data_3a_dax44
_audit_creation_date              2011-12-29
_audit_creation_method
;
  Olex2 1.1-beta
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;

_publ_requested_journal           'J.Org.Chem.'
_publ_section_title
;
Domino reactions of 2H-azirines with acylketenes from
furan-2,3-diones: competition between ortho-fused/bridged 
heterocyclic system formations
;


_publ_contact_author_address
;
Department of Chemistry
Durham University
South Rd.
Durham
DH1 3LE
UK
;
_publ_contact_author_email        d.s.yufit@durham.ac.uk
_publ_contact_author_name         'Dmitry Yufit'
_publ_contact_author_phone        ?

_publ_contact_letter
;
The CIF file contains data for the structure 3a from
the paper 

"Domino reactions of 2H-azirines with acylketenes from
furan-2,3-diones: competition between ortho-fused/bridged 
heterocyclic system formations"

by  A.F.Khlebnikov, M.S.Novikov, V.V. Pakalnis, R.O.Iakovenko 
and D.S.Yufit. 

The paper will be submitted to J.Org.Chem. 
;
loop_
_publ_author_name
_publ_author_address
'Khlebnikov, Alexander F.'
;
Department of Chemistry
Saint-Petersburg State University
Universitetskii pr. 26
198504
St.Petersburg
Russia
;
'Novikov, Mikhail S.'
;
Department of Chemistry
Saint-Petersburg State University
Universitetskii pr. 26
198504
St.Petersburg
Russia
;
'Pakalnis, Viktoriia V.'
;
Department of Chemistry
Saint-Petersburg State University
Universitetskii pr. 26
198504
St.Petersburg
Russia
;
'Iakovenko, Roman O.'
;
Department of Chemistry
Saint-Petersburg State University
Universitetskii pr. 26
198504
St.Petersburg
Russia
;

'Yufit, Dmitry S.'
;
Department of Chemistry
Durham University
South Rd.
Durham
DH1 3LE
UK
;


_chemical_name_common             ?
_chemical_name_systematic
;
4,6,8-Triphenyl-5,7-dioxa-1-azabicyclo[4.4.1]undeca-3,8-diene-2,10-dione 
;
_chemical_formula_moiety          'C26 H19 N O4'
_chemical_formula_sum             'C26 H19 N O4'
_chemical_formula_weight          409.42
_chemical_melting_point           ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system       'monoclinic'
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 1 21/n 1'
_space_group_name_Hall            '-P 2yn'
loop_
  _space_group_symop_id
  _space_group_symop_operation_xyz
 1 'x, y, z'
 2 '-x+1/2, y+1/2, -z+1/2'
 3 '-x, -y, -z'
 4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                    14.5600(5)
_cell_length_b                    17.9642(6)
_cell_length_c                    17.1799(6)
_cell_angle_alpha                 90.00
_cell_angle_beta                  105.8500(10)
_cell_angle_gamma                 90.00
_cell_volume                      4322.7(3)
_cell_formula_units_Z             8
_cell_measurement_reflns_used     4346
_cell_measurement_temperature     100
_cell_measurement_theta_max       56.608
_cell_measurement_theta_min       3.634
_exptl_absorpt_coefficient_mu     0.692
_exptl_absorpt_correction_T_max   1.0000
_exptl_absorpt_correction_T_min   0.8419
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.0725 before and 0.0533 after correction.
The Ratio of minimum to maximum transmission is 0.8419.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour             'clear light colourless'
_exptl_crystal_colour_lustre      clear
_exptl_crystal_colour_modifier    light
_exptl_crystal_colour_primary     colourless
_exptl_crystal_density_diffrn     1.258
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_description        needle
_exptl_crystal_F_000              1712
_exptl_crystal_size_max           0.2
_exptl_crystal_size_mid           0.03
_exptl_crystal_size_min           0.02
_exptl_special_details
;
 ? 
;
_diffrn_reflns_av_R_equivalents   0.0506
_diffrn_reflns_av_unetI/netI      0.0623
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_k_max        19
_diffrn_reflns_limit_k_min        -19
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_number             21195
_diffrn_reflns_theta_full         58.00
_diffrn_reflns_theta_max          60.57
_diffrn_reflns_theta_min          2.46
_diffrn_ambient_temperature       100.0
_diffrn_detector                  'CCD area detector'
_diffrn_detector_area_resol_mean  ?
