# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H4 Ba N4 O4'
_chemical_formula_weight         381.51

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'
Ba Ba -0.3244 2.2819 '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                   8.2417(16)
_cell_length_b                   10.946(2)
_cell_length_c                   11.113(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.86(3)
_cell_angle_gamma                90.00
_cell_volume                     1000.3(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       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             720
_exptl_absorpt_coefficient_mu    3.989
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.601
_exptl_absorpt_correction_T_max  0.671
_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-scan
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            9586
_diffrn_reflns_av_R_equivalents  0.0172
_diffrn_reflns_av_sigmaI/netI    0.0138
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.10
_diffrn_reflns_theta_max         27.44
_reflns_number_total             2288
_reflns_number_gt                2045
_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    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0324P)²+1.0427P] where P=(Fo²+2Fc²)/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         2288
_refine_ls_number_parameters     188
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0204
_refine_ls_wR_factor_ref         0.0602
_refine_ls_wR_factor_gt          0.0591
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_restrained_S_all      1.119
_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
Ba1 Ba 0.262424(18) 0.000911(10) 0.536888(13) 0.01992(8) Uani 1 1 d . . .
O1 O 0.50609(19) 0.16120(18) 0.50094(13) 0.0214(4) Uani 1 1 d . . .
O2 O 0.2988(3) 0.51612(15) 0.78775(19) 0.0289(5) Uani 1 1 d . . .
O3 O 0.2258(2) -0.10716(16) 0.74256(16) 0.0280(4) Uani 1 1 d . . .
O4 O -0.1089(2) -0.31492(16) 1.08548(16) 0.0259(4) Uani 1 1 d . . .
N1 N 0.3728(3) 0.22241(17) 0.66030(18) 0.0193(4) Uani 1 1 d . . .
N2 N 0.3194(3) 0.31917(18) 0.72830(18) 0.0207(4) Uani 1 1 d . . .
N3 N 0.1232(3) -0.2684(2) 0.8378(2) 0.0235(5) Uani 1 1 d . . .
N4 N 0.0391(3) -0.32870(18) 0.9252(2) 0.0225(4) Uani 1 1 d . . .
C1 C 0.4543(3) 0.24961(19) 0.5656(2) 0.0160(4) Uani 1 1 d . . .
C2 C 0.4794(3) 0.3768(2) 0.5311(2) 0.0154(4) Uani 1 1 d . . .
C3 C 0.4266(3) 0.4719(2) 0.6054(2) 0.0155(4) Uani 1 1 d . . .
C4 C 0.3451(3) 0.4394(2) 0.7136(2) 0.0178(4) Uani 1 1 d . . .
C5 C 0.4471(3) 0.5945(2) 0.5748(2) 0.0169(4) Uani 1 1 d . . .
C6 C 0.1442(3) -0.1482(2) 0.8237(2) 0.0199(5) Uani 1 1 d . . .
C7 C 0.0682(3) -0.0710(2) 0.9123(2) 0.0176(4) Uani 1 1 d . . .
C8 C -0.0157(3) -0.1269(2) 1.00465(19) 0.0172(5) Uani 1 1 d . . .
C9 C -0.0294(3) -0.2609(2) 1.0062(2) 0.0181(5) Uani 1 1 d . . .
C10 C 0.0827(3) 0.0559(2) 0.9080(2) 0.0194(5) Uani 1 1 d . . .
H00 H 0.274(3) 0.299(3) 0.786(3) 0.018(7) Uiso 1 1 d . . .
H01 H 0.163(4) -0.307(3) 0.801(3) 0.025(8) Uiso 1 1 d . . .
H04 H 0.136(3) 0.088(3) 0.844(3) 0.023(7) Uiso 1 1 d . . .
H03 H 0.410(3) 0.657(2) 0.630(2) 0.008(6) Uiso 1 1 d . . .


_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
Ba1 O3 2.6093(18) . ?
Ba1 O1 2.6596(17) 3_656 ?
Ba1 O4 2.6986(19) 2_556 ?
Ba1 O1 2.7165(18) . ?
Ba1 O2 2.811(2) 4_565 ?
Ba1 N4 2.859(2) 4 ?
Ba1 N1 2.902(2) . ?
Ba1 C1 3.154(2) . ?
Ba1 N4 3.158(2) 2_556 ?
Ba1 C9 3.254(2) 2_556 ?
Ba1 Ba1 4.0546(9) 3_656 ?
Ba1 Ba1 4.3482(10) 3_556 ?
O1 C1 1.295(3) . ?
O1 Ba1 2.6596(17) 3_656 ?
O2 C4 1.254(3) . ?
O2 Ba1 2.811(2) 4_566 ?
O3 C6 1.245(3) . ?
O4 C9 1.278(3) . ?
O4 Ba1 2.6986(19) 2_546 ?
N1 C1 1.320(3) . ?
N1 N2 1.390(3) . ?
N2 C4 1.345(3) . ?
N3 C6 1.337(3) . ?
N3 N4 1.396(3) . ?
N4 C9 1.322(3) . ?
N4 Ba1 2.859(2) 4_556 ?
N4 Ba1 3.158(2) 2_546 ?
C1 C2 1.462(3) . ?
C2 C5 1.395(3) 3_666 ?
C2 C3 1.415(3) . ?
C3 C5 1.397(3) . ?
C3 C4 1.461(3) . ?
C5 C2 1.395(3) 3_666 ?
C6 C7 1.470(3) . ?
C7 C10 1.395(4) . ?
C7 C8 1.414(3) . ?
C8 C10 1.387(3) 3_557 ?
C8 C9 1.472(3) . ?
C9 Ba1 3.254(2) 2_546 ?
C10 C8 1.387(3) 3_557 ?

