Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2002

data_global 

_journal_coden_Cambridge      182

loop_
_publ_author_name
'Doedens, Robert J.'
'Khan, M Ishaque'
'Yohannes, Elizabeth'

_publ_contact_author_name	  'Prof Robert J. Doedens'
_publ_contact_author_address
;
Department of Chemistry
University of California
Irvine, California
92697-2025
USA
;
_publ_contact_author_email       'RDOEDENS@UCI.EDU'

_publ_requested_journal		  'Chemical Communications'
_publ_section_title
;
Water clusters in the solid state: a symmetrical, cyclic 
hexamer and an "opened-cube" octamer
;

data_isk16a 

_database_code_CSD	171785


_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'H72 Li6 Ni3 O82 S V18' 
_chemical_formula_weight          2551.33 

loop_ 
_atom_type_symbol 
_atom_type_description 
_atom_type_scat_dispersion_real 
_atom_type_scat_dispersion_imag 
_atom_type_scat_source 
'O'  'O'   0.0106   0.0060 
'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' 
'V'  'V'   0.3005   0.5294 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'Ni'  'Ni'   0.3393   1.1124 
'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' 
'Li'  'Li'  -0.0003   0.0001 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

_symmetry_cell_setting            Cubic 
_symmetry_space_group_name_H-M    Im-3m 

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

_cell_length_a                    15.4344(4) 
_cell_length_b                    15.4344(4) 
_cell_length_c                    15.4344(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      3676.79(17) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     163(2) 
_cell_measurement_reflns_used     8192 
_cell_measurement_theta_min       2.0 
_cell_measurement_theta_max       28.3 

_exptl_crystal_description        Octahedron 
_exptl_crystal_colour             'Deep Green' 
_exptl_crystal_size_max           0.21 
_exptl_crystal_size_mid           0.21 
_exptl_crystal_size_min           0.20 
_exptl_crystal_density_meas       none 
_exptl_crystal_density_diffrn     2.304 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2520 
_exptl_absorpt_coefficient_mu     3.077 
_exptl_absorpt_correction_type    empirical 
_exptl_absorpt_correction_T_min   0.602 
_exptl_absorpt_correction_T_max   0.647 
_exptl_absorpt_process_details    'computed via SADABS'

_exptl_special_details 
; 
Crystal orientation and preliminary unit cell constants were obtained from  
reflections gathered from three sets of 15 frames each, chosen to cover a 
wide range of reciprocal space.  Refined cell parameters were computed after 
data collection on the basis of the setting angles of 8192 reflections with 
a resolution limit of 0.75 Angstroms.
; 

_diffrn_ambient_temperature       163(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'normal focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Bruker SMART system'
_diffrn_measurement_method        '20s frames at 0.3 deg increments in \w' 
_diffrn_standards_number          n/a 
_diffrn_standards_interval_count  n/a 
_diffrn_standards_interval_time   n/a
_diffrn_standards_decay_%         0 
_diffrn_reflns_number             12057 
_diffrn_reflns_av_R_equivalents   0.0206 
_diffrn_reflns_av_sigmaI/netI     0.0081 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        20 
_diffrn_reflns_limit_k_min        -20 
_diffrn_reflns_limit_k_max        20 
_diffrn_reflns_limit_l_min        -19 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          1.87 
_diffrn_reflns_theta_max          28.30 

_diffrn_special_details
;
A hemisphere of data was collected by use of 0.3 degree omega increments 
and 20s frame counting times.  The first 50 frames were remeasured at the
end of data collection and no evidence of decay was observed.  To a limiting 
resolution of 0.75 A, the completeness of coverage was 100.0%, the average 
redundancy was 21.3, and R(sym) for the uncorrected data was 0.030.
;

_reflns_number_total              488 
_reflns_number_gt                 484 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SMART/SAINT' 
_computing_data_reduction         'Bruker SAINT/SHELXTL'
_computing_structure_solution     'Bruker SHELXTL' 
_computing_structure_refinement   'Bruker SHELXTL' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 

_refine_special_details 
; 
Only the hydrogen atoms on O5 were included in the refinement.  Space group 
symmetry requires twofold disorder of H5B and also of oxygen atom O4.  Atoms 
O6 and Li1 are also disordered.
; 

_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
'w=1/[\s^2^(Fo^2^)+(0.065P)^2^+32.0P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    difmap
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        n/a
_refine_ls_number_reflns          488 
_refine_ls_number_parameters      41 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0353 
_refine_ls_R_factor_gt            0.0349 
_refine_ls_wR_factor_ref          0.1271 
_refine_ls_wR_factor_gt           0.1267 
_refine_ls_goodness_of_fit_ref    1.218 
_refine_ls_restrained_S_all       1.218 
_refine_ls_shift/su_max           0.049 
_refine_ls_shift/su_mean          0.008 

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 
Ni1 Ni 0.5000 0.0000 0.0000 0.0190(4) Uani 1 16 d S . . 
V1 V 0.16744(4) 0.16744(4) 0.0000 0.0068(3) Uani 1 4 d S . . 
V2 V 0.25927(10) 0.0000 0.0000 0.0113(4) Uani 1 8 d S . . 
S1 S 0.0000 0.0000 0.0000 0.0048(8) Uiso 1 48 d S . . 
O1 O 0.08292(16) 0.08292(16) 0.2119(2) 0.0197(8) Uani 1 2 d S . . 
O2 O 0.2403(2) 0.2403(2) 0.0000 0.0145(9) Uani 1 4 d S . . 
O3 O 0.3653(4) 0.0000 0.0000 0.0185(14) Uani 1 8 d S . . 
O4 O 0.0551(4) 0.0551(4) 0.0551(4) 0.0099(19) Uani 0.50 6 d SP . . 
O5 O 0.33896(17) 0.33896(17) 0.1444(2) 0.0211(7) Uani 1 2 d S . . 
O6A O 0.5000 -0.1175(6) -0.0632(6) 0.0176(17) Uiso 0.38 2 d SP . . 
O6B O 0.5000 -0.0930(9) -0.0930(9) 0.017(4) Uiso 0.24 4 d SP . . 
H5A H 0.3624 0.3624 0.1889 0.032 Uiso 1 2 d S . . 
H5B H 0.3436 0.2812 0.1519 0.032 Uiso 0.50 1 d P . . 
Li1 Li 0.5000 -0.250(3) -0.048(3) 0.028(7) Uiso 0.25 2 d SP . . 

