# Supplementary Material (ESI) for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Claudio Pettinari'
_publ_contact_author_email       CLAUDIO.PETTINARI@UNICAM.IT

_publ_section_title              
;
Crystal structure, supramolecular assembly and preliminary
reactivity behaviour of new heteropolytopic ligands based on oxalate/malonate
skeleton and azolate moieties
;
loop_
_publ_author_name
'Claudio Pettinari'
'Federica Garau'
'Magda Monari'
'Luciano Pandolfo'
'Alfonso Venzo'

# Attachment 'comp1a.cif'

data_legpa
_database_code_depnum_ccdc_archive 'CCDC 746838'
#TrackingRef 'comp1a.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H6 N4 O2'
_chemical_formula_weight         190.17

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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

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

_cell_length_a                   11.0178(5)
_cell_length_b                   7.5596(4)
_cell_length_c                   10.9232(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.5910(10)
_cell_angle_gamma                90.00
_cell_volume                     871.92(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             392
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11100
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.93
_diffrn_reflns_theta_max         30.05
_reflns_number_total             2558
_reflns_number_gt                1827
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(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^)+(0.0697P)^2^+0.1266P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2558
_refine_ls_number_parameters     127
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0477
_refine_ls_wR_factor_ref         0.1381
_refine_ls_wR_factor_gt          0.1235
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_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
N2 N 0.68554(12) 0.21799(16) 0.53893(10) 0.0358(3) Uani 1 1 d . . .
N1 N 0.66698(10) 0.29356(15) 0.64688(10) 0.0296(3) Uani 1 1 d . . .
O2 O 0.61880(11) 0.61523(15) 0.45373(10) 0.0461(3) Uani 1 1 d . . .
C1 C 0.67343(13) 0.47547(18) 0.66009(12) 0.0323(3) Uani 1 1 d . . .
O1 O 0.65261(12) 0.55378(15) 0.74771(10) 0.0489(3) Uani 1 1 d . . .
N3 N 0.82633(12) 0.62158(16) 0.57010(12) 0.0391(3) Uani 1 1 d . . .
C2 C 0.70080(14) 0.57347(18) 0.54747(13) 0.0328(3) Uani 1 1 d . . .
C5 C 0.63530(14) 0.17042(19) 0.72457(13) 0.0354(3) Uani 1 1 d . . .
H5 H 0.6182 0.1918 0.8018 0.042 Uiso 1 1 calc R . .
C3 C 0.66431(16) 0.0485(2) 0.55255(14) 0.0409(3) Uani 1 1 d . . .
H3 H 0.6689 -0.0376 0.4932 0.049 Uiso 1 1 calc R . .
C4 C 0.63384(15) 0.0121(2) 0.66703(14) 0.0406(3) Uani 1 1 d . . .
H4 H 0.6164 -0.0977 0.6966 0.049 Uiso 1 1 calc R . .
N4 N 0.91133(13) 0.5755(2) 0.68431(14) 0.0536(4) Uani 1 1 d . . .
C8 C 0.88253(18) 0.7176(2) 0.49392(18) 0.0516(4) Uani 1 1 d . . .
H8 H 0.8433 0.7626 0.4130 0.062 Uiso 1 1 calc R . .
C7 C 1.0049(2) 0.7333(3) 0.5595(2) 0.0703(6) Uani 1 1 d . . .
H7 H 1.0680 0.7907 0.5335 0.084 Uiso 1 1 calc R . .
C6 C 1.01841(19) 0.6443(3) 0.6766(2) 0.0713(6) Uani 1 1 d . . .
H6 H 1.0945 0.6354 0.7409 0.086 Uiso 1 1 calc R . .

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
N2 0.0473(7) 0.0342(6) 0.0281(5) -0.0010(4) 0.0145(5) 0.0021(5)
N1 0.0346(6) 0.0305(6) 0.0245(5) -0.0005(4) 0.0100(4) -0.0007(4)
O2 0.0462(6) 0.0473(6) 0.0400(6) 0.0098(5) 0.0046(5) 0.0016(5)
C1 0.0352(7) 0.0328(7) 0.0286(6) -0.0015(5) 0.0086(5) -0.0008(5)
O1 0.0722(8) 0.0399(6) 0.0416(6) -0.0088(5) 0.0277(6) -0.0032(5)
N3 0.0381(7) 0.0386(7) 0.0403(7) 0.0045(5) 0.0111(5) -0.0017(5)
C2 0.0400(7) 0.0275(6) 0.0310(6) -0.0009(5) 0.0105(6) 0.0006(5)
C5 0.0409(7) 0.0375(7) 0.0298(6) 0.0030(5) 0.0132(6) -0.0025(6)
C3 0.0540(9) 0.0324(7) 0.0366(7) -0.0032(6) 0.0135(7) 0.0021(6)
C4 0.0506(8) 0.0316(7) 0.0398(7) 0.0042(6) 0.0134(7) -0.0039(6)
N4 0.0401(7) 0.0655(10) 0.0488(8) 0.0075(7) 0.0023(6) -0.0038(7)
C8 0.0584(11) 0.0462(9) 0.0583(10) 0.0074(8) 0.0296(9) -0.0040(8)
C7 0.0555(12) 0.0709(13) 0.0943(16) -0.0018(12) 0.0370(12) -0.0187(10)
C6 0.0391(9) 0.0891(16) 0.0793(15) -0.0021(12) 0.0070(9) -0.0110(9)

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
N2 C3 1.3183(19) . ?
N2 N1 1.3771(14) . ?
N1 C5 1.3703(17) . ?
N1 C1 1.3825(18) . ?
O2 C2 1.1983(17) . ?
C1 O1 1.2018(16) . ?
C1 C2 1.5378(18) . ?
N3 N4 1.3738(18) . ?
N3 C8 1.377(2) . ?
N3 C2 1.3824(19) . ?
C5 C4 1.350(2) . ?
C3 C4 1.411(2) . ?
N4 C6 1.314(3) . ?
C8 C7 1.339(3) . ?
C7 C6 1.415(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 N2 N1 103.41(11) . . ?
C5 N1 N2 112.02(11) . . ?
C5 N1 C1 128.73(11) . . ?
N2 N1 C1 119.10(10) . . ?
O1 C1 N1 123.87(12) . . ?
O1 C1 C2 121.69(12) . . ?
N1 C1 C2 114.31(10) . . ?
N4 N3 C8 112.01(13) . . ?
N4 N3 C2 118.92(12) . . ?
C8 N3 C2 129.05(13) . . ?
O2 C2 N3 123.72(13) . . ?
O2 C2 C1 122.57(13) . . ?
N3 C2 C1 113.47(12) . . ?
C4 C5 N1 106.58(12) . . ?
N2 C3 C4 112.61(13) . . ?
C5 C4 C3 105.38(13) . . ?
C6 N4 N3 103.50(16) . . ?
C7 C8 N3 106.30(17) . . ?
C8 C7 C6 105.76(16) . . ?
N4 C6 C7 112.42(19) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C2 C1 O1 -89.93(18) . . . . ?
N1 C1 C2 N3 -99.32(14) . . . . ?
O1 C1 C2 O2 -89.93(18) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        30.05
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.047

# Attachment 'comp1c.cif'

data_ind_0m
_database_code_depnum_ccdc_archive 'CCDC 746839'
#TrackingRef 'comp1c.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H10 N4 O2'
_chemical_formula_weight         290.28

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           ?
_symmetry_space_group_name_H-M   ?

