# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2014

####################################################################### 
# 
# 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_mj101b_teply_uochb
_database_code_depnum_ccdc_archive 'CCDC 925828'
_audit_update_record             
;
2013-02-20 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;
#TrackingRef 'mj101b_teply_uochb.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H26 N2, C H4 O, 2(I)'
_chemical_formula_sum            'C28 H30 I2 N2 O'
_chemical_formula_weight         664.34
_chemical_compound_source        'synthesized by the authors'

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'
I I -0.4742 1.8119 '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                   9.5036(4)
_cell_length_b                   11.1664(4)
_cell_length_c                   12.3553(5)
_cell_angle_alpha                87.9080(10)
_cell_angle_beta                 83.3910(10)
_cell_angle_gamma                82.4680(10)
_cell_volume                     1290.90(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9620
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      26.18

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             652
_exptl_absorpt_coefficient_mu    2.459
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.3182
_exptl_absorpt_correction_T_max  0.6714
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28212
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0132
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5067
_reflns_number_gt                4614
_reflns_threshold_expression     I>2σ(I)

_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-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 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)+(0.0098P)²+1.3139P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5067
_refine_ls_number_parameters     302
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0158
_refine_ls_wR_factor_ref         0.0378
_refine_ls_wR_factor_gt          0.0359
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.109
_refine_ls_shift/su_max          0.002
_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 0.8948(2) 0.84851(16) 0.32469(15) 0.0152(4) Uani 1 1 d . . .
H1 H 0.9891 0.8069 0.3168 0.018 Uiso 1 1 calc R . .
C2 C 0.8362(2) 0.89315(16) 0.42609(15) 0.0167(4) Uani 1 1 d . . .
C3 C 0.6992(2) 0.95722(18) 0.43401(16) 0.0211(4) Uani 1 1 d . . .
H3 H 0.6564 0.9895 0.5018 0.025 Uiso 1 1 calc R . .
C4 C 0.6263(2) 0.97361(18) 0.34417(17) 0.0209(4) Uani 1 1 d . . .
H4 H 0.5333 1.0177 0.3500 0.025 Uiso 1 1 calc R . .
N5 N 0.68533(16) 0.92777(14) 0.24728(13) 0.0160(3) Uani 1 1 d . . .
C6 C 0.6057(2) 0.94987(18) 0.15078(16) 0.0199(4) Uani 1 1 d . . .
H6A H 0.5230 1.0129 0.1667 0.024 Uiso 1 1 calc R . .
H6B H 0.5694 0.8749 0.1323 0.024 Uiso 1 1 calc R . .
C7 C 0.7046(2) 0.99051(18) 0.05643(16) 0.0204(4) Uani 1 1 d . . .
H7A H 0.7342 1.0690 0.0729 0.024 Uiso 1 1 calc R . .
H7B H 0.6541 1.0017 -0.0097 0.024 Uiso 1 1 calc R . .
C8 C 0.8346(2) 0.89792(17) 0.03577(16) 0.0165(4) Uani 1 1 d . . .
C9 C 0.9087(2) 0.88247(17) -0.06885(16) 0.0183(4) Uani 1 1 d . . .
C10 C 1.0243(2) 0.79178(18) -0.08604(15) 0.0191(4) Uani 1 1 d . . .
C11 C 1.0635(2) 0.71439(17) 0.00033(15) 0.0171(4) Uani 1 1 d . . .
C12 C 1.1942(2) 0.62130(18) -0.00897(16) 0.0214(4) Uani 1 1 d . . .
H12A H 1.2640 0.6438 -0.0696 0.026 Uiso 1 1 calc R . .
H12B H 1.1675 0.5413 -0.0241 0.026 Uiso 1 1 calc R . .
C13 C 1.2595(2) 0.61573(18) 0.09745(16) 0.0201(4) Uani 1 1 d . . .
H13A H 1.3470 0.5566 0.0931 0.024 Uiso 1 1 calc R . .
H13B H 1.2853 0.6959 0.1132 0.024 Uiso 1 1 calc R . .
N14 N 1.15207(16) 0.57855(14) 0.18467(13) 0.0167(3) Uani 1 1 d . . .
C15 C 1.1961(2) 0.49419(17) 0.26084(16) 0.0206(4) Uani 1 1 d . . .
H15 H 1.2944 0.4634 0.2585 0.025 Uiso 1 1 calc R . .
C16 C 1.1015(2) 0.45416(17) 0.33920(16) 0.0214(4) Uani 1 1 d . . .
H16 H 1.1342 0.4004 0.3950 0.026 Uiso 1 1 calc R . .
C17 C 0.9539(2) 0.49217(17) 0.33836(15) 0.0184(4) Uani 1 1 d . . .
C18 C 0.8501(2) 0.44555(18) 0.41389(16) 0.0227(4) Uani 1 1 d . . .
H18 H 0.8794 0.3911 0.4703 0.027 Uiso 1 1 calc R . .
C19 C 0.7082(2) 0.47852(19) 0.40596(17) 0.0255(5) Uani 1 1 d . . .
H19 H 0.6393 0.4489 0.4585 0.031 Uiso 1 1 calc R . .
C20 C 0.6626(2) 0.55605(19) 0.32060(18) 0.0252(4) Uani 1 1 d . . .
H20 H 0.5635 0.5751 0.3141 0.030 Uiso 1 1 calc R . .
C21 C 0.7603(2) 0.60412(17) 0.24695(16) 0.0196(4) Uani 1 1 d . . .
H21 H 0.7286 0.6559 0.1895 0.024 Uiso 1 1 calc R . .
C22 C 0.9085(2) 0.57680(16) 0.25614(15) 0.0157(4) Uani 1 1 d . . .
C23 C 1.01495(19) 0.62728(16) 0.18425(15) 0.0150(4) Uani 1 1 d . . .
C24 C 0.98476(19) 0.72577(17) 0.10360(15) 0.0151(4) Uani 1 1 d . . .
C25 C 0.87648(19) 0.82426(16) 0.12359(15) 0.0142(4) Uani 1 1 d . . .
C26 C 0.81821(19) 0.86362(16) 0.23473(15) 0.0139(4) Uani 1 1 d . . .
C27 C 0.9159(2) 0.87422(18) 0.52444(16) 0.0212(4) Uani 1 1 d . . .
H27A H 0.8778 0.8109 0.5717 0.032 Uiso 1 1 calc R . .
H27B H 0.9046 0.9497 0.5645 0.032 Uiso 1 1 calc R . .
H27C H 1.0174 0.8497 0.5014 0.032 Uiso 1 1 calc R . .
C28 C 0.8618(2) 0.9651(2) -0.16048(17) 0.0263(5) Uani 1 1 d . . .
H28A H 0.9423 0.9688 -0.2172 0.039 Uiso 1 1 calc R . .
H28B H 0.8290 1.0463 -0.1326 0.039 Uiso 1 1 calc R . .
H28C H 0.7835 0.9341 -0.1913 0.039 Uiso 1 1 calc R . .
C29 C 1.1038(2) 0.7730(2) -0.19885(17) 0.0293(5) Uani 1 1 d . . .
H29A H 1.0351 0.7742 -0.2523 0.044 Uiso 1 1 calc R . .
H29B H 1.1645 0.6949 -0.2005 0.044 Uiso 1 1 calc R . .
H29C H 1.1635 0.8378 -0.2167 0.044 Uiso 1 1 calc R . .
I1 I 0.424466(15) 0.282614(12) 0.066949(11) 0.02550(4) Uani 1 1 d . . .
I2 I 0.310916(13) 0.785392(12) 0.351828(11) 0.02218(4) Uani 1 1 d . . .
C1M C 0.5336(3) 0.7255(2) 0.6167(2) 0.0391(6) Uani 1 1 d . . .
H1M1 H 0.4450 0.7271 0.6660 0.059 Uiso 1 1 calc R . .
H1M2 H 0.5796 0.6420 0.6089 0.059 Uiso 1 1 calc R . .
H1M3 H 0.5118 0.7589 0.5451 0.059 Uiso 1 1 calc R . .
O1M O 0.62664(17) 0.79564(15) 0.65992(13) 0.0327(4) Uani 1 1 d . . .
H1M H 0.6282 0.7793 0.7274 0.039 Uiso 1 1 d 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
C1 C26 1.391(3) . ?
C1 C2 1.393(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.396(3) . ?
C2 C27 1.499(3) . ?
C3 C4 1.369(3) . ?
C3 H3 0.9500 . ?
C4 N5 1.351(3) . ?
C4 H4 0.9500 . ?
N5 C26 1.363(2) . ?
N5 C6 1.481(2) . ?
C6 C7 1.507(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.508(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C25 1.400(3) . ?
C8 C9 1.404(3) . ?
C9 C10 1.395(3) . ?
C9 C28 1.505(3) . ?
C10 C11 1.401(3) . ?
C10 C29 1.515(3) . ?
C11 C24 1.404(3) . ?
C11 C12 1.508(3) . ?
C12 C13 1.513(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N14 1.483(2) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
N14 C23 1.345(2) . ?
N14 C15 1.368(2) . ?
C15 C16 1.348(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.412(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.415(3) . ?
C17 C22 1.427(3) . ?
C18 C19 1.365(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.411(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.371(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.419(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.427(3) . ?
C23 C24 1.479(3) . ?
C24 C25 1.412(3) . ?
C25 C26 1.480(2) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C1M O1M 1.415(3) . ?
C1M H1M1 0.9800 . ?
C1M H1M2 0.9800 . ?
C1M H1M3 0.9800 . ?
O1M H1M 0.8482 . ?

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
C26 C1 C2 121.39(17) . . ?
C26 C1 H1 119.3 . . ?
C2 C1 H1 119.3 . . ?
C1 C2 C3 117.81(17) . . ?
C1 C2 C27 121.93(17) . . ?
C3 C2 C27 120.26(17) . . ?
C4 C3 C2 120.10(18) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
N5 C4 C3 120.66(18) . . ?
N5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 N5 C26 121.92(16) . . ?
C4 N5 C6 119.47(16) . . ?
C26 N5 C6 118.59(15) . . ?
N5 C6 C7 108.77(15) . . ?
N5 C6 H6A 109.9 . . ?
C7 C6 H6A 109.9 . . ?
N5 C6 H6B 109.9 . . ?
C7 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
C6 C7 C8 110.16(16) . . ?
C6 C7 H7A 109.6 . . ?
C8 C7 H7A 109.6 . . ?
C6 C7 H7B 109.6 . . ?
C8 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
C25 C8 C9 120.73(17) . . ?
C25 C8 C7 117.88(17) . . ?
C9 C8 C7 121.34(17) . . ?
C10 C9 C8 119.77(17) . . ?
C10 C9 C28 121.25(18) . . ?
C8 C9 C28 118.97(18) . . ?
C9 C10 C11 119.96(17) . . ?
C9 C10 C29 120.30(18) . . ?
C11 C10 C29 119.69(18) . . ?
C10 C11 C24 120.27(17) . . ?
C10 C11 C12 123.21(17) . . ?
C24 C11 C12 116.41(17) . . ?
C11 C12 C13 108.38(16) . . ?
C11 C12 H12A 110.0 . . ?
C13 C12 H12A 110.0 . . ?
C11 C12 H12B 110.0 . . ?
C13 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
N14 C13 C12 107.76(15) . . ?
N14 C13 H13A 110.2 . . ?
C12 C13 H13A 110.2 . . ?
N14 C13 H13B 110.2 . . ?
C12 C13 H13B 110.2 . . ?
H13A C13 H13B 108.5 . . ?
C23 N14 C15 122.71(17) . . ?
C23 N14 C13 118.65(16) . . ?
C15 N14 C13 118.62(16) . . ?
C16 C15 N14 120.77(18) . . ?
C16 C15 H15 119.6 . . ?
N14 C15 H15 119.6 . . ?
C15 C16 C17 120.02(18) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C16 C17 C18 122.00(18) . . ?
C16 C17 C22 118.69(18) . . ?
C18 C17 C22 119.27(18) . . ?
C19 C18 C17 120.24(19) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C18 C19 C20 120.74(19) . . ?
C18 C19 H19 119.6 . . ?
C20 C19 H19 119.6 . . ?
C21 C20 C19 120.47(19) . . ?
C21 C20 H20 119.8 . . ?
C19 C20 H20 119.8 . . ?
C20 C21 C22 120.26(19) . . ?
C20 C21 H21 119.9 . . ?
C22 C21 H21 119.9 . . ?
C21 C22 C17 118.79(17) . . ?
C21 C22 C23 122.82(17) . . ?
C17 C22 C23 118.36(17) . . ?
N14 C23 C22 118.49(17) . . ?
N14 C23 C24 116.86(16) . . ?
C22 C23 C24 124.55(16) . . ?
C11 C24 C25 119.61(17) . . ?
C11 C24 C23 116.90(16) . . ?
C25 C24 C23 123.37(16) . . ?
C8 C25 C24 119.01(17) . . ?
C8 C25 C26 117.61(16) . . ?
C24 C25 C26 122.86(16) . . ?
N5 C26 C1 118.07(16) . . ?
N5 C26 C25 117.49(16) . . ?
C1 C26 C25 124.19(16) . . ?
C2 C27 H27A 109.5 . . ?
C2 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C2 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C9 C28 H28A 109.5 . . ?
C9 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C9 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C10 C29 H29A 109.5 . . ?
C10 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C10 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O1M C1M H1M1 109.5 . . ?
O1M C1M H1M2 109.5 . . ?
H1M1 C1M H1M2 109.5 . . ?
O1M C1M H1M3 109.5 . . ?
H1M1 C1M H1M3 109.5 . . ?
H1M2 C1M H1M3 109.5 . . ?
C1M O1M H1M 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.059
####################################################################### 
# 
# 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_mj102a_teply_uochb
_database_code_depnum_ccdc_archive 'CCDC 925829'
_audit_update_record             
;
2013-02-20 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;
#TrackingRef 'mj102a_teply_uochb.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H26 N2, 2(I)'
_chemical_formula_sum            'C27 H26 I2 N2'
_chemical_formula_weight         632.30
_chemical_compound_source        'synthesized by the authors'

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'


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                   7.8813(2)
_cell_length_b                   16.2049(4)
_cell_length_c                   19.5829(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.0670(10)
_cell_angle_gamma                90.00
_cell_volume                     2469.79(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9934
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      27.50

_exptl_crystal_description       bar
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1232
_exptl_absorpt_coefficient_mu    2.563
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.4012
_exptl_absorpt_correction_T_max  0.7693
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            31665
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         27.50
_reflns_number_total             5678
_reflns_number_gt                5069
_reflns_threshold_expression     I>2σ(I)

_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-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 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)+(0.0178P)²+2.7834P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5678
_refine_ls_number_parameters     283
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0217
_refine_ls_wR_factor_ref         0.0471
_refine_ls_wR_factor_gt          0.0452
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.002
_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 0.5433(3) 0.28885(13) 0.62438(11) 0.0175(4) Uani 1 1 d . . .
H1 H 0.5150 0.2988 0.5761 0.021 Uiso 1 1 calc R . .
C2 C 0.4999(3) 0.34708(14) 0.67074(12) 0.0228(5) Uani 1 1 d . . .
C3 C 0.5292(3) 0.32663(15) 0.74096(12) 0.0275(5) Uani 1 1 d . . .
H3 H 0.5029 0.3651 0.7744 0.033 Uiso 1 1 calc R . .
C4 C 0.5960(3) 0.25102(16) 0.76134(12) 0.0268(5) Uani 1 1 d . . .
H4 H 0.6071 0.2357 0.8087 0.032 Uiso 1 1 calc R . .
C6 C 0.7202(3) 0.11687(14) 0.73932(12) 0.0261(5) Uani 1 1 d . . .
H6A H 0.6879 0.1029 0.7848 0.031 Uiso 1 1 calc R . .
H6B H 0.8471 0.1195 0.7447 0.031 Uiso 1 1 calc R . .
C7 C 0.6538(3) 0.05089(14) 0.68698(13) 0.0262(5) Uani 1 1 d . . .
H7A H 0.7099 -0.0024 0.7013 0.031 Uiso 1 1 calc R . .
H7B H 0.5285 0.0441 0.6856 0.031 Uiso 1 1 calc R . .
C8 C 0.6896(3) 0.07340(13) 0.61568(12) 0.0212(5) Uani 1 1 d . . .
C9 C 0.7174(3) 0.01483(13) 0.56595(13) 0.0241(5) Uani 1 1 d . . .
C10 C 0.7522(3) 0.04029(14) 0.50085(13) 0.0231(5) Uani 1 1 d . . .
C11 C 0.7638(3) 0.12489(13) 0.48690(12) 0.0208(4) Uani 1 1 d . . .
C12 C 0.7875(3) 0.16056(15) 0.41782(12) 0.0267(5) Uani 1 1 d . . .
H12A H 0.7494 0.1201 0.3807 0.032 Uiso 1 1 calc R . .
H12B H 0.9105 0.1728 0.4176 0.032 Uiso 1 1 calc R . .
C13 C 0.6828(3) 0.23907(15) 0.40488(11) 0.0252(5) Uani 1 1 d . . .
H13A H 0.6971 0.2628 0.3595 0.030 Uiso 1 1 calc R . .
H13B H 0.5595 0.2267 0.4041 0.030 Uiso 1 1 calc R . .
C15 C 0.7485(3) 0.38148(14) 0.44562(12) 0.0249(5) Uani 1 1 d . . .
H15 H 0.7154 0.3999 0.3994 0.030 Uiso 1 1 calc R . .
C16 C 0.8014(3) 0.43677(14) 0.49626(12) 0.0241(5) Uani 1 1 d . . .
H16 H 0.7921 0.4942 0.4866 0.029 Uiso 1 1 calc R . .
C17 C 0.8699(3) 0.40975(13) 0.56315(11) 0.0187(4) Uani 1 1 d . . .
C18 C 0.9386(3) 0.46408(14) 0.61707(12) 0.0239(5) Uani 1 1 d . . .
H18 H 0.9318 0.5220 0.6098 0.029 Uiso 1 1 calc R . .
C19 C 1.0143(3) 0.43382(14) 0.67941(13) 0.0260(5) Uani 1 1 d . . .
H19 H 1.0565 0.4709 0.7157 0.031 Uiso 1 1 calc R . .
C20 C 1.0308(3) 0.34787(14) 0.69053(12) 0.0241(5) Uani 1 1 d . . .
H20 H 1.0902 0.3277 0.7333 0.029 Uiso 1 1 calc R . .
C21 C 0.9621(3) 0.29335(13) 0.64035(11) 0.0189(4) Uani 1 1 d . . .
H21 H 0.9734 0.2356 0.6483 0.023 Uiso 1 1 calc R . .
C22 C 0.8743(3) 0.32312(12) 0.57664(11) 0.0164(4) Uani 1 1 d . . .
C23 C 0.7881(3) 0.27002(13) 0.52510(11) 0.0167(4) Uani 1 1 d . . .
C24 C 0.7459(3) 0.18319(12) 0.53816(11) 0.0159(4) Uani 1 1 d . . .
C25 C 0.6942(3) 0.15762(13) 0.60041(11) 0.0169(4) Uani 1 1 d . . .
C26 C 0.6272(3) 0.21640(13) 0.64736(11) 0.0168(4) Uani 1 1 d . . .
C27 C 0.4280(4) 0.42851(15) 0.64433(14) 0.0336(6) Uani 1 1 d . . .
H27A H 0.5154 0.4591 0.6242 0.050 Uiso 1 1 calc R . .
H27B H 0.3943 0.4603 0.6826 0.050 Uiso 1 1 calc R . .
H27C H 0.3273 0.4194 0.6089 0.050 Uiso 1 1 calc R . .
C28 C 0.7026(4) -0.07632(15) 0.58119(16) 0.0372(6) Uani 1 1 d . . .
H28A H 0.6400 -0.1042 0.5404 0.056 Uiso 1 1 calc R . .
H28B H 0.6404 -0.0835 0.6204 0.056 Uiso 1 1 calc R . .
H28C H 0.8178 -0.1002 0.5926 0.056 Uiso 1 1 calc R . .
C29 C 0.7814(3) -0.02295(15) 0.44743(14) 0.0337(6) Uani 1 1 d . . .
H29A H 0.8585 -0.0661 0.4693 0.051 Uiso 1 1 calc R . .
H29B H 0.8334 0.0038 0.4109 0.051 Uiso 1 1 calc R . .
H29C H 0.6713 -0.0476 0.4273 0.051 Uiso 1 1 calc R . .
I1 I 0.712357(19) 0.382953(9) 0.238363(8) 0.02395(4) Uani 1 1 d . . .
I2 I 0.23466(2) 0.312502(9) 0.452857(8) 0.02602(5) Uani 1 1 d . . .
N5 N 0.6460(2) 0.19808(11) 0.71581(10) 0.0203(4) Uani 1 1 d . . .
N14 N 0.7424(2) 0.29902(11) 0.46071(9) 0.0197(4) 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 C26 1.387(3) . ?
C1 C2 1.389(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.398(3) . ?
C2 C27 1.496(3) . ?
C3 C4 1.368(4) . ?
C3 H3 0.9500 . ?
C4 N5 1.340(3) . ?
C4 H4 0.9500 . ?
C6 N5 1.483(3) . ?
C6 C7 1.516(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.512(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C25 1.399(3) . ?
C8 C9 1.401(3) . ?
C9 C10 1.408(3) . ?
C9 C28 1.515(3) . ?
C10 C11 1.404(3) . ?
C10 C29 1.508(3) . ?
C11 C24 1.402(3) . ?
C11 C12 1.509(3) . ?
C12 C13 1.516(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N14 1.483(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C15 C16 1.353(3) . ?
C15 N14 1.371(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.406(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.415(3) . ?
C17 C22 1.428(3) . ?
C18 C19 1.363(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.413(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.368(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.413(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.416(3) . ?
C23 N14 1.341(3) . ?
C23 C24 1.477(3) . ?
C24 C25 1.407(3) . ?
C25 C26 1.478(3) . ?
C26 N5 1.358(3) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?

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
C26 C1 C2 121.1(2) . . ?
C26 C1 H1 119.4 . . ?
C2 C1 H1 119.4 . . ?
C1 C2 C3 117.5(2) . . ?
C1 C2 C27 119.5(2) . . ?
C3 C2 C27 123.0(2) . . ?
C4 C3 C2 119.7(2) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
N5 C4 C3 121.3(2) . . ?
N5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
N5 C6 C7 109.81(18) . . ?
N5 C6 H6A 109.7 . . ?
C7 C6 H6A 109.7 . . ?
N5 C6 H6B 109.7 . . ?
C7 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
C8 C7 C6 111.08(19) . . ?
C8 C7 H7A 109.4 . . ?
C6 C7 H7A 109.4 . . ?
C8 C7 H7B 109.4 . . ?
C6 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
C25 C8 C9 120.0(2) . . ?
C25 C8 C7 116.6(2) . . ?
C9 C8 C7 123.4(2) . . ?
C8 C9 C10 120.3(2) . . ?
C8 C9 C28 119.9(2) . . ?
C10 C9 C28 119.8(2) . . ?
C11 C10 C9 119.4(2) . . ?
C11 C10 C29 120.5(2) . . ?
C9 C10 C29 120.1(2) . . ?
C24 C11 C10 120.1(2) . . ?
C24 C11 C12 115.11(19) . . ?
C10 C11 C12 124.7(2) . . ?
C11 C12 C13 109.30(19) . . ?
C11 C12 H12A 109.8 . . ?
C13 C12 H12A 109.8 . . ?
C11 C12 H12B 109.8 . . ?
C13 C12 H12B 109.8 . . ?
H12A C12 H12B 108.3 . . ?
N14 C13 C12 109.03(18) . . ?
N14 C13 H13A 109.9 . . ?
C12 C13 H13A 109.9 . . ?
N14 C13 H13B 109.9 . . ?
C12 C13 H13B 109.9 . . ?
H13A C13 H13B 108.3 . . ?
C16 C15 N14 120.3(2) . . ?
C16 C15 H15 119.8 . . ?
N14 C15 H15 119.8 . . ?
C15 C16 C17 120.4(2) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C16 C17 C18 123.2(2) . . ?
C16 C17 C22 118.2(2) . . ?
C18 C17 C22 118.6(2) . . ?
C19 C18 C17 120.4(2) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C18 C19 C20 120.6(2) . . ?
C18 C19 H19 119.7 . . ?
C20 C19 H19 119.7 . . ?
C21 C20 C19 120.6(2) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C20 C21 C22 119.8(2) . . ?
C20 C21 H21 120.1 . . ?
C22 C21 H21 120.1 . . ?
C21 C22 C23 122.36(19) . . ?
C21 C22 C17 119.56(19) . . ?
C23 C22 C17 118.08(19) . . ?
N14 C23 C22 119.02(19) . . ?
N14 C23 C24 117.52(19) . . ?
C22 C23 C24 123.45(19) . . ?
C11 C24 C25 119.84(19) . . ?
C11 C24 C23 117.84(19) . . ?
C25 C24 C23 122.29(18) . . ?
C8 C25 C24 119.5(2) . . ?
C8 C25 C26 118.18(19) . . ?
C24 C25 C26 121.98(18) . . ?
N5 C26 C1 118.52(19) . . ?
N5 C26 C25 118.61(19) . . ?
C1 C26 C25 122.85(19) . . ?
C2 C27 H27A 109.5 . . ?
C2 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C2 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C9 C28 H28A 109.5 . . ?
C9 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C9 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C10 C29 H29A 109.5 . . ?
C10 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C10 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C4 N5 C26 121.25(19) . . ?
C4 N5 C6 120.27(19) . . ?
C26 N5 C6 118.47(19) . . ?
C23 N14 C15 122.07(19) . . ?
C23 N14 C13 118.09(18) . . ?
C15 N14 C13 119.84(19) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.020
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.073
####################################################################### 
# 
# 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_mj168_teply_uochb
_database_code_depnum_ccdc_archive 'CCDC 925830'
_audit_update_record             
;
2013-02-20 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;
#TrackingRef 'mj168_teply_uochb.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H35 N3, 2(C10 H7 O3 S), C H3 N O2'
_chemical_formula_sum            'C57 H52 N4 O8 S2'
_chemical_formula_weight         985.15
_chemical_compound_source        'synthesized by the authors'

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'
S S 0.1246 0.1234 '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                   8.2074(6)
_cell_length_b                   16.4498(11)
_cell_length_c                   19.3506(12)
_cell_angle_alpha                70.455(2)
_cell_angle_beta                 86.370(2)
_cell_angle_gamma                77.900(2)
_cell_volume                     2407.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5043
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      24.71

_exptl_crystal_description       bar
_exptl_crystal_colour            violet
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1036
_exptl_absorpt_coefficient_mu    0.174
_exptl_absorpt_correction_type   multi-scans
_exptl_absorpt_correction_T_min  0.8751
_exptl_absorpt_correction_T_max  0.9835
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16715
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.34
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8251
_reflns_number_gt                5700
_reflns_threshold_expression     I>2σ(I)

_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-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 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)+(0.0651P)²+1.5108P] 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         8251
_refine_ls_number_parameters     648
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0527
_refine_ls_wR_factor_ref         0.1413
_refine_ls_wR_factor_gt          0.1265
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.004
_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 0.5392(3) 0.54530(17) 0.17921(15) 0.0208(6) Uani 1 1 d . . .
H1 H 0.5071 0.5756 0.2135 0.025 Uiso 1 1 calc R . .
C2 C 0.6000(3) 0.58982(18) 0.11073(15) 0.0244(6) Uani 1 1 d . . .
C3 C 0.6473(4) 0.54184(19) 0.06277(16) 0.0285(7) Uani 1 1 d . . .
H3 H 0.6826 0.5703 0.0146 0.034 Uiso 1 1 calc R . .
C4 C 0.6431(4) 0.45459(19) 0.08464(16) 0.0270(7) Uani 1 1 d . . .
H4 H 0.6821 0.4221 0.0524 0.032 Uiso 1 1 calc R . .
N5 N 0.5850(3) 0.41346(14) 0.15090(12) 0.0209(5) Uani 1 1 d . . .
C6 C 0.5870(4) 0.31753(18) 0.17358(16) 0.0262(7) Uani 1 1 d . . .
H6A H 0.6689 0.2902 0.1439 0.031 Uiso 1 1 calc R . .
H6B H 0.4757 0.3081 0.1652 0.031 Uiso 1 1 calc R . .
C7 C 0.6331(4) 0.27540(18) 0.25385(16) 0.0290(7) Uani 1 1 d . . .
H7A H 0.6291 0.2121 0.2697 0.035 Uiso 1 1 calc R . .
H7B H 0.7483 0.2805 0.2613 0.035 Uiso 1 1 calc R . .
C8 C 0.5155(3) 0.31925(18) 0.29927(16) 0.0247(6) Uani 1 1 d . . .
C9 C 0.4642(4) 0.27341(19) 0.37015(16) 0.0294(7) Uani 1 1 d . . .
C10 C 0.3569(4) 0.3190(2) 0.40986(15) 0.0276(7) Uani 1 1 d . . .
C11 C 0.2918(3) 0.40839(19) 0.37775(15) 0.0249(7) Uani 1 1 d . . .
C12 C 0.1803(4) 0.4623(2) 0.41859(16) 0.0298(7) Uani 1 1 d . . .
H12A H 0.0633 0.4573 0.4149 0.036 Uiso 1 1 calc R . .
H12B H 0.2124 0.4390 0.4711 0.036 Uiso 1 1 calc R . .
C13 C 0.1945(4) 0.5577(2) 0.38725(16) 0.0319(7) Uani 1 1 d . . .
H13A H 0.1137 0.5929 0.4116 0.038 Uiso 1 1 calc R . .
H13B H 0.3079 0.5636 0.3966 0.038 Uiso 1 1 calc R . .
N14 N 0.1612(3) 0.59115(15) 0.30741(13) 0.0254(6) Uani 1 1 d . . .
C15 C 0.0718(4) 0.67462(19) 0.27619(19) 0.0324(8) Uani 1 1 d . . .
H15 H 0.0331 0.7102 0.3061 0.039 Uiso 1 1 calc R . .
C16 C 0.0375(4) 0.7073(2) 0.20390(19) 0.0340(8) Uani 1 1 d . . .
H16 H -0.0141 0.7674 0.1824 0.041 Uiso 1 1 calc R . .
C17 C 0.0778(3) 0.65283(18) 0.15989(16) 0.0260(7) Uani 1 1 d . . .
C18 C 0.0295(4) 0.6799(2) 0.08581(17) 0.0316(7) Uani 1 1 d . . .
H18 H -0.0181 0.7400 0.0614 0.038 Uiso 1 1 calc R . .
C19 C 0.0500(4) 0.6214(2) 0.04860(17) 0.0350(8) Uani 1 1 d . . .
H19 H 0.0192 0.6410 -0.0017 0.042 Uiso 1 1 calc R . .
C20 C 0.1165(4) 0.5324(2) 0.08466(15) 0.0273(7) Uani 1 1 d . . .
H20 H 0.1222 0.4910 0.0597 0.033 Uiso 1 1 calc R . .
C21 C 0.1736(3) 0.50403(18) 0.15554(15) 0.0215(6) Uani 1 1 d . . .
H21 H 0.2216 0.4437 0.1787 0.026 Uiso 1 1 calc R . .
C22 C 0.1616(3) 0.56398(17) 0.19438(15) 0.0210(6) Uani 1 1 d . . .
C23 C 0.2190(3) 0.53766(17) 0.26776(15) 0.0204(6) Uani 1 1 d . . .
C24 C 0.3280(3) 0.45237(17) 0.30469(14) 0.0203(6) Uani 1 1 d . . .
C25 C 0.4523(3) 0.40926(17) 0.26777(15) 0.0204(6) Uani 1 1 d . . .
C26 C 0.5248(3) 0.45817(17) 0.19816(14) 0.0193(6) Uani 1 1 d . . .
C27 C 0.5294(5) 0.1752(2) 0.40218(19) 0.0456(9) Uani 1 1 d . . .
H27A H 0.5572 0.1598 0.4541 0.068 Uiso 1 1 calc R . .
H27B H 0.6294 0.1583 0.3757 0.068 Uiso 1 1 calc R . .
H27C H 0.4438 0.1438 0.3975 0.068 Uiso 1 1 calc R . .
C28 C 0.3035(4) 0.2722(2) 0.48682(16) 0.0399(8) Uani 1 1 d . . .
H28A H 0.3713 0.2814 0.5224 0.060 Uiso 1 1 calc R . .
H28B H 0.3191 0.2091 0.4946 0.060 Uiso 1 1 calc R . .
H28C H 0.1858 0.2959 0.4932 0.060 Uiso 1 1 calc R . .
C29 C 0.6210(4) 0.68053(19) 0.08745(17) 0.0292(7) Uani 1 1 d . . .
H29 H 0.6478 0.7063 0.0374 0.035 Uiso 1 1 calc R . .
C30 C 0.6062(4) 0.7305(2) 0.12967(16) 0.0298(7) Uani 1 1 d . . .
H30 H 0.5732 0.7056 0.1789 0.036 Uiso 1 1 calc R . .
C31 C 0.6355(4) 0.82006(19) 0.10781(17) 0.0296(7) Uani 1 1 d . . .
C32 C 0.6859(4) 0.86546(19) 0.03761(17) 0.0293(7) Uani 1 1 d . . .
H32 H 0.7036 0.8369 0.0017 0.035 Uiso 1 1 calc R . .
C33 C 0.7109(4) 0.9515(2) 0.01872(18) 0.0336(7) Uani 1 1 d . . .
H33 H 0.7496 0.9797 -0.0289 0.040 Uiso 1 1 calc R . .
C34 C 0.6793(4) 0.9967(2) 0.06976(18) 0.0333(7) Uani 1 1 d . . .
C35 C 0.6313(4) 0.9508(2) 0.14043(19) 0.0387(8) Uani 1 1 d . . .
H35 H 0.6120 0.9791 0.1765 0.046 Uiso 1 1 calc R . .
C36 C 0.6115(4) 0.8646(2) 0.15848(18) 0.0356(8) Uani 1 1 d . . .
H36 H 0.5806 0.8349 0.2071 0.043 Uiso 1 1 calc R . .
N37 N 0.6948(4) 1.08333(17) 0.05081(16) 0.0429(7) Uani 1 1 d . . .
C38 C 0.7620(5) 1.1264(2) -0.0194(2) 0.0508(10) Uani 1 1 d . . .
H38A H 0.8758 1.0951 -0.0236 0.076 Uiso 1 1 calc R . .
H38B H 0.7636 1.1874 -0.0238 0.076 Uiso 1 1 calc R . .
H38C H 0.6924 1.1261 -0.0586 0.076 Uiso 1 1 calc R . .
C39 C 0.6266(5) 1.1347(2) 0.0978(2) 0.0539(10) Uani 1 1 d . . .
H39A H 0.5112 1.1283 0.1100 0.081 Uiso 1 1 calc R . .
H39B H 0.6292 1.1969 0.0721 0.081 Uiso 1 1 calc R . .
H39C H 0.6932 1.1136 0.1429 0.081 Uiso 1 1 calc R . .
C40 C 0.8551(4) 0.83396(19) 0.82073(16) 0.0271(7) Uani 1 1 d . . .
C41 C 0.7659(4) 0.8893(2) 0.76044(17) 0.0333(7) Uani 1 1 d . . .
H41 H 0.7141 0.8658 0.7309 0.040 Uiso 1 1 calc R . .
C42 C 0.7492(4) 0.9824(2) 0.74099(19) 0.0389(8) Uani 1 1 d . . .
C43 C 0.6561(5) 1.0415(2) 0.6796(2) 0.0552(11) Uani 1 1 d . . .
H43 H 0.6053 1.0196 0.6486 0.066 Uiso 1 1 calc R . .
C44 C 0.6379(5) 1.1303(3) 0.6641(3) 0.0690(14) Uani 1 1 d . . .
H44 H 0.5736 1.1697 0.6227 0.083 Uiso 1 1 calc R . .
C45 C 0.7133(5) 1.1639(3) 0.7088(3) 0.0724(15) Uani 1 1 d . . .
H45 H 0.6989 1.2257 0.6980 0.087 Uiso 1 1 calc R . .
C46 C 0.8064(5) 1.1083(2) 0.7674(3) 0.0590(11) Uani 1 1 d . . .
H46 H 0.8584 1.1317 0.7968 0.071 Uiso 1 1 calc R . .
C47 C 0.8279(4) 1.0156(2) 0.7857(2) 0.0434(9) Uani 1 1 d . . .
C48 C 0.9244(5) 0.9563(2) 0.8464(2) 0.0466(9) Uani 1 1 d . . .
H48 H 0.9817 0.9782 0.8753 0.056 Uiso 1 1 calc R . .
C49 C 0.9361(4) 0.8680(2) 0.86412(18) 0.0393(8) Uani 1 1 d . . .
H49 H 0.9992 0.8289 0.9060 0.047 Uiso 1 1 calc R . .
C50 C 0.7280(3) 0.50738(19) 0.36698(15) 0.0250(7) Uani 1 1 d . . .
C51 C 0.7148(4) 0.4368(2) 0.42790(16) 0.0274(7) Uani 1 1 d . . .
H51 H 0.6483 0.4455 0.4678 0.033 Uiso 1 1 calc R . .
C52 C 0.8000(4) 0.3505(2) 0.43198(16) 0.0296(7) Uani 1 1 d . . .
C53 C 0.7923(4) 0.2774(2) 0.49475(17) 0.0344(8) Uani 1 1 d . . .
H53 H 0.7276 0.2848 0.5355 0.041 Uiso 1 1 calc R . .
C54 C 0.8779(4) 0.1953(2) 0.4973(2) 0.0435(9) Uani 1 1 d . . .
H54 H 0.8718 0.1460 0.5399 0.052 Uiso 1 1 calc R . .
C55 C 0.9749(4) 0.1835(2) 0.43744(19) 0.0414(8) Uani 1 1 d . . .
H55 H 1.0342 0.1263 0.4402 0.050 Uiso 1 1 calc R . .
C56 C 0.9846(4) 0.2528(2) 0.37586(18) 0.0343(8) Uani 1 1 d . . .
H56 H 1.0498 0.2438 0.3358 0.041 Uiso 1 1 calc R . .
C57 C 0.8973(4) 0.3392(2) 0.37108(16) 0.0285(7) Uani 1 1 d . . .
C58 C 0.9043(4) 0.4131(2) 0.30807(16) 0.0276(7) Uani 1 1 d . . .
H58 H 0.9662 0.4055 0.2667 0.033 Uiso 1 1 calc R . .
C59 C 0.8229(3) 0.4955(2) 0.30598(16) 0.0266(7) Uani 1 1 d . . .
H59 H 0.8300 0.5448 0.2636 0.032 Uiso 1 1 calc R . .
S1 S 0.86838(9) 0.71943(5) 0.84760(4) 0.02663(19) Uani 1 1 d . . .
O1 O 0.7645(3) 0.69742(13) 0.91178(11) 0.0340(5) Uani 1 1 d . . .
O2 O 1.0418(3) 0.67942(14) 0.86324(13) 0.0413(6) Uani 1 1 d . . .
O3 O 0.8038(3) 0.70451(13) 0.78544(11) 0.0368(5) Uani 1 1 d . . .
S2 S 0.62417(9) 0.61553(5) 0.36172(4) 0.02703(19) Uani 1 1 d . . .
O4 O 0.5432(3) 0.60789(13) 0.43173(11) 0.0316(5) Uani 1 1 d . . .
O5 O 0.7520(3) 0.66764(15) 0.34699(14) 0.0487(7) Uani 1 1 d . . .
O6 O 0.5049(3) 0.64206(13) 0.30177(11) 0.0344(5) Uani 1 1 d . . .
N1S N 0.2334(6) 0.0382(3) 0.6577(3) 0.0995(16) Uani 1 1 d . . .
C1S C 0.1803(5) 0.1239(3) 0.6637(2) 0.0428(11) Uani 0.80 1 d P A .
H11S H 0.1312 0.1189 0.7121 0.064 Uiso 0.80 1 calc PR . .
H12S H 0.0969 0.1592 0.6255 0.064 Uiso 0.80 1 calc PR . .
H13S H 0.2762 0.1524 0.6576 0.064 Uiso 0.80 1 calc PR . .
O1S O 0.2835(5) -0.0272(2) 0.7090(2) 0.0978(12) Uani 1 1 d . A .
O2S O 0.2626(8) 0.0419(4) 0.5919(4) 0.125(2) Uiso 0.80 1 d P A 1
C2S C 0.118(2) -0.0025(10) 0.6280(9) 0.035(4) Uiso 0.20 1 d P A 2
H21S H 0.1573 -0.0665 0.6441 0.053 Uiso 0.20 1 calc PR A 2
H22S H 0.1178 0.0209 0.5743 0.053 Uiso 0.20 1 calc PR A 2
H23S H 0.0055 0.0116 0.6461 0.053 Uiso 0.20 1 calc PR A 2
O3S O 0.347(3) 0.0538(17) 0.5835(14) 0.125(2) Uiso 0.20 1 d P A 2


_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 C26 1.384(4) . ?
C1 C2 1.401(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.397(4) . ?
C2 C29 1.452(4) . ?
C3 C4 1.361(4) . ?
C3 H3 0.9500 . ?
C4 N5 1.344(4) . ?
C4 H4 0.9500 . ?
N5 C26 1.365(3) . ?
N5 C6 1.487(3) . ?
C6 C7 1.510(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.500(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C25 1.395(4) . ?
C8 C9 1.412(4) . ?
C9 C10 1.397(4) . ?
C9 C27 1.514(4) . ?
C10 C11 1.391(4) . ?
C10 C28 1.514(4) . ?
C11 C24 1.401(4) . ?
C11 C12 1.511(4) . ?
C12 C13 1.508(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N14 1.479(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
N14 C23 1.349(3) . ?
N14 C15 1.367(4) . ?
C15 C16 1.345(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.410(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.408(4) . ?
C17 C22 1.428(4) . ?
C18 C19 1.361(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.400(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.371(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.412(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.419(4) . ?
C23 C24 1.471(4) . ?
C24 C25 1.413(4) . ?
C25 C26 1.480(4) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.324(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.458(4) . ?
C30 H30 0.9500 . ?
C31 C36 1.390(4) . ?
C31 C32 1.398(4) . ?
C32 C33 1.395(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.405(4) . ?
C33 H33 0.9500 . ?
C34 N37 1.379(4) . ?
C34 C35 1.401(5) . ?
C35 C36 1.384(4) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
N37 C38 1.442(5) . ?
N37 C39 1.451(4) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C41 1.358(4) . ?
C40 C49 1.415(4) . ?
C40 S1 1.760(3) . ?
C41 C42 1.428(4) . ?
C41 H41 0.9500 . ?
C42 C43 1.404(5) . ?
C42 C47 1.414(5) . ?
C43 C44 1.367(6) . ?
C43 H43 0.9500 . ?
C44 C45 1.402(7) . ?
C44 H44 0.9500 . ?
C45 C46 1.352(6) . ?
C45 H45 0.9500 . ?
C46 C47 1.419(5) . ?
C46 H46 0.9500 . ?
C47 C48 1.409(5) . ?
C48 C49 1.360(5) . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
C50 C51 1.367(4) . ?
C50 C59 1.419(4) . ?
C50 S2 1.777(3) . ?
C51 C52 1.424(4) . ?
C51 H51 0.9500 . ?
C52 C53 1.404(4) . ?
C52 C57 1.423(4) . ?
C53 C54 1.372(5) . ?
C53 H53 0.9500 . ?
C54 C55 1.408(5) . ?
C54 H54 0.9500 . ?
C55 C56 1.358(5) . ?
C55 H55 0.9500 . ?
C56 C57 1.426(4) . ?
C56 H56 0.9500 . ?
C57 C58 1.413(4) . ?
C58 C59 1.368(4) . ?
C58 H58 0.9500 . ?
C59 H59 0.9500 . ?
S1 O2 1.442(2) . ?
S1 O1 1.448(2) . ?
S1 O3 1.456(2) . ?
S2 O5 1.446(2) . ?
S2 O4 1.449(2) . ?
S2 O6 1.456(2) . ?
N1S O1S 1.210(5) . ?
N1S O2S 1.263(7) . ?
N1S C1S 1.426(6) . ?
N1S C2S 1.503(16) . ?
N1S O3S 1.64(3) . ?
C1S H11S 0.9800 . ?
C1S H12S 0.9800 . ?
C1S H13S 0.9800 . ?
C2S H21S 0.9800 . ?
C2S H22S 0.9800 . ?
C2S H23S 0.9800 . ?

