#------------------------------------------------------------------------------
#$Date: 2020-06-05 14:29:34 +0300 (Fri, 05 Jun 2020) $
#$Revision: 252916 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/15/74/7157494.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7157494
loop_
_publ_author_name
'Ravindran, Jaice'
'Yadhukrishnan, Velickakathu O.'
'Asha, Reghuvaran S.'
'Lankalapalli, Ravi S.'
_publ_section_title
;
 Dienaminodioate based multicomponent reactions with post-benzylic
 oxidative transformations mediated by DDQ.
;
_journal_issue                   20
_journal_name_full               'Organic & biomolecular chemistry'
_journal_page_first              3927
_journal_page_last               3937
_journal_paper_doi               10.1039/d0ob00721h
_journal_volume                  18
_journal_year                    2020
_chemical_formula_moiety         'C33 H30 Cl N3 O9'
_chemical_formula_sum            'C33 H30 Cl N3 O9'
_chemical_formula_weight         648.05
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-12-12 deposited with the CCDC.	2020-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                102.592(3)
_cell_angle_beta                 95.138(4)
_cell_angle_gamma                101.978(3)
_cell_formula_units_Z            2
_cell_length_a                   9.3935(6)
_cell_length_b                   10.3136(7)
_cell_length_c                   17.8351(12)
_cell_measurement_reflns_used    9858
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.07
_cell_measurement_theta_min      3.01
_cell_volume                     1633.08(19)
_computing_cell_refinement       'APEX3/SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3(Bruker, 2016)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2016)'
_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker axs kappa apex3 CMOS Diffractometer'
_diffrn_measurement_method       'ω and φ scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            46502
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.018
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7151
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       block
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.032(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         5738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0729P)²+0.4651P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1504
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4161
_reflns_number_total             5738
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ob00721h2.cif
_cod_data_source_block           JR637
_cod_depositor_comments
'Adding full bibliography for 7157493--7157494.cif.'
_cod_database_code               7157494
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.974
_shelx_estimated_absorpt_t_max   0.983
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2386(5) 0.1573(7) 0.3578(2) 0.174(3) Uani 1 1 d . . . . .
H1A H 0.1813 0.1288 0.3072 0.260 Uiso 1 1 calc R U . . .
H1B H 0.3239 0.2272 0.3578 0.260 Uiso 1 1 calc R U . . .
H1C H 0.2687 0.0806 0.3708 0.260 Uiso 1 1 calc R U . . .
C2 C 0.0129(5) 0.1091(5) 0.4189(2) 0.155(2) Uani 1 1 d . . . . .
H2A H -0.0473 0.0819 0.3691 0.233 Uiso 1 1 calc R U . . .
H2B H 0.0401 0.0309 0.4315 0.233 Uiso 1 1 calc R U . . .
H2C H -0.0411 0.1480 0.4576 0.233 Uiso 1 1 calc R U . . .
C3 C 0.0999(6) 0.3339(5) 0.3973(2) 0.1486(19) Uani 1 1 d . . . . .
H3A H 0.0396 0.3059 0.3476 0.223 Uiso 1 1 calc R U . . .
H3B H 0.0446 0.3700 0.4362 0.223 Uiso 1 1 calc R U . . .
H3C H 0.1849 0.4030 0.3960 0.223 Uiso 1 1 calc R U . . .
C4 C 0.1478(3) 0.2126(3) 0.41644(14) 0.0740(8) Uani 1 1 d . . . . .
C5 C 0.2085(3) 0.3156(2) 0.56017(13) 0.0518(5) Uani 1 1 d . . . . .
C6 C 0.3358(2) 0.3525(2) 0.62806(12) 0.0460(5) Uani 1 1 d . . . . .
H6 H 0.4211 0.4103 0.6142 0.055 Uiso 1 1 calc R U . . .
C7 C 0.3812(2) 0.2293(2) 0.64680(13) 0.0482(5) Uani 1 1 d . . . . .
C8 C 0.3136(2) 0.1720(2) 0.69822(13) 0.0509(5) Uani 1 1 d . . . . .
