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


data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Pradyut Ghosh'
_publ_contact_author_email       ICPG@IACS.RES.IN

_publ_section_title              
;
Ditopic recognition of solvated fluoride in a simple
tripodal amide receptor: cryatallographic proof of strong water***?
interaction
;
loop_
_publ_author_name
'Pradyut Ghosh'
'P. S. Lakshminarayanan'
'I. Ravikumar'

# Attachment 'FREE_LIGAND_FINAL.cif'


data_lakshpsl

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H15 F15 N4 O3'
_chemical_formula_weight         728.43

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'
F F 0.0171 0.0103 '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           MONOCLINIC
_symmetry_space_group_name_H-M   P2(1)/c

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                   16.963(3)
_cell_length_b                   13.596(2)
_cell_length_c                   12.654(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.632(2)
_cell_angle_gamma                90.00
_cell_volume                     2796.3(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       PLATE
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1456
_exptl_absorpt_coefficient_mu    0.181
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.9310
_exptl_absorpt_correction_T_max  0.9681
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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 CCD AREA DETECTOR'
_diffrn_measurement_method       'OMEGA SCAN'
_diffrn_detector_area_resol_mean 3
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17817
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.25
_diffrn_reflns_theta_max         21.04
_reflns_number_total             3013
_reflns_number_gt                2249
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER APEX II'
_computing_cell_refinement       'BRUKER APEX II'
_computing_data_reduction        'BRUKER AXS SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'BRUKER SHELXTL'
_computing_publication_material  'MERCURY 1.4'

_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)+(0.0590P)²+0.0871P] 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         3013
_refine_ls_number_parameters     442
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0359
_refine_ls_wR_factor_ref         0.0973
_refine_ls_wR_factor_gt          0.0846
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_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 0.5510(2) 0.2324(3) 0.1625(3) 0.0249(9) Uani 1 1 d . . .
H1A H 0.5659 0.3015 0.1693 0.030 Uiso 1 1 calc R . .
H1B H 0.5930 0.1974 0.1392 0.030 Uiso 1 1 calc R . .
C2 C 0.5486(2) 0.1938(2) 0.2732(3) 0.0217(9) Uani 1 1 d . . .
H2A H 0.5095 0.2318 0.2993 0.026 Uiso 1 1 calc R . .
H2B H 0.5304 0.1258 0.2658 0.026 Uiso 1 1 calc R . .
C3 C 0.6611(2) 0.2861(3) 0.3915(3) 0.0217(9) Uani 1 1 d . . .
C4 C 0.7513(2) 0.2887(2) 0.4518(3) 0.0185(9) Uani 1 1 d . . .
C5 C 0.7814(2) 0.3396(2) 0.5501(3) 0.0205(9) Uani 1 1 d . . .
C6 C 0.8640(2) 0.3531(3) 0.5996(3) 0.0253(9) Uani 1 1 d . . .
C7 C 0.9199(2) 0.3144(3) 0.5508(3) 0.0263(10) Uani 1 1 d . . .
C8 C 0.8930(2) 0.2617(3) 0.4549(3) 0.0265(10) Uani 1 1 d . . .
C9 C 0.8101(2) 0.2503(3) 0.4065(3) 0.0225(9) Uani 1 1 d . . .
C10 C 0.4699(2) 0.1300(2) 0.0150(3) 0.0247(9) Uani 1 1 d . . .
H10A H 0.5003 0.0793 0.0639 0.030 Uiso 1 1 calc R . .
H10B H 0.4974 0.1417 -0.0412 0.030 Uiso 1 1 calc R . .
C11 C 0.3837(2) 0.0935(3) -0.0394(3) 0.0217(9) Uani 1 1 d . . .
H11A H 0.3513 0.1469 -0.0809 0.026 Uiso 1 1 calc R . .
H11B H 0.3861 0.0417 -0.0911 0.026 Uiso 1 1 calc R . .
C12 C 0.2832(2) 0.1033(3) 0.0652(3) 0.0208(9) Uani 1 1 d . . .
C13 C 0.2459(2) 0.0481(2) 0.1426(3) 0.0190(9) Uani 1 1 d . . .
C14 C 0.1627(2) 0.0289(2) 0.1120(3) 0.0197(9) Uani 1 1 d . . .
C15 C 0.1256(2) -0.0227(3) 0.1778(3) 0.0245(9) Uani 1 1 d . . .
C16 C 0.1732(2) -0.0565(3) 0.2790(3) 0.0250(9) Uani 1 1 d . . .
C17 C 0.2558(2) -0.0381(3) 0.3117(3) 0.0244(9) Uani 1 1 d . . .
C18 C 0.2914(2) 0.0143(2) 0.2445(3) 0.0220(9) Uani 1 1 d . . .
C19 C 0.4520(2) 0.3081(2) 0.0085(3) 0.0237(9) Uani 1 1 d . . .
H19A H 0.4100 0.2916 -0.0591 0.028 Uiso 1 1 calc R . .
H19B H 0.5007 0.3291 -0.0110 0.028 Uiso 1 1 calc R . .
C20 C 0.4218(2) 0.3918(3) 0.0654(3) 0.0262(9) Uani 1 1 d . . .
H20A H 0.4626 0.4068 0.1346 0.031 Uiso 1 1 calc R . .
H20B H 0.4139 0.4501 0.0193 0.031 Uiso 1 1 calc R . .
C21 C 0.3096(2) 0.4236(3) 0.1430(3) 0.0245(9) Uani 1 1 d . . .
C22 C 0.2330(2) 0.3866(2) 0.1666(3) 0.0215(9) Uani 1 1 d . . .
C23 C 0.1604(2) 0.4396(3) 0.1356(3) 0.0281(10) Uani 1 1 d . . .
C24 C 0.0920(2) 0.4126(3) 0.1654(3) 0.0314(10) Uani 1 1 d . . .
C26 C 0.1652(2) 0.2749(3) 0.2609(3) 0.0275(10) Uani 1 1 d . . .
C25 C 0.0954(2) 0.3304(3) 0.2304(3) 0.0320(10) Uani 1 1 d . . .
C27 C 0.2323(2) 0.3028(3) 0.2283(3) 0.0235(9) Uani 1 1 d . . .
N1 N 0.47170(16) 0.22092(19) 0.0786(2) 0.0203(7) Uani 1 1 d . . .
N2 N 0.62955(17) 0.2003(2) 0.3525(2) 0.0228(7) Uani 1 1 d . . .
H2 H 0.6573 0.1474 0.3744 0.027 Uiso 1 1 calc R . .
N3 N 0.34323(17) 0.05606(19) 0.0391(2) 0.0207(7) Uani 1 1 d . . .
H3 H 0.3591 0.0004 0.0703 0.025 Uiso 1 1 calc R . .
N4 N 0.34457(17) 0.3651(2) 0.0862(2) 0.0244(7) Uani 1 1 d . . .
H4 H 0.3213 0.3103 0.0611 0.029 Uiso 1 1 calc R . .
F1 F 0.72834(12) 0.37888(14) 0.59987(15) 0.0283(5) Uani 1 1 d . . .
F2 F 0.89026(12) 0.40410(15) 0.69315(16) 0.0350(6) Uani 1 1 d . . .
F3 F 1.00039(12) 0.32929(15) 0.59652(17) 0.0379(6) Uani 1 1 d . . .
F4 F 0.94731(13) 0.22447(15) 0.40711(18) 0.0403(6) Uani 1 1 d . . .
F5 F 0.78605(12) 0.20456(14) 0.30818(17) 0.0337(6) Uani 1 1 d . . .
F6 F 0.11527(11) 0.05686(13) 0.01183(16) 0.0282(5) Uani 1 1 d . . .
F7 F 0.04496(12) -0.04257(14) 0.14404(16) 0.0341(6) Uani 1 1 d . . .
F8 F 0.13867(12) -0.10943(15) 0.34359(16) 0.0361(6) Uani 1 1 d . . .
F9 F 0.30186(12) -0.07215(15) 0.41016(16) 0.0364(6) Uani 1 1 d . . .
F10 F 0.37272(12) 0.03247(14) 0.28148(15) 0.0292(5) Uani 1 1 d . . .
F11 F 0.15601(12) 0.52018(14) 0.07214(17) 0.0377(6) Uani 1 1 d . . .
F12 F 0.02244(12) 0.46496(16) 0.13221(18) 0.0447(6) Uani 1 1 d . . .
F13 F 0.02946(14) 0.30491(16) 0.26181(19) 0.0469(7) Uani 1 1 d . . .
F14 F 0.16757(13) 0.19346(15) 0.32175(17) 0.0403(6) Uani 1 1 d . . .
F15 F 0.30131(12) 0.24744(13) 0.26201(15) 0.0288(5) Uani 1 1 d . . .
O1 O 0.62095(14) 0.36303(17) 0.37743(18) 0.0242(6) Uani 1 1 d . . .
O2 O 0.25597(14) 0.18470(17) 0.02869(19) 0.0236(6) Uani 1 1 d . . .
O3 O 0.33691(15) 0.50529(17) 0.1784(2) 0.0306(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
C1 N1 1.464(4) . ?
C1 C2 1.507(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.454(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 O1 1.234(4) . ?
C3 N2 1.318(4) . ?
C3 C4 1.502(5) . ?
C4 C9 1.386(5) . ?
C4 C5 1.386(5) . ?
C5 F1 1.348(4) . ?
C5 C6 1.374(5) . ?
C6 F2 1.333(4) . ?
C6 C7 1.376(5) . ?
C7 F3 1.338(4) . ?
C7 C8 1.369(5) . ?
C8 F4 1.338(4) . ?
C8 C9 1.373(5) . ?
C9 F5 1.346(4) . ?
C10 N1 1.470(4) . ?
C10 C11 1.510(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N3 1.453(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 O2 1.236(4) . ?
C12 N3 1.323(4) . ?
C12 C13 1.510(5) . ?
C13 C14 1.377(5) . ?
C13 C18 1.380(5) . ?
C14 F6 1.347(4) . ?
C14 C15 1.372(5) . ?
C15 F7 1.339(4) . ?
C15 C16 1.383(5) . ?
C16 F8 1.342(4) . ?
C16 C17 1.365(5) . ?
C17 F9 1.349(4) . ?
C17 C18 1.374(5) . ?
C18 F10 1.346(4) . ?
C19 N1 1.461(4) . ?
C19 C20 1.513(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 N4 1.454(4) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 O3 1.236(4) . ?
C21 N4 1.322(4) . ?
C21 C22 1.502(5) . ?
C22 C27 1.383(5) . ?
C22 C23 1.384(5) . ?
C23 F11 1.348(4) . ?
C23 C24 1.368(5) . ?
C24 F12 1.338(4) . ?
C24 C25 1.379(5) . ?
C26 F14 1.343(4) . ?
C26 C25 1.364(5) . ?
C26 C27 1.370(5) . ?
C25 F13 1.335(4) . ?
C27 F15 1.354(4) . ?
N2 H2 0.8600 . ?
N3 H3 0.8600 . ?
N4 H4 0.8600 . ?

