# Electronic Supplementary Material (ESI) for RSC Advances.
# 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_fin
_database_code_depnum_ccdc_archive 'CCDC 1041757'
_audit_update_record             
;
2015-01-01 deposited with the CCDC.
2015-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        KSH
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C49 H34 Cl N O4'
_chemical_formula_sum            'C49 H34 Cl N O4'
_chemical_formula_weight         736.22

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'

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

_cell_length_a                   8.890(5)
_cell_length_b                   10.257(5)
_cell_length_c                   20.323(5)
_cell_angle_alpha                91.701(5)
_cell_angle_beta                 90.533(5)
_cell_angle_gamma                98.252(5)
_cell_volume                     1833.0(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             768
_exptl_absorpt_coefficient_mu    0.154
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.9698
_exptl_absorpt_correction_T_max  0.9848
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27769
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         26.61
_reflns_number_total             7610
_reflns_number_gt                6162
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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 > 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)+(0.0666P)²+0.3762P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7610
_refine_ls_number_parameters     497
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0395
_refine_ls_wR_factor_ref         0.1189
_refine_ls_wR_factor_gt          0.1103
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_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
C1 C 0.72967(17) -0.27218(13) 0.83736(7) 0.0383(3) Uani 1 1 d . . .
C2 C 0.60227(17) -0.38027(14) 0.83320(8) 0.0422(3) Uani 1 1 d . . .
C3 C 0.5781(2) -0.50290(15) 0.86063(10) 0.0544(4) Uani 1 1 d . . .
H3 H 0.6484 -0.5295 0.8896 0.065 Uiso 1 1 calc R . .
C4 C 0.4428(2) -0.58614(16) 0.84302(11) 0.0640(5) Uani 1 1 d . . .
H4 H 0.4256 -0.6700 0.8601 0.077 Uiso 1 1 calc R . .
C5 C 0.3362(2) -0.54826(16) 0.80187(10) 0.0597(5) Uani 1 1 d . . .
H5 H 0.2497 -0.6075 0.7909 0.072 Uiso 1 1 calc R . .
C6 C 0.35392(18) -0.42089(15) 0.77550(8) 0.0483(4) Uani 1 1 d . . .
C7 C 0.25056(19) -0.36484(17) 0.73568(9) 0.0552(4) Uani 1 1 d . . .
H7 H 0.1577 -0.4138 0.7235 0.066 Uiso 1 1 calc R . .
C8 C 0.28673(18) -0.23910(17) 0.71507(8) 0.0511(4) Uani 1 1 d . . .
H8 H 0.2159 -0.2031 0.6900 0.061 Uiso 1 1 calc R . .
C9 C 0.42896(17) -0.16067(15) 0.73049(7) 0.0422(3) Uani 1 1 d . . .
H9 H 0.4513 -0.0758 0.7150 0.051 Uiso 1 1 calc R . .
C10 C 0.53172(16) -0.21224(13) 0.76832(7) 0.0355(3) Uani 1 1 d . . .
C11 C 0.49208(17) -0.34059(13) 0.79159(7) 0.0395(3) Uani 1 1 d . . .
C12 C 0.69177(15) -0.15969(12) 0.79327(7) 0.0327(3) Uani 1 1 d . . .
C13 C 0.81170(15) -0.13934(13) 0.73763(7) 0.0351(3) Uani 1 1 d . . .
H13A H 0.8625 -0.2165 0.7322 0.042 Uiso 1 1 calc R . .
H13B H 0.7631 -0.1243 0.6962 0.042 Uiso 1 1 calc R . .
C14 C 0.92575(15) -0.01902(13) 0.75880(6) 0.0328(3) Uani 1 1 d . . .
C15 C 1.02685(15) 0.04036(13) 0.70414(7) 0.0345(3) Uani 1 1 d . . .
C16 C 0.98184(17) 0.03104(16) 0.63837(7) 0.0460(4) Uani 1 1 d . . .
H16 H 0.8838 -0.0079 0.6269 0.055 Uiso 1 1 calc R . .
C17 C 1.08064(18) 0.07883(17) 0.58963(8) 0.0492(4) Uani 1 1 d . . .
H17 H 1.0474 0.0713 0.5460 0.059 Uiso 1 1 calc R . .
C18 C 1.22817(16) 0.13770(15) 0.60431(7) 0.0413(3) Uani 1 1 d . . .
C19 C 1.27073(17) 0.15182(16) 0.67045(8) 0.0455(4) Uani 1 1 d . . .
H19 H 1.3672 0.1944 0.6821 0.055 Uiso 1 1 calc R . .
C20 C 1.17255(16) 0.10381(15) 0.71919(7) 0.0413(3) Uani 1 1 d . . .
H20 H 1.2045 0.1141 0.7630 0.050 Uiso 1 1 calc R . .
C21 C 1.33603(17) 0.18077(17) 0.55114(8) 0.0456(4) Uani 1 1 d . . .
C22 C 1.3405(2) 0.1023(2) 0.49420(9) 0.0568(4) Uani 1 1 d . . .
H22 H 1.2745 0.0235 0.4894 0.068 Uiso 1 1 calc R . .
C23 C 1.4417(2) 0.1402(2) 0.44480(10) 0.0716(6) Uani 1 1 d . . .
H23 H 1.4429 0.0874 0.4069 0.086 Uiso 1 1 calc R . .
C24 C 1.5406(2) 0.2557(3) 0.45151(11) 0.0792(7) Uani 1 1 d . . .
H24 H 1.6090 0.2809 0.4183 0.095 Uiso 1 1 calc R . .
C25 C 1.5384(2) 0.3340(2) 0.50746(11) 0.0753(6) Uani 1 1 d . . .
H25 H 1.6058 0.4120 0.5121 0.090 Uiso 1 1 calc R . .
C26 C 1.4359(2) 0.29717(19) 0.55705(9) 0.0582(4) Uani 1 1 d . . .
H26 H 1.4343 0.3512 0.5945 0.070 Uiso 1 1 calc R . .
C27 C 0.81859(14) 0.07522(12) 0.79028(6) 0.0307(3) Uani 1 1 d . . .
C28 C 0.89911(14) 0.19421(13) 0.82792(6) 0.0318(3) Uani 1 1 d . . .
C29 C 0.98682(16) 0.20514(14) 0.88471(7) 0.0376(3) Uani 1 1 d . . .
H29 H 1.0084 0.1307 0.9059 0.045 Uiso 1 1 calc R . .
C30 C 1.04200(16) 0.33111(16) 0.90928(7) 0.0423(3) Uani 1 1 d . . .
C31 C 1.01231(17) 0.44289(15) 0.87898(8) 0.0453(4) Uani 1 1 d . . .
H31 H 1.0501 0.5256 0.8971 0.054 Uiso 1 1 calc R . .
C32 C 0.92590(16) 0.43238(14) 0.82129(8) 0.0408(3) Uani 1 1 d . . .
H32 H 0.9065 0.5071 0.7997 0.049 Uiso 1 1 calc R . .
C33 C 0.86962(15) 0.30746(13) 0.79690(7) 0.0342(3) Uani 1 1 d . . .
C34 C 0.73518(15) 0.13920(13) 0.73566(7) 0.0336(3) Uani 1 1 d . . .
C35 C 0.71147(18) 0.36355(15) 0.70011(8) 0.0452(4) Uani 1 1 d . . .
H35A H 0.6627 0.4229 0.7281 0.054 Uiso 1 1 calc R . .
H35B H 0.6333 0.3137 0.6722 0.054 Uiso 1 1 calc R . .
C36 C 0.82342(18) 0.44469(14) 0.65706(7) 0.0427(3) Uani 1 1 d . . .
C37 C 0.9567(2) 0.40304(18) 0.63681(9) 0.0559(4) Uani 1 1 d . . .
H37 H 0.9823 0.3239 0.6514 0.067 Uiso 1 1 calc R . .
C38 C 1.0528(3) 0.4786(2) 0.59476(10) 0.0739(6) Uani 1 1 d . . .
H38 H 1.1425 0.4497 0.5813 0.089 Uiso 1 1 calc R . .
C39 C 1.0171(3) 0.5946(2) 0.57300(10) 0.0812(7) Uani 1 1 d . . .
H39 H 1.0826 0.6452 0.5451 0.097 Uiso 1 1 calc R . .
C40 C 0.8848(3) 0.6367(2) 0.59224(11) 0.0794(7) Uani 1 1 d . . .
H40 H 0.8598 0.7155 0.5769 0.095 Uiso 1 1 calc R . .
C41 C 0.7875(2) 0.56264(16) 0.63441(9) 0.0602(5) Uani 1 1 d . . .
H41 H 0.6980 0.5922 0.6475 0.072 Uiso 1 1 calc R . .
C42 C 0.71492(14) -0.02288(12) 0.83225(6) 0.0307(3) Uani 1 1 d . . .
H42 H 0.7736 -0.0352 0.8721 0.037 Uiso 1 1 calc R . .
