#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:31:37 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179583 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/48/4504857.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4504857
loop_
_publ_author_name
'Rujiwatra, Apinpus'
'Mander, Gavin J.'
'Kepert, Cameron J.'
'Rosseinsky, Matthew J.'
_publ_contact_author
;
      Apinpus Rujiwatra
      Department of Chemistry
    Faculty of Science
    Chiang Mai University
    Chiang Mai  50200
      Thailand 
;
_publ_section_title
;
 Synthesis and Characterization of Subcell−Supercell Related
 Ethylenediamine-Pillared Zinc Hydroxysulfates
;
_journal_issue                   1
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              183
_journal_paper_doi               10.1021/cg034242x
_journal_volume                  5
_journal_year                    2005
_chemical_compound_source
;
 'hydrothermal synthesis at 180 deg C for 3 days'
;
_chemical_formula_moiety         '(CNH4)7 (SO4)7 (OH)42 Zn28 (H2O)18'
_chemical_formula_sum            'C7 H106 N7 O88 S7 Zn28'
_chemical_formula_weight         3752.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   21.926(2)
_cell_length_b                   21.926(2)
_cell_length_c                   10.5643(9)
_cell_measurement_reflns_used    6444
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.98
_cell_measurement_theta_min      3.33
_cell_volume                     4398.4(7)
_computing_cell_refinement       'LSCELL (Clegg, 1997)'
_computing_data_collection       'Bruker AXS SMART'
_computing_data_reduction        'Bruker AXS SAINT'
_computing_molecular_graphics    X-STEP/DIAMOND
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_environment
;
 'In thin film of perfluorpolyether oil on glass fibre'
;
_diffrn_ambient_temperature      150(2)
_diffrn_crystal_treatment        'Flash cooled in nitrogen stream'
_diffrn_detector_area_resol_mean 8.912
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Brucker AXS SMART CCD diffractometer'
_diffrn_measurement_method       'omega rotation with narrow frames'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Daresbury SRS Station 9.8'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.69230
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            30736
_diffrn_reflns_theta_full        29.37
_diffrn_reflns_theta_max         29.37
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    7.542
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.832452
_exptl_absorpt_correction_type   Multiscans
_exptl_absorpt_process_details
;
 Mean and maximum errors in direction cosine check functions 
 are 0.001 and 0.003 respectively. 9323 reflections were 
 employed for parameter determination. R(int)= 0.1025 and 
 R(int) = 0.0279 before and after the  refinements with 
 final corrected 30736 reflections. The settings for 
 parameter refinements are (Intensity/sigma)threshold = 5.000 and 
 (Intensity + sigma)/(Mean intensity) threshold = 0.2500. 
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.805
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             3633
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.972
_refine_diff_density_min         -1.269
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         8089
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0792P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1555
_reflns_number_gt                3835
_reflns_number_total             8089
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg034242xsi20031203_072537.cif
_cod_data_source_block           rehydrated_phase_of_Zn8(SO4)2(OH)12(en).6(H2O)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4398.5(7)
_cod_database_code               4504857
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
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
Zn1 Zn 0.0000 0.0000 -0.16991(7) 0.00672(18) Uani 1 3 d S
Zn2 Zn 0.42898(2) 0.14121(2) -0.17286(4) 0.00559(12) Uani 1 1 d .
Zn3 Zn 0.71545(2) 0.56950(2) 0.16682(4) 0.00600(12) Uani 1 1 d .
Zn4 Zn 0.28788(2) 0.14027(2) -0.00628(5) 0.00712(13) Uani 1 1 d .
Zn5 Zn 0.42503(2) 0.28093(2) -0.00676(5) 0.00778(13) Uani 1 1 d .
Zn6 Zn 0.28833(2) 0.29106(2) -0.00768(4) 0.00753(13) Uani 1 1 d .
Zn7 Zn 0.42647(2) 0.43184(2) 0.00135(4) 0.00693(13) Uani 1 1 d .
Zn8 Zn 0.13812(2) 0.14115(2) -0.00656(5) 0.00779(13) Uani 1 1 d .
Zn9 Zn 0.57647(2) 0.42993(2) 0.00115(4) 0.00650(13) Uani 1 1 d .
Zn10 Zn 0.56597(2) 0.28388(2) -0.01616(5) 0.00772(13) Uani 1 1 d .
S1 S 0.23785(5) 0.19104(5) 0.26495(10) 0.0089(2) Uani 1 1 d .
S2 S 0.47421(5) 0.38230(5) -0.27628(10) 0.0087(2) Uani 1 1 d .
S3 S 0.6667 0.3333 0.26633(16) 0.0081(3) Uani 1 3 d S
O1 O 0.23742(13) 0.19051(13) 0.1223(3) 0.0086(6) Uani 1 1 d .
O2 O 0.6667 0.3333 0.1232(4) 0.0098(11) Uani 1 3 d S
O3 O 0.47345(13) 0.38108(13) -0.1334(3) 0.0087(6) Uani 1 1 d .
O4 O 0.61383(15) 0.26278(15) 0.3109(3) 0.0161(7) Uani 1 1 d .
O5 O 0.31114(15) 0.22048(16) 0.3068(3) 0.0194(7) Uani 1 1 d .
