# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_enero
_database_code_depnum_ccdc_archive 'CCDC 1436301'
_audit_update_record             
;
2015-11-18 deposited with the CCDC.
2015-12-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H31 Cl N4 O3, C4 H8 O2'
_chemical_formula_sum            'C36 H39 Cl N4 O5'
_chemical_formula_weight         643.16

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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n
_symmetry_space_group_name_Hall  -P2yn

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

_cell_length_a                   11.6441(4)
_cell_length_b                   19.0040(11)
_cell_length_c                   15.7545(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.803(3)
_cell_angle_gamma                90.00
_cell_volume                     3370.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1603
_cell_measurement_theta_min      3.72
_cell_measurement_theta_max      63.46

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1360
_exptl_absorpt_coefficient_mu    1.390
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_T_max  0.870
_exptl_absorpt_process_details   'SADABS (Bruker, 2006)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14091
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_av_sigmaI/netI    0.0967
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.72
_diffrn_reflns_theta_max         67.20
_reflns_number_total             5575
_reflns_number_gt                2794
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX 2 (Bruker 2006)'
_computing_cell_refinement       'SAINT (Bruker 2006)'
_computing_data_reduction        'SAINT (Bruker 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Mercury 2.3 (Macrae et al, 2008)'
_computing_publication_material  'Bruker SHELXTL'
_chemical_absolute_configuration rm

_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. 
;

