# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2007

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182
loop_
_publ_author_name
_publ_author_address
R.Custelcean ''
B.A.Moyer ''
V.Sellin ''

_publ_contact_author_name        'Radu Custelcean'
_publ_contact_author_address     
;
Chemical Sciences Division
Oak Ridge National Laboratory
PO Box 2008 MS-6119
Oak Ridge
Tennessee
37831-6119
UNITED STATES OF AMERICA
;

_publ_contact_author_email       CUSTELCEANR@ORNL.GOV

_publ_section_title              
;
Sulfate separation by selective crystallization of a
urea-functionalized metal-organic framework
;

data_1
_database_code_depnum_ccdc_archive 'CCDC 623115'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H46 N12 Ni O13 S'
_chemical_formula_weight         873.52

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'
Ni Ni 0.3393 1.1124 '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                   13.237(3)
_cell_length_b                   13.908(3)
_cell_length_c                   23.358(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.11(3)
_cell_angle_gamma                90.00
_cell_volume                     4283.0(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1856
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8334
_exptl_absorpt_correction_T_max  0.9830
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            54655
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.54
_diffrn_reflns_theta_max         28.34
_reflns_number_total             10669
_reflns_number_gt                7124
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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 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^)+(0.1540P)^2^+3.8445P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10669
_refine_ls_number_parameters     544
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1153
_refine_ls_R_factor_gt           0.0825
_refine_ls_wR_factor_ref         0.2542
_refine_ls_wR_factor_gt          0.2213
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_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
Ni1 Ni 0.5000 0.0000 0.5000 0.01777(17) Uani 1 2 d S . .
S1 S 0.22540(8) -0.08114(7) 0.25013(4) 0.0283(2) Uani 1 1 d . . .
O1 O -0.1954(2) 0.0947(2) 0.10687(13) 0.0354(7) Uani 1 1 d . . .
N1 N -0.4426(2) 0.3581(2) 0.01316(12) 0.0212(6) Uani 1 1 d . . .
C1 C -0.3828(3) 0.3349(3) 0.05994(14) 0.0223(7) Uani 1 1 d . . .
H1 H -0.3685 0.3833 0.0882 0.027 Uiso 1 1 calc R . .
Ni2 Ni 0.0000 0.0000 0.0000 0.01493(17) Uani 1 2 d S . .
O2 O 0.0162(3) 0.1792(3) 0.37445(15) 0.0560(10) Uani 1 1 d . . .
N2 N -0.2808(3) 0.2334(3) 0.12287(13) 0.0317(8) Uani 1 1 d . . .
H2N H -0.2918 0.2751 0.1500 0.038 Uiso 1 1 calc R . .
C2 C -0.3396(3) 0.2440(3) 0.07048(14) 0.0230(7) Uani 1 1 d . . .
O3 O 0.5169(2) 0.01765(18) 0.41267(11) 0.0235(5) Uani 1 1 d . . .
N3 N -0.1521(4) 0.1849(4) 0.18537(18) 0.0778(19) Uani 1 1 d . . .
H3N H -0.1662 0.2377 0.2039 0.093 Uiso 1 1 calc R . .
C3 C -0.3580(3) 0.1734(3) 0.02875(16) 0.0282(8) Uani 1 1 d . . .
H3 H -0.3290 0.1111 0.0335 0.034 Uiso 1 1 calc R . .
O4 O 0.6891(2) 0.1018(2) 0.38725(12) 0.0298(6) Uani 1 1 d . . .
N4 N 0.0202(4) 0.0788(4) 0.29868(18) 0.0685(16) Uani 1 1 d . . .
H4N H 0.0522 0.0315 0.2829 0.082 Uiso 1 1 calc R . .
C4 C -0.4200(3) 0.1973(3) -0.01999(16) 0.0287(8) Uani 1 1 d . . .
H4 H -0.4344 0.1505 -0.0492 0.034 Uiso 1 1 calc R . .
O5 O 0.4401(3) 0.2167(2) 0.15582(13) 0.0464(8) Uani 1 1 d . . .
