Supplementary Material for Organic & Biomolecular Chemistry
This journal is (c) The Royal Society of Chemistry 2006

data_global
_journal_name_full               Org.Biomol.Chem.

_journal_coden_Cambridge         0177

_publ_contact_author_name        'Wim Dehaen'
_publ_contact_author_address     
;Department of Chemistry,
University of Leuven,
Celestijnenlaan 200F,
B-3001 Leuven,
Belgium
;
_publ_contact_author_email       wim.dehaen@chem.kuleuven.be
_publ_contact_author_phone       '32 16 327439'
_publ_contact_author_fax         '32 16 327990'
loop_
_publ_author_name
_publ_author_address
'Rong Gu'
;Department of Chemistry,
University of Leuven,
Celestijnenlaan 200F,
B-3001 Leuven,
Belgium
;
'K.Van Hecke'
;Department of Chemistry,
University of Leuven,
Celestijnenlaan 200F,
B-3001 Leuven,
Belgium
;
'L.Van Meervelt'
;Department of Chemistry,
University of Leuven,
Celestijnenlaan 200F,
B-3001 Leuven,
Belgium
;
S.Toppet
;Department of Chemistry,
University of Leuven,
Celestijnenlaan 200F,
B-3001 Leuven,
Belgium
;
'Wim Dehaen.'
;Department of Chemistry,
University of Leuven,
Celestijnenlaan 200F,
B-3001 Leuven,
Belgium
;

data_wim36
_database_code_depnum_ccdc_archive 'CCDC 611501'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H44 N4 O2, C H Cl3'
_chemical_formula_sum            'C49 H45 Cl3 N4 O2'
_chemical_formula_weight         828.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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

_cell_length_a                   24.3549(8)
_cell_length_b                   13.9993(4)
_cell_length_c                   26.1244(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.689(2)
_cell_angle_gamma                90.00
_cell_volume                     8877.3(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3472
_exptl_absorpt_coefficient_mu    2.204
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4071
_exptl_absorpt_correction_T_max  0.576
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'crossed Goebel mirrors'
_diffrn_measurement_device_type  'SMART 6000'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43823
_diffrn_reflns_av_R_equivalents  0.1040
_diffrn_reflns_av_sigmaI/netI    0.0603
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         3.39
_diffrn_reflns_theta_max         66.58
_reflns_number_total             7781
_reflns_number_gt                5097
_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    Pluton
_computing_publication_material  Platon

_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^)+(0.0010P)^2^+70.0000P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7781
_refine_ls_number_parameters     573
_refine_ls_number_restraints     79
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0776
_refine_ls_wR_factor_ref         0.1793
_refine_ls_wR_factor_gt          0.1669
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.37173(13) 0.5122(2) 0.13806(11) 0.0264(7) Uani 1 1 d . . .
C2 C 0.40577(13) 0.5835(2) 0.12121(13) 0.0323(8) Uani 1 1 d . . .
H2 H 0.3915 0.6328 0.0990 0.039 Uiso 1 1 calc R . .
C3 C 0.46084(14) 0.5801(3) 0.13782(14) 0.0391(9) Uani 1 1 d . . .
H3 H 0.4850 0.6276 0.1267 0.047 Uiso 1 1 calc R . .
C4 C 0.48161(13) 0.5083(2) 0.17067(13) 0.0360(9) Uani 1 1 d . . .
H4 H 0.5197 0.5080 0.1819 0.043 Uiso 1 1 calc R . .
C5 C 0.44809(13) 0.4373(2) 0.18732(12) 0.0291(8) Uani 1 1 d . . .
H5 H 0.4630 0.3887 0.2097 0.035 Uiso 1 1 calc R . .
C6 C 0.39247(12) 0.4377(2) 0.17113(11) 0.0253(7) Uani 1 1 d . . .
C7 C 0.34479(12) 0.3781(2) 0.18084(11) 0.0234(7) Uani 1 1 d . . .
C8 C 0.33975(12) 0.2940(2) 0.20959(11) 0.0241(7) Uani 1 1 d . . .
C9 C 0.28610(12) 0.2594(2) 0.21044(11) 0.0243(7) Uani 1 1 d . . .
C10 C 0.23907(12) 0.3044(2) 0.18555(11) 0.0235(7) Uani 1 1 d . . .
C11 C 0.24571(12) 0.3869(2) 0.15654(11) 0.0229(7) Uani 1 1 d . . .
C12 C 0.29835(12) 0.4218(2) 0.15400(11) 0.0227(7) Uani 1 1 d . . .
C13 C 0.21130(13) 0.1733(2) 0.22834(12) 0.0280(8) Uani 1 1 d . . .
C14 C 0.17566(14) 0.1059(2) 0.24748(12) 0.0321(8) Uani 1 1 d . . .
H14 H 0.1893 0.0548 0.2688 0.039 Uiso 1 1 calc R . .
C15 C 0.12007(14) 0.1166(2) 0.23415(13) 0.0367(9) Uani 1 1 d . . .
H15 H 0.0950 0.0720 0.2466 0.044 Uiso 1 1 calc R . .
C16 C 0.09971(14) 0.1916(3) 0.20273(13) 0.0384(9) Uani 1 1 d . . .
H16 H 0.0612 0.1968 0.1941 0.046 Uiso 1 1 calc R . .
C17 C 0.13480(13) 0.2582(2) 0.18413(12) 0.0316(8) Uani 1 1 d . . .
H17 H 0.1206 0.3089 0.1628 0.038 Uiso 1 1 calc R . .
C18 C 0.19131(13) 0.2501(2) 0.19704(11) 0.0259(7) Uani 1 1 d . . .
C19 C 0.38744(12) 0.2437(2) 0.23785(12) 0.0276(7) Uani 1 1 d . . .
H19A H 0.4199 0.2497 0.2176 0.033 Uiso 1 1 calc R . .
H19B H 0.3785 0.1749 0.2399 0.033 Uiso 1 1 calc R . .
C20 C 0.40298(13) 0.2806(2) 0.29196(12) 0.0313(8) Uani 1 1 d . . .
H20A H 0.4105 0.3500 0.2905 0.038 Uiso 1 1 calc R . .
H20B H 0.3715 0.2711 0.3131 0.038 Uiso 1 1 calc R . .
C21 C 0.45341(13) 0.2301(3) 0.31740(13) 0.0355(9) Uani 1 1 d . . .
H21A H 0.4464 0.1605 0.3168 0.043 Uiso 1 1 calc R . .
H21B H 0.4850 0.2422 0.2967 0.043 Uiso 1 1 calc R . .
C22 C 0.46962(15) 0.2601(3) 0.37255(14) 0.0471(10) Uani 1 1 d . . .
H22A H 0.4748 0.3302 0.3736 0.057 Uiso 1 1 calc R . .
H22B H 0.4391 0.2445 0.3939 0.057 Uiso 1 1 calc R . .
C23 C 0.52194(18) 0.2124(4) 0.39577(17) 0.0745(16) Uani 1 1 d . . .
H23A H 0.5164 0.1432 0.3969 0.112 Uiso 1 1 calc R . .
H23B H 0.5308 0.2366 0.4307 0.112 Uiso 1 1 calc R . .
H23C H 0.5524 0.2269 0.3747 0.112 Uiso 1 1 calc R . .
C24 C 0.17588(12) 0.5017(2) 0.15469(12) 0.0268(7) Uani 1 1 d . . .
C25 C 0.13008(13) 0.5453(2) 0.12186(13) 0.0356(9) Uani 1 1 d . . .
H25A H 0.0949 0.5196 0.1314 0.053 Uiso 1 1 calc R . .
H25B H 0.1344 0.5304 0.0858 0.053 Uiso 1 1 calc R . .
H25C H 0.1306 0.6147 0.1267 0.053 Uiso 1 1 calc R . .
C26 C 0.26142(14) 0.4196(2) -0.03277(13) 0.0361(9) Uani 1 1 d . A .
C27 C 0.27077(17) 0.3469(3) -0.06753(15) 0.0488(11) Uani 1 1 d . . .
H27 H 0.2527 0.3458 -0.1012 0.059 Uiso 1 1 calc R . .
C28 C 0.30761(17) 0.2765(3) -0.05047(15) 0.0514(11) Uani 1 1 d . . .
H28 H 0.3153 0.2263 -0.0733 0.062 Uiso 1 1 calc R . .
C29 C 0.33385(17) 0.2764(3) -0.00124(16) 0.0489(11) Uani 1 1 d . . .
H29 H 0.3580 0.2255 0.0091 0.059 Uiso 1 1 calc R . .
C30 C 0.32535(15) 0.3495(2) 0.03314(14) 0.0396(9) Uani 1 1 d . . .
H30 H 0.3441 0.3502 0.0665 0.048 Uiso 1 1 calc R . .
C31 C 0.28806(14) 0.4225(2) 0.01697(13) 0.0332(8) Uani 1 1 d . . .
C32 C 0.27016(13) 0.5099(2) 0.04036(12) 0.0281(7) Uani 1 1 d . . .
C33 C 0.28220(13) 0.5518(2) 0.08845(12) 0.0261(7) Uani 1 1 d . . .
C34 C 0.25938(13) 0.6408(2) 0.09659(11) 0.0262(7) Uani 1 1 d . A .
C35 C 0.22218(12) 0.6863(2) 0.05974(12) 0.0273(7) Uani 1 1 d . A .