C43 C 0.56736(15) 0.01991(13) 0.85536(7) 0.0343(3) Uani 1 1 d . . .
C44 C 0.47620(16) -0.06635(14) 0.90275(7) 0.0370(3) Uani 1 1 d . . .
C45 C 0.31910(18) -0.0744(2) 0.90082(9) 0.0566(4) Uani 1 1 d . . .
H45 H 0.2732 -0.0232 0.8718 0.068 Uiso 1 1 calc R . .
C46 C 0.2307(2) -0.1577(2) 0.94167(11) 0.0751(6) Uani 1 1 d . . .
H46 H 0.1253 -0.1636 0.9396 0.090 Uiso 1 1 calc R . .
C47 C 0.2976(2) -0.2321(2) 0.98539(10) 0.0715(6) Uani 1 1 d . . .
H47 H 0.2375 -0.2888 1.0126 0.086 Uiso 1 1 calc R . .
C48 C 0.4523(2) -0.22294(19) 0.98893(9) 0.0609(5) Uani 1 1 d . . .
H48 H 0.4973 -0.2721 1.0192 0.073 Uiso 1 1 calc R . .
C49 C 0.54229(18) -0.14089(16) 0.94764(8) 0.0452(4) Uani 1 1 d . . .
H49 H 0.6475 -0.1357 0.9500 0.054 Uiso 1 1 calc R . .
N1 N 0.77635(13) 0.27266(11) 0.74150(6) 0.0360(3) Uani 1 1 d . . .
O1 O 0.84985(13) -0.26860(10) 0.86694(6) 0.0496(3) Uani 1 1 d . . .
O2 O 1.02431(11) -0.05064(10) 0.80973(5) 0.0389(2) Uani 1 1 d . . .
H2 H 0.9853 -0.1177 0.8275 0.058 Uiso 1 1 calc R . .
O3 O 0.65304(11) 0.08340(10) 0.69237(5) 0.0429(2) Uani 1 1 d . . .
O4 O 0.52422(13) 0.11748(11) 0.83453(6) 0.0520(3) Uani 1 1 d . . .
Cl1 Cl 1.14863(6) 0.34617(5) 0.98213(2) 0.06756(15) Uani 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
C1 O1 1.2164(19) . ?
C1 C2 1.467(2) . ?
C1 C12 1.554(2) . ?
C2 C3 1.380(2) . ?
C2 C11 1.400(2) . ?
C3 C4 1.408(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.364(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.415(2) . ?
C5 H5 0.9300 . ?
C6 C11 1.407(2) . ?
C6 C7 1.412(3) . ?
C7 C8 1.363(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.425(2) . ?
C8 H8 0.9300 . ?
C9 C10 1.362(2) . ?
C9 H9 0.9300 . ?
C10 C11 1.410(2) . ?
C10 C12 1.524(2) . ?
C12 C13 1.5593(19) . ?
C12 C42 1.5771(19) . ?
C13 C14 1.5288(19) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 O2 1.4244(16) . ?
C14 C15 1.5213(19) . ?
C14 C27 1.5781(19) . ?
C15 C16 1.388(2) . ?
C15 C20 1.391(2) . ?
C16 C17 1.384(2) . ?
C16 H16 0.9300 . ?
C17 C18 1.389(2) . ?
C17 H17 0.9300 . ?
C18 C19 1.391(2) . ?
C18 C21 1.486(2) . ?
C19 C20 1.381(2) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C26 1.383(2) . ?
C21 C22 1.394(2) . ?
C22 C23 1.382(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.372(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.375(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.389(3) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 C28 1.5069(18) . ?
C27 C34 1.5428(19) . ?
C27 C42 1.5455(18) . ?
C28 C29 1.380(2) . ?
C28 C33 1.394(2) . ?
C29 C30 1.391(2) . ?
C29 H29 0.9300 . ?
C30 C31 1.375(2) . ?
C30 Cl1 1.7413(16) . ?
C31 C32 1.389(2) . ?
C31 H31 0.9300 . ?
C32 C33 1.383(2) . ?
C32 H32 0.9300 . ?
C33 N1 1.3986(18) . ?
C34 O3 1.2137(17) . ?
C34 N1 1.3666(18) . ?
C35 N1 1.4496(19) . ?
C35 C36 1.507(2) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 C37 1.378(3) . ?
C36 C41 1.385(2) . ?
C37 C38 1.387(3) . ?
C37 H37 0.9300 . ?
C38 C39 1.360(3) . ?
C38 H38 0.9300 . ?
C39 C40 1.367(4) . ?
C39 H39 0.9300 . ?
C40 C41 1.387(3) . ?
C40 H40 0.9300 . ?
C41 H41 0.9300 . ?
C42 C43 1.516(2) . ?
C42 H42 0.9800 . ?
C43 O4 1.2083(18) . ?
C43 C44 1.4921(19) . ?
C44 C49 1.387(2) . ?
C44 C45 1.387(2) . ?
C45 C46 1.378(3) . ?
C45 H45 0.9300 . ?
C46 C47 1.373(3) . ?
C46 H46 0.9300 . ?
C47 C48 1.366(3) . ?
C47 H47 0.9300 . ?
C48 C49 1.383(2) . ?
C48 H48 0.9300 . ?
C49 H49 0.9300 . ?
O2 H2 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 128.00(14) . . ?
O1 C1 C12 123.38(13) . . ?
C2 C1 C12 108.53(13) . . ?
C3 C2 C11 120.20(15) . . ?
C3 C2 C1 132.71(16) . . ?
C11 C2 C1 107.09(13) . . ?
C2 C3 C4 117.45(18) . . ?
C2 C3 H3 121.3 . . ?
C4 C3 H3 121.3 . . ?
C5 C4 C3 122.41(16) . . ?
C5 C4 H4 118.8 . . ?
C3 C4 H4 118.8 . . ?
C4 C5 C6 121.57(16) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C11 C6 C7 116.48(15) . . ?
C11 C6 C5 115.31(17) . . ?
C7 C6 C5 128.21(16) . . ?
C8 C7 C6 120.10(15) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C9 122.51(16) . . ?
C7 C8 H8 118.7 . . ?
C9 C8 H8 118.7 . . ?
C10 C9 C8 118.83(15) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 H9 120.6 . . ?
C9 C10 C11 118.62(13) . . ?
C9 C10 C12 133.29(13) . . ?
C11 C10 C12 108.09(12) . . ?
C2 C11 C6 122.94(14) . . ?
C2 C11 C10 113.67(13) . . ?
C6 C11 C10 123.39(15) . . ?
C10 C12 C1 102.46(11) . . ?
C10 C12 C13 113.72(11) . . ?
C1 C12 C13 108.73(11) . . ?
C10 C12 C42 117.32(11) . . ?
C1 C12 C42 111.25(11) . . ?
C13 C12 C42 103.35(10) . . ?
C14 C13 C12 106.53(11) . . ?
C14 C13 H13A 110.4 . . ?
C12 C13 H13A 110.4 . . ?
C14 C13 H13B 110.4 . . ?
C12 C13 H13B 110.4 . . ?
H13A C13 H13B 108.6 . . ?
O2 C14 C15 106.73(11) . . ?
O2 C14 C13 110.94(11) . . ?
C15 C14 C13 114.84(11) . . ?
O2 C14 C27 107.38(10) . . ?
C15 C14 C27 115.00(11) . . ?
C13 C14 C27 101.77(11) . . ?
C16 C15 C20 117.46(13) . . ?
C16 C15 C14 122.75(12) . . ?
C20 C15 C14 119.76(12) . . ?
C17 C16 C15 121.02(14) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C16 C17 C18 121.61(14) . . ?
C16 C17 H17 119.2 . . ?
C18 C17 H17 119.2 . . ?
C17 C18 C19 117.17(13) . . ?
C17 C18 C21 120.97(14) . . ?
C19 C18 C21 121.85(14) . . ?
C20 C19 C18 121.29(14) . . ?
C20 C19 H19 119.4 . . ?
C18 C19 H19 119.4 . . ?
C19 C20 C15 121.34(14) . . ?
C19 C20 H20 119.3 . . ?
C15 C20 H20 119.3 . . ?
C26 C21 C22 118.36(15) . . ?
C26 C21 C18 121.47(15) . . ?
C22 C21 C18 120.17(15) . . ?
C23 C22 C21 120.76(18) . . ?
C23 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
C24 C23 C22 120.2(2) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 119.83(18) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C24 C25 C26 120.3(2) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C21 C26 C25 120.54(19) . . ?
C21 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
C28 C27 C34 101.88(11) . . ?
C28 C27 C42 114.82(11) . . ?
C34 C27 C42 114.73(11) . . ?
C28 C27 C14 115.19(11) . . ?
C34 C27 C14 110.11(11) . . ?
C42 C27 C14 100.61(10) . . ?
C29 C28 C33 119.87(12) . . ?
C29 C28 C27 131.31(12) . . ?
C33 C28 C27 108.79(12) . . ?
