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


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#  This CIF contains data from an original supplementary publication 
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#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
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data_lb059s_compound_1a
_database_code_depnum_ccdc_archive 'CCDC 872249'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C66 H86 Cl6 N6 O6'
_chemical_formula_weight         1272.11

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   9.9123(13)
_cell_length_b                   11.7727(16)
_cell_length_c                   14.746(2)
_cell_angle_alpha                73.492(2)
_cell_angle_beta                 73.172(2)
_cell_angle_gamma                86.333(2)
_cell_volume                     1578.9(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3792
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      25.18

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             674
_exptl_absorpt_coefficient_mu    0.329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8992
_exptl_absorpt_correction_T_max  0.9805
_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 SMART APEX CCD'
_diffrn_measurement_method       \w-scan
_diffrn_detector_area_resol_mean 8.26
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19245
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0572
_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       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.80
_diffrn_reflns_theta_max         28.68
_reflns_number_total             7391
_reflns_number_gt                5808
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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.
;

_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^)+(0.0552P)^2^+1.8721P] 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    'NH free, others riding'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7391
_refine_ls_number_parameters     416
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0830
_refine_ls_wR_factor_ref         0.1736
_refine_ls_wR_factor_gt          0.1629
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_restrained_S_all      1.157
_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
N1 N 0.6203(3) 0.6334(2) 0.0768(2) 0.0221(5) Uani 1 1 d . . .
H01 H 0.609(4) 0.692(3) 0.028(3) 0.035(10) Uiso 1 1 d . . .
N2 N 0.6879(3) 1.1784(3) 0.1452(2) 0.0331(7) Uani 1 1 d . . .
H02 H 0.610(4) 1.181(3) 0.135(3) 0.030(10) Uiso 1 1 d . . .
O1 O 0.5412(2) 0.4631(2) 0.19555(17) 0.0323(5) Uani 1 1 d . . .
O2 O 0.9047(3) 1.2577(3) 0.1049(2) 0.0522(8) Uani 1 1 d . . .
C1 C 0.3933(3) 0.5503(3) 0.0945(2) 0.0222(6) Uani 1 1 d . . .
C2 C 0.2926(3) 0.4603(3) 0.1456(3) 0.0318(8) Uani 1 1 d . . .
H2 H 0.3090 0.3985 0.1965 0.038 Uiso 1 1 calc R . .
C3 C 0.1677(3) 0.4628(3) 0.1205(3) 0.0403(9) Uani 1 1 d . . .
H3 H 0.1005 0.4025 0.1548 0.048 Uiso 1 1 calc R . .
C4 C 0.1425(3) 0.5542(3) 0.0452(3) 0.0371(9) Uani 1 1 d . . .
H4 H 0.0577 0.5559 0.0298 0.044 Uiso 1 1 calc R . .
C5 C 0.2433(3) 0.6440(3) -0.0079(3) 0.0273(7) Uani 1 1 d . . .
C6 C 0.3683(3) 0.6416(3) 0.0177(2) 0.0234(6) Uani 1 1 d . . .
H6 H 0.4358 0.7017 -0.0169 0.028 Uiso 1 1 calc R . .
C7 C 0.5253(3) 0.5452(2) 0.1266(2) 0.0196(6) Uani 1 1 d . . .
C8 C 0.7508(3) 0.6440(3) 0.1011(2) 0.0230(6) Uani 1 1 d . . .
H8A H 0.8306 0.6489 0.0434 0.028 Uiso 1 1 calc R . .
H8B H 0.7613 0.5742 0.1525 0.028 Uiso 1 1 calc R . .
C11 C 0.7493(3) 0.7530(3) 0.1358(2) 0.0190(6) Uani 1 1 d . . .
C12 C 0.8250(3) 0.8541(3) 0.0734(2) 0.0196(6) Uani 1 1 d . . .
H12 H 0.8840 0.8524 0.0120 0.024 Uiso 1 1 calc R . .
C13 C 0.8135(3) 0.9582(3) 0.1018(2) 0.0220(6) Uani 1 1 d . . .
H13 H 0.8644 1.0256 0.0590 0.026 Uiso 1 1 calc R . .
