# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2013


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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
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#  fide research purposes only. It may contain copyright material 
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data_1
_database_code_depnum_ccdc_archive 'CCDC 883737'
#TrackingRef 'Compound 1.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H28 Co3 N20 O4'
_chemical_formula_sum            'C28 H28 Co3 N20 O4'
_chemical_formula_weight         885.49

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'
Co Co 0.3494 0.9721 '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           monoclinic
_symmetry_space_group_name_H-M   P21/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                   6.7098(13)
_cell_length_b                   21.342(4)
_cell_length_c                   13.358(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.86(3)
_cell_angle_gamma                90.00
_cell_volume                     1830.7(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      3.17
_cell_measurement_theta_max      27.43

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             898
_exptl_absorpt_coefficient_mu    1.408
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   Process-auto

_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  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-sca
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17739
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.17
_diffrn_reflns_theta_max         27.43
_reflns_number_total             4167
_reflns_number_gt                3626
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97

_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^)+(0.0328P)^2^+1.7280P] 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         4167
_refine_ls_number_parameters     266
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_ref         0.0785
_refine_ls_wR_factor_gt          0.0755
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.002
_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
Co2 Co 1.0000 0.5000 0.0000 0.01603(10) Uani 1 2 d S . .
Co1 Co 0.52880(4) 0.566927(12) 0.046824(19) 0.01477(8) Uani 1 1 d . . .
N10 N 0.6712(3) 0.65733(9) 0.01465(14) 0.0268(4) Uani 1 1 d . . .
H10A H 0.7666 0.6474 -0.0182 0.032 Uiso 1 1 calc R . .
H10B H 0.5700 0.6789 -0.0315 0.032 Uiso 1 1 calc R . .
C12 C 0.7692(4) 0.69971(10) 0.09738(18) 0.0268(5) Uani 1 1 d . . .
C11 C 0.6448(4) 0.73690(13) 0.1398(2) 0.0431(7) Uani 1 1 d . . .
H11 H 0.5006 0.7340 0.1145 0.052 Uiso 1 1 calc R . .
C10 C 0.7351(4) 0.77826(13) 0.2197(2) 0.0450(7) Uani 1 1 d . . .
H10 H 0.6505 0.8024 0.2487 0.054 Uiso 1 1 calc R . .
O2 O 0.4457(3) 0.60890(9) 0.17559(14) 0.0343(4) Uani 1 1 d . . .
O1 O 0.6629(2) 0.51211(6) -0.04999(10) 0.0190(3) Uani 1 1 d . . .
N3 N 0.9893(3) 0.53776(9) 0.14670(13) 0.0238(4) Uani 1 1 d . . .
N2 N 0.8112(3) 0.54929(9) 0.16572(14) 0.0245(4) Uani 1 1 d . . .
N1 N 0.8451(3) 0.56466(10) 0.26658(14) 0.0305(4) Uani 1 1 d . . .
N4 N 1.1449(3) 0.54450(10) 0.23506(14) 0.0286(4) Uani 1 1 d . . .
N8 N 1.2525(3) 0.89336(8) 0.44103(14) 0.0242(4) Uani 1 1 d . . .
N7 N 1.0637(3) 0.91297(8) 0.43324(14) 0.0227(4) Uani 1 1 d . . .
N6 N 0.9246(3) 0.87617(9) 0.36649(15) 0.0282(4) Uani 1 1 d . . .
N9 N 1.2429(3) 0.84249(9) 0.37989(16) 0.0307(4) Uani 1 1 d . . .
C8 C 1.0404(3) 0.83319(10) 0.33538(17) 0.0255(4) Uani 1 1 d . . .
N5 N 1.4745(4) 0.58206(12) 0.73983(16) 0.0388(5) Uani 1 1 d . . .
C1 C 1.0518(4) 0.56135(11) 0.30743(17) 0.0280(5) Uani 1 1 d . . .
C13 C 0.9837(4) 0.70333(12) 0.1375(2) 0.0364(6) Uani 1 1 d . . .
H13 H 1.0681 0.6774 0.1112 0.044 Uiso 1 1 calc R . .
C9 C 0.9497(4) 0.78438(11) 0.25733(19) 0.0303(5) Uani 1 1 d . . .
C14 C 1.0730(4) 0.74557(12) 0.2168(2) 0.0374(6) Uani 1 1 d . . .
H14 H 1.2172 0.7479 0.2431 0.045 Uiso 1 1 calc R . .