C36 C 0.20769(12) 0.6437(2) 0.01198(12) 0.0301(8) Uani 1 1 d D . .
C37 C 0.23316(13) 0.5563(2) 0.00347(12) 0.0311(8) Uani 1 1 d . A .
C38 C 0.23631(13) 0.7784(2) 0.13251(13) 0.0323(8) Uani 1 1 d . A .
C39 C 0.23223(15) 0.8572(2) 0.16560(14) 0.0399(9) Uani 1 1 d . . .
H39 H 0.2524 0.8592 0.1983 0.048 Uiso 1 1 calc R . .
C40 C 0.19820(16) 0.9308(3) 0.14896(16) 0.0464(10) Uani 1 1 d . . .
H40 H 0.1956 0.9852 0.1703 0.056 Uiso 1 1 calc R . .
C41 C 0.16737(15) 0.9284(3) 0.10180(16) 0.0478(10) Uani 1 1 d . . .
H41 H 0.1433 0.9797 0.0920 0.057 Uiso 1 1 calc R . .
C42 C 0.17156(14) 0.8515(3) 0.06906(15) 0.0409(9) Uani 1 1 d . A .
H42 H 0.1506 0.8504 0.0368 0.049 Uiso 1 1 calc R . .
C43 C 0.20662(13) 0.7753(2) 0.08350(12) 0.0306(8) Uani 1 1 d . . .
C49 C 0.12584(19) 0.4372(3) 0.29335(17) 0.0602(13) Uani 1 1 d . . .
H49 H 0.1580 0.4348 0.2719 0.072 Uiso 1 1 calc R . .
C44A C 0.16475(17) 0.6823(4) -0.0272(2) 0.0375(12) Uani 0.761(4) 1 d PDU A 1
H44A H 0.1726 0.6611 -0.0620 0.045 Uiso 0.761(4) 1 calc PR A 1
H44B H 0.1651 0.7530 -0.0265 0.045 Uiso 0.761(4) 1 calc PR A 1
C45A C 0.10756(16) 0.6446(4) -0.01438(17) 0.0363(12) Uani 0.761(4) 1 d PDU A 1
H45A H 0.1082 0.5739 -0.0149 0.044 Uiso 0.761(4) 1 calc PR A 1
H45B H 0.1009 0.6649 0.0209 0.044 Uiso 0.761(4) 1 calc PR A 1
C46A C 0.06105(17) 0.6788(4) -0.05049(18) 0.0457(13) Uani 0.761(4) 1 d PDU A 1
H46A H 0.0698 0.6649 -0.0861 0.055 Uiso 0.761(4) 1 calc PR A 1
H46B H 0.0580 0.7490 -0.0471 0.055 Uiso 0.761(4) 1 calc PR A 1
C47A C 0.00592(18) 0.6342(4) -0.04177(19) 0.0436(13) Uani 0.761(4) 1 d PU A 1
H47A H 0.0086 0.5641 -0.0461 0.052 Uiso 0.761(4) 1 calc PR A 1
H47B H -0.0025 0.6467 -0.0060 0.052 Uiso 0.761(4) 1 calc PR A 1
C48A C -0.0408(2) 0.6716(5) -0.0779(2) 0.0587(17) Uani 0.761(4) 1 d PU A 1
H48A H -0.0446 0.7406 -0.0729 0.088 Uiso 0.761(4) 1 calc PR A 1
H48B H -0.0752 0.6397 -0.0706 0.088 Uiso 0.761(4) 1 calc PR A 1
H48C H -0.0330 0.6587 -0.1134 0.088 Uiso 0.761(4) 1 calc PR A 1
C44B C 0.1656(5) 0.6931(13) -0.0242(7) 0.0367(9) Uani 0.239(4) 1 d PDU A 2
H44C H 0.1746 0.6747 -0.0592 0.044 Uiso 0.239(4) 1 calc PR A 2
H44D H 0.1738 0.7621 -0.0208 0.044 Uiso 0.239(4) 1 calc PR A 2
C45B C 0.1036(5) 0.6850(8) -0.0247(6) 0.035(3) Uani 0.239(4) 1 d PDU A 2
H45C H 0.0922 0.7041 0.0093 0.041 Uiso 0.239(4) 1 calc PR A 2
H45D H 0.0864 0.7299 -0.0506 0.041 Uiso 0.239(4) 1 calc PR A 2
C46B C 0.0830(4) 0.5859(9) -0.0369(6) 0.041(3) Uani 0.239(4) 1 d PDU A 2
H46C H 0.1022 0.5400 -0.0128 0.049 Uiso 0.239(4) 1 calc PR A 2
H46D H 0.0914 0.5686 -0.0722 0.049 Uiso 0.239(4) 1 calc PR A 2
C47B C 0.0214(4) 0.5787(10) -0.0327(5) 0.054(3) Uani 0.239(4) 1 d PDU A 2
H47C H 0.0102 0.5109 -0.0367 0.065 Uiso 0.239(4) 1 calc PR A 2
H47D H 0.0131 0.5996 0.0020 0.065 Uiso 0.239(4) 1 calc PR A 2
C48B C -0.0123(7) 0.6373(13) -0.0720(8) 0.093(6) Uani 0.239(4) 1 d PDU A 2
H48D H -0.0062 0.6143 -0.1065 0.139 Uiso 0.239(4) 1 calc PR A 2
H48E H -0.0011 0.7045 -0.0687 0.139 Uiso 0.239(4) 1 calc PR A 2
H48F H -0.0514 0.6315 -0.0662 0.139 Uiso 0.239(4) 1 calc PR A 2
Cl1 Cl 0.11794(5) 0.32268(8) 0.31944(4) 0.0641(3) Uani 1 1 d . . .
Cl2 Cl 0.06851(5) 0.46897(9) 0.25341(5) 0.0725(4) Uani 1 1 d . . .
Cl3 Cl 0.14084(6) 0.52112(9) 0.34197(6) 0.0863(4) Uani 1 1 d . . .
N1 N 0.31514(10) 0.50328(17) 0.12841(9) 0.0245(6) Uani 1 1 d . . .
N2 N 0.26784(10) 0.17981(18) 0.23583(10) 0.0270(6) Uani 1 1 d . . .
H22 H 0.2892 0.1395 0.2540 0.032 Uiso 1 1 calc R . .
N3 N 0.22665(12) 0.4985(2) -0.04001(10) 0.0374(7) Uani 1 1 d . . .
H33 H 0.2043 0.5099 -0.0675 0.045 Uiso 1 1 calc R A .
N4 N 0.26688(11) 0.69668(18) 0.14000(10) 0.0293(7) Uani 1 1 d . . .
H44 H 0.2879 0.6823 0.1680 0.035 Uiso 1 1 calc R A .
O1 O 0.19944(8) 0.42932(14) 0.13033(8) 0.0244(5) Uani 1 1 d . . .