_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)+(0.1122P)²+5.7661P] 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         5575
_refine_ls_number_parameters     390
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1818
_refine_ls_R_factor_gt           0.1032
_refine_ls_wR_factor_ref         0.3048
_refine_ls_wR_factor_gt          0.2658
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.104
_refine_ls_shift/su_max          0.009
_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
Cl1 Cl 0.34912(17) 0.03130(11) 0.42800(13) 0.0760(6) Uani 1 1 d . . .
O1 O 0.0429(3) -0.2895(2) 0.7486(2) 0.0478(11) Uani 1 1 d . . .
O2 O 0.0805(4) -0.1447(3) 0.7030(3) 0.0562(12) Uani 1 1 d . . .
O3 O 0.2726(4) -0.3230(3) 0.9431(3) 0.0629(13) Uani 1 1 d . . .
N1 N -0.0974(4) -0.1965(3) 0.6371(3) 0.0499(14) Uani 1 1 d . . .
H1N H -0.1465 -0.2048 0.5873 0.060 Uiso 1 1 calc R . .
N2 N 0.0130(4) -0.1488(3) 0.5535(3) 0.0599(16) Uani 1 1 d . . .
H2N H -0.0393 -0.1684 0.5116 0.072 Uiso 1 1 calc R . .
N3 N 0.2091(4) -0.2222(3) 0.8664(3) 0.0530(14) Uani 1 1 d . . .
H3N H 0.1622 -0.2073 0.8184 0.064 Uiso 1 1 calc R . .
N4 N 0.2774(7) -0.1024(5) 0.8859(6) 0.104(3) Uani 1 1 d . . .
C1 C -0.2356(5) -0.1972(4) 0.7282(4) 0.0554(18) Uani 1 1 d . . .
H1 H -0.2823 -0.1652 0.6897 0.066 Uiso 1 1 calc R . .
C2 C -0.2752(5) -0.2218(4) 0.7986(4) 0.0589(19) Uani 1 1 d . . .
C3 C -0.2047(6) -0.2702(4) 0.8535(4) 0.0581(18) Uani 1 1 d . . .
H3 H -0.2305 -0.2878 0.9006 0.070 Uiso 1 1 calc R . .
C4 C -0.0958(5) -0.2943(4) 0.8415(4) 0.0526(17) Uani 1 1 d . . .
C5 C -0.0213(6) -0.3481(4) 0.8993(4) 0.063(2) Uani 1 1 d . . .
H5A H -0.0723 -0.3812 0.9192 0.076 Uiso 1 1 calc R . .
H5B H 0.0289 -0.3252 0.9505 0.076 Uiso 1 1 calc R . .
C6 C 0.0550(6) -0.3871(4) 0.8509(4) 0.0570(18) Uani 1 1 d . . .
H6A H 0.0055 -0.4168 0.8062 0.068 Uiso 1 1 calc R . .
H6B H 0.1108 -0.4169 0.8915 0.068 Uiso 1 1 calc R . .
C7 C 0.1227(5) -0.3349(4) 0.8080(4) 0.0483(16) Uani 1 1 d . . .
C8 C -0.0586(5) -0.2677(4) 0.7702(4) 0.0475(16) Uani 1 1 d . . .
C9 C -0.1285(5) -0.2190(3) 0.7133(4) 0.0436(15) Uani 1 1 d . . .
C10 C 0.2013(5) -0.3687(4) 0.7553(4) 0.0537(17) Uani 1 1 d . . .
C11 C 0.2626(6) -0.4304(4) 0.7823(5) 0.065(2) Uani 1 1 d . . .
H11 H 0.2506 -0.4541 0.8310 0.079 Uiso 1 1 calc R . .
C12 C 0.3414(7) -0.4576(5) 0.7384(5) 0.076(2) Uani 1 1 d . . .
H12 H 0.3815 -0.4993 0.7575 0.091 Uiso 1 1 calc R . .
C13 C 0.3605(7) -0.4233(5) 0.6669(6) 0.082(3) Uani 1 1 d . . .
H13 H 0.4130 -0.4416 0.6370 0.098 Uiso 1 1 calc R . .
C14 C 0.3012(7) -0.3614(6) 0.6396(6) 0.085(3) Uani 1 1 d . . .
H14 H 0.3140 -0.3377 0.5912 0.102 Uiso 1 1 calc R . .
C15 C 0.2231(6) -0.3345(4) 0.6835(5) 0.069(2) Uani 1 1 d . . .
H15 H 0.1840 -0.2925 0.6645 0.083 Uiso 1 1 calc R . .
C16 C -0.3942(6) -0.1970(5) 0.8141(6) 0.079(3) Uani 1 1 d . . .
C17 C -0.4664(12) -0.1586(13) 0.7410(10) 0.292(15) Uani 1 1 d . . .
H17A H -0.5468 -0.1753 0.7288 0.438 Uiso 1 1 calc R . .
H17B H -0.4363 -0.1656 0.6903 0.438 Uiso 1 1 calc R . .
H17C H -0.4644 -0.1094 0.7551 0.438 Uiso 1 1 calc R . .
C18 C -0.4652(11) -0.2581(7) 0.8289(14) 0.230(10) Uani 1 1 d . . .
H18A H -0.5418 -0.2423 0.8333 0.345 Uiso 1 1 calc R . .
H18B H -0.4251 -0.2813 0.8824 0.345 Uiso 1 1 calc R . .
H18C H -0.4749 -0.2903 0.7807 0.345 Uiso 1 1 calc R . .
C19 C -0.3687(12) -0.1524(14) 0.8920(13) 0.323(17) Uani 1 1 d . . .
H19A H -0.3474 -0.1061 0.8769 0.485 Uiso 1 1 calc R . .
H19B H -0.3041 -0.1722 0.9360 0.485 Uiso 1 1 calc R . .
H19C H -0.4379 -0.1495 0.9145 0.485 Uiso 1 1 calc R . .
C20 C 0.0044(5) -0.1627(3) 0.6372(4) 0.0469(15) Uani 1 1 d . . .
C21 C 0.0967(5) -0.1066(4) 0.5283(4) 0.0525(17) Uani 1 1 d . . .