C2 C 1.1620(4) 0.57199(12) 0.41853(17) 0.0328(5) Uani 1 1 d . . .
C5 C 1.3707(4) 0.58171(12) 0.63262(18) 0.0345(5) Uani 1 1 d . . .
C7 C 1.3771(4) 0.57218(17) 0.4538(2) 0.0508(8) Uani 1 1 d . . .
H7 H 1.4536 0.5688 0.4060 0.061 Uiso 1 1 calc R . .
C6 C 1.4800(4) 0.57744(18) 0.5598(2) 0.0533(9) Uani 1 1 d . . .
H6 H 1.6248 0.5781 0.5821 0.064 Uiso 1 1 calc R . .
C4 C 1.1551(4) 0.58283(16) 0.59708(19) 0.0467(7) Uani 1 1 d . . .
H4 H 1.0788 0.5869 0.6448 0.056 Uiso 1 1 calc R . .
C3 C 1.0524(4) 0.57796(16) 0.49161(19) 0.0462(7) Uani 1 1 d . . .
H3 H 0.9076 0.5787 0.4692 0.055 Uiso 1 1 calc R . .
H2A H 0.562(6) 0.6050(18) 0.228(3) 0.076(12) Uiso 1 1 d . . .
H2B H 0.347(6) 0.5816(18) 0.198(3) 0.073(11) Uiso 1 1 d . . .
H5B H 1.412(5) 0.6067(15) 0.777(2) 0.047(9) Uiso 1 1 d . . .
H5A H 1.616(6) 0.5930(17) 0.758(3) 0.065(11) Uiso 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
Co2 0.01583(19) 0.01701(18) 0.01482(18) 0.00042(14) 0.00378(14) -0.00029(14)
Co1 0.01258(13) 0.01526(13) 0.01479(13) -0.00185(9) 0.00133(9) -0.00020(9)
N10 0.0240(10) 0.0249(9) 0.0300(10) -0.0067(8) 0.0056(8) -0.0042(7)
C12 0.0256(11) 0.0204(10) 0.0326(11) -0.0079(9) 0.0056(9) -0.0044(9)
C11 0.0217(12) 0.0393(14) 0.0644(18) -0.0252(13) 0.0063(12) -0.0042(10)
C10 0.0264(13) 0.0434(15) 0.0660(19) -0.0322(14) 0.0147(12) -0.0043(11)
O2 0.0281(9) 0.0419(10) 0.0340(9) -0.0098(8) 0.0107(8) -0.0044(8)
O1 0.0188(7) 0.0195(7) 0.0170(6) -0.0004(5) 0.0029(5) 0.0005(5)
N3 0.0195(9) 0.0307(10) 0.0195(8) -0.0017(7) 0.0029(7) 0.0003(7)
N2 0.0206(9) 0.0323(10) 0.0192(8) -0.0049(7) 0.0035(7) 0.0002(7)
N1 0.0232(10) 0.0486(12) 0.0177(8) -0.0049(8) 0.0031(7) 0.0000(9)
N4 0.0217(9) 0.0422(11) 0.0188(8) -0.0043(8) 0.0008(7) -0.0010(8)
N8 0.0217(9) 0.0218(9) 0.0269(9) -0.0052(7) 0.0037(7) 0.0019(7)
N7 0.0184(9) 0.0240(9) 0.0244(9) -0.0047(7) 0.0042(7) -0.0015(7)
N6 0.0224(10) 0.0290(10) 0.0314(10) -0.0110(8) 0.0052(8) -0.0045(8)
N9 0.0242(10) 0.0279(10) 0.0372(11) -0.0138(8) 0.0045(8) -0.0009(8)
C8 0.0247(11) 0.0234(10) 0.0278(11) -0.0053(9) 0.0068(9) -0.0025(8)
N5 0.0368(13) 0.0529(14) 0.0223(10) -0.0033(10) 0.0015(9) -0.0041(11)
C1 0.0248(11) 0.0370(12) 0.0207(10) -0.0024(9) 0.0041(9) -0.0017(9)
C13 0.0259(12) 0.0374(13) 0.0456(14) -0.0205(11) 0.0096(11) -0.0014(10)
C9 0.0265(12) 0.0262(11) 0.0370(12) -0.0117(10) 0.0074(10) -0.0037(9)
C14 0.0198(12) 0.0394(14) 0.0483(14) -0.0199(12) 0.0027(10) -0.0020(10)
C2 0.0278(12) 0.0480(15) 0.0190(10) -0.0034(10) 0.0014(9) -0.0020(10)
C5 0.0335(13) 0.0431(14) 0.0224(11) -0.0024(10) 0.0011(9) -0.0038(11)
C7 0.0293(14) 0.098(3) 0.0237(12) -0.0064(14) 0.0058(10) -0.0051(15)
C6 0.0257(13) 0.103(3) 0.0269(13) -0.0070(14) 0.0000(10) -0.0041(15)
C4 0.0349(14) 0.081(2) 0.0235(12) -0.0099(13) 0.0075(10) -0.0013(14)
C3 0.0260(13) 0.084(2) 0.0248(12) -0.0096(13) 0.0023(10) 0.0011(13)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co2 N3 2.1392(18) . ?
Co2 N3 2.1392(18) 3_765 ?
Co2 N7 2.1562(18) 2_745 ?
Co2 N7 2.1562(18) 4_575 ?
Co2 O1 2.1799(15) 3_765 ?
Co2 O1 2.1799(15) . ?
Co1 N2 2.124(2) . ?
Co1 O1 2.1274(15) . ?
Co1 O1 2.1293(14) 3_665 ?
Co1 O2 2.1514(18) . ?
Co1 N8 2.1523(19) 4_475 ?
Co1 N10 2.2489(19) . ?
N10 C12 1.432(3) . ?
N10 H10A 0.9000 . ?
N10 H10B 0.9000 . ?
C12 C13 1.384(3) . ?
C12 C11 1.387(3) . ?
C11 C10 1.382(3) . ?
C11 H11 0.9300 . ?
C10 C9 1.387(3) . ?
C10 H10 0.9300 . ?
O2 H2A 0.89(4) . ?
O2 H2B 0.99(4) . ?
O1 Co1 2.1293(14) 3_665 ?
N3 N2 1.315(2) . ?
N3 N4 1.338(2) . ?
N2 N1 1.340(2) . ?
N1 C1 1.337(3) . ?
N4 C1 1.343(3) . ?
N8 N7 1.309(2) . ?
N8 N9 1.349(2) . ?
N8 Co1 2.1523(19) 4_676 ?
N7 N6 1.342(2) . ?
N7 Co2 2.1562(18) 2_755 ?
N6 C8 1.344(3) . ?
N9 C8 1.331(3) . ?
C8 C9 1.475(3) . ?
N5 C5 1.399(3) . ?
N5 H5B 0.91(3) . ?
N5 H5A 0.94(4) . ?
C1 C2 1.471(3) . ?
C13 C14 1.388(3) . ?
C13 H13 0.9300 . ?
C9 C14 1.387(3) . ?
C14 H14 0.9300 . ?
C2 C7 1.382(4) . ?
C2 C3 1.388(4) . ?
C5 C6 1.381(4) . ?
C5 C4 1.385(4) . ?
C7 C6 1.389(4) . ?
C7 H7 0.9300 . ?
C6 H6 0.9300 . ?
C4 C3 1.381(3) . ?
C4 H4 0.9300 . ?
C3 H3 0.9300 . ?