H8 H 0.3351 0.0922 0.7073 0.061 Uiso 1 1 calc R U . . .
C9 C 0.2087(2) 0.2295(2) 0.74006(13) 0.0484(5) Uani 1 1 d . . . . .
C10 C 0.2103(2) 0.3644(2) 0.74349(12) 0.0434(5) Uani 1 1 d . . . . .
C11 C 0.1124(3) 0.1505(2) 0.78317(14) 0.0575(6) Uani 1 1 d . . . . .
C12 C 0.0830(4) -0.0365(3) 0.84164(19) 0.0952(10) Uani 1 1 d . . . . .
H12A H 0.1304 -0.1081 0.8482 0.143 Uiso 1 1 calc R U . . .
H12B H 0.0788 0.0196 0.8916 0.143 Uiso 1 1 calc R U . . .
H12C H -0.0149 -0.0758 0.8148 0.143 Uiso 1 1 calc R U . . .
C13 C 0.5025(3) 0.1782(3) 0.61392(15) 0.0622(6) Uani 1 1 d . . . . .
C14 C 0.6935(4) 0.2173(4) 0.5375(2) 0.1177(13) Uani 1 1 d . . . . .
H14A H 0.7281 0.2749 0.5042 0.177 Uiso 1 1 calc R U . . .
H14B H 0.7687 0.2307 0.5805 0.177 Uiso 1 1 calc R U . . .
H14C H 0.6702 0.1234 0.5089 0.177 Uiso 1 1 calc R U . . .
C15 C 0.1323(2) 0.4489(2) 0.79577(12) 0.0438(5) Uani 1 1 d . . . . .
C16 C 0.1556(2) 0.4693(2) 0.87542(13) 0.0544(6) Uani 1 1 d . . . . .
H16 H 0.2199 0.4263 0.8977 0.065 Uiso 1 1 calc R U . . .
C17 C 0.0852(3) 0.5523(3) 0.92234(14) 0.0603(6) Uani 1 1 d . . . . .
H17 H 0.1022 0.5660 0.9760 0.072 Uiso 1 1 calc R U . . .
C18 C -0.0106(3) 0.6148(2) 0.88898(15) 0.0585(6) Uani 1 1 d . . . . .
C19 C -0.0373(3) 0.5951(2) 0.80976(14) 0.0551(6) Uani 1 1 d . . . . .
H19 H -0.1036 0.6366 0.7878 0.066 Uiso 1 1 calc R U . . .
C20 C 0.0351(2) 0.5134(2) 0.76338(13) 0.0491(5) Uani 1 1 d . . . . .
H20 H 0.0189 0.5011 0.7098 0.059 Uiso 1 1 calc R U . . .
C21 C 0.3520(2) 0.5751(2) 0.71956(12) 0.0458(5) Uani 1 1 d . . . . .
C22 C 0.4545(2) 0.6326(2) 0.78452(13) 0.0517(5) Uani 1 1 d . . . . .
C23 C 0.5166(3) 0.7712(3) 0.80556(16) 0.0705(7) Uani 1 1 d . . . . .
H23 H 0.5853 0.8094 0.8499 0.085 Uiso 1 1 calc R U . . .
C24 C 0.4746(4) 0.8520(3) 0.75928(19) 0.0796(8) Uani 1 1 d . . . . .
H24 H 0.5148 0.9457 0.7729 0.096 Uiso 1 1 calc R U . . .
C25 C 0.3752(3) 0.7961(3) 0.69397(17) 0.0727(8) Uani 1 1 d . . . . .
H25 H 0.3491 0.8514 0.6629 0.087 Uiso 1 1 calc R U . . .
C26 C 0.3128(3) 0.6576(2) 0.67363(14) 0.0590(6) Uani 1 1 d . . . . .
H26 H 0.2445 0.6198 0.6291 0.071 Uiso 1 1 calc R U . . .
C27 C 0.5825(2) 0.4671(2) 0.80386(14) 0.0556(6) Uani 1 1 d . . . . .