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
N1 C1 C2 111.9(3) . . ?
N1 C1 H1A 109.2 . . ?
C2 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
N2 C2 C1 110.4(3) . . ?
N2 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
N2 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
O1 C3 N2 123.2(3) . . ?
O1 C3 C4 119.5(3) . . ?
N2 C3 C4 117.2(3) . . ?
C9 C4 C5 115.8(3) . . ?
C9 C4 C3 122.0(3) . . ?
C5 C4 C3 121.8(3) . . ?
F1 C5 C6 117.6(3) . . ?
F1 C5 C4 119.6(3) . . ?
C6 C5 C4 122.8(3) . . ?
F2 C6 C5 120.8(3) . . ?
F2 C6 C7 120.0(3) . . ?
C5 C6 C7 119.2(3) . . ?
F3 C7 C8 120.1(4) . . ?
F3 C7 C6 119.8(3) . . ?
C8 C7 C6 120.1(3) . . ?
F4 C8 C7 120.0(3) . . ?
F4 C8 C9 120.4(3) . . ?
C7 C8 C9 119.5(4) . . ?
F5 C9 C8 117.7(3) . . ?
F5 C9 C4 119.6(3) . . ?
C8 C9 C4 122.6(3) . . ?
N1 C10 C11 113.1(3) . . ?
N1 C10 H10A 109.0 . . ?
C11 C10 H10A 109.0 . . ?
N1 C10 H10B 109.0 . . ?
C11 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
N3 C11 C10 112.8(3) . . ?
N3 C11 H11A 109.0 . . ?
C10 C11 H11A 109.0 . . ?
N3 C11 H11B 109.0 . . ?
C10 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
O2 C12 N3 125.0(3) . . ?
O2 C12 C13 120.4(3) . . ?
N3 C12 C13 114.6(3) . . ?
C14 C13 C18 117.0(3) . . ?
C14 C13 C12 119.9(3) . . ?
C18 C13 C12 123.1(3) . . ?
F6 C14 C15 117.5(3) . . ?
F6 C14 C13 119.9(3) . . ?
C15 C14 C13 122.5(3) . . ?
F7 C15 C14 120.9(3) . . ?
F7 C15 C16 120.1(3) . . ?
C14 C15 C16 119.0(3) . . ?
F8 C16 C17 120.2(3) . . ?
F8 C16 C15 120.0(3) . . ?
C17 C16 C15 119.8(3) . . ?
F9 C17 C16 119.3(3) . . ?
F9 C17 C18 120.5(3) . . ?
C16 C17 C18 120.1(3) . . ?
F10 C18 C17 117.9(3) . . ?
F10 C18 C13 120.5(3) . . ?
C17 C18 C13 121.6(3) . . ?
N1 C19 C20 111.8(3) . . ?
N1 C19 H19A 109.3 . . ?
C20 C19 H19A 109.3 . . ?
N1 C19 H19B 109.3 . . ?
C20 C19 H19B 109.3 . . ?
H19A C19 H19B 107.9 . . ?
N4 C20 C19 110.1(3) . . ?
N4 C20 H20A 109.6 . . ?
C19 C20 H20A 109.6 . . ?
N4 C20 H20B 109.6 . . ?
C19 C20 H20B 109.6 . . ?
H20A C20 H20B 108.1 . . ?
O3 C21 N4 123.9(3) . . ?
O3 C21 C22 119.0(3) . . ?
N4 C21 C22 117.0(3) . . ?
C27 C22 C23 116.0(3) . . ?
C27 C22 C21 122.5(3) . . ?
C23 C22 C21 121.3(3) . . ?
F11 C23 C24 118.4(3) . . ?
F11 C23 C22 119.0(3) . . ?
C24 C23 C22 122.6(4) . . ?
F12 C24 C23 120.8(4) . . ?
F12 C24 C25 120.1(4) . . ?
C23 C24 C25 119.2(4) . . ?
F14 C26 C25 120.0(4) . . ?
F14 C26 C27 120.6(3) . . ?
C25 C26 C27 119.4(4) . . ?
F13 C25 C26 120.3(4) . . ?
F13 C25 C24 119.5(4) . . ?
C26 C25 C24 120.1(4) . . ?
F15 C27 C26 118.0(3) . . ?
F15 C27 C22 119.2(3) . . ?
C26 C27 C22 122.7(3) . . ?
C19 N1 C1 110.9(3) . . ?
C19 N1 C10 112.6(3) . . ?
C1 N1 C10 110.9(3) . . ?
C3 N2 C2 121.0(3) . . ?
C3 N2 H2 119.5 . . ?
C2 N2 H2 119.5 . . ?
C12 N3 C11 123.3(3) . . ?
C12 N3 H3 118.4 . . ?
C11 N3 H3 118.4 . . ?
C21 N4 C20 121.0(3) . . ?
C21 N4 H4 119.5 . . ?
C20 N4 H4 119.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2 O3 0.86 2.06 2.763(4) 138.9 2_645
N3 H3 O1 0.86 1.98 2.829(3) 170.2 2_645
C10 H10B O1 0.97 2.59 3.487(4) 154.6 4_565
C11 H11A F15 0.97 2.40 3.307(4) 155.0 4_565
C19 H19A F15 0.97 2.53 3.503(4) 178.4 4_565

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        21.04
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.167
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.050


_database_code_depnum_ccdc_archive 'CCDC 701762'

data_L1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H18 F12 N4 O3'
_chemical_formula_weight         674.45

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/c  '

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                   10.8910(17)
_cell_length_b                   17.196(3)
_cell_length_c                   14.431(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.322(4)
_cell_angle_gamma                90.00
_cell_volume                     2629.9(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2751
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      20.14

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1360
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.9932
_exptl_absorpt_correction_T_max  0.9966
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15142
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         20.21
_reflns_number_total             2531
_reflns_number_gt                1990
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'MERCURY 2.3'
_computing_publication_material  'ORTEP 3v.2'

