C30 C25 120.9(2) . . ?
C29 C30 C25 120.1(2) . . ?
C30 O31 H31 109.5 . . ?

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
C17 S1 C2 C3 -4.0(2) . . . . ?
C17 S1 C2 C7 176.77(16) . . . . ?
C7 C2 C3 C4 -0.8(3) . . . . ?
S1 C2 C3 C4 179.98(16) . . . . ?
C2 C3 C4 C5 -0.4(3) . . . . ?
C3 C4 C5 C6 1.3(3) . . . . ?
C3 C4 C5 N8 -179.05(19) . . . . ?
C4 C5 C6 C7 -1.0(3) . . . . ?
N8 C5 C6 C7 179.38(19) . . . . ?
C5 C6 C7 C2 -0.2(3) . . . . ?
C3 C2 C7 C6 1.1(3) . . . . ?
S1 C2 C7 C6 -179.61(17) . . . . ?
C4 C5 N8 C9 176.1(2) . . . . ?
C6 C5 N8 C9 -4.3(3) . . . . ?
C5 N8 C9 C10 -178.28(18) . . . . ?
N8 C9 C10 C11 -178.2(2) . . . . ?
N8 C9 C10 C15 3.1(3) . . . . ?
C15 C10 C11 C12 0.0(3) . . . . ?
C9 C10 C11 C12 -178.8(2) . . . . ?
C10 C11 C12 C13 0.0(4) . . . . ?
C11 C12 C13 C14 -0.1(4) . . . . ?
C12 C13 C14 C15 0.2(4) . . . . ?
C13 C14 C15 O16 179.8(2) . . . . ?
C13 C14 C15 C10 -0.2(3) . . . . ?
C11 C10 C15 O16 -179.9(2) . . . . ?
C9 C10 C15 O16 -1.1(3) . . . . ?
C11 C10 C15 C14 0.1(3) . . . . ?
C9 C10 C15 C14 178.9(2) . . . . ?
C2 S1 C17 C22 109.14(18) . . . . ?
C2 S1 C17 C18 -74.6(2) . . . . ?
C22 C17 C18 C19 -0.2(3) . . . . ?
S1 C17 C18 C19 -176.49(18) . . . . ?
C17 C18 C19 C20 0.1(4) . . . . ?
C18 C19 C20 C21 0.1(3) . . . . ?
C18 C19 C20 N23 -179.2(2) . . . . ?
C19 C20 C21 C22 -0.2(3) . . . . ?
N23 C20 C21 C22 179.18(19) . . . . ?
C20 C21 C22 C17 0.1(3) . . . . ?
C18 C17 C22 C21 0.2(3) . . . . ?
S1 C17 C22 C21 176.49(17) . . . . ?
C21 C20 N23 C24 179.9(2) . . . . ?
C19 C20 N23 C24 -0.8(3) . . . . ?
C20 N23 C24 C25 -179.08(18) . . . . ?
N23 C24 C25 C26 179.6(2) . . . . ?
N23 C24 C25 C30 1.0(3) . . . . ?
C30 C25 C26 C27 1.7(4) . . . . ?
C24 C25 C26 C27 -177.0(2) . . . . ?
C25 C26 C27 C28 -1.5(4) . . . . ?
C26 C27 C28 C29 0.5(4) . . . . ?
C27 C28 C29 C30 0.3(4) . . . . ?
C28 C29 C30 O31 -179.3(2) . . . . ?
C28 C29 C30 C25 -0.1(4) . . . . ?
C26 C25 C30 O31 178.3(2) . . . . ?
C24 C25 C30 O31 -3.1(3) . . . . ?
C26 C25 C30 C29 -0.9(3) . . . . ?
C24 C25 C30 C29 177.8(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.075


data_safin38
_database_code_depnum_ccdc_archive 'CCDC 828845'
#TrackingRef 'web_deposit_cif_file_3_DamirSafin_1336409175.8a.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H20 N2 O4 S'
_chemical_formula_sum            'C26 H20 N2 O4 S'
_chemical_formula_weight         456.50

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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

_cell_length_a                   35.744(7)
_cell_length_b                   4.8494(11)
_cell_length_c                   12.392(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.97(2)
_cell_angle_gamma                90.00
_cell_volume                     2132.1(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    297(2)
_cell_measurement_reflns_used    1293
_cell_measurement_theta_min      1.8929
_cell_measurement_theta_max      25.1882