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
O3 Ba1 O1 87.85(6) . 3_656 ?
O3 Ba1 O4 134.60(6) . 2_556 ?
O1 Ba1 O4 137.37(5) 3_656 2_556 ?
O3 Ba1 O1 123.50(6) . . ?
O1 Ba1 O1 82.09(7) 3_656 . ?
O4 Ba1 O1 76.67(6) 2_556 . ?
O3 Ba1 O2 149.21(5) . 4_565 ?
O1 Ba1 O2 71.03(6) 3_656 4_565 ?
O4 Ba1 O2 68.32(6) 2_556 4_565 ?
O1 Ba1 O2 76.66(6) . 4_565 ?
O3 Ba1 N4 88.41(6) . 4 ?
O1 Ba1 N4 86.51(6) 3_656 4 ?
O4 Ba1 N4 90.43(7) 2_556 4 ?
O1 Ba1 N4 145.36(5) . 4 ?
O2 Ba1 N4 68.70(6) 4_565 4 ?
O3 Ba1 N1 90.91(6) . . ?
O1 Ba1 N1 115.27(6) 3_656 . ?
O4 Ba1 N1 74.65(6) 2_556 . ?
O1 Ba1 N1 47.04(5) . . ?
O2 Ba1 N1 118.05(5) 4_565 . ?
N4 Ba1 N1 158.17(6) 4 . ?
O3 Ba1 C1 112.93(6) . . ?
O1 Ba1 C1 103.41(6) 3_656 . ?
O4 Ba1 C1 67.72(6) 2_556 . ?
O1 Ba1 C1 24.03(5) . . ?
O2 Ba1 C1 94.07(6) 4_565 . ?
N4 Ba1 C1 156.46(6) 4 . ?
N1 Ba1 C1 24.74(5) . . ?
O3 Ba1 N4 90.71(6) . 2_556 ?
O1 Ba1 N4 173.96(5) 3_656 2_556 ?
O4 Ba1 N4 43.91(6) 2_556 2_556 ?
O1 Ba1 N4 103.55(6) . 2_556 ?
O2 Ba1 N4 107.91(7) 4_565 2_556 ?
N4 Ba1 N4 87.59(6) 4 2_556 ?
N1 Ba1 N4 70.60(6) . 2_556 ?
C1 Ba1 N4 82.55(6) . 2_556 ?
O3 Ba1 C9 112.97(6) . 2_556 ?
O1 Ba1 C9 159.02(5) 3_656 2_556 ?
O4 Ba1 C9 22.39(5) 2_556 2_556 ?
O1 Ba1 C9 84.01(6) . 2_556 ?
O2 Ba1 C9 90.52(6) 4_565 2_556 ?
N4 Ba1 C9 96.20(6) 4 2_556 ?
N1 Ba1 C9 64.10(6) . 2_556 ?
C1 Ba1 C9 67.06(6) . 2_556 ?
N4 Ba1 C9 23.74(6) 2_556 2_556 ?
O3 Ba1 Ba1 110.20(5) . 3_656 ?
O1 Ba1 Ba1 41.57(4) 3_656 3_656 ?
O4 Ba1 Ba1 109.16(4) 2_556 3_656 ?
O1 Ba1 Ba1 40.52(4) . 3_656 ?
O2 Ba1 Ba1 68.42(6) 4_565 3_656 ?
N4 Ba1 Ba1 120.75(4) 4 3_656 ?
N1 Ba1 Ba1 79.83(4) . 3_656 ?
C1 Ba1 Ba1 62.63(4) . 3_656 ?
N4 Ba1 Ba1 144.03(4) 2_556 3_656 ?
C9 Ba1 Ba1 122.86(4) 2_556 3_656 ?
O3 Ba1 Ba1 89.47(5) . 3_556 ?
O1 Ba1 Ba1 133.02(4) 3_656 3_556 ?
O4 Ba1 Ba1 58.78(4) 2_556 3_556 ?
O1 Ba1 Ba1 135.33(4) . 3_556 ?
O2 Ba1 Ba1 89.11(6) 4_565 3_556 ?
N4 Ba1 Ba1 46.52(4) 4 3_556 ?
N1 Ba1 Ba1 111.66(4) . 3_556 ?
C1 Ba1 Ba1 120.57(4) . 3_556 ?
N4 Ba1 Ba1 41.07(4) 2_556 3_556 ?
C9 Ba1 Ba1 53.57(4) 2_556 3_556 ?
Ba1 Ba1 Ba1 157.510(10) 3_656 3_556 ?
C1 O1 Ba1 148.59(15) . 3_656 ?
C1 O1 Ba1 97.26(13) . . ?
Ba1 O1 Ba1 97.91(7) 3_656 . ?
C4 O2 Ba1 131.31(16) . 4_566 ?
C6 O3 Ba1 153.98(17) . . ?
C9 O4 Ba1 104.06(15) . 2_546 ?
C1 N1 N2 117.28(18) . . ?
C1 N1 Ba1 88.38(13) . . ?
N2 N1 Ba1 142.49(15) . . ?
C4 N2 N1 128.43(19) . . ?
C6 N3 N4 128.4(2) . . ?
C9 N4 N3 117.6(2) . . ?
C9 N4 Ba1 111.49(16) . 4_556 ?
N3 N4 Ba1 106.18(15) . 4_556 ?
C9 N4 Ba1 82.22(14) . 2_546 ?
N3 N4 Ba1 143.49(16) . 2_546 ?
Ba1 N4 Ba1 92.41(6) 4_556 2_546 ?
O1 C1 N1 118.6(2) . . ?
O1 C1 C2 120.6(2) . . ?
N1 C1 C2 120.80(19) . . ?
O1 C1 Ba1 58.70(11) . . ?
N1 C1 Ba1 66.88(12) . . ?
C2 C1 Ba1 150.97(16) . . ?
C5 C2 C3 119.6(2) 3_666 . ?
C5 C2 C1 120.8(2) 3_666 . ?
C3 C2 C1 119.6(2) . . ?
C5 C3 C2 121.2(2) . . ?
C5 C3 C4 120.3(2) . . ?
C2 C3 C4 118.5(2) . . ?
O2 C4 N2 121.2(2) . . ?
O2 C4 C3 123.7(2) . . ?
N2 C4 C3 115.05(19) . . ?
C2 C5 C3 119.22(19) 3_666 . ?
O3 C6 N3 121.4(2) . . ?
O3 C6 C7 123.6(2) . . ?
N3 C6 C7 115.1(2) . . ?
C10 C7 C8 120.2(2) . . ?
C10 C7 C6 120.55(19) . . ?
C8 C7 C6 119.2(2) . . ?
C10 C8 C7 120.1(2) 3_557 . ?
C10 C8 C9 121.0(2) 3_557 . ?
C7 C8 C9 118.8(2) . . ?
O4 C9 N4 118.2(2) . . ?
O4 C9 C8 120.8(2) . . ?
N4 C9 C8 121.0(2) . . ?
O4 C9 Ba1 53.55(12) . 2_546 ?
N4 C9 Ba1 74.05(14) . 2_546 ?
C8 C9 Ba1 147.36(16) . 2_546 ?
C8 C10 C7 119.6(2) 3_557 . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.44
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.108
_database_code_depnum_ccdc_archive 'CCDC 991312'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H13 Ba N4 O8.50 S'
_chemical_formula_weight         566.69

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'
Ba Ba -0.3244 2.2819 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/m