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

_cell_length_a                   7.3930(10)
_cell_length_b                   7.6748(11)
_cell_length_c                   12.1165(17)
_cell_angle_alpha                75.374(2)
_cell_angle_beta                 83.368(2)
_cell_angle_gamma                79.040(2)
_cell_volume                     651.43(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             300
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5408
_diffrn_reflns_av_R_equivalents  0.0128
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.74
_diffrn_reflns_theta_max         27.48
_reflns_number_total             2908
_reflns_number_gt                2599
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(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^)+(0.0556P)^2^+0.1821P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2908
_refine_ls_number_parameters     199
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0361
_refine_ls_wR_factor_ref         0.1002
_refine_ls_wR_factor_gt          0.0966
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_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
C2 C 0.22486(15) 0.33673(15) 0.27997(9) 0.0160(2) Uani 1 1 d . . .
C9 C 0.26854(15) 0.01842(15) 0.07960(9) 0.0165(2) Uani 1 1 d . . .
C1 C 0.26188(15) 0.14989(15) 0.24971(9) 0.0167(2) Uani 1 1 d . . .
C6 C 0.29044(17) -0.18662(18) -0.07794(11) 0.0249(3) Uani 1 1 d . . .
H6 H 0.2985 -0.2588 -0.1301 0.030 Uiso 1 1 calc R . .
C8 C 0.33929(16) -0.16687(15) 0.11369(10) 0.0190(2) Uani 1 1 d . . .
H8 H 0.3785 -0.2200 0.1867 0.023 Uiso 1 1 calc R . .
C4 C 0.21109(15) 0.10203(16) -0.03017(10) 0.0191(2) Uani 1 1 d . . .
C7 C 0.34785(17) -0.26743(16) 0.03255(11) 0.0225(3) Uani 1 1 d . . .
H7 H 0.3929 -0.3921 0.0518 0.027 Uiso 1 1 calc R . .
C3 C 0.15009(16) 0.29075(16) -0.02963(10) 0.0213(2) Uani 1 1 d . . .
H3 H 0.1040 0.3791 -0.0924 0.026 Uiso 1 1 calc R . .
C5 C 0.22227(17) -0.00250(18) -0.11093(10) 0.0235(3) Uani 1 1 d . . .
H5 H 0.1850 0.0505 -0.1844 0.028 Uiso 1 1 calc R . .
C16 C -0.03489(15) 0.55068(15) 0.35192(9) 0.0161(2) Uani 1 1 d . . .
C11 C -0.22372(16) 0.54295(16) 0.37155(9) 0.0189(2) Uani 1 1 d . . .
C13 C -0.26982(19) 0.82223(17) 0.43058(10) 0.0261(3) Uani 1 1 d . . .
H13 H -0.3471 0.9159 0.4571 0.031 Uiso 1 1 calc R . .
C14 C -0.07993(18) 0.82630(16) 0.41143(10) 0.0232(3) Uani 1 1 d . . .
H14 H -0.0345 0.9226 0.4260 0.028 Uiso 1 1 calc R . .
C12 C -0.34460(17) 0.68222(17) 0.41092(10) 0.0238(3) Uani 1 1 d . . .
H12 H -0.4708 0.6803 0.4233 0.029 Uiso 1 1 calc R . .
C15 C 0.04239(16) 0.69109(15) 0.37143(9) 0.0189(2) Uani 1 1 d . . .
H15 H 0.1683 0.6941 0.3584 0.023 Uiso 1 1 calc R . .
C10 C -0.24398(16) 0.37661(16) 0.34398(10) 0.0213(2) Uani 1 1 d . . .
H10 H -0.3563 0.3361 0.3497 0.026 Uiso 1 1 calc R . .
O2 O 0.34912(11) 0.41859(11) 0.28045(7) 0.0211(2) Uani 1 1 d . . .
O1 O 0.31768(12) 0.01183(11) 0.31909(7) 0.0220(2) Uani 1 1 d . . .
N1 N 0.23911(13) 0.15782(12) 0.13781(8) 0.0168(2) Uani 1 1 d . . .
N3 N 0.04442(13) 0.39427(12) 0.31377(8) 0.0161(2) Uani 1 1 d . . .
N4 N -0.08696(13) 0.28868(13) 0.31005(8) 0.0196(2) Uani 1 1 d . . .
N2 N 0.16646(13) 0.32481(13) 0.06861(8) 0.0196(2) 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
C2 0.0170(5) 0.0159(5) 0.0143(5) -0.0028(4) -0.0033(4) -0.0003(4)
C9 0.0158(5) 0.0174(5) 0.0174(5) -0.0062(4) 0.0011(4) -0.0035(4)
C1 0.0143(5) 0.0177(5) 0.0181(5) -0.0055(4) -0.0014(4) -0.0010(4)
C6 0.0271(6) 0.0287(7) 0.0245(6) -0.0149(5) 0.0029(5) -0.0093(5)
C8 0.0193(5) 0.0179(6) 0.0188(5) -0.0045(4) 0.0010(4) -0.0022(4)
C4 0.0168(5) 0.0223(6) 0.0178(5) -0.0043(4) 0.0000(4) -0.0039(4)
C7 0.0236(6) 0.0189(6) 0.0261(6) -0.0086(5) 0.0044(5) -0.0055(5)
C3 0.0221(6) 0.0218(6) 0.0180(5) -0.0020(4) -0.0027(4) -0.0019(4)
C5 0.0242(6) 0.0303(7) 0.0180(5) -0.0080(5) -0.0012(4) -0.0067(5)
C16 0.0196(5) 0.0148(5) 0.0124(5) -0.0032(4) -0.0026(4) 0.0019(4)
C11 0.0196(5) 0.0205(6) 0.0150(5) -0.0031(4) -0.0026(4) 0.0001(4)
C13 0.0342(7) 0.0217(6) 0.0183(5) -0.0064(5) 0.0001(5) 0.0064(5)
C14 0.0362(7) 0.0162(5) 0.0167(5) -0.0049(4) -0.0031(5) -0.0013(5)
C12 0.0211(6) 0.0261(6) 0.0195(6) -0.0042(5) 0.0005(4) 0.0043(5)
C15 0.0244(6) 0.0167(5) 0.0154(5) -0.0032(4) -0.0024(4) -0.0030(4)
C10 0.0173(5) 0.0247(6) 0.0223(6) -0.0061(5) -0.0027(4) -0.0033(4)
O2 0.0176(4) 0.0210(4) 0.0258(4) -0.0067(3) -0.0027(3) -0.0035(3)
O1 0.0269(4) 0.0177(4) 0.0196(4) -0.0039(3) -0.0058(3) 0.0025(3)
N1 0.0185(5) 0.0134(4) 0.0174(5) -0.0036(3) -0.0025(4) 0.0012(3)
N3 0.0168(5) 0.0139(4) 0.0192(5) -0.0063(3) -0.0027(4) -0.0020(4)
N4 0.0181(5) 0.0202(5) 0.0227(5) -0.0065(4) -0.0037(4) -0.0050(4)
N2 0.0208(5) 0.0155(5) 0.0199(5) -0.0012(4) -0.0031(4) 0.0004(4)

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
C2 O2 1.2089(14) . ?
C2 N3 1.3724(14) . ?
C2 C1 1.5357(15) . ?
C9 C8 1.3917(16) . ?
C9 N1 1.3951(14) . ?
C9 C4 1.3989(16) . ?
C1 O1 1.2098(14) . ?
C1 N1 1.3702(14) . ?
C6 C5 1.3788(18) . ?
C6 C7 1.4031(18) . ?
C6 H6 0.9300 . ?
C8 C7 1.3844(16) . ?
C8 H8 0.9300 . ?
C4 C5 1.4002(16) . ?
C4 C3 1.4342(17) . ?
C7 H7 0.9300 . ?
C3 N2 1.3047(16) . ?
C3 H3 0.9300 . ?
C5 H5 0.9300 . ?
C16 C15 1.3919(16) . ?
C16 N3 1.3959(14) . ?
C16 C11 1.3988(16) . ?
C11 C12 1.4016(16) . ?
C11 C10 1.4365(17) . ?
C13 C12 1.3793(19) . ?
C13 C14 1.4013(19) . ?
C13 H13 0.9300 . ?
C14 C15 1.3876(16) . ?
C14 H14 0.9300 . ?
C12 H12 0.9300 . ?
C15 H15 0.9300 . ?
C10 N4 1.3054(15) . ?
C10 H10 0.9300 . ?
N1 N2 1.3905(13) . ?
N3 N4 1.3892(13) . ?