C28 C 0.6049(2) 0.3723(2) 0.85345(13) 0.0537(6) Uani 1 1 d . . . . .
C29 C 0.5323(3) 0.3639(3) 0.91678(15) 0.0688(7) Uani 1 1 d . . . . .
H29 H 0.4681 0.4200 0.9299 0.083 Uiso 1 1 calc R U . . .
C30 C 0.5539(3) 0.2732(3) 0.96098(15) 0.0730(7) Uani 1 1 d . . . . .
H30 H 0.5053 0.2675 1.0038 0.088 Uiso 1 1 calc R U . . .
C31 C 0.6490(3) 0.1919(3) 0.93987(14) 0.0586(6) Uani 1 1 d . . . . .
C32 C 0.7233(3) 0.1988(3) 0.87825(15) 0.0642(7) Uani 1 1 d . . . . .
H32 H 0.7879 0.1428 0.8657 0.077 Uiso 1 1 calc R U . . .
C33 C 0.7013(3) 0.2905(3) 0.83429(15) 0.0626(6) Uani 1 1 d . . . . .
H33 H 0.7514 0.2966 0.7921 0.075 Uiso 1 1 calc R U . . .
N1 N 0.2401(3) 0.2546(3) 0.49252(12) 0.0719(7) Uani 1 1 d . . . . .
N2 N 0.29305(18) 0.43044(16) 0.69775(10) 0.0442(4) Uani 1 1 d . . . . .
N3 N 0.6757(3) 0.0964(2) 0.98770(14) 0.0728(6) Uani 1 1 d . . . . .
O1 O 0.0912(2) 0.3427(2) 0.56978(11) 0.0896(7) Uani 1 1 d . . . . .
O2 O 0.5444(2) 0.0819(2) 0.62678(14) 0.1009(8) Uani 1 1 d . . . . .
O3 O 0.5624(2) 0.25179(19) 0.56630(11) 0.0747(5) Uani 1 1 d . . . . .
O4 O -0.0001(2) 0.1713(2) 0.80309(14) 0.0919(7) Uani 1 1 d . . . . .
O5 O 0.1657(2) 0.04620(18) 0.79695(11) 0.0758(5) Uani 1 1 d . . . . .
O6 O 0.49399(17) 0.54985(16) 0.83245(9) 0.0590(4) Uani 1 1 d . . . . .
O7 O 0.63425(19) 0.47127(19) 0.74493(10) 0.0692(5) Uani 1 1 d . . . . .
O8 O 0.6302(3) 0.1090(3) 1.05037(14) 0.1092(8) Uani 1 1 d . . . . .
O9 O 0.7409(3) 0.0099(2) 0.96213(13) 0.0931(6) Uani 1 1 d . . . . .
Cl1 Cl -0.10151(10) 0.71899(8) 0.94750(5) 0.0976(3) Uani 1 1 d . . . . .
H1 H 0.321(3) 0.244(3) 0.4936(16) 0.071(9) Uiso 1 1 d . . . . .
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C4 C1 H1A 109.5 . . ?
C4 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C4 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C4 C2 H2A 109.5 . . ?
C4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C4 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 C2 109.6(3) . . ?
N1 C4 C1 107.3(2) . . ?
C2 C4 C1 112.1(4) . . ?
N1 C4 C3 109.9(3) . . ?
C2 C4 C3 107.6(4) . . ?
C1 C4 C3 110.4(3) . . ?
O1 C5 N1 124.1(2) . . ?
O1 C5 C6 121.3(2) . . ?
N1 C5 C6 114.51(19) . . ?
N2 C6 C7 108.53(16) . . ?
N2 C6 C5 109.57(16) . . ?
C7 C6 C5 113.60(17) . . ?
N2 C6 H6 108.3 . . ?
C7 C6 H6 108.3 . . ?
C5 C6 H6 108.3 . . ?
C8 C7 C13 120.0(2) . . ?
C8 C7 C6 118.15(19) . . ?
C13 C7 C6 121.8(2) . . ?
C7 C8 C9 122.13(19) . . ?