O2 O 0.19101(9) 0.52530(16) 0.19794(9) 0.0369(6) 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
C1 0.0289(15) 0.0260(15) 0.0249(15) -0.0044(12) 0.0070(13) -0.0017(13)
C2 0.0350(17) 0.0286(16) 0.0338(17) 0.0014(14) 0.0065(14) -0.0073(14)
C3 0.0342(18) 0.0395(19) 0.045(2) 0.0020(16) 0.0083(16) -0.0127(15)
C4 0.0246(16) 0.0419(19) 0.0422(19) -0.0049(16) 0.0065(15) -0.0025(14)
C5 0.0283(16) 0.0288(16) 0.0305(16) -0.0021(13) 0.0055(13) 0.0023(13)
C6 0.0269(15) 0.0249(15) 0.0252(15) -0.0028(12) 0.0093(13) -0.0009(12)
C7 0.0219(14) 0.0240(15) 0.0249(15) -0.0063(12) 0.0048(12) 0.0017(12)
C8 0.0261(15) 0.0245(15) 0.0223(15) -0.0029(12) 0.0052(12) -0.0006(12)
C9 0.0305(16) 0.0230(15) 0.0195(14) 0.0003(12) 0.0034(12) 0.0017(12)
C10 0.0261(15) 0.0240(15) 0.0205(14) -0.0020(12) 0.0035(12) -0.0051(12)
C11 0.0243(15) 0.0227(14) 0.0218(14) -0.0016(12) 0.0033(12) 0.0019(12)
C12 0.0263(15) 0.0207(14) 0.0217(14) -0.0021(11) 0.0046(12) -0.0013(12)
C13 0.0326(16) 0.0288(16) 0.0225(15) -0.0003(12) 0.0013(13) -0.0049(13)
C14 0.0405(18) 0.0297(17) 0.0261(16) 0.0030(13) 0.0020(14) -0.0086(14)
C15 0.0345(18) 0.0354(18) 0.0403(19) 0.0018(15) 0.0047(15) -0.0145(15)
C16 0.0299(17) 0.045(2) 0.0395(19) 0.0026(16) 0.0008(15) -0.0117(15)
C17 0.0325(17) 0.0298(17) 0.0324(17) 0.0007(14) 0.0023(14) -0.0065(14)
C18 0.0286(16) 0.0287(16) 0.0207(14) -0.0007(12) 0.0038(12) -0.0041(13)
C19 0.0239(15) 0.0249(15) 0.0342(17) 0.0019(13) 0.0042(13) -0.0002(13)
C20 0.0283(16) 0.0332(17) 0.0329(17) 0.0015(14) 0.0047(14) -0.0008(14)
C21 0.0273(16) 0.0437(19) 0.0359(18) 0.0109(15) 0.0045(14) -0.0072(15)
C22 0.0350(19) 0.066(2) 0.040(2) 0.0145(18) -0.0008(16) -0.0154(18)
C23 0.047(2) 0.123(4) 0.051(3) 0.029(3) -0.007(2) -0.008(3)
C24 0.0240(15) 0.0221(15) 0.0355(17) 0.0013(13) 0.0087(13) -0.0035(12)
C25 0.0308(17) 0.0341(18) 0.0429(19) 0.0047(15) 0.0090(15) 0.0026(14)
C26 0.0408(19) 0.0359(18) 0.0321(17) -0.0078(14) 0.0062(15) -0.0080(15)
C27 0.056(2) 0.051(2) 0.041(2) -0.0158(17) 0.0076(18) -0.0092(19)
C28 0.062(3) 0.045(2) 0.048(2) -0.0254(18) 0.012(2) -0.0049(19)
C29 0.058(2) 0.0337(19) 0.056(2) -0.0108(17) 0.013(2) 0.0031(17)
C30 0.053(2) 0.0331(18) 0.0340(18) -0.0071(15) 0.0088(16) -0.0046(16)
C31 0.0385(18) 0.0277(16) 0.0342(17) -0.0046(14) 0.0076(15) -0.0078(14)
C32 0.0295(16) 0.0266(16) 0.0289(16) -0.0004(13) 0.0058(13) -0.0057(13)
C33 0.0293(16) 0.0239(15) 0.0254(15) 0.0047(12) 0.0048(13) -0.0036(13)
C34 0.0294(16) 0.0260(15) 0.0244(15) 0.0039(12) 0.0083(13) -0.0043(13)
C35 0.0243(15) 0.0292(16) 0.0299(16) 0.0051(13) 0.0104(13) -0.0044(13)
C36 0.0226(15) 0.0405(18) 0.0280(16) 0.0081(14) 0.0070(13) -0.0051(13)
C37 0.0327(17) 0.0388(18) 0.0222(15) -0.0004(13) 0.0046(13) -0.0108(14)
C38 0.0327(17) 0.0282(17) 0.0383(18) 0.0027(14) 0.0161(14) -0.0013(14)
C39 0.045(2) 0.0351(19) 0.041(2) -0.0021(15) 0.0132(17) -0.0007(16)
C40 0.053(2) 0.0294(18) 0.061(2) -0.0027(17) 0.0266(19) 0.0023(17)
C41 0.043(2) 0.0356(19) 0.068(3) 0.0062(18) 0.0210(19) 0.0138(16)
C42 0.0319(18) 0.042(2) 0.049(2) 0.0130(17) 0.0099(16) 0.0034(15)
C43 0.0303(16) 0.0294(16) 0.0339(17) 0.0071(13) 0.0128(14) -0.0007(13)
C49 0.060(3) 0.068(3) 0.052(3) 0.009(2) 0.002(2) 0.000(2)
C44A 0.0240(18) 0.057(3) 0.031(2) 0.004(2) -0.0008(18) 0.004(2)
C45A 0.0271(18) 0.052(3) 0.029(2) 0.008(2) 0.0018(17) 0.001(2)
C46A 0.0247(17) 0.071(3) 0.040(3) 0.015(2) -0.0009(18) -0.007(2)
C47A 0.0266(19) 0.062(3) 0.042(3) 0.005(2) 0.0000(19) -0.003(2)
C48A 0.027(2) 0.084(4) 0.063(4) 0.012(3) -0.010(2) -0.004(3)
C44B 0.0368(11) 0.0367(11) 0.0367(12) -0.0001(8) 0.0030(8) 0.0001(8)
C45B 0.037(3) 0.034(4) 0.033(7) 0.009(5) 0.006(6) 0.006(4)
C46B 0.039(3) 0.044(5) 0.038(7) 0.001(6) -0.002(5) -0.004(3)
C47B 0.041(4) 0.059(7) 0.062(8) 0.003(6) -0.005(6) -0.008(4)
C48B 0.050(6) 0.080(12) 0.139(15) 0.033(10) -0.050(9) -0.021(8)
Cl1 0.0742(7) 0.0590(6) 0.0599(6) 0.0037(5) 0.0105(6) 0.0068(6)
Cl2 0.0557(6) 0.0858(8) 0.0734(8) 0.0147(6) -0.0116(6) 0.0004(6)
Cl3 0.0990(9) 0.0639(7) 0.0892(9) 0.0039(7) -0.0336(8) 0.0011(7)
N1 0.0270(13) 0.0234(12) 0.0234(12) 0.0017(10) 0.0039(10) -0.0023(10)
N2 0.0276(13) 0.0252(13) 0.0285(13) 0.0047(11) 0.0038(11) 0.0012(11)
N3 0.0381(15) 0.0474(17) 0.0260(14) -0.0055(12) -0.0021(12) -0.0032(14)
N4 0.0372(15) 0.0278(14) 0.0236(13) 0.0003(11) 0.0074(11) 0.0036(11)
O1 0.0256(10) 0.0230(10) 0.0247(10) 0.0001(8) 0.0032(9) 0.0020(8)
O2 0.0365(12) 0.0343(12) 0.0403(13) -0.0118(10) 0.0057(11) 0.0011(10)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.386(4) . ?
C1 C2 1.392(4) . ?
C1 C6 1.420(4) . ?
C2 C3 1.376(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.390(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.378(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.386(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.469(4) . ?
C7 C8 1.407(4) . ?
C7 C12 1.419(4) . ?
C8 C9 1.395(4) . ?
C8 C19 1.500(4) . ?
C9 N2 1.389(4) . ?
C9 C10 1.417(4) . ?
C10 C11 1.398(4) . ?
C10 C18 1.441(4) . ?
C11 C12 1.379(4) . ?
C11 O1 1.402(3) . ?
C12 N1 1.401(4) . ?
C13 N2 1.378(4) . ?
C13 C14 1.402(4) . ?
C13 C18 1.413(4) . ?
C14 C15 1.379(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.398(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.379(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.394(4) . ?
C17 H17 0.9500 . ?
C19 C20 1.523(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.521(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.521(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.520(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 O2 1.205(4) . ?
C24 O1 1.350(4) . ?
C24 C25 1.482(4) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 N3 1.395(4) . ?
C26 C27 1.396(5) . ?
C26 C31 1.405(5) . ?
C27 C28 1.382(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.389(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.388(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.409(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.451(4) . ?
C32 C33 1.395(4) . ?
C32 C37 1.422(4) . ?
C33 C34 1.388(4) . ?
C33 N1 1.434(4) . ?
C34 N4 1.378(4) . ?
C34 C35 1.419(4) . ?
C35 C36 1.402(4) . ?
C35 C43 1.456(4) . ?
C36 C37 1.397(5) . ?
C36 C44A 1.503(5) . ?
C36 C44B 1.505(13) . ?
C37 N3 1.393(4) . ?
C38 N4 1.370(4) . ?
C38 C39 1.410(5) . ?
C38 C43 1.419(5) . ?
C39 C40 1.371(5) . ?
C39 H39 0.9500 . ?
C40 C41 1.390(6) . ?
C40 H40 0.9500 . ?
C41 C42 1.384(5) . ?
C41 H41 0.9500 . ?
C42 C43 1.398(5) . ?
C42 H42 0.9500 . ?
C49 Cl2 1.731(4) . ?
C49 Cl3 1.747(5) . ?
C49 Cl1 1.759(5) . ?
C49 H49 1.0000 . ?
C44A C45A 1.552(6) . ?
C44A H44A 0.9900 . ?
C44A H44B 0.9900 . ?
C45A C46A 1.492(5) . ?
C45A H45A 0.9900 . ?
C45A H45B 0.9900 . ?
C46A C47A 1.515(6) . ?
C46A H46A 0.9900 . ?
C46A H46B 0.9900 . ?
C47A C48A 1.511(7) . ?
C47A H47A 0.9900 . ?
C47A H47B 0.9900 . ?
C48A H48A 0.9800 . ?
C48A H48B 0.9800 . ?
C48A H48C 0.9800 . ?
C44B C45B 1.512(14) . ?
C44B H44C 0.9900 . ?
C44B H44D 0.9900 . ?
C45B C46B 1.501(14) . ?
C45B H45C 0.9900 . ?
C45B H45D 0.9900 . ?
C46B C47B 1.516(13) . ?
C46B H46C 0.9900 . ?
C46B H46D 0.9900 . ?
C47B C48B 1.503(9) . ?
C47B H47C 0.9900 . ?
C47B H47D 0.9900 . ?
C48B H48D 0.9800 . ?
C48B H48E 0.9800 . ?
C48B H48F 0.9800 . ?
N2 H22 0.8800 . ?
N3 H33 0.8800 . ?
N4 H44 0.8800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 128.0(3) . . ?
N1 C1 C6 110.1(3) . . ?
C2 C1 C6 121.8(3) . . ?
C3 C2 C1 117.8(3) . . ?
C3 C2 H2 121.1 . . ?
C1 C2 H2 121.1 . . ?
C2 C3 C4 121.0(3) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C5 C4 C3 121.4(3) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C4 C5 C6 119.4(3) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C5 C6 C1 118.6(3) . . ?
C5 C6 C7 135.4(3) . . ?
C1 C6 C7 106.0(3) . . ?
C8 C7 C12 121.5(3) . . ?