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             952
_exptl_absorpt_coefficient_mu    0.190
_exptl_absorpt_correction_T_min  0.37224
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      297(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'RU200 rotating anode'
_diffrn_radiation_monochromator  'Zr filter'
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method       '70 images, \D\F 3.1\%'
_diffrn_detector_area_resol_mean 6.66
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7907
_diffrn_reflns_av_R_equivalents  0.0958
_diffrn_reflns_av_sigmaI/netI    0.0699
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.31
_diffrn_reflns_theta_max         25.24
_reflns_number_total             1918
_reflns_number_gt                1412
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    PLATON
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+1.1435P] 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         1918
_refine_ls_number_parameters     150
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0530
_refine_ls_wR_factor_ref         0.1350
_refine_ls_wR_factor_gt          0.1213
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_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
S1 S 0.0000 0.57018(18) 0.2500 0.0333(3) Uani 1 2 d S . .
O2 O -0.01488(5) 0.7178(4) 0.15363(15) 0.0430(5) Uani 1 1 d . . .
O18 O 0.14503(7) -0.4736(5) -0.02649(16) 0.0670(7) Uani 1 1 d . . .
H18 H 0.1313 -0.3698 0.0005 0.100 Uiso 1 1 d R . .
N10 N 0.11597(6) -0.2176(4) 0.12828(18) 0.0373(6) Uani 1 1 d . . .
C4 C 0.03584(7) 0.3468(5) 0.2149(2) 0.0304(6) Uani 1 1 d . . .
C5 C 0.03495(8) 0.2537(5) 0.1086(2) 0.0389(7) Uani 1 1 d . . .
H5 H 0.0161 0.3124 0.0552 0.047 Uiso 1 1 calc R . .
C6 C 0.06239(8) 0.0730(6) 0.0834(2) 0.0395(7) Uani 1 1 d . . .
H6 H 0.0624 0.0156 0.0118 0.047 Uiso 1 1 calc R . .
C7 C 0.08980(7) -0.0243(5) 0.1621(2) 0.0329(6) Uani 1 1 d . . .
C8 C 0.09090(7) 0.0765(6) 0.2684(2) 0.0386(6) Uani 1 1 d . . .
H8 H 0.1098 0.0183 0.3219 0.046 Uiso 1 1 calc R . .
C9 C 0.06406(7) 0.2617(5) 0.2941(2) 0.0370(6) Uani 1 1 d . . .
H9 H 0.0650 0.3293 0.3646 0.044 Uiso 1 1 calc R . .
C11 C 0.13711(7) -0.3639(5) 0.1968(2) 0.0375(6) Uani 1 1 d . . .
H11 H 0.1352 -0.3432 0.2705 0.045 Uiso 1 1 calc R . .
C12 C 0.16389(7) -0.5609(5) 0.1628(2) 0.0354(6) Uani 1 1 d . . .
C13 C 0.18691(8) -0.7121(6) 0.2408(2) 0.0446(7) Uani 1 1 d . . .
H13 H 0.1849 -0.6835 0.3140 0.054 Uiso 1 1 calc R . .
C14 C 0.21237(8) -0.9010(6) 0.2120(3) 0.0533(8) Uani 1 1 d . . .
H14 H 0.2276 -0.9987 0.2650 0.064 Uiso 1 1 calc R . .
C15 C 0.21510(9) -0.9443(7) 0.1028(3) 0.0591(9) Uani 1 1 d . . .
H15 H 0.2324 -1.0721 0.0825 0.071 Uiso 1 1 calc R . .
C16 C 0.19272(9) -0.8017(7) 0.0239(3) 0.0590(9) Uani 1 1 d . . .
H16 H 0.1949 -0.8334 -0.0491 0.071 Uiso 1 1 calc R . .
C17 C 0.16678(8) -0.6100(6) 0.0528(2) 0.0442(7) 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
S1 0.0339(5) 0.0271(5) 0.0401(6) 0.000 0.0094(4) 0.000
O2 0.0492(12) 0.0338(11) 0.0473(11) 0.0124(9) 0.0120(9) 0.0071(8)
O18 0.0774(16) 0.0819(17) 0.0425(12) 0.0012(12) 0.0114(11) 0.0308(13)
N10 0.0335(12) 0.0368(13) 0.0429(13) -0.0004(11) 0.0091(10) 0.0034(10)
C4 0.0312(13) 0.0258(13) 0.0357(14) 0.0024(11) 0.0094(11) -0.0023(10)
C5 0.0418(16) 0.0411(16) 0.0325(15) -0.0003(13) -0.0002(12) 0.0088(12)
C6 0.0455(16) 0.0410(15) 0.0328(14) -0.0055(13) 0.0082(12) 0.0068(13)
C7 0.0287(13) 0.0336(14) 0.0376(14) 0.0001(12) 0.0087(11) -0.0017(11)
C8 0.0346(14) 0.0435(16) 0.0367(15) 0.0012(13) -0.0001(11) 0.0042(13)
C9 0.0372(15) 0.0408(15) 0.0330(14) -0.0027(13) 0.0045(12) 0.0021(12)
C11 0.0366(15) 0.0353(15) 0.0414(15) -0.0006(13) 0.0083(12) -0.0015(12)
C12 0.0297(13) 0.0317(14) 0.0454(16) -0.0003(13) 0.0065(12) -0.0008(11)
C13 0.0388(16) 0.0432(17) 0.0519(18) -0.0013(14) 0.0055(13) 0.0012(13)
C14 0.0385(17) 0.0452(17) 0.075(2) 0.0023(18) 0.0033(15) 0.0050(14)
C15 0.0425(18) 0.0485(19) 0.090(3) -0.0091(19) 0.0214(17) 0.0103(15)
C16 0.061(2) 0.061(2) 0.059(2) -0.0107(18) 0.0220(17) 0.0117(17)
C17 0.0425(16) 0.0446(16) 0.0466(17) -0.0012(15) 0.0104(13) 0.0038(13)