O6 O 0.49885(16) 0.33527(15) -0.3212(3) 0.0181(7) Uani 1 1 d .
O7 O 0.40222(15) 0.35882(17) -0.3214(3) 0.0201(7) Uani 1 1 d .
O8 O 0.19324(15) 0.11861(15) 0.3088(3) 0.0174(7) Uani 1 1 d .
O9 O 0.52224(15) 0.45557(15) -0.3168(3) 0.0177(7) Uani 1 1 d .
O10 O 0.20999(17) 0.23572(16) 0.3080(3) 0.0193(7) Uani 1 1 d .
O11 O 0.66801(14) 0.47186(14) 0.1047(3) 0.0081(6) Uani 1 1 d D
H11 H 0.661(3) 0.450(3) 0.177(3) 0.044(17) Uiso 1 1 d D
O12 O 0.47421(14) 0.24018(14) -0.1253(3) 0.0079(6) Uani 1 1 d .
H12 H 0.483(2) 0.258(2) -0.194(4) 0.023(14) Uiso 1 1 d .
O13 O 0.33134(14) 0.09135(14) -0.1136(3) 0.0076(6) Uani 1 1 d D
H13 H 0.307(2) 0.081(2) -0.184(3) 0.030(15) Uiso 1 1 d D
O14 O 0.81318(13) 0.62196(13) 0.1086(3) 0.0063(6) Uani 1 1 d D
H14 H 0.834(2) 0.632(2) 0.179(2) 0.009(11) Uiso 1 1 d D
O15 O 0.48100(13) 0.09540(13) -0.1136(3) 0.0069(6) Uani 1 1 d D
H15 H 0.4967 0.0813 -0.1917 0.008 Uiso 1 1 calc RD
O16 O 0.66392(14) 0.61712(14) 0.1165(3) 0.0085(6) Uani 1 1 d D
H16 H 0.654(3) 0.627(3) 0.191(3) 0.032(16) Uiso 1 1 d D
O17 O 0.04646(14) 0.09806(14) -0.1135(3) 0.0081(6) Uani 1 1 d D
H17 H 0.052(2) 0.119(2) -0.183(3) 0.023(14) Uiso 1 1 d D
O18 O 0.38334(13) 0.33606(13) 0.0846(3) 0.0076(6) Uani 1 1 d .
H18 H 0.3822 0.3347 0.1792 0.009 Uiso 1 1 calc R
O19 O 0.23867(13) 0.04639(13) 0.0908(3) 0.0072(6) Uani 1 1 d .
H19 H 0.2401 0.0491 0.1854 0.009 Uiso 1 1 calc R
O20 O 0.52025(14) 0.33235(13) 0.0787(3) 0.0082(6) Uani 1 1 d .
H20 H 0.5203 0.3298 0.1733 0.010 Uiso 1 1 calc R
O21 O 0.52386(13) 0.47290(13) 0.0895(3) 0.0071(6) Uani 1 1 d .
H21 H 0.5244 0.4736 0.1841 0.008 Uiso 1 1 calc R
O22 O 0.18958(13) 0.09686(13) -0.0920(3) 0.0077(6) Uani 1 1 d .
H22 H 0.1880 0.0942 -0.1865 0.009 Uiso 1 1 calc R
O23 O 0.62191(13) 0.38157(13) -0.0992(3) 0.0066(6) Uani 1 1 d .
H23 H 0.6204 0.3835 -0.1937 0.008 Uiso 1 1 calc R
O24 O 0.32946(14) 0.23495(13) -0.0938(3) 0.0074(6) Uani 1 1 d .
H24 H 0.3296 0.2346 -0.1884 0.009 Uiso 1 1 calc R
N1 N 0.0137(7) 0.0195(4) -0.3597(7) 0.009(2) Uiso 0.33 1 d P
H1A H -0.0064 0.0460 -0.3829 0.011 Uiso 0.33 1 calc PR
H1B H 0.0611 0.0454 -0.3771 0.011 Uiso 0.33 1 calc PR
C2 C -0.0173(9) -0.0446(7) -0.4339(9) 0.035(4) Uiso 0.33 1 d PD
H2A H -0.0572 -0.0832 -0.3877 0.044 Uiso 0.33 1 calc PR
H2B H 0.0181 -0.0589 -0.4515 0.044 Uiso 0.33 1 calc PR
N3 N 0.71752(19) 0.5581(2) 0.3559(3) 0.0232(9) Uani 1 1 d .
H3A H 0.6719 0.5319 0.3842 0.028 Uiso 1 1 calc R
H3B H 0.7397 0.5327 0.3725 0.028 Uiso 1 1 calc R
C4 C 0.7513(3) 0.6211(3) 0.4265(4) 0.0320(12) Uani 1 1 d D
H4A H 0.7216 0.6434 0.4255 0.040 Uiso 1 1 calc R
H4B H 0.7966 0.6540 0.3852 0.040 Uiso 1 1 calc R
C5 C 0.3904(3) 0.1562(3) -0.4323(4) 0.0342(13) Uani 1 1 d .
