# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2007

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Philip Gale'
_publ_contact_author_address     
;
Department of Chemistry
University of Southampton
Southampton
SO17 1BJ
UNITED KINGDOM
;

_publ_contact_author_email       PHILIP.GALE@SOTON.AC.UK

_publ_section_title              
;
Acridinone-based anion receptors and sensors
;
loop_
_publ_author_name
'Philip Gale'
'Claudia Caltagirone'
'Sergio E. Garcia-Garrido'
'Mark E. Light'

# Attachment 'Gale.cif'

data_2006sot0587
_database_code_depnum_ccdc_archive 'CCDC 629281'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H54 N4 O3'
_chemical_formula_weight         674.90

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'

_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                   11.0115(7)
_cell_length_b                   13.5609(7)
_cell_length_c                   13.9492(7)
_cell_angle_alpha                86.153(3)
_cell_angle_beta                 73.058(3)
_cell_angle_gamma                72.371(2)
_cell_volume                     1898.49(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    8228
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      27.48

_exptl_crystal_description       Shard
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             728
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9753
_exptl_absorpt_correction_T_max  0.9948
_exptl_absorpt_process_details   
;
SADABS V2.10 (Sheldrick, G.M., 2003)
;

_exptl_special_details           
;
SADABS was used to perform the Absorption correction
Parameter refinement on 12469 reflections reduced R(int) from 0.0605 to 0.0409
Ratio of minimum to maximum apparent transmission: 0.719213
The given Tmin and Tmax were generated using the SHELX SIZE command
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker Nonius FR591 Rotating Anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans to fill the asymmetric unit'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29200
_diffrn_reflns_av_R_equivalents  0.0809
_diffrn_reflns_av_sigmaI/netI    0.1344
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         27.48
_reflns_number_total             8676
_reflns_number_gt                3994
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin, et al., 1993)'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_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^)+(0.1133P)^2^+0.0000P] 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    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0184(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         8676
_refine_ls_number_parameters     484
_refine_ls_number_restraints     74
_refine_ls_R_factor_all          0.1800
_refine_ls_R_factor_gt           0.0695
_refine_ls_wR_factor_ref         0.2056
_refine_ls_wR_factor_gt          0.1579
_refine_ls_goodness_of_fit_ref   0.929
_refine_ls_restrained_S_all      0.931
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.001