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
C26 C1 C2 121.6(3) . . ?
C26 C1 H1 119.2 . . ?
C2 C1 H1 119.2 . . ?
C3 C2 C1 116.8(3) . . ?
C3 C2 C29 118.4(3) . . ?
C1 C2 C29 124.7(3) . . ?
C4 C3 C2 120.4(3) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
N5 C4 C3 121.3(3) . . ?
N5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C4 N5 C26 121.1(2) . . ?
C4 N5 C6 119.7(2) . . ?
C26 N5 C6 119.2(2) . . ?
N5 C6 C7 109.4(2) . . ?
N5 C6 H6A 109.8 . . ?
C7 C6 H6A 109.8 . . ?
N5 C6 H6B 109.8 . . ?
C7 C6 H6B 109.8 . . ?
H6A C6 H6B 108.3 . . ?
C8 C7 C6 110.5(2) . . ?
C8 C7 H7A 109.5 . . ?
C6 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
C25 C8 C9 119.8(3) . . ?
C25 C8 C7 117.0(2) . . ?
C9 C8 C7 123.2(3) . . ?
C10 C9 C8 120.0(3) . . ?
C10 C9 C27 121.1(3) . . ?
C8 C9 C27 118.9(3) . . ?
C11 C10 C9 120.0(3) . . ?
C11 C10 C28 118.7(3) . . ?
C9 C10 C28 121.2(3) . . ?
C10 C11 C24 120.3(3) . . ?
C10 C11 C12 122.6(3) . . ?
C24 C11 C12 117.0(3) . . ?
C13 C12 C11 110.6(2) . . ?
C13 C12 H12A 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
N14 C13 C12 110.2(2) . . ?
N14 C13 H13A 109.6 . . ?
C12 C13 H13A 109.6 . . ?
N14 C13 H13B 109.6 . . ?
C12 C13 H13B 109.6 . . ?
H13A C13 H13B 108.1 . . ?
C23 N14 C15 122.1(3) . . ?
C23 N14 C13 118.6(2) . . ?
C15 N14 C13 119.3(2) . . ?
C16 C15 N14 121.1(3) . . ?
C16 C15 H15 119.4 . . ?
N14 C15 H15 119.4 . . ?
C15 C16 C17 120.4(3) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C18 C17 C16 123.3(3) . . ?
C18 C17 C22 119.0(3) . . ?
C16 C17 C22 117.6(3) . . ?
C19 C18 C17 121.1(3) . . ?
C19 C18 H18 119.4 . . ?
C17 C18 H18 119.4 . . ?
C18 C19 C20 119.8(3) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.1 . . ?
C21 C20 C19 120.9(3) . . ?
C21 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
C20 C21 C22 120.4(3) . . ?
C20 C21 H21 119.8 . . ?
C22 C21 H21 119.8 . . ?
C21 C22 C23 122.4(2) . . ?
C21 C22 C17 118.2(2) . . ?
C23 C22 C17 119.2(2) . . ?
N14 C23 C22 118.1(2) . . ?
N14 C23 C24 118.1(2) . . ?
C22 C23 C24 123.6(2) . . ?
C11 C24 C25 119.3(2) . . ?
C11 C24 C23 117.2(2) . . ?
C25 C24 C23 123.1(2) . . ?
C8 C25 C24 119.6(3) . . ?
C8 C25 C26 118.7(2) . . ?
C24 C25 C26 121.6(2) . . ?
N5 C26 C1 118.3(2) . . ?
N5 C26 C25 117.6(2) . . ?
C1 C26 C25 124.1(2) . . ?
C9 C27 H27A 109.5 . . ?
C9 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C9 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C10 C28 H28A 109.5 . . ?
C10 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C10 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 C2 125.8(3) . . ?
C30 C29 H29 117.1 . . ?
C2 C29 H29 117.1 . . ?
C29 C30 C31 126.3(3) . . ?
C29 C30 H30 116.9 . . ?
C31 C30 H30 116.9 . . ?
C36 C31 C32 116.9(3) . . ?
C36 C31 C30 119.3(3) . . ?
C32 C31 C30 123.8(3) . . ?
C33 C32 C31 121.9(3) . . ?
C33 C32 H32 119.0 . . ?
C31 C32 H32 119.0 . . ?
C32 C33 C34 120.3(3) . . ?
C32 C33 H33 119.8 . . ?
C34 C33 H33 119.8 . . ?
N37 C34 C35 121.2(3) . . ?
N37 C34 C33 121.1(3) . . ?
C35 C34 C33 117.7(3) . . ?
C36 C35 C34 120.9(3) . . ?
C36 C35 H35 119.5 . . ?
C34 C35 H35 119.5 . . ?
C35 C36 C31 122.2(3) . . ?
C35 C36 H36 118.9 . . ?
C31 C36 H36 118.9 . . ?
C34 N37 C38 120.3(3) . . ?
C34 N37 C39 120.2(3) . . ?
C38 N37 C39 119.2(3) . . ?
N37 C38 H38A 109.5 . . ?
N37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
N37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N37 C39 H39A 109.5 . . ?
N37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
N37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C41 C40 C49 120.2(3) . . ?
C41 C40 S1 121.0(2) . . ?
C49 C40 S1 118.8(2) . . ?
C40 C41 C42 120.6(3) . . ?
C40 C41 H41 119.7 . . ?
C42 C41 H41 119.7 . . ?
C43 C42 C47 119.3(3) . . ?
C43 C42 C41 122.1(3) . . ?
C47 C42 C41 118.6(3) . . ?
C44 C43 C42 120.5(4) . . ?
C44 C43 H43 119.8 . . ?
C42 C43 H43 119.8 . . ?
C43 C44 C45 120.6(4) . . ?
C43 C44 H44 119.7 . . ?
C45 C44 H44 119.7 . . ?
C46 C45 C44 120.0(4) . . ?
C46 C45 H45 120.0 . . ?
C44 C45 H45 120.0 . . ?
C45 C46 C47 121.3(4) . . ?
C45 C46 H46 119.3 . . ?
C47 C46 H46 119.3 . . ?
C48 C47 C42 119.4(3) . . ?
C48 C47 C46 122.4(4) . . ?
C42 C47 C46 118.3(4) . . ?
C49 C48 C47 120.6(3) . . ?
C49 C48 H48 119.7 . . ?
C47 C48 H48 119.7 . . ?
C48 C49 C40 120.5(3) . . ?
C48 C49 H49 119.7 . . ?
C40 C49 H49 119.7 . . ?
C51 C50 C59 120.6(3) . . ?
C51 C50 S2 120.9(2) . . ?
C59 C50 S2 118.5(2) . . ?
C50 C51 C52 120.5(3) . . ?
C50 C51 H51 119.7 . . ?
C52 C51 H51 119.7 . . ?
C53 C52 C57 119.8(3) . . ?
C53 C52 C51 121.6(3) . . ?
C57 C52 C51 118.6(3) . . ?
C54 C53 C52 120.1(3) . . ?
C54 C53 H53 120.0 . . ?
C52 C53 H53 120.0 . . ?
C53 C54 C55 120.5(3) . . ?
C53 C54 H54 119.7 . . ?
C55 C54 H54 119.7 . . ?
C56 C55 C54 120.8(3) . . ?
C56 C55 H55 119.6 . . ?
C54 C55 H55 119.6 . . ?
C55 C56 C57 120.3(3) . . ?
C55 C56 H56 119.8 . . ?
C57 C56 H56 119.8 . . ?
C58 C57 C52 119.5(3) . . ?
C58 C57 C56 122.1(3) . . ?
C52 C57 C56 118.5(3) . . ?
C59 C58 C57 120.7(3) . . ?
C59 C58 H58 119.7 . . ?
C57 C58 H58 119.7 . . ?
C58 C59 C50 120.1(3) . . ?
C58 C59 H59 119.9 . . ?
C50 C59 H59 119.9 . . ?
O2 S1 O1 112.68(13) . . ?
O2 S1 O3 113.44(14) . . ?
O1 S1 O3 112.36(13) . . ?
O2 S1 C40 106.46(14) . . ?
O1 S1 C40 105.91(13) . . ?
O3 S1 C40 105.22(13) . . ?
O5 S2 O4 113.50(13) . . ?
O5 S2 O6 113.38(15) . . ?
O4 S2 O6 112.26(13) . . ?
O5 S2 C50 105.99(14) . . ?
O4 S2 C50 106.27(13) . . ?
O6 S2 C50 104.53(12) . . ?
O1S N1S O2S 122.4(5) . . ?
O1S N1S C1S 123.8(4) . . ?
O2S N1S C1S 111.5(5) . . ?
O1S N1S C2S 95.4(8) . . ?
C1S N1S C2S 121.0(7) . . ?
O1S N1S O3S 116.4(9) . . ?
C1S N1S O3S 104.4(10) . . ?
C2S N1S O3S 92.0(12) . . ?
N1S C1S H11S 109.5 . . ?
N1S C1S H12S 109.5 . . ?
H11S C1S H12S 109.5 . . ?
N1S C1S H13S 109.5 . . ?
H11S C1S H13S 109.5 . . ?
H12S C1S H13S 109.5 . . ?
N1S C2S H21S 109.5 . . ?
N1S C2S H22S 109.5 . . ?
H21S C2S H22S 109.5 . . ?
N1S C2S H23S 109.5 . . ?
H21S C2S H23S 109.5 . . ?
H22S C2S H23S 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.058
####################################################################### 
# 
# 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_mj210c_uochb
_database_code_depnum_ccdc_archive 'CCDC 925831'
_audit_update_record             
;
2013-02-20 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;
#TrackingRef 'mj210c_uochb.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C35 H32 N2 O), 4(C F3 O3 S), C H3 N O2'
_chemical_formula_sum            'C75 H67 F12 N5 O16 S4'
_chemical_formula_weight         1650.58
_chemical_compound_source        'synthesized by the authors'

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'
S S 0.1246 0.1234 '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                   12.8456(3)
_cell_length_b                   13.7518(3)
_cell_length_c                   21.7960(4)
_cell_angle_alpha                75.1430(10)
_cell_angle_beta                 84.4540(10)
_cell_angle_gamma                87.5830(10)
_cell_volume                     3703.52(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9881
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      27.47

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1704
_exptl_absorpt_coefficient_mu    0.230
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9194
_exptl_absorpt_correction_T_max  0.9623
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            47477
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.53
_diffrn_reflns_theta_max         27.50
_reflns_number_total             16927
_reflns_number_gt                12139
_reflns_threshold_expression     I>2σ(I)

_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-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 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)+(0.0498P)²+1.7253P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         16927
_refine_ls_number_parameters     1016
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0455
_refine_ls_wR_factor_ref         0.1164
_refine_ls_wR_factor_gt          0.1034
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_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
C11 C 0.10967(15) 0.49988(14) 0.72242(8) 0.0196(4) Uani 1 1 d . . .
H11 H 0.1120 0.4967 0.7663 0.024 Uiso 1 1 calc R . .
C12 C 0.17634(15) 0.56498(14) 0.67724(9) 0.0206(4) Uani 1 1 d . . .
C13 C 0.16309(17) 0.57373(16) 0.61297(9) 0.0278(5) Uani 1 1 d . . .
H13 H 0.2053 0.6186 0.5806 0.033 Uiso 1 1 calc R . .
C14 C 0.09026(16) 0.51851(15) 0.59664(9) 0.0266(4) Uani 1 1 d . . .
H14 H 0.0808 0.5266 0.5529 0.032 Uiso 1 1 calc R . .
N15 N 0.03093(12) 0.45221(12) 0.64144(7) 0.0210(3) Uani 1 1 d . . .
C16 C -0.04700(15) 0.39231(16) 0.62193(9) 0.0251(4) Uani 1 1 d . . .
H16A H -0.0197 0.3229 0.6255 0.030 Uiso 1 1 calc R . .
H16B H -0.0603 0.4226 0.5770 0.030 Uiso 1 1 calc R . .
C17 C -0.14726(16) 0.39027(17) 0.66431(9) 0.0277(4) Uani 1 1 d . . .
H17A H -0.1979 0.3465 0.6533 0.033 Uiso 1 1 calc R . .
H17B H -0.1781 0.4590 0.6572 0.033 Uiso 1 1 calc R . .
C18 C -0.12736(15) 0.35130(14) 0.73358(9) 0.0218(4) Uani 1 1 d . . .
C19 C -0.20371(15) 0.30122(15) 0.78006(10) 0.0260(4) Uani 1 1 d . . .
C110 C -0.18132(16) 0.26677(15) 0.84370(10) 0.0269(4) Uani 1 1 d . . .
C111 C -0.07999(16) 0.27670(14) 0.86013(9) 0.0243(4) Uani 1 1 d . . .
C112 C -0.04790(16) 0.24779(16) 0.92728(9) 0.0297(5) Uani 1 1 d . . .
H11A H -0.0134 0.1805 0.9359 0.036 Uiso 1 1 calc R . .
H11B H -0.1104 0.2448 0.9580 0.036 Uiso 1 1 calc R . .
C113 C 0.02677(17) 0.32521(16) 0.93500(9) 0.0292(5) Uani 1 1 d . . .
H11C H -0.0079 0.3924 0.9268 0.035 Uiso 1 1 calc R . .
H11D H 0.0479 0.3076 0.9791 0.035 Uiso 1 1 calc R . .
N114 N 0.12011(13) 0.32701(12) 0.88895(7) 0.0219(3) Uani 1 1 d . . .
C115 C 0.21657(17) 0.33946(15) 0.90703(9) 0.0283(5) Uani 1 1 d . . .
H115 H 0.2228 0.3477 0.9485 0.034 Uiso 1 1 calc R . .
C116 C 0.30285(17) 0.34010(16) 0.86654(10) 0.0312(5) Uani 1 1 d . . .
H116 H 0.3685 0.3565 0.8776 0.037 Uiso 1 1 calc R . .
C117 C 0.29601(16) 0.31658(15) 0.80784(9) 0.0261(4) Uani 1 1 d . . .
C118 C 0.38467(17) 0.30873(18) 0.76533(11) 0.0386(6) Uani 1 1 d . . .
H118 H 0.4519 0.3234 0.7750 0.046 Uiso 1 1 calc R . .
C119 C 0.37477(18) 0.28051(18) 0.71079(11) 0.0407(6) Uani 1 1 d . . .
H119 H 0.4348 0.2775 0.6822 0.049 Uiso 1 1 calc R . .
C120 C 0.27619(17) 0.25571(16) 0.69644(10) 0.0327(5) Uani 1 1 d . . .
H120 H 0.2706 0.2325 0.6595 0.039 Uiso 1 1 calc R . .
C121 C 0.18897(16) 0.26498(14) 0.73543(9) 0.0245(4) Uani 1 1 d . . .
H121 H 0.1227 0.2487 0.7252 0.029 Uiso 1 1 calc R . .
C122 C 0.19605(15) 0.29868(14) 0.79118(8) 0.0204(4) Uani 1 1 d . . .
C123 C 0.10632(15) 0.31565(13) 0.83107(8) 0.0191(4) Uani 1 1 d . . .
C124 C -0.00196(15) 0.32087(14) 0.81287(9) 0.0203(4) Uani 1 1 d . . .
C125 C -0.02841(14) 0.36649(13) 0.75052(8) 0.0188(4) Uani 1 1 d . . .
C126 C 0.04041(14) 0.44002(14) 0.70468(8) 0.0188(4) Uani 1 1 d . . .
C127 C 0.25538(16) 0.61958(14) 0.69772(9) 0.0234(4) Uani 1 1 d . . .
H127 H 0.2515 0.6207 0.7413 0.028 Uiso 1 1 calc R . .
C128 C 0.33307(16) 0.66816(15) 0.65803(9) 0.0257(4) Uani 1 1 d . . .
H128 H 0.3315 0.6690 0.6144 0.031 Uiso 1 1 calc R . .
C129 C 0.41994(16) 0.72001(15) 0.67315(9) 0.0247(4) Uani 1 1 d . . .
C130 C 0.42963(16) 0.73545(15) 0.73351(9) 0.0270(4) Uani 1 1 d . . .
H130 H 0.3757 0.7143 0.7668 0.032 Uiso 1 1 calc R . .
C131 C 0.51655(17) 0.78094(15) 0.74501(10) 0.0291(5) Uani 1 1 d . . .
H131 H 0.5222 0.7910 0.7861 0.035 Uiso 1 1 calc R . .
C132 C 0.59665(16) 0.81237(15) 0.69649(10) 0.0268(4) Uani 1 1 d . . .
C133 C 0.58833(16) 0.79913(15) 0.63631(10) 0.0277(4) Uani 1 1 d . . .
H133 H 0.6422 0.8211 0.6031 0.033 Uiso 1 1 calc R . .
C134 C 0.50034(16) 0.75340(15) 0.62522(9) 0.0278(4) Uani 1 1 d . . .
H134 H 0.4945 0.7445 0.5839 0.033 Uiso 1 1 calc R . .
C135 C -0.26577(18) 0.21782(18) 0.89394(11) 0.0404(6) Uani 1 1 d . . .
H13A H -0.3220 0.2671 0.8975 0.061 Uiso 1 1 calc R . .
H13B H -0.2361 0.1937 0.9350 0.061 Uiso 1 1 calc R . .
H13C H -0.2940 0.1609 0.8819 0.061 Uiso 1 1 calc R . .
C136 C -0.31200(16) 0.28703(18) 0.76206(12) 0.0371(5) Uani 1 1 d . . .
H13D H -0.3214 0.2159 0.7640 0.056 Uiso 1 1 calc R . .
H13E H -0.3200 0.3277 0.7187 0.056 Uiso 1 1 calc R . .
H13F H -0.3647 0.3083 0.7918 0.056 Uiso 1 1 calc R . .
C137 C 0.76015(17) 0.89583(17) 0.66413(11) 0.0371(5) Uani 1 1 d . . .
H13G H 0.7838 0.8453 0.6410 0.056 Uiso 1 1 calc R . .
H13H H 0.8194 0.9158 0.6830 0.056 Uiso 1 1 calc R . .
H13I H 0.7316 0.9549 0.6346 0.056 Uiso 1 1 calc R . .
O11 O -0.43846(13) 0.44752(13) 0.87115(8) 0.0443(4) Uani 1 1 d . . .
C21 C 0.10969(15) 0.83291(14) 0.69404(9) 0.0225(4) Uani 1 1 d . . .
H21 H 0.1205 0.8193 0.7380 0.027 Uiso 1 1 calc R . .
C22 C 0.03361(16) 0.77982(15) 0.67528(9) 0.0245(4) Uani 1 1 d . . .
C23 C 0.02547(17) 0.79768(17) 0.60919(10) 0.0329(5) Uani 1 1 d . . .
H23 H -0.0239 0.7621 0.5940 0.040 Uiso 1 1 calc R . .
C24 C 0.08821(18) 0.86559(18) 0.56753(10) 0.0342(5) Uani 1 1 d . . .
H24 H 0.0833 0.8756 0.5231 0.041 Uiso 1 1 calc R . .
N25 N 0.15750(13) 0.91944(13) 0.58733(7) 0.0261(4) Uani 1 1 d . . .
C26 C 0.22198(18) 0.99497(17) 0.54021(9) 0.0329(5) Uani 1 1 d . . .
H26A H 0.1952 1.0635 0.5404 0.039 Uiso 1 1 calc R . .
H26B H 0.2180 0.9854 0.4970 0.039 Uiso 1 1 calc R . .
C27 C 0.33342(17) 0.98380(16) 0.55652(9) 0.0302(5) Uani 1 1 d . . .
H27A H 0.3758 1.0372 0.5267 0.036 Uiso 1 1 calc R . .
H27B H 0.3623 0.9179 0.5520 0.036 Uiso 1 1 calc R . .
C28 C 0.33958(16) 0.99114(14) 0.62389(9) 0.0235(4) Uani 1 1 d . . .
C29 C 0.43012(16) 1.02616(14) 0.64214(9) 0.0249(4) Uani 1 1 d . . .
C210 C 0.43542(16) 1.02884(14) 0.70526(9) 0.0245(4) Uani 1 1 d . . .
C211 C 0.34786(16) 1.00113(14) 0.74906(9) 0.0237(4) Uani 1 1 d . . .
C212 C 0.35106(16) 0.99284(16) 0.81934(9) 0.0282(4) Uani 1 1 d . . .
H21A H 0.3298 1.0579 0.8288 0.034 Uiso 1 1 calc R . .
H21B H 0.4231 0.9758 0.8317 0.034 Uiso 1 1 calc R . .
C213 C 0.27712(16) 0.91153(16) 0.85656(9) 0.0276(4) Uani 1 1 d . . .
H21C H 0.2991 0.8462 0.8478 0.033 Uiso 1 1 calc R . .
H21D H 0.2780 0.9049 0.9028 0.033 Uiso 1 1 calc R . .
N214 N 0.17062(13) 0.93966(12) 0.83690(7) 0.0237(4) Uani 1 1 d . . .
C215 C 0.08838(17) 0.93112(16) 0.88266(9) 0.0291(5) Uani 1 1 d . . .
H215 H 0.1001 0.9047 0.9262 0.035 Uiso 1 1 calc R . .
C216 C -0.00851(17) 0.95965(16) 0.86672(10) 0.0313(5) Uani 1 1 d . . .
H216 H -0.0656 0.9489 0.8987 0.038 Uiso 1 1 calc R . .
C217 C -0.02614(16) 1.00551(15) 0.80278(9) 0.0259(4) Uani 1 1 d . . .
C218 C -0.12539(17) 1.04282(16) 0.78457(10) 0.0312(5) Uani 1 1 d . . .
H218 H -0.1837 1.0342 0.8157 0.037 Uiso 1 1 calc R . .
C219 C -0.13883(17) 1.09097(16) 0.72309(11) 0.0325(5) Uani 1 1 d . . .
H219 H -0.2067 1.1134 0.7112 0.039 Uiso 1 1 calc R . .
C220 C -0.05227(16) 1.10782(15) 0.67680(10) 0.0284(5) Uani 1 1 d . . .
H220 H -0.0619 1.1443 0.6343 0.034 Uiso 1 1 calc R . .
C221 C 0.04485(16) 1.07234(14) 0.69241(9) 0.0240(4) Uani 1 1 d . . .
H221 H 0.1025 1.0848 0.6608 0.029 Uiso 1 1 calc R . .
C222 C 0.06071(15) 1.01691(14) 0.75552(9) 0.0213(4) Uani 1 1 d . . .
C223 C 0.15941(15) 0.97513(14) 0.77435(8) 0.0210(4) Uani 1 1 d . . .
C224 C 0.25384(15) 0.97607(14) 0.72979(8) 0.0212(4) Uani 1 1 d . . .
C225 C 0.25264(15) 0.96219(14) 0.66778(9) 0.0221(4) Uani 1 1 d . . .
C226 C 0.17011(15) 0.90510(14) 0.65046(9) 0.0225(4) Uani 1 1 d . . .
C227 C -0.03424(16) 0.71047(15) 0.72251(10) 0.0266(4) Uani 1 1 d . . .
H227 H -0.0203 0.6973 0.7659 0.032 Uiso 1 1 calc R . .
C228 C -0.11488(16) 0.66423(15) 0.70845(10) 0.0274(4) Uani 1 1 d . . .
H228 H -0.1227 0.6733 0.6644 0.033 Uiso 1 1 calc R . .
C229 C -0.19226(16) 0.60149(15) 0.75293(10) 0.0272(4) Uani 1 1 d . . .
C230 C -0.18087(17) 0.56262(16) 0.81767(10) 0.0307(5) Uani 1 1 d . . .
H230 H -0.1171 0.5717 0.8340 0.037 Uiso 1 1 calc R . .
C231 C -0.26105(18) 0.51095(16) 0.85844(10) 0.0337(5) Uani 1 1 d . . .
H231 H -0.2522 0.4850 0.9025 0.040 Uiso 1 1 calc R . .
C232 C -0.35471(17) 0.49713(16) 0.83475(11) 0.0327(5) Uani 1 1 d . . .
C233 C -0.36571(17) 0.53228(16) 0.77035(11) 0.0332(5) Uani 1 1 d . . .
H233 H -0.4288 0.5213 0.7539 0.040 Uiso 1 1 calc R . .
C234 C -0.28575(17) 0.58308(15) 0.73009(11) 0.0304(5) Uani 1 1 d . . .
H234 H -0.2940 0.6062 0.6858 0.036 Uiso 1 1 calc R . .
C235 C 0.52112(17) 1.05493(16) 0.59208(10) 0.0318(5) Uani 1 1 d . . .
H23A H 0.5823 1.0679 0.6122 0.048 Uiso 1 1 calc R . .
H23B H 0.5026 1.1157 0.5600 0.048 Uiso 1 1 calc R . .
H23C H 0.5375 0.9998 0.5716 0.048 Uiso 1 1 calc R . .
C236 C 0.53266(17) 1.06139(17) 0.72768(10) 0.0321(5) Uani 1 1 d . . .
H23D H 0.5780 1.0026 0.7425 0.048 Uiso 1 1 calc R . .
H23E H 0.5130 1.0929 0.7628 0.048 Uiso 1 1 calc R . .
H23F H 0.5702 1.1098 0.6924 0.048 Uiso 1 1 calc R . .
C237 C -0.4410(2) 0.4315(2) 0.93892(13) 0.0605(8) Uani 1 1 d . . .
H23G H -0.3867 0.3819 0.9553 0.091 Uiso 1 1 calc R . .
H23H H -0.5097 0.4066 0.9587 0.091 Uiso 1 1 calc R . .
H23I H -0.4281 0.4952 0.9491 0.091 Uiso 1 1 calc R . .
O21 O 0.68088(11) 0.85418(11) 0.71343(7) 0.0347(4) Uani 1 1 d . . .
C1 C 0.70951(18) 0.66956(17) 0.49496(11) 0.0360(5) Uani 1 1 d . . .
C2 C 0.62239(19) 0.34697(18) 0.55095(10) 0.0371(5) Uani 1 1 d . . .
C3 C 0.65245(19) 0.94168(18) 0.00632(11) 0.0392(5) Uani 1 1 d . . .
C4 C 0.2009(2) 0.60165(19) 0.94126(11) 0.0468(6) Uani 1 1 d . . .
F1 F 0.66907(12) 0.61799(12) 0.55176(7) 0.0595(4) Uani 1 1 d . . .
F2 F 0.64845(11) 0.75059(12) 0.47647(8) 0.0574(4) Uani 1 1 d . . .
F3 F 0.70525(13) 0.61328(12) 0.45426(7) 0.0577(4) Uani 1 1 d . . .
F4 F 0.63262(13) 0.40123(12) 0.59218(8) 0.0624(4) Uani 1 1 d . . .
F5 F 0.53063(11) 0.30144(12) 0.56775(8) 0.0578(4) Uani 1 1 d . . .
F6 F 0.61634(14) 0.41029(12) 0.49383(7) 0.0658(5) Uani 1 1 d . . .
F7 F 0.60670(12) 1.01372(13) 0.03075(8) 0.0621(4) Uani 1 1 d . . .
F8 F 0.63998(12) 0.96692(12) -0.05581(7) 0.0542(4) Uani 1 1 d . . .
F9 F 0.60089(12) 0.85722(13) 0.03182(8) 0.0646(5) Uani 1 1 d . . .
F10 F 0.28831(14) 0.56028(14) 0.92148(9) 0.0694(5) Uani 1 1 d . . .
F11 F 0.15601(17) 0.53273(13) 0.99018(7) 0.0766(6) Uani 1 1 d . . .
F12 F 0.22789(16) 0.67783(13) 0.96392(8) 0.0731(5) Uani 1 1 d . . .
O1T O 0.89774(13) 0.61460(13) 0.51909(8) 0.0495(4) Uani 1 1 d . . .
O2T O 0.87026(13) 0.76292(12) 0.43377(7) 0.0436(4) Uani 1 1 d . . .
O3T O 0.82683(13) 0.76834(13) 0.54319(8) 0.0444(4) Uani 1 1 d . . .
O4T O 0.82077(12) 0.31650(13) 0.53450(7) 0.0434(4) Uani 1 1 d . . .
O5T O 0.70557(13) 0.20957(12) 0.50132(7) 0.0400(4) Uani 1 1 d . . .
O6T O 0.71894(13) 0.19380(13) 0.61407(7) 0.0435(4) Uani 1 1 d . . .
O7T O 0.79005(12) 0.89609(11) 0.08841(6) 0.0330(3) Uani 1 1 d . . .
O8T O 0.82667(12) 0.85144(11) -0.01230(7) 0.0355(4) Uani 1 1 d . . .
O9T O 0.83146(13) 1.02539(11) -0.00883(7) 0.0375(4) Uani 1 1 d . . .
O10T O 0.17705(14) 0.71571(12) 0.83140(7) 0.0427(4) Uani 1 1 d . . .
O11T O 0.02686(15) 0.68654(15) 0.90932(9) 0.0578(5) Uani 1 1 d . . .
O12T O 0.09418(14) 0.55393(11) 0.86086(7) 0.0406(4) Uani 1 1 d . . .
S1 S 0.84189(4) 0.70754(4) 0.49807(2) 0.02809(12) Uani 1 1 d . . .
S2 S 0.72943(4) 0.25616(4) 0.54998(2) 0.02930(13) Uani 1 1 d . . .
S3 S 0.79092(4) 0.92686(4) 0.02012(2) 0.02701(12) Uani 1 1 d . . .
S4 S 0.11469(5) 0.64403(4) 0.87883(2) 0.03001(13) Uani 1 1 d . . .
N1S N 0.6644(3) 0.7267(2) 0.91441(11) 0.0647(7) Uani 1 1 d . . .
C1S C 0.7535(3) 0.7770(2) 0.87202(12) 0.0618(8) Uani 1 1 d . . .
H1S1 H 0.8191 0.7448 0.8871 0.093 Uiso 1 1 calc R . .
H1S2 H 0.7531 0.8482 0.8723 0.093 Uiso 1 1 calc R . .
H1S3 H 0.7477 0.7714 0.8286 0.093 Uiso 1 1 calc R . .
O1S O 0.5767(2) 0.7567(3) 0.90091(12) 0.1106(11) Uani 1 1 d . . .
O2S O 0.6821(2) 0.65888(16) 0.96077(9) 0.0743(7) 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
C11 C126 1.382(3) . ?
C11 C12 1.398(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.401(3) . ?
C12 C127 1.455(3) . ?
C13 C14 1.357(3) . ?
C13 H13 0.9500 . ?
C14 N15 1.350(2) . ?
C14 H14 0.9500 . ?
N15 C126 1.362(2) . ?
N15 C16 1.481(2) . ?
C16 C17 1.508(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.510(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C125 1.396(3) . ?
C18 C19 1.403(3) . ?
C19 C110 1.400(3) . ?
C19 C136 1.515(3) . ?
C110 C111 1.404(3) . ?
C110 C135 1.511(3) . ?
C111 C124 1.402(3) . ?
C111 C112 1.508(3) . ?
C112 C113 1.514(3) . ?
C112 H11A 0.9900 . ?
C112 H11B 0.9900 . ?
C113 N114 1.484(2) . ?
C113 H11C 0.9900 . ?
C113 H11D 0.9900 . ?
N114 C123 1.340(2) . ?
N114 C115 1.366(3) . ?
C115 C116 1.347(3) . ?
C115 H115 0.9500 . ?
C116 C117 1.409(3) . ?
C116 H116 0.9500 . ?
C117 C122 1.415(3) . ?
C117 C118 1.416(3) . ?
C118 C119 1.360(3) . ?
C118 H118 0.9500 . ?
C119 C120 1.409(3) . ?
C119 H119 0.9500 . ?
C120 C121 1.361(3) . ?
C120 H120 0.9500 . ?
C121 C122 1.419(3) . ?
C121 H121 0.9500 . ?
C122 C123 1.424(3) . ?
C123 C124 1.477(3) . ?
C124 C125 1.411(3) . ?
C125 C126 1.479(2) . ?
C127 C128 1.336(3) . ?
C127 H127 0.9500 . ?
C128 C129 1.456(3) . ?
C128 H128 0.9500 . ?
C129 C134 1.398(3) . ?
C129 C130 1.403(3) . ?
C130 C131 1.376(3) . ?
C130 H130 0.9500 . ?
C131 C132 1.399(3) . ?
C131 H131 0.9500 . ?
C132 O21 1.370(2) . ?
C132 C133 1.384(3) . ?
C133 C134 1.386(3) . ?
C133 H133 0.9500 . ?
C134 H134 0.9500 . ?
C135 H13A 0.9800 . ?
C135 H13B 0.9800 . ?
C135 H13C 0.9800 . ?
C136 H13D 0.9800 . ?
C136 H13E 0.9800 . ?
C136 H13F 0.9800 . ?
C137 O21 1.429(3) . ?
C137 H13G 0.9800 . ?
C137 H13H 0.9800 . ?
C137 H13I 0.9800 . ?
O11 C232 1.368(3) . ?
O11 C237 1.434(3) . ?
C21 C226 1.389(3) . ?
C21 C22 1.395(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.411(3) . ?
C22 C227 1.457(3) . ?
C23 C24 1.354(3) . ?
C23 H23 0.9500 . ?
C24 N25 1.349(3) . ?
C24 H24 0.9500 . ?
N25 C226 1.364(2) . ?
N25 C26 1.477(3) . ?
C26 C27 1.500(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.507(3) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C225 1.399(3) . ?
C28 C29 1.406(3) . ?
C29 C210 1.394(3) . ?
C29 C235 1.512(3) . ?
C210 C211 1.401(3) . ?
C210 C236 1.509(3) . ?
C211 C224 1.401(3) . ?
C211 C212 1.511(3) . ?
C212 C213 1.512(3) . ?
C212 H21A 0.9900 . ?
C212 H21B 0.9900 . ?
C213 N214 1.479(3) . ?
C213 H21C 0.9900 . ?
C213 H21D 0.9900 . ?
N214 C223 1.345(2) . ?
N214 C215 1.368(2) . ?
C215 C216 1.340(3) . ?
C215 H215 0.9500 . ?
C216 C217 1.410(3) . ?
C216 H216 0.9500 . ?
C217 C218 1.409(3) . ?
C217 C222 1.428(3) . ?
C218 C219 1.358(3) . ?
C218 H218 0.9500 . ?
C219 C220 1.412(3) . ?
C219 H219 0.9500 . ?
C220 C221 1.362(3) . ?
C220 H220 0.9500 . ?
C221 C222 1.421(3) . ?
C221 H221 0.9500 . ?
C222 C223 1.423(3) . ?
C223 C224 1.477(3) . ?
C224 C225 1.414(3) . ?
C225 C226 1.477(3) . ?
C227 C228 1.337(3) . ?
C227 H227 0.9500 . ?
C228 C229 1.459(3) . ?
C228 H228 0.9500 . ?
C229 C230 1.394(3) . ?
C229 C234 1.400(3) . ?
C230 C231 1.384(3) . ?
C230 H230 0.9500 . ?
C231 C232 1.393(3) . ?
C231 H231 0.9500 . ?
C232 C233 1.381(3) . ?
C233 C234 1.373(3) . ?
C233 H233 0.9500 . ?
C234 H234 0.9500 . ?
C235 H23A 0.9800 . ?
C235 H23B 0.9800 . ?
C235 H23C 0.9800 . ?
C236 H23D 0.9800 . ?
C236 H23E 0.9800 . ?
C236 H23F 0.9800 . ?
C237 H23G 0.9800 . ?
C237 H23H 0.9800 . ?
C237 H23I 0.9800 . ?
C1 F3 1.324(3) . ?
C1 F1 1.327(3) . ?
C1 F2 1.333(3) . ?
C1 S1 1.812(2) . ?
C2 F4 1.325(3) . ?
C2 F6 1.331(3) . ?
C2 F5 1.333(3) . ?
C2 S2 1.820(3) . ?
C3 F9 1.326(3) . ?
C3 F7 1.331(3) . ?
C3 F8 1.333(3) . ?
C3 S3 1.827(3) . ?
C4 F10 1.322(3) . ?
C4 F11 1.333(3) . ?
C4 F12 1.338(3) . ?
C4 S4 1.802(3) . ?
O1T S1 1.4297(17) . ?
O2T S1 1.4332(16) . ?
O3T S1 1.4404(16) . ?
O4T S2 1.4288(15) . ?
O5T S2 1.4342(15) . ?
O6T S2 1.4368(15) . ?
O7T S3 1.4383(14) . ?
O8T S3 1.4349(15) . ?
O9T S3 1.4362(15) . ?
O10T S4 1.4375(16) . ?
O11T S4 1.4335(18) . ?
O12T S4 1.4333(16) . ?
N1S O2S 1.219(3) . ?
N1S O1S 1.220(4) . ?
N1S C1S 1.476(4) . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 0.9800 . ?

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
C126 C11 C12 121.50(17) . . ?
C126 C11 H11 119.3 . . ?
C12 C11 H11 119.3 . . ?
C11 C12 C13 116.95(17) . . ?
C11 C12 C127 120.12(16) . . ?
C13 C12 C127 122.93(17) . . ?
C14 C13 C12 120.36(18) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
N15 C14 C13 121.21(17) . . ?
N15 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C14 N15 C126 121.18(16) . . ?
C14 N15 C16 119.80(15) . . ?
C126 N15 C16 119.02(15) . . ?
N15 C16 C17 109.27(15) . . ?
N15 C16 H16A 109.8 . . ?
C17 C16 H16A 109.8 . . ?
N15 C16 H16B 109.8 . . ?
C17 C16 H16B 109.8 . . ?
H16A C16 H16B 108.3 . . ?
C16 C17 C18 110.75(17) . . ?
C16 C17 H17A 109.5 . . ?
C18 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C18 C17 H17B 109.5 . . ?
H17A C17 H17B 108.1 . . ?
C125 C18 C19 120.13(17) . . ?
C125 C18 C17 117.37(16) . . ?
C19 C18 C17 122.50(17) . . ?
C110 C19 C18 120.24(18) . . ?
C110 C19 C136 119.54(18) . . ?
C18 C19 C136 120.19(19) . . ?
C19 C110 C111 119.63(17) . . ?
C19 C110 C135 119.83(19) . . ?
C111 C110 C135 120.54(19) . . ?
C124 C111 C110 119.94(18) . . ?
C124 C111 C112 115.45(17) . . ?
C110 C111 C112 124.53(17) . . ?
C111 C112 C113 109.07(16) . . ?
C111 C112 H11A 109.9 . . ?
C113 C112 H11A 109.9 . . ?
C111 C112 H11B 109.9 . . ?
C113 C112 H11B 109.9 . . ?
H11A C112 H11B 108.3 . . ?
N114 C113 C112 108.58(16) . . ?
N114 C113 H11C 110.0 . . ?
C112 C113 H11C 110.0 . . ?
N114 C113 H11D 110.0 . . ?
C112 C113 H11D 110.0 . . ?
H11C C113 H11D 108.4 . . ?
C123 N114 C115 122.45(16) . . ?
C123 N114 C113 118.38(16) . . ?
C115 N114 C113 119.17(16) . . ?
C116 C115 N114 120.50(18) . . ?
C116 C115 H115 119.8 . . ?
N114 C115 H115 119.8 . . ?
C115 C116 C117 120.18(19) . . ?
C115 C116 H116 119.9 . . ?
C117 C116 H116 119.9 . . ?
C116 C117 C122 118.38(18) . . ?
C116 C117 C118 122.9(2) . . ?
C122 C117 C118 118.69(19) . . ?
C119 C118 C117 120.8(2) . . ?
C119 C118 H118 119.6 . . ?
C117 C118 H118 119.6 . . ?
C118 C119 C120 120.5(2) . . ?
C118 C119 H119 119.8 . . ?
C120 C119 H119 119.8 . . ?
C121 C120 C119 120.2(2) . . ?
C121 C120 H120 119.9 . . ?
C119 C120 H120 119.9 . . ?
C120 C121 C122 120.66(19) . . ?
C120 C121 H121 119.7 . . ?
C122 C121 H121 119.7 . . ?
C117 C122 C121 118.94(17) . . ?
C117 C122 C123 118.53(17) . . ?
C121 C122 C123 122.53(17) . . ?
N114 C123 C122 118.43(17) . . ?
N114 C123 C124 117.50(16) . . ?
C122 C123 C124 124.07(16) . . ?
C111 C124 C125 119.81(17) . . ?
C111 C124 C123 117.47(16) . . ?
C125 C124 C123 122.71(16) . . ?
C18 C125 C124 119.33(16) . . ?
C18 C125 C126 118.29(16) . . ?
C124 C125 C126 121.95(16) . . ?
N15 C126 C11 118.52(16) . . ?
N15 C126 C125 117.61(16) . . ?
C11 C126 C125 123.80(16) . . ?
C128 C127 C12 122.95(17) . . ?
C128 C127 H127 118.5 . . ?
C12 C127 H127 118.5 . . ?
C127 C128 C129 128.21(18) . . ?
C127 C128 H128 115.9 . . ?
C129 C128 H128 115.9 . . ?
C134 C129 C130 117.97(18) . . ?
C134 C129 C128 118.01(17) . . ?
C130 C129 C128 123.98(17) . . ?
C131 C130 C129 120.65(18) . . ?
C131 C130 H130 119.7 . . ?
C129 C130 H130 119.7 . . ?
C130 C131 C132 120.28(19) . . ?
C130 C131 H131 119.9 . . ?
C132 C131 H131 119.9 . . ?
O21 C132 C133 124.25(18) . . ?
O21 C132 C131 115.57(18) . . ?
C133 C132 C131 120.17(18) . . ?
C132 C133 C134 119.07(18) . . ?
C132 C133 H133 120.5 . . ?
C134 C133 H133 120.5 . . ?
C133 C134 C129 121.86(19) . . ?
C133 C134 H134 119.1 . . ?
C129 C134 H134 119.1 . . ?
C110 C135 H13A 109.5 . . ?
C110 C135 H13B 109.5 . . ?
H13A C135 H13B 109.5 . . ?
C110 C135 H13C 109.5 . . ?
H13A C135 H13C 109.5 . . ?
H13B C135 H13C 109.5 . . ?
C19 C136 H13D 109.5 . . ?
C19 C136 H13E 109.5 . . ?
H13D C136 H13E 109.5 . . ?
C19 C136 H13F 109.5 . . ?
H13D C136 H13F 109.5 . . ?
H13E C136 H13F 109.5 . . ?
O21 C137 H13G 109.5 . . ?
O21 C137 H13H 109.5 . . ?
H13G C137 H13H 109.5 . . ?
O21 C137 H13I 109.5 . . ?
H13G C137 H13I 109.5 . . ?
H13H C137 H13I 109.5 . . ?
C232 O11 C237 117.57(18) . . ?
C226 C21 C22 122.00(18) . . ?
C226 C21 H21 119.0 . . ?
C22 C21 H21 119.0 . . ?
C21 C22 C23 116.85(18) . . ?
C21 C22 C227 120.71(17) . . ?
C23 C22 C227 122.44(18) . . ?
C24 C23 C22 119.89(19) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
N25 C24 C23 121.83(19) . . ?
N25 C24 H24 119.1 . . ?
C23 C24 H24 119.1 . . ?
C24 N25 C226 121.24(17) . . ?
C24 N25 C26 119.92(16) . . ?
C226 N25 C26 118.83(17) . . ?
N25 C26 C27 109.51(17) . . ?
N25 C26 H26A 109.8 . . ?
C27 C26 H26A 109.8 . . ?
N25 C26 H26B 109.8 . . ?
C27 C26 H26B 109.8 . . ?
H26A C26 H26B 108.2 . . ?
C26 C27 C28 110.25(16) . . ?
C26 C27 H27A 109.6 . . ?
C28 C27 H27A 109.6 . . ?
C26 C27 H27B 109.6 . . ?
C28 C27 H27B 109.6 . . ?
H27A C27 H27B 108.1 . . ?
C225 C28 C29 120.89(17) . . ?
C225 C28 C27 118.12(18) . . ?
C29 C28 C27 120.98(17) . . ?
C210 C29 C28 119.94(17) . . ?
C210 C29 C235 122.32(19) . . ?
C28 C29 C235 117.67(18) . . ?
C29 C210 C211 119.14(18) . . ?
C29 C210 C236 121.81(17) . . ?
C211 C210 C236 119.05(18) . . ?
C224 C211 C210 121.16(17) . . ?
C224 C211 C212 116.74(16) . . ?
C210 C211 C212 122.06(18) . . ?
C211 C212 C213 108.73(16) . . ?
C211 C212 H21A 109.9 . . ?
C213 C212 H21A 109.9 . . ?
C211 C212 H21B 109.9 . . ?
C213 C212 H21B 109.9 . . ?
H21A C212 H21B 108.3 . . ?
N214 C213 C212 108.34(16) . . ?
N214 C213 H21C 110.0 . . ?
C212 C213 H21C 110.0 . . ?
N214 C213 H21D 110.0 . . ?
C212 C213 H21D 110.0 . . ?
H21C C213 H21D 108.4 . . ?
C223 N214 C215 122.75(18) . . ?
C223 N214 C213 118.09(16) . . ?
C215 N214 C213 119.14(16) . . ?
C216 C215 N214 120.73(19) . . ?
C216 C215 H215 119.6 . . ?
N214 C215 H215 119.6 . . ?
C215 C216 C217 120.37(18) . . ?
C215 C216 H216 119.8 . . ?
C217 C216 H216 119.8 . . ?
C218 C217 C216 122.23(18) . . ?
C218 C217 C222 119.30(18) . . ?
C216 C217 C222 118.44(19) . . ?
C219 C218 C217 120.83(19) . . ?
C219 C218 H218 119.6 . . ?
C217 C218 H218 119.6 . . ?
C218 C219 C220 120.2(2) . . ?
C218 C219 H219 119.9 . . ?
C220 C219 H219 119.9 . . ?
C221 C220 C219 120.7(2) . . ?
C221 C220 H220 119.7 . . ?
C219 C220 H220 119.7 . . ?
C220 C221 C222 120.56(18) . . ?
C220 C221 H221 119.7 . . ?
C222 C221 H221 119.7 . . ?
C221 C222 C223 123.27(17) . . ?
C221 C222 C217 118.20(19) . . ?
C223 C222 C217 118.50(17) . . ?
N214 C223 C222 118.51(16) . . ?
N214 C223 C224 117.21(18) . . ?
C222 C223 C224 124.06(17) . . ?
C211 C224 C225 119.00(17) . . ?
C211 C224 C223 116.76(16) . . ?
C225 C224 C223 123.99(17) . . ?
C28 C225 C224 118.87(18) . . ?
C28 C225 C226 118.27(16) . . ?
C224 C225 C226 122.26(16) . . ?
N25 C226 C21 118.04(17) . . ?
N25 C226 C225 117.74(16) . . ?
C21 C226 C225 124.07(17) . . ?
C228 C227 C22 123.98(19) . . ?
C228 C227 H227 118.0 . . ?
C22 C227 H227 118.0 . . ?
C227 C228 C229 127.48(19) . . ?
C227 C228 H228 116.3 . . ?
C229 C228 H228 116.3 . . ?
C230 C229 C234 117.83(19) . . ?
C230 C229 C228 123.87(19) . . ?
C234 C229 C228 118.22(19) . . ?
C231 C230 C229 121.0(2) . . ?
C231 C230 H230 119.5 . . ?
C229 C230 H230 119.5 . . ?
C230 C231 C232 119.8(2) . . ?
C230 C231 H231 120.1 . . ?
C232 C231 H231 120.1 . . ?
O11 C232 C233 116.06(19) . . ?
O11 C232 C231 124.2(2) . . ?
C233 C232 C231 119.7(2) . . ?
C234 C233 C232 120.2(2) . . ?
C234 C233 H233 119.9 . . ?
C232 C233 H233 119.9 . . ?
C233 C234 C229 121.3(2) . . ?
C233 C234 H234 119.3 . . ?
C229 C234 H234 119.3 . . ?
C29 C235 H23A 109.5 . . ?
C29 C235 H23B 109.5 . . ?
H23A C235 H23B 109.5 . . ?
C29 C235 H23C 109.5 . . ?
H23A C235 H23C 109.5 . . ?
H23B C235 H23C 109.5 . . ?
C210 C236 H23D 109.5 . . ?
C210 C236 H23E 109.5 . . ?
H23D C236 H23E 109.5 . . ?
C210 C236 H23F 109.5 . . ?
H23D C236 H23F 109.5 . . ?
H23E C236 H23F 109.5 . . ?
O11 C237 H23G 109.5 . . ?
O11 C237 H23H 109.5 . . ?
H23G C237 H23H 109.5 . . ?
O11 C237 H23I 109.5 . . ?
H23G C237 H23I 109.5 . . ?
H23H C237 H23I 109.5 . . ?
C132 O21 C137 117.54(16) . . ?
F3 C1 F1 108.19(18) . . ?
F3 C1 F2 107.91(19) . . ?
F1 C1 F2 107.41(19) . . ?
F3 C1 S1 111.83(16) . . ?
F1 C1 S1 111.43(16) . . ?
F2 C1 S1 109.91(15) . . ?
F4 C2 F6 107.7(2) . . ?
F4 C2 F5 106.62(19) . . ?
F6 C2 F5 107.39(19) . . ?
F4 C2 S2 112.07(16) . . ?
F6 C2 S2 111.42(17) . . ?
F5 C2 S2 111.35(16) . . ?
F9 C3 F7 108.1(2) . . ?
F9 C3 F8 107.14(19) . . ?
F7 C3 F8 107.3(2) . . ?
F9 C3 S3 111.75(17) . . ?
F7 C3 S3 111.34(16) . . ?
F8 C3 S3 111.07(16) . . ?
F10 C4 F11 106.8(2) . . ?
F10 C4 F12 107.3(2) . . ?
F11 C4 F12 107.3(2) . . ?
F10 C4 S4 112.23(17) . . ?
F11 C4 S4 111.6(2) . . ?
F12 C4 S4 111.31(18) . . ?
O1T S1 O2T 115.53(10) . . ?
O1T S1 O3T 115.46(11) . . ?
O2T S1 O3T 114.41(10) . . ?
O1T S1 C1 103.99(11) . . ?
O2T S1 C1 102.97(11) . . ?
O3T S1 C1 101.86(10) . . ?
O4T S2 O5T 114.71(9) . . ?
O4T S2 O6T 114.58(10) . . ?
O5T S2 O6T 115.90(10) . . ?
O4T S2 C2 103.94(11) . . ?
O5T S2 C2 102.90(10) . . ?
O6T S2 C2 102.29(11) . . ?
O8T S3 O9T 114.60(9) . . ?
O8T S3 O7T 115.19(9) . . ?
O9T S3 O7T 114.82(9) . . ?
O8T S3 C3 102.84(10) . . ?
O9T S3 C3 103.25(11) . . ?
O7T S3 C3 103.82(10) . . ?
O12T S4 O11T 115.33(12) . . ?
O12T S4 O10T 114.51(10) . . ?
O11T S4 O10T 114.81(11) . . ?
O12T S4 C4 103.53(11) . . ?
O11T S4 C4 103.50(12) . . ?
O10T S4 C4 102.82(12) . . ?
O2S N1S O1S 123.9(3) . . ?
O2S N1S C1S 118.7(3) . . ?
O1S N1S C1S 117.4(3) . . ?
N1S C1S H1S1 109.5 . . ?
N1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
N1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.053
####################################################################### 
# 
# 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_pr271_teply
_database_code_depnum_ccdc_archive 'CCDC 1004339'
_audit_update_record             
;
2014-05-20 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H26 N2, 2(C F3 O3 S)'
_chemical_formula_sum            'C26 H26 F6 N2 O6 S2'
_chemical_formula_weight         640.61
_chemical_compound_source        'synthesized by the authors'