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
N3 Co2 N3 180.00(10) . 3_765 ?
N3 Co2 N7 83.24(7) . 2_745 ?
N3 Co2 N7 96.76(7) 3_765 2_745 ?
N3 Co2 N7 96.76(7) . 4_575 ?
N3 Co2 N7 83.24(7) 3_765 4_575 ?
N7 Co2 N7 180.00(5) 2_745 4_575 ?
N3 Co2 O1 94.10(7) . 3_765 ?
N3 Co2 O1 85.90(7) 3_765 3_765 ?
N7 Co2 O1 94.80(6) 2_745 3_765 ?
N7 Co2 O1 85.20(6) 4_575 3_765 ?
N3 Co2 O1 85.90(7) . . ?
N3 Co2 O1 94.10(7) 3_765 . ?
N7 Co2 O1 85.20(6) 2_745 . ?
N7 Co2 O1 94.80(6) 4_575 . ?
O1 Co2 O1 180.0 3_765 . ?
N2 Co1 O1 85.07(6) . . ?
N2 Co1 O1 104.95(7) . 3_665 ?
O1 Co1 O1 86.61(6) . 3_665 ?
N2 Co1 O2 81.83(7) . . ?
O1 Co1 O2 165.56(6) . . ?
O1 Co1 O2 90.90(6) 3_665 . ?
N2 Co1 N8 166.59(7) . 4_475 ?
O1 Co1 N8 104.66(7) . 4_475 ?
O1 Co1 N8 85.11(6) 3_665 4_475 ?
O2 Co1 N8 89.27(8) . 4_475 ?
N2 Co1 N10 87.63(7) . . ?
O1 Co1 N10 94.45(6) . . ?
O1 Co1 N10 167.42(6) 3_665 . ?
O2 Co1 N10 91.06(7) . . ?
N8 Co1 N10 82.50(7) 4_475 . ?
C12 N10 Co1 121.33(14) . . ?
C12 N10 H10A 107.0 . . ?
Co1 N10 H10A 107.0 . . ?
C12 N10 H10B 107.0 . . ?
Co1 N10 H10B 107.0 . . ?
H10A N10 H10B 106.7 . . ?
C13 C12 C11 119.4(2) . . ?
C13 C12 N10 121.8(2) . . ?
C11 C12 N10 118.7(2) . . ?
C10 C11 C12 120.0(2) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C10 C9 121.1(2) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
Co1 O2 H2A 103(2) . . ?
Co1 O2 H2B 110(2) . . ?
H2A O2 H2B 102(3) . . ?
Co1 O1 Co1 93.39(6) . 3_665 ?
Co1 O1 Co2 117.60(6) . . ?
Co1 O1 Co2 118.63(6) 3_665 . ?
N2 N3 N4 109.25(17) . . ?
N2 N3 Co2 121.42(13) . . ?
N4 N3 Co2 128.61(14) . . ?
N3 N2 N1 109.96(17) . . ?
N3 N2 Co1 123.54(13) . . ?
N1 N2 Co1 124.24(14) . . ?
C1 N1 N2 104.52(18) . . ?
N3 N4 C1 104.89(18) . . ?
N7 N8 N9 109.50(17) . . ?
N7 N8 Co1 123.75(13) . 4_676 ?
N9 N8 Co1 126.54(14) . 4_676 ?
N8 N7 N6 109.67(17) . . ?
N8 N7 Co2 123.08(13) . 2_755 ?
N6 N7 Co2 126.56(14) . 2_755 ?
N7 N6 C8 104.57(18) . . ?
C8 N9 N8 104.72(18) . . ?
N9 C8 N6 111.54(19) . . ?
N9 C8 C9 125.4(2) . . ?
N6 C8 C9 122.9(2) . . ?
C5 N5 H5B 113(2) . . ?
C5 N5 H5A 115(2) . . ?
H5B N5 H5A 108(3) . . ?
N1 C1 N4 111.37(19) . . ?
N1 C1 C2 124.2(2) . . ?
N4 C1 C2 124.4(2) . . ?
C12 C13 C14 120.1(2) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C14 C9 C10 118.5(2) . . ?
C14 C9 C8 121.8(2) . . ?
C10 C9 C8 119.7(2) . . ?
C9 C14 C13 120.8(2) . . ?
C9 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C7 C2 C3 118.3(2) . . ?
C7 C2 C1 120.9(2) . . ?
C3 C2 C1 120.7(2) . . ?
C6 C5 C4 118.4(2) . . ?
C6 C5 N5 120.8(2) . . ?
C4 C5 N5 120.7(2) . . ?
C2 C7 C6 120.6(3) . . ?
C2 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C5 C6 C7 121.0(3) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C3 C4 C5 120.7(2) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C4 C3 C2 121.0(3) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N5 H5B N8 0.91(3) 2.70(3) 3.470(3) 143(3) 4_576
N5 H5B N9 0.91(3) 2.29(3) 3.193(3) 173(3) 4_576
O2 H2B N3 0.99(4) 2.48(4) 3.338(3) 145(3) 1_455
O2 H2B N4 0.99(4) 1.77(4) 2.743(3) 170(3) 1_455
O2 H2A N1 0.89(4) 2.01(4) 2.768(3) 142(3) .
N10 H10B N9 0.90 2.22 2.915(3) 133.9 4_475
N10 H10A N7 0.90 2.61 3.469(3) 160.2 4_575
N10 H10A N6 0.90 2.17 3.045(3) 164.7 4_575
N5 H5A N6 0.94(4) 2.26(4) 3.133(3) 155(3) 4_676