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

_cell_length_a                   19.372(3)
_cell_length_b                   23.436(3)
_cell_length_c                   4.7214(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.727(11)
_cell_angle_gamma                90.00
_cell_volume                     2136.2(5)
_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       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1108
_exptl_absorpt_coefficient_mu    2.009
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.786
_exptl_absorpt_correction_T_max  0.818
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            6086
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_sigmaI/netI    0.0554
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         25.15
_reflns_number_total             1963
_reflns_number_gt                1561
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMAR'
_computing_cell_refinement       'Bruker SMAR'
_computing_data_reduction        'Bruker SMAR'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.1420P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1963
_refine_ls_number_parameters     144
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0600
_refine_ls_wR_factor_ref         0.2010
_refine_ls_wR_factor_gt          0.1877
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.092
_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
Ba1 Ba 0.0000 0.15974(3) 0.0000 0.0390(4) Uani 1 2 d S . .
S1 S 0.2621(2) 0.0000 1.1576(6) 0.0405(8) Uani 1 2 d S . .
N1 N 0.1356(3) 0.1867(3) 0.2751(14) 0.0350(16) Uani 1 1 d . . .
N2 N 0.1992(3) 0.2062(3) 0.2054(13) 0.0280(14) Uani 1 1 d . . .
H2A H 0.1983 0.2304 0.0681 0.034 Uiso 1 1 calc R . .
C1 C 0.1995(4) 0.1268(3) 0.6182(15) 0.0274(16) Uani 1 1 d . . .
C2 C 0.2636(4) 0.1483(3) 0.5453(16) 0.0253(16) Uani 1 1 d . . .
C3 C 0.3257(4) 0.1275(4) 0.6734(17) 0.0338(18) Uani 1 1 d . . .
H3A H 0.3676 0.1434 0.6307 0.041 Uiso 1 1 calc R . .
C4 C 0.3247(5) 0.0829(4) 0.8649(18) 0.039(2) Uani 1 1 d . . .
H4A H 0.3659 0.0686 0.9513 0.047 Uiso 1 1 calc R . .
C5 C 0.2620(4) 0.0598(3) 0.9273(15) 0.0300(17) Uani 1 1 d . . .
C6 C 0.2000(5) 0.0808(3) 0.8138(16) 0.0346(19) Uani 1 1 d . . .
H6A H 0.1587 0.0652 0.8642 0.042 Uiso 1 1 calc R . .
C7 C 0.1345(3) 0.1486(3) 0.4803(18) 0.0330(19) Uani 1 1 d D . .
C8 C 0.2626(3) 0.1923(3) 0.3241(15) 0.0271(16) Uani 1 1 d D . .
O1 O 0.0760(3) 0.1315(3) 0.5562(14) 0.0476(16) Uani 1 1 d D . .
O2 O 0.3164(2) 0.2146(2) 0.2401(11) 0.0340(13) Uani 1 1 d D . .
O3 O 0.1973(6) 0.0000 1.2859(18) 0.056(3) Uani 1 2 d S . .
O4 O 0.3254(7) 0.0000 1.3362(19) 0.065(3) Uani 1 2 d S . .
OW1 O -0.0429(4) 0.2677(4) 0.2487(17) 0.074(2) Uani 1 1 d . . .
OW2 O 0.054(2) 0.0000 0.509(9) 0.125(12) Uiso 0.50 2 d SP . .


_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
S1 O4 1.430(11) . ?
S1 O3 1.438(11) . ?
S1 C5 1.773(8) . ?
S1 C5 1.773(8) 6 ?
N1 C7 1.319(11) . ?
N1 N2 1.381(9) . ?
N2 C8 1.347(9) . ?
N2 H2A 0.8600 . ?
C1 C2 1.409(11) . ?
C1 C6 1.419(11) . ?
C1 C7 1.461(11) . ?
C2 C3 1.389(11) . ?
C2 C8 1.466(10) . ?
C3 C4 1.382(12) . ?
C3 H3A 0.9300 . ?
C4 C5 1.384(12) . ?
C4 H4A 0.9300 . ?
C5 C6 1.365(12) . ?
C6 H6A 0.9300 . ?
C7 O1 1.2807(10) . ?
C8 O2 1.2592(10) . ?

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
O4 S1 O3 119.2(6) . . ?
O4 S1 C5 108.6(4) . . ?
O3 S1 C5 107.5(4) . . ?
O4 S1 C5 108.6(4) . 6 ?
O3 S1 C5 107.5(4) . 6 ?
C5 S1 C5 104.4(5) . 6 ?
C7 N1 N2 117.8(6) . . ?
C8 N2 N1 128.5(6) . . ?
C8 N2 H2A 115.8 . . ?
N1 N2 H2A 115.8 . . ?
C2 C1 C6 118.2(7) . . ?
C2 C1 C7 120.7(7) . . ?
C6 C1 C7 121.0(7) . . ?
C3 C2 C1 121.1(7) . . ?
C3 C2 C8 121.2(7) . . ?
C1 C2 C8 117.7(7) . . ?
C4 C3 C2 119.5(8) . . ?
C4 C3 H3A 120.3 . . ?
C2 C3 H3A 120.3 . . ?
C3 C4 C5 119.7(7) . . ?
C3 C4 H4A 120.2 . . ?
C5 C4 H4A 120.2 . . ?
C6 C5 C4 122.2(7) . . ?
C6 C5 S1 118.9(7) . . ?
C4 C5 S1 118.9(6) . . ?
C5 C6 C1 119.2(8) . . ?
C5 C6 H6A 120.4 . . ?
C1 C6 H6A 120.4 . . ?
O1 C7 N1 118.9(7) . . ?
O1 C7 C1 121.1(7) . . ?
N1 C7 C1 120.0(5) . . ?
O2 C8 N2 121.2(6) . . ?
O2 C8 C2 123.7(7) . . ?
N2 C8 C2 115.1(5) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.15
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         2.222
_refine_diff_density_min         -1.233
_refine_diff_density_rms         0.306
_database_code_depnum_ccdc_archive 'CCDC 991313'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H12 Ba2 N4 O10'
_chemical_formula_weight         719.00

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'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pna2(1)