N5 N 0.1499(3) 0.0749(3) 0.36964(15) 0.0444(10) Uani 1 1 d . . .
H5N H 0.1810 0.0385 0.3459 0.053 Uiso 1 1 calc R . .
C5 C -0.4614(3) 0.2882(3) -0.02685(15) 0.0248(7) Uani 1 1 d . . .
H5 H -0.5043 0.3022 -0.0606 0.030 Uiso 1 1 calc R . .
O6 O -0.02560(19) 0.00577(17) 0.08600(10) 0.0210(5) Uani 1 1 d . . .
N6 N 0.3498(2) 0.0610(2) 0.48587(13) 0.0231(6) Uani 1 1 d . . .
C6 C -0.2080(3) 0.1653(3) 0.13659(17) 0.0324(9) Uani 1 1 d . . .
O7 O 0.2919(3) -0.1585(2) 0.27423(13) 0.0444(8) Uani 1 1 d . . .
N7 N 0.9334(2) 0.3616(2) 0.48989(12) 0.0183(6) Uani 1 1 d . . .
C7 C -0.0692(6) 0.1253(6) 0.2102(2) 0.089(3) Uani 1 1 d . . .
H7 H -0.0732 0.0609 0.1921 0.107 Uiso 1 1 calc R . .
H7A H -0.0036 0.1546 0.2025 0.107 Uiso 1 1 calc R . .
O8 O 0.2553(3) 0.0106(2) 0.27746(15) 0.0459(8) Uani 1 1 d . . .
N8 N 0.7666(2) 0.2479(2) 0.37904(13) 0.0255(7) Uani 1 1 d . . .
H8N H 0.7698 0.2978 0.3562 0.031 Uiso 1 1 calc R . .
C8 C -0.0740(4) 0.1160(6) 0.2697(2) 0.075(2) Uani 1 1 d . . .
H8A H -0.1304 0.0723 0.2770 0.090 Uiso 1 1 calc R . .
H8 H -0.0887 0.1797 0.2861 0.090 Uiso 1 1 calc R . .
O9 O 0.1186(2) -0.1038(3) 0.26127(14) 0.0451(8) Uani 1 1 d . . .
N9 N 0.6670(3) 0.1876(3) 0.30390(15) 0.0347(8) Uani 1 1 d . . .
H9N H 0.6893 0.2375 0.2856 0.042 Uiso 1 1 calc R . .
C9 C 0.0585(4) 0.1158(4) 0.3491(2) 0.0462(12) Uani 1 1 d . . .
O10 O 0.2322(2) -0.0757(2) 0.18769(12) 0.0405(7) Uani 1 1 d . . .
N10 N 0.4122(3) 0.1248(3) 0.23393(15) 0.0412(9) Uani 1 1 d . . .
H10N H 0.3780 0.0764 0.2468 0.049 Uiso 1 1 calc R . .
C10 C 0.2979(3) 0.0609(3) 0.43404(16) 0.0258(8) Uani 1 1 d . . .
H10 H 0.3324 0.0420 0.4019 0.031 Uiso 1 1 calc R . .
O11 O 0.4899(2) -0.1022(2) 0.32281(13) 0.0392(7) Uani 1 1 d . . .
N11 N 0.3166(3) 0.1013(3) 0.14927(14) 0.0399(10) Uani 1 1 d . . .
H11N H 0.2850 0.0588 0.1692 0.048 Uiso 1 1 calc R . .
C11 C 0.1962(3) 0.0870(3) 0.42464(17) 0.0309(9) Uani 1 1 d . . .
O12 O -0.0177(2) -0.1348(2) 0.16548(13) 0.0416(8) Uani 1 1 d . . .
N12 N 0.1448(2) 0.0699(2) 0.02061(12) 0.0201(6) Uani 1 1 d . . .
C12 C 0.1467(4) 0.1186(4) 0.4710(2) 0.0482(13) Uani 1 1 d . . .
H12 H 0.0773 0.1369 0.4664 0.058 Uiso 1 1 calc R . .