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 
Ni1 0.0110(8) 0.0230(6) 0.0230(6) 0.000 0.000 0.000 
V1 0.0065(4) 0.0065(4) 0.0075(5) 0.000 0.000 -0.0020(3) 
V2 0.0067(7) 0.0136(5) 0.0136(5) 0.000 0.000 0.000 
O1 0.0147(10) 0.0147(10) 0.030(2) 0.0119(10) 0.0119(10) 0.0092(12) 
O2 0.0119(13) 0.0119(13) 0.020(2) 0.000 0.000 -0.0043(16) 
O3 0.007(3) 0.024(2) 0.024(2) 0.000 0.000 0.000 
O4 0.0099(19) 0.0099(19) 0.0099(19) -0.001(2) -0.001(2) -0.001(2) 
O5 0.0224(11) 0.0224(11) 0.0184(17) -0.0051(10) -0.0051(10) -0.0029(14) 

_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 
Ni1 O3  2.079(7) . y
Ni1 O6B 2.03(2) 49_655 ? 
Ni1 O6B 2.03(2) . y 
Ni1 O6B 2.03(2) 50 ? 
Ni1 O6B 2.03(2) 2_655 ? 
Ni1 O6A 2.060(9) 66 ? 
Ni1 O6A 2.060(9) 49_655 ? 
Ni1 O6A 2.060(9) . y 
Ni1 O6A 2.060(9) 2_655 ? 
Ni1 O6A 2.060(9) 17 ? 
Ni1 O6A 2.060(9) 18_655 ? 
Ni1 O6A 2.060(9) 50 ? 
Ni1 O6A 2.060(9) 65_655 ? 
V1 O2 1.590(4) . y 
V1 O1 1.9523(13) 9 ? 
V1 O1 1.9523(13) 5 y 
V1 O1 1.9523(13) 60 ? 
V1 O1 1.9524(13) 55 ? 
V1 O4 2.596(6) . ? 
V1 V2 2.9475(8) 5 ? 
V1 V2 2.9475(8) . y 
V2 O3 1.636(7) . y 
V2 O1 1.952(3) 5 y 
V2 O1 1.952(3) 56 ? 
V2 O1 1.952(3) 55 ? 
V2 O1 1.952(3) 6 ? 
V2 V1 2.9475(8) 51 ? 
V2 V1 2.9475(8) 11 ? 
V2 V1 2.9475(8) 9 ? 
V2 O4 3.373(3) . ? 
S1 O4 1.473(10) . y 
S1 O4 1.473(10) 52 ? 
S1 O4 1.473(10) 3 ? 
S1 O4 1.473(10) 50 ? 
S1 O4 1.473(10) 49 ? 
S1 O4 1.473(10) 2 ? 
S1 O4 1.473(10) 51 ? 
S1 O4 1.473(10) 4 ? 
O1 V2 1.952(3) 9 ? 
O1 V1 1.9523(13) 5 ? 
O1 V1 1.9523(13) 9 ? 
O1 O4 2.496(8) . ? 
O4 O4 1.700(12) 52 ? 
O4 O4 1.700(12) 50 ? 
O4 O4 1.700(12) 51 ? 
O6A O6B 0.595(10) . ? 
O6A O6A 1.19(2) 18_655 ? 
O6A Li1 2.06(4) . ? 
O6A Li1 2.39(4) 46_544 y 
O6A Li1 2.39(4) 93_544 ? 
O6B O6A 0.595(10) 18_655 ? 
O6B Li1 2.52(4) . y 
O6B Li1 2.52(4) 18_655 ? 
Li1 Li1 1.06(6) 93_544 ? 
Li1 Li1 1.06(6) 46_544 ? 
Li1 Li1 1.49(8) 50 ? 
Li1 O6A 2.39(4) 46_544 ? 
Li1 O6A 2.39(4) 93_544 ? 