_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)+(0.0775P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2531
_refine_ls_number_parameters     415
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0391
_refine_ls_wR_factor_ref         0.1123
_refine_ls_wR_factor_gt          0.1005
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_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
C4 C 0.5633(3) 0.39191(18) 0.3264(2) 0.0317(9) Uani 1 1 d . . .
C17 C 0.7513(4) 0.3374(2) 0.7646(2) 0.0374(9) Uani 1 1 d . . .
C16 C 0.6217(3) 0.33694(18) 0.7291(2) 0.0340(9) Uani 1 1 d . . .
C3 C 0.4255(3) 0.37690(18) 0.2822(3) 0.0328(9) Uani 1 1 d . . .
C15 C 0.5642(3) 0.38649(18) 0.6577(2) 0.0306(8) Uani 1 1 d . . .
C10 C 0.2548(3) 0.11974(19) 0.4689(2) 0.0402(9) Uani 1 1 d . . .
H10A H 0.2176 0.1141 0.5235 0.048 Uiso 1 1 calc R . .
H10B H 0.2344 0.0733 0.4303 0.048 Uiso 1 1 calc R . .
C20 C 0.6411(3) 0.43815(18) 0.6225(2) 0.0356(9) Uani 1 1 d . . .
H20 H 0.6056 0.4728 0.5743 0.043 Uiso 1 1 calc R . .
C9 C 0.6326(3) 0.35321(18) 0.4055(2) 0.0343(9) Uani 1 1 d . . .
C21 C 0.6677(3) 0.15082(19) 0.5696(2) 0.0358(9) Uani 1 1 d . . .
C24 C 0.6860(3) 0.06892(19) 0.4424(2) 0.0385(9) Uani 1 1 d . . .
H24 H 0.6502 0.0408 0.3878 0.046 Uiso 1 1 calc R . .
C8 C 0.7598(3) 0.3664(2) 0.4393(2) 0.0390(9) Uani 1 1 d . . .
C18 C 0.8242(3) 0.3876(2) 0.7284(2) 0.0387(9) Uani 1 1 d . . .
C19 C 0.7689(3) 0.43798(19) 0.6587(2) 0.0363(9) Uani 1 1 d . . .
C22 C 0.4683(3) 0.10900(18) 0.4463(2) 0.0352(9) Uani 1 1 d . . .
C23 C 0.6090(3) 0.10957(18) 0.4895(2) 0.0322(9) Uani 1 1 d . . .
C5 C 0.6277(3) 0.44393(19) 0.2812(2) 0.0378(9) Uani 1 1 d . . .
H5 H 0.5845 0.4701 0.2270 0.045 Uiso 1 1 calc R . .
C12 C 0.2104(3) 0.3437(2) 0.6026(2) 0.0389(9) Uani 1 1 d . . .
H12A H 0.1869 0.3891 0.5627 0.047 Uiso 1 1 calc R . .
H12B H 0.1634 0.3452 0.6521 0.047 Uiso 1 1 calc R . .
C2 C 0.2202(3) 0.3362(2) 0.3033(2) 0.0383(9) Uani 1 1 d . . .
H2A H 0.2085 0.2896 0.2643 0.046 Uiso 1 1 calc R . .
H2B H 0.1810 0.3793 0.2641 0.046 Uiso 1 1 calc R . .
C25 C 0.8142(4) 0.0698(2) 0.4753(3) 0.0404(9) Uani 1 1 d . . .
C26 C 0.8699(3) 0.1115(2) 0.5542(3) 0.0437(10) Uani 1 1 d . . .
C13 C 0.4259(3) 0.38546(18) 0.6067(2) 0.0327(9) Uani 1 1 d . . .
C6 C 0.7541(3) 0.4572(2) 0.3155(3) 0.0404(9) Uani 1 1 d . . .
C11 C 0.1725(3) 0.27100(19) 0.5423(2) 0.0361(9) Uani 1 1 d . . .
H11A H 0.2020 0.2258 0.5814 0.043 Uiso 1 1 calc R . .
H11B H 0.0811 0.2684 0.5246 0.043 Uiso 1 1 calc R . .
C27 C 0.7961(3) 0.1510(2) 0.6019(2) 0.0387(9) Uani 1 1 d . . .
C14 C 0.1941(3) 0.18900(18) 0.4108(2) 0.0380(9) Uani 1 1 d . . .
H14A H 0.2218 0.1896 0.3515 0.046 Uiso 1 1 calc R . .
H14B H 0.1035 0.1811 0.3948 0.046 Uiso 1 1 calc R . .
C1 C 0.1587(3) 0.32558(19) 0.3864(2) 0.0368(9) Uani 1 1 d . . .
H1A H 0.1604 0.3749 0.4193 0.044 Uiso 1 1 calc R . .
H1B H 0.0710 0.3114 0.3620 0.044 Uiso 1 1 calc R . .
C7 C 0.8196(3) 0.4191(2) 0.3950(3) 0.0418(9) Uani 1 1 d . . .
N3 N 0.3451(3) 0.34799(15) 0.64721(18) 0.0370(7) Uani 1 1 d . . .
H3 H 0.3729 0.3256 0.7013 0.044 Uiso 1 1 calc R . .
N4 N 0.3911(2) 0.12413(15) 0.50275(18) 0.0347(7) Uani 1 1 d . . .
H4 H 0.4225 0.1369 0.5610 0.042 Uiso 1 1 calc R . .
N2 N 0.3538(2) 0.35134(15) 0.33816(18) 0.0374(8) Uani 1 1 d . . .
H2 H 0.3876 0.3434 0.3974 0.045 Uiso 1 1 calc R . .
N1 N 0.2198(2) 0.26582(15) 0.45546(17) 0.0316(7) Uani 1 1 d . . .
F12 F 0.60020(18) 0.19347(11) 0.61900(13) 0.0485(6) Uani 1 1 d . . .
F4 F 0.57924(17) 0.29934(11) 0.45207(12) 0.0435(5) Uani 1 1 d . . .
F8 F 0.55554(18) 0.28437(10) 0.76812(12) 0.0444(5) Uani 1 1 d . . .
F5 F 0.84436(18) 0.48633(11) 0.62269(14) 0.0545(6) Uani 1 1 d . . .
F11 F 0.84995(19) 0.19280(12) 0.68033(14) 0.0600(6) Uani 1 1 d . . .
F6 F 0.95058(19) 0.38620(12) 0.76050(14) 0.0611(7) Uani 1 1 d . . .
F1 F 0.81670(19) 0.50753(11) 0.27126(14) 0.0579(6) Uani 1 1 d . . .
F3 F 0.82476(17) 0.32591(12) 0.51496(13) 0.0533(6) Uani 1 1 d . . .
F9 F 0.88878(19) 0.03135(12) 0.42710(14) 0.0603(6) Uani 1 1 d . . .
F7 F 0.80400(18) 0.28672(11) 0.83452(13) 0.0530(6) Uani 1 1 d . . .
F10 F 0.99688(19) 0.11338(12) 0.58566(15) 0.0623(6) Uani 1 1 d . . .
F2 F 0.94350(18) 0.43355(12) 0.42980(15) 0.0609(6) Uani 1 1 d . . .
O3 O 0.3936(2) 0.41931(12) 0.52996(16) 0.0392(6) Uani 1 1 d . . .
O2 O 0.4310(2) 0.09261(13) 0.36088(17) 0.0457(7) Uani 1 1 d . . .
O1 O 0.3833(2) 0.39056(15) 0.19680(17) 0.0506(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
C4 C9 1.385(4) . ?
C4 C5 1.389(4) . ?
C4 C3 1.511(4) . ?
C17 F7 1.356(4) . ?
C17 C18 1.357(5) . ?
C17 C16 1.386(5) . ?
C16 F8 1.357(4) . ?
C16 C15 1.373(4) . ?
C3 O1 1.234(4) . ?
C3 N2 1.322(4) . ?
C15 C20 1.395(4) . ?
C15 C13 1.516(5) . ?
C10 N4 1.454(4) . ?
C10 C14 1.517(4) . ?
C20 C19 1.369(5) . ?
C9 F4 1.352(4) . ?
C9 C8 1.378(5) . ?
C21 F12 1.352(4) . ?
C21 C27 1.369(5) . ?
C21 C23 1.381(4) . ?
C24 C25 1.367(5) . ?
C24 C23 1.385(4) . ?
C8 F3 1.349(4) . ?
C8 C7 1.359(5) . ?
C18 F6 1.347(4) . ?
C18 C19 1.359(4) . ?
C19 F5 1.354(4) . ?
C22 O2 1.238(4) . ?
C22 N4 1.324(4) . ?
C22 C23 1.515(4) . ?
C5 C6 1.371(5) . ?
C12 N3 1.461(4) . ?
C12 C11 1.525(4) . ?
C2 N2 1.449(4) . ?
C2 C1 1.513(4) . ?
C25 F9 1.357(4) . ?
C25 C26 1.363(5) . ?
C26 F10 1.353(4) . ?
C26 C27 1.355(5) . ?
C13 O3 1.229(3) . ?
C13 N3 1.330(4) . ?
C6 F1 1.350(4) . ?
C6 C7 1.370(5) . ?
C11 N1 1.464(4) . ?
C27 F11 1.355(4) . ?
C14 N1 1.468(4) . ?
C1 N1 1.479(4) . ?
C7 F2 1.350(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C9 C4 C5 117.3(3) . . ?
C9 C4 C3 124.4(3) . . ?
C5 C4 C3 118.1(3) . . ?
F7 C17 C18 120.7(3) . . ?
F7 C17 C16 119.5(3) . . ?
C18 C17 C16 119.8(3) . . ?
F8 C16 C15 122.1(3) . . ?
F8 C16 C17 116.3(3) . . ?
C15 C16 C17 121.6(3) . . ?
O1 C3 N2 122.5(3) . . ?
O1 C3 C4 119.6(3) . . ?
N2 C3 C4 117.9(3) . . ?
C16 C15 C20 117.4(3) . . ?
C16 C15 C13 126.0(3) . . ?
C20 C15 C13 116.4(3) . . ?
N4 C10 C14 115.2(3) . . ?
C19 C20 C15 120.2(3) . . ?
F4 C9 C8 116.7(3) . . ?
F4 C9 C4 121.6(3) . . ?
C8 C9 C4 121.7(3) . . ?
F12 C21 C27 117.1(3) . . ?
F12 C21 C23 121.1(3) . . ?
C27 C21 C23 121.7(3) . . ?
C25 C24 C23 120.6(3) . . ?
F3 C8 C7 120.4(3) . . ?
F3 C8 C9 119.9(3) . . ?
C7 C8 C9 119.6(3) . . ?
F6 C18 C17 119.9(3) . . ?
F6 C18 C19 120.6(3) . . ?
C17 C18 C19 119.5(3) . . ?
F5 C19 C18 118.1(3) . . ?
F5 C19 C20 120.4(3) . . ?
C18 C19 C20 121.5(3) . . ?
O2 C22 N4 123.2(3) . . ?
O2 C22 C23 118.7(3) . . ?
N4 C22 C23 118.0(3) . . ?
C21 C23 C24 117.0(3) . . ?
C21 C23 C22 125.3(3) . . ?
C24 C23 C22 117.6(3) . . ?
C6 C5 C4 120.8(3) . . ?
N3 C12 C11 113.9(3) . . ?
N2 C2 C1 109.8(3) . . ?
F9 C25 C26 118.7(3) . . ?
F9 C25 C24 120.0(3) . . ?
C26 C25 C24 121.2(3) . . ?
F10 C26 C27 119.8(3) . . ?
F10 C26 C25 121.1(3) . . ?
C27 C26 C25 119.1(3) . . ?
O3 C13 N3 123.0(3) . . ?
O3 C13 C15 118.5(3) . . ?
N3 C13 C15 118.5(3) . . ?
F1 C6 C7 118.7(3) . . ?
F1 C6 C5 120.7(3) . . ?
C7 C6 C5 120.6(3) . . ?
N1 C11 C12 115.9(3) . . ?
F11 C27 C26 119.8(3) . . ?
F11 C27 C21 119.8(3) . . ?
C26 C27 C21 120.3(3) . . ?
N1 C14 C10 116.7(3) . . ?
N1 C1 C2 113.9(3) . . ?
F2 C7 C8 119.6(3) . . ?
F2 C7 C6 120.4(3) . . ?
C8 C7 C6 119.9(3) . . ?
C13 N3 C12 122.0(3) . . ?
C22 N4 C10 121.8(3) . . ?
C3 N2 C2 122.3(3) . . ?
C11 N1 C14 111.2(2) . . ?
C11 N1 C1 110.0(2) . . ?
C14 N1 C1 108.6(2) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        20.21
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.051
_database_code_depnum_ccdc_archive 'CCDC 973404'

data_Complex1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H52 Cl3 F16 N5 O3'
_chemical_formula_weight         1109.26

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   11.8227(9)
_cell_length_b                   13.8754(10)
_cell_length_c                   15.4686(11)
_cell_angle_alpha                86.2310(10)
_cell_angle_beta                 76.2490(10)
_cell_angle_gamma                86.8740(10)
_cell_volume                     2457.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       PLATE
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1140
_exptl_absorpt_coefficient_mu    0.292
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.9174
_exptl_absorpt_correction_T_max  0.9770
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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 CCD AREA DETECTOR'
_diffrn_measurement_method       'OMEGA SCAN'
_diffrn_detector_area_resol_mean 3
_diffrn_reflns_number            21679
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.36
_diffrn_reflns_theta_max         23.94
_reflns_number_total             7667
_reflns_number_gt                5610
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER APEX II'
_computing_cell_refinement       'BRUKER APEX II'
_computing_data_reduction        'BRUKER AXS SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'MERCURY 2.3'
_computing_publication_material  'ORTEP 3v.2'