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 0.06769(8) 0.17931(6) 0.40091(5) 0.0411(3) Uani 1 1 d . . .
H991 H 0.0463 0.1572 0.3520 0.049 Uiso 1 1 calc R . .
N2 N 0.15386(7) 0.19723(6) 0.20867(5) 0.0316(2) Uani 1 1 d . . .
N3 N 0.02669(7) 0.13279(6) 0.10379(5) 0.0340(2) Uani 1 1 d . . .
H993 H 0.0314 0.1143 0.1646 0.041 Uiso 1 1 calc R . .
O1 O 0.00913(7) 0.19049(6) 0.57135(5) 0.0511(2) Uani 1 1 d . . .
O2 O 0.45482(7) 0.33149(5) 0.07724(5) 0.0484(2) Uani 1 1 d . . .
O3 O -0.08658(6) 0.12812(5) -0.00774(4) 0.0438(2) Uani 1 1 d . . .
C1 C -0.18605(11) 0.08745(8) 0.57053(7) 0.0464(4) Uani 1 1 d . . .
H1 H -0.1414 0.0628 0.6202 0.056 Uiso 1 1 calc R . .
C2 C -0.30174(12) 0.06309(9) 0.57473(8) 0.0570(4) Uani 1 1 d . . .
H2 H -0.3355 0.0212 0.6267 0.068 Uiso 1 1 calc R . .
C3 C -0.36702(11) 0.10013(9) 0.50295(8) 0.0564(4) Uani 1 1 d . . .
H3 H -0.4462 0.0842 0.5058 0.068 Uiso 1 1 calc R . .
C4 C -0.31736(10) 0.16038(9) 0.42694(8) 0.0500(4) Uani 1 1 d . . .
H4 H -0.3628 0.1860 0.3779 0.060 Uiso 1 1 calc R . .
C5 C -0.20292(9) 0.18338(8) 0.42194(7) 0.0415(3) Uani 1 1 d . . .
H5 H -0.1688 0.2241 0.3688 0.050 Uiso 1 1 calc R . .
C6 C -0.13612(10) 0.14759(8) 0.49402(7) 0.0397(3) Uani 1 1 d . . .
C7 C -0.01350(10) 0.17400(8) 0.49312(7) 0.0399(3) Uani 1 1 d . . .
C8 C 0.18065(9) 0.21421(7) 0.36957(7) 0.0360(3) Uani 1 1 d . . .
C9 C 0.24432(9) 0.23953(8) 0.43041(7) 0.0424(3) Uani 1 1 d . . .
H9 H 0.2154 0.2313 0.5008 0.051 Uiso 1 1 calc R . .
C10 C 0.35262(10) 0.27772(8) 0.38836(7) 0.0445(3) Uani 1 1 d . . .
H10 H 0.3976 0.2944 0.4307 0.053 Uiso 1 1 calc R . .
C11 C 0.39489(10) 0.29148(7) 0.28718(7) 0.0417(3) Uani 1 1 d . . .
H11 H 0.4684 0.3177 0.2602 0.050 Uiso 1 1 calc R . .
C12 C 0.32979(9) 0.26683(7) 0.22277(7) 0.0353(3) Uani 1 1 d . . .
C13 C 0.22345(9) 0.22558(7) 0.26260(7) 0.0328(3) Uani 1 1 d . . .
C14 C 0.36549(9) 0.28906(7) 0.11663(7) 0.0356(3) Uani 1 1 d . . .
C15 C 0.28703(9) 0.26266(7) 0.06040(7) 0.0338(3) Uani 1 1 d . . .
C16 C 0.30903(10) 0.28272(7) -0.04339(7) 0.0404(3) Uani 1 1 d . . .
H16 H 0.3722 0.3178 -0.0758 0.049 Uiso 1 1 calc R . .
C17 C 0.24090(10) 0.25251(8) -0.09723(7) 0.0423(3) Uani 1 1 d . . .
H17 H 0.2576 0.2664 -0.1668 0.051 Uiso 1 1 calc R . .
C18 C 0.14602(10) 0.20097(7) -0.05137(7) 0.0377(3) Uani 1 1 d . . .
H18 H 0.1008 0.1785 -0.0900 0.045 Uiso 1 1 calc R . .
C19 C 0.11952(9) 0.18350(7) 0.04951(7) 0.0323(3) Uani 1 1 d . . .
C20 C 0.18904(9) 0.21507(7) 0.10863(6) 0.0308(3) Uani 1 1 d . . .
C21 C -0.06902(9) 0.10860(7) 0.07495(6) 0.0336(3) Uani 1 1 d . . .
C22 C -0.15615(9) 0.05891(7) 0.15276(6) 0.0330(3) Uani 1 1 d . . .
C23 C -0.28773(9) 0.08032(8) 0.15301(7) 0.0404(3) Uani 1 1 d . . .
H23 H -0.3210 0.1284 0.1072 0.048 Uiso 1 1 calc R . .
C24 C -0.37028(10) 0.03228(8) 0.21926(7) 0.0436(3) Uani 1 1 d . . .
H24 H -0.4610 0.0491 0.2205 0.052 Uiso 1 1 calc R . .
C25 C -0.32227(10) -0.04029(8) 0.28410(7) 0.0445(3) Uani 1 1 d . . .
H25 H -0.3788 -0.0751 0.3281 0.053 Uiso 1 1 calc R . .
C26 C -0.19119(10) -0.06198(7) 0.28456(7) 0.0403(3) Uani 1 1 d . . .
H26 H -0.1580 -0.1111 0.3296 0.048 Uiso 1 1 calc R . .
C27 C -0.10868(9) -0.01243(7) 0.21982(6) 0.0346(3) Uani 1 1 d . . .
H27 H -0.0191 -0.0270 0.2210 0.042 Uiso 1 1 calc R . .
N4 N 0.76628(7) 0.36534(6) -0.18772(5) 0.0363(2) Uani 1 1 d D . .
C32 C 0.79202(3) 0.24802(3) -0.18492(7) 0.0346(3) Uani 1 1 d D A .
H32A H 0.8399 0.2191 -0.2536 0.042 Uiso 1 1 calc R . .
H32B H 0.8516 0.2190 -0.1422 0.042 Uiso 1 1 calc R . .
C33 C 0.66964(3) 0.21157(2) -0.14646(7) 0.0371(3) Uani 1 1 d D . .
H33A H 0.6130 0.2339 -0.1923 0.045 Uiso 1 1 calc R A .
H33B H 0.6174 0.2432 -0.0794 0.045 Uiso 1 1 calc R . .
C34 C 0.71011(3) 0.09353(2) -0.13966(6) 0.0357(3) Uani 1 1 d D A .
H34A H 0.7631 0.0627 -0.2069 0.043 Uiso 1 1 calc R . .
H34B H 0.7673 0.0720 -0.0942 0.043 Uiso 1 1 calc R . .
C35 C 0.59391(4) 0.05285(3) -0.10237(9) 0.0616(4) Uani 1 1 d D . .
H35A H 0.5447 0.0791 -0.0339 0.092 Uiso 1 1 calc R A .
H35B H 0.6250 -0.0230 -0.1027 0.092 Uiso 1 1 calc R . .
H35C H 0.5356 0.0756 -0.1460 0.092 Uiso 1 1 calc R . .
C36 C 0.66569(9) 0.41655(8) -0.24448(7) 0.0406(3) Uani 1 1 d . A .
H36A H 0.5801 0.4040 -0.2082 0.049 Uiso 1 1 calc R . .
H36B H 0.6512 0.4922 -0.2429 0.049 Uiso 1 1 calc R . .
C37 C 0.70171(10) 0.38164(9) -0.35228(7) 0.0527(4) Uani 1 1 d . . .
H37A H 0.7275 0.3051 -0.3563 0.063 Uiso 1 1 calc R A .
H37B H 0.7787 0.4040 -0.3923 0.063 Uiso 1 1 calc R . .
C38 C 0.58360(11) 0.42759(9) -0.39576(8) 0.0559(4) Uani 1 1 d . A .
H38A H 0.5474 0.5027 -0.3795 0.067 Uiso 1 1 calc R . .
H38B H 0.6160 0.4192 -0.4697 0.067 Uiso 1 1 calc R . .
C39 C 0.47304(11) 0.37843(9) -0.35700(8) 0.0586(4) Uani 1 1 d . . .
H39A H 0.5086 0.3036 -0.3704 0.088 Uiso 1 1 calc R A .
H39B H 0.4039 0.4080 -0.3908 0.088 Uiso 1 1 calc R . .
H39C H 0.4348 0.3918 -0.2846 0.088 Uiso 1 1 calc R . .
C28A C 0.70904(4) 0.40615(11) -0.07878(3) 0.0374(2) Uani 0.50 1 d PDU A 1
H28A H 0.6883 0.4824 -0.0808 0.045 Uiso 0.50 1 calc PR A 1
H28B H 0.6233 0.3908 -0.0513 0.045 Uiso 0.50 1 calc PR A 1
C29A C 0.78752(5) 0.36925(7) -0.00351(2) 0.0491(3) Uani 0.50 1 d PDU A 1
H29A H 0.8723 0.3867 -0.0265 0.059 Uiso 0.50 1 calc PR A 1
H29B H 0.8086 0.2931 0.0018 0.059 Uiso 0.50 1 calc PR A 1
C30A C 0.70696(6) 0.42052(6) 0.09917(2) 0.0531(3) Uani 0.50 1 d PDU A 1
H30A H 0.7022 0.4947 0.0964 0.064 Uiso 0.50 1 calc PR A 1
H30B H 0.6151 0.4162 0.1145 0.064 Uiso 0.50 1 calc PR A 1
C31A C 0.76426(7) 0.37226(10) 0.18133(3) 0.0694(5) Uani 0.50 1 d PDU A 1
H31A H 0.7592 0.3011 0.1900 0.104 Uiso 0.50 1 calc PR A 1
H31B H 0.7139 0.4123 0.2438 0.104 Uiso 0.50 1 calc PR A 1
H31C H 0.8574 0.3715 0.1644 0.104 Uiso 0.50 1 calc PR A 1
C28B C 0.70423(4) 0.42222(13) -0.08735(3) 0.0374(2) Uani 0.50 1 d PDU A 2
H28C H 0.6223 0.4038 -0.0519 0.045 Uiso 0.50 1 calc PR A 2
H28D H 0.6788 0.4977 -0.0984 0.045 Uiso 0.50 1 calc PR A 2
C29B C 0.79789(4) 0.39641(10) -0.02222(2) 0.0491(3) Uani 0.50 1 d PDU A 2
H29C H 0.8663 0.4328 -0.0466 0.059 Uiso 0.50 1 calc PR A 2
H29D H 0.8434 0.3210 -0.0264 0.059 Uiso 0.50 1 calc PR A 2
C30B C 0.72023(4) 0.42930(10) 0.08670(2) 0.0531(3) Uani 0.50 1 d PDU A 2
H30C H 0.6672 0.5030 0.0890 0.064 Uiso 0.50 1 calc PR A 2
H30D H 0.6575 0.3880 0.1122 0.064 Uiso 0.50 1 calc PR A 2
C31B C 0.80723(4) 0.41572(14) 0.15351(3) 0.0694(5) Uani 0.50 1 d PDU A 2
H31D H 0.8591 0.3427 0.1524 0.104 Uiso 0.50 1 calc PR A 2
H31E H 0.7523 0.4373 0.2221 0.104 Uiso 0.50 1 calc PR A 2
H31F H 0.8677 0.4581 0.1300 0.104 Uiso 0.50 1 calc PR A 2
C40A C 0.90112(8) 0.38504(3) -0.2399(2) 0.0460(3) Uani 0.33 1 d PDU A 3
H40A H 0.9657 0.3505 -0.2025 0.055 Uiso 0.33 1 calc PR A 3
H40B H 0.9358 0.3543 -0.3086 0.055 Uiso 0.33 1 calc PR A 3
C41A C 0.88831(3) 0.49960(3) -0.24555(6) 0.0594(3) Uani 0.33 1 d PDU A 3
H41A H 0.8565 0.5303 -0.1770 0.071 Uiso 0.33 1 calc PR A 3
H41B H 0.8224 0.5348 -0.2817 0.071 Uiso 0.33 1 calc PR A 3
C42A C 1.02289(4) 0.51579(5) -0.30020(3) 0.0623(2) Uani 0.33 1 d PDU A 3
H42A H 1.0178 0.5887 -0.2902 0.075 Uiso 0.33 1 calc PR A 3
H42B H 1.0912 0.4713 -0.2701 0.075 Uiso 0.33 1 calc PR A 3
C43A C 1.06493(12) 0.49167(13) -0.40953(3) 0.0707(3) Uani 0.33 1 d PDU A 3
H43A H 1.0539 0.4246 -0.4203 0.106 Uiso 0.33 1 calc PR A 3
H43B H 1.1585 0.4888 -0.4378 0.106 Uiso 0.33 1 calc PR A 3
H43C H 1.0101 0.5456 -0.4425 0.106 Uiso 0.33 1 calc PR A 3
C40B C 0.90026(6) 0.37799(3) -0.23859(10) 0.0460(3) Uani 0.67 1 d PDU A 4
H40C H 0.9359 0.3370 -0.3021 0.055 Uiso 0.67 1 calc PR A 4
H40D H 0.9587 0.3454 -0.1959 0.055 Uiso 0.67 1 calc PR A 4
C41B C 0.91607(3) 0.48478(3) -0.26355(8) 0.0594(3) Uani 0.67 1 d PDU A 4
H41C H 0.8913 0.5257 -0.2009 0.071 Uiso 0.67 1 calc PR A 4
H41D H 0.8562 0.5212 -0.3040 0.071 Uiso 0.67 1 calc PR A 4
C42B C 1.06025(4) 0.47542(3) -0.32224(7) 0.0623(2) Uani 0.67 1 d PDU A 4
H42C H 1.1174 0.4494 -0.2773 0.075 Uiso 0.67 1 calc PR A 4
H42D H 1.0892 0.4239 -0.3776 0.075 Uiso 0.67 1 calc PR A 4
C43B C 1.07997(7) 0.57469(3) -0.36473(8) 0.0707(3) Uani 0.67 1 d PDU A 4
H43D H 1.0251 0.6004 -0.4105 0.106 Uiso 0.67 1 calc PR A 4
H43E H 1.1738 0.5636 -0.4015 0.106 Uiso 0.67 1 calc PR A 4
H43F H 1.0540 0.6256 -0.3103 0.106 Uiso 0.67 1 calc PR A 4

