# Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and 
# The Centre National de la Recherche Scientifique, 2007

data_global

#====================================================================

_journal_coden_Cambridge         440

_publ_contact_author             'Malcolm A. Halcrow'
_publ_contact_author_address     
;
School of Chemistry,
University of Leeds,
Woodhouse Lane,
Leeds LS2 9JT,
UK
;
_publ_contact_author_phone       '+44 (0)113 3436506'
_publ_contact_author_fax         '+44 (0)113 3436565'
_publ_contact_author_email       m.a.halcrow@leeds.ac.uk
_publ_requested_journal          'New Journal of Chemistry'
_publ_contact_letter             
;
The following set of data is for a structure included in a
manuscript we have just submitted to the New J. Chem. office.
;

#=======================================================================

# 2. TITLE AND AUTHOR LIST

_publ_section_title              
;
A Comparison of Different Methods for Fitting Susceptibility Data of
Cobalt(II) Coordination Polymers in a New Cobalt(II)/Sulfate 1-D Chain
;
loop_
_publ_author_name
_publ_author_address
'Leigh F. Jones'
;
School of Chemistry,
University of Leeds,
Woodhouse Lane,
Leeds LS2 9JT,
UK
;
'Colin A. Kilner'
;
School of Chemistry,
University of Leeds,
Woodhouse Lane,
Leeds LS2 9JT,
UK
;
'Malcolm A. Halcrow'
;
School of Chemistry,
University of Leeds,
Woodhouse Lane,
Leeds LS2 9JT,
UK
;

#=================================================================

data_c:\datasets\leeds\lfj26d\lfj26d
_database_code_depnum_ccdc_archive 'CCDC 646395'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Catena-[tris(5-tertbutylpyrazole)sulfatocobalt(II)]
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H36 Co N6 O4 S'
_chemical_formula_sum            'C21 H36 Co N6 O4 S'
_chemical_formula_weight         527.55

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'
Co Co 0.3494 0.9721 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'

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

_cell_length_a                   10.7470(2)
_cell_length_b                   13.1706(2)
_cell_length_c                   18.1220(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2565.07(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    35378
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      27.48

_exptl_crystal_description       Cube
_exptl_crystal_colour            Purple
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1116
_exptl_absorpt_coefficient_mu    0.788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.623
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_process_details   
;
Using multiple and symmetry-related data measurements via the program SORTAV
See R.H. Blessing, Acta Cryst (1995), A51, 33-38
;

_exptl_special_details           
;
Detector set at 30mm from sample with different 2theta offsets
1 degree phi exposures for chi=0 degree settings
1 degree omega exposures for chi=90 degree settings
;

_diffrn_ambient_temperature      150(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  'Nonius KappaCCD area detector diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            35378
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.45
_diffrn_reflns_theta_max         27.48
_reflns_number_total             5834
_reflns_number_gt                5431
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  'local program'

_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.

The crystal was a racemic twin.

No disorder was detected during refinement, and no restraints were applied.
All non-H atoms were refined anisotropically, while all H atoms were
placed in calculated positions and refined using a riding model.
;