_diffrn_detector_type             'Bruker Platinum-135 area detector'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device        'three-circle diffractometer'
_diffrn_measurement_device_type   'Bruker Proteum R'
_diffrn_measurement_method        'ω scans'
_diffrn_radiation_collimation     'focusing mirrors'
_diffrn_radiation_monochromator   graphite
_diffrn_radiation_probe           x-ray
_diffrn_radiation_type            CuK\a
_diffrn_radiation_wavelength      1.54178
_diffrn_radiation_xray_symbol     K-L~3~
_diffrn_source                    'rotating anode'
_diffrn_source_target             Cu
_diffrn_source_type               'Bruker Microstar rotating anode'
_diffrn_standards_decay_%         ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_number          ?
_reflns_number_gt                 4157
_reflns_number_total              5904
_reflns_threshold_expression      >2sigma(I)
_computing_cell_refinement        'SAINT V7.60A (Bruker, 2003)'
_computing_data_collection        'Proteum2 V2011.2-0 (Bruker, 2001)'
_computing_data_reduction         'SAINT V7.60A (Bruker, 2003)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max          0.214
_refine_diff_density_min          -0.219
_refine_diff_density_rms          0.046
_refine_ls_extinction_coef        ?
_refine_ls_extinction_method      none
_refine_ls_goodness_of_fit_ref    0.991
_refine_ls_hydrogen_treatment     constr
_refine_ls_matrix_type            full
_refine_ls_number_parameters      559
_refine_ls_number_reflns          5904
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0704
_refine_ls_R_factor_gt            0.0440
_refine_ls_restrained_S_all       0.991
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0600P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme       calc
_refine_ls_wR_factor_gt           0.0993
_refine_ls_wR_factor_ref          0.1073
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
The structure contains a severely disordered
solvent molecule (hexane?) which was impossible to model satisfactorily. 
The contribution of the solvent to the structural factors was taken into 
account by applying MASK procedure of OLEX2 program package.
See _smtbx_masks_special_details below. 

;
_atom_sites_solution_hydrogens    geom
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
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 0.58882(12) 0.94899(9) -0.07378(10) 0.0327(4) Uani 1 1 d . . .
 O2 O 0.39004(12) 0.94735(9) -0.10470(10) 0.0339(5) Uani 1 1 d . . .
 O3 O 0.44357(11) 0.76940(8) 0.03607(9) 0.0234(4) Uani 1 1 d . . .
 O4 O 0.60062(11) 0.77280(8) 0.09569(9) 0.0241(4) Uani 1 1 d . . .
 N1 N 0.50075(14) 0.90772(10) 0.01061(11) 0.0209(5) Uani 1 1 d . . .
 C1 C 0.40898(17) 0.91158(13) -0.04273(15) 0.0263(6) Uani 1 1 d . . .
 C2 C 0.33576(17) 0.86639(13) -0.01950(14) 0.0259(6) Uani 1 1 d . . .
 H2 H 0.2733 0.8866 -0.0293 0.031 Uiso 1 1 calc R . .
 C3 C 0.35194(17) 0.79871(13) 0.01460(13) 0.0229(6) Uani 1 1 d . . .
 C4 C 0.51330(16) 0.80366(13) 0.10409(13) 0.0207(6) Uani 1 1 d . . .
 C5 C 0.67415(16) 0.81235(13) 0.08042(13) 0.0219(6) Uani 1 1 d . . .
 C6 C 0.66825(17) 0.87432(13) 0.03529(13) 0.0224(6) Uani 1 1 d . . .
 H6 H 0.7280 0.8959 0.0357 0.027 Uiso 1 1 calc R . .
 C7 C 0.58521(17) 0.91375(13) -0.01406(14) 0.0240(6) Uani 1 1 d . . .
 C8 C 0.50971(17) 0.88644(12) 0.09436(13) 0.0226(6) Uani 1 1 d . . .
 H8A H 0.4547 0.9063 0.1112 0.027 Uiso 1 1 calc R . .