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.43
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.068


data_2
_database_code_depnum_ccdc_archive 'CCDC 883738'
#TrackingRef 'Compound 2.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H12 N10 Zn'
_chemical_formula_sum            'C14 H12 N10 Zn'
_chemical_formula_weight         385.71

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   P-4n2

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

_cell_length_a                   10.1598(2)
_cell_length_b                   10.1598(2)
_cell_length_c                   14.4082(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1487.24(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      28.24

_exptl_crystal_description       block
_exptl_crystal_colour            Purple
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             784
_exptl_absorpt_coefficient_mu    1.674
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   Process-auto

_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  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-sca
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10422
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.45
_diffrn_reflns_theta_max         28.24
_reflns_number_total             1852
_reflns_number_gt                1546
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97

_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^)+(0.0291P)^2^+0.6276P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_number_reflns         1852
_refine_ls_number_parameters     148
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0241
_refine_ls_wR_factor_ref         0.0653
_refine_ls_wR_factor_gt          0.0613
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_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
H5B H -0.118(4) 0.613(4) 0.403(4) 0.15(2) Uiso 1 1 d D . .
H5A H -0.025(4) 0.685(4) 0.4852(15) 0.085(13) Uiso 1 1 d D . .
H6 H -0.145(5) 0.708(5) 0.263(4) 0.043(16) Uiso 0.50 1 d P . .
H6' H -0.013(4) 0.622(5) 0.238(4) 0.024(12) Uiso 0.50 1 d P . .
C6 C -0.0509(5) 0.7714(5) 0.2751(4) 0.0401(12) Uani 0.50 1 d P . .
C6' C 0.0233(5) 0.6996(6) 0.2602(4) 0.0415(12) Uani 0.50 1 d P . .
C7 C 0.0854(6) 0.7791(6) 0.1968(3) 0.0334(10) Uani 0.50 1 d P . .
H7 H 0.0868 0.7566 0.1342 0.040 Uiso 0.50 1 calc PR . .
C7' C 0.0262(6) 0.8314(6) 0.2076(4) 0.0334(11) Uani 0.50 1 d P . .
H7' H -0.0026 0.8295 0.1463 0.040 Uiso 0.50 1 calc PR . .
C4 C 0.1000(3) 0.8406(3) 0.38744(17) 0.0421(6) Uani 1 1 d . . .
H4 H 0.1180 0.8529 0.4501 0.050 Uiso 1 1 calc R . .
C3 C 0.1687(2) 0.9120(3) 0.32198(15) 0.0371(5) Uani 1 1 d . . .
H3 H 0.2312 0.9729 0.3416 0.045 Uiso 1 1 calc R . .
C2 C 0.1472(2) 0.8957(2) 0.22800(16) 0.0314(5) Uani 1 1 d . . .
N5 N -0.0637(4) 0.6791(4) 0.4265(2) 0.0895(12) Uani 1 1 d D . .
C5 C 0.0071(4) 0.7531(5) 0.3618(2) 0.0682(11) Uani 1 1 d . . .
Zn1 Zn 0.0000 1.0000 0.0000 0.02333(13) Uani 1 4 d S . .
Zn2 Zn 0.5000 1.0000 0.2500 0.02229(13) Uani 1 4 d S . .
N4 N 0.3420(2) 1.01433(18) 0.16476(16) 0.0274(4) Uani 1 1 d . . .
N1 N 0.1682(2) 1.01013(19) 0.07558(16) 0.0297(5) Uani 1 1 d . . .
N2 N 0.26480(19) 1.0799(2) 0.03269(14) 0.0348(4) Uani 1 1 d . . .
N3 N 0.36774(19) 1.0825(2) 0.08489(14) 0.0361(5) Uani 1 1 d . . .
C1 C 0.2180(2) 0.9710(2) 0.15818(16) 0.0262(4) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C6 0.030(2) 0.036(3) 0.054(3) 0.014(2) -0.002(2) -0.013(2)
C6' 0.039(3) 0.038(3) 0.047(3) 0.006(2) -0.005(2) -0.011(2)
C7 0.028(3) 0.042(3) 0.030(2) 0.003(2) 0.000(2) -0.004(2)
C7' 0.030(3) 0.039(3) 0.031(2) 0.007(2) -0.005(2) -0.003(2)
C4 0.0396(14) 0.0549(16) 0.0317(12) 0.0043(11) 0.0014(11) -0.0042(12)
C3 0.0358(12) 0.0431(13) 0.0325(12) -0.0018(11) 0.0038(10) -0.0068(10)
C2 0.0281(11) 0.0359(12) 0.0300(11) 0.0076(9) -0.0042(9) -0.0065(9)
N5 0.082(2) 0.124(3) 0.063(2) 0.050(2) -0.0160(19) -0.055(2)
C5 0.072(2) 0.092(2) 0.041(2) 0.036(2) -0.0136(14) -0.0481(18)
Zn1 0.02456(18) 0.02456(18) 0.0209(2) 0.000 0.000 0.000
Zn2 0.02156(17) 0.02156(17) 0.0237(3) 0.000 0.000 -0.00256(17)
N4 0.0227(11) 0.0316(11) 0.0280(10) 0.0028(8) -0.0021(8) -0.0024(7)
N1 0.0299(11) 0.0349(12) 0.0244(9) 0.0032(8) -0.0020(9) -0.0061(8)
N2 0.0314(10) 0.0428(12) 0.0302(9) 0.0088(9) -0.0031(8) -0.0078(8)
N3 0.0298(10) 0.0485(12) 0.0301(10) 0.0088(9) -0.0014(8) -0.0081(9)
C1 0.0245(10) 0.0262(10) 0.0280(10) 0.0005(8) -0.0027(8) -0.0018(8)

_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
C6 C7' 1.389(7) . ?
C6 C5 1.394(6) . ?
C6 H6 1.17(5) . ?
C6' C7 1.372(7) . ?
C6' C5 1.570(7) . ?
C6' H6' 0.93(5) . ?
C7 C2 1.414(5) . ?
C7 H7 0.9300 . ?
C7' C2 1.422(5) . ?
C7' H7' 0.9300 . ?
C4 C5 1.348(4) . ?
C4 C3 1.380(3) . ?
C4 H4 0.9300 . ?
C3 C2 1.382(3) . ?
C3 H3 0.9300 . ?
C2 C1 1.454(3) . ?
N5 C5 1.398(4) . ?
N5 H5B 0.929(10) . ?
N5 H5A 0.935(10) . ?
Zn1 N1 2.029(2) 3_465 ?
Zn1 N1 2.029(2) . ?
Zn1 N1 2.029(2) 4_665 ?
Zn1 N1 2.029(2) 2_575 ?
Zn2 N4 2.026(2) 8_665 ?
Zn2 N4 2.026(2) . ?
Zn2 N4 2.026(2) 2_675 ?
Zn2 N4 2.026(2) 7_455 ?
N4 C1 1.339(3) . ?
N4 N3 1.368(3) . ?
N1 C1 1.353(3) . ?
N1 N2 1.359(3) . ?
N2 N3 1.288(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7' C6 C5 116.5(4) . . ?
C7' C6 H6 127(3) . . ?
C5 C6 H6 114(3) . . ?
C7 C6' C5 117.7(5) . . ?
C7 C6' H6' 117(3) . . ?
C5 C6' H6' 125(3) . . ?
C6' C7 C2 119.0(5) . . ?
C6' C7 H7 120.5 . . ?
C2 C7 H7 120.5 . . ?
C6 C7' C2 123.0(4) . . ?
C6 C7' H7' 118.5 . . ?
C2 C7' H7' 118.5 . . ?
C5 C4 C3 120.9(3) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C4 C3 C2 121.7(2) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C3 C2 C7 118.9(3) . . ?
C3 C2 C7' 113.2(3) . . ?
C7 C2 C7' 33.5(3) . . ?
C3 C2 C1 122.4(2) . . ?
C7 C2 C1 116.1(3) . . ?
C7' C2 C1 121.7(3) . . ?
C5 N5 H5B 117(4) . . ?
C5 N5 H5A 111(3) . . ?
H5B N5 H5A 128(4) . . ?
C4 C5 C6 117.0(3) . . ?
C4 C5 N5 122.1(3) . . ?
C6 C5 N5 116.9(3) . . ?
C4 C5 C6' 114.3(3) . . ?
C6 C5 C6' 41.8(3) . . ?
N5 C5 C6' 119.4(4) . . ?
N1 Zn1 N1 106.73(6) 3_465 . ?
N1 Zn1 N1 115.10(13) 3_465 4_665 ?
N1 Zn1 N1 106.73(6) . 4_665 ?
N1 Zn1 N1 106.73(6) 3_465 2_575 ?
N1 Zn1 N1 115.10(13) . 2_575 ?
N1 Zn1 N1 106.73(6) 4_665 2_575 ?
N4 Zn2 N4 104.69(12) 8_665 . ?
N4 Zn2 N4 118.77(11) 8_665 2_675 ?
N4 Zn2 N4 105.37(13) . 2_675 ?
N4 Zn2 N4 105.37(13) 8_665 7_455 ?
N4 Zn2 N4 118.77(11) . 7_455 ?
N4 Zn2 N4 104.69(12) 2_675 7_455 ?
C1 N4 N3 106.7(2) . . ?
C1 N4 Zn2 139.92(17) . . ?
N3 N4 Zn2 113.28(16) . . ?
C1 N1 N2 106.5(2) . . ?
C1 N1 Zn1 140.51(17) . . ?
N2 N1 Zn1 112.99(16) . . ?
N3 N2 N1 109.3(2) . . ?
N2 N3 N4 109.02(19) . . ?
N4 C1 N1 108.5(2) . . ?
N4 C1 C2 126.1(2) . . ?
N1 C1 C2 125.4(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N5 H5A N3 0.935(10) 2.39(3) 3.184(4) 143(3) 6_545