_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^)+(0.0371P)^2^+0.7572P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.196(11)
_refine_ls_number_reflns         5834
_refine_ls_number_parameters     308
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0314
_refine_ls_wR_factor_ref         0.0770
_refine_ls_wR_factor_gt          0.0743
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.50793(2) 0.154567(19) 0.745630(13) 0.01964(7) Uani 1 1 d . . .
N2 N 0.42252(16) 0.13935(13) 0.64607(9) 0.0228(3) Uani 1 1 d . . .
N3 N 0.36183(16) 0.21416(13) 0.60854(9) 0.0230(4) Uani 1 1 d . . .
H3 H 0.3574 0.2776 0.6235 0.028 Uiso 1 1 calc R . .
C4 C 0.30948(19) 0.17940(16) 0.54597(11) 0.0239(4) Uani 1 1 d . . .
C5 C 0.3379(2) 0.07711(17) 0.54197(12) 0.0296(5) Uani 1 1 d . . .
H5 H 0.3150 0.0309 0.5040 0.036 Uiso 1 1 calc R . .
C6 C 0.4070(2) 0.05592(16) 0.60508(11) 0.0270(5) Uani 1 1 d . . .
H6 H 0.4389 -0.0092 0.6174 0.032 Uiso 1 1 calc R . .
C7 C 0.2333(2) 0.24820(19) 0.49604(13) 0.0291(5) Uani 1 1 d . . .
C8 C 0.1639(2) 0.1817(2) 0.44016(14) 0.0406(6) Uani 1 1 d . . .
H8A H 0.1086 0.1349 0.4664 0.061 Uiso 1 1 calc R . .
H8B H 0.2241 0.1428 0.4110 0.061 Uiso 1 1 calc R . .
H8C H 0.1146 0.2249 0.4073 0.061 Uiso 1 1 calc R . .
C9 C 0.1402(2) 0.3079(2) 0.54228(14) 0.0390(6) Uani 1 1 d . . .
H9A H 0.0902 0.2607 0.5718 0.059 Uiso 1 1 calc R . .
H9B H 0.0854 0.3469 0.5097 0.059 Uiso 1 1 calc R . .
H9C H 0.1850 0.3543 0.5751 0.059 Uiso 1 1 calc R . .
C10 C 0.3181(3) 0.3226(2) 0.45499(15) 0.0455(6) Uani 1 1 d . . .
H10A H 0.2673 0.3683 0.4247 0.068 Uiso 1 1 calc R . .
H10B H 0.3754 0.2847 0.4232 0.068 Uiso 1 1 calc R . .
H10C H 0.3658 0.3625 0.4908 0.068 Uiso 1 1 calc R . .
N11 N 0.42364(15) 0.15807(13) 0.84594(9) 0.0229(3) Uani 1 1 d . . .
N12 N 0.36213(16) 0.23810(13) 0.87648(9) 0.0228(4) Uani 1 1 d . . .
H12 H 0.3482 0.2958 0.8535 0.027 Uiso 1 1 calc R . .
C13 C 0.32526(19) 0.21870(17) 0.94562(11) 0.0249(4) Uani 1 1 d . . .
C14 C 0.3659(2) 0.12158(17) 0.96185(12) 0.0290(5) Uani 1 1 d . . .
H14 H 0.3548 0.0857 1.0068 0.035 Uiso 1 1 calc R . .
C15 C 0.4261(2) 0.08742(17) 0.89870(11) 0.0260(4) Uani 1 1 d . . .
H15 H 0.4639 0.0226 0.8938 0.031 Uiso 1 1 calc R . .
C16 C 0.2547(2) 0.29450(18) 0.99276(12) 0.0329(5) Uani 1 1 d . . .
C17 C 0.1653(3) 0.3562(2) 0.94587(14) 0.0469(7) Uani 1 1 d . . .
H17A H 0.1174 0.4021 0.9776 0.070 Uiso 1 1 calc R . .
H17B H 0.1082 0.3103 0.9200 0.070 Uiso 1 1 calc R . .
H17C H 0.2124 0.3960 0.9097 0.070 Uiso 1 1 calc R . .
C18 C 0.1802(3) 0.2348(2) 1.05067(15) 0.0508(8) Uani 1 1 d . . .
H18A H 0.1352 0.2824 1.0826 0.076 Uiso 1 1 calc R . .
H18B H 0.2373 0.1939 1.0806 0.076 Uiso 1 1 calc R . .
H18C H 0.1206 0.1901 1.0258 0.076 Uiso 1 1 calc R . .
C19 C 0.3468(3) 0.3638(3) 1.0313(2) 0.0691(10) Uani 1 1 d . . .
H19A H 0.3907 0.4049 0.9945 0.104 Uiso 1 1 calc R . .
H19B H 0.4070 0.3227 1.0588 0.104 Uiso 1 1 calc R . .
H19C H 0.3022 0.4086 1.0654 0.104 Uiso 1 1 calc R . .
N20 N 0.69683(14) 0.17526(12) 0.74481(9) 0.0229(3) Uani 1 1 d . . .
N21 N 0.78452(13) 0.10062(12) 0.74224(9) 0.0234(3) Uani 1 1 d . . .
H21 H 0.7676 0.0359 0.7357 0.028 Uiso 1 1 calc R . .
C22 C 0.90057(17) 0.13807(15) 0.75099(11) 0.0250(4) Uani 1 1 d . . .
C23 C 0.88791(18) 0.24167(16) 0.75889(13) 0.0306(5) Uani 1 1 d . . .
H23 H 0.9526 0.2899 0.7658 0.037 Uiso 1 1 calc R . .
C24 C 0.76056(18) 0.26121(15) 0.75467(12) 0.0272(4) Uani 1 1 d . . .