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

_cell_length_a                   6.9812(4)
_cell_length_b                   14.8221(9)
_cell_length_c                   19.0460(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1970.8(2)
_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       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1360
_exptl_absorpt_coefficient_mu    4.043
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.653
_exptl_absorpt_correction_T_max  0.695
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            10417
_diffrn_reflns_av_R_equivalents  0.0708
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.74
_diffrn_reflns_theta_max         25.04
_reflns_number_total             2649
_reflns_number_gt                2634
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMAR'
_computing_cell_refinement       'Bruker SMAR'
_computing_data_reduction        'Bruker SMAR'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0559P)²+8.0913P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.87(3)
_refine_ls_number_reflns         2649
_refine_ls_number_parameters     307
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_ref         0.0863
_refine_ls_wR_factor_gt          0.0862
_refine_ls_goodness_of_fit_ref   1.055
_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
Ba1 Ba 0.75477(6) -0.01916(3) 0.54712(3) 0.01690(14) Uani 1 1 d . . .
Ba2 Ba 0.79178(7) -0.64292(3) 0.45306(3) 0.01857(14) Uani 1 1 d . . .
O1 O 0.9173(9) -0.1246(3) 0.4435(4) 0.0305(15) Uani 1 1 d . . .
O2 O 0.9625(9) -0.4855(3) 0.4263(3) 0.0243(13) Uani 1 1 d . . .
O3 O 0.6823(13) -0.4743(4) 0.1850(4) 0.0331(18) Uani 1 1 d . . .
O4 O 0.7066(9) -0.3473(4) 0.1232(4) 0.0253(16) Uani 1 1 d . . .
O5 O 0.7694(10) -0.1727(4) 0.6196(4) 0.0316(18) Uani 1 1 d . . .
O6 O 0.8732(10) -0.2930(4) 0.8830(3) 0.0280(14) Uani 1 1 d . . .
O7 O 0.6298(8) -0.5172(3) 0.5504(4) 0.0261(13) Uani 1 1 d . . .
O8 O 0.9164(8) -0.5699(3) 0.5813(3) 0.0244(13) Uani 1 1 d . . .
OW1 O 0.8995(11) 0.0815(5) 0.4285(4) 0.048(2) Uani 1 1 d . . .
OW2 O 0.5484(8) -0.7435(3) 0.5411(4) 0.0251(13) Uani 1 1 d . . .
N1 N 0.9634(11) -0.2637(4) 0.4881(4) 0.0271(17) Uani 1 1 d . . .
H1A H 0.9851 -0.2379 0.5278 0.033 Uiso 1 1 calc R . .
N2 N 0.9764(13) -0.3579(4) 0.4885(4) 0.0255(18) Uani 1 1 d . . .
N3 N 0.8105(11) -0.1526(4) 0.7373(5) 0.0247(17) Uani 1 1 d . . .
H3A H 0.8108 -0.0954 0.7300 0.030 Uiso 1 1 calc R . .
N4 N 0.8347(11) -0.1799(4) 0.8060(4) 0.0222(16) Uani 1 1 d . . .
C1 C 0.8244(13) -0.3908(5) 0.3045(5) 0.0199(18) Uani 1 1 d . . .
H1B H 0.8220 -0.4535 0.3029 0.024 Uiso 1 1 calc R . .
C2 C 0.8776(12) -0.3474(5) 0.3666(5) 0.0201(18) Uani 1 1 d . . .
C3 C 0.8782(12) -0.2536(5) 0.3691(4) 0.0198(18) Uani 1 1 d . . .
C4 C 0.8297(13) -0.2037(5) 0.3098(5) 0.0219(19) Uani 1 1 d . . .
H4B H 0.8289 -0.1410 0.3120 0.026 Uiso 1 1 calc R . .
C5 C 0.7825(12) -0.2468(6) 0.2473(6) 0.0222(19) Uani 1 1 d . . .
H5A H 0.7559 -0.2135 0.2071 0.027 Uiso 1 1 calc R . .
C6 C 0.7755(14) -0.3417(6) 0.2458(5) 0.017(2) Uani 1 1 d . . .
C7 C 0.9223(12) -0.2082(5) 0.4352(5) 0.0239(19) Uani 1 1 d . . .
C8 C 0.9380(11) -0.3998(5) 0.4292(4) 0.0185(17) Uani 1 1 d . . .
C9 C 0.7179(12) -0.3915(6) 0.1802(5) 0.0173(18) Uani 1 1 d . . .
C10 C 0.8339(15) -0.4846(5) 0.7178(5) 0.022(2) Uani 1 1 d . . .
H10A H 0.8588 -0.5456 0.7246 0.027 Uiso 1 1 calc R . .
C11 C 0.8476(13) -0.4263(5) 0.7739(5) 0.0225(18) Uani 1 1 d . . .
H11A H 0.8692 -0.4482 0.8190 0.027 Uiso 1 1 calc R . .
C12 C 0.8283(13) -0.3323(6) 0.7617(5) 0.0179(17) Uani 1 1 d . . .
C13 C 0.7893(13) -0.3018(6) 0.6933(5) 0.0188(18) Uani 1 1 d . . .
C14 C 0.7611(16) -0.3628(5) 0.6393(6) 0.0194(19) Uani 1 1 d . . .
H14A H 0.7270 -0.3421 0.5950 0.023 Uiso 1 1 calc R . .
C15 C 0.7831(11) -0.4539(6) 0.6506(5) 0.0173(17) Uani 1 1 d . . .
C16 C 0.7866(13) -0.2053(6) 0.6804(5) 0.0209(19) Uani 1 1 d . . .
C17 C 0.8478(12) -0.2657(5) 0.8192(5) 0.0196(17) Uani 1 1 d . . .
C18 C 0.7731(12) -0.5188(5) 0.5905(5) 0.017(2) Uani 1 1 d . . .


_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
Ba1 O5 2.665(6) . ?
Ba1 O7 2.674(6) 3_545 ?
Ba1 O3 2.745(8) 4_655 ?
Ba1 O1 2.762(7) . ?
Ba1 O8 2.783(6) 3_445 ?
Ba1 N2 2.888(7) 3_445 ?
Ba1 OW1 2.890(7) . ?
Ba1 O4 2.942(7) 4_655 ?
Ba1 O2 3.076(7) 3_445 ?
Ba1 C9 3.169(9) 4_655 ?
Ba1 C8 3.374(8) 3_445 ?
Ba1 Ba2 4.4076(7) 3_445 ?
Ba2 O2 2.668(5) . ?
Ba2 O8 2.809(6) . ?
Ba2 OW2 2.815(6) . ?
Ba2 O6 2.838(6) 4_644 ?
Ba2 O6 2.855(6) 2_744 ?
Ba2 O7 2.861(6) . ?
Ba2 OW1 2.923(7) 3_445 ?
Ba2 OW2 2.975(6) 3_535 ?
Ba2 N4 2.987(8) 4_644 ?
Ba2 C18 3.202(9) . ?
Ba2 C17 3.281(8) 4_644 ?
Ba2 Ba1 4.4076(7) 3_545 ?
O1 C7 1.249(9) . ?
O2 C8 1.284(9) . ?
O2 Ba1 3.076(6) 3_545 ?
O3 C9 1.256(11) . ?
O3 Ba1 2.745(8) 4_644 ?
O4 C9 1.271(12) . ?
O4 Ba1 2.942(7) 4_644 ?
O5 C16 1.260(12) . ?
O6 C17 1.293(10) . ?
O6 Ba2 2.838(6) 4_655 ?
O6 Ba2 2.855(6) 2_745 ?
O7 C18 1.258(11) . ?
O7 Ba1 2.674(6) 3_445 ?
O8 C18 1.267(10) . ?
O8 Ba1 2.783(6) 3_545 ?
OW1 Ba2 2.923(7) 3_545 ?
OW2 Ba2 2.975(6) 3_435 ?
N1 C7 1.333(11) . ?
N1 N2 1.399(9) . ?
N2 C8 1.318(11) . ?
N2 Ba1 2.888(7) 3_545 ?
N3 C16 1.345(13) . ?
N3 N4 1.381(11) . ?
N4 C17 1.300(10) . ?
N4 Ba2 2.987(8) 4_655 ?
C1 C6 1.379(14) . ?
C1 C2 1.396(13) . ?
C2 C3 1.390(11) . ?
C2 C8 1.484(12) . ?
C3 C4 1.392(12) . ?
C3 C7 1.461(11) . ?
C4 C5 1.391(14) . ?
C5 C6 1.407(12) . ?
C6 C9 1.505(12) . ?
C8 Ba1 3.374(8) 3_545 ?
C9 Ba1 3.169(9) 4_644 ?
C10 C11 1.378(13) . ?
C10 C15 1.404(14) . ?
C11 C12 1.420(11) . ?
C12 C13 1.404(13) . ?
C12 C17 1.481(11) . ?
C13 C14 1.384(14) . ?
C13 C16 1.452(12) . ?
C14 C15 1.376(12) . ?
C15 C18 1.496(12) . ?
C17 Ba2 3.281(8) 4_655 ?