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 0.0441(4) 0.0573(5) 0.0278(4) -0.0036(3) -0.0119(3) -0.0212(4)
N2 0.0308(4) 0.0330(4) 0.0299(4) -0.0008(3) -0.0084(3) -0.0079(3)
N3 0.0370(4) 0.0401(4) 0.0260(3) 0.0018(3) -0.0087(3) -0.0137(3)
O1 0.0480(4) 0.0745(5) 0.0302(3) -0.0030(3) -0.0150(3) -0.0127(3)
O2 0.0406(4) 0.0496(4) 0.0541(4) -0.0009(3) -0.0042(3) -0.0207(3)
O3 0.0512(3) 0.0540(4) 0.0340(3) 0.0088(3) -0.0209(2) -0.0202(3)
C1 0.0486(6) 0.0519(6) 0.0337(5) -0.0021(5) -0.0027(4) -0.0159(5)
C2 0.0618(7) 0.0499(6) 0.0481(6) -0.0051(5) 0.0073(6) -0.0213(5)
C3 0.0448(6) 0.0689(7) 0.0519(6) -0.0205(5) 0.0015(5) -0.0217(5)
C4 0.0409(5) 0.0667(7) 0.0408(5) -0.0112(5) -0.0056(4) -0.0170(5)
C5 0.0383(5) 0.0554(6) 0.0297(5) -0.0035(4) -0.0056(4) -0.0153(4)
C6 0.0390(5) 0.0483(6) 0.0279(5) -0.0061(4) -0.0022(4) -0.0131(4)
C7 0.0392(5) 0.0501(6) 0.0274(4) 0.0008(4) -0.0107(4) -0.0079(5)
C8 0.0350(5) 0.0360(5) 0.0381(5) -0.0025(4) -0.0133(4) -0.0088(4)
C9 0.0410(5) 0.0489(6) 0.0385(5) -0.0014(4) -0.0149(4) -0.0110(4)
C10 0.0409(5) 0.0444(6) 0.0532(5) -0.0088(4) -0.0236(4) -0.0081(4)
C11 0.0351(5) 0.0380(5) 0.0537(5) -0.0032(4) -0.0142(4) -0.0112(4)
C12 0.0310(4) 0.0285(5) 0.0459(5) -0.0034(4) -0.0125(4) -0.0059(4)
C13 0.0302(4) 0.0288(5) 0.0382(5) -0.0035(4) -0.0099(4) -0.0060(4)
C14 0.0308(5) 0.0259(5) 0.0445(5) -0.0032(4) -0.0026(4) -0.0072(4)
C15 0.0301(5) 0.0251(5) 0.0395(5) -0.0011(4) -0.0053(4) -0.0028(4)
C16 0.0394(5) 0.0388(5) 0.0389(5) 0.0069(4) -0.0044(4) -0.0134(4)
C17 0.0456(6) 0.0449(5) 0.0301(5) 0.0055(4) -0.0051(4) -0.0109(5)
C18 0.0406(5) 0.0395(5) 0.0308(5) 0.0018(4) -0.0081(4) -0.0107(4)
C19 0.0307(5) 0.0298(5) 0.0323(4) 0.0007(4) -0.0051(4) -0.0068(4)
C20 0.0302(4) 0.0280(5) 0.0306(4) 0.0009(4) -0.0065(4) -0.0057(4)
C21 0.0358(5) 0.0329(5) 0.0332(4) 0.0000(4) -0.0132(4) -0.0083(4)
C22 0.0311(4) 0.0405(5) 0.0285(4) -0.0050(4) -0.0096(3) -0.0098(4)
C23 0.0419(5) 0.0468(6) 0.0354(5) -0.0007(4) -0.0151(4) -0.0131(4)
C24 0.0357(5) 0.0518(6) 0.0450(5) -0.0049(5) -0.0103(4) -0.0155(4)
C25 0.0437(5) 0.0546(6) 0.0375(5) -0.0019(4) -0.0053(4) -0.0234(4)
C26 0.0445(5) 0.0463(6) 0.0305(4) 0.0022(4) -0.0096(4) -0.0153(4)
C27 0.0340(4) 0.0417(5) 0.0305(4) -0.0020(4) -0.0102(4) -0.0131(4)
N4 0.0303(4) 0.0372(4) 0.0408(4) 0.0041(3) -0.0088(3) -0.0110(3)
C32 0.0366(5) 0.0299(5) 0.0345(4) 0.0004(4) -0.0109(4) -0.0051(4)
C33 0.0368(5) 0.0376(5) 0.0390(5) 0.0030(4) -0.0119(4) -0.0133(4)
C34 0.0390(5) 0.0353(5) 0.0339(4) 0.0007(4) -0.0118(4) -0.0111(4)
C35 0.0469(6) 0.0397(6) 0.0940(8) 0.0030(6) -0.0124(6) -0.0147(5)
C36 0.0316(5) 0.0368(5) 0.0523(5) 0.0115(4) -0.0152(4) -0.0078(4)
C37 0.0403(6) 0.0724(7) 0.0373(5) 0.0164(5) -0.0093(4) -0.0101(5)
C38 0.0528(6) 0.0621(7) 0.0505(6) 0.0125(5) -0.0217(5) -0.0094(5)
C39 0.0565(6) 0.0630(7) 0.0600(6) -0.0042(5) -0.0239(5) -0.0150(5)
C28A 0.0416(3) 0.0214(5) 0.0468(2) 0.0035(4) -0.0142(2) -0.0050(4)
C29A 0.0623(4) 0.0294(7) 0.0541(2) -0.0065(4) -0.0284(2) 0.0012(5)
C30A 0.0647(4) 0.0458(6) 0.0535(2) -0.0081(3) -0.0221(2) -0.0160(5)
C31A 0.0819(5) 0.0690(13) 0.0575(2) -0.0165(5) -0.0330(2) -0.0062(8)
C28B 0.0416(3) 0.0214(5) 0.0468(2) 0.0035(4) -0.0142(2) -0.0050(4)
C29B 0.0623(4) 0.0294(7) 0.0541(2) -0.0065(4) -0.0284(2) 0.0012(5)
C30B 0.0647(4) 0.0458(6) 0.0535(2) -0.0081(3) -0.0221(2) -0.0160(5)
C31B 0.0819(5) 0.0690(13) 0.0575(2) -0.0165(5) -0.0330(2) -0.0062(8)
C40A 0.0328(4) 0.0497(2) 0.0559(6) 0.0100(4) -0.0120(4) -0.0155(2)
C41A 0.0345(3) 0.0513(3) 0.0954(6) 0.0235(5) -0.0235(3) -0.0170(3)
C42A 0.0372(3) 0.0603(3) 0.0948(4) 0.0254(4) -0.0236(4) -0.0227(2)
C43A 0.0565(6) 0.0668(4) 0.0928(4) 0.0280(5) -0.0197(4) -0.0312(4)
C40B 0.0328(4) 0.0497(2) 0.0559(6) 0.0100(4) -0.0120(4) -0.0155(2)
C41B 0.0345(3) 0.0513(3) 0.0954(6) 0.0235(5) -0.0235(3) -0.0170(3)
C42B 0.0372(3) 0.0603(3) 0.0948(4) 0.0254(4) -0.0236(4) -0.0227(2)
C43B 0.0565(6) 0.0668(4) 0.0928(4) 0.0280(5) -0.0197(4) -0.0312(4)