C29 C 0.4308(7) 0.4897(6) 0.3763(4) 0.0340(18) Uani 0.50 1 d P . .
C13 C 0.2012(4) 0.1228(4) 0.5241(2) 0.0534(14) Uani 1 1 d . . .
H13 H 0.1699 0.1463 0.5564 0.064 Uiso 1 1 calc R . .
O14 O 0.2122(6) 0.3575(8) 0.2948(4) 0.080(3) Uani 0.50 1 d P . .
C14 C 0.3013(3) 0.0928(3) 0.53066(18) 0.0375(10) Uani 1 1 d . . .
H14 H 0.3369 0.0948 0.5678 0.045 Uiso 1 1 calc R . .
C15 C 0.8722(3) 0.3422(2) 0.44310(14) 0.0189(7) Uani 1 1 d . . .
H15 H 0.8600 0.3919 0.4154 0.023 Uiso 1 1 calc R . .
C16 C 0.8245(2) 0.2536(2) 0.43173(14) 0.0191(7) Uani 1 1 d . . .
C17 C 0.8400(3) 0.1810(3) 0.47281(15) 0.0241(7) Uani 1 1 d . . .
H17 H 0.8084 0.1200 0.4675 0.029 Uiso 1 1 calc R . .
C18 C 0.9037(3) 0.2017(3) 0.52187(15) 0.0246(7) Uani 1 1 d . . .
H18 H 0.9162 0.1538 0.5507 0.030 Uiso 1 1 calc R . .
C19 C 0.9492(3) 0.2911(3) 0.52935(14) 0.0212(7) Uani 1 1 d . . .
H19 H 0.9927 0.3030 0.5632 0.025 Uiso 1 1 calc R . .
C20 C 0.7051(3) 0.1738(3) 0.35836(15) 0.0235(7) Uani 1 1 d . . .
C21 C 0.5920(3) 0.1270(3) 0.27273(18) 0.0342(9) Uani 1 1 d . . .
H21A H 0.5910 0.0630 0.2912 0.041 Uiso 1 1 calc R . .
H21 H 0.6095 0.1181 0.2327 0.041 Uiso 1 1 calc R . .
C22 C 0.4882(3) 0.1736(3) 0.27253(17) 0.0361(9) Uani 1 1 d . . .
H22A H 0.4665 0.1725 0.3120 0.043 Uiso 1 1 calc R . .
H22 H 0.4930 0.2416 0.2606 0.043 Uiso 1 1 calc R . .
C23 C 0.3936(3) 0.1527(3) 0.17872(18) 0.0353(9) Uani 1 1 d . . .
C24 C 0.1863(3) 0.0736(3) 0.07479(15) 0.0229(7) Uani 1 1 d . . .
H24 H 0.1476 0.0503 0.1042 0.028 Uiso 1 1 calc R . .
C25 C 0.2836(3) 0.1099(3) 0.09077(16) 0.0288(8) Uani 1 1 d . . .
C26 C 0.3385(3) 0.1486(4) 0.04866(18) 0.0395(11) Uani 1 1 d . . .
H26 H 0.4041 0.1750 0.0579 0.047 Uiso 1 1 calc R . .
C27 C 0.2943(3) 0.1475(4) -0.00758(18) 0.0434(12) Uani 1 1 d . . .
H27 H 0.3295 0.1741 -0.0376 0.052 Uiso 1 1 calc R . .
C28 C 0.1991(3) 0.1076(3) -0.01991(17) 0.0329(9) Uani 1 1 d . . .
H28 H 0.1707 0.1069 -0.0587 0.040 Uiso 1 1 calc R . .
O13 O 0.3938(6) 0.3219(5) 0.3616(3) 0.057(2) Uani 0.50 1 d P . .
C30 C 0.4577(9) 0.4079(8) 0.3430(3) 0.052(3) Uani 0.50 1 d P . .
C31 C 0.165(2) 0.3404(19) 0.1939(7) 0.174(13) Uani 0.50 1 d P . .
C32 C 0.2098(11) 0.2972(13) 0.2437(8) 0.096(6) Uani 0.50 1 d P . .

