##############################################################################
###                                                                        ###
###           Full Paper (Acta Crystallographica Section C)                ###
###                                                                        ###
##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section C. It conforms to the editorial and technical    #
# requirements of Notes for Authors for Section C, and has been peer         #
# reviewed under the auspices of the IUCr Commission on Journals.            #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
# cif/home.html                                                              #
#                                                                            #
#            Copyright International Union of Crystallography                #
#                                                                            #
##############################################################################
data_global
_audit_creation_method     'manual editing of SHELXL-97-output file'
_journal_date_recd_electronic     2004-02-20
_journal_date_accepted     2004-04-22
_journal_name_full     'Acta Crystallographica, Section C'
_journal_year     2004
_journal_volume     60
_journal_issue      6
_journal_page_first     m291
_journal_page_last     m295
_journal_paper_category     FM
_publ_contact_author_name     'Michel Fleck'
_publ_contact_author_address
;
 Universität Wien -- Geozentrum
 Institut für Mineralogie und Kristallographie
 Althanstraße 14
 A-1090 Wien, Austria
;
_publ_contact_author_email     michel.fleck@univie.ac.at
_publ_contact_author_fax     '43 1 4277 9532'
_publ_contact_author_phone     '43 1 4277 53244'
_publ_section_title
;
Three novel non-centrosymmetric compounds of glycine:
glycine lithium sulfate,
glycine nickel dichloride dihydrate and
glycine zinc sulfate trihydrate
;
loop_
    _publ_author_name
    _publ_author_address
    'Michel Fleck'
;
 Universität Wien -- Geozentrum
 Institut für Mineralogie und Kristallographie
 Althanstraße 14
 A-1090 Wien, Austria
;
    'Ladislav Bohatý'
;
 Universität zu Köln
 Institut für Kristallographie
 Zülpicher Str. 49b
 D 50674 Köln, Germany
;
data_I
_chemical_name_common     'Glycine lithium sulfate'
_chemical_formula_moiety     'C2 H5 Li2 N O6 S'
_chemical_formula_sum     'C2 H5 Li2 N O6 S'
_chemical_formula_iupac     '[Li2 (S O4) (C2 H5 O2 N)]'
_chemical_formula_weight     185.01
_chemical_melting_point     'not determined'
_symmetry_cell_setting     orthorhombic
_symmetry_space_group_name_H-M     'P n a 21'
_symmetry_space_group_name_Hall     'P 2c -2n'
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     16.423(3)
_cell_length_b     5.0050(10)
_cell_length_c     7.654(2)
_cell_angle_alpha     90.00
_cell_angle_beta     90.00
_cell_angle_gamma     90.00
_cell_volume     629.1(2)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     1054
_cell_measurement_theta_min     4.076
_cell_measurement_theta_max     30.034
_cell_measurement_temperature     293(2)
_exptl_crystal_description     prism
_exptl_crystal_colour     colourless
_exptl_crystal_size_max     0.40
_exptl_crystal_size_mid     0.20
_exptl_crystal_size_min     0.20
_exptl_crystal_density_diffrn     1.953
_exptl_crystal_density_meas     'not measured'
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     376
_exptl_absorpt_coefficient_mu     0.494
_exptl_absorpt_correction_type     'multi-scan'
_exptl_absorpt_process_details     '(Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min     0.8268
_exptl_absorpt_correction_T_max     0.9076
_exptl_special_details
;
Single-crystal X-ray intensity data were collected
at 293 K on a Nonius Kappa diffractometer with CCD-area detector, using
282 frames  with phi- and omega-increments of 1
degrees and a counting time of 20 seconds per frame. The crystal-
to-detector-distance was 30 mm. The whole ewald sphere was measured.
The reflection data were processed
with the Nonius program suite DENZO-SMN and corrected for Lorentz,
polarisation, background and absorption effects (Otwinowski and Minor, 1997).
The crystal structure was determined by Direct methods (SHELXS-97,
Sheldrick, 1997) and subsequent Fourier and difference
Fourier syntheses, followed by full-matrix least-squares refinements on F²
(SHELXL-97, Sheldrick, 1997). All hydrogen atoms were refined freely.
;
_diffrn_ambient_temperature     293(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Nonius Kappa CCD diffractometer'
_diffrn_measurement_device     '95mm CCD camera on κ-goniostat'
_diffrn_measurement_method     'φ and ω scans'
_diffrn_detector_area_resol_mean     9
_diffrn_reflns_number     1653
_diffrn_reflns_av_R_equivalents     0.0000
_diffrn_reflns_av_sigmaI/netI     0.0244
_diffrn_reflns_theta_min     4.26
_diffrn_reflns_theta_max     30.03
_diffrn_reflns_theta_full     30.03
_diffrn_measured_fraction_theta_max     0.984
_diffrn_measured_fraction_theta_full     0.984
_diffrn_reflns_limit_h_min     -22
_diffrn_reflns_limit_h_max     23
_diffrn_reflns_limit_k_min     -7
_diffrn_reflns_limit_k_max     7
_diffrn_reflns_limit_l_min     -10
_diffrn_reflns_limit_l_max     10
_diffrn_standards_number     none
_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.