C7 C8 H8 118.9 . . ?
C9 C8 H8 118.9 . . ?
C10 C9 C8 117.39(19) . . ?
C10 C9 C11 121.4(2) . . ?
C8 C9 C11 121.02(19) . . ?
N2 C10 C9 119.18(19) . . ?
N2 C10 C15 115.60(16) . . ?
C9 C10 C15 125.18(18) . . ?
O4 C11 O5 122.4(2) . . ?
O4 C11 C9 126.6(2) . . ?
O5 C11 C9 111.0(2) . . ?
O5 C12 H12A 109.5 . . ?
O5 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O5 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O2 C13 O3 123.0(2) . . ?
O2 C13 C7 125.1(2) . . ?
O3 C13 C7 112.0(2) . . ?
O3 C14 H14A 109.5 . . ?
O3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C20 118.8(2) . . ?
C16 C15 C10 122.56(18) . . ?
C20 C15 C10 118.65(18) . . ?
C17 C16 C15 121.0(2) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C18 C17 C16 119.2(2) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
C19 C18 C17 121.1(2) . . ?
C19 C18 Cl1 119.2(2) . . ?
C17 C18 Cl1 119.7(2) . . ?
C18 C19 C20 119.3(2) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 H19 120.3 . . ?
C19 C20 C15 120.7(2) . . ?
C19 C20 H20 119.7 . . ?
C15 C20 H20 119.7 . . ?
C22 C21 C26 119.1(2) . . ?
C22 C21 N2 120.05(18) . . ?
C26 C21 N2 120.7(2) . . ?
C21 C22 C23 121.3(2) . . ?
C21 C22 O6 119.69(19) . . ?
C23 C22 O6 119.0(2) . . ?
C22 C23 C24 118.6(3) . . ?
C22 C23 H23 120.7 . . ?
C24 C23 H23 120.7 . . ?
C25 C24 C23 120.7(2) . . ?
C25 C24 H24 119.6 . . ?
C23 C24 H24 119.6 . . ?
C24 C25 C26 120.3(2) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C21 119.9(2) . . ?
C25 C26 H26 120.0 . . ?
C21 C26 H26 120.0 . . ?
O7 C27 O6 122.9(2) . . ?
O7 C27 C28 124.9(2) . . ?
O6 C27 C28 112.1(2) . . ?
C33 C28 C29 119.8(2) . . ?
C33 C28 C27 117.9(2) . . ?
C29 C28 C27 122.3(2) . . ?
C28 C29 C30 120.8(2) . . ?
C28 C29 H29 119.6 . . ?
C30 C29 H29 119.6 . . ?
C31 C30 C29 118.0(2) . . ?
C31 C30 H30 121.0 . . ?
C29 C30 H30 121.0 . . ?
C32 C31 C30 122.6(2) . . ?
C32 C31 N3 118.8(2) . . ?
C30 C31 N3 118.6(2) . . ?
C31 C32 C33 119.1(2) . . ?
C31 C32 H32 120.5 . . ?
C33 C32 H32 120.5 . . ?
C28 C33 C32 119.7(2) . . ?
C28 C33 H33 120.1 . . ?
C32 C33 H33 120.1 . . ?
C5 N1 C4 128.4(2) . . ?
C5 N1 H1 115(2) . . ?
C4 N1 H1 117(2) . . ?
C10 N2 C21 121.77(17) . . ?
C10 N2 C6 120.32(16) . . ?
C21 N2 C6 117.66(16) . . ?
O9 N3 O8 124.0(2) . . ?
O9 N3 C31 118.1(2) . . ?
O8 N3 C31 117.9(2) . . ?
C13 O3 C14 115.6(2) . . ?
C11 O5 C12 116.2(2) . . ?
C27 O6 C22 115.62(17) . . ?
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 C4 1.500(4) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C4 1.488(5) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.509(5) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 N1 1.469(3) . ?
C5 O1 1.210(3) . ?
C5 N1 1.323(3) . ?
C5 C6 1.547(3) . ?