C28 C29 C30 117.86(14) . . ?
C28 C29 H29 121.1 . . ?
C30 C29 H29 121.1 . . ?
C31 C30 C29 122.36(14) . . ?
C31 C30 Cl1 119.36(12) . . ?
C29 C30 Cl1 118.27(12) . . ?
C30 C31 C32 119.99(13) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C33 C32 C31 117.94(14) . . ?
C33 C32 H32 121.0 . . ?
C31 C32 H32 121.0 . . ?
C32 C33 C28 121.97(13) . . ?
C32 C33 N1 128.17(13) . . ?
C28 C33 N1 109.85(11) . . ?
O3 C34 N1 124.53(13) . . ?
O3 C34 C27 127.31(12) . . ?
N1 C34 C27 108.06(11) . . ?
N1 C35 C36 114.96(13) . . ?
N1 C35 H35A 108.5 . . ?
C36 C35 H35A 108.5 . . ?
N1 C35 H35B 108.5 . . ?
C36 C35 H35B 108.5 . . ?
H35A C35 H35B 107.5 . . ?
C37 C36 C41 118.74(16) . . ?
C37 C36 C35 122.50(14) . . ?
C41 C36 C35 118.69(16) . . ?
C36 C37 C38 120.30(18) . . ?
C36 C37 H37 119.8 . . ?
C38 C37 H37 119.8 . . ?
C39 C38 C37 120.6(2) . . ?
C39 C38 H38 119.7 . . ?
C37 C38 H38 119.7 . . ?
C38 C39 C40 119.76(19) . . ?
C38 C39 H39 120.1 . . ?
C40 C39 H39 120.1 . . ?
C39 C40 C41 120.5(2) . . ?
C39 C40 H40 119.8 . . ?
C41 C40 H40 119.8 . . ?
C36 C41 C40 120.1(2) . . ?
C36 C41 H41 119.9 . . ?
C40 C41 H41 119.9 . . ?
C43 C42 C27 116.73(11) . . ?
C43 C42 C12 113.37(10) . . ?
C27 C42 C12 107.12(10) . . ?
C43 C42 H42 106.3 . . ?
C27 C42 H42 106.3 . . ?
C12 C42 H42 106.3 . . ?
O4 C43 C44 121.95(13) . . ?
O4 C43 C42 121.02(12) . . ?
C44 C43 C42 116.99(12) . . ?
C49 C44 C45 118.79(14) . . ?
C49 C44 C43 122.51(13) . . ?
C45 C44 C43 118.68(14) . . ?
C46 C45 C44 120.38(17) . . ?
C46 C45 H45 119.8 . . ?
C44 C45 H45 119.8 . . ?
C47 C46 C45 120.20(18) . . ?
C47 C46 H46 119.9 . . ?
C45 C46 H46 119.9 . . ?
C48 C47 C46 120.08(17) . . ?
C48 C47 H47 120.0 . . ?
C46 C47 H47 120.0 . . ?
C47 C48 C49 120.28(18) . . ?
C47 C48 H48 119.9 . . ?
C49 C48 H48 119.9 . . ?
C48 C49 C44 120.25(16) . . ?
C48 C49 H49 119.9 . . ?
C44 C49 H49 119.9 . . ?
C34 N1 C33 111.24(11) . . ?
C34 N1 C35 122.48(12) . . ?
C33 N1 C35 125.72(12) . . ?
C14 O2 H2 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
O1 C1 C2 C3 1.5(3) . . . . ?
C12 C1 C2 C3 178.21(16) . . . . ?
O1 C1 C2 C11 -177.70(15) . . . . ?
C12 C1 C2 C11 -0.96(15) . . . . ?
C11 C2 C3 C4 2.4(2) . . . . ?
C1 C2 C3 C4 -176.69(16) . . . . ?
C2 C3 C4 C5 -1.6(3) . . . . ?
C3 C4 C5 C6 -1.5(3) . . . . ?
C4 C5 C6 C11 3.6(2) . . . . ?
C4 C5 C6 C7 -176.01(17) . . . . ?
C11 C6 C7 C8 -0.2(2) . . . . ?
C5 C6 C7 C8 179.45(17) . . . . ?
C6 C7 C8 C9 1.9(3) . . . . ?
C7 C8 C9 C10 -1.3(2) . . . . ?
C8 C9 C10 C11 -1.0(2) . . . . ?
C8 C9 C10 C12 178.97(14) . . . . ?
C3 C2 C11 C6 -0.1(2) . . . . ?
C1 C2 C11 C6 179.19(13) . . . . ?
C3 C2 C11 C10 178.97(14) . . . . ?
C1 C2 C11 C10 -1.74(17) . . . . ?
C7 C6 C11 C2 176.81(14) . . . . ?
C5 C6 C11 C2 -2.9(2) . . . . ?
C7 C6 C11 C10 -2.2(2) . . . . ?
C5 C6 C11 C10 178.15(14) . . . . ?
C9 C10 C11 C2 -176.27(13) . . . . ?
C12 C10 C11 C2 3.75(16) . . . . ?
C9 C10 C11 C6 2.8(2) . . . . ?
C12 C10 C11 C6 -177.19(13) . . . . ?
C9 C10 C12 C1 176.09(15) . . . . ?
C11 C10 C12 C1 -3.93(14) . . . . ?
C9 C10 C12 C13 -66.8(2) . . . . ?
C11 C10 C12 C13 113.22(13) . . . . ?
C9 C10 C12 C42 54.0(2) . . . . ?
C11 C10 C12 C42 -126.06(12) . . . . ?
O1 C1 C12 C10 179.89(13) . . . . ?
C2 C1 C12 C10 2.97(14) . . . . ?
O1 C1 C12 C13 59.23(17) . . . . ?
C2 C1 C12 C13 -117.69(12) . . . . ?
O1 C1 C12 C42 -53.94(18) . . . . ?
C2 C1 C12 C42 129.14(12) . . . . ?
C10 C12 C13 C14 145.88(11) . . . . ?
C1 C12 C13 C14 -100.67(13) . . . . ?
C42 C12 C13 C14 17.61(13) . . . . ?
C12 C13 C14 O2 74.70(13) . . . . ?
C12 C13 C14 C15 -164.19(11) . . . . ?
C12 C13 C14 C27 -39.29(13) . . . . ?
O2 C14 C15 C16 151.29(14) . . . . ?
C13 C14 C15 C16 27.90(19) . . . . ?
C27 C14 C15 C16 -89.74(16) . . . . ?
O2 C14 C15 C20 -26.79(17) . . . . ?
C13 C14 C15 C20 -150.18(13) . . . . ?
C27 C14 C15 C20 92.18(16) . . . . ?
C20 C15 C16 C17 2.4(2) . . . . ?
C14 C15 C16 C17 -175.75(15) . . . . ?
C15 C16 C17 C18 0.1(3) . . . . ?
C16 C17 C18 C19 -2.7(3) . . . . ?
C16 C17 C18 C21 176.04(16) . . . . ?
C17 C18 C19 C20 2.9(2) . . . . ?
C21 C18 C19 C20 -175.81(15) . . . . ?
C18 C19 C20 C15 -0.5(2) . . . . ?
C16 C15 C20 C19 -2.2(2) . . . . ?
C14 C15 C20 C19 176.02(14) . . . . ?
C17 C18 C21 C26 140.67(18) . . . . ?
C19 C18 C21 C26 -40.7(2) . . . . ?
C17 C18 C21 C22 -40.6(2) . . . . ?
C19 C18 C21 C22 138.08(18) . . . . ?
C26 C21 C22 C23 -0.3(3) . . . . ?
C18 C21 C22 C23 -179.06(17) . . . . ?
C21 C22 C23 C24 0.6(3) . . . . ?
C22 C23 C24 C25 -0.3(4) . . . . ?
C23 C24 C25 C26 -0.4(4) . . . . ?
C22 C21 C26 C25 -0.4(3) . . . . ?
C18 C21 C26 C25 178.39(18) . . . . ?
C24 C25 C26 C21 0.7(3) . . . . ?
O2 C14 C27 C28 52.33(14) . . . . ?
C15 C14 C27 C28 -66.27(15) . . . . ?
C13 C14 C27 C28 168.93(11) . . . . ?
O2 C14 C27 C34 166.82(10) . . . . ?
C15 C14 C27 C34 48.22(14) . . . . ?
C13 C14 C27 C34 -76.57(12) . . . . ?
O2 C14 C27 C42 -71.73(12) . . . . ?
C15 C14 C27 C42 169.67(11) . . . . ?
C13 C14 C27 C42 44.88(12) . . . . ?
C34 C27 C28 C29 176.05(14) . . . . ?
C42 C27 C28 C29 51.42(19) . . . . ?
C14 C27 C28 C29 -64.79(18) . . . . ?
C34 C27 C28 C33 -2.19(13) . . . . ?
C42 C27 C28 C33 -126.82(12) . . . . ?
C14 C27 C28 C33 116.97(12) . . . . ?