_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
S1 O2 1.4378(18) 2 ?
S1 O2 1.4378(18) . ?
S1 C4 1.772(2) . ?
S1 C4 1.772(2) 2 ?
O18 C17 1.349(3) . ?
O18 H18 0.8033 . ?
N10 C11 1.280(3) . ?
N10 C7 1.423(3) . ?
C4 C9 1.382(3) . ?
C4 C5 1.389(3) . ?
C5 C6 1.379(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.379(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.401(4) . ?
C8 C9 1.379(4) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C11 C12 1.451(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.398(4) . ?
C12 C17 1.400(4) . ?
C13 C14 1.369(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.385(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.372(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.390(4) . ?
C16 H16 0.9300 . ?

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
O2 S1 O2 120.29(16) 2 . ?
O2 S1 C4 107.60(11) 2 . ?
O2 S1 C4 107.84(11) . . ?
O2 S1 C4 107.84(11) 2 2 ?
O2 S1 C4 107.60(11) . 2 ?
C4 S1 C4 104.63(15) . 2 ?
C17 O18 H18 109.4 . . ?
C11 N10 C7 121.7(2) . . ?
C9 C4 C5 120.4(2) . . ?
C9 C4 S1 119.74(19) . . ?
C5 C4 S1 119.81(19) . . ?
C6 C5 C4 119.1(2) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C7 C6 C5 121.4(2) . . ?
C7 C6 H6 119.3 . . ?
C5 C6 H6 119.3 . . ?
C6 C7 C8 118.8(2) . . ?
C6 C7 N10 116.9(2) . . ?
C8 C7 N10 124.2(2) . . ?
C9 C8 C7 120.2(2) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C8 C9 C4 120.0(2) . . ?
C8 C9 H9 120.0 . . ?
C4 C9 H9 120.0 . . ?
N10 C11 C12 122.0(2) . . ?
N10 C11 H11 119.0 . . ?
C12 C11 H11 119.0 . . ?
C13 C12 C17 118.5(2) . . ?
C13 C12 C11 119.9(2) . . ?
C17 C12 C11 121.6(2) . . ?
C14 C13 C12 121.7(3) . . ?
C14 C13 H13 119.2 . . ?
C12 C13 H13 119.2 . . ?
C13 C14 C15 118.9(3) . . ?
C13 C14 H14 120.5 . . ?
C15 C14 H14 120.5 . . ?
C16 C15 C14 121.0(3) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 C17 120.2(3) . . ?
C15 C16 H16 119.9 . . ?
C17 C16 H16 119.9 . . ?
O18 C17 C16 118.9(3) . . ?
O18 C17 C12 121.4(2) . . ?
C16 C17 C12 119.6(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 S1 C4 C9 24.1(2) 2 . . . ?
O2 S1 C4 C9 155.3(2) . . . . ?
C4 S1 C4 C9 -90.4(2) 2 . . . ?
O2 S1 C4 C5 -157.3(2) 2 . . . ?
O2 S1 C4 C5 -26.1(2) . . . . ?
C4 S1 C4 C5 88.2(2) 2 . . . ?
C9 C4 C5 C6 0.6(4) . . . . ?
S1 C4 C5 C6 -178.0(2) . . . . ?
C4 C5 C6 C7 2.4(4) . . . . ?
C5 C6 C7 C8 -3.9(4) . . . . ?
C5 C6 C7 N10 177.8(2) . . . . ?
C11 N10 C7 C6 -164.8(2) . . . . ?
C11 N10 C7 C8 16.9(4) . . . . ?
C6 C7 C8 C9 2.4(4) . . . . ?
N10 C7 C8 C9 -179.3(2) . . . . ?
C7 C8 C9 C4 0.4(4) . . . . ?
C5 C4 C9 C8 -2.0(4) . . . . ?
S1 C4 C9 C8 176.6(2) . . . . ?
C7 N10 C11 C12 -179.9(2) . . . . ?
N10 C11 C12 C13 178.7(2) . . . . ?
N10 C11 C12 C17 -2.9(4) . . . . ?
C17 C12 C13 C14 1.2(4) . . . . ?
C11 C12 C13 C14 179.6(3) . . . . ?
C12 C13 C14 C15 -0.5(4) . . . . ?
C13 C14 C15 C16 -0.1(5) . . . . ?
C14 C15 C16 C17 0.0(5) . . . . ?
C15 C16 C17 O18 -179.7(3) . . . . ?
C15 C16 C17 C12 0.7(5) . . . . ?
C13 C12 C17 O18 179.1(3) . . . . ?
C11 C12 C17 O18 0.8(4) . . . . ?
C13 C12 C17 C16 -1.3(4) . . . . ?
C11 C12 C17 C16 -179.7(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.051




data_safin31
_database_code_depnum_ccdc_archive 'CCDC 830149'
#TrackingRef 'web_deposit_cif_file_0_DamirSafin_1308220361.UCL089_safin31.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H10 Br2 N2 O2'
_chemical_formula_sum            'C14 H10 Br2 N2 O2'
_chemical_formula_weight         398.06