H5A H 0.4150 0.2083 -0.4307 0.043 Uiso 1 1 calc R
H5B H 0.3440 0.1384 -0.3908 0.043 Uiso 1 1 calc R
N6 N 0.43133(19) 0.13206(19) -0.3625(3) 0.0191(9) Uani 1 1 d .
H6A H 0.4774 0.1573 -0.3891 0.023 Uiso 1 1 calc R
H6B H 0.4149 0.0855 -0.3821 0.023 Uiso 1 1 calc R
O25 O 0.3862(2) 0.35453(19) 0.4058(4) 0.0414(10) Uani 1 1 d .
O26 O 0.5631(2) 0.4840(2) -0.5838(4) 0.0452(11) Uani 1 1 d .
O27 O 0.5000(2) 0.3219(2) 0.3409(4) 0.0482(11) Uani 1 1 d .
O28 O 0.0819(3) 0.1767(3) 0.4316(5) 0.092(2) Uani 1 1 d .
O29 O 0.6403(2) 0.4082(3) -0.4029(5) 0.0773(17) Uani 1 1 d .
O30 O 0.0371(3) 0.2631(3) 0.3311(5) 0.0841(17) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Zn Zn 0.2220 1.4310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1100 0.1240 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0020 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0080 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'
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
O17 Zn1 O17 111.16(8) . 3
O17 Zn1 O17 111.16(8) . 2
O17 Zn1 O17 111.16(8) 3 2
O17 Zn1 N1 110.2(5) . 2
O17 Zn1 N1 115.1(4) 3 2
O17 Zn1 N1 97.3(3) 2 2
O17 Zn1 N1 115.1(4) . 3
O17 Zn1 N1 97.3(3) 3 3
O17 Zn1 N1 110.2(5) 2 3
N1 Zn1 N1 18.6(4) 2 3
O17 Zn1 N1 97.3(3) . .
O17 Zn1 N1 110.2(5) 3 .
O17 Zn1 N1 115.1(4) 2 .
N1 Zn1 N1 18.6(4) 2 .
N1 Zn1 N1 18.6(4) 3 .
O12 Zn2 O13 110.19(12) . .
O12 Zn2 O15 112.69(11) . .
O13 Zn2 O15 111.45(11) . .
O12 Zn2 N6 110.06(14) . .
O13 Zn2 N6 109.73(14) . .
O15 Zn2 N6 102.47(13) . .
O14 Zn3 O16 110.84(11) . .
O14 Zn3 O11 111.27(12) . .
O16 Zn3 O11 110.97(12) . .
O14 Zn3 N3 107.37(14) . .
O16 Zn3 N3 112.94(15) . .
O11 Zn3 N3 103.18(14) . .
O24 Zn4 O19 174.35(11) . .
O24 Zn4 O22 95.90(11) . .
O19 Zn4 O22 81.61(11) . .
O24 Zn4 O13 101.04(12) . .
O19 Zn4 O13 84.41(11) . .
O22 Zn4 O13 99.40(11) . .
O24 Zn4 O14 84.09(11) . 2_655
O19 Zn4 O14 97.31(11) . 2_655
O22 Zn4 O14 168.25(11) . 2_655
O13 Zn4 O14 92.11(11) . 2_655
O24 Zn4 O1 81.90(10) . .
O19 Zn4 O1 92.67(10) . .
O22 Zn4 O1 80.94(10) . .
O13 Zn4 O1 176.97(10) . .
O14 Zn4 O1 87.44(11) 2_655 .
O20 Zn5 O24 176.51(11) . .
O20 Zn5 O18 95.73(11) . .
O24 Zn5 O18 81.65(11) . .
O20 Zn5 O14 98.60(11) . 2_655
O24 Zn5 O14 84.06(11) . 2_655
O18 Zn5 O14 97.06(10) . 2_655
O20 Zn5 O12 84.14(11) . .
O24 Zn5 O12 98.00(11) . .
O18 Zn5 O12 169.23(11) . .
O14 Zn5 O12 93.60(12) 2_655 .
O20 Zn5 O3 82.76(10) . .
O24 Zn5 O3 94.52(10) . .
O18 Zn5 O3 81.04(10) . .
O14 Zn5 O3 177.79(9) 2_655 .
O12 Zn5 O3 88.27(10) . .
O19 Zn6 O18 174.98(10) 6 .
O19 Zn6 O24 96.37(11) 6 .
O18 Zn6 O24 81.66(11) . .
O19 Zn6 O16 100.70(11) 6 4_665
O18 Zn6 O16 84.21(11) . 4_665
O24 Zn6 O16 100.02(11) . 4_665
O19 Zn6 O13 84.47(11) 6 6
O18 Zn6 O13 96.41(11) . 6
O24 Zn6 O13 166.94(11) . 6
O16 Zn6 O13 92.60(12) 4_665 6
O19 Zn6 O1 81.37(10) 6 .
O18 Zn6 O1 93.74(10) . .
O24 Zn6 O1 80.94(10) . .
O16 Zn6 O1 177.57(10) 4_665 .
O13 Zn6 O1 86.32(11) 6 .
O18 Zn7 O21 175.28(11) . 4_665
O18 Zn7 O21 95.78(11) . .
O21 Zn7 O21 82.00(12) 4_665 .
