# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_psu-26(md-313)
_audit_block_doi                 10.5517/ccdc.csd.cc24lb25
_database_code_depnum_ccdc_archive 'CCDC 1983816'
loop_
_audit_author_name
_audit_author_address
'Vladimir Zhulanov'
;Perm State University
Russia
;
_audit_update_record             
;
2020-02-13 deposited with the CCDC.	2020-04-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
"Methyl (1R,3S,5r,7r)-8'-(4-methylbenzoyl)-4',4'-diphenyl-4'H-spiro-[adamantane-2,2'-pyrazolo[5,1-d][1,3,5]dioxazine]-7'-carboxylate"
_chemical_name_common            none
_chemical_melting_point          '165 -- 170 \%C (decomposition, acetone).'
_chemical_formula_moiety         'C35 H32 N2 O5'
_chemical_formula_sum            'C35 H32 N2 O5'
_chemical_formula_weight         560.63

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5718(13)
_cell_length_b                   10.6288(12)
_cell_length_c                   13.5806(17)
_cell_angle_alpha                100.473(10)
_cell_angle_beta                 97.068(10)
_cell_angle_gamma                103.526(10)
_cell_volume                     1436.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    4200
_cell_measurement_theta_min      3.7850
_cell_measurement_theta_max      28.8550

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             592
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.92745
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13186
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.85
_diffrn_reflns_theta_max         29.61
_reflns_number_total             6834
_reflns_number_gt                5019
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 > 2σ(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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0665P)²+0.1032P] where P=(Fo²+2Fc²)/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         6834
_refine_ls_number_parameters     380
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0523
_refine_ls_wR_factor_ref         0.1459
_refine_ls_wR_factor_gt          0.1289
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C33 C 0.35704(16) 0.87170(17) 0.43581(14) 0.0532(4) Uani 1 1 d . . .
H33A H 0.3751 0.8983 0.5094 0.064 Uiso 1 1 calc R . .
H33B H 0.3595 0.9504 0.4087 0.064 Uiso 1 1 calc R . .
O5 O 0.52319(8) 0.70515(9) 0.23570(7) 0.0362(2) Uani 1 1 d . . .
O4 O 0.42680(9) 0.88050(10) 0.24071(8) 0.0455(3) Uani 1 1 d . . .
N2 N 0.65476(11) 0.91802(11) 0.24943(9) 0.0367(3) Uani 1 1 d . . .
C7 C 0.65755(12) 0.77888(13) 0.24509(10) 0.0344(3) Uani 1 1 d . . .
N1 N 0.76421(11) 1.01367(12) 0.24308(9) 0.0400(3) Uani 1 1 d . . .
C6 C 0.74273(13) 0.76219(14) 0.33777(10) 0.0350(3) Uani 1 1 d . . .
C34 C 0.46282(14) 0.80572(15) 0.39861(11) 0.0411(3) Uani 1 1 d . . .
H34 H 0.5505 0.8682 0.4207 0.049 Uiso 1 1 calc R . .
C25 C 0.54465(13) 0.95969(14) 0.23954(11) 0.0369(3) Uani 1 1 d . . .
C26 C 0.43299(13) 0.76463(13) 0.28304(11) 0.0362(3) Uani 1 1 d . . .
C27 C 0.29733(14) 0.66751(15) 0.24799(12) 0.0434(4) Uani 1 1 d . . .
H27 H 0.2792 0.6409 0.1736 0.052 Uiso 1 1 calc R . .
C17 C 0.57913(13) 1.09029(14) 0.22964(11) 0.0386(3) Uani 1 1 d . . .
C8 C 0.70430(13) 0.72899(14) 0.14641(10) 0.0375(3) Uani 1 1 d . . .
C15 C 0.80632(14) 1.24045(15) 0.21954(13) 0.0438(4) Uani 1 1 d . . .
C29 C 0.22013(15) 0.77438(17) 0.40085(14) 0.0535(4) Uani 1 1 d . . .
H29 H 0.1531 0.8169 0.4243 0.064 Uiso 1 1 calc R . .
O3 O 0.76338(13) 1.26797(13) 0.13243(10) 0.0676(4) Uani 1 1 d . . .
O1 O 0.55147(12) 1.30465(12) 0.26326(11) 0.0688(4) Uani 1 1 d . . .
C9 C 0.83658(15) 0.74303(16) 0.14482(12) 0.0459(4) Uani 1 1 d . . .
H9 H 0.8975 0.7785 0.2047 0.055 Uiso 1 1 calc R . .
C19 C 0.35470(14) 1.13442(15) 0.20075(12) 0.0422(3) Uani 1 1 d . . .
C31 C 0.32157(16) 0.58610(16) 0.40913(12) 0.0490(4) Uani 1 1 d . . .
H31 H 0.3193 0.5075 0.4378 0.059 Uiso 1 1 calc R . .
C14 C 0.71691(13) 1.11616(14) 0.23249(11) 0.0378(3) Uani 1 1 d . . .
C5 C 0.75231(15) 0.63444(16) 0.33960(12) 0.0451(4) Uani 1 1 d . . .
H5 H 0.7060 0.5643 0.2863 0.054 Uiso 1 1 calc R . .
C32 C 0.29517(15) 0.54533(15) 0.29361(12) 0.0474(4) Uani 1 1 d . . .
H32A H 0.2097 0.4815 0.2706 0.057 Uiso 1 1 calc R . .
H32B H 0.3620 0.5037 0.2709 0.057 Uiso 1 1 calc R . .
C18 C 0.49932(14) 1.18609(15) 0.23303(12) 0.0434(3) Uani 1 1 d . . .
C1 C 0.81016(14) 0.86512(16) 0.41756(11) 0.0442(4) Uani 1 1 d . . .
H1 H 0.8051 0.9511 0.4169 0.053 Uiso 1 1 calc R . .
O2 O 0.90283(12) 1.30503(13) 0.27767(11) 0.0753(4) Uani 1 1 d . . .
C30 C 0.21669(17) 0.65220(18) 0.44558(14) 0.0551(4) Uani 1 1 d . . .
H30A H 0.1300 0.5902 0.4243 0.066 Uiso 1 1 calc R . .
H30B H 0.2337 0.6779 0.5192 0.066 Uiso 1 1 calc R . .
C28 C 0.19267(14) 0.73407(18) 0.28512(14) 0.0537(4) Uani 1 1 d . . .
H28A H 0.1944 0.8118 0.2568 0.064 Uiso 1 1 calc R . .
H28B H 0.1056 0.6731 0.2622 0.064 Uiso 1 1 calc R . .
C35 C 0.45806(15) 0.68309(17) 0.44325(12) 0.0482(4) Uani 1 1 d . . .
H35A H 0.5244 0.6406 0.4207 0.058 Uiso 1 1 calc R . .
H35B H 0.4772 0.7090 0.5169 0.058 Uiso 1 1 calc R . .
C20 C 0.30120(16) 1.03649(17) 0.11330(13) 0.0527(4) Uani 1 1 d . . .
H20 H 0.3566 1.0012 0.0747 0.063 Uiso 1 1 calc R . .
C4 C 0.82986(17) 0.61101(19) 0.41970(13) 0.0549(4) Uani 1 1 d . . .
H4 H 0.8369 0.5254 0.4198 0.066 Uiso 1 1 calc R . .
C11 C 0.79134(19) 0.65313(18) -0.03407(13) 0.0615(5) Uani 1 1 d . . .
H11 H 0.8206 0.6274 -0.0945 0.074 Uiso 1 1 calc R . .
C24 C 0.27104(16) 1.18561(18) 0.25782(14) 0.0546(4) Uani 1 1 d . . .
H24 H 0.3059 1.2527 0.3158 0.066 Uiso 1 1 calc R . .
C2 C 0.88581(15) 0.83990(19) 0.49904(12) 0.0556(4) Uani 1 1 d . . .
H2 H 0.9294 0.9090 0.5539 0.067 Uiso 1 1 calc R . .
C3 C 0.89671(17) 0.7134(2) 0.49925(14) 0.0598(5) Uani 1 1 d . . .
H3 H 0.9493 0.6974 0.5533 0.072 Uiso 1 1 calc R . .