_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 1.3474(11) . ?
N1 C8 1.4050(13) . ?
N2 C20 1.3610(11) . ?
N2 C13 1.3617(14) . ?
N3 C21 1.3617(14) . ?
N3 C19 1.4128(12) . ?
O1 C7 1.2360(13) . ?
O2 C14 1.2594(12) . ?
O3 C21 1.2231(11) . ?
C1 C6 1.3854(14) . ?
C1 C2 1.3944(19) . ?
C2 C3 1.3801(18) . ?
C3 C4 1.3810(16) . ?
C4 C5 1.3689(16) . ?
C5 C6 1.3917(14) . ?
C6 C7 1.4946(16) . ?
C8 C9 1.3643(16) . ?
C8 C13 1.4407(12) . ?
C9 C10 1.4000(15) . ?
C10 C11 1.3703(14) . ?
C11 C12 1.4119(16) . ?
C12 C13 1.4031(14) . ?
C12 C14 1.4526(13) . ?
C14 C15 1.4525(16) . ?
C15 C20 1.4049(14) . ?
C15 C16 1.4183(13) . ?
C16 C17 1.3604(17) . ?
C17 C18 1.4078(15) . ?
C18 C19 1.3708(13) . ?
C19 C20 1.4364(15) . ?
C21 C22 1.4964(13) . ?
C22 C23 1.3878(14) . ?
C22 C27 1.3934(13) . ?
C23 C24 1.3758(14) . ?
C24 C25 1.3820(14) . ?
C25 C26 1.3849(15) . ?
C26 C27 1.3794(14) . ?
N4 C40B 1.4954(10) . ?
N4 C28B 1.5134(11) . ?
N4 C36 1.5191(13) . ?
N4 C32 1.5290(9) . ?
N4 C28A 1.5349(9) . ?
N4 C40A 1.5461(12) . ?
C32 C33 1.5148(5) . ?
C33 C34 1.5304(4) . ?
C34 C35 1.4878(5) . ?
C36 C37 1.5089(14) . ?
C37 C38 1.5381(16) . ?
C38 C39 1.5096(18) . ?
C28A C29A 1.5153(6) . ?
C29A C30A 1.5302(5) . ?
C30A C31A 1.4870(6) . ?
C28B C29B 1.5154(5) . ?
C29B C30B 1.5302(5) . ?
C30B C31B 1.4868(6) . ?
C40A C41A 1.5155(5) . ?
C41A C42A 1.5303(5) . ?
C42A C43A 1.4868(5) . ?
C40B C41B 1.5161(5) . ?
C41B C42B 1.5302(5) . ?
C42B C43B 1.4853(6) . ?

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 130.95(9) . . ?
C20 N2 C13 115.89(8) . . ?
C21 N3 C19 128.91(8) . . ?
C6 C1 C2 120.13(11) . . ?
C3 C2 C1 119.68(11) . . ?
C2 C3 C4 120.11(12) . . ?
C5 C4 C3 120.34(11) . . ?
C4 C5 C6 120.51(10) . . ?
C1 C6 C5 119.23(11) . . ?
C1 C6 C7 118.64(9) . . ?
C5 C6 C7 122.11(9) . . ?
O1 C7 N1 123.61(10) . . ?
O1 C7 C6 121.89(8) . . ?
N1 C7 C6 114.50(9) . . ?
C9 C8 N1 126.07(8) . . ?
C9 C8 C13 121.10(9) . . ?
N1 C8 C13 112.80(9) . . ?
C8 C9 C10 119.52(9) . . ?
C11 C10 C9 121.19(11) . . ?
C10 C11 C12 120.35(10) . . ?
C13 C12 C11 119.62(8) . . ?
C13 C12 C14 119.04(10) . . ?
C11 C12 C14 121.24(9) . . ?
N2 C13 C12 125.41(8) . . ?
N2 C13 C8 116.40(9) . . ?
C12 C13 C8 118.17(10) . . ?
O2 C14 C15 122.60(9) . . ?
O2 C14 C12 122.26(10) . . ?
C15 C14 C12 115.09(9) . . ?
C20 C15 C16 119.11(10) . . ?
C20 C15 C14 119.88(8) . . ?
C16 C15 C14 121.00(9) . . ?
C17 C16 C15 120.93(10) . . ?
C16 C17 C18 120.94(9) . . ?
C19 C18 C17 119.43(10) . . ?
C18 C19 N3 124.62(10) . . ?
C18 C19 C20 121.00(9) . . ?
N3 C19 C20 114.37(8) . . ?
N2 C20 C15 124.45(10) . . ?
N2 C20 C19 117.06(9) . . ?
C15 C20 C19 118.49(8) . . ?
O3 C21 N3 123.16(9) . . ?
O3 C21 C22 121.25(10) . . ?
N3 C21 C22 115.57(8) . . ?
C23 C22 C27 119.11(9) . . ?
C23 C22 C21 117.89(8) . . ?
C27 C22 C21 122.85(8) . . ?
C24 C23 C22 120.32(9) . . ?
C23 C24 C25 120.51(10) . . ?
C24 C25 C26 119.56(10) . . ?
C27 C26 C25 120.19(9) . . ?
C26 C27 C22 120.27(9) . . ?
C40B N4 C28B 111.72(8) . . ?
C40B N4 C36 112.07(8) . . ?
C28B N4 C36 102.27(6) . . ?
C40B N4 C32 103.77(4) . . ?
C28B N4 C32 115.89(8) . . ?
C36 N4 C32 111.42(8) . . ?
C40B N4 C28A 113.74(8) . . ?
C28B N4 C28A 9.01(8) . . ?
C36 N4 C28A 108.57(6) . . ?
C32 N4 C28A 107.13(8) . . ?
C40B N4 C40A 3.204(19) . . ?
C28B N4 C40A 109.94(11) . . ?
C36 N4 C40A 110.32(11) . . ?
C32 N4 C40A 106.97(4) . . ?
C28A N4 C40A 112.42(12) . . ?
C33 C32 N4 115.65(4) . . ?
C32 C33 C34 110.18(3) . . ?
C35 C34 C33 112.76(3) . . ?
C37 C36 N4 116.25(7) . . ?
C36 C37 C38 110.66(8) . . ?
C39 C38 C37 113.69(9) . . ?
C29A C28A N4 120.83(6) . . ?
C28A C29A C30A 110.07(4) . . ?
C31A C30A C29A 113.11(5) . . ?
N4 C28B C29B 112.15(6) . . ?
C28B C29B C30B 110.02(4) . . ?
C31B C30B C29B 113.10(4) . . ?
C41A C40A N4 111.76(5) . . ?
C40A C41A C42A 110.09(5) . . ?
C43A C42A C41A 113.13(7) . . ?
N4 C40B C41B 120.48(4) . . ?
C40B C41B C42B 109.85(3) . . ?
C43B C42B C41B 113.41(4) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.060

#===END

data_2006sot1001
_database_code_depnum_ccdc_archive 'CCDC 629282'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C59 H93 Cl2 N7 O3'
_chemical_formula_weight         1019.30

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                   8.6137(6)
_cell_length_b                   16.7161(14)
_cell_length_c                   20.8520(16)
_cell_angle_alpha                104.273(4)
_cell_angle_beta                 93.257(4)
_cell_angle_gamma                93.788(4)
_cell_volume                     2895.1(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    11213
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.10

_exptl_crystal_description       Rod
_exptl_crystal_colour            'Pale Yellow'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1108
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9586
_exptl_absorpt_correction_T_max  0.9952
_exptl_absorpt_process_details   
;
SADABS V2.10 (Sheldrick, G.M., 2003)
;