 H8B H 0.5686 0.9086 0.1299 0.027 Uiso 1 1 calc R . .
 C9 C 0.27919(17) 0.74610(13) 0.02659(14) 0.0231(6) Uani 1 1 d . . .
 C10 C 0.18119(18) 0.76196(14) -0.00122(14) 0.0280(6) Uani 1 1 d . . .
 H10 H 0.1607 0.8072 -0.0293 0.034 Uiso 1 1 calc R . .
 C11 C 0.11410(18) 0.71241(14) 0.01188(14) 0.0289(6) Uani 1 1 d . . .
 H11 H 0.0481 0.7240 -0.0068 0.035 Uiso 1 1 calc R . .
 C12 C 0.14281(19) 0.64626(14) 0.05199(15) 0.0318(7) Uani 1 1 d . . .
 H12 H 0.0966 0.6129 0.0618 0.038 Uiso 1 1 calc R . .
 C13 C 0.23872(19) 0.62856(14) 0.07782(15) 0.0325(7) Uani 1 1 d . . .
 H13 H 0.2585 0.5825 0.1043 0.039 Uiso 1 1 calc R . .
 C14 C 0.30640(18) 0.67839(13) 0.06486(14) 0.0281(6) Uani 1 1 d . . .
 H14 H 0.3722 0.6658 0.0825 0.034 Uiso 1 1 calc R . .
 C15 C 0.49974(16) 0.77248(13) 0.18196(13) 0.0226(6) Uani 1 1 d . . .
 C16 C 0.45777(17) 0.81272(14) 0.23184(14) 0.0289(6) Uani 1 1 d . . .
 H16 H 0.4389 0.8629 0.2191 0.035 Uiso 1 1 calc R . .
 C17 C 0.44335(18) 0.77946(14) 0.30063(15) 0.0345(7) Uani 1 1 d . . .
 H17 H 0.4138 0.8070 0.3343 0.041 Uiso 1 1 calc R . .
 C18 C 0.47121(18) 0.70739(14) 0.32052(15) 0.0325(7) Uani 1 1 d . . .
 H18 H 0.4619 0.6856 0.3682 0.039 Uiso 1 1 calc R . .
 C19 C 0.51258(18) 0.66693(15) 0.27129(15) 0.0357(7) Uani 1 1 d . . .
 H19 H 0.5314 0.6168 0.2844 0.043 Uiso 1 1 calc R . .
 C20 C 0.52682(18) 0.69938(14) 0.20248(15) 0.0313(6) Uani 1 1 d . . .
 H20 H 0.5556 0.6712 0.1687 0.038 Uiso 1 1 calc R . .
 C21 C 0.76550(17) 0.77371(13) 0.11905(13) 0.0229(6) Uani 1 1 d . . .
 C22 C 0.77339(18) 0.73014(13) 0.18760(14) 0.0291(6) Uani 1 1 d . . .
 H22 H 0.7192 0.7230 0.2074 0.035 Uiso 1 1 calc R . .
 C23 C 0.85941(19) 0.69711(14) 0.22717(16) 0.0345(7) Uani 1 1 d . . .
 H23 H 0.8642 0.6679 0.2742 0.041 Uiso 1 1 calc R . .
 C24 C 0.93838(19) 0.70667(14) 0.19820(16) 0.0339(7) Uani 1 1 d . . .
 H24 H 0.9978 0.6849 0.2259 0.041 Uiso 1 1 calc R . .
 C25 C 0.93056(18) 0.74779(13) 0.12925(16) 0.0314(7) Uani 1 1 d . . .
 H25 H 0.9846 0.7531 0.1088 0.038 Uiso 1 1 calc R . .
 C26 C 0.84505(17) 0.78169(13) 0.08902(15) 0.0274(6) Uani 1 1 d . . .
 H26 H 0.8406 0.8101 0.0415 0.033 Uiso 1 1 calc R . .
 O1A O 0.58374(11) 0.57457(9) 0.45466(9) 0.0262(4) Uani 1 1 d . . .
 O2A O 0.39284(11) 0.59122(9) 0.45876(9) 0.0274(4) Uani 1 1 d . . .