C33 C28 C29 C30 0.5(2) . . . . ?
C27 C28 C29 C30 -177.55(13) . . . . ?
C28 C29 C30 C31 -0.1(2) . . . . ?
C28 C29 C30 Cl1 178.32(10) . . . . ?
C29 C30 C31 C32 -0.8(2) . . . . ?
Cl1 C30 C31 C32 -179.23(11) . . . . ?
C30 C31 C32 C33 1.3(2) . . . . ?
C31 C32 C33 C28 -0.9(2) . . . . ?
C31 C32 C33 N1 177.55(13) . . . . ?
C29 C28 C33 C32 0.0(2) . . . . ?
C27 C28 C33 C32 178.48(12) . . . . ?
C29 C28 C33 N1 -178.71(12) . . . . ?
C27 C28 C33 N1 -0.23(15) . . . . ?
C28 C27 C34 O3 -179.59(14) . . . . ?
C42 C27 C34 O3 -54.90(18) . . . . ?
C14 C27 C34 O3 57.71(17) . . . . ?
C28 C27 C34 N1 3.94(13) . . . . ?
C42 C27 C34 N1 128.63(12) . . . . ?
C14 C27 C34 N1 -118.76(12) . . . . ?
N1 C35 C36 C37 25.9(2) . . . . ?
N1 C35 C36 C41 -157.30(15) . . . . ?
C41 C36 C37 C38 0.3(3) . . . . ?
C35 C36 C37 C38 177.09(17) . . . . ?
C36 C37 C38 C39 0.0(3) . . . . ?
C37 C38 C39 C40 -0.6(3) . . . . ?
C38 C39 C40 C41 0.8(3) . . . . ?
C37 C36 C41 C40 -0.1(3) . . . . ?
C35 C36 C41 C40 -177.01(17) . . . . ?
C39 C40 C41 C36 -0.4(3) . . . . ?
C28 C27 C42 C43 72.69(15) . . . . ?
C34 C27 C42 C43 -44.88(16) . . . . ?
C14 C27 C42 C43 -163.00(11) . . . . ?
C28 C27 C42 C12 -159.02(11) . . . . ?
C34 C27 C42 C12 83.42(13) . . . . ?
C14 C27 C42 C12 -34.71(12) . . . . ?
C10 C12 C42 C43 15.65(16) . . . . ?
C1 C12 C42 C43 -101.83(13) . . . . ?
C13 C12 C42 C43 141.65(11) . . . . ?
C10 C12 C42 C27 -114.57(12) . . . . ?
C1 C12 C42 C27 127.95(12) . . . . ?
C13 C12 C42 C27 11.43(13) . . . . ?
C27 C42 C43 O4 9.68(19) . . . . ?
C12 C42 C43 O4 -115.53(15) . . . . ?
C27 C42 C43 C44 -172.50(11) . . . . ?
C12 C42 C43 C44 62.29(15) . . . . ?
O4 C43 C44 C49 -151.92(15) . . . . ?
C42 C43 C44 C49 30.27(19) . . . . ?
O4 C43 C44 C45 29.5(2) . . . . ?
C42 C43 C44 C45 -148.31(15) . . . . ?
C49 C44 C45 C46 -1.7(3) . . . . ?
C43 C44 C45 C46 176.94(18) . . . . ?
C44 C45 C46 C47 1.0(3) . . . . ?
C45 C46 C47 C48 0.5(4) . . . . ?
C46 C47 C48 C49 -1.3(3) . . . . ?
C47 C48 C49 C44 0.6(3) . . . . ?
C45 C44 C49 C48 0.9(2) . . . . ?
C43 C44 C49 C48 -177.67(15) . . . . ?
O3 C34 N1 C33 179.01(13) . . . . ?
C27 C34 N1 C33 -4.39(15) . . . . ?
O3 C34 N1 C35 7.1(2) . . . . ?
C27 C34 N1 C35 -176.25(12) . . . . ?
C32 C33 N1 C34 -175.61(13) . . . . ?
C28 C33 N1 C34 3.00(16) . . . . ?
C32 C33 N1 C35 -4.1(2) . . . . ?
C28 C33 N1 C35 174.55(13) . . . . ?
C36 C35 N1 C34 -117.54(15) . . . . ?
C36 C35 N1 C33 71.80(19) . . . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        26.61
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.034
####################################################################### 
# 
# 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_ksd3
_database_code_depnum_ccdc_archive 'CCDC 1041758'
_audit_update_record             
;
2015-01-01 deposited with the CCDC.
2015-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C51 H38 F2 N4 O4'
_chemical_formula_weight         808.85

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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. 
;

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

_cell_length_a                   11.9700(5)
_cell_length_b                   15.5516(8)
_cell_length_c                   23.1725(11)
_cell_angle_alpha                90
_cell_angle_beta                 103.1855(19)
_cell_angle_gamma                90
_cell_volume                     4199.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7458
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      21.91

_exptl_crystal_description       Rectangular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_F_000             1688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.088
_shelx_estimated_absorpt_T_min   0.970
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18978
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.590
_diffrn_reflns_theta_max         21.936
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.669
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.669
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.669
_reflns_number_total             5092
_reflns_number_gt                4010
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0641P)²+2.6923P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5092
_refine_ls_number_parameters     558
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0470
_refine_ls_wR_factor_ref         0.1361
_refine_ls_wR_factor_gt          0.1222
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_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_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 0.0653(2) 0.44899(17) 0.86900(11) 0.0325(7) Uani 1 1 d . . . . .
C2 C 0.0251(2) 0.36709(18) 0.89878(11) 0.0336(7) Uani 1 1 d . . . . .
H2 H 0.0050 0.3224 0.8684 0.040 Uiso 1 1 calc R U . . .
C3 C 0.1312(2) 0.33616(18) 0.94520(11) 0.0324(7) Uani 1 1 d . . . . .
C4 C 0.2315(2) 0.35240(17) 0.91292(11) 0.0301(6) Uani 1 1 d . . . . .
C5 C 0.2006(2) 0.44162(17) 0.88449(12) 0.0321(7) Uani 1 1 d . . . . .
H5 H 0.2287 0.4840 0.9158 0.038 Uiso 1 1 calc R U . . .
C6 C 0.2575(2) 0.46328(19) 0.83434(13) 0.0394(7) Uani 1 1 d . . . . .
C7 C 0.2369(2) 0.5500(2) 0.80627(15) 0.0523(9) Uani 1 1 d . . . . .
C8 C 0.2385(3) 0.5570(3) 0.74723(18) 0.0855(13) Uani 1 1 d . . . . .
H8 H 0.2555 0.5096 0.7264 0.103 Uiso 1 1 calc R U . . .
C9 C 0.2140(5) 0.6370(5) 0.7189(3) 0.121(2) Uani 1 1 d . . . . .
H9 H 0.2133 0.6429 0.6789 0.145 Uiso 1 1 calc R U . . .
C10 C 0.1914(5) 0.7062(5) 0.7509(4) 0.124(2) Uani 1 1 d . . . . .
H10 H 0.1740 0.7588 0.7319 0.148 Uiso 1 1 calc R U . . .
C11 C 0.1935(3) 0.7003(3) 0.8089(3) 0.0983(17) Uani 1 1 d . . . . .
H11 H 0.1805 0.7488 0.8299 0.118 Uiso 1 1 calc R U . . .
C12 C 0.2151(3) 0.6221(2) 0.83729(19) 0.0646(10) Uani 1 1 d . . . . .
H12 H 0.2151 0.6176 0.8773 0.077 Uiso 1 1 calc R U . . .
C13 C 0.0094(2) 0.46098(18) 0.80464(12) 0.0351(7) Uani 1 1 d . . . . .
C14 C 0.0088(2) 0.4097(2) 0.75620(13) 0.0432(8) Uani 1 1 d . . . . .
H14 H 0.0450 0.3564 0.7601 0.052 Uiso 1 1 calc R U . . .
C15 C -0.0479(3) 0.4406(2) 0.70171(13) 0.0545(9) Uani 1 1 d . . . . .
C16 C -0.1013(3) 0.5191(3) 0.69391(15) 0.0629(10) Uani 1 1 d . . . . .
H16 H -0.1378 0.5377 0.6562 0.076 Uiso 1 1 calc R U . . .
C17 C -0.1003(3) 0.5703(2) 0.74265(15) 0.0554(9) Uani 1 1 d . . . . .
H17 H -0.1353 0.6240 0.7385 0.066 Uiso 1 1 calc R U . . .
C18 C -0.0466(2) 0.53988(19) 0.79725(13) 0.0400(7) Uani 1 1 d . . . . .
C19 C 0.0313(2) 0.53171(19) 0.89628(13) 0.0385(7) Uani 1 1 d . . . . .
C20 C -0.0738(3) 0.6664(2) 0.86291(16) 0.0561(9) Uani 1 1 d . . . . .
H20A H -0.0329 0.7068 0.8434 0.067 Uiso 1 1 calc R U . . .
