# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_name        'Jeppesen, Jan'
_publ_contact_author_email       joj@chem.sdu.dk
loop_
_publ_author_name
S.Andersen
A.Sorensen
E.Miyazaki
K.Takimiya
B.Laursen
A.Flood
;
J.Jeppesen
;

data_TRISPHAT_CBPQT
_database_code_depnum_ccdc_archive 'CCDC 801415'
#TrackingRef '- 9) TRISPHAT_CBPQT_revised.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            TRISPHAT
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C120 H50 Cl48 N10 O24 P4'
_chemical_formula_weight         3841.18

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'
P P 0.1023 0.0942 '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                   14.821(4)
_cell_length_b                   15.650(5)
_cell_length_c                   17.686(5)
_cell_angle_alpha                74.787(4)
_cell_angle_beta                 87.859(4)
_cell_angle_gamma                66.476(4)
_cell_volume                     3618.9(18)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6218
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      27.94

_exptl_crystal_description       yellow
_exptl_crystal_colour            block
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1908
_exptl_absorpt_coefficient_mu    1.011
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20594
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_sigmaI/netI    0.1020
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.20
_diffrn_reflns_theta_max         28.09
_reflns_number_total             16007
_reflns_number_gt                8590
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'SHELXS-97 (Sheldrick, 1990)'
_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 F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
Furthermore, we restrain the bond length of CH3CN as follows: bond lengths of
C-C and C-N were restrained for 1.47 and 1.16 ? by using the DFIX command of
SHELXL-97, respectively. In addition, we restrained the thermal factors of CH3CN
by using the EADP command of the SHELXL-97 to reduce the shift error.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+21.7354P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         16007
_refine_ls_number_parameters     895
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1793
_refine_ls_R_factor_gt           0.1045
_refine_ls_wR_factor_ref         0.2347
_refine_ls_wR_factor_gt          0.2054
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_restrained_S_all      1.118
_refine_ls_shift/su_max          0.014
_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
C61 C 0.1508(9) 0.7908(7) 0.3367(6) 0.075(3) Uani 1 1 d . . .
H22 H 0.2095 0.7962 0.3532 0.090 Uiso 1 1 calc R . .
H23 H 0.1176 0.8447 0.2913 0.090 Uiso 1 1 calc R . .
C1 C 0.1783(8) 0.6958(7) 0.3161(5) 0.059(3) Uani 1 1 d . . .
C2 C 0.1088(8) 0.6769(7) 0.2842(6) 0.070(3) Uani 1 1 d . . .
H1 H 0.0448 0.7244 0.2725 0.084 Uiso 1 1 calc R . .
C3 C 0.1302(9) 0.5897(8) 0.2686(6) 0.069(3) Uani 1 1 d . . .
H2 H 0.0808 0.5787 0.2472 0.083 Uiso 1 1 calc R . .
C4 C 0.2249(9) 0.5181(8) 0.2847(6) 0.065(3) Uani 1 1 d . . .
C5 C 0.2956(8) 0.5375(9) 0.3151(6) 0.076(3) Uani 1 1 d . . .
H3 H 0.3600 0.4908 0.3255 0.091 Uiso 1 1 calc R . .
C6 C 0.2725(9) 0.6271(9) 0.3310(6) 0.075(3) Uani 1 1 d . . .
H4 H 0.3215 0.6393 0.3516 0.090 Uiso 1 1 calc R . .
C62 C 0.2485(9) 0.4215(8) 0.2677(7) 0.082(3) Uani 1 1 d . . .
H24 H 0.2286 0.4320 0.2132 0.098 Uiso 1 1 calc R . .
H25 H 0.3190 0.3828 0.2763 0.098 Uiso 1 1 calc R . .
N6 N 0.1946(7) 0.3686(6) 0.3208(5) 0.071(2) Uani 1 1 d . . .
C8 C 0.1126(9) 0.3654(8) 0.2934(6) 0.070(3) Uani 1 1 d . . .
H5 H 0.0903 0.3929 0.2407 0.084 Uiso 1 1 calc R . .
C9 C 0.0631(8) 0.3213(7) 0.3441(6) 0.063(3) Uani 1 1 d . . .
H6 H 0.0070 0.3184 0.3251 0.076 Uiso 1 1 calc R . .
C10 C 0.0939(7) 0.2806(7) 0.4235(5) 0.055(2) Uani 1 1 d . . .
C11 C 0.1812(8) 0.2820(7) 0.4479(6) 0.068(3) Uani 1 1 d . . .
H7 H 0.2067 0.2528 0.4999 0.082 Uiso 1 1 calc R . .
C12 C 0.2306(8) 0.3268(8) 0.3947(7) 0.072(3) Uani 1 1 d . . .
H8 H 0.2891 0.3275 0.4110 0.086 Uiso 1 1 calc R . .
C13 C 0.0338(8) 0.2446(6) 0.4817(5) 0.056(2) Uani 1 1 d . . .
C14 C -0.0674(8) 0.2844(7) 0.4688(6) 0.065(3) Uani 1 1 d . . .
H9 H -0.0968 0.3252 0.4198 0.078 Uiso 1 1 calc R . .
C15 C -0.1252(8) 0.2650(7) 0.5269(6) 0.066(3) Uani 1 1 d . . .
H10 H -0.1934 0.2912 0.5170 0.079 Uiso 1 1 calc R . .
N7 N -0.0838(7) 0.2083(5) 0.5980(5) 0.063(2) Uani 1 1 d . . .
C17 C 0.0127(9) 0.1627(7) 0.6109(6) 0.070(3) Uani 1 1 d . . .
H11 H 0.0395 0.1183 0.6592 0.085 Uiso 1 1 calc R . .
C18 C 0.0747(8) 0.1789(7) 0.5548(6) 0.066(3) Uani 1 1 d . . .
H12 H 0.1427 0.1468 0.5651 0.079 Uiso 1 1 calc R . .
P1 P 0.01434(15) 1.10127(14) 0.24055(11) 0.0347(4) Uani 1 1 d . . .
O1 O 0.1075(4) 1.1417(3) 0.2361(3) 0.0376(12) Uani 1 1 d . . .
C19 C 0.1664(6) 1.1031(5) 0.3031(4) 0.0362(17) Uani 1 1 d . . .
C20 C 0.2511(6) 1.1168(6) 0.3161(5) 0.0421(19) Uani 1 1 d . . .
C21 C 0.3022(6) 1.0726(6) 0.3903(4) 0.045(2) Uani 1 1 d . . .
C22 C 0.2678(6) 1.0184(6) 0.4483(4) 0.046(2) Uani 1 1 d . . .
C23 C 0.1834(6) 1.0029(6) 0.4349(4) 0.0412(19) Uani 1 1 d . . .
C24 C 0.1349(6) 1.0446(5) 0.3615(4) 0.0356(17) Uani 1 1 d . . .
O2 O 0.0546(4) 1.0355(4) 0.3373(3) 0.0395(12) Uani 1 1 d . . .
Cl1 Cl 0.29044(18) 1.18526(17) 0.24119(13) 0.0563(6) Uani 1 1 d . . .
Cl2 Cl 0.40779(19) 1.0869(2) 0.40808(16) 0.0744(8) Uani 1 1 d . . .
Cl3 Cl 0.3288(2) 0.9672(2) 0.54148(14) 0.0778(8) Uani 1 1 d . . .
Cl4 Cl 0.13742(19) 0.93868(19) 0.50802(12) 0.0632(7) Uani 1 1 d . . .
O3 O -0.0210(4) 1.1666(3) 0.1457(3) 0.0393(13) Uani 1 1 d . . .
C25 C 0.0249(6) 1.1142(5) 0.0958(4) 0.0366(17) Uani 1 1 d . . .
C26 C 0.0180(6) 1.1467(6) 0.0146(4) 0.0396(19) Uani 1 1 d . . .