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 
O6B Ni1 O6B 180.0(12) 49_655 . ? 
O6B Ni1 O6B 90.0 49_655 50 ? 
O6B Ni1 O6B 90.0 . 50 ? 
O6B Ni1 O6B 90.0 49_655 2_655 ? 
O6B Ni1 O6B 90.0 . 2_655 ? 
O6B Ni1 O6B 180.0(12) 50 2_655 ? 
O6B Ni1 O6A 16.7(3) 49_655 66 ? 
O6B Ni1 O6A 163.3(3) . 66 ? 
O6B Ni1 O6A 73.3(3) 50 66 ? 
O6B Ni1 O6A 106.7(3) 2_655 66 ? 
O6B Ni1 O6A 16.7(3) 49_655 49_655 ? 
O6B Ni1 O6A 163.3(3) . 49_655 ? 
O6B Ni1 O6A 106.7(3) 50 49_655 ? 
O6B Ni1 O6A 73.3(3) 2_655 49_655 ? 
O6A Ni1 O6A 33.4(6) 66 49_655 ? 
O6B Ni1 O6A 163.3(3) 49_655 . ? 
O6B Ni1 O6A 16.7(3) . . ? 
O6B Ni1 O6A 73.3(3) 50 . ? 
O6B Ni1 O6A 106.7(3) 2_655 . ? 
O6A Ni1 O6A 146.6(6) 66 . ? 
O6A Ni1 O6A 180.0(5) 49_655 . ? 
O6B Ni1 O6A 73.3(3) 49_655 2_655 ? 
O6B Ni1 O6A 106.7(3) . 2_655 ? 
O6B Ni1 O6A 163.3(3) 50 2_655 ? 
O6B Ni1 O6A 16.7(3) 2_655 2_655 ? 
O6A Ni1 O6A 90.0 66 2_655 ? 
O6A Ni1 O6A 56.6(6) 49_655 2_655 ? 
O6A Ni1 O6A 123.4(6) . 2_655 ? 
O6B Ni1 O6A 73.3(3) 49_655 17 ? 
O6B Ni1 O6A 106.7(3) . 17 ? 
O6B Ni1 O6A 16.7(3) 50 17 ? 
O6B Ni1 O6A 163.3(3) 2_655 17 ? 
O6A Ni1 O6A 56.6(6) 66 17 ? 
O6A Ni1 O6A 90.0 49_655 17 ? 
O6A Ni1 O6A 90.0 . 17 ? 
O6A Ni1 O6A 146.6(6) 2_655 17 ? 
O6B Ni1 O6A 163.3(3) 49_655 18_655 ? 
O6B Ni1 O6A 16.7(3) . 18_655 ? 
O6B Ni1 O6A 106.7(3) 50 18_655 ? 
O6B Ni1 O6A 73.3(3) 2_655 18_655 ? 
O6A Ni1 O6A 180.0(5) 66 18_655 ? 
O6A Ni1 O6A 146.6(6) 49_655 18_655 ? 
O6A Ni1 O6A 33.4(6) . 18_655 ? 
O6A Ni1 O6A 90.0 2_655 18_655 ? 
O6A Ni1 O6A 123.4(6) 17 18_655 ? 
O6B Ni1 O6A 106.7(3) 49_655 50 ? 
O6B Ni1 O6A 73.3(3) . 50 ? 
O6B Ni1 O6A 16.7(3) 50 50 ? 
O6B Ni1 O6A 163.3(3) 2_655 50 ? 
O6A Ni1 O6A 90.0 66 50 ? 
O6A Ni1 O6A 123.4(6) 49_655 50 ? 
O6A Ni1 O6A 56.6(6) . 50 ? 
O6A Ni1 O6A 180.0(5) 2_655 50 ? 
O6A Ni1 O6A 33.4(6) 17 50 ? 
O6A Ni1 O6A 90.0 18_655 50 ? 
O6B Ni1 O6A 106.7(3) 49_655 65_655 ? 
O6B Ni1 O6A 73.3(3) . 65_655 ? 
O6B Ni1 O6A 163.3(3) 50 65_655 ? 
O6B Ni1 O6A 16.7(3) 2_655 65_655 ? 
O6A Ni1 O6A 123.4(6) 66 65_655 ? 
O6A Ni1 O6A 90.0 49_655 65_655 ? 
O6A Ni1 O6A 90.0 . 65_655 ? 
O6A Ni1 O6A 33.4(6) 2_655 65_655 ? 
O6A Ni1 O6A 180.0(5) 17 65_655 ? 
O6A Ni1 O6A 56.6(6) 18_655 65_655 ? 
O6A Ni1 O6A 146.6(6) 50 65_655 ? 
O2 V1 O1 102.93(11) . 9 ? 
O2 V1 O1 102.93(11) . 5 ? 
O1 V1 O1 92.32(18) 9 5 ? 
O2 V1 O1 102.93(11) . 60 ? 
O1 V1 O1 81.92(19) 9 60 ? 
O1 V1 O1 154.1(2) 5 60 ? 
O2 V1 O1 102.93(11) . 55 ? 
O1 V1 O1 154.1(2) 9 55 ? 
O1 V1 O1 81.92(19) 5 55 ? 
O1 V1 O1 92.32(18) 60 55 ? 
O2 V1 O4 160.88(18) . . ? 
O1 V1 O4 64.78(15) 9 . ? 
O1 V1 O4 64.78(15) 5 . ? 
O1 V1 O4 90.19(18) 60 . ? 
O1 V1 O4 90.19(18) 55 . ? 
O2 V1 V2 106.26(3) . 5 ? 
O1 V1 V2 40.97(9) 9 5 ? 
O1 V1 V2 129.03(10) 5 5 ? 
O1 V1 V2 40.97(9) 60 5 ? 
O1 V1 V2 129.03(10) 55 5 ? 
O4 V1 V2 74.66(3) . 5 ? 
O2 V1 V2 106.26(3) . . ? 
O1 V1 V2 129.03(10) 9 . ? 
O1 V1 V2 40.97(9) 5 . ? 
O1 V1 V2 129.03(10) 60 . ? 
O1 V1 V2 40.97(9) 55 . ? 
O4 V1 V2 74.66(3) . . ? 
V2 V1 V2 147.48(6) 5 . ? 
O3 V2 O1 111.98(12) . 5 ? 
O3 V2 O1 111.98(12) . 56 ? 
O1 V2 O1 81.95(9) 5 56 ? 
O3 V2 O1 111.98(12) . 55 ? 
O1 V2 O1 81.95(9) 5 55 ? 
O1 V2 O1 136.0(2) 56 55 ? 
O3 V2 O1 111.98(12) . 6 ? 
O1 V2 O1 136.0(2) 5 6 ? 
O1 V2 O1 81.95(9) 56 6 ? 
O1 V2 O1 81.95(9) 55 6 ? 
O3 V2 V1 118.74(3) . 51 ? 
O1 V2 V1 113.26(10) 5 51 ? 
O1 V2 V1 40.98(4) 56 51 ? 
O1 V2 V1 113.26(10) 55 51 ? 
O1 V2 V1 40.98(4) 6 51 ? 
O3 V2 V1 118.74(3) . 11 ? 
O1 V2 V1 113.26(10) 5 11 ? 
O1 V2 V1 113.26(10) 56 11 ? 
O1 V2 V1 40.98(4) 55 11 ? 
O1 V2 V1 40.98(4) 6 11 ? 
V1 V2 V1 76.63(3) 51 11 ? 