O18 Zn7 O15 101.01(11) . 6
O21 Zn7 O15 83.45(11) 4_665 6
O21 Zn7 O15 97.79(11) . 6
O18 Zn7 O16 84.05(11) . 4_665
O21 Zn7 O16 97.29(11) 4_665 4_665
O21 Zn7 O16 168.50(11) . 4_665
O15 Zn7 O16 93.51(12) 6 4_665
O18 Zn7 O3 81.91(10) . .
O21 Zn7 O3 93.66(10) 4_665 .
O21 Zn7 O3 82.95(10) . .
O15 Zn7 O3 176.88(10) 6 .
O16 Zn7 O3 85.65(10) 4_665 .
O22 Zn8 O19 97.73(11) . 6
O22 Zn8 O22 174.99(9) . 6
O19 Zn8 O22 81.94(11) 6 6
O22 Zn8 O17 100.57(11) . .
O19 Zn8 O17 99.31(11) 6 .
O22 Zn8 O17 84.41(11) 6 .
O22 Zn8 O17 83.99(11) . 5
O19 Zn8 O17 167.38(11) 6 5
O22 Zn8 O17 95.25(11) 6 5
O17 Zn8 O17 92.63(15) . 5
O22 Zn8 O1 82.40(10) . .
O19 Zn8 O1 81.37(10) 6 .
O22 Zn8 O1 92.61(10) 6 .
O17 Zn8 O1 176.81(10) . .
O17 Zn8 O1 86.49(10) 5 .
O20 Zn9 O21 96.66(11) . .
O20 Zn9 O11 101.46(11) . .
O21 Zn9 O11 101.58(12) . .
O20 Zn9 O23 82.04(11) . .
O21 Zn9 O23 174.75(10) . .
O11 Zn9 O23 83.66(11) . .
O20 Zn9 O15 165.44(12) . 3_665
O21 Zn9 O15 83.48(11) . 3_665
O11 Zn9 O15 92.73(11) . 3_665
O23 Zn9 O15 96.49(11) . 3_665
O20 Zn9 O3 80.23(10) . .
O21 Zn9 O3 81.67(10) . .
O11 Zn9 O3 176.06(10) . .
O23 Zn9 O3 93.10(10) . .
O15 Zn9 O3 85.40(10) 3_665 .
O23 Zn10 O20 174.93(11) 2_655 .
O23 Zn10 O23 97.03(15) 2_655 .
O20 Zn10 O23 81.98(11) . .
O23 Zn10 O12 100.85(11) 2_655 .
O20 Zn10 O12 84.22(11) . .
O23 Zn10 O12 100.25(11) . .
O23 Zn10 O11 83.64(11) 2_655 2_655
O20 Zn10 O11 96.07(11) . 2_655
O23 Zn10 O11 165.49(11) . 2_655
O12 Zn10 O11 93.82(12) . 2_655
O23 Zn10 O2 82.45(10) 2_655 .
O20 Zn10 O2 92.49(10) . .
O23 Zn10 O2 81.80(10) . .
O12 Zn10 O2 175.81(11) . .
O11 Zn10 O2 83.94(10) 2_655 .
O10 S1 O8 110.63(18) . .
O10 S1 O5 110.10(18) . .
O8 S1 O5 111.87(18) . .
O10 S1 O1 108.27(16) . .
O8 S1 O1 108.06(16) . .
O5 S1 O1 107.77(16) . .
O6 S2 O7 110.96(18) . .
O6 S2 O9 111.03(17) . .
O7 S2 O9 110.06(18) . .
O6 S2 O3 108.47(16) . .
O7 S2 O3 108.47(16) . .
O9 S2 O3 107.75(16) . .
O4 S3 O4 110.28(12) 2_655 .
O4 S3 O4 110.28(12) 2_655 3_665
O4 S3 O4 110.28(12) . 3_665
O4 S3 O2 108.65(13) 2_655 .
O4 S3 O2 108.65(13) . .
O4 S3 O2 108.65(13) 3_665 .
S1 O1 Zn8 126.12(15) . .
S1 O1 Zn4 125.45(15) . .
Zn8 O1 Zn4 89.68(10) . .
S1 O1 Zn6 125.33(15) . .
Zn8 O1 Zn6 89.42(10) . .
Zn4 O1 Zn6 89.32(10) . .
S3 O2 Zn10 127.60(9) . .
S2 O3 Zn5 126.00(15) . .
S2 O3 Zn7 127.13(15) . .
Zn5 O3 Zn7 89.84(10) . .
S2 O3 Zn9 125.47(14) . .
Zn5 O3 Zn9 87.96(10) . .
Zn7 O3 Zn9 88.14(10) . .
S3 O4 O27 88.33(14) . .
S1 O5 O25 121.39(18) . .
S2 O6 O29 112.88(19) . .
S2 O9 O26 119.12(17) . .
S2 O9 O29 89.01(16) . .
O26 O9 O29 66.70(14) . .
S1 O10 O28 120.1(2) . .
Zn3 O11 Zn9 122.08(14) . .
Zn3 O11 Zn10 122.37(13) . 3_665
Zn9 O11 Zn10 94.85(12) . 3_665
Zn3 O11 H11 99(4) . .