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        28.24
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.049


data_3
_database_code_depnum_ccdc_archive 'CCDC 883739'
#TrackingRef 'Compound 3.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C7 H6 Ag N5'
_chemical_formula_sum            'C7 H6 Ag N5'
_chemical_formula_weight         268.04

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'
Ag Ag -0.8971 1.1015 '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           monoclinic
_symmetry_space_group_name_H-M   'P 21/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                   9.6538(11)
_cell_length_b                   6.8521(7)
_cell_length_c                   12.5458(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.164(6)
_cell_angle_gamma                90.00
_cell_volume                     797.08(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      28.39

_exptl_crystal_description       needle-like
_exptl_crystal_colour            'pale brown'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             520
_exptl_absorpt_coefficient_mu    2.480
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   none

_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 AXS SMART APEX CCD'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5486
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         28.39
_reflns_number_total             1982
_reflns_number_gt                1535
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 1997-2002)'
_computing_cell_refinement       'SAINT-Plus (Bruker, 2003)'
_computing_data_reduction        SAINT-Plus
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+1.9949P] 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         1982
_refine_ls_number_parameters     118
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0386
_refine_ls_wR_factor_ref         0.1075
_refine_ls_wR_factor_gt          0.1012
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.100
_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
Ag1 Ag 0.39396(4) 0.65728(7) 0.71369(3) 0.04111(16) Uani 1 1 d . . .
N1 N 0.4419(4) 0.7173(6) 0.5596(3) 0.0262(8) Uani 1 1 d . . .
N4 N 0.4436(4) 0.7697(6) 0.3876(3) 0.0268(8) Uani 1 1 d . . .
N5 N -0.2489(4) 0.6451(6) 0.2979(4) 0.0329(9) Uani 1 1 d . . .
H5A H -0.2726 0.6944 0.2287 0.040 Uiso 1 1 calc R . .
H5B H -0.2842 0.7290 0.3390 0.040 Uiso 1 1 calc R . .
C5 C -0.0970(5) 0.6617(7) 0.3375(4) 0.0254(9) Uani 1 1 d . . .
N3 N 0.5794(4) 0.7874(6) 0.4549(3) 0.0306(9) Uani 1 1 d . . .
N2 N 0.5789(4) 0.7581(7) 0.5572(3) 0.0298(8) Uani 1 1 d . . .
C1 C 0.3606(5) 0.7252(7) 0.4542(3) 0.0242(9) Uani 1 1 d . . .
C3 C 0.1153(5) 0.7525(8) 0.4821(4) 0.0299(10) Uani 1 1 d . . .
H3 H 0.1566 0.8029 0.5526 0.036 Uiso 1 1 calc R . .
C7 C 0.1394(5) 0.6188(7) 0.3121(4) 0.0287(10) Uani 1 1 d . . .
H7 H 0.1968 0.5762 0.2682 0.034 Uiso 1 1 calc R . .
C6 C -0.0087(5) 0.6029(7) 0.2728(4) 0.0282(10) Uani 1 1 d . . .
H6 H -0.0498 0.5523 0.2023 0.034 Uiso 1 1 calc R . .
C4 C -0.0324(5) 0.7332(8) 0.4442(4) 0.0309(10) Uani 1 1 d . . .
H4 H -0.0894 0.7680 0.4899 0.037 Uiso 1 1 calc R . .
C2 C 0.2041(5) 0.6974(6) 0.4162(4) 0.0248(9) 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
Ag1 0.0330(2) 0.0722(3) 0.01952(19) 0.00140(18) 0.00958(14) 0.0057(2)
N1 0.0240(19) 0.037(2) 0.0172(17) -0.0028(15) 0.0059(14) 0.0007(16)
N4 0.0219(18) 0.039(2) 0.0209(18) -0.0010(16) 0.0081(14) -0.0002(16)
N5 0.0211(18) 0.047(2) 0.030(2) 0.0010(18) 0.0066(15) -0.0033(18)
C5 0.0188(19) 0.031(2) 0.025(2) 0.0028(18) 0.0038(16) -0.0013(18)
N3 0.0252(19) 0.042(2) 0.026(2) 0.0021(17) 0.0095(16) 0.0020(17)
N2 0.0224(19) 0.043(2) 0.0239(19) -0.0004(18) 0.0058(15) -0.0013(17)
C1 0.027(2) 0.028(2) 0.0176(19) -0.0020(17) 0.0064(16) 0.0013(18)
C3 0.027(2) 0.045(3) 0.0168(19) -0.005(2) 0.0057(17) -0.001(2)
C7 0.028(2) 0.037(3) 0.024(2) -0.0055(19) 0.0120(17) -0.0006(19)
C6 0.028(2) 0.034(2) 0.022(2) -0.0062(18) 0.0054(17) -0.0038(19)
C4 0.025(2) 0.046(3) 0.023(2) 0.000(2) 0.0083(18) 0.000(2)
C2 0.026(2) 0.028(2) 0.021(2) 0.0038(16) 0.0066(17) 0.0009(17)

_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
Ag1 N1 2.148(4) . ?
Ag1 N4 2.159(4) 4_576 ?
Ag1 N5 2.482(4) 3_566 ?
N1 C1 1.339(5) . ?
N1 N2 1.361(5) . ?
N4 C1 1.343(5) . ?
N4 N3 1.353(5) . ?
N4 Ag1 2.159(4) 4_575 ?
N5 C5 1.416(6) . ?
N5 Ag1 2.482(4) 3_566 ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
C5 C6 1.391(6) . ?
C5 C4 1.399(6) . ?
N3 N2 1.301(5) . ?
C1 C2 1.465(6) . ?
C3 C4 1.378(6) . ?
C3 C2 1.397(6) . ?
C3 H3 0.9300 . ?
C7 C6 1.381(6) . ?
C7 C2 1.390(6) . ?
C7 H7 0.9300 . ?
C6 H6 0.9300 . ?
C4 H4 0.9300 . ?