C27 C 0.0706(6) 1.0822(6) -0.0272(4) 0.042(2) Uani 1 1 d . . .
C28 C 0.1298(6) 0.9864(6) 0.0097(5) 0.0423(19) Uani 1 1 d . . .
C29 C 0.1366(6) 0.9546(5) 0.0924(4) 0.0368(18) Uani 1 1 d . . .
C30 C 0.0860(5) 1.0189(5) 0.1339(4) 0.0345(17) Uani 1 1 d . . .
O4 O 0.0872(4) 1.0005(3) 0.2128(3) 0.0364(12) Uani 1 1 d . . .
Cl5 Cl -0.05364(18) 1.26667(17) -0.02965(13) 0.0646(7) Uani 1 1 d . . .
Cl6 Cl 0.06304(19) 1.1210(2) -0.12914(12) 0.0647(7) Uani 1 1 d . . .
Cl7 Cl 0.19454(18) 0.90698(19) -0.04345(13) 0.0598(6) Uani 1 1 d . . .
Cl8 Cl 0.21010(17) 0.83587(15) 0.14017(13) 0.0519(5) Uani 1 1 d . . .
O5 O -0.0774(4) 1.0598(4) 0.2490(3) 0.0383(12) Uani 1 1 d . . .
C31 C -0.1637(6) 1.1256(5) 0.2631(4) 0.0344(17) Uani 1 1 d . . .
C32 C -0.2519(6) 1.1165(6) 0.2654(4) 0.0408(19) Uani 1 1 d . . .
C33 C -0.3352(6) 1.1928(7) 0.2797(4) 0.046(2) Uani 1 1 d . . .
C34 C -0.3285(6) 1.2739(6) 0.2903(4) 0.046(2) Uani 1 1 d . . .
C35 C -0.2360(6) 1.2817(6) 0.2868(4) 0.0413(19) Uani 1 1 d . . .
C36 C -0.1546(6) 1.2059(5) 0.2735(4) 0.0351(17) Uani 1 1 d . . .
O6 O -0.0623(4) 1.2024(4) 0.2678(3) 0.0417(13) Uani 1 1 d . . .
Cl9 Cl -0.25785(18) 1.01521(19) 0.25173(15) 0.0646(7) Uani 1 1 d . . .
Cl10 Cl -0.44860(17) 1.1857(2) 0.28148(15) 0.0736(8) Uani 1 1 d . . .
Cl11 Cl -0.42969(19) 1.3688(2) 0.30650(16) 0.0786(8) Uani 1 1 d . . .
Cl12 Cl -0.22514(18) 1.38426(16) 0.29492(14) 0.0604(6) Uani 1 1 d . . .
P2 P 0.56207(17) 0.67753(15) 0.16025(13) 0.0444(5) Uani 1 1 d . . .
O7 O 0.6659(4) 0.6956(4) 0.1775(3) 0.0472(14) Uani 1 1 d . . .
C37 C 0.7052(6) 0.6526(5) 0.2514(4) 0.0421(19) Uani 1 1 d . . .
C38 C 0.7914(7) 0.6480(6) 0.2815(5) 0.056(2) Uani 1 1 d . . .
C39 C 0.8219(7) 0.6001(6) 0.3607(5) 0.059(3) Uani 1 1 d . . .
C40 C 0.7644(8) 0.5606(6) 0.4075(5) 0.063(3) Uani 1 1 d . . .
C41 C 0.6761(8) 0.5644(6) 0.3779(5) 0.054(2) Uani 1 1 d . . .
C42 C 0.6486(7) 0.6094(6) 0.2979(5) 0.048(2) Uani 1 1 d . . .
O8 O 0.5696(4) 0.6166(4) 0.2588(3) 0.0518(15) Uani 1 1 d . . .
Cl13 Cl 0.8567(2) 0.7035(2) 0.22108(16) 0.0905(10) Uani 1 1 d . . .
Cl14 Cl 0.9317(2) 0.5909(2) 0.39915(17) 0.0920(10) Uani 1 1 d . . .
Cl15 Cl 0.8004(3) 0.5056(2) 0.50635(14) 0.0913(10) Uani 1 1 d . . .
Cl16 Cl 0.6049(3) 0.5136(2) 0.43422(15) 0.0879(9) Uani 1 1 d . . .
O9 O 0.4619(4) 0.6546(4) 0.1456(3) 0.0460(14) Uani 1 1 d . . .
C43 C 0.4887(6) 0.5698(5) 0.1269(4) 0.0366(18) Uani 1 1 d . . .
C44 C 0.4256(6) 0.5305(5) 0.1122(4) 0.0356(17) Uani 1 1 d . . .
C45 C 0.4650(6) 0.4402(6) 0.0974(4) 0.042(2) Uani 1 1 d . . .
C46 C 0.5673(6) 0.3950(5) 0.0910(4) 0.0407(19) Uani 1 1 d . . .
C47 C 0.6299(6) 0.4375(5) 0.1030(4) 0.0368(18) Uani 1 1 d . . .
C48 C 0.5890(6) 0.5248(5) 0.1219(4) 0.0383(18) Uani 1 1 d . . .
O10 O 0.6394(4) 0.5757(4) 0.1363(3) 0.0428(13) Uani 1 1 d . . .
Cl17 Cl 0.30024(16) 0.59402(17) 0.11285(13) 0.0564(6) Uani 1 1 d . . .
Cl18 Cl 0.38875(19) 0.38650(17) 0.08306(14) 0.0618(6) Uani 1 1 d . . .
Cl19 Cl 0.61516(19) 0.28490(16) 0.07023(14) 0.0613(6) Uani 1 1 d . . .
Cl20 Cl 0.75447(16) 0.38537(16) 0.09403(12) 0.0534(6) Uani 1 1 d . . .
O11 O 0.4846(4) 0.7792(4) 0.1853(3) 0.0533(15) Uani 1 1 d . . .
C49 C 0.4469(6) 0.8541(6) 0.1205(6) 0.053(2) Uani 1 1 d . . .
C50 C 0.3766(7) 0.9440(7) 0.1203(7) 0.061(3) Uani 1 1 d . . .
C51 C 0.3445(7) 1.0148(7) 0.0494(9) 0.072(3) Uani 1 1 d . . .
C52 C 0.3829(7) 0.9946(6) -0.0181(7) 0.066(3) Uani 1 1 d . . .
C53 C 0.4565(6) 0.9030(6) -0.0193(6) 0.054(2) Uani 1 1 d . . .
C54 C 0.4864(6) 0.8340(6) 0.0522(6) 0.048(2) Uani 1 1 d . . .
O12 O 0.5554(4) 0.7420(4) 0.0647(3) 0.0472(14) Uani 1 1 d . . .
Cl21 Cl 0.3277(2) 0.9639(2) 0.2066(2) 0.0901(10) Uani 1 1 d . . .
Cl22 Cl 0.2567(2) 1.12808(18) 0.0480(3) 0.1096(14) Uani 1 1 d . . .
Cl23 Cl 0.3423(2) 1.08280(19) -0.1070(2) 0.1057(13) Uani 1 1 d . . .
Cl24 Cl 0.5075(2) 0.87637(18) -0.10243(15) 0.0711(8) Uani 1 1 d . . .
C55 C 0.8857(19) 0.5568(18) -0.0925(13) 0.232(7) Uani 1 1 d D . .
H13 H 0.9561 0.5355 -0.0907 0.348 Uiso 1 1 calc R . .
H14 H 0.8564 0.6084 -0.1392 0.348 Uiso 1 1 calc R . .
H15 H 0.8686 0.5038 -0.0928 0.348 Uiso 1 1 calc R . .
N3 N 0.8360(18) 0.6024(18) 0.0478(12) 0.232(7) Uani 1 1 d D . .
C58 C 0.6253(14) 0.8553(14) 0.3487(12) 0.177(4) Uani 1 1 d D . .