C22 C 0.2153(5) -0.1014(4) 0.5744(4) 0.0581(18) Uani 1 1 d . . .
H22 H 0.2434 -0.1266 0.6262 0.070 Uiso 1 1 calc R . .
C23 C 0.2912(6) -0.0587(4) 0.5428(4) 0.0575(18) Uani 1 1 d . . .
H23 H 0.3703 -0.0551 0.5742 0.069 Uiso 1 1 calc R . .
C24 C 0.2525(6) -0.0217(4) 0.4665(4) 0.0535(17) Uani 1 1 d . . .
C25 C 0.1354(6) -0.0261(5) 0.4197(5) 0.071(2) Uani 1 1 d . . .
H25 H 0.1080 -0.0008 0.3680 0.085 Uiso 1 1 calc R . .
C26 C 0.0591(6) -0.0689(5) 0.4509(5) 0.075(2) Uani 1 1 d . . .
H26 H -0.0197 -0.0725 0.4189 0.090 Uiso 1 1 calc R . .
C27 C 0.2078(5) -0.2916(4) 0.8804(4) 0.0473(15) Uani 1 1 d . . .
C28 C 0.2778(5) -0.1709(4) 0.9205(5) 0.0551(17) Uani 1 1 d . . .
C29 C 0.3419(7) -0.0518(5) 0.9410(7) 0.096(3) Uani 1 1 d . . .
H29 H 0.3426 -0.0056 0.9217 0.115 Uiso 1 1 calc R . .
C30 C 0.4038(7) -0.0695(5) 1.0229(6) 0.085(3) Uani 1 1 d . . .
H30 H 0.4474 -0.0360 1.0608 0.102 Uiso 1 1 calc R . .
C31 C 0.4005(7) -0.1382(5) 1.0487(5) 0.081(2) Uani 1 1 d . . .
H31 H 0.4445 -0.1506 1.1047 0.097 Uiso 1 1 calc R . .
C32 C 0.3386(5) -0.1876(4) 0.9986(4) 0.0494(16) Uani 1 1 d . . .
H32 H 0.3386 -0.2335 1.0189 0.059 Uiso 1 1 calc R . .
O4 O 0.5440(10) -0.3054(7) 0.5364(8) 0.206(5) Uiso 1 1 d . . .
O5 O 0.6077(7) -0.4107(5) 0.5700(6) 0.144(3) Uiso 1 1 d . . .
C33 C 0.7235(12) -0.4468(8) 0.7023(9) 0.169(5) Uiso 1 1 d . . .
H33A H 0.6724 -0.4865 0.6839 0.254 Uiso 1 1 calc R . .
H33B H 0.7366 -0.4403 0.7645 0.254 Uiso 1 1 calc R . .
H33C H 0.7982 -0.4549 0.6886 0.254 Uiso 1 1 calc R . .
C34 C 0.6653(11) -0.3808(7) 0.6545(8) 0.138(4) Uiso 1 1 d . . .
H34A H 0.6084 -0.3603 0.6829 0.165 Uiso 1 1 calc R . .
H34B H 0.7238 -0.3456 0.6498 0.165 Uiso 1 1 calc R . .
C35 C 0.5393(14) -0.3643(10) 0.5065(12) 0.164(5) Uiso 1 1 d . . .
C36 C 0.4809(12) -0.3967(8) 0.4285(9) 0.159(5) Uiso 1 1 d . . .
H36A H 0.4151 -0.3681 0.3985 0.238 Uiso 1 1 calc R . .
H36B H 0.4523 -0.4419 0.4410 0.238 Uiso 1 1 calc R . .
H36C H 0.5349 -0.4026 0.3921 0.238 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
Cl1 C24 1.730(7) . ?
O1 C8 1.375(7) . ?
O1 C7 1.429(7) . ?
O2 C20 1.228(7) . ?
O3 C27 1.233(7) . ?
N1 C20 1.347(8) . ?
N1 C9 1.405(7) . ?
N1 H1N 0.8600 . ?
N2 C20 1.374(7) . ?
N2 C21 1.396(8) . ?
N2 H2N 0.8600 . ?
N3 C27 1.338(8) . ?
N3 C28 1.403(8) . ?
N3 H3N 0.8600 . ?
N4 C29 1.382(11) . ?
N4 C28 1.412(10) . ?
C1 C2 1.387(9) . ?
C1 C9 1.390(8) . ?
C1 H1 0.9300 . ?
C2 C3 1.380(9) . ?
C2 C16 1.541(9) . ?
C3 C4 1.406(9) . ?
C3 H3 0.9300 . ?
C4 C8 1.397(8) . ?
C4 C5 1.491(9) . ?
C5 C6 1.506(9) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.527(8) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C10 1.525(9) . ?
C7 C27 1.543(9) . ?
C8 C9 1.397(8) . ?
C10 C15 1.383(9) . ?
C10 C11 1.383(9) . ?
C11 C12 1.382(10) . ?
C11 H11 0.9300 . ?
C12 C13 1.369(11) . ?
C12 H12 0.9300 . ?
C13 C14 1.376(12) . ?
C13 H13 0.9300 . ?
C14 C15 1.374(10) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.439(14) . ?
C16 C19 1.459(15) . ?
C16 C18 1.478(14) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C21 C26 1.385(9) . ?
C21 C22 1.390(8) . ?
C22 C23 1.384(9) . ?
C22 H22 0.9300 . ?
C23 C24 1.366(9) . ?
C23 H23 0.9300 . ?
C24 C25 1.378(9) . ?
C25 C26 1.384(10) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C28 C32 1.292(8) . ?
C29 C30 1.350(11) . ?
C29 H29 0.9300 . ?
C30 C31 1.370(11) . ?
C30 H30 0.9300 . ?
C31 C32 1.316(10) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
O4 C35 1.210(17) . ?
O5 C35 1.417(16) . ?
O5 C34 1.447(12) . ?
C33 C34 1.529(16) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.387(17) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 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
C8 O1 C7 118.4(4) . . ?
C20 N1 C9 124.3(5) . . ?
C20 N1 H1N 117.9 . . ?