Zn9 O11 H11 111(4) . .
Zn10 O11 H11 108(4) 3_665 .
Zn2 O12 Zn10 119.35(14) . .
Zn2 O12 Zn5 122.63(14) . .
Zn10 O12 Zn5 93.26(12) . .
Zn2 O12 H12 100(4) . .
Zn10 O12 H12 110(3) . .
Zn5 O12 H12 113(3) . .
Zn2 O13 Zn4 122.63(13) . .
Zn2 O13 Zn6 122.97(13) . 5
Zn4 O13 Zn6 93.15(12) . 5
Zn2 O13 H13 103(3) . .
Zn4 O13 H13 103(3) . .
Zn6 O13 H13 110(3) 5 .
Zn3 O14 Zn5 121.42(13) . 3_665
Zn3 O14 Zn4 123.16(13) . 3_665
Zn5 O14 Zn4 93.07(12) 3_665 3_665
Zn3 O14 H14 100(3) . .
Zn5 O14 H14 108(3) 3_665 .
Zn4 O14 H14 111(3) 3_665 .
Zn2 O15 Zn7 120.61(13) . 5
Zn2 O15 Zn9 122.55(13) . 2_655
Zn7 O15 Zn9 94.61(11) 5 2_655
Zn2 O15 H15 105.8 . .
Zn7 O15 H15 105.8 5 .
Zn9 O15 H15 105.8 2_655 .
Zn3 O16 Zn6 121.25(13) . 4_665
Zn3 O16 Zn7 122.13(13) . 4_665
Zn6 O16 Zn7 93.20(12) 4_665 4_665
Zn3 O16 H16 100(3) . .
Zn6 O16 H16 109(3) 4_665 .
Zn7 O16 H16 112(3) 4_665 .
Zn1 O17 Zn8 121.30(14) . .
Zn1 O17 Zn8 122.92(13) . 6
Zn8 O17 Zn8 93.73(12) . 6
Zn1 O17 H17 101(3) . .
Zn8 O17 H17 113(3) . .
Zn8 O17 H17 105(3) 6 .
Zn7 O18 Zn6 97.34(11) . .
Zn7 O18 Zn5 106.74(12) . .
Zn6 O18 Zn5 97.78(12) . .
Zn7 O18 O25 109.73(12) . .
Zn6 O18 O25 118.90(12) . .
Zn5 O18 O25 122.86(12) . .
Zn7 O18 H18 117.2 . .
Zn6 O18 H18 117.2 . .
Zn5 O18 H18 117.2 . .
O25 O18 H18 7.6 . .
Zn6 O19 Zn4 96.82(12) 5 .
Zn6 O19 Zn8 107.32(13) 5 5
Zn4 O19 Zn8 98.65(12) . 5
Zn6 O19 H19 117.0 5 .
Zn4 O19 H19 117.0 . .
Zn8 O19 H19 117.0 5 .
Zn5 O20 Zn9 108.68(13) . .
Zn5 O20 Zn10 97.39(12) . .
Zn9 O20 Zn10 98.74(12) . .
Zn5 O20 O27 108.63(13) . .
Zn9 O20 O27 118.26(14) . .
Zn10 O20 O27 122.71(15) . .
Zn5 O20 H20 116.4 . .
Zn9 O20 H20 116.4 . .
Zn10 O20 H20 116.4 . .
O27 O20 H20 8.5 . .
Zn9 O21 Zn7 96.96(11) . 4_665
Zn9 O21 Zn7 106.89(13) . .
Zn7 O21 Zn7 98.00(12) 4_665 .
Zn9 O21 H21 117.2 . .
Zn7 O21 H21 117.2 4_665 .
Zn7 O21 H21 117.2 . .
Zn8 O22 Zn8 96.92(12) . 5
Zn8 O22 Zn4 106.52(13) . .
Zn8 O22 Zn4 97.80(12) 5 .
Zn8 O22 H22 117.4 . .
Zn8 O22 H22 117.4 5 .
Zn4 O22 H22 117.4 . .
Zn10 O23 Zn10 108.39(13) 3_665 .
Zn10 O23 Zn9 96.69(11) 3_665 .
Zn10 O23 Zn9 97.21(11) . .
Zn10 O23 O29 109.00(13) 3_665 .
Zn10 O23 O29 124.31(14) . .
Zn9 O23 O29 117.47(13) . .
Zn10 O23 H23 117.0 3_665 .
Zn10 O23 H23 117.0 . .
Zn9 O23 H23 117.0 . .
O29 O23 H23 8.5 . .
Zn4 O24 Zn5 97.23(11) . .
Zn4 O24 Zn6 107.63(13) . .
Zn5 O24 Zn6 98.87(12) . .
Zn4 O24 H24 116.7 . .
Zn5 O24 H24 116.7 . .
Zn6 O24 H24 116.7 . .
C2 N1 Zn1 112.3(6) . .
C2 N1 H1A 109.1 . .
Zn1 N1 H1A 109.1 . .
C2 N1 H1B 109.1 . .
Zn1 N1 H1B 109.1 . .
H1A N1 H1B 107.9 . .
N1 C2 C2 106.6(8) . 5_554
N1 C2 H2A 110.4 . .