N4 N 0.6919(12) 0.8180(11) 0.3919(9) 0.177(4) Uani 1 1 d D . .
C57 C 0.5510(13) 0.9107(12) 0.2879(10) 0.177(4) Uani 1 1 d D . .
H16 H 0.5771 0.9017 0.2386 0.265 Uiso 1 1 calc R . .
H17 H 0.5277 0.9778 0.2866 0.265 Uiso 1 1 calc R . .
H18 H 0.4974 0.8904 0.2966 0.265 Uiso 1 1 calc R . .
N5 N 0.3462(14) 0.7459(16) 0.4592(15) 0.232(6) Uani 1 1 d D . .
C59 C 0.5197(15) 0.7403(17) 0.4997(15) 0.232(6) Uani 1 1 d D . .
H19 H 0.5088 0.7727 0.5405 0.347 Uiso 1 1 calc R . .
H20 H 0.5500 0.7697 0.4579 0.347 Uiso 1 1 calc R . .
H21 H 0.5622 0.6733 0.5205 0.347 Uiso 1 1 calc R . .
C60 C 0.4213(15) 0.749(2) 0.4682(18) 0.232(6) Uani 1 1 d D . .
C56 C 0.847(2) 0.593(2) -0.0203(14) 0.232(7) Uani 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C61 0.097(8) 0.061(7) 0.064(7) -0.001(5) 0.015(6) -0.038(6)
C1 0.081(7) 0.046(6) 0.047(5) -0.005(4) 0.007(5) -0.027(6)
C2 0.071(7) 0.053(6) 0.072(7) -0.006(5) -0.008(6) -0.018(6)
C3 0.080(8) 0.068(7) 0.067(7) -0.019(5) 0.004(6) -0.036(7)
C4 0.084(8) 0.069(7) 0.051(6) -0.019(5) 0.023(5) -0.040(7)
C5 0.065(7) 0.079(8) 0.069(7) -0.025(6) 0.016(6) -0.014(6)
C6 0.076(8) 0.089(9) 0.072(7) -0.033(6) 0.013(6) -0.040(7)
C62 0.106(9) 0.085(8) 0.073(7) -0.039(6) 0.045(7) -0.049(8)
N6 0.087(7) 0.056(5) 0.073(6) -0.035(5) 0.029(5) -0.025(5)
C8 0.085(8) 0.072(7) 0.056(6) -0.029(5) 0.018(6) -0.029(6)
C9 0.076(7) 0.058(6) 0.058(6) -0.023(5) 0.008(5) -0.024(6)
C10 0.069(6) 0.053(6) 0.048(5) -0.031(4) 0.009(5) -0.018(5)
C11 0.080(7) 0.060(6) 0.062(6) -0.023(5) 0.003(6) -0.023(6)
C12 0.077(7) 0.073(7) 0.076(8) -0.039(6) 0.012(6) -0.031(6)
C13 0.076(7) 0.047(5) 0.046(5) -0.018(4) 0.003(5) -0.021(5)
C14 0.078(7) 0.062(6) 0.047(6) -0.010(5) -0.004(5) -0.024(6)
C15 0.070(7) 0.066(7) 0.058(6) -0.007(5) 0.001(5) -0.030(6)
N7 0.087(6) 0.041(4) 0.059(5) -0.009(4) 0.000(5) -0.025(5)
C17 0.090(8) 0.039(5) 0.067(7) -0.005(5) -0.004(6) -0.015(6)
C18 0.072(7) 0.049(6) 0.062(6) -0.012(5) 0.003(5) -0.012(5)
P1 0.0392(11) 0.0314(10) 0.0314(10) -0.0117(8) 0.0034(8) -0.0102(9)
O1 0.043(3) 0.034(3) 0.035(3) -0.009(2) 0.003(2) -0.015(2)
C19 0.046(5) 0.030(4) 0.037(4) -0.017(3) 0.010(4) -0.017(4)
C20 0.058(5) 0.040(5) 0.043(5) -0.032(4) 0.012(4) -0.022(4)
C21 0.052(5) 0.060(5) 0.033(4) -0.030(4) 0.013(4) -0.023(4)
C22 0.044(5) 0.056(5) 0.035(4) -0.020(4) -0.003(4) -0.012(4)
C23 0.053(5) 0.040(5) 0.036(4) -0.021(3) 0.006(4) -0.017(4)
C24 0.040(4) 0.035(4) 0.036(4) -0.023(3) 0.006(3) -0.012(4)
O2 0.043(3) 0.039(3) 0.035(3) -0.009(2) 0.002(2) -0.016(3)
Cl1 0.0676(15) 0.0563(14) 0.0615(14) -0.0265(11) 0.0194(11) -0.0364(12)
Cl2 0.0607(15) 0.101(2) 0.0785(18) -0.0344(15) -0.0011(13) -0.0436(16)
Cl3 0.0792(18) 0.106(2) 0.0457(13) -0.0120(14) -0.0177(13) -0.0383(17)
Cl4 0.0774(16) 0.0752(17) 0.0386(12) -0.0061(11) 0.0037(11) -0.0383(14)
O3 0.040(3) 0.030(3) 0.038(3) -0.006(2) -0.003(2) -0.006(2)
C25 0.038(4) 0.032(4) 0.034(4) -0.010(3) -0.001(3) -0.009(4)
C26 0.038(4) 0.044(5) 0.034(4) -0.007(3) -0.001(3) -0.016(4)
C27 0.049(5) 0.063(6) 0.020(4) -0.007(4) 0.007(3) -0.031(5)
C28 0.037(4) 0.045(5) 0.050(5) -0.020(4) 0.003(4) -0.017(4)
C29 0.040(4) 0.034(4) 0.039(4) -0.011(3) -0.003(3) -0.016(4)
C30 0.037(4) 0.029(4) 0.041(4) -0.015(3) 0.002(3) -0.013(3)
O4 0.041(3) 0.028(3) 0.032(3) -0.008(2) 0.001(2) -0.005(2)
Cl5 0.0656(15) 0.0505(13) 0.0504(13) 0.0057(10) -0.0071(11) -0.0070(12)
Cl6 0.0722(16) 0.0882(18) 0.0327(11) -0.0108(11) 0.0049(11) -0.0349(15)
Cl7 0.0640(15) 0.0729(16) 0.0541(13) -0.0375(12) 0.0202(11) -0.0281(13)
Cl8 0.0577(13) 0.0337(11) 0.0595(13) -0.0159(9) 0.0075(11) -0.0119(10)
O5 0.041(3) 0.034(3) 0.042(3) -0.018(2) 0.005(2) -0.012(3)
C31 0.040(4) 0.038(4) 0.020(3) -0.010(3) 0.007(3) -0.009(4)
C32 0.046(5) 0.053(5) 0.025(4) -0.011(3) 0.007(3) -0.021(4)
C33 0.047(5) 0.068(6) 0.019(4) -0.008(4) 0.008(3) -0.020(5)
C34 0.046(5) 0.053(5) 0.020(4) -0.009(3) 0.008(3) -0.003(4)
C35 0.053(5) 0.041(5) 0.020(4) -0.012(3) 0.009(3) -0.008(4)
C36 0.040(4) 0.039(4) 0.019(3) -0.011(3) 0.010(3) -0.008(4)
O6 0.040(3) 0.033(3) 0.051(3) -0.019(2) 0.005(3) -0.010(3)
Cl9 0.0657(15) 0.0738(17) 0.0735(16) -0.0288(13) 0.0111(12) -0.0423(14)
Cl10 0.0457(13) 0.104(2) 0.0643(16) -0.0145(14) 0.0051(12) -0.0285(14)
Cl11 0.0540(15) 0.0770(18) 0.0723(17) -0.0216(14) 0.0137(13) 0.0065(14)
Cl12 0.0721(16) 0.0397(12) 0.0581(14) -0.0214(10) -0.0040(12) -0.0053(11)
P2 0.0505(13) 0.0336(11) 0.0453(12) -0.0135(9) -0.0036(10) -0.0106(10)
O7 0.054(3) 0.041(3) 0.041(3) -0.005(3) -0.008(3) -0.017(3)