C14 C 0.7263(3) 0.9624(3) 0.1939(2) 0.0243(7) Uani 1 1 d . . .
C15 C 0.6544(3) 0.8600(3) 0.2574(2) 0.0288(7) Uani 1 1 d . . .
H15 H 0.5981 0.8609 0.3197 0.035 Uiso 1 1 calc R . .
C16 C 0.6653(3) 0.7561(3) 0.2294(2) 0.0256(7) Uani 1 1 d . . .
H16 H 0.6166 0.6881 0.2730 0.031 Uiso 1 1 calc R . .
C17 C 0.7089(4) 1.0769(3) 0.2232(3) 0.0350(8) Uani 1 1 d . . .
H17A H 0.6287 1.0684 0.2812 0.042 Uiso 1 1 calc R . .
H17B H 0.7921 1.0914 0.2406 0.042 Uiso 1 1 calc R . .
C18 C 0.7902(3) 1.2607(3) 0.0899(3) 0.0339(8) Uani 1 1 d . . .
N3 N 0.7737(3) 0.9876(3) -0.15942(18) 0.0287(6) Uani 1 1 d D . .
O3 O 0.5952(3) 0.85335(19) -0.09074(16) 0.0347(6) Uani 1 1 d . . .
C21 C 0.8545(3) 1.1948(3) -0.2642(2) 0.0305(8) Uani 1 1 d . . .
H21 H 0.9051 1.1640 -0.3196 0.037 Uiso 1 1 calc R A .
C22 C 0.9384(3) 1.3004(4) -0.2668(3) 0.0408(9) Uani 1 1 d . A .
H22A H 1.0321 1.2753 -0.2627 0.049 Uiso 1 1 calc R . .
H22B H 0.8926 1.3290 -0.2100 0.049 Uiso 1 1 calc R . .
C23 C 0.9505(4) 1.4012(4) -0.3610(3) 0.0443(10) Uani 1 1 d . . .
H23A H 0.9972 1.4690 -0.3573 0.053 Uiso 1 1 calc R A .
H23B H 1.0083 1.3761 -0.4170 0.053 Uiso 1 1 calc R . .
C24 C 0.8083(4) 1.4379(3) -0.3770(3) 0.0374(8) Uani 1 1 d . A .
H24A H 0.8215 1.4955 -0.4408 0.045 Uiso 1 1 calc R . .
H24B H 0.7559 1.4750 -0.3268 0.045 Uiso 1 1 calc R . .
C25 C 0.7240(3) 1.3316(3) -0.3725(2) 0.0312(7) Uani 1 1 d . . .
H25A H 0.6309 1.3567 -0.3782 0.037 Uiso 1 1 calc R A .
H25B H 0.7707 1.3002 -0.4276 0.037 Uiso 1 1 calc R . .
C26 C 0.7097(3) 1.2351(3) -0.2767(2) 0.0272(7) Uani 1 1 d . A .
H26A H 0.6573 1.1681 -0.2764 0.033 Uiso 1 1 calc R . .
H26B H 0.6574 1.2647 -0.2217 0.033 Uiso 1 1 calc R . .
C27 C 0.8445(3) 1.0972(4) -0.1685(2) 0.0370(9) Uani 1 1 d . A .
H27A H 0.9392 1.0786 -0.1632 0.044 Uiso 1 1 calc R . .
H27B H 0.7947 1.1276 -0.1135 0.044 Uiso 1 1 calc R . .