C10 C 0.87986(17) 0.70470(17) 0.05461(13) 0.0566(4) Uani 1 1 d . . .
H10 H 0.9695 0.7141 0.0544 0.068 Uiso 1 1 calc R . .
C13 C 0.61540(17) 0.67733(18) 0.05631(12) 0.0539(4) Uani 1 1 d . . .
H13 H 0.5256 0.6679 0.0559 0.065 Uiso 1 1 calc R . .
C23 C 0.13620(18) 1.1370(2) 0.22864(16) 0.0671(5) Uani 1 1 d . . .
H23 H 0.0800 1.1695 0.2681 0.080 Uiso 1 1 calc R . .
C22 C 0.08479(17) 1.0411(2) 0.14176(18) 0.0706(6) Uani 1 1 d . . .
H22 H -0.0063 1.0094 0.1221 0.085 Uiso 1 1 calc R . .
C12 C 0.6601(2) 0.6396(2) -0.03342(13) 0.0658(5) Uani 1 1 d . . .
H12 H 0.5999 0.6047 -0.0938 0.079 Uiso 1 1 calc R . .
C21 C 0.16610(18) 0.9914(2) 0.08350(16) 0.0674(5) Uani 1 1 d . . .
H21 H 0.1303 0.9273 0.0239 0.081 Uiso 1 1 calc R . .
C16 C 0.8335(2) 1.3919(2) 0.11181(19) 0.0899(7) Uani 1 1 d . . .
H16A H 0.8372 1.4633 0.1676 0.135 Uiso 1 1 calc R . .
H16B H 0.7882 1.4061 0.0507 0.135 Uiso 1 1 calc R . .
H16C H 0.9216 1.3886 0.1034 0.135 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
C33 C29 1.530(2) . ?
C33 C34 1.541(2) . ?
O5 C26 1.4168(16) . ?
O5 C7 1.4305(15) . ?
O4 C25 1.3342(16) . ?
O4 C26 1.4620(17) . ?
N2 C25 1.3393(18) . ?
N2 N1 1.3733(15) . ?
N2 C7 1.4766(17) . ?
C7 C6 1.5177(19) . ?
C7 C8 1.5326(19) . ?
N1 C14 1.3235(18) . ?
C6 C1 1.376(2) . ?
C6 C5 1.389(2) . ?
C34 C26 1.523(2) . ?
C34 C35 1.527(2) . ?
C25 C17 1.3861(19) . ?
C26 C27 1.5198(18) . ?
C27 C28 1.534(2) . ?
C27 C32 1.534(2) . ?
C17 C14 1.4119(19) . ?
C17 C18 1.465(2) . ?
C8 C9 1.375(2) . ?
C8 C13 1.383(2) . ?
C15 O2 1.1885(19) . ?
C15 O3 1.3217(19) . ?
C15 C14 1.487(2) . ?
C29 C28 1.524(2) . ?
C29 C30 1.525(2) . ?
O3 C16 1.446(2) . ?
O1 C18 1.2213(18) . ?
C9 C10 1.386(2) . ?
C19 C24 1.385(2) . ?
C19 C20 1.387(2) . ?
C19 C18 1.478(2) . ?
C31 C32 1.522(2) . ?
C31 C35 1.525(2) . ?
C31 C30 1.530(2) . ?
C5 C4 1.375(2) . ?
C1 C2 1.388(2) . ?
C20 C21 1.379(2) . ?
C4 C3 1.369(3) . ?
C11 C12 1.362(3) . ?
C11 C10 1.367(3) . ?
C24 C23 1.378(2) . ?
C2 C3 1.377(3) . ?
C13 C12 1.386(2) . ?
C23 C22 1.368(3) . ?
C22 C21 1.368(3) . ?

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
C29 C33 C34 109.84(13) . . ?
C26 O5 C7 120.08(10) . . ?
C25 O4 C26 114.14(10) . . ?
C25 N2 N1 112.02(11) . . ?
C25 N2 C7 124.72(11) . . ?
N1 N2 C7 122.00(11) . . ?
O5 C7 N2 106.11(10) . . ?
O5 C7 C6 111.20(10) . . ?
N2 C7 C6 112.73(11) . . ?
O5 C7 C8 106.72(10) . . ?
N2 C7 C8 107.88(10) . . ?
C6 C7 C8 111.84(11) . . ?
C14 N1 N2 103.50(11) . . ?
C1 C6 C5 119.41(14) . . ?
C1 C6 C7 123.91(13) . . ?
C5 C6 C7 116.67(13) . . ?
C26 C34 C35 109.53(12) . . ?
C26 C34 C33 109.04(12) . . ?
C35 C34 C33 108.71(12) . . ?
O4 C25 N2 121.56(12) . . ?
O4 C25 C17 130.23(13) . . ?
N2 C25 C17 108.21(11) . . ?
O5 C26 O4 107.29(10) . . ?
O5 C26 C27 106.84(11) . . ?
O4 C26 C27 106.02(11) . . ?
O5 C26 C34 116.51(11) . . ?
O4 C26 C34 109.41(11) . . ?
C27 C26 C34 110.22(11) . . ?
C26 C27 C28 109.20(13) . . ?
C26 C27 C32 108.74(12) . . ?
C28 C27 C32 109.58(12) . . ?
C25 C17 C14 102.71(12) . . ?
C25 C17 C18 129.23(12) . . ?
C14 C17 C18 127.31(13) . . ?
C9 C8 C13 118.88(14) . . ?
C9 C8 C7 120.31(13) . . ?
C13 C8 C7 120.67(13) . . ?
O2 C15 O3 124.74(15) . . ?
O2 C15 C14 125.57(15) . . ?
O3 C15 C14 109.69(13) . . ?
C28 C29 C30 109.83(14) . . ?
C28 C29 C33 109.14(13) . . ?
C30 C29 C33 109.19(14) . . ?
C15 O3 C16 116.72(16) . . ?
C8 C9 C10 120.49(15) . . ?
C24 C19 C20 119.32(15) . . ?
C24 C19 C18 119.65(15) . . ?
C20 C19 C18 121.02(14) . . ?
C32 C31 C35 108.54(12) . . ?
C32 C31 C30 109.99(14) . . ?
C35 C31 C30 109.86(14) . . ?
N1 C14 C17 113.52(12) . . ?
N1 C14 C15 119.89(12) . . ?
C17 C14 C15 126.50(13) . . ?
C4 C5 C6 120.43(16) . . ?
C31 C32 C27 109.90(13) . . ?
O1 C18 C17 120.47(13) . . ?
O1 C18 C19 121.56(14) . . ?
C17 C18 C19 117.96(13) . . ?
C6 C1 C2 119.66(16) . . ?
C29 C30 C31 109.47(13) . . ?
C29 C28 C27 109.80(13) . . ?
C31 C35 C34 109.87(12) . . ?
C21 C20 C19 120.12(17) . . ?
C3 C4 C5 120.16(17) . . ?
C12 C11 C10 119.67(16) . . ?
C23 C24 C19 119.92(18) . . ?
C3 C2 C1 120.48(16) . . ?
C4 C3 C2 119.82(15) . . ?
C11 C10 C9 120.29(16) . . ?
C8 C13 C12 120.01(16) . . ?
C22 C23 C24 120.11(18) . . ?
C23 C22 C21 120.66(17) . . ?
C11 C12 C13 120.65(17) . . ?
C22 C21 C20 119.83(19) . . ?