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
O2 C2 N3 123.67(10) . . ?
O2 C2 C1 121.44(10) . . ?
N3 C2 C1 114.73(9) . . ?
C8 C9 N1 131.56(10) . . ?
C8 C9 C4 123.04(10) . . ?
N1 C9 C4 105.40(10) . . ?
O1 C1 N1 124.55(10) . . ?
O1 C1 C2 121.09(10) . . ?
N1 C1 C2 114.19(9) . . ?
C5 C6 C7 121.45(11) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
C7 C8 C9 116.08(11) . . ?
C7 C8 H8 122.0 . . ?
C9 C8 H8 122.0 . . ?
C9 C4 C5 119.77(11) . . ?
C9 C4 C3 105.14(10) . . ?
C5 C4 C3 135.09(11) . . ?
C8 C7 C6 121.87(11) . . ?
C8 C7 H7 119.1 . . ?
C6 C7 H7 119.1 . . ?
N2 C3 C4 112.51(10) . . ?
N2 C3 H3 123.7 . . ?
C4 C3 H3 123.7 . . ?
C6 C5 C4 117.79(11) . . ?
C6 C5 H5 121.1 . . ?
C4 C5 H5 121.1 . . ?
C15 C16 N3 131.60(10) . . ?
C15 C16 C11 122.95(10) . . ?
N3 C16 C11 105.44(10) . . ?
C16 C11 C12 119.98(11) . . ?
C16 C11 C10 105.12(10) . . ?
C12 C11 C10 134.90(11) . . ?
C12 C13 C14 121.41(11) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C15 C14 C13 122.06(11) . . ?
C15 C14 H14 119.0 . . ?
C13 C14 H14 119.0 . . ?
C13 C12 C11 117.66(11) . . ?
C13 C12 H12 121.2 . . ?
C11 C12 H12 121.2 . . ?
C14 C15 C16 115.94(11) . . ?
C14 C15 H15 122.0 . . ?
C16 C15 H15 122.0 . . ?
N4 C10 C11 112.39(10) . . ?
N4 C10 H10 123.8 . . ?
C11 C10 H10 123.8 . . ?
C1 N1 N2 118.42(9) . . ?
C1 N1 C9 129.91(10) . . ?
N2 N1 C9 111.58(9) . . ?
C2 N3 N4 118.70(9) . . ?
C2 N3 C16 129.74(10) . . ?
N4 N3 C16 111.56(9) . . ?
C10 N4 N3 105.49(9) . . ?
C3 N2 N1 105.37(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 O2 79.35(14) . . . . ?
O1 C1 C2 O2 79.35(14) . . . . ?
N1 C1 C2 O2 -96.18(13) . . . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.049

# Attachment 'comp2a.cif'

data_ligim
_database_code_depnum_ccdc_archive 'CCDC 746840'
#TrackingRef 'comp2a.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H8 N4 O2'
_chemical_formula_weight         204.19

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           ?
_symmetry_space_group_name_H-M   ?

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

_cell_length_a                   10.0116(4)
_cell_length_b                   9.8622(4)
_cell_length_c                   19.4872(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.4370(10)
_cell_angle_gamma                90.00
_cell_volume                     1863.34(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             848
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23968
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.11
_diffrn_reflns_theta_max         30.05
_reflns_number_total             5432
_reflns_number_gt                3760
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(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^)+(0.0525P)^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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5432
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0436
_refine_ls_wR_factor_ref         0.1114
_refine_ls_wR_factor_gt          0.1016
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_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
N7 N 0.97913(11) 0.24720(11) 0.26006(6) 0.0175(2) Uani 1 1 d . . .
N8 N 1.05436(12) 0.15707(12) 0.30841(6) 0.0216(3) Uani 1 1 d . . .
N6 N 0.65727(11) 0.04119(11) 0.16328(6) 0.0186(2) Uani 1 1 d . . .
N5 N 0.56783(11) 0.09754(11) 0.19821(6) 0.0172(2) Uani 1 1 d . . .
O4 O 0.77294(10) 0.33879(9) 0.20611(5) 0.0220(2) Uani 1 1 d . . .
O3 O 0.53635(10) 0.20273(11) 0.29600(5) 0.0295(3) Uani 1 1 d . . .
C12 C 0.83593(13) 0.25722(13) 0.24839(7) 0.0172(3) Uani 1 1 d . . .
C11 C 0.77172(13) 0.16329(13) 0.29182(7) 0.0188(3) Uani 1 1 d . . .
H112 H 0.7954 0.1933 0.3408 0.023 Uiso 1 1 calc R . .
H111 H 0.8086 0.0727 0.2903 0.023 Uiso 1 1 calc R . .
C10 C 0.61675(14) 0.15950(13) 0.26454(7) 0.0192(3) Uani 1 1 d . . .
C16 C 1.18249(15) 0.17610(14) 0.30403(8) 0.0240(3) Uani 1 1 d . . .
H16 H 1.2578 0.1287 0.3310 0.029 Uiso 1 1 calc R . .
C17 C 1.19236(14) 0.27661(14) 0.25380(7) 0.0221(3) Uani 1 1 d . . .
H17 H 1.2718 0.3068 0.2420 0.027 Uiso 1 1 calc R . .
C18 C 1.06163(14) 0.31931(13) 0.22660(7) 0.0194(3) Uani 1 1 d . . .
H18 H 1.0330 0.3851 0.1918 0.023 Uiso 1 1 calc R . .
C13 C 0.57561(14) -0.00549(13) 0.10400(7) 0.0197(3) Uani 1 1 d . . .
H13 H 0.6073 -0.0499 0.0690 0.024 Uiso 1 1 calc R . .
C14 C 0.43486(14) 0.01946(14) 0.09969(7) 0.0202(3) Uani 1 1 d . . .
H14 H 0.3595 -0.0044 0.0631 0.024 Uiso 1 1 calc R . .
C15 C 0.43320(13) 0.08554(13) 0.16031(7) 0.0190(3) Uani 1 1 d . . .
H15 H 0.3557 0.1168 0.1737 0.023 Uiso 1 1 calc R . .
N1 N -0.00980(11) 0.16437(11) 0.05416(6) 0.0176(2) Uani 1 1 d . . .
O1 O -0.12670(11) 0.34636(11) -0.00024(6) 0.0327(3) Uani 1 1 d . . .
O2 O 0.20313(10) 0.39679(10) 0.10402(5) 0.0237(2) Uani 1 1 d . . .
N2 N 0.10675(11) 0.08587(11) 0.06720(6) 0.0202(3) Uani 1 1 d . . .
N3 N 0.35322(11) 0.34951(11) 0.03750(6) 0.0172(2) Uani 1 1 d . . .
N4 N 0.37740(12) 0.29925(11) -0.02405(6) 0.0193(2) Uani 1 1 d . . .
C1 C -0.02128(14) 0.28133(14) 0.01232(7) 0.0203(3) Uani 1 1 d . . .
C2 C 0.10428(14) 0.31560(14) -0.01367(7) 0.0205(3) Uani 1 1 d . . .
H2A H 0.1317 0.2375 -0.0371 0.025 Uiso 1 1 calc R . .
H2B H 0.0831 0.3893 -0.0476 0.025 Uiso 1 1 calc R . .
C3 C 0.22029(14) 0.35665(12) 0.04818(7) 0.0176(3) Uani 1 1 d . . .
C4 C 0.08187(14) -0.01035(14) 0.10927(7) 0.0224(3) Uani 1 1 d . . .
H4 H 0.1432 -0.0803 0.1269 0.027 Uiso 1 1 calc R . .
C5 C -0.04804(14) 0.00411(14) 0.12476(7) 0.0223(3) Uani 1 1 d . . .
H5 H -0.0866 -0.0512 0.1534 0.027 Uiso 1 1 calc R . .
C6 C -0.10409(14) 0.11677(14) 0.08859(7) 0.0202(3) Uani 1 1 d . . .
H6 H -0.1898 0.1543 0.0874 0.024 Uiso 1 1 calc R . .
C7 C 0.51249(14) 0.30860(13) -0.01362(7) 0.0208(3) Uani 1 1 d . . .
H7 H 0.5599 0.2827 -0.0469 0.025 Uiso 1 1 calc R . .
C8 C 0.57701(15) 0.36225(13) 0.05359(7) 0.0205(3) Uani 1 1 d . . .
H8 H 0.6708 0.3773 0.0722 0.025 Uiso 1 1 calc R . .
C9 C 0.47339(14) 0.38714(13) 0.08515(7) 0.0193(3) Uani 1 1 d . . .
H9 H 0.4818 0.4227 0.1302 0.023 Uiso 1 1 calc R . .