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
O5 Ba1 O7 97.0(2) . 3_545 ?
O5 Ba1 O3 72.8(2) . 4_655 ?
O7 Ba1 O3 76.8(2) 3_545 4_655 ?
O5 Ba1 O1 82.6(2) . . ?
O7 Ba1 O1 74.26(19) 3_545 . ?
O3 Ba1 O1 139.0(2) 4_655 . ?
O5 Ba1 O8 108.5(2) . 3_445 ?
O7 Ba1 O8 136.87(16) 3_545 3_445 ?
O3 Ba1 O8 78.3(2) 4_655 3_445 ?
O1 Ba1 O8 141.6(2) . 3_445 ?
O5 Ba1 N2 71.8(2) . 3_445 ?
O7 Ba1 N2 142.7(2) 3_545 3_445 ?
O3 Ba1 N2 129.1(2) 4_655 3_445 ?
O1 Ba1 N2 69.1(2) . 3_445 ?
O8 Ba1 N2 79.5(2) 3_445 3_445 ?
O5 Ba1 OW1 146.4(2) . . ?
O7 Ba1 OW1 64.6(2) 3_545 . ?
O3 Ba1 OW1 124.5(2) 4_655 . ?
O1 Ba1 OW1 65.8(2) . . ?
O8 Ba1 OW1 103.6(2) 3_445 . ?
N2 Ba1 OW1 105.0(2) 3_445 . ?
O5 Ba1 O4 118.7(2) . 4_655 ?
O7 Ba1 O4 73.98(18) 3_545 4_655 ?
O3 Ba1 O4 45.94(19) 4_655 4_655 ?
O1 Ba1 O4 143.52(18) . 4_655 ?
O8 Ba1 O4 63.39(17) 3_445 4_655 ?
N2 Ba1 O4 142.9(2) 3_445 4_655 ?
OW1 Ba1 O4 84.6(2) . 4_655 ?
O5 Ba1 O2 115.63(19) . 3_445 ?
O7 Ba1 O2 131.5(2) 3_545 3_445 ?
O3 Ba1 O2 144.7(2) 4_655 3_445 ?
O1 Ba1 O2 75.57(18) . 3_445 ?
O8 Ba1 O2 66.48(18) 3_445 3_445 ?
N2 Ba1 O2 43.86(17) 3_445 3_445 ?
OW1 Ba1 O2 68.64(17) . 3_445 ?
O4 Ba1 O2 114.16(17) 4_655 3_445 ?
O5 Ba1 C9 95.3(2) . 4_655 ?
O7 Ba1 C9 78.6(2) 3_545 4_655 ?
O3 Ba1 C9 23.1(2) 4_655 4_655 ?
O1 Ba1 C9 152.2(2) . 4_655 ?
O8 Ba1 C9 65.2(2) 3_445 4_655 ?
N2 Ba1 C9 136.6(2) 3_445 4_655 ?
OW1 Ba1 C9 107.2(2) . 4_655 ?
O4 Ba1 C9 23.6(2) 4_655 4_655 ?
O2 Ba1 C9 128.66(19) 3_445 4_655 ?
O5 Ba1 C8 93.8(2) . 3_445 ?
O7 Ba1 C8 136.8(2) 3_545 3_445 ?
O3 Ba1 C8 145.9(2) 4_655 3_445 ?
O1 Ba1 C8 65.9(2) . 3_445 ?
O8 Ba1 C8 76.60(18) 3_445 3_445 ?
N2 Ba1 C8 22.63(19) 3_445 3_445 ?
OW1 Ba1 C8 83.8(2) . 3_445 ?
O4 Ba1 C8 134.12(19) 4_655 3_445 ?
O2 Ba1 C8 22.35(16) 3_445 3_445 ?
C9 Ba1 C8 141.7(2) 4_655 3_445 ?
O5 Ba1 Ba2 134.79(16) . 3_445 ?
O7 Ba1 Ba2 128.14(12) 3_545 3_445 ?
O3 Ba1 Ba2 111.98(15) 4_655 3_445 ?
O1 Ba1 Ba2 108.62(15) . 3_445 ?
O8 Ba1 Ba2 38.19(13) 3_445 3_445 ?
N2 Ba1 Ba2 72.15(14) 3_445 3_445 ?
OW1 Ba1 Ba2 69.96(16) . 3_445 ?
O4 Ba1 Ba2 78.20(14) 4_655 3_445 ?
O2 Ba1 Ba2 36.60(10) 3_445 3_445 ?
C9 Ba1 Ba2 92.51(16) 4_655 3_445 ?
C8 Ba1 Ba2 56.14(13) 3_445 3_445 ?
O2 Ba2 O8 71.98(18) . . ?
O2 Ba2 OW2 147.82(18) . . ?
O8 Ba2 OW2 82.72(18) . . ?
O2 Ba2 O6 140.95(18) . 4_644 ?
O8 Ba2 O6 146.77(17) . 4_644 ?
OW2 Ba2 O6 67.66(18) . 4_644 ?
O2 Ba2 O6 80.56(18) . 2_744 ?
O8 Ba2 O6 106.32(18) . 2_744 ?
OW2 Ba2 O6 126.63(15) . 2_744 ?
O6 Ba2 O6 81.48(12) 4_644 2_744 ?
O2 Ba2 O7 74.39(18) . . ?
O8 Ba2 O7 46.23(17) . . ?
OW2 Ba2 O7 73.76(16) . . ?
O6 Ba2 O7 130.88(17) 4_644 . ?
O6 Ba2 O7 147.49(17) 2_744 . ?
O2 Ba2 OW1 96.7(2) . 3_445 ?
O8 Ba2 OW1 108.01(18) . 3_445 ?
OW2 Ba2 OW1 72.2(2) . 3_445 ?
O6 Ba2 OW1 77.8(2) 4_644 3_445 ?
O6 Ba2 OW1 142.74(19) 2_744 3_445 ?
O7 Ba2 OW1 62.02(19) . 3_445 ?
O2 Ba2 OW2 109.45(17) . 3_535 ?
O8 Ba2 OW2 62.72(15) . 3_535 ?
OW2 Ba2 OW2 74.22(12) . 3_535 ?
O6 Ba2 OW2 93.80(16) 4_644 3_535 ?
O6 Ba2 OW2 65.30(17) 2_744 3_535 ?
O7 Ba2 OW2 103.94(18) . 3_535 ?
OW1 Ba2 OW2 146.1(2) 3_445 3_535 ?
O2 Ba2 N4 96.52(19) . 4_644 ?
O8 Ba2 N4 167.74(17) . 4_644 ?
OW2 Ba2 N4 106.4(2) . 4_644 ?
O6 Ba2 N4 45.20(17) 4_644 4_644 ?
O6 Ba2 N4 75.09(19) 2_744 4_644 ?
O7 Ba2 N4 127.60(19) . 4_644 ?
OW1 Ba2 N4 68.3(2) 3_445 4_644 ?
OW2 Ba2 N4 127.06(18) 3_535 4_644 ?
O2 Ba2 C18 70.8(2) . . ?
O8 Ba2 C18 23.17(19) . . ?
OW2 Ba2 C18 78.0(2) . . ?
O6 Ba2 C18 144.9(2) 4_644 . ?
O6 Ba2 C18 127.36(19) 2_744 . ?
O7 Ba2 C18 23.08(19) . . ?
OW1 Ba2 C18 85.1(2) 3_445 . ?
OW2 Ba2 C18 83.62(19) 3_535 . ?
N4 Ba2 C18 149.3(2) 4_644 . ?
O2 Ba2 C17 118.0(2) . 4_644 ?
O8 Ba2 C17 168.91(18) . 4_644 ?
OW2 Ba2 C17 89.4(2) . 4_644 ?
O6 Ba2 C17 22.95(18) 4_644 4_644 ?
O6 Ba2 C17 72.3(2) 2_744 4_644 ?
O7 Ba2 C17 138.36(19) . 4_644 ?
OW1 Ba2 C17 76.7(2) 3_445 4_644 ?
OW2 Ba2 C17 107.64(18) 3_535 4_644 ?
N4 Ba2 C17 23.34(19) 4_644 4_644 ?
C18 Ba2 C17 160.4(2) . 4_644 ?
O2 Ba2 Ba1 43.41(14) . 3_545 ?
O8 Ba2 Ba1 37.78(12) . 3_545 ?
OW2 Ba2 Ba1 119.30(14) . 3_545 ?
O6 Ba2 Ba1 156.33(14) 4_644 3_545 ?
O6 Ba2 Ba1 76.75(13) 2_744 3_545 ?
O7 Ba2 Ba1 70.83(11) . 3_545 ?
OW1 Ba2 Ba1 125.62(14) 3_445 3_545 ?
OW2 Ba2 Ba1 68.76(10) 3_535 3_545 ?
N4 Ba2 Ba1 134.24(14) 4_644 3_545 ?
C18 Ba2 Ba1 52.01(15) . 3_545 ?
C17 Ba2 Ba1 146.73(15) 4_644 3_545 ?
C7 O1 Ba1 131.5(6) . . ?
C8 O2 Ba2 143.0(6) . . ?
C8 O2 Ba1 92.0(5) . 3_545 ?
Ba2 O2 Ba1 99.99(18) . 3_545 ?
C9 O3 Ba1 97.8(6) . 4_644 ?
C9 O4 Ba1 88.2(5) . 4_644 ?
C16 O5 Ba1 143.8(6) . . ?
C17 O6 Ba2 98.1(4) . 4_655 ?
C17 O6 Ba2 131.0(6) . 2_745 ?
Ba2 O6 Ba2 111.9(2) 4_655 2_745 ?
C18 O7 Ba1 142.8(6) . 3_445 ?
C18 O7 Ba2 93.9(5) . . ?
Ba1 O7 Ba2 120.2(2) 3_445 . ?
C18 O8 Ba1 114.7(5) . 3_545 ?
C18 O8 Ba2 96.1(5) . . ?
Ba1 O8 Ba2 104.0(2) 3_545 . ?
Ba1 OW1 Ba2 111.3(2) . 3_545 ?
Ba2 OW2 Ba2 109.1(2) . 3_435 ?
C7 N1 N2 129.4(7) . . ?
C8 N2 N1 116.9(7) . . ?
C8 N2 Ba1 99.9(5) . 3_545 ?
N1 N2 Ba1 132.5(6) . 3_545 ?
C16 N3 N4 127.5(7) . . ?
C17 N4 N3 118.5(7) . . ?
C17 N4 Ba2 91.1(5) . 4_655 ?
N3 N4 Ba2 143.1(5) . 4_655 ?
C6 C1 C2 120.7(8) . . ?
C3 C2 C1 119.4(8) . . ?
C3 C2 C8 119.7(8) . . ?
C1 C2 C8 120.9(7) . . ?
C2 C3 C4 120.2(8) . . ?
C2 C3 C7 119.4(8) . . ?
C4 C3 C7 120.4(7) . . ?
C5 C4 C3 120.5(8) . . ?
C4 C5 C6 119.0(9) . . ?
C1 C6 C5 120.2(9) . . ?
C1 C6 C9 118.7(8) . . ?
C5 C6 C9 121.1(9) . . ?
O1 C7 N1 121.6(8) . . ?
O1 C7 C3 124.0(8) . . ?
N1 C7 C3 114.4(7) . . ?
O2 C8 N2 118.4(7) . . ?
O2 C8 C2 121.5(7) . . ?
N2 C8 C2 120.0(7) . . ?
O2 C8 Ba1 65.7(4) . 3_545 ?
N2 C8 Ba1 57.5(4) . 3_545 ?
C2 C8 Ba1 155.2(5) . 3_545 ?
O3 C9 O4 123.6(9) . . ?
O3 C9 C6 118.2(9) . . ?
O4 C9 C6 118.2(8) . . ?
O3 C9 Ba1 59.1(5) . 4_644 ?
O4 C9 Ba1 68.1(5) . 4_644 ?
C6 C9 Ba1 160.1(6) . 4_644 ?
C11 C10 C15 121.5(8) . . ?
C10 C11 C12 118.8(9) . . ?
C13 C12 C11 119.1(8) . . ?
C13 C12 C17 119.3(7) . . ?
C11 C12 C17 121.6(8) . . ?
C14 C13 C12 120.4(8) . . ?
C14 C13 C16 121.1(9) . . ?
C12 C13 C16 118.5(8) . . ?
C15 C14 C13 120.6(10) . . ?
C14 C15 C10 119.2(9) . . ?
C14 C15 C18 120.4(9) . . ?
C10 C15 C18 120.1(8) . . ?
O5 C16 N3 122.0(8) . . ?
O5 C16 C13 122.3(9) . . ?
N3 C16 C13 115.7(9) . . ?
O6 C17 N4 119.8(8) . . ?
O6 C17 C12 120.0(7) . . ?
N4 C17 C12 120.2(8) . . ?
O6 C17 Ba2 58.9(4) . 4_655 ?
N4 C17 Ba2 65.5(5) . 4_655 ?
C12 C17 Ba2 156.5(6) . 4_655 ?
O7 C18 O8 123.6(8) . . ?
O7 C18 C15 119.3(7) . . ?
O8 C18 C15 117.0(7) . . ?
O7 C18 Ba2 63.1(5) . . ?
O8 C18 Ba2 60.7(5) . . ?
C15 C18 Ba2 173.0(6) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.04
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.682
_refine_diff_density_min         -1.583
_refine_diff_density_rms         0.171
_database_code_depnum_ccdc_archive 'CCDC 991314'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H10 N6 O9 Zn2'
_chemical_formula_weight         561.04