;
_reflns_number_total     1653
_reflns_number_gt     1582
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0266
_refine_ls_R_factor_gt     0.0246
_refine_ls_wR_factor_gt     0.0646
_refine_ls_wR_factor_ref     0.0660
_refine_ls_goodness_of_fit_ref     1.090
_refine_ls_restrained_S_all     1.089
_refine_ls_number_reflns     1653
_refine_ls_number_parameters     130
_refine_ls_number_restraints     1
_refine_ls_hydrogen_treatment     refall
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
          'calc w=1/[σ²(Fo²)+(0.0387P)²+0.088P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.001
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.279
_refine_diff_density_min     -0.358
_refine_ls_extinction_method     SHELXL97
_refine_ls_extinction_coef     0.013(7)
_refine_ls_extinction_expression
                                  'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details
                                    'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack     0.021(4)
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'
    'Li' 'Li' -0.0003 0.0001
                         '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'
_computing_data_collection     'COLLECT (Nonius, 2003)'
_computing_cell_refinement     'HKL SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction
                            'HKL DENZO (Otwinowski & Minor, 1997) and SCALEPACK'
_computing_structure_solution     'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics     'DIAMOND (Bergerhoff et al., 1997)'
_computing_publication_material     'SHELXL97'
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Li1 0.6948(3) 0.7389(6) 0.4648(5) 0.0179(8) Uani d . 1 . . Li
    Li2 0.7977(2) 0.2373(7) 0.5271(5) 0.0201(8) Uani d . 1 . . Li
    S 0.668617(16) 0.23198(5) 0.24330(12) 0.01183(11) Uani d . 1 . . S
    O1S 0.58049(6) 0.2620(2) 0.2328(5) 0.0247(3) Uani d . 1 . . O
    O2S 0.69785(7) 0.3563(3) 0.40610(17) 0.0203(3) Uani d . 1 . . O
    O3S 0.70821(8) 0.3604(3) 0.09065(18) 0.0196(3) Uani d . 1 . . O
    O4S 0.69165(5) -0.05380(17) 0.2446(3) 0.01856(19) Uani d . 1 . . O
    O1 0.60013(8) 0.8445(3) 0.59255(17) 0.0234(3) Uani d . 1 . . O
    O2 0.61244(9) 0.8091(3) 0.8828(2) 0.0266(3) Uani d . 1 . . O
    C1 0.59173(7) 0.9283(2) 0.7464(3) 0.0167(2) Uani d . 1 . . C
    C2 0.55194(11) 1.1987(3) 0.7733(2) 0.0227(4) Uani d . 1 . . C
    H1C 0.5123(18) 1.183(6) 0.863(4) 0.039(7) Uiso d . 1 . . H
    H2C 0.5921(15) 1.320(5) 0.810(3) 0.034(6) Uiso d . 1 . . H
    N 0.51813(10) 1.3043(4) 0.6094(2) 0.0266(3) Uani d . 1 . . N
    H1N 0.5538(18) 1.294(5) 0.530(5) 0.043(7) Uiso d . 1 . . H
    H2N 0.471(2) 1.205(6) 0.597(5) 0.064(9) Uiso d . 1 . . H
    H3N 0.4959(18) 1.452(6) 0.627(4) 0.052(8) Uiso d . 1 . . H
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    Li1 0.0202(16) 0.0154(19) 0.0182(19) 0.0008(10) -0.0008(14) 0.0011(11)
    Li2 0.0257(19) 0.0181(19) 0.0166(19) 0.0004(11) -0.0002(15) 0.0021(11)
    S 0.01380(15) 0.01120(15) 0.01050(15) 0.00120(9) 0.0003(2) 0.0005(2)
    O1S 0.0128(5) 0.0316(5) 0.0296(8) 0.0031(3) 0.0002(7) 0.0056(6)
    O2S 0.0305(6) 0.0165(7) 0.0138(6) 0.0024(5) -0.0042(5) -0.0034(6)
    O3S 0.0250(6) 0.0154(6) 0.0183(6) 0.0023(5) 0.0076(5) 0.0051(6)
    O4S 0.0316(5) 0.0114(4) 0.0127(4) 0.0032(3) -0.0005(6) 0.0003(6)
    O1 0.0256(6) 0.0248(6) 0.0199(6) 0.0035(5) 0.0041(5) -0.0024(6)
    O2 0.0307(7) 0.0295(7) 0.0197(7) 0.0047(6) -0.0049(6) 0.0041(6)
    C1 0.0148(5) 0.0172(5) 0.0181(5) -0.0018(4) 0.0000(8) 0.0012(8)
    C2 0.0307(8) 0.0189(6) 0.0183(10) 0.0023(6) -0.0039(6) -0.0016(6)
    N 0.0350(8) 0.0245(7) 0.0203(7) 0.0119(6) -0.0020(6) -0.0023(6)
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Li1 O1 . 1.911(4) y
    Li1 O3S 4_655 1.958(4) y
    Li1 O2S . 1.968(4) y
    Li1 O4S 1_565 1.980(4) y
    Li2 O2 4_644 1.878(4) y
    Li2 O3S 4_645 1.950(4) y
    Li2 O4S 4_655 1.973(5) y
    Li2 O2S . 1.976(4) y
    S O1S . 1.4573(11) y
    S O2S . 1.4732(17) y
    S O4S . 1.4796(9) y
    S O3S . 1.4837(17) y
    O3S Li2 4_654 1.950(4) y
    O3S Li1 4_644 1.958(4) y
    O4S Li2 4_644 1.973(5) y
    O4S Li1 1_545 1.980(4) ?