C37 0.055(5) 0.030(4) 0.038(4) -0.013(3) 0.000(4) -0.011(4)
C38 0.065(6) 0.042(5) 0.055(6) -0.004(4) -0.013(5) -0.019(5)
C39 0.079(7) 0.044(5) 0.043(5) -0.012(4) -0.014(5) -0.012(5)
C40 0.110(8) 0.038(5) 0.035(5) -0.007(4) -0.017(5) -0.023(5)
C41 0.087(7) 0.041(5) 0.037(5) -0.023(4) 0.008(5) -0.024(5)
C42 0.060(6) 0.037(5) 0.045(5) -0.018(4) -0.001(4) -0.014(4)
O8 0.063(4) 0.046(3) 0.043(3) -0.010(3) 0.004(3) -0.021(3)
Cl13 0.087(2) 0.107(2) 0.0719(18) 0.0210(16) -0.0300(15) -0.0591(19)
Cl14 0.097(2) 0.102(2) 0.0673(17) -0.0035(16) -0.0366(16) -0.0379(19)
Cl15 0.160(3) 0.0731(18) 0.0363(13) -0.0085(12) -0.0167(16) -0.045(2)
Cl16 0.141(3) 0.094(2) 0.0510(15) -0.0244(14) 0.0291(16) -0.068(2)
O9 0.042(3) 0.040(3) 0.055(3) -0.025(3) 0.004(3) -0.008(3)
C43 0.049(5) 0.034(4) 0.024(4) -0.015(3) 0.005(3) -0.010(4)
C44 0.053(5) 0.040(4) 0.015(3) -0.017(3) 0.005(3) -0.014(4)
C45 0.062(6) 0.047(5) 0.023(4) -0.014(3) 0.000(4) -0.023(4)
C46 0.060(5) 0.031(4) 0.023(4) -0.011(3) 0.003(4) -0.008(4)
C47 0.053(5) 0.037(4) 0.015(3) -0.013(3) 0.006(3) -0.009(4)
C48 0.048(5) 0.035(4) 0.027(4) -0.013(3) 0.002(3) -0.009(4)
O10 0.044(3) 0.032(3) 0.046(3) -0.011(2) -0.002(3) -0.009(3)
Cl17 0.0486(13) 0.0631(15) 0.0568(13) -0.0192(11) 0.0094(10) -0.0204(12)
Cl18 0.0768(16) 0.0558(14) 0.0644(15) -0.0199(11) 0.0035(12) -0.0361(13)
Cl19 0.0840(17) 0.0371(12) 0.0602(14) -0.0217(10) 0.0064(12) -0.0166(12)
Cl20 0.0514(13) 0.0483(13) 0.0458(12) -0.0152(10) 0.0066(10) -0.0038(11)
O11 0.055(4) 0.040(3) 0.064(4) -0.025(3) -0.005(3) -0.009(3)
C49 0.044(5) 0.029(5) 0.087(7) -0.025(5) -0.010(5) -0.010(4)
C50 0.046(5) 0.041(5) 0.107(8) -0.040(5) -0.005(5) -0.014(5)
C51 0.042(6) 0.036(5) 0.142(11) -0.028(7) -0.020(7) -0.013(5)
C52 0.049(6) 0.028(5) 0.113(9) 0.004(5) -0.031(6) -0.019(4)
C53 0.046(5) 0.036(5) 0.080(7) -0.008(4) -0.019(5) -0.020(4)
C54 0.038(5) 0.031(4) 0.071(6) -0.010(4) -0.017(4) -0.010(4)
O12 0.049(3) 0.030(3) 0.049(3) -0.008(2) -0.009(3) -0.004(3)
Cl21 0.0582(16) 0.0776(19) 0.149(3) -0.080(2) 0.0030(17) -0.0103(15)
Cl22 0.0535(16) 0.0367(14) 0.228(4) -0.0393(19) -0.031(2) -0.0019(12)
Cl23 0.0812(19) 0.0464(15) 0.160(3) 0.0288(17) -0.054(2) -0.0255(14)
Cl24 0.0795(17) 0.0580(15) 0.0698(16) 0.0072(12) -0.0212(14) -0.0346(14)
C55 0.273(15) 0.275(15) 0.176(15) -0.019(16) 0.008(16) -0.162(13)
N3 0.273(15) 0.275(15) 0.176(15) -0.019(16) 0.008(16) -0.162(13)
C58 0.182(11) 0.149(9) 0.171(11) -0.057(8) -0.082(7) -0.020(8)
N4 0.182(11) 0.149(9) 0.171(11) -0.057(8) -0.082(7) -0.020(8)
C57 0.182(11) 0.149(9) 0.171(11) -0.057(8) -0.082(7) -0.020(8)
N5 0.171(15) 0.206(12) 0.325(17) -0.123(12) -0.048(14) -0.046(13)
C59 0.171(15) 0.206(12) 0.325(17) -0.123(12) -0.048(14) -0.046(13)
C60 0.171(15) 0.206(12) 0.325(17) -0.123(12) -0.048(14) -0.046(13)
C56 0.273(15) 0.275(15) 0.176(15) -0.019(16) 0.008(16) -0.162(13)

_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
C61 N7 1.493(13) 2_566 yes
C61 C1 1.516(14) . yes
C61 H22 0.9700 . no
C61 H23 0.9700 . no
C1 C2 1.358(13) . yes
C1 C6 1.362(14) . yes
C2 C3 1.372(14) . yes
C2 H1 0.9300 . no
C3 C4 1.384(14) . yes
C3 H2 0.9300 . no
C4 C5 1.364(14) . yes
C4 C62 1.520(14) . yes
C5 C6 1.406(15) . yes
C5 H3 0.9300 . no
C6 H4 0.9300 . no
C62 N6 1.507(13) . yes
C62 H24 0.9700 . no
C62 H25 0.9700 . no
N6 C12 1.321(13) . yes
N6 C8 1.348(13) . yes
C8 C9 1.358(13) . yes
C8 H5 0.9300 . no
C9 C10 1.391(12) . yes
C9 H6 0.9300 . no
C10 C11 1.389(13) . yes
C10 C13 1.483(13) . yes
C11 C12 1.388(14) . yes
C11 H7 0.9300 . no
C12 H8 0.9300 . no
C13 C14 1.377(13) . yes
C13 C18 1.399(12) . yes
C14 C15 1.364(13) . yes
C14 H9 0.9300 . no
C15 N7 1.335(11) . yes
C15 H10 0.9300 . no
N7 C17 1.316(13) . yes
N7 C61 1.493(13) 2_566 yes
C17 C18 1.370(14) . yes
C17 H11 0.9300 . no
C18 H12 0.9300 . no
P1 O3 1.694(5) . yes
P1 O4 1.703(5) . yes
P1 O5 1.712(5) . yes
P1 O6 1.718(6) . yes
P1 O1 1.725(5) . yes
P1 O2 1.733(5) . yes
O1 C19 1.346(8) . yes
C19 C24 1.390(10) . yes
C19 C20 1.392(10) . yes
C20 C21 1.397(11) . yes
C20 Cl1 1.714(8) . yes
C21 C22 1.372(11) . yes
C21 Cl2 1.719(8) . yes
C22 C23 1.405(11) . yes
C22 Cl3 1.736(8) . yes
C23 C24 1.371(10) . yes
C23 Cl4 1.717(8) . yes
C24 O2 1.352(8) . yes
O3 C25 1.342(9) . yes
C25 C26 1.386(10) . yes
C25 C30 1.392(10) . yes
C26 C27 1.376(11) . yes
C26 Cl5 1.722(8) . yes
C27 C28 1.386(11) . yes
C27 Cl6 1.737(7) . yes
C28 C29 1.410(10) . yes
C28 Cl7 1.715(9) . yes
C29 C30 1.362(10) . yes