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
N7 0.0195(6) 0.0174(6) 0.0152(5) 0.0012(4) 0.0036(4) 0.0003(4)
N8 0.0220(6) 0.0237(6) 0.0179(6) 0.0057(5) 0.0029(5) 0.0028(5)
N6 0.0202(6) 0.0186(5) 0.0184(6) -0.0007(5) 0.0073(5) 0.0017(4)
N5 0.0168(5) 0.0184(5) 0.0164(6) -0.0017(4) 0.0041(4) 0.0007(4)
O4 0.0233(5) 0.0184(5) 0.0212(5) 0.0014(4) -0.0004(4) 0.0011(4)
O3 0.0247(5) 0.0395(6) 0.0255(6) -0.0127(5) 0.0084(4) 0.0003(5)
C12 0.0191(6) 0.0166(6) 0.0147(6) -0.0050(5) 0.0018(5) -0.0011(5)
C11 0.0187(6) 0.0202(7) 0.0159(6) -0.0002(5) 0.0014(5) -0.0020(5)
C10 0.0211(7) 0.0192(7) 0.0168(7) -0.0007(5) 0.0039(5) -0.0016(5)
C16 0.0210(7) 0.0264(7) 0.0237(7) 0.0025(6) 0.0036(6) 0.0028(6)
C17 0.0244(7) 0.0217(7) 0.0226(7) -0.0036(6) 0.0102(6) -0.0036(6)
C18 0.0245(7) 0.0189(7) 0.0157(6) -0.0006(5) 0.0068(5) -0.0029(5)
C13 0.0240(7) 0.0191(6) 0.0171(6) -0.0015(5) 0.0072(5) -0.0009(5)
C14 0.0196(7) 0.0214(7) 0.0178(7) -0.0013(5) 0.0014(5) -0.0028(5)
C15 0.0149(6) 0.0211(7) 0.0206(7) -0.0009(5) 0.0035(5) -0.0006(5)
N1 0.0152(5) 0.0184(5) 0.0195(6) 0.0003(4) 0.0050(4) 0.0000(4)
O1 0.0265(6) 0.0284(6) 0.0454(7) 0.0131(5) 0.0130(5) 0.0076(5)
O2 0.0301(6) 0.0233(5) 0.0205(5) -0.0025(4) 0.0119(4) -0.0046(4)
N2 0.0165(6) 0.0210(6) 0.0222(6) -0.0006(5) 0.0030(5) 0.0027(4)
N3 0.0214(6) 0.0175(5) 0.0126(5) -0.0014(4) 0.0044(4) -0.0020(4)
N4 0.0244(6) 0.0193(6) 0.0152(6) -0.0015(4) 0.0070(5) -0.0011(5)
C1 0.0211(7) 0.0195(7) 0.0204(7) 0.0005(5) 0.0052(5) -0.0015(5)
C2 0.0226(7) 0.0219(7) 0.0173(7) 0.0023(5) 0.0055(5) -0.0028(5)
C3 0.0230(7) 0.0129(6) 0.0182(7) 0.0014(5) 0.0073(5) -0.0014(5)
C4 0.0236(7) 0.0192(7) 0.0230(7) 0.0015(6) 0.0033(6) 0.0019(5)
C5 0.0253(7) 0.0208(7) 0.0213(7) 0.0003(6) 0.0071(6) -0.0035(6)
C6 0.0196(7) 0.0202(7) 0.0227(7) -0.0023(6) 0.0088(5) -0.0021(5)
C7 0.0237(7) 0.0188(7) 0.0214(7) 0.0010(5) 0.0083(6) 0.0001(5)
C8 0.0207(7) 0.0173(6) 0.0227(7) 0.0023(5) 0.0035(6) -0.0006(5)
C9 0.0234(7) 0.0179(6) 0.0149(6) 0.0001(5) 0.0015(5) -0.0025(5)

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
N7 C18 1.3718(17) . ?
N7 N8 1.3753(15) . ?
N7 C12 1.3980(17) . ?
N8 C16 1.3201(18) . ?
N6 C13 1.3207(17) . ?
N6 N5 1.3702(15) . ?
N5 C15 1.3711(16) . ?
N5 C10 1.4030(17) . ?
O4 C12 1.2102(16) . ?
O3 C10 1.2049(16) . ?
C12 C11 1.5030(18) . ?
C11 C10 1.5099(19) . ?
C16 C17 1.414(2) . ?
C17 C18 1.3510(19) . ?
C13 C14 1.4122(19) . ?
C14 C15 1.3528(18) . ?
N1 C6 1.3701(17) . ?
N1 N2 1.3703(15) . ?
N1 C1 1.4007(17) . ?
O1 C1 1.2068(17) . ?
O2 C3 1.2097(16) . ?
N2 C4 1.3178(18) . ?
N3 N4 1.3740(15) . ?
N3 C9 1.3749(17) . ?
N3 C3 1.3991(17) . ?
N4 C7 1.3198(18) . ?
C1 C2 1.5061(19) . ?
C2 C3 1.5059(19) . ?
C4 C5 1.414(2) . ?
C5 C6 1.360(2) . ?
C7 C8 1.411(2) . ?
C8 C9 1.3537(19) . ?