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 0.0150(3) 0.0210(3) 0.0163(3) -0.0031(2) -0.0044(2) -0.0041(2)
S1 0.0372(5) 0.0278(5) 0.0192(4) -0.0001(3) -0.0015(3) -0.0026(4)
O1 0.0340(16) 0.0318(15) 0.0403(16) 0.0013(12) 0.0023(12) 0.0176(12)
N1 0.0184(14) 0.0215(14) 0.0229(14) 0.0032(11) -0.0023(11) 0.0039(11)
C1 0.0217(17) 0.0265(18) 0.0179(15) 0.0001(13) -0.0025(13) 0.0060(14)
Ni2 0.0132(3) 0.0178(3) 0.0127(3) 0.0018(2) -0.0049(2) 0.0022(2)
O2 0.055(2) 0.059(2) 0.053(2) -0.0051(17) -0.0038(17) 0.0318(18)
N2 0.0372(19) 0.0368(19) 0.0204(15) 0.0007(13) -0.0020(13) 0.0215(15)
C2 0.0232(17) 0.0267(18) 0.0190(16) 0.0027(13) 0.0016(13) 0.0076(14)
O3 0.0240(13) 0.0277(13) 0.0181(12) -0.0021(10) -0.0008(10) -0.0063(10)
N3 0.100(4) 0.092(4) 0.034(2) -0.015(2) -0.031(2) 0.079(3)
C3 0.033(2) 0.0225(18) 0.0287(19) 0.0016(15) 0.0015(15) 0.0046(15)
O4 0.0275(14) 0.0296(14) 0.0312(14) -0.0003(11) -0.0031(11) -0.0133(11)
N4 0.057(3) 0.106(4) 0.037(2) -0.016(2) -0.025(2) 0.050(3)
C4 0.032(2) 0.0243(19) 0.0283(19) -0.0029(15) -0.0024(15) -0.0002(15)
O5 0.0469(19) 0.050(2) 0.0393(17) 0.0080(14) -0.0120(14) -0.0269(16)
N5 0.036(2) 0.063(3) 0.0310(18) -0.0160(17) -0.0140(15) 0.0251(18)
C5 0.0249(18) 0.0292(19) 0.0194(16) 0.0019(14) -0.0039(13) -0.0022(15)
O6 0.0210(12) 0.0254(13) 0.0158(11) 0.0014(9) -0.0022(9) 0.0028(9)
N6 0.0180(14) 0.0253(16) 0.0248(15) -0.0033(12) -0.0045(11) -0.0003(12)
C6 0.034(2) 0.038(2) 0.0253(18) 0.0076(16) 0.0027(15) 0.0197(18)
O7 0.052(2) 0.0484(19) 0.0317(16) 0.0040(14) -0.0045(14) 0.0113(15)
N7 0.0171(13) 0.0196(14) 0.0177(13) -0.0026(11) -0.0019(10) -0.0025(11)
C7 0.101(5) 0.126(6) 0.035(3) -0.009(3) -0.022(3) 0.093(5)
O8 0.050(2) 0.045(2) 0.0435(19) -0.0138(15) 0.0115(15) -0.0147(15)
N8 0.0286(16) 0.0254(16) 0.0208(14) 0.0016(12) -0.0075(12) -0.0112(13)
C8 0.045(3) 0.124(6) 0.054(3) 0.010(4) -0.015(3) 0.036(4)
O9 0.0387(18) 0.054(2) 0.0427(17) 0.0000(15) 0.0014(14) -0.0110(15)
N9 0.0341(19) 0.0385(19) 0.0290(17) 0.0009(14) -0.0118(14) -0.0187(15)
C9 0.040(3) 0.058(3) 0.039(2) -0.001(2) -0.0076(19) 0.026(2)
O10 0.054(2) 0.0390(17) 0.0275(14) 0.0002(12) -0.0016(13) -0.0044(14)
N10 0.036(2) 0.055(2) 0.0292(17) 0.0080(16) -0.0141(15) -0.0219(17)