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 Ag1 N4 145.31(15) . 4_576 ?
N1 Ag1 N5 111.47(15) . 3_566 ?
N4 Ag1 N5 102.45(15) 4_576 3_566 ?
C1 N1 N2 106.0(3) . . ?
C1 N1 Ag1 133.1(3) . . ?
N2 N1 Ag1 120.9(3) . . ?
C1 N4 N3 106.0(3) . . ?
C1 N4 Ag1 132.7(3) . 4_575 ?
N3 N4 Ag1 120.9(3) . 4_575 ?
C5 N5 Ag1 126.9(3) . 3_566 ?
C5 N5 H5A 105.6 . . ?
Ag1 N5 H5A 105.6 3_566 . ?
C5 N5 H5B 105.6 . . ?
Ag1 N5 H5B 105.6 3_566 . ?
H5A N5 H5B 106.1 . . ?
C6 C5 C4 118.5(4) . . ?
C6 C5 N5 121.0(4) . . ?
C4 C5 N5 120.4(4) . . ?
N2 N3 N4 109.4(4) . . ?
N3 N2 N1 108.9(4) . . ?
N1 C1 N4 109.7(4) . . ?
N1 C1 C2 125.7(4) . . ?
N4 C1 C2 124.6(4) . . ?
C4 C3 C2 121.1(4) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C6 C7 C2 121.0(4) . . ?
C6 C7 H7 119.5 . . ?
C2 C7 H7 119.5 . . ?
C7 C6 C5 120.7(4) . . ?
C7 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C3 C4 C5 120.4(4) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C7 C2 C3 118.1(4) . . ?
C7 C2 C1 120.6(4) . . ?
C3 C2 C1 121.3(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N5 H5B N3 0.90 2.25 3.065(6) 150.0 1_455
N5 H5A N2 0.90 2.25 3.087(6) 154.1 4_475

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        28.39
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         1.086
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.127


data_4
_database_code_depnum_ccdc_archive 'CCDC 883740'
#TrackingRef 'Compound 4.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C8 H6 Co N4 O3'
_chemical_formula_sum            'C8 H6 Co N4 O3'
_chemical_formula_weight         265.10

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/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                   12.0719(6)
_cell_length_b                   7.3729(4)
_cell_length_c                   10.1929(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.4340(10)
_cell_angle_gamma                90.00
_cell_volume                     870.15(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6195
_cell_measurement_theta_min      1.76
_cell_measurement_theta_max      28.36

_exptl_crystal_description       block
_exptl_crystal_colour            Purple
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.024
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             532
_exptl_absorpt_coefficient_mu    1.968
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.573
_exptl_absorpt_correction_T_max  0.675
_exptl_absorpt_process_details   Process-auto

_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  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6195
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.76
_diffrn_reflns_theta_max         28.36
_reflns_number_total             2170
_reflns_number_gt                1962
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97