H24 H 0.7241 0.3267 0.7583 0.033 Uiso 1 1 calc R . .
C25 C 1.01463(17) 0.07016(16) 0.75074(12) 0.0290(4) Uani 1 1 d . . .
C26 C 1.1306(2) 0.1351(2) 0.7629(2) 0.0680(10) Uani 1 1 d . . .
H26A H 1.1402 0.1826 0.7216 0.102 Uiso 1 1 calc R . .
H26B H 1.2040 0.0912 0.7658 0.102 Uiso 1 1 calc R . .
H26C H 1.1220 0.1733 0.8090 0.102 Uiso 1 1 calc R . .
C27 C 1.0261(3) 0.0163(2) 0.67675(14) 0.0451(6) Uani 1 1 d . . .
H27A H 0.9521 -0.0256 0.6684 0.068 Uiso 1 1 calc R . .
H27B H 1.1003 -0.0270 0.6770 0.068 Uiso 1 1 calc R . .
H27C H 1.0333 0.0668 0.6373 0.068 Uiso 1 1 calc R . .
C28 C 1.0020(3) -0.0092(2) 0.81215(14) 0.0508(7) Uani 1 1 d . . .
H28A H 0.9958 0.0252 0.8600 0.076 Uiso 1 1 calc R . .
H28B H 1.0751 -0.0537 0.8119 0.076 Uiso 1 1 calc R . .
H28C H 0.9269 -0.0498 0.8038 0.076 Uiso 1 1 calc R . .
S29 S 0.41661(4) 0.40758(4) 0.73176(3) 0.02242(11) Uani 1 1 d . . .
O30 O 0.49276(11) 0.31522(10) 0.74273(7) 0.0238(3) Uani 1 1 d . . .
O31 O 0.36957(14) 0.41185(12) 0.65600(8) 0.0295(3) Uani 1 1 d . . .
O32 O 0.31183(14) 0.40662(12) 0.78474(9) 0.0332(4) Uani 1 1 d . . .
O33 O 0.49620(12) 0.49674(10) 0.74698(7) 0.0273(3) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.01926(12) 0.01890(14) 0.02077(12) 0.00002(9) -0.00067(10) 0.00030(9)
N2 0.0235(9) 0.0189(9) 0.0259(8) 0.0016(7) -0.0025(7) 0.0010(7)
N3 0.0256(9) 0.0177(9) 0.0258(8) 0.0005(7) -0.0040(7) 0.0005(7)
C4 0.0224(10) 0.0272(11) 0.0221(9) 0.0000(8) -0.0023(8) -0.0012(8)
C5 0.0333(11) 0.0271(13) 0.0283(11) -0.0053(9) -0.0049(9) -0.0011(9)
C6 0.0311(11) 0.0219(11) 0.0280(10) -0.0020(8) -0.0035(9) 0.0004(9)
C7 0.0253(11) 0.0323(12) 0.0296(11) 0.0022(8) -0.0082(9) 0.0003(9)
C8 0.0388(13) 0.0437(15) 0.0391(13) -0.0026(11) -0.0167(11) 0.0038(11)
C9 0.0326(13) 0.0429(15) 0.0416(13) -0.0015(11) -0.0077(10) 0.0105(11)
C10 0.0382(14) 0.0508(17) 0.0474(14) 0.0208(12) -0.0055(11) -0.0032(12)
N11 0.0221(8) 0.0186(9) 0.0282(8) -0.0008(7) 0.0002(7) 0.0004(7)
N12 0.0239(9) 0.0176(9) 0.0269(9) -0.0006(7) 0.0026(7) 0.0022(7)
C13 0.0226(10) 0.0271(12) 0.0250(10) 0.0000(9) 0.0010(8) -0.0015(9)
C14 0.0323(12) 0.0308(13) 0.0238(10) 0.0041(8) 0.0046(8) -0.0010(9)
C15 0.0289(11) 0.0207(11) 0.0283(10) 0.0036(8) 0.0006(8) 0.0012(9)
C16 0.0308(12) 0.0383(13) 0.0297(12) -0.0053(10) 0.0056(9) 0.0068(10)
C17 0.0495(15) 0.0505(16) 0.0406(13) 0.0084(13) 0.0146(12) 0.0246(13)
C18 0.0555(17) 0.0591(19) 0.0378(14) 0.0099(13) 0.0184(13) 0.0234(15)
C19 0.0508(18) 0.068(2) 0.088(2) -0.0508(19) 0.0014(17) 0.0064(16)
N20 0.0221(7) 0.0191(8) 0.0275(9) -0.0007(7) 0.0006(7) 0.0003(6)
N21 0.0202(7) 0.0181(8) 0.0321(9) 0.0009(7) 0.0005(7) 0.0002(6)
C22 0.0220(8) 0.0251(10) 0.0280(10) -0.0002(9) -0.0004(9) -0.0023(7)
C23 0.0254(9) 0.0258(11) 0.0407(12) -0.0018(9) -0.0029(10) -0.0054(7)
C24 0.0262(9) 0.0199(10) 0.0354(11) -0.0006(9) -0.0018(9) -0.0020(7)
C25 0.0208(9) 0.0280(11) 0.0383(11) -0.0027(9) -0.0030(10) 0.0002(7)
C26 0.0248(11) 0.0477(17) 0.132(3) -0.023(2) -0.0149(17) 0.0012(11)
C27 0.0412(14) 0.0530(17) 0.0410(14) -0.0066(12) -0.0009(11) 0.0163(13)
C28 0.0533(17) 0.0540(17) 0.0453(14) 0.0075(12) 0.0050(13) 0.0278(15)
S29 0.0253(2) 0.0158(2) 0.0262(2) 0.00021(19) -0.00020(19) 0.00082(19)
O30 0.0254(6) 0.0154(7) 0.0307(7) 0.0018(5) -0.0005(7) 0.0027(5)
O31 0.0359(8) 0.0213(8) 0.0314(8) -0.0001(6) -0.0076(6) -0.0004(6)
O32 0.0316(8) 0.0283(8) 0.0396(9) 0.0086(7) 0.0119(6) 0.0089(7)
O33 0.0346(7) 0.0174(7) 0.0300(7) -0.0003(5) -0.0058(8) -0.0032(5)