_diffrn_measured_fraction_theta_max 0.845
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.049
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: ethanol'
_chemical_compound_source        none
_chemical_properties_physical    Moisture-sensitive,Heat-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_psu-876(vzh-134)-1
_audit_block_doi                 10.5517/ccdc.csd.cc24lbdh
_database_code_depnum_ccdc_archive 'CCDC 1983826'
loop_
_audit_author_name
_audit_author_address
'Vladimir Zhulanov'
;Perm State University
Russia
;
_audit_update_record             
;
2020-02-13 deposited with the CCDC.	2020-04-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
"Methyl 8'-(4-methylbenzoyl)-4',4'-diphenyl-4'H-spiro[cyclohexane-1,2'-pyrazolo[5,1-d][1,3,5]dioxazine]-7'-carboxylate"
_chemical_name_common            none
_chemical_melting_point          '143 -- 145 \%C (decomposition, acetone)'
_chemical_formula_moiety         '2(C32 H30 N2 O5), C2 H6 O'
_chemical_formula_sum            'C66 H66 N4 O11'
_chemical_formula_weight         1091.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   9.2689(14)
_cell_length_b                   9.7820(12)
_cell_length_c                   35.199(3)
_cell_angle_alpha                94.886(9)
_cell_angle_beta                 92.570(10)
_cell_angle_gamma                115.038(13)
_cell_volume                     2869.5(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    4873
_cell_measurement_theta_min      2.4210
_cell_measurement_theta_max      24.5490

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1156
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_min  0.61769
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'New Xcalibur, Ruby'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28351
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_sigmaI/netI    0.0780
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_theta_min         2.31
_diffrn_reflns_theta_max         29.53
_reflns_number_total             13469
_reflns_number_gt                7998
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 > 2σ(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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0986P)²+0.5034P] where P=(Fo²+2Fc²)/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       0.0100(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         13469
_refine_ls_number_parameters     744
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1265
_refine_ls_R_factor_gt           0.0759
_refine_ls_wR_factor_ref         0.2195
_refine_ls_wR_factor_gt          0.1856
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.003
_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 -0.0136(5) -0.2852(4) 0.14978(13) 0.0752(15) Uani 0.801(7) 1 d P A 1
H1A H -0.0634 -0.3756 0.1320 0.113 Uiso 0.801(7) 1 calc PR A 1
H1B H -0.0872 -0.2841 0.1680 0.113 Uiso 0.801(7) 1 calc PR A 1
H1C H 0.0802 -0.2836 0.1629 0.113 Uiso 0.801(7) 1 calc PR A 1
C1B C 0.051(3) -0.180(2) 0.1911(5) 0.101(9) Uani 0.199(7) 1 d P A 2
H1B1 H 0.0579 -0.1883 0.2180 0.152 Uiso 0.199(7) 1 calc PR A 2
H1B2 H 0.1121 -0.2253 0.1784 0.152 Uiso 0.199(7) 1 calc PR A 2
H1B3 H -0.0586 -0.2305 0.1808 0.152 Uiso 0.199(7) 1 calc PR A 2
C2S C 0.8213(15) 0.9512(8) 0.2512(3) 0.409(13) Uani 1 1 d D . .
H2S1 H 0.8691 0.9232 0.2298 0.490 Uiso 1 1 calc R . .
H2S2 H 0.7460 0.8588 0.2603 0.490 Uiso 1 1 calc R . .
O1S O 0.7416(8) 1.0364(9) 0.2397(3) 0.366(6) Uani 1 1 d D . .
H1S H 0.7740 1.0701 0.2196 0.549 Uiso 1 1 calc R . .
C1S C 0.9501(9) 1.0455(10) 0.2831(3) 0.303(7) Uani 1 1 d D . .
H1S1 H 1.0107 0.9908 0.2898 0.455 Uiso 1 1 calc R . .
H1S2 H 0.9012 1.0655 0.3050 0.455 Uiso 1 1 calc R . .
H1S3 H 1.0199 1.1399 0.2745 0.455 Uiso 1 1 calc R . .
O4A O 0.2637(2) 0.62570(17) 0.39950(5) 0.0429(4) Uani 1 1 d . . .
O5A O 0.1238(2) 0.51851(17) 0.45096(4) 0.0415(4) Uani 1 1 d . . .
N1A N 0.2672(3) 0.2688(2) 0.40136(6) 0.0441(5) Uani 1 1 d . . .
N2A N 0.2229(2) 0.3816(2) 0.41267(5) 0.0394(5) Uani 1 1 d . . .
O1A O 0.5798(2) 0.3043(2) 0.34839(5) 0.0554(5) Uani 1 1 d . . .
C13A C 0.2892(3) 0.5024(2) 0.39278(6) 0.0366(5) Uani 1 1 d . . .
C4A C 0.3797(3) 0.4696(3) 0.36626(7) 0.0408(6) Uani 1 1 d . . .
C14A C 0.1191(3) 0.3712(2) 0.44383(6) 0.0382(5) Uani 1 1 d . . .
C15A C 0.1217(3) 0.6006(3) 0.41970(7) 0.0404(5) Uani 1 1 d . . .
C6A C 0.4857(3) 0.4982(3) 0.30051(7) 0.0457(6) Uani 1 1 d . . .
C21A C 0.1934(3) 0.3427(3) 0.48031(6) 0.0388(5) Uani 1 1 d . . .
C3A C 0.3598(3) 0.3221(3) 0.37340(7) 0.0421(6) Uani 1 1 d . . .
C27A C -0.0518(3) 0.2499(3) 0.43312(7) 0.0420(6) Uani 1 1 d . . .
O3A O 0.5235(3) 0.7057(2) 0.34505(6) 0.0735(6) Uani 1 1 d . . .
O2A O 0.3515(3) 0.0905(2) 0.34487(6) 0.0766(7) Uani 1 1 d . . .
C20A C 0.1433(4) 0.7548(3) 0.43676(8) 0.0530(7) Uani 1 1 d . . .
H20A H 0.2429 0.8028 0.4530 0.064 Uiso 1 1 calc R . .
H20B H 0.0568 0.7436 0.4526 0.064 Uiso 1 1 calc R . .
C22A C 0.2954(3) 0.4631(3) 0.50650(7) 0.0464(6) Uani 1 1 d . . .
H22A H 0.3191 0.5623 0.5020 0.056 Uiso 1 1 calc R . .
C32A C -0.0933(4) 0.1335(3) 0.40372(8) 0.0546(7) Uani 1 1 d . . .
H32A H -0.0154 0.1256 0.3891 0.065 Uiso 1 1 calc R . .
C5A C 0.4682(3) 0.5682(3) 0.33785(7) 0.0468(6) Uani 1 1 d . . .
C23A C 0.3618(3) 0.4358(3) 0.53928(8) 0.0578(7) Uani 1 1 d . . .
H23A H 0.4276 0.5170 0.5571 0.069 Uiso 1 1 calc R . .
C7A C 0.3706(3) 0.3596(3) 0.28301(7) 0.0507(7) Uani 1 1 d . . .
H7A H 0.2775 0.3091 0.2947 0.061 Uiso 1 1 calc R . .
C2A C 0.4269(4) 0.2243(3) 0.35448(7) 0.0498(7) Uani 1 1 d . . .
C26A C 0.1634(3) 0.1968(3) 0.48723(8) 0.0538(7) Uani 1 1 d . . .
H26A H 0.0953 0.1150 0.4699 0.065 Uiso 1 1 calc R . .
C11A C 0.6221(3) 0.5724(4) 0.28190(8) 0.0596(8) Uani 1 1 d . . .
H11A H 0.6995 0.6667 0.2927 0.072 Uiso 1 1 calc R . .
C9A C 0.5305(4) 0.3675(4) 0.23075(8) 0.0700(9) Uani 1 1 d . . .
C19A C 0.1454(4) 0.8562(3) 0.40589(9) 0.0634(8) Uani 1 1 d . . .
H19A H 0.1523 0.9521 0.4179 0.076 Uiso 1 1 calc R . .
H19B H 0.2391 0.8774 0.3919 0.076 Uiso 1 1 calc R . .
C28A C -0.1685(3) 0.2574(3) 0.45488(9) 0.0575(7) Uani 1 1 d . . .
H28A H -0.1410 0.3337 0.4752 0.069 Uiso 1 1 calc R . .
C16A C -0.0244(3) 0.5237(3) 0.39109(8) 0.0535(7) Uani 1 1 d . . .
H16A H -0.1202 0.4979 0.4044 0.064 Uiso 1 1 calc R . .
H16B H -0.0266 0.4303 0.3787 0.064 Uiso 1 1 calc R . .
C24A C 0.3321(4) 0.2912(3) 0.54586(8) 0.0601(8) Uani 1 1 d . . .
H24A H 0.3782 0.2739 0.5679 0.072 Uiso 1 1 calc R . .
C25A C 0.2336(4) 0.1711(3) 0.51972(9) 0.0645(8) Uani 1 1 d . . .
H25A H 0.2141 0.0724 0.5239 0.077 Uiso 1 1 calc R . .