_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^)+(0.0308P)^2^+0.5046P] 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         2170
_refine_ls_number_parameters     169
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0240
_refine_ls_wR_factor_ref         0.0624
_refine_ls_wR_factor_gt          0.0606
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.001
_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
H7 H -0.402(2) 0.241(4) 0.437(3) 0.044(7) Uiso 1 1 d . . .
H8 H -0.294(3) 0.246(4) 0.473(3) 0.045(8) Uiso 1 1 d . . .
H4 H 0.0388(19) -0.025(3) 0.753(2) 0.021(5) Uiso 1 1 d . . .
H3 H 0.230(2) 0.020(3) 0.864(2) 0.027(6) Uiso 1 1 d . . .
H2 H -0.061(2) 0.323(3) 1.005(2) 0.033(6) Uiso 1 1 d . . .
H1 H 0.1367(19) 0.361(3) 1.123(2) 0.031(6) Uiso 1 1 d . . .
O3 O -0.34556(12) 0.2302(2) 0.50356(14) 0.0237(3) Uani 1 1 d . . .
N3 N 0.49010(11) 0.35712(19) 1.13901(14) 0.0150(3) Uani 1 1 d . . .
N2 N 0.47993(12) 0.2636(2) 1.24371(14) 0.0181(3) Uani 1 1 d . . .
N1 N 0.37588(12) 0.1832(2) 1.21130(14) 0.0167(3) Uani 1 1 d . . .
N4 N 0.39258(11) 0.34109(19) 1.03402(13) 0.0147(3) Uani 1 1 d . . .
Co1 Co -0.348536(18) 0.01890(3) 0.64364(2) 0.01324(8) Uani 1 1 d . . .
O1 O -0.17240(11) 0.00185(17) 0.68472(13) 0.0223(3) Uani 1 1 d . . .
O2 O -0.23479(10) 0.18632(19) 0.81568(12) 0.0224(3) Uani 1 1 d . . .
C3 C 0.05724(14) 0.0505(2) 0.82604(17) 0.0163(3) Uani 1 1 d . . .
C1 C 0.20169(14) 0.1936(2) 1.00697(16) 0.0146(3) Uani 1 1 d . . .
C7 C -0.15206(13) 0.1096(2) 0.78509(16) 0.0148(3) Uani 1 1 d . . .
C5 C -0.00018(14) 0.2580(2) 0.97725(17) 0.0170(3) Uani 1 1 d . . .
C6 C 0.11557(15) 0.2830(2) 1.04760(17) 0.0181(3) Uani 1 1 d . . .
C4 C -0.02914(14) 0.1416(2) 0.86517(16) 0.0146(3) Uani 1 1 d . . .
C8 C 0.32331(14) 0.2346(2) 1.08178(15) 0.0139(3) Uani 1 1 d . . .
C2 C 0.17292(14) 0.0764(2) 0.89596(17) 0.0173(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
O3 0.0171(6) 0.0336(7) 0.0187(6) 0.0074(5) 0.0020(5) -0.0047(6)
N3 0.0103(6) 0.0195(7) 0.0128(6) 0.0022(5) -0.0005(5) -0.0010(5)
N2 0.0120(6) 0.0250(8) 0.0152(6) 0.0027(6) 0.0004(5) -0.0033(6)
N1 0.0114(6) 0.0230(7) 0.0134(6) 0.0026(5) -0.0005(5) -0.0030(5)
N4 0.0095(6) 0.0203(7) 0.0122(6) 0.0012(5) -0.0002(5) -0.0018(5)
Co1 0.00895(12) 0.01842(13) 0.01113(12) -0.00063(8) 0.00086(8) -0.00023(8)
O1 0.0121(6) 0.0310(7) 0.0212(6) -0.0091(5) 0.0005(5) -0.0027(5)
O2 0.0119(6) 0.0332(7) 0.0205(6) -0.0036(5) 0.0020(5) 0.0031(5)
C3 0.0142(8) 0.0181(8) 0.0152(7) -0.0029(6) 0.0018(6) -0.0013(6)
C1 0.0107(7) 0.0183(7) 0.0132(7) 0.0042(6) 0.0005(6) -0.0024(6)
C7 0.0113(7) 0.0181(8) 0.0138(7) 0.0031(6) 0.0014(6) -0.0012(6)
C5 0.0128(8) 0.0210(8) 0.0171(8) -0.0007(6) 0.0041(6) 0.0002(6)
C6 0.0150(8) 0.0235(8) 0.0140(7) -0.0038(6) 0.0011(6) -0.0021(7)
C4 0.0119(7) 0.0163(7) 0.0138(7) 0.0031(6) 0.0007(6) -0.0021(6)
C8 0.0117(7) 0.0169(7) 0.0125(7) 0.0010(6) 0.0022(6) -0.0005(6)
C2 0.0129(7) 0.0197(8) 0.0185(8) -0.0003(6) 0.0033(6) 0.0016(6)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O3 Co1 2.1203(14) . ?
O3 H7 0.82(3) . ?
O3 H8 0.78(3) . ?
N3 N2 1.3051(19) . ?
N3 N4 1.3536(18) . ?
N3 Co1 2.1402(14) 4_666 ?
N2 N1 1.3429(19) . ?
N1 C8 1.3471(19) . ?
N1 Co1 2.1892(14) 3_557 ?
N4 C8 1.335(2) . ?
N4 Co1 2.1762(13) 2_556 ?
Co1 O1 2.0514(13) . ?
Co1 N3 2.1402(14) 4_465 ?
Co1 N4 2.1762(14) 2_546 ?
Co1 N1 2.1892(14) 3_557 ?
Co1 O2 2.2631(12) . ?
O1 C7 1.263(2) . ?
O2 C7 1.261(2) . ?
C3 C2 1.390(2) . ?
C3 C4 1.390(2) . ?
C3 H4 0.91(2) . ?
C1 C2 1.388(2) . ?
C1 C6 1.390(2) . ?
C1 C8 1.481(2) . ?
C7 C4 1.496(2) . ?
C5 C6 1.391(2) . ?
C5 C4 1.392(2) . ?
C5 H2 0.99(2) . ?
C6 H1 0.93(2) . ?
C2 H3 0.93(2) . ?

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
Co1 O3 H7 117.6(19) . . ?
Co1 O3 H8 123(2) . . ?
H7 O3 H8 103(3) . . ?
N2 N3 N4 109.78(13) . . ?
N2 N3 Co1 120.21(10) . 4_666 ?
N4 N3 Co1 129.59(10) . 4_666 ?
N3 N2 N1 109.25(12) . . ?
N2 N1 C8 105.41(13) . . ?
N2 N1 Co1 116.33(10) . 3_557 ?
C8 N1 Co1 137.22(11) . 3_557 ?
C8 N4 N3 104.92(12) . . ?
C8 N4 Co1 128.82(11) . 2_556 ?
N3 N4 Co1 123.94(10) . 2_556 ?
O1 Co1 O3 88.19(6) . . ?
O1 Co1 N3 156.21(5) . 4_465 ?
O3 Co1 N3 81.96(6) . 4_465 ?
O1 Co1 N4 97.35(5) . 2_546 ?
O3 Co1 N4 85.93(5) . 2_546 ?
N3 Co1 N4 103.44(5) 4_465 2_546 ?
O1 Co1 N1 99.56(5) . 3_557 ?
O3 Co1 N1 171.70(6) . 3_557 ?
N3 Co1 N1 89.74(5) 4_465 3_557 ?
N4 Co1 N1 95.96(5) 2_546 3_557 ?
O1 Co1 O2 60.57(5) . . ?
O3 Co1 O2 89.94(5) . . ?
N3 Co1 O2 97.65(5) 4_465 . ?
N4 Co1 O2 157.70(5) 2_546 . ?
N1 Co1 O2 91.28(5) 3_557 . ?
C7 O1 Co1 94.56(10) . . ?
C7 O2 Co1 85.02(10) . . ?
C2 C3 C4 120.86(16) . . ?
C2 C3 H4 118.9(14) . . ?
C4 C3 H4 120.2(14) . . ?
C2 C1 C6 120.19(15) . . ?
C2 C1 C8 121.98(15) . . ?
C6 C1 C8 117.77(15) . . ?
O2 C7 O1 119.74(15) . . ?
O2 C7 C4 121.79(15) . . ?
O1 C7 C4 118.47(15) . . ?
C6 C5 C4 119.17(16) . . ?
C6 C5 H2 120.9(14) . . ?
C4 C5 H2 119.9(14) . . ?
C1 C6 C5 120.72(16) . . ?
C1 C6 H1 118.8(14) . . ?
C5 C6 H1 120.5(14) . . ?
C3 C4 C5 119.91(15) . . ?
C3 C4 C7 118.41(15) . . ?
C5 C4 C7 121.68(15) . . ?
N4 C8 N1 110.64(14) . . ?
N4 C8 C1 124.32(14) . . ?
N1 C8 C1 124.80(14) . . ?
C1 C2 C3 119.14(16) . . ?
C1 C2 H3 121.4(14) . . ?
C3 C2 H3 119.4(14) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        28.36
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.071


data_5
_database_code_depnum_ccdc_archive 'CCDC 883741'
#TrackingRef 'Compound 5.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H4 N4 O2 Pb'
_chemical_formula_sum            'C8 H4 N4 O2 Pb'
_chemical_formula_weight         395.34

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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   C2221