C29 Cl8 1.727(8) . yes
C30 O4 1.349(8) . yes
O5 C31 1.348(9) . yes
C31 C32 1.368(10) . yes
C31 C36 1.374(10) . yes
C32 C33 1.405(12) . yes
C32 Cl9 1.701(9) . yes
C33 C34 1.372(12) . yes
C33 Cl10 1.727(8) . yes
C34 C35 1.421(11) . yes
C34 Cl11 1.719(9) . yes
C35 C36 1.379(11) . yes
C35 Cl12 1.719(8) . yes
C36 O6 1.349(9) . yes
P2 O10 1.701(6) . yes
P2 O9 1.703(6) . yes
P2 O11 1.709(6) . yes
P2 O12 1.709(6) . yes
P2 O7 1.723(6) . yes
P2 O8 1.737(6) . yes
O7 C37 1.334(9) . yes
C37 C38 1.372(11) . yes
C37 C42 1.394(11) . yes
C38 C39 1.397(11) . yes
C38 Cl13 1.714(9) . yes
C39 C40 1.377(14) . yes
C39 Cl14 1.726(10) . yes
C40 C41 1.401(13) . yes
C40 Cl15 1.730(8) . yes
C41 C42 1.398(11) . yes
C41 Cl16 1.707(10) . yes
C42 O8 1.332(9) . yes
O9 C43 1.352(9) . yes
C43 C44 1.372(10) . yes
C43 C48 1.378(11) . yes
C44 C45 1.391(11) . yes
C44 Cl17 1.723(8) . yes
C45 C46 1.409(11) . yes
C45 Cl18 1.713(8) . yes
C46 C47 1.390(11) . yes
C46 Cl19 1.716(8) . yes
C47 C48 1.382(10) . yes
C47 Cl20 1.715(8) . yes
C48 O10 1.361(9) . yes
O11 C49 1.349(10) . yes
C49 C50 1.376(12) . yes
C49 C54 1.379(13) . yes
C50 C51 1.386(15) . yes
C50 Cl21 1.715(11) . yes
C51 C52 1.362(16) . yes
C51 Cl22 1.724(11) . yes
C52 C53 1.417(14) . yes
C52 Cl23 1.733(10) . yes
C53 C54 1.379(11) . yes
C53 Cl24 1.702(11) . yes
C54 O12 1.358(9) . yes
C55 C56 1.528(17) . yes
C55 H13 0.9600 . no
C55 H14 0.9600 . no
C55 H15 0.9600 . no
N3 C56 1.249(17) . yes
C58 N4 1.123(13) . yes
C58 C57 1.400(14) . yes
C57 H16 0.9600 . no
C57 H17 0.9600 . no
C57 H18 0.9600 . no
N5 C60 1.151(16) . yes
C59 C60 1.523(16) . yes
C59 H19 0.9600 . no
C59 H20 0.9600 . no
C59 H21 0.9600 . no

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
N7 C61 C1 107.3(8) 2_566 . yes
N7 C61 H22 110.2 2_566 . no
C1 C61 H22 110.2 . . no
N7 C61 H23 110.2 2_566 . no
C1 C61 H23 110.2 . . no
H22 C61 H23 108.5 . . no
C2 C1 C6 118.8(10) . . yes
C2 C1 C61 120.4(10) . . yes
C6 C1 C61 120.7(10) . . yes
C1 C2 C3 121.9(10) . . yes
C1 C2 H1 119.1 . . no
C3 C2 H1 119.1 . . no
C2 C3 C4 120.3(10) . . yes
C2 C3 H2 119.9 . . no
C4 C3 H2 119.9 . . no
C5 C4 C3 118.1(10) . . yes
C5 C4 C62 121.6(11) . . yes
C3 C4 C62 120.3(10) . . yes
C4 C5 C6 121.0(11) . . yes
C4 C5 H3 119.5 . . no
C6 C5 H3 119.5 . . no
C1 C6 C5 119.9(10) . . yes
C1 C6 H4 120.0 . . no
C5 C6 H4 120.0 . . no
N6 C62 C4 109.6(8) . . yes
N6 C62 H24 109.7 . . no
C4 C62 H24 109.7 . . no
N6 C62 H25 109.7 . . no
C4 C62 H25 109.7 . . no
H24 C62 H25 108.2 . . no
C12 N6 C8 122.0(9) . . yes
C12 N6 C62 117.2(10) . . yes
C8 N6 C62 120.8(10) . . yes
N6 C8 C9 119.1(10) . . yes
N6 C8 H5 120.5 . . no
C9 C8 H5 120.5 . . no
C8 C9 C10 121.8(10) . . yes
C8 C9 H6 119.1 . . no
C10 C9 H6 119.1 . . no
C11 C10 C9 116.7(9) . . yes
C11 C10 C13 120.4(9) . . yes
C9 C10 C13 122.7(9) . . yes
C12 C11 C10 120.0(10) . . yes
C12 C11 H7 120.0 . . no
C10 C11 H7 120.0 . . no
N6 C12 C11 120.2(10) . . yes
N6 C12 H8 119.9 . . no
C11 C12 H8 119.9 . . no
C14 C13 C18 117.3(9) . . yes
C14 C13 C10 119.9(8) . . yes
C18 C13 C10 122.4(9) . . yes
C15 C14 C13 120.9(9) . . yes
C15 C14 H9 119.5 . . no
C13 C14 H9 119.5 . . no
N7 C15 C14 120.0(10) . . yes
N7 C15 H10 120.0 . . no
C14 C15 H10 120.0 . . no
C17 N7 C15 120.8(9) . . yes
C17 N7 C61 121.9(9) . 2_566 yes
C15 N7 C61 116.9(9) . 2_566 yes
N7 C17 C18 121.6(9) . . yes
N7 C17 H11 119.2 . . no
C18 C17 H11 119.2 . . no
C17 C18 C13 118.9(10) . . yes
C17 C18 H12 120.5 . . no
C13 C18 H12 120.5 . . no
O3 P1 O4 91.6(3) . . yes
O3 P1 O5 94.2(3) . . yes
O4 P1 O5 87.8(3) . . yes
O3 P1 O6 87.9(3) . . yes
O4 P1 O6 178.2(3) . . yes
O5 P1 O6 90.5(3) . . yes
O3 P1 O1 88.0(2) . . yes
O4 P1 O1 92.8(3) . . yes
O5 P1 O1 177.7(3) . . yes
O6 P1 O1 88.9(3) . . yes
O3 P1 O2 177.7(3) . . yes
O4 P1 O2 88.2(3) . . yes
O5 P1 O2 88.0(2) . . yes
O6 P1 O2 92.3(3) . . yes
O1 P1 O2 89.8(2) . . yes
C19 O1 P1 112.4(4) . . yes
O1 C19 C24 112.9(6) . . yes
O1 C19 C20 126.1(7) . . yes
C24 C19 C20 121.0(7) . . yes
C19 C20 C21 118.3(7) . . yes
C19 C20 Cl1 119.5(6) . . yes
C21 C20 Cl1 122.2(6) . . yes
C22 C21 C20 120.0(7) . . yes
C22 C21 Cl2 120.4(6) . . yes
C20 C21 Cl2 119.5(6) . . yes
C21 C22 C23 121.8(7) . . yes
C21 C22 Cl3 120.0(6) . . yes
C23 C22 Cl3 118.3(6) . . yes
C24 C23 C22 117.9(7) . . yes
C24 C23 Cl4 119.8(6) . . yes
C22 C23 Cl4 122.2(6) . . yes
O2 C24 C23 126.2(7) . . yes
O2 C24 C19 112.9(6) . . yes
C23 C24 C19 120.9(7) . . yes
C24 O2 P1 111.9(4) . . yes
C25 O3 P1 111.5(4) . . yes
O3 C25 C26 126.7(7) . . yes