 O3A O 0.34080(11) 0.48278(8) 0.24480(9) 0.0221(4) Uani 1 1 d . . .
 O4A O 0.48505(11) 0.44132(8) 0.24456(9) 0.0227(4) Uani 1 1 d . . .
 N1A N 0.45729(13) 0.49702(10) 0.39825(11) 0.0210(5) Uani 1 1 d . . .
 C1A C 0.38170(17) 0.53999(13) 0.41056(14) 0.0239(6) Uani 1 1 d . . .
 C2A C 0.28669(17) 0.52047(13) 0.35804(14) 0.0240(6) Uani 1 1 d . . .
 H2A H 0.2342 0.5238 0.3807 0.029 Uiso 1 1 calc R . .
 C3A C 0.26820(16) 0.49822(12) 0.28018(14) 0.0210(6) Uani 1 1 d . . .
 C4A C 0.40692(16) 0.42211(12) 0.27641(13) 0.0204(6) Uani 1 1 d . . .
 C5A C 0.57757(17) 0.45231(13) 0.29022(14) 0.0213(6) Uani 1 1 d . . .
 C6A C 0.60614(17) 0.48450(13) 0.36293(14) 0.0232(6) Uani 1 1 d . . .
 H6A H 0.6729 0.4824 0.3877 0.028 Uiso 1 1 calc R . .
 C7A C 0.55081(17) 0.52242(13) 0.41046(13) 0.0215(6) Uani 1 1 d . . .
 C8A C 0.43459(17) 0.42190(12) 0.36689(13) 0.0214(6) Uani 1 1 d . . .
 H8AA H 0.3814 0.4018 0.3861 0.026 Uiso 1 1 calc R . .
 H8AB H 0.4908 0.3893 0.3875 0.026 Uiso 1 1 calc R . .
 C9A C 0.17280(17) 0.49412(12) 0.22258(14) 0.0233(6) Uani 1 1 d . . .
 C10A C 0.09357(17) 0.52807(13) 0.23936(15) 0.0266(6) Uani 1 1 d . . .
 H10A H 0.1013 0.5553 0.2882 0.032 Uiso 1 1 calc R . .
 C11A C 0.00389(18) 0.52203(13) 0.18483(15) 0.0292(6) Uani 1 1 d . . .
 H11A H -0.0493 0.5455 0.1966 0.035 Uiso 1 1 calc R . .
 C12A C -0.00905(18) 0.48240(13) 0.11374(15) 0.0299(6) Uani 1 1 d . . .
 H12A H -0.0709 0.4773 0.0774 0.036 Uiso 1 1 calc R . .
 C13A C 0.06904(18) 0.45029(13) 0.09618(15) 0.0282(6) Uani 1 1 d . . .
 H13A H 0.0608 0.4242 0.0467 0.034 Uiso 1 1 calc R . .
 C14A C 0.15938(18) 0.45560(13) 0.14979(14) 0.0263(6) Uani 1 1 d . . .
 H14A H 0.2123 0.4329 0.1369 0.032 Uiso 1 1 calc R . .
 C15A C 0.36502(16) 0.35046(13) 0.23524(13) 0.0206(6) Uani 1 1 d . . .
 C16A C 0.32777(16) 0.29488(13) 0.27426(15) 0.0263(6) Uani 1 1 d . . .
 H16A H 0.3287 0.3009 0.3294 0.032 Uiso 1 1 calc R . .
 C17A C 0.28941(18) 0.23100(14) 0.23307(16) 0.0337(7) Uani 1 1 d . . .
 H17A H 0.2642 0.1934 0.2602 0.040 Uiso 1 1 calc R . .
 C18A C 0.28737(18) 0.22143(14) 0.15332(16) 0.0344(7) Uani 1 1 d . . .
 H18A H 0.2618 0.1770 0.1258 0.041 Uiso 1 1 calc R . .
 C19A C 0.32257(17) 0.27643(14) 0.11310(15) 0.0312(6) Uani 1 1 d . . .
 H19A H 0.3197 0.2706 0.0575 0.037 Uiso 1 1 calc R . .
 C20A C 0.36208(17) 0.34021(14) 0.15426(14) 0.0275(6) Uani 1 1 d . . .