C31 C 0.8202(8) 0.8759(6) -0.2828(6) 0.0229(17) Uani 0.524(8) 1 d PD A 1
H31 H 0.7628 0.8053 -0.2411 0.028 Uiso 0.524(8) 1 calc PR A 1
C32 C 0.7281(6) 0.9577(6) -0.3390(4) 0.0236(15) Uani 0.524(8) 1 d PD A 1
H32A H 0.7799 1.0307 -0.3787 0.028 Uiso 0.524(8) 1 calc PR A 1
H32B H 0.6449 0.9774 -0.2926 0.028 Uiso 0.524(8) 1 calc PR A 1
C33 C 0.6839(9) 0.8980(6) -0.4054(6) 0.0303(18) Uani 0.524(8) 1 d PD A 1
H33A H 0.6271 0.8278 -0.3650 0.036 Uiso 0.524(8) 1 calc PR A 1
H33B H 0.6264 0.9517 -0.4411 0.036 Uiso 0.524(8) 1 calc PR A 1
C34 C 0.8097(8) 0.8633(8) -0.4782(5) 0.040(2) Uani 0.524(8) 1 d PD A 1
H34A H 0.8639 0.9337 -0.5214 0.048 Uiso 0.524(8) 1 calc PR A 1
H34B H 0.7777 0.8247 -0.5185 0.048 Uiso 0.524(8) 1 calc PR A 1
C35 C 0.9020(10) 0.7799(6) -0.4241(6) 0.044(2) Uani 0.524(8) 1 d PD A 1
H35A H 0.9854 0.7625 -0.4717 0.053 Uiso 0.524(8) 1 calc PR A 1
H35B H 0.8508 0.7060 -0.3867 0.053 Uiso 0.524(8) 1 calc PR A 1
C36 C 0.9465(7) 0.8345(9) -0.3542(5) 0.0301(19) Uani 0.524(8) 1 d PD A 1
H36A H 1.0096 0.9016 -0.3929 0.036 Uiso 0.524(8) 1 calc PR A 1
H36B H 0.9979 0.7764 -0.3165 0.036 Uiso 0.524(8) 1 calc PR A 1
C37 C 0.8763(6) 0.9253(6) -0.2154(4) 0.0189(13) Uani 0.524(8) 1 d PD A 1
H37A H 0.9102 0.8604 -0.1706 0.023 Uiso 0.524(8) 1 calc PR A 1
H37B H 0.9558 0.9782 -0.2552 0.023 Uiso 0.524(8) 1 calc PR A 1
C31' C 0.8519(9) 0.8941(8) -0.3099(6) 0.020(2) Uiso 0.476(8) 1 d PD A 2
H31' H 0.9001 0.9696 -0.3502 0.024 Uiso 0.476(8) 1 calc PR A 2
C32' C 0.7081(7) 0.8937(7) -0.3288(5) 0.0222(16) Uiso 0.476(8) 1 d PD A 2
H32C H 0.6574 0.8204 -0.2884 0.027 Uiso 0.476(8) 1 calc PR A 2
H32D H 0.6532 0.9590 -0.3103 0.027 Uiso 0.476(8) 1 calc PR A 2
C33' C 0.7258(10) 0.9053(8) -0.4373(6) 0.026(2) Uiso 0.476(8) 1 d PD A 2
H33C H 0.6339 0.9025 -0.4475 0.031 Uiso 0.476(8) 1 calc PR A 2
H33D H 0.7702 0.9813 -0.4772 0.031 Uiso 0.476(8) 1 calc PR A 2
C34' C 0.8152(8) 0.8065(8) -0.4696(6) 0.029(2) Uiso 0.476(8) 1 d PD A 2
H34C H 0.8296 0.8186 -0.5397 0.035 Uiso 0.476(8) 1 calc PR A 2
H34D H 0.7658 0.7312 -0.4348 0.035 Uiso 0.476(8) 1 calc PR A 2
C35' C 0.9579(8) 0.8024(7) -0.4491(6) 0.0252(19) Uiso 0.476(8) 1 d PD A 2
H35C H 1.0089 0.7341 -0.4648 0.030 Uiso 0.476(8) 1 calc PR A 2
H35D H 1.0129 0.8730 -0.4910 0.030 Uiso 0.476(8) 1 calc PR A 2
C36' C 0.9406(10) 0.7947(8) -0.3422(7) 0.026(3) Uiso 0.476(8) 1 d PD A 2
H36C H 1.0329 0.7981 -0.3326 0.032 Uiso 0.476(8) 1 calc PR A 2
H36D H 0.8965 0.7192 -0.3010 0.032 Uiso 0.476(8) 1 calc PR A 2
C37' C 0.8419(8) 0.8819(7) -0.2019(5) 0.0187(17) Uiso 0.476(8) 1 d PD A 2
H37C H 0.9362 0.8712 -0.1944 0.022 Uiso 0.476(8) 1 calc PR A 2
H37D H 0.7878 0.8103 -0.1616 0.022 Uiso 0.476(8) 1 calc PR A 2
C38 C 0.6448(3) 0.9507(3) -0.0995(2) 0.0239(6) Uani 1 1 d . A .