_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)+(0.0475P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7667
_refine_ls_number_parameters     644
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0390
_refine_ls_wR_factor_ref         0.0974
_refine_ls_wR_factor_gt          0.0866
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_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 0.3586(2) 0.30427(18) 0.36822(17) 0.0269(6) Uani 1 1 d . . .
H1A H 0.3387 0.3343 0.4250 0.032 Uiso 1 1 calc R . .
H1B H 0.2866 0.2882 0.3537 0.032 Uiso 1 1 calc R . .
C2 C 0.4229(2) 0.37497(18) 0.29683(18) 0.0273(6) Uani 1 1 d . . .
H2A H 0.4445 0.3445 0.2402 0.033 Uiso 1 1 calc R . .
H2B H 0.3721 0.4309 0.2904 0.033 Uiso 1 1 calc R . .
C3 C 0.5515(2) 0.49796(19) 0.31855(16) 0.0243(6) Uani 1 1 d . . .
C4 C 0.6560(2) 0.51694(17) 0.35353(16) 0.0219(6) Uani 1 1 d . . .
C5 C 0.6702(2) 0.48183(18) 0.43656(17) 0.0249(6) Uani 1 1 d . . .
C6 C 0.7619(2) 0.50561(19) 0.47024(17) 0.0288(6) Uani 1 1 d . . .
C7 C 0.8431(2) 0.56729(19) 0.42142(18) 0.0283(6) Uani 1 1 d . . .
C8 C 0.8324(2) 0.60369(18) 0.33893(18) 0.0267(6) Uani 1 1 d . . .
C9 C 0.7410(2) 0.57790(18) 0.30590(17) 0.0252(6) Uani 1 1 d . . .
C10 C 0.4254(2) 0.14766(18) 0.30828(17) 0.0240(6) Uani 1 1 d . . .
H10A H 0.4088 0.1827 0.2561 0.029 Uiso 1 1 calc R . .
H10B H 0.3631 0.1036 0.3318 0.029 Uiso 1 1 calc R . .
C11 C 0.5403(2) 0.09054(17) 0.28186(16) 0.0230(6) Uani 1 1 d . . .
H11A H 0.5612 0.0617 0.3351 0.028 Uiso 1 1 calc R . .
H11B H 0.5314 0.0387 0.2452 0.028 Uiso 1 1 calc R . .
C12 C 0.6623(2) 0.15553(18) 0.14465(17) 0.0244(6) Uani 1 1 d . . .
C13 C 0.7601(2) 0.22096(19) 0.10073(16) 0.0241(6) Uani 1 1 d . . .
C14 C 0.8697(2) 0.1835(2) 0.06330(17) 0.0304(7) Uani 1 1 d . . .
C15 C 0.9577(2) 0.2410(2) 0.01709(17) 0.0329(7) Uani 1 1 d . . .
C16 C 0.9366(2) 0.3380(2) 0.00624(18) 0.0354(7) Uani 1 1 d . . .
C17 C 0.8293(3) 0.3782(2) 0.04229(19) 0.0357(7) Uani 1 1 d . . .
C18 C 0.7428(2) 0.3195(2) 0.08958(18) 0.0298(7) Uani 1 1 d . . .
C19 C 0.4041(2) 0.17013(19) 0.46564(16) 0.0257(6) Uani 1 1 d . . .
H19A H 0.4242 0.1015 0.4625 0.031 Uiso 1 1 calc R . .
H19B H 0.3214 0.1777 0.4923 0.031 Uiso 1 1 calc R . .
C20 C 0.4725(2) 0.2148(2) 0.52374(17) 0.0278(6) Uani 1 1 d . . .
H20A H 0.4561 0.2841 0.5236 0.033 Uiso 1 1 calc R . .
H20B H 0.4473 0.1886 0.5846 0.033 Uiso 1 1 calc R . .
C21 C 0.6562(2) 0.13690(18) 0.53806(16) 0.0239(6) Uani 1 1 d . . .
C22 C 0.7860(2) 0.12766(18) 0.49913(16) 0.0220(6) Uani 1 1 d . . .
C23 C 0.8625(2) 0.16639(18) 0.54116(16) 0.0260(6) Uani 1 1 d . . .
C24 C 0.9818(2) 0.15500(19) 0.51140(18) 0.0288(7) Uani 1 1 d . . .
C25 C 1.0266(2) 0.10392(18) 0.43731(18) 0.0260(6) Uani 1 1 d . . .
C26 C 0.9535(2) 0.06392(18) 0.39406(17) 0.0258(6) Uani 1 1 d . . .
C27 C 0.8345(2) 0.07654(18) 0.42512(17) 0.0233(6) Uani 1 1 d . . .
C28 C 0.9502(2) 0.32945(18) 0.27631(16) 0.0244(6) Uani 1 1 d . . .
H28 H 0.8674 0.3160 0.2979 0.029 Uiso 1 1 calc R . .
C29 C 0.5450(2) 0.80318(18) 0.20428(16) 0.0215(6) Uani 1 1 d . . .
H29A H 0.5038 0.8403 0.2540 0.026 Uiso 1 1 calc R . .
H29B H 0.5569 0.7378 0.2277 0.026 Uiso 1 1 calc R . .
C30 C 0.6640(2) 0.84561(18) 0.16821(16) 0.0240(6) Uani 1 1 d . . .
H30A H 0.6554 0.9090 0.1395 0.029 Uiso 1 1 calc R . .
H30B H 0.7117 0.8043 0.1243 0.029 Uiso 1 1 calc R . .
C31 C 0.7225(2) 0.85371(19) 0.24535(17) 0.0259(6) Uani 1 1 d . . .
H31A H 0.6794 0.9019 0.2844 0.031 Uiso 1 1 calc R . .
H31B H 0.7182 0.7923 0.2795 0.031 Uiso 1 1 calc R . .
C32 C 0.8486(2) 0.8807(2) 0.2163(2) 0.0409(8) Uani 1 1 d . . .
H32A H 0.8920 0.8337 0.1773 0.061 Uiso 1 1 calc R . .
H32B H 0.8805 0.8824 0.2678 0.061 Uiso 1 1 calc R . .
H32C H 0.8534 0.9432 0.1855 0.061 Uiso 1 1 calc R . .
C33 C 0.4231(2) 0.90083(17) 0.11433(16) 0.0223(6) Uani 1 1 d . . .
H33A H 0.4895 0.9419 0.0978 0.027 Uiso 1 1 calc R . .
H33B H 0.3924 0.8970 0.0619 0.027 Uiso 1 1 calc R . .
C34 C 0.3304(2) 0.94939(17) 0.18536(16) 0.0239(6) Uani 1 1 d . . .
H34A H 0.3597 0.9545 0.2383 0.029 Uiso 1 1 calc R . .
H34B H 0.2620 0.9104 0.2015 0.029 Uiso 1 1 calc R . .
C35 C 0.2970(2) 1.04956(18) 0.15113(17) 0.0289(6) Uani 1 1 d . . .
H35A H 0.2528 1.0851 0.2010 0.035 Uiso 1 1 calc R . .
H35B H 0.3674 1.0839 0.1252 0.035 Uiso 1 1 calc R . .
C36 C 0.2250(3) 1.0471(2) 0.08162(18) 0.0381(7) Uani 1 1 d . . .
H36A H 0.2684 1.0125 0.0319 0.057 Uiso 1 1 calc R . .
H36B H 0.2075 1.1120 0.0617 0.057 Uiso 1 1 calc R . .
H36C H 0.1537 1.0154 0.1075 0.057 Uiso 1 1 calc R . .
C37 C 0.5296(2) 0.75619(17) 0.05348(15) 0.0223(6) Uani 1 1 d . . .
H37A H 0.4769 0.7593 0.0138 0.027 Uiso 1 1 calc R . .
H37B H 0.5946 0.7961 0.0258 0.027 Uiso 1 1 calc R . .
C38 C 0.5758(2) 0.65245(18) 0.06095(17) 0.0275(6) Uani 1 1 d . . .
H38A H 0.5154 0.6134 0.0982 0.033 Uiso 1 1 calc R . .
H38B H 0.6413 0.6502 0.0888 0.033 Uiso 1 1 calc R . .
C39 C 0.6144(2) 0.61126(19) -0.03111(17) 0.0296(6) Uani 1 1 d . . .
H39A H 0.6361 0.5433 -0.0240 0.035 Uiso 1 1 calc R . .
H39B H 0.5490 0.6160 -0.0592 0.035 Uiso 1 1 calc R . .
C40 C 0.7160(2) 0.6619(2) -0.09204(18) 0.0368(7) Uani 1 1 d . . .
H40A H 0.6928 0.7277 -0.1046 0.055 Uiso 1 1 calc R . .
H40B H 0.7399 0.6294 -0.1467 0.055 Uiso 1 1 calc R . .