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'
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'
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   I4(1)/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   17.6446(9)
_cell_length_b                   17.6446(9)
_cell_length_c                   22.742(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7080.4(10)
_cell_formula_units_Z            16
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.105
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4480
_exptl_absorpt_coefficient_mu    2.784
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.744
_exptl_absorpt_correction_T_max  0.757
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            19798
_diffrn_reflns_av_R_equivalents  0.0961
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.46
_diffrn_reflns_theta_max         25.03
_reflns_number_total             3130
_reflns_number_gt                2744
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMAR'
_computing_cell_refinement       'Bruker SMAR'
_computing_data_reduction        'Bruker SMAR'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0377P)²+54.3482P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3130
_refine_ls_number_parameters     293
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0418
_refine_ls_wR_factor_ref         0.1180
_refine_ls_wR_factor_gt          0.1082
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_restrained_S_all      1.119
_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
Zn1 Zn 0.15973(3) 0.77630(3) -0.06183(2) 0.02745(18) Uani 1 1 d . . .
Zn2 Zn 0.36171(3) 0.72046(3) 0.10681(2) 0.02354(17) Uani 1 1 d . . .
O1 O 0.1130(2) 0.70098(18) -0.11948(13) 0.0320(8) Uani 1 1 d . . .
O2 O 0.1422(2) 0.7834(2) -0.34391(15) 0.0468(10) Uani 1 1 d . . .
O3 O 0.41661(18) 0.79546(18) 0.16707(12) 0.0261(7) Uani 1 1 d . . .
O4 O 0.3610(2) 0.7174(2) 0.39137(14) 0.0462(10) Uani 1 1 d . . .
O5 O 0.1950(2) 0.68921(18) -0.01099(15) 0.0361(8) Uani 1 1 d . . .
O6 O 0.24090(19) 0.83397(17) -0.01128(14) 0.0312(7) Uani 1 1 d . . .
OW1 O -0.1464(7) 0.9841(7) 0.1459(5) 0.199(5) Uiso 1 1 d . . .
O8 O 0.32161(19) 0.80923(17) 0.06189(14) 0.0314(8) Uani 1 1 d . . .
O7 O 0.27877(19) 0.66235(17) 0.05921(13) 0.0300(7) Uani 1 1 d . . .
C1 C 0.2257(3) 0.8706(3) -0.2553(2) 0.0395(13) Uani 1 1 d . . .
H1A H 0.2319 0.8895 -0.2932 0.047 Uiso 1 1 calc R . .
C2 C 0.2636(3) 0.9029(3) -0.2089(3) 0.0431(13) Uani 1 1 d . . .
H2A H 0.2971 0.9428 -0.2151 0.052 Uiso 1 1 calc R . .
C3 C 0.2512(3) 0.8749(3) -0.1525(3) 0.0390(12) Uani 1 1 d . . .
H3A H 0.2771 0.8969 -0.1213 0.047 Uiso 1 1 calc R . .
C4 C 0.1684(3) 0.7858(2) -0.18731(19) 0.0253(10) Uani 1 1 d . . .
C5 C 0.1777(3) 0.8091(3) -0.2448(2) 0.0301(10) Uani 1 1 d . . .
C6 C 0.1194(2) 0.7215(2) -0.17281(18) 0.0240(9) Uani 1 1 d . . .
C7 C 0.1362(3) 0.7683(3) -0.2910(2) 0.0343(11) Uani 1 1 d . . .
C8 C 0.2766(3) 0.6393(3) 0.2990(2) 0.0338(11) Uani 1 1 d . . .
H8A H 0.2627 0.6246 0.3367 0.041 Uiso 1 1 calc R . .
C9 C 0.2434(3) 0.6065(3) 0.2507(2) 0.0349(11) Uani 1 1 d . . .
H9A H 0.2065 0.5694 0.2553 0.042 Uiso 1 1 calc R . .
C10 C 0.2659(3) 0.6297(3) 0.1944(2) 0.0313(11) Uani 1 1 d . . .
H10A H 0.2440 0.6064 0.1619 0.038 Uiso 1 1 calc R . .
C11 C 0.3499(2) 0.7160(2) 0.23307(19) 0.0222(9) Uani 1 1 d . . .
C12 C 0.3317(3) 0.6953(3) 0.2902(2) 0.0273(10) Uani 1 1 d . . .
C13 C 0.4029(2) 0.7773(2) 0.22264(18) 0.0229(9) Uani 1 1 d . . .
C14 C 0.3704(3) 0.7339(3) 0.3386(2) 0.0329(11) Uani 1 1 d . . .
C15 C 0.2718(3) 0.7908(2) 0.02503(19) 0.0254(10) Uani 1 1 d . . .
C16 C 0.2465(3) 0.7065(2) 0.02467(19) 0.0250(9) Uani 1 1 d . . .
N1 N 0.0838(2) 0.6855(2) -0.21490(15) 0.0272(8) Uani 1 1 d . . .
H1B H 0.0556 0.6471 -0.2070 0.033 Uiso 1 1 calc R . .
N2 N 0.0922(2) 0.7104(2) -0.27290(16) 0.0321(9) Uani 1 1 d . . .
N3 N 0.2040(2) 0.8183(2) -0.14128(17) 0.0285(9) Uani 1 1 d . . .
N4 N 0.4345(2) 0.8134(2) 0.26544(15) 0.0287(9) Uani 1 1 d . . .
H4A H 0.4653 0.8503 0.2590 0.034 Uiso 1 1 calc R . .
N5 N 0.4171(2) 0.7909(2) 0.32201(16) 0.0333(9) Uani 1 1 d . . .
N6 N 0.3171(2) 0.6836(2) 0.18559(16) 0.0242(8) Uani 1 1 d . . .