H20B H -0.0535 0.6788 0.9050 0.067 Uiso 1 1 calc R U . . .
C21 C -0.2009(3) 0.6806(2) 0.84036(13) 0.0454(8) Uani 1 1 d . . . . .
C22 C -0.2401(3) 0.7577(2) 0.81335(14) 0.0543(9) Uani 1 1 d . . . . .
H22 H -0.1877 0.7987 0.8070 0.065 Uiso 1 1 calc R U . . .
C23 C -0.3554(3) 0.7743(3) 0.79583(15) 0.0658(10) Uani 1 1 d . . . . .
H23 H -0.3805 0.8265 0.7780 0.079 Uiso 1 1 calc R U . . .
C24 C -0.4328(3) 0.7149(3) 0.80443(16) 0.0710(11) Uani 1 1 d . . . . .
H24 H -0.5109 0.7267 0.7928 0.085 Uiso 1 1 calc R U . . .
C25 C -0.3965(3) 0.6379(3) 0.83014(17) 0.0722(11) Uani 1 1 d . . . . .
H25 H -0.4498 0.5969 0.8355 0.087 Uiso 1 1 calc R U . . .
C26 C -0.2797(3) 0.6207(2) 0.84833(15) 0.0602(9) Uani 1 1 d . . . . .
H26 H -0.2550 0.5682 0.8660 0.072 Uiso 1 1 calc R U . . .
C27 C -0.1820(2) 0.38494(18) 0.89450(13) 0.0384(7) Uani 1 1 d . . . . .
C28 C -0.3088(3) 0.3849(3) 0.80464(16) 0.0728(11) Uani 1 1 d . . . . .
H28 H -0.3226 0.3800 0.7636 0.087 Uiso 1 1 calc R U . . .
C29 C -0.4003(3) 0.4006(2) 0.82948(17) 0.0665(10) Uani 1 1 d . . . . .
H29 H -0.4743 0.4051 0.8061 0.080 Uiso 1 1 calc R U . . .
C30 C -0.3794(3) 0.4096(2) 0.88988(16) 0.0537(9) Uani 1 1 d . . . . .
H30 H -0.4395 0.4211 0.9081 0.064 Uiso 1 1 calc R U . . .
C31 C -0.2698(2) 0.4015(2) 0.92310(14) 0.0468(8) Uani 1 1 d . . . . .
H31 H -0.2543 0.4069 0.9641 0.056 Uiso 1 1 calc R U . . .
C32 C 0.1276(2) 0.24435(18) 0.96618(12) 0.0379(7) Uani 1 1 d . . . . .
C33 C 0.0595(3) 0.1819(2) 0.93277(15) 0.0554(9) Uani 1 1 d . . . . .
H33 H 0.0116 0.1967 0.8966 0.066 Uiso 1 1 calc R U . . .
C34 C 0.0619(3) 0.0978(2) 0.95249(18) 0.0716(11) Uani 1 1 d . . . . .
H34 H 0.0160 0.0565 0.9294 0.086 Uiso 1 1 calc R U . . .
C35 C 0.1312(4) 0.0751(3) 1.00559(19) 0.0761(11) Uani 1 1 d . . . . .
H35 H 0.1324 0.0186 1.0188 0.091 Uiso 1 1 calc R U . . .
C36 C 0.1992(3) 0.1360(3) 1.03949(16) 0.0695(11) Uani 1 1 d . . . . .
H36 H 0.2465 0.1207 1.0757 0.083 Uiso 1 1 calc R U . . .
C37 C 0.1972(3) 0.2202(2) 1.01974(13) 0.0507(8) Uani 1 1 d . . . . .
H37 H 0.2435 0.2610 1.0430 0.061 Uiso 1 1 calc R U . . .
C38 C 0.3493(2) 0.34681(17) 0.95358(12) 0.0320(7) Uani 1 1 d . . . . .
C39 C 0.4012(2) 0.39701(18) 1.00121(12) 0.0390(7) Uani 1 1 d . . . . .
H39 H 0.3636 0.4438 1.0132 0.047 Uiso 1 1 calc R U . . .
C40 C 0.5108(2) 0.3749(2) 1.03017(13) 0.0450(8) Uani 1 1 d . . . . .
C41 C 0.5680(2) 0.3054(2) 1.01479(14) 0.0517(9) Uani 1 1 d . . . . .
H41 H 0.6412 0.2918 1.0366 0.062 Uiso 1 1 calc R U . . .
C42 C 0.5165(2) 0.2555(2) 0.96666(13) 0.0459(8) Uani 1 1 d . . . . .
H42 H 0.5541 0.2085 0.9551 0.055 Uiso 1 1 calc R U . . .
C43 C 0.4076(2) 0.27776(18) 0.93640(12) 0.0350(7) Uani 1 1 d . . . . .
C44 C 0.2363(2) 0.28051(18) 0.86845(12) 0.0335(7) Uani 1 1 d . . . . .
C45 C 0.3826(3) 0.17846(19) 0.84878(13) 0.0449(8) Uani 1 1 d . . . . .
H45A H 0.4544 0.2007 0.8422 0.054 Uiso 1 1 calc R U . . .
H45B H 0.3287 0.1761 0.8106 0.054 Uiso 1 1 calc R U . . .
C46 C 0.4026(3) 0.0887(2) 0.87244(14) 0.0505(8) Uani 1 1 d . . . . .
C47 C 0.3653(3) 0.0595(2) 0.92001(17) 0.0671(10) Uani 1 1 d . . . . .
H47 H 0.3265 0.0966 0.9401 0.080 Uiso 1 1 calc R U . . .
C48 C 0.3844(5) -0.0248(3) 0.9389(2) 0.1040(16) Uani 1 1 d . . . . .
H48 H 0.3591 -0.0440 0.9718 0.125 Uiso 1 1 calc R U . . .
C49 C 0.4400(7) -0.0791(3) 0.9095(3) 0.142(3) Uani 1 1 d . . . . .
H49 H 0.4530 -0.1357 0.9222 0.170 Uiso 1 1 calc R U . . .
C50 C 0.4766(7) -0.0519(4) 0.8622(3) 0.154(3) Uani 1 1 d . . . . .
H50 H 0.5147 -0.0896 0.8421 0.185 Uiso 1 1 calc R U . . .
C51 C 0.4579(5) 0.0316(3) 0.8432(2) 0.1083(18) Uani 1 1 d . . . . .
H51 H 0.4830 0.0499 0.8101 0.130 Uiso 1 1 calc R U . . .
F1 F -0.04871(19) 0.39089(15) 0.65330(8) 0.0841(7) Uani 1 1 d . . . . .
O3 O 0.14823(16) 0.38943(15) 0.99650(8) 0.0402(5) Uani 1 1 d . . . . .
F3 F 0.56438(14) 0.42493(12) 1.07649(8) 0.0659(6) Uani 1 1 d . . . . .
N1 N -0.03533(19) 0.57936(15) 0.85345(11) 0.0436(6) Uani 1 1 d . . . . .
N2 N -0.2002(2) 0.37599(19) 0.83612(12) 0.0558(8) Uani 1 1 d . . . . .
N3 N 0.33923(18) 0.23846(14) 0.88612(10) 0.0368(6) Uani 1 1 d . . . . .
O1 O 0.31866(18) 0.41115(15) 0.81767(9) 0.0542(6) Uani 1 1 d . . . . .
O2 O 0.06364(17) 0.55175(13) 0.94899(9) 0.0501(6) Uani 1 1 d . . . . .
N4 N -0.07041(19) 0.37779(17) 0.92594(12) 0.0424(7) Uani 1 1 d . . . . .
O4 O 0.16145(16) 0.26086(12) 0.82558(8) 0.0415(5) Uani 1 1 d . . . . .
H1N H -0.059(3) 0.391(2) 0.9624(14) 0.051(10) Uiso 1 1 d . . . . .
H1O H 0.127(3) 0.440(2) 0.9875(15) 0.061(12) 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
C1 C13 1.501(4) . ?
C1 C19 1.529(4) . ?
C1 C2 1.575(4) . ?
C1 C5 1.581(4) . ?
C2 N4 1.435(4) . ?
C2 C3 1.542(4) . ?
C2 H2 0.9800 . ?
C3 O3 1.425(3) . ?
C3 C32 1.512(4) . ?
C3 C4 1.573(4) . ?
C4 C38 1.510(4) . ?
C4 C44 1.530(4) . ?
C4 C5 1.544(4) . ?
C5 C6 1.513(4) . ?
C5 H5 0.9800 . ?
C6 O1 1.213(3) . ?
C6 C7 1.493(4) . ?
C7 C8 1.377(5) . ?
C7 C12 1.388(5) . ?
C8 C9 1.406(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.368(8) . ?
C9 H9 0.9300 . ?
C10 C11 1.342(8) . ?
C10 H10 0.9300 . ?
C11 C12 1.379(5) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.376(4) . ?
C13 C18 1.390(4) . ?
C14 C15 1.377(4) . ?
C14 H14 0.9300 . ?