C8 C7 C6 132.2(3) . . ?
C12 C7 C6 106.2(3) . . ?
C9 C8 C7 114.9(3) . . ?
C9 C8 C19 121.2(3) . . ?
C7 C8 C19 123.9(3) . . ?
N2 C9 C8 128.5(3) . . ?
N2 C9 C10 107.3(3) . . ?
C8 C9 C10 124.2(3) . . ?
C11 C10 C9 119.4(3) . . ?
C11 C10 C18 132.8(3) . . ?
C9 C10 C18 107.8(3) . . ?
C12 C11 C10 117.9(3) . . ?
C12 C11 O1 122.7(3) . . ?
C10 C11 O1 119.4(3) . . ?
C11 C12 N1 128.4(3) . . ?
C11 C12 C7 122.0(3) . . ?
N1 C12 C7 109.6(3) . . ?
N2 C13 C14 129.4(3) . . ?
N2 C13 C18 109.0(3) . . ?
C14 C13 C18 121.6(3) . . ?
C15 C14 C13 117.4(3) . . ?
C15 C14 H14 121.3 . . ?
C13 C14 H14 121.3 . . ?
C14 C15 C16 121.6(3) . . ?
C14 C15 H15 119.2 . . ?
C16 C15 H15 119.2 . . ?
C17 C16 C15 120.9(3) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C16 C17 C18 119.2(3) . . ?
C16 C17 H17 120.4 . . ?
C18 C17 H17 120.4 . . ?
C17 C18 C13 119.2(3) . . ?
C17 C18 C10 134.8(3) . . ?
C13 C18 C10 106.0(3) . . ?
C8 C19 C20 114.9(3) . . ?
C8 C19 H19A 108.5 . . ?
C20 C19 H19A 108.5 . . ?
C8 C19 H19B 108.5 . . ?
C20 C19 H19B 108.5 . . ?
H19A C19 H19B 107.5 . . ?
C21 C20 C19 112.2(3) . . ?
C21 C20 H20A 109.2 . . ?
C19 C20 H20A 109.2 . . ?
C21 C20 H20B 109.2 . . ?
C19 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
C22 C21 C20 115.1(3) . . ?
C22 C21 H21A 108.5 . . ?
C20 C21 H21A 108.5 . . ?
C22 C21 H21B 108.5 . . ?
C20 C21 H21B 108.5 . . ?
H21A C21 H21B 107.5 . . ?
C23 C22 C21 113.7(4) . . ?
C23 C22 H22A 108.8 . . ?
C21 C22 H22A 108.8 . . ?
C23 C22 H22B 108.8 . . ?
C21 C22 H22B 108.8 . . ?
H22A C22 H22B 107.7 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O2 C24 O1 122.6(3) . . ?
O2 C24 C25 126.0(3) . . ?
O1 C24 C25 111.4(3) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N3 C26 C27 128.2(3) . . ?
N3 C26 C31 109.4(3) . . ?
C27 C26 C31 122.3(3) . . ?
C28 C27 C26 116.5(4) . . ?
C28 C27 H27 121.7 . . ?
C26 C27 H27 121.7 . . ?
C27 C28 C29 122.5(4) . . ?
C27 C28 H28 118.8 . . ?
C29 C28 H28 118.8 . . ?
C30 C29 C28 121.1(4) . . ?
C30 C29 H29 119.4 . . ?
C28 C29 H29 119.4 . . ?
C29 C30 C31 117.8(3) . . ?
C29 C30 H30 121.1 . . ?
C31 C30 H30 121.1 . . ?
C26 C31 C30 119.6(3) . . ?
C26 C31 C32 106.3(3) . . ?
C30 C31 C32 134.0(3) . . ?
C33 C32 C37 119.6(3) . . ?
C33 C32 C31 133.2(3) . . ?
C37 C32 C31 107.2(3) . . ?
C34 C33 C32 117.2(3) . . ?
C34 C33 N1 121.4(3) . . ?
C32 C33 N1 121.4(3) . . ?
N4 C34 C33 127.5(3) . . ?
N4 C34 C35 109.7(3) . . ?
C33 C34 C35 122.8(3) . . ?
C36 C35 C34 120.8(3) . . ?
C36 C35 C43 133.5(3) . . ?
C34 C35 C43 105.6(3) . . ?
C37 C36 C35 115.6(3) . . ?
C37 C36 C44A 120.0(3) . . ?
C35 C36 C44A 124.3(3) . . ?
C37 C36 C44B 126.2(8) . . ?
C35 C36 C44B 118.2(8) . . ?
N3 C37 C36 128.0(3) . . ?
N3 C37 C32 108.1(3) . . ?
C36 C37 C32 123.8(3) . . ?
N4 C38 C39 129.1(3) . . ?
N4 C38 C43 109.6(3) . . ?
C39 C38 C43 121.4(3) . . ?
C40 C39 C38 117.7(3) . . ?
C40 C39 H39 121.1 . . ?
C38 C39 H39 121.1 . . ?
C39 C40 C41 122.1(3) . . ?
C39 C40 H40 118.9 . . ?
C41 C40 H40 118.9 . . ?
C42 C41 C40 120.4(3) . . ?
C42 C41 H41 119.8 . . ?
C40 C41 H41 119.8 . . ?
C41 C42 C43 120.0(3) . . ?
C41 C42 H42 120.0 . . ?
C43 C42 H42 120.0 . . ?
C42 C43 C38 118.4(3) . . ?
C42 C43 C35 135.4(3) . . ?
C38 C43 C35 106.2(3) . . ?
Cl2 C49 Cl3 112.1(3) . . ?
Cl2 C49 Cl1 111.1(3) . . ?
Cl3 C49 Cl1 110.8(2) . . ?
Cl2 C49 H49 107.6 . . ?
Cl3 C49 H49 107.6 . . ?
Cl1 C49 H49 107.6 . . ?
C36 C44A C45A 108.5(4) . . ?
C36 C44A H44A 110.0 . . ?
C45A C44A H44A 110.0 . . ?
C36 C44A H44B 110.0 . . ?
C45A C44A H44B 110.0 . . ?
H44A C44A H44B 108.4 . . ?
C46A C45A C44A 113.7(4) . . ?
C46A C45A H45A 108.8 . . ?
C44A C45A H45A 108.8 . . ?
C46A C45A H45B 108.8 . . ?
C44A C45A H45B 108.8 . . ?
H45A C45A H45B 107.7 . . ?
C45A C46A C47A 114.1(4) . . ?
C45A C46A H46A 108.7 . . ?
C47A C46A H46A 108.7 . . ?
C45A C46A H46B 108.7 . . ?
C47A C46A H46B 108.7 . . ?
H46A C46A H46B 107.6 . . ?
C48A C47A C46A 113.3(4) . . ?
C48A C47A H47A 108.9 . . ?
C46A C47A H47A 108.9 . . ?
C48A C47A H47B 108.9 . . ?
C46A C47A H47B 108.9 . . ?
H47A C47A H47B 107.7 . . ?
C36 C44B C45B 126.8(12) . . ?
C36 C44B H44C 105.6 . . ?
C45B C44B H44C 105.6 . . ?
C36 C44B H44D 105.6 . . ?
C45B C44B H44D 105.6 . . ?
H44C C44B H44D 106.1 . . ?
C46B C45B C44B 112.8(11) . . ?
C46B C45B H45C 109.0 . . ?
C44B C45B H45C 109.0 . . ?
C46B C45B H45D 109.0 . . ?
C44B C45B H45D 109.0 . . ?
H45C C45B H45D 107.8 . . ?
C45B C46B C47B 111.3(10) . . ?
C45B C46B H46C 109.4 . . ?
C47B C46B H46C 109.4 . . ?
C45B C46B H46D 109.4 . . ?
C47B C46B H46D 109.4 . . ?
H46C C46B H46D 108.0 . . ?
C48B C47B C46B 113.7(12) . . ?
C48B C47B H47C 108.8 . . ?
C46B C47B H47C 108.8 . . ?
C48B C47B H47D 108.8 . . ?
C46B C47B H47D 108.8 . . ?
H47C C47B H47D 107.7 . . ?
C47B C48B H48D 109.5 . . ?
C47B C48B H48E 109.5 . . ?
H48D C48B H48E 109.5 . . ?
C47B C48B H48F 109.5 . . ?
H48D C48B H48F 109.5 . . ?
H48E C48B H48F 109.5 . . ?
C1 N1 C12 108.1(2) . . ?
C1 N1 C33 125.4(2) . . ?
C12 N1 C33 124.4(2) . . ?
C13 N2 C9 109.9(2) . . ?
C13 N2 H22 125.0 . . ?
C9 N2 H22 125.0 . . ?
C37 N3 C26 108.8(3) . . ?
C37 N3 H33 125.6 . . ?
C26 N3 H33 125.6 . . ?
C38 N4 C34 108.8(3) . . ?
C38 N4 H44 125.6 . . ?
C34 N4 H44 125.6 . . ?
C24 O1 C11 116.3(2) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        66.58
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.088

#===END

data_wim38
_database_code_depnum_ccdc_archive 'CCDC 611502'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H42 N4, 3(C3 H6 O)'
_chemical_formula_sum            'C55 H60 N4 O3'
_chemical_formula_weight         825.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   12.4498(7)
_cell_length_b                   13.0721(6)
_cell_length_c                   17.1213(8)
_cell_angle_alpha                76.028(3)
_cell_angle_beta                 88.352(4)
_cell_angle_gamma                64.368(3)
_cell_volume                     2428.7(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             884
_exptl_absorpt_coefficient_mu    0.542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_process_details   Sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'crossed Goebel mirrors'
_diffrn_measurement_device_type  'SMART 6000'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24657
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.67
_diffrn_reflns_theta_max         70.97
_reflns_number_total             8856
_reflns_number_gt                7354
_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    ?