O3 V2 V1 118.74(3) . 9 ? 
O1 V2 V1 40.98(4) 5 9 ? 
O1 V2 V1 40.98(4) 56 9 ? 
O1 V2 V1 113.26(10) 55 9 ? 
O1 V2 V1 113.26(10) 6 9 ? 
V1 V2 V1 76.63(3) 51 9 ? 
V1 V2 V1 122.52(6) 11 9 ? 
O3 V2 V1 118.74(3) . . ? 
O1 V2 V1 40.98(4) 5 . ? 
O1 V2 V1 113.26(10) 56 . ? 
O1 V2 V1 40.98(4) 55 . ? 
O1 V2 V1 113.26(10) 6 . ? 
V1 V2 V1 122.52(6) 51 . ? 
V1 V2 V1 76.63(3) 11 . ? 
V1 V2 V1 76.63(3) 9 . ? 
O3 V2 O4 159.12(17) . . ? 
O1 V2 O4 47.1(2) 5 . ? 
O1 V2 O4 69.53(12) 56 . ? 
O1 V2 O4 69.53(12) 55 . ? 
O1 V2 O4 88.9(2) 6 . ? 
V1 V2 O4 76.81(13) 51 . ? 
V1 V2 O4 76.81(13) 11 . ? 
V1 V2 O4 47.91(9) 9 . ? 
V1 V2 O4 47.91(9) . . ? 
O4 S1 O4 70.5 . 52 ? 
O4 S1 O4 109.5 . 3 ? 
O4 S1 O4 70.5 52 3 ? 
O4 S1 O4 70.5 . 50 ? 
O4 S1 O4 109.5 52 50 ? 
O4 S1 O4 70.5 3 50 ? 
O4 S1 O4 180.0(11) . 49 ? 
O4 S1 O4 109.5 52 49 ? 
O4 S1 O4 70.5 3 49 ? 
O4 S1 O4 109.5 50 49 ? 
O4 S1 O4 109.5 . 2 ? 
O4 S1 O4 70.5 52 2 ? 
O4 S1 O4 109.5 3 2 ? 
O4 S1 O4 180.0(11) 50 2 ? 
O4 S1 O4 70.5 49 2 ? 
O4 S1 O4 70.5 . 51 ? 
O4 S1 O4 109.5 52 51 ? 
O4 S1 O4 180.0(11) 3 51 ? 
O4 S1 O4 109.5 50 51 ? 
O4 S1 O4 109.5 49 51 ? 
O4 S1 O4 70.5 2 51 ? 
O4 S1 O4 109.5 . 4 ? 
O4 S1 O4 180.0(11) 52 4 ? 
O4 S1 O4 109.5 3 4 ? 
O4 S1 O4 70.5 50 4 ? 
O4 S1 O4 70.5 49 4 ? 
O4 S1 O4 109.5 2 4 ? 
O4 S1 O4 70.5 51 4 ? 
V2 O1 V1 98.05(11) 9 5 ? 
V2 O1 V1 98.05(11) 9 9 ? 
V1 O1 V1 138.8(2) 5 9 ? 
V2 O1 O4 97.9(2) 9 . ? 
V1 O1 O4 70.18(11) 5 . ? 
V1 O1 O4 70.18(11) 9 . ? 
V2 O3 Ni1 180.0 . . ? 
S1 O4 O4 54.738(1) . 52 ? 
S1 O4 O4 54.734(1) . 50 ? 
O4 O4 O4 90.0 52 50 ? 
S1 O4 O4 54.734(1) . 51 ? 
O4 O4 O4 90.0 52 51 ? 
O4 O4 O4 90.0 50 51 ? 
S1 O4 O1 139.35(16) . . ? 
O4 O4 O1 99.91(11) 52 . ? 
O4 O4 O1 165.91(16) 50 . ? 
O4 O4 O1 99.91(11) 51 . ? 
S1 O4 V1 125.61(18) . . ? 
O4 O4 V1 131.92(6) 52 . ? 
O4 O4 V1 70.88(18) 50 . ? 
O4 O4 V1 131.92(6) 51 . ? 
O1 O4 V1 95.0(3) . . ? 
S1 O4 V2 104.38(17) . . ? 
O4 O4 V2 159.12(17) 52 . ? 
O4 O4 V2 75.40(11) 50 . ? 
O4 O4 V2 75.40(11) 51 . ? 
O1 O4 V2 97.3(2) . . ? 
V1 O4 V2 57.43(7) . . ? 
O6B O6A O6A 6(2) . 18_655 ? 
O6B O6A Li1 136(3) . . ? 
O6A O6A Li1 141.4(12) 18_655 . ? 
O6B O6A Ni1 79(2) . . ? 
O6A O6A Ni1 73.3(3) 18_655 . ? 
Li1 O6A Ni1 145.3(13) . . ? 
O6B O6A Li1 149(2) . 46_544 ? 
O6A O6A Li1 153.6(7) 18_655 46_544 ? 
Li1 O6A Li1 26.2(15) . 46_544 ? 
Ni1 O6A Li1 124.1(7) . 46_544 ? 
O6B O6A Li1 149(2) . 93_544 ? 
O6A O6A Li1 153.6(7) 18_655 93_544 ? 
Li1 O6A Li1 26.2(15) . 93_544 ? 
Ni1 O6A Li1 124.1(7) . 93_544 ? 
Li1 O6A Li1 36(2) 46_544 93_544 ? 
O6A O6B O6A 169(5) 18_655 . ? 
O6A O6B Ni1 84(2) 18_655 . ? 
O6A O6B Ni1 84(2) . . ? 
O6A O6B Li1 156(3) 18_655 . ? 
O6A O6B Li1 35(2) . . ? 
Ni1 O6B Li1 119.1(10) . . ? 
O6A O6B Li1 35(2) 18_655 18_655 ? 
O6A O6B Li1 156(3) . 18_655 ? 
Ni1 O6B Li1 119.1(10) . 18_655 ? 
Li1 O6B Li1 122(2) . 18_655 ? 
Li1 Li1 Li1 90.000(14) 93_544 46_544 ? 
Li1 Li1 Li1 45.000(9) 93_544 50 ? 
Li1 Li1 Li1 45.000(11) 46_544 50 ? 
Li1 Li1 O6A 95(5) 93_544 . ? 
Li1 Li1 O6A 95(5) 46_544 . ? 
Li1 Li1 O6A 96.4(12) 50 . ? 
Li1 Li1 O6A 94(4) 93_544 46_544 ? 
Li1 Li1 O6A 59(4) 46_544 46_544 ? 
Li1 Li1 O6A 71.8(10) 50 46_544 ? 
O6A Li1 O6A 152.5(10) . 46_544 ? 
Li1 Li1 O6A 59(4) 93_544 93_544 ? 
Li1 Li1 O6A 94(4) 46_544 93_544 ? 
Li1 Li1 O6A 71.8(10) 50 93_544 ? 
O6A Li1 O6A 152.5(10) . 93_544 ? 
O6A Li1 O6A 48.3(9) 46_544 93_544 ? 
Li1 Li1 O6B 101(5) 93_544 . ? 
Li1 Li1 O6B 101(5) 46_544 . ? 
Li1 Li1 O6B 105.9(10) 50 . ? 
O6A Li1 O6B 9.5(6) . . ? 
O6A Li1 O6B 155.5(6) 46_544 . ? 
O6A Li1 O6B 155.5(6) 93_544 . ? 