C15 F1 1.361(4) . ?
C15 C16 1.371(5) . ?
C16 C17 1.379(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.366(4) . ?
C17 H17 0.9300 . ?
C18 N1 1.418(4) . ?
C19 O2 1.234(3) . ?
C19 N1 1.345(4) . ?
C20 N1 1.462(4) . ?
C20 C21 1.509(4) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C26 1.367(5) . ?
C21 C22 1.385(4) . ?
C22 C23 1.371(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.355(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.364(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.392(5) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 N2 1.327(4) . ?
C27 N4 1.372(4) . ?
C27 C31 1.389(4) . ?
C28 N2 1.344(4) . ?
C28 C29 1.370(5) . ?
C28 H28 0.9300 . ?
C29 C30 1.372(5) . ?
C29 H29 0.9300 . ?
C30 C31 1.367(4) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C32 C37 1.380(4) . ?
C32 C33 1.385(4) . ?
C33 C34 1.384(5) . ?
C33 H33 0.9300 . ?
C34 C35 1.364(5) . ?
C34 H34 0.9300 . ?
C35 C36 1.372(5) . ?
C35 H35 0.9300 . ?
C36 C37 1.386(5) . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
C38 C39 1.379(4) . ?
C38 C43 1.387(4) . ?
C39 C40 1.374(4) . ?
C39 H39 0.9300 . ?
C40 F3 1.362(3) . ?
C40 C41 1.370(4) . ?
C41 C42 1.383(4) . ?
C41 H41 0.9300 . ?
C42 C43 1.376(4) . ?
C42 H42 0.9300 . ?
C43 N3 1.402(3) . ?
C44 O4 1.215(3) . ?
C44 N3 1.373(3) . ?
C45 N3 1.447(4) . ?
C45 C46 1.499(4) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 C47 1.358(5) . ?
C46 C51 1.374(5) . ?
C47 C48 1.386(6) . ?
C47 H47 0.9300 . ?
C48 C49 1.353(8) . ?
C48 H48 0.9300 . ?
C49 C50 1.339(9) . ?
C49 H49 0.9300 . ?
C50 C51 1.373(7) . ?
C50 H50 0.9300 . ?
C51 H51 0.9300 . ?
O3 H1O 0.84(4) . ?
N4 H1N 0.85(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
C13 C1 C19 101.9(2) . . ?
C13 C1 C2 115.1(2) . . ?
C19 C1 C2 111.2(2) . . ?
C13 C1 C5 115.9(2) . . ?
C19 C1 C5 108.8(2) . . ?
C2 C1 C5 103.97(19) . . ?
N4 C2 C3 110.0(2) . . ?
N4 C2 C1 116.9(2) . . ?
C3 C2 C1 105.8(2) . . ?
N4 C2 H2 107.9 . . ?
C3 C2 H2 107.9 . . ?
C1 C2 H2 107.9 . . ?
O3 C3 C32 106.8(2) . . ?
O3 C3 C2 109.8(2) . . ?
C32 C3 C2 116.1(2) . . ?
O3 C3 C4 108.9(2) . . ?
C32 C3 C4 112.7(2) . . ?
C2 C3 C4 102.4(2) . . ?
C38 C4 C44 101.8(2) . . ?
C38 C4 C5 114.6(2) . . ?
C44 C4 C5 114.3(2) . . ?
C38 C4 C3 113.6(2) . . ?
C44 C4 C3 110.7(2) . . ?
C5 C4 C3 102.3(2) . . ?
C6 C5 C4 115.0(2) . . ?
C6 C5 C1 115.2(2) . . ?
C4 C5 C1 107.1(2) . . ?
C6 C5 H5 106.3 . . ?
C4 C5 H5 106.3 . . ?
C1 C5 H5 106.3 . . ?
O1 C6 C7 121.1(3) . . ?
O1 C6 C5 120.4(3) . . ?
C7 C6 C5 118.5(3) . . ?
C8 C7 C12 119.8(3) . . ?
C8 C7 C6 117.8(4) . . ?
C12 C7 C6 122.4(3) . . ?
C7 C8 C9 119.1(5) . . ?
C7 C8 H8 120.5 . . ?
C9 C8 H8 120.5 . . ?
C10 C9 C8 119.2(6) . . ?
C10 C9 H9 120.4 . . ?
C8 C9 H9 120.4 . . ?
C11 C10 C9 121.9(6) . . ?
C11 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
C10 C11 C12 119.8(6) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C11 C12 C7 120.1(4) . . ?
C11 C12 H12 119.9 . . ?
C7 C12 H12 119.9 . . ?
C14 C13 C18 119.9(3) . . ?
C14 C13 C1 131.1(3) . . ?
C18 C13 C1 109.0(2) . . ?
C13 C14 C15 117.1(3) . . ?
C13 C14 H14 121.5 . . ?
C15 C14 H14 121.5 . . ?
F1 C15 C16 118.8(3) . . ?
F1 C15 C14 117.8(3) . . ?
C16 C15 C14 123.3(3) . . ?
C15 C16 C17 119.3(3) . . ?
C15 C16 H16 120.4 . . ?
C17 C16 H16 120.4 . . ?
C18 C17 C16 118.3(3) . . ?
C18 C17 H17 120.9 . . ?
C16 C17 H17 120.9 . . ?
C17 C18 C13 122.1(3) . . ?
C17 C18 N1 128.8(3) . . ?
C13 C18 N1 109.1(2) . . ?
O2 C19 N1 126.2(3) . . ?
O2 C19 C1 124.7(2) . . ?
N1 C19 C1 109.1(2) . . ?
N1 C20 C21 114.2(3) . . ?
N1 C20 H20A 108.7 . . ?
C21 C20 H20A 108.7 . . ?
N1 C20 H20B 108.7 . . ?
C21 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
C26 C21 C22 118.6(3) . . ?
C26 C21 C20 121.7(3) . . ?
C22 C21 C20 119.6(3) . . ?
C23 C22 C21 120.8(3) . . ?
C23 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
C24 C23 C22 120.3(3) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 120.1(3) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C24 C25 C26 119.9(4) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C21 C26 C25 120.3(3) . . ?
C21 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
N2 C27 N4 116.5(3) . . ?
N2 C27 C31 122.6(3) . . ?
N4 C27 C31 120.8(3) . . ?
N2 C28 C29 123.8(3) . . ?
N2 C28 H28 118.1 . . ?
C29 C28 H28 118.1 . . ?
C28 C29 C30 118.0(3) . . ?
C28 C29 H29 121.0 . . ?
C30 C29 H29 121.0 . . ?
C31 C30 C29 119.5(3) . . ?
C31 C30 H30 120.2 . . ?
C29 C30 H30 120.2 . . ?
C30 C31 C27 118.8(3) . . ?
C30 C31 H31 120.6 . . ?
C27 C31 H31 120.6 . . ?
C37 C32 C33 118.0(3) . . ?
C37 C32 C3 119.4(3) . . ?
C33 C32 C3 122.6(3) . . ?
C34 C33 C32 120.9(3) . . ?
C34 C33 H33 119.6 . . ?
C32 C33 H33 119.6 . . ?
C35 C34 C33 120.3(4) . . ?
C35 C34 H34 119.9 . . ?
C33 C34 H34 119.9 . . ?
C34 C35 C36 119.8(4) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 H35 120.1 . . ?
C35 C36 C37 120.0(3) . . ?
C35 C36 H36 120.0 . . ?
C37 C36 H36 120.0 . . ?
C32 C37 C36 121.1(3) . . ?
C32 C37 H37 119.5 . . ?
C36 C37 H37 119.5 . . ?
C39 C38 C43 120.3(2) . . ?
C39 C38 C4 130.8(2) . . ?
C43 C38 C4 109.0(2) . . ?
C40 C39 C38 117.0(3) . . ?
C40 C39 H39 121.5 . . ?
C38 C39 H39 121.5 . . ?
F3 C40 C41 118.8(2) . . ?
F3 C40 C39 117.8(3) . . ?
C41 C40 C39 123.3(3) . . ?
C40 C41 C42 119.6(3) . . ?
C40 C41 H41 120.2 . . ?
C42 C41 H41 120.2 . . ?
C43 C42 C41 117.8(3) . . ?
C43 C42 H42 121.1 . . ?
C41 C42 H42 121.1 . . ?
C42 C43 C38 121.9(3) . . ?
C42 C43 N3 128.3(3) . . ?
C38 C43 N3 109.9(2) . . ?
O4 C44 N3 124.6(3) . . ?
O4 C44 C4 126.9(2) . . ?
N3 C44 C4 108.4(2) . . ?
N3 C45 C46 115.5(3) . . ?
N3 C45 H45A 108.4 . . ?
C46 C45 H45A 108.4 . . ?
N3 C45 H45B 108.4 . . ?
C46 C45 H45B 108.4 . . ?
H45A C45 H45B 107.5 . . ?
C47 C46 C51 117.9(4) . . ?
C47 C46 C45 123.6(3) . . ?