C2 C2 H2A 110.4 5_554 .
N1 C2 H2B 110.4 . .
C2 C2 H2B 110.4 5_554 .
H2A C2 H2B 108.6 . .
C4 N3 Zn3 115.8(3) . .
C4 N3 H3A 108.3 . .
Zn3 N3 H3A 108.3 . .
C4 N3 H3B 108.3 . .
Zn3 N3 H3B 108.3 . .
H3A N3 H3B 107.4 . .
N3 C4 C5 113.2(4) . 3_666
N3 C4 H4A 108.9 . .
C5 C4 H4A 108.9 3_666 .
N3 C4 H4B 108.9 . .
C5 C4 H4B 108.9 3_666 .
H4A C4 H4B 107.8 . .
N6 C5 C4 111.5(4) . 2_654
N6 C5 H5A 109.3 . .
C4 C5 H5A 109.3 2_654 .
N6 C5 H5B 109.3 . .
C4 C5 H5B 109.3 2_654 .
H5A C5 H5B 108.0 . .
C5 N6 Zn2 114.7(3) . .
C5 N6 H6A 108.6 . .
Zn2 N6 H6A 108.6 . .
C5 N6 H6B 108.6 . .
Zn2 N6 H6B 108.6 . .
H6A N6 H6B 107.6 . .
O5 O25 O7 114.19(16) . 1_556
O5 O25 O27 77.48(14) . .
O7 O25 O27 97.62(14) 1_556 .
O5 O25 N6 108.51(15) . 6
O7 O25 N6 102.92(15) 1_556 6
O27 O25 N6 153.38(18) . 6
O5 O25 O18 62.02(11) . .
O7 O25 O18 170.57(16) 1_556 .
O27 O25 O18 73.30(12) . .
N6 O25 O18 86.51(12) 6 .
O5 O25 O26 135.15(16) . 1_556
O7 O25 O26 82.78(12) 1_556 1_556
O27 O25 O26 58.70(11) . 1_556
N6 O25 O26 107.14(14) 6 1_556
O18 O25 O26 94.29(12) . 1_556
O9 O26 O9 103.93(14) . 4_664
O9 O26 N3 117.49(16) . 1_554
O9 O26 N3 118.38(16) 4_664 1_554
O9 O26 O27 94.94(14) . 1_554
O9 O26 O27 112.82(16) 4_664 1_554
N3 O26 O27 107.01(15) 1_554 1_554
O9 O26 O7 113.68(14) . 4_664
O9 O26 O7 45.05(9) 4_664 4_664
N3 O26 O7 76.20(13) 1_554 4_664
O27 O26 O7 146.26(16) 1_554 4_664
O9 O26 O29 62.58(13) . .
O9 O26 O29 166.45(17) 4_664 .
N3 O26 O29 71.86(13) 1_554 .
O27 O26 O29 69.46(14) 1_554 .
O7 O26 O29 139.03(15) 4_664 .
O9 O26 O25 76.05(12) . 1_554
O9 O26 O25 70.04(12) 4_664 1_554
N3 O26 O25 158.56(17) 1_554 1_554
O27 O26 O25 53.14(11) 1_554 1_554
O7 O26 O25 115.08(14) 4_664 1_554
O29 O26 O25 103.75(14) . 1_554
O20 O27 O4 75.76(12) . 3_665
O20 O27 O25 108.87(17) . .
O4 O27 O25 142.25(17) 3_665 .
O20 O27 N3 95.80(14) . 2_655
O4 O27 N3 106.37(15) 3_665 2_655
O25 O27 N3 110.24(15) . 2_655
O20 O27 O26 101.07(15) . 1_556
O4 O27 O26 74.15(13) 3_665 1_556
O25 O27 O26 68.16(12) . 1_556
N3 O27 O26 162.61(18) 2_655 1_556
O20 O27 O4 79.61(12) . .
O4 O27 O4 44.89(12) 3_665 .
O25 O27 O4 169.34(17) . .
N3 O27 O4 61.52(11) 2_655 .
O26 O27 O4 117.41(14) 1_556 .
C2 O28 O30 127.6(4) 4 .
C2 O28 O10 113.6(4) 4 .
O30 O28 O10 97.2(2) . .
C2 O28 O8 96.0(3) 4 6_556
O30 O28 O8 103.2(2) . 6_556
O10 O28 O8 121.1(2) . 6_556
C2 O28 N1 14.7(3) 4 6
O30 O28 N1 117.2(3) . 6
O10 O28 N1 108.3(3) . 6
O8 O28 N1 109.8(2) 6_556 6
C2 O28 C2 29.2(4) 4 2_556
O30 O28 C2 149.4(3) . 2_556
O10 O28 C2 111.1(3) . 2_556
O8 O28 C2 72.6(2) 6_556 2_556
N1 O28 C2 43.4(2) 6 2_556
C2 O28 N1 15.8(3) 4 5
O30 O28 N1 126.4(3) . 5
O10 O28 N1 99.6(2) . 5
O8 O28 N1 110.4(2) 6_556 5
N1 O28 N1 11.1(3) 6 5
C2 O28 N1 39.4(2) 2_556 5
C2 O28 C2 27.1(4) 4 3_556
O30 O28 C2 124.0(3) . 3_556
O10 O28 C2 134.9(3) . 3_556
O8 O28 C2 70.5(2) 6_556 3_556
N1 O28 C2 39.5(2) 6 3_556
C2 O28 C2 25.5(5) 2_556 3_556
N1 O28 C2 42.8(2) 5 3_556
O6 O29 O4 110.35(17) . 3_664
O6 O29 O23 66.04(13) . .