_diffrn_measured_fraction_theta_max    0.996 
_diffrn_reflns_theta_full              28.30 
_diffrn_measured_fraction_theta_full   0.996 
_refine_diff_density_max    0.582 
_refine_diff_density_min   -2.153 
_refine_diff_density_rms    0.153 

#===END

data_isk34 

_database_code_CSD	171786


_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C24 H24 N4 O8.50 S V' 
_chemical_formula_weight          587.47 

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' 
'S'  'S'   0.1246   0.1234 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'V'  'V'   0.3005   0.5294 
'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/c 

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

_cell_length_a                    21.2997(12) 
_cell_length_b                    14.1986(8) 
_cell_length_c                    16.3825(9) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  98.0460(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      4905.7(5) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     158(2) 
_cell_measurement_reflns_used     7348 
_cell_measurement_theta_min       2.21 
_cell_measurement_theta_max       28.0 

_exptl_crystal_description        'thin plate' 
_exptl_crystal_colour             'dark purple' 
_exptl_crystal_size_max           0.31 
_exptl_crystal_size_mid           0.25 
_exptl_crystal_size_min           0.06 
_exptl_crystal_density_meas       'not measured' 
_exptl_crystal_density_diffrn     1.591 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2424 
_exptl_absorpt_coefficient_mu     0.551 
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.8478 
_exptl_absorpt_correction_T_max   0.9677 
_exptl_absorpt_process_details    'computed via SADABS' 

_exptl_special_details 

; 
Crystal orientation and preliminary unit cell constants were obtained from  
reflections gathered from three sets of 15 frames each, chosen to cover a 
wide range of reciprocal space.  Refined cell parameters were computed after 
data collection on the basis of the setting angles of 7348 reflections with 
a resolution limit of 0.75 Angstroms.
; 

_diffrn_ambient_temperature       158(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'normal-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'CCD area detector' 
_diffrn_measurement_method        '25s frames at 0.3 deg omega increments' 
_diffrn_standards_number          n/a 
_diffrn_standards_interval_count  n/a 
_diffrn_standards_interval_time   n/a 
_diffrn_standards_decay_%         none 
_diffrn_reflns_number             25833 
_diffrn_reflns_av_R_equivalents   0.0382 
_diffrn_reflns_av_sigmaI/netI     0.0342 
_diffrn_reflns_limit_h_min        -28 
_diffrn_reflns_limit_h_max        28 
_diffrn_reflns_limit_k_min        -18 
_diffrn_reflns_limit_k_max        18 
_diffrn_reflns_limit_l_min        -21 
_diffrn_reflns_limit_l_max        21 
_diffrn_reflns_theta_min          1.73 
_diffrn_reflns_theta_max          28.29 

_diffrn_special_details
;
A full sphere of data was collected by use of 0.3 degree omega increments 
and 25s frame counting times.  The first 50 frames were remeasured at the
end of data collection and no evidence of decay was observed.  To a limiting 
resolution of 0.75 A, the completeness of coverage was 98.1%, the average 
redundancy was 4.3, and R(sym) for the uncorrected data was 0.061.
;

_reflns_number_total              5962 
_reflns_number_gt                 4727 
_reflns_threshold_expression      >2sigma(I) 

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

_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
'w=1/[\s^2^(Fo^2^)+(0.045P)^2^+8.5P] where P=(Fo^2^+2Fc^2^)/3' 

_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        n/a 
_refine_ls_number_reflns          5962 
_refine_ls_number_parameters      380 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0548 
_refine_ls_R_factor_gt            0.0393 
_refine_ls_wR_factor_ref          0.1042 
_refine_ls_wR_factor_gt           0.0952 
_refine_ls_goodness_of_fit_ref    1.046 
_refine_ls_restrained_S_all       1.046 
_refine_ls_shift/su_max           0.004 
_refine_ls_shift/su_mean          0.000 
_refine_diff_density_max    0.620 
_refine_diff_density_min   -0.456 
_refine_diff_density_rms    0.070 

_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. 
Hydrogen atoms of the aromatic rings were included at idealized positions.  
Water hydrogen atoms were located on a difference Fourier map and and moved 
along their bond vectors to idealized O-H distances of 0.86 Angstroms.  
Refinement of all hydrogen atoms was carried out by use of the riding model.
; 