 H20A H 0.3875 0.3775 0.1268 0.033 Uiso 1 1 calc R . .
 C21A C 0.64397(17) 0.42594(13) 0.24422(13) 0.0213(6) Uani 1 1 d . . .
 C22A C 0.61524(18) 0.37046(13) 0.18607(14) 0.0279(6) Uani 1 1 d . . .
 H22A H 0.5520 0.3515 0.1740 0.033 Uiso 1 1 calc R . .
 C23A C 0.67839(19) 0.34259(15) 0.14554(15) 0.0347(7) Uani 1 1 d . . .
 H23A H 0.6580 0.3047 0.1060 0.042 Uiso 1 1 calc R . .
 C24A C 0.77011(19) 0.36949(15) 0.16230(15) 0.0352(7) Uani 1 1 d . . .
 H24A H 0.8133 0.3499 0.1349 0.042 Uiso 1 1 calc R . .
 C25A C 0.79904(19) 0.42479(15) 0.21875(15) 0.0340(7) Uani 1 1 d . . .
 H25A H 0.8623 0.4435 0.2301 0.041 Uiso 1 1 calc R . .
 C26A C 0.73652(18) 0.45374(14) 0.25963(14) 0.0288(6) Uani 1 1 d . . .
 H26A H 0.7571 0.4925 0.2981 0.035 Uiso 1 1 calc R . .


_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 C7 1.219(3) . ?
 O2 C1 1.209(3) . ?
 O3 C3 1.387(3) . ?
 O3 C4 1.458(3) . ?
 O4 C4 1.430(3) . ?
 O4 C5 1.369(3) . ?
 N1 C1 1.400(3) . ?
 N1 C7 1.410(3) . ?
 N1 C8 1.460(3) . ?
 C1 C2 1.479(3) . ?
 C2 H2 0.9500 . ?
 C2 C3 1.342(3) . ?
 C3 C9 1.475(3) . ?
 C4 C8 1.496(3) . ?
 C4 C15 1.512(3) . ?
 C5 C6 1.346(3) . ?
 C5 C21 1.486(3) . ?
 C6 H6 0.9500 . ?
 C6 C7 1.457(3) . ?
 C8 H8A 0.9900 . ?
 C8 H8B 0.9900 . ?
 C9 C10 1.405(3) . ?
 C9 C14 1.388(3) . ?
 C10 H10 0.9500 . ?
 C10 C11 1.385(3) . ?
 C11 H11 0.9500 . ?
 C11 C12 1.380(3) . ?
 C12 H12 0.9500 . ?
 C12 C13 1.382(3) . ?
 C13 H13 0.9500 . ?
 C13 C14 1.394(3) . ?
 C14 H14 0.9500 . ?
 C15 C16 1.384(3) . ?
 C15 C20 1.389(3) . ?
 C16 H16 0.9500 . ?
 C16 C17 1.390(3) . ?
 C17 H17 0.9500 . ?
 C17 C18 1.372(3) . ?
 C18 H18 0.9500 . ?
 C18 C19 1.373(3) . ?
 C19 H19 0.9500 . ?
 C19 C20 1.384(3) . ?
 C20 H20 0.9500 . ?
 C21 C22 1.392(3) . ?
 C21 C26 1.398(3) . ?
 C22 H22 0.9500 . ?
 C22 C23 1.385(3) . ?
 C23 H23 0.9500 . ?
 C23 C24 1.383(3) . ?
 C24 H24 0.9500 . ?
 C24 C25 1.374(3) . ?
 C25 H25 0.9500 . ?
 C25 C26 1.389(3) . ?
 C26 H26 0.9500 . ?
 O1A C7A 1.219(3) . ?
 O2A C1A 1.219(3) . ?
 O3A C3A 1.384(2) . ?
 O3A C4A 1.457(3) . ?
 O4A C4A 1.433(3) . ?
 O4A C5A 1.375(3) . ?
 N1A C1A 1.407(3) . ?
 N1A C7A 1.396(3) . ?
 N1A C8A 1.457(3) . ?
 C1A C2A 1.473(3) . ?
 C2A H2A 0.9500 . ?
 C2A C3A 1.351(3) . ?
 C3A C9A 1.471(3) . ?