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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   14.2532(9)
_cell_length_b                   8.9518(5)
_cell_length_c                   21.2552(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.286(2)
_cell_angle_gamma                90.00
_cell_volume                     2709.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9835
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      27.

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1320
_exptl_absorpt_coefficient_mu    0.284
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8920
_exptl_absorpt_correction_T_max  0.9496
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43735
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0160
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.43
_diffrn_reflns_theta_max         27.50
_reflns_number_total             6221
_reflns_number_gt                5347
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_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)+(0.0463P)²+1.5489P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6221
_refine_ls_number_parameters     380
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0339
_refine_ls_wR_factor_ref         0.0928
_refine_ls_wR_factor_gt          0.0878
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_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 0.76956(9) 0.79650(15) 0.35013(6) 0.0171(3) Uani 1 1 d . . .
H1 H 0.7538 0.7608 0.3090 0.021 Uiso 1 1 calc R . .
C2 C 0.86194(10) 0.78471(16) 0.37372(7) 0.0208(3) Uani 1 1 d . . .
C3 C 0.88262(10) 0.84138(18) 0.43357(7) 0.0242(3) Uani 1 1 d . . .
H3 H 0.9452 0.8379 0.4506 0.029 Uiso 1 1 calc R . .
C4 C 0.81329(10) 0.90208(17) 0.46797(7) 0.0223(3) Uani 1 1 d . . .
H4 H 0.8282 0.9404 0.5088 0.027 Uiso 1 1 calc R . .
N5 N 0.72392(8) 0.90847(13) 0.44476(5) 0.0169(2) Uani 1 1 d . . .
C6 C 0.65162(10) 0.97116(17) 0.48555(7) 0.0215(3) Uani 1 1 d . . .
H6A H 0.6118 1.0426 0.4610 0.026 Uiso 1 1 calc R . .
H6B H 0.6827 1.0262 0.5210 0.026 Uiso 1 1 calc R . .
C7 C 0.59062(10) 0.84773(19) 0.51116(7) 0.0242(3) Uani 1 1 d . . .
H7A H 0.5369 0.8935 0.5321 0.029 Uiso 1 1 calc R . .
H7B H 0.6278 0.7908 0.5434 0.029 Uiso 1 1 calc R . .
C8 C 0.55301(10) 0.73914(16) 0.46017(6) 0.0211(3) Uani 1 1 d . . .
H8A H 0.6009 0.6613 0.4533 0.025 Uiso 1 1 calc R . .
H8B H 0.4962 0.6890 0.4752 0.025 Uiso 1 1 calc R . .
C9 C 0.52894(9) 0.81594(15) 0.39842(6) 0.0164(3) Uani 1 1 d . . .
C10 C 0.43629(9) 0.82961(15) 0.37619(6) 0.0177(3) Uani 1 1 d . . .
H10 H 0.3872 0.7935 0.4010 0.021 Uiso 1 1 calc R . .
C11 C 0.41452(9) 0.89533(15) 0.31826(7) 0.0181(3) Uani 1 1 d . . .
H11 H 0.3506 0.9042 0.3042 0.022 Uiso 1 1 calc R . .
C12 C 0.48446(9) 0.94825(15) 0.28044(6) 0.0159(3) Uani 1 1 d . . .
C13 C 0.46114(10) 1.01387(16) 0.21610(6) 0.0193(3) Uani 1 1 d . . .
H13A H 0.4905 1.1137 0.2132 0.023 Uiso 1 1 calc R . .
H13B H 0.3923 1.0268 0.2109 0.023 Uiso 1 1 calc R . .
C14 C 0.49547(10) 0.91472(17) 0.16267(7) 0.0226(3) Uani 1 1 d . . .
H14A H 0.4511 0.8306 0.1559 0.027 Uiso 1 1 calc R . .
H14B H 0.4956 0.9739 0.1233 0.027 Uiso 1 1 calc R . .
C15 C 0.59372(10) 0.85260(16) 0.17664(7) 0.0199(3) Uani 1 1 d . . .
H15A H 0.5901 0.7686 0.2067 0.024 Uiso 1 1 calc R . .
H15B H 0.6194 0.8136 0.1373 0.024 Uiso 1 1 calc R . .
N16 N 0.65781(8) 0.96912(12) 0.20359(5) 0.0163(2) Uani 1 1 d . . .
C17 C 0.72063(10) 1.03445(16) 0.16629(7) 0.0207(3) Uani 1 1 d . . .
H17 H 0.7236 1.0041 0.1236 0.025 Uiso 1 1 calc R . .
C18 C 0.78005(10) 1.14370(16) 0.18911(7) 0.0217(3) Uani 1 1 d . . .
H18 H 0.8240 1.1880 0.1623 0.026 Uiso 1 1 calc R . .
C19 C 0.77612(9) 1.19010(15) 0.25164(7) 0.0189(3) Uani 1 1 d . . .
C20 C 0.71069(9) 1.12052(15) 0.28909(6) 0.0168(3) Uani 1 1 d . . .
H20 H 0.7066 1.1496 0.3319 0.020 Uiso 1 1 calc R . .
C21 C 0.65174(9) 1.01019(15) 0.26501(6) 0.0150(3) Uani 1 1 d . . .
C22 C 0.57846(9) 0.93921(14) 0.30305(6) 0.0145(2) Uani 1 1 d . . .
C23 C 0.60075(9) 0.87381(14) 0.36210(6) 0.0143(2) Uani 1 1 d . . .
C24 C 0.70057(9) 0.85909(14) 0.38557(6) 0.0150(3) Uani 1 1 d . . .
C25 C 0.93618(11) 0.7122(2) 0.33616(8) 0.0323(4) Uani 1 1 d . . .
H25A H 0.9101 0.6874 0.2941 0.039 Uiso 0.50 1 d PR A 1
H25B H 0.9580 0.6207 0.3574 0.039 Uiso 0.50 1 d PR A 1
H25C H 0.9891 0.7811 0.3324 0.039 Uiso 0.50 1 d PR A 1
H25D H 0.9982 0.7468 0.3514 0.039 Uiso 0.50 1 d PR A 2
H25E H 0.9265 0.7389 0.2917 0.039 Uiso 0.50 1 d PR A 2
H25F H 0.9324 0.6035 0.3408 0.039 Uiso 0.50 1 d PR A 2
C26 C 0.83603(10) 1.31383(18) 0.27833(8) 0.0263(3) Uani 1 1 d . . .
H26A H 0.8012 1.4081 0.2753 0.039 Uiso 1 1 calc R . .
H26B H 0.8933 1.3219 0.2546 0.039 Uiso 1 1 calc R . .
H26C H 0.8528 1.2925 0.3226 0.039 Uiso 1 1 calc R . .
S1 S 0.73563(3) 0.38084(4) 0.460309(18) 0.02458(10) Uani 1 1 d . . .
S2 S 0.80818(2) 0.62245(4) 0.146405(17) 0.02061(9) Uani 1 1 d . . .
C27 C 0.85441(13) 0.4052(2) 0.49305(9) 0.0365(4) Uani 1 1 d . . .
C28 C 0.93280(11) 0.6682(2) 0.14863(8) 0.0305(3) Uani 1 1 d . . .
F1 F 0.91631(8) 0.41407(18) 0.44855(6) 0.0617(4) Uani 1 1 d . . .
F2 F 0.86223(10) 0.52832(18) 0.52700(8) 0.0733(5) Uani 1 1 d . . .
F3 F 0.87951(10) 0.29195(19) 0.53055(7) 0.0732(4) Uani 1 1 d . . .
F4 F 0.94699(8) 0.80984(12) 0.16549(6) 0.0483(3) Uani 1 1 d . . .
F5 F 0.96861(8) 0.64815(15) 0.09215(5) 0.0501(3) Uani 1 1 d . . .
F6 F 0.98150(7) 0.58232(13) 0.18967(5) 0.0433(3) Uani 1 1 d . . .
O1 O 0.74020(11) 0.23751(14) 0.43003(6) 0.0465(4) Uani 1 1 d . . .
O2 O 0.72349(9) 0.50367(15) 0.41733(7) 0.0426(3) Uani 1 1 d . . .
O3 O 0.67945(9) 0.38548(17) 0.51504(6) 0.0435(3) Uani 1 1 d . . .
O4 O 0.80632(9) 0.46931(13) 0.12606(6) 0.0343(3) Uani 1 1 d . . .
O5 O 0.78014(8) 0.64759(14) 0.20998(5) 0.0304(3) Uani 1 1 d . . .
O6 O 0.76997(8) 0.72729(13) 0.10082(5) 0.0278(2) 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 C24 1.3812(19) . ?
C1 C2 1.3940(19) . ?
C1 H1 0.9500 . ?
C2 C3 1.390(2) . ?
C2 C25 1.499(2) . ?
C3 C4 1.365(2) . ?
C3 H3 0.9500 . ?
C4 N5 1.3487(18) . ?
C4 H4 0.9500 . ?
N5 C24 1.3620(17) . ?
N5 C6 1.4833(17) . ?
C6 C7 1.520(2) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.536(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.5090(19) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.3900(19) . ?
C9 C23 1.4054(18) . ?
C10 C11 1.388(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.3887(19) . ?
C11 H11 0.9500 . ?
C12 C22 1.4076(18) . ?
C12 C13 1.5131(18) . ?
C13 C14 1.537(2) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.525(2) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 N16 1.4861(17) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
N16 C17 1.3524(18) . ?
N16 C21 1.3625(17) . ?
C17 C18 1.370(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.396(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.3966(19) . ?
C19 C26 1.496(2) . ?
C20 C21 1.3816(19) . ?
C20 H20 0.9500 . ?
C21 C22 1.4885(18) . ?
C22 C23 1.4096(18) . ?
C23 C24 1.4946(18) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C25 H25D 0.9800 . ?
C25 H25E 0.9800 . ?
C25 H25F 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
S1 O2 1.4356(13) . ?
S1 O1 1.4381(13) . ?
S1 O3 1.4389(13) . ?
S1 C27 1.8176(19) . ?
S2 O4 1.4374(12) . ?
S2 O6 1.4403(11) . ?
S2 O5 1.4420(11) . ?
S2 C28 1.8215(17) . ?
C27 F2 1.320(2) . ?
C27 F1 1.321(2) . ?
C27 F3 1.330(2) . ?
C28 F4 1.331(2) . ?
C28 F5 1.335(2) . ?
C28 F6 1.336(2) . ?

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
C24 C1 C2 121.16(13) . . ?
C24 C1 H1 119.4 . . ?
C2 C1 H1 119.4 . . ?
C3 C2 C1 117.66(13) . . ?
C3 C2 C25 121.14(13) . . ?
C1 C2 C25 121.20(13) . . ?
C4 C3 C2 120.25(13) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
N5 C4 C3 120.93(13) . . ?
N5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 N5 C24 121.10(12) . . ?
C4 N5 C6 118.04(12) . . ?
C24 N5 C6 120.85(11) . . ?
N5 C6 C7 110.79(12) . . ?
N5 C6 H6A 109.5 . . ?
C7 C6 H6A 109.5 . . ?
N5 C6 H6B 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
C6 C7 C8 113.31(11) . . ?
C6 C7 H7A 108.9 . . ?
C8 C7 H7A 108.9 . . ?
C6 C7 H7B 108.9 . . ?
C8 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
C9 C8 C7 112.72(12) . . ?
C9 C8 H8A 109.0 . . ?
C7 C8 H8A 109.0 . . ?
C9 C8 H8B 109.0 . . ?
C7 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C10 C9 C23 118.92(12) . . ?
C10 C9 C8 121.05(12) . . ?
C23 C9 C8 120.03(12) . . ?
C11 C10 C9 120.97(12) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C10 C11 C12 121.17(12) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 H11 119.4 . . ?
C11 C12 C22 118.57(12) . . ?
C11 C12 C13 121.25(12) . . ?
C22 C12 C13 120.18(12) . . ?
C12 C13 C14 112.26(11) . . ?
C12 C13 H13A 109.2 . . ?
C14 C13 H13A 109.2 . . ?
C12 C13 H13B 109.2 . . ?
C14 C13 H13B 109.2 . . ?
H13A C13 H13B 107.9 . . ?
C15 C14 C13 112.56(11) . . ?
C15 C14 H14A 109.1 . . ?
C13 C14 H14A 109.1 . . ?
C15 C14 H14B 109.1 . . ?
C13 C14 H14B 109.1 . . ?
H14A C14 H14B 107.8 . . ?
N16 C15 C14 111.39(11) . . ?
N16 C15 H15A 109.4 . . ?
C14 C15 H15A 109.3 . . ?
N16 C15 H15B 109.4 . . ?
C14 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
C17 N16 C21 120.92(12) . . ?
C17 N16 C15 119.26(12) . . ?
C21 N16 C15 119.81(11) . . ?
N16 C17 C18 121.03(13) . . ?
N16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C17 C18 C19 120.14(13) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C18 C19 C20 117.58(13) . . ?
C18 C19 C26 122.51(13) . . ?
C20 C19 C26 119.87(13) . . ?
C21 C20 C19 121.19(13) . . ?
C21 C20 H20 119.4 . . ?
C19 C20 H20 119.4 . . ?
N16 C21 C20 119.14(12) . . ?
N16 C21 C22 118.56(12) . . ?
C20 C21 C22 122.24(12) . . ?
C12 C22 C23 120.36(12) . . ?
C12 C22 C21 117.97(12) . . ?
C23 C22 C21 121.52(12) . . ?
C9 C23 C22 119.93(12) . . ?
C9 C23 C24 119.25(12) . . ?
C22 C23 C24 120.77(12) . . ?
N5 C24 C1 118.84(12) . . ?
N5 C24 C23 118.30(12) . . ?
C1 C24 C23 122.86(12) . . ?
C2 C25 H25A 109.5 . . ?
C2 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C2 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C2 C25 H25D 109.5 . . ?
H25A C25 H25D 132.8 . . ?
H25B C25 H25D 81.1 . . ?
H25C C25 H25D 30.8 . . ?
C2 C25 H25E 109.5 . . ?
H25A C25 H25E 30.8 . . ?
H25B C25 H25E 132.8 . . ?
H25C C25 H25E 81.1 . . ?
H25D C25 H25E 109.5 . . ?
C2 C25 H25F 109.5 . . ?
H25A C25 H25F 81.1 . . ?
H25B C25 H25F 30.8 . . ?
H25C C25 H25F 132.8 . . ?
H25D C25 H25F 109.5 . . ?
H25E C25 H25F 109.5 . . ?
C19 C26 H26A 109.5 . . ?
C19 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C19 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O2 S1 O1 113.89(8) . . ?
O2 S1 O3 115.82(9) . . ?
O1 S1 O3 115.10(9) . . ?
O2 S1 C27 103.80(9) . . ?
O1 S1 C27 102.72(9) . . ?
O3 S1 C27 103.12(8) . . ?
O4 S2 O6 114.66(7) . . ?
O4 S2 O5 115.36(7) . . ?
O6 S2 O5 114.66(7) . . ?
O4 S2 C28 103.21(8) . . ?
O6 S2 C28 102.31(7) . . ?
O5 S2 C28 104.30(7) . . ?
F2 C27 F1 107.26(17) . . ?
F2 C27 F3 107.10(16) . . ?
F1 C27 F3 107.67(16) . . ?
F2 C27 S1 111.50(13) . . ?
F1 C27 S1 111.81(13) . . ?
F3 C27 S1 111.25(14) . . ?
F4 C28 F5 108.09(15) . . ?
F4 C28 F6 107.63(14) . . ?
F5 C28 F6 107.60(14) . . ?
F4 C28 S2 111.02(12) . . ?
F5 C28 S2 110.72(11) . . ?
F6 C28 S2 111.61(12) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.050
#===END
####################################################################### 
# 
# 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_am008_severa_uochb
_database_code_depnum_ccdc_archive 'CCDC 1004340'
_audit_update_record             
;
2014-05-20 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H26 N2, 2(C F3 O3 S), 0.5(C3 H6 O)'
_chemical_formula_sum            'C27.50 H29 F6 N2 O6.50 S2'
_chemical_formula_weight         669.65
_chemical_compound_source        'synthesized by the authors'

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'
S S 0.1246 0.1234 '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                   9.0232(4)
_cell_length_b                   12.5214(6)
_cell_length_c                   14.3223(6)
_cell_angle_alpha                101.780(2)
_cell_angle_beta                 106.4230(10)
_cell_angle_gamma                101.248(2)
_cell_volume                     1463.37(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9926
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      27.49

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.59
_exptl_crystal_size_min          0.42
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             692
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7648
_exptl_absorpt_correction_T_max  0.8959
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32985
_diffrn_reflns_av_R_equivalents  0.0133
_diffrn_reflns_av_sigmaI/netI    0.0102
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.73
_diffrn_reflns_theta_max         27.49
_reflns_number_total             6718
_reflns_number_gt                6101
_reflns_threshold_expression     I>2σ(I)

_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-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 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)+(0.0442P)²+0.9707P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6718
_refine_ls_number_parameters     408
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0361
_refine_ls_wR_factor_ref         0.0959
_refine_ls_wR_factor_gt          0.0927
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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 0.66069(17) 0.88698(12) 0.66212(11) 0.0242(3) Uani 1 1 d . . .
H1 H 0.6468 0.8146 0.6745 0.029 Uiso 1 1 calc R . .
C2 C 0.68022(18) 0.90011(13) 0.57215(11) 0.0280(3) Uani 1 1 d . . .
H2 H 0.6810 0.8370 0.5227 0.034 Uiso 1 1 calc R . .
C3 C 0.69847(18) 1.00569(13) 0.55507(11) 0.0285(3) Uani 1 1 d . . .
H3 H 0.7102 1.0146 0.4930 0.034 Uiso 1 1 calc R . .
C4 C 0.69992(17) 1.09866(12) 0.62696(11) 0.0246(3) Uani 1 1 d . . .
N5 N 0.67992(13) 1.08361(9) 0.71459(8) 0.0196(2) Uani 1 1 d . . .
C6 C 0.68487(16) 1.18097(11) 0.79610(10) 0.0214(3) Uani 1 1 d . . .
H6A H 0.6026 1.1570 0.8265 0.026 Uiso 1 1 calc R . .
H6B H 0.6595 1.2429 0.7666 0.026 Uiso 1 1 calc R . .
C7 C 0.84979(16) 1.22425(11) 0.87813(11) 0.0237(3) Uani 1 1 d . . .
H7A H 0.8418 1.2734 0.9391 0.028 Uiso 1 1 calc R . .
H7B H 0.9248 1.2709 0.8539 0.028 Uiso 1 1 calc R . .
C8 C 0.91793(16) 1.12756(12) 0.90701(11) 0.0229(3) Uani 1 1 d . . .
H8A H 0.9575 1.0929 0.8536 0.027 Uiso 1 1 calc R . .
H8B H 1.0100 1.1587 0.9711 0.027 Uiso 1 1 calc R . .
C9 C 0.79279(15) 1.03774(11) 0.91982(10) 0.0198(3) Uani 1 1 d . . .
C10 C 0.80506(16) 1.01832(11) 1.01357(10) 0.0214(3) Uani 1 1 d . . .
H10 H 0.8939 1.0627 1.0715 0.026 Uiso 1 1 calc R . .
C11 C 0.68910(16) 0.93493(11) 1.02342(10) 0.0210(3) Uani 1 1 d . . .
H11 H 0.7024 0.9211 1.0877 0.025 Uiso 1 1 calc R . .
C12 C 0.55384(15) 0.87103(11) 0.94141(10) 0.0184(2) Uani 1 1 d . . .
C13 C 0.42477(16) 0.78309(11) 0.95242(10) 0.0211(3) Uani 1 1 d . . .
H13A H 0.3208 0.8009 0.9280 0.025 Uiso 1 1 calc R . .
H13B H 0.4484 0.7871 1.0251 0.025 Uiso 1 1 calc R . .
C14 C 0.40942(17) 0.66183(12) 0.89378(11) 0.0231(3) Uani 1 1 d . . .
H14A H 0.4954 0.6335 0.9326 0.028 Uiso 1 1 calc R . .
H14B H 0.3050 0.6119 0.8869 0.028 Uiso 1 1 calc R . .
C15 C 0.42117(16) 0.65616(11) 0.78903(10) 0.0212(3) Uani 1 1 d . . .
H15A H 0.5345 0.6868 0.7956 0.025 Uiso 1 1 calc R . .
H15B H 0.3856 0.5760 0.7482 0.025 Uiso 1 1 calc R . .
N16 N 0.32132(13) 0.72137(9) 0.73561(8) 0.0181(2) Uani 1 1 d . . .
C17 C 0.17445(16) 0.66800(12) 0.66467(10) 0.0216(3) Uani 1 1 d . . .
C18 C 0.08921(17) 0.73167(13) 0.61352(10) 0.0259(3) Uani 1 1 d . . .
H18 H -0.0119 0.6952 0.5622 0.031 Uiso 1 1 calc R . .
C19 C 0.14964(17) 0.84741(13) 0.63630(11) 0.0261(3) Uani 1 1 d . . .
H19 H 0.0908 0.8906 0.6010 0.031 Uiso 1 1 calc R . .
C20 C 0.29757(16) 0.90007(12) 0.71148(10) 0.0222(3) Uani 1 1 d . . .
H20 H 0.3395 0.9799 0.7288 0.027 Uiso 1 1 calc R . .
C21 C 0.38374(15) 0.83622(11) 0.76117(9) 0.0183(2) Uani 1 1 d . . .
C22 C 0.53761(15) 0.89117(10) 0.84634(10) 0.0176(2) Uani 1 1 d . . .
C23 C 0.65926(15) 0.97192(11) 0.83559(10) 0.0184(2) Uani 1 1 d . . .
C24 C 0.66160(15) 0.98001(11) 0.73381(10) 0.0193(2) Uani 1 1 d . . .
C25 C 0.7240(2) 1.21414(14) 0.61075(12) 0.0352(4) Uani 1 1 d . . .
H25A H 0.6280 1.2403 0.6092 0.053 Uiso 1 1 calc R . .
H25B H 0.7429 1.2111 0.5463 0.053 Uiso 1 1 calc R . .
H25C H 0.8168 1.2667 0.6662 0.053 Uiso 1 1 calc R . .
C26 C 0.10718(18) 0.54336(12) 0.64450(11) 0.0277(3) Uani 1 1 d . . .
H26A H 0.1676 0.5025 0.6101 0.042 Uiso 1 1 calc R . .
H26B H -0.0058 0.5210 0.6014 0.042 Uiso 1 1 calc R . .
H26C H 0.1156 0.5249 0.7088 0.042 Uiso 1 1 calc R . .
S1 S 0.18567(4) 0.17944(3) 0.66820(3) 0.02908(10) Uani 1 1 d . . .
O1 O 0.32804(14) 0.14460(10) 0.66621(9) 0.0359(3) Uani 1 1 d . . .
O2 O 0.07445(18) 0.10405(12) 0.69556(14) 0.0632(5) Uani 1 1 d . . .
O3 O 0.1178(2) 0.22241(17) 0.58573(10) 0.0704(5) Uani 1 1 d . . .
C27 C 0.26012(19) 0.30365(13) 0.77614(12) 0.0301(3) Uani 1 1 d . . .
F1 F 0.14528(14) 0.35166(9) 0.78825(9) 0.0477(3) Uani 1 1 d . . .
F2 F 0.3254(2) 0.27869(12) 0.86073(9) 0.0800(5) Uani 1 1 d . . .
F3 F 0.36999(16) 0.38215(10) 0.76541(13) 0.0706(4) Uani 1 1 d . . .
S2 S 0.87446(4) 0.67161(3) 0.79834(3) 0.02588(9) Uani 1 1 d . . .
O4 O 0.79547(17) 0.62912(13) 0.69083(10) 0.0511(4) Uani 1 1 d . . .
O5 O 1.04682(12) 0.70295(10) 0.83170(9) 0.0333(2) Uani 1 1 d . . .
O6 O 0.80705(14) 0.75050(10) 0.84858(12) 0.0457(3) Uani 1 1 d . . .
C28 C 0.82810(19) 0.54768(14) 0.84349(13) 0.0347(3) Uani 1 1 d . . .
F4 F 0.88558(19) 0.57237(13) 0.94306(10) 0.0762(5) Uani 1 1 d . . .
F5 F 0.88912(19) 0.46754(10) 0.80618(14) 0.0760(5) Uani 1 1 d . . .
F6 F 0.67114(13) 0.50205(11) 0.81557(11) 0.0586(3) Uani 1 1 d . . .
O1A O 0.6084(4) 0.3923(3) 0.4540(2) 0.0560(8) Uani 0.50 1 d P . .
C1A C 0.5399(4) 0.4577(3) 0.4845(2) 0.0331(7) Uani 0.50 1 d P . .
C2A C 0.5530(2) 0.56811(16) 0.45445(15) 0.0447(4) Uani 1 1 d . . .
H1S H 0.6643 0.6003 0.4600 0.067 Uiso 0.50 1 d PR . .
H2S H 0.5205 0.6218 0.4995 0.067 Uiso 0.50 1 d PR . .
H3S H 0.4828 0.5532 0.3844 0.067 Uiso 0.50 1 d PR . .
H4S H 0.4872 0.5359 0.3828 0.067 Uiso 0.50 1 d PR . .
H5S H 0.6448 0.5358 0.4694 0.067 Uiso 0.50 1 d PR . .
H6S H 0.5917 0.6505 0.4689 0.067 Uiso 0.50 1 d PR . .


_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 C24 1.3836(19) . ?
C1 C2 1.386(2) . ?
C1 H1 0.9500 . ?
C2 C3 1.380(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.383(2) . ?
C3 H3 0.9500 . ?
C4 N5 1.3618(18) . ?
C4 C25 1.495(2) . ?
N5 C24 1.3688(17) . ?
N5 C6 1.4898(17) . ?
C6 C7 1.5249(19) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.5381(19) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.5098(18) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.3908(19) . ?
C9 C23 1.4039(18) . ?
C10 C11 1.386(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.3907(19) . ?
C11 H11 0.9500 . ?
C12 C22 1.4074(18) . ?
C12 C13 1.5060(18) . ?
C13 C14 1.5368(19) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.5219(19) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 N16 1.4887(16) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
N16 C17 1.3605(17) . ?
N16 C21 1.3681(17) . ?
C17 C18 1.387(2) . ?
C17 C26 1.4950(19) . ?
C18 C19 1.379(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.3893(19) . ?
C19 H19 0.9500 . ?
C20 C21 1.3828(18) . ?
C20 H20 0.9500 . ?
C21 C22 1.4887(17) . ?
C22 C23 1.4061(18) . ?
C23 C24 1.4875(18) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
S1 O3 1.4280(14) . ?
S1 O2 1.4338(15) . ?
S1 O1 1.4407(12) . ?
S1 C27 1.8121(16) . ?
C27 F2 1.3173(19) . ?
C27 F3 1.3192(19) . ?
C27 F1 1.3294(19) . ?
S2 O6 1.4337(13) . ?
S2 O4 1.4350(13) . ?
S2 O5 1.4374(11) . ?
S2 C28 1.8194(17) . ?
C28 F4 1.318(2) . ?
C28 F5 1.326(2) . ?
C28 F6 1.3277(19) . ?
O1A C1A 1.203(4) . ?
C1A C2A 1.413(4) 2_666 ?
C1A C1A 1.457(6) 2_666 ?
C1A C2A 1.523(4) . ?
C2A C1A 1.412(4) 2_666 ?
C2A H1S 0.9800 . ?
C2A H2S 0.9800 . ?
C2A H3S 0.9800 . ?
C2A H4S 0.9800 . ?
C2A H5S 0.9800 . ?
C2A H6S 0.9800 . ?

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
C24 C1 C2 119.56(13) . . ?
C24 C1 H1 120.2 . . ?
C2 C1 H1 120.2 . . ?
C3 C2 C1 119.39(14) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C2 C3 C4 120.96(13) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
N5 C4 C3 118.59(13) . . ?
N5 C4 C25 119.83(13) . . ?
C3 C4 C25 121.59(13) . . ?
C4 N5 C24 121.85(12) . . ?
C4 N5 C6 121.11(11) . . ?
C24 N5 C6 116.98(11) . . ?
N5 C6 C7 110.96(11) . . ?
N5 C6 H6A 109.4 . . ?
C7 C6 H6A 109.4 . . ?
N5 C6 H6B 109.4 . . ?
C7 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
C6 C7 C8 112.50(11) . . ?
C6 C7 H7A 109.1 . . ?
C8 C7 H7A 109.1 . . ?
C6 C7 H7B 109.1 . . ?
C8 C7 H7B 109.1 . . ?
H7A C7 H7B 107.8 . . ?
C9 C8 C7 111.52(11) . . ?
C9 C8 H8A 109.3 . . ?
C7 C8 H8A 109.3 . . ?
C9 C8 H8B 109.3 . . ?
C7 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
C10 C9 C23 118.48(12) . . ?
C10 C9 C8 121.78(12) . . ?
C23 C9 C8 119.74(12) . . ?
C11 C10 C9 120.77(12) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C10 C11 C12 121.54(12) . . ?
C10 C11 H11 119.2 . . ?
C12 C11 H11 119.2 . . ?
C11 C12 C22 118.47(12) . . ?
C11 C12 C13 121.76(12) . . ?
C22 C12 C13 119.76(12) . . ?
C12 C13 C14 113.31(11) . . ?
C12 C13 H13A 108.9 . . ?
C14 C13 H13A 108.9 . . ?
C12 C13 H13B 108.9 . . ?
C14 C13 H13B 108.9 . . ?
H13A C13 H13B 107.7 . . ?
C15 C14 C13 111.89(11) . . ?
C15 C14 H14A 109.2 . . ?
C13 C14 H14A 109.2 . . ?
C15 C14 H14B 109.2 . . ?
C13 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
N16 C15 C14 111.89(11) . . ?
N16 C15 H15A 109.2 . . ?
C14 C15 H15A 109.2 . . ?
N16 C15 H15B 109.2 . . ?
C14 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
C17 N16 C21 122.02(11) . . ?
C17 N16 C15 120.86(11) . . ?
C21 N16 C15 117.12(11) . . ?
N16 C17 C18 118.72(12) . . ?
N16 C17 C26 119.86(12) . . ?
C18 C17 C26 121.41(13) . . ?
C19 C18 C17 120.73(13) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C18 C19 C20 119.23(13) . . ?
C18 C19 H19 120.4 . . ?
C20 C19 H19 120.4 . . ?
C21 C20 C19 119.97(13) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
N16 C21 C20 119.26(12) . . ?
N16 C21 C22 119.58(11) . . ?
C20 C21 C22 121.03(12) . . ?
C23 C22 C12 119.82(12) . . ?
C23 C22 C21 120.50(11) . . ?
C12 C22 C21 119.32(11) . . ?
C9 C23 C22 120.81(12) . . ?
C9 C23 C24 117.59(12) . . ?
C22 C23 C24 121.14(11) . . ?
N5 C24 C1 119.64(12) . . ?
N5 C24 C23 119.06(11) . . ?
C1 C24 C23 121.02(12) . . ?
C4 C25 H25A 109.5 . . ?
C4 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C4 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C17 C26 H26A 109.5 . . ?
C17 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C17 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O3 S1 O2 116.12(12) . . ?
O3 S1 O1 114.50(9) . . ?
O2 S1 O1 114.55(9) . . ?
O3 S1 C27 103.13(9) . . ?
O2 S1 C27 102.69(9) . . ?
O1 S1 C27 103.32(7) . . ?
F2 C27 F3 107.71(16) . . ?
F2 C27 F1 107.69(15) . . ?
F3 C27 F1 106.24(13) . . ?
F2 C27 S1 111.40(11) . . ?
F3 C27 S1 111.14(12) . . ?
F1 C27 S1 112.39(11) . . ?
O6 S2 O4 114.61(9) . . ?
O6 S2 O5 114.54(7) . . ?
O4 S2 O5 115.52(8) . . ?
O6 S2 C28 103.81(9) . . ?
O4 S2 C28 103.30(8) . . ?
O5 S2 C28 102.73(7) . . ?
F4 C28 F5 107.86(16) . . ?
F4 C28 F6 107.18(16) . . ?
F5 C28 F6 106.65(15) . . ?
F4 C28 S2 111.85(12) . . ?
F5 C28 S2 111.02(13) . . ?
F6 C28 S2 112.02(12) . . ?
O1A C1A C2A 120.8(3) . 2_666 ?
O1A C1A C1A 175.1(4) . 2_666 ?
O1A C1A C2A 118.6(3) . . ?
C2A C1A C2A 120.6(2) 2_666 . ?
C1A C2A H1S 109.3 . . ?
C1A C2A H2S 109.6 . . ?
H1S C2A H2S 109.5 . . ?
C1A C2A H3S 109.9 2_666 . ?
C1A C2A H3S 109.5 . . ?
H1S C2A H3S 109.5 . . ?
H2S C2A H3S 109.5 . . ?
C1A C2A H4S 109.5 2_666 . ?
C1A C2A H4S 97.7 . . ?
H1S C2A H4S 109.4 . . ?
H2S C2A H4S 120.5 . . ?
C1A C2A H5S 109.4 2_666 . ?
H3S C2A H5S 120.3 . . ?
H4S C2A H5S 109.5 . . ?
C1A C2A H6S 109.5 2_666 . ?
H3S C2A H6S 97.5 . . ?
H4S C2A H6S 109.5 . . ?
H5S C2A H6S 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.049
#===END
####################################################################### 
# 
# 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_ls805_s_uochb
_database_code_depnum_ccdc_archive 'CCDC 1004341'
_audit_update_record             
;
2014-05-20 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H26 N2, 2(I)'
_chemical_formula_sum            'C24 H26 I2 N2'
_chemical_formula_weight         596.27
_chemical_compound_source        'synthesized by the authors'

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

_cell_length_a                   8.7530(2)
_cell_length_b                   13.2791(4)
_cell_length_c                   19.7500(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2295.58(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9685
_cell_measurement_theta_min      2.9720
_cell_measurement_theta_max      27.4750

_exptl_crystal_description       prism_irregular
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1160
_exptl_absorpt_coefficient_mu    2.752
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.4126
_exptl_absorpt_correction_T_max  0.6460
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14692
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_av_sigmaI/netI    0.0243
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.85
_diffrn_reflns_theta_max         27.48
_reflns_number_total             5263
_reflns_number_gt                4990
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'Bruker Instrument Service v2012.12.0.0'
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 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)+(0.0203P)²+0.7628P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.030(15)
_refine_ls_number_reflns         5263
_refine_ls_number_parameters     255
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0197
_refine_ls_wR_factor_ref         0.0452
_refine_ls_wR_factor_gt          0.0445
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3842(3) 0.53237(18) 0.93145(11) 0.0179(5) Uani 1 1 d . . .
H1 H 0.3554 0.5510 0.8868 0.021 Uiso 1 1 calc R . .
C2 C 0.3185(3) 0.4473(2) 0.96090(13) 0.0205(5) Uani 1 1 d . . .
C3 C 0.3601(4) 0.4234(2) 1.02699(13) 0.0272(6) Uani 1 1 d . . .
H3 H 0.3168 0.3664 1.0488 0.033 Uiso 1 1 calc R . .
C4 C 0.4643(3) 0.4829(2) 1.06056(14) 0.0257(6) Uani 1 1 d . . .
H4 H 0.4919 0.4664 1.1057 0.031 Uiso 1 1 calc R . .
N5 N 0.5279(2) 0.56390(18) 1.03086(10) 0.0194(4) Uani 1 1 d . . .
C6 C 0.6438(3) 0.6236(2) 1.06839(13) 0.0234(6) Uani 1 1 d . . .
H6A H 0.7318 0.6372 1.0382 0.028 Uiso 1 1 calc R . .
H6B H 0.6814 0.5836 1.1073 0.028 Uiso 1 1 calc R . .
C7 C 0.5800(3) 0.7229(2) 1.09406(13) 0.0281(7) Uani 1 1 d . . .
H7A H 0.6657 0.7671 1.1076 0.034 Uiso 1 1 calc R . .
H7B H 0.5169 0.7100 1.1348 0.034 Uiso 1 1 calc R . .
C8 C 0.4823(3) 0.7773(2) 1.04078(13) 0.0224(6) Uani 1 1 d . . .
H8A H 0.3797 0.7460 1.0394 0.027 Uiso 1 1 calc R . .
H8B H 0.4694 0.8486 1.0545 0.027 Uiso 1 1 calc R . .
C9 C 0.5518(3) 0.7737(2) 0.97081(12) 0.0183(5) Uani 1 1 d . . .
C10 C 0.6058(3) 0.8601(2) 0.93985(13) 0.0205(5) Uani 1 1 d . . .
H10 H 0.5977 0.9226 0.9629 0.025 Uiso 1 1 calc R . .
C11 C 0.6716(3) 0.8576(2) 0.87581(14) 0.0207(6) Uani 1 1 d . . .
H11 H 0.7057 0.9184 0.8554 0.025 Uiso 1 1 calc R . .
C12 C 0.6879(3) 0.7665(2) 0.84131(13) 0.0187(5) Uani 1 1 d . . .
C13 C 0.7639(3) 0.7628(2) 0.77293(12) 0.0207(6) Uani 1 1 d . . .
H13A H 0.8413 0.7084 0.7727 0.025 Uiso 1 1 calc R . .
H13B H 0.8172 0.8274 0.7645 0.025 Uiso 1 1 calc R . .
C14 C 0.6482(4) 0.7440(2) 0.71616(12) 0.0254(6) Uani 1 1 d . . .
H14A H 0.5959 0.8080 0.7051 0.030 Uiso 1 1 calc R . .
H14B H 0.7032 0.7211 0.6751 0.030 Uiso 1 1 calc R . .
C15 C 0.5292(3) 0.6653(2) 0.73553(14) 0.0246(6) Uani 1 1 d . . .
H15A H 0.4545 0.6954 0.7673 0.030 Uiso 1 1 calc R . .
H15B H 0.4733 0.6434 0.6945 0.030 Uiso 1 1 calc R . .
N16 N 0.6028(2) 0.57680(16) 0.76788(10) 0.0177(5) Uani 1 1 d . . .
C17 C 0.6252(4) 0.4934(2) 0.73009(12) 0.0255(6) Uani 1 1 d . . .
H17 H 0.5921 0.4928 0.6843 0.031 Uiso 1 1 calc R . .
C18 C 0.6942(3) 0.4103(2) 0.75637(14) 0.0246(6) Uani 1 1 d . . .
H18 H 0.7093 0.3525 0.7288 0.030 Uiso 1 1 calc R . .
C19 C 0.7429(3) 0.4097(2) 0.82372(13) 0.0237(6) Uani 1 1 d . . .
C20 C 0.7200(3) 0.4978(2) 0.86119(13) 0.0193(5) Uani 1 1 d . . .
H20 H 0.7535 0.4999 0.9069 0.023 Uiso 1 1 calc R . .
C21 C 0.6510(3) 0.58082(18) 0.83409(11) 0.0165(5) Uani 1 1 d . . .
C22 C 0.6292(3) 0.67763(17) 0.87100(11) 0.0159(4) Uani 1 1 d . . .
C23 C 0.5614(3) 0.6813(2) 0.93545(12) 0.0163(5) Uani 1 1 d . . .
C24 C 0.4905(3) 0.5903(2) 0.96583(12) 0.0172(5) Uani 1 1 d . . .
C26 C 0.2042(3) 0.3848(2) 0.92284(15) 0.0292(7) Uani 1 1 d . . .
H26A H 0.2378 0.3144 0.9222 0.044 Uiso 1 1 calc R . .
H26B H 0.1957 0.4097 0.8763 0.044 Uiso 1 1 calc R . .
H26C H 0.1044 0.3894 0.9452 0.044 Uiso 1 1 calc R . .
C27 C 0.8201(5) 0.3192(3) 0.85312(18) 0.0508(11) Uani 1 1 d . . .
H27A H 0.7748 0.2580 0.8340 0.076 Uiso 1 1 calc R . .
H27B H 0.8068 0.3191 0.9024 0.076 Uiso 1 1 calc R . .
H27C H 0.9293 0.3213 0.8423 0.076 Uiso 1 1 calc R . .
I1 I 0.12286(2) 0.561051(13) 0.756816(8) 0.02683(5) Uani 1 1 d . . .
I2 I 0.63178(3) 0.602608(14) 0.547024(8) 0.02897(5) 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 C24 1.385(4) . ?
C1 C2 1.395(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.392(4) . ?
C2 C26 1.502(4) . ?
C3 C4 1.376(4) . ?
C3 H3 0.9500 . ?
C4 N5 1.346(4) . ?
C4 H4 0.9500 . ?
N5 C24 1.371(3) . ?
N5 C6 1.486(4) . ?
C6 C7 1.519(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.537(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.511(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.383(4) . ?
C9 C23 1.414(4) . ?
C10 C11 1.390(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.396(4) . ?
C11 H11 0.9500 . ?
C12 C22 1.414(3) . ?
C12 C13 1.506(3) . ?
C13 C14 1.531(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.524(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 N16 1.485(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
N16 C17 1.349(3) . ?
N16 C21 1.375(3) . ?
C17 C18 1.362(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.397(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.399(4) . ?
C19 C27 1.496(4) . ?
C20 C21 1.367(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.490(3) . ?
C22 C23 1.405(3) . ?
C23 C24 1.485(4) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?