O4 O29 O23 162.19(19) 3_664 .
O6 O29 O9 45.11(10) . .
O4 O29 O9 115.54(17) 3_664 .
O23 O29 O9 75.10(12) . .
O6 O29 O29 74.34(19) . 2_655
O4 O29 O29 80.43(10) 3_664 2_655
O23 O29 O29 81.84(10) . 2_655
O9 O29 O29 119.4(2) . 2_655
O6 O29 O29 130.98(19) . 3_665
O4 O29 O29 80.15(10) 3_664 3_665
O23 O29 O29 89.51(9) . 3_665
O9 O29 O29 164.29(11) . 3_665
O29 O29 O29 60.0 2_655 3_665
O6 O29 O26 77.26(14) . .
O4 O29 O26 67.58(14) 3_664 .
O23 O29 O26 125.61(16) . .
O9 O29 O26 50.72(10) . .
O29 O29 O26 125.68(18) 2_655 .
O29 O29 O26 144.06(13) 3_665 .
O28 O30 O24 118.2(2) . 6
O28 O30 O7 150.3(2) . 6
O24 O30 O7 70.47(14) 6 6
O28 O30 O19 107.5(2) . 2
O24 O30 O19 61.95(12) 6 2
O7 O30 O19 101.54(17) 6 2
O28 O30 O22 68.72(16) . 6
O24 O30 O22 55.87(11) 6 6
O7 O30 O22 126.34(17) 6 6
O19 O30 O22 55.23(10) 2 6
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O17 1.956(3) .
Zn1 O17 1.956(3) 3
Zn1 O17 1.956(3) 2
Zn1 N1 2.041(7) 2
Zn1 N1 2.041(7) 3
Zn1 N1 2.041(7) .
Zn2 O12 1.948(3) .
Zn2 O13 1.957(3) .
Zn2 O15 1.962(3) .
Zn2 N6 2.016(4) .
Zn3 O14 1.957(3) .
Zn3 O16 1.957(3) .
Zn3 O11 1.967(3) .
Zn3 N3 2.017(4) .
Zn4 O24 2.026(3) .
Zn4 O19 2.057(3) .
Zn4 O22 2.078(3) .
Zn4 O13 2.089(3) .
Zn4 O14 2.102(3) 2_655
Zn4 O1 2.345(3) .
Zn5 O20 2.023(3) .
Zn5 O24 2.035(3) .
Zn5 O18 2.082(3) .
Zn5 O14 2.095(3) 2_655
Zn5 O12 2.120(3) .
Zn5 O3 2.326(3) .
Zn6 O19 2.027(3) 6
Zn6 O18 2.051(3) .
Zn6 O24 2.065(3) .
Zn6 O16 2.089(3) 4_665
Zn6 O13 2.117(3) 6
Zn6 O1 2.352(3) .
Zn7 O18 2.023(3) .
Zn7 O21 2.048(3) 4_665
Zn7 O21 2.077(3) .
Zn7 O15 2.082(3) 6
Zn7 O16 2.122(3) 4_665
Zn7 O3 2.340(3) .
Zn8 O22 2.031(3) .
Zn8 O19 2.058(3) 6
Zn8 O22 2.064(3) 6
Zn8 O17 2.076(3) .
Zn8 O17 2.124(3) 5
Zn8 O1 2.325(3) .
Zn9 O20 2.033(3) .
Zn9 O21 2.044(3) .
Zn9 O11 2.056(3) .
Zn9 O23 2.073(3) .
Zn9 O15 2.086(3) 3_665
Zn9 O3 2.419(3) .
Zn10 O23 2.026(3) 2_655
Zn10 O20 2.051(3) .
Zn10 O23 2.058(3) .
Zn10 O12 2.090(3) .
Zn10 O11 2.103(3) 2_655
Zn10 O2 2.413(3) .
S1 O10 1.462(3) .
S1 O8 1.463(3) .
S1 O5 1.469(3) .
S1 O1 1.508(3) .
S2 O6 1.462(3) .
S2 O7 1.473(3) .
S2 O9 1.477(3) .
S2 O3 1.509(3) .
S3 O4 1.471(3) 2_655
S3 O4 1.471(3) .
S3 O4 1.471(3) 3_665
S3 O2 1.512(5) .
O4 O27 3.353(5) .
O5 O25 2.758(5) .
O6 O29 2.821(5) .
O9 O26 2.931(5) .
O9 O29 3.361(5) .
O10 O28 2.763(5) .
O11 Zn10 2.103(3) 3_665
O11 H11 0.868(19) .
O12 H12 0.80(4) .
O13 Zn6 2.117(3) 5
O13 H13 0.870(19) .