_exptl_special_details           
;
SADABS was used to perform the Absorption correction
Parameter refinement on 14349 reflections reduced R(int) from 0.1961 to 0.0726
Ratio of minimum to maximum apparent transmission: 0.490863
The given Tmin and Tmax were generated using the SHELX SIZE command
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker Nonius FR591 Rotating Anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans to fill the asymmetric unit'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            39582
_diffrn_reflns_av_R_equivalents  0.1696
_diffrn_reflns_av_sigmaI/netI    0.2150
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.98
_diffrn_reflns_theta_max         27.47
_reflns_number_total             12741
_reflns_number_gt                5710
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin, et al., 1993)'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_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^)+(0.0554P)^2^+3.2345P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12741
_refine_ls_number_parameters     649
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2402
_refine_ls_R_factor_gt           0.1080
_refine_ls_wR_factor_ref         0.2258
_refine_ls_wR_factor_gt          0.1831
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.5860(4) 1.0456(2) 0.14113(17) 0.0502(10) Uani 1 1 d . . .
O2 O 0.1220(4) 0.6278(2) -0.02747(16) 0.0479(10) Uani 1 1 d . . .
H992 H 0.1087 0.6528 -0.0575 0.072 Uiso 1 1 calc R . .
O3 O 0.4151(4) 0.6332(2) 0.31993(16) 0.0413(9) Uani 1 1 d . . .
N1 N 0.5718(4) 1.0377(2) 0.2479(2) 0.0374(10) Uani 1 1 d . . .
H101 H 0.5404 1.0051 0.2728 0.045 Uiso 1 1 calc R . .
N2 N 0.4546(4) 0.9335(3) 0.16358(19) 0.0361(10) Uani 1 1 d . . .
H102 H 0.4347 0.9101 0.1960 0.043 Uiso 1 1 calc R . .
N3 N 0.3338(4) 0.7784(2) 0.14958(19) 0.0318(10) Uani 1 1 d . . .
N4 N 0.3456(4) 0.7247(2) 0.26050(19) 0.0316(10) Uani 1 1 d . . .
H104 H 0.3519 0.7777 0.2612 0.038 Uiso 1 1 calc R . .
N5 N 0.4546(4) 0.7730(2) 0.36581(19) 0.0346(10) Uani 1 1 d . . .
H105 H 0.4390 0.8209 0.3572 0.042 Uiso 1 1 calc R . .
C1 C 0.7582(5) 1.1596(3) 0.2532(3) 0.0400(13) Uani 1 1 d . . .
H1 H 0.7822 1.1392 0.2085 0.048 Uiso 1 1 calc R . .
C2 C 0.8300(6) 1.2332(3) 0.2912(3) 0.0429(13) Uani 1 1 d . . .
H2 H 0.9028 1.2637 0.2719 0.052 Uiso 1 1 calc R . .
C3 C 0.8002(6) 1.2637(3) 0.3557(3) 0.0457(14) Uani 1 1 d . . .
H3 H 0.8537 1.3140 0.3812 0.055 Uiso 1 1 calc R . .
C4 C 0.6912(6) 1.2209(3) 0.3836(3) 0.0483(14) Uani 1 1 d . . .
H4 H 0.6676 1.2420 0.4283 0.058 Uiso 1 1 calc R . .
C5 C 0.6173(6) 1.1474(3) 0.3461(3) 0.0421(13) Uani 1 1 d . . .
H5 H 0.5423 1.1183 0.3654 0.051 Uiso 1 1 calc R . .
C6 C 0.6490(5) 1.1148(3) 0.2811(2) 0.0344(12) Uani 1 1 d . . .
C7 C 0.5409(5) 1.0085(3) 0.1814(3) 0.0369(13) Uani 1 1 d . . .
C8 C 0.3943(5) 0.8894(3) 0.0999(2) 0.0351(12) Uani 1 1 d . . .
C9 C 0.3946(6) 0.9220(3) 0.0462(2) 0.0423(13) Uani 1 1 d . . .
H9 H 0.4419 0.9761 0.0501 0.051 Uiso 1 1 calc R . .
C10 C 0.3230(6) 0.8740(4) -0.0161(3) 0.0472(14) Uani 1 1 d . . .
H10 H 0.3219 0.8973 -0.0533 0.057 Uiso 1 1 calc R . .
C11 C 0.2567(6) 0.7962(3) -0.0234(2) 0.0424(14) Uani 1 1 d . . .
H11 H 0.2097 0.7656 -0.0654 0.051 Uiso 1 1 calc R . .
C12 C 0.2577(5) 0.7606(3) 0.0316(2) 0.0331(12) Uani 1 1 d . . .
C13 C 0.1915(6) 0.6805(3) 0.0271(2) 0.0394(13) Uani 1 1 d . . .
C14 C 0.1963(5) 0.6482(3) 0.0845(2) 0.0327(12) Uani 1 1 d . . .
C15 C 0.1338(5) 0.5684(3) 0.0843(3) 0.0380(13) Uani 1 1 d . . .
H15 H 0.0876 0.5327 0.0440 0.046 Uiso 1 1 calc R . .
C16 C 0.1380(6) 0.5413(3) 0.1400(3) 0.0384(13) Uani 1 1 d . . .
H16 H 0.0930 0.4875 0.1388 0.046 Uiso 1 1 calc R . .
C17 C 0.2090(5) 0.5926(3) 0.2001(2) 0.0371(13) Uani 1 1 d . . .
H17 H 0.2111 0.5731 0.2392 0.045 Uiso 1 1 calc R . .
C18 C 0.2751(5) 0.6702(3) 0.2024(2) 0.0328(12) Uani 1 1 d . . .
C19 C 0.2687(5) 0.7010(3) 0.1444(2) 0.0286(11) Uani 1 1 d . . .
C20 C 0.3279(5) 0.8068(3) 0.0943(2) 0.0342(12) Uani 1 1 d . . .
C21 C 0.4060(5) 0.7047(3) 0.3164(2) 0.0313(12) Uani 1 1 d . . .
C22 C 0.5261(5) 0.7771(3) 0.4285(2) 0.0359(13) Uani 1 1 d . . .
C23 C 0.5624(6) 0.7079(4) 0.4502(3) 0.0446(14) Uani 1 1 d . . .
H23 H 0.5347 0.6537 0.4229 0.053 Uiso 1 1 calc R . .
C24 C 0.6400(6) 0.7191(4) 0.5125(3) 0.0542(16) Uani 1 1 d . . .
H24 H 0.6637 0.6719 0.5277 0.065 Uiso 1 1 calc R . .
C25 C 0.6826(7) 0.7959(4) 0.5521(3) 0.0576(17) Uani 1 1 d . . .
H25 H 0.7390 0.8021 0.5938 0.069 Uiso 1 1 calc R . .
C26 C 0.6434(6) 0.8650(4) 0.5313(3) 0.0513(16) Uani 1 1 d . . .
H26 H 0.6715 0.9188 0.5591 0.062 Uiso 1 1 calc R . .
C27 C 0.5637(5) 0.8558(3) 0.4705(2) 0.0390(13) Uani 1 1 d . . .
H27 H 0.5342 0.9033 0.4570 0.047 Uiso 1 1 calc R . .
N6 N -0.1236(4) 0.8164(2) 0.26779(19) 0.0350(10) Uani 1 1 d . . .
C28 C -0.2540(5) 0.7513(3) 0.2339(2) 0.0400(13) Uani 1 1 d . . .
H28A H -0.3306 0.7781 0.2107 0.048 Uiso 1 1 calc R . .
H28B H -0.3081 0.7320 0.2687 0.048 Uiso 1 1 calc R . .
C29 C -0.2054(5) 0.6758(3) 0.1842(2) 0.0390(13) Uani 1 1 d . . .
H29A H -0.1422 0.6940 0.1514 0.047 Uiso 1 1 calc R . .
H29B H -0.1401 0.6438 0.2077 0.047 Uiso 1 1 calc R . .
C30 C -0.3480(5) 0.6209(3) 0.1485(2) 0.0409(13) Uani 1 1 d . . .
H30A H -0.4121 0.6043 0.1817 0.049 Uiso 1 1 calc R . .
H30B H -0.4119 0.6531 0.1246 0.049 Uiso 1 1 calc R . .
C31 C -0.3051(6) 0.5436(3) 0.0993(3) 0.0503(15) Uani 1 1 d . . .
H31A H -0.2426 0.5597 0.0659 0.076 Uiso 1 1 calc R . .
H31B H -0.4004 0.5107 0.0774 0.076 Uiso 1 1 calc R . .
H31C H -0.2444 0.5106 0.1228 0.076 Uiso 1 1 calc R . .
C32 C -0.0337(5) 0.8490(3) 0.2173(2) 0.0353(13) Uani 1 1 d . . .
H32A H 0.0498 0.8907 0.2417 0.042 Uiso 1 1 calc R . .
H32B H 0.0176 0.8025 0.1898 0.042 Uiso 1 1 calc R . .
C33 C -0.1283(5) 0.8877(3) 0.1711(2) 0.0383(13) Uani 1 1 d . . .
H33A H -0.1586 0.9422 0.1960 0.046 Uiso 1 1 calc R . .
H33B H -0.2247 0.8517 0.1530 0.046 Uiso 1 1 calc R . .
C34 C -0.0309(6) 0.8986(3) 0.1145(3) 0.0435(14) Uani 1 1 d . . .
H34A H 0.0688 0.9309 0.1334 0.052 Uiso 1 1 calc R . .
H34B H -0.0061 0.8434 0.0887 0.052 Uiso 1 1 calc R . .
C35 C -0.1129(6) 0.9422(3) 0.0681(3) 0.0521(15) Uani 1 1 d . . .
H35A H -0.2159 0.9134 0.0523 0.078 Uiso 1 1 calc R . .
H35B H -0.0506 0.9420 0.0302 0.078 Uiso 1 1 calc R . .
H35C H -0.1251 0.9996 0.0919 0.078 Uiso 1 1 calc R . .
C36 C -0.0070(5) 0.7794(3) 0.3068(2) 0.0376(13) Uani 1 1 d . . .
H36A H 0.0838 0.8206 0.3223 0.045 Uiso 1 1 calc R . .
H36B H 0.0306 0.7306 0.2762 0.045 Uiso 1 1 calc R . .
C37 C -0.0641(6) 0.7526(3) 0.3667(2) 0.0422(13) Uani 1 1 d . . .
H37A H -0.0966 0.8010 0.3995 0.051 Uiso 1 1 calc R . .
H37B H -0.1553 0.7114 0.3526 0.051 Uiso 1 1 calc R . .
C38 C 0.0666(6) 0.7149(3) 0.3979(3) 0.0464(14) Uani 1 1 d . . .
H38A H 0.1580 0.7561 0.4102 0.056 Uiso 1 1 calc R . .
H38B H 0.0977 0.6666 0.3645 0.056 Uiso 1 1 calc R . .
C39 C 0.0231(7) 0.6871(4) 0.4591(3) 0.0547(16) Uani 1 1 d . . .
H39A H -0.0021 0.7350 0.4934 0.082 Uiso 1 1 calc R . .
H39B H 0.1112 0.6618 0.4758 0.082 Uiso 1 1 calc R . .
H39C H -0.0678 0.6464 0.4474 0.082 Uiso 1 1 calc R . .
C40 C -0.2023(6) 0.8852(3) 0.3123(3) 0.0426(14) Uani 1 1 d . . .
H40A H -0.2794 0.9059 0.2846 0.051 Uiso 1 1 calc R . .
H40B H -0.2604 0.8617 0.3439 0.051 Uiso 1 1 calc R . .
C41 C -0.0937(6) 0.9579(3) 0.3514(3) 0.0479(15) Uani 1 1 d . . .
H41A H -0.0667 0.9952 0.3227 0.057 Uiso 1 1 calc R . .
H41B H 0.0039 0.9378 0.3666 0.057 Uiso 1 1 calc R . .
C42 C -0.1731(6) 1.0050(3) 0.4110(3) 0.0483(14) Uani 1 1 d . . .
H42A H -0.2757 1.0196 0.3955 0.058 Uiso 1 1 calc R . .
H42B H -0.1920 0.9684 0.4410 0.058 Uiso 1 1 calc R . .
C43 C -0.0792(7) 1.0827(4) 0.4493(3) 0.0661(18) Uani 1 1 d . . .
H43A H 0.0214 1.0686 0.4660 0.099 Uiso 1 1 calc R . .