C6 N2 1.463(3) . ?
C6 C7 1.514(3) . ?
C6 H6 0.9800 . ?
C7 C8 1.333(3) . ?
C7 C13 1.467(3) . ?
C8 C9 1.436(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.376(3) . ?
C9 C11 1.471(3) . ?
C10 N2 1.367(3) . ?
C10 C15 1.483(3) . ?
C11 O4 1.190(3) . ?
C11 O5 1.337(3) . ?
C12 O5 1.449(3) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 O2 1.200(3) . ?
C13 O3 1.343(3) . ?
C14 O3 1.457(3) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.380(3) . ?
C15 C20 1.391(3) . ?
C16 C17 1.376(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.375(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.375(3) . ?
C18 Cl1 1.739(2) . ?
C19 C20 1.375(3) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C22 1.373(3) . ?
C21 C26 1.382(3) . ?
C21 N2 1.432(3) . ?
C22 C23 1.380(3) . ?
C22 O6 1.411(3) . ?
C23 C24 1.382(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.361(4) . ?
C24 H24 0.9300 . ?
C25 C26 1.379(4) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 O7 1.202(3) . ?
C27 O6 1.364(3) . ?
C27 C28 1.487(3) . ?
C28 C33 1.377(3) . ?
C28 C29 1.380(3) . ?
C29 C30 1.382(4) . ?
C29 H29 0.9300 . ?
C30 C31 1.369(4) . ?
C30 H30 0.9300 . ?
C31 C32 1.360(3) . ?
C31 N3 1.481(3) . ?
C32 C33 1.388(4) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
N1 H1 0.79(3) . ?
N3 O9 1.215(3) . ?
N3 O8 1.222(3) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C2 H2C O1 0.96 2.52 3.110(5) 119.8 .
C3 H3B O1 0.96 2.47 3.067(4) 120.1 .
C19 H19 O7 0.93 2.63 3.093(3) 111.6 1_455
C23 H23 O9 0.93 2.61 3.478(4) 154.6 1_565
C32 H32 O4 0.93 2.37 3.065(3) 131.7 1_655
N1 H1 O3 0.79(3) 2.49(3) 3.199(3) 151(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
O1 C5 C6 N2 -4.7(3) . . . . ?
N1 C5 C6 N2 174.7(2) . . . . ?
O1 C5 C6 C7 116.9(3) . . . . ?
N1 C5 C6 C7 -63.7(3) . . . . ?
N2 C6 C7 C8 32.7(3) . . . . ?
C5 C6 C7 C8 -89.5(2) . . . . ?
N2 C6 C7 C13 -143.3(2) . . . . ?
C5 C6 C7 C13 94.6(2) . . . . ?
C13 C7 C8 C9 171.2(2) . . . . ?
C6 C7 C8 C9 -4.8(3) . . . . ?
C7 C8 C9 C10 -18.7(3) . . . . ?
C7 C8 C9 C11 166.5(2) . . . . ?
C8 C9 C10 N2 10.3(3) . . . . ?
C11 C9 C10 N2 -174.97(19) . . . . ?
C8 C9 C10 C15 -167.40(19) . . . . ?
C11 C9 C10 C15 7.4(3) . . . . ?
C10 C9 C11 O4 25.6(4) . . . . ?
C8 C9 C11 O4 -159.8(3) . . . . ?
C10 C9 C11 O5 -155.7(2) . . . . ?
C8 C9 C11 O5 18.9(3) . . . . ?
C8 C7 C13 O2 3.6(4) . . . . ?
C6 C7 C13 O2 179.5(2) . . . . ?
C8 C7 C13 O3 -176.9(2) . . . . ?
C6 C7 C13 O3 -1.0(3) . . . . ?
N2 C10 C15 C16 -120.5(2) . . . . ?
C9 C10 C15 C16 57.3(3) . . . . ?
N2 C10 C15 C20 57.6(3) . . . . ?
C9 C10 C15 C20 -124.7(2) . . . . ?
C20 C15 C16 C17 -0.4(3) . . . . ?