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 
V1 V 0.449116(15) 0.74150(2) 0.15421(2) 0.01526(10) Uani 1 1 d . . . 
S2 S 0.33491(2) 0.57661(4) 0.16533(3) 0.01936(12) Uani 1 1 d . . . 
O1 O 0.5000 0.73623(13) 0.2500 0.0158(4) Uani 1 2 d S . . 
O2 O 0.39628(7) 0.62976(11) 0.17073(9) 0.0247(3) Uani 1 1 d . . . 
O3 O 0.30533(8) 0.57644(13) 0.07929(10) 0.0341(4) Uani 1 1 d . . . 
O4 O 0.35073(8) 0.48159(12) 0.19501(11) 0.0345(4) Uani 1 1 d . . . 
O5 O 0.29461(8) 0.62426(12) 0.21788(10) 0.0314(4) Uani 1 1 d . . . 
O6 O 0.33049(10) 0.30223(15) 0.14405(13) 0.0364(4) Uani 1 1 d . . . 
H6B H 0.3333(13) 0.358(2) 0.1514(17) 0.035(8) Uiso 1 1 d . . . 
H6C H 0.3371(14) 0.294(2) 0.104(2) 0.036(9) Uiso 1 1 d . . . 
O7 O 0.15649(9) 0.27428(15) 0.01058(12) 0.0349(4) Uani 1 1 d . . . 
H7B H 0.1798(15) 0.245(2) 0.050(2) 0.048(9) Uiso 1 1 d . . . 
H7C H 0.1764(15) 0.319(3) 0.015(2) 0.049(11) Uiso 1 1 d . . . 
O8 O 0.23500(9) 0.16971(15) 0.12899(11) 0.0351(4) Uani 1 1 d . . . 
H8B H 0.2217(14) 0.147(2) 0.172(2) 0.045(9) Uiso 1 1 d . . . 
H8C H 0.2599(16) 0.209(3) 0.141(2) 0.052(10) Uiso 1 1 d . . . 
O9 O 0.21526(10) 0.45403(17) -0.01122(15) 0.0438(5) Uani 1 1 d . . . 
H9B H 0.2395(18) 0.480(3) 0.015(2) 0.061(12) Uiso 1 1 d . . . 
H9C H 0.2337(15) 0.433(2) -0.045(2) 0.043(10) Uiso 1 1 d . . . 
N1 N 0.49337(8) 0.86970(12) 0.12165(10) 0.0173(3) Uani 1 1 d . . . 
N2 N 0.38809(8) 0.84645(12) 0.19278(10) 0.0182(3) Uani 1 1 d . . . 
N3 N 0.50964(8) 0.65922(12) 0.09052(10) 0.0170(3) Uani 1 1 d . . . 
N4 N 0.40179(8) 0.74527(12) 0.02680(10) 0.0184(3) Uani 1 1 d . . . 
C1 C 0.54651(10) 0.87981(15) 0.08782(13) 0.0214(4) Uani 1 1 d . . . 
H1A H 0.5676 0.8250 0.0725 0.026 Uiso 1 1 calc R . . 
C2 C 0.57245(10) 0.96847(16) 0.07405(13) 0.0253(5) Uani 1 1 d . . . 
H2A H 0.6103 0.9730 0.0498 0.030 Uiso 1 1 calc R . . 
C3 C 0.54277(11) 1.04801(16) 0.09573(13) 0.0260(5) Uani 1 1 d . . . 
H3A H 0.5599 1.1082 0.0866 0.031 Uiso 1 1 calc R . . 
C4 C 0.48654(10) 1.04046(15) 0.13174(13) 0.0220(4) Uani 1 1 d . . . 
C5 C 0.45167(11) 1.11955(16) 0.15589(14) 0.0288(5) Uani 1 1 d . . . 
H5A H 0.4659 1.1815 0.1463 0.035 Uiso 1 1 calc R . . 
C6 C 0.39912(11) 1.10791(16) 0.19187(15) 0.0290(5) Uani 1 1 d . . . 
H6A H 0.3773 1.1617 0.2079 0.035 Uiso 1 1 calc R . . 
C7 C 0.37554(10) 1.01565(15) 0.20635(13) 0.0233(4) Uani 1 1 d . . . 
C8 C 0.32125(11) 0.99918(17) 0.24488(15) 0.0297(5) Uani 1 1 d . . . 
H8A H 0.2981 1.0506 0.2629 0.036 Uiso 1 1 calc R . . 
C9 C 0.30228(11) 0.90900(17) 0.25597(15) 0.0302(5) Uani 1 1 d . . . 
H9A H 0.2659 0.8973 0.2819 0.036 Uiso 1 1 calc R . . 
C10 C 0.33653(10) 0.83359(17) 0.22909(14) 0.0257(5) Uani 1 1 d . . . 
H10A H 0.3225 0.7712 0.2370 0.031 Uiso 1 1 calc R . . 
C11 C 0.40765(9) 0.93675(14) 0.18171(12) 0.0181(4) Uani 1 1 d . . . 
C12 C 0.46377(10) 0.94919(14) 0.14370(12) 0.0180(4) Uani 1 1 d . . . 
C13 C 0.56297(9) 0.61622(15) 0.12397(13) 0.0201(4) Uani 1 1 d . . . 
H13A H 0.5755 0.6208 0.1818 0.024 Uiso 1 1 calc R . . 
C14 C 0.60086(10) 0.56487(15) 0.07692(14) 0.0232(4) Uani 1 1 d . . . 
H14A H 0.6383 0.5349 0.1029 0.028 Uiso 1 1 calc R . . 
C15 C 0.58413(10) 0.55772(15) -0.00648(14) 0.0240(5) Uani 1 1 d . . . 
H15A H 0.6100 0.5234 -0.0388 0.029 Uiso 1 1 calc R . . 
C16 C 0.52763(10) 0.60215(15) -0.04427(13) 0.0206(4) Uani 1 1 d . . . 
C17 C 0.50462(11) 0.59560(16) -0.13053(13) 0.0262(5) Uani 1 1 d . . . 