    O1 C1 . 1.258(3) y
    O2 C1 . 1.249(3) y
    C1 C2 . 1.517(2) y
    C2 N . 1.470(2) y
    C2 H1C . 0.95(3) y
    C2 H2C . 0.94(3) y
    N H1N . 0.84(3) y
    N H2N . 0.92(4) y
    N H3N . 0.83(3) y
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    O1 Li1 O3S . 4_655 108.9(2) ?
    O1 Li1 O2S . . 114.0(2) ?
    O3S Li1 O2S 4_655 . 113.21(19) ?
    O1 Li1 O4S . 1_565 105.62(18) ?
    O3S Li1 O4S 4_655 1_565 106.10(19) ?
    O2S Li1 O4S . 1_565 108.42(19) ?
    O1 Li1 S . 1_565 86.87(13) ?
    O3S Li1 S 4_655 1_565 97.93(13) ?
    O2S Li1 S . 1_565 132.03(18) ?
    O4S Li1 S 1_565 1_565 24.72(6) ?
    O1 Li1 Li2 . 1_565 98.32(15) ?
    O3S Li1 Li2 4_655 1_565 38.60(9) ?
    O2S Li1 Li2 . 1_565 144.83(17) ?
    O4S Li1 Li2 1_565 1_565 73.69(13) ?
    S Li1 Li2 1_565 1_565 59.96(10) ?
    O1 Li1 Li2 . . 126.58(16) ?
    O3S Li1 Li2 4_655 . 74.29(10) ?
    O2S Li1 Li2 . . 39.12(14) ?
    O4S Li1 Li2 1_565 . 125.18(15) ?
    S Li1 Li2 1_565 . 146.52(12) ?
    Li2 Li1 Li2 1_565 . 109.87(11) ?
    O1 Li1 Li2 . 4_654 122.8(2) ?
    O3S Li1 Li2 4_655 4_654 117.6(2) ?
    O2S Li1 Li2 . 4_654 76.61(14) ?
    O4S Li1 Li2 1_565 4_654 31.94(9) ?
    S Li1 Li2 1_565 4_654 56.42(10) ?
    Li2 Li1 Li2 1_565 4_654 97.92(14) ?
    Li2 Li1 Li2 . 4_654 97.67(13) ?
    O2 Li2 O3S 4_644 4_645 111.8(2) ?
    O2 Li2 O4S 4_644 4_655 109.00(19) ?
    O3S Li2 O4S 4_645 4_655 107.9(2) ?
    O2 Li2 O2S 4_644 . 108.6(2) ?
    O3S Li2 O2S 4_645 . 111.51(19) ?
    O4S Li2 O2S 4_655 . 108.00(19) ?
    O2 Li2 S 4_644 4_655 91.25(14) ?
    O3S Li2 S 4_645 4_655 131.57(19) ?
    O4S Li2 S 4_655 4_655 24.49(6) ?
    O2S Li2 S . 4_655 99.28(14) ?
    O2 Li2 S 4_644 . 97.43(16) ?
    O3S Li2 S 4_645 . 97.75(15) ?
    O4S Li2 S 4_655 . 132.06(17) ?
    O2S Li2 S . . 24.11(8) ?
    S Li2 S 4_655 . 121.71(12) ?
    O2 Li2 Li1 4_644 1_545 119.99(16) ?
    O3S Li2 Li1 4_645 1_545 38.77(13) ?
    O4S Li2 Li1 4_655 1_545 127.87(14) ?
    O2S Li2 Li1 . 1_545 73.32(10) ?
    S Li2 Li1 4_655 1_545 148.74(12) ?
    S Li2 Li1 . 1_545 59.60(7) ?
    O2 Li2 Li1 4_644 . 100.67(16) ?
    O3S Li2 Li1 4_645 . 143.47(16) ?
    O4S Li2 Li1 4_655 . 75.27(14) ?
    O2S Li2 Li1 . . 38.93(8) ?
    S Li2 Li1 4_655 . 61.04(11) ?
    S Li2 Li1 . . 60.69(7) ?
    Li1 Li2 Li1 1_545 . 109.87(11) ?
    O2 Li2 Li1 4_644 4_645 124.0(2) ?
    O3S Li2 Li1 4_645 4_645 75.82(15) ?
    O4S Li2 Li1 4_655 4_645 32.07(9) ?
    O2S Li2 Li1 . 4_645 119.9(2) ?
    S Li2 Li1 4_655 4_645 56.32(10) ?
    S Li2 Li1 . 4_645 137.78(19) ?
    Li1 Li2 Li1 1_545 4_645 100.27(14) ?
    Li1 Li2 Li1 . 4_645 100.00(14) ?
    O1S S O2S . . 109.07(13) ?
    O1S S O4S . . 110.73(6) ?
    O2S S O4S . . 108.62(11) ?
    O1S S O3S . . 110.32(12) ?
    O2S S O3S . . 109.89(6) ?
    O4S S O3S . . 108.18(10) ?
    O1S S Li1 . 1_545 104.84(11) ?
    O2S S Li1 . 1_545 79.86(10) ?
    O3S S Li1 . 1_545 137.11(10) ?
    O1S S Li2 . 4_644 103.61(12) ?
    O2S S Li2 . 4_644 138.41(10) ?
    O3S S Li2 . 4_644 81.03(10) ?
    Li1 S Li2 1_545 4_644 67.26(6) ?
    O1S S Li2 . . 137.07(15) ?