C10 0.0216(18) 0.031(2) 0.0243(17) -0.0021(14) -0.0023(14) 0.0040(14)
O11 0.0498(19) 0.0327(16) 0.0344(15) -0.0105(12) 0.0002(13) -0.0074(14)
N11 0.037(2) 0.051(2) 0.0285(17) 0.0157(16) -0.0170(15) -0.0260(17)
C11 0.0242(19) 0.037(2) 0.0298(19) -0.0061(16) -0.0059(15) 0.0098(16)
O12 0.0392(17) 0.0480(19) 0.0366(16) 0.0151(14) -0.0017(13) 0.0017(14)
N12 0.0163(13) 0.0229(15) 0.0198(13) 0.0014(11) -0.0057(10) 0.0000(11)
C12 0.032(2) 0.070(3) 0.041(2) -0.012(2) -0.0031(19) 0.024(2)
C29 0.039(5) 0.029(4) 0.034(4) 0.007(3) 0.006(3) 0.004(3)
C13 0.046(3) 0.082(4) 0.033(2) -0.016(2) 0.003(2) 0.027(3)
O14 0.044(5) 0.127(8) 0.071(6) -0.021(5) 0.013(4) -0.011(5)
C14 0.036(2) 0.048(3) 0.0274(19) -0.0113(18) -0.0033(16) 0.0123(19)
C15 0.0192(16) 0.0196(16) 0.0171(15) -0.0004(12) -0.0023(12) -0.0036(13)
C16 0.0162(15) 0.0224(17) 0.0181(15) -0.0033(13) -0.0014(12) -0.0062(13)
C17 0.0268(18) 0.0202(17) 0.0245(17) 0.0002(13) -0.0025(14) -0.0055(14)
C18 0.0283(19) 0.0222(17) 0.0224(17) 0.0026(13) -0.0036(14) -0.0005(14)
C19 0.0220(17) 0.0224(17) 0.0179(15) -0.0016(13) -0.0061(12) 0.0013(13)
C20 0.0189(16) 0.0262(18) 0.0249(17) -0.0045(14) -0.0017(13) -0.0056(14)
C21 0.033(2) 0.037(2) 0.030(2) -0.0065(17) -0.0106(16) -0.0125(18)
C22 0.034(2) 0.045(2) 0.0272(19) 0.0002(17) -0.0086(16) -0.0093(19)
C23 0.028(2) 0.042(2) 0.033(2) 0.0060(18) -0.0121(16) -0.0118(18)
C24 0.0206(17) 0.0251(18) 0.0217(16) 0.0040(14) -0.0054(13) -0.0041(14)
C25 0.0249(19) 0.033(2) 0.0260(18) 0.0056(15) -0.0096(15) -0.0060(15)
C26 0.028(2) 0.054(3) 0.035(2) 0.009(2) -0.0064(17) -0.0212(19)
C27 0.038(2) 0.062(3) 0.030(2) 0.010(2) 0.0001(18) -0.025(2)
C28 0.034(2) 0.042(2) 0.0228(18) 0.0052(16) -0.0024(15) -0.0113(18)
O13 0.096(6) 0.052(4) 0.024(3) -0.009(3) 0.006(3) 0.017(4)
C30 0.086(8) 0.052(6) 0.017(4) 0.001(4) 0.007(4) 0.017(5)
C31 0.26(3) 0.21(3) 0.054(10) 0.021(12) 0.030(14) 0.13(2)
C32 0.050(7) 0.110(13) 0.131(14) -0.062(11) 0.031(8) 0.007(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
Ni1 O3 2.086(3) . ?
Ni1 O3 2.086(3) 3_656 ?
Ni1 N1 2.127(3) 4_666 ?
Ni1 N1 2.127(3) 2_545 ?
Ni1 N6 2.160(3) . ?
Ni1 N6 2.160(3) 3_656 ?
S1 O8 1.465(3) . ?
S1 O7 1.471(3) . ?
S1 O10 1.471(3) . ?
S1 O9 1.493(3) . ?