 C4A C8A 1.495(3) . ?
 C4A C15A 1.514(3) . ?
 C5A C6A 1.336(3) . ?
 C5A C21A 1.484(3) . ?
 C6A H6A 0.9500 . ?
 C6A C7A 1.463(3) . ?
 C8A H8AA 0.9900 . ?
 C8A H8AB 0.9900 . ?
 C9A C10A 1.403(3) . ?
 C9A C14A 1.396(3) . ?
 C10A H10A 0.9500 . ?
 C10A C11A 1.388(3) . ?
 C11A H11A 0.9500 . ?
 C11A C12A 1.381(3) . ?
 C12A H12A 0.9500 . ?
 C12A C13A 1.380(3) . ?
 C13A H13A 0.9500 . ?
 C13A C14A 1.388(3) . ?
 C14A H14A 0.9500 . ?
 C15A C16A 1.393(3) . ?
 C15A C20A 1.392(3) . ?
 C16A H16A 0.9500 . ?
 C16A C17A 1.383(3) . ?
 C17A H17A 0.9500 . ?
 C17A C18A 1.373(3) . ?
 C18A H18A 0.9500 . ?
 C18A C19A 1.382(3) . ?
 C19A H19A 0.9500 . ?
 C19A C20A 1.386(3) . ?
 C20A H20A 0.9500 . ?
 C21A C22A 1.392(3) . ?
 C21A C26A 1.393(3) . ?
 C22A H22A 0.9500 . ?
 C22A C23A 1.389(3) . ?
 C23A H23A 0.9500 . ?
 C23A C24A 1.375(3) . ?
 C24A H24A 0.9500 . ?
 C24A C25A 1.372(3) . ?
 C25A H25A 0.9500 . ?
 C25A C26A 1.393(3) . ?
 C26A H26A 0.9500 . ?

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 O3 C4 117.48(16) . . ?
 C5 O4 C4 125.57(17) . . ?
 C1 N1 C7 123.65(19) . . ?
 C1 N1 C8 118.05(19) . . ?
 C7 N1 C8 117.77(19) . . ?
 O2 C1 N1 123.4(2) . . ?
 O2 C1 C2 121.4(2) . . ?
 N1 C1 C2 115.2(2) . . ?
 C1 C2 H2 117.9 . . ?
 C3 C2 C1 124.2(2) . . ?
 C3 C2 H2 117.9 . . ?
 O3 C3 C9 113.3(2) . . ?
 C2 C3 O3 120.1(2) . . ?
 C2 C3 C9 126.4(2) . . ?
 O3 C4 C8 109.54(18) . . ?
 O3 C4 C15 108.79(18) . . ?
 O4 C4 O3 101.49(16) . . ?
 O4 C4 C8 112.28(18) . . ?
 O4 C4 C15 106.28(17) . . ?
 C8 C4 C15 117.25(19) . . ?
 O4 C5 C21 108.87(19) . . ?
 C6 C5 O4 127.6(2) . . ?
 C6 C5 C21 123.5(2) . . ?
 C5 C6 H6 114.7 . . ?
 C5 C6 C7 130.5(2) . . ?
 C7 C6 H6 114.7 . . ?
 O1 C7 N1 122.3(2) . . ?
 O1 C7 C6 121.5(2) . . ?
 N1 C7 C6 116.2(2) . . ?
 N1 C8 C4 111.19(18) . . ?
 N1 C8 H8A 109.4 . . ?
 N1 C8 H8B 109.4 . . ?
 C4 C8 H8A 109.4 . . ?
 C4 C8 H8B 109.4 . . ?
 H8A C8 H8B 108.0 . . ?
 C10 C9 C3 121.6(2) . . ?
 C14 C9 C3 120.3(2) . . ?
 C14 C9 C10 118.1(2) . . ?
 C9 C10 H10 119.7 . . ?
 C11 C10 C9 120.7(2) . . ?
 C11 C10 H10 119.7 . . ?
 C10 C11 H11 119.9 . . ?
 C12 C11 C10 120.3(2) . . ?
 C12 C11 H11 119.9 . . ?
 C11 C12 H12 120.0 . . ?
 C11 C12 C13 120.0(2) . . ?