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'
Br Br -0.2901 2.4595 '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'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.4795(16)
_cell_length_b                   7.343(2)
_cell_length_c                   7.8656(12)
_cell_angle_alpha                78.621(17)
_cell_angle_beta                 79.482(16)
_cell_angle_gamma                73.05(2)
_cell_volume                     347.83(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    297(2)
_cell_measurement_reflns_used    2088
_cell_measurement_theta_min      2.9286
_cell_measurement_theta_max      25.4054

_exptl_crystal_description       plate
_exptl_crystal_colour            translucent
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.900
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             194
_exptl_absorpt_coefficient_mu    5.828
_exptl_absorpt_correction_T_min  0.64923
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      297(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'RU200 rotating anode'
_diffrn_radiation_monochromator  'Zr filter'
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method       '100 images, \D\F 3.0\%'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3579
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0514
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.93
_diffrn_reflns_theta_max         25.46
_reflns_number_total             1202
_reflns_number_gt                971
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       MAR
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1143P)^2^+0.1062P] 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         1202
_refine_ls_number_parameters     92
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0621
_refine_ls_wR_factor_ref         0.1714
_refine_ls_wR_factor_gt          0.1599
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_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
Br1 Br 0.33958(7) 0.82886(7) 0.13073(5) 0.07355(17) Uani 1 1 d . . .
C2 C 0.1216(6) 0.7952(5) 0.3228(5) 0.0487(9) Uani 1 1 d . . .
C3 C 0.1782(6) 0.7113(5) 0.4861(5) 0.0489(9) Uani 1 1 d . . .
H3 H 0.3239 0.6753 0.5030 0.059 Uiso 1 1 calc R . .
C4 C 0.0220(6) 0.6796(5) 0.6255(5) 0.0480(9) Uani 1 1 d . . .
C5 C -0.1987(6) 0.7378(5) 0.5970(5) 0.0493(9) Uani 1 1 d . . .
C6 C -0.2538(7) 0.8268(5) 0.4327(6) 0.0561(10) Uani 1 1 d . . .
H6 H -0.3993 0.8673 0.4148 0.067 Uiso 1 1 calc R . .
C7 C -0.0946(7) 0.8556(5) 0.2956(5) 0.0552(10) Uani 1 1 d . . .
H7 H -0.1323 0.9153 0.1857 0.066 Uiso 1 1 calc R . .
O8 O -0.3614(5) 0.7082(5) 0.7236(4) 0.0672(9) Uani 1 1 d . . .
H8 H -0.3105 0.6489 0.8129 0.101 Uiso 1 1 calc R . .
C9 C 0.0881(6) 0.5865(5) 0.7957(5) 0.0482(9) Uani 1 1 d . . .
H9 H 0.2344 0.5549 0.8099 0.058 Uiso 1 1 calc R . .
N10 N -0.0477(5) 0.5477(4) 0.9243(4) 0.0530(8) 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
Br1 0.0724(3) 0.0987(3) 0.0484(3) 0.0116(2) -0.0057(2) -0.0375(2)
C2 0.060(2) 0.0499(16) 0.0385(17) -0.0022(13) -0.0048(15) -0.0211(14)
C3 0.0532(18) 0.0591(17) 0.0385(17) 0.0012(14) -0.0130(14) -0.0226(15)
C4 0.060(2) 0.0440(14) 0.0436(17) -0.0053(13) -0.0102(15) -0.0190(14)
C5 0.056(2) 0.0463(15) 0.0460(19) -0.0094(14) -0.0036(16) -0.0153(14)
C6 0.057(2) 0.0519(17) 0.061(2) -0.0058(15) -0.0194(17) -0.0108(16)
C7 0.066(2) 0.0519(17) 0.049(2) -0.0041(15) -0.0182(17) -0.0143(16)
O8 0.0520(16) 0.0861(17) 0.0588(17) -0.0088(14) -0.0028(14) -0.0157(14)
C9 0.0493(18) 0.0538(16) 0.0433(17) -0.0059(14) -0.0095(15) -0.0156(14)
N10 0.0594(18) 0.0594(15) 0.0433(15) -0.0090(12) -0.0094(14) -0.0183(14)

_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
Br1 C2 1.901(4) . ?
C2 C3 1.376(5) . ?
C2 C7 1.383(6) . ?
C3 C4 1.383(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.415(6) . ?
C4 C9 1.457(5) . ?
C5 O8 1.347(5) . ?
C5 C6 1.387(5) . ?
C6 C7 1.379(6) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
O8 H8 0.8200 . ?
C9 N10 1.259(5) . ?
C9 H9 0.9300 . ?
N10 N10 1.407(6) 2_567 ?