    O4S S Li2 . . 79.94(10) ?
    O3S S Li2 . . 104.69(10) ?
    Li1 S Li2 1_545 . 60.45(11) ?
    Li2 S Li2 4_644 . 105.71(8) ?
    Li2 O4S Li1 4_644 1_545 116.00(10) ?
    O2 C1 O1 . . 126.41(13) ?
    O2 C1 C2 . . 115.5(2) ?
    O1 C1 C2 . . 118.13(18) ?
    N C2 C1 . . 111.59(16) ?
    N C2 H1C . . 112.8(18) ?
    C1 C2 H1C . . 108.7(19) ?
    N C2 H2C . . 106.8(16) ?
    C1 C2 H2C . . 108.3(16) ?
    H1C C2 H2C . . 109(2) ?
    C2 N H1N . . 109(2) ?
    C2 N H2N . . 102(2) ?
    H1N N H2N . . 118(3) ?
    C2 N H3N . . 110(2) ?
    H1N N H3N . . 118(3) ?
    H2N N H3N . . 97(3) ?
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    N H1N O1S 1_565 0.84(3) 2.32(4) 3.066(4) 147(3)
    N H2N O2 2_674 0.92(4) 2.14(4) 2.816(2) 130(3)
    N H3N O1S 2_675 0.83(3) 2.07(3) 2.868(2) 160(3)
data_II
_chemical_name_common     'Glycine nickel dichloride dihydrate'
_chemical_formula_moiety     'C2 H9 Cl2 N Ni O4'
_chemical_formula_sum     'C2 H9 Cl2 N Ni O4'
_chemical_formula_iupac     '[Ni Cl2 (C2 H5 O2 N) (H2 O)2]'
_chemical_formula_weight     240.71
_chemical_melting_point     'not determined'
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'P 21'
_symmetry_space_group_name_Hall     'P 2yb'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, y+1/2, -z'
_cell_length_a     8.203(2)
_cell_length_b     5.4750(10)
_cell_length_c     8.311(2)
_cell_angle_alpha     90.00
_cell_angle_beta     90.97(3)
_cell_angle_gamma     90.00
_cell_volume     373.21(14)
_cell_formula_units_Z     2
_cell_measurement_reflns_used     1197
_cell_measurement_theta_min     4.076
_cell_measurement_theta_max     30.034
_cell_measurement_temperature     293(2)
_exptl_crystal_description     prism
_exptl_crystal_colour     green
_exptl_crystal_size_max     0.20
_exptl_crystal_size_mid     0.10
_exptl_crystal_size_min     0.10
_exptl_crystal_density_diffrn     2.142
_exptl_crystal_density_meas     'not measured'
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     244
_exptl_absorpt_coefficient_mu     3.271
_exptl_absorpt_correction_type     'multi-scan'
_exptl_absorpt_process_details     '(Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min     0.5607
_exptl_absorpt_correction_T_max     0.7356
_exptl_special_details
;
Single-crystal X-ray intensity data were collected
at 293 K on a Nonius Kappa diffractometer with CCD-area detector,
using 318 frames with an omega-increment of 2 degrees and
a counting time of 30 seconds per frame. The crystal to detector
distance was 25 mm. The whole ewald sphere was measured.
The reflection data were processed
with the Nonius program suite DENZO-SMN and corrected for Lorentz,
polarisation, background and absorption effects (Otwinowski and Minor, 1997).
The crystal structure was determined by automatic patterson methods
(SHELXS-97, Sheldrick, 1997) and subsequent Fourier and difference
Fourier syntheses, followed by full-matrix least-squares refinements on F²
(SHELXL-97, Sheldrick, 1997). All hydrogen atoms were refined freely.
;
_diffrn_ambient_temperature     293(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Nonius Kappa CCD diffractometer'
_diffrn_measurement_device     '95mm CCD camera on κ-goniostat'
_diffrn_measurement_method     'ω scans'
_diffrn_detector_area_resol_mean     9
_diffrn_reflns_number     2170
_diffrn_reflns_av_R_equivalents     0.0000
_diffrn_reflns_av_sigmaI/netI     0.0201
_diffrn_reflns_theta_min     4.46
_diffrn_reflns_theta_max     30.03
_diffrn_reflns_theta_full     30.03
_diffrn_measured_fraction_theta_max     0.997
_diffrn_measured_fraction_theta_full     0.997
_diffrn_reflns_limit_h_min     -11
_diffrn_reflns_limit_h_max     11
_diffrn_reflns_limit_k_min     -7
_diffrn_reflns_limit_k_max     7
_diffrn_reflns_limit_l_min     -11
_diffrn_reflns_limit_l_max     11
_diffrn_standards_number     none
_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.