H40C H 0.7798 0.6607 -0.0634 0.055 Uiso 1 1 calc R . .
C41 C 0.3656(2) 0.73837(18) 0.18844(16) 0.0217(6) Uani 1 1 d . . .
H41A H 0.3971 0.6764 0.2067 0.026 Uiso 1 1 calc R . .
H41B H 0.3255 0.7698 0.2420 0.026 Uiso 1 1 calc R . .
C42 C 0.2775(2) 0.72066(19) 0.13491(17) 0.0268(6) Uani 1 1 d . . .
H42A H 0.3114 0.6765 0.0888 0.032 Uiso 1 1 calc R . .
H42B H 0.2564 0.7811 0.1064 0.032 Uiso 1 1 calc R . .
C43 C 0.1690(2) 0.67775(19) 0.19632(17) 0.0274(6) Uani 1 1 d . . .
H43A H 0.1336 0.7239 0.2403 0.033 Uiso 1 1 calc R . .
H43B H 0.1131 0.6672 0.1614 0.033 Uiso 1 1 calc R . .
C44 C 0.1945(2) 0.5832(2) 0.2440(2) 0.0395(8) Uani 1 1 d . . .
H44A H 0.2326 0.5380 0.2010 0.059 Uiso 1 1 calc R . .
H44B H 0.1228 0.5576 0.2783 0.059 Uiso 1 1 calc R . .
H44C H 0.2442 0.5942 0.2829 0.059 Uiso 1 1 calc R . .
N1 N 0.42948(17) 0.21597(14) 0.37568(13) 0.0213(5) Uani 1 1 d . . .
N2 N 0.52666(17) 0.40553(15) 0.31993(14) 0.0254(5) Uani 1 1 d . . .
H2 H 0.5741 0.3621 0.3351 0.030 Uiso 1 1 calc R . .
N3 N 0.63354(17) 0.15136(14) 0.23277(13) 0.0218(5) Uani 1 1 d . . .
H3 H 0.6702 0.1848 0.2614 0.026 Uiso 1 1 calc R . .
N4 N 0.59745(17) 0.19590(15) 0.49238(13) 0.0237(5) Uani 1 1 d . . .
H4 H 0.6338 0.2237 0.4431 0.028 Uiso 1 1 calc R . .
N5 N 0.46633(17) 0.79957(14) 0.13981(12) 0.0194(5) Uani 1 1 d . . .
O1 O 0.49466(15) 0.56693(12) 0.29357(12) 0.0307(4) Uani 1 1 d . . .
O2 O 0.61680(16) 0.10997(13) 0.09651(12) 0.0346(5) Uani 1 1 d . . .
O3 O 0.61453(15) 0.09132(13) 0.60840(11) 0.0331(5) Uani 1 1 d . . .
F1 F 0.59112(12) 0.42337(10) 0.48791(9) 0.0324(4) Uani 1 1 d . . .
F2 F 0.77224(14) 0.46988(12) 0.55072(10) 0.0413(4) Uani 1 1 d . . .
F3 F 0.93374(13) 0.58989(11) 0.45342(11) 0.0424(4) Uani 1 1 d . . .
F4 F 0.91300(13) 0.66188(11) 0.28982(11) 0.0398(4) Uani 1 1 d . . .
F5 F 0.73713(12) 0.61209(10) 0.22314(9) 0.0318(4) Uani 1 1 d . . .
F6 F 0.89242(14) 0.08801(12) 0.07238(11) 0.0479(5) Uani 1 1 d . . .
F7 F 1.06460(14) 0.20263(14) -0.01601(11) 0.0531(5) Uani 1 1 d . . .
F8 F 1.02226(14) 0.39476(13) -0.03896(11) 0.0515(5) Uani 1 1 d . . .
F9 F 0.80875(15) 0.47374(12) 0.03308(13) 0.0582(5) Uani 1 1 d . . .
F10 F 0.63698(13) 0.36094(11) 0.12265(11) 0.0432(4) Uani 1 1 d . . .
F11 F 0.82075(13) 0.21824(11) 0.61317(10) 0.0395(4) Uani 1 1 d . . .
F12 F 1.05402(13) 0.19392(12) 0.55341(11) 0.0435(4) Uani 1 1 d . . .
F13 F 1.14265(12) 0.09238(11) 0.40689(10) 0.0377(4) Uani 1 1 d . . .
F14 F 0.99879(13) 0.01211(11) 0.32248(10) 0.0367(4) Uani 1 1 d . . .
F15 F 0.76500(12) 0.03541(11) 0.38193(10) 0.0348(4) Uani 1 1 d . . .
F16 F 0.70853(11) 0.27546(9) 0.33266(8) 0.0231(3) Uani 1 1 d . . .
Cl1 Cl 1.02485(6) 0.22689(5) 0.22493(4) 0.03354(18) Uani 1 1 d . . .
Cl2 Cl 1.00689(6) 0.35597(5) 0.36749(4) 0.03247(18) Uani 1 1 d . . .
Cl3 Cl 0.96463(6) 0.42994(5) 0.19850(4) 0.03123(18) 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 N1 1.460(3) . ?
C1 C2 1.517(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.448(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 O1 1.233(3) 1 ?
C3 O1 1.233(3) . ?
C3 N2 1.329(3) . ?
C3 C4 1.504(3) . ?
C4 C5 1.388(3) . ?
C4 C9 1.389(3) . ?
C5 F1 1.344(3) . ?
C5 C6 1.374(4) . ?
C6 F2 1.340(3) . ?
C6 C7 1.372(4) . ?
C7 F3 1.342(3) . ?
C7 C8 1.372(4) . ?
C8 F4 1.340(3) . ?
C8 C9 1.373(4) . ?
C9 F5 1.346(3) . ?
C10 N1 1.465(3) . ?
C10 C11 1.518(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N3 1.457(3) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 O2 1.238(3) . ?
C12 N3 1.322(3) . ?
C12 C13 1.511(3) . ?
C13 C14 1.376(4) . ?
C13 C18 1.378(4) . ?
C14 F6 1.343(3) . ?
C14 C15 1.375(4) . ?
C15 F7 1.341(3) . ?
C15 C16 1.362(4) . ?
C16 F8 1.346(3) . ?
C16 C17 1.364(4) . ?
C17 F9 1.339(3) . ?
C17 C18 1.378(4) . ?
C18 F10 1.346(3) . ?
C19 N1 1.462(3) . ?
C19 C20 1.523(3) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 N4 1.456(3) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 O3 1.231(3) . ?
C21 N4 1.322(3) . ?
C21 C22 1.511(3) . ?
C22 C27 1.376(3) . ?
C22 C23 1.381(3) . ?
C23 F11 1.344(3) . ?
C23 C24 1.379(4) . ?
C24 F12 1.343(3) . ?
C24 C25 1.369(4) . ?
C25 F13 1.345(3) . ?
C25 C26 1.371(4) . ?
C26 F14 1.345(3) . ?
C26 C27 1.380(3) . ?
C27 F15 1.345(3) . ?
C28 Cl1 1.765(3) . ?
C28 Cl2 1.766(3) . ?
C28 Cl3 1.769(2) . ?
C28 H28 0.9800 . ?
C29 C30 1.520(3) . ?
C29 N5 1.522(3) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.527(3) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 C32 1.511(3) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.519(3) . ?
C33 N5 1.528(3) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.520(3) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.525(4) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 C38 1.519(3) . ?
C37 N5 1.512(3) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 C39 1.527(3) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 C40 1.514(4) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 C42 1.515(3) . ?
C41 N5 1.518(3) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C43 1.527(3) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.514(4) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
N2 H2 0.8600 . ?
N3 H3 0.8600 . ?
N4 H4 0.8600 . ?
O1 O1 0.000(5) 1 ?
F16 F16 0.000(4) 1 ?