C51 C46 C45 118.4(3) . . ?
C46 C47 C48 120.8(4) . . ?
C46 C47 H47 119.6 . . ?
C48 C47 H47 119.6 . . ?
C49 C48 C47 119.8(5) . . ?
C49 C48 H48 120.1 . . ?
C47 C48 H48 120.1 . . ?
C50 C49 C48 120.4(5) . . ?
C50 C49 H49 119.8 . . ?
C48 C49 H49 119.8 . . ?
C49 C50 C51 120.0(5) . . ?
C49 C50 H50 120.0 . . ?
C51 C50 H50 120.0 . . ?
C50 C51 C46 121.1(5) . . ?
C50 C51 H51 119.5 . . ?
C46 C51 H51 119.5 . . ?
C3 O3 H1O 111(2) . . ?
C19 N1 C18 110.8(2) . . ?
C19 N1 C20 123.6(3) . . ?
C18 N1 C20 124.8(2) . . ?
C27 N2 C28 117.1(3) . . ?
C44 N3 C43 110.7(2) . . ?
C44 N3 C45 123.3(2) . . ?
C43 N3 C45 123.9(2) . . ?
C27 N4 C2 123.6(3) . . ?
C27 N4 H1N 116(2) . . ?
C2 N4 H1N 120(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C13 C1 C2 N4 -90.7(3) . . . . ?
C19 C1 C2 N4 24.5(3) . . . . ?
C5 C1 C2 N4 141.5(2) . . . . ?
C13 C1 C2 C3 146.4(2) . . . . ?
C19 C1 C2 C3 -98.3(2) . . . . ?
C5 C1 C2 C3 18.6(3) . . . . ?
N4 C2 C3 O3 -49.6(3) . . . . ?
C1 C2 C3 O3 77.4(3) . . . . ?
N4 C2 C3 C32 71.6(3) . . . . ?
C1 C2 C3 C32 -161.3(2) . . . . ?
N4 C2 C3 C4 -165.2(2) . . . . ?
C1 C2 C3 C4 -38.1(2) . . . . ?
O3 C3 C4 C38 50.4(3) . . . . ?
C32 C3 C4 C38 -67.9(3) . . . . ?
C2 C3 C4 C38 166.7(2) . . . . ?
O3 C3 C4 C44 164.2(2) . . . . ?
C32 C3 C4 C44 45.9(3) . . . . ?
C2 C3 C4 C44 -79.5(2) . . . . ?
O3 C3 C4 C5 -73.6(2) . . . . ?
C32 C3 C4 C5 168.0(2) . . . . ?
C2 C3 C4 C5 42.6(2) . . . . ?
C38 C4 C5 C6 75.7(3) . . . . ?
C44 C4 C5 C6 -41.3(3) . . . . ?
C3 C4 C5 C6 -160.9(2) . . . . ?
C38 C4 C5 C1 -154.8(2) . . . . ?
C44 C4 C5 C1 88.2(3) . . . . ?
C3 C4 C5 C1 -31.4(2) . . . . ?
C13 C1 C5 C6 10.4(3) . . . . ?
C19 C1 C5 C6 -103.6(3) . . . . ?
C2 C1 C5 C6 137.7(2) . . . . ?
C13 C1 C5 C4 -118.9(2) . . . . ?
C19 C1 C5 C4 127.0(2) . . . . ?
C2 C1 C5 C4 8.4(3) . . . . ?
C4 C5 C6 O1 2.6(4) . . . . ?
C1 C5 C6 O1 -122.8(3) . . . . ?
C4 C5 C6 C7 -177.1(2) . . . . ?
C1 C5 C6 C7 57.5(3) . . . . ?
O1 C6 C7 C8 30.9(4) . . . . ?
C5 C6 C7 C8 -149.4(3) . . . . ?
O1 C6 C7 C12 -150.0(3) . . . . ?
C5 C6 C7 C12 29.7(4) . . . . ?
C12 C7 C8 C9 -2.1(5) . . . . ?
C6 C7 C8 C9 177.0(4) . . . . ?
C7 C8 C9 C10 1.2(7) . . . . ?
C8 C9 C10 C11 1.0(9) . . . . ?
C9 C10 C11 C12 -2.3(8) . . . . ?
C10 C11 C12 C7 1.3(6) . . . . ?
C8 C7 C12 C11 0.9(5) . . . . ?
C6 C7 C12 C11 -178.2(3) . . . . ?
C19 C1 C13 C14 179.0(3) . . . . ?
C2 C1 C13 C14 -60.5(4) . . . . ?
C5 C1 C13 C14 61.0(4) . . . . ?
C19 C1 C13 C18 0.6(3) . . . . ?
C2 C1 C13 C18 121.1(3) . . . . ?
C5 C1 C13 C18 -117.3(3) . . . . ?
C18 C13 C14 C15 0.6(4) . . . . ?
C1 C13 C14 C15 -177.6(3) . . . . ?
C13 C14 C15 F1 179.5(3) . . . . ?
C13 C14 C15 C16 0.8(5) . . . . ?
F1 C15 C16 C17 -179.5(3) . . . . ?
C14 C15 C16 C17 -0.8(5) . . . . ?
C15 C16 C17 C18 -0.6(5) . . . . ?
C16 C17 C18 C13 2.0(5) . . . . ?
C16 C17 C18 N1 -179.1(3) . . . . ?
C14 C13 C18 C17 -2.1(4) . . . . ?
C1 C13 C18 C17 176.5(3) . . . . ?
C14 C13 C18 N1 178.9(2) . . . . ?
C1 C13 C18 N1 -2.5(3) . . . . ?
C13 C1 C19 O2 -176.3(3) . . . . ?
C2 C1 C19 O2 60.5(3) . . . . ?
C5 C1 C19 O2 -53.4(3) . . . . ?
C13 C1 C19 N1 1.6(3) . . . . ?
C2 C1 C19 N1 -121.6(2) . . . . ?
C5 C1 C19 N1 124.4(2) . . . . ?
N1 C20 C21 C26 42.0(4) . . . . ?
N1 C20 C21 C22 -141.1(3) . . . . ?
C26 C21 C22 C23 1.1(5) . . . . ?
C20 C21 C22 C23 -175.9(3) . . . . ?
C21 C22 C23 C24 -0.4(5) . . . . ?
C22 C23 C24 C25 -0.6(6) . . . . ?
C23 C24 C25 C26 0.9(6) . . . . ?
C22 C21 C26 C25 -0.7(5) . . . . ?
C20 C21 C26 C25 176.2(3) . . . . ?
C24 C25 C26 C21 -0.2(6) . . . . ?
N2 C28 C29 C30 1.4(6) . . . . ?
C28 C29 C30 C31 -0.9(5) . . . . ?
C29 C30 C31 C27 0.5(5) . . . . ?
N2 C27 C31 C30 -0.6(5) . . . . ?
N4 C27 C31 C30 178.8(3) . . . . ?
O3 C3 C32 C37 -35.8(3) . . . . ?
C2 C3 C32 C37 -158.6(3) . . . . ?
C4 C3 C32 C37 83.8(3) . . . . ?
O3 C3 C32 C33 146.4(3) . . . . ?
C2 C3 C32 C33 23.6(4) . . . . ?
C4 C3 C32 C33 -94.0(3) . . . . ?
C37 C32 C33 C34 -0.3(5) . . . . ?
C3 C32 C33 C34 177.5(3) . . . . ?
C32 C33 C34 C35 0.4(6) . . . . ?
C33 C34 C35 C36 -0.2(6) . . . . ?
C34 C35 C36 C37 0.0(6) . . . . ?
C33 C32 C37 C36 0.1(5) . . . . ?
C3 C32 C37 C36 -177.8(3) . . . . ?
C35 C36 C37 C32 0.0(5) . . . . ?
C44 C4 C38 C39 176.4(3) . . . . ?
C5 C4 C38 C39 52.5(4) . . . . ?
C3 C4 C38 C39 -64.6(4) . . . . ?
C44 C4 C38 C43 -3.7(3) . . . . ?
C5 C4 C38 C43 -127.6(2) . . . . ?
C3 C4 C38 C43 115.3(2) . . . . ?
C43 C38 C39 C40 -0.4(4) . . . . ?
C4 C38 C39 C40 179.4(3) . . . . ?
C38 C39 C40 F3 178.5(2) . . . . ?
C38 C39 C40 C41 -1.5(5) . . . . ?
F3 C40 C41 C42 -177.9(3) . . . . ?
C39 C40 C41 C42 2.2(5) . . . . ?
C40 C41 C42 C43 -0.8(5) . . . . ?
C41 C42 C43 C38 -1.1(4) . . . . ?
C41 C42 C43 N3 178.7(3) . . . . ?
C39 C38 C43 C42 1.8(4) . . . . ?
C4 C38 C43 C42 -178.1(3) . . . . ?
C39 C38 C43 N3 -178.1(2) . . . . ?
C4 C38 C43 N3 2.0(3) . . . . ?