C9 N1 H1N 117.9 . . ?
C20 N2 C21 127.6(5) . . ?
C20 N2 H2N 116.2 . . ?
C21 N2 H2N 116.2 . . ?
C27 N3 C28 127.8(6) . . ?
C27 N3 H3N 116.1 . . ?
C28 N3 H3N 116.1 . . ?
C29 N4 C28 116.9(8) . . ?
C2 C1 C9 122.1(6) . . ?
C2 C1 H1 119.0 . . ?
C9 C1 H1 119.0 . . ?
C3 C2 C1 117.4(6) . . ?
C3 C2 C16 121.3(6) . . ?
C1 C2 C16 121.3(7) . . ?
C2 C3 C4 123.0(6) . . ?
C2 C3 H3 118.5 . . ?
C4 C3 H3 118.5 . . ?
C8 C4 C3 117.8(6) . . ?
C8 C4 C5 119.2(6) . . ?
C3 C4 C5 123.0(6) . . ?
C4 C5 C6 110.8(5) . . ?
C4 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
C5 C6 C7 110.0(6) . . ?
C5 C6 H6A 109.7 . . ?
C7 C6 H6A 109.7 . . ?
C5 C6 H6B 109.7 . . ?
C7 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
O1 C7 C10 106.1(5) . . ?
O1 C7 C6 111.0(5) . . ?
C10 C7 C6 114.6(6) . . ?
O1 C7 C27 110.5(5) . . ?
C10 C7 C27 105.4(5) . . ?
C6 C7 C27 109.0(5) . . ?
O1 C8 C4 123.6(6) . . ?
O1 C8 C9 115.9(5) . . ?
C4 C8 C9 120.4(6) . . ?
C1 C9 C8 119.3(5) . . ?
C1 C9 N1 119.5(6) . . ?
C8 C9 N1 121.0(5) . . ?
C15 C10 C11 117.5(7) . . ?
C15 C10 C7 120.6(6) . . ?
C11 C10 C7 121.6(6) . . ?
C12 C11 C10 121.3(8) . . ?
C12 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
C13 C12 C11 120.1(8) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C12 C13 C14 119.4(8) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 H13 120.3 . . ?
C13 C14 C15 120.3(8) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C14 C15 C10 121.4(8) . . ?
C14 C15 H15 119.3 . . ?
C10 C15 H15 119.3 . . ?
C17 C16 C19 109.3(14) . . ?
C17 C16 C18 106.7(12) . . ?
C19 C16 C18 109.0(13) . . ?
C17 C16 C2 113.2(7) . . ?
C19 C16 C2 108.2(8) . . ?
C18 C16 C2 110.3(8) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O2 C20 N1 125.3(6) . . ?
O2 C20 N2 122.9(6) . . ?
N1 C20 N2 111.8(5) . . ?
C26 C21 C22 118.2(6) . . ?
C26 C21 N2 117.4(6) . . ?
C22 C21 N2 124.3(6) . . ?
C23 C22 C21 119.6(6) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
C24 C23 C22 121.4(6) . . ?
C24 C23 H23 119.3 . . ?
C22 C23 H23 119.3 . . ?
C23 C24 C25 119.9(6) . . ?
C23 C24 Cl1 120.7(5) . . ?
C25 C24 Cl1 119.5(5) . . ?
C24 C25 C26 118.9(7) . . ?
C24 C25 H25 120.5 . . ?
C26 C25 H25 120.5 . . ?
C25 C26 C21 121.9(6) . . ?
C25 C26 H26 119.0 . . ?
C21 C26 H26 119.0 . . ?
O3 C27 N3 125.4(6) . . ?
O3 C27 C7 118.6(6) . . ?
N3 C27 C7 115.8(5) . . ?
C32 C28 N3 119.8(7) . . ?
C32 C28 N4 122.7(7) . . ?
N3 C28 N4 117.5(6) . . ?
C30 C29 N4 119.9(9) . . ?
C30 C29 H29 120.1 . . ?
N4 C29 H29 120.1 . . ?
C29 C30 C31 118.2(8) . . ?
C29 C30 H30 120.9 . . ?
C31 C30 H30 120.9 . . ?
C32 C31 C30 123.6(8) . . ?
C32 C31 H31 118.2 . . ?
C30 C31 H31 118.2 . . ?
C28 C32 C31 118.6(7) . . ?
C28 C32 H32 120.7 . . ?
C31 C32 H32 120.7 . . ?
C35 O5 C34 116.7(12) . . ?
C34 C33 H33A 109.5 . . ?
C34 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C34 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O5 C34 C33 100.0(11) . . ?
O5 C34 H34A 111.8 . . ?
C33 C34 H34A 111.8 . . ?
O5 C34 H34B 111.8 . . ?
C33 C34 H34B 111.8 . . ?
H34A C34 H34B 109.5 . . ?
O4 C35 C36 136.0(19) . . ?
O4 C35 O5 109.9(16) . . ?
C36 C35 O5 114.1(16) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.925
_diffrn_reflns_theta_full        67.20
_diffrn_measured_fraction_theta_full 0.925
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.070
####################################################################### 
# 
# 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_2fin
_database_code_depnum_ccdc_archive 'CCDC 1436302'
_audit_update_record             
;
2015-11-18 deposited with the CCDC.
2015-12-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H31 Cl N4 O3, H2 O'
_chemical_formula_sum            'C32 H33 Cl N4 O4'
_chemical_formula_weight         573.07