O3 C25 C30 113.1(6) . . yes
C26 C25 C30 120.2(8) . . yes
C27 C26 C25 118.6(7) . . yes
C27 C26 Cl5 122.8(6) . . yes
C25 C26 Cl5 118.6(7) . . yes
C26 C27 C28 121.8(7) . . yes
C26 C27 Cl6 119.5(6) . . yes
C28 C27 Cl6 118.7(7) . . yes
C27 C28 C29 118.9(8) . . yes
C27 C28 Cl7 121.2(6) . . yes
C29 C28 Cl7 119.9(6) . . yes
C30 C29 C28 119.2(7) . . yes
C30 C29 Cl8 120.8(6) . . yes
C28 C29 Cl8 120.0(6) . . yes
O4 C30 C29 126.3(6) . . yes
O4 C30 C25 112.6(7) . . yes
C29 C30 C25 121.1(7) . . yes
C30 O4 P1 111.2(4) . . yes
C31 O5 P1 111.8(5) . . yes
O5 C31 C32 125.0(7) . . yes
O5 C31 C36 112.4(7) . . yes
C32 C31 C36 122.6(8) . . yes
C31 C32 C33 117.6(8) . . yes
C31 C32 Cl9 120.1(7) . . yes
C33 C32 Cl9 122.3(6) . . yes
C34 C33 C32 121.1(8) . . yes
C34 C33 Cl10 119.5(7) . . yes
C32 C33 Cl10 119.4(7) . . yes
C33 C34 C35 120.0(8) . . yes
C33 C34 Cl11 122.0(7) . . yes
C35 C34 Cl11 118.1(7) . . yes
C36 C35 C34 118.3(7) . . yes
C36 C35 Cl12 120.0(6) . . yes
C34 C35 Cl12 121.6(6) . . yes
O6 C36 C31 114.0(7) . . yes
O6 C36 C35 125.6(7) . . yes
C31 C36 C35 120.4(7) . . yes
C36 O6 P1 110.7(5) . . yes
O10 P2 O9 91.5(3) . . yes
O10 P2 O11 179.4(3) . . yes
O9 P2 O11 88.5(3) . . yes
O10 P2 O12 89.1(3) . . yes
O9 P2 O12 93.5(3) . . yes
O11 P2 O12 91.4(3) . . yes
O10 P2 O7 86.8(3) . . yes
O9 P2 O7 177.5(3) . . yes
O11 P2 O7 93.1(3) . . yes
O12 P2 O7 88.4(3) . . yes
O10 P2 O8 92.9(3) . . yes
O9 P2 O8 88.5(3) . . yes
O11 P2 O8 86.5(3) . . yes
O12 P2 O8 177.1(3) . . yes
O7 P2 O8 89.7(3) . . yes
C37 O7 P2 112.5(5) . . yes
O7 C37 C38 126.3(8) . . yes
O7 C37 C42 112.4(7) . . yes
C38 C37 C42 121.3(7) . . yes
C37 C38 C39 118.9(8) . . yes
C37 C38 Cl13 118.7(6) . . yes
C39 C38 Cl13 122.3(7) . . yes
C40 C39 C38 120.0(9) . . yes
C40 C39 Cl14 120.4(7) . . yes
C38 C39 Cl14 119.7(8) . . yes
C39 C40 C41 122.0(8) . . yes
C39 C40 Cl15 119.6(8) . . yes
C41 C40 Cl15 118.4(8) . . yes
C42 C41 C40 117.3(8) . . yes
C42 C41 Cl16 119.9(7) . . yes
C40 C41 Cl16 122.8(7) . . yes
O8 C42 C37 113.8(7) . . yes
O8 C42 C41 125.7(8) . . yes
C37 C42 C41 120.5(8) . . yes
C42 O8 P2 111.4(5) . . yes
C43 O9 P2 111.3(5) . . yes
O9 C43 C44 125.6(7) . . yes
O9 C43 C48 113.0(7) . . yes
C44 C43 C48 121.5(7) . . yes
C43 C44 C45 118.7(7) . . yes
C43 C44 Cl17 119.4(6) . . yes
C45 C44 Cl17 121.9(6) . . yes
C44 C45 C46 119.6(7) . . yes
C44 C45 Cl18 120.1(7) . . yes
C46 C45 Cl18 120.3(6) . . yes
C47 C46 C45 120.8(7) . . yes
C47 C46 Cl19 119.7(6) . . yes
C45 C46 Cl19 119.5(6) . . yes
C48 C47 C46 118.1(7) . . yes
C48 C47 Cl20 120.0(6) . . yes
C46 C47 Cl20 121.9(6) . . yes
O10 C48 C43 113.1(7) . . yes
O10 C48 C47 125.8(7) . . yes
C43 C48 C47 121.1(7) . . yes
C48 O10 P2 110.9(5) . . yes
C49 O11 P2 110.4(6) . . yes
O11 C49 C50 124.6(10) . . yes
O11 C49 C54 114.0(8) . . yes
C50 C49 C54 121.3(9) . . yes
C49 C50 C51 118.7(10) . . yes
C49 C50 Cl21 119.3(8) . . yes
C51 C50 Cl21 121.9(8) . . yes
C52 C51 C50 119.8(10) . . yes
C52 C51 Cl22 120.8(9) . . yes
C50 C51 Cl22 119.4(11) . . yes
C51 C52 C53 122.5(9) . . yes
C51 C52 Cl23 119.9(9) . . yes
C53 C52 Cl23 117.6(10) . . yes
C54 C53 C52 116.3(10) . . yes
C54 C53 Cl24 120.2(7) . . yes
C52 C53 Cl24 123.5(8) . . yes
O12 C54 C53 126.2(9) . . yes
O12 C54 C49 112.5(7) . . yes
C53 C54 C49 121.3(9) . . yes
C54 O12 P2 110.9(6) . . yes
C56 C55 H13 109.5 . . no
C56 C55 H14 109.5 . . no
H13 C55 H14 109.5 . . no
C56 C55 H15 109.5 . . no
H13 C55 H15 109.5 . . no
H14 C55 H15 109.5 . . no
N4 C58 C57 170(3) . . yes
C58 C57 H16 109.5 . . no
C58 C57 H17 109.5 . . no
H16 C57 H17 109.5 . . no
C58 C57 H18 109.5 . . no
H16 C57 H18 109.5 . . no
H17 C57 H18 109.5 . . no
C60 C59 H19 109.5 . . no
C60 C59 H20 109.5 . . no
H19 C59 H20 109.5 . . no
C60 C59 H21 109.5 . . no
H19 C59 H21 109.5 . . no
H20 C59 H21 109.5 . . no
N5 C60 C59 167(4) . . yes
N3 C56 C55 165(3) . . yes

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
N7 C61 C1 C2 66.4(11) 2_566 . . . yes
N7 C61 C1 C6 -112.1(11) 2_566 . . . yes
C6 C1 C2 C3 1.9(15) . . . . yes
C61 C1 C2 C3 -176.6(9) . . . . yes
C1 C2 C3 C4 -0.6(16) . . . . yes
C2 C3 C4 C5 -0.9(15) . . . . yes
C2 C3 C4 C62 179.8(9) . . . . yes
C3 C4 C5 C6 1.1(15) . . . . yes
C62 C4 C5 C6 -179.6(9) . . . . yes
C2 C1 C6 C5 -1.7(15) . . . . yes
C61 C1 C6 C5 176.9(9) . . . . yes
C4 C5 C6 C1 0.2(16) . . . . yes
C5 C4 C62 N6 114.6(11) . . . . yes
C3 C4 C62 N6 -66.2(13) . . . . yes
C4 C62 N6 C12 -76.4(12) . . . . yes
C4 C62 N6 C8 103.1(11) . . . . yes
C12 N6 C8 C9 2.8(15) . . . . yes