C18A C -0.0040(4) 0.7806(4) 0.37818(10) 0.0771(10) Uani 1 1 d . . .
H18A H -0.0970 0.7686 0.3916 0.093 Uiso 1 1 calc R . .
H18B H 0.0028 0.8446 0.3581 0.093 Uiso 1 1 calc R . .
C1A C 0.6484(4) 0.2236(4) 0.32437(9) 0.0693(9) Uani 1 1 d . . .
H1A1 H 0.6327 0.1307 0.3345 0.104 Uiso 1 1 calc R . .
H1A2 H 0.7607 0.2856 0.3239 0.104 Uiso 1 1 calc R . .
H1A3 H 0.5971 0.2010 0.2988 0.104 Uiso 1 1 calc R . .
C8A C 0.3922(4) 0.2957(4) 0.24852(8) 0.0617(8) Uani 1 1 d . . .
H8A H 0.3130 0.2035 0.2371 0.074 Uiso 1 1 calc R . .
C30A C -0.3676(4) 0.0377(4) 0.41723(11) 0.0744(10) Uani 1 1 d . . .
H30A H -0.4736 -0.0328 0.4117 0.089 Uiso 1 1 calc R . .
C29A C -0.3267(4) 0.1524(4) 0.44687(11) 0.0742(9) Uani 1 1 d . . .
H29A H -0.4050 0.1595 0.4615 0.089 Uiso 1 1 calc R . .
C17A C -0.0227(4) 0.6276(3) 0.36069(9) 0.0686(9) Uani 1 1 d . . .
H17A H 0.0647 0.6412 0.3450 0.082 Uiso 1 1 calc R . .
H17B H -0.1217 0.5794 0.3442 0.082 Uiso 1 1 calc R . .
C10A C 0.6432(4) 0.5074(4) 0.24764(9) 0.0743(10) Uani 1 1 d . . .
H10A H 0.7351 0.5586 0.2356 0.089 Uiso 1 1 calc R . .
C31A C -0.2529(4) 0.0275(3) 0.39602(10) 0.0703(10) Uani 1 1 d . . .
H31A H -0.2808 -0.0506 0.3762 0.084 Uiso 1 1 calc R . .
C12A C 0.5561(5) 0.2959(6) 0.19328(10) 0.1120(16) Uani 1 1 d . . .
H12A H 0.6359 0.3726 0.1807 0.168 Uiso 1 1 calc R . .
H12B H 0.4575 0.2507 0.1771 0.168 Uiso 1 1 calc R . .
H12C H 0.5911 0.2193 0.1983 0.168 Uiso 1 1 calc R . .
O5 O 0.28015(19) 0.49183(17) 0.11098(5) 0.0417(4) Uani 1 1 d . . .
O4 O 0.37964(19) 0.45653(17) 0.05278(4) 0.0402(4) Uani 1 1 d . . .
N2 N 0.2974(2) 0.2644(2) 0.09141(5) 0.0379(4) Uani 1 1 d . . .
N1 N 0.2439(2) 0.1179(2) 0.10006(6) 0.0417(5) Uani 1 1 d . . .
O3 O -0.0669(2) 0.1759(2) 0.17488(6) 0.0684(6) Uani 1 1 d . . .
C14 C 0.3887(3) 0.3176(2) 0.05834(6) 0.0362(5) Uani 1 1 d . . .
C4 C 0.1592(3) 0.2554(3) 0.14176(7) 0.0378(5) Uani 1 1 d . . .
C15 C 0.4015(3) 0.5646(3) 0.08473(7) 0.0412(6) Uani 1 1 d . . .
C13 C 0.2495(3) 0.3480(2) 0.11574(7) 0.0367(5) Uani 1 1 d . . .
C27 C 0.3040(3) 0.2081(3) 0.02252(7) 0.0405(6) Uani 1 1 d . . .
C21 C 0.5619(3) 0.3399(2) 0.06510(6) 0.0362(5) Uani 1 1 d . . .
C3 C 0.1610(3) 0.1146(3) 0.13007(7) 0.0399(5) Uani 1 1 d . . .
O1 O 0.0323(3) -0.1494(2) 0.12870(6) 0.0706(6) Uani 1 1 d . . .
C26 C 0.6131(3) 0.2763(3) 0.09367(7) 0.0438(6) Uani 1 1 d . . .
H26 H 0.5408 0.2174 0.1098 0.053 Uiso 1 1 calc R . .
C5 C 0.0639(3) 0.2797(3) 0.17198(7) 0.0431(6) Uani 1 1 d . . .
C6 C 0.1249(3) 0.4232(3) 0.19783(7) 0.0443(6) Uani 1 1 d . . .
C16 C 0.3615(4) 0.6841(3) 0.06942(8) 0.0562(7) Uani 1 1 d . . .
H16C H 0.2517 0.6374 0.0581 0.067 Uiso 1 1 calc R . .
H16D H 0.4301 0.7268 0.0494 0.067 Uiso 1 1 calc R . .
C24 C 0.8783(3) 0.3868(3) 0.07432(9) 0.0622(8) Uani 1 1 d . . .
H24 H 0.9848 0.4034 0.0776 0.075 Uiso 1 1 calc R . .
C32 C 0.1860(3) 0.2241(3) 0.00034(7) 0.0499(6) Uani 1 1 d . . .
H32 H 0.1577 0.3026 0.0075 0.060 Uiso 1 1 calc R . .
C25 C 0.7704(3) 0.3004(3) 0.09815(8) 0.0540(7) Uani 1 1 d . . .
H25 H 0.8042 0.2582 0.1174 0.065 Uiso 1 1 calc R . .
C31 C 0.1094(3) 0.1246(3) -0.03241(8) 0.0598(8) Uani 1 1 d . . .
H31 H 0.0323 0.1381 -0.0474 0.072 Uiso 1 1 calc R . .
C20 C 0.5660(3) 0.6329(3) 0.10701(8) 0.0502(7) Uani 1 1 d . . .
H20C H 0.5799 0.5545 0.1197 0.060 Uiso 1 1 calc R . .
H20D H 0.6475 0.6684 0.0892 0.060 Uiso 1 1 calc R . .
C7 C 0.2827(3) 0.5301(3) 0.20021(7) 0.0510(7) Uani 1 1 d . . .
H7 H 0.3532 0.5135 0.1845 0.061 Uiso 1 1 calc R . .
C22 C 0.6707(3) 0.4247(3) 0.04071(7) 0.0479(6) Uani 1 1 d . . .
H22 H 0.6373 0.4655 0.0211 0.058 Uiso 1 1 calc R . .
C28 C 0.3396(3) 0.0871(3) 0.01195(8) 0.0530(7) Uani 1 1 d . . .
H28 H 0.4172 0.0733 0.0267 0.064 Uiso 1 1 calc R . .
O2 O 0.1170(4) -0.0143(2) 0.18495(7) 0.0972(9) Uani 1 1 d . . .
C2 C 0.1003(3) -0.0225(3) 0.15098(9) 0.0546(7) Uani 1 1 d . A .
C11 C 0.0231(4) 0.4492(4) 0.22231(9) 0.0653(8) Uani 1 1 d . . .
H11 H -0.0831 0.3786 0.2215 0.078 Uiso 1 1 calc R . .
C23 C 0.8283(3) 0.4483(3) 0.04573(9) 0.0588(7) Uani 1 1 d . . .
H23 H 0.9013 0.5063 0.0296 0.071 Uiso 1 1 calc R . .
C8 C 0.3369(4) 0.6610(3) 0.22555(8) 0.0635(8) Uani 1 1 d . . .
H8 H 0.4430 0.7319 0.2264 0.076 Uiso 1 1 calc R . .
C30 C 0.1480(3) 0.0067(4) -0.04244(8) 0.0618(8) Uani 1 1 d . . .
H30 H 0.0972 -0.0601 -0.0644 0.074 Uiso 1 1 calc R . .
C29 C 0.2615(4) -0.0130(3) -0.02014(9) 0.0651(8) Uani 1 1 d . . .
H29 H 0.2858 -0.0945 -0.0267 0.078 Uiso 1 1 calc R . .
C19 C 0.5896(4) 0.7645(3) 0.13683(9) 0.0637(8) Uani 1 1 d . . .