 C13 C12 H12 120.0 . . ?
 C12 C13 H13 120.1 . . ?
 C12 C13 C14 119.8(2) . . ?
 C14 C13 H13 120.1 . . ?
 C9 C14 C13 121.0(2) . . ?
 C9 C14 H14 119.5 . . ?
 C13 C14 H14 119.5 . . ?
 C16 C15 C4 122.7(2) . . ?
 C16 C15 C20 118.7(2) . . ?
 C20 C15 C4 118.6(2) . . ?
 C15 C16 H16 120.1 . . ?
 C15 C16 C17 119.8(2) . . ?
 C17 C16 H16 120.1 . . ?
 C16 C17 H17 119.5 . . ?
 C18 C17 C16 121.0(2) . . ?
 C18 C17 H17 119.5 . . ?
 C17 C18 H18 120.1 . . ?
 C17 C18 C19 119.7(2) . . ?
 C19 C18 H18 120.1 . . ?
 C18 C19 H19 120.1 . . ?
 C18 C19 C20 119.8(2) . . ?
 C20 C19 H19 120.1 . . ?
 C15 C20 H20 119.4 . . ?
 C19 C20 C15 121.1(2) . . ?
 C19 C20 H20 119.4 . . ?
 C22 C21 C5 119.8(2) . . ?
 C22 C21 C26 119.0(2) . . ?
 C26 C21 C5 121.2(2) . . ?
 C21 C22 H22 119.6 . . ?
 C23 C22 C21 120.7(2) . . ?
 C23 C22 H22 119.6 . . ?
 C22 C23 H23 120.0 . . ?
 C24 C23 C22 120.0(2) . . ?
 C24 C23 H23 120.0 . . ?
 C23 C24 H24 120.1 . . ?
 C25 C24 C23 119.7(2) . . ?
 C25 C24 H24 120.1 . . ?
 C24 C25 H25 119.4 . . ?
 C24 C25 C26 121.1(2) . . ?
 C26 C25 H25 119.4 . . ?
 C21 C26 H26 120.3 . . ?
 C25 C26 C21 119.5(2) . . ?
 C25 C26 H26 120.3 . . ?
 C3A O3A C4A 119.49(16) . . ?
 C5A O4A C4A 124.96(17) . . ?
 C1A N1A C8A 117.13(19) . . ?
 C7A N1A C1A 124.7(2) . . ?
 C7A N1A C8A 118.13(19) . . ?
 O2A C1A N1A 123.5(2) . . ?
 O2A C1A C2A 121.6(2) . . ?
 N1A C1A C2A 114.8(2) . . ?
 C1A C2A H2A 117.4 . . ?
 C3A C2A C1A 125.2(2) . . ?
 C3A C2A H2A 117.4 . . ?
 O3A C3A C9A 112.89(19) . . ?
 C2A C3A O3A 121.7(2) . . ?
 C2A C3A C9A 125.2(2) . . ?
 O3A C4A C8A 110.63(17) . . ?
 O3A C4A C15A 108.70(18) . . ?
 O4A C4A O3A 100.96(16) . . ?
 O4A C4A C8A 112.40(18) . . ?
 O4A C4A C15A 106.67(17) . . ?
 C8A C4A C15A 116.31(19) . . ?
 O4A C5A C21A 109.24(19) . . ?
 C6A C5A O4A 127.0(2) . . ?
 C6A C5A C21A 123.7(2) . . ?
 C5A C6A H6A 114.9 . . ?
 C5A C6A C7A 130.2(2) . . ?
 C7A C6A H6A 114.9 . . ?
 O1A C7A N1A 123.1(2) . . ?
 O1A C7A C6A 121.5(2) . . ?
 N1A C7A C6A 115.3(2) . . ?
 N1A C8A C4A 110.58(18) . . ?
 N1A C8A H8AA 109.5 . . ?
 N1A C8A H8AB 109.5 . . ?
 C4A C8A H8AA 109.5 . . ?
 C4A C8A H8AB 109.5 . . ?
 H8AA C8A H8AB 108.1 . . ?
 C10A C9A C3A 121.2(2) . . ?
 C14A C9A C3A 120.2(2) . . ?