;
_reflns_number_total     2170
_reflns_number_gt     2142
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0161
_refine_ls_R_factor_gt     0.0157
_refine_ls_wR_factor_gt     0.0375
_refine_ls_wR_factor_ref     0.0376
_refine_ls_goodness_of_fit_ref     1.125
_refine_ls_restrained_S_all     1.125
_refine_ls_number_reflns     2170
_refine_ls_number_parameters     128
_refine_ls_number_restraints     1
_refine_ls_hydrogen_treatment     refall
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
          'calc w=1/[σ²(Fo²)+(0.0166P)²+0.065P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.003
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.289
_refine_diff_density_min     -0.338
_refine_ls_extinction_method     SHELXL97
_refine_ls_extinction_coef     0.127(3)
_refine_ls_extinction_expression
                                  'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details
                                    'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack     0.002(8)
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'
    'Cl' 'Cl' 0.1484 0.1585
                         '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'
_computing_data_collection     'COLLECT (Nonius, 2003)'
_computing_cell_refinement     'HKL SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction
                            'HKL DENZO (Otwinowski & Minor, 1997) and SCALEPACK'
_computing_structure_solution     'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics     'ATOMS  (Dowty, 1999)'
_computing_publication_material     'SHELXL97'
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Ni 0.784803(18) 0.78457(3) 0.334887(18) 0.01347(6) Uani d . 1 . . Ni
    Cl1 0.54116(4) 0.54991(7) 0.25002(4) 0.02017(8) Uani d . 1 . . Cl
    Cl2 0.77352(4) 0.99840(7) 0.08732(4) 0.02162(9) Uani d . 1 . . Cl
    O1 1.00165(12) 0.4518(2) 0.58500(13) 0.0183(2) Uani d . 1 . . O
    O2 0.76111(13) 0.6377(2) 0.56224(13) 0.0179(2) Uani d . 1 . . O
    C1 0.86615(16) 0.5169(3) 0.63931(16) 0.0149(2) Uani d . 1 . . C
    C2 0.8260(2) 0.4484(4) 0.8103(2) 0.0277(4) Uani d . 1 . . C
    H1C 0.830(3) 0.259(6) 0.821(3) 0.041(6) Uiso d . 1 . . H
    H2C 0.895(3) 0.509(5) 0.879(3) 0.043(7) Uiso d . 1 . . H
    N 0.66229(16) 0.5314(3) 0.85727(17) 0.0212(3) Uani d . 1 . . N
    H1N 0.648(4) 0.541(8) 0.960(4) 0.074(10) Uiso d . 1 . . H
    H2N 0.580(5) 0.435(8) 0.804(5) 0.090(13) Uiso d . 1 . . H
    H3N 0.637(5) 0.679(8) 0.814(5) 0.086(13) Uiso d . 1 . . H
    O1W 0.92928(14) 0.4953(2) 0.26258(14) 0.0200(2) Uani d . 1 . . O
    H1W1 0.889(4) 0.364(6) 0.225(4) 0.063(9) Uiso d . 1 . . H
    H2W1 0.964(3) 0.449(6) 0.364(4) 0.046(7) Uiso d . 1 . . H
    O2W 0.65320(18) 1.0653(3) 0.43031(17) 0.0329(3) Uani d . 1 . . O
    H1W2 0.598(3) 1.046(7) 0.520(4) 0.063(9) Uiso d . 1 . . H
    H2W2 0.631(3) 1.180(6) 0.386(4) 0.047(8) Uiso d . 1 . . H
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    Ni 0.01401(8) 0.01378(9) 0.01262(9) 0.00057(6) 0.00000(5) 0.00155(7)
    Cl1 0.01818(15) 0.02103(17) 0.02124(16) -0.00242(12) -0.00178(11)
                                                                     0.00289(13)
    Cl2 0.02621(17) 0.02273(18) 0.01585(15) -0.00328(13) -0.00192(12)
                                                                     0.00540(13)
    O1 0.0166(5) 0.0224(5) 0.0160(5) 0.0052(4) 0.0011(4) 0.0028(4)
    O2 0.0175(5) 0.0220(5) 0.0143(5) 0.0047(4) 0.0007(4) 0.0052(4)
    C1 0.0165(6) 0.0140(6) 0.0142(6) -0.0013(5) 0.0000(4) 0.0013(5)
    C2 0.0197(7) 0.0439(11) 0.0198(7) 0.0079(7) 0.0042(6) 0.0145(7)
    N 0.0212(6) 0.0249(7) 0.0177(6) -0.0015(5) 0.0042(4) -0.0010(5)
    O1W 0.0228(5) 0.0183(5) 0.0191(5) 0.0032(4) 0.0006(4) -0.0011(4)
    O2W 0.0459(8) 0.0223(6) 0.0312(6) 0.0161(6) 0.0197(6) 0.0100(6)
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Ni O2W . 2.0457(14) y
    Ni O2 . 2.0658(11) y
    Ni O1W . 2.0732(12) y
    Ni O1 2_756 2.0762(11) y
    Ni Cl2 . 2.3677(6) y
    Ni Cl1 . 2.4688(6) y
    O1 C1 . 1.2582(17) y
    O2 C1 . 1.2534(18) y
    C1 C2 . 1.512(2) y
    C2 N . 1.477(2) y
    C2 H1C . 1.04(4) y
    C2 H2C . 0.86(3) y
    N H1N . 0.86(3) y
    N H2N . 0.96(4) y
    N H3N . 0.91(4) y
    O1W H1W1 . 0.85(4) y
    O1W H2W1 . 0.92(3) y
    O2W H1W2 . 0.89(3) y
    O2W H2W2 . 0.75(3) y
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    O2W Ni O2 . . 83.08(5) ?
    O2W Ni O1W . . 173.85(5) ?
    O2 Ni O1W . . 91.76(5) ?
    O2W Ni O1 . 2_756 89.56(6) ?
    O2 Ni O1 . 2_756 88.30(5) ?
    O1W Ni O1 . 2_756 86.93(5) ?
    O2W Ni Cl2 . . 87.27(4) ?
    O2 Ni Cl2 . . 169.89(3) ?