C39 C 0.5581(3) 1.0327(3) -0.0426(2) 0.0238(6) Uani 1 1 d . . .
H39A H 0.6191 1.0709 -0.0186 0.029 Uiso 1 1 calc R A .
H39B H 0.5184 1.0939 -0.0865 0.029 Uiso 1 1 calc R . .
C99 C 0.6116(4) 0.3359(3) 0.3830(3) 0.0320(7) Uani 1 1 d . . .
H99 H 0.5941 0.3389 0.3202 0.038 Uiso 1 1 calc R . .
Cl1 Cl 0.45942(12) 0.37839(9) 0.46050(9) 0.0595(3) Uani 1 1 d . . .
Cl2 Cl 0.65274(9) 0.18984(7) 0.43887(7) 0.0342(2) Uani 1 1 d . . .
Cl3 Cl 0.75275(13) 0.43282(9) 0.36019(9) 0.0617(4) Uani 1 1 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
N1 0.0191(12) 0.0183(12) 0.0286(14) 0.0011(11) -0.0138(11) 0.0008(10)
N2 0.0314(15) 0.0359(16) 0.0520(19) -0.0271(15) -0.0318(14) 0.0203(13)
O1 0.0351(12) 0.0278(12) 0.0317(13) 0.0034(10) -0.0166(10) -0.0043(10)
O2 0.0258(13) 0.090(2) 0.0518(17) -0.0249(16) -0.0263(12) 0.0140(13)
C1 0.0189(14) 0.0185(14) 0.0350(17) -0.0163(13) -0.0086(12) 0.0041(11)
C2 0.0214(15) 0.0196(15) 0.057(2) -0.0190(15) -0.0076(15) 0.0031(12)
C3 0.0209(16) 0.0243(17) 0.083(3) -0.0302(19) -0.0115(17) 0.0005(13)
C4 0.0163(15) 0.0360(19) 0.080(3) -0.043(2) -0.0203(16) 0.0104(13)
C5 0.0207(15) 0.0322(17) 0.0453(19) -0.0300(15) -0.0181(14) 0.0132(13)
C6 0.0193(14) 0.0268(15) 0.0310(17) -0.0155(13) -0.0109(12) 0.0040(12)
C7 0.0185(13) 0.0189(14) 0.0231(15) -0.0086(12) -0.0065(11) 0.0032(11)
C8 0.0176(14) 0.0230(15) 0.0306(17) -0.0052(13) -0.0127(12) 0.0027(11)
C11 0.0139(13) 0.0238(14) 0.0217(14) -0.0057(12) -0.0100(11) 0.0039(11)
C12 0.0148(13) 0.0267(15) 0.0171(14) -0.0053(12) -0.0055(11) 0.0021(11)
C13 0.0193(14) 0.0264(15) 0.0253(15) -0.0090(13) -0.0124(12) 0.0018(12)
C14 0.0203(14) 0.0342(17) 0.0279(16) -0.0161(14) -0.0163(12) 0.0133(12)
C15 0.0189(14) 0.049(2) 0.0182(15) -0.0118(15) -0.0058(12) 0.0137(14)
C16 0.0181(14) 0.0345(17) 0.0203(15) -0.0011(13) -0.0065(12) 0.0027(12)
C17 0.0367(18) 0.043(2) 0.044(2) -0.0274(17) -0.0287(16) 0.0229(16)
C18 0.0281(17) 0.048(2) 0.043(2) -0.0326(18) -0.0211(15) 0.0200(16)
N3 0.0183(12) 0.0467(17) 0.0167(12) -0.0053(12) -0.0050(10) 0.0166(12)
O3 0.0578(16) 0.0195(11) 0.0200(11) -0.0053(9) -0.0027(10) 0.0093(10)
C21 0.0136(14) 0.057(2) 0.0172(15) -0.0048(15) -0.0023(11) -0.0056(14)
C22 0.0186(15) 0.077(3) 0.0261(18) -0.0111(18) -0.0056(13) -0.0116(17)
C23 0.0341(19) 0.067(3) 0.0287(19) -0.0093(18) -0.0020(15) -0.0288(18)