_computing_publication_material  platon

_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^)+(0.0010P)^2^+4.0000P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8856
_refine_ls_number_parameters     614
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0711
_refine_ls_wR_factor_ref         0.1497
_refine_ls_wR_factor_gt          0.1454
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0140(2) -0.1304(2) 0.15866(14) 0.0294(5) Uani 1 1 d . A .
C2 C -0.0413(2) -0.2025(2) 0.19472(14) 0.0306(5) Uani 1 1 d . . .
C3 C -0.0523(2) -0.2768(2) 0.15151(15) 0.0362(6) Uani 1 1 d . . .
H3 H -0.0879 -0.3273 0.1743 0.043 Uiso 1 1 calc R . .
C4 C -0.0110(3) -0.2757(2) 0.07552(15) 0.0381(6) Uani 1 1 d . . .
H4 H -0.0196 -0.3249 0.0459 0.046 Uiso 1 1 calc R . .
C5 C 0.0434(2) -0.2031(2) 0.04170(15) 0.0369(6) Uani 1 1 d . . .
H5 H 0.0714 -0.2041 -0.0104 0.044 Uiso 1 1 calc R . .
C6 C 0.0569(2) -0.1302(2) 0.08276(15) 0.0335(5) Uani 1 1 d . . .
H6 H 0.0943 -0.0813 0.0599 0.040 Uiso 1 1 calc R . .
C7 C -0.0404(2) -0.0894(2) 0.27917(14) 0.0298(5) Uani 1 1 d . A .
C8 C -0.0622(2) -0.0398(2) 0.34413(14) 0.0314(5) Uani 1 1 d . . .
H8 H -0.0384 0.0192 0.3471 0.038 Uiso 1 1 calc R . .
C9 C -0.1210(2) -0.0813(2) 0.40507(15) 0.0356(6) Uani 1 1 d . . .
C10 C -0.1560(3) -0.1694(3) 0.39847(15) 0.0396(6) Uani 1 1 d . . .
C11 C -0.1381(3) -0.2166(2) 0.33211(15) 0.0370(6) Uani 1 1 d . . .
C12 C -0.0771(2) -0.1764(2) 0.27188(14) 0.0318(5) Uani 1 1 d . . .
C13 C -0.1629(3) -0.0499(3) 0.48003(15) 0.0398(6) Uani 1 1 d . . .
C14 C -0.1582(3) 0.0310(3) 0.51861(16) 0.0418(6) Uani 1 1 d . . .
H14 H -0.1222 0.0807 0.4949 0.050 Uiso 1 1 calc R . .
C15 C -0.2069(3) 0.0374(3) 0.59212(17) 0.0518(8) Uani 1 1 d . . .
H15 H -0.2045 0.0922 0.6189 0.062 Uiso 1 1 calc R . .
C16 C -0.2598(3) -0.0364(4) 0.62729(19) 0.0643(10) Uani 1 1 d . . .
H16 H -0.2920 -0.0311 0.6779 0.077 Uiso 1 1 calc R . .
C17 C -0.2660(4) -0.1160(4) 0.59032(19) 0.0650(10) Uani 1 1 d . . .
H17 H -0.3021 -0.1653 0.6146 0.078 Uiso 1 1 calc R . .
C18 C -0.2176(3) -0.1224(3) 0.51573(17) 0.0492(8) Uani 1 1 d . . .
C19 C -0.1829(3) -0.3052(3) 0.32581(17) 0.0430(7) Uani 1 1 d . . .
H19A H -0.2151 -0.2874 0.2694 0.052 Uiso 1 1 calc R . .
H19B H -0.2495 -0.2969 0.3607 0.052 Uiso 1 1 calc R . .
C20 C -0.0874(3) -0.4311(3) 0.35009(18) 0.0485(7) Uani 1 1 d . . .
H20A H -0.0580 -0.4503 0.4073 0.058 Uiso 1 1 calc R . .
H20B H -0.0191 -0.4387 0.3170 0.058 Uiso 1 1 calc R . .
C21 C -0.1322(3) -0.5195(3) 0.33968(17) 0.0493(8) Uani 1 1 d . . .
H21A H -0.2027 -0.5096 0.3709 0.059 Uiso 1 1 calc R . .
H21B H -0.1583 -0.5026 0.2820 0.059 Uiso 1 1 calc R . .
C22 C -0.0388(3) -0.6447(3) 0.3671(2) 0.0581(9) Uani 1 1 d . . .
H22A H -0.0106 -0.6607 0.4242 0.070 Uiso 1 1 calc R . .
H22B H 0.0305 -0.6551 0.3346 0.070 Uiso 1 1 calc R . .
C23 C -0.0837(4) -0.7335(3) 0.35970(19) 0.0606(9) Uani 1 1 d . . .
H23A H -0.1508 -0.7254 0.3930 0.091 Uiso 1 1 calc R . .
H23B H -0.0190 -0.8130 0.3782 0.091 Uiso 1 1 calc R . .
H23C H -0.1103 -0.7193 0.3031 0.091 Uiso 1 1 calc R . .
C24 C -0.0766(2) 0.3398(2) 0.13040(14) 0.0337(5) Uani 1 1 d . . .
C25 C -0.1769(2) 0.3151(2) 0.14326(15) 0.0348(6) Uani 1 1 d . . .
C26 C -0.2932(3) 0.4026(2) 0.13209(16) 0.0411(6) Uani 1 1 d . . .
H26 H -0.3594 0.3843 0.1404 0.049 Uiso 1 1 calc R . .
C27 C -0.3096(3) 0.5174(3) 0.10852(17) 0.0475(7) Uani 1 1 d . . .
H27 H -0.3884 0.5792 0.1000 0.057 Uiso 1 1 calc R . .
C28 C -0.2125(3) 0.5447(2) 0.09687(16) 0.0453(7) Uani 1 1 d . . .
H28 H -0.2265 0.6246 0.0813 0.054 Uiso 1 1 calc R . .
C29 C -0.0969(3) 0.4577(2) 0.10756(15) 0.0405(6) Uani 1 1 d . . .
H29 H -0.0316 0.4773 0.0995 0.049 Uiso 1 1 calc R . .
C30 C 0.0293(2) 0.2273(2) 0.14720(14) 0.0309(5) Uani 1 1 d . A .
C31 C 0.1511(2) 0.1951(2) 0.13915(14) 0.0327(5) Uani 1 1 d D . .
C32 C 0.2255(2) 0.0752(2) 0.15966(14) 0.0321(5) Uani 1 1 d . A .
C33 C 0.1841(2) -0.0125(2) 0.18684(14) 0.0295(5) Uani 1 1 d . . .
C34 C 0.0619(2) 0.0211(2) 0.19158(13) 0.0279(5) Uani 1 1 d . A .
C35 C -0.0137(2) 0.1400(2) 0.17159(14) 0.0294(5) Uani 1 1 d . . .
C36 C 0.3892(2) -0.0999(2) 0.18760(15) 0.0378(6) Uani 1 1 d . . .
C37 C 0.5053(3) -0.1888(3) 0.19938(17) 0.0452(7) Uani 1 1 d . A .
H37 H 0.5715 -0.1716 0.1867 0.054 Uiso 1 1 calc R . .
C38 C 0.5216(3) -0.3023(3) 0.23001(18) 0.0508(7) Uani 1 1 d . . .
H38 H 0.6003 -0.3643 0.2395 0.061 Uiso 1 1 calc R A .
C39 C 0.4243(3) -0.3284(3) 0.24748(18) 0.0475(7) Uani 1 1 d . A .
H39 H 0.4381 -0.4077 0.2683 0.057 Uiso 1 1 calc R . .
C40 C 0.3088(3) -0.2408(2) 0.23496(16) 0.0390(6) Uani 1 1 d . . .
H40 H 0.2433 -0.2594 0.2465 0.047 Uiso 1 1 calc R A .
C41 C 0.2892(2) -0.1244(2) 0.20514(14) 0.0340(6) Uani 1 1 d . A .