    O1W Ni Cl2 . . 98.05(4) ?
    O1 Ni Cl2 2_756 . 94.64(4) ?
    O2W Ni Cl1 . . 94.11(5) ?
    O2 Ni Cl1 . . 88.31(4) ?
    O1W Ni Cl1 . . 89.06(4) ?
    O1 Ni Cl1 2_756 . 174.67(3) ?
    Cl2 Ni Cl1 . . 89.40(3) ?
    O2 C1 O1 . . 124.74(13) ?
    O2 C1 C2 . . 116.91(13) ?
    O1 C1 C2 . . 118.35(13) ?
    N C2 C1 . . 112.68(13) ?
    N C2 H1C . . 108.1(14) ?
    C1 C2 H1C . . 108.7(14) ?
    N C2 H2C . . 107.1(17) ?
    C1 C2 H2C . . 112.0(17) ?
    H1C C2 H2C . . 108(2) ?
    C2 N H1N . . 115(2) ?
    C2 N H2N . . 110(2) ?
    H1N N H2N . . 113(3) ?
    C2 N H3N . . 112(3) ?
    H1N N H3N . . 108(4) ?
    H2N N H3N . . 99(3) ?
    Ni O1W H1W1 . . 122(2) ?
    Ni O1W H2W1 . . 96.6(18) ?
    H1W1 O1W H2W1 . . 102(3) ?
    Ni O2W H1W2 . . 121(2) ?
    Ni O2W H2W2 . . 125(2) ?
    H1W2 O2W H2W2 . . 113(3) ?
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    N H1N Cl1 1_556 0.86(3) 2.58(3) 3.4296(17) 167(3)
    N H2N Cl1 2_646 0.96(4) 2.37(4) 3.2372(16) 150(4)
    N H3N Cl1 2_656 0.91(4) 2.55(4) 3.4042(17) 156(4)
    O1W H1W1 Cl2 1_545 0.85(4) 2.49(4) 3.3304(14) 174(3)
    O1W H2W1 O1 . 0.92(3) 1.86(3) 2.7451(17) 161(3)
    O2W H1W2 Cl1 2_656 0.89(3) 2.24(3) 3.1226(16) 172(3)
    O2W H2W2 Cl1 1_565 0.75(3) 2.43(3) 3.1756(15) 176(3)
data_III
_chemical_name_common     'Glycine zinc sulfate trihydrate'
_chemical_formula_moiety     'C2 H11 N O9 S Zn'
_chemical_formula_sum     'C2 H11 N O9 S Zn'
_chemical_formula_iupac     '[Zn (S O4) (C2 H5 O2 N) (H2 O)3]'
_chemical_formula_weight     290.55
_chemical_melting_point     'not determined'
_symmetry_cell_setting     orthorhombic
_symmetry_space_group_name_H-M     'P c a 21'
_symmetry_space_group_name_Hall     'P 2c -2ac'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, -y, z+1/2'
    'x+1/2, -y, z'
    '-x+1/2, y, z+1/2'
_cell_length_a     8.440(2)
_cell_length_b     8.278(2)
_cell_length_c     12.521(3)
_cell_angle_alpha     90.00
_cell_angle_beta     90.00
_cell_angle_gamma     90.00
_cell_volume     874.8(4)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     2456
_cell_measurement_theta_min     3.45
_cell_measurement_theta_max     37.78
_cell_measurement_temperature     293(2)
_exptl_crystal_description     prism
_exptl_crystal_colour     colourless
_exptl_crystal_size_max     0.10
_exptl_crystal_size_mid     0.05
_exptl_crystal_size_min     0.05
_exptl_crystal_density_diffrn     2.206
_exptl_crystal_density_meas     'not measured'
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     592
_exptl_absorpt_coefficient_mu     3.079
_exptl_absorpt_correction_type     'multi-scan'
_exptl_absorpt_process_details     '(Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min     0.7482
_exptl_absorpt_correction_T_max     0.8613
_exptl_special_details
;
Single-crystal X-ray intensity data were collected
at 293 K on a Nonius Kappa diffractometer with CCD-area detector,
using 476 frames with an omega-increment of 2 degrees and
a counting time of 100 seconds per frame. The crystal to detector
distance was 25 mm. The whole ewald sphere was measured.
The reflection data were processed
with the Nonius program suite DENZO-SMN and corrected for Lorentz,
polarisation, background and absorption effects (Otwinowski and Minor, 1997).
The crystal structure was determined by automatic patterson methods
(SHELXS-97, Sheldrick, 1997) and subsequent Fourier and difference
Fourier syntheses, followed by full-matrix least-squares refinements on F²
(SHELXL-97, Sheldrick, 1997). All hydrogen atoms were refined freely.
The crystals proved to racemic twins, therefore TWIN refinement was employed.
;
_diffrn_ambient_temperature     293(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Nonius Kappa CCD diffractometer'
_diffrn_measurement_device     '95mm CCD camera on κ-goniostat'
_diffrn_measurement_method     'omega-scans'
_diffrn_detector_area_resol_mean     9
_diffrn_reflns_number     4460
_diffrn_reflns_av_R_equivalents     0.0000
_diffrn_reflns_av_sigmaI/netI     0.0370
_diffrn_reflns_theta_min     3.45
_diffrn_reflns_theta_max     37.78
_diffrn_reflns_theta_full     37.78
_diffrn_measured_fraction_theta_max     0.996
_diffrn_measured_fraction_theta_full     0.996
_diffrn_reflns_limit_h_min     -14
_diffrn_reflns_limit_h_max     14
_diffrn_reflns_limit_k_min     -14
_diffrn_reflns_limit_k_max     14
_diffrn_reflns_limit_l_min     -21
_diffrn_reflns_limit_l_max     21
_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.