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
N1 C1 C2 111.2(2) . . ?
N1 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
N2 C2 C1 110.6(2) . . ?
N2 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
N2 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
O1 C3 O1 0.00(18) 1 . ?
O1 C3 N2 125.4(2) 1 . ?
O1 C3 N2 125.4(2) . . ?
O1 C3 C4 119.2(2) 1 . ?
O1 C3 C4 119.2(2) . . ?
N2 C3 C4 115.4(2) . . ?
C5 C4 C9 115.7(2) . . ?
C5 C4 C3 123.3(2) . . ?
C9 C4 C3 120.8(2) . . ?
F1 C5 C6 117.5(2) . . ?
F1 C5 C4 119.8(2) . . ?
C6 C5 C4 122.6(2) . . ?
F2 C6 C7 119.7(2) . . ?
F2 C6 C5 120.6(2) . . ?
C7 C6 C5 119.7(2) . . ?
F3 C7 C6 120.0(2) . . ?
F3 C7 C8 120.3(2) . . ?
C6 C7 C8 119.6(2) . . ?
F4 C8 C7 120.0(2) . . ?
F4 C8 C9 120.2(2) . . ?
C7 C8 C9 119.8(2) . . ?
F5 C9 C8 117.6(2) . . ?
F5 C9 C4 119.8(2) . . ?
C8 C9 C4 122.6(2) . . ?
N1 C10 C11 110.8(2) . . ?
N1 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
N3 C11 C10 111.7(2) . . ?
N3 C11 H11A 109.3 . . ?
C10 C11 H11A 109.3 . . ?
N3 C11 H11B 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 107.9 . . ?
O2 C12 N3 125.5(2) . . ?
O2 C12 C13 118.4(2) . . ?
N3 C12 C13 116.1(2) . . ?
C14 C13 C18 116.5(2) . . ?
C14 C13 C12 121.0(2) . . ?
C18 C13 C12 122.3(2) . . ?
F6 C14 C15 118.6(2) . . ?
F6 C14 C13 119.4(2) . . ?
C15 C14 C13 122.1(3) . . ?
F7 C15 C16 119.7(2) . . ?
F7 C15 C14 120.6(3) . . ?
C16 C15 C14 119.7(2) . . ?
F8 C16 C15 120.1(3) . . ?
F8 C16 C17 119.8(3) . . ?
C15 C16 C17 120.1(3) . . ?
F9 C17 C16 120.3(3) . . ?
F9 C17 C18 120.4(3) . . ?
C16 C17 C18 119.2(3) . . ?
F10 C18 C17 117.9(2) . . ?
F10 C18 C13 119.7(2) . . ?
C17 C18 C13 122.3(3) . . ?
N1 C19 C20 111.0(2) . . ?
N1 C19 H19A 109.4 . . ?
C20 C19 H19A 109.4 . . ?
N1 C19 H19B 109.4 . . ?
C20 C19 H19B 109.4 . . ?
H19A C19 H19B 108.0 . . ?
N4 C20 C19 111.7(2) . . ?
N4 C20 H20A 109.3 . . ?
C19 C20 H20A 109.3 . . ?
N4 C20 H20B 109.3 . . ?
C19 C20 H20B 109.3 . . ?
H20A C20 H20B 107.9 . . ?
O3 C21 N4 125.8(2) . . ?
O3 C21 C22 118.8(2) . . ?
N4 C21 C22 115.4(2) . . ?
C27 C22 C23 116.7(2) . . ?
C27 C22 C21 123.0(2) . . ?
C23 C22 C21 120.1(2) . . ?
F11 C23 C24 117.9(2) . . ?
F11 C23 C22 119.7(2) . . ?
C24 C23 C22 122.4(2) . . ?
F12 C24 C25 119.8(2) . . ?
F12 C24 C23 121.1(2) . . ?
C25 C24 C23 119.1(2) . . ?
F13 C25 C24 120.1(2) . . ?
F13 C25 C26 119.7(2) . . ?
C24 C25 C26 120.2(2) . . ?
F14 C26 C25 119.5(2) . . ?
F14 C26 C27 121.0(2) . . ?
C25 C26 C27 119.5(2) . . ?
F15 C27 C22 119.8(2) . . ?
F15 C27 C26 118.1(2) . . ?
C22 C27 C26 122.0(2) . . ?
Cl1 C28 Cl2 110.04(14) . . ?
Cl1 C28 Cl3 110.00(13) . . ?
Cl2 C28 Cl3 109.63(13) . . ?
Cl1 C28 H28 109.0 . . ?
Cl2 C28 H28 109.0 . . ?
Cl3 C28 H28 109.0 . . ?
C30 C29 N5 117.35(19) . . ?
C30 C29 H29A 108.0 . . ?
N5 C29 H29A 108.0 . . ?
C30 C29 H29B 108.0 . . ?
N5 C29 H29B 108.0 . . ?
H29A C29 H29B 107.2 . . ?
C29 C30 C31 108.9(2) . . ?
C29 C30 H30A 109.9 . . ?
C31 C30 H30A 109.9 . . ?
C29 C30 H30B 109.9 . . ?
C31 C30 H30B 109.9 . . ?
H30A C30 H30B 108.3 . . ?
C32 C31 C30 113.9(2) . . ?
C32 C31 H31A 108.8 . . ?
C30 C31 H31A 108.8 . . ?
C32 C31 H31B 108.8 . . ?
C30 C31 H31B 108.8 . . ?
H31A C31 H31B 107.7 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 N5 116.19(19) . . ?
C34 C33 H33A 108.2 . . ?
N5 C33 H33A 108.2 . . ?
C34 C33 H33B 108.2 . . ?
N5 C33 H33B 108.2 . . ?
H33A C33 H33B 107.4 . . ?
C33 C34 C35 110.3(2) . . ?
C33 C34 H34A 109.6 . . ?
C35 C34 H34A 109.6 . . ?
C33 C34 H34B 109.6 . . ?
C35 C34 H34B 109.6 . . ?
H34A C34 H34B 108.1 . . ?
C36 C35 C34 113.0(2) . . ?
C36 C35 H35A 109.0 . . ?
C34 C35 H35A 109.0 . . ?
C36 C35 H35B 109.0 . . ?
C34 C35 H35B 109.0 . . ?
H35A C35 H35B 107.8 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 N5 116.17(19) . . ?
C38 C37 H37A 108.2 . . ?
N5 C37 H37A 108.2 . . ?
C38 C37 H37B 108.2 . . ?
N5 C37 H37B 108.2 . . ?
H37A C37 H37B 107.4 . . ?
C37 C38 C39 110.5(2) . . ?
C37 C38 H38A 109.5 . . ?
C39 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C39 C38 H38B 109.5 . . ?
H38A C38 H38B 108.1 . . ?
C40 C39 C38 113.7(2) . . ?
C40 C39 H39A 108.8 . . ?
C38 C39 H39A 108.8 . . ?
C40 C39 H39B 108.8 . . ?
C38 C39 H39B 108.8 . . ?
H39A C39 H39B 107.7 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 N5 115.01(19) . . ?
C42 C41 H41A 108.5 . . ?
N5 C41 H41A 108.5 . . ?
C42 C41 H41B 108.5 . . ?
N5 C41 H41B 108.5 . . ?
H41A C41 H41B 107.5 . . ?
C41 C42 C43 109.8(2) . . ?
C41 C42 H42A 109.7 . . ?
C43 C42 H42A 109.7 . . ?
C41 C42 H42B 109.7 . . ?
C43 C42 H42B 109.7 . . ?
H42A C42 H42B 108.2 . . ?
C44 C43 C42 113.1(2) . . ?
C44 C43 H43A 109.0 . . ?
C42 C43 H43A 109.0 . . ?
C44 C43 H43B 109.0 . . ?
C42 C43 H43B 109.0 . . ?
H43A C43 H43B 107.8 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C1 N1 C19 112.93(19) . . ?
C1 N1 C10 112.75(19) . . ?
C19 N1 C10 111.97(19) . . ?
C3 N2 C2 122.6(2) . . ?
C3 N2 H2 118.7 . . ?
C2 N2 H2 118.7 . . ?
C12 N3 C11 120.6(2) . . ?
C12 N3 H3 119.7 . . ?
C11 N3 H3 119.7 . . ?
C21 N4 C20 121.4(2) . . ?
C21 N4 H4 119.3 . . ?
C20 N4 H4 119.3 . . ?
C37 N5 C41 111.00(18) . . ?
C37 N5 C29 111.86(18) . . ?
C41 N5 C29 105.45(17) . . ?
C37 N5 C33 106.15(17) . . ?
C41 N5 C33 111.16(18) . . ?
C29 N5 C33 111.32(18) . . ?
O1 O1 C3 0(10) 1 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C44 H44C F11 0.96 3.11 3.614(3) 114.1 2_666
C41 H41A O1 0.97 2.39 3.302(3) 156.2 1
C36 H36B F7 0.96 2.53 3.319(3) 139.2 1_465
C34 H34A O3 0.97 2.50 3.411(3) 156.5 2_666
C33 H33B O2 0.97 2.49 3.419(3) 161.0 2_665
C32 H32A F7 0.96 2.50 3.290(3) 139.0 2_765
C29 H29A O3 0.97 2.47 3.429(3) 170.4 2_666
C29 H29B O1 0.97 2.59 3.498(3) 155.6 1
C28 H28 F16 0.98 1.93 2.906(3) 173.1 1
N4 H4 F16 0.86 1.84 2.703(2) 175.4 1
N3 H3 F16 0.86 1.87 2.703(2) 163.7 1
N2 H2 F16 0.86 1.93 2.766(2) 162.2 1