C42A C 0.2126(14) 0.2740(12) 0.1134(8) 0.031(2) Uani 0.579(7) 1 d PDU A 1
H42A H 0.1559 0.3493 0.0772 0.037 Uiso 0.579(7) 1 calc PR A 1
H42B H 0.2810 0.2364 0.0826 0.037 Uiso 0.579(7) 1 calc PR A 1
C43A C 0.2575(7) 0.2978(7) 0.1855(6) 0.0391(18) Uani 0.579(7) 1 d PDU A 1
H43A H 0.3023 0.2225 0.2261 0.047 Uiso 0.579(7) 1 calc PR A 1
H43B H 0.1880 0.3472 0.2106 0.047 Uiso 0.579(7) 1 calc PR A 1
C44A C 0.3382(4) 0.3592(4) 0.1630(3) 0.0392(13) Uani 0.579(7) 1 d PDU A 1
H44A H 0.3760 0.3589 0.2132 0.047 Uiso 0.579(7) 1 calc PR A 1
H44B H 0.4028 0.3140 0.1326 0.047 Uiso 0.579(7) 1 calc PR A 1
C45A C 0.2742(5) 0.4831(4) 0.1133(3) 0.0418(14) Uani 0.579(7) 1 d PDU A 1
H45A H 0.2126 0.5301 0.1446 0.050 Uiso 0.579(7) 1 calc PR A 1
H45B H 0.2332 0.4846 0.0640 0.050 Uiso 0.579(7) 1 calc PR A 1
C46A C 0.3609(11) 0.5382(9) 0.0889(5) 0.047(2) Uani 0.579(7) 1 d PDU A 1
H46A H 0.3985 0.5405 0.1375 0.071 Uiso 0.579(7) 1 calc PR A 1
H46B H 0.3167 0.6182 0.0550 0.071 Uiso 0.579(7) 1 calc PR A 1
H46C H 0.4227 0.4911 0.0587 0.071 Uiso 0.579(7) 1 calc PR A 1
C42B C 0.190(2) 0.2930(17) 0.1118(12) 0.036(4) Uani 0.421(7) 1 d PDU A 2
H42C H 0.2624 0.2650 0.0826 0.044 Uiso 0.421(7) 1 calc PR A 2
H42D H 0.1258 0.3603 0.0737 0.044 Uiso 0.421(7) 1 calc PR A 2
C43B C 0.2154(12) 0.3340(10) 0.1816(11) 0.061(4) Uani 0.421(7) 1 d PDU A 2
H43C H 0.1444 0.3568 0.2130 0.073 Uiso 0.421(7) 1 calc PR A 2
H43D H 0.2829 0.2679 0.2178 0.073 Uiso 0.421(7) 1 calc PR A 2
C44B C 0.2460(8) 0.4367(8) 0.1548(7) 0.072(3) Uani 0.421(7) 1 d PDU A 2
H44C H 0.1804 0.5002 0.1157 0.087 Uiso 0.421(7) 1 calc PR A 2
H44D H 0.2481 0.4664 0.2025 0.087 Uiso 0.421(7) 1 calc PR A 2
C45B C 0.3599(8) 0.4133(8) 0.1173(6) 0.062(2) Uani 0.421(7) 1 d PDU A 2
H45C H 0.3605 0.3812 0.0705 0.075 Uiso 0.421(7) 1 calc PR A 2
H45D H 0.4272 0.3539 0.1569 0.075 Uiso 0.421(7) 1 calc PR A 2
C46B C 0.377(2) 0.5249(16) 0.0895(14) 0.126(9) Uani 0.421(7) 1 d PDU A 2
H46D H 0.3047 0.5876 0.0570 0.188 Uiso 0.421(7) 1 calc PR A 2
H46E H 0.4455 0.5103 0.0570 0.188 Uiso 0.421(7) 1 calc PR A 2
H46F H 0.3912 0.5487 0.1368 0.188 Uiso 0.421(7) 1 calc PR A 2
C47 C 0.5941(2) 0.0985(3) 0.04283(16) 0.0416(6) Uani 1 1 d . . .
C48 C 0.6273(3) 0.1971(3) 0.00882(18) 0.0495(7) Uani 1 1 d . . .
H48A H 0.6305 0.2082 -0.0497 0.074 Uiso 1 1 calc R . .
H48B H 0.7057 0.1781 0.0338 0.074 Uiso 1 1 calc R . .
H48C H 0.5672 0.2695 0.0202 0.074 Uiso 1 1 calc R . .
C49 C 0.6877(3) -0.0228(3) 0.0477(2) 0.0553(8) Uani 1 1 d . . .
H49A H 0.7434 -0.0495 0.0957 0.083 Uiso 1 1 calc R . .
H49B H 0.7315 -0.0231 -0.0008 0.083 Uiso 1 1 calc R . .
H49C H 0.6498 -0.0755 0.0515 0.083 Uiso 1 1 calc R . .
C50 C 0.6340(3) 0.1111(3) 0.26771(19) 0.0522(7) Uani 1 1 d . . .
C51 C 0.6292(4) 0.1953(4) 0.3153(2) 0.0836(13) Uani 1 1 d . . .
H51A H 0.6748 0.2378 0.2901 0.125 Uiso 1 1 calc R . .
H51B H 0.6638 0.1518 0.3707 0.125 Uiso 1 1 calc R . .
H51C H 0.5458 0.2514 0.3162 0.125 Uiso 1 1 calc R . .
C52 C 0.5697(3) 0.0365(4) 0.2967(2) 0.0698(10) Uani 1 1 d . . .
H52A H 0.4832 0.0855 0.2865 0.105 Uiso 1 1 calc R . .
H52B H 0.5904 0.0005 0.3548 0.105 Uiso 1 1 calc R . .
H52C H 0.5935 -0.0251 0.2677 0.105 Uiso 1 1 calc R . .
C57 C 0.8079(5) 0.3751(4) 0.5676(3) 0.0954(16) Uani 1 1 d . . .
H57A H 0.8152 0.3765 0.5103 0.143 Uiso 1 1 calc R . .
H57B H 0.7404 0.3584 0.5856 0.143 Uiso 1 1 calc R . .
H57C H 0.8817 0.3140 0.5993 0.143 Uiso 1 1 calc R . .
C56 C 0.7877(5) 0.4890(4) 0.5791(3) 0.0878(13) Uani 1 1 d . . .
C58 C 0.7681(5) 0.5042(5) 0.6637(3) 0.1071(17) Uani 1 1 d . . .
H58A H 0.7740 0.5753 0.6672 0.161 Uiso 1 1 calc R . .
H58B H 0.8289 0.4360 0.7020 0.161 Uiso 1 1 calc R . .
H58C H 0.6885 0.5112 0.6769 0.161 Uiso 1 1 calc R . .
N1 N 0.01538(18) -0.06352(17) 0.21015(12) 0.0299(4) Uani 1 1 d . . .
N2 N -0.2150(2) -0.1923(2) 0.46638(14) 0.0503(7) Uani 1 1 d . . .
H2 H -0.2456 -0.2431 0.4760 0.060 Uiso 1 1 calc R . .
N3 N -0.13735(19) 0.19480(18) 0.16765(12) 0.0326(5) Uani 1 1 d . A .
H3A H -0.1836 0.1587 0.1789 0.039 Uiso 1 1 calc R . .
N4 N 0.34996(19) 0.0191(2) 0.16120(13) 0.0374(5) Uani 1 1 d . A .
H4A H 0.3962 0.0547 0.1473 0.045 Uiso 1 1 calc R . .
O1 O 0.49566(19) 0.1179(2) 0.06507(14) 0.0578(6) Uani 1 1 d . . .
O2 O 0.68794(19) 0.10315(19) 0.20760(13) 0.0512(5) Uani 1 1 d . . .