;
_reflns_number_total     4460
_reflns_number_gt     3901
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0399
_refine_ls_R_factor_gt     0.0301
_refine_ls_wR_factor_gt     0.0628
_refine_ls_wR_factor_ref     0.0669
_refine_ls_goodness_of_fit_ref     1.018
_refine_ls_restrained_S_all     1.018
_refine_ls_number_reflns     4460
_refine_ls_number_parameters     172
_refine_ls_number_restraints     1
_refine_ls_hydrogen_treatment     refall
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
          'calc w=1/[σ²(Fo²)+(0.0230P)²+0.336P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.001
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.643
_refine_diff_density_min     -0.474
_refine_ls_extinction_method     SHELXL97
_refine_ls_extinction_coef     0.0018(8)
_refine_ls_extinction_expression
                                  'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details
                                    'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack     0.006(3)
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'
    'Zn' 'Zn' 0.2839 1.4301
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'COLLECT (Nonius, 2003)'
_computing_cell_refinement     'HKL SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction
                            'HKL DENZO (Otwinowski & Minor, 1997) and SCALEPACK'
_computing_structure_solution     'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics     'ATOMS  (Dowty, 1999)'
_computing_publication_material     'SHELXL97'
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Zn 0.04955(2) 0.19651(2) 0.497340(18) 0.01759(5) Uani d . 1 . . Zn
    S 0.02497(5) 0.27959(5) 0.75223(4) 0.01762(7) Uani d . 1 . . S
    O1S -0.1399(2) 0.2522(2) 0.78387(15) 0.0325(3) Uani d . 1 . . O
    O2S 0.1220(2) 0.1356(2) 0.77214(14) 0.0294(3) Uani d . 1 . . O
    O3S 0.0306(2) 0.32374(19) 0.63729(12) 0.0290(3) Uani d . 1 . . O
    O4S 0.0917(2) 0.4204(2) 0.81091(14) 0.0284(3) Uani d . 1 . . O
    O1 0.27904(15) 0.11371(17) 0.50738(15) 0.0246(3) Uani d . 1 . . O
    O2 0.51595(18) 0.03689(17) 0.56383(14) 0.0262(3) Uani d . 1 . . O
    C1 0.4077(2) 0.1384(2) 0.55399(14) 0.0171(3) Uani d . 1 . . C
    C2 0.4362(2) 0.3058(2) 0.60084(19) 0.0231(3) Uani d . 1 . . C
    H1C 0.370(5) 0.318(5) 0.660(3) 0.049(10) Uiso d . 1 . . H
    H2C 0.416(4) 0.386(5) 0.539(3) 0.038(9) Uiso d . 1 . . H
    N 0.5949(3) 0.3198(3) 0.6477(2) 0.0326(4) Uani d . 1 . . N
    H1N 0.668(5) 0.306(4) 0.590(3) 0.043(10) Uiso d . 1 . . H
    H2N 0.606(5) 0.406(7) 0.688(4) 0.067(12) Uiso d . 1 . . H
    H3N 0.592(6) 0.254(7) 0.688(5) 0.077(17) Uiso d . 1 . . H
    O1W 0.1282(2) 0.41992(19) 0.43295(13) 0.0243(3) Uani d . 1 . . O
    H1W1 0.065(4) 0.460(4) 0.406(3) 0.027(8) Uiso d . 1 . . H
    H2W1 0.195(6) 0.404(5) 0.399(4) 0.066(14) Uiso d . 1 . . H
    O2W 0.0595(2) 0.1182(2) 0.33418(14) 0.0268(3) Uani d . 1 . . O
    H1W2 0.150(5) 0.120(5) 0.317(3) 0.045(10) Uiso d . 1 . . H
    H2W2 0.015(6) 0.030(6) 0.318(4) 0.070(13) Uiso d . 1 . . H
    O3W -0.19955(18) 0.2132(2) 0.47292(13) 0.0249(3) Uani d . 1 . . O
    H1W3 -0.218(5) 0.223(5) 0.403(4) 0.059(12) Uiso d . 1 . . H
    H2W3 -0.223(5) 0.120(6) 0.477(4) 0.066(13) Uiso d . 1 . . H
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    Zn 0.01679(7) 0.01588(8) 0.02010(8) 0.00075(6) -0.00041(9) 0.00027(8)
    S 0.01806(16) 0.01866(16) 0.01614(16) -0.00037(13) 0.00055(13) 0.00120(14)