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        23.94
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.052
_database_code_depnum_ccdc_archive 'CCDC 701764'

data_Complex2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H52 Cl4 F15 N5 O3'
_chemical_formula_weight         1125.71

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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                   14.4149(8)
_cell_length_b                   16.8287(10)
_cell_length_c                   22.6106(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.373(2)
_cell_angle_gamma                90.00
_cell_volume                     5377.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2312
_exptl_absorpt_coefficient_mu    0.314
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.8848
_exptl_absorpt_correction_T_max  0.9753
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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 CCD AREA DETECTOR'
_diffrn_measurement_method       'OMEGA SCAN'
_diffrn_detector_area_resol_mean 3
_diffrn_reflns_number            40806
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         22.82
_reflns_number_total             7147
_reflns_number_gt                5365
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER APEX II'
_computing_cell_refinement       'BRUKER APEX II'
_computing_data_reduction        'BRUKER AXS SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'MERCURY 2.3'
_computing_publication_material  'ORTEP 3v.2'

_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. 
;
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 0.500 0.500 0.500 139 54 ' '
2 0.500 1.000 0.000 139 54 ' '
_platon_squeeze_details          
;
The unit cell contains one disordered chloroform molecules which have been treated as a diffuse contribution to the overall scatterin without 
specific atom positions by SQUEEZE/PLATON.
;
_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)+(0.1917P)²+16.4231P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7147
_refine_ls_number_parameters     634
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_gt           0.0987
_refine_ls_wR_factor_ref         0.3073
_refine_ls_wR_factor_gt          0.2871
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_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
F14 F 1.0359(4) 0.2340(3) 0.29780(19) 0.1039(18) Uani 1 1 d . . .
F13 F 1.0794(3) 0.3879(3) 0.3017(2) 0.0943(16) Uani 1 1 d . . .
F10 F 0.8152(3) 0.6239(3) 0.1894(2) 0.0763(12) Uani 1 1 d . . .
F9 F 0.7980(5) 0.6349(3) 0.3052(2) 0.0983(16) Uani 1 1 d . . .
F8 F 0.6438(5) 0.5713(4) 0.3398(2) 0.123(2) Uani 1 1 d . . .
F7 F 0.5100(4) 0.4941(3) 0.2589(2) 0.0962(16) Uani 1 1 d . . .
F6 F 0.5277(3) 0.4841(3) 0.1430(2) 0.0702(12) Uani 1 1 d . . .
F5 F 0.4520(3) 0.2465(3) 0.2261(2) 0.0898(16) Uani 1 1 d . . .
F4 F 0.5454(3) 0.1853(3) 0.33192(18) 0.0834(14) Uani 1 1 d . . .
F3 F 0.7056(3) 0.1011(2) 0.33513(17) 0.0653(11) Uani 1 1 d . . .
F2 F 0.7705(3) 0.0749(3) 0.2323(2) 0.0837(14) Uani 1 1 d . . .
F1 F 0.6789(3) 0.1361(3) 0.12716(18) 0.0782(13) Uani 1 1 d . . .
Cl1 Cl 0.74060(11) 0.34813(9) 0.17911(6) 0.0482(5) Uani 1 1 d . . .
N1 N 0.6473(4) 0.3432(4) 0.0020(2) 0.0549(14) Uani 1 1 d . . .
C19 C 0.7128(4) 0.2953(4) -0.0261(3) 0.0525(16) Uani 1 1 d . . .
H19A H 0.7642 0.3288 -0.0334 0.063 Uiso 1 1 calc R . .
H19B H 0.6794 0.2753 -0.0646 0.063 Uiso 1 1 calc R . .
C20 C 0.7535(4) 0.2254(4) 0.0141(3) 0.0476(15) Uani 1 1 d . . .
H20A H 0.7022 0.1929 0.0227 0.057 Uiso 1 1 calc R . .
H20B H 0.7919 0.1927 -0.0070 0.057 Uiso 1 1 calc R . .
N4 N 0.8104(3) 0.2536(3) 0.0697(2) 0.0425(12) Uani 1 1 d . . .
H4 H 0.7826 0.2752 0.0960 0.051 Uiso 1 1 calc R . .
C21 C 0.9039(4) 0.2474(3) 0.0820(2) 0.0384(13) Uani 1 1 d . . .
O3 O 0.9525(3) 0.2150(3) 0.05035(18) 0.0490(10) Uani 1 1 d . . .
C22 C 0.9515(4) 0.2848(3) 0.1414(3) 0.0399(14) Uani 1 1 d . . .
C23 C 0.9729(4) 0.2426(3) 0.1938(3) 0.0461(15) Uani 1 1 d . . .
C24 C 1.0160(5) 0.2777(5) 0.2470(3) 0.0548(18) Uani 1 1 d . . .
C25 C 1.0364(5) 0.3552(4) 0.2495(3) 0.0593(18) Uani 1 1 d . . .
C26 C 1.0134(8) 0.3988(5) 0.1997(4) 0.095(3) Uani 1 1 d . . .
C27 C 0.9733(6) 0.3631(4) 0.1465(3) 0.073(2) Uani 1 1 d . . .
C10 C 0.6466(6) 0.4267(5) -0.0176(3) 0.073(2) Uani 1 1 d . . .
H10A H 0.5869 0.4508 -0.0139 0.087 Uiso 1 1 calc R . .
H10B H 0.6511 0.4283 -0.0599 0.087 Uiso 1 1 calc R . .
C11 C 0.7266(6) 0.4745(5) 0.0185(3) 0.067(2) Uani 1 1 d . . .
H11A H 0.7860 0.4475 0.0185 0.080 Uiso 1 1 calc R . .
H11B H 0.7291 0.5260 -0.0003 0.080 Uiso 1 1 calc R . .
N3 N 0.7151(4) 0.4854(3) 0.0801(3) 0.0631(16) Uani 1 1 d . . .
H3 H 0.7311 0.4476 0.1056 0.076 Uiso 1 1 calc R . .
C12 C 0.6809(4) 0.5511(4) 0.0981(3) 0.0525(17) Uani 1 1 d . . .
O2 O 0.6593(4) 0.6106(3) 0.0665(2) 0.0694(14) Uani 1 1 d . . .
C13 C 0.6724(5) 0.5542(3) 0.1637(3) 0.0487(16) Uani 1 1 d . . .
C14 C 0.7394(5) 0.5914(4) 0.2064(3) 0.0571(18) Uani 1 1 d . . .
C15 C 0.7303(7) 0.5979(4) 0.2643(4) 0.071(2) Uani 1 1 d . . .
C16 C 0.6540(8) 0.5653(5) 0.2823(4) 0.078(2) Uani 1 1 d . . .
C17 C 0.5848(6) 0.5263(5) 0.2423(4) 0.072(2) Uani 1 1 d . . .
C18 C 0.5958(5) 0.5212(4) 0.1830(3) 0.0541(17) Uani 1 1 d . . .
C1 C 0.5522(5) 0.3090(6) -0.0085(3) 0.067(2) Uani 1 1 d . . .
H1A H 0.5564 0.2516 -0.0105 0.080 Uiso 1 1 calc R . .
H1B H 0.5163 0.3279 -0.0468 0.080 Uiso 1 1 calc R . .
C2 C 0.5017(5) 0.3321(5) 0.0417(3) 0.068(2) Uani 1 1 d . . .
H2A H 0.5053 0.3893 0.0472 0.081 Uiso 1 1 calc R . .
H2B H 0.4354 0.3177 0.0302 0.081 Uiso 1 1 calc R . .
N2 N 0.5419(4) 0.2938(4) 0.0980(2) 0.0590(15) Uani 1 1 d . . .
H2 H 0.5886 0.3163 0.1216 0.071 Uiso 1 1 calc R . .
C3 C 0.5099(5) 0.2255(4) 0.1146(3) 0.0576(18) Uani 1 1 d . . .
C4 C 0.5641(5) 0.1935(4) 0.1739(3) 0.0518(16) Uani 1 1 d . . .
C5 C 0.5323(5) 0.2046(4) 0.2269(3) 0.0611(19) Uani 1 1 d . . .
C6 C 0.5790(5) 0.1740(4) 0.2812(3) 0.0547(17) Uani 1 1 d . . .
C7 C 0.6601(5) 0.1317(4) 0.2824(3) 0.0504(16) Uani 1 1 d . . .
C8 C 0.6925(5) 0.1181(4) 0.2309(3) 0.0552(17) Uani 1 1 d . . .
C9 C 0.6446(5) 0.1490(4) 0.1773(3) 0.0542(17) Uani 1 1 d . . .
N5 N 0.1748(4) 0.2828(3) 0.4851(2) 0.0470(13) Uani 1 1 d . . .
C41 C 0.1153(5) 0.3588(4) 0.4710(4) 0.064(2) Uani 1 1 d . . .
H41A H 0.1055 0.3689 0.4280 0.077 Uiso 1 1 calc R . .
H41B H 0.0538 0.3496 0.4809 0.077 Uiso 1 1 calc R . .
C42 C 0.1582(7) 0.4316(4) 0.5040(4) 0.080(3) Uani 1 1 d . . .
H42A H 0.2257 0.4326 0.5048 0.096 Uiso 1 1 calc R . .
H42B H 0.1490 0.4300 0.5454 0.096 Uiso 1 1 calc R . .
C43 C 0.1114(8) 0.5080(5) 0.4723(6) 0.114(4) Uani 1 1 d . . .
H43A H 0.0433 0.5011 0.4647 0.137 Uiso 1 1 calc R . .
H43B H 0.1267 0.5523 0.5000 0.137 Uiso 1 1 calc R . .
C44 C 0.1387(7) 0.5287(5) 0.4161(5) 0.091(3) Uani 1 1 d . . .
H44A H 0.2043 0.5435 0.4238 0.136 Uiso 1 1 calc R . .
H44B H 0.1010 0.5726 0.3979 0.136 Uiso 1 1 calc R . .
H44C H 0.1289 0.4839 0.3894 0.136 Uiso 1 1 calc R . .
C37 C 0.1854(5) 0.2661(4) 0.5506(3) 0.0506(16) Uani 1 1 d . . .
H37A H 0.2236 0.3077 0.5731 0.061 Uiso 1 1 calc R . .
H37B H 0.1234 0.2681 0.5612 0.061 Uiso 1 1 calc R . .
C38 C 0.2295(6) 0.1879(4) 0.5698(3) 0.0657(19) Uani 1 1 d . . .
H38A H 0.2903 0.1841 0.5577 0.079 Uiso 1 1 calc R . .
H38B H 0.1895 0.1455 0.5499 0.079 Uiso 1 1 calc R . .
C39 C 0.2433(6) 0.1778(5) 0.6391(4) 0.074(2) Uani 1 1 d . . .
H39A H 0.2851 0.2191 0.6591 0.089 Uiso 1 1 calc R . .
H39B H 0.1829 0.1831 0.6515 0.089 Uiso 1 1 calc R . .
C40 C 0.2851(7) 0.0975(4) 0.6573(3) 0.076(2) Uani 1 1 d . . .
H40A H 0.2467 0.0570 0.6346 0.114 Uiso 1 1 calc R . .
H40B H 0.2873 0.0893 0.6996 0.114 Uiso 1 1 calc R . .
H40C H 0.3480 0.0948 0.6494 0.114 Uiso 1 1 calc R . .
C29 C 0.2681(5) 0.2900(4) 0.4665(3) 0.0545(17) Uani 1 1 d . . .
H29A H 0.2980 0.2381 0.4698 0.065 Uiso 1 1 calc R . .
H29B H 0.3081 0.3251 0.4946 0.065 Uiso 1 1 calc R . .
C30 C 0.2642(7) 0.3209(5) 0.4035(3) 0.077(3) Uani 1 1 d . . .
H30A H 0.2404 0.3749 0.3999 0.093 Uiso 1 1 calc R . .
H30B H 0.2229 0.2880 0.3743 0.093 Uiso 1 1 calc R . .
F15 F 0.9523(5) 0.1654(2) 0.1930(2) 0.1028(19) Uani 1 1 d . . .
F11 F 0.9508(6) 0.4086(3) 0.0971(2) 0.169(4) Uani 1 1 d . . .
F12 F 1.0339(8) 0.4767(4) 0.2020(3) 0.205(5) Uani 1 1 d . . .
O1 O 0.4450(5) 0.1899(3) 0.0858(3) 0.097(2) Uani 1 1 d . . .
C31 C 0.3719(8) 0.3179(7) 0.3918(5) 0.108(3) Uiso 1 1 d . . .
H31A H 0.4135 0.3490 0.4221 0.130 Uiso 1 1 calc R . .
H31B H 0.3947 0.2635 0.3939 0.130 Uiso 1 1 calc R . .
C33 C 0.1244(8) 0.2166(5) 0.4475(4) 0.106(4) Uani 1 1 d . . .
H33A H 0.1117 0.2358 0.4063 0.127 Uiso 1 1 calc R . .
H33B H 0.1703 0.1741 0.4492 0.127 Uiso 1 1 calc R . .
C34 C 0.0430(7) 0.1815(7) 0.4558(5) 0.106(3) Uani 1 1 d . . .
H34A H -0.0090 0.2187 0.4453 0.127 Uiso 1 1 calc R . .