O1 C6 1.223(5) . ?
N1 C1 1.330(4) . ?
N1 C5 1.356(5) . ?
N1 Ni1 2.127(3) 2 ?
C1 C2 1.400(5) . ?
Ni2 O6 2.068(2) . ?
Ni2 O6 2.068(2) 3 ?
Ni2 N7 2.121(3) 4_465 ?
Ni2 N7 2.121(3) 2_645 ?
Ni2 N12 2.165(3) . ?
Ni2 N12 2.165(3) 3 ?
O2 C9 1.225(6) . ?
N2 C6 1.368(5) . ?
N2 C2 1.399(4) . ?
C2 C3 1.389(5) . ?
N3 C6 1.331(6) . ?
N3 C7 1.455(6) . ?
C3 C4 1.384(5) . ?
O4 C20 1.236(4) . ?
N4 C9 1.342(6) . ?
N4 C8 1.459(6) . ?
C4 C5 1.381(5) . ?
O5 C23 1.230(5) . ?
N5 C11 1.383(5) . ?
N5 C9 1.384(5) . ?
N6 C10 1.337(4) . ?
N6 C14 1.350(5) . ?
N7 C15 1.329(4) . ?
N7 C19 1.350(4) . ?
N7 Ni2 2.121(3) 2_655 ?
C7 C8 1.404(8) . ?
N8 C20 1.374(4) . ?
N8 C16 1.393(4) . ?
N9 C20 1.340(5) . ?
N9 C21 1.449(5) . ?
N10 C23 1.348(5) . ?
N10 C22 1.457(5) . ?
C10 C11 1.393(5) . ?
N11 C23 1.378(5) . ?
N11 C25 1.402(5) . ?
C11 C12 1.386(6) . ?
N12 C24 1.335(4) . ?
N12 C28 1.344(5) . ?
C12 C13 1.380(6) . ?
C29 C30 1.441(13) . ?
C13 C14 1.384(6) . ?
O14 C32 1.457(16) . ?
C15 C16 1.398(5) . ?
C16 C17 1.396(5) . ?
C17 C18 1.391(5) . ?
C18 C19 1.386(5) . ?
C21 C22 1.518(6) . ?
C24 C25 1.403(5) . ?
C25 C26 1.383(6) . ?
C26 C27 1.390(6) . ?
C27 C28 1.384(6) . ?
O13 C30 1.549(14) . ?
C31 C32 1.39(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
O3 Ni1 O3 180.000(1) . 3_656 ?
O3 Ni1 N1 87.94(10) . 4_666 ?
O3 Ni1 N1 92.06(10) 3_656 4_666 ?
O3 Ni1 N1 92.06(10) . 2_545 ?
O3 Ni1 N1 87.94(10) 3_656 2_545 ?
N1 Ni1 N1 180.0 4_666 2_545 ?
O3 Ni1 N6 88.96(11) . . ?
O3 Ni1 N6 91.04(11) 3_656 . ?
N1 Ni1 N6 88.28(11) 4_666 . ?
N1 Ni1 N6 91.72(11) 2_545 . ?
O3 Ni1 N6 91.04(11) . 3_656 ?
O3 Ni1 N6 88.96(11) 3_656 3_656 ?
N1 Ni1 N6 91.72(11) 4_666 3_656 ?
N1 Ni1 N6 88.28(11) 2_545 3_656 ?
N6 Ni1 N6 180.0 . 3_656 ?
O8 S1 O7 110.0(2) . . ?
O8 S1 O10 110.43(19) . . ?
O7 S1 O10 109.29(19) . . ?
O8 S1 O9 109.3(2) . . ?
O7 S1 O9 108.8(2) . . ?
O10 S1 O9 109.01(18) . . ?
C1 N1 C5 116.8(3) . . ?
C1 N1 Ni1 121.5(2) . 2 ?
C5 N1 Ni1 121.6(2) . 2 ?
N1 C1 C2 124.6(3) . . ?
O6 Ni2 O6 180.0 . 3 ?
O6 Ni2 N7 88.31(10) . 4_465 ?