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
C3 C2 C7 120.5(4) . . ?
C3 C2 Br1 120.4(3) . . ?
C7 C2 Br1 119.0(3) . . ?
C2 C3 C4 121.0(4) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C3 C4 C5 118.4(3) . . ?
C3 C4 C9 119.6(4) . . ?
C5 C4 C9 121.9(3) . . ?
O8 C5 C6 117.5(4) . . ?
O8 C5 C4 122.6(3) . . ?
C6 C5 C4 119.8(4) . . ?
C7 C6 C5 120.5(4) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C7 C2 119.6(4) . . ?
C6 C7 H7 120.2 . . ?
C2 C7 H7 120.2 . . ?
C5 O8 H8 109.5 . . ?
N10 C9 C4 121.7(4) . . ?
N10 C9 H9 119.2 . . ?
C4 C9 H9 119.2 . . ?
C9 N10 N10 113.4(4) . 2_567 ?

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
C7 C2 C3 C4 2.1(5) . . . . ?
Br1 C2 C3 C4 -177.6(3) . . . . ?
C2 C3 C4 C5 -0.8(5) . . . . ?
C2 C3 C4 C9 178.6(3) . . . . ?
C3 C4 C5 O8 178.2(3) . . . . ?
C9 C4 C5 O8 -1.2(5) . . . . ?
C3 C4 C5 C6 -0.9(5) . . . . ?
C9 C4 C5 C6 179.7(3) . . . . ?
O8 C5 C6 C7 -177.9(3) . . . . ?
C4 C5 C6 C7 1.3(6) . . . . ?
C5 C6 C7 C2 0.0(6) . . . . ?
C3 C2 C7 C6 -1.7(6) . . . . ?
Br1 C2 C7 C6 178.1(3) . . . . ?
C3 C4 C9 N10 -177.0(3) . . . . ?
C5 C4 C9 N10 2.3(5) . . . . ?
C4 C9 N10 N10 178.0(3) . . . 2_567 ?

_diffrn_measured_fraction_theta_max 0.930
_diffrn_reflns_theta_full        25.46
_diffrn_measured_fraction_theta_full 0.930
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.134




data_safin15_3
_database_code_depnum_ccdc_archive 'CCDC 840365'
#TrackingRef 'web_deposit_cif_file_1_DamirSafin_1336409175.6a.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H20 N2 O3'
_chemical_formula_sum            'C26 H20 N2 O3'
_chemical_formula_weight         408.44

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   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   6.0244(6)
_cell_length_b                   46.278(3)
_cell_length_c                   9.4342(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 129.701(17)
_cell_angle_gamma                90.00
_cell_volume                     2023.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2598
_cell_measurement_theta_min      2.6354
_cell_measurement_theta_max      18.7428