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
C24 C1 C2 121.5(2) . . ?
C24 C1 H1 119.2 . . ?
C2 C1 H1 119.2 . . ?
C3 C2 C1 117.8(2) . . ?
C3 C2 C26 121.2(3) . . ?
C1 C2 C26 120.9(2) . . ?
C4 C3 C2 119.7(3) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
N5 C4 C3 121.5(2) . . ?
N5 C4 H4 119.2 . . ?
C3 C4 H4 119.2 . . ?
C4 N5 C24 120.9(2) . . ?
C4 N5 C6 119.5(2) . . ?
C24 N5 C6 119.6(2) . . ?
N5 C6 C7 112.2(2) . . ?
N5 C6 H6A 109.2 . . ?
C7 C6 H6A 109.2 . . ?
N5 C6 H6B 109.2 . . ?
C7 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
C6 C7 C8 112.6(2) . . ?
C6 C7 H7A 109.1 . . ?
C8 C7 H7A 109.1 . . ?
C6 C7 H7B 109.1 . . ?
C8 C7 H7B 109.1 . . ?
H7A C7 H7B 107.8 . . ?
C9 C8 C7 112.8(2) . . ?
C9 C8 H8A 109.0 . . ?
C7 C8 H8A 109.0 . . ?
C9 C8 H8B 109.0 . . ?
C7 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C10 C9 C23 118.7(2) . . ?
C10 C9 C8 121.0(2) . . ?
C23 C9 C8 120.3(2) . . ?
C9 C10 C11 121.6(2) . . ?
C9 C10 H10 119.2 . . ?
C11 C10 H10 119.2 . . ?
C10 C11 C12 120.5(3) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C11 C12 C22 118.9(2) . . ?
C11 C12 C13 120.7(2) . . ?
C22 C12 C13 120.3(2) . . ?
C12 C13 C14 111.7(2) . . ?
C12 C13 H13A 109.3 . . ?
C14 C13 H13A 109.3 . . ?
C12 C13 H13B 109.3 . . ?
C14 C13 H13B 109.3 . . ?
H13A C13 H13B 107.9 . . ?
C15 C14 C13 112.4(2) . . ?
C15 C14 H14A 109.1 . . ?
C13 C14 H14A 109.1 . . ?
C15 C14 H14B 109.1 . . ?
C13 C14 H14B 109.1 . . ?
H14A C14 H14B 107.9 . . ?
N16 C15 C14 110.7(2) . . ?
N16 C15 H15A 109.5 . . ?
C14 C15 H15A 109.5 . . ?
N16 C15 H15B 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 108.1 . . ?
C17 N16 C21 120.9(2) . . ?
C17 N16 C15 118.3(2) . . ?
C21 N16 C15 120.8(2) . . ?
N16 C17 C18 121.2(2) . . ?
N16 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C17 C18 C19 120.2(3) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C18 C19 C20 117.1(3) . . ?
C18 C19 C27 120.8(3) . . ?
C20 C19 C27 122.1(3) . . ?
C21 C20 C19 122.1(2) . . ?
C21 C20 H20 119.0 . . ?
C19 C20 H20 119.0 . . ?
C20 C21 N16 118.5(2) . . ?
C20 C21 C22 124.1(2) . . ?
N16 C21 C22 117.4(2) . . ?
C23 C22 C12 120.0(2) . . ?
C23 C22 C21 121.8(2) . . ?
C12 C22 C21 118.1(2) . . ?
C22 C23 C9 120.2(2) . . ?
C22 C23 C24 121.0(2) . . ?
C9 C23 C24 118.8(2) . . ?
N5 C24 C1 118.5(2) . . ?
N5 C24 C23 119.1(2) . . ?
C1 C24 C23 122.3(2) . . ?
C2 C26 H26A 109.5 . . ?
C2 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C2 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C19 C27 H27A 109.5 . . ?
C19 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C19 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 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
C24 C1 C2 C3 1.6(4) . . . . ?
C24 C1 C2 C26 -179.6(2) . . . . ?
C1 C2 C3 C4 -0.7(4) . . . . ?
C26 C2 C3 C4 -179.4(3) . . . . ?
C2 C3 C4 N5 -0.3(4) . . . . ?
C3 C4 N5 C24 0.3(4) . . . . ?
C3 C4 N5 C6 -177.9(3) . . . . ?
C4 N5 C6 C7 -105.1(3) . . . . ?
C24 N5 C6 C7 76.8(3) . . . . ?
N5 C6 C7 C8 -43.9(3) . . . . ?
C6 C7 C8 C9 -42.2(3) . . . . ?
C7 C8 C9 C10 -112.6(3) . . . . ?
C7 C8 C9 C23 68.0(3) . . . . ?
C23 C9 C10 C11 -1.3(4) . . . . ?
C8 C9 C10 C11 179.3(2) . . . . ?
C9 C10 C11 C12 -1.4(4) . . . . ?
C10 C11 C12 C22 3.3(4) . . . . ?
C10 C11 C12 C13 -177.9(2) . . . . ?
C11 C12 C13 C14 -107.7(3) . . . . ?
C22 C12 C13 C14 71.1(3) . . . . ?
C12 C13 C14 C15 -41.4(3) . . . . ?
C13 C14 C15 N16 -45.4(3) . . . . ?
C14 C15 N16 C17 -101.0(3) . . . . ?
C14 C15 N16 C21 77.2(3) . . . . ?
C21 N16 C17 C18 0.8(4) . . . . ?
C15 N16 C17 C18 178.9(3) . . . . ?
N16 C17 C18 C19 0.3(4) . . . . ?
C17 C18 C19 C20 -1.2(4) . . . . ?
C17 C18 C19 C27 -179.5(3) . . . . ?
C18 C19 C20 C21 1.0(4) . . . . ?
C27 C19 C20 C21 179.3(3) . . . . ?
C19 C20 C21 N16 0.1(4) . . . . ?
C19 C20 C21 C22 -177.6(3) . . . . ?
C17 N16 C21 C20 -1.0(4) . . . . ?
C15 N16 C21 C20 -179.1(2) . . . . ?
C17 N16 C21 C22 176.8(2) . . . . ?
C15 N16 C21 C22 -1.3(3) . . . . ?
C11 C12 C22 C23 -2.6(4) . . . . ?
C13 C12 C22 C23 178.6(3) . . . . ?
C11 C12 C22 C21 -178.6(2) . . . . ?
C13 C12 C22 C21 2.6(4) . . . . ?
C20 C21 C22 C23 -51.7(4) . . . . ?
N16 C21 C22 C23 130.6(3) . . . . ?
C20 C21 C22 C12 124.2(3) . . . . ?
N16 C21 C22 C12 -53.4(3) . . . . ?
C12 C22 C23 C9 -0.1(4) . . . . ?
C21 C22 C23 C9 175.8(2) . . . . ?
C12 C22 C23 C24 176.2(2) . . . . ?
C21 C22 C23 C24 -7.9(4) . . . . ?
C10 C9 C23 C22 2.0(4) . . . . ?
C8 C9 C23 C22 -178.6(2) . . . . ?
C10 C9 C23 C24 -174.3(2) . . . . ?
C8 C9 C23 C24 5.1(4) . . . . ?
C4 N5 C24 C1 0.7(4) . . . . ?
C6 N5 C24 C1 178.8(2) . . . . ?
C4 N5 C24 C23 178.9(2) . . . . ?
C6 N5 C24 C23 -2.9(3) . . . . ?
C2 C1 C24 N5 -1.6(4) . . . . ?
C2 C1 C24 C23 -179.8(2) . . . . ?
C22 C23 C24 N5 130.7(3) . . . . ?
C9 C23 C24 N5 -53.0(3) . . . . ?
C22 C23 C24 C1 -51.1(4) . . . . ?
C9 C23 C24 C1 125.2(3) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.068
#===END
####################################################################### 
# 
# 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_ls808_teply_uochb_sqd
_database_code_depnum_ccdc_archive 'CCDC 1004342'
_audit_update_record             
;
2014-05-20 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H26 N2, 2(Br)'
_chemical_formula_sum            'C24 H26 Br2 N2'
_chemical_formula_weight         502.29
_chemical_compound_source        'synthesized by the authors'
_chemical_absolute_configuration ad

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'

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

_cell_length_a                   27.6754(9)
_cell_length_b                   10.0575(3)
_cell_length_c                   14.6734(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4084.3(2)
_cell_formula_units_Z            6
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4212
_cell_measurement_theta_min      2.5631
_cell_measurement_theta_max      22.5133

_exptl_crystal_description       plate_needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1524
_exptl_absorpt_coefficient_mu    2.987
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.2919
_exptl_absorpt_correction_T_max  0.7918
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphit
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20906
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0818
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.39
_diffrn_reflns_theta_max         26.00
_reflns_number_total             8032
_reflns_number_gt                6052
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'Bruker Instrument Service v2012.12.0.0'
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 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)+(0.0326P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.006(8)
_refine_ls_number_reflns         8032
_refine_ls_number_parameters     382
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_ref         0.0772
_refine_ls_wR_factor_gt          0.0732
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_restrained_S_all      0.936
_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
Br1 Br 0.814934(16) 0.67103(4) 0.11891(3) 0.03011(12) Uani 1 1 d . . .
Br2 Br 0.811485(17) 0.89214(4) 0.72647(3) 0.03190(12) Uani 1 1 d . . .
Br3 Br 0.570996(16) 0.86303(4) 0.95399(4) 0.04100(15) Uani 1 1 d . . .
C11 C 0.55559(13) 0.5028(4) 0.9437(4) 0.0237(11) Uani 1 1 d . . .
H11 H 0.5523 0.5955 0.9331 0.028 Uiso 1 1 calc R . .
C12 C 0.57316(16) 0.4590(4) 1.0267(4) 0.0284(11) Uani 1 1 d . . .
C13 C 0.58043(17) 0.3247(4) 1.0384(4) 0.0391(13) Uani 1 1 d . . .
H13 H 0.5932 0.2919 1.0941 0.047 Uiso 1 1 calc R . .
C14 C 0.56912(17) 0.2378(4) 0.9686(4) 0.0384(14) Uani 1 1 d . . .
H14 H 0.5754 0.1456 0.9760 0.046 Uiso 1 1 calc R . .
N15 N 0.54969(12) 0.2810(3) 0.8915(3) 0.0204(9) Uani 1 1 d . . .
C16 C 0.53577(14) 0.1817(4) 0.8204(3) 0.0228(10) Uani 1 1 d . . .
H16A H 0.5030 0.2026 0.7976 0.027 Uiso 1 1 calc R . .
H16B H 0.5349 0.0919 0.8479 0.027 Uiso 1 1 calc R . .
C17 C 0.57073(15) 0.1820(4) 0.7418(3) 0.0275(11) Uani 1 1 d . . .
H17A H 0.5566 0.1305 0.6909 0.033 Uiso 1 1 calc R . .
H17B H 0.6008 0.1367 0.7609 0.033 Uiso 1 1 calc R . .
C18 C 0.58343(14) 0.3226(4) 0.7074(3) 0.0272(11) Uani 1 1 d . . .
H18A H 0.6085 0.3616 0.7475 0.033 Uiso 1 1 calc R . .
H18B H 0.5970 0.3162 0.6452 0.033 Uiso 1 1 calc R . .
C19 C 0.54006(13) 0.4129(3) 0.7059(3) 0.0175(10) Uani 1 1 d . . .
C21 C 0.71654(13) 0.0254(4) 0.2489(3) 0.0217(11) Uani 1 1 d . . .
H21 H 0.7220 0.1185 0.2518 0.026 Uiso 1 1 calc R . .
C22 C 0.67745(15) -0.0228(4) 0.1984(3) 0.0292(12) Uani 1 1 d . . .
C23 C 0.67002(15) -0.1590(4) 0.1985(4) 0.0341(13) Uani 1 1 d . . .
H23 H 0.6436 -0.1954 0.1656 0.041 Uiso 1 1 calc R . .
C24 C 0.70007(15) -0.2406(4) 0.2451(3) 0.0284(12) Uani 1 1 d . . .
H24 H 0.6940 -0.3336 0.2447 0.034 Uiso 1 1 calc R . .
N25 N 0.73838(11) -0.1937(3) 0.2920(2) 0.0186(8) Uani 1 1 d . . .
C26 C 0.77049(16) -0.2891(4) 0.3392(3) 0.0298(12) Uani 1 1 d . . .
H26A H 0.8046 -0.2671 0.3252 0.036 Uiso 1 1 calc R . .
H26B H 0.7640 -0.3799 0.3163 0.036 Uiso 1 1 calc R . .
C27 C 0.76297(17) -0.2859(4) 0.4417(4) 0.0352(13) Uani 1 1 d . . .
H27A H 0.7896 -0.3347 0.4717 0.042 Uiso 1 1 calc R . .
H27B H 0.7324 -0.3319 0.4567 0.042 Uiso 1 1 calc R . .
C28 C 0.76111(14) -0.1412(4) 0.4796(3) 0.0289(11) Uani 1 1 d . . .
H28A H 0.7285 -0.1038 0.4694 0.035 Uiso 1 1 calc R . .
H28B H 0.7670 -0.1429 0.5462 0.035 Uiso 1 1 calc R . .
C29 C 0.79797(13) -0.0535(3) 0.4348(3) 0.0182(10) Uani 1 1 d . . .
C110 C 0.51988(13) 0.4573(4) 0.6265(4) 0.0256(11) Uani 1 1 d . . .
H110 H 0.5332 0.4295 0.5700 0.031 Uiso 1 1 calc R . .
C111 C 0.52014(13) 0.4560(3) 0.7894(3) 0.0173(10) Uani 1 1 d U . .
C112 C 0.54289(13) 0.4151(3) 0.8764(3) 0.0176(10) Uani 1 1 d . . .
C113 C 0.58281(18) 0.5566(4) 1.1027(4) 0.0484(15) Uani 1 1 d . . .
H11A H 0.5534 0.5688 1.1388 0.073 Uiso 1 1 calc R . .
H11B H 0.5927 0.6421 1.0767 0.073 Uiso 1 1 calc R . .
H11C H 0.6086 0.5223 1.1419 0.073 Uiso 1 1 calc R . .
C210 C 0.83802(14) -0.0056(4) 0.4822(3) 0.0237(11) Uani 1 1 d . . .
H210 H 0.8432 -0.0328 0.5435 0.028 Uiso 1 1 calc R . .
C211 C 0.86997(14) 0.0797(3) 0.4420(3) 0.0223(10) Uani 1 1 d . . .
H211 H 0.8969 0.1103 0.4761 0.027 Uiso 1 1 calc R . .
C212 C 0.86422(13) 0.1233(4) 0.3524(3) 0.0194(10) Uani 1 1 d . . .
C213 C 0.89884(14) 0.2176(3) 0.3077(3) 0.0225(11) Uani 1 1 d . . .
H21A H 0.9084 0.1814 0.2476 0.027 Uiso 1 1 calc R . .
H21B H 0.9283 0.2252 0.3456 0.027 Uiso 1 1 calc R . .
C214 C 0.87648(14) 0.3580(3) 0.2944(3) 0.0271(11) Uani 1 1 d . . .
H21C H 0.8790 0.4081 0.3523 0.033 Uiso 1 1 calc R . .
H21D H 0.8953 0.4067 0.2477 0.033 Uiso 1 1 calc R . .
C215 C 0.82382(13) 0.3529(3) 0.2651(3) 0.0230(10) Uani 1 1 d . . .
H21E H 0.8035 0.3277 0.3178 0.028 Uiso 1 1 calc R . .
H21F H 0.8135 0.4422 0.2443 0.028 Uiso 1 1 calc R . .
N216 N 0.81651(12) 0.2549(3) 0.1898(2) 0.0184(8) Uani 1 1 d . . .
C217 C 0.81025(15) 0.2997(4) 0.1051(3) 0.0286(11) Uani 1 1 d . . .
H217 H 0.8115 0.3927 0.0939 0.034 Uiso 1 1 calc R . .
C218 C 0.80206(15) 0.2140(4) 0.0337(3) 0.0251(11) Uani 1 1 d . . .
H218 H 0.7958 0.2483 -0.0255 0.030 Uiso 1 1 calc R . .
C219 C 0.80293(13) 0.0776(4) 0.0478(3) 0.0185(10) Uani 1 1 d . . .
C220 C 0.81215(14) 0.0343(3) 0.1347(3) 0.0188(10) Uani 1 1 d . . .
H220 H 0.8150 -0.0585 0.1454 0.023 Uiso 1 1 calc R . .
C221 C 0.81744(13) 0.1202(3) 0.2070(3) 0.0138(8) Uani 1 1 d . . .
C222 C 0.82366(13) 0.0778(3) 0.3030(3) 0.0160(10) Uani 1 1 d . . .
C223 C 0.79072(13) -0.0125(3) 0.3439(3) 0.0172(10) Uani 1 1 d . . .
C224 C 0.74737(14) -0.0600(4) 0.2946(3) 0.0176(10) Uani 1 1 d . . .
C226 C 0.79405(15) -0.0176(4) -0.0284(3) 0.0276(11) Uani 1 1 d . . .
H22A H 0.8180 -0.0030 -0.0766 0.041 Uiso 1 1 calc R . .
H22B H 0.7615 -0.0033 -0.0530 0.041 Uiso 1 1 calc R . .
H22C H 0.7968 -0.1089 -0.0057 0.041 Uiso 1 1 calc R . .
C227 C 0.64647(15) 0.0697(4) 0.1447(4) 0.0434(15) Uani 1 1 d . . .
H22D H 0.6597 0.0792 0.0831 0.065 Uiso 1 1 calc R . .
H22E H 0.6458 0.1568 0.1746 0.065 Uiso 1 1 calc R . .
H22F H 0.6136 0.0340 0.1411 0.065 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
C11 C112 1.370(6) . ?
C11 C12 1.384(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.376(6) . ?
C12 C113 1.509(6) . ?
C13 C14 1.382(6) . ?
C13 H13 0.9500 . ?
C14 N15 1.326(6) . ?
C14 H14 0.9500 . ?
N15 C112 1.380(4) . ?
N15 C16 1.495(5) . ?
C16 C17 1.505(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.542(5) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.505(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C110 1.367(6) . ?
C19 C111 1.411(6) . ?
C21 C224 1.384(5) . ?
C21 C22 1.398(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.385(6) . ?
C22 C227 1.491(6) . ?
C23 C24 1.354(6) . ?
C23 H23 0.9500 . ?
C24 N25 1.350(5) . ?
C24 H24 0.9500 . ?
N25 C224 1.368(4) . ?
N25 C26 1.480(5) . ?
C26 C27 1.519(6) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.560(6) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.500(5) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C210 1.394(5) . ?
C29 C223 1.410(6) . ?
C110 C110 1.396(7) 4_665 ?
C110 H110 0.9500 . ?
C111 C111 1.424(7) 4_665 ?
C111 C112 1.482(6) . ?
C113 H11A 0.9800 . ?
C113 H11B 0.9800 . ?
C113 H11C 0.9800 . ?
C210 C211 1.366(5) . ?
C210 H210 0.9500 . ?
C211 C212 1.394(6) . ?
C211 H211 0.9500 . ?
C212 C222 1.413(5) . ?
C212 C213 1.500(5) . ?
C213 C214 1.554(5) . ?
C213 H21A 0.9900 . ?
C213 H21B 0.9900 . ?
C214 C215 1.520(5) . ?
C214 H21C 0.9900 . ?
C214 H21D 0.9900 . ?
C215 N216 1.493(5) . ?
C215 H21E 0.9900 . ?
C215 H21F 0.9900 . ?
N216 C217 1.334(5) . ?
N216 C221 1.378(4) . ?
C217 C218 1.376(6) . ?
C217 H217 0.9500 . ?
C218 C219 1.388(5) . ?
C218 H218 0.9500 . ?
C219 C220 1.370(6) . ?
C219 C226 1.493(6) . ?
C220 C221 1.376(5) . ?
C220 H220 0.9500 . ?
C221 C222 1.482(5) . ?
C222 C223 1.420(5) . ?
C223 C224 1.480(5) . ?
C226 H22A 0.9800 . ?
C226 H22B 0.9800 . ?
C226 H22C 0.9800 . ?
C227 H22D 0.9800 . ?
C227 H22E 0.9800 . ?
C227 H22F 0.9800 . ?

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
C112 C11 C12 121.3(4) . . ?
C112 C11 H11 119.3 . . ?
C12 C11 H11 119.3 . . ?
C13 C12 C11 118.2(4) . . ?
C13 C12 C113 121.4(5) . . ?
C11 C12 C113 120.4(4) . . ?
C12 C13 C14 119.7(5) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
N15 C14 C13 121.1(4) . . ?
N15 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C14 N15 C112 120.8(4) . . ?
C14 N15 C16 118.8(3) . . ?
C112 N15 C16 120.4(4) . . ?
N15 C16 C17 111.6(3) . . ?
N15 C16 H16A 109.3 . . ?
C17 C16 H16A 109.3 . . ?
N15 C16 H16B 109.3 . . ?
C17 C16 H16B 109.3 . . ?
H16A C16 H16B 108.0 . . ?
C16 C17 C18 113.5(3) . . ?
C16 C17 H17A 108.9 . . ?
C18 C17 H17A 108.9 . . ?
C16 C17 H17B 108.9 . . ?
C18 C17 H17B 108.9 . . ?
H17A C17 H17B 107.7 . . ?
C19 C18 C17 112.1(3) . . ?
C19 C18 H18A 109.2 . . ?
C17 C18 H18A 109.2 . . ?
C19 C18 H18B 109.2 . . ?
C17 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
C110 C19 C111 118.6(4) . . ?
C110 C19 C18 122.4(4) . . ?
C111 C19 C18 119.0(4) . . ?
C224 C21 C22 121.3(3) . . ?
C224 C21 H21 119.4 . . ?
C22 C21 H21 119.4 . . ?
C23 C22 C21 117.2(4) . . ?
C23 C22 C227 122.2(4) . . ?
C21 C22 C227 120.6(4) . . ?
C24 C23 C22 120.6(4) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
N25 C24 C23 121.9(4) . . ?
N25 C24 H24 119.1 . . ?
C23 C24 H24 119.1 . . ?
C24 N25 C224 120.0(4) . . ?
C24 N25 C26 118.9(3) . . ?
C224 N25 C26 121.0(3) . . ?
N25 C26 C27 111.5(4) . . ?
N25 C26 H26A 109.3 . . ?
C27 C26 H26A 109.3 . . ?
N25 C26 H26B 109.3 . . ?
C27 C26 H26B 109.3 . . ?
H26A C26 H26B 108.0 . . ?
C26 C27 C28 112.2(4) . . ?
C26 C27 H27A 109.2 . . ?
C28 C27 H27A 109.2 . . ?
C26 C27 H27B 109.2 . . ?
C28 C27 H27B 109.2 . . ?
H27A C27 H27B 107.9 . . ?
C29 C28 C27 111.7(3) . . ?
C29 C28 H28A 109.3 . . ?
C27 C28 H28A 109.3 . . ?
C29 C28 H28B 109.3 . . ?
C27 C28 H28B 109.3 . . ?
H28A C28 H28B 107.9 . . ?
C210 C29 C223 119.0(4) . . ?
C210 C29 C28 121.6(4) . . ?
C223 C29 C28 119.3(4) . . ?
C19 C110 C110 121.5(3) . 4_665 ?
C19 C110 H110 119.2 . . ?
C110 C110 H110 119.2 4_665 . ?
C19 C111 C111 119.8(2) . 4_665 ?
C19 C111 C112 119.8(3) . . ?
C111 C111 C112 120.4(2) 4_665 . ?
C11 C112 N15 118.6(4) . . ?
C11 C112 C111 123.4(3) . . ?
N15 C112 C111 117.9(4) . . ?
C12 C113 H11A 109.5 . . ?
C12 C113 H11B 109.5 . . ?
H11A C113 H11B 109.5 . . ?
C12 C113 H11C 109.5 . . ?
H11A C113 H11C 109.5 . . ?
H11B C113 H11C 109.5 . . ?
C211 C210 C29 121.0(4) . . ?
C211 C210 H210 119.5 . . ?
C29 C210 H210 119.5 . . ?
C210 C211 C212 122.1(4) . . ?
C210 C211 H211 119.0 . . ?
C212 C211 H211 119.0 . . ?
C211 C212 C222 118.2(4) . . ?
C211 C212 C213 122.6(4) . . ?
C222 C212 C213 119.2(4) . . ?
C212 C213 C214 112.1(3) . . ?
C212 C213 H21A 109.2 . . ?
C214 C213 H21A 109.2 . . ?
C212 C213 H21B 109.2 . . ?
C214 C213 H21B 109.2 . . ?
H21A C213 H21B 107.9 . . ?
C215 C214 C213 112.7(3) . . ?
C215 C214 H21C 109.0 . . ?
C213 C214 H21C 109.0 . . ?
C215 C214 H21D 109.0 . . ?
C213 C214 H21D 109.0 . . ?
H21C C214 H21D 107.8 . . ?
N216 C215 C214 111.2(3) . . ?
N216 C215 H21E 109.4 . . ?
C214 C215 H21E 109.4 . . ?
N216 C215 H21F 109.4 . . ?
C214 C215 H21F 109.4 . . ?
H21E C215 H21F 108.0 . . ?
C217 N216 C221 120.3(3) . . ?
C217 N216 C215 118.9(3) . . ?
C221 N216 C215 120.8(3) . . ?
N216 C217 C218 121.3(3) . . ?
N216 C217 H217 119.3 . . ?
C218 C217 H217 119.3 . . ?
C217 C218 C219 120.2(4) . . ?
C217 C218 H218 119.9 . . ?
C219 C218 H218 119.9 . . ?
C220 C219 C218 117.1(4) . . ?
C220 C219 C226 121.6(3) . . ?
C218 C219 C226 121.3(4) . . ?
C219 C220 C221 122.5(3) . . ?
C219 C220 H220 118.8 . . ?
C221 C220 H220 118.8 . . ?
C220 C221 N216 118.4(4) . . ?
C220 C221 C222 124.4(3) . . ?
N216 C221 C222 117.3(3) . . ?
C212 C222 C223 120.0(4) . . ?
C212 C222 C221 119.2(3) . . ?
C223 C222 C221 120.8(3) . . ?
C29 C223 C222 119.7(4) . . ?
C29 C223 C224 118.9(4) . . ?
C222 C223 C224 121.3(4) . . ?
N25 C224 C21 119.0(4) . . ?
N25 C224 C223 118.5(3) . . ?
C21 C224 C223 122.5(3) . . ?
C219 C226 H22A 109.5 . . ?
C219 C226 H22B 109.5 . . ?
H22A C226 H22B 109.5 . . ?
C219 C226 H22C 109.5 . . ?
H22A C226 H22C 109.5 . . ?
H22B C226 H22C 109.5 . . ?
C22 C227 H22D 109.5 . . ?
C22 C227 H22E 109.5 . . ?
H22D C227 H22E 109.5 . . ?
C22 C227 H22F 109.5 . . ?
H22D C227 H22F 109.5 . . ?
H22E C227 H22F 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
C112 C11 C12 C13 3.9(7) . . . . ?
C112 C11 C12 C113 -174.7(4) . . . . ?
C11 C12 C13 C14 -1.5(7) . . . . ?
C113 C12 C13 C14 177.1(5) . . . . ?
C12 C13 C14 N15 -2.5(8) . . . . ?
C13 C14 N15 C112 4.0(7) . . . . ?
C13 C14 N15 C16 -176.8(4) . . . . ?
C14 N15 C16 C17 -105.4(4) . . . . ?
C112 N15 C16 C17 73.8(5) . . . . ?
N15 C16 C17 C18 -46.3(5) . . . . ?
C16 C17 C18 C19 -40.0(5) . . . . ?
C17 C18 C19 C110 -111.3(4) . . . . ?
C17 C18 C19 C111 70.3(5) . . . . ?
C224 C21 C22 C23 2.0(7) . . . . ?
C224 C21 C22 C227 -176.0(4) . . . . ?
C21 C22 C23 C24 -0.8(7) . . . . ?
C227 C22 C23 C24 177.2(5) . . . . ?
C22 C23 C24 N25 -0.7(7) . . . . ?
C23 C24 N25 C224 0.9(7) . . . . ?
C23 C24 N25 C26 -178.3(4) . . . . ?
C24 N25 C26 C27 -106.2(4) . . . . ?
C224 N25 C26 C27 74.6(5) . . . . ?
N25 C26 C27 C28 -46.1(5) . . . . ?
C26 C27 C28 C29 -40.4(5) . . . . ?
C27 C28 C29 C210 -110.8(4) . . . . ?
C27 C28 C29 C223 72.7(5) . . . . ?
C111 C19 C110 C110 -0.6(6) . . . 4_665 ?
C18 C19 C110 C110 -179.0(4) . . . 4_665 ?
C110 C19 C111 C111 -0.1(6) . . . 4_665 ?
C18 C19 C111 C111 178.4(4) . . . 4_665 ?
C110 C19 C111 C112 -176.8(3) . . . . ?
C18 C19 C111 C112 1.7(5) . . . . ?
C12 C11 C112 N15 -2.5(6) . . . . ?
C12 C11 C112 C111 174.7(4) . . . . ?
C14 N15 C112 C11 -1.5(6) . . . . ?
C16 N15 C112 C11 179.3(4) . . . . ?
C14 N15 C112 C111 -178.9(4) . . . . ?
C16 N15 C112 C111 1.9(6) . . . . ?
C19 C111 C112 C11 128.3(4) . . . . ?
C111 C111 C112 C11 -48.3(6) 4_665 . . . ?
C19 C111 C112 N15 -54.4(5) . . . . ?
C111 C111 C112 N15 128.9(4) 4_665 . . . ?
C223 C29 C210 C211 0.0(5) . . . . ?
C28 C29 C210 C211 -176.5(3) . . . . ?
C29 C210 C211 C212 0.2(6) . . . . ?
C210 C211 C212 C222 0.6(5) . . . . ?
C210 C211 C212 C213 179.6(3) . . . . ?
C211 C212 C213 C214 -108.5(4) . . . . ?
C222 C212 C213 C214 70.5(5) . . . . ?
C212 C213 C214 C215 -40.0(5) . . . . ?
C213 C214 C215 N216 -46.5(5) . . . . ?
C214 C215 N216 C217 -104.3(4) . . . . ?
C214 C215 N216 C221 74.0(5) . . . . ?
C221 N216 C217 C218 3.5(7) . . . . ?
C215 N216 C217 C218 -178.2(4) . . . . ?
N216 C217 C218 C219 -3.7(7) . . . . ?
C217 C218 C219 C220 0.0(6) . . . . ?
C217 C218 C219 C226 179.9(4) . . . . ?
C218 C219 C220 C221 4.0(6) . . . . ?
C226 C219 C220 C221 -175.9(4) . . . . ?
C219 C220 C221 N216 -4.3(6) . . . . ?
C219 C220 C221 C222 175.1(4) . . . . ?
C217 N216 C221 C220 0.5(6) . . . . ?
C215 N216 C221 C220 -177.8(3) . . . . ?
C217 N216 C221 C222 -178.9(4) . . . . ?
C215 N216 C221 C222 2.8(5) . . . . ?
C211 C212 C222 C223 -1.5(5) . . . . ?
C213 C212 C222 C223 179.4(3) . . . . ?
C211 C212 C222 C221 -178.5(3) . . . . ?
C213 C212 C222 C221 2.4(5) . . . . ?
C220 C221 C222 C212 124.6(4) . . . . ?
N216 C221 C222 C212 -56.0(5) . . . . ?
C220 C221 C222 C223 -52.4(5) . . . . ?
N216 C221 C222 C223 127.0(4) . . . . ?
C210 C29 C223 C222 -1.0(5) . . . . ?
C28 C29 C223 C222 175.6(3) . . . . ?
C210 C29 C223 C224 -178.1(3) . . . . ?
C28 C29 C223 C224 -1.4(5) . . . . ?
C212 C222 C223 C29 1.8(5) . . . . ?
C221 C222 C223 C29 178.7(3) . . . . ?
C212 C222 C223 C224 178.8(3) . . . . ?
C221 C222 C223 C224 -4.3(5) . . . . ?
C24 N25 C224 C21 0.3(6) . . . . ?
C26 N25 C224 C21 179.5(4) . . . . ?
C24 N25 C224 C223 -177.8(4) . . . . ?
C26 N25 C224 C223 1.4(6) . . . . ?
C22 C21 C224 N25 -1.8(7) . . . . ?
C22 C21 C224 C223 176.2(4) . . . . ?
C29 C223 C224 N25 -52.7(5) . . . . ?
C222 C223 C224 N25 130.3(4) . . . . ?
C29 C223 C224 C21 129.3(4) . . . . ?
C222 C223 C224 C21 -47.7(6) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.070

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.000 -0.032 0.633 519 151 ' '
2 0.500 -0.012 0.367 519 151 ' '
_platon_squeeze_details          
;
Mix of disordered solvents (toluene, acetonitrile) were removed.
;

#===END

####################################################################### 
# 
# 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_ls803_teply
_database_code_depnum_ccdc_archive 'CCDC 1004343'
_audit_update_record             
;
2014-05-20 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H26 N2, 2(Br), 3(H2 O)'
_chemical_formula_sum            'C24 H32 Br2 N2 O3'
_chemical_formula_weight         556.34
_chemical_compound_source        'synthesized by the authors'
_chemical_absolute_configuration ad


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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

_cell_length_a                   12.7303(4)
_cell_length_b                   12.7933(5)
_cell_length_c                   14.8125(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2412.40(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5777
_cell_measurement_theta_min      2.6430
_cell_measurement_theta_max      27.3999

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1136
_exptl_absorpt_coefficient_mu    3.388
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.3843
_exptl_absorpt_correction_T_max  0.5902
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13720
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.10
_diffrn_reflns_theta_max         27.49
_reflns_number_total             5525
_reflns_number_gt                4905
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'Bruker Instrument Service v2012.12.0.0'
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_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)+(0.0244P)²+0.4250P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.022(6)
_refine_ls_number_reflns         5525
_refine_ls_number_parameters     282
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0272
_refine_ls_wR_factor_ref         0.0547
_refine_ls_wR_factor_gt          0.0529
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_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 0.38530(17) 0.31890(17) 0.42632(16) 0.0170(5) Uani 1 1 d . . .
H1 H 0.4003 0.3819 0.4578 0.020 Uiso 1 1 calc R . .
C2 C 0.43519(18) 0.29778(19) 0.34567(17) 0.0195(5) Uani 1 1 d . . .
H2 H 0.4835 0.3465 0.3207 0.023 Uiso 1 1 calc R . .
C3 C 0.41392(17) 0.20462(18) 0.30147(17) 0.0201(5) Uani 1 1 d . . .
H3 H 0.4483 0.1892 0.2461 0.024 Uiso 1 1 calc R . .
C4 C 0.34305(18) 0.13399(19) 0.33739(17) 0.0181(5) Uani 1 1 d . . .
N5 N 0.29435(13) 0.15725(14) 0.41628(15) 0.0160(4) Uani 1 1 d . . .
C6 C 0.21972(17) 0.0821(2) 0.46005(18) 0.0225(5) Uani 1 1 d . . .
H6A H 0.1935 0.0320 0.4144 0.027 Uiso 1 1 calc R . .
H6B H 0.1587 0.1209 0.4845 0.027 Uiso 1 1 calc R . .
C7 C 0.2732(2) 0.02321(19) 0.5353(2) 0.0268(6) Uani 1 1 d . . .
H7A H 0.3219 -0.0288 0.5089 0.032 Uiso 1 1 calc R . .
H7B H 0.2196 -0.0153 0.5705 0.032 Uiso 1 1 calc R . .
C8 C 0.33514(18) 0.09538(19) 0.59972(18) 0.0227(6) Uani 1 1 d . . .
H8A H 0.3486 0.0580 0.6571 0.027 Uiso 1 1 calc R . .
H8B H 0.4039 0.1126 0.5722 0.027 Uiso 1 1 calc R . .
C9 C 0.27637(17) 0.19505(18) 0.61922(17) 0.0169(5) Uani 1 1 d . . .
C10 C 0.23719(17) 0.21914(19) 0.70420(18) 0.0211(5) Uani 1 1 d . . .
H10 H 0.2478 0.1714 0.7525 0.025 Uiso 1 1 calc R . .
C11 C 0.18291(18) 0.31134(18) 0.72027(17) 0.0198(5) Uani 1 1 d . . .
H11 H 0.1573 0.3259 0.7792 0.024 Uiso 1 1 calc R . .
C12 C 0.16558(17) 0.38284(18) 0.65088(17) 0.0170(5) Uani 1 1 d . . .
C13 C 0.10867(19) 0.48414(18) 0.66676(17) 0.0199(5) Uani 1 1 d . . .
H13A H 0.0754 0.4825 0.7272 0.024 Uiso 1 1 calc R . .
H13B H 0.0522 0.4918 0.6212 0.024 Uiso 1 1 calc R . .
C14 C 0.18286(18) 0.57886(19) 0.66099(17) 0.0206(5) Uani 1 1 d . . .
H14A H 0.1408 0.6430 0.6512 0.025 Uiso 1 1 calc R . .
H14B H 0.2207 0.5866 0.7190 0.025 Uiso 1 1 calc R . .
C15 C 0.26254(16) 0.56770(17) 0.58467(17) 0.0168(5) Uani 1 1 d . . .
H15A H 0.2995 0.6350 0.5756 0.020 Uiso 1 1 calc R . .
H15B H 0.3155 0.5143 0.6011 0.020 Uiso 1 1 calc R . .
N16 N 0.20909(14) 0.53656(15) 0.49947(13) 0.0141(4) Uani 1 1 d . . .
C17 C 0.18428(16) 0.60900(18) 0.43636(17) 0.0185(5) Uani 1 1 d . . .
C18 C 0.13541(16) 0.5771(2) 0.35779(16) 0.0217(5) Uani 1 1 d . . .
H18 H 0.1187 0.6271 0.3126 0.026 Uiso 1 1 calc R . .
C19 C 0.11083(19) 0.4738(2) 0.34443(18) 0.0251(6) Uani 1 1 d . . .
H19 H 0.0779 0.4523 0.2899 0.030 Uiso 1 1 calc R . .
C20 C 0.13402(16) 0.4013(2) 0.41043(17) 0.0195(5) Uani 1 1 d . . .
H20 H 0.1163 0.3298 0.4019 0.023 Uiso 1 1 calc R . .
C21 C 0.18330(16) 0.43317(18) 0.48911(17) 0.0156(5) Uani 1 1 d . . .
C22 C 0.20560(17) 0.36008(17) 0.56481(16) 0.0134(5) Uani 1 1 d . . .
C23 C 0.26068(17) 0.26709(18) 0.54974(16) 0.0162(5) Uani 1 1 d . . .
C24 C 0.31384(17) 0.24902(17) 0.46130(16) 0.0154(5) Uani 1 1 d . . .
C25 C 0.3222(2) 0.0315(2) 0.2926(2) 0.0289(6) Uani 1 1 d . . .
H25A H 0.3378 -0.0254 0.3347 0.043 Uiso 1 1 calc R . .
H25B H 0.3669 0.0248 0.2390 0.043 Uiso 1 1 calc R . .
H25C H 0.2482 0.0279 0.2746 0.043 Uiso 1 1 calc R . .
C26 C 0.21096(19) 0.72191(19) 0.45287(19) 0.0252(6) Uani 1 1 d . . .
H26A H 0.1857 0.7427 0.5128 0.038 Uiso 1 1 calc R . .
H26B H 0.1772 0.7654 0.4068 0.038 Uiso 1 1 calc R . .
H26C H 0.2873 0.7312 0.4498 0.038 Uiso 1 1 calc R . .
Br1 Br 0.510833(18) 0.08717(2) 0.081467(17) 0.02325(6) Uani 1 1 d . . .
Br2 Br 0.38733(2) 0.78568(2) 0.70180(2) 0.03879(9) Uani 1 1 d . . .
O1W O 0.45334(14) 0.09227(15) 0.86204(12) 0.0328(4) Uani 1 1 d . . .
H11W H 0.4802 0.1478 0.8430 0.039 Uiso 1 1 d R . .
H12W H 0.4514 0.0913 0.9256 0.039 Uiso 1 1 d R . .
O2W O 0.46745(18) 0.38219(19) 0.63430(16) 0.0601(7) Uani 1 1 d . . .
H21W H 0.4954 0.4458 0.6322 0.072 Uiso 1 1 d R . .
H22W H 0.5114 0.3408 0.6728 0.072 Uiso 1 1 d R . .
O3W O 0.46521(14) 0.84114(15) 0.47987(15) 0.0385(5) Uani 1 1 d . . .
H31W H 0.4527 0.8247 0.5400 0.046 Uiso 1 1 d R . .
H32W H 0.4787 0.7753 0.4538 0.046 Uiso 1 1 d 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
C1 C24 1.377(3) . ?
C1 C2 1.380(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.387(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.383(3) . ?
C3 H3 0.9500 . ?
C4 N5 1.356(3) . ?
C4 C25 1.493(3) . ?
N5 C24 1.373(3) . ?
N5 C6 1.499(3) . ?
C6 C7 1.508(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.544(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.506(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.389(3) . ?
C9 C23 1.396(3) . ?
C10 C11 1.388(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.394(3) . ?
C11 H11 0.9500 . ?
C12 C22 1.404(3) . ?
C12 C13 1.503(3) . ?
C13 C14 1.539(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.526(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 N16 1.488(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
N16 C17 1.354(3) . ?
N16 C21 1.371(3) . ?
C17 C18 1.381(3) . ?
C17 C26 1.504(3) . ?
C18 C19 1.372(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.380(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.385(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.487(3) . ?
C22 C23 1.399(3) . ?
C23 C24 1.493(3) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
O1W H11W 0.8372 . ?
O1W H12W 0.9423 . ?
O2W H21W 0.8886 . ?
O2W H22W 0.9587 . ?
O3W H31W 0.9295 . ?
O3W H32W 0.9419 . ?