O4 O 0.7828(3) 0.5728(3) 0.52443(17) 0.0994(11) 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
C1 0.0339(13) 0.0286(12) 0.0299(12) -0.0112(10) 0.0077(10) -0.0159(10)
C2 0.0367(13) 0.0303(12) 0.0297(12) -0.0086(10) 0.0062(10) -0.0188(11)
C3 0.0482(16) 0.0312(13) 0.0371(14) -0.0104(11) 0.0072(12) -0.0239(12)
C4 0.0526(16) 0.0348(14) 0.0357(13) -0.0162(11) 0.0081(12) -0.0237(13)
C5 0.0468(16) 0.0380(14) 0.0318(13) -0.0153(11) 0.0124(11) -0.0213(12)
C6 0.0403(14) 0.0345(13) 0.0326(13) -0.0114(10) 0.0113(11) -0.0217(12)
C7 0.0331(13) 0.0330(13) 0.0299(12) -0.0097(10) 0.0099(10) -0.0201(11)
C8 0.0383(14) 0.0354(13) 0.0319(12) -0.0126(10) 0.0103(11) -0.0247(11)
C9 0.0430(15) 0.0447(15) 0.0324(13) -0.0152(11) 0.0110(11) -0.0290(13)
C10 0.0532(17) 0.0520(16) 0.0321(13) -0.0131(12) 0.0140(12) -0.0392(14)
C11 0.0486(16) 0.0425(15) 0.0336(13) -0.0114(11) 0.0097(12) -0.0318(13)
C12 0.0390(14) 0.0334(13) 0.0306(12) -0.0092(10) 0.0066(10) -0.0224(11)
C13 0.0502(16) 0.0577(17) 0.0291(13) -0.0154(12) 0.0139(12) -0.0380(14)
C14 0.0483(16) 0.0569(17) 0.0367(14) -0.0191(13) 0.0152(12) -0.0351(14)
C15 0.065(2) 0.078(2) 0.0402(16) -0.0313(15) 0.0207(15) -0.0496(18)
C16 0.088(3) 0.110(3) 0.0392(16) -0.0382(18) 0.0341(17) -0.075(2)
C17 0.095(3) 0.105(3) 0.0422(17) -0.0328(18) 0.0337(18) -0.082(3)
C18 0.067(2) 0.075(2) 0.0336(14) -0.0215(14) 0.0195(14) -0.0535(18)
C19 0.0602(18) 0.0547(17) 0.0367(14) -0.0149(13) 0.0138(13) -0.0444(16)
C20 0.071(2) 0.0516(18) 0.0408(15) -0.0082(13) 0.0071(14) -0.0450(17)
C21 0.078(2) 0.0538(18) 0.0386(15) -0.0125(13) 0.0103(15) -0.0487(17)
C22 0.084(2) 0.0544(19) 0.0551(19) -0.0169(15) 0.0131(17) -0.0468(19)
C23 0.101(3) 0.0552(19) 0.0472(18) -0.0149(15) 0.0081(18) -0.053(2)
C24 0.0459(15) 0.0347(13) 0.0266(12) -0.0112(10) 0.0080(11) -0.0218(12)
C25 0.0422(15) 0.0353(13) 0.0310(13) -0.0128(11) 0.0067(11) -0.0187(12)
C26 0.0423(15) 0.0406(15) 0.0413(15) -0.0166(12) 0.0064(12) -0.0160(13)
C27 0.0538(18) 0.0390(15) 0.0419(15) -0.0156(12) 0.0027(13) -0.0106(14)
C28 0.066(2) 0.0308(14) 0.0377(15) -0.0102(11) 0.0043(13) -0.0190(14)
C29 0.0603(18) 0.0376(14) 0.0325(13) -0.0120(11) 0.0100(12) -0.0283(14)
C30 0.0429(14) 0.0336(13) 0.0255(11) -0.0116(10) 0.0096(10) -0.0234(11)
C31 0.0436(15) 0.0404(14) 0.0267(12) -0.0121(10) 0.0110(11) -0.0285(12)
C32 0.0369(14) 0.0444(15) 0.0279(12) -0.0147(11) 0.0129(10) -0.0273(12)
C33 0.0366(13) 0.0345(13) 0.0252(11) -0.0126(10) 0.0106(10) -0.0206(11)
C34 0.0367(13) 0.0319(12) 0.0254(11) -0.0115(9) 0.0120(10) -0.0226(11)
C35 0.0352(13) 0.0357(13) 0.0256(11) -0.0134(10) 0.0109(10) -0.0208(11)
C36 0.0382(14) 0.0488(16) 0.0335(13) -0.0179(12) 0.0109(11) -0.0222(13)
C37 0.0380(15) 0.0575(18) 0.0447(16) -0.0207(14) 0.0097(12) -0.0215(14)
C38 0.0402(16) 0.0534(18) 0.0515(17) -0.0232(15) 0.0043(13) -0.0088(14)
C39 0.0519(18) 0.0394(15) 0.0496(17) -0.0163(13) 0.0045(14) -0.0160(14)
C40 0.0438(15) 0.0394(15) 0.0372(14) -0.0143(11) 0.0097(12) -0.0194(12)
C41 0.0387(14) 0.0420(14) 0.0281(12) -0.0154(11) 0.0105(10) -0.0210(12)
C42A 0.033(5) 0.030(4) 0.034(3) -0.009(3) 0.009(3) -0.019(4)
C43A 0.044(4) 0.046(4) 0.036(3) -0.007(3) 0.003(3) -0.030(4)
C44A 0.041(3) 0.047(3) 0.044(3) -0.020(2) 0.013(2) -0.028(3)
C45A 0.043(3) 0.048(3) 0.042(3) -0.015(2) 0.012(2) -0.027(3)
C46A 0.062(5) 0.056(4) 0.038(3) -0.004(3) -0.005(3) -0.042(4)
C42B 0.033(7) 0.037(6) 0.045(6) -0.012(4) 0.019(4) -0.020(6)
C43B 0.067(9) 0.061(8) 0.081(8) -0.034(7) 0.013(8) -0.044(8)
C44B 0.083(7) 0.060(6) 0.100(8) -0.035(5) 0.025(5) -0.049(6)
C45B 0.066(6) 0.048(5) 0.073(6) -0.007(4) 0.006(4) -0.030(5)
C46B 0.128(18) 0.100(13) 0.21(2) -0.061(13) 0.053(14) -0.096(15)
C47 0.0385(15) 0.0589(18) 0.0384(14) -0.0175(13) 0.0124(12) -0.0292(14)
C48 0.0505(18) 0.0615(19) 0.0485(17) -0.0170(15) 0.0190(14) -0.0348(16)
C49 0.0563(19) 0.059(2) 0.0548(19) -0.0230(16) 0.0133(15) -0.0254(16)
C50 0.0455(17) 0.061(2) 0.0506(18) -0.0157(15) 0.0027(14) -0.0229(15)
C51 0.100(3) 0.075(3) 0.065(2) -0.030(2) -0.008(2) -0.021(2)
C52 0.051(2) 0.090(3) 0.072(2) -0.013(2) 0.0170(18) -0.039(2)
C57 0.160(5) 0.105(4) 0.064(2) -0.023(2) 0.030(3) -0.097(4)
C56 0.116(4) 0.097(3) 0.072(3) -0.023(2) 0.029(3) -0.068(3)
C58 0.138(5) 0.130(5) 0.087(3) -0.038(3) 0.027(3) -0.086(4)
N1 0.0386(11) 0.0326(11) 0.0294(10) -0.0134(8) 0.0132(9) -0.0234(9)
N2 0.0762(18) 0.0766(18) 0.0351(12) -0.0236(12) 0.0244(12) -0.0634(16)
N3 0.0346(11) 0.0336(11) 0.0377(11) -0.0135(9) 0.0114(9) -0.0205(9)
N4 0.0369(12) 0.0486(13) 0.0390(12) -0.0150(10) 0.0125(10) -0.0285(11)
O1 0.0466(12) 0.0702(15) 0.0720(15) -0.0244(12) 0.0272(11) -0.0375(11)
O2 0.0497(12) 0.0653(14) 0.0521(12) -0.0184(10) 0.0111(10) -0.0360(11)
O4 0.161(3) 0.111(2) 0.0648(17) -0.0042(16) 0.0163(18) -0.105(3)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.388(3) . ?
C1 C6 1.390(3) . ?
C1 C2 1.415(3) . ?
C2 C3 1.406(3) . ?
C2 C12 1.454(3) . ?
C3 C4 1.384(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.401(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.378(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.382(3) . ?
C7 N1 1.399(3) . ?
C7 C12 1.428(3) . ?
C8 C9 1.395(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.424(3) . ?
C9 C13 1.455(3) . ?
C10 N2 1.398(3) . ?
C10 C11 1.388(4) . ?
C11 C12 1.398(3) . ?
C11 C19 1.513(3) . ?
C13 C14 1.397(4) . ?
C13 C18 1.410(4) . ?
C14 C15 1.386(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.405(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.370(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.402(4) . ?
C17 H17 0.9500 . ?
C18 N2 1.377(4) . ?
C19 C20 1.517(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.530(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.505(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.522(4) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C29 1.402(3) . ?
C24 C25 1.419(4) . ?
C24 C30 1.457(4) . ?
C25 N3 1.384(3) . ?
C25 C26 1.385(4) . ?
C26 C27 1.380(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.396(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.378(4) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 C31 1.400(3) . ?
C30 C35 1.431(3) . ?
C31 C32 1.391(4) . ?
C31 C42A 1.512(11) . ?
C31 C42B 1.522(15) . ?
C32 N4 1.396(3) . ?
C32 C33 1.427(3) . ?
C33 C34 1.395(3) . ?
C33 C41 1.448(4) . ?
C34 C35 1.384(3) . ?
C34 N1 1.426(3) . ?
C35 N3 1.385(3) . ?
C36 N4 1.371(3) . ?
C36 C37 1.390(4) . ?
C36 C41 1.421(4) . ?
C37 C38 1.375(4) . ?
C37 H37 0.9500 . ?
C38 C39 1.399(4) . ?
C38 H38 0.9500 . ?
C39 C40 1.378(4) . ?
C39 H39 0.9500 . ?
C40 C41 1.395(4) . ?
C40 H40 0.9500 . ?
C42A C43A 1.521(7) . ?
C42A H42A 0.9900 . ?
C42A H42B 0.9900 . ?
C43A C44A 1.525(6) . ?
C43A H43A 0.9900 . ?
C43A H43B 0.9900 . ?
C44A C45A 1.496(6) . ?
C44A H44A 0.9900 . ?
C44A H44B 0.9900 . ?
C45A C46A 1.536(7) . ?
C45A H45A 0.9900 . ?
C45A H45B 0.9900 . ?
C46A H46A 0.9800 . ?
C46A H46B 0.9800 . ?
C46A H46C 0.9800 . ?
C42B C43B 1.515(9) . ?
C42B H42C 0.9900 . ?
C42B H42D 0.9900 . ?
C43B C44B 1.514(9) . ?
C43B H43C 0.9900 . ?
C43B H43D 0.9900 . ?
C44B C45B 1.478(8) . ?
C44B H44C 0.9900 . ?
C44B H44D 0.9900 . ?
C45B C46B 1.524(9) . ?
C45B H45C 0.9900 . ?
C45B H45D 0.9900 . ?
C46B H46D 0.9800 . ?
C46B H46E 0.9800 . ?
C46B H46F 0.9800 . ?
C47 O1 1.209(3) . ?
C47 C49 1.491(4) . ?
C47 C48 1.502(4) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 O2 1.214(4) . ?
C50 C52 1.501(5) . ?
C50 C51 1.502(5) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C57 C56 1.460(6) . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C56 O4 1.238(5) . ?
C56 C58 1.507(6) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
N2 H2 0.8800 . ?
N3 H3A 0.8800 . ?
N4 H4A 0.8800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C6 128.2(2) . . ?
N1 C1 C2 109.2(2) . . ?
C6 C1 C2 122.6(2) . . ?