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             856
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_min  0.78999
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'RU200 rotating anode'
_diffrn_radiation_monochromator  'Zr filter'
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method       '360 images, \D\F 0.5\%'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            1392
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.64
_diffrn_reflns_theta_max         18.00
_reflns_number_total             1392
_reflns_number_gt                1234
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       MAR
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1708P)^2^+1.2736P] 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         1392
_refine_ls_number_parameters     281
_refine_ls_number_restraints     247
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0841
_refine_ls_wR_factor_ref         0.2251
_refine_ls_wR_factor_gt          0.2193
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_restrained_S_all      1.027
_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 -0.4564(3) 0.39132(3) 0.26939(18) 0.0521(6) Uani 1 1 d U . .
H1 H -0.3690 0.3763 0.2883 0.078 Uiso 1 1 calc R . .
O16 O 0.3624(2) 0.25000(3) 0.35304(16) 0.0270(5) Uani 1 1 d U . .
O31 O -0.2879(3) 0.10983(3) 0.44084(17) 0.0461(6) Uani 1 1 d U . .
H31 H -0.2506 0.1247 0.4126 0.069 Uiso 1 1 calc R . .
N9 N -0.0285(3) 0.35853(4) 0.36503(19) 0.0293(6) Uani 1 1 d U . .
N23 N -0.0547(3) 0.14159(3) 0.33921(19) 0.0232(6) Uani 1 1 d U . .
C2 C -0.2846(3) 0.41401(5) 0.3124(2) 0.0252(7) Uani 1 1 d U . .
C3 C -0.3902(4) 0.44154(5) 0.2829(3) 0.0384(8) Uani 1 1 d U . .
H3 H -0.5825 0.4442 0.2292 0.046 Uiso 1 1 calc R . .
C4 C -0.2177(4) 0.46522(6) 0.3311(3) 0.0483(9) Uani 1 1 d U . .
H4 H -0.2928 0.4837 0.3113 0.058 Uiso 1 1 calc R . .
C5 C 0.0680(4) 0.46155(5) 0.4090(3) 0.0431(9) Uani 1 1 d U . .
H5 H 0.1859 0.4776 0.4446 0.052 Uiso 1 1 calc R . .
C6 C 0.1767(4) 0.43468(5) 0.4338(2) 0.0325(8) Uani 1 1 d U . .
H6 H 0.3677 0.4326 0.4833 0.039 Uiso 1 1 calc R . .
C7 C 0.0069(4) 0.40966(5) 0.3864(2) 0.0218(7) Uani 1 1 d U . .
C8 C 0.1127(4) 0.38160(4) 0.3984(2) 0.0263(7) Uani 1 1 d U . .
H8 H 0.2950 0.3800 0.4324 0.032 Uiso 1 1 calc R . .
C10 C 0.0744(4) 0.33138(4) 0.3642(2) 0.0178(7) Uani 1 1 d U . .
C11 C 0.1985(4) 0.32640(5) 0.2799(2) 0.0261(7) Uani 1 1 d U . .
H11 H 0.2219 0.3417 0.2266 0.031 Uiso 1 1 calc R . .
C12 C 0.2838(3) 0.29932(5) 0.2761(2) 0.0223(7) Uani 1 1 d U . .
H12 H 0.3649 0.2965 0.2202 0.027 Uiso 1 1 calc R . .
C13 C 0.2527(3) 0.27636(4) 0.3526(2) 0.0163(7) Uani 1 1 d U . .
C14 C 0.1270(4) 0.28046(4) 0.4340(2) 0.0178(4) Uani 1 1 d U . .
H14 H 0.1019 0.2649 0.4850 0.021 Uiso 1 1 calc R . .
C15 C 0.0401(4) 0.30781(4) 0.4382(2) 0.0236(7) Uani 1 1 d U . .
H15 H -0.0440 0.3104 0.4925 0.028 Uiso 1 1 calc R . .
C17 C 0.2511(4) 0.22374(4) 0.3534(2) 0.0192(7) Uani 1 1 d U . .
C18 C 0.4371(3) 0.20081(4) 0.4302(2) 0.0186(7) Uani 1 1 d U . .
H18 H 0.6310 0.2036 0.4879 0.022 Uiso 1 1 calc R . .
C19 C 0.3367(4) 0.17336(4) 0.4221(2) 0.0216(7) Uani 1 1 d U . .
H19 H 0.4640 0.1578 0.4723 0.026 Uiso 1 1 calc R . .
C20 C 0.0521(4) 0.16865(4) 0.3411(2) 0.0168(4) Uani 1 1 d U . .
C21 C -0.1286(4) 0.19233(4) 0.2680(2) 0.0246(8) Uani 1 1 d U . .
H21 H -0.3198 0.1896 0.2167 0.030 Uiso 1 1 calc R . .
C22 C -0.0437(4) 0.21924(5) 0.2667(2) 0.0276(8) Uani 1 1 d U . .
H22 H -0.1750 0.2344 0.2103 0.033 Uiso 1 1 calc R . .
C24 C 0.0245(4) 0.11771(4) 0.3097(2) 0.0242(8) Uani 1 1 d U . .
H24 H 0.1370 0.1188 0.2741 0.029 Uiso 1 1 calc R . .
C25 C -0.0544(4) 0.09021(4) 0.3299(2) 0.0243(7) Uani 1 1 d U . .
C26 C 0.0178(5) 0.06533(4) 0.2825(3) 0.0338(8) Uani 1 1 d U . .
H26 H 0.1099 0.0673 0.2330 0.041 Uiso 1 1 calc R . .
C27 C -0.0438(4) 0.03830(5) 0.3071(3) 0.0478(9) Uani 1 1 d U . .
H27 H 0.0069 0.0220 0.2760 0.057 Uiso 1 1 calc R . .
C28 C -0.1845(4) 0.03579(5) 0.3798(3) 0.0415(8) Uani 1 1 d U . .
H28 H -0.2263 0.0175 0.3982 0.050 Uiso 1 1 calc R . .
C29 C -0.2620(4) 0.05959(5) 0.4246(3) 0.0397(8) Uani 1 1 d U . .
H29 H -0.3534 0.0574 0.4744 0.048 Uiso 1 1 calc R . .
C30 C -0.2058(4) 0.08677(5) 0.3966(2) 0.0291(8) Uani 1 1 d U . .