C24 0.041(2) 0.043(2) 0.0246(17) -0.0047(15) -0.0043(15) -0.0157(16)
C25 0.0264(16) 0.0410(19) 0.0237(16) -0.0012(14) -0.0094(13) -0.0074(14)
C26 0.0186(14) 0.0381(18) 0.0210(15) 0.0000(14) -0.0068(12) -0.0044(13)
C27 0.0111(14) 0.070(3) 0.0214(16) 0.0028(16) -0.0051(12) -0.0065(15)
C31 0.018(3) 0.015(3) 0.029(4) -0.005(3) 0.001(3) 0.005(3)
C32 0.021(3) 0.024(4) 0.026(3) -0.009(3) -0.007(2) 0.001(2)
C33 0.035(4) 0.025(4) 0.029(4) -0.005(3) -0.006(4) -0.011(3)
C34 0.059(5) 0.035(5) 0.025(4) -0.005(3) -0.008(3) -0.019(4)
C35 0.047(5) 0.030(4) 0.045(5) -0.022(4) 0.013(4) -0.005(4)
C36 0.025(4) 0.029(5) 0.024(4) -0.008(3) 0.012(3) 0.002(3)
C37 0.012(3) 0.017(3) 0.025(3) -0.003(2) -0.002(2) 0.000(2)
C38 0.0300(16) 0.0195(15) 0.0145(14) 0.0016(12) -0.0034(12) 0.0117(12)
C39 0.0215(14) 0.0169(14) 0.0245(16) -0.0034(12) 0.0034(12) 0.0037(11)
C99 0.0387(18) 0.0246(16) 0.0365(19) -0.0005(14) -0.0236(15) -0.0021(14)
Cl1 0.0639(7) 0.0442(6) 0.0816(8) -0.0301(6) -0.0311(6) 0.0289(5)
Cl2 0.0383(5) 0.0242(4) 0.0449(5) -0.0103(4) -0.0196(4) 0.0068(3)
Cl3 0.0726(7) 0.0464(6) 0.0665(7) 0.0226(5) -0.0514(6) -0.0303(5)

_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
N1 C7 1.340(4) . ?
N1 C8 1.460(3) . ?
N2 C18 1.353(5) . ?
N2 C17 1.457(4) . ?
O1 C7 1.227(4) . ?
O2 C18 1.214(4) . ?
C1 C2 1.390(4) . ?
C1 C6 1.391(4) . ?
C1 C7 1.508(4) . ?
C2 C3 1.387(5) . ?
C3 C4 1.378(6) . ?
C4 C5 1.393(5) . ?
C5 C6 1.393(4) . ?
C5 C18 1.498(5) 2_675 ?
C8 C11 1.508(4) . ?
C11 C12 1.385(4) . ?
C11 C16 1.400(4) . ?
C12 C13 1.392(4) . ?
C13 C14 1.395(4) . ?
C14 C15 1.386(5) . ?
C14 C17 1.513(4) . ?
C15 C16 1.386(5) . ?
C18 C5 1.498(5) 2_675 ?
N3 C38 1.342(4) . ?
N3 C37 1.420(6) . ?
N3 C27 1.463(5) . ?
N3 C37' 1.577(7) . ?
O3 C38 1.234(4) . ?
C21 C22 1.525(5) . ?
C21 C27 1.527(5) . ?
C21 C26 1.528(4) . ?
C22 C23 1.529(5) . ?
C23 C24 1.512(5) . ?
C24 C25 1.524(5) . ?
C25 C26 1.516(4) . ?
C31 C32 1.523(8) . ?
C31 C37 1.524(8) . ?
C31 C36 1.538(9) . ?
C32 C33 1.525(8) . ?
C33 C34 1.511(10) . ?
C34 C35 1.516(10) . ?
C35 C36 1.531(9) . ?
C31' C36' 1.520(10) . ?
C31' C32' 1.530(9) . ?
C31' C37' 1.532(9) . ?
C32' C33' 1.525(10) . ?
C33' C34' 1.518(10) . ?
C34' C35' 1.525(9) . ?
C35' C36' 1.512(10) . ?
C38 C39 1.520(4) . ?
C39 C39 1.490(5) 2_675 ?
C99 Cl1 1.750(4) . ?