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

_cell_length_a                   17.362(15)
_cell_length_b                   7.135(6)
_cell_length_c                   7.475(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     926.0(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      3.09
_cell_measurement_theta_max      24.99

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.836
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             712
_exptl_absorpt_coefficient_mu    18.202
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   Process-auto

_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  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-sca
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            1462
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0594
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         24.99
_reflns_number_total             810
_reflns_number_gt                780
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97

_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^)+(0.0288P)^2^+0.2306P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0063(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.24(4)
_refine_ls_number_reflns         810
_refine_ls_number_parameters     57
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0300
_refine_ls_wR_factor_ref         0.0766
_refine_ls_wR_factor_gt          0.0762
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_restrained_S_all      1.112
_refine_ls_shift/su_max          0.010
_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
Pb1 Pb 0.440808(18) 0.5000 1.0000 0.0183(3) Uani 1 2 d S . .
O1 O 0.5672(3) 0.5117(13) 1.1465(9) 0.0233(15) Uani 1 1 d . . .
N1 N 1.0568(4) 0.4077(13) 0.9831(19) 0.0314(14) Uani 1 1 d . . .
N2 N 0.9826(4) 0.3452(9) 0.9861(19) 0.0314(14) Uani 1 1 d . . .
C1 C 0.6055(6) 0.5000 1.0000 0.016(2) Uani 1 2 d S . .
C2 C 0.6903(7) 0.5000 1.0000 0.0225(15) Uani 1 2 d S . .
C3 C 0.7314(5) 0.3950(13) 0.8698(13) 0.0225(15) Uani 1 1 d . . .
H3 H 0.7050 0.3246 0.7850 0.027 Uiso 1 1 calc R . .
C4 C 0.8125(6) 0.3985(14) 0.8701(14) 0.027(2) Uani 1 1 d . . .
H4 H 0.8395 0.3325 0.7829 0.032 Uiso 1 1 calc R . .
C5 C 0.8534(6) 0.5000 1.0000 0.0203(17) Uani 1 2 d S . .
C6 C 0.9397(5) 0.5000 1.0000 0.0203(17) 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
Pb1 0.0038(3) 0.0284(4) 0.0228(3) -0.0025(5) 0.000 0.000
O1 0.008(3) 0.040(4) 0.022(3) -0.006(5) -0.003(2) -0.007(6)
N1 0.006(3) 0.030(3) 0.058(4) -0.004(5) 0.006(5) 0.0026(17)
N2 0.006(3) 0.030(3) 0.058(4) -0.004(5) 0.006(5) 0.0026(17)
C1 0.013(5) 0.019(4) 0.017(5) -0.002(13) 0.000 0.000
C2 0.009(4) 0.029(4) 0.029(3) -0.014(4) 0.000 0.000
C3 0.009(4) 0.029(4) 0.029(3) -0.014(4) 0.000 0.000
C4 0.011(5) 0.038(5) 0.032(5) -0.010(5) 0.004(4) 0.011(4)
C5 0.003(4) 0.023(4) 0.035(5) -0.003(8) 0.000 0.000
C6 0.003(4) 0.023(4) 0.035(5) -0.003(8) 0.000 0.000

_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
Pb1 O1 2.454(6) . ?
Pb1 O1 2.454(6) 3_567 ?
Pb1 N2 2.570(7) 5_455 ?
Pb1 N2 2.570(7) 7_457 ?
Pb1 O1 2.648(7) 2_664 ?
Pb1 O1 2.648(7) 4_657 ?
O1 C1 1.283(8) . ?
O1 Pb1 2.648(7) 2_665 ?
N1 N1 1.341(19) 3_567 ?
N1 N2 1.363(9) . ?
N2 C6 1.336(8) . ?
N2 Pb1 2.570(7) 5_545 ?
C1 O1 1.283(8) 3_567 ?
C1 C2 1.472(15) . ?
C2 C3 1.421(11) 3_567 ?
C2 C3 1.421(11) . ?
C3 C4 1.409(13) . ?
C3 H3 0.9300 . ?
C4 C5 1.404(12) . ?
C4 H4 0.9300 . ?
C5 C4 1.404(12) 3_567 ?
C5 C6 1.498(13) . ?
C6 N2 1.336(8) 3_567 ?

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
O1 Pb1 O1 53.2(3) . 3_567 ?
O1 Pb1 N2 74.5(3) . 5_455 ?
O1 Pb1 N2 76.2(3) 3_567 5_455 ?
O1 Pb1 N2 76.2(3) . 7_457 ?
O1 Pb1 N2 74.5(3) 3_567 7_457 ?
N2 Pb1 N2 147.2(3) 5_455 7_457 ?
O1 Pb1 O1 119.57(16) . 2_664 ?
O1 Pb1 O1 66.5(2) 3_567 2_664 ?
N2 Pb1 O1 90.3(4) 5_455 2_664 ?
N2 Pb1 O1 91.4(3) 7_457 2_664 ?
O1 Pb1 O1 66.5(2) . 4_657 ?
O1 Pb1 O1 119.57(16) 3_567 4_657 ?
N2 Pb1 O1 91.4(3) 5_455 4_657 ?
N2 Pb1 O1 90.3(4) 7_457 4_657 ?
O1 Pb1 O1 174.0(2) 2_664 4_657 ?
C1 O1 Pb1 94.6(5) . . ?
C1 O1 Pb1 151.3(5) . 2_665 ?
Pb1 O1 Pb1 113.4(2) . 2_665 ?
N1 N1 N2 108.6(5) 3_567 . ?
C6 N2 N1 104.9(6) . . ?
C6 N2 Pb1 129.2(5) . 5_545 ?
N1 N2 Pb1 125.5(5) . 5_545 ?
O1 C1 O1 117.7(9) 3_567 . ?
O1 C1 C2 121.2(4) 3_567 . ?
O1 C1 C2 121.2(4) . . ?
C3 C2 C3 119.7(11) 3_567 . ?
C3 C2 C1 120.2(5) 3_567 . ?
C3 C2 C1 120.2(5) . . ?
C4 C3 C2 119.5(8) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C5 C4 C3 121.0(8) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C5 C4 119.3(10) . 3_567 ?
C4 C5 C6 120.4(5) . . ?
C4 C5 C6 120.4(5) 3_567 . ?
N2 C6 N2 112.3(8) . 3_567 ?
N2 C6 C5 123.9(4) . . ?
N2 C6 C5 123.9(4) 3_567 . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.479
_refine_diff_density_min         -1.470
_refine_diff_density_rms         0.233