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
C24 C1 C2 120.2(2) . . ?
C24 C1 H1 119.9 . . ?
C2 C1 H1 119.9 . . ?
C1 C2 C3 119.2(2) . . ?
C1 C2 H2 120.4 . . ?
C3 C2 H2 120.4 . . ?
C4 C3 C2 120.5(2) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
N5 C4 C3 119.1(2) . . ?
N5 C4 C25 119.6(2) . . ?
C3 C4 C25 121.2(2) . . ?
C4 N5 C24 121.6(2) . . ?
C4 N5 C6 121.4(2) . . ?
C24 N5 C6 116.9(2) . . ?
N5 C6 C7 110.74(19) . . ?
N5 C6 H6A 109.5 . . ?
C7 C6 H6A 109.5 . . ?
N5 C6 H6B 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
C6 C7 C8 112.9(2) . . ?
C6 C7 H7A 109.0 . . ?
C8 C7 H7A 109.0 . . ?
C6 C7 H7B 109.0 . . ?
C8 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C9 C8 C7 111.8(2) . . ?
C9 C8 H8A 109.3 . . ?
C7 C8 H8A 109.3 . . ?
C9 C8 H8B 109.3 . . ?
C7 C8 H8B 109.3 . . ?
H8A C8 H8B 107.9 . . ?
C10 C9 C23 118.1(2) . . ?
C10 C9 C8 122.7(2) . . ?
C23 C9 C8 119.2(2) . . ?
C11 C10 C9 121.5(2) . . ?
C11 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
C10 C11 C12 120.7(2) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C11 C12 C22 118.4(2) . . ?
C11 C12 C13 121.8(2) . . ?
C22 C12 C13 119.7(2) . . ?
C12 C13 C14 111.99(19) . . ?
C12 C13 H13A 109.2 . . ?
C14 C13 H13A 109.2 . . ?
C12 C13 H13B 109.2 . . ?
C14 C13 H13B 109.2 . . ?
H13A C13 H13B 107.9 . . ?
C15 C14 C13 112.06(19) . . ?
C15 C14 H14A 109.2 . . ?
C13 C14 H14A 109.2 . . ?
C15 C14 H14B 109.2 . . ?
C13 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
N16 C15 C14 110.46(17) . . ?
N16 C15 H15A 109.6 . . ?
C14 C15 H15A 109.6 . . ?
N16 C15 H15B 109.6 . . ?
C14 C15 H15B 109.6 . . ?
H15A C15 H15B 108.1 . . ?
C17 N16 C21 121.8(2) . . ?
C17 N16 C15 120.60(19) . . ?
C21 N16 C15 117.55(19) . . ?
N16 C17 C18 119.0(2) . . ?
N16 C17 C26 119.5(2) . . ?
C18 C17 C26 121.5(2) . . ?
C19 C18 C17 120.6(2) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C18 C19 C20 119.8(2) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.1 . . ?
C19 C20 C21 119.7(2) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 H20 120.2 . . ?
N16 C21 C20 119.1(2) . . ?
N16 C21 C22 118.4(2) . . ?
C20 C21 C22 122.4(2) . . ?
C23 C22 C12 120.2(2) . . ?
C23 C22 C21 120.7(2) . . ?
C12 C22 C21 119.0(2) . . ?
C9 C23 C22 121.0(2) . . ?
C9 C23 C24 118.7(2) . . ?
C22 C23 C24 119.9(2) . . ?
N5 C24 C1 119.5(2) . . ?
N5 C24 C23 118.5(2) . . ?
C1 C24 C23 122.0(2) . . ?
C4 C25 H25A 109.5 . . ?
C4 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C4 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C17 C26 H26A 109.5 . . ?
C17 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C17 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
H11W O1W H12W 111.0 . . ?
H21W O2W H22W 107.0 . . ?
H31W O3W H32W 102.8 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.059
#===END
####################################################################### 
# 
# 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_pr274_teply_sqd
_database_code_depnum_ccdc_archive 'CCDC 1004344'
_audit_update_record             
;
2014-05-20 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H44 N4, 2(C F3 O3 S)'
_chemical_formula_sum            'C44 H44 F6 N4 O6 S2'
_chemical_formula_weight         902.95
_chemical_compound_source        'synthesized by the authors'

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'
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'
S S 0.1246 0.1234 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

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

_cell_length_a                   25.3083(18)
_cell_length_b                   17.1165(12)
_cell_length_c                   42.198(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     18280(2)
_cell_formula_units_Z            16
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8325
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      25.6

_exptl_crystal_description       plate
_exptl_crystal_colour            violet
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7520
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9018
_exptl_absorpt_correction_T_max  0.9842
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            96260
_diffrn_reflns_av_R_equivalents  0.0949
_diffrn_reflns_av_sigmaI/netI    0.1243
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_theta_min         1.26
_diffrn_reflns_theta_max         26.00
_reflns_number_total             17955
_reflns_number_gt                8822
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'Bruker Instrument Service v2012.12.0.3'
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 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)+(0.1525P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         17955
_refine_ls_number_parameters     1105
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1946
_refine_ls_R_factor_gt           0.1056
_refine_ls_wR_factor_ref         0.2946
_refine_ls_wR_factor_gt          0.2538
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_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
C11 C 0.18837(17) 0.7119(3) 0.90987(10) 0.0180(11) Uani 1 1 d . . .
H11 H 0.1768 0.7048 0.8886 0.022 Uiso 1 1 calc R . .
C12 C 0.17430(19) 0.7804(3) 0.92587(10) 0.0198(11) Uani 1 1 d . . .
C13 C 0.1914(2) 0.7860(3) 0.95801(11) 0.0281(13) Uani 1 1 d . . .
H13 H 0.1830 0.8313 0.9700 0.034 Uiso 1 1 calc R . .
C14 C 0.2194(2) 0.7275(3) 0.97155(11) 0.0264(13) Uani 1 1 d . . .
H14 H 0.2288 0.7312 0.9933 0.032 Uiso 1 1 calc R . .
N15 N 0.23423(15) 0.6642(2) 0.95483(8) 0.0200(10) Uani 1 1 d . . .
C16 C 0.2660(2) 0.6032(3) 0.97109(11) 0.0238(12) Uani 1 1 d . . .
H16A H 0.2842 0.6262 0.9896 0.029 Uiso 1 1 calc R . .
H16B H 0.2932 0.5826 0.9564 0.029 Uiso 1 1 calc R . .
C17 C 0.2297(2) 0.5364(3) 0.98197(11) 0.0325(14) Uani 1 1 d . . .
H17A H 0.2515 0.4907 0.9879 0.039 Uiso 1 1 calc R . .
H17B H 0.2099 0.5532 1.0010 0.039 Uiso 1 1 calc R . .
C18 C 0.1905(2) 0.5125(3) 0.95598(11) 0.0306(14) Uani 1 1 d . . .
H18A H 0.1755 0.4605 0.9610 0.037 Uiso 1 1 calc R . .
H18B H 0.1610 0.5506 0.9552 0.037 Uiso 1 1 calc R . .
C19 C 0.2176(2) 0.5096(3) 0.92407(11) 0.0244(12) Uani 1 1 d . . .
C110 C 0.2293(2) 0.4381(3) 0.91023(12) 0.0278(13) Uani 1 1 d . . .
H110 H 0.2206 0.3910 0.9209 0.033 Uiso 1 1 calc R . .
C111 C 0.2535(2) 0.4351(3) 0.88098(12) 0.0280(13) Uani 1 1 d . . .
H111 H 0.2609 0.3856 0.8718 0.034 Uiso 1 1 calc R . .
C112 C 0.2674(2) 0.5022(3) 0.86458(11) 0.0245(13) Uani 1 1 d . . .
C113 C 0.2915(2) 0.4982(3) 0.83208(12) 0.0312(14) Uani 1 1 d . . .
H11A H 0.3033 0.4442 0.8277 0.037 Uiso 1 1 calc R . .
H11B H 0.3227 0.5329 0.8311 0.037 Uiso 1 1 calc R . .
C114 C 0.2510(2) 0.5235(3) 0.80694(12) 0.0343(14) Uani 1 1 d . . .
H11C H 0.2698 0.5346 0.7868 0.041 Uiso 1 1 calc R . .
H11D H 0.2262 0.4799 0.8030 0.041 Uiso 1 1 calc R . .
C115 C 0.2199(2) 0.5955(3) 0.81678(11) 0.0277(13) Uani 1 1 d . . .
H11E H 0.2020 0.6181 0.7981 0.033 Uiso 1 1 calc R . .
H11F H 0.1926 0.5806 0.8324 0.033 Uiso 1 1 calc R . .
N116 N 0.25606(16) 0.6544(2) 0.83090(9) 0.0218(10) Uani 1 1 d . . .
C117 C 0.2728(2) 0.7155(3) 0.81303(11) 0.0286(13) Uani 1 1 d . . .
H117 H 0.2609 0.7196 0.7917 0.034 Uiso 1 1 calc R . .
C118 C 0.3058(2) 0.7707(3) 0.82457(11) 0.0288(13) Uani 1 1 d . . .
H118 H 0.3172 0.8120 0.8112 0.035 Uiso 1 1 calc R . .
C119 C 0.32337(18) 0.7678(3) 0.85625(10) 0.0196(12) Uani 1 1 d . . .
C120 C 0.30597(18) 0.7023(3) 0.87396(10) 0.0191(11) Uani 1 1 d . . .
H120 H 0.3172 0.6972 0.8953 0.023 Uiso 1 1 calc R . .
C121 C 0.27365(19) 0.6464(3) 0.86143(10) 0.0188(11) Uani 1 1 d . . .
C122 C 0.25660(19) 0.5754(3) 0.87853(10) 0.0215(12) Uani 1 1 d . . .
C123 C 0.23199(18) 0.5788(3) 0.90842(11) 0.0201(12) Uani 1 1 d . . .
C124 C 0.21848(18) 0.6545(3) 0.92395(10) 0.0173(11) Uani 1 1 d . . .
C125 C 0.14549(19) 0.8419(3) 0.91003(11) 0.0224(12) Uani 1 1 d . . .
H125 H 0.1362 0.8348 0.8884 0.027 Uiso 1 1 calc R . .
C126 C 0.13111(19) 0.9090(3) 0.92453(11) 0.0258(13) Uani 1 1 d . . .
H126 H 0.1376 0.9110 0.9467 0.031 Uiso 1 1 calc R . .
C127 C 0.1072(2) 0.9782(3) 0.91101(11) 0.0246(12) Uani 1 1 d . . .
C128 C 0.09734(19) 0.9898(3) 0.87882(11) 0.0236(12) Uani 1 1 d . . .
H128 H 0.1039 0.9483 0.8644 0.028 Uiso 1 1 calc R . .
C129 C 0.07838(18) 1.0595(3) 0.86725(11) 0.0227(12) Uani 1 1 d . . .
H129 H 0.0725 1.0654 0.8451 0.027 Uiso 1 1 calc R . .
C130 C 0.06764(19) 1.1226(3) 0.88796(11) 0.0224(12) Uani 1 1 d . . .
C131 C 0.0768(2) 1.1111(3) 0.92009(12) 0.0318(14) Uani 1 1 d . . .
H131 H 0.0696 1.1521 0.9346 0.038 Uiso 1 1 calc R . .
C132 C 0.0961(2) 1.0412(3) 0.93112(12) 0.0353(15) Uani 1 1 d . . .
H132 H 0.1020 1.0353 0.9532 0.042 Uiso 1 1 calc R . .
C133 C 0.0423(2) 1.2056(3) 0.84314(11) 0.0315(14) Uani 1 1 d . . .
H13A H 0.0748 1.1925 0.8317 0.047 Uiso 1 1 calc R . .
H13B H 0.0332 1.2604 0.8392 0.047 Uiso 1 1 calc R . .
H13C H 0.0134 1.1721 0.8357 0.047 Uiso 1 1 calc R . .
C134 C 0.0289(2) 1.2510(3) 0.89868(13) 0.0369(15) Uani 1 1 d . . .
H13D H -0.0009 1.2282 0.9103 0.055 Uiso 1 1 calc R . .
H13E H 0.0168 1.2968 0.8868 0.055 Uiso 1 1 calc R . .
H13F H 0.0564 1.2667 0.9137 0.055 Uiso 1 1 calc R . .
C135 C 0.35425(19) 0.8281(3) 0.87055(11) 0.0228(12) Uani 1 1 d . . .
H135 H 0.3636 0.8225 0.8922 0.027 Uiso 1 1 calc R . .
C136 C 0.37114(19) 0.8930(3) 0.85500(11) 0.0236(12) Uani 1 1 d . . .
H136 H 0.3664 0.8927 0.8327 0.028 Uiso 1 1 calc R . .
C137 C 0.39522(19) 0.9622(3) 0.86795(11) 0.0229(12) Uani 1 1 d . . .
C138 C 0.40721(19) 0.9726(3) 0.89988(11) 0.0254(13) Uani 1 1 d . . .
H138 H 0.4017 0.9304 0.9141 0.030 Uiso 1 1 calc R . .
C139 C 0.4265(2) 1.0410(4) 0.91138(12) 0.0327(14) Uani 1 1 d . . .
H139 H 0.4345 1.0453 0.9333 0.039 Uiso 1 1 calc R . .
C140 C 0.4351(2) 1.1065(3) 0.89117(12) 0.0294(13) Uani 1 1 d . . .
C141 C 0.4255(2) 1.0946(3) 0.85893(12) 0.0320(14) Uani 1 1 d . . .
H141 H 0.4327 1.1357 0.8444 0.038 Uiso 1 1 calc R . .
C142 C 0.4059(2) 1.0248(3) 0.84759(12) 0.0259(13) Uani 1 1 d . . .
H142 H 0.3995 1.0191 0.8255 0.031 Uiso 1 1 calc R . .
C143 C 0.4627(3) 1.1868(4) 0.93580(16) 0.062(2) Uani 1 1 d . . .
H14A H 0.4320 1.1708 0.9484 0.094 Uiso 1 1 calc R . .
H14B H 0.4706 1.2418 0.9400 0.094 Uiso 1 1 calc R . .
H14C H 0.4932 1.1546 0.9416 0.094 Uiso 1 1 calc R . .
C144 C 0.4644(2) 1.2390(4) 0.88128(15) 0.0452(17) Uani 1 1 d . . .
H14D H 0.4965 1.2255 0.8696 0.068 Uiso 1 1 calc R . .
H14E H 0.4703 1.2871 0.8934 0.068 Uiso 1 1 calc R . .
H14F H 0.4353 1.2471 0.8663 0.068 Uiso 1 1 calc R . .
N11 N 0.05022(18) 1.1936(3) 0.87688(10) 0.0300(11) Uani 1 1 d . . .
N12 N 0.45115(19) 1.1766(3) 0.90258(11) 0.0414(13) Uani 1 1 d . . .
C21 C 0.30789(18) 0.0368(3) 0.16228(10) 0.0203(12) Uani 1 1 d . . .
H21 H 0.3205 0.0311 0.1412 0.024 Uiso 1 1 calc R . .
C22 C 0.32293(19) 0.1032(3) 0.17997(11) 0.0234(12) Uani 1 1 d . . .
C23 C 0.3037(2) 0.1062(3) 0.21155(11) 0.0275(13) Uani 1 1 d . . .
H23 H 0.3135 0.1486 0.2249 0.033 Uiso 1 1 calc R . .
C24 C 0.27195(19) 0.0499(3) 0.22280(11) 0.0232(12) Uani 1 1 d . . .
H24 H 0.2596 0.0534 0.2440 0.028 Uiso 1 1 calc R . .
N25 N 0.25702(16) -0.0118(2) 0.20484(8) 0.0204(10) Uani 1 1 d . . .
C26 C 0.2204(2) -0.0714(3) 0.21855(12) 0.0264(13) Uani 1 1 d . . .
H26A H 0.1943 -0.0876 0.2024 0.032 Uiso 1 1 calc R . .
H26B H 0.2010 -0.0487 0.2367 0.032 Uiso 1 1 calc R . .
C27 C 0.2522(2) -0.1426(4) 0.22956(12) 0.0366(15) Uani 1 1 d . . .
H27A H 0.2699 -0.1302 0.2499 0.044 Uiso 1 1 calc R . .
H27B H 0.2278 -0.1868 0.2333 0.044 Uiso 1 1 calc R . .
C28 C 0.2937(2) -0.1669(3) 0.20521(11) 0.0320(14) Uani 1 1 d . . .
H28A H 0.3243 -0.1309 0.2065 0.038 Uiso 1 1 calc R . .
H28B H 0.3064 -0.2203 0.2101 0.038 Uiso 1 1 calc R . .
C29 C 0.2713(2) -0.1651(3) 0.17238(11) 0.0262(13) Uani 1 1 d . . .
C210 C 0.2588(2) -0.2332(3) 0.15614(13) 0.0321(14) Uani 1 1 d . . .
H210 H 0.2653 -0.2821 0.1660 0.038 Uiso 1 1 calc R . .
C211 C 0.2374(2) -0.2319(3) 0.12626(13) 0.0299(14) Uani 1 1 d . . .
H211 H 0.2300 -0.2799 0.1159 0.036 Uiso 1 1 calc R . .
C212 C 0.2262(2) -0.1622(3) 0.11092(11) 0.0260(13) Uani 1 1 d . . .
C213 C 0.2037(2) -0.1600(3) 0.07837(11) 0.0300(13) Uani 1 1 d . . .
H21A H 0.1734 -0.1236 0.0779 0.036 Uiso 1 1 calc R . .
H21B H 0.1906 -0.2126 0.0727 0.036 Uiso 1 1 calc R . .
C214 C 0.2448(2) -0.1339(3) 0.05391(11) 0.0331(14) Uani 1 1 d . . .
H21C H 0.2687 -0.1782 0.0491 0.040 Uiso 1 1 calc R . .
H21D H 0.2266 -0.1189 0.0341 0.040 Uiso 1 1 calc R . .
C215 C 0.2770(2) -0.0657(3) 0.06577(11) 0.0277(13) Uani 1 1 d . . .
H21E H 0.3032 -0.0842 0.0815 0.033 Uiso 1 1 calc R . .
H21F H 0.2965 -0.0418 0.0479 0.033 Uiso 1 1 calc R . .
N216 N 0.24181(16) -0.0060(3) 0.08067(8) 0.0204(10) Uani 1 1 d . . .
C217 C 0.2270(2) 0.0569(3) 0.06440(11) 0.0296(13) Uani 1 1 d . . .
H217 H 0.2394 0.0628 0.0433 0.036 Uiso 1 1 calc R . .
C218 C 0.1949(2) 0.1132(3) 0.07668(11) 0.0286(13) Uani 1 1 d . . .
H218 H 0.1848 0.1569 0.0642 0.034 Uiso 1 1 calc R . .
C219 C 0.17670(19) 0.1060(3) 0.10815(10) 0.0195(11) Uani 1 1 d . . .
C220 C 0.19202(18) 0.0384(3) 0.12459(10) 0.0201(12) Uani 1 1 d . . .
H220 H 0.1800 0.0309 0.1457 0.024 Uiso 1 1 calc R . .
C221 C 0.22415(19) -0.0174(3) 0.11084(10) 0.0187(11) Uani 1 1 d . . .
C222 C 0.23881(19) -0.0913(3) 0.12697(11) 0.0226(12) Uani 1 1 d . . .
C223 C 0.26091(19) -0.0932(3) 0.15756(10) 0.0204(12) Uani 1 1 d . . .
C224 C 0.27550(19) -0.0200(3) 0.17466(10) 0.0183(11) Uani 1 1 d . . .
C225 C 0.35375(18) 0.1656(3) 0.16608(11) 0.0224(12) Uani 1 1 d . . .
H225 H 0.3633 0.1614 0.1444 0.027 Uiso 1 1 calc R . .
C226 C 0.36953(19) 0.2284(3) 0.18195(11) 0.0240(12) Uani 1 1 d . . .
H226 H 0.3647 0.2268 0.2043 0.029 Uiso 1 1 calc R . .
C227 C 0.39317(19) 0.2989(3) 0.16950(11) 0.0247(13) Uani 1 1 d . . .
C228 C 0.40201(19) 0.3137(3) 0.13704(11) 0.0245(12) Uani 1 1 d . . .
H228 H 0.3953 0.2732 0.1222 0.029 Uiso 1 1 calc R . .
C229 C 0.41982(18) 0.3838(3) 0.12628(11) 0.0240(13) Uani 1 1 d . . .
H229 H 0.4250 0.3912 0.1042 0.029 Uiso 1 1 calc R . .
C230 C 0.43081(18) 0.4458(3) 0.14726(11) 0.0213(12) Uani 1 1 d . . .
C231 C 0.4235(2) 0.4324(3) 0.17989(11) 0.0262(13) Uani 1 1 d . . .
H231 H 0.4311 0.4726 0.1947 0.031 Uiso 1 1 calc R . .
C232 C 0.40523(19) 0.3612(3) 0.19030(11) 0.0241(12) Uani 1 1 d . . .
H232 H 0.4006 0.3535 0.2124 0.029 Uiso 1 1 calc R . .
C233 C 0.4564(2) 0.5304(3) 0.10270(12) 0.0364(15) Uani 1 1 d . . .
H23A H 0.4865 0.4986 0.0957 0.055 Uiso 1 1 calc R . .
H23B H 0.4642 0.5858 0.0990 0.055 Uiso 1 1 calc R . .
H23C H 0.4248 0.5155 0.0907 0.055 Uiso 1 1 calc R . .
C234 C 0.4670(2) 0.5762(3) 0.15840(13) 0.0384(15) Uani 1 1 d . . .
H23D H 0.4400 0.5877 0.1744 0.058 Uiso 1 1 calc R . .
H23E H 0.4754 0.6239 0.1466 0.058 Uiso 1 1 calc R . .
H23F H 0.4989 0.5567 0.1689 0.058 Uiso 1 1 calc R . .
C235 C 0.1454(2) 0.1656(3) 0.12352(12) 0.0247(12) Uani 1 1 d . . .
H235 H 0.1355 0.1572 0.1450 0.030 Uiso 1 1 calc R . .
C236 C 0.12940(19) 0.2323(3) 0.10952(11) 0.0249(12) Uani 1 1 d . . .
H236 H 0.1341 0.2348 0.0872 0.030 Uiso 1 1 calc R . .
C237 C 0.10621(19) 0.2999(3) 0.12392(11) 0.0239(12) Uani 1 1 d . . .
C238 C 0.0974(2) 0.3077(3) 0.15641(12) 0.0274(13) Uani 1 1 d . . .
H238 H 0.1047 0.2647 0.1700 0.033 Uiso 1 1 calc R . .
C239 C 0.0785(2) 0.3763(3) 0.16940(13) 0.0326(14) Uani 1 1 d . . .
H239 H 0.0724 0.3795 0.1916 0.039 Uiso 1 1 calc R . .
C240 C 0.0681(2) 0.4421(3) 0.14989(13) 0.0296(13) Uani 1 1 d . . .
C241 C 0.0753(2) 0.4328(3) 0.11711(12) 0.0298(13) Uani 1 1 d . . .
H241 H 0.0667 0.4746 0.1032 0.036 Uiso 1 1 calc R . .
C242 C 0.0942(2) 0.3648(3) 0.10485(12) 0.0293(13) Uani 1 1 d . . .
H242 H 0.0996 0.3611 0.0826 0.035 Uiso 1 1 calc R . .
C243 C 0.0429(3) 0.5187(4) 0.19594(15) 0.0524(18) Uani 1 1 d . . .
H24A H 0.0128 0.4856 0.2017 0.079 Uiso 1 1 calc R . .
H24B H 0.0348 0.5732 0.2012 0.079 Uiso 1 1 calc R . .
H24C H 0.0742 0.5018 0.2077 0.079 Uiso 1 1 calc R . .
C244 C 0.0352(2) 0.5744(4) 0.14210(15) 0.0444(16) Uani 1 1 d . . .
H24D H 0.0616 0.5832 0.1255 0.067 Uiso 1 1 calc R . .
H24E H 0.0306 0.6224 0.1545 0.067 Uiso 1 1 calc R . .
H24F H 0.0014 0.5599 0.1323 0.067 Uiso 1 1 calc R . .
N21 N 0.44712(18) 0.5173(3) 0.13677(10) 0.0310(11) Uani 1 1 d . . .
N22 N 0.05271(19) 0.5121(3) 0.16271(11) 0.0390(13) Uani 1 1 d . . .
S1 S 0.35692(8) 0.21180(12) 0.29600(4) 0.0597(5) Uani 1 1 d . . .
C145 C 0.4288(6) 0.2538(8) 0.2861(3) 0.051(2) Uiso 0.50 1 d P . .
C245 C 0.4132(6) 0.1699(9) 0.2857(3) 0.051(2) Uiso 0.50 1 d P . .
F1 F 0.4403(3) 0.2115(5) 0.25643(17) 0.0599(15) Uiso 0.50 1 d P . .
F1B F 0.4218(3) 0.1542(5) 0.25655(18) 0.0599(15) Uiso 0.50 1 d P . .
F2 F 0.4094(4) 0.1020(4) 0.30025(18) 0.185(3) Uani 1 1 d . . .
F3 F 0.4621(4) 0.2324(6) 0.3021(2) 0.085(2) Uiso 0.50 1 d P . .
F3B F 0.4552(4) 0.1895(6) 0.2994(2) 0.085(2) Uiso 0.50 1 d P . .
O1 O 0.35262(17) 0.2300(3) 0.32777(9) 0.0669(15) Uani 1 1 d . . .
O2 O 0.3618(5) 0.2895(8) 0.2797(3) 0.090(3) Uiso 0.50 1 d P . .
O2B O 0.3372(5) 0.2550(8) 0.2697(3) 0.090(3) Uiso 0.50 1 d P . .
O3 O 0.3196(5) 0.1869(8) 0.2785(3) 0.083(3) Uiso 0.50 1 d P . .
O3B O 0.3118(5) 0.1497(7) 0.2851(3) 0.083(3) Uiso 0.50 1 d P . .
S2 S 0.34934(6) 0.78586(9) 0.98777(3) 0.0365(4) Uani 1 1 d . . .
C146 C 0.4170(3) 0.8202(4) 0.99146(14) 0.0500(18) Uani 1 1 d . . .
F4 F 0.42643(15) 0.8801(3) 0.97230(9) 0.0677(12) Uani 1 1 d . . .
F5 F 0.45090(17) 0.7646(3) 0.98405(11) 0.0896(15) Uani 1 1 d . . .
F6 F 0.42722(18) 0.8441(3) 1.02049(9) 0.0792(14) Uani 1 1 d . . .
O4 O 0.31795(18) 0.8540(3) 0.99510(11) 0.0631(14) Uani 1 1 d . . .
O5 O 0.34584(18) 0.7626(3) 0.95568(10) 0.0662(15) Uani 1 1 d . . .
O6 O 0.3443(2) 0.7257(3) 1.01123(10) 0.0611(14) Uani 1 1 d . . .
S3 S 0.13287(6) 0.63570(9) 0.06070(3) 0.0298(4) Uani 1 1 d . . .
C147 C 0.0858(3) 0.5808(4) 0.03702(15) 0.0491(18) Uani 1 1 d . . .
F7 F 0.06706(19) 0.6224(3) 0.01321(10) 0.0909(16) Uani 1 1 d . . .
F8 F 0.10903(19) 0.5168(3) 0.02478(12) 0.0901(15) Uani 1 1 d . . .
F9 F 0.04484(16) 0.5578(3) 0.05349(9) 0.0709(13) Uani 1 1 d . . .
O7 O 0.17244(17) 0.6580(2) 0.03841(9) 0.0477(11) Uani 1 1 d . . .
O8 O 0.15039(16) 0.5809(3) 0.08406(9) 0.0487(12) Uani 1 1 d . . .
O9 O 0.10207(18) 0.6985(3) 0.07283(10) 0.0561(13) Uani 1 1 d . . .
S4 S 0.35774(7) 0.62047(11) 0.24117(4) 0.0491(5) Uani 1 1 d . . .
C148 C 0.4109(8) 0.6788(13) 0.2493(5) 0.079(4) Uiso 0.50 1 d P . .
C248 C 0.4238(9) 0.6438(11) 0.2488(5) 0.079(4) Uiso 0.50 1 d P . .
F10 F 0.4268(3) 0.6894(5) 0.27852(19) 0.0661(17) Uiso 0.50 1 d P . .
F10B F 0.4352(3) 0.6392(5) 0.28180(19) 0.0661(17) Uiso 0.50 1 d P . .
F11 F 0.4260(4) 0.7224(4) 0.23144(15) 0.176(4) Uani 1 1 d . . .
F12 F 0.4603(4) 0.6188(6) 0.2390(2) 0.0702(18) Uiso 0.50 1 d P . .
F12B F 0.4565(4) 0.5798(5) 0.2402(2) 0.0702(18) Uiso 0.50 1 d P . .
O10 O 0.3611(5) 0.5457(7) 0.2607(3) 0.078(2) Uiso 0.50 1 d P . .
O10B O 0.3395(5) 0.5755(7) 0.2666(3) 0.078(2) Uiso 0.50 1 d P . .
O11 O 0.3237(5) 0.6936(7) 0.2512(3) 0.084(3) Uiso 0.50 1 d P . .
O11B O 0.3173(5) 0.6542(7) 0.2555(3) 0.084(3) Uiso 0.50 1 d P . .
O12 O 0.35304(16) 0.5997(3) 0.20961(9) 0.0569(14) 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
C11 C124 1.378(6) . ?
C11 C12 1.398(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.427(6) . ?
C12 C125 1.445(7) . ?
C13 C14 1.353(7) . ?
C13 H13 0.9500 . ?
C14 N15 1.347(6) . ?
C14 H14 0.9500 . ?
N15 C124 1.373(5) . ?
N15 C16 1.486(6) . ?
C16 C17 1.537(7) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.536(7) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.512(7) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C110 1.388(7) . ?
C19 C123 1.404(7) . ?
C110 C111 1.379(7) . ?
C110 H110 0.9500 . ?
C111 C112 1.386(7) . ?
C111 H111 0.9500 . ?
C112 C122 1.411(7) . ?
C112 C113 1.502(7) . ?
C113 C114 1.536(8) . ?
C113 H11A 0.9900 . ?
C113 H11B 0.9900 . ?
C114 C115 1.519(7) . ?
C114 H11C 0.9900 . ?
C114 H11D 0.9900 . ?
C115 N116 1.486(6) . ?
C115 H11E 0.9900 . ?
C115 H11F 0.9900 . ?
N116 C117 1.357(6) . ?
N116 C121 1.370(6) . ?
C117 C118 1.351(7) . ?
C117 H117 0.9500 . ?
C118 C119 1.410(6) . ?
C118 H118 0.9500 . ?
C119 C120 1.417(7) . ?
C119 C135 1.428(7) . ?
C120 C121 1.366(7) . ?
C120 H120 0.9500 . ?
C121 C122 1.478(7) . ?
C122 C123 1.408(6) . ?
C123 C124 1.492(7) . ?
C125 C126 1.351(7) . ?
C125 H125 0.9500 . ?
C126 C127 1.447(7) . ?
C126 H126 0.9500 . ?
C127 C128 1.396(7) . ?
C127 C132 1.401(7) . ?
C128 C129 1.375(7) . ?
C128 H128 0.9500 . ?
C129 C130 1.415(7) . ?
C129 H129 0.9500 . ?
C130 N11 1.375(6) . ?
C130 C131 1.389(7) . ?
C131 C132 1.374(7) . ?
C131 H131 0.9500 . ?
C132 H132 0.9500 . ?
C133 N11 1.453(6) . ?
C133 H13A 0.9800 . ?
C133 H13B 0.9800 . ?
C133 H13C 0.9800 . ?
C134 N11 1.450(7) . ?
C134 H13D 0.9800 . ?
C134 H13E 0.9800 . ?
C134 H13F 0.9800 . ?
C135 C136 1.360(7) . ?
C135 H135 0.9500 . ?
C136 C137 1.440(7) . ?
C136 H136 0.9500 . ?
C137 C138 1.393(7) . ?
C137 C142 1.399(7) . ?
C138 C139 1.358(7) . ?
C138 H138 0.9500 . ?
C139 C140 1.425(8) . ?
C139 H139 0.9500 . ?
C140 N12 1.356(7) . ?
C140 C141 1.396(7) . ?
C141 C142 1.379(7) . ?
C141 H141 0.9500 . ?
C142 H142 0.9500 . ?
C143 N12 1.442(8) . ?
C143 H14A 0.9800 . ?
C143 H14B 0.9800 . ?
C143 H14C 0.9800 . ?
C144 N12 1.436(7) . ?
C144 H14D 0.9800 . ?
C144 H14E 0.9800 . ?
C144 H14F 0.9800 . ?
C21 C224 1.375(7) . ?
C21 C22 1.413(7) . ?
C21 H21 0.9500 . ?
C22 C23 1.420(7) . ?
C22 C225 1.446(7) . ?
C23 C24 1.343(7) . ?
C23 H23 0.9500 . ?
C24 N25 1.353(6) . ?
C24 H24 0.9500 . ?
N25 C224 1.364(6) . ?
N25 C26 1.495(6) . ?
C26 C27 1.531(7) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.528(7) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.497(7) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C210 1.388(7) . ?
C29 C223 1.405(7) . ?
C210 C211 1.373(8) . ?
C210 H210 0.9500 . ?
C211 C212 1.387(7) . ?
C211 H211 0.9500 . ?
C212 C222 1.426(7) . ?
C212 C213 1.487(7) . ?
C213 C214 1.532(7) . ?
C213 H21A 0.9900 . ?
C213 H21B 0.9900 . ?
C214 C215 1.510(7) . ?
C214 H21C 0.9900 . ?
C214 H21D 0.9900 . ?
C215 N216 1.494(6) . ?
C215 H21E 0.9900 . ?
C215 H21F 0.9900 . ?
N216 C217 1.331(7) . ?
N216 C221 1.363(6) . ?
C217 C218 1.364(7) . ?
C217 H217 0.9500 . ?
C218 C219 1.411(6) . ?
C218 H218 0.9500 . ?
C219 C220 1.403(7) . ?
C219 C235 1.445(7) . ?
C220 C221 1.383(7) . ?
C220 H220 0.9500 . ?
C221 C222 1.483(7) . ?
C222 C223 1.407(6) . ?
C223 C224 1.491(7) . ?
C225 C226 1.328(7) . ?
C225 H225 0.9500 . ?
C226 C227 1.446(7) . ?
C226 H226 0.9500 . ?
C227 C228 1.410(6) . ?
C227 C232 1.414(7) . ?
C228 C229 1.361(7) . ?
C228 H228 0.9500 . ?
C229 C230 1.409(7) . ?
C229 H229 0.9500 . ?
C230 N21 1.366(7) . ?
C230 C231 1.408(7) . ?
C231 C232 1.376(7) . ?
C231 H231 0.9500 . ?
C232 H232 0.9500 . ?
C233 N21 1.474(7) . ?
C233 H23A 0.9800 . ?
C233 H23B 0.9800 . ?
C233 H23C 0.9800 . ?
C234 N21 1.449(7) . ?
C234 H23D 0.9800 . ?
C234 H23E 0.9800 . ?
C234 H23F 0.9800 . ?
C235 C236 1.347(7) . ?
C235 H235 0.9500 . ?
C236 C237 1.433(7) . ?
C236 H236 0.9500 . ?
C237 C238 1.395(7) . ?
C237 C242 1.404(7) . ?
C238 C239 1.382(7) . ?
C238 H238 0.9500 . ?
C239 C240 1.420(7) . ?
C239 H239 0.9500 . ?
C240 N22 1.370(7) . ?
C240 C241 1.404(7) . ?
C241 C242 1.361(7) . ?
C241 H241 0.9500 . ?
C242 H242 0.9500 . ?
C243 N22 1.429(7) . ?
C243 H24A 0.9800 . ?
C243 H24B 0.9800 . ?
C243 H24C 0.9800 . ?
C244 N22 1.446(7) . ?
C244 H24D 0.9800 . ?
C244 H24E 0.9800 . ?
C244 H24F 0.9800 . ?
S1 O3 1.272(13) . ?
S1 O1 1.380(4) . ?
S1 O2B 1.424(13) . ?
S1 O2 1.502(13) . ?
S1 O3B 1.627(12) . ?
S1 C245 1.653(14) . ?
S1 C145 2.000(14) . ?
C145 F3 1.141(15) . ?
C145 F3B 1.405(17) . ?
C145 F1 1.474(15) . ?
C145 C245 1.488(19) . ?
C145 O2 1.821(19) . ?
C245 F3B 1.254(15) . ?
C245 F1B 1.279(14) . ?
C245 F2 1.317(15) . ?
C245 F1 1.582(16) . ?
C245 F3 1.773(18) . ?
F1 F1B 1.086(9) . ?
F3 F3B 0.762(13) . ?
O2 O2B 0.956(15) . ?
O2B O3 1.303(15) . ?
O3 O3B 0.722(17) . ?
S2 O5 1.414(4) . ?
S2 O6 1.434(4) . ?
S2 O4 1.444(4) . ?
S2 C146 1.817(7) . ?
C146 F6 1.317(7) . ?
C146 F5 1.318(8) . ?
C146 F4 1.327(7) . ?
S3 O9 1.422(4) . ?
S3 O7 1.426(4) . ?
S3 O8 1.431(4) . ?
S3 C147 1.817(7) . ?
C147 F9 1.308(7) . ?
C147 F7 1.319(7) . ?
C147 F8 1.348(8) . ?
S4 O11B 1.322(13) . ?
S4 O12 1.383(4) . ?
S4 O10B 1.398(12) . ?
S4 O10 1.524(12) . ?
S4 O11 1.578(13) . ?
S4 C148 1.71(2) . ?
S4 C248 1.75(2) . ?
C148 C248 0.68(3) . ?
C148 F11 1.13(2) . ?
C148 F10 1.31(2) . ?
C148 F10B 1.65(2) . ?
C148 F12 1.68(2) . ?
C248 F12 1.10(2) . ?
C248 F12B 1.42(2) . ?
C248 F10B 1.42(2) . ?
C248 F10 1.48(2) . ?
C248 F11 1.53(2) . ?
F10 F10B 0.896(10) . ?
F12 F12B 0.677(13) . ?
O10 O10B 0.787(15) . ?
O10B O11B 1.533(16) . ?
O11 O11B 0.717(16) . ?