H43B H -0.1362 1.1105 0.4867 0.099 Uiso 1 1 calc R . .
H43C H -0.0614 1.1198 0.4202 0.099 Uiso 1 1 calc R . .
N7 N -0.3948(4) 0.6589(2) -0.22177(19) 0.0336(10) Uani 1 1 d . . .
C44 C -0.3746(6) 0.7519(3) -0.2107(3) 0.0406(13) Uani 1 1 d . . .
H44A H -0.4572 0.7765 -0.1829 0.049 Uiso 1 1 calc R . .
H44B H -0.3904 0.7654 -0.2542 0.049 Uiso 1 1 calc R . .
C45 C -0.2165(6) 0.7923(3) -0.1778(3) 0.0447(14) Uani 1 1 d . . .
H45A H -0.2065 0.7868 -0.1316 0.054 Uiso 1 1 calc R . .
H45B H -0.1326 0.7631 -0.2019 0.054 Uiso 1 1 calc R . .
C46 C -0.1965(7) 0.8836(3) -0.1774(3) 0.0534(15) Uani 1 1 d . . .
H46A H -0.2852 0.9114 -0.1562 0.064 Uiso 1 1 calc R . .
H46B H -0.1000 0.9089 -0.1497 0.064 Uiso 1 1 calc R . .
C47 C -0.1873(6) 0.9001(3) -0.2453(3) 0.0538(15) Uani 1 1 d . . .
H47A H -0.0951 0.8765 -0.2655 0.081 Uiso 1 1 calc R . .
H47B H -0.1795 0.9600 -0.2409 0.081 Uiso 1 1 calc R . .
H47C H -0.2813 0.8745 -0.2735 0.081 Uiso 1 1 calc R . .
C48 C -0.3639(5) 0.6321(3) -0.1589(2) 0.0349(12) Uani 1 1 d . . .
H48A H -0.2536 0.6491 -0.1424 0.042 Uiso 1 1 calc R . .
H48B H -0.3773 0.5708 -0.1696 0.042 Uiso 1 1 calc R . .
C49 C -0.4669(6) 0.6662(3) -0.1030(2) 0.0454(14) Uani 1 1 d . . .
H49A H -0.5744 0.6396 -0.1144 0.055 Uiso 1 1 calc R . .
H49B H -0.4709 0.7266 -0.0971 0.055 Uiso 1 1 calc R . .
C50 C -0.3998(6) 0.6488(4) -0.0377(2) 0.0460(14) Uani 1 1 d . . .
H50A H -0.4830 0.6517 -0.0066 0.055 Uiso 1 1 calc R . .
H50B H -0.3652 0.5920 -0.0474 0.055 Uiso 1 1 calc R . .
C51 C -0.2634(7) 0.7100(4) -0.0051(3) 0.0660(18) Uani 1 1 d . . .
H51A H -0.1800 0.7067 -0.0355 0.099 Uiso 1 1 calc R . .
H51B H -0.2243 0.6968 0.0358 0.099 Uiso 1 1 calc R . .
H51C H -0.2977 0.7662 0.0055 0.099 Uiso 1 1 calc R . .
C52 C -0.5616(5) 0.6320(3) -0.2512(3) 0.0405(13) Uani 1 1 d . . .
H52A H -0.5738 0.6472 -0.2941 0.049 Uiso 1 1 calc R . .
H52B H -0.6328 0.6642 -0.2212 0.049 Uiso 1 1 calc R . .
C53 C -0.6146(6) 0.5404(3) -0.2631(3) 0.0456(14) Uani 1 1 d . . .
H53A H -0.5309 0.5064 -0.2826 0.055 Uiso 1 1 calc R . .
H53B H -0.6358 0.5276 -0.2204 0.055 Uiso 1 1 calc R . .
C54 C -0.7618(6) 0.5190(4) -0.3101(3) 0.0569(16) Uani 1 1 d . . .
H54A H -0.8360 0.5614 -0.2955 0.068 Uiso 1 1 calc R . .
H54B H -0.8115 0.4650 -0.3073 0.068 Uiso 1 1 calc R . .
C55 C -0.7311(8) 0.5142(4) -0.3827(3) 0.088(2) Uani 1 1 d . . .
H55A H -0.6740 0.5658 -0.3856 0.132 Uiso 1 1 calc R . .
H55B H -0.8307 0.5063 -0.4095 0.132 Uiso 1 1 calc R . .
H55C H -0.6689 0.4675 -0.3994 0.132 Uiso 1 1 calc R . .
C56 C -0.2789(5) 0.6167(3) -0.2691(2) 0.0353(12) Uani 1 1 d . . .
H56A H -0.1740 0.6263 -0.2453 0.042 Uiso 1 1 calc R . .
H56B H -0.3078 0.5562 -0.2811 0.042 Uiso 1 1 calc R . .
C57 C -0.2693(6) 0.6452(4) -0.3326(3) 0.0511(15) Uani 1 1 d . . .
H57A H -0.3758 0.6455 -0.3530 0.061 Uiso 1 1 calc R . .
H57B H -0.2191 0.7023 -0.3222 0.061 Uiso 1 1 calc R . .
C58 C -0.1762(7) 0.5882(4) -0.3809(3) 0.0605(17) Uani 1 1 d . . .
H58A H -0.1394 0.6175 -0.4137 0.073 Uiso 1 1 calc R . .
H58B H -0.0831 0.5755 -0.3563 0.073 Uiso 1 1 calc R . .
C59 C -0.2641(9) 0.5094(4) -0.4168(3) 0.082(2) Uani 1 1 d . . .
H59A H -0.2857 0.4755 -0.3856 0.123 Uiso 1 1 calc R . .
H59B H -0.2020 0.4794 -0.4515 0.123 Uiso 1 1 calc R . .
H59C H -0.3627 0.5210 -0.4371 0.123 Uiso 1 1 calc R . .
Cl1 Cl 0.35639(14) 0.93113(8) 0.32173(6) 0.0362(3) Uani 1 1 d . . .
Cl2 Cl 0.08078(14) 0.64677(9) -0.16496(6) 0.0441(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
O1 0.056(2) 0.053(2) 0.044(2) 0.0200(19) 0.0131(19) -0.009(2)
O2 0.063(2) 0.041(2) 0.037(2) 0.0089(18) -0.0005(19) 0.003(2)
O3 0.049(2) 0.032(2) 0.044(2) 0.0119(17) 0.0012(17) 0.0062(17)
N1 0.038(2) 0.035(3) 0.042(3) 0.015(2) 0.004(2) -0.003(2)
N2 0.037(2) 0.038(3) 0.036(2) 0.015(2) 0.002(2) -0.003(2)
N3 0.025(2) 0.036(3) 0.037(2) 0.012(2) 0.0065(18) 0.012(2)
N4 0.032(2) 0.028(2) 0.038(2) 0.012(2) 0.0048(19) 0.0064(19)
N5 0.036(2) 0.030(2) 0.039(3) 0.012(2) 0.000(2) -0.0022(19)
C1 0.031(3) 0.044(3) 0.047(3) 0.015(3) 0.004(3) 0.009(3)
C2 0.033(3) 0.037(3) 0.062(4) 0.020(3) 0.002(3) 0.000(3)
C3 0.036(3) 0.038(3) 0.063(4) 0.016(3) -0.012(3) 0.001(3)
C4 0.049(3) 0.048(4) 0.044(3) 0.009(3) -0.002(3) -0.006(3)
C5 0.037(3) 0.045(4) 0.048(3) 0.018(3) 0.006(3) 0.003(3)
C6 0.030(3) 0.033(3) 0.044(3) 0.014(3) 0.002(2) 0.010(2)
C7 0.029(3) 0.046(4) 0.039(3) 0.013(3) 0.007(2) 0.007(3)
C8 0.033(3) 0.036(3) 0.037(3) 0.011(3) 0.005(2) 0.004(2)
C9 0.047(3) 0.044(3) 0.042(3) 0.022(3) 0.009(3) 0.001(3)
C10 0.050(3) 0.053(4) 0.046(3) 0.022(3) 0.009(3) 0.014(3)
C11 0.045(3) 0.049(4) 0.031(3) 0.005(3) 0.005(2) 0.010(3)
C12 0.027(3) 0.031(3) 0.044(3) 0.014(3) 0.006(2) 0.007(2)
C13 0.034(3) 0.047(4) 0.036(3) 0.005(3) 0.006(2) 0.011(3)
C14 0.032(3) 0.034(3) 0.032(3) 0.005(2) 0.009(2) 0.008(2)
C15 0.034(3) 0.035(3) 0.043(3) 0.006(3) 0.002(2) 0.004(2)
C16 0.037(3) 0.029(3) 0.053(3) 0.013(3) 0.006(3) 0.011(2)
C17 0.029(3) 0.044(3) 0.038(3) 0.009(3) 0.004(2) 0.010(3)
C18 0.024(3) 0.032(3) 0.043(3) 0.007(3) 0.009(2) 0.007(2)
C19 0.023(2) 0.033(3) 0.034(3) 0.011(2) 0.011(2) 0.012(2)
C20 0.026(3) 0.042(3) 0.034(3) 0.004(3) 0.005(2) 0.009(2)
C21 0.026(3) 0.038(3) 0.036(3) 0.017(3) 0.015(2) 0.008(2)
C22 0.026(3) 0.051(4) 0.030(3) 0.009(3) 0.007(2) 0.003(2)
C23 0.041(3) 0.057(4) 0.038(3) 0.015(3) 0.002(3) 0.010(3)
C24 0.054(4) 0.069(5) 0.045(4) 0.022(3) 0.003(3) 0.019(3)
C25 0.052(4) 0.085(5) 0.041(3) 0.028(4) -0.003(3) 0.003(4)
C26 0.042(3) 0.069(4) 0.039(3) 0.007(3) 0.008(3) -0.009(3)
C27 0.032(3) 0.051(4) 0.035(3) 0.011(3) 0.006(2) 0.001(3)
N6 0.027(2) 0.033(2) 0.045(2) 0.010(2) 0.0104(19) 0.0047(19)
C28 0.028(3) 0.044(3) 0.049(3) 0.014(3) 0.011(2) 0.003(2)
C29 0.033(3) 0.041(3) 0.045(3) 0.011(3) 0.006(2) 0.009(2)
C30 0.032(3) 0.040(3) 0.049(3) 0.009(3) 0.007(3) 0.000(2)
C31 0.039(3) 0.049(4) 0.056(4) 0.003(3) 0.000(3) -0.003(3)
C32 0.023(2) 0.030(3) 0.054(3) 0.007(2) 0.017(2) 0.005(2)
C33 0.032(3) 0.032(3) 0.050(3) 0.007(3) 0.012(2) 0.001(2)
C34 0.037(3) 0.037(3) 0.058(3) 0.012(3) 0.011(3) 0.003(3)
C35 0.055(4) 0.047(4) 0.057(4) 0.018(3) 0.012(3) 0.002(3)
C36 0.029(3) 0.037(3) 0.045(3) 0.007(2) 0.003(2) 0.005(2)
C37 0.036(3) 0.045(3) 0.048(3) 0.013(3) 0.012(3) 0.008(3)
C38 0.039(3) 0.049(4) 0.052(3) 0.012(3) 0.008(3) 0.008(3)
C39 0.060(4) 0.050(4) 0.052(4) 0.009(3) 0.006(3) 0.008(3)
C40 0.037(3) 0.041(3) 0.049(3) 0.007(3) 0.011(3) 0.008(3)
C41 0.040(3) 0.033(3) 0.068(4) 0.005(3) 0.020(3) 0.002(3)
C42 0.045(3) 0.043(4) 0.055(4) 0.010(3) -0.002(3) 0.008(3)
C43 0.053(4) 0.054(4) 0.078(4) -0.005(3) -0.001(3) -0.005(3)
N7 0.025(2) 0.038(3) 0.041(2) 0.013(2) 0.0029(18) 0.0078(19)
C44 0.038(3) 0.033(3) 0.053(3) 0.014(3) -0.001(3) 0.007(2)
C45 0.041(3) 0.040(3) 0.056(3) 0.018(3) -0.003(3) 0.006(3)
C46 0.049(3) 0.037(4) 0.073(4) 0.014(3) -0.006(3) 0.008(3)
C47 0.045(3) 0.045(4) 0.077(4) 0.025(3) 0.006(3) 0.002(3)
C48 0.029(3) 0.037(3) 0.041(3) 0.014(2) 0.000(2) 0.005(2)
C49 0.041(3) 0.053(4) 0.043(3) 0.012(3) 0.006(3) 0.008(3)
C50 0.039(3) 0.061(4) 0.038(3) 0.012(3) 0.004(3) 0.005(3)
C51 0.079(5) 0.063(4) 0.045(3) 0.005(3) -0.017(3) -0.020(4)
C52 0.029(3) 0.046(4) 0.045(3) 0.011(3) 0.001(2) 0.007(2)
C53 0.035(3) 0.044(4) 0.056(3) 0.013(3) -0.002(3) -0.001(3)
C54 0.045(3) 0.059(4) 0.061(4) 0.007(3) -0.003(3) 0.002(3)
C55 0.074(5) 0.085(6) 0.092(6) -0.003(4) -0.017(4) 0.017(4)
C56 0.029(3) 0.041(3) 0.037(3) 0.011(2) -0.002(2) 0.005(2)
C57 0.037(3) 0.074(4) 0.046(3) 0.020(3) 0.000(3) 0.012(3)
C58 0.046(3) 0.082(5) 0.051(4) 0.012(3) 0.006(3) 0.009(3)
C59 0.116(6) 0.051(4) 0.081(5) 0.013(4) 0.030(5) 0.008(4)
Cl1 0.0367(7) 0.0331(7) 0.0402(7) 0.0119(6) 0.0045(6) 0.0011(6)
Cl2 0.0359(7) 0.0577(9) 0.0410(7) 0.0184(7) -0.0005(6) 0.0018(6)