_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
Zn1 O5 2.021(3) . ?
Zn1 O1 2.041(3) . ?
Zn1 N1 2.055(4) 16_665 ?
Zn1 O6 2.100(3) . ?
Zn1 N3 2.103(4) . ?
Zn2 O3 1.970(3) 12_766 ?
Zn2 O8 1.999(3) . ?
Zn2 N6 2.062(4) . ?
Zn2 O7 2.089(3) . ?
Zn2 O3 2.137(3) . ?
O1 C6 1.271(5) . ?
O2 C7 1.237(6) . ?
O3 C13 1.326(5) . ?
O3 Zn2 1.970(3) 15_565 ?
O4 C14 1.245(6) . ?
O5 C16 1.255(5) . ?
O6 C15 1.249(5) . ?
O8 C15 1.258(5) . ?
O7 C16 1.245(5) . ?
C1 C2 1.373(8) . ?
C1 C5 1.397(7) . ?
C2 C3 1.391(8) . ?
C3 N3 1.325(6) . ?
C4 N3 1.349(6) . ?
C4 C5 1.381(6) . ?
C4 C6 1.464(6) . ?
C5 C7 1.470(7) . ?
C6 N1 1.309(6) . ?
C7 N2 1.347(7) . ?
C8 C9 1.372(7) . ?
C8 C12 1.401(7) . ?
C9 C10 1.400(7) . ?
C10 N6 1.327(6) . ?
C11 N6 1.353(6) . ?
C11 C12 1.388(6) . ?
C11 C13 1.448(6) . ?
C12 C14 1.463(7) . ?
C13 N4 1.290(6) . ?
C14 N5 1.355(7) . ?
C15 C16 1.553(6) . ?
N1 N2 1.398(5) . ?
N1 Zn1 2.055(4) 11_565 ?
N4 N5 1.381(5) . ?