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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  -P1



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

_cell_length_a                   8.4156(5)
_cell_length_b                   11.6638(8)
_cell_length_c                   14.9936(8)
_cell_angle_alpha                87.286(5)
_cell_angle_beta                 83.220(4)
_cell_angle_gamma                82.716(5)
_cell_volume                     1448.87(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2180
_cell_measurement_theta_min      2.97
_cell_measurement_theta_max      62.69

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             604
_exptl_absorpt_coefficient_mu    1.525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.803
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_process_details   'SADABS (Bruker, 2006)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8298
_diffrn_reflns_av_R_equivalents  0.0755
_diffrn_reflns_av_sigmaI/netI    0.0915
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.97
_diffrn_reflns_theta_max         67.29
_reflns_number_total             4419
_reflns_number_gt                2357
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX 2 (Bruker 2006)'
_computing_cell_refinement       'SAINT (Bruker 2006)'
_computing_data_reduction        'SAINT (Bruker 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Mercury 2.3 (Macrae et al, 2008)'
_computing_publication_material  'Bruker SHELXTL'
_chemical_absolute_configuration rm

_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. 
;

_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.020(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4419
_refine_ls_number_parameters     382
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2429
_refine_ls_R_factor_gt           0.1298
_refine_ls_wR_factor_ref         0.4035
_refine_ls_wR_factor_gt          0.3206
_refine_ls_goodness_of_fit_ref   2.257
_refine_ls_restrained_S_all      2.257
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl -0.0101(3) 0.9673(3) 0.38499(15) 0.1013(11) Uani 1 1 d . . .
O1 O -0.5153(6) 1.2036(5) -0.2147(3) 0.0538(14) Uani 1 1 d . . .
O2 O -0.2235(7) 0.9048(6) -0.0315(3) 0.0658(17) Uani 1 1 d . . .
O3 O -0.7175(8) 1.4691(6) -0.2883(4) 0.085(2) Uani 1 1 d . . .
N1 N -0.3573(7) 1.0615(6) -0.0993(4) 0.0574(18) Uani 1 1 d . . .
H1N H -0.3979 1.1320 -0.0903 0.069 Uiso 1 1 calc R . .
N2 N -0.2767(7) 1.0764(6) 0.0392(4) 0.0566(17) Uani 1 1 d . . .
H2 H -0.3171 1.1475 0.0329 0.068 Uiso 1 1 calc R . .
N3 N -0.6543(8) 1.4007(6) -0.1511(4) 0.0628(19) Uani 1 1 d . . .
H3N H -0.6032 1.3425 -0.1249 0.075 Uiso 1 1 calc R . .
N4 N -0.7016(9) 1.4699(7) -0.0091(4) 0.071(2) Uani 1 1 d . . .
C1 C -0.3154(9) 0.9065(7) -0.2088(4) 0.055(2) Uani 1 1 d . . .
H1 H -0.2618 0.8569 -0.1687 0.066 Uiso 1 1 calc R . .
C2 C -0.3333(9) 0.8677(8) -0.2925(5) 0.060(2) Uani 1 1 d . . .
C3 C -0.4135(9) 0.9436(8) -0.3504(5) 0.061(2) Uani 1 1 d . . .
H3 H -0.4275 0.9187 -0.4067 0.074 Uiso 1 1 calc R . .
C4 C -0.4737(9) 1.0554(8) -0.3275(4) 0.054(2) Uani 1 1 d . . .
C5 C -0.5630(10) 1.1345(8) -0.3929(5) 0.064(2) Uani 1 1 d . . .
H5A H -0.4867 1.1587 -0.4416 0.076 Uiso 1 1 calc R . .
H5B H -0.6383 1.0926 -0.4184 0.076 Uiso 1 1 calc R . .