_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
Co1 N11 2.0315(16) . ?
Co1 N2 2.0342(16) . ?
Co1 N20 2.0483(15) . ?
Co1 O33 2.0835(14) 4_646 ?
Co1 O30 2.1228(13) . ?
N2 C6 1.337(3) . ?
N2 N3 1.363(2) . ?
N3 C4 1.346(3) . ?
C4 C5 1.383(3) . ?
C4 C7 1.520(3) . ?
C5 C6 1.392(3) . ?
C7 C9 1.523(3) . ?
C7 C10 1.531(3) . ?
C7 C8 1.532(3) . ?
N11 C15 1.334(3) . ?
N11 N12 1.362(2) . ?
N12 C13 1.339(3) . ?
C13 C14 1.383(3) . ?
C13 C16 1.517(3) . ?
C14 C15 1.390(3) . ?
C16 C19 1.517(4) . ?
C16 C17 1.518(3) . ?
C16 C18 1.536(3) . ?
N20 C24 1.335(2) . ?
N20 N21 1.363(2) . ?
N21 C22 1.351(2) . ?
C22 C23 1.379(3) . ?
C22 C25 1.517(3) . ?
C23 C24 1.395(3) . ?
C25 C27 1.522(3) . ?
C25 C26 1.528(3) . ?
C25 C28 1.533(3) . ?
S29 O31 1.4642(15) . ?
S29 O33 1.4788(14) . ?
S29 O30 1.4795(13) . ?
S29 O32 1.4799(15) . ?