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
O5 Zn1 O1 89.81(13) . . ?
O5 Zn1 N1 117.24(15) . 16_665 ?
O1 Zn1 N1 100.43(15) . 16_665 ?
O5 Zn1 O6 81.11(12) . . ?
O1 Zn1 O6 160.56(14) . . ?
N1 Zn1 O6 99.01(14) 16_665 . ?
O5 Zn1 N3 130.14(15) . . ?
O1 Zn1 N3 80.06(14) . . ?
N1 Zn1 N3 112.60(15) 16_665 . ?
O6 Zn1 N3 92.66(14) . . ?
O3 Zn2 O8 122.09(14) 12_766 . ?
O3 Zn2 N6 113.87(13) 12_766 . ?
O8 Zn2 N6 123.78(14) . . ?
O3 Zn2 O7 101.70(13) 12_766 . ?
O8 Zn2 O7 82.64(12) . . ?
N6 Zn2 O7 91.59(14) . . ?
O3 Zn2 O3 95.65(17) 12_766 . ?
O8 Zn2 O3 90.17(12) . . ?
N6 Zn2 O3 79.13(13) . . ?
O7 Zn2 O3 162.49(13) . . ?
C6 O1 Zn1 113.0(3) . . ?
C13 O3 Zn2 123.5(3) . 15_565 ?
C13 O3 Zn2 112.3(3) . . ?
Zn2 O3 Zn2 123.83(14) 15_565 . ?
C16 O5 Zn1 114.0(3) . . ?
C15 O6 Zn1 111.3(3) . . ?
C15 O8 Zn2 112.7(3) . . ?
C16 O7 Zn2 109.9(3) . . ?
C2 C1 C5 119.1(5) . . ?
C1 C2 C3 119.0(5) . . ?
N3 C3 C2 123.0(5) . . ?
N3 C4 C5 123.6(4) . . ?
N3 C4 C6 115.4(4) . . ?
C5 C4 C6 121.0(4) . . ?
C4 C5 C1 117.7(5) . . ?
C4 C5 C7 118.1(4) . . ?
C1 C5 C7 124.1(5) . . ?
O1 C6 N1 121.1(4) . . ?
O1 C6 C4 119.2(4) . . ?
N1 C6 C4 119.6(4) . . ?
O2 C7 N2 120.7(5) . . ?
O2 C7 C5 123.1(5) . . ?
N2 C7 C5 116.1(4) . . ?
C9 C8 C12 118.7(4) . . ?
C8 C9 C10 119.2(5) . . ?
N6 C10 C9 122.7(4) . . ?
N6 C11 C12 122.4(4) . . ?
N6 C11 C13 117.5(4) . . ?
C12 C11 C13 120.0(4) . . ?
C11 C12 C8 118.7(4) . . ?
C11 C12 C14 118.3(4) . . ?
C8 C12 C14 123.0(4) . . ?
N4 C13 O3 121.4(4) . . ?
N4 C13 C11 121.6(4) . . ?
O3 C13 C11 117.0(4) . . ?
O4 C14 N5 121.6(5) . . ?
O4 C14 C12 123.6(5) . . ?
N5 C14 C12 114.8(4) . . ?
O6 C15 O8 126.0(4) . . ?
O6 C15 C16 117.1(4) . . ?
O8 C15 C16 116.9(4) . . ?
O7 C16 O5 125.9(4) . . ?
O7 C16 C15 117.7(4) . . ?
O5 C16 C15 116.4(4) . . ?
C6 N1 N2 119.2(4) . . ?
C6 N1 Zn1 114.7(3) . 11_565 ?
N2 N1 Zn1 126.0(3) . 11_565 ?
C7 N2 N1 126.0(4) . . ?
C3 N3 C4 117.6(4) . . ?
C3 N3 Zn1 131.6(4) . . ?
C4 N3 Zn1 110.1(3) . . ?
C13 N4 N5 117.7(4) . . ?
C14 N5 N4 127.5(4) . . ?
C10 N6 C11 118.3(4) . . ?
C10 N6 Zn2 128.2(3) . . ?
C11 N6 Zn2 113.3(3) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.132
_database_code_depnum_ccdc_archive 'CCDC 976685'