O6 Ni2 N7 91.69(10) 3 4_465 ?
O6 Ni2 N7 91.69(10) . 2_645 ?
O6 Ni2 N7 88.31(10) 3 2_645 ?
N7 Ni2 N7 180.00(6) 4_465 2_645 ?
O6 Ni2 N12 89.14(11) . . ?
O6 Ni2 N12 90.86(11) 3 . ?
N7 Ni2 N12 88.21(11) 4_465 . ?
N7 Ni2 N12 91.79(11) 2_645 . ?
O6 Ni2 N12 90.86(11) . 3 ?
O6 Ni2 N12 89.14(11) 3 3 ?
N7 Ni2 N12 91.80(11) 4_465 3 ?
N7 Ni2 N12 88.20(11) 2_645 3 ?
N12 Ni2 N12 180.0 . 3 ?
C6 N2 C2 127.1(3) . . ?
C3 C2 N2 126.1(3) . . ?
C3 C2 C1 118.1(3) . . ?
N2 C2 C1 115.8(3) . . ?
C6 N3 C7 124.5(5) . . ?
C4 C3 C2 117.4(3) . . ?
C9 N4 C8 120.7(5) . . ?
C5 C4 C3 121.1(3) . . ?
C11 N5 C9 125.0(4) . . ?
N1 C5 C4 122.0(3) . . ?
C10 N6 C14 117.4(3) . . ?
C10 N6 Ni1 122.0(2) . . ?
C14 N6 Ni1 120.3(2) . . ?
O1 C6 N3 123.8(4) . . ?
O1 C6 N2 123.5(4) . . ?
N3 C6 N2 112.6(4) . . ?
C15 N7 C19 117.4(3) . . ?
C15 N7 Ni2 119.6(2) . 2_655 ?
C19 N7 Ni2 123.1(2) . 2_655 ?
C8 C7 N3 110.4(5) . . ?
C20 N8 C16 128.0(3) . . ?
C7 C8 N4 112.3(5) . . ?
C20 N9 C21 125.2(3) . . ?
O2 C9 N4 123.2(4) . . ?
O2 C9 N5 123.4(4) . . ?
N4 C9 N5 113.4(4) . . ?
C23 N10 C22 121.0(4) . . ?
N6 C10 C11 123.6(4) . . ?
C23 N11 C25 126.5(3) . . ?
N5 C11 C12 124.3(4) . . ?
N5 C11 C10 117.2(4) . . ?
C12 C11 C10 118.5(4) . . ?
C24 N12 C28 116.9(3) . . ?
C24 N12 Ni2 120.6(2) . . ?
C28 N12 Ni2 122.4(2) . . ?
C13 C12 C11 118.1(4) . . ?
C12 C13 C14 120.4(4) . . ?
N6 C14 C13 122.0(4) . . ?
N7 C15 C16 124.6(3) . . ?
N8 C16 C17 127.0(3) . . ?
N8 C16 C15 115.0(3) . . ?
C17 C16 C15 118.1(3) . . ?
C18 C17 C16 117.3(3) . . ?
C19 C18 C17 120.9(3) . . ?
N7 C19 C18 121.8(3) . . ?
O4 C20 N9 124.5(3) . . ?
O4 C20 N8 122.7(3) . . ?
N9 C20 N8 112.8(3) . . ?
N9 C21 C22 109.4(4) . . ?
N10 C22 C21 112.2(4) . . ?
O5 C23 N10 124.6(4) . . ?
O5 C23 N11 122.3(4) . . ?
N10 C23 N11 113.1(4) . . ?
N12 C24 C25 123.8(3) . . ?
C26 C25 N11 126.0(3) . . ?
C26 C25 C24 118.6(3) . . ?
N11 C25 C24 115.3(3) . . ?
C25 C26 C27 117.7(4) . . ?
C28 C27 C26 120.0(4) . . ?
N12 C28 C27 122.9(4) . . ?
C29 C30 O13 106.9(8) . . ?
C31 C32 O14 114.4(15) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.34
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         3.134
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.207