C62 N6 C8 C9 -176.6(9) . . . . yes
N6 C8 C9 C10 0.8(16) . . . . yes
C8 C9 C10 C11 -3.7(14) . . . . yes
C8 C9 C10 C13 171.2(9) . . . . yes
C9 C10 C11 C12 3.1(14) . . . . yes
C13 C10 C11 C12 -171.9(9) . . . . yes
C8 N6 C12 C11 -3.4(15) . . . . yes
C62 N6 C12 C11 176.1(9) . . . . yes
C10 C11 C12 N6 0.2(16) . . . . yes
C11 C10 C13 C14 147.0(10) . . . . yes
C9 C10 C13 C14 -27.6(14) . . . . yes
C11 C10 C13 C18 -25.0(14) . . . . yes
C9 C10 C13 C18 160.3(9) . . . . yes
C18 C13 C14 C15 4.0(15) . . . . yes
C10 C13 C14 C15 -168.5(9) . . . . yes
C13 C14 C15 N7 1.5(16) . . . . yes
C14 C15 N7 C17 -7.1(15) . . . . yes
C14 C15 N7 C61 165.6(9) . . . 2_566 yes
C15 N7 C17 C18 6.8(16) . . . . yes
C61 N7 C17 C18 -165.5(9) 2_566 . . . yes
N7 C17 C18 C13 -1.0(16) . . . . yes
C14 C13 C18 C17 -4.2(14) . . . . yes
C10 C13 C18 C17 168.0(9) . . . . yes
O3 P1 O1 C19 -177.0(5) . . . . yes
O4 P1 O1 C19 -85.5(5) . . . . yes
O6 P1 O1 C19 95.0(5) . . . . yes
O2 P1 O1 C19 2.7(5) . . . . yes
P1 O1 C19 C24 -3.6(8) . . . . yes
P1 O1 C19 C20 175.8(6) . . . . yes
O1 C19 C20 C21 178.6(7) . . . . yes
C24 C19 C20 C21 -2.1(11) . . . . yes
O1 C19 C20 Cl1 -2.2(11) . . . . yes
C24 C19 C20 Cl1 177.2(6) . . . . yes
C19 C20 C21 C22 -0.7(12) . . . . yes
Cl1 C20 C21 C22 -180.0(7) . . . . yes
C19 C20 C21 Cl2 179.4(6) . . . . yes
Cl1 C20 C21 Cl2 0.1(10) . . . . yes
C20 C21 C22 C23 2.1(13) . . . . yes
Cl2 C21 C22 C23 -178.0(7) . . . . yes
C20 C21 C22 Cl3 -177.7(6) . . . . yes
Cl2 C21 C22 Cl3 2.2(11) . . . . yes
C21 C22 C23 C24 -0.6(13) . . . . yes
Cl3 C22 C23 C24 179.2(6) . . . . yes
C21 C22 C23 Cl4 -177.8(7) . . . . yes
Cl3 C22 C23 Cl4 2.0(10) . . . . yes
C22 C23 C24 O2 178.0(7) . . . . yes
Cl4 C23 C24 O2 -4.7(11) . . . . yes
C22 C23 C24 C19 -2.2(12) . . . . yes
Cl4 C23 C24 C19 175.0(6) . . . . yes
O1 C19 C24 O2 2.8(9) . . . . yes
C20 C19 C24 O2 -176.6(7) . . . . yes
O1 C19 C24 C23 -176.9(7) . . . . yes
C20 C19 C24 C23 3.6(12) . . . . yes
C23 C24 O2 P1 179.0(7) . . . . yes
C19 C24 O2 P1 -0.7(8) . . . . yes
O4 P1 O2 C24 91.7(5) . . . . yes
O5 P1 O2 C24 179.6(5) . . . . yes
O6 P1 O2 C24 -90.0(5) . . . . yes
O1 P1 O2 C24 -1.1(5) . . . . yes
O4 P1 O3 C25 -2.8(5) . . . . yes
O5 P1 O3 C25 -90.7(5) . . . . yes
O6 P1 O3 C25 178.9(5) . . . . yes
O1 P1 O3 C25 89.9(5) . . . . yes
P1 O3 C25 C26 -175.7(6) . . . . yes
P1 O3 C25 C30 2.8(8) . . . . yes
O3 C25 C26 C27 -179.9(7) . . . . yes
C30 C25 C26 C27 1.6(11) . . . . yes
O3 C25 C26 Cl5 1.7(11) . . . . yes
C30 C25 C26 Cl5 -176.8(6) . . . . yes
C25 C26 C27 C28 0.0(11) . . . . yes
Cl5 C26 C27 C28 178.4(6) . . . . yes
C25 C26 C27 Cl6 179.9(6) . . . . yes
Cl5 C26 C27 Cl6 -1.8(9) . . . . yes
C26 C27 C28 C29 -0.5(11) . . . . yes
Cl6 C27 C28 C29 179.7(5) . . . . yes
C26 C27 C28 Cl7 179.8(6) . . . . yes
Cl6 C27 C28 Cl7 -0.1(9) . . . . yes
C27 C28 C29 C30 -0.8(11) . . . . yes
Cl7 C28 C29 C30 179.0(6) . . . . yes
C27 C28 C29 Cl8 -179.7(6) . . . . yes
Cl7 C28 C29 Cl8 0.0(9) . . . . yes
C28 C29 C30 O4 -177.9(7) . . . . yes
Cl8 C29 C30 O4 1.0(10) . . . . yes
C28 C29 C30 C25 2.5(11) . . . . yes
Cl8 C29 C30 C25 -178.6(6) . . . . yes
O3 C25 C30 O4 -1.2(9) . . . . yes
C26 C25 C30 O4 177.4(6) . . . . yes
O3 C25 C30 C29 178.4(6) . . . . yes
C26 C25 C30 C29 -2.9(11) . . . . yes
C29 C30 O4 P1 179.4(6) . . . . yes
C25 C30 O4 P1 -0.9(7) . . . . yes
O3 P1 O4 C30 2.1(5) . . . . yes
O5 P1 O4 C30 96.3(5) . . . . yes
O1 P1 O4 C30 -85.9(5) . . . . yes
O2 P1 O4 C30 -175.6(5) . . . . yes
O3 P1 O5 C31 -81.4(5) . . . . yes
O4 P1 O5 C31 -172.8(4) . . . . yes
O6 P1 O5 C31 6.6(5) . . . . yes
O2 P1 O5 C31 98.9(5) . . . . yes
P1 O5 C31 C32 173.7(6) . . . . yes
P1 O5 C31 C36 -4.9(7) . . . . yes
O5 C31 C32 C33 -179.0(6) . . . . yes
C36 C31 C32 C33 -0.5(10) . . . . yes
O5 C31 C32 Cl9 1.3(10) . . . . yes
C36 C31 C32 Cl9 179.8(5) . . . . yes
C31 C32 C33 C34 0.5(10) . . . . yes
Cl9 C32 C33 C34 -179.8(6) . . . . yes
C31 C32 C33 Cl10 178.9(5) . . . . yes
Cl9 C32 C33 Cl10 -1.4(9) . . . . yes
C32 C33 C34 C35 0.1(11) . . . . yes
Cl10 C33 C34 C35 -178.3(5) . . . . yes
C32 C33 C34 Cl11 179.1(5) . . . . yes
Cl10 C33 C34 Cl11 0.7(9) . . . . yes
C33 C34 C35 C36 -0.7(10) . . . . yes
Cl11 C34 C35 C36 -179.7(5) . . . . yes
C33 C34 C35 Cl12 176.7(5) . . . . yes
Cl11 C34 C35 Cl12 -2.3(8) . . . . yes
O5 C31 C36 O6 -0.2(8) . . . . yes
C32 C31 C36 O6 -178.8(6) . . . . yes
O5 C31 C36 C35 178.6(6) . . . . yes
C32 C31 C36 C35 -0.1(10) . . . . yes
C34 C35 C36 O6 179.3(6) . . . . yes
Cl12 C35 C36 O6 1.8(10) . . . . yes