H34B H 0.0488 0.1677 0.4981 0.127 Uiso 1 1 calc R . .
C32 C 0.3696(13) 0.3528(11) 0.3281(8) 0.187(7) Uiso 1 1 d . . .
H32A H 0.3115 0.3379 0.3018 0.280 Uiso 1 1 calc R . .
H32B H 0.4221 0.3324 0.3124 0.280 Uiso 1 1 calc R . .
H32C H 0.3737 0.4097 0.3306 0.280 Uiso 1 1 calc R . .
C35 C 0.0207(5) 0.1042(4) 0.4162(3) 0.0572(18) Uani 1 1 d . . .
H35A H 0.0107 0.1168 0.3735 0.069 Uiso 1 1 calc R . .
H35B H 0.0718 0.0660 0.4258 0.069 Uiso 1 1 calc R . .
C36 C -0.0663(6) 0.0735(5) 0.4324(4) 0.085(3) Uani 1 1 d . . .
H36A H -0.0583 0.0706 0.4755 0.127 Uiso 1 1 calc R . .
H36B H -0.0795 0.0214 0.4154 0.127 Uiso 1 1 calc R . .
H36C H -0.1181 0.1083 0.4168 0.127 Uiso 1 1 calc R . .
Cl2 Cl 0.84016(18) 0.22789(15) 0.85290(10) 0.0911(7) Uani 1 1 d . . .
Cl4 Cl 0.87118(18) 0.05978(16) 0.84573(12) 0.0991(8) Uani 1 1 d . . .
Cl3 Cl 0.68774(19) 0.1221(2) 0.85736(12) 0.1235(12) Uani 1 1 d . . .
C28 C 0.7894(6) 0.1365(5) 0.8275(3) 0.073(2) Uani 1 1 d . . .
H28 H 0.7704 0.1389 0.7835 0.088 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
F14 C24 1.346(8) . ?
F13 C25 1.337(8) . ?
F10 C14 1.344(8) . ?
F9 C15 1.358(10) . ?
F8 C16 1.341(9) . ?
F7 C17 1.324(9) . ?
F6 C18 1.349(8) . ?
F5 C5 1.353(8) . ?
F4 C6 1.344(7) . ?
F3 C7 1.346(7) . ?
F2 C8 1.335(7) . ?
F1 C9 1.341(7) . ?
N1 C10 1.472(10) . ?
N1 C1 1.463(9) . ?
N1 C19 1.477(8) . ?
C19 C20 1.530(9) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 N4 1.440(7) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
N4 C21 1.325(8) . ?
N4 H4 0.8600 . ?
C21 O3 1.224(7) . ?
C21 C22 1.519(8) . ?
C22 C27 1.355(9) . ?
C22 C23 1.364(8) . ?
C23 F15 1.333(7) . ?
C23 C24 1.374(9) . ?
C24 C25 1.336(10) . ?
C25 C26 1.330(11) . ?
C26 F12 1.343(10) . ?
C26 C27 1.365(11) . ?
C27 F11 1.341(8) . ?
C10 C11 1.508(11) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N3 1.446(8) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
N3 C12 1.307(8) . ?
N3 H3 0.8600 . ?
C12 O2 1.234(8) . ?
C12 C13 1.513(9) . ?
C13 C14 1.374(10) . ?
C13 C18 1.382(9) . ?
C14 C15 1.345(10) . ?
C15 C16 1.360(12) . ?
C16 C17 1.375(13) . ?
C17 C18 1.385(10) . ?
C1 C2 1.515(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.442(9) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
N2 C3 1.321(9) . ?
N2 H2 0.8600 . ?
C3 O1 1.190(9) . ?
C3 C4 1.512(9) . ?
C4 C9 1.370(9) . ?
C4 C5 1.377(9) . ?
C5 C6 1.379(10) . ?
C6 C7 1.364(9) . ?
C7 C8 1.356(9) . ?
C8 C9 1.372(9) . ?
N5 C29 1.491(8) . ?
N5 C37 1.487(8) . ?
N5 C33 1.500(9) . ?
N5 C41 1.537(8) . ?
C41 C42 1.504(11) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C43 1.559(12) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.445(13) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C37 C38 1.489(10) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 C39 1.551(11) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 C40 1.504(10) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C29 C30 1.506(9) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.626(14) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 C32 1.550(19) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C33 C34 1.359(14) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.576(12) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C35 C36 1.468(11) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
Cl2 C28 1.751(9) . ?
Cl4 C28 1.742(9) . ?
Cl3 C28 1.746(8) . ?
C28 H28 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
C10 N1 C1 112.1(6) . . ?
C10 N1 C19 111.0(5) . . ?
C1 N1 C19 111.9(6) . . ?
N1 C19 C20 111.6(5) . . ?
N1 C19 H19A 109.3 . . ?
C20 C19 H19A 109.3 . . ?
N1 C19 H19B 109.3 . . ?
C20 C19 H19B 109.3 . . ?
H19A C19 H19B 108.0 . . ?
N4 C20 C19 110.5(5) . . ?
N4 C20 H20A 109.5 . . ?
C19 C20 H20A 109.5 . . ?
N4 C20 H20B 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 108.1 . . ?
C21 N4 C20 122.5(5) . . ?
C21 N4 H4 118.8 . . ?
C20 N4 H4 118.8 . . ?
O3 C21 N4 126.1(5) . . ?
O3 C21 C22 119.3(5) . . ?
N4 C21 C22 114.6(5) . . ?
C27 C22 C23 115.0(6) . . ?
C27 C22 C21 122.4(5) . . ?
C23 C22 C21 122.6(5) . . ?
F15 C23 C22 118.9(6) . . ?
F15 C23 C24 119.5(6) . . ?
C22 C23 C24 121.6(6) . . ?
C25 C24 F14 119.3(6) . . ?
C25 C24 C23 121.0(6) . . ?
F14 C24 C23 119.7(7) . . ?
F13 C25 C24 119.9(7) . . ?
F13 C25 C26 121.0(7) . . ?
C24 C25 C26 119.1(6) . . ?
F12 C26 C25 119.3(7) . . ?
F12 C26 C27 121.0(8) . . ?
C25 C26 C27 119.7(7) . . ?
F11 C27 C22 118.0(6) . . ?
F11 C27 C26 118.3(6) . . ?
C22 C27 C26 123.6(6) . . ?
N1 C10 C11 112.7(6) . . ?
N1 C10 H10A 109.0 . . ?
C11 C10 H10A 109.0 . . ?
N1 C10 H10B 109.0 . . ?
C11 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
N3 C11 C10 111.7(6) . . ?
N3 C11 H11A 109.3 . . ?
C10 C11 H11A 109.3 . . ?
N3 C11 H11B 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 107.9 . . ?
C12 N3 C11 121.9(6) . . ?
C12 N3 H3 119.1 . . ?
C11 N3 H3 119.1 . . ?
O2 C12 N3 125.1(6) . . ?
O2 C12 C13 118.6(6) . . ?
N3 C12 C13 116.2(5) . . ?
C14 C13 C18 117.1(6) . . ?
C14 C13 C12 121.6(6) . . ?
C18 C13 C12 121.3(7) . . ?
C15 C14 F10 119.1(7) . . ?
C15 C14 C13 122.1(7) . . ?
F10 C14 C13 118.8(6) . . ?
C14 C15 F9 120.4(8) . . ?
C14 C15 C16 119.8(8) . . ?
F9 C15 C16 119.7(7) . . ?
F8 C16 C15 120.7(9) . . ?
F8 C16 C17 117.9(8) . . ?
C15 C16 C17 121.4(7) . . ?
F7 C17 C18 120.3(9) . . ?
F7 C17 C16 122.3(7) . . ?
C18 C17 C16 117.3(7) . . ?
F6 C18 C13 119.7(6) . . ?
F6 C18 C17 118.0(7) . . ?
C13 C18 C17 122.2(8) . . ?
N1 C1 C2 110.5(6) . . ?
N1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N2 C2 C1 112.1(6) . . ?
N2 C2 H2A 109.2 . . ?
C1 C2 H2A 109.2 . . ?
N2 C2 H2B 109.2 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
C3 N2 C2 122.5(6) . . ?
C3 N2 H2 118.7 . . ?
C2 N2 H2 118.7 . . ?
O1 C3 N2 124.3(7) . . ?
O1 C3 C4 121.3(7) . . ?
N2 C3 C4 114.4(6) . . ?
C9 C4 C5 116.7(6) . . ?
C9 C4 C3 121.9(6) . . ?
C5 C4 C3 121.3(6) . . ?
F5 C5 C6 118.2(6) . . ?
F5 C5 C4 119.5(6) . . ?
C6 C5 C4 122.4(6) . . ?
F4 C6 C7 120.6(6) . . ?
F4 C6 C5 120.8(6) . . ?
C7 C6 C5 118.6(6) . . ?
F3 C7 C8 120.4(6) . . ?
F3 C7 C6 118.9(6) . . ?
C8 C7 C6 120.6(6) . . ?
F2 C8 C7 120.1(6) . . ?
F2 C8 C9 120.2(6) . . ?
C7 C8 C9 119.7(6) . . ?
F1 C9 C4 119.3(6) . . ?
F1 C9 C8 118.7(6) . . ?
C4 C9 C8 122.0(6) . . ?
C29 N5 C37 112.1(5) . . ?
C29 N5 C33 105.3(7) . . ?
C37 N5 C33 111.5(5) . . ?
C29 N5 C41 111.8(5) . . ?
C37 N5 C41 107.9(5) . . ?
C33 N5 C41 108.2(6) . . ?
C42 C41 N5 114.6(6) . . ?
C42 C41 H41A 108.6 . . ?
N5 C41 H41A 108.6 . . ?
C42 C41 H41B 108.6 . . ?
N5 C41 H41B 108.6 . . ?
H41A C41 H41B 107.6 . . ?
C41 C42 C43 110.2(8) . . ?
C41 C42 H42A 109.6 . . ?
C43 C42 H42A 109.6 . . ?
C41 C42 H42B 109.6 . . ?
C43 C42 H42B 109.6 . . ?
H42A C42 H42B 108.1 . . ?
C44 C43 C42 115.8(7) . . ?
C44 C43 H43A 108.3 . . ?
C42 C43 H43A 108.3 . . ?
C44 C43 H43B 108.3 . . ?
C42 C43 H43B 108.3 . . ?
H43A C43 H43B 107.4 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C38 C37 N5 114.2(5) . . ?
C38 C37 H37A 108.7 . . ?
N5 C37 H37A 108.7 . . ?
C38 C37 H37B 108.7 . . ?
N5 C37 H37B 108.7 . . ?
H37A C37 H37B 107.6 . . ?
C37 C38 C39 110.6(6) . . ?
C37 C38 H38A 109.5 . . ?
C39 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C39 C38 H38B 109.5 . . ?
H38A C38 H38B 108.1 . . ?
C40 C39 C38 109.8(7) . . ?
C40 C39 H39A 109.7 . . ?
C38 C39 H39A 109.7 . . ?
C40 C39 H39B 109.7 . . ?
C38 C39 H39B 109.7 . . ?
H39A C39 H39B 108.2 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N5 C29 C30 115.3(6) . . ?
N5 C29 H29A 108.5 . . ?
C30 C29 H29A 108.5 . . ?
N5 C29 H29B 108.5 . . ?
C30 C29 H29B 108.5 . . ?
H29A C29 H29B 107.5 . . ?
C29 C30 C31 106.5(7) . . ?
C29 C30 H30A 110.4 . . ?
C31 C30 H30A 110.4 . . ?
C29 C30 H30B 110.4 . . ?
C31 C30 H30B 110.4 . . ?
H30A C30 H30B 108.6 . . ?
C32 C31 C30 107.0(10) . . ?
C32 C31 H31A 110.3 . . ?
C30 C31 H31A 110.3 . . ?
C32 C31 H31B 110.3 . . ?
C30 C31 H31B 110.3 . . ?
H31A C31 H31B 108.6 . . ?
C34 C33 N5 125.5(11) . . ?
C34 C33 H33A 106.0 . . ?
N5 C33 H33A 106.0 . . ?
C34 C33 H33B 106.0 . . ?
N5 C33 H33B 106.0 . . ?
H33A C33 H33B 106.3 . . ?
C33 C34 C35 111.4(8) . . ?
C33 C34 H34A 109.3 . . ?
C35 C34 H34A 109.3 . . ?
C33 C34 H34B 109.3 . . ?
C35 C34 H34B 109.3 . . ?
H34A C34 H34B 108.0 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C36 C35 C34 103.7(7) . . ?
C36 C35 H35A 111.0 . . ?
C34 C35 H35A 111.0 . . ?
C36 C35 H35B 111.0 . . ?
C34 C35 H35B 111.0 . . ?
H35A C35 H35B 109.0 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
Cl3 C28 Cl4 112.7(5) . . ?
Cl3 C28 Cl2 108.9(4) . . ?
Cl4 C28 Cl2 110.7(5) . . ?
Cl3 C28 H28 108.1 . . ?
Cl4 C28 H28 108.1 . . ?
Cl2 C28 H28 108.1 . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        22.82
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         1.574
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.086
_database_code_depnum_ccdc_archive 'CCDC 710730'