H17A H 0.5289 0.5630 -0.1659 0.031 Uiso 1 1 calc R . . 
C18 C 0.44857(11) 0.63542(16) -0.16238(13) 0.0271(5) Uani 1 1 d . . . 
H18A H 0.4339 0.6294 -0.2196 0.033 Uiso 1 1 calc R . . 
C19 C 0.41104(10) 0.68646(15) -0.11107(13) 0.0224(4) Uani 1 1 d . . . 
C20 C 0.35177(11) 0.72792(17) -0.13994(14) 0.0285(5) Uani 1 1 d . . . 
H20A H 0.3341 0.7222 -0.1963 0.034 Uiso 1 1 calc R . . 
C21 C 0.31982(11) 0.77654(18) -0.08620(15) 0.0298(5) Uani 1 1 d . . . 
H21A H 0.2800 0.8048 -0.1050 0.036 Uiso 1 1 calc R . . 
C22 C 0.34657(10) 0.78413(16) -0.00326(14) 0.0252(5) Uani 1 1 d . . . 
H22A H 0.3242 0.8186 0.0332 0.030 Uiso 1 1 calc R . . 
C23 C 0.43354(9) 0.69582(14) -0.02629(12) 0.0178(4) Uani 1 1 d . . . 
C24 C 0.49192(9) 0.65191(14) 0.00734(12) 0.0172(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 
V1 0.01524(17) 0.01578(18) 0.01567(16) 0.00011(12) 0.00534(12) 0.00100(13) 
S2 0.0177(2) 0.0194(3) 0.0219(3) -0.00324(19) 0.00622(19) -0.00293(19) 
O1 0.0178(9) 0.0150(10) 0.0159(9) 0.000 0.0064(7) 0.000 
O2 0.0197(7) 0.0257(8) 0.0295(8) 0.0002(6) 0.0064(6) -0.0058(6) 
O3 0.0313(9) 0.0410(10) 0.0285(9) -0.0079(7) -0.0017(7) -0.0003(8) 
O4 0.0367(10) 0.0228(9) 0.0448(10) 0.0042(7) 0.0085(8) -0.0018(7) 
O5 0.0297(9) 0.0325(9) 0.0360(9) -0.0081(7) 0.0185(7) -0.0032(7) 
O6 0.0541(12) 0.0240(10) 0.0330(11) -0.0009(8) 0.0123(9) -0.0052(9) 
O7 0.0332(10) 0.0338(11) 0.0390(11) 0.0019(8) 0.0094(8) 0.0009(9) 
O8 0.0356(10) 0.0414(11) 0.0294(9) 0.0016(8) 0.0084(8) -0.0086(9) 
O9 0.0368(11) 0.0534(13) 0.0420(12) -0.0149(10) 0.0086(10) -0.0137(10) 
N1 0.0174(8) 0.0177(9) 0.0175(8) 0.0011(6) 0.0046(6) 0.0006(7) 
N2 0.0172(8) 0.0189(9) 0.0192(8) -0.0007(7) 0.0056(7) 0.0017(7) 
N3 0.0170(8) 0.0166(8) 0.0183(8) -0.0010(6) 0.0059(6) -0.0011(6) 
N4 0.0169(8) 0.0181(9) 0.0207(8) 0.0016(7) 0.0048(7) -0.0007(7) 
C1 0.0214(10) 0.0225(11) 0.0215(10) 0.0016(8) 0.0072(8) -0.0003(8) 
C2 0.0225(11) 0.0302(12) 0.0241(11) 0.0028(9) 0.0058(9) -0.0061(9) 
C3 0.0308(12) 0.0236(12) 0.0234(11) 0.0038(9) 0.0029(9) -0.0094(9) 
C4 0.0260(11) 0.0185(10) 0.0208(10) 0.0019(8) 0.0005(8) -0.0022(8) 
C5 0.0385(13) 0.0148(10) 0.0318(12) 0.0013(9) 0.0008(10) -0.0006(9) 
C6 0.0352(13) 0.0172(11) 0.0341(12) -0.0028(9) 0.0035(10) 0.0078(9) 
C7 0.0248(11) 0.0203(11) 0.0247(11) -0.0019(8) 0.0028(9) 0.0054(9) 
C8 0.0257(12) 0.0282(12) 0.0362(13) -0.0058(10) 0.0076(10) 0.0100(10) 
C9 0.0204(11) 0.0340(13) 0.0392(13) -0.0051(10) 0.0147(10) 0.0018(10) 
C10 0.0209(10) 0.0258(12) 0.0324(12) -0.0030(9) 0.0109(9) -0.0005(9) 
C11 0.0175(9) 0.0176(10) 0.0189(10) 0.0006(7) 0.0013(8) 0.0028(8) 
C12 0.0205(10) 0.0174(10) 0.0159(9) 0.0007(7) 0.0016(8) 0.0016(8) 
C13 0.0189(10) 0.0195(10) 0.0222(10) -0.0005(8) 0.0040(8) 0.0003(8) 
C14 0.0178(10) 0.0188(11) 0.0337(12) -0.0003(9) 0.0058(9) 0.0012(8) 
C15 0.0245(11) 0.0186(11) 0.0318(12) -0.0048(9) 0.0147(9) -0.0019(8) 
C16 0.0228(10) 0.0177(10) 0.0238(10) -0.0022(8) 0.0114(8) -0.0051(8) 
C17 0.0343(12) 0.0244(11) 0.0232(11) -0.0053(9) 0.0153(9) -0.0068(10) 
C18 0.0391(13) 0.0276(12) 0.0157(10) -0.0035(8) 0.0075(9) -0.0078(10) 
C19 0.0264(11) 0.0212(11) 0.0199(10) 0.0018(8) 0.0041(8) -0.0076(9) 
C20 0.0311(12) 0.0329(13) 0.0194(10) 0.0057(9) -0.0038(9) -0.0078(10) 
C21 0.0216(11) 0.0356(13) 0.0306(12) 0.0073(10) -0.0017(9) 0.0003(10) 
C22 0.0213(10) 0.0271(12) 0.0278(11) 0.0030(9) 0.0055(9) 0.0030(9) 