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
N11 Co1 N2 126.49(6) . . ?
N11 Co1 N20 116.45(7) . . ?
N2 Co1 N20 116.99(7) . . ?
N11 Co1 O33 87.46(6) . 4_646 ?
N2 Co1 O33 87.08(6) . 4_646 ?
N20 Co1 O33 98.88(6) . 4_646 ?
N11 Co1 O30 88.01(6) . . ?
N2 Co1 O30 92.38(6) . . ?
N20 Co1 O30 86.75(6) . . ?
O33 Co1 O30 173.94(5) 4_646 . ?
C6 N2 N3 104.90(16) . . ?
C6 N2 Co1 129.07(14) . . ?
N3 N2 Co1 125.95(13) . . ?
C4 N3 N2 111.98(17) . . ?
N3 C4 C5 106.44(18) . . ?
N3 C4 C7 121.59(19) . . ?
C5 C4 C7 131.94(19) . . ?
C4 C5 C6 105.67(19) . . ?
N2 C6 C5 111.01(19) . . ?
C4 C7 C9 109.52(19) . . ?
C4 C7 C10 110.49(19) . . ?
C9 C7 C10 109.1(2) . . ?
C4 C7 C8 108.4(2) . . ?
C9 C7 C8 109.81(19) . . ?
C10 C7 C8 109.5(2) . . ?
C15 N11 N12 104.96(16) . . ?
C15 N11 Co1 128.05(14) . . ?
N12 N11 Co1 126.71(13) . . ?
C13 N12 N11 112.11(17) . . ?
N12 C13 C14 106.39(19) . . ?
N12 C13 C16 123.3(2) . . ?
C14 C13 C16 130.3(2) . . ?
C13 C14 C15 105.74(19) . . ?
N11 C15 C14 110.80(19) . . ?
C19 C16 C13 109.18(19) . . ?
C19 C16 C17 110.4(3) . . ?
C13 C16 C17 110.71(19) . . ?
C19 C16 C18 109.5(2) . . ?
C13 C16 C18 108.0(2) . . ?
C17 C16 C18 109.1(2) . . ?
C24 N20 N21 105.15(15) . . ?
C24 N20 Co1 128.34(13) . . ?
N21 N20 Co1 126.14(12) . . ?
C22 N21 N20 111.79(15) . . ?
N21 C22 C23 106.41(17) . . ?
N21 C22 C25 122.03(17) . . ?
C23 C22 C25 131.56(17) . . ?
C22 C23 C24 105.89(17) . . ?
N20 C24 C23 110.75(17) . . ?
C22 C25 C27 110.05(18) . . ?
C22 C25 C26 109.18(18) . . ?
C27 C25 C26 108.8(2) . . ?
C22 C25 C28 109.15(17) . . ?
C27 C25 C28 109.2(2) . . ?
C26 C25 C28 110.5(2) . . ?
O31 S29 O33 110.13(8) . . ?
O31 S29 O30 110.39(9) . . ?
O33 S29 O30 107.93(8) . . ?
O31 S29 O32 110.24(9) . . ?
O33 S29 O32 109.02(9) . . ?
O30 S29 O32 109.07(8) . . ?
S29 O30 Co1 149.92(8) . . ?
S29 O33 Co1 142.37(8) . 4_656 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3 O31 0.88 1.87 2.743(2) 172.9 .
N12 H12 O32 0.88 1.96 2.825(2) 168.3 .
N21 H21 O32 0.88 1.94 2.800(2) 165.3 4_646

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.054