H19C H 0.5224 0.7254 0.1573 0.076 Uiso 1 1 calc R . .
H19D H 0.6999 0.8115 0.1477 0.076 Uiso 1 1 calc R . .
C17 C 0.3819(5) 0.8112(3) 0.10031(10) 0.0736(10) Uani 1 1 d . . .
H17C H 0.3606 0.8882 0.0888 0.088 Uiso 1 1 calc R . .
H17D H 0.3050 0.7708 0.1189 0.088 Uiso 1 1 calc R . .
C18 C 0.5497(5) 0.8830(3) 0.12044(11) 0.0789(10) Uani 1 1 d . . .
H18C H 0.6261 0.9325 0.1024 0.095 Uiso 1 1 calc R . .
H18D H 0.5575 0.9596 0.1409 0.095 Uiso 1 1 calc R . .
C10 C 0.0798(5) 0.5796(4) 0.24769(10) 0.0810(11) Uani 1 1 d . . .
H10 H 0.0106 0.5949 0.2640 0.097 Uiso 1 1 calc R . .
C9 C 0.2357(4) 0.6879(4) 0.24966(9) 0.0709(9) Uani 1 1 d . . .
C12 C 0.2966(6) 0.8314(5) 0.27762(12) 0.1117(15) Uani 1 1 d . . .
H12D H 0.2180 0.8230 0.2952 0.167 Uiso 1 1 calc R . .
H12E H 0.3163 0.9172 0.2638 0.167 Uiso 1 1 calc R . .
H12F H 0.3941 0.8448 0.2915 0.167 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 1.489(4) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1B O2 1.507(18) . ?
C1B H1B1 0.9600 . ?
C1B H1B2 0.9600 . ?
C1B H1B3 0.9600 . ?
C2S O1S 1.400(5) . ?
C2S C1S 1.518(5) . ?
C2S H2S1 0.9700 . ?
C2S H2S2 0.9700 . ?
O1S H1S 0.8200 . ?
C1S H1S1 0.9600 . ?
C1S H1S2 0.9600 . ?
C1S H1S3 0.9600 . ?
O4A C13A 1.328(3) . ?
O4A C15A 1.462(3) . ?
O5A C15A 1.421(3) . ?
O5A C14A 1.423(3) . ?
N1A C3A 1.327(3) . ?
N1A N2A 1.367(3) . ?
N2A C13A 1.353(3) . ?
N2A C14A 1.473(3) . ?
O1A C2A 1.336(3) . ?
O1A C1A 1.450(3) . ?
C13A C4A 1.388(3) . ?
C4A C3A 1.421(3) . ?
C4A C5A 1.474(3) . ?
C14A C27A 1.530(3) . ?
C14A C21A 1.531(3) . ?
C15A C20A 1.502(3) . ?
C15A C16A 1.517(3) . ?
C6A C7A 1.389(4) . ?
C6A C11A 1.390(4) . ?
C6A C5A 1.477(4) . ?
C21A C26A 1.380(3) . ?
C21A C22A 1.387(3) . ?
C3A C2A 1.475(4) . ?
C27A C28A 1.376(4) . ?
C27A C32A 1.382(4) . ?
O3A C5A 1.218(3) . ?
O2A C2A 1.202(3) . ?
C20A C19A 1.528(4) . ?
C20A H20A 0.9700 . ?
C20A H20B 0.9700 . ?
C22A C23A 1.382(4) . ?
C22A H22A 0.9300 . ?
C32A C31A 1.398(4) . ?
C32A H32A 0.9300 . ?
C23A C24A 1.365(4) . ?
C23A H23A 0.9300 . ?
C7A C8A 1.379(4) . ?
C7A H7A 0.9300 . ?
C26A C25A 1.384(4) . ?
C26A H26A 0.9300 . ?
C11A C10A 1.376(4) . ?
C11A H11A 0.9300 . ?
C9A C8A 1.383(4) . ?
C9A C10A 1.383(5) . ?
C9A C12A 1.516(4) . ?
C19A C18A 1.518(4) . ?
C19A H19A 0.9700 . ?
C19A H19B 0.9700 . ?
C28A C29A 1.387(4) . ?
C28A H28A 0.9300 . ?
C16A C17A 1.534(4) . ?
C16A H16A 0.9700 . ?
C16A H16B 0.9700 . ?
C24A C25A 1.376(4) . ?
C24A H24A 0.9300 . ?
C25A H25A 0.9300 . ?
C18A C17A 1.504(4) . ?
C18A H18A 0.9700 . ?
C18A H18B 0.9700 . ?
C1A H1A1 0.9600 . ?
C1A H1A2 0.9600 . ?
C1A H1A3 0.9600 . ?
C8A H8A 0.9300 . ?
C30A C31A 1.359(5) . ?
C30A C29A 1.378(5) . ?
C30A H30A 0.9300 . ?
C29A H29A 0.9300 . ?
C17A H17A 0.9700 . ?
C17A H17B 0.9700 . ?
C10A H10A 0.9300 . ?
C31A H31A 0.9300 . ?
C12A H12A 0.9600 . ?
C12A H12B 0.9600 . ?
C12A H12C 0.9600 . ?
O5 C13 1.339(3) . ?
O5 C15 1.467(3) . ?
O4 C15 1.421(3) . ?
O4 C14 1.426(3) . ?
N2 C13 1.350(3) . ?
N2 N1 1.371(3) . ?
N2 C14 1.470(3) . ?
N1 C3 1.329(3) . ?
O3 C5 1.224(3) . ?
C14 C27 1.524(3) . ?
C14 C21 1.530(3) . ?
C4 C13 1.389(3) . ?
C4 C3 1.411(3) . ?
C4 C5 1.479(3) . ?
C15 C16 1.500(3) . ?
C15 C20 1.526(4) . ?
C27 C28 1.384(4) . ?
C27 C32 1.385(3) . ?
C21 C22 1.390(3) . ?
C21 C26 1.392(3) . ?
C3 C2 1.491(4) . ?
O1 C2 1.296(3) . ?
C26 C25 1.374(4) . ?
C26 H26 0.9300 . ?
C5 C6 1.477(3) . ?
C6 C7 1.386(4) . ?
C6 C11 1.391(4) . ?
C16 C17 1.522(4) . ?
C16 H16C 0.9700 . ?
C16 H16D 0.9700 . ?
C24 C23 1.374(4) . ?
C24 C25 1.378(4) . ?
C24 H24 0.9300 . ?
C32 C31 1.389(4) . ?
C32 H32 0.9300 . ?
C25 H25 0.9300 . ?
C31 C30 1.369(4) . ?
C31 H31 0.9300 . ?
C20 C19 1.522(4) . ?
C20 H20C 0.9700 . ?
C20 H20D 0.9700 . ?
C7 C8 1.381(4) . ?
C7 H7 0.9300 . ?
C22 C23 1.380(4) . ?
C22 H22 0.9300 . ?
C28 C29 1.377(4) . ?
C28 H28 0.9300 . ?
O2 C2 1.190(3) . ?
C11 C10 1.377(4) . ?
C11 H11 0.9300 . ?
C23 H23 0.9300 . ?
C8 C9 1.383(4) . ?
C8 H8 0.9300 . ?
C30 C29 1.373(4) . ?
C30 H30 0.9300 . ?
C29 H29 0.9300 . ?
C19 C18 1.507(5) . ?
C19 H19C 0.9700 . ?
C19 H19D 0.9700 . ?
C17 C18 1.519(5) . ?
C17 H17C 0.9700 . ?
C17 H17D 0.9700 . ?
C18 H18C 0.9700 . ?
C18 H18D 0.9700 . ?
C10 C9 1.378(5) . ?
C10 H10 0.9300 . ?
C9 C12 1.517(4) . ?
C12 H12D 0.9600 . ?
C12 H12E 0.9600 . ?
C12 H12F 0.9600 . ?

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
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 C1B H1B1 109.5 . . ?
O2 C1B H1B2 109.5 . . ?
H1B1 C1B H1B2 109.5 . . ?
O2 C1B H1B3 109.5 . . ?
H1B1 C1B H1B3 109.5 . . ?
H1B2 C1B H1B3 109.5 . . ?