_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
O1 C7 1.227(6) . ?
O2 C13 1.338(6) . ?
O3 C21 1.223(5) . ?
N1 C7 1.355(6) . ?
N1 C6 1.406(6) . ?
N2 C7 1.371(6) . ?
N2 C8 1.401(6) . ?
N3 C20 1.350(6) . ?
N3 C19 1.351(6) . ?
N4 C21 1.374(6) . ?
N4 C18 1.402(6) . ?
N5 C21 1.360(6) . ?
N5 C22 1.398(6) . ?
C1 C2 1.374(7) . ?
C1 C6 1.403(7) . ?
C2 C3 1.361(7) . ?
C3 C4 1.382(7) . ?
C4 C5 1.375(7) . ?
C5 C6 1.380(6) . ?
C8 C9 1.361(7) . ?
C8 C20 1.434(7) . ?
C9 C10 1.428(7) . ?
C10 C11 1.355(7) . ?
C11 C12 1.417(7) . ?
C12 C13 1.399(7) . ?
C12 C20 1.421(7) . ?
C13 C14 1.429(7) . ?
C14 C15 1.405(7) . ?
C14 C19 1.421(6) . ?
C15 C16 1.345(7) . ?
C16 C17 1.412(7) . ?
C17 C18 1.370(7) . ?
C18 C19 1.428(7) . ?
C22 C23 1.389(7) . ?
C22 C27 1.395(7) . ?
C23 C24 1.389(7) . ?
C24 C25 1.358(8) . ?
C25 C26 1.385(8) . ?
C26 C27 1.377(7) . ?
N6 C36 1.514(6) . ?
N6 C40 1.514(6) . ?
N6 C28 1.522(6) . ?
N6 C32 1.525(6) . ?
C28 C29 1.522(6) . ?
C29 C30 1.522(6) . ?
C30 C31 1.520(6) . ?
C32 C33 1.515(7) . ?
C33 C34 1.526(6) . ?
C34 C35 1.519(7) . ?
C36 C37 1.522(7) . ?
C37 C38 1.517(7) . ?
C38 C39 1.519(7) . ?
C40 C41 1.513(7) . ?
C41 C42 1.523(6) . ?
C42 C43 1.502(7) . ?
N7 C48 1.503(6) . ?
N7 C44 1.511(6) . ?
N7 C52 1.524(6) . ?
N7 C56 1.527(5) . ?
C44 C45 1.526(7) . ?
C45 C46 1.522(7) . ?
C46 C47 1.514(8) . ?
C48 C49 1.525(6) . ?
C49 C50 1.549(7) . ?
C50 C51 1.516(7) . ?
C52 C53 1.524(7) . ?
C53 C54 1.524(7) . ?
C54 C55 1.535(9) . ?
C56 C57 1.518(7) . ?
C57 C58 1.511(7) . ?
C58 C59 1.478(8) . ?