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 0.0381(6) 0.0590(10) 0.0743(7) -0.0022(7) 0.0430(4) -0.0024(7)
O16 0.0244(5) 0.0275(8) 0.0400(6) -0.0012(5) 0.0256(4) -0.0014(6)
O31 0.0547(6) 0.0485(10) 0.0644(6) 0.0060(7) 0.0517(4) 0.0048(7)
N9 0.0413(6) 0.0263(9) 0.0462(7) 0.0052(7) 0.0400(4) 0.0038(7)
N23 0.0220(6) 0.0340(9) 0.0110(6) 0.0037(7) 0.0093(4) -0.0012(7)
C2 0.0255(7) 0.0408(12) 0.0256(8) -0.0051(9) 0.0239(5) 0.0018(9)
C3 0.0374(8) 0.0552(13) 0.0356(9) -0.0029(10) 0.0293(6) 0.0112(10)
C4 0.0585(9) 0.0434(14) 0.0510(10) -0.0044(10) 0.0387(7) 0.0079(11)
C5 0.0541(10) 0.0342(13) 0.0384(10) -0.0046(9) 0.0284(7) -0.0035(11)
C6 0.0316(8) 0.0419(12) 0.0209(8) 0.0099(9) 0.0154(6) 0.0019(9)
C7 0.0275(7) 0.0320(11) 0.0158(8) 0.0025(8) 0.0184(5) 0.0066(8)
C8 0.0296(8) 0.0336(12) 0.0266(8) 0.0036(9) 0.0230(5) 0.0046(9)
C10 0.0188(7) 0.0221(10) 0.0133(7) -0.0032(8) 0.0106(5) -0.0024(8)
C11 0.0265(7) 0.0258(11) 0.0393(8) 0.0050(8) 0.0272(5) -0.0034(9)
C12 0.0233(7) 0.0339(12) 0.0244(7) 0.0018(8) 0.0220(5) -0.0027(9)
C13 0.0066(7) 0.0217(11) 0.0202(8) -0.0005(8) 0.0083(5) -0.0008(8)
C14 0.0183(4) 0.0186(5) 0.0171(4) 0.0011(4) 0.0116(2) -0.0006(4)
C15 0.0248(7) 0.0339(12) 0.0196(8) 0.0041(8) 0.0176(5) 0.0049(9)
C17 0.0231(8) 0.0227(11) 0.0223(8) -0.0025(8) 0.0194(5) 0.0023(8)
C18 0.0113(7) 0.0303(12) 0.0174(8) -0.0007(8) 0.0106(5) 0.0006(8)
C19 0.0210(7) 0.0258(12) 0.0185(8) 0.0041(8) 0.0128(6) 0.0121(9)
C20 0.0174(4) 0.0172(5) 0.0158(4) 0.0002(4) 0.0106(2) 0.0000(4)
C21 0.0200(7) 0.0320(12) 0.0253(9) -0.0032(8) 0.0161(6) -0.0002(9)
C22 0.0219(8) 0.0298(12) 0.0303(9) -0.0031(9) 0.0163(6) 0.0076(9)
C24 0.0267(8) 0.0286(11) 0.0168(8) -0.0070(8) 0.0136(6) -0.0024(9)
C25 0.0226(7) 0.0285(11) 0.0245(8) -0.0025(8) 0.0163(5) 0.0007(9)
C26 0.0380(8) 0.0386(12) 0.0305(8) -0.0111(9) 0.0245(6) -0.0052(10)
C27 0.0500(10) 0.0415(13) 0.0537(10) -0.0009(11) 0.0340(7) 0.0051(11)
C28 0.0415(9) 0.0358(13) 0.0399(10) 0.0045(9) 0.0226(6) -0.0105(10)
C29 0.0358(9) 0.0459(13) 0.0431(9) 0.0078(9) 0.0279(6) -0.0035(10)
C30 0.0294(8) 0.0348(12) 0.0266(9) -0.0009(8) 0.0195(6) 0.0021(9)

_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 C2 1.342(3) . ?
O1 H1 0.8200 . ?
O16 C13 1.387(2) . ?
O16 C17 1.389(2) . ?
O31 C30 1.350(3) . ?
O31 H31 0.8200 . ?
N9 C8 1.273(3) . ?
N9 C10 1.404(3) . ?
N23 C24 1.302(3) . ?
N23 C20 1.403(3) . ?
C2 C3 1.371(3) . ?
C2 C7 1.430(3) . ?
C3 C4 1.373(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.384(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.354(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.415(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.419(3) . ?
C8 H8 0.9300 . ?
C10 C15 1.380(3) . ?
C10 C11 1.416(4) . ?
C11 C12 1.363(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.363(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.393(4) . ?
C14 C15 1.380(3) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C17 C18 1.367(3) . ?
C17 C22 1.418(3) . ?
C18 C19 1.388(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.377(3) . ?
C19 H19 0.9300 . ?
C20 C21 1.379(3) . ?
C21 C22 1.349(3) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C24 C25 1.413(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.401(3) . ?
C25 C30 1.409(4) . ?
C26 C27 1.366(3) . ?
C26 H26 0.9300 . ?
C27 C28 1.395(4) . ?
C27 H27 0.9300 . ?
C28 C29 1.365(4) . ?
C28 H28 0.9300 . ?
C29 C30 1.372(3) . ?
C29 H29 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 O1 H1 109.5 . . ?
C13 O16 C17 122.64(17) . . ?
C30 O31 H31 109.5 . . ?
C8 N9 C10 121.64(19) . . ?
C24 N23 C20 122.2(2) . . ?
O1 C2 C3 119.82(18) . . ?
O1 C2 C7 120.46(19) . . ?
C3 C2 C7 119.7(2) . . ?
C2 C3 C4 121.3(2) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C3 C4 C5 120.0(2) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 120.3(2) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C6 C7 121.6(2) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C6 C7 C8 121.8(2) . . ?
C6 C7 C2 116.96(19) . . ?
C8 C7 C2 121.11(19) . . ?
N9 C8 C7 123.5(2) . . ?
N9 C8 H8 118.2 . . ?
C7 C8 H8 118.2 . . ?
C15 C10 N9 119.7(2) . . ?
C15 C10 C11 117.4(2) . . ?
N9 C10 C11 122.8(2) . . ?
C12 C11 C10 120.5(2) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C13 C12 C11 121.4(2) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C12 C13 O16 117.4(2) . . ?
C12 C13 C14 119.52(19) . . ?
O16 C13 C14 122.97(19) . . ?
C15 C14 C13 119.4(2) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C10 C15 C14 121.9(2) . . ?
C10 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
C18 C17 O16 116.51(17) . . ?
C18 C17 C22 119.50(19) . . ?
O16 C17 C22 123.77(16) . . ?
C17 C18 C19 120.01(17) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C20 C19 C18 121.31(18) . . ?
C20 C19 H19 119.3 . . ?
C18 C19 H19 119.3 . . ?
C19 C20 C21 117.19(19) . . ?
C19 C20 N23 123.13(17) . . ?
C21 C20 N23 119.60(18) . . ?
C22 C21 C20 123.7(2) . . ?
C22 C21 H21 118.1 . . ?
C20 C21 H21 118.1 . . ?
C21 C22 C17 118.22(18) . . ?
C21 C22 H22 120.9 . . ?
C17 C22 H22 120.9 . . ?
N23 C24 C25 122.3(3) . . ?
N23 C24 H24 118.8 . . ?
C25 C24 H24 118.8 . . ?
C26 C25 C30 118.1(2) . . ?
C26 C25 C24 119.8(3) . . ?
C30 C25 C24 122.1(2) . . ?
C27 C26 C25 121.7(3) . . ?
C27 C26 H26 119.2 . . ?
C25 C26 H26 119.2 . . ?
C26 C27 C28 118.4(3) . . ?
C26 C27 H27 120.8 . . ?
C28 C27 H27 120.8 . . ?
C29 C28 C27 121.4(2) . . ?
C29 C28 H28 119.3 . . ?
C27 C28 H28 119.3 . . ?
C28 C29 C30 120.3(3) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
O31 C30 C29 118.7(3) . . ?
O31 C30 C25 121.2(2) . . ?
C29 C30 C25 120.0(2) . . ?