O1S C2S C1S 109.0(5) . . ?
O1S C2S H2S1 109.9 . . ?
C1S C2S H2S1 109.9 . . ?
O1S C2S H2S2 109.9 . . ?
C1S C2S H2S2 109.9 . . ?
H2S1 C2S H2S2 108.3 . . ?
C2S O1S H1S 109.5 . . ?
C2S C1S H1S1 109.5 . . ?
C2S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
C2S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
C13A O4A C15A 113.81(18) . . ?
C15A O5A C14A 119.55(17) . . ?
C3A N1A N2A 103.99(19) . . ?
C13A N2A N1A 112.02(19) . . ?
C13A N2A C14A 125.17(19) . . ?
N1A N2A C14A 122.77(18) . . ?
C2A O1A C1A 115.4(2) . . ?
O4A C13A N2A 122.0(2) . . ?
O4A C13A C4A 130.0(2) . . ?
N2A C13A C4A 108.0(2) . . ?
C13A C4A C3A 102.8(2) . . ?
C13A C4A C5A 126.0(2) . . ?
C3A C4A C5A 131.2(2) . . ?
O5A C14A N2A 105.29(18) . . ?
O5A C14A C27A 111.42(19) . . ?
N2A C14A C27A 112.13(19) . . ?
O5A C14A C21A 106.69(17) . . ?
N2A C14A C21A 109.41(19) . . ?
C27A C14A C21A 111.58(19) . . ?
O5A C15A O4A 108.10(18) . . ?
O5A C15A C20A 106.36(19) . . ?
O4A C15A C20A 106.0(2) . . ?
O5A C15A C16A 115.1(2) . . ?
O4A C15A C16A 108.4(2) . . ?
C20A C15A C16A 112.4(2) . . ?
C7A C6A C11A 118.1(2) . . ?
C7A C6A C5A 122.5(2) . . ?
C11A C6A C5A 119.4(2) . . ?
C26A C21A C22A 118.8(2) . . ?
C26A C21A C14A 120.5(2) . . ?
C22A C21A C14A 120.7(2) . . ?
N1A C3A C4A 113.2(2) . . ?
N1A C3A C2A 117.5(2) . . ?
C4A C3A C2A 129.3(2) . . ?
C28A C27A C32A 119.2(3) . . ?
C28A C27A C14A 117.1(2) . . ?
C32A C27A C14A 123.7(2) . . ?
C15A C20A C19A 111.7(2) . . ?
C15A C20A H20A 109.3 . . ?
C19A C20A H20A 109.3 . . ?
C15A C20A H20B 109.3 . . ?
C19A C20A H20B 109.3 . . ?
H20A C20A H20B 107.9 . . ?
C23A C22A C21A 120.1(2) . . ?
C23A C22A H22A 119.9 . . ?
C21A C22A H22A 119.9 . . ?
C27A C32A C31A 119.7(3) . . ?
C27A C32A H32A 120.2 . . ?
C31A C32A H32A 120.2 . . ?
O3A C5A C4A 119.9(2) . . ?
O3A C5A C6A 120.8(2) . . ?
C4A C5A C6A 119.3(2) . . ?
C24A C23A C22A 120.8(3) . . ?
C24A C23A H23A 119.6 . . ?
C22A C23A H23A 119.6 . . ?
C8A C7A C6A 121.1(3) . . ?
C8A C7A H7A 119.5 . . ?
C6A C7A H7A 119.5 . . ?
O2A C2A O1A 124.6(3) . . ?
O2A C2A C3A 124.0(3) . . ?
O1A C2A C3A 111.4(2) . . ?
C21A C26A C25A 120.6(2) . . ?
C21A C26A H26A 119.7 . . ?
C25A C26A H26A 119.7 . . ?
C10A C11A C6A 120.4(3) . . ?
C10A C11A H11A 119.8 . . ?
C6A C11A H11A 119.8 . . ?
C8A C9A C10A 118.3(3) . . ?
C8A C9A C12A 120.7(3) . . ?
C10A C9A C12A 120.9(3) . . ?
C18A C19A C20A 111.1(2) . . ?
C18A C19A H19A 109.4 . . ?
C20A C19A H19A 109.4 . . ?
C18A C19A H19B 109.4 . . ?
C20A C19A H19B 109.4 . . ?
H19A C19A H19B 108.0 . . ?
C27A C28A C29A 120.7(3) . . ?
C27A C28A H28A 119.6 . . ?
C29A C28A H28A 119.6 . . ?
C15A C16A C17A 111.0(2) . . ?
C15A C16A H16A 109.4 . . ?
C17A C16A H16A 109.4 . . ?
C15A C16A H16B 109.4 . . ?
C17A C16A H16B 109.4 . . ?
H16A C16A H16B 108.0 . . ?
C23A C24A C25A 119.6(3) . . ?
C23A C24A H24A 120.2 . . ?
C25A C24A H24A 120.2 . . ?
C24A C25A C26A 120.2(3) . . ?
C24A C25A H25A 119.9 . . ?
C26A C25A H25A 119.9 . . ?
C17A C18A C19A 110.7(3) . . ?
C17A C18A H18A 109.5 . . ?
C19A C18A H18A 109.5 . . ?
C17A C18A H18B 109.5 . . ?
C19A C18A H18B 109.5 . . ?
H18A C18A H18B 108.1 . . ?
O1A C1A H1A1 109.5 . . ?
O1A C1A H1A2 109.5 . . ?
H1A1 C1A H1A2 109.5 . . ?
O1A C1A H1A3 109.5 . . ?
H1A1 C1A H1A3 109.5 . . ?
H1A2 C1A H1A3 109.5 . . ?
C7A C8A C9A 120.6(3) . . ?
C7A C8A H8A 119.7 . . ?
C9A C8A H8A 119.7 . . ?
C31A C30A C29A 119.9(3) . . ?
C31A C30A H30A 120.0 . . ?
C29A C30A H30A 120.0 . . ?
C30A C29A C28A 119.8(3) . . ?
C30A C29A H29A 120.1 . . ?
C28A C29A H29A 120.1 . . ?
C18A C17A C16A 112.2(3) . . ?
C18A C17A H17A 109.2 . . ?
C16A C17A H17A 109.2 . . ?
C18A C17A H17B 109.2 . . ?
C16A C17A H17B 109.2 . . ?
H17A C17A H17B 107.9 . . ?
C11A C10A C9A 121.4(3) . . ?
C11A C10A H10A 119.3 . . ?
C9A C10A H10A 119.3 . . ?
C30A C31A C32A 120.7(3) . . ?
C30A C31A H31A 119.7 . . ?
C32A C31A H31A 119.7 . . ?
C9A C12A H12A 109.5 . . ?
C9A C12A H12B 109.5 . . ?
H12A C12A H12B 109.5 . . ?
C9A C12A H12C 109.5 . . ?
H12A C12A H12C 109.5 . . ?
H12B C12A H12C 109.5 . . ?
C13 O5 C15 115.99(17) . . ?
C15 O4 C14 120.04(17) . . ?
C13 N2 N1 111.60(19) . . ?
C13 N2 C14 125.59(19) . . ?
N1 N2 C14 122.75(18) . . ?
C3 N1 N2 103.96(18) . . ?
O4 C14 N2 105.00(17) . . ?
O4 C14 C27 106.41(18) . . ?
N2 C14 C27 109.82(18) . . ?
O4 C14 C21 111.75(18) . . ?
N2 C14 C21 112.17(18) . . ?
C27 C14 C21 111.36(18) . . ?
C13 C4 C3 102.8(2) . . ?
C13 C4 C5 132.3(2) . . ?
C3 C4 C5 124.5(2) . . ?
O4 C15 O5 108.35(17) . . ?
O4 C15 C16 105.8(2) . . ?
O5 C15 C16 105.9(2) . . ?
O4 C15 C20 115.7(2) . . ?
O5 C15 C20 108.7(2) . . ?
C16 C15 C20 111.9(2) . . ?
O5 C13 N2 121.4(2) . . ?
O5 C13 C4 130.2(2) . . ?
N2 C13 C4 108.24(19) . . ?
C28 C27 C32 118.2(2) . . ?
C28 C27 C14 120.8(2) . . ?
C32 C27 C14 121.0(2) . . ?