    O1S 0.0208(7) 0.0430(10) 0.0338(8) -0.0044(6) 0.0043(6) 0.0028(7)
    O2S 0.0280(7) 0.0230(7) 0.0371(9) 0.0044(6) -0.0079(6) 0.0046(6)
    O3S 0.0494(10) 0.0202(6) 0.0173(6) 0.0033(6) 0.0047(6) 0.0017(5)
    O4S 0.0273(7) 0.0261(7) 0.0319(8) 0.0000(6) -0.0051(6) -0.0085(6)
    O1 0.0170(5) 0.0229(5) 0.0339(8) 0.0015(4) -0.0035(6) -0.0044(6)
    O2 0.0231(6) 0.0169(6) 0.0387(8) 0.0039(5) -0.0089(6) -0.0068(6)
    C1 0.0167(6) 0.0175(7) 0.0173(6) -0.0006(5) 0.0016(5) -0.0011(5)
    C2 0.0213(8) 0.0170(7) 0.0311(9) -0.0001(6) -0.0020(6) -0.0047(7)
    N 0.0244(8) 0.0311(10) 0.0425(11) 0.0000(7) -0.0061(8) -0.0173(9)
    O1W 0.0271(7) 0.0212(6) 0.0244(7) 0.0012(5) 0.0038(5) 0.0051(5)
    O2W 0.0269(7) 0.0261(7) 0.0274(7) -0.0008(6) 0.0007(5) -0.0073(6)
    O3W 0.0192(6) 0.0250(7) 0.0305(8) 0.0005(5) -0.0016(5) 0.0038(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_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Zn O3S . 2.0507(16) y
    Zn O1 . 2.0584(13) y
    Zn O2 3_455 2.1229(15) y
    Zn O1W . 2.1238(16) y
    Zn O3W . 2.1290(16) y
    Zn O2W . 2.1449(18) y
    S O1S . 1.4642(18) y
    S O2S . 1.4675(16) y
    S O3S . 1.4857(17) y
    S O4S . 1.4888(16) y
    O1 C1 . 1.249(2) y
    O2 C1 . 1.248(2) y
    C1 C2 . 1.524(3) y
    C2 N . 1.467(3) y
    C2 H1C . 0.93(4) y
    C2 H2C . 1.03(4) y
    N H1N . 0.95(4) y
    N H2N . 0.88(5) y
    N H3N . 0.75(6) y
    O1W H1W1 . 0.71(3) y
    O1W H2W1 . 0.72(5) y
    O2W H1W2 . 0.79(4) y
    O2W H2W2 . 0.85(5) y
    O3W H1W3 . 0.89(5) y
    O3W H2W3 . 0.80(5) y
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    O3S Zn O1 . . 101.09(7) ?
    O3S Zn O2 . 3_455 97.00(7) ?
    O1 Zn O2 . 3_455 78.38(6) ?
    O3S Zn O1W . . 84.35(7) ?
    O1 Zn O1W . . 91.10(7) ?
    O2 Zn O1W 3_455 . 169.47(6) ?
    O3S Zn O3W . . 90.70(7) ?
    O1 Zn O3W . . 163.65(6) ?
    O2 Zn O3W 3_455 . 89.05(6) ?
    O1W Zn O3W . . 101.40(7) ?
    O3S Zn O2W . . 166.43(7) ?
    O1 Zn O2W . . 85.45(7) ?
    O2 Zn O2W 3_455 . 95.96(7) ?
    O1W Zn O2W . . 83.64(7) ?
    O3W Zn O2W . . 85.50(6) ?
    O1S S O2S . . 111.00(11) ?
    O1S S O3S . . 109.29(11) ?
    O2S S O3S . . 110.28(10) ?
    O1S S O4S . . 110.34(10) ?
    O2S S O4S . . 109.94(10) ?
    O3S S O4S . . 105.87(10) ?
    O2 C1 O1 . . 124.95(17) ?
    O2 C1 C2 . . 117.30(16) ?
    O1 C1 C2 . . 117.75(16) ?
    N C2 C1 . . 111.71(16) ?
    N C2 H1C . . 103(3) ?
    C1 C2 H1C . . 108(2) ?
    N C2 H2C . . 113.6(18) ?
    C1 C2 H2C . . 106(2) ?
    H1C C2 H2C . . 115(3) ?
    C2 N H1N . . 106(2) ?
    C2 N H2N . . 113(3) ?
    H1N N H2N . . 117(3) ?
    C2 N H3N . . 101(4) ?
    H1N N H3N . . 116(5) ?
    H2N N H3N . . 102(6) ?
    Zn O1W H1W1 . . 110(3) ?
    Zn O1W H2W1 . . 108(4) ?
    H1W1 O1W H2W1 . . 113(5) ?
    Zn O2W H1W2 . . 107(3) ?
    Zn O2W H2W2 . . 118(3) ?
    H1W2 O2W H2W2 . . 112(4) ?
    Zn O3W H1W3 . . 109(3) ?
    Zn O3W H2W3 . . 100(3) ?
    H1W3 O3W H2W3 . . 96(4) ?
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    N H1N O3W 1_655 0.95(4) 2.00(4) 2.929(3) 164(3)
    N H2N O4S 3_565 0.88(5) 2.11(5) 2.967(3) 165(4)
    N H3N O2W 4 0.75(6) 2.49(6) 3.151(3) 148(5)
    O1W H1W1 O4S 2_564 0.71(3) 2.04(4) 2.744(2) 171(4)
    O1W H2W1 O4S 4_554 0.72(5) 2.12(5) 2.815(2) 164(5)
    O2W H1W2 O2S 4_554 0.79(4) 2.01(4) 2.802(2) 177(4)
    O2W H2W2 O2S 2_554 0.85(5) 1.88(5) 2.714(2) 167(5)
    O3W H1W3 O1S 4_454 0.89(5) 1.93(5) 2.747(2) 152(4)
    O3W H2W3 O1 3_455 0.80(5) 1.97(5) 2.746(2) 164(4)