C6 C -0.6532(10) 1.2392(8) -0.3476(5) 0.061(2) Uani 1 1 d . . .
H6A H -0.7511 1.2184 -0.3133 0.073 Uiso 1 1 calc R . .
H6B H -0.6837 1.2975 -0.3928 0.073 Uiso 1 1 calc R . .
C7 C -0.5511(9) 1.2890(7) -0.2853(4) 0.0514(19) Uani 1 1 d . . .
C8 C -0.4552(9) 1.0921(7) -0.2441(4) 0.053(2) Uani 1 1 d . . .
C9 C -0.3759(8) 1.0182(7) -0.1835(4) 0.0501(19) Uani 1 1 d . . .
C10 C -0.3935(10) 1.3247(7) -0.3310(5) 0.061(2) Uani 1 1 d . . .
C11 C -0.2612(11) 1.3257(8) -0.2834(7) 0.074(2) Uani 1 1 d . . .
H11 H -0.2715 1.3037 -0.2228 0.088 Uiso 1 1 calc R . .
C12 C -0.1200(14) 1.3568(10) -0.3208(9) 0.102(4) Uani 1 1 d . . .
H12 H -0.0342 1.3539 -0.2866 0.122 Uiso 1 1 calc R . .
C13 C -0.1013(16) 1.3927(11) -0.4090(11) 0.115(4) Uani 1 1 d . . .
H13 H -0.0023 1.4122 -0.4355 0.138 Uiso 1 1 calc R . .
C14 C -0.2317(18) 1.3999(10) -0.4590(8) 0.112(4) Uani 1 1 d . . .
H14 H -0.2211 1.4273 -0.5184 0.134 Uiso 1 1 calc R . .
C15 C -0.3806(14) 1.3655(9) -0.4195(6) 0.087(3) Uani 1 1 d . . .
H15 H -0.4681 1.3702 -0.4526 0.104 Uiso 1 1 calc R . .
C16 C -0.2696(10) 0.7395(8) -0.3176(5) 0.066(2) Uani 1 1 d . . .
C17 C -0.390(3) 0.6669(15) -0.2824(18) 0.285(16) Uani 1 1 d . . .
H17A H -0.3395 0.5888 -0.2754 0.428 Uiso 1 1 calc R . .
H17B H -0.4697 0.6693 -0.3232 0.428 Uiso 1 1 calc R . .
H17C H -0.4395 0.6940 -0.2251 0.428 Uiso 1 1 calc R . .
C18 C -0.121(2) 0.7020(15) -0.2806(16) 0.261(16) Uani 1 1 d . . .
H18A H -0.1418 0.6542 -0.2276 0.391 Uiso 1 1 calc R . .
H18B H -0.0740 0.7683 -0.2652 0.391 Uiso 1 1 calc R . .
H18C H -0.0476 0.6586 -0.3241 0.391 Uiso 1 1 calc R . .
C19 C -0.236(3) 0.7276(15) -0.4135(9) 0.269(16) Uani 1 1 d . . .
H19A H -0.1456 0.7674 -0.4357 0.403 Uiso 1 1 calc R . .
H19B H -0.3286 0.7602 -0.4419 0.403 Uiso 1 1 calc R . .
H19C H -0.2115 0.6471 -0.4268 0.403 Uiso 1 1 calc R . .
C20 C -0.2830(9) 1.0056(9) -0.0305(4) 0.059(2) Uani 1 1 d . . .
C21 C -0.2105(8) 1.0441(7) 0.1204(4) 0.052(2) Uani 1 1 d . . .
C22 C -0.0944(10) 0.9538(9) 0.1294(5) 0.070(3) Uani 1 1 d . . .
H22 H -0.0563 0.9072 0.0808 0.084 Uiso 1 1 calc R . .
C23 C -0.0326(10) 0.9308(8) 0.2107(5) 0.066(2) Uani 1 1 d . . .
H23 H 0.0456 0.8680 0.2172 0.079 Uiso 1 1 calc R . .
C24 C -0.0862(10) 1.0003(9) 0.2816(5) 0.065(2) Uani 1 1 d . . .
C25 C -0.1982(11) 1.0941(9) 0.2729(5) 0.070(3) Uani 1 1 d . . .
H25 H -0.2324 1.1430 0.3205 0.084 Uiso 1 1 calc R . .
C26 C -0.2592(10) 1.1147(8) 0.1913(5) 0.064(2) Uani 1 1 d . . .
H26 H -0.3358 1.1784 0.1844 0.077 Uiso 1 1 calc R . .
C27 C -0.6504(9) 1.3957(7) -0.2420(5) 0.057(2) Uani 1 1 d . . .
C28 C -0.7315(10) 1.4890(9) -0.0949(5) 0.068(2) Uani 1 1 d . . .
C29 C -0.7741(13) 1.5470(9) 0.0504(6) 0.088(3) Uani 1 1 d . . .
H29 H -0.7541 1.5354 0.1101 0.105 Uiso 1 1 calc R . .
C30 C -0.8745(12) 1.6405(9) 0.0286(6) 0.083(3) Uani 1 1 d . . .
H30 H -0.9243 1.6911 0.0724 0.100 Uiso 1 1 calc R . .
C31 C -0.9021(11) 1.6596(9) -0.0594(6) 0.077(3) Uani 1 1 d . . .
H31 H -0.9710 1.7240 -0.0755 0.093 Uiso 1 1 calc R . .
C32 C -0.8295(11) 1.5853(9) -0.1235(6) 0.074(3) Uani 1 1 d . . .
H32 H -0.8448 1.5985 -0.1837 0.089 Uiso 1 1 calc R . .
O4 O -0.5397(8) 1.2508(7) 0.0083(4) 0.0705(17) Uani 1 1 d . . .
H1O H -0.610(12) 1.195(9) 0.026(6) 0.09(3) Uiso 1 1 d . . .
H2O H -0.603(7) 1.314(5) 0.014(3) 0.017(15) Uiso 1 1 d . . .