C22 C21 C26 119.2(2) . . ?
C22 C21 C14 117.7(2) . . ?
C26 C21 C14 123.0(2) . . ?
N1 C3 C4 113.4(2) . . ?
N1 C3 C2 119.8(2) . . ?
C4 C3 C2 126.3(2) . . ?
C2 O1 C1 113.0(3) . . ?
C25 C26 C21 120.1(3) . . ?
C25 C26 H26 119.9 . . ?
C21 C26 H26 119.9 . . ?
O3 C5 C6 121.3(2) . . ?
O3 C5 C4 117.4(2) . . ?
C6 C5 C4 121.3(2) . . ?
C7 C6 C11 118.3(3) . . ?
C7 C6 C5 122.5(2) . . ?
C11 C6 C5 119.1(2) . . ?
C15 C16 C17 112.4(2) . . ?
C15 C16 H16C 109.1 . . ?
C17 C16 H16C 109.1 . . ?
C15 C16 H16D 109.1 . . ?
C17 C16 H16D 109.1 . . ?
H16C C16 H16D 107.9 . . ?
C23 C24 C25 119.9(3) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C27 C32 C31 121.0(3) . . ?
C27 C32 H32 119.5 . . ?
C31 C32 H32 119.5 . . ?
C26 C25 C24 120.4(3) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C30 C31 C32 119.6(3) . . ?
C30 C31 H31 120.2 . . ?
C32 C31 H31 120.2 . . ?
C19 C20 C15 112.8(2) . . ?
C19 C20 H20C 109.0 . . ?
C15 C20 H20C 109.0 . . ?
C19 C20 H20D 109.0 . . ?
C15 C20 H20D 109.0 . . ?
H20C C20 H20D 107.8 . . ?
C8 C7 C6 121.0(3) . . ?
C8 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C23 C22 C21 119.8(2) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C29 C28 C27 120.8(3) . . ?
C29 C28 H28 119.6 . . ?
C27 C28 H28 119.6 . . ?
C2 O2 C1B 101.4(8) . . ?
O2 C2 O1 123.9(3) . . ?
O2 C2 C3 122.3(3) . . ?
O1 C2 C3 113.7(3) . . ?
C10 C11 C6 119.9(3) . . ?
C10 C11 H11 120.1 . . ?
C6 C11 H11 120.1 . . ?
C24 C23 C22 120.5(3) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C7 C8 C9 120.9(3) . . ?
C7 C8 H8 119.5 . . ?
C9 C8 H8 119.5 . . ?
C31 C30 C29 120.0(3) . . ?
C31 C30 H30 120.0 . . ?
C29 C30 H30 120.0 . . ?
C30 C29 C28 120.4(3) . . ?
C30 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
C18 C19 C20 112.6(3) . . ?
C18 C19 H19C 109.1 . . ?
C20 C19 H19C 109.1 . . ?
C18 C19 H19D 109.1 . . ?
C20 C19 H19D 109.1 . . ?
H19C C19 H19D 107.8 . . ?
C18 C17 C16 111.4(3) . . ?
C18 C17 H17C 109.4 . . ?
C16 C17 H17C 109.4 . . ?
C18 C17 H17D 109.4 . . ?
C16 C17 H17D 109.4 . . ?
H17C C17 H17D 108.0 . . ?
C19 C18 C17 110.6(2) . . ?
C19 C18 H18C 109.5 . . ?
C17 C18 H18C 109.5 . . ?
C19 C18 H18D 109.5 . . ?
C17 C18 H18D 109.5 . . ?
H18C C18 H18D 108.1 . . ?
C11 C10 C9 122.2(3) . . ?
C11 C10 H10 118.9 . . ?
C9 C10 H10 118.9 . . ?
C10 C9 C8 117.8(3) . . ?
C10 C9 C12 121.7(3) . . ?
C8 C9 C12 120.5(3) . . ?
C9 C12 H12D 109.5 . . ?
C9 C12 H12E 109.5 . . ?
H12D C12 H12E 109.5 . . ?
C9 C12 H12F 109.5 . . ?
H12D C12 H12F 109.5 . . ?
H12E C12 H12F 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
C3A N1A N2A C13A -1.3(3) . . . . ?
C3A N1A N2A C14A -179.4(2) . . . . ?
C15A O4A C13A N2A -19.6(3) . . . . ?
C15A O4A C13A C4A 159.9(2) . . . . ?
N1A N2A C13A O4A -179.11(19) . . . . ?
C14A N2A C13A O4A -1.0(3) . . . . ?
N1A N2A C13A C4A 1.3(3) . . . . ?
C14A N2A C13A C4A 179.4(2) . . . . ?
O4A C13A C4A C3A 179.8(2) . . . . ?
N2A C13A C4A C3A -0.7(2) . . . . ?
O4A C13A C4A C5A -1.6(4) . . . . ?
N2A C13A C4A C5A 177.9(2) . . . . ?
C15A O5A C14A N2A 39.9(3) . . . . ?
C15A O5A C14A C27A -81.9(2) . . . . ?
C15A O5A C14A C21A 156.1(2) . . . . ?
C13A N2A C14A O5A -7.4(3) . . . . ?
N1A N2A C14A O5A 170.45(18) . . . . ?
C13A N2A C14A C27A 113.9(2) . . . . ?
N1A N2A C14A C27A -68.2(3) . . . . ?
C13A N2A C14A C21A -121.8(2) . . . . ?
N1A N2A C14A C21A 56.1(3) . . . . ?
C14A O5A C15A O4A -61.4(2) . . . . ?
C14A O5A C15A C20A -174.8(2) . . . . ?
C14A O5A C15A C16A 60.0(3) . . . . ?
C13A O4A C15A O5A 46.7(2) . . . . ?
C13A O4A C15A C20A 160.44(19) . . . . ?
C13A O4A C15A C16A -78.7(2) . . . . ?
O5A C14A C21A C26A 160.0(2) . . . . ?
N2A C14A C21A C26A -86.6(3) . . . . ?
C27A C14A C21A C26A 38.0(3) . . . . ?
O5A C14A C21A C22A -21.8(3) . . . . ?
N2A C14A C21A C22A 91.6(3) . . . . ?
C27A C14A C21A C22A -143.7(2) . . . . ?
N2A N1A C3A C4A 0.8(3) . . . . ?
N2A N1A C3A C2A -179.4(2) . . . . ?
C13A C4A C3A N1A -0.1(3) . . . . ?
C5A C4A C3A N1A -178.6(2) . . . . ?
C13A C4A C3A C2A -179.9(2) . . . . ?
C5A C4A C3A C2A 1.6(4) . . . . ?
O5A C14A C27A C28A -44.9(3) . . . . ?
N2A C14A C27A C28A -162.6(2) . . . . ?
C21A C14A C27A C28A 74.3(3) . . . . ?
O5A C14A C27A C32A 136.6(2) . . . . ?
N2A C14A C27A C32A 18.9(3) . . . . ?
C21A C14A C27A C32A -104.3(3) . . . . ?
O5A C15A C20A C19A 179.3(2) . . . . ?
O4A C15A C20A C19A 64.4(3) . . . . ?
C16A C15A C20A C19A -53.9(3) . . . . ?
C26A C21A C22A C23A -1.6(4) . . . . ?
C14A C21A C22A C23A -179.9(2) . . . . ?
C28A C27A C32A C31A 1.4(4) . . . . ?
C14A C27A C32A C31A 180.0(2) . . . . ?
C13A C4A C5A O3A 30.9(4) . . . . ?
C3A C4A C5A O3A -151.0(3) . . . . ?
C13A C4A C5A C6A -147.8(2) . . . . ?
C3A C4A C5A C6A 30.4(4) . . . . ?
C7A C6A C5A O3A -147.5(3) . . . . ?
C11A C6A C5A O3A 32.7(4) . . . . ?
C7A C6A C5A C4A 31.2(4) . . . . ?
C11A C6A C5A C4A -148.6(3) . . . . ?
C21A C22A C23A C24A 1.9(4) . . . . ?
C11A C6A C7A C8A 1.3(4) . . . . ?
C5A C6A C7A C8A -178.5(3) . . . . ?
C1A O1A C2A O2A 7.8(4) . . . . ?