 C14A C9A C10A 118.6(2) . . ?
 C9A C10A H10A 119.9 . . ?
 C11A C10A C9A 120.2(2) . . ?
 C11A C10A H10A 119.9 . . ?
 C10A C11A H11A 119.6 . . ?
 C12A C11A C10A 120.9(2) . . ?
 C12A C11A H11A 119.6 . . ?
 C11A C12A H12A 120.4 . . ?
 C13A C12A C11A 119.2(2) . . ?
 C13A C12A H12A 120.4 . . ?
 C12A C13A H13A 119.5 . . ?
 C12A C13A C14A 120.9(2) . . ?
 C14A C13A H13A 119.5 . . ?
 C9A C14A H14A 119.9 . . ?
 C13A C14A C9A 120.3(2) . . ?
 C13A C14A H14A 119.9 . . ?
 C16A C15A C4A 123.0(2) . . ?
 C20A C15A C4A 118.5(2) . . ?
 C20A C15A C16A 118.5(2) . . ?
 C15A C16A H16A 119.9 . . ?
 C17A C16A C15A 120.3(2) . . ?
 C17A C16A H16A 119.9 . . ?
 C16A C17A H17A 119.7 . . ?
 C18A C17A C16A 120.7(2) . . ?
 C18A C17A H17A 119.7 . . ?
 C17A C18A H18A 120.0 . . ?
 C17A C18A C19A 120.0(2) . . ?
 C19A C18A H18A 120.0 . . ?
 C18A C19A H19A 120.2 . . ?
 C18A C19A C20A 119.7(2) . . ?
 C20A C19A H19A 120.2 . . ?
 C15A C20A H20A 119.5 . . ?
 C19A C20A C15A 120.9(2) . . ?
 C19A C20A H20A 119.5 . . ?
 C22A C21A C5A 119.9(2) . . ?
 C22A C21A C26A 118.6(2) . . ?
 C26A C21A C5A 121.4(2) . . ?
 C21A C22A H22A 119.8 . . ?
 C23A C22A C21A 120.5(2) . . ?
 C23A C22A H22A 119.8 . . ?
 C22A C23A H23A 119.8 . . ?
 C24A C23A C22A 120.4(2) . . ?
 C24A C23A H23A 119.8 . . ?
 C23A C24A H24A 120.1 . . ?
 C25A C24A C23A 119.7(2) . . ?
 C25A C24A H24A 120.1 . . ?
 C24A C25A H25A 119.7 . . ?
 C24A C25A C26A 120.7(2) . . ?
 C26A C25A H25A 119.7 . . ?
 C21A C26A C25A 120.1(2) . . ?
 C21A C26A H26A 119.9 . . ?
 C25A C26A H26A 119.9 . . ?

_smtbx_masks_special_details      ?
loop_
  _smtbx_masks_void_nr
  _smtbx_masks_void_average_x
  _smtbx_masks_void_average_y
  _smtbx_masks_void_average_z
  _smtbx_masks_void_volume
  _smtbx_masks_void_count_electrons
  _smtbx_masks_void_content
 1 0.000 0.000 0.500 243.7 57.0 ?
 2 0.500 0.500 1.000 243.7 57.0 ?
 3 0.222 0.874 0.808 9.0 0.0 ?
 4 0.278 0.374 0.692 9.0 0.0 ?
 5 0.722 0.626 0.308 9.0 0.0 ?
 6 0.778 0.126 0.192 9.0 0.0 ?
# start Validation Reply Form
_vrf_PLAT027_I
;
PROBLEM: _diffrn_reflns_theta_full (too) Low ............      58.00 Deg.  
RESPONSE: extremely thin needle-like crystals did not diffact X-ray above that
treshhold. No reflections were observed there even at maximum power setting 
of rotating anode generator and long (30 sec/frame) exposure time. Longer 
exposure time did not help either. 
;
_vrf_PLAT601_I
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        231 Ang3  
RESPONSE: The structure contains a severely disordered
solvent molecule (hexane?) which was impossible to model satisfactory. 
The contribution of the solvent to the structural factors was taken into 
account by applying MASK procedure of OLEX2 program package. 
See _smtbx_masks_special_details.
;
# end Validation Reply Form