C23 0.0189(9) 0.0170(10) 0.0183(9) 0.0013(7) 0.0055(8) -0.0040(8) 
C24 0.0206(10) 0.0145(9) 0.0175(9) 0.0003(7) 0.0065(8) -0.0038(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 
V1 O1 1.7796(3) . ? 
V1 O2 1.9855(15) . ? 
V1 N3 2.1194(17) . ? 
V1 N2 2.1306(17) . ? 
V1 N1 2.1511(17) . ? 
V1 N4 2.1878(17) . ? 
S2 O4 1.4576(17) . ? 
S2 O3 1.4612(17) . ? 
S2 O5 1.4637(16) . ? 
S2 O2 1.5012(15) . ? 
O1 V1 1.7796(3) 2_655 ? 
N1 C1 1.336(3) . ? 
N1 C12 1.366(3) . ? 
N2 C10 1.333(3) . ? 
N2 C11 1.368(3) . ? 
N3 C13 1.338(3) . ? 
N3 C24 1.366(2) . ? 
N4 C22 1.330(3) . ? 
N4 C23 1.368(3) . ? 
C1 C2 1.406(3) . ? 
C2 C3 1.365(3) . ? 
C3 C4 1.411(3) . ? 
C4 C12 1.407(3) . ? 
C4 C5 1.432(3) . ? 
C5 C6 1.346(3) . ? 
C6 C7 1.434(3) . ? 
C7 C11 1.401(3) . ? 
C7 C8 1.412(3) . ? 
C8 C9 1.362(3) . ? 
C9 C10 1.401(3) . ? 
C11 C12 1.434(3) . ? 
C13 C14 1.397(3) . ? 
C14 C15 1.367(3) . ? 
C15 C16 1.422(3) . ? 
C16 C24 1.404(3) . ? 
C16 C17 1.433(3) . ? 
C17 C18 1.358(3) . ? 
C18 C19 1.435(3) . ? 
C19 C23 1.411(3) . ? 
C19 C20 1.413(3) . ? 
C20 C21 1.372(4) . ? 
C21 C22 1.402(3) . ? 
C23 C24 1.431(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 
O1 V1 O2 97.64(7) . . ? 
O1 V1 N3 94.22(6) . . ? 
O2 V1 N3 91.26(6) . . ? 
O1 V1 N2 95.13(6) . . ? 
O2 V1 N2 97.90(7) . . ? 
N3 V1 N2 165.91(7) . . ? 
O1 V1 N1 91.16(7) . . ? 
O2 V1 N1 170.54(6) . . ? 
N3 V1 N1 91.52(6) . . ? 
N2 V1 N1 77.79(7) . . ? 
O1 V1 N4 169.98(5) . . ? 
O2 V1 N4 87.44(6) . . ? 
N3 V1 N4 76.98(6) . . ? 
N2 V1 N4 92.70(6) . . ? 
N1 V1 N4 84.38(6) . . ? 
O4 S2 O3 111.62(10) . . ? 
O4 S2 O5 111.03(10) . . ? 
O3 S2 O5 111.03(10) . . ? 
O4 S2 O2 106.67(10) . . ? 
O3 S2 O2 108.18(10) . . ? 
O5 S2 O2 108.10(9) . . ? 
V1 O1 V1 175.19(12) . 2_655 ? 
S2 O2 V1 154.04(10) . . ? 
C1 N1 C12 118.05(18) . . ? 
C1 N1 V1 128.32(14) . . ? 
C12 N1 V1 113.52(13) . . ? 
C10 N2 C11 118.22(18) . . ? 
C10 N2 V1 127.71(15) . . ? 
C11 N2 V1 113.98(13) . . ? 
C13 N3 C24 118.31(17) . . ? 
C13 N3 V1 126.16(14) . . ? 
C24 N3 V1 115.52(13) . . ? 
C22 N4 C23 117.89(18) . . ? 
C22 N4 V1 128.98(15) . . ? 
C23 N4 V1 113.03(13) . . ? 
N1 C1 C2 122.5(2) . . ? 
C3 C2 C1 119.5(2) . . ? 
C2 C3 C4 119.8(2) . . ? 
C12 C4 C3 117.2(2) . . ? 
C12 C4 C5 118.8(2) . . ? 
C3 C4 C5 124.0(2) . . ? 
C6 C5 C4 121.3(2) . . ? 
C5 C6 C7 121.1(2) . . ? 
C11 C7 C8 117.4(2) . . ? 
C11 C7 C6 119.1(2) . . ? 
C8 C7 C6 123.5(2) . . ? 
C9 C8 C7 119.5(2) . . ? 
C8 C9 C10 119.9(2) . . ? 
N2 C10 C9 122.2(2) . . ? 
N2 C11 C7 122.77(19) . . ? 
N2 C11 C12 117.45(17) . . ? 
C7 C11 C12 119.78(19) . . ? 
N1 C12 C4 122.91(19) . . ? 
N1 C12 C11 117.18(18) . . ? 
C4 C12 C11 119.90(19) . . ? 
N3 C13 C14 122.36(19) . . ? 
C15 C14 C13 120.0(2) . . ? 
C14 C15 C16 119.25(19) . . ? 
C24 C16 C15 117.25(19) . . ? 
C24 C16 C17 119.2(2) . . ? 
C15 C16 C17 123.54(19) . . ? 
C18 C17 C16 120.9(2) . . ? 
C17 C18 C19 121.1(2) . . ? 
C23 C19 C20 117.0(2) . . ? 
C23 C19 C18 118.9(2) . . ? 
C20 C19 C18 124.0(2) . . ? 
C21 C20 C19 119.7(2) . . ? 
C20 C21 C22 119.3(2) . . ? 
N4 C22 C21 123.1(2) . . ? 
N4 C23 C19 122.97(19) . . ? 
N4 C23 C24 117.33(17) . . ? 
C19 C23 C24 119.69(19) . . ? 
N3 C24 C16 122.79(19) . . ? 
N3 C24 C23 117.06(17) . . ? 
C16 C24 C23 120.13(18) . . ? 

_diffrn_measured_fraction_theta_max    0.980 
_diffrn_reflns_theta_full              28.29 
_diffrn_measured_fraction_theta_full   0.980