C3 C2 C1 118.0(2) . . ?
C3 C2 C12 135.1(2) . . ?
C1 C2 C12 106.9(2) . . ?
C4 C3 C2 119.5(2) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C4 C5 120.9(2) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C6 C5 C4 121.1(2) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C5 C6 C1 117.8(2) . . ?
C5 C6 H6 121.1 . . ?
C1 C6 H6 121.1 . . ?
C8 C7 N1 128.0(2) . . ?
C8 C7 C12 123.4(2) . . ?
N1 C7 C12 108.6(2) . . ?
C7 C8 C9 116.2(2) . . ?
C7 C8 H8 121.9 . . ?
C9 C8 H8 121.9 . . ?
C8 C9 C10 120.4(2) . . ?
C8 C9 C13 133.0(2) . . ?
C10 C9 C13 106.5(2) . . ?
N2 C10 C11 127.9(2) . . ?
N2 C10 C9 108.4(2) . . ?
C11 C10 C9 123.6(2) . . ?
C10 C11 C12 115.8(2) . . ?
C10 C11 C19 121.6(2) . . ?
C12 C11 C19 122.6(2) . . ?
C11 C12 C7 120.6(2) . . ?
C11 C12 C2 133.0(2) . . ?
C7 C12 C2 106.4(2) . . ?
C14 C13 C18 119.9(2) . . ?
C14 C13 C9 133.8(2) . . ?
C18 C13 C9 106.3(2) . . ?
C15 C14 C13 118.8(2) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
C14 C15 C16 120.6(3) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
C17 C16 C15 121.6(3) . . ?
C17 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
C16 C17 C18 118.1(3) . . ?
C16 C17 H17 120.9 . . ?
C18 C17 H17 120.9 . . ?
N2 C18 C17 129.2(3) . . ?
N2 C18 C13 109.8(2) . . ?
C17 C18 C13 121.0(3) . . ?
C11 C19 C20 113.5(2) . . ?
C11 C19 H19A 108.9 . . ?
C20 C19 H19A 108.9 . . ?
C11 C19 H19B 108.9 . . ?
C20 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
C19 C20 C21 113.1(3) . . ?
C19 C20 H20A 109.0 . . ?
C21 C20 H20A 109.0 . . ?
C19 C20 H20B 109.0 . . ?
C21 C20 H20B 109.0 . . ?
H20A C20 H20B 107.8 . . ?
C22 C21 C20 112.9(3) . . ?
C22 C21 H21A 109.0 . . ?
C20 C21 H21A 109.0 . . ?
C22 C21 H21B 109.0 . . ?
C20 C21 H21B 109.0 . . ?
H21A C21 H21B 107.8 . . ?
C21 C22 C23 113.3(3) . . ?
C21 C22 H22A 108.9 . . ?
C23 C22 H22A 108.9 . . ?
C21 C22 H22B 108.9 . . ?
C23 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C29 C24 C25 118.2(3) . . ?
C29 C24 C30 134.9(3) . . ?
C25 C24 C30 106.9(2) . . ?
N3 C25 C26 128.6(2) . . ?
N3 C25 C24 108.9(2) . . ?
C26 C25 C24 122.5(2) . . ?
C27 C26 C25 117.6(3) . . ?
C27 C26 H26 121.2 . . ?
C25 C26 H26 121.2 . . ?
C26 C27 C28 121.4(3) . . ?
C26 C27 H27 119.3 . . ?
C28 C27 H27 119.3 . . ?
C29 C28 C27 121.1(3) . . ?
C29 C28 H28 119.5 . . ?
C27 C28 H28 119.5 . . ?
C28 C29 C24 119.3(3) . . ?
C28 C29 H29 120.3 . . ?
C24 C29 H29 120.3 . . ?
C31 C30 C35 120.7(2) . . ?
C31 C30 C24 133.3(2) . . ?
C35 C30 C24 105.8(2) . . ?
C32 C31 C30 115.8(2) . . ?
C32 C31 C42A 115.8(6) . . ?
C30 C31 C42A 128.4(6) . . ?
C32 C31 C42B 126.5(9) . . ?
C30 C31 C42B 117.7(9) . . ?
N4 C32 C31 127.9(2) . . ?
N4 C32 C33 108.1(2) . . ?
C31 C32 C33 123.9(2) . . ?
C34 C33 C32 119.5(2) . . ?
C34 C33 C41 134.0(2) . . ?
C32 C33 C41 106.5(2) . . ?
C35 C34 C33 117.5(2) . . ?
C35 C34 N1 121.0(2) . . ?
C33 C34 N1 121.4(2) . . ?
N3 C35 C34 128.4(2) . . ?
N3 C35 C30 109.0(2) . . ?
C34 C35 C30 122.5(2) . . ?
N4 C36 C37 129.3(3) . . ?
N4 C36 C41 109.1(2) . . ?
C37 C36 C41 121.7(3) . . ?
C38 C37 C36 118.0(3) . . ?
C38 C37 H37 121.0 . . ?
C36 C37 H37 121.0 . . ?
C37 C38 C39 121.3(3) . . ?
C37 C38 H38 119.4 . . ?
C39 C38 H38 119.4 . . ?
C40 C39 C38 121.1(3) . . ?
C40 C39 H39 119.5 . . ?
C38 C39 H39 119.5 . . ?
C39 C40 C41 119.2(3) . . ?
C39 C40 H40 120.4 . . ?
C41 C40 H40 120.4 . . ?
C40 C41 C36 118.9(2) . . ?
C40 C41 C33 134.5(2) . . ?
C36 C41 C33 106.7(2) . . ?
C31 C42A C43A 111.7(8) . . ?
C31 C42A H42A 109.3 . . ?
C43A C42A H42A 109.3 . . ?
C31 C42A H42B 109.3 . . ?
C43A C42A H42B 109.3 . . ?
H42A C42A H42B 107.9 . . ?
C42A C43A C44A 113.0(7) . . ?
C42A C43A H43A 109.0 . . ?
C44A C43A H43A 109.0 . . ?
C42A C43A H43B 109.0 . . ?
C44A C43A H43B 109.0 . . ?
H43A C43A H43B 107.8 . . ?
C45A C44A C43A 113.8(5) . . ?
C45A C44A H44A 108.8 . . ?
C43A C44A H44A 108.8 . . ?
C45A C44A H44B 108.8 . . ?
C43A C44A H44B 108.8 . . ?
H44A C44A H44B 107.7 . . ?
C44A C45A C46A 111.5(6) . . ?
C44A C45A H45A 109.3 . . ?
C46A C45A H45A 109.3 . . ?
C44A C45A H45B 109.3 . . ?
C46A C45A H45B 109.3 . . ?
H45A C45A H45B 108.0 . . ?
C43B C42B C31 112.6(12) . . ?
C43B C42B H42C 109.1 . . ?
C31 C42B H42C 109.1 . . ?
C43B C42B H42D 109.1 . . ?
C31 C42B H42D 109.1 . . ?
H42C C42B H42D 107.8 . . ?
C44B C43B C42B 113.2(11) . . ?
C44B C43B H43C 108.9 . . ?
C42B C43B H43C 108.9 . . ?
C44B C43B H43D 108.9 . . ?
C42B C43B H43D 108.9 . . ?
H43C C43B H43D 107.8 . . ?
C45B C44B C43B 116.5(9) . . ?
C45B C44B H44C 108.2 . . ?
C43B C44B H44C 108.2 . . ?
C45B C44B H44D 108.2 . . ?
C43B C44B H44D 108.2 . . ?
H44C C44B H44D 107.3 . . ?
C44B C45B C46B 111.1(12) . . ?
C44B C45B H45C 109.4 . . ?
C46B C45B H45C 109.4 . . ?
C44B C45B H45D 109.4 . . ?
C46B C45B H45D 109.4 . . ?
H45C C45B H45D 108.0 . . ?
C45B C46B H46D 109.5 . . ?
C45B C46B H46E 109.5 . . ?
H46D C46B H46E 109.5 . . ?
C45B C46B H46F 109.5 . . ?
H46D C46B H46F 109.5 . . ?
H46E C46B H46F 109.5 . . ?
O1 C47 C49 122.2(3) . . ?
O1 C47 C48 120.8(3) . . ?
C49 C47 C48 116.9(2) . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
O2 C50 C52 120.8(3) . . ?
O2 C50 C51 121.3(3) . . ?
C52 C50 C51 117.9(3) . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C50 C52 H52A 109.5 . . ?
C50 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C50 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
O4 C56 C57 124.5(4) . . ?
O4 C56 C58 118.9(4) . . ?
C57 C56 C58 116.5(4) . . ?
C56 C58 H58A 109.5 . . ?
C56 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C56 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C1 N1 C7 108.92(18) . . ?
C1 N1 C34 123.98(19) . . ?
C7 N1 C34 127.03(19) . . ?
C18 N2 C10 108.9(2) . . ?
C18 N2 H2 125.6 . . ?
C10 N2 H2 125.6 . . ?
C35 N3 C25 109.3(2) . . ?
C35 N3 H3A 125.3 . . ?
C25 N3 H3A 125.3 . . ?
C36 N4 C32 109.6(2) . . ?
C36 N4 H4A 125.2 . . ?
C32 N4 H4A 125.2 . . ?

_diffrn_measured_fraction_theta_max 0.945
_diffrn_reflns_theta_full        70.97
_diffrn_measured_fraction_theta_full 0.945
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.058