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
C18 N7 N8 111.65(11) . . ?
C18 N7 C12 126.92(11) . . ?
N8 N7 C12 121.43(11) . . ?
C16 N8 N7 103.82(11) . . ?
C13 N6 N5 103.72(11) . . ?
N6 N5 C15 111.95(11) . . ?
N6 N5 C10 120.87(11) . . ?
C15 N5 C10 127.18(11) . . ?
O4 C12 N7 119.80(12) . . ?
O4 C12 C11 124.73(12) . . ?
N7 C12 C11 115.47(11) . . ?
C12 C11 C10 111.30(11) . . ?
O3 C10 N5 119.93(12) . . ?
O3 C10 C11 124.77(13) . . ?
N5 C10 C11 115.29(11) . . ?
N8 C16 C17 112.41(13) . . ?
C18 C17 C16 105.20(12) . . ?
C17 C18 N7 106.92(12) . . ?
N6 C13 C14 112.47(12) . . ?
C15 C14 C13 105.15(12) . . ?
C14 C15 N5 106.70(12) . . ?
C6 N1 N2 111.99(11) . . ?
C6 N1 C1 126.92(12) . . ?
N2 N1 C1 121.04(11) . . ?
C4 N2 N1 103.76(11) . . ?
N4 N3 C9 111.84(11) . . ?
N4 N3 C3 121.95(11) . . ?
C9 N3 C3 126.20(11) . . ?
C7 N4 N3 103.72(11) . . ?
O1 C1 N1 119.76(13) . . ?
O1 C1 C2 125.00(13) . . ?
N1 C1 C2 115.24(12) . . ?
C3 C2 C1 109.45(11) . . ?
O2 C3 N3 120.26(12) . . ?
O2 C3 C2 123.63(13) . . ?
N3 C3 C2 116.09(11) . . ?
N2 C4 C5 112.76(12) . . ?
C6 C5 C4 104.74(12) . . ?
C5 C6 N1 106.74(12) . . ?
N4 C7 C8 112.56(12) . . ?
C9 C8 C7 105.33(13) . . ?
C8 C9 N3 106.56(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -67.86(15) . . . . ?
C1 C2 C3 N3 160.23(11) . . . . ?
O1 C1 C3 O2 66.26(16) . . . . ?
N5 C10 C11 C12 68.74(14) . . . . ?
C10 C11 C12 N7 -167.55(11) . . . . ?
O4 C12 C10 O3 -74.68(16) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        30.05
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.053

# Attachment 'comp2c.cif'

data_panleg
_database_code_depnum_ccdc_archive 'CCDC 746841'
#TrackingRef 'comp2c.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H12 N4 O2'
_chemical_formula_weight         304.31

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           ?
_symmetry_space_group_name_H-M   ?

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

_cell_length_a                   7.6935(4)
_cell_length_b                   14.8559(8)
_cell_length_c                   12.8855(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.972(2)
_cell_angle_gamma                90.00
_cell_volume                     1415.88(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             632
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18297
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         30.02
_reflns_number_total             4133
_reflns_number_gt                2652
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(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^)+(0.0611P)^2^+0.1003P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4133
_refine_ls_number_parameters     208
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0448
_refine_ls_wR_factor_ref         0.1265
_refine_ls_wR_factor_gt          0.1126
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.12470(15) 0.02779(7) 0.40129(9) 0.0414(3) Uani 1 1 d . . .
N2 N 0.12664(17) -0.06532(8) 0.38973(10) 0.0499(3) Uani 1 1 d . . .
N3 N 0.02494(13) 0.10233(8) 0.07403(9) 0.0418(3) Uani 1 1 d . . .
N4 N 0.19757(14) 0.07360(9) 0.12923(10) 0.0506(3) Uani 1 1 d . . .
O1 O 0.03507(14) 0.16186(7) 0.32165(8) 0.0545(3) Uani 1 1 d . . .
O2 O -0.26651(13) 0.11567(8) 0.07295(9) 0.0622(3) Uani 1 1 d . . .
C1 C 0.03134(17) 0.08052(9) 0.31525(11) 0.0413(3) Uani 1 1 d . . .
C2 C -0.07530(19) 0.02956(10) 0.21750(11) 0.0472(3) Uani 1 1 d . . .
H2A H -0.0066 -0.0227 0.2069 0.057 Uiso 1 1 calc R . .
H2B H -0.1871 0.0084 0.2300 0.057 Uiso 1 1 calc R . .
C3 C -0.11857(18) 0.08632(10) 0.11714(11) 0.0434(3) Uani 1 1 d . . .
C4 C 0.2405(2) -0.09464(9) 0.47761(12) 0.0515(4) Uani 1 1 d . . .
H4 H 0.2680 -0.1552 0.4912 0.062 Uiso 1 1 calc R . .
C5 C 0.31869(19) -0.02417(9) 0.55094(11) 0.0441(3) Uani 1 1 d . . .
C6 C 0.4476(2) -0.01971(11) 0.65056(12) 0.0520(4) Uani 1 1 d . . .
H6 H 0.5023 -0.0717 0.6847 0.062 Uiso 1 1 calc R . .
C7 C 0.4919(2) 0.06284(12) 0.69697(12) 0.0565(4) Uani 1 1 d . . .
H7 H 0.5790 0.0672 0.7631 0.068 Uiso 1 1 calc R . .
C8 C 0.4084(2) 0.14061(11) 0.64665(12) 0.0542(4) Uani 1 1 d . . .
H8 H 0.4397 0.1957 0.6809 0.065 Uiso 1 1 calc R . .
C9 C 0.2810(2) 0.13853(9) 0.54779(11) 0.0471(3) Uani 1 1 d . . .
H9 H 0.2255 0.1907 0.5147 0.057 Uiso 1 1 calc R . .
C10 C 0.23973(16) 0.05443(9) 0.50013(10) 0.0390(3) Uani 1 1 d . . .
C11 C 0.30177(19) 0.10007(11) 0.07073(12) 0.0529(4) Uani 1 1 d . . .
H11 H 0.4257 0.0896 0.0891 0.064 Uiso 1 1 calc R . .
C12 C 0.20574(18) 0.14686(9) -0.02454(11) 0.0446(3) Uani 1 1 d . . .
C13 C 0.2521(2) 0.18680(10) -0.11137(13) 0.0562(4) Uani 1 1 d . . .
H13 H 0.3713 0.1875 -0.1146 0.067 Uiso 1 1 calc R . .
C14 C 0.1179(3) 0.22469(11) -0.19107(13) 0.0633(5) Uani 1 1 d . . .
H14 H 0.1463 0.2514 -0.2496 0.076 Uiso 1 1 calc R . .
C15 C -0.0609(2) 0.22418(10) -0.18668(12) 0.0585(4) Uani 1 1 d . . .
H15 H -0.1491 0.2508 -0.2424 0.070 Uiso 1 1 calc R . .
C16 C -0.1109(2) 0.18540(9) -0.10217(11) 0.0481(3) Uani 1 1 d . . .
H16 H -0.2306 0.1848 -0.0997 0.058 Uiso 1 1 calc R . .
C17 C 0.02610(17) 0.14734(8) -0.02099(10) 0.0397(3) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0477(6) 0.0358(6) 0.0435(6) -0.0009(5) 0.0169(5) -0.0004(5)
N2 0.0648(8) 0.0357(6) 0.0531(7) -0.0016(5) 0.0225(6) -0.0041(5)
N3 0.0331(5) 0.0519(7) 0.0412(6) 0.0001(5) 0.0114(5) 0.0015(5)
N4 0.0356(6) 0.0655(8) 0.0493(7) 0.0015(6) 0.0092(5) 0.0054(5)
O1 0.0662(7) 0.0410(6) 0.0535(6) -0.0003(4) 0.0118(5) 0.0053(5)
O2 0.0374(6) 0.0863(8) 0.0653(7) 0.0116(6) 0.0180(5) 0.0066(5)
C1 0.0405(7) 0.0431(7) 0.0452(7) -0.0014(6) 0.0199(6) -0.0003(6)
C2 0.0469(7) 0.0501(8) 0.0469(8) -0.0021(6) 0.0168(6) -0.0092(6)
C3 0.0382(7) 0.0490(8) 0.0446(7) -0.0063(6) 0.0142(6) -0.0044(6)
C4 0.0679(10) 0.0362(7) 0.0544(9) 0.0061(6) 0.0237(7) 0.0029(7)
C5 0.0494(8) 0.0436(7) 0.0456(7) 0.0051(6) 0.0238(6) 0.0017(6)
C6 0.0546(8) 0.0566(9) 0.0478(8) 0.0117(7) 0.0193(7) 0.0063(7)
C7 0.0560(9) 0.0675(11) 0.0451(8) 0.0018(7) 0.0123(7) -0.0044(7)
C8 0.0614(9) 0.0526(9) 0.0503(8) -0.0074(7) 0.0182(7) -0.0102(7)
C9 0.0549(8) 0.0415(7) 0.0480(8) -0.0005(6) 0.0192(7) 0.0004(6)
C10 0.0404(7) 0.0420(7) 0.0395(7) 0.0000(5) 0.0189(5) -0.0010(5)
C11 0.0344(7) 0.0679(10) 0.0572(9) -0.0074(7) 0.0137(6) 0.0006(7)
C12 0.0434(7) 0.0439(7) 0.0502(8) -0.0114(6) 0.0193(6) -0.0065(6)
C13 0.0635(10) 0.0532(9) 0.0625(10) -0.0116(7) 0.0349(8) -0.0130(7)
C14 0.0932(13) 0.0512(9) 0.0562(10) -0.0025(7) 0.0383(10) -0.0090(9)
C15 0.0785(11) 0.0507(9) 0.0461(8) 0.0020(7) 0.0170(8) 0.0051(8)
C16 0.0495(8) 0.0491(8) 0.0450(7) -0.0040(6) 0.0117(6) 0.0037(6)
C17 0.0429(7) 0.0385(7) 0.0396(7) -0.0063(5) 0.0145(6) -0.0024(5)