C99 Cl3 1.756(3) . ?
C99 Cl2 1.761(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 N1 C8 123.5(2) . . ?
C18 N2 C17 122.8(3) . . ?
C2 C1 C6 119.5(3) . . ?
C2 C1 C7 117.8(3) . . ?
C6 C1 C7 122.7(3) . . ?
C3 C2 C1 120.0(3) . . ?
C4 C3 C2 120.4(3) . . ?
C3 C4 C5 120.5(3) . . ?
C4 C5 C6 119.0(3) . . ?
C4 C5 C18 117.5(3) . 2_675 ?
C6 C5 C18 123.4(3) . 2_675 ?
C1 C6 C5 120.7(3) . . ?
O1 C7 N1 123.4(3) . . ?
O1 C7 C1 119.9(3) . . ?
N1 C7 C1 116.7(2) . . ?
N1 C8 C11 110.5(2) . . ?
C12 C11 C16 118.8(3) . . ?
C12 C11 C8 120.5(3) . . ?
C16 C11 C8 120.6(3) . . ?
C11 C12 C13 120.6(3) . . ?
C12 C13 C14 120.6(3) . . ?
C15 C14 C13 118.6(3) . . ?
C15 C14 C17 120.7(3) . . ?
C13 C14 C17 120.7(3) . . ?
C14 C15 C16 121.0(3) . . ?
C15 C16 C11 120.4(3) . . ?
N2 C17 C14 112.8(3) . . ?
O2 C18 N2 122.0(3) . . ?
O2 C18 C5 121.0(4) . 2_675 ?
N2 C18 C5 116.9(3) . 2_675 ?
C38 N3 C37 128.9(4) . . ?
C38 N3 C27 125.2(3) . . ?
C37 N3 C27 105.4(4) . . ?
C38 N3 C37' 107.2(4) . . ?
C37 N3 C37' 21.7(3) . . ?
C27 N3 C37' 126.8(4) . . ?
C22 C21 C27 109.6(3) . . ?
C22 C21 C26 109.7(3) . . ?
C27 C21 C26 112.5(2) . . ?
C21 C22 C23 111.7(3) . . ?
C24 C23 C22 112.3(3) . . ?
C23 C24 C25 111.2(3) . . ?
C26 C25 C24 111.2(3) . . ?
C25 C26 C21 110.9(2) . . ?
N3 C27 C21 115.2(3) . . ?
C32 C31 C37 116.4(5) . . ?
C32 C31 C36 110.7(7) . . ?
C37 C31 C36 108.0(6) . . ?
C31 C32 C33 110.4(5) . . ?
C34 C33 C32 111.9(6) . . ?
C33 C34 C35 110.3(6) . . ?
C34 C35 C36 111.2(6) . . ?
C35 C36 C31 112.6(6) . . ?
N3 C37 C31 113.2(5) . . ?
C36' C31' C32' 109.9(7) . . ?
C36' C31' C37' 109.3(7) . . ?
C32' C31' C37' 113.3(7) . . ?
C33' C32' C31' 110.5(6) . . ?
C34' C33' C32' 111.0(7) . . ?
C33' C34' C35' 111.4(7) . . ?
C36' C35' C34' 111.2(7) . . ?
C35' C36' C31' 112.3(7) . . ?
C31' C37' N3 116.9(6) . . ?
O3 C38 N3 121.7(3) . . ?
O3 C38 C39 119.8(3) . . ?
N3 C38 C39 118.5(3) . . ?
C39 C39 C38 111.8(3) 2_675 . ?
Cl1 C99 Cl3 110.11(19) . . ?
Cl1 C99 Cl2 109.32(19) . . ?
Cl3 C99 Cl2 110.18(18) . . ?

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
N1 H01 O3 0.87(4) 2.21(4) 3.084(3) 173(3) .
N2 H02 O3 0.82(4) 2.40(4) 3.204(4) 165(3) 2_675
C6 H6 O3 0.93 2.27 3.193(4) 175.6 .
C37 H37A O2 0.97 2.49 3.385(6) 154.2 2_775
C99 H99 O1 0.98 2.17 3.000(4) 141.0 .

_diffrn_measured_fraction_theta_max 0.907
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.068