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
C124 C11 C12 122.0(4) . . ?
C124 C11 H11 119.0 . . ?
C12 C11 H11 119.0 . . ?
C11 C12 C13 116.0(4) . . ?
C11 C12 C125 121.1(4) . . ?
C13 C12 C125 122.9(5) . . ?
C14 C13 C12 120.7(5) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
N15 C14 C13 121.4(4) . . ?
N15 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
C14 N15 C124 120.9(4) . . ?
C14 N15 C16 118.3(4) . . ?
C124 N15 C16 120.8(4) . . ?
N15 C16 C17 109.6(4) . . ?
N15 C16 H16A 109.7 . . ?
C17 C16 H16A 109.7 . . ?
N15 C16 H16B 109.7 . . ?
C17 C16 H16B 109.7 . . ?
H16A C16 H16B 108.2 . . ?
C18 C17 C16 111.8(4) . . ?
C18 C17 H17A 109.3 . . ?
C16 C17 H17A 109.3 . . ?
C18 C17 H17B 109.3 . . ?
C16 C17 H17B 109.3 . . ?
H17A C17 H17B 107.9 . . ?
C19 C18 C17 110.5(4) . . ?
C19 C18 H18A 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
C110 C19 C123 119.4(5) . . ?
C110 C19 C18 120.0(5) . . ?
C123 C19 C18 120.6(5) . . ?
C111 C110 C19 120.2(5) . . ?
C111 C110 H110 119.9 . . ?
C19 C110 H110 119.9 . . ?
C110 C111 C112 122.0(5) . . ?
C110 C111 H111 119.0 . . ?
C112 C111 H111 119.0 . . ?
C111 C112 C122 118.5(5) . . ?
C111 C112 C113 121.4(5) . . ?
C122 C112 C113 120.0(5) . . ?
C112 C113 C114 110.4(5) . . ?
C112 C113 H11A 109.6 . . ?
C114 C113 H11A 109.6 . . ?
C112 C113 H11B 109.6 . . ?
C114 C113 H11B 109.6 . . ?
H11A C113 H11B 108.1 . . ?
C115 C114 C113 112.6(4) . . ?
C115 C114 H11C 109.1 . . ?
C113 C114 H11C 109.1 . . ?
C115 C114 H11D 109.1 . . ?
C113 C114 H11D 109.1 . . ?
H11C C114 H11D 107.8 . . ?
N116 C115 C114 110.0(4) . . ?
N116 C115 H11E 109.7 . . ?
C114 C115 H11E 109.7 . . ?
N116 C115 H11F 109.7 . . ?
C114 C115 H11F 109.7 . . ?
H11E C115 H11F 108.2 . . ?
C117 N116 C121 119.9(4) . . ?
C117 N116 C115 119.5(4) . . ?
C121 N116 C115 120.6(4) . . ?
C118 C117 N116 122.1(4) . . ?
C118 C117 H117 119.0 . . ?
N116 C117 H117 119.0 . . ?
C117 C118 C119 120.8(5) . . ?
C117 C118 H118 119.6 . . ?
C119 C118 H118 119.6 . . ?
C118 C119 C120 115.5(5) . . ?
C118 C119 C135 123.2(5) . . ?
C120 C119 C135 121.2(4) . . ?
C121 C120 C119 122.4(4) . . ?
C121 C120 H120 118.8 . . ?
C119 C120 H120 118.8 . . ?
C120 C121 N116 119.2(4) . . ?
C120 C121 C122 124.2(4) . . ?
N116 C121 C122 116.5(4) . . ?
C123 C122 C112 119.8(5) . . ?
C123 C122 C121 122.2(4) . . ?
C112 C122 C121 118.0(4) . . ?
C19 C123 C122 120.1(5) . . ?
C19 C123 C124 117.8(4) . . ?
C122 C123 C124 122.1(4) . . ?
N15 C124 C11 118.9(4) . . ?
N15 C124 C123 117.1(4) . . ?
C11 C124 C123 123.8(4) . . ?
C126 C125 C12 123.1(4) . . ?
C126 C125 H125 118.5 . . ?
C12 C125 H125 118.5 . . ?
C125 C126 C127 129.0(4) . . ?
C125 C126 H126 115.5 . . ?
C127 C126 H126 115.5 . . ?
C128 C127 C132 116.3(5) . . ?
C128 C127 C126 125.2(5) . . ?
C132 C127 C126 118.4(4) . . ?
C129 C128 C127 122.2(5) . . ?
C129 C128 H128 118.9 . . ?
C127 C128 H128 118.9 . . ?
C128 C129 C130 120.6(4) . . ?
C128 C129 H129 119.7 . . ?
C130 C129 H129 119.7 . . ?
N11 C130 C131 120.7(5) . . ?
N11 C130 C129 121.7(4) . . ?
C131 C130 C129 117.6(5) . . ?
C132 C131 C130 120.9(5) . . ?
C132 C131 H131 119.6 . . ?
C130 C131 H131 119.6 . . ?
C131 C132 C127 122.5(5) . . ?
C131 C132 H132 118.8 . . ?
C127 C132 H132 118.8 . . ?
N11 C133 H13A 109.5 . . ?
N11 C133 H13B 109.5 . . ?
H13A C133 H13B 109.5 . . ?
N11 C133 H13C 109.5 . . ?
H13A C133 H13C 109.5 . . ?
H13B C133 H13C 109.5 . . ?
N11 C134 H13D 109.5 . . ?
N11 C134 H13E 109.5 . . ?
H13D C134 H13E 109.5 . . ?
N11 C134 H13F 109.5 . . ?
H13D C134 H13F 109.5 . . ?
H13E C134 H13F 109.5 . . ?
C136 C135 C119 124.0(4) . . ?
C136 C135 H135 118.0 . . ?
C119 C135 H135 118.0 . . ?
C135 C136 C137 128.5(4) . . ?
C135 C136 H136 115.8 . . ?
C137 C136 H136 115.8 . . ?
C138 C137 C142 117.0(5) . . ?
C138 C137 C136 124.4(5) . . ?
C142 C137 C136 118.6(5) . . ?
C139 C138 C137 122.3(5) . . ?
C139 C138 H138 118.9 . . ?
C137 C138 H138 118.9 . . ?
C138 C139 C140 121.2(5) . . ?
C138 C139 H139 119.4 . . ?
C140 C139 H139 119.4 . . ?
N12 C140 C141 121.8(5) . . ?
N12 C140 C139 121.9(5) . . ?
C141 C140 C139 116.3(5) . . ?
C142 C141 C140 121.8(5) . . ?
C142 C141 H141 119.1 . . ?
C140 C141 H141 119.1 . . ?
C141 C142 C137 121.3(5) . . ?
C141 C142 H142 119.4 . . ?
C137 C142 H142 119.4 . . ?
N12 C143 H14A 109.5 . . ?
N12 C143 H14B 109.5 . . ?
H14A C143 H14B 109.5 . . ?
N12 C143 H14C 109.5 . . ?
H14A C143 H14C 109.5 . . ?
H14B C143 H14C 109.5 . . ?
N12 C144 H14D 109.5 . . ?
N12 C144 H14E 109.5 . . ?
H14D C144 H14E 109.5 . . ?
N12 C144 H14F 109.5 . . ?
H14D C144 H14F 109.5 . . ?
H14E C144 H14F 109.5 . . ?
C130 N11 C134 120.2(4) . . ?
C130 N11 C133 120.2(4) . . ?
C134 N11 C133 118.3(4) . . ?
C140 N12 C144 120.4(5) . . ?
C140 N12 C143 120.9(5) . . ?
C144 N12 C143 118.1(5) . . ?
C224 C21 C22 122.0(4) . . ?
C224 C21 H21 119.0 . . ?
C22 C21 H21 119.0 . . ?
C21 C22 C23 115.7(5) . . ?
C21 C22 C225 121.7(4) . . ?
C23 C22 C225 122.6(5) . . ?
C24 C23 C22 120.7(5) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C23 C24 N25 122.0(4) . . ?
C23 C24 H24 119.0 . . ?
N25 C24 H24 119.0 . . ?
C24 N25 C224 120.5(4) . . ?
C24 N25 C26 119.3(4) . . ?
C224 N25 C26 120.2(4) . . ?
N25 C26 C27 109.6(4) . . ?
N25 C26 H26A 109.7 . . ?
C27 C26 H26A 109.7 . . ?
N25 C26 H26B 109.7 . . ?
C27 C26 H26B 109.7 . . ?
H26A C26 H26B 108.2 . . ?
C28 C27 C26 111.9(4) . . ?
C28 C27 H27A 109.2 . . ?
C26 C27 H27A 109.2 . . ?
C28 C27 H27B 109.2 . . ?
C26 C27 H27B 109.2 . . ?
H27A C27 H27B 107.9 . . ?
C29 C28 C27 110.9(4) . . ?
C29 C28 H28A 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C29 C28 H28B 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 108.1 . . ?
C210 C29 C223 118.2(5) . . ?
C210 C29 C28 121.7(5) . . ?
C223 C29 C28 120.0(5) . . ?
C211 C210 C29 122.0(5) . . ?
C211 C210 H210 119.0 . . ?
C29 C210 H210 119.0 . . ?
C210 C211 C212 121.5(5) . . ?
C210 C211 H211 119.2 . . ?
C212 C211 H211 119.2 . . ?
C211 C212 C222 117.7(5) . . ?
C211 C212 C213 122.1(5) . . ?
C222 C212 C213 120.2(5) . . ?
C212 C213 C214 111.7(4) . . ?
C212 C213 H21A 109.3 . . ?
C214 C213 H21A 109.3 . . ?
C212 C213 H21B 109.3 . . ?
C214 C213 H21B 109.3 . . ?
H21A C213 H21B 107.9 . . ?
C215 C214 C213 111.6(4) . . ?
C215 C214 H21C 109.3 . . ?
C213 C214 H21C 109.3 . . ?
C215 C214 H21D 109.3 . . ?
C213 C214 H21D 109.3 . . ?
H21C C214 H21D 108.0 . . ?
N216 C215 C214 110.2(4) . . ?
N216 C215 H21E 109.6 . . ?
C214 C215 H21E 109.6 . . ?
N216 C215 H21F 109.6 . . ?
C214 C215 H21F 109.6 . . ?
H21E C215 H21F 108.1 . . ?
C217 N216 C221 120.4(4) . . ?
C217 N216 C215 120.2(4) . . ?
C221 N216 C215 119.4(4) . . ?
N216 C217 C218 122.9(4) . . ?
N216 C217 H217 118.5 . . ?
C218 C217 H217 118.5 . . ?
C217 C218 C219 119.4(5) . . ?
C217 C218 H218 120.3 . . ?
C219 C218 H218 120.3 . . ?
C220 C219 C218 116.6(5) . . ?
C220 C219 C235 120.8(4) . . ?
C218 C219 C235 122.6(5) . . ?
C221 C220 C219 121.7(4) . . ?
C221 C220 H220 119.2 . . ?
C219 C220 H220 119.2 . . ?
N216 C221 C220 119.0(4) . . ?
N216 C221 C222 117.9(4) . . ?
C220 C221 C222 123.0(4) . . ?
C223 C222 C212 120.3(5) . . ?
C223 C222 C221 122.7(4) . . ?
C212 C222 C221 116.9(4) . . ?
C29 C223 C222 120.2(5) . . ?
C29 C223 C224 118.3(4) . . ?
C222 C223 C224 121.5(4) . . ?
N25 C224 C21 119.1(4) . . ?
N25 C224 C223 117.0(4) . . ?
C21 C224 C223 123.9(4) . . ?
C226 C225 C22 123.7(4) . . ?
C226 C225 H225 118.1 . . ?
C22 C225 H225 118.1 . . ?
C225 C226 C227 128.1(4) . . ?
C225 C226 H226 115.9 . . ?
C227 C226 H226 115.9 . . ?
C228 C227 C232 115.7(5) . . ?
C228 C227 C226 124.6(5) . . ?
C232 C227 C226 119.5(4) . . ?
C229 C228 C227 122.3(5) . . ?
C229 C228 H228 118.9 . . ?
C227 C228 H228 118.9 . . ?
C228 C229 C230 121.3(5) . . ?
C228 C229 H229 119.3 . . ?
C230 C229 H229 119.3 . . ?
N21 C230 C231 120.2(5) . . ?
N21 C230 C229 122.0(4) . . ?
C231 C230 C229 117.8(5) . . ?
C232 C231 C230 120.0(5) . . ?
C232 C231 H231 120.0 . . ?
C230 C231 H231 120.0 . . ?
C231 C232 C227 122.8(5) . . ?
C231 C232 H232 118.6 . . ?
C227 C232 H232 118.6 . . ?
N21 C233 H23A 109.5 . . ?
N21 C233 H23B 109.5 . . ?
H23A C233 H23B 109.5 . . ?
N21 C233 H23C 109.5 . . ?
H23A C233 H23C 109.5 . . ?
H23B C233 H23C 109.5 . . ?
N21 C234 H23D 109.5 . . ?
N21 C234 H23E 109.5 . . ?
H23D C234 H23E 109.5 . . ?
N21 C234 H23F 109.5 . . ?
H23D C234 H23F 109.5 . . ?
H23E C234 H23F 109.5 . . ?
C236 C235 C219 124.5(5) . . ?
C236 C235 H235 117.8 . . ?
C219 C235 H235 117.8 . . ?
C235 C236 C237 128.4(5) . . ?
C235 C236 H236 115.8 . . ?
C237 C236 H236 115.8 . . ?
C238 C237 C242 116.9(5) . . ?
C238 C237 C236 124.0(5) . . ?
C242 C237 C236 119.0(5) . . ?
C239 C238 C237 121.7(5) . . ?
C239 C238 H238 119.1 . . ?
C237 C238 H238 119.1 . . ?
C238 C239 C240 120.6(5) . . ?
C238 C239 H239 119.7 . . ?
C240 C239 H239 119.7 . . ?
N22 C240 C241 121.7(5) . . ?
N22 C240 C239 121.1(5) . . ?
C241 C240 C239 117.2(5) . . ?
C242 C241 C240 121.1(5) . . ?
C242 C241 H241 119.4 . . ?
C240 C241 H241 119.4 . . ?
C241 C242 C237 122.3(5) . . ?
C241 C242 H242 118.8 . . ?
C237 C242 H242 118.8 . . ?
N22 C243 H24A 109.5 . . ?
N22 C243 H24B 109.5 . . ?
H24A C243 H24B 109.5 . . ?
N22 C243 H24C 109.5 . . ?
H24A C243 H24C 109.5 . . ?
H24B C243 H24C 109.5 . . ?
N22 C244 H24D 109.5 . . ?
N22 C244 H24E 109.5 . . ?
H24D C244 H24E 109.5 . . ?
N22 C244 H24F 109.5 . . ?
H24D C244 H24F 109.5 . . ?
H24E C244 H24F 109.5 . . ?
C230 N21 C234 121.6(4) . . ?
C230 N21 C233 120.0(4) . . ?
C234 N21 C233 117.0(5) . . ?
C240 N22 C243 120.4(5) . . ?
C240 N22 C244 119.7(5) . . ?
C243 N22 C244 118.6(5) . . ?
O3 S1 O1 125.5(6) . . ?
O3 S1 O2B 57.5(7) . . ?
O1 S1 O2B 127.8(6) . . ?
O3 S1 O2 95.3(7) . . ?
O1 S1 O2 104.5(5) . . ?
O2B S1 O2 38.0(6) . . ?
O3 S1 O3B 25.2(7) . . ?
O1 S1 O3B 111.5(5) . . ?
O2B S1 O3B 82.7(7) . . ?
O2 S1 O3B 120.5(7) . . ?
O3 S1 C245 110.0(8) . . ?
O1 S1 C245 114.8(5) . . ?
O2B S1 C245 108.8(7) . . ?
O2 S1 C245 101.2(7) . . ?
O3B S1 C245 104.3(7) . . ?
O3 S1 C145 132.3(7) . . ?
O1 S1 C145 101.2(4) . . ?
O2B S1 C145 88.1(7) . . ?
O2 S1 C145 60.7(6) . . ?
O3B S1 C145 144.5(6) . . ?
C245 S1 C145 46.9(6) . . ?
F3 C145 F3B 32.8(8) . . ?
F3 C145 F1 101.4(12) . . ?
F3B C145 F1 82.0(9) . . ?
F3 C145 C245 83.7(11) . . ?
F3B C145 C245 51.3(8) . . ?
F1 C145 C245 64.6(8) . . ?
F3 C145 O2 151.9(13) . . ?
F3B C145 O2 139.9(11) . . ?
F1 C145 O2 103.0(9) . . ?
C245 C145 O2 94.4(10) . . ?
F3 C145 S1 115.6(11) . . ?
F3B C145 S1 93.9(8) . . ?
F1 C145 S1 100.4(8) . . ?
C245 C145 S1 54.2(7) . . ?
O2 C145 S1 46.0(5) . . ?
F3B C245 F1B 110.7(12) . . ?
F3B C245 F2 94.9(11) . . ?
F1B C245 F2 105.9(12) . . ?
F3B C245 C145 60.9(10) . . ?
F1B C245 C145 99.6(11) . . ?
F2 C245 C145 150.0(13) . . ?
F3B C245 F1 82.6(10) . . ?
F1B C245 F1 43.0(6) . . ?
F2 C245 F1 142.4(12) . . ?
C145 C245 F1 57.3(8) . . ?
F3B C245 S1 119.6(11) . . ?
F1B C245 S1 119.3(11) . . ?
F2 C245 S1 101.3(10) . . ?
C145 C245 S1 78.9(9) . . ?
F1 C245 S1 112.5(9) . . ?
F3B C245 F3 21.6(7) . . ?
F1B C245 F3 112.5(11) . . ?
F2 C245 F3 113.8(11) . . ?
C145 C245 F3 39.7(7) . . ?
F1 C245 F3 74.4(8) . . ?
S1 C245 F3 103.8(8) . . ?
F1B F1 C145 110.8(9) . . ?
F1B F1 C245 53.5(7) . . ?
C145 F1 C245 58.2(8) . . ?
F1 F1B C245 83.5(10) . . ?
F3B F3 C145 93.0(16) . . ?
F3B F3 C245 37.2(12) . . ?
C145 F3 C245 56.5(9) . . ?
F3 F3B C245 121.3(18) . . ?
F3 F3B C145 54.2(12) . . ?
C245 F3B C145 67.8(10) . . ?
O2B O2 S1 66.6(12) . . ?
O2B O2 C145 117.6(15) . . ?
S1 O2 C145 73.3(7) . . ?
O2 O2B O3 130.4(17) . . ?
O2 O2B S1 75.4(12) . . ?
O3 O2B S1 55.4(8) . . ?
O3B O3 S1 106(2) . . ?
O3B O3 O2B 173(2) . . ?
S1 O3 O2B 67.1(9) . . ?
O3 O3B S1 48.7(16) . . ?
O5 S2 O6 117.0(3) . . ?
O5 S2 O4 113.4(3) . . ?
O6 S2 O4 112.5(3) . . ?
O5 S2 C146 103.4(3) . . ?
O6 S2 C146 104.9(3) . . ?
O4 S2 C146 103.8(3) . . ?
F6 C146 F5 108.5(6) . . ?
F6 C146 F4 107.0(6) . . ?
F5 C146 F4 107.2(6) . . ?
F6 C146 S2 111.4(5) . . ?
F5 C146 S2 111.1(5) . . ?
F4 C146 S2 111.5(4) . . ?
O9 S3 O7 114.8(3) . . ?
O9 S3 O8 114.6(3) . . ?
O7 S3 O8 114.4(3) . . ?
O9 S3 C147 103.2(3) . . ?
O7 S3 C147 103.7(3) . . ?
O8 S3 C147 104.1(3) . . ?
F9 C147 F7 106.4(6) . . ?
F9 C147 F8 107.7(6) . . ?
F7 C147 F8 107.7(6) . . ?
F9 C147 S3 112.5(4) . . ?
F7 C147 S3 112.1(5) . . ?
F8 C147 S3 110.2(5) . . ?
O11B S4 O12 119.2(6) . . ?
O11B S4 O10B 68.6(7) . . ?
O12 S4 O10B 124.6(5) . . ?
O11B S4 O10 99.3(7) . . ?
O12 S4 O10 108.0(5) . . ?
O10B S4 O10 30.8(6) . . ?
O11B S4 O11 26.8(7) . . ?
O12 S4 O11 114.6(5) . . ?
O10B S4 O11 92.9(7) . . ?
O10 S4 O11 123.5(6) . . ?
O11B S4 C148 105.1(9) . . ?
O12 S4 C148 114.2(8) . . ?
O10B S4 C148 115.3(9) . . ?
O10 S4 C148 109.8(9) . . ?
O11 S4 C148 84.9(8) . . ?
O11B S4 C248 123.7(9) . . ?
O12 S4 C248 108.6(7) . . ?
O10B S4 C248 107.4(8) . . ?
O10 S4 C248 92.2(8) . . ?
O11 S4 C248 106.9(8) . . ?
C148 S4 C248 22.7(9) . . ?
C248 C148 F11 114(4) . . ?
C248 C148 F10 90(3) . . ?
F11 C148 F10 115.6(19) . . ?
C248 C148 F10B 59(3) . . ?
F11 C148 F10B 134.4(18) . . ?
F10 C148 F10B 32.7(7) . . ?
C248 C148 F12 26(3) . . ?
F11 C148 F12 88.8(14) . . ?
F10 C148 F12 95.7(13) . . ?
F10B C148 F12 71.6(9) . . ?
C248 C148 S4 82(3) . . ?
F11 C148 S4 121.4(17) . . ?
F10 C148 S4 120.7(16) . . ?
F10B C148 S4 102.7(13) . . ?
F12 C148 S4 100.2(11) . . ?
C148 C248 F12 139(4) . . ?
C148 C248 F12B 164(4) . . ?
F12 C248 F12B 27.6(9) . . ?
C148 C248 F10B 97(3) . . ?
F12 C248 F10B 100.2(16) . . ?
F12B C248 F10B 95.1(13) . . ?
C148 C248 F10 63(3) . . ?
F12 C248 F10 118.8(18) . . ?
F12B C248 F10 126.4(16) . . ?
F10B C248 F10 35.9(6) . . ?
C148 C248 F11 42(3) . . ?
F12 C248 F11 97.4(16) . . ?
F12B C248 F11 122.2(17) . . ?
F10B C248 F11 120.6(14) . . ?
F10 C248 F11 86.6(11) . . ?
C148 C248 S4 75(3) . . ?
F12 C248 S4 130.1(17) . . ?
F12B C248 S4 109.5(13) . . ?
F10B C248 S4 111.3(14) . . ?
F10 C248 S4 109.1(14) . . ?
F11 C248 S4 98.4(11) . . ?
F10B F10 C148 95.0(13) . . ?
F10B F10 C248 68.7(11) . . ?
C148 F10 C248 27.5(11) . . ?
F10 F10B C248 75.4(11) . . ?
F10 F10B C148 52.3(10) . . ?
C248 F10B C148 24.2(11) . . ?
C148 F11 C248 24.1(14) . . ?
F12B F12 C248 103.5(19) . . ?
F12B F12 C148 118.5(19) . . ?
C248 F12 C148 15.6(15) . . ?
F12 F12B C248 48.9(14) . . ?
O10B O10 S4 65.7(13) . . ?
O10 O10B S4 83.4(14) . . ?
O10 O10B O11B 136.7(18) . . ?
S4 O10B O11B 53.4(7) . . ?
O11B O11 S4 56.2(16) . . ?
O11 O11B S4 97.0(19) . . ?
O11 O11B O10B 145(2) . . ?
S4 O11B O10B 58.1(7) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.071
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.095


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 315 124 ' '
2 0.500 0.000 0.000 10 1 ' '
3 0.961 -0.102 0.241 121 43 ' '
4 0.461 -0.102 0.259 121 43 ' '
5 0.500 0.000 0.500 315 121 ' '
6 0.000 0.000 0.500 10 1 ' '
7 0.539 0.102 0.741 121 44 ' '
8 0.039 0.102 0.759 121 42 ' '
9 0.500 0.500 0.000 315 121 ' '
10 1.000 0.500 0.500 315 125 ' '
11 0.539 0.398 0.241 121 43 ' '
12 0.039 0.398 0.259 121 40 ' '
13 0.000 0.500 0.000 10 1 ' '
14 0.500 0.500 0.500 10 1 ' '
15 0.961 0.602 0.741 121 44 ' '
16 0.461 0.602 0.759 121 42 ' '
_platon_squeeze_details          
;
There are heavilly disordered triflate anions in the unit cell 
accompany with even more disordered solvents. The contributions
of solvent were removed to enable to refine the important
helquate molecule.
;

#===END
####################################################################### 
# 
# 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_pr230_teply
_database_code_depnum_ccdc_archive 'CCDC 1004345'
_audit_update_record             
;
2014-05-20 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H44 N4, 2(C F3 O3 S)'
_chemical_formula_sum            'C44 H44 F6 N4 O6 S2'
_chemical_formula_weight         902.95
_chemical_compound_source        'synthesized by the authors'

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'
S S 0.1246 0.1234 '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                   10.9183(3)
_cell_length_b                   13.1838(3)
_cell_length_c                   15.8627(3)
_cell_angle_alpha                69.6030(10)
_cell_angle_beta                 77.8740(10)
_cell_angle_gamma                78.1550(10)
_cell_volume                     2070.60(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9832
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      27.0

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.31
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             940
_exptl_absorpt_coefficient_mu    0.211
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8883
_exptl_absorpt_correction_T_max  0.9380
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34575
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         27.50
_reflns_number_total             9476
_reflns_number_gt                7847
_reflns_threshold_expression     I>2σ(I)

_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-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 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)+(0.0540P)²+1.1788P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9476
_refine_ls_number_parameters     563
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0405
_refine_ls_wR_factor_ref         0.1134
_refine_ls_wR_factor_gt          0.1040
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.002
_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 0.50622(15) 0.86748(13) 0.13622(10) 0.0245(3) Uani 1 1 d . . .
H1 H 0.4913 0.8240 0.1036 0.029 Uiso 1 1 calc R . .
C2 C 0.59107(16) 0.94173(13) 0.09626(11) 0.0275(3) Uani 1 1 d . . .
H2 H 0.6375 0.9475 0.0374 0.033 Uiso 1 1 calc R . .
C3 C 0.60712(16) 1.00709(13) 0.14317(11) 0.0275(3) Uani 1 1 d . . .
H3 H 0.6633 1.0598 0.1153 0.033 Uiso 1 1 calc R . .
C4 C 0.54277(15) 0.99764(12) 0.23064(11) 0.0238(3) Uani 1 1 d . . .
N5 N 0.46475(12) 0.91979(10) 0.26988(8) 0.0214(3) Uani 1 1 d . . .
C6 C 0.40692(15) 0.89552(13) 0.36730(10) 0.0247(3) Uani 1 1 d . . .
H6A H 0.4548 0.9239 0.3987 0.030 Uiso 1 1 calc R . .
H6B H 0.4131 0.8153 0.3966 0.030 Uiso 1 1 calc R . .
C7 C 0.26874(16) 0.94658(14) 0.37796(11) 0.0294(3) Uani 1 1 d . . .
H7A H 0.2639 1.0256 0.3680 0.035 Uiso 1 1 calc R . .
H7B H 0.2275 0.9125 0.4408 0.035 Uiso 1 1 calc R . .
C8 C 0.19718(16) 0.93150(14) 0.31015(12) 0.0291(3) Uani 1 1 d . . .
H8A H 0.1050 0.9477 0.3294 0.035 Uiso 1 1 calc R . .
H8B H 0.2193 0.9845 0.2493 0.035 Uiso 1 1 calc R . .
C9 C 0.22772(15) 0.81720(13) 0.30343(10) 0.0253(3) Uani 1 1 d . . .
C10 C 0.13627(16) 0.74779(14) 0.33206(11) 0.0294(3) Uani 1 1 d . . .
H10 H 0.0532 0.7723 0.3571 0.035 Uiso 1 1 calc R . .
C11 C 0.16414(16) 0.64370(14) 0.32465(11) 0.0301(4) Uani 1 1 d . . .
H11 H 0.0987 0.5995 0.3420 0.036 Uiso 1 1 calc R . .
C12 C 0.28570(16) 0.60237(13) 0.29244(11) 0.0264(3) Uani 1 1 d . . .
C13 C 0.31797(18) 0.48593(14) 0.29107(13) 0.0334(4) Uani 1 1 d . . .
H13A H 0.2441 0.4472 0.3219 0.040 Uiso 1 1 calc R . .
H13B H 0.3891 0.4484 0.3256 0.040 Uiso 1 1 calc R . .
C14 C 0.35482(18) 0.47875(16) 0.19437(14) 0.0374(4) Uani 1 1 d . . .
H14A H 0.3971 0.4039 0.1972 0.045 Uiso 1 1 calc R . .
H14B H 0.2774 0.4931 0.1664 0.045 Uiso 1 1 calc R . .
C15 C 0.44298(17) 0.56047(14) 0.13545(11) 0.0298(4) Uani 1 1 d . . .
H15A H 0.4821 0.5412 0.0798 0.036 Uiso 1 1 calc R . .
H15B H 0.3933 0.6343 0.1167 0.036 Uiso 1 1 calc R . .
N16 N 0.54442(13) 0.56232(10) 0.18430(9) 0.0233(3) Uani 1 1 d . . .
C17 C 0.66383(16) 0.50926(13) 0.16796(10) 0.0258(3) Uani 1 1 d . . .
C18 C 0.75969(16) 0.52683(13) 0.20495(11) 0.0273(3) Uani 1 1 d . . .
H18 H 0.8440 0.4928 0.1926 0.033 Uiso 1 1 calc R . .
C19 C 0.73370(16) 0.59295(13) 0.25916(11) 0.0273(3) Uani 1 1 d . . .
H19 H 0.7999 0.6069 0.2822 0.033 Uiso 1 1 calc R . .
C20 C 0.60944(15) 0.63894(13) 0.27978(10) 0.0248(3) Uani 1 1 d . . .
H20 H 0.5898 0.6808 0.3202 0.030 Uiso 1 1 calc R . .
C21 C 0.51442(15) 0.62426(12) 0.24187(10) 0.0224(3) Uani 1 1 d . . .
C22 C 0.38026(15) 0.67047(12) 0.26403(10) 0.0224(3) Uani 1 1 d . . .
C23 C 0.34984(15) 0.77868(12) 0.26705(10) 0.0223(3) Uani 1 1 d . . .
C24 C 0.44315(14) 0.85629(12) 0.22333(10) 0.0212(3) Uani 1 1 d . . .
C25 C 0.55666(16) 1.06891(13) 0.27947(11) 0.0269(3) Uani 1 1 d . . .
H25 H 0.4868 1.0895 0.3202 0.032 Uiso 1 1 calc R . .
C26 C 0.66643(16) 1.10587(14) 0.26789(12) 0.0298(3) Uani 1 1 d . . .
H26 H 0.7337 1.0818 0.2273 0.036 Uiso 1 1 calc R . .
C27 C 0.69498(16) 1.17832(13) 0.30997(11) 0.0277(3) Uani 1 1 d . . .
C28 C 0.82025(16) 1.19466(14) 0.30096(13) 0.0326(4) Uani 1 1 d . . .
H28 H 0.8847 1.1588 0.2663 0.039 Uiso 1 1 calc R . .
C29 C 0.85351(16) 1.26103(14) 0.34064(13) 0.0319(4) Uani 1 1 d . . .
H29 H 0.9399 1.2690 0.3339 0.038 Uiso 1 1 calc R . .
C30 C 0.76031(16) 1.31713(13) 0.39110(11) 0.0258(3) Uani 1 1 d . . .
C31 C 0.63342(15) 1.30075(13) 0.40073(11) 0.0260(3) Uani 1 1 d . . .
H31 H 0.5685 1.3370 0.4348 0.031 Uiso 1 1 calc R . .
C32 C 0.60272(15) 1.23300(13) 0.36140(11) 0.0271(3) Uani 1 1 d . . .
H32 H 0.5168 1.2231 0.3693 0.032 Uiso 1 1 calc R . .
C33 C 0.91977(18) 1.40069(17) 0.42210(14) 0.0399(4) Uani 1 1 d . . .
H33A H 0.9659 1.3315 0.4561 0.060 Uiso 1 1 calc R . .
H33B H 0.9223 1.4576 0.4480 0.060 Uiso 1 1 calc R . .
H33C H 0.9593 1.4219 0.3582 0.060 Uiso 1 1 calc R . .
C34 C 0.69081(18) 1.43829(14) 0.48391(12) 0.0326(4) Uani 1 1 d . . .
H34A H 0.6228 1.4802 0.4486 0.049 Uiso 1 1 calc R . .
H34B H 0.7267 1.4875 0.5032 0.049 Uiso 1 1 calc R . .
H34C H 0.6567 1.3816 0.5376 0.049 Uiso 1 1 calc R . .
C35 C 0.68600(17) 0.43452(13) 0.11539(11) 0.0293(3) Uani 1 1 d . . .
H35 H 0.6185 0.3987 0.1160 0.035 Uiso 1 1 calc R . .
C36 C 0.79849(18) 0.41447(14) 0.06609(11) 0.0311(4) Uani 1 1 d . . .
H36 H 0.8622 0.4550 0.0642 0.037 Uiso 1 1 calc R . .
C37 C 0.83347(16) 0.33743(13) 0.01528(11) 0.0285(3) Uani 1 1 d . . .
C38 C 0.95401(17) 0.33029(15) -0.03601(13) 0.0358(4) Uani 1 1 d . . .
H38 H 1.0102 0.3777 -0.0381 0.043 Uiso 1 1 calc R . .
C39 C 0.99406(17) 0.25667(16) -0.08376(13) 0.0367(4) Uani 1 1 d . . .
H39 H 1.0762 0.2549 -0.1186 0.044 Uiso 1 1 calc R . .
C40 C 0.91425(16) 0.18449(14) -0.08120(11) 0.0294(3) Uani 1 1 d . . .
C41 C 0.79179(16) 0.19291(13) -0.03102(11) 0.0275(3) Uani 1 1 d . . .
H41 H 0.7349 0.1465 -0.0297 0.033 Uiso 1 1 calc R . .
C42 C 0.75275(16) 0.26705(13) 0.01618(11) 0.0273(3) Uani 1 1 d . . .
H42 H 0.6699 0.2704 0.0498 0.033 Uiso 1 1 calc R . .
C43 C 1.0739(2) 0.1055(2) -0.18205(17) 0.0558(6) Uani 1 1 d . . .
H43A H 1.0850 0.1802 -0.2211 0.084 Uiso 1 1 calc R . .
H43B H 1.0774 0.0598 -0.2200 0.084 Uiso 1 1 calc R . .
H43C H 1.1415 0.0756 -0.1443 0.084 Uiso 1 1 calc R . .
C44 C 0.8872(2) 0.01256(17) -0.09584(15) 0.0461(5) Uani 1 1 d . . .
H44A H 0.8794 -0.0206 -0.0296 0.069 Uiso 1 1 calc R . .
H44B H 0.9352 -0.0410 -0.1249 0.069 Uiso 1 1 calc R . .
H44C H 0.8027 0.0355 -0.1138 0.069 Uiso 1 1 calc R . .
N1 N 0.78893(14) 1.38745(12) 0.42808(10) 0.0303(3) Uani 1 1 d . . .
N2 N 0.95273(16) 0.10681(13) -0.12423(11) 0.0388(4) Uani 1 1 d . . .
S1 S 0.74164(4) 0.74425(3) 0.43281(3) 0.02663(10) Uani 1 1 d . . .
S2 S 0.32337(4) 0.23705(4) 0.06987(3) 0.03195(11) Uani 1 1 d . . .
C45 C 0.76217(19) 0.84108(17) 0.48544(14) 0.0395(4) Uani 1 1 d . . .
C46 C 0.18687(18) 0.27486(16) 0.14686(13) 0.0353(4) Uani 1 1 d . . .
F1 F 0.85561(14) 0.89677(13) 0.43925(14) 0.0790(5) Uani 1 1 d . . .
F2 F 0.65849(12) 0.91376(10) 0.49063(9) 0.0495(3) Uani 1 1 d . . .
F3 F 0.78551(19) 0.79003(13) 0.57000(11) 0.0840(6) Uani 1 1 d . . .
F4 F 0.21345(15) 0.24804(13) 0.23060(8) 0.0651(4) Uani 1 1 d . . .
F5 F 0.09018(11) 0.22448(11) 0.15233(10) 0.0568(4) Uani 1 1 d . . .
F6 F 0.14560(12) 0.38171(10) 0.12047(10) 0.0531(3) Uani 1 1 d . . .
O1 O 0.71140(17) 0.81316(12) 0.34526(10) 0.0523(4) Uani 1 1 d . . .
O2 O 0.86044(12) 0.67444(12) 0.43193(11) 0.0439(3) Uani 1 1 d . . .
O3 O 0.63732(14) 0.69357(13) 0.49080(12) 0.0559(4) Uani 1 1 d . . .
O4 O 0.33962(14) 0.11943(11) 0.10521(10) 0.0457(3) Uani 1 1 d . . .
O5 O 0.28053(16) 0.28172(13) -0.01726(9) 0.0518(4) Uani 1 1 d . . .
O6 O 0.42072(14) 0.28821(15) 0.07962(13) 0.0611(5) 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 C24 1.380(2) . ?
C1 C2 1.383(2) . ?
C1 H1 0.9500 . ?
C2 C3 1.375(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.393(2) . ?
C3 H3 0.9500 . ?
C4 N5 1.363(2) . ?
C4 C25 1.456(2) . ?
N5 C24 1.3736(18) . ?
N5 C6 1.4892(19) . ?
C6 C7 1.521(2) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.540(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.511(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.391(2) . ?
C9 C23 1.404(2) . ?
C10 C11 1.384(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.390(2) . ?
C11 H11 0.9500 . ?
C12 C22 1.406(2) . ?
C12 C13 1.510(2) . ?
C13 C14 1.533(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.519(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 N16 1.487(2) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
N16 C17 1.366(2) . ?
N16 C21 1.3757(19) . ?
C17 C18 1.395(2) . ?
C17 C35 1.454(2) . ?
C18 C19 1.378(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.389(2) . ?
C19 H19 0.9500 . ?
C20 C21 1.379(2) . ?
C20 H20 0.9500 . ?
C21 C22 1.486(2) . ?
C22 C23 1.412(2) . ?
C23 C24 1.484(2) . ?
C25 C26 1.339(2) . ?
C25 H25 0.9500 . ?
C26 C27 1.452(2) . ?
C26 H26 0.9500 . ?
C27 C28 1.398(2) . ?
C27 C32 1.402(2) . ?
C28 C29 1.380(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.409(2) . ?
C29 H29 0.9500 . ?
C30 N1 1.370(2) . ?
C30 C31 1.414(2) . ?
C31 C32 1.378(2) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 N1 1.454(2) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 N1 1.450(2) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.341(3) . ?
C35 H35 0.9500 . ?
C36 C37 1.452(2) . ?
C36 H36 0.9500 . ?
C37 C38 1.398(2) . ?
C37 C42 1.400(2) . ?
C38 C39 1.381(3) . ?
C38 H38 0.9500 . ?
C39 C40 1.402(3) . ?
C39 H39 0.9500 . ?
C40 N2 1.372(2) . ?
C40 C41 1.410(2) . ?
C41 C42 1.379(2) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 N2 1.443(3) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 N2 1.448(3) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
S1 O3 1.4261(14) . ?
S1 O2 1.4286(13) . ?
S1 O1 1.4329(15) . ?
S1 C45 1.8210(18) . ?
S2 O6 1.4300(16) . ?
S2 O5 1.4377(15) . ?
S2 O4 1.4399(14) . ?
S2 C46 1.8209(19) . ?
C45 F1 1.317(3) . ?
C45 F3 1.327(2) . ?
C45 F2 1.333(2) . ?
C46 F4 1.329(2) . ?
C46 F6 1.331(2) . ?
C46 F5 1.331(2) . ?

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
C24 C1 C2 120.20(14) . . ?
C24 C1 H1 119.9 . . ?
C2 C1 H1 119.9 . . ?
C3 C2 C1 118.89(15) . . ?
C3 C2 H2 120.6 . . ?
C1 C2 H2 120.6 . . ?
C2 C3 C4 121.43(15) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
N5 C4 C3 118.18(14) . . ?
N5 C4 C25 120.24(14) . . ?
C3 C4 C25 121.58(14) . . ?
C4 N5 C24 121.58(13) . . ?
C4 N5 C6 120.69(12) . . ?
C24 N5 C6 117.59(12) . . ?
N5 C6 C7 111.82(13) . . ?
N5 C6 H6A 109.3 . . ?
C7 C6 H6A 109.3 . . ?
N5 C6 H6B 109.3 . . ?
C7 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
C6 C7 C8 111.69(13) . . ?
C6 C7 H7A 109.3 . . ?
C8 C7 H7A 109.3 . . ?
C6 C7 H7B 109.3 . . ?
C8 C7 H7B 109.3 . . ?
H7A C7 H7B 107.9 . . ?
C9 C8 C7 112.64(14) . . ?
C9 C8 H8A 109.1 . . ?
C7 C8 H8A 109.1 . . ?
C9 C8 H8B 109.1 . . ?
C7 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
C10 C9 C23 118.19(15) . . ?
C10 C9 C8 121.34(15) . . ?
C23 C9 C8 120.46(14) . . ?
C11 C10 C9 121.17(16) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C10 C11 C12 121.50(15) . . ?
C10 C11 H11 119.2 . . ?
C12 C11 H11 119.2 . . ?
C11 C12 C22 118.40(15) . . ?
C11 C12 C13 121.34(15) . . ?
C22 C12 C13 120.22(15) . . ?
C12 C13 C14 112.69(15) . . ?
C12 C13 H13A 109.1 . . ?
C14 C13 H13A 109.1 . . ?
C12 C13 H13B 109.1 . . ?
C14 C13 H13B 109.1 . . ?
H13A C13 H13B 107.8 . . ?
C15 C14 C13 111.54(13) . . ?
C15 C14 H14A 109.3 . . ?
C13 C14 H14A 109.3 . . ?
C15 C14 H14B 109.3 . . ?
C13 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
N16 C15 C14 111.84(14) . . ?
N16 C15 H15A 109.2 . . ?
C14 C15 H15A 109.2 . . ?
N16 C15 H15B 109.2 . . ?
C14 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
C17 N16 C21 122.08(13) . . ?
C17 N16 C15 120.60(13) . . ?
C21 N16 C15 117.23(13) . . ?
N16 C17 C18 118.24(14) . . ?
N16 C17 C35 119.34(15) . . ?
C18 C17 C35 122.39(15) . . ?
C19 C18 C17 120.83(15) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C18 C19 C20 119.19(15) . . ?
C18 C19 H19 120.4 . . ?
C20 C19 H19 120.4 . . ?
C21 C20 C19 120.40(14) . . ?
C21 C20 H20 119.8 . . ?
C19 C20 H20 119.8 . . ?
N16 C21 C20 118.97(14) . . ?
N16 C21 C22 119.31(13) . . ?
C20 C21 C22 121.69(13) . . ?
C12 C22 C23 119.90(14) . . ?
C12 C22 C21 119.71(14) . . ?
C23 C22 C21 119.96(13) . . ?
C9 C23 C22 120.68(14) . . ?
C9 C23 C24 119.05(13) . . ?
C22 C23 C24 119.99(13) . . ?
N5 C24 C1 119.57(14) . . ?
N5 C24 C23 119.19(13) . . ?
C1 C24 C23 121.22(13) . . ?
C26 C25 C4 121.00(15) . . ?
C26 C25 H25 119.5 . . ?
C4 C25 H25 119.5 . . ?
C25 C26 C27 127.77(16) . . ?
C25 C26 H26 116.1 . . ?
C27 C26 H26 116.1 . . ?
C28 C27 C32 117.04(15) . . ?
C28 C27 C26 119.62(15) . . ?
C32 C27 C26 123.33(15) . . ?
C29 C28 C27 122.28(16) . . ?
C29 C28 H28 118.9 . . ?
C27 C28 H28 118.9 . . ?
C28 C29 C30 120.51(15) . . ?
C28 C29 H29 119.7 . . ?
C30 C29 H29 119.7 . . ?
N1 C30 C29 122.19(15) . . ?
N1 C30 C31 120.27(15) . . ?
C29 C30 C31 117.52(14) . . ?
C32 C31 C30 120.91(15) . . ?
C32 C31 H31 119.5 . . ?
C30 C31 H31 119.5 . . ?
C31 C32 C27 121.73(15) . . ?
C31 C32 H32 119.1 . . ?
C27 C32 H32 119.1 . . ?
N1 C33 H33A 109.5 . . ?
N1 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N1 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N1 C34 H34A 109.5 . . ?
N1 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N1 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 C17 122.20(16) . . ?
C36 C35 H35 118.9 . . ?
C17 C35 H35 118.9 . . ?
C35 C36 C37 127.00(17) . . ?
C35 C36 H36 116.5 . . ?
C37 C36 H36 116.5 . . ?
C38 C37 C42 117.40(15) . . ?
C38 C37 C36 119.45(16) . . ?
C42 C37 C36 123.14(16) . . ?
C39 C38 C37 122.18(17) . . ?
C39 C38 H38 118.9 . . ?
C37 C38 H38 118.9 . . ?
C38 C39 C40 120.42(16) . . ?
C38 C39 H39 119.8 . . ?
C40 C39 H39 119.8 . . ?
N2 C40 C39 122.12(16) . . ?
N2 C40 C41 120.34(16) . . ?
C39 C40 C41 117.54(15) . . ?
C42 C41 C40 121.46(16) . . ?
C42 C41 H41 119.3 . . ?
C40 C41 H41 119.3 . . ?
C41 C42 C37 120.96(15) . . ?
C41 C42 H42 119.5 . . ?
C37 C42 H42 119.5 . . ?
N2 C43 H43A 109.5 . . ?
N2 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
N2 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N2 C44 H44A 109.5 . . ?
N2 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
N2 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C30 N1 C34 120.05(14) . . ?
C30 N1 C33 120.50(15) . . ?
C34 N1 C33 118.95(14) . . ?
C40 N2 C43 119.71(17) . . ?
C40 N2 C44 119.72(16) . . ?
C43 N2 C44 119.05(17) . . ?
O3 S1 O2 115.47(9) . . ?
O3 S1 O1 112.82(11) . . ?
O2 S1 O1 115.37(10) . . ?
O3 S1 C45 103.61(10) . . ?
O2 S1 C45 104.37(8) . . ?
O1 S1 C45 103.18(9) . . ?
O6 S2 O5 114.94(11) . . ?
O6 S2 O4 116.08(10) . . ?
O5 S2 O4 114.10(9) . . ?
O6 S2 C46 103.74(9) . . ?
O5 S2 C46 103.29(9) . . ?
O4 S2 C46 102.17(9) . . ?
F1 C45 F3 108.55(18) . . ?
F1 C45 F2 107.00(17) . . ?
F3 C45 F2 106.51(16) . . ?
F1 C45 S1 111.71(13) . . ?
F3 C45 S1 110.91(14) . . ?
F2 C45 S1 111.93(13) . . ?
F4 C46 F6 106.96(15) . . ?
F4 C46 F5 107.32(16) . . ?
F6 C46 F5 106.94(16) . . ?
F4 C46 S2 111.59(14) . . ?
F6 C46 S2 112.52(13) . . ?
F5 C46 S2 111.23(12) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.049
#===END
####################################################################### 
# 
# 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_mj264_ined_teply_sqd
_database_code_depnum_ccdc_archive 'CCDC 1004883'
_audit_update_record             
;
2014-05-22 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;
_publcif_datablock.id            {3698f1b2-230d-49e3-b5c3-2badbc8da17e}
# publcif _publ_body_element loop end

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H34 N2 O, 2(I)'
_chemical_formula_sum            'C39 H34 I2 N2 O'
_chemical_formula_weight         800.48
_chemical_compound_source        'synthesized by the authors'

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'
I I -0.4742 1.8119 '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'
_space_group_name_Hall           '-P 1'

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

_cell_length_a                   13.5867(4)
_cell_length_b                   14.1603(4)
_cell_length_c                   19.3953(6)
_cell_angle_alpha                87.9609(10)
_cell_angle_beta                 76.1122(10)
_cell_angle_gamma                86.1412(11)
_cell_volume                     3613.48(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7331
_cell_measurement_theta_min      2.2754
_cell_measurement_theta_max      25.9289

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1584
_exptl_absorpt_coefficient_mu    1.771
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6331
_exptl_absorpt_correction_T_max  0.8569
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'

_exptl_special_details           ?