C38 C4 C44 O4 -178.0(3) . . . . ?
C5 C4 C44 O4 -53.9(4) . . . . ?
C3 C4 C44 O4 61.0(3) . . . . ?
C38 C4 C44 N3 4.2(3) . . . . ?
C5 C4 C44 N3 128.3(2) . . . . ?
C3 C4 C44 N3 -116.8(2) . . . . ?
N3 C45 C46 C47 11.1(5) . . . . ?
N3 C45 C46 C51 -171.4(3) . . . . ?
C51 C46 C47 C48 1.1(6) . . . . ?
C45 C46 C47 C48 178.6(3) . . . . ?
C46 C47 C48 C49 -0.5(7) . . . . ?
C47 C48 C49 C50 -0.1(10) . . . . ?
C48 C49 C50 C51 0.1(12) . . . . ?
C49 C50 C51 C46 0.5(10) . . . . ?
C47 C46 C51 C50 -1.1(7) . . . . ?
C45 C46 C51 C50 -178.7(5) . . . . ?
O2 C19 N1 C18 174.6(3) . . . . ?
C1 C19 N1 C18 -3.2(3) . . . . ?
O2 C19 N1 C20 4.2(5) . . . . ?
C1 C19 N1 C20 -173.7(3) . . . . ?
C17 C18 N1 C19 -175.3(3) . . . . ?
C13 C18 N1 C19 3.7(3) . . . . ?
C17 C18 N1 C20 -4.9(5) . . . . ?
C13 C18 N1 C20 174.0(3) . . . . ?
C21 C20 N1 C19 -130.2(3) . . . . ?
C21 C20 N1 C18 60.7(4) . . . . ?
N4 C27 N2 C28 -178.5(3) . . . . ?
C31 C27 N2 C28 1.0(5) . . . . ?
C29 C28 N2 C27 -1.4(6) . . . . ?
O4 C44 N3 C43 178.9(3) . . . . ?
C4 C44 N3 C43 -3.3(3) . . . . ?
O4 C44 N3 C45 14.8(4) . . . . ?
C4 C44 N3 C45 -167.4(2) . . . . ?
C42 C43 N3 C44 -179.0(3) . . . . ?
C38 C43 N3 C44 0.9(3) . . . . ?
C42 C43 N3 C45 -15.0(4) . . . . ?
C38 C43 N3 C45 164.8(3) . . . . ?
C46 C45 N3 C44 -119.7(3) . . . . ?
C46 C45 N3 C43 78.3(3) . . . . ?
N2 C27 N4 C2 4.2(4) . . . . ?
C31 C27 N4 C2 -175.3(3) . . . . ?
C3 C2 N4 C27 -164.2(3) . . . . ?
C1 C2 N4 C27 75.2(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
O3 H1O O2 0.84(4) 2.02(4) 2.846(3) 168(3) .
N4 H1N O2 0.85(3) 2.26(3) 3.082(3) 165(3) 3_567
C29 H29 O1 0.93 2.56 3.317(4) 139.4 1_455
C17 H17 O4 0.93 2.57 3.361(4) 142.8 2_556
C14 H14 O4 0.93 2.34 3.153(4) 145.4 .
C5 H5 O2 0.98 2.51 2.996(3) 110.3 .
C2 H2 O4 0.98 2.50 3.087(3) 118.3 .
O3 H1O O2 0.84(4) 2.02(4) 2.846(3) 168(3) .
N4 H1N O2 0.85(3) 2.26(3) 3.082(3) 165(3) 3_567
C29 H29 O1 0.93 2.56 3.317(4) 139.4 1_455
C17 H17 O4 0.93 2.57 3.361(4) 142.8 2_556
C14 H14 O4 0.93 2.34 3.153(4) 145.4 .
C5 H5 O2 0.98 2.51 2.996(3) 110.3 .
C2 H2 O4 0.98 2.50 3.087(3) 118.3 .
O3 H1O O2 0.84(4) 2.02(4) 2.846(3) 168(3) .
N4 H1N O2 0.85(3) 2.26(3) 3.082(3) 165(3) 3_567
C29 H29 O1 0.93 2.56 3.317(4) 139.4 1_455
C17 H17 O4 0.93 2.57 3.361(4) 142.8 2_556
C14 H14 O4 0.93 2.34 3.153(4) 145.4 .
C5 H5 O2 0.98 2.51 2.996(3) 110.3 .
C2 H2 O4 0.98 2.50 3.087(3) 118.3 .
N4 H1N O2 0.85(3) 2.26(3) 3.082(3) 165(3) 3_567
C29 H29 O1 0.93 2.56 3.317(4) 139.4 1_455
C17 H17 O4 0.93 2.57 3.361(4) 142.8 2_556
C14 H14 O4 0.93 2.34 3.153(4) 145.4 .
C5 H5 O2 0.98 2.51 2.996(3) 110.3 .
C2 H2 O4 0.98 2.50 3.087(3) 118.3 .
N4 H1N O2 0.85(3) 2.26(3) 3.082(3) 165(3) 3_567
C29 H29 O1 0.93 2.56 3.317(4) 139.4 1_455
C17 H17 O4 0.93 2.57 3.361(4) 142.8 2_556
C14 H14 O4 0.93 2.34 3.153(4) 145.4 .
C5 H5 O2 0.98 2.51 2.996(3) 110.3 .
C2 H2 O4 0.98 2.50 3.087(3) 118.3 .
N4 H1N O2 0.85(3) 2.26(3) 3.082(3) 165(3) 3_567
C29 H29 O1 0.93 2.56 3.317(4) 139.4 1_455
C17 H17 O4 0.93 2.57 3.361(4) 142.8 2_556
C14 H14 O4 0.93 2.34 3.153(4) 145.4 .
C5 H5 O2 0.98 2.51 2.996(3) 110.3 .
C2 H2 O4 0.98 2.50 3.087(3) 118.3 .
C2 H2 O4 0.98 2.50 3.087(3) 118.3 .
C5 H5 O2 0.98 2.51 2.996(3) 110.3 .
C14 H14 O4 0.93 2.34 3.153(4) 145.4 .
C17 H17 O4 0.93 2.57 3.361(4) 142.8 2_556
C29 H29 O1 0.93 2.56 3.317(4) 139.4 1_455
N4 H1N O2 0.85(3) 2.26(3) 3.082(3) 165(3) 3_567
C2 H2 O4 0.98 2.50 3.087(3) 118.3 .
C5 H5 O2 0.98 2.51 2.996(3) 110.3 .
C14 H14 O4 0.93 2.34 3.153(4) 145.4 .
C17 H17 O4 0.93 2.57 3.361(4) 142.8 2_556
C29 H29 O1 0.93 2.56 3.317(4) 139.4 1_455
N4 H1N O2 0.85(3) 2.26(3) 3.082(3) 165(3) 3_567
C2 H2 O4 0.98 2.50 3.087(3) 118.3 .
C5 H5 O2 0.98 2.51 2.996(3) 110.3 .
C14 H14 O4 0.93 2.34 3.153(4) 145.4 .
C17 H17 O4 0.93 2.57 3.361(4) 142.8 2_556
C29 H29 O1 0.93 2.56 3.317(4) 139.4 1_455
N4 H1N O2 0.85(3) 2.26(3) 3.082(3) 165(3) 3_567
C2 H2 O4 0.98 2.50 3.087(3) 118.3 .
C5 H5 O2 0.98 2.51 2.996(3) 110.3 .
C14 H14 O4 0.93 2.34 3.153(4) 145.4 .
C17 H17 O4 0.93 2.57 3.361(4) 142.8 2_556
C29 H29 O1 0.93 2.56 3.317(4) 139.4 1_455
N4 H1N O2 0.85(3) 2.26(3) 3.082(3) 165(3) 3_567
C2 H2 O4 0.98 2.50 3.087(3) 118.3 .
C5 H5 O2 0.98 2.51 2.996(3) 110.3 .
C14 H14 O4 0.93 2.34 3.153(4) 145.4 .
C17 H17 O4 0.93 2.57 3.361(4) 142.8 2_556
C29 H29 O1 0.93 2.56 3.317(4) 139.4 1_455
N4 H1N O2 0.85(3) 2.26(3) 3.082(3) 165(3) 3_567
O3 H1O O2 0.84(4) 2.02(4) 2.846(3) 168(3) .
C2 H2 O4 0.98 2.50 3.087(3) 118.3 .
C5 H5 O2 0.98 2.51 2.996(3) 110.3 .
C14 H14 O4 0.93 2.34 3.153(4) 145.4 .
C17 H17 O4 0.93 2.57 3.361(4) 142.8 2_556
C29 H29 O1 0.93 2.56 3.317(4) 139.4 1_455
N4 H1N O2 0.85(3) 2.26(3) 3.082(3) 165(3) 3_567
O3 H1O O2 0.84(4) 2.02(4) 2.846(3) 168(3) .

_refine_diff_density_max         0.704
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.044

_shelxl_version_number           2013-4