O14 Zn5 2.095(3) 3_665
O14 Zn4 2.102(3) 3_665
O14 H14 0.848(18) .
O15 Zn7 2.082(3) 5
O15 Zn9 2.086(3) 2_655
O15 H15 1.0000 .
O16 Zn6 2.089(3) 4_665
O16 Zn7 2.122(3) 4_665
O16 H16 0.870(19) .
O17 Zn8 2.124(3) 6
O17 H17 0.846(19) .
O18 O25 3.414(5) .
O18 H18 1.0000 .
O19 Zn6 2.027(3) 5
O19 Zn8 2.058(3) 5
O19 H19 1.0000 .
O20 O27 2.796(5) .
O20 H20 1.0000 .
O21 Zn7 2.048(3) 4_665
O21 H21 1.0000 .
O22 Zn8 2.064(3) 5
O22 H22 1.0000 .
O23 Zn10 2.026(3) 3_665
O23 O29 3.249(6) .
O23 H23 1.0000 .
O24 H24 1.0000 .
N1 C2 1.448(15) .
N1 H1A 0.9200 .
N1 H1B 0.9200 .
C2 C2 1.637(16) 5_554
C2 H2A 0.9900 .
C2 H2B 0.9900 .
N3 C4 1.410(6) .
N3 H3A 0.9200 .
N3 H3B 0.9200 .
C4 C5 1.572(7) 3_666
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 N6 1.452(6) .
C5 C4 1.572(7) 2_654
C5 H5A 0.9900 .
C5 H5B 0.9900 .
N6 H6A 0.9200 .
N6 H6B 0.9200 .
O25 O7 2.900(5) 1_556
O25 O27 3.000(6) .
O25 N6 3.144(5) 6
O25 O26 3.481(5) 1_556
O26 O9 2.973(5) 4_664
O26 N3 3.000(5) 1_554
O26 O27 3.204(6) 1_554
O26 O7 3.292(5) 4_664
O26 O29 3.478(7) .
O26 O25 3.481(5) 1_554
O27 O4 2.855(5) 3_665
O27 N3 3.131(6) 2_655
O27 O26 3.204(6) 1_556
O28 C2 2.510(15) 4
O28 O30 2.745(8) .
O28 O8 2.782(6) 6_556
O28 N1 3.190(15) 6
O28 C2 3.277(17) 2_556
O28 N1 3.371(17) 5
O28 C2 3.407(18) 3_556
O29 O4 3.083(6) 3_664
O29 O29 3.454(9) 2_655
O29 O29 3.454(9) 3_665
O30 O24 2.856(6) 6
O30 O7 2.986(6) 6
O30 O19 3.060(6) 2
O30 O22 3.526(6) 6
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
O11 H11 O4 0.868(19) 1.92(2) 2.768(4) 166(5) 3_665
O11 H11 S3 0.868(19) 2.79(4) 3.472(3) 136(4) .
O12 H12 O6 0.80(4) 2.06(5) 2.792(4) 153(5) .
O12 H12 S2 0.80(4) 2.97(5) 3.501(3) 127(4) .
O13 H13 O10 0.870(19) 1.94(2) 2.769(4) 160(5) 5
O13 H13 S1 0.870(19) 2.81(4) 3.446(3) 131(4) 5
O14 H14 O5 0.848(18) 2.00(2) 2.808(4) 158(4) 3_665
O14 H14 S1 0.848(18) 2.88(3) 3.488(3) 130(3) 3_665
O15 H15 O9 1.00 1.81 2.796(4) 167.1 2_655
O15 H15 S2 1.00 2.70 3.489(3) 136.2 2_655
O16 H16 O7 0.870(19) 1.98(3) 2.798(4) 157(5) 4_665
O16 H16 S2 0.870(19) 2.86(4) 3.473(3) 128(4) 4_665
O17 H17 O8 0.846(19) 1.96(2) 2.775(4) 162(5) 6
O17 H17 S1 0.846(19) 2.80(4) 3.454(3) 135(4) 6
O18 H18 O25 1.00 2.43 3.414(5) 169.3 .
O18 H18 O5 1.00 2.57 3.228(4) 123.1 .
O19 H19 O30 1.00 2.34 3.060(6) 128.5 3
O19 H19 O8 1.00 2.58 3.222(4) 122.1 .
O20 H20 O27 1.00 1.81 2.796(5) 166.8 .
O21 H21 O26 1.00 2.57 3.536(5) 163.2 1_556
O21 H21 O9 1.00 2.65 3.292(4) 122.1 4_665
O22 H22 O10 1.00 2.56 3.201(4) 121.5 5
O22 H22 O28 1.00 2.60 3.597(6) 173.9 5
O23 H23 O29 1.00 2.27 3.249(6) 167.8 .
O24 H24 O30 1.00 2.04 2.856(6) 137.3 5
N1 H1A O28 0.92 2.48 3.371(17) 161.9 6
N3 H3A O26 0.92 2.10 3.000(5) 167.1 1_556
N3 H3B O27 0.92 2.27 3.131(6) 154.8 3_665
N6 H6A O29 0.92 2.21 3.108(6) 164.4 2_655
N6 H6B O25 0.92 2.24 3.144(5) 167.6 5