_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
Cl1 C24 1.753(7) . ?
O1 C8 1.405(9) . ?
O1 C7 1.450(8) . ?
O2 C20 1.218(10) . ?
O3 C27 1.202(9) . ?
N1 C20 1.365(9) . ?
N1 C9 1.415(8) . ?
N1 H1N 0.8600 . ?
N2 C20 1.373(10) . ?
N2 C21 1.414(9) . ?
N2 H2 0.8600 . ?
N3 C27 1.363(9) . ?
N3 C28 1.406(10) . ?
N3 H3N 0.8600 . ?
N4 C29 1.336(11) . ?
N4 C28 1.343(10) . ?
C1 C2 1.385(9) . ?
C1 C9 1.390(11) . ?
C1 H1 0.9300 . ?
C2 C3 1.381(11) . ?
C2 C16 1.571(12) . ?
C3 C4 1.381(11) . ?
C3 H3 0.9300 . ?
C4 C8 1.373(9) . ?
C4 C5 1.513(11) . ?
C5 C6 1.500(11) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.522(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C10 1.517(11) . ?
C7 C27 1.534(11) . ?
C8 C9 1.392(11) . ?
C10 C15 1.385(11) . ?
C10 C11 1.393(12) . ?
C11 C12 1.338(14) . ?
C11 H11 0.9300 . ?
C12 C13 1.366(16) . ?
C12 H12 0.9300 . ?
C13 C14 1.392(17) . ?
C13 H13 0.9300 . ?
C14 C15 1.418(16) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.44(2) . ?
C16 C18 1.438(15) . ?
C16 C19 1.442(15) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C21 C22 1.356(12) . ?
C21 C26 1.368(10) . ?
C22 C23 1.384(10) . ?
C22 H22 0.9300 . ?
C23 C24 1.366(12) . ?
C23 H23 0.9300 . ?
C24 C25 1.363(13) . ?
C25 C26 1.381(10) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C28 C32 1.388(12) . ?
C29 C30 1.345(13) . ?
C29 H29 0.9300 . ?
C30 C31 1.370(12) . ?
C30 H30 0.9300 . ?
C31 C32 1.361(12) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
O4 H1O 0.94(11) . ?
O4 H2O 0.86(6) . ?