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 1.3858(17) . ?
N1 N2 1.3917(15) . ?
N1 C10 1.3934(17) . ?
N2 C4 1.3012(19) . ?
N3 C3 1.3862(16) . ?
N3 N4 1.3900(15) . ?
N3 C17 1.3974(16) . ?
N4 C11 1.3032(18) . ?
O1 C1 1.2110(16) . ?
O2 C3 1.2055(16) . ?
C1 C2 1.5047(19) . ?
C2 C3 1.502(2) . ?
C4 C5 1.428(2) . ?
C5 C6 1.391(2) . ?
C5 C10 1.3937(18) . ?
C6 C7 1.366(2) . ?
C7 C8 1.392(2) . ?
C8 C9 1.377(2) . ?
C9 C10 1.3897(19) . ?
C11 C12 1.427(2) . ?
C12 C17 1.3953(18) . ?
C12 C13 1.397(2) . ?
C13 C14 1.361(2) . ?
C14 C15 1.393(2) . ?
C15 C16 1.377(2) . ?
C16 C17 1.3850(19) . ?

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
C1 N1 N2 119.65(11) . . ?
C1 N1 C10 129.02(11) . . ?
N2 N1 C10 110.94(10) . . ?
C4 N2 N1 105.31(11) . . ?
C3 N3 N4 119.77(11) . . ?
C3 N3 C17 129.13(11) . . ?
N4 N3 C17 111.08(10) . . ?
C11 N4 N3 105.34(12) . . ?
O1 C1 N1 120.81(12) . . ?
O1 C1 C2 123.80(13) . . ?
N1 C1 C2 115.37(12) . . ?
C3 C2 C1 112.26(12) . . ?
O2 C3 N3 120.09(13) . . ?
O2 C3 C2 124.49(12) . . ?
N3 C3 C2 115.40(12) . . ?
N2 C4 C5 113.00(13) . . ?
C6 C5 C10 120.10(13) . . ?
C6 C5 C4 135.18(14) . . ?
C10 C5 C4 104.69(13) . . ?
C7 C6 C5 118.39(14) . . ?
C6 C7 C8 120.91(14) . . ?
C9 C8 C7 122.12(14) . . ?
C8 C9 C10 116.54(13) . . ?
C9 C10 N1 132.05(12) . . ?
C9 C10 C5 121.90(13) . . ?
N1 C10 C5 106.05(11) . . ?
N4 C11 C12 112.91(12) . . ?
C17 C12 C13 119.83(14) . . ?
C17 C12 C11 104.91(12) . . ?
C13 C12 C11 135.25(14) . . ?
C14 C13 C12 118.19(14) . . ?
C13 C14 C15 121.30(15) . . ?
C16 C15 C14 121.90(15) . . ?
C15 C16 C17 116.61(14) . . ?
C16 C17 C12 122.16(13) . . ?
C16 C17 N3 132.08(12) . . ?
C12 C17 N3 105.75(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -160.21(11) . . . . ?
C1 C2 C3 N3 74.44(15) . . . . ?
O1 C1 C3 O2 -64.23(15) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        30.02
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.168
_refine_diff_density_min         -0.179
_refine_diff_density_rms         0.037

# Attachment 'comp3.cif'

data_comp(3)
_database_code_depnum_ccdc_archive 'CCDC 746842'
#TrackingRef 'comp3.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H26 Cu N8 O8'
_chemical_formula_weight         570.03