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 C6 126.6(4) . . ?
C7 N2 C8 127.9(4) . . ?
C20 N3 C19 117.3(4) . . ?
C21 N4 C18 127.3(4) . . ?
C21 N5 C22 128.4(4) . . ?
C2 C1 C6 119.4(5) . . ?
C3 C2 C1 122.0(5) . . ?
C2 C3 C4 119.4(5) . . ?
C5 C4 C3 119.4(5) . . ?
C4 C5 C6 121.9(5) . . ?
C5 C6 C1 118.0(5) . . ?
C5 C6 N1 117.5(4) . . ?
C1 C6 N1 124.5(4) . . ?
O1 C7 N1 123.2(5) . . ?
O1 C7 N2 123.3(5) . . ?
N1 C7 N2 113.5(5) . . ?
C9 C8 N2 123.2(5) . . ?
C9 C8 C20 120.9(5) . . ?
N2 C8 C20 115.8(4) . . ?
C8 C9 C10 119.4(5) . . ?
C11 C10 C9 121.7(5) . . ?
C10 C11 C12 119.8(5) . . ?
C13 C12 C11 122.5(5) . . ?
C13 C12 C20 117.7(5) . . ?
C11 C12 C20 119.8(5) . . ?
O2 C13 C12 126.2(5) . . ?
O2 C13 C14 114.0(5) . . ?
C12 C13 C14 119.8(5) . . ?
C15 C14 C19 119.5(5) . . ?
C15 C14 C13 123.5(5) . . ?
C19 C14 C13 117.0(5) . . ?
C16 C15 C14 121.3(5) . . ?
C15 C16 C17 120.3(5) . . ?
C18 C17 C16 120.5(5) . . ?
C17 C18 N4 123.6(5) . . ?
C17 C18 C19 120.2(5) . . ?
N4 C18 C19 116.2(4) . . ?
N3 C19 C14 124.1(4) . . ?
N3 C19 C18 117.8(4) . . ?
C14 C19 C18 118.1(5) . . ?
N3 C20 C12 124.2(5) . . ?
N3 C20 C8 117.5(4) . . ?
C12 C20 C8 118.4(5) . . ?
O3 C21 N5 125.0(5) . . ?
O3 C21 N4 122.9(5) . . ?
N5 C21 N4 112.2(4) . . ?
C23 C22 C27 119.3(5) . . ?
C23 C22 N5 123.7(5) . . ?
C27 C22 N5 116.9(5) . . ?
C24 C23 C22 119.0(5) . . ?
C25 C24 C23 121.7(6) . . ?
C24 C25 C26 119.6(6) . . ?
C27 C26 C25 120.1(6) . . ?
C26 C27 C22 120.3(5) . . ?
C36 N6 C40 111.8(4) . . ?
C36 N6 C28 110.3(4) . . ?
C40 N6 C28 105.8(3) . . ?
C36 N6 C32 106.8(3) . . ?
C40 N6 C32 110.8(4) . . ?
C28 N6 C32 111.4(4) . . ?
N6 C28 C29 116.2(4) . . ?
C30 C29 C28 110.7(4) . . ?
C31 C30 C29 112.6(4) . . ?
C33 C32 N6 116.2(3) . . ?
C32 C33 C34 109.3(4) . . ?
C35 C34 C33 113.0(4) . . ?
N6 C36 C37 116.9(4) . . ?
C38 C37 C36 109.2(4) . . ?
C37 C38 C39 113.7(4) . . ?
C41 C40 N6 115.2(4) . . ?
C40 C41 C42 109.5(4) . . ?
C43 C42 C41 113.2(5) . . ?
C48 N7 C44 112.4(4) . . ?
C48 N7 C52 111.1(4) . . ?
C44 N7 C52 106.5(3) . . ?
C48 N7 C56 105.5(3) . . ?
C44 N7 C56 111.1(4) . . ?
C52 N7 C56 110.3(3) . . ?
N7 C44 C45 114.9(4) . . ?
C46 C45 C44 111.8(4) . . ?
C47 C46 C45 114.5(5) . . ?
N7 C48 C49 115.7(4) . . ?
C48 C49 C50 109.5(4) . . ?
C51 C50 C49 112.1(5) . . ?
N7 C52 C53 116.7(4) . . ?
C54 C53 C52 110.0(5) . . ?
C53 C54 C55 113.4(5) . . ?
C57 C56 N7 115.3(4) . . ?
C58 C57 C56 110.3(5) . . ?
C59 C58 C57 114.1(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
N1 H101 Cl1 0.88 2.37 3.198(4) 156.2 .
N2 H102 Cl1 0.88 2.69 3.460(4) 147.1 .
N4 H104 Cl1 0.88 2.56 3.364(4) 152.1 .
N5 H105 Cl1 0.88 2.29 3.154(4) 168.6 .
O2 H992 Cl2 0.84 2.22 2.965(4) 148.3 .

_diffrn_measured_fraction_theta_max 0.961
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.961
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.062