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
C8 O1 C7 115.3(5) . . ?
C20 N1 C9 128.2(7) . . ?
C20 N1 H1N 115.9 . . ?
C9 N1 H1N 115.9 . . ?
C20 N2 C21 126.4(7) . . ?
C20 N2 H2 116.8 . . ?
C21 N2 H2 116.8 . . ?
C27 N3 C28 128.1(7) . . ?
C27 N3 H3N 116.0 . . ?
C28 N3 H3N 116.0 . . ?
C29 N4 C28 117.2(8) . . ?
C2 C1 C9 121.4(7) . . ?
C2 C1 H1 119.3 . . ?
C9 C1 H1 119.3 . . ?
C3 C2 C1 117.8(8) . . ?
C3 C2 C16 122.0(6) . . ?
C1 C2 C16 120.1(7) . . ?
C2 C3 C4 122.2(6) . . ?
C2 C3 H3 118.9 . . ?
C4 C3 H3 118.9 . . ?
C8 C4 C3 119.1(7) . . ?
C8 C4 C5 120.8(8) . . ?
C3 C4 C5 120.0(6) . . ?
C6 C5 C4 111.4(6) . . ?
C6 C5 H5A 109.4 . . ?
C4 C5 H5A 109.4 . . ?
C6 C5 H5B 109.4 . . ?
C4 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?
C5 C6 C7 111.2(6) . . ?
C5 C6 H6A 109.4 . . ?
C7 C6 H6A 109.4 . . ?
C5 C6 H6B 109.4 . . ?
C7 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
O1 C7 C10 108.5(6) . . ?
O1 C7 C6 108.7(6) . . ?
C10 C7 C6 114.6(6) . . ?
O1 C7 C27 108.4(5) . . ?
C10 C7 C27 108.2(7) . . ?
C6 C7 C27 108.2(6) . . ?
C4 C8 C9 120.6(8) . . ?
C4 C8 O1 122.8(7) . . ?
C9 C8 O1 116.5(6) . . ?
C1 C9 C8 118.9(6) . . ?
C1 C9 N1 122.9(7) . . ?
C8 C9 N1 118.1(7) . . ?
C15 C10 C11 117.9(9) . . ?
C15 C10 C7 120.9(8) . . ?
C11 C10 C7 121.0(7) . . ?
C12 C11 C10 123.1(10) . . ?
C12 C11 H11 118.4 . . ?
C10 C11 H11 118.4 . . ?
C11 C12 C13 120.2(12) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C12 C13 C14 119.5(11) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 H13 120.3 . . ?
C13 C14 C15 120.1(11) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C10 C15 C14 119.0(10) . . ?
C10 C15 H15 120.5 . . ?
C14 C15 H15 120.5 . . ?
C17 C16 C18 109.8(15) . . ?
C17 C16 C19 109.6(15) . . ?
C18 C16 C19 106.5(14) . . ?
C17 C16 C2 108.5(9) . . ?
C18 C16 C2 110.6(8) . . ?
C19 C16 C2 111.7(9) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O2 C20 N1 124.1(7) . . ?
O2 C20 N2 123.1(7) . . ?
N1 C20 N2 112.8(8) . . ?
C22 C21 C26 119.0(7) . . ?
C22 C21 N2 124.0(7) . . ?
C26 C21 N2 116.8(7) . . ?
C21 C22 C23 120.0(8) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C24 C23 C22 120.1(9) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C25 C24 C23 120.8(7) . . ?
C25 C24 Cl1 119.9(7) . . ?
C23 C24 Cl1 119.3(7) . . ?
C24 C25 C26 118.1(8) . . ?
C24 C25 H25 121.0 . . ?
C26 C25 H25 121.0 . . ?
C21 C26 C25 122.0(9) . . ?
C21 C26 H26 119.0 . . ?
C25 C26 H26 119.0 . . ?
O3 C27 N3 124.1(7) . . ?
O3 C27 C7 119.9(7) . . ?
N3 C27 C7 116.0(7) . . ?
N4 C28 C32 122.9(8) . . ?
N4 C28 N3 112.5(8) . . ?
C32 C28 N3 124.5(7) . . ?
N4 C29 C30 123.4(9) . . ?
N4 C29 H29 118.3 . . ?
C30 C29 H29 118.3 . . ?
C29 C30 C31 118.7(9) . . ?
C29 C30 H30 120.6 . . ?
C31 C30 H30 120.6 . . ?
C32 C31 C30 120.6(9) . . ?
C32 C31 H31 119.7 . . ?
C30 C31 H31 119.7 . . ?
C31 C32 C28 117.1(8) . . ?
C31 C32 H32 121.5 . . ?
C28 C32 H32 121.5 . . ?
H1O O4 H2O 102(7) . . ?

_diffrn_measured_fraction_theta_max 0.853
_diffrn_reflns_theta_full        67.29
_diffrn_measured_fraction_theta_full 0.853
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.212