_diffrn_ambient_temperature      150(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            33318
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0752
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.08
_diffrn_reflns_theta_max         26.00
_reflns_number_total             14184
_reflns_number_gt                9525
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'Bruker Instrument Service v2013.12.0.0'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2013)'
_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)+(0.0335P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14184
_refine_ls_number_parameters     799
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0441
_refine_ls_wR_factor_ref         0.0811
_refine_ls_wR_factor_gt          0.0737
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_restrained_S_all      0.937
_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
C11 C 0.4896(3) 0.3953(3) 0.7697(2) 0.0236(10) Uani 1 1 d . . .
H11 H 0.4913 0.3850 0.7213 0.028 Uiso 1 1 calc R . .
C12 C 0.4293(3) 0.3397(3) 0.8223(2) 0.0225(10) Uani 1 1 d . . .
C13 C 0.4226(3) 0.3625(3) 0.8926(2) 0.0302(11) Uani 1 1 d . . .
H13 H 0.3832 0.3263 0.9301 0.036 Uiso 1 1 calc R . .
C14 C 0.4723(3) 0.4365(3) 0.9078(2) 0.0308(11) Uani 1 1 d . . .
H14 H 0.4633 0.4537 0.9560 0.037 Uiso 1 1 calc R . .
N15 N 0.5341(2) 0.4861(2) 0.85615(18) 0.0249(8) Uani 1 1 d . . .
C16 C 0.5881(3) 0.5637(3) 0.8757(2) 0.0300(11) Uani 1 1 d . . .
H16A H 0.6581 0.5407 0.8768 0.036 Uiso 1 1 calc R . .
H16B H 0.5530 0.5859 0.9237 0.036 Uiso 1 1 calc R . .
C17 C 0.5914(3) 0.6444(3) 0.8228(2) 0.0290(11) Uani 1 1 d . . .
H17A H 0.6335 0.6936 0.8338 0.035 Uiso 1 1 calc R . .
H17B H 0.5219 0.6731 0.8266 0.035 Uiso 1 1 calc R . .
C18 C 0.6353(3) 0.6110(3) 0.7478(2) 0.0251(10) Uani 1 1 d . . .
C19 C 0.6901(3) 0.6706(3) 0.6941(2) 0.0248(10) Uani 1 1 d . . .
C110 C 0.7235(3) 0.6382(3) 0.6252(2) 0.0240(10) Uani 1 1 d . . .
C111 C 0.7117(3) 0.5439(3) 0.6108(2) 0.0235(10) Uani 1 1 d . . .
C112 C 0.7412(3) 0.5033(3) 0.5371(2) 0.0286(11) Uani 1 1 d . . .
H11A H 0.8087 0.4690 0.5294 0.034 Uiso 1 1 calc R . .
H11B H 0.7451 0.5551 0.5010 0.034 Uiso 1 1 calc R . .
C113 C 0.6624(3) 0.4361(3) 0.5295(2) 0.0317(11) Uani 1 1 d . . .
H11C H 0.5947 0.4702 0.5370 0.038 Uiso 1 1 calc R . .
H11D H 0.6800 0.4096 0.4812 0.038 Uiso 1 1 calc R . .
N114 N 0.6605(2) 0.3588(2) 0.58357(18) 0.0246(8) Uani 1 1 d . . .
C115 C 0.6511(3) 0.2679(3) 0.5642(2) 0.0314(11) Uani 1 1 d . . .
H115 H 0.6427 0.2567 0.5180 0.038 Uiso 1 1 calc R . .
C116 C 0.6537(3) 0.1948(3) 0.6101(2) 0.0294(11) Uani 1 1 d . . .
H116 H 0.6408 0.1332 0.5979 0.035 Uiso 1 1 calc R . .
C117 C 0.6755(3) 0.2095(3) 0.6764(2) 0.0268(11) Uani 1 1 d . . .
C118 C 0.6844(3) 0.1356(3) 0.7253(3) 0.0343(12) Uani 1 1 d . . .
H118 H 0.6730 0.0728 0.7148 0.041 Uiso 1 1 calc R . .
C119 C 0.7090(3) 0.1529(3) 0.7876(3) 0.0363(12) Uani 1 1 d . . .
H119 H 0.7128 0.1024 0.8206 0.044 Uiso 1 1 calc R . .
C120 C 0.7289(3) 0.2446(3) 0.8037(2) 0.0335(11) Uani 1 1 d . . .
H120 H 0.7487 0.2554 0.8464 0.040 Uiso 1 1 calc R . .
C121 C 0.7197(3) 0.3182(3) 0.7580(2) 0.0259(10) Uani 1 1 d . . .
H121 H 0.7335 0.3800 0.7690 0.031 Uiso 1 1 calc R . .
C122 C 0.6901(3) 0.3037(3) 0.6944(2) 0.0228(10) Uani 1 1 d . . .
C123 C 0.6717(3) 0.3797(3) 0.6486(2) 0.0218(10) Uani 1 1 d . . .
C124 C 0.6666(3) 0.4817(3) 0.6648(2) 0.0207(9) Uani 1 1 d . . .
C125 C 0.6196(3) 0.5189(3) 0.7332(2) 0.0204(9) Uani 1 1 d . . .
C126 C 0.5468(3) 0.4647(3) 0.7861(2) 0.0224(10) Uani 1 1 d . . .
C127 C 0.7092(3) 0.7697(3) 0.7108(2) 0.0358(12) Uani 1 1 d . . .
H12A H 0.7767 0.7858 0.6835 0.054 Uiso 1 1 calc R . .
H12B H 0.7059 0.7736 0.7617 0.054 Uiso 1 1 calc R . .
H12C H 0.6575 0.8141 0.6982 0.054 Uiso 1 1 calc R . .
C128 C 0.7739(3) 0.7042(3) 0.5660(2) 0.0310(11) Uani 1 1 d . . .
H12D H 0.7427 0.7684 0.5747 0.046 Uiso 1 1 calc R . .
H12E H 0.7651 0.6826 0.5205 0.046 Uiso 1 1 calc R . .
H12F H 0.8465 0.7042 0.5645 0.046 Uiso 1 1 calc R . .
C129 C 0.3793(3) 0.2629(3) 0.8007(2) 0.0260(10) Uani 1 1 d . . .
H129 H 0.3779 0.2604 0.7520 0.031 Uiso 1 1 calc R . .
C130 C 0.3347(3) 0.1951(3) 0.8449(2) 0.0291(11) Uani 1 1 d . . .
H130 H 0.3349 0.1985 0.8937 0.035 Uiso 1 1 calc R . .
C131 C 0.2858(3) 0.1157(3) 0.8230(2) 0.0280(11) Uani 1 1 d . . .
C132 C 0.2620(3) 0.0403(3) 0.8703(2) 0.0319(11) Uani 1 1 d . . .
H132 H 0.2730 0.0427 0.9167 0.038 Uiso 1 1 calc R . .
C133 C 0.2208(3) -0.0410(3) 0.8490(2) 0.0310(12) Uani 1 1 d . . .
C134 C 0.2022(3) -0.1218(3) 0.8943(3) 0.0387(13) Uani 1 1 d . . .
H134 H 0.2138 -0.1216 0.9407 0.046 Uiso 1 1 calc R . .
C135 C 0.1679(3) -0.1995(3) 0.8711(3) 0.0388(13) Uani 1 1 d . . .
H135 H 0.1557 -0.2535 0.9017 0.047 Uiso 1 1 calc R . .
C136 C 0.1496(3) -0.2022(3) 0.8025(3) 0.0366(12) Uani 1 1 d . . .
C137 C 0.1654(3) -0.1255(3) 0.7581(3) 0.0339(12) Uani 1 1 d . . .
H137 H 0.1521 -0.1269 0.7122 0.041 Uiso 1 1 calc R . .
C138 C 0.2024(3) -0.0423(3) 0.7808(2) 0.0304(11) Uani 1 1 d . . .
C139 C 0.2230(3) 0.0370(3) 0.7344(2) 0.0328(11) Uani 1 1 d . . .
H139 H 0.2087 0.0371 0.6888 0.039 Uiso 1 1 calc R . .
C140 C 0.2638(3) 0.1137(3) 0.7555(2) 0.0309(11) Uani 1 1 d . . .
H140 H 0.2775 0.1667 0.7240 0.037 Uiso 1 1 calc R . .
C141 C 0.1263(4) -0.2982(3) 0.7111(3) 0.0518(15) Uani 1 1 d . . .
H14A H 0.0720 -0.2584 0.6974 0.078 Uiso 1 1 calc R . .
H14B H 0.1182 -0.3647 0.7025 0.078 Uiso 1 1 calc R . .
H14C H 0.1923 -0.2795 0.6829 0.078 Uiso 1 1 calc R . .
C21 C 0.8493(3) 0.6244(3) 0.1963(2) 0.0221(10) Uani 1 1 d . . .
H21 H 0.8344 0.6395 0.2452 0.026 Uiso 1 1 calc R . .
C22 C 0.8011(3) 0.5500(3) 0.1754(2) 0.0217(10) Uani 1 1 d . . .
C23 C 0.8205(3) 0.5335(3) 0.1028(2) 0.0290(11) Uani 1 1 d . . .
H23 H 0.7906 0.4829 0.0862 0.035 Uiso 1 1 calc R . .
C24 C 0.8825(3) 0.5900(3) 0.0558(2) 0.0303(11) Uani 1 1 d . . .
H24 H 0.8922 0.5805 0.0063 0.036 Uiso 1 1 calc R . .
N25 N 0.9304(2) 0.6592(2) 0.07788(18) 0.0239(8) Uani 1 1 d . . .
C26 C 0.9979(3) 0.7192(3) 0.0246(2) 0.0320(11) Uani 1 1 d . . .
H26A H 0.9835 0.7132 -0.0227 0.038 Uiso 1 1 calc R . .
H26B H 1.0698 0.6983 0.0212 0.038 Uiso 1 1 calc R . .
C27 C 0.9791(3) 0.8207(3) 0.0473(2) 0.0294(11) Uani 1 1 d . . .
H27A H 0.9083 0.8425 0.0473 0.035 Uiso 1 1 calc R . .
H27B H 1.0251 0.8608 0.0129 0.035 Uiso 1 1 calc R . .
C28 C 0.9965(3) 0.8314(3) 0.1203(2) 0.0237(10) Uani 1 1 d . . .
C29 C 1.0319(3) 0.9122(3) 0.1426(2) 0.0271(11) Uani 1 1 d . . .
C210 C 1.0419(3) 0.9190(3) 0.2118(2) 0.0276(11) Uani 1 1 d . . .
C211 C 1.0193(3) 0.8406(3) 0.2590(2) 0.0255(10) Uani 1 1 d . . .
C212 C 1.0167(3) 0.8454(3) 0.3375(2) 0.0318(11) Uani 1 1 d . . .
H21A H 1.0839 0.8244 0.3459 0.038 Uiso 1 1 calc R . .
H21B H 0.9997 0.9111 0.3539 0.038 Uiso 1 1 calc R . .
C213 C 0.9369(3) 0.7811(3) 0.3772(2) 0.0315(11) Uani 1 1 d . . .
H21C H 0.9320 0.7833 0.4289 0.038 Uiso 1 1 calc R . .
H21D H 0.8698 0.8017 0.3685 0.038 Uiso 1 1 calc R . .
N214 N 0.9672(2) 0.6836(2) 0.35153(17) 0.0235(8) Uani 1 1 d . . .
C215 C 0.9640(3) 0.6107(3) 0.4005(2) 0.0311(11) Uani 1 1 d . . .
H215 H 0.9392 0.6231 0.4496 0.037 Uiso 1 1 calc R . .
C216 C 0.9959(3) 0.5218(3) 0.3795(2) 0.0310(11) Uani 1 1 d . . .
H216 H 0.9897 0.4711 0.4134 0.037 Uiso 1 1 calc R . .
C217 C 1.0386(3) 0.5043(3) 0.3067(2) 0.0239(10) Uani 1 1 d . . .
C218 C 1.0787(3) 0.4129(3) 0.2827(2) 0.0279(11) Uani 1 1 d . . .
H218 H 1.0758 0.3614 0.3158 0.034 Uiso 1 1 calc R . .
C219 C 1.1211(3) 0.3987(3) 0.2131(2) 0.0301(11) Uani 1 1 d . . .
H219 H 1.1450 0.3367 0.1974 0.036 Uiso 1 1 calc R . .
C220 C 1.1302(3) 0.4742(3) 0.1636(2) 0.0284(11) Uani 1 1 d . . .
H220 H 1.1617 0.4629 0.1151 0.034 Uiso 1 1 calc R . .
C221 C 1.0941(3) 0.5641(3) 0.1845(2) 0.0237(10) Uani 1 1 d . . .
H221 H 1.1031 0.6150 0.1509 0.028 Uiso 1 1 calc R . .
C222 C 1.0433(3) 0.5812(3) 0.2565(2) 0.0213(10) Uani 1 1 d . . .
C223 C 0.9992(3) 0.6712(3) 0.2812(2) 0.0211(10) Uani 1 1 d . . .
C224 C 0.9937(3) 0.7564(3) 0.2349(2) 0.0211(10) Uani 1 1 d . . .
C225 C 0.9733(3) 0.7540(3) 0.1680(2) 0.0215(10) Uani 1 1 d . . .
C226 C 0.9184(3) 0.6772(3) 0.1480(2) 0.0220(10) Uani 1 1 d . . .
C227 C 1.0562(4) 0.9963(3) 0.0911(3) 0.0417(13) Uani 1 1 d . . .
H22A H 1.1300 0.9975 0.0730 0.063 Uiso 1 1 calc R . .
H22B H 1.0301 1.0552 0.1160 0.063 Uiso 1 1 calc R . .
H22C H 1.0242 0.9903 0.0514 0.063 Uiso 1 1 calc R . .
C228 C 1.0761(3) 1.0075(3) 0.2377(3) 0.0366(12) Uani 1 1 d . . .
H22D H 1.0180 1.0534 0.2515 0.055 Uiso 1 1 calc R . .
H22E H 1.1281 1.0350 0.1997 0.055 Uiso 1 1 calc R . .
H22F H 1.1046 0.9917 0.2789 0.055 Uiso 1 1 calc R . .
C229 C 0.7334(3) 0.4953(3) 0.2300(2) 0.0237(10) Uani 1 1 d . . .
H229 H 0.7184 0.5170 0.2774 0.028 Uiso 1 1 calc R . .
C230 C 0.6908(3) 0.4162(3) 0.2176(2) 0.0254(10) Uani 1 1 d . . .
H230 H 0.7031 0.3970 0.1697 0.030 Uiso 1 1 calc R . .
C231 C 0.6278(3) 0.3580(3) 0.2716(2) 0.0220(10) Uani 1 1 d . . .
C232 C 0.5867(3) 0.3896(3) 0.3427(2) 0.0263(10) Uani 1 1 d . . .
H232 H 0.5967 0.4519 0.3551 0.032 Uiso 1 1 calc R . .
C233 C 0.5329(3) 0.3298(3) 0.3928(2) 0.0246(10) Uani 1 1 d . . .
H233 H 0.5048 0.3519 0.4395 0.030 Uiso 1 1 calc R . .
C234 C 0.5181(3) 0.2361(3) 0.3767(2) 0.0230(10) Uani 1 1 d . . .
C235 C 0.4645(3) 0.1737(3) 0.4291(2) 0.0265(10) Uani 1 1 d . . .
H235 H 0.4370 0.1947 0.4762 0.032 Uiso 1 1 calc R . .
C236 C 0.4527(3) 0.0836(3) 0.4115(2) 0.0305(11) Uani 1 1 d . . .
C237 C 0.4932(3) 0.0508(3) 0.3417(2) 0.0311(11) Uani 1 1 d . . .
H237 H 0.4847 -0.0124 0.3304 0.037 Uiso 1 1 calc R . .
C238 C 0.5442(3) 0.1099(3) 0.2910(2) 0.0293(11) Uani 1 1 d . . .
H238 H 0.5718 0.0873 0.2444 0.035 Uiso 1 1 calc R . .
C239 C 0.5569(3) 0.2044(3) 0.3063(2) 0.0231(10) Uani 1 1 d . . .
C240 C 0.6109(3) 0.2675(3) 0.2552(2) 0.0236(10) Uani 1 1 d . . .
H240 H 0.6363 0.2468 0.2078 0.028 Uiso 1 1 calc R . .
C241 C 0.3569(3) 0.0467(3) 0.5287(2) 0.0446(14) Uani 1 1 d . . .
H24A H 0.4093 0.0700 0.5497 0.067 Uiso 1 1 calc R . .
H24B H 0.3262 -0.0071 0.5571 0.067 Uiso 1 1 calc R . .
H24C H 0.3044 0.0974 0.5278 0.067 Uiso 1 1 calc R . .
I1 I 0.64581(2) 0.66431(2) 0.395405(15) 0.03483(9) Uani 1 1 d . . .
I2 I 0.30085(2) 0.63296(2) 0.005851(16) 0.03471(9) Uani 1 1 d . . .
I3 I 0.23661(2) 0.23487(2) 0.057909(16) 0.03639(9) Uani 1 1 d . . .
I4 I 0.91861(2) 0.26732(2) 0.473430(18) 0.03804(9) Uani 1 1 d . . .
O1 O 0.1210(2) -0.2867(2) 0.78474(19) 0.0438(9) Uani 1 1 d . . .
O2 O 0.4018(2) 0.01713(19) 0.45794(16) 0.0371(8) 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
C11 C126 1.383(6) . ?
C11 C12 1.400(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.392(6) . ?
C12 C129 1.446(6) . ?
C13 C14 1.361(6) . ?
C13 H13 0.9500 . ?
C14 N15 1.353(5) . ?
C14 H14 0.9500 . ?
N15 C126 1.371(5) . ?
N15 C16 1.470(5) . ?
C16 C17 1.503(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.513(6) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C125 1.386(6) . ?
C18 C19 1.414(5) . ?
C19 C110 1.389(6) . ?
C19 C127 1.504(6) . ?
C110 C111 1.401(6) . ?
C110 C128 1.514(5) . ?
C111 C124 1.396(5) . ?
C111 C112 1.513(6) . ?
C112 C113 1.515(6) . ?
C112 H11A 0.9900 . ?
C112 H11B 0.9900 . ?
C113 N114 1.487(5) . ?
C113 H11C 0.9900 . ?
C113 H11D 0.9900 . ?
N114 C123 1.351(5) . ?
N114 C115 1.375(5) . ?
C115 C116 1.345(6) . ?
C115 H115 0.9500 . ?
C116 C117 1.414(6) . ?
C116 H116 0.9500 . ?
C117 C118 1.405(6) . ?
C117 C122 1.428(6) . ?
C118 C119 1.363(6) . ?
C118 H118 0.9500 . ?
C119 C120 1.405(6) . ?
C119 H119 0.9500 . ?
C120 C121 1.362(6) . ?
C120 H120 0.9500 . ?
C121 C122 1.413(6) . ?
C121 H121 0.9500 . ?
C122 C123 1.418(6) . ?
C123 C124 1.483(5) . ?
C124 C125 1.428(5) . ?
C125 C126 1.476(5) . ?
C127 H12A 0.9800 . ?
C127 H12B 0.9800 . ?
C127 H12C 0.9800 . ?
C128 H12D 0.9800 . ?
C128 H12E 0.9800 . ?
C128 H12F 0.9800 . ?
C129 C130 1.340(5) . ?
C129 H129 0.9500 . ?
C130 C131 1.468(6) . ?
C130 H130 0.9500 . ?
C131 C132 1.386(6) . ?
C131 C140 1.413(6) . ?
C132 C133 1.428(6) . ?
C132 H132 0.9500 . ?
C133 C138 1.405(6) . ?
C133 C134 1.418(6) . ?
C134 C135 1.355(6) . ?
C134 H134 0.9500 . ?
C135 C136 1.412(7) . ?
C135 H135 0.9500 . ?
C136 C137 1.358(6) . ?
C136 O1 1.363(5) . ?
C137 C138 1.433(6) . ?
C137 H137 0.9500 . ?
C138 C139 1.414(6) . ?
C139 C140 1.369(6) . ?
C139 H139 0.9500 . ?
C140 H140 0.9500 . ?
C141 O1 1.427(6) . ?
C141 H14A 0.9800 . ?
C141 H14B 0.9800 . ?
C141 H14C 0.9800 . ?
C21 C226 1.393(5) . ?
C21 C22 1.397(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.393(6) . ?
C22 C229 1.463(5) . ?
C23 C24 1.360(5) . ?
C23 H23 0.9500 . ?
C24 N25 1.348(5) . ?
C24 H24 0.9500 . ?
N25 C226 1.362(5) . ?
N25 C26 1.489(5) . ?
C26 C27 1.504(6) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.506(6) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.390(6) . ?
C28 C225 1.411(5) . ?
C29 C210 1.389(6) . ?
C29 C227 1.529(6) . ?
C210 C211 1.416(6) . ?
C210 C228 1.508(6) . ?
C211 C224 1.390(6) . ?
C211 C212 1.519(6) . ?
C212 C213 1.510(5) . ?
C212 H21A 0.9900 . ?
C212 H21B 0.9900 . ?
C213 N214 1.483(5) . ?
C213 H21C 0.9900 . ?
C213 H21D 0.9900 . ?
N214 C223 1.343(5) . ?
N214 C215 1.373(5) . ?
C215 C216 1.349(6) . ?
C215 H215 0.9500 . ?
C216 C217 1.415(6) . ?
C216 H216 0.9500 . ?
C217 C218 1.419(5) . ?
C217 C222 1.429(5) . ?
C218 C219 1.352(6) . ?
C218 H218 0.9500 . ?
C219 C220 1.401(6) . ?
C219 H219 0.9500 . ?
C220 C221 1.372(5) . ?
C220 H220 0.9500 . ?
C221 C222 1.422(5) . ?
C221 H221 0.9500 . ?
C222 C223 1.419(5) . ?
C223 C224 1.487(5) . ?
C224 C225 1.393(6) . ?
C225 C226 1.471(6) . ?
C227 H22A 0.9800 . ?
C227 H22B 0.9800 . ?
C227 H22C 0.9800 . ?
C228 H22D 0.9800 . ?
C228 H22E 0.9800 . ?
C228 H22F 0.9800 . ?
C229 C230 1.349(6) . ?
C229 H229 0.9500 . ?
C230 C231 1.454(5) . ?
C230 H230 0.9500 . ?
C231 C240 1.378(6) . ?
C231 C232 1.434(5) . ?
C232 C233 1.371(5) . ?
C232 H232 0.9500 . ?
C233 C234 1.411(5) . ?
C233 H233 0.9500 . ?
C234 C235 1.418(5) . ?
C234 C239 1.418(5) . ?
C235 C236 1.362(6) . ?
C235 H235 0.9500 . ?
C236 O2 1.380(5) . ?
C236 C237 1.416(6) . ?
C237 C238 1.356(6) . ?
C237 H237 0.9500 . ?
C238 C239 1.412(6) . ?
C238 H238 0.9500 . ?
C239 C240 1.413(5) . ?
C240 H240 0.9500 . ?
C241 O2 1.426(5) . ?
C241 H24A 0.9800 . ?
C241 H24B 0.9800 . ?
C241 H24C 0.9800 . ?

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
C126 C11 C12 122.1(4) . . ?
C126 C11 H11 119.0 . . ?
C12 C11 H11 119.0 . . ?
C13 C12 C11 116.9(4) . . ?
C13 C12 C129 124.5(4) . . ?
C11 C12 C129 118.6(4) . . ?
C14 C13 C12 120.3(4) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
N15 C14 C13 121.6(4) . . ?
N15 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
C14 N15 C126 120.7(4) . . ?
C14 N15 C16 119.4(4) . . ?
C126 N15 C16 119.9(3) . . ?
N15 C16 C17 110.1(4) . . ?
N15 C16 H16A 109.6 . . ?
C17 C16 H16A 109.6 . . ?
N15 C16 H16B 109.6 . . ?
C17 C16 H16B 109.6 . . ?
H16A C16 H16B 108.2 . . ?
C16 C17 C18 111.1(3) . . ?
C16 C17 H17A 109.4 . . ?
C18 C17 H17A 109.4 . . ?
C16 C17 H17B 109.4 . . ?
C18 C17 H17B 109.4 . . ?
H17A C17 H17B 108.0 . . ?
C125 C18 C19 120.7(4) . . ?
C125 C18 C17 117.3(4) . . ?
C19 C18 C17 122.0(4) . . ?
C110 C19 C18 119.6(4) . . ?
C110 C19 C127 120.0(4) . . ?
C18 C19 C127 120.4(4) . . ?
C19 C110 C111 119.7(4) . . ?
C19 C110 C128 120.1(4) . . ?
C111 C110 C128 120.2(4) . . ?
C124 C111 C110 121.0(4) . . ?
C124 C111 C112 115.3(4) . . ?
C110 C111 C112 123.6(4) . . ?
C111 C112 C113 109.1(3) . . ?
C111 C112 H11A 109.9 . . ?
C113 C112 H11A 109.9 . . ?
C111 C112 H11B 109.9 . . ?
C113 C112 H11B 109.9 . . ?
H11A C112 H11B 108.3 . . ?
N114 C113 C112 108.0(4) . . ?
N114 C113 H11C 110.1 . . ?
C112 C113 H11C 110.1 . . ?
N114 C113 H11D 110.1 . . ?
C112 C113 H11D 110.1 . . ?
H11C C113 H11D 108.4 . . ?
C123 N114 C115 122.7(4) . . ?
C123 N114 C113 119.1(3) . . ?
C115 N114 C113 118.2(4) . . ?
C116 C115 N114 120.6(4) . . ?
C116 C115 H115 119.7 . . ?
N114 C115 H115 119.7 . . ?
C115 C116 C117 120.1(4) . . ?
C115 C116 H116 119.9 . . ?
C117 C116 H116 119.9 . . ?
C118 C117 C116 123.0(4) . . ?
C118 C117 C122 118.5(4) . . ?
C116 C117 C122 118.4(4) . . ?
C119 C118 C117 120.8(4) . . ?
C119 C118 H118 119.6 . . ?
C117 C118 H118 119.6 . . ?
C118 C119 C120 120.8(4) . . ?
C118 C119 H119 119.6 . . ?
C120 C119 H119 119.6 . . ?
C121 C120 C119 119.9(5) . . ?
C121 C120 H120 120.0 . . ?
C119 C120 H120 120.0 . . ?
C120 C121 C122 120.9(4) . . ?
C120 C121 H121 119.6 . . ?
C122 C121 H121 119.6 . . ?
C121 C122 C123 122.2(4) . . ?
C121 C122 C117 118.9(4) . . ?
C123 C122 C117 118.9(4) . . ?
N114 C123 C122 118.1(4) . . ?
N114 C123 C124 116.3(4) . . ?
C122 C123 C124 125.6(4) . . ?
C111 C124 C125 118.6(3) . . ?
C111 C124 C123 118.1(3) . . ?
C125 C124 C123 123.3(4) . . ?
C18 C125 C124 119.4(4) . . ?
C18 C125 C126 119.1(3) . . ?
C124 C125 C126 121.3(3) . . ?
N15 C126 C11 118.0(4) . . ?
N15 C126 C125 117.4(4) . . ?
C11 C126 C125 124.6(4) . . ?
C19 C127 H12A 109.5 . . ?
C19 C127 H12B 109.5 . . ?
H12A C127 H12B 109.5 . . ?
C19 C127 H12C 109.5 . . ?
H12A C127 H12C 109.5 . . ?
H12B C127 H12C 109.5 . . ?
C110 C128 H12D 109.5 . . ?
C110 C128 H12E 109.5 . . ?
H12D C128 H12E 109.5 . . ?
C110 C128 H12F 109.5 . . ?
H12D C128 H12F 109.5 . . ?
H12E C128 H12F 109.5 . . ?
C130 C129 C12 124.1(4) . . ?
C130 C129 H129 118.0 . . ?
C12 C129 H129 118.0 . . ?
C129 C130 C131 124.3(4) . . ?
C129 C130 H130 117.8 . . ?
C131 C130 H130 117.8 . . ?
C132 C131 C140 119.5(4) . . ?
C132 C131 C130 118.2(4) . . ?
C140 C131 C130 122.2(4) . . ?
C131 C132 C133 119.8(4) . . ?
C131 C132 H132 120.1 . . ?
C133 C132 H132 120.1 . . ?
C138 C133 C134 119.4(5) . . ?
C138 C133 C132 119.4(4) . . ?
C134 C133 C132 121.2(5) . . ?
C135 C134 C133 119.6(5) . . ?
C135 C134 H134 120.2 . . ?
C133 C134 H134 120.2 . . ?
C134 C135 C136 121.7(5) . . ?
C134 C135 H135 119.2 . . ?
C136 C135 H135 119.2 . . ?
C137 C136 O1 124.4(5) . . ?
C137 C136 C135 120.2(5) . . ?
O1 C136 C135 115.3(4) . . ?
C136 C137 C138 119.5(5) . . ?
C136 C137 H137 120.2 . . ?
C138 C137 H137 120.2 . . ?
C133 C138 C139 119.9(4) . . ?
C133 C138 C137 119.6(4) . . ?
C139 C138 C137 120.5(5) . . ?
C140 C139 C138 119.7(5) . . ?
C140 C139 H139 120.2 . . ?
C138 C139 H139 120.2 . . ?
C139 C140 C131 121.5(4) . . ?
C139 C140 H140 119.3 . . ?
C131 C140 H140 119.3 . . ?
O1 C141 H14A 109.5 . . ?
O1 C141 H14B 109.5 . . ?
H14A C141 H14B 109.5 . . ?
O1 C141 H14C 109.5 . . ?
H14A C141 H14C 109.5 . . ?
H14B C141 H14C 109.5 . . ?
C226 C21 C22 122.4(4) . . ?
C226 C21 H21 118.8 . . ?
C22 C21 H21 118.8 . . ?
C23 C22 C21 117.1(4) . . ?
C23 C22 C229 124.2(4) . . ?
C21 C22 C229 118.7(4) . . ?
C24 C23 C22 119.9(4) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
N25 C24 C23 121.4(4) . . ?
N25 C24 H24 119.3 . . ?
C23 C24 H24 119.3 . . ?
C24 N25 C226 122.0(3) . . ?
C24 N25 C26 119.7(4) . . ?
C226 N25 C26 118.3(4) . . ?
N25 C26 C27 108.9(3) . . ?
N25 C26 H26A 109.9 . . ?
C27 C26 H26A 109.9 . . ?
N25 C26 H26B 109.9 . . ?
C27 C26 H26B 109.9 . . ?
H26A C26 H26B 108.3 . . ?
C26 C27 C28 111.1(3) . . ?
C26 C27 H27A 109.4 . . ?
C28 C27 H27A 109.4 . . ?
C26 C27 H27B 109.4 . . ?
C28 C27 H27B 109.4 . . ?
H27A C27 H27B 108.0 . . ?
C29 C28 C225 119.7(4) . . ?
C29 C28 C27 124.0(4) . . ?
C225 C28 C27 116.3(4) . . ?
C210 C29 C28 121.1(4) . . ?
C210 C29 C227 119.3(4) . . ?
C28 C29 C227 119.6(4) . . ?
C29 C210 C211 118.8(4) . . ?
C29 C210 C228 121.8(4) . . ?
C211 C210 C228 119.5(4) . . ?
C224 C211 C210 120.3(4) . . ?
C224 C211 C212 117.3(4) . . ?
C210 C211 C212 122.4(4) . . ?
C213 C212 C211 107.7(4) . . ?
C213 C212 H21A 110.2 . . ?
C211 C212 H21A 110.2 . . ?
C213 C212 H21B 110.2 . . ?
C211 C212 H21B 110.2 . . ?
H21A C212 H21B 108.5 . . ?
N214 C213 C212 107.8(3) . . ?
N214 C213 H21C 110.1 . . ?
C212 C213 H21C 110.1 . . ?
N214 C213 H21D 110.1 . . ?
C212 C213 H21D 110.1 . . ?
H21C C213 H21D 108.5 . . ?
C223 N214 C215 123.1(3) . . ?
C223 N214 C213 118.1(3) . . ?
C215 N214 C213 118.7(3) . . ?
C216 C215 N214 120.6(4) . . ?
C216 C215 H215 119.7 . . ?
N214 C215 H215 119.7 . . ?
C215 C216 C217 119.7(4) . . ?
C215 C216 H216 120.1 . . ?
C217 C216 H216 120.1 . . ?
C216 C217 C218 121.7(4) . . ?
C216 C217 C222 118.9(4) . . ?
C218 C217 C222 119.4(4) . . ?
C219 C218 C217 120.3(4) . . ?
C219 C218 H218 119.8 . . ?
C217 C218 H218 119.8 . . ?
C218 C219 C220 121.0(4) . . ?
C218 C219 H219 119.5 . . ?
C220 C219 H219 119.5 . . ?
C221 C220 C219 120.7(4) . . ?
C221 C220 H220 119.7 . . ?
C219 C220 H220 119.7 . . ?
C220 C221 C222 120.2(4) . . ?
C220 C221 H221 119.9 . . ?
C222 C221 H221 119.9 . . ?
C223 C222 C221 123.3(4) . . ?
C223 C222 C217 118.5(4) . . ?
C221 C222 C217 118.2(4) . . ?
N214 C223 C222 118.5(4) . . ?
N214 C223 C224 116.7(3) . . ?
C222 C223 C224 124.6(4) . . ?
C211 C224 C225 119.8(4) . . ?
C211 C224 C223 116.2(4) . . ?
C225 C224 C223 123.8(4) . . ?
C224 C225 C28 119.5(4) . . ?
C224 C225 C226 121.7(4) . . ?
C28 C225 C226 118.5(4) . . ?
N25 C226 C21 116.9(4) . . ?
N25 C226 C225 118.9(3) . . ?
C21 C226 C225 124.2(4) . . ?
C29 C227 H22A 109.5 . . ?
C29 C227 H22B 109.5 . . ?
H22A C227 H22B 109.5 . . ?
C29 C227 H22C 109.5 . . ?
H22A C227 H22C 109.5 . . ?
H22B C227 H22C 109.5 . . ?
C210 C228 H22D 109.5 . . ?
C210 C228 H22E 109.5 . . ?
H22D C228 H22E 109.5 . . ?
C210 C228 H22F 109.5 . . ?
H22D C228 H22F 109.5 . . ?
H22E C228 H22F 109.5 . . ?
C230 C229 C22 124.4(4) . . ?
C230 C229 H229 117.8 . . ?
C22 C229 H229 117.8 . . ?
C229 C230 C231 125.4(4) . . ?
C229 C230 H230 117.3 . . ?
C231 C230 H230 117.3 . . ?
C240 C231 C232 118.6(4) . . ?
C240 C231 C230 119.2(4) . . ?
C232 C231 C230 122.2(4) . . ?
C233 C232 C231 119.9(4) . . ?
C233 C232 H232 120.0 . . ?
C231 C232 H232 120.0 . . ?
C232 C233 C234 121.7(4) . . ?
C232 C233 H233 119.2 . . ?
C234 C233 H233 119.2 . . ?
C233 C234 C235 121.5(4) . . ?
C233 C234 C239 119.0(4) . . ?
C235 C234 C239 119.5(4) . . ?
C236 C235 C234 119.6(4) . . ?
C236 C235 H235 120.2 . . ?
C234 C235 H235 120.2 . . ?
C235 C236 O2 124.6(4) . . ?
C235 C236 C237 121.2(4) . . ?
O2 C236 C237 114.2(4) . . ?
C238 C237 C236 119.8(4) . . ?
C238 C237 H237 120.1 . . ?
C236 C237 H237 120.1 . . ?
C237 C238 C239 121.2(4) . . ?
C237 C238 H238 119.4 . . ?
C239 C238 H238 119.4 . . ?
C238 C239 C240 122.7(4) . . ?
C238 C239 C234 118.7(4) . . ?
C240 C239 C234 118.5(4) . . ?
C231 C240 C239 122.3(4) . . ?
C231 C240 H240 118.9 . . ?
C239 C240 H240 118.9 . . ?
O2 C241 H24A 109.5 . . ?
O2 C241 H24B 109.5 . . ?
H24A C241 H24B 109.5 . . ?
O2 C241 H24C 109.5 . . ?
H24A C241 H24C 109.5 . . ?
H24B C241 H24C 109.5 . . ?
C136 O1 C141 115.9(4) . . ?
C236 O2 C241 116.9(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.104

# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.000 -0.000 0.500 198 52 ' '
2 0.500 1.000 0.000 286 73 ' '
_platon_squeeze_details          ?
#===END

####################################################################### 
# 
# 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_mj256_i_teply
_database_code_depnum_ccdc_archive 'CCDC 1004884'
_audit_update_record             
;
2014-05-22 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H34 N2, 2(I)'
_chemical_formula_sum            'C42 H34 I2 N2'
_chemical_formula_weight         820.51
_chemical_compound_source        'synthesized by the authors'

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

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

_cell_length_a                   7.7728(2)
_cell_length_b                   23.8635(6)
_cell_length_c                   36.1252(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6700.7(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9876
_cell_measurement_theta_min      2.8132
_cell_measurement_theta_max      27.4650