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   10.3247(4)
_cell_length_b                   15.4035(7)
_cell_length_c                   8.3413(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.0560(10)
_cell_angle_gamma                90.00
_cell_volume                     1313.48(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            0.30
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             590
_exptl_absorpt_coefficient_mu    0.890
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.868
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART Apex II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16930
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         30.06
_reflns_number_total             3853
_reflns_number_gt                2640
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       SMART
_computing_cell_refinement       SMART
_computing_data_reduction        SAINT+
_computing_structure_solution    'SIR-97 (Giacovazzo, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SCHAKAL99 (Keller 1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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^ > 2\s(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^)+(0.1015P)^2^+0.0647P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3853
_refine_ls_number_parameters     169
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0534
_refine_ls_wR_factor_ref         0.1711
_refine_ls_wR_factor_gt          0.1567
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.094
_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
Cu1 Cu 0.5000 0.0000 0.5000 0.03870(17) Uani 1 2 d S . .
O1 O 0.64574(18) 0.11865(15) 0.5151(3) 0.0567(6) Uani 1 1 d . . .
N1 N 0.4432(2) 0.03772(17) 0.2711(3) 0.0442(5) Uani 1 1 d . . .
N4 N 0.2375(2) 0.06635(16) 0.5579(3) 0.0506(6) Uani 1 1 d D . .
H4N H 0.2007 0.0192 0.5198 0.061 Uiso 1 1 calc RD . .
N3 N 0.3666(2) 0.08188(15) 0.5721(3) 0.0435(5) Uani 1 1 d . . .
N2 N 0.5033(2) 0.10216(17) 0.2060(3) 0.0521(6) Uani 1 1 d D . .
H2N H 0.5692 0.1301 0.2552 0.063 Uiso 1 1 calc RD . .
O2 O 0.8575(2) 0.08828(16) 0.5872(4) 0.0756(8) Uani 1 1 d . . .
C1 C 0.7606(3) 0.1370(2) 0.5710(4) 0.0524(7) Uani 1 1 d . . .
C8 C 0.3826(3) 0.15988(19) 0.6342(4) 0.0530(7) Uani 1 1 d . . .
H8 H 0.4630 0.1878 0.6571 0.064 Uiso 1 1 calc R . .
C10 C 0.1738(3) 0.1336(2) 0.6105(4) 0.0583(8) Uani 1 1 d . . .
H10 H 0.0841 0.1375 0.6121 0.070 Uiso 1 1 calc R . .
C9 C 0.2642(3) 0.1955(2) 0.6614(4) 0.0624(8) Uani 1 1 d . . .
H9 H 0.2499 0.2497 0.7048 0.075 Uiso 1 1 calc R . .
C5 C 0.4481(4) 0.1182(2) 0.0535(4) 0.0633(9) Uani 1 1 d . . .
H5 H 0.4735 0.1608 -0.0146 0.076 Uiso 1 1 calc R . .
C6 C 0.3500(4) 0.0616(2) 0.0172(4) 0.0660(9) Uani 1 1 d . . .
H6 H 0.2948 0.0561 -0.0804 0.079 Uiso 1 1 calc R . .
C7 C 0.3485(4) 0.0128(2) 0.1572(5) 0.0627(9) Uani 1 1 d . . .
H7 H 0.2890 -0.0313 0.1690 0.075 Uiso 1 1 calc R . .
C2 C 0.7820(3) 0.2283(2) 0.6363(5) 0.0703(10) Uani 1 1 d . . .
O3 O 0.7040(3) 0.2649(2) 0.7051(6) 0.1367(17) Uani 1 1 d . . .
O4 O 0.8901(3) 0.26240(19) 0.6088(5) 0.1143(13) Uani 1 1 d D . .
C3 C 0.9176(8) 0.3476(4) 0.6858(11) 0.186(4) Uani 1 1 d D . .
H3A H 0.8366 0.3791 0.6882 0.223 Uiso 1 1 calc R . .
H3B H 0.9599 0.3401 0.7963 0.223 Uiso 1 1 calc R . .
C4 C 0.9973(8) 0.3929(5) 0.5991(13) 0.227(5) Uani 1 1 d D . .
H4A H 1.0162 0.4487 0.6482 0.341 Uiso 1 1 calc R . .
H4B H 0.9546 0.4005 0.4902 0.341 Uiso 1 1 calc R . .
H4C H 1.0774 0.3614 0.5977 0.341 Uiso 1 1 calc R . .

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
Cu1 0.0307(2) 0.0453(3) 0.0407(3) 0.00233(18) 0.00730(16) 0.00511(17)
O1 0.0382(10) 0.0610(13) 0.0704(14) -0.0018(10) 0.0053(9) -0.0098(9)
N1 0.0402(11) 0.0504(13) 0.0420(12) 0.0048(10) 0.0059(9) 0.0043(10)
N4 0.0331(11) 0.0530(14) 0.0655(16) -0.0055(11) 0.0066(10) 0.0010(9)
N3 0.0333(10) 0.0486(12) 0.0496(13) 0.0010(10) 0.0095(9) 0.0036(9)
N2 0.0558(14) 0.0485(13) 0.0520(14) 0.0046(10) 0.0068(11) -0.0018(11)
O2 0.0400(11) 0.0593(14) 0.126(2) -0.0209(14) 0.0073(12) 0.0019(10)
C1 0.0392(14) 0.0539(17) 0.0656(19) -0.0066(14) 0.0125(13) -0.0049(12)
C8 0.0444(15) 0.0462(15) 0.0686(19) 0.0000(14) 0.0082(13) 0.0043(12)
C10 0.0397(14) 0.0636(19) 0.073(2) 0.0009(15) 0.0138(14) 0.0166(13)
C9 0.0521(17) 0.0535(18) 0.083(2) -0.0045(16) 0.0156(16) 0.0148(14)
C5 0.080(2) 0.0581(19) 0.0525(18) 0.0126(14) 0.0129(17) 0.0111(17)
C6 0.076(2) 0.073(2) 0.0459(17) 0.0025(15) -0.0030(15) 0.0072(18)
C7 0.0554(19) 0.073(2) 0.0565(19) 0.0059(15) -0.0041(15) -0.0110(15)
C2 0.0455(16) 0.059(2) 0.105(3) -0.0251(19) 0.0063(17) 0.0008(14)
O3 0.080(2) 0.117(3) 0.217(5) -0.092(3) 0.035(3) 0.006(2)
O4 0.087(2) 0.0701(18) 0.193(4) -0.041(2) 0.045(2) -0.0381(16)
C3 0.181(7) 0.100(4) 0.295(11) -0.089(6) 0.100(7) -0.078(5)
C4 0.163(8) 0.076(4) 0.442(17) -0.011(8) 0.038(8) -0.023(4)

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
Cu1 N1 2.003(2) 3_656 ?
Cu1 N1 2.003(2) . ?
Cu1 N3 2.021(2) 3_656 ?
Cu1 N3 2.021(2) . ?
Cu1 O1 2.359(2) . ?
Cu1 O1 2.359(2) 3_656 ?
O1 C1 1.244(3) . ?
N1 C7 1.322(4) . ?
N1 N2 1.327(3) . ?
N4 C10 1.334(4) . ?
N4 N3 1.343(3) . ?
N3 C8 1.310(4) . ?
N2 C5 1.341(4) . ?
O2 C1 1.243(4) . ?
C1 C2 1.513(5) . ?
C8 C9 1.387(4) . ?
C10 C9 1.360(5) . ?
C5 C6 1.339(5) . ?
C6 C7 1.391(5) . ?
C2 O3 1.194(4) . ?
C2 O4 1.283(4) . ?
O4 C3 1.471(6) . ?
C3 C4 1.362(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
N1 Cu1 N1 180.0 3_656 . ?
N1 Cu1 N3 88.96(9) 3_656 3_656 ?
N1 Cu1 N3 91.04(9) . 3_656 ?
N1 Cu1 N3 91.04(9) 3_656 . ?
N1 Cu1 N3 88.96(9) . . ?
N3 Cu1 N3 180.00(12) 3_656 . ?
N1 Cu1 O1 94.27(9) 3_656 . ?
N1 Cu1 O1 85.73(9) . . ?
N3 Cu1 O1 92.46(8) 3_656 . ?
N3 Cu1 O1 87.54(8) . . ?
N1 Cu1 O1 85.73(9) 3_656 3_656 ?
N1 Cu1 O1 94.27(9) . 3_656 ?
N3 Cu1 O1 87.54(8) 3_656 3_656 ?
N3 Cu1 O1 92.46(8) . 3_656 ?
O1 Cu1 O1 180.00(13) . 3_656 ?
C1 O1 Cu1 139.7(2) . . ?
C7 N1 N2 105.3(3) . . ?
C7 N1 Cu1 133.6(2) . . ?
N2 N1 Cu1 121.08(19) . . ?
C10 N4 N3 111.2(3) . . ?
C8 N3 N4 105.5(2) . . ?
C8 N3 Cu1 129.52(19) . . ?
N4 N3 Cu1 124.89(19) . . ?
N1 N2 C5 111.4(3) . . ?
O2 C1 O1 127.9(3) . . ?
O2 C1 C2 116.5(3) . . ?
O1 C1 C2 115.4(3) . . ?
N3 C8 C9 111.2(3) . . ?
N4 C10 C9 107.3(3) . . ?
C10 C9 C8 104.8(3) . . ?
C6 C5 N2 107.6(3) . . ?
C5 C6 C7 105.0(3) . . ?
N1 C7 C6 110.6(3) . . ?
O3 C2 O4 123.8(3) . . ?
O3 C2 C1 122.5(3) . . ?
O4 C2 C1 113.8(3) . . ?
C2 O4 C3 114.0(4) . . ?
C4 C3 O4 108.6(6) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        30.06
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.091
#===END