C34 C35 C36 C31 0.7(10) . . . . yes
Cl12 C35 C36 C31 -176.8(5) . . . . yes
C31 C36 O6 P1 5.2(7) . . . . yes
C35 C36 O6 P1 -173.5(6) . . . . yes
O3 P1 O6 C36 87.6(5) . . . . yes
O5 P1 O6 C36 -6.6(5) . . . . yes
O1 P1 O6 C36 175.6(5) . . . . yes
O2 P1 O6 C36 -94.7(5) . . . . yes
O10 P2 O7 C37 -89.0(5) . . . . yes
O11 P2 O7 C37 90.4(6) . . . . yes
O12 P2 O7 C37 -178.3(5) . . . . yes
O8 P2 O7 C37 3.9(6) . . . . yes
P2 O7 C37 C38 175.1(7) . . . . yes
P2 O7 C37 C42 -4.3(8) . . . . yes
O7 C37 C38 C39 179.8(8) . . . . yes
C42 C37 C38 C39 -0.9(13) . . . . yes
O7 C37 C38 Cl13 1.1(13) . . . . yes
C42 C37 C38 Cl13 -179.6(7) . . . . yes
C37 C38 C39 C40 -1.7(14) . . . . yes
Cl13 C38 C39 C40 176.9(8) . . . . yes
C37 C38 C39 Cl14 178.4(7) . . . . yes
Cl13 C38 C39 Cl14 -2.9(12) . . . . yes
C38 C39 C40 C41 1.8(15) . . . . yes
Cl14 C39 C40 C41 -178.3(7) . . . . yes
C38 C39 C40 Cl15 -177.4(7) . . . . yes
Cl14 C39 C40 Cl15 2.4(12) . . . . yes
C39 C40 C41 C42 0.7(14) . . . . yes
Cl15 C40 C41 C42 179.9(7) . . . . yes
C39 C40 C41 Cl16 178.4(8) . . . . yes
Cl15 C40 C41 Cl16 -2.4(11) . . . . yes
O7 C37 C42 O8 2.4(10) . . . . yes
C38 C37 C42 O8 -177.0(8) . . . . yes
O7 C37 C42 C41 -177.2(7) . . . . yes
C38 C37 C42 C41 3.4(13) . . . . yes
C40 C41 C42 O8 177.3(8) . . . . yes
Cl16 C41 C42 O8 -0.6(12) . . . . yes
C40 C41 C42 C37 -3.2(12) . . . . yes
Cl16 C41 C42 C37 179.0(7) . . . . yes
C37 C42 O8 P2 0.6(9) . . . . yes
C41 C42 O8 P2 -179.8(7) . . . . yes
O10 P2 O8 C42 84.3(6) . . . . yes
O9 P2 O8 C42 175.8(6) . . . . yes
O11 P2 O8 C42 -95.6(6) . . . . yes
O7 P2 O8 C42 -2.5(6) . . . . yes
O10 P2 O9 C43 2.8(5) . . . . yes
O11 P2 O9 C43 -176.6(5) . . . . yes
O12 P2 O9 C43 92.1(5) . . . . yes
O8 P2 O9 C43 -90.0(5) . . . . yes
P2 O9 C43 C44 179.5(6) . . . . yes
P2 O9 C43 C48 -1.9(7) . . . . yes
O9 C43 C44 C45 -176.9(6) . . . . yes
C48 C43 C44 C45 4.5(10) . . . . yes
O9 C43 C44 Cl17 2.9(10) . . . . yes
C48 C43 C44 Cl17 -175.6(5) . . . . yes
C43 C44 C45 C46 -5.5(10) . . . . yes
Cl17 C44 C45 C46 174.7(5) . . . . yes
C43 C44 C45 Cl18 177.1(5) . . . . yes
Cl17 C44 C45 Cl18 -2.7(9) . . . . yes
C44 C45 C46 C47 3.0(10) . . . . yes
Cl18 C45 C46 C47 -179.6(5) . . . . yes
C44 C45 C46 Cl19 -178.4(5) . . . . yes
Cl18 C45 C46 Cl19 -1.0(8) . . . . yes
C45 C46 C47 C48 0.5(10) . . . . yes
Cl19 C46 C47 C48 -178.2(5) . . . . yes
C45 C46 C47 Cl20 -178.9(5) . . . . yes
Cl19 C46 C47 Cl20 2.5(8) . . . . yes
O9 C43 C48 O10 -0.4(9) . . . . yes
C44 C43 C48 O10 178.3(6) . . . . yes
O9 C43 C48 C47 -179.8(6) . . . . yes
C44 C43 C48 C47 -1.1(11) . . . . yes
C46 C47 C48 O10 179.3(6) . . . . yes
Cl20 C47 C48 O10 -1.4(10) . . . . yes
C46 C47 C48 C43 -1.5(10) . . . . yes
Cl20 C47 C48 C43 177.9(5) . . . . yes
C43 C48 O10 P2 2.5(7) . . . . yes
C47 C48 O10 P2 -178.2(6) . . . . yes
O9 P2 O10 C48 -3.0(5) . . . . yes
O12 P2 O10 C48 -96.5(5) . . . . yes
O7 P2 O10 C48 175.1(5) . . . . yes
O8 P2 O10 C48 85.5(5) . . . . yes
O9 P2 O11 C49 -85.5(5) . . . . yes
O12 P2 O11 C49 7.9(5) . . . . yes
O7 P2 O11 C49 96.4(5) . . . . yes
O8 P2 O11 C49 -174.1(5) . . . . yes
P2 O11 C49 C50 175.0(7) . . . . yes
P2 O11 C49 C54 -6.2(8) . . . . yes
O11 C49 C50 C51 179.7(8) . . . . yes
C54 C49 C50 C51 1.0(12) . . . . yes
O11 C49 C50 Cl21 -3.0(11) . . . . yes
C54 C49 C50 Cl21 178.3(6) . . . . yes
C49 C50 C51 C52 -0.2(13) . . . . yes
Cl21 C50 C51 C52 -177.5(7) . . . . yes
C49 C50 C51 Cl22 -179.8(6) . . . . yes
Cl21 C50 C51 Cl22 2.9(11) . . . . yes
C50 C51 C52 C53 -0.9(13) . . . . yes
Cl22 C51 C52 C53 178.7(6) . . . . yes
C50 C51 C52 Cl23 179.6(6) . . . . yes
Cl22 C51 C52 Cl23 -0.8(11) . . . . yes
C51 C52 C53 C54 1.2(12) . . . . yes
Cl23 C52 C53 C54 -179.3(6) . . . . yes
C51 C52 C53 Cl24 -178.7(7) . . . . yes
Cl23 C52 C53 Cl24 0.8(10) . . . . yes
C52 C53 C54 O12 179.9(7) . . . . yes
Cl24 C53 C54 O12 -0.2(11) . . . . yes
C52 C53 C54 C49 -0.5(11) . . . . yes
Cl24 C53 C54 C49 179.4(6) . . . . yes
O11 C49 C54 O12 0.3(10) . . . . yes
C50 C49 C54 O12 179.1(7) . . . . yes
O11 C49 C54 C53 -179.4(7) . . . . yes
C50 C49 C54 C53 -0.6(12) . . . . yes
C53 C54 O12 P2 -174.5(6) . . . . yes
C49 C54 O12 P2 5.8(8) . . . . yes
O10 P2 O12 C54 172.3(5) . . . . yes
O9 P2 O12 C54 80.8(5) . . . . yes
O11 P2 O12 C54 -7.8(5) . . . . yes
O7 P2 O12 C54 -100.9(5) . . . . yes

_diffrn_measured_fraction_theta_max 0.909
_diffrn_reflns_theta_full        28.09
_diffrn_measured_fraction_theta_full 0.909
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.099