_exptl_crystal_description       bar
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3248
_exptl_absorpt_coefficient_mu    1.911
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5080
_exptl_absorpt_correction_T_max  0.8231
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43985
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_theta_min         1.13
_diffrn_reflns_theta_max         26.00
_reflns_number_total             6591
_reflns_number_gt                5580
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'Bruker Instrument Service v2013.12.0.0'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_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)+(0.0318P)²+53.8696P] 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         6591
_refine_ls_number_parameters     417
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0611
_refine_ls_wR_factor_ref         0.1329
_refine_ls_wR_factor_gt          0.1264
_refine_ls_goodness_of_fit_ref   1.269
_refine_ls_restrained_S_all      1.269
_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
C1 C 0.1142(8) 0.0419(2) 0.09838(17) 0.0162(13) Uani 1 1 d . . .
H1 H 0.1127 0.0400 0.1246 0.019 Uiso 1 1 calc R . .
C2 C 0.1691(9) -0.0052(3) 0.07805(18) 0.0223(14) Uani 1 1 d . . .
C3 C 0.1885(9) 0.0016(3) 0.04006(18) 0.0242(15) Uani 1 1 d . . .
H3 H 0.2286 -0.0288 0.0254 0.029 Uiso 1 1 calc R . .
C4 C 0.1502(10) 0.0513(3) 0.02385(18) 0.0276(16) Uani 1 1 d . . .
H4 H 0.1699 0.0560 -0.0019 0.033 Uiso 1 1 calc R . .
N5 N 0.0850(7) 0.0942(2) 0.04352(14) 0.0196(12) Uani 1 1 d . . .
C6 C 0.0411(10) 0.1474(3) 0.02430(18) 0.0275(16) Uani 1 1 d . . .
H6A H -0.0844 0.1490 0.0197 0.033 Uiso 1 1 calc R . .
H6B H 0.1010 0.1491 0.0002 0.033 Uiso 1 1 calc R . .
C7 C 0.0946(10) 0.1964(3) 0.04797(18) 0.0260(15) Uani 1 1 d . . .
H7A H 0.0592 0.2318 0.0359 0.031 Uiso 1 1 calc R . .
H7B H 0.2214 0.1968 0.0505 0.031 Uiso 1 1 calc R . .
C8 C 0.0124(8) 0.1925(2) 0.08599(17) 0.0185(13) Uani 1 1 d . . .
C9 C -0.0374(9) 0.2400(3) 0.10575(19) 0.0262(15) Uani 1 1 d . . .
C10 C -0.1172(9) 0.2346(3) 0.14031(18) 0.0223(14) Uani 1 1 d . . .
C11 C -0.1423(9) 0.1815(3) 0.15483(17) 0.0211(14) Uani 1 1 d . . .
C12 C -0.2069(9) 0.1718(3) 0.19458(18) 0.0256(15) Uani 1 1 d . . .
H12A H -0.1818 0.2051 0.2101 0.031 Uiso 1 1 calc R . .
H12B H -0.3329 0.1656 0.1945 0.031 Uiso 1 1 calc R . .
C13 C -0.1165(10) 0.1213(3) 0.20980(17) 0.0261(15) Uani 1 1 d . . .
H13A H 0.0094 0.1276 0.2098 0.031 Uiso 1 1 calc R . .
H13B H -0.1539 0.1144 0.2356 0.031 Uiso 1 1 calc R . .
N14 N -0.1592(7) 0.0727(2) 0.18632(14) 0.0214(11) Uani 1 1 d . . .
C15 C -0.1947(9) 0.0227(3) 0.20299(18) 0.0235(15) Uani 1 1 d . . .
H15 H -0.1866 0.0197 0.2292 0.028 Uiso 1 1 calc R . .
C16 C -0.2405(9) -0.0223(3) 0.18322(17) 0.0236(14) Uani 1 1 d . . .
H16 H -0.2517 -0.0578 0.1949 0.028 Uiso 1 1 calc R . .
C17 C -0.2724(9) -0.0166(3) 0.14472(19) 0.0252(15) Uani 1 1 d . . .
C18 C -0.3355(11) -0.0611(3) 0.1226(2) 0.0330(17) Uani 1 1 d . . .
H18 H -0.3507 -0.0972 0.1333 0.040 Uiso 1 1 calc R . .
C19 C -0.3745(10) -0.0530(3) 0.0865(2) 0.0319(17) Uani 1 1 d . . .
H19 H -0.4126 -0.0837 0.0719 0.038 Uiso 1 1 calc R . .
C20 C -0.3592(9) 0.0004(3) 0.07038(18) 0.0259(15) Uani 1 1 d . . .
H20 H -0.3937 0.0061 0.0454 0.031 Uiso 1 1 calc R . .
C21 C -0.2944(8) 0.0444(3) 0.09064(18) 0.0202(14) Uani 1 1 d . . .
H21 H -0.2831 0.0802 0.0795 0.024 Uiso 1 1 calc R . .
C22 C -0.2445(9) 0.0365(2) 0.12805(17) 0.0208(14) Uani 1 1 d . . .
C23 C -0.1697(8) 0.0795(2) 0.14943(17) 0.0186(13) Uani 1 1 d . . .
C24 C -0.1047(8) 0.1333(2) 0.13441(16) 0.0171(13) Uani 1 1 d . . .
C25 C -0.0171(9) 0.1386(3) 0.10040(17) 0.0201(14) Uani 1 1 d . . .
C26 C 0.0627(8) 0.0904(3) 0.08116(16) 0.0186(13) Uani 1 1 d . . .
C27 C -0.0008(11) 0.2977(3) 0.0901(2) 0.0341(18) Uani 1 1 d . . .
H27A H 0.1004 0.2959 0.0740 0.051 Uiso 1 1 calc R . .
H27B H 0.0211 0.3239 0.1105 0.051 Uiso 1 1 calc R . .
H27C H -0.1004 0.3105 0.0758 0.051 Uiso 1 1 calc R . .
C28 C -0.1827(10) 0.2855(3) 0.1604(2) 0.0295(16) Uani 1 1 d . . .
H28A H -0.2615 0.2738 0.1801 0.044 Uiso 1 1 calc R . .
H28B H -0.2438 0.3098 0.1429 0.044 Uiso 1 1 calc R . .
H28C H -0.0856 0.3059 0.1712 0.044 Uiso 1 1 calc R . .
C29 C 0.1970(9) -0.0605(3) 0.09460(18) 0.0232(15) Uani 1 1 d . . .
H29 H 0.2471 -0.0884 0.0792 0.028 Uiso 1 1 calc R . .
C30 C 0.1588(10) -0.0755(3) 0.12915(19) 0.0277(15) Uani 1 1 d . . .
H30 H 0.1187 -0.0466 0.1451 0.033 Uiso 1 1 calc R . .
C31 C 0.1722(9) -0.1318(3) 0.14513(19) 0.0264(15) Uani 1 1 d . . .
C32 C 0.1058(9) -0.1795(3) 0.12639(19) 0.0275(15) Uani 1 1 d . . .
C33 C 0.0148(10) -0.1775(3) 0.0918(2) 0.0331(17) Uani 1 1 d . . .
H33 H -0.0087 -0.1422 0.0808 0.040 Uiso 1 1 calc R . .
C34 C -0.0381(11) -0.2248(3) 0.0746(2) 0.042(2) Uani 1 1 d . . .
H34 H -0.0935 -0.2221 0.0512 0.050 Uiso 1 1 calc R . .
C35 C -0.0132(12) -0.2782(3) 0.0905(2) 0.046(2) Uani 1 1 d . . .
H35 H -0.0544 -0.3108 0.0783 0.055 Uiso 1 1 calc R . .
C36 C 0.0706(12) -0.2825(3) 0.1235(2) 0.046(2) Uani 1 1 d . . .
H36 H 0.0911 -0.3186 0.1337 0.055 Uiso 1 1 calc R . .
C37 C 0.1280(10) -0.2344(3) 0.1430(2) 0.0333(17) Uani 1 1 d . . .
C38 C 0.2077(10) -0.2388(3) 0.1775(2) 0.0360(19) Uani 1 1 d . . .
H38 H 0.2208 -0.2749 0.1882 0.043 Uiso 1 1 calc R . .
C39 C 0.2681(9) -0.1928(3) 0.19647(19) 0.0286(16) Uani 1 1 d . . .
C40 C 0.3475(11) -0.1976(4) 0.2319(2) 0.042(2) Uani 1 1 d . . .
H40 H 0.3564 -0.2333 0.2433 0.051 Uiso 1 1 calc R . .
C41 C 0.4106(11) -0.1520(4) 0.2496(2) 0.046(2) Uani 1 1 d . . .
H41 H 0.4603 -0.1557 0.2735 0.055 Uiso 1 1 calc R . .
C42 C 0.4024(11) -0.0995(4) 0.2327(2) 0.0384(19) Uani 1 1 d . . .
H42 H 0.4519 -0.0681 0.2449 0.046 Uiso 1 1 calc R . .
C43 C 0.3258(10) -0.0921(3) 0.1994(2) 0.0324(17) Uani 1 1 d . . .
H43 H 0.3202 -0.0555 0.1891 0.039 Uiso 1 1 calc R . .
C44 C 0.2538(10) -0.1378(3) 0.17971(19) 0.0291(16) Uani 1 1 d . . .
I1 I 0.34267(7) 0.07473(2) 0.187784(12) 0.03078(14) Uani 1 1 d . . .
I2 I 0.54506(7) 0.12740(2) 0.002919(12) 0.03238(14) 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 C26 1.374(8) . ?
C1 C2 1.408(9) . ?
C1 H1 0.9500 . ?
C2 C3 1.390(9) . ?
C2 C29 1.466(9) . ?
C3 C4 1.357(9) . ?
C3 H3 0.9500 . ?
C4 N5 1.344(8) . ?
C4 H4 0.9500 . ?
N5 C26 1.374(8) . ?
N5 C6 1.488(8) . ?
C6 C7 1.507(9) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.518(9) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.394(9) . ?
C8 C25 1.407(8) . ?
C9 C10 1.400(10) . ?
C9 C27 1.514(9) . ?
C10 C11 1.386(9) . ?
C10 C28 1.502(9) . ?
C11 C24 1.397(8) . ?
C11 C12 1.539(9) . ?
C12 C13 1.499(9) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N14 1.475(8) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
N14 C23 1.345(8) . ?
N14 C15 1.366(8) . ?
C15 C16 1.337(9) . ?
C15 H15 0.9500 . ?
C16 C17 1.419(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.416(9) . ?
C17 C22 1.420(9) . ?
C18 C19 1.354(10) . ?
C18 H18 0.9500 . ?
C19 C20 1.406(9) . ?
C19 H19 0.9500 . ?
C20 C21 1.375(9) . ?
C20 H20 0.9500 . ?
C21 C22 1.418(9) . ?
C21 H21 0.9500 . ?
C22 C23 1.410(9) . ?
C23 C24 1.483(8) . ?
C24 C25 1.410(9) . ?
C25 C26 1.481(9) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.332(9) . ?
C29 H29 0.9500 . ?
C30 C31 1.467(9) . ?
C30 H30 0.9500 . ?
C31 C44 1.409(10) . ?
C31 C32 1.421(10) . ?
C32 C33 1.437(10) . ?
C32 C37 1.451(10) . ?
C33 C34 1.354(11) . ?
C33 H33 0.9500 . ?
C34 C35 1.411(12) . ?
C34 H34 0.9500 . ?
C35 C36 1.362(13) . ?
C35 H35 0.9500 . ?
C36 C37 1.420(11) . ?
C36 H36 0.9500 . ?
C37 C38 1.395(11) . ?
C38 C39 1.377(11) . ?
C38 H38 0.9500 . ?
C39 C40 1.426(11) . ?
C39 C44 1.449(9) . ?
C40 C41 1.354(12) . ?
C40 H40 0.9500 . ?
C41 C42 1.394(12) . ?
C41 H41 0.9500 . ?
C42 C43 1.353(10) . ?
C42 H42 0.9500 . ?
C43 C44 1.419(10) . ?
C43 H43 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C26 C1 C2 121.6(6) . . ?
C26 C1 H1 119.2 . . ?
C2 C1 H1 119.2 . . ?
C3 C2 C1 117.1(6) . . ?
C3 C2 C29 119.4(6) . . ?
C1 C2 C29 123.4(6) . . ?
C4 C3 C2 120.3(6) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
N5 C4 C3 121.3(6) . . ?
N5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C4 N5 C26 121.4(5) . . ?
C4 N5 C6 119.3(5) . . ?
C26 N5 C6 119.3(5) . . ?
N5 C6 C7 109.6(5) . . ?
N5 C6 H6A 109.8 . . ?
C7 C6 H6A 109.8 . . ?
N5 C6 H6B 109.8 . . ?
C7 C6 H6B 109.8 . . ?
H6A C6 H6B 108.2 . . ?
C6 C7 C8 110.5(5) . . ?
C6 C7 H7A 109.6 . . ?
C8 C7 H7A 109.6 . . ?
C6 C7 H7B 109.6 . . ?
C8 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
C9 C8 C25 120.6(6) . . ?
C9 C8 C7 122.0(5) . . ?
C25 C8 C7 117.3(5) . . ?
C8 C9 C10 120.3(6) . . ?
C8 C9 C27 119.7(6) . . ?
C10 C9 C27 119.9(6) . . ?
C11 C10 C9 118.9(6) . . ?
C11 C10 C28 120.6(6) . . ?
C9 C10 C28 120.4(6) . . ?
C10 C11 C24 121.6(6) . . ?
C10 C11 C12 122.4(6) . . ?
C24 C11 C12 116.0(5) . . ?
C13 C12 C11 108.0(5) . . ?
C13 C12 H12A 110.1 . . ?
C11 C12 H12A 110.1 . . ?
C13 C12 H12B 110.1 . . ?
C11 C12 H12B 110.1 . . ?
H12A C12 H12B 108.4 . . ?
N14 C13 C12 108.4(5) . . ?
N14 C13 H13A 110.0 . . ?
C12 C13 H13A 110.0 . . ?
N14 C13 H13B 110.0 . . ?
C12 C13 H13B 110.0 . . ?
H13A C13 H13B 108.4 . . ?
C23 N14 C15 122.0(6) . . ?
C23 N14 C13 119.2(5) . . ?
C15 N14 C13 118.7(5) . . ?
C16 C15 N14 121.3(6) . . ?
C16 C15 H15 119.3 . . ?
N14 C15 H15 119.3 . . ?
C15 C16 C17 119.6(6) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C18 C17 C16 122.8(6) . . ?
C18 C17 C22 118.9(6) . . ?
C16 C17 C22 118.3(6) . . ?
C19 C18 C17 120.9(6) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C18 C19 C20 120.7(6) . . ?
C18 C19 H19 119.6 . . ?
C20 C19 H19 119.6 . . ?
C21 C20 C19 120.1(6) . . ?
C21 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
C20 C21 C22 120.4(6) . . ?
C20 C21 H21 119.8 . . ?
C22 C21 H21 119.8 . . ?
C23 C22 C21 122.5(5) . . ?
C23 C22 C17 118.7(6) . . ?
C21 C22 C17 118.7(6) . . ?
N14 C23 C22 118.7(6) . . ?
N14 C23 C24 116.5(5) . . ?
C22 C23 C24 124.8(5) . . ?
C11 C24 C25 119.2(5) . . ?
C11 C24 C23 116.6(5) . . ?
C25 C24 C23 124.1(5) . . ?
C8 C25 C24 118.8(6) . . ?
C8 C25 C26 118.0(6) . . ?
C24 C25 C26 122.8(5) . . ?
C1 C26 N5 117.8(6) . . ?
C1 C26 C25 124.4(6) . . ?
N5 C26 C25 117.8(5) . . ?
C9 C27 H27A 109.5 . . ?
C9 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C9 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C10 C28 H28A 109.5 . . ?
C10 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C10 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 C2 126.2(6) . . ?
C30 C29 H29 116.9 . . ?
C2 C29 H29 116.9 . . ?
C29 C30 C31 126.7(6) . . ?
C29 C30 H30 116.6 . . ?
C31 C30 H30 116.6 . . ?
C44 C31 C32 120.3(6) . . ?
C44 C31 C30 118.3(6) . . ?
C32 C31 C30 121.4(6) . . ?
C31 C32 C33 124.5(6) . . ?
C31 C32 C37 118.9(6) . . ?
C33 C32 C37 116.6(7) . . ?
C34 C33 C32 121.4(7) . . ?
C34 C33 H33 119.3 . . ?
C32 C33 H33 119.3 . . ?
C33 C34 C35 121.7(8) . . ?
C33 C34 H34 119.1 . . ?
C35 C34 H34 119.1 . . ?
C36 C35 C34 119.3(8) . . ?
C36 C35 H35 120.3 . . ?
C34 C35 H35 120.3 . . ?
C35 C36 C37 121.6(8) . . ?
C35 C36 H36 119.2 . . ?
C37 C36 H36 119.2 . . ?
C38 C37 C36 121.5(7) . . ?
C38 C37 C32 119.3(7) . . ?
C36 C37 C32 119.2(7) . . ?
C39 C38 C37 122.5(7) . . ?
C39 C38 H38 118.8 . . ?
C37 C38 H38 118.8 . . ?
C38 C39 C40 122.1(7) . . ?
C38 C39 C44 119.1(7) . . ?
C40 C39 C44 118.7(7) . . ?
C41 C40 C39 121.1(7) . . ?
C41 C40 H40 119.4 . . ?
C39 C40 H40 119.4 . . ?
C40 C41 C42 119.9(8) . . ?
C40 C41 H41 120.1 . . ?
C42 C41 H41 120.1 . . ?
C43 C42 C41 121.8(8) . . ?
C43 C42 H42 119.1 . . ?
C41 C42 H42 119.1 . . ?
C42 C43 C44 121.2(7) . . ?
C42 C43 H43 119.4 . . ?
C44 C43 H43 119.4 . . ?
C31 C44 C43 123.0(6) . . ?
C31 C44 C39 119.8(7) . . ?
C43 C44 C39 117.2(7) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.613
_refine_diff_density_min         -1.381
_refine_diff_density_rms         0.145
#===END
####################################################################### 
# 
# 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_ls935_teply
_database_code_depnum_ccdc_archive 'CCDC 1008162'
_audit_update_record             
;
2014-06-12 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H44 N4, 2(ClO4)'
_chemical_formula_sum            'C42 H44 Cl2 N4 O8'
_chemical_formula_weight         803.71
_chemical_compound_source        'synthesized by the authors'
_chemical_absolute_configuration ad

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 42 21 2'
_space_group_name_Hall           'P 4n 2n'

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

_cell_length_a                   13.3242(4)
_cell_length_b                   13.3242(4)
_cell_length_c                   24.3016(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4314.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4342
_cell_measurement_theta_min      2.2685
_cell_measurement_theta_max      24.7018

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.443
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.132
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1688
_exptl_absorpt_coefficient_mu    0.204
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24485
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_sigmaI/netI    0.0638
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         26.05
_reflns_number_total             4285
_reflns_number_gt                2512
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'Bruker Instrument Service v2012.12.0.0'
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 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)+(0.2000P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(3)
_refine_ls_number_reflns         4285
_refine_ls_number_parameters     263
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.1721
_refine_ls_R_factor_gt           0.1219
_refine_ls_wR_factor_ref         0.3585
_refine_ls_wR_factor_gt          0.3303
_refine_ls_goodness_of_fit_ref   1.266
_refine_ls_restrained_S_all      1.283
_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
C1 C 0.1039(5) 0.5786(5) -0.0662(2) 0.0419(14) Uani 1 1 d . . .
H1 H 0.0549 0.6291 -0.0726 0.050 Uiso 1 1 calc R . .
C2 C 0.1653(4) 0.5857(4) -0.0192(3) 0.0425(14) Uani 1 1 d . . .
C3 C 0.2367(5) 0.5127(6) -0.0141(3) 0.0570(18) Uani 1 1 d . . .
H3 H 0.2833 0.5167 0.0154 0.068 Uiso 1 1 calc R . .
C4 C 0.2432(6) 0.4344(5) -0.0499(3) 0.0536(17) Uani 1 1 d . . .
H4 H 0.2922 0.3837 -0.0443 0.064 Uiso 1 1 calc R . .
N5 N 0.1804(4) 0.4283(4) -0.0934(2) 0.0463(13) Uani 1 1 d . . .
C6 C 0.1897(5) 0.3418(5) -0.1318(3) 0.0537(16) Uani 1 1 d . . .
H6A H 0.1218 0.3197 -0.1430 0.064 Uiso 1 1 calc R . .
H6B H 0.2224 0.2852 -0.1125 0.064 Uiso 1 1 calc R . .
C7 C 0.2493(5) 0.3675(6) -0.1821(3) 0.063(2) Uani 1 1 d . . .
H7A H 0.2387 0.3154 -0.2106 0.076 Uiso 1 1 calc R . .
H7B H 0.3216 0.3688 -0.1729 0.076 Uiso 1 1 calc R . .
C8 C 0.2170(6) 0.4710(7) -0.2049(3) 0.073(2) Uani 1 1 d . . .
H8A H 0.2488 0.5243 -0.1825 0.087 Uiso 1 1 calc R . .
H8B H 0.2422 0.4779 -0.2430 0.087 Uiso 1 1 calc R . .
C9 C 0.1060(5) 0.4868(6) -0.2049(3) 0.0582(18) Uani 1 1 d . . .
C10 C 0.0502(6) 0.4918(7) -0.2542(3) 0.0632(19) Uani 1 1 d . . .
H10 H 0.0840 0.4835 -0.2883 0.076 Uiso 1 1 calc R . .
C11 C 0.0518(4) 0.4927(5) -0.1553(2) 0.0429(14) Uani 1 1 d . . .
C12 C 0.1127(4) 0.5003(5) -0.1035(2) 0.0421(14) Uani 1 1 d . . .
C13 C 0.1514(5) 0.6701(5) 0.0169(2) 0.0498(16) Uani 1 1 d . . .
H13 H 0.1020 0.7186 0.0075 0.060 Uiso 1 1 calc R . .
C14 C 0.2052(5) 0.6844(5) 0.0638(3) 0.0494(16) Uani 1 1 d . . .
H14 H 0.2524 0.6341 0.0736 0.059 Uiso 1 1 calc R . .
C15 C 0.1961(5) 0.7701(5) 0.1002(3) 0.0473(16) Uani 1 1 d . . .
C16 C 0.2510(5) 0.7730(5) 0.1498(2) 0.0474(15) Uani 1 1 d . . .
H16 H 0.2924 0.7176 0.1593 0.057 Uiso 1 1 calc R . .
C17 C 0.2461(5) 0.8529(5) 0.1846(2) 0.0521(17) Uani 1 1 d . . .
H17 H 0.2842 0.8521 0.2177 0.062 Uiso 1 1 calc R . .
C18 C 0.1868(5) 0.9354(5) 0.1726(3) 0.0541(17) Uani 1 1 d . . .
C19 C 0.1357(5) 0.9359(6) 0.1234(3) 0.0600(18) Uani 1 1 d . . .
H19 H 0.0976 0.9934 0.1136 0.072 Uiso 1 1 calc R . .
C20 C 0.1383(5) 0.8546(5) 0.0880(3) 0.0520(16) Uani 1 1 d . . .
H20 H 0.1003 0.8564 0.0549 0.062 Uiso 1 1 calc R . .
C21 C 0.2248(7) 1.0150(7) 0.2628(3) 0.080(3) Uani 1 1 d . . .
H21A H 0.1874 0.9655 0.2845 0.121 Uiso 1 1 calc R . .
H21B H 0.2194 1.0810 0.2804 0.121 Uiso 1 1 calc R . .
H21C H 0.2956 0.9951 0.2609 0.121 Uiso 1 1 calc R . .
C22 C 0.1134(6) 1.1005(6) 0.1974(4) 0.074(2) Uani 1 1 d . . .
H22A H 0.1216 1.1246 0.1596 0.111 Uiso 1 1 calc R . .
H22B H 0.1264 1.1557 0.2231 0.111 Uiso 1 1 calc R . .
H22C H 0.0447 1.0759 0.2026 0.111 Uiso 1 1 calc R . .
N1 N 0.1835(5) 1.0199(5) 0.2077(2) 0.0708(18) Uani 1 1 d . . .
Cl1 Cl 0.0000 0.0000 0.38876(13) 0.0741(11) Uani 0.80 2 d SPD . .
O11 O 0.0185(12) 0.0783(12) 0.3541(6) 0.087(4) Uiso 0.40 1 d P . .
O21 O -0.0978(5) 0.0332(10) 0.4044(5) 0.071(4) Uiso 0.40 1 d PD . .
O31 O 0.0537(16) -0.0146(19) 0.4325(9) 0.137(7) Uiso 0.40 1 d P . .
O41 O 0.0492(12) 0.0940(6) 0.3817(7) 0.093(5) Uiso 0.40 1 d PD . .
Cl2 Cl 0.15519(18) 0.15519(18) 0.0000 0.0967(14) Uani 0.80 2 d SPD . .
O12 O 0.2257(14) 0.2257(14) 0.0000 0.105(10) Uiso 0.40 2 d SP . .
O22 O 0.1135(12) 0.1699(13) 0.0534(3) 0.092(5) Uiso 0.40 1 d PD . .
O32 O 0.2367(8) 0.0970(9) 0.0212(6) 0.080(4) Uiso 0.40 1 d PD . .
O42 O 0.189(4) 0.2559(13) 0.0035(16) 0.113(12) Uiso 0.20 1 d PD . .
O52 O 0.0793(17) 0.0793(17) 0.0000 0.122(9) Uiso 0.40 2 d SP . .
O62 O 0.0717(10) 0.1236(16) 0.0318(8) 0.050(5) Uiso 0.20 1 d PD . .
Cl3 Cl 0.1389(6) 0.4005(7) 0.1185(3) 0.083(3) Uiso 0.20 1 d PD . .
O13 O 0.1363(6) 0.3335(7) 0.1651(3) 0.037 Uiso 0.20 1 d PRD . .
O23 O 0.0629(6) 0.3702(7) 0.0798(3) 0.060(6) Uiso 0.20 1 d PRD . .
O33 O 0.1189(6) 0.5006(7) 0.1365(3) 0.066(6) Uiso 0.20 1 d PRD . .
O43 O 0.2357(6) 0.3954(7) 0.0935(3) 0.141(15) Uiso 0.20 1 d PRD . .


_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 C12 1.387(9) . ?
C1 C2 1.409(8) . ?
C1 H1 0.9500 . ?
C2 C3 1.366(9) . ?
C2 C13 1.439(9) . ?
C3 C4 1.361(9) . ?
C3 H3 0.9500 . ?
C4 N5 1.349(8) . ?
C4 H4 0.9500 . ?
N5 C12 1.340(8) . ?
N5 C6 1.489(8) . ?
C6 C7 1.497(9) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.548(11) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.494(11) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C11 1.407(8) . ?
C9 C10 1.412(9) . ?
C10 C10 1.355(15) 3_565 ?
C10 H10 0.9500 . ?
C11 C11 1.394(12) 3_565 ?
C11 C12 1.501(8) . ?
C13 C14 1.359(8) . ?
C13 H13 0.9500 . ?
C14 C15 1.449(9) . ?
C14 H14 0.9500 . ?
C15 C20 1.396(9) . ?
C15 C16 1.411(9) . ?
C16 C17 1.360(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.384(10) . ?
C17 H17 0.9500 . ?
C18 C19 1.377(10) . ?
C18 N1 1.413(9) . ?
C19 C20 1.384(10) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 N1 1.450(9) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 N1 1.445(11) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
Cl1 O31 1.30(2) 3 ?
Cl1 O31 1.30(2) . ?
Cl1 O11 1.364(15) . ?
Cl1 O11 1.364(15) 3 ?
Cl1 O41 1.424(3) . ?
Cl1 O41 1.424(3) 3 ?
Cl1 O21 1.428(3) 3 ?
Cl1 O21 1.428(3) . ?
O11 O41 0.814(18) . ?
O21 O31 0.94(2) 3 ?
O31 O21 0.94(2) 3 ?
O31 O31 1.48(4) 3 ?
Cl2 O12 1.33(3) . ?
Cl2 O62 1.418(3) . ?
Cl2 O62 1.418(3) 6 ?
Cl2 O42 1.419(3) . ?
Cl2 O42 1.419(3) 6 ?
Cl2 O22 1.425(3) 6 ?
Cl2 O22 1.425(3) . ?
Cl2 O52 1.43(3) . ?
Cl2 O32 1.431(3) . ?
Cl2 O32 1.431(3) 6 ?
O12 O42 0.64(5) . ?
O12 O42 0.64(5) 6 ?
O12 O32 1.80(2) . ?
O12 O32 1.80(2) 6 ?
O22 O62 0.98(2) . ?
O32 O42 1.39(4) 6 ?
O42 O42 1.27(9) 6 ?
O42 O32 1.39(4) 6 ?
O52 O62 0.98(2) . ?
O52 O62 0.98(2) 6 ?
Cl3 O43 1.4273 . ?
Cl3 O33 1.4284 . ?
Cl3 O23 1.4394 . ?
Cl3 O13 1.4416 . ?

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
C12 C1 C2 122.1(6) . . ?
C12 C1 H1 119.0 . . ?
C2 C1 H1 119.0 . . ?
C3 C2 C1 115.5(6) . . ?
C3 C2 C13 126.2(6) . . ?
C1 C2 C13 118.2(6) . . ?
C4 C3 C2 122.1(6) . . ?
C4 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
N5 C4 C3 120.5(6) . . ?
N5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C12 N5 C4 121.3(6) . . ?
C12 N5 C6 119.6(5) . . ?
C4 N5 C6 119.1(6) . . ?
N5 C6 C7 112.3(5) . . ?
N5 C6 H6A 109.1 . . ?
C7 C6 H6A 109.1 . . ?
N5 C6 H6B 109.1 . . ?
C7 C6 H6B 109.1 . . ?
H6A C6 H6B 107.9 . . ?
C6 C7 C8 110.3(6) . . ?
C6 C7 H7A 109.6 . . ?
C8 C7 H7A 109.6 . . ?
C6 C7 H7B 109.6 . . ?
C8 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
C9 C8 C7 113.6(6) . . ?
C9 C8 H8A 108.8 . . ?
C7 C8 H8A 108.8 . . ?
C9 C8 H8B 108.8 . . ?
C7 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
C11 C9 C10 117.0(6) . . ?
C11 C9 C8 121.1(7) . . ?
C10 C9 C8 121.9(6) . . ?
C10 C10 C9 121.8(4) 3_565 . ?
C10 C10 H10 119.1 3_565 . ?
C9 C10 H10 119.1 . . ?
C11 C11 C9 121.1(4) 3_565 . ?
C11 C11 C12 121.7(3) 3_565 . ?
C9 C11 C12 116.4(5) . . ?
N5 C12 C1 118.4(5) . . ?
N5 C12 C11 118.1(6) . . ?
C1 C12 C11 123.6(6) . . ?
C14 C13 C2 123.6(6) . . ?
C14 C13 H13 118.2 . . ?
C2 C13 H13 118.2 . . ?
C13 C14 C15 125.3(7) . . ?
C13 C14 H14 117.4 . . ?
C15 C14 H14 117.4 . . ?
C20 C15 C16 116.5(6) . . ?
C20 C15 C14 123.5(6) . . ?
C16 C15 C14 120.0(6) . . ?
C17 C16 C15 121.8(6) . . ?
C17 C16 H16 119.1 . . ?
C15 C16 H16 119.1 . . ?
C16 C17 C18 121.2(6) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C19 C18 C17 118.0(6) . . ?
C19 C18 N1 120.3(7) . . ?
C17 C18 N1 121.6(6) . . ?
C18 C19 C20 121.6(7) . . ?
C18 C19 H19 119.2 . . ?
C20 C19 H19 119.2 . . ?
C19 C20 C15 120.9(6) . . ?
C19 C20 H20 119.6 . . ?
C15 C20 H20 119.6 . . ?
N1 C21 H21A 109.5 . . ?
N1 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N1 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N1 C22 H22A 109.5 . . ?
N1 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N1 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 N1 C22 120.6(7) . . ?
C18 N1 C21 120.6(7) . . ?
C22 N1 C21 116.0(7) . . ?
O31 Cl1 O31 70(2) 3 . ?
O31 Cl1 O11 119.5(12) 3 . ?
O31 Cl1 O11 121.5(12) . . ?
O31 Cl1 O11 121.5(12) 3 3 ?
O31 Cl1 O11 119.5(12) . 3 ?
O11 Cl1 O11 103.6(14) . 3 ?
O31 Cl1 O41 102.7(13) 3 . ?
O31 Cl1 O41 88.7(13) . . ?
O11 Cl1 O41 33.9(8) . . ?
O11 Cl1 O41 133.0(12) 3 . ?
O31 Cl1 O41 88.7(13) 3 3 ?
O31 Cl1 O41 102.7(13) . 3 ?
O11 Cl1 O41 133.0(12) . 3 ?
O11 Cl1 O41 33.9(8) 3 3 ?
O41 Cl1 O41 166.2(15) . 3 ?
O31 Cl1 O21 109.4(13) 3 3 ?
O31 Cl1 O21 39.8(10) . 3 ?
O11 Cl1 O21 103.7(9) . 3 ?
O11 Cl1 O21 95.3(9) 3 3 ?
O41 Cl1 O21 83.4(9) . 3 ?
O41 Cl1 O21 100.3(9) 3 3 ?
O31 Cl1 O21 39.8(10) 3 . ?
O31 Cl1 O21 109.4(13) . . ?
O11 Cl1 O21 95.3(9) . . ?
O11 Cl1 O21 103.7(9) 3 . ?
O41 Cl1 O21 100.3(9) . . ?
O41 Cl1 O21 83.4(9) 3 . ?
O21 Cl1 O21 149.1(11) 3 . ?
O41 O11 Cl1 77.2(11) . . ?
O31 O21 Cl1 62.5(13) 3 . ?
O21 O31 Cl1 77.7(15) 3 . ?
O21 O31 O31 132.6(14) 3 3 ?
Cl1 O31 O31 55.1(10) . 3 ?
O11 O41 Cl1 69.0(11) . . ?
O12 Cl2 O62 139.8(10) . . ?
O12 Cl2 O62 139.8(10) . 6 ?
O62 Cl2 O62 80.4(19) . 6 ?
O12 Cl2 O42 27(2) . . ?
O62 Cl2 O42 120(2) . . ?
O62 Cl2 O42 150.4(19) 6 . ?
O12 Cl2 O42 27(2) . 6 ?
O62 Cl2 O42 150.4(19) . 6 ?
O62 Cl2 O42 120(2) 6 6 ?
O42 Cl2 O42 53(4) . 6 ?
O12 Cl2 O22 100.3(7) . 6 ?
O62 Cl2 O22 119.3(14) . 6 ?
O62 Cl2 O22 40.4(9) 6 6 ?
O42 Cl2 O22 112.3(18) . 6 ?
O42 Cl2 O22 86.5(18) 6 6 ?
O12 Cl2 O22 100.3(7) . . ?
O62 Cl2 O22 40.4(9) . . ?
O62 Cl2 O22 119.3(14) 6 . ?
O42 Cl2 O22 86.5(18) . . ?
O42 Cl2 O22 112.3(18) 6 . ?
O22 Cl2 O22 159.5(15) 6 . ?
O12 Cl2 O52 180.0(18) . . ?
O62 Cl2 O52 40.2(10) . . ?
O62 Cl2 O52 40.2(10) 6 . ?
O42 Cl2 O52 153(2) . . ?
O42 Cl2 O52 153(2) 6 . ?
O22 Cl2 O52 79.7(7) 6 . ?
O22 Cl2 O52 79.7(7) . . ?
O12 Cl2 O32 81.2(6) . . ?
O62 Cl2 O32 103.7(10) . . ?
O62 Cl2 O32 89.8(11) 6 . ?
O42 Cl2 O32 104(2) . . ?
O42 Cl2 O32 58.5(19) 6 . ?
O22 Cl2 O32 90.8(9) 6 . ?
O22 Cl2 O32 92.4(9) . . ?
O52 Cl2 O32 98.8(6) . . ?
O12 Cl2 O32 81.2(6) . 6 ?
O62 Cl2 O32 89.8(11) . 6 ?
O62 Cl2 O32 103.7(10) 6 6 ?
O42 Cl2 O32 58.5(19) . 6 ?
O42 Cl2 O32 104(2) 6 6 ?
O22 Cl2 O32 92.4(9) 6 6 ?
O22 Cl2 O32 90.8(9) . 6 ?
O52 Cl2 O32 98.8(6) . 6 ?
O32 Cl2 O32 162.3(13) . 6 ?
O42 O12 O42 169(7) . 6 ?
O42 O12 Cl2 85(3) . . ?
O42 O12 Cl2 85(3) 6 . ?
O42 O12 O32 129(4) . . ?
O42 O12 O32 42(3) 6 . ?
Cl2 O12 O32 51.9(8) . . ?
O42 O12 O32 42(3) . 6 ?
O42 O12 O32 129(4) 6 6 ?
Cl2 O12 O32 51.9(8) . 6 ?
O32 O12 O32 103.7(16) . 6 ?
O62 O22 Cl2 69.4(5) . . ?
O42 O32 Cl2 60.3(10) 6 . ?
O42 O32 O12 17.9(14) 6 . ?
Cl2 O32 O12 47.0(7) . . ?
O12 O42 O42 5(3) . 6 ?
O12 O42 O32 120(3) . 6 ?
O42 O42 O32 116(3) 6 6 ?
O12 O42 Cl2 69(2) . . ?
O42 O42 Cl2 63(2) 6 . ?
O32 O42 Cl2 61.2(10) 6 . ?
O62 O52 O62 139(4) . 6 ?
O62 O52 Cl2 69.3(18) . . ?
O62 O52 Cl2 69.3(18) 6 . ?
O52 O62 O22 138(2) . . ?
O52 O62 Cl2 70.5(19) . . ?
O22 O62 Cl2 70.2(5) . . ?
O43 Cl3 O33 110.1 . . ?
O43 Cl3 O23 110.1 . . ?
O33 Cl3 O23 109.3 . . ?
O43 Cl3 O13 109.0 . . ?
O33 Cl3 O13 109.5 . . ?
O23 Cl3 O13 108.8 . . ?

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
C12 C1 C2 C3 2.7(9) . . . . ?
C12 C1 C2 C13 179.5(5) . . . . ?
C1 C2 C3 C4 -4.6(9) . . . . ?
C13 C2 C3 C4 178.9(6) . . . . ?
C2 C3 C4 N5 2.4(11) . . . . ?
C3 C4 N5 C12 2.3(10) . . . . ?
C3 C4 N5 C6 179.8(6) . . . . ?
C12 N5 C6 C7 79.7(7) . . . . ?
C4 N5 C6 C7 -97.9(7) . . . . ?
N5 C6 C7 C8 -44.3(8) . . . . ?
C6 C7 C8 C9 -42.6(9) . . . . ?
C7 C8 C9 C11 65.9(10) . . . . ?
C7 C8 C9 C10 -111.1(9) . . . . ?
C11 C9 C10 C10 4.2(15) . . . 3_565 ?
C8 C9 C10 C10 -178.7(10) . . . 3_565 ?
C10 C9 C11 C11 -2.8(12) . . . 3_565 ?
C8 C9 C11 C11 -179.9(8) . . . 3_565 ?
C10 C9 C11 C12 -172.6(7) . . . . ?
C8 C9 C11 C12 10.3(10) . . . . ?
C4 N5 C12 C1 -4.1(9) . . . . ?
C6 N5 C12 C1 178.4(5) . . . . ?
C4 N5 C12 C11 174.7(5) . . . . ?
C6 N5 C12 C11 -2.9(8) . . . . ?
C2 C1 C12 N5 1.5(9) . . . . ?
C2 C1 C12 C11 -177.2(5) . . . . ?
C11 C11 C12 N5 133.8(8) 3_565 . . . ?
C9 C11 C12 N5 -56.4(8) . . . . ?
C11 C11 C12 C1 -47.5(10) 3_565 . . . ?
C9 C11 C12 C1 122.3(7) . . . . ?
C3 C2 C13 C14 -4.5(10) . . . . ?
C1 C2 C13 C14 179.1(6) . . . . ?
C2 C13 C14 C15 177.6(6) . . . . ?
C13 C14 C15 C20 -7.4(10) . . . . ?
C13 C14 C15 C16 175.4(6) . . . . ?
C20 C15 C16 C17 1.4(9) . . . . ?
C14 C15 C16 C17 178.7(6) . . . . ?
C15 C16 C17 C18 0.0(10) . . . . ?
C16 C17 C18 C19 -2.4(10) . . . . ?
C16 C17 C18 N1 -178.1(6) . . . . ?
C17 C18 C19 C20 3.5(10) . . . . ?
N1 C18 C19 C20 179.3(6) . . . . ?
C18 C19 C20 C15 -2.2(10) . . . . ?
C16 C15 C20 C19 -0.3(9) . . . . ?
C14 C15 C20 C19 -177.5(6) . . . . ?
C19 C18 N1 C22 10.9(10) . . . . ?
C17 C18 N1 C22 -173.5(6) . . . . ?
C19 C18 N1 C21 171.0(7) . . . . ?
C17 C18 N1 C21 -13.4(10) . . . . ?
O31 Cl1 O11 O41 67(2) 3 . . . ?
O31 Cl1 O11 O41 -16(3) . . . . ?
O11 Cl1 O11 O41 -154(2) 3 . . . ?
O41 Cl1 O11 O41 -173.5(9) 3 . . . ?
O21 Cl1 O11 O41 -55(2) 3 . . . ?
O21 Cl1 O11 O41 100.6(18) . . . . ?
O31 Cl1 O21 O31 -5(3) . . . 3 ?
O11 Cl1 O21 O31 -131(2) . . . 3 ?
O11 Cl1 O21 O31 123(2) 3 . . 3 ?
O41 Cl1 O21 O31 -98(2) . . . 3 ?
O41 Cl1 O21 O31 96(2) 3 . . 3 ?
O21 Cl1 O21 O31 -3.2(19) 3 . . 3 ?
O31 Cl1 O31 O21 175(3) 3 . . 3 ?
O11 Cl1 O31 O21 -72(2) . . . 3 ?
O11 Cl1 O31 O21 59(2) 3 . . 3 ?
O41 Cl1 O31 O21 -81.3(19) . . . 3 ?
O41 Cl1 O31 O21 90.9(19) 3 . . 3 ?
O21 Cl1 O31 O21 178.3(10) . . . 3 ?
O11 Cl1 O31 O31 112.9(16) . . . 3 ?
O11 Cl1 O31 O31 -115.5(16) 3 . . 3 ?
O41 Cl1 O31 O31 104.1(17) . . . 3 ?
O41 Cl1 O31 O31 -83.7(18) 3 . . 3 ?
O21 Cl1 O31 O31 -175(3) 3 . . 3 ?
O21 Cl1 O31 O31 4(2) . . . 3 ?
O31 Cl1 O41 O11 -125(2) 3 . . . ?
O31 Cl1 O41 O11 166(2) . . . . ?
O11 Cl1 O41 O11 36(3) 3 . . . ?
O41 Cl1 O41 O11 20.4(17) 3 . . . ?
O21 Cl1 O41 O11 126.9(19) 3 . . . ?
O21 Cl1 O41 O11 -84.1(18) . . . . ?
O62 Cl2 O12 O42 -50(4) . . . . ?
O62 Cl2 O12 O42 130(4) 6 . . . ?
O42 Cl2 O12 O42 180.0 6 . . . ?
O22 Cl2 O12 O42 120(4) 6 . . . ?
O22 Cl2 O12 O42 -60(4) . . . . ?
O52 Cl2 O12 O42 -172(4) . . . . ?
O32 Cl2 O12 O42 -151(4) . . . . ?
O32 Cl2 O12 O42 29(4) 6 . . . ?
O62 Cl2 O12 O42 130(4) . . . 6 ?
O62 Cl2 O12 O42 -50(4) 6 . . 6 ?
O42 Cl2 O12 O42 -180.0 . . . 6 ?
O22 Cl2 O12 O42 -60(4) 6 . . 6 ?
O22 Cl2 O12 O42 120(4) . . . 6 ?
O52 Cl2 O12 O42 8(4) . . . 6 ?
O32 Cl2 O12 O42 29(4) . . . 6 ?
O32 Cl2 O12 O42 -151(4) 6 . . 6 ?
O62 Cl2 O12 O32 100.9(14) . . . . ?
O62 Cl2 O12 O32 -79.1(14) 6 . . . ?
O42 Cl2 O12 O32 151(4) . . . . ?
O42 Cl2 O12 O32 -29(4) 6 . . . ?
O22 Cl2 O12 O32 -89.2(9) 6 . . . ?
O22 Cl2 O12 O32 90.8(9) . . . . ?
O52 Cl2 O12 O32 -21.4(6) . . . . ?
O32 Cl2 O12 O32 180.0 6 . . . ?
O62 Cl2 O12 O32 -79.1(14) . . . 6 ?
O62 Cl2 O12 O32 100.9(14) 6 . . 6 ?
O42 Cl2 O12 O32 -29(4) . . . 6 ?
O42 Cl2 O12 O32 151(4) 6 . . 6 ?
O22 Cl2 O12 O32 90.8(9) 6 . . 6 ?
O22 Cl2 O12 O32 -89.2(9) . . . 6 ?
O52 Cl2 O12 O32 158.6(6) . . . 6 ?
O32 Cl2 O12 O32 180.0 . . . 6 ?
O12 Cl2 O22 O62 170.0(16) . . . . ?
O62 Cl2 O22 O62 -17(3) 6 . . . ?
O42 Cl2 O22 O62 147(3) . . . . ?
O42 Cl2 O22 O62 -165(3) 6 . . . ?
O22 Cl2 O22 O62 -10.0(16) 6 . . . ?
O52 Cl2 O22 O62 -10.0(16) . . . . ?
O32 Cl2 O22 O62 -108.6(17) . . . . ?
O32 Cl2 O22 O62 88.8(18) 6 . . . ?
O12 Cl2 O32 O42 -15(2) . . . 6 ?
O62 Cl2 O32 O42 -154(2) . . . 6 ?
O62 Cl2 O32 O42 126(2) 6 . . 6 ?
O42 Cl2 O32 O42 -28(4) . . . 6 ?
O22 Cl2 O32 O42 85(2) 6 . . 6 ?
O22 Cl2 O32 O42 -115(2) . . . 6 ?
O52 Cl2 O32 O42 165(2) . . . 6 ?
O32 Cl2 O32 O42 -15(2) 6 . . 6 ?
O62 Cl2 O32 O12 -139.3(10) . . . . ?
O62 Cl2 O32 O12 140.7(10) 6 . . . ?
O42 Cl2 O32 O12 -13.0(17) . . . . ?
O42 Cl2 O32 O12 15(2) 6 . . . ?
O22 Cl2 O32 O12 100.3(7) 6 . . . ?
O22 Cl2 O32 O12 -100.0(8) . . . . ?
O52 Cl2 O32 O12 180.0 . . . . ?
O32 Cl2 O32 O12 0.013(1) 6 . . . ?
O42 O12 O32 O42 172(5) . . . 6 ?
Cl2 O12 O32 O42 134(5) . . . 6 ?
O32 O12 O32 O42 134(5) 6 . . 6 ?
O42 O12 O32 Cl2 38(5) . . . . ?
O42 O12 O32 Cl2 -134(5) 6 . . . ?
O32 O12 O32 Cl2 0.0 6 . . . ?
Cl2 O12 O42 O42 -0.028(18) . . . 6 ?
O32 O12 O42 O42 -29(3) . . . 6 ?
O32 O12 O42 O42 35(3) 6 . . 6 ?
O42 O12 O42 O32 -35(3) 6 . . 6 ?
Cl2 O12 O42 O32 -35(3) . . . 6 ?
O32 O12 O42 O32 -64(6) . . . 6 ?
O42 O12 O42 Cl2 0.03(2) 6 . . . ?
O32 O12 O42 Cl2 -29(3) . . . . ?
O32 O12 O42 Cl2 35(3) 6 . . . ?
O62 Cl2 O42 O12 145(3) . . . . ?
O62 Cl2 O42 O12 -87(6) 6 . . . ?
O42 Cl2 O42 O12 -0.003(2) 6 . . . ?
O22 Cl2 O42 O12 -67(4) 6 . . . ?
O22 Cl2 O42 O12 121(3) . . . . ?
O52 Cl2 O42 O12 180.0 . . . . ?
O32 Cl2 O42 O12 30(3) . . . . ?
O32 Cl2 O42 O12 -146(4) 6 . . . ?
O12 Cl2 O42 O42 0.003(3) . . . 6 ?
O62 Cl2 O42 O42 145(3) . . . 6 ?
O62 Cl2 O42 O42 -87(6) 6 . . 6 ?
O22 Cl2 O42 O42 -67(4) 6 . . 6 ?
O22 Cl2 O42 O42 121(3) . . . 6 ?
O52 Cl2 O42 O42 180.003(2) . . . 6 ?
O32 Cl2 O42 O42 30(3) . . . 6 ?
O32 Cl2 O42 O42 -146(4) 6 . . 6 ?
O12 Cl2 O42 O32 146(4) . . . 6 ?
O62 Cl2 O42 O32 -69.1(19) . . . 6 ?
O62 Cl2 O42 O32 59(5) 6 . . 6 ?
O42 Cl2 O42 O32 146(4) 6 . . 6 ?
O22 Cl2 O42 O32 78.5(19) 6 . . 6 ?
O22 Cl2 O42 O32 -93.0(14) . . . 6 ?
O52 Cl2 O42 O32 -34(4) . . . 6 ?
O32 Cl2 O42 O32 175.4(7) . . . 6 ?
O12 Cl2 O52 O62 122.3(13) . . . . ?
O62 Cl2 O52 O62 -180.0 6 . . . ?
O42 Cl2 O52 O62 -50(4) . . . . ?
O42 Cl2 O52 O62 130(4) 6 . . . ?
O22 Cl2 O52 O62 -169.9(15) 6 . . . ?
O22 Cl2 O52 O62 10.1(15) . . . . ?
O32 Cl2 O52 O62 100.9(14) . . . . ?
O32 Cl2 O52 O62 -79.1(14) 6 . . . ?
O12 Cl2 O52 O62 -57.7(13) . . . 6 ?
O62 Cl2 O52 O62 180.0 . . . 6 ?
O42 Cl2 O52 O62 130(4) . . . 6 ?
O42 Cl2 O52 O62 -50(4) 6 . . 6 ?
O22 Cl2 O52 O62 10.0(15) 6 . . 6 ?
O22 Cl2 O52 O62 -170.0(15) . . . 6 ?
O32 Cl2 O52 O62 -79.1(14) . . . 6 ?
O32 Cl2 O52 O62 100.9(14) 6 . . 6 ?
O62 O52 O62 O22 -22(3) 6 . . . ?
Cl2 O52 O62 O22 -22(3) . . . . ?
O62 O52 O62 Cl2 -0.009(3) 6 . . . ?
Cl2 O22 O62 O52 22(3) . . . . ?
O12 Cl2 O62 O52 180.000(2) . . . . ?
O62 Cl2 O62 O52 0.004(2) 6 . . . ?
O42 Cl2 O62 O52 157(2) . . . . ?
O42 Cl2 O62 O52 -136(4) 6 . . . ?
O22 Cl2 O62 O52 11.4(17) 6 . . . ?
O22 Cl2 O62 O52 -165(2) . . . . ?
O32 Cl2 O62 O52 -87.4(12) . . . . ?
O32 Cl2 O62 O52 104.0(12) 6 . . . ?
O12 Cl2 O62 O22 -15(2) . . . . ?
O62 Cl2 O62 O22 165(2) 6 . . . ?
O42 Cl2 O62 O22 -39(3) . . . . ?
O42 Cl2 O62 O22 28(5) 6 . . . ?
O22 Cl2 O62 O22 176.0(7) 6 . . . ?
O52 Cl2 O62 O22 165(2) . . . . ?
O32 Cl2 O62 O22 77.2(17) . . . . ?
O32 Cl2 O62 O22 -91.4(17) 6 . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.05
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.134
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.138


_vrf_PLAT430_ls935_teply         
;
PROBLEM:ALERT_2_A Short Inter D...A Contact O21..O43 .. 2.41 Ang.
RESPONSE: The both anions ClO4 are totaly disordered over more than
two positions, leaving no chance for meaningfull description.  
However only part of interest is hleguat cation without disorder. 
;
_vrf_RFACR01_ls935_teply         
;
PROBLEM:ALERT_3_B The value of the weighted R factor is > 0.35 
RESPONSE: The both anions ClO4 are totaly disordered over more than
two positions, leaving no chance for meaningfull description.  
However only part of interest is hleguat cation without disorder. 
;
_vrf_PLAT084_ls935_teply         
;
PROBLEM: ALERT_3_B High wR2 Value (i.e. > 0.25)  0.36 Why ?
RESPONSE: see above 
;

#===END