C10 C15 C16 C17 177.6(2) . . . . ?
C15 C16 C17 C18 0.5(3) . . . . ?
C16 C17 C18 C19 0.3(4) . . . . ?
C16 C17 C18 Cl1 179.49(17) . . . . ?
C17 C18 C19 C20 -1.2(3) . . . . ?
Cl1 C18 C19 C20 179.65(17) . . . . ?
C18 C19 C20 C15 1.2(3) . . . . ?
C16 C15 C20 C19 -0.5(3) . . . . ?
C10 C15 C20 C19 -178.60(19) . . . . ?
C26 C21 C22 C23 1.3(3) . . . . ?
N2 C21 C22 C23 177.9(2) . . . . ?
C26 C21 C22 O6 179.17(19) . . . . ?
N2 C21 C22 O6 -4.2(3) . . . . ?
C21 C22 C23 C24 -0.6(4) . . . . ?
O6 C22 C23 C24 -178.5(2) . . . . ?
C22 C23 C24 C25 -0.6(4) . . . . ?
C23 C24 C25 C26 1.1(4) . . . . ?
C24 C25 C26 C21 -0.3(4) . . . . ?
C22 C21 C26 C25 -0.8(3) . . . . ?
N2 C21 C26 C25 -177.4(2) . . . . ?
O7 C27 C28 C33 5.5(4) . . . . ?
O6 C27 C28 C33 -175.1(2) . . . . ?
O7 C27 C28 C29 -174.2(2) . . . . ?
O6 C27 C28 C29 5.2(3) . . . . ?
C33 C28 C29 C30 -0.7(4) . . . . ?
C27 C28 C29 C30 179.0(2) . . . . ?
C28 C29 C30 C31 -0.2(4) . . . . ?
C29 C30 C31 C32 0.8(4) . . . . ?
C29 C30 C31 N3 178.7(2) . . . . ?
C30 C31 C32 C33 -0.7(4) . . . . ?
N3 C31 C32 C33 -178.5(2) . . . . ?
C29 C28 C33 C32 0.8(4) . . . . ?
C27 C28 C33 C32 -178.8(2) . . . . ?
C31 C32 C33 C28 -0.2(4) . . . . ?
O1 C5 N1 C4 2.7(5) . . . . ?
C6 C5 N1 C4 -176.7(3) . . . . ?
C2 C4 N1 C5 -62.1(4) . . . . ?
C1 C4 N1 C5 176.0(4) . . . . ?
C3 C4 N1 C5 56.0(4) . . . . ?
C9 C10 N2 C21 -152.4(2) . . . . ?
C15 C10 N2 C21 25.5(3) . . . . ?
C9 C10 N2 C6 21.7(3) . . . . ?
C15 C10 N2 C6 -160.41(17) . . . . ?
C22 C21 N2 C10 64.4(3) . . . . ?
C26 C21 N2 C10 -119.0(2) . . . . ?
C22 C21 N2 C6 -109.9(2) . . . . ?
C26 C21 N2 C6 66.7(3) . . . . ?
C7 C6 N2 C10 -41.9(2) . . . . ?
C5 C6 N2 C10 82.7(2) . . . . ?
C7 C6 N2 C21 132.47(18) . . . . ?
C5 C6 N2 C21 -103.0(2) . . . . ?
C32 C31 N3 O9 -13.6(4) . . . . ?
C30 C31 N3 O9 168.5(3) . . . . ?
C32 C31 N3 O8 166.7(3) . . . . ?
C30 C31 N3 O8 -11.2(4) . . . . ?
O2 C13 O3 C14 -6.7(4) . . . . ?
C7 C13 O3 C14 173.8(3) . . . . ?
O4 C11 O5 C12 -3.4(4) . . . . ?
C9 C11 O5 C12 177.8(2) . . . . ?
O7 C27 O6 C22 5.9(3) . . . . ?
C28 C27 O6 C22 -173.46(18) . . . . ?
C21 C22 O6 C27 74.6(3) . . . . ?
C23 C22 O6 C27 -107.5(2) . . . . ?