C1A O1A C2A C3A -170.2(2) . . . . ?
N1A C3A C2A O2A 44.1(4) . . . . ?
C4A C3A C2A O2A -136.1(3) . . . . ?
N1A C3A C2A O1A -137.9(2) . . . . ?
C4A C3A C2A O1A 41.9(4) . . . . ?
C22A C21A C26A C25A 0.1(4) . . . . ?
C14A C21A C26A C25A 178.4(3) . . . . ?
C7A C6A C11A C10A -1.7(4) . . . . ?
C5A C6A C11A C10A 178.1(3) . . . . ?
C15A C20A C19A C18A 55.3(3) . . . . ?
C32A C27A C28A C29A -1.9(4) . . . . ?
C14A C27A C28A C29A 179.5(3) . . . . ?
O5A C15A C16A C17A 174.6(2) . . . . ?
O4A C15A C16A C17A -64.2(3) . . . . ?
C20A C15A C16A C17A 52.6(3) . . . . ?
C22A C23A C24A C25A -0.7(5) . . . . ?
C23A C24A C25A C26A -0.9(5) . . . . ?
C21A C26A C25A C24A 1.2(5) . . . . ?
C20A C19A C18A C17A -56.1(4) . . . . ?
C6A C7A C8A C9A 0.9(4) . . . . ?
C10A C9A C8A C7A -2.6(5) . . . . ?
C12A C9A C8A C7A 178.7(3) . . . . ?
C31A C30A C29A C28A 0.1(5) . . . . ?
C27A C28A C29A C30A 1.1(5) . . . . ?
C19A C18A C17A C16A 55.8(4) . . . . ?
C15A C16A C17A C18A -53.9(4) . . . . ?
C6A C11A C10A C9A 0.0(5) . . . . ?
C8A C9A C10A C11A 2.1(5) . . . . ?
C12A C9A C10A C11A -179.1(3) . . . . ?
C29A C30A C31A C32A -0.6(5) . . . . ?
C27A C32A C31A C30A -0.2(4) . . . . ?
C13 N2 N1 C3 0.6(2) . . . . ?
C14 N2 N1 C3 -176.6(2) . . . . ?
C15 O4 C14 N2 43.9(2) . . . . ?
C15 O4 C14 C27 160.30(19) . . . . ?
C15 O4 C14 C21 -77.9(2) . . . . ?
C13 N2 C14 O4 -13.6(3) . . . . ?
N1 N2 C14 O4 163.26(18) . . . . ?
C13 N2 C14 C27 -127.6(2) . . . . ?
N1 N2 C14 C27 49.2(3) . . . . ?
C13 N2 C14 C21 108.0(2) . . . . ?
N1 N2 C14 C21 -75.2(3) . . . . ?
C14 O4 C15 O5 -58.9(2) . . . . ?
C14 O4 C15 C16 -172.2(2) . . . . ?
C14 O4 C15 C20 63.4(3) . . . . ?
C13 O5 C15 O4 40.3(3) . . . . ?
C13 O5 C15 C16 153.4(2) . . . . ?
C13 O5 C15 C20 -86.2(2) . . . . ?
C15 O5 C13 N2 -15.3(3) . . . . ?
C15 O5 C13 C4 170.5(2) . . . . ?
N1 N2 C13 O5 -175.74(19) . . . . ?
C14 N2 C13 O5 1.4(3) . . . . ?
N1 N2 C13 C4 -0.4(3) . . . . ?
C14 N2 C13 C4 176.7(2) . . . . ?
C3 C4 C13 O5 174.9(2) . . . . ?
C5 C4 C13 O5 1.7(4) . . . . ?
C3 C4 C13 N2 0.1(2) . . . . ?
C5 C4 C13 N2 -173.0(2) . . . . ?
O4 C14 C27 C28 156.0(2) . . . . ?
N2 C14 C27 C28 -90.9(3) . . . . ?
C21 C14 C27 C28 34.0(3) . . . . ?
O4 C14 C27 C32 -26.0(3) . . . . ?
N2 C14 C27 C32 87.1(3) . . . . ?
C21 C14 C27 C32 -148.0(2) . . . . ?
O4 C14 C21 C22 -46.6(3) . . . . ?
N2 C14 C21 C22 -164.16(19) . . . . ?
C27 C14 C21 C22 72.3(3) . . . . ?
O4 C14 C21 C26 135.1(2) . . . . ?
N2 C14 C21 C26 17.5(3) . . . . ?
C27 C14 C21 C26 -106.0(2) . . . . ?
N2 N1 C3 C4 -0.5(3) . . . . ?
N2 N1 C3 C2 -172.3(2) . . . . ?
C13 C4 C3 N1 0.2(3) . . . . ?
C5 C4 C3 N1 174.1(2) . . . . ?
C13 C4 C3 C2 171.4(2) . . . . ?
C5 C4 C3 C2 -14.8(4) . . . . ?
C22 C21 C26 C25 1.5(3) . . . . ?
C14 C21 C26 C25 179.8(2) . . . . ?
C13 C4 C5 O3 137.2(3) . . . . ?
C3 C4 C5 O3 -34.7(4) . . . . ?
C13 C4 C5 C6 -43.3(4) . . . . ?
C3 C4 C5 C6 144.8(2) . . . . ?
O3 C5 C6 C7 167.3(3) . . . . ?
C4 C5 C6 C7 -12.2(4) . . . . ?
O3 C5 C6 C11 -9.1(4) . . . . ?
C4 C5 C6 C11 171.4(2) . . . . ?
O4 C15 C16 C17 -179.0(2) . . . . ?
O5 C15 C16 C17 66.1(3) . . . . ?
C20 C15 C16 C17 -52.2(3) . . . . ?
C28 C27 C32 C31 -2.2(4) . . . . ?
C14 C27 C32 C31 179.7(2) . . . . ?
C21 C26 C25 C24 -0.4(4) . . . . ?
C23 C24 C25 C26 -0.5(4) . . . . ?
C27 C32 C31 C30 1.7(4) . . . . ?
O4 C15 C20 C19 171.1(2) . . . . ?
O5 C15 C20 C19 -66.7(3) . . . . ?
C16 C15 C20 C19 49.9(3) . . . . ?
C11 C6 C7 C8 -1.5(4) . . . . ?
C5 C6 C7 C8 -178.0(3) . . . . ?
C26 C21 C22 C23 -1.8(4) . . . . ?
C14 C21 C22 C23 179.8(2) . . . . ?
C32 C27 C28 C29 1.0(4) . . . . ?
C14 C27 C28 C29 179.1(3) . . . . ?
C1B O2 C2 O1 3.4(10) . . . . ?
C1B O2 C2 C3 -174.8(9) . . . . ?
C1 O1 C2 O2 -3.8(5) . . . . ?
C1 O1 C2 C3 174.5(3) . . . . ?
N1 C3 C2 O2 132.2(3) . . . . ?
C4 C3 C2 O2 -38.4(4) . . . . ?
N1 C3 C2 O1 -46.2(3) . . . . ?
C4 C3 C2 O1 143.2(3) . . . . ?
C7 C6 C11 C10 0.8(5) . . . . ?
C5 C6 C11 C10 177.4(3) . . . . ?
C25 C24 C23 C22 0.2(4) . . . . ?
C21 C22 C23 C24 0.9(4) . . . . ?
C6 C7 C8 C9 0.9(5) . . . . ?
C32 C31 C30 C29 0.2(5) . . . . ?
C31 C30 C29 C28 -1.3(5) . . . . ?
C27 C28 C29 C30 0.7(5) . . . . ?
C15 C20 C19 C18 -51.5(3) . . . . ?
C15 C16 C17 C18 55.8(3) . . . . ?
C20 C19 C18 C17 54.2(4) . . . . ?
C16 C17 C18 C19 -56.0(4) . . . . ?
C6 C11 C10 C9 0.6(6) . . . . ?
C11 C10 C9 C8 -1.2(6) . . . . ?
C11 C10 C9 C12 179.7(4) . . . . ?
C7 C8 C9 C10 0.4(5) . . . . ?
C7 C8 C9 C12 179.5(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.840
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.056
_chemical_compound_source        none
_chemical_properties_physical    Moisture-sensitive,Heat-sensitive