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
O1 C2 C3 C4 177.8(2) . . . . ?
C7 C2 C3 C4 -3.1(3) . . . . ?
C2 C3 C4 C5 0.8(4) . . . . ?
C3 C4 C5 C6 1.7(4) . . . . ?
C4 C5 C6 C7 -1.8(4) . . . . ?
C5 C6 C7 C8 174.9(2) . . . . ?
C5 C6 C7 C2 -0.5(3) . . . . ?
O1 C2 C7 C6 -177.95(19) . . . . ?
C3 C2 C7 C6 2.9(3) . . . . ?
O1 C2 C7 C8 6.6(3) . . . . ?
C3 C2 C7 C8 -172.5(2) . . . . ?
C10 N9 C8 C7 174.83(18) . . . . ?
C6 C7 C8 N9 176.7(2) . . . . ?
C2 C7 C8 N9 -8.1(3) . . . . ?
C8 N9 C10 C15 140.47(18) . . . . ?
C8 N9 C10 C11 -43.6(2) . . . . ?
C15 C10 C11 C12 -1.1(2) . . . . ?
N9 C10 C11 C12 -177.16(13) . . . . ?
C10 C11 C12 C13 0.0(2) . . . . ?
C11 C12 C13 O16 -175.90(12) . . . . ?
C11 C12 C13 C14 1.0(2) . . . . ?
C17 O16 C13 C12 -152.81(14) . . . . ?
C17 O16 C13 C14 30.4(2) . . . . ?
C12 C13 C14 C15 -1.0(2) . . . . ?
O16 C13 C14 C15 175.76(13) . . . . ?
N9 C10 C15 C14 177.32(13) . . . . ?
C11 C10 C15 C14 1.1(2) . . . . ?
C13 C14 C15 C10 -0.1(2) . . . . ?
C13 O16 C17 C18 -153.04(17) . . . . ?
C13 O16 C17 C22 32.4(3) . . . . ?
O16 C17 C18 C19 -174.56(18) . . . . ?
C22 C17 C18 C19 0.3(3) . . . . ?
C17 C18 C19 C20 -1.4(3) . . . . ?
C18 C19 C20 C21 0.3(3) . . . . ?
C18 C19 C20 N23 -176.3(2) . . . . ?
C24 N23 C20 C19 -41.0(3) . . . . ?
C24 N23 C20 C21 142.5(2) . . . . ?
C19 C20 C21 C22 2.2(3) . . . . ?
N23 C20 C21 C22 178.8(2) . . . . ?
C20 C21 C22 C17 -3.3(4) . . . . ?
C18 C17 C22 C21 2.0(3) . . . . ?
O16 C17 C22 C21 176.4(2) . . . . ?
C20 N23 C24 C25 172.05(14) . . . . ?
N23 C24 C25 C26 175.01(14) . . . . ?
N23 C24 C25 C30 -4.9(2) . . . . ?
C30 C25 C26 C27 -2.9(2) . . . . ?
C24 C25 C26 C27 177.24(15) . . . . ?
C25 C26 C27 C28 0.6(2) . . . . ?
C26 C27 C28 C29 0.5(3) . . . . ?
C27 C28 C29 C30 0.8(3) . . . . ?
C28 C29 C30 O31 179.38(14) . . . . ?
C28 C29 C30 C25 -3.2(2) . . . . ?
C26 C25 C30 O31 -178.47(13) . . . . ?
C24 C25 C30 O31 1.4(2) . . . . ?
C26 C25 C30 C29 4.2(2) . . . . ?
C24 C25 C30 C29 -175.96(15) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        18.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.104