# Attachment 'comp6.cif'

data_comp(6)
_database_code_depnum_ccdc_archive 'CCDC 746843'
#TrackingRef 'comp6.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H26 Cu N4 O5'
_chemical_formula_weight         405.94

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbcn

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

_cell_length_a                   15.6709(13)
_cell_length_b                   10.8951(9)
_cell_length_c                   11.3147(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1931.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            light-blue
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             852
_exptl_absorpt_coefficient_mu    1.162
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.856
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART Apex II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23562
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.28
_diffrn_reflns_theta_max         30.11
_reflns_number_total             2838
_reflns_number_gt                1964
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       SMART
_computing_cell_refinement       SMART
_computing_data_reduction        SAINT+
_computing_structure_solution    'SIR-97 (Giacovazzo, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SCHAKAL99 (Keller 1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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^ > 2\s(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^)+(0.0487P)^2^+0.8875P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2838
_refine_ls_number_parameters     126
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0315
_refine_ls_wR_factor_ref         0.1001
_refine_ls_wR_factor_gt          0.0849
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.003
_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
Cu Cu 0.0000 0.58099(3) 0.2500 0.02752(10) Uani 1 2 d S . .
O1 O -0.08045(9) 0.71302(13) 0.30246(12) 0.0368(3) Uani 1 1 d . . .
O2 O -0.01039(10) 0.65054(17) 0.45799(14) 0.0513(4) Uani 1 1 d . . .
N1 N 0.09104(10) 0.45472(15) 0.23564(13) 0.0308(3) Uani 1 1 d . . .
N2 N 0.08688(10) 0.35952(15) 0.15813(14) 0.0348(4) Uani 1 1 d D . .
H2N H 0.0453(12) 0.358(2) 0.1060(18) 0.042 Uiso 1 1 d D . .
C3 C 0.16636(12) 0.44395(18) 0.29029(18) 0.0344(4) Uani 1 1 d . . .
C1 C 0.15823(13) 0.29154(18) 0.16118(18) 0.0396(4) Uani 1 1 d . . .
C6 C -0.06338(12) 0.72037(18) 0.41168(17) 0.0349(4) Uani 1 1 d . . .
C5 C 0.19227(15) 0.5319(2) 0.3846(2) 0.0517(6) Uani 1 1 d . . .
H5A H 0.1705 0.5043 0.4593 0.078 Uiso 1 1 calc R . .
H5B H 0.1696 0.6117 0.3671 0.078 Uiso 1 1 calc R . .
H5C H 0.2534 0.5362 0.3881 0.078 Uiso 1 1 calc R . .
C4 C 0.17004(19) 0.1825(2) 0.0823(3) 0.0633(7) Uani 1 1 d . . .
H4A H 0.1182 0.1671 0.0397 0.095 Uiso 1 1 calc R . .
H4B H 0.1842 0.1120 0.1292 0.095 Uiso 1 1 calc R . .
H4C H 0.2154 0.1985 0.0273 0.095 Uiso 1 1 calc R . .
C7 C -0.10816(17) 0.8168(2) 0.4837(2) 0.0561(6) Uani 1 1 d . . .
H7A H -0.0685 0.8805 0.5042 0.084 Uiso 1 1 calc R . .
H7B H -0.1305 0.7804 0.5545 0.084 Uiso 1 1 calc R . .
H7C H -0.1541 0.8512 0.4384 0.084 Uiso 1 1 calc R . .
C2 C 0.21023(13) 0.3427(2) 0.24548(19) 0.0417(5) Uani 1 1 d . . .
H2 H 0.2640 0.3152 0.2682 0.050 Uiso 1 1 calc R . .
O5 O -0.0612(4) 0.9546(4) 0.1956(5) 0.112(2) Uani 0.564(8) 1 d P A -1
H10 H -0.0580 0.8804 0.2068 0.168 Uiso 0.564(8) 1 calc PR A -1
C8 C 0.0000 1.0088(6) 0.2500 0.0959(18) Uani 1 2 d S . .

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
Cu 0.02702(16) 0.02679(16) 0.02874(16) 0.000 -0.00378(12) 0.000
O1 0.0407(7) 0.0346(7) 0.0349(7) -0.0012(6) -0.0047(6) 0.0087(6)
O2 0.0556(10) 0.0601(10) 0.0384(8) 0.0011(7) -0.0107(7) 0.0158(8)
N1 0.0304(8) 0.0304(7) 0.0315(8) -0.0033(6) -0.0032(6) 0.0011(6)
N2 0.0340(8) 0.0359(8) 0.0343(8) -0.0058(7) -0.0022(7) -0.0006(7)
C3 0.0315(9) 0.0376(10) 0.0341(9) 0.0016(8) -0.0046(8) 0.0005(8)
C1 0.0431(11) 0.0360(10) 0.0398(10) -0.0012(8) 0.0087(9) 0.0056(9)
C6 0.0361(10) 0.0340(10) 0.0346(9) -0.0006(8) 0.0026(8) -0.0001(8)
C5 0.0474(12) 0.0535(13) 0.0542(13) -0.0092(11) -0.0215(10) 0.0030(11)
C4 0.0727(17) 0.0499(14) 0.0672(17) -0.0184(12) 0.0135(14) 0.0085(13)
C7 0.0637(16) 0.0564(14) 0.0481(13) -0.0110(11) 0.0108(11) 0.0113(12)
C2 0.0338(10) 0.0452(11) 0.0460(11) 0.0035(10) -0.0007(9) 0.0092(8)
O5 0.142(5) 0.071(3) 0.123(5) 0.038(3) -0.008(4) 0.013(3)
C8 0.095(4) 0.066(3) 0.127(5) 0.000 0.006(4) 0.000

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
Cu N1 1.9886(16) 3 ?
Cu N1 1.9886(16) . ?
Cu O1 2.0027(13) . ?
Cu O1 2.0027(14) 3 ?
O1 C6 1.267(2) . ?
O2 C6 1.242(2) . ?
N1 C3 1.338(2) . ?
N1 N2 1.360(2) . ?
N2 C1 1.342(3) . ?
C3 C2 1.396(3) . ?
C3 C5 1.490(3) . ?
C1 C2 1.373(3) . ?
C1 C4 1.498(3) . ?
C6 C7 1.504(3) . ?
O5 C8 1.284(6) . ?
C8 O5 1.284(6) 3 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu N1 92.45(9) 3 . ?
N1 Cu O1 91.21(6) 3 . ?
N1 Cu O1 166.59(6) . . ?
N1 Cu O1 166.59(6) 3 3 ?
N1 Cu O1 91.21(6) . 3 ?
O1 Cu O1 88.18(8) . 3 ?
C6 O1 Cu 101.63(12) . . ?
C3 N1 N2 105.88(16) . . ?
C3 N1 Cu 130.99(14) . . ?
N2 N1 Cu 123.09(12) . . ?
C1 N2 N1 111.38(16) . . ?
N1 C3 C2 109.64(18) . . ?
N1 C3 C5 121.00(18) . . ?
C2 C3 C5 129.35(19) . . ?
N2 C1 C2 106.77(17) . . ?
N2 C1 C4 121.7(2) . . ?
C2 C1 C4 131.5(2) . . ?
O2 C6 O1 120.93(19) . . ?
O2 C6 C7 120.76(19) . . ?
O1 C6 C7 118.31(19) . . ?
C1 C2 C3 106.31(18) . . ?
O5 C8 O5 125.2(6) . 3 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        30.11
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.059
#===END