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

data_global

_journal_coden_Cambridge      186

_publ_requested_journal       'Dalton Transactions'

loop_
_publ_author_name
'Natarajan, Srinivasan'
'Chakrabarti, Sandip'

_publ_contact_author_name     	'Srinivasan Natarajan'  
_publ_contact_author_address 
;
Chemistry & Physics of Materials Unit
Jawaharlal Nehru Centre for Advanced Scientific Research
Jaakur P.O.
Bangalore 560 064
INDIA
;

_publ_contact_author_email       'RAJ@JNCASR.AC.IN'

_publ_section_title		
;
Hydrothermal Synthesis and Structure of a Zinc Arsenate-Oxalate,
[NH3(CH2)3NH2(CH2)NH3][Zn3(AsO4)2(C2O4)], and a Zinc Arsenate,
[{NH3(CH3)2NH2(CH3)3NH3}2][Zn69AsO4)4(HAsO4)3].H2O, with Three-dimensional
Structures
;


data_junk
_database_code_CSD                  184189


_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
'C8 H22 As3 N3 O16 Zn3'
_chemical_formula_weight          837.16

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'
'Zn'  'Zn'   0.2839   1.4301
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'As'  'As'   0.0499   2.0058
'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                    16.0857(2)
_cell_length_b                    9.1973(2)
_cell_length_c                    15.4216(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  112.0330(10)
_cell_angle_gamma                 90.00
_cell_volume                      2114.92(7)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?

_exptl_crystal_description        needle-like
_exptl_crystal_colour             colorless
_exptl_crystal_size_max           0.20
_exptl_crystal_size_mid           0.16
_exptl_crystal_size_min           0.10
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.629
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1632
_exptl_absorpt_coefficient_mu     8.118
_exptl_absorpt_correction_type    SADABS
_exptl_absorpt_correction_T_min   0.571303
_exptl_absorpt_correction_T_max   1.000000
_exptl_absorpt_process_details    ?

_exptl_special_details
;
?
;

_diffrn_ambient_temperature       293(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        '\w scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             11648
_diffrn_reflns_av_R_equivalents   0.0651
_diffrn_reflns_av_sigmaI/netI     0.0597
_diffrn_reflns_limit_h_min        -17
_diffrn_reflns_limit_h_max        17
_diffrn_reflns_limit_k_min        -10
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -17
_diffrn_reflns_limit_l_max        17
_diffrn_reflns_theta_min          1.37
_diffrn_reflns_theta_max          23.25
_reflns_number_total              3035
_reflns_number_gt                 2405
_reflns_threshold_expression      >2sigma(I)

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

_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^)+(0.0170P)^2^+0.0000P] 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     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          3035
_refine_ls_number_parameters      298
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0448
_refine_ls_R_factor_gt            0.0293
_refine_ls_wR_factor_ref          0.0633
_refine_ls_wR_factor_gt           0.0587
_refine_ls_goodness_of_fit_ref    0.969
_refine_ls_restrained_S_all       0.969
_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
As1 As 0.71917(4) -0.55043(6) -0.15945(4) 0.01646(16) Uani 1 1 d . . .
As2 As 0.77730(4) -0.70336(7) -0.38143(4) 0.01627(16) Uani 1 1 d . . .
As3 As 0.52912(4) -0.22967(6) -0.45923(4) 0.01476(16) Uani 1 1 d . . .
Zn1 Zn 0.89358(4) -0.74915(7) -0.02535(4) 0.01719(18) Uani 1 1 d . . .
Zn2 Zn 0.64665(4) -0.53096(7) 0.01269(4) 0.01776(18) Uani 1 1 d . . .
Zn3 Zn 0.59249(4) -0.56654(7) -0.37066(4) 0.01720(18) Uani 1 1 d . . .
O1 O 0.7155(3) -0.4761(4) -0.0628(3) 0.0236(10) Uani 1 1 d . . .
O2 O 0.7921(3) -0.6853(4) -0.1453(3) 0.0257(10) Uani 1 1 d . . .
O3 O 0.6170(2) -0.5957(4) -0.2361(2) 0.0198(10) Uani 1 1 d . . .
O4 O 0.7561(3) -0.4060(4) -0.2086(3) 0.0328(11) Uani 1 1 d . . .
H30 H 0.7602 -0.4324 -0.2576 0.049 Uiso 1 1 calc R . .
O5 O 0.7279(3) -0.8620(4) -0.3805(3) 0.0240(10) Uani 1 1 d . . .
O6 O 0.8093(3) -0.6689(4) -0.4692(3) 0.0276(11) Uani 1 1 d . . .
O7 O 0.7121(2) -0.5596(4) -0.3776(3) 0.0223(10) Uani 1 1 d . . .
O8 O 0.8717(2) -0.6963(5) -0.2800(3) 0.0295(11) Uani 1 1 d . . .
H40 H 0.8579 -0.7131 -0.2350 0.044 Uiso 1 1 calc R . .
O9 O 0.5348(3) -0.3782(4) -0.3948(3) 0.0255(10) Uani 1 1 d . . .
O10 O 0.6326(2) -0.1627(4) -0.4384(3) 0.0193(10) Uani 1 1 d . . .
O11 O 0.4819(2) -0.2677(4) -0.5743(3) 0.0219(10) Uani 1 1 d . . .
O12 O 0.4667(3) -0.1078(4) -0.4297(3) 0.0224(10) Uani 1 1 d . . .
O13 O 0.9313(3) -0.5597(4) 0.0582(3) 0.0209(10) Uani 1 1 d . . .
O14 O 1.0022(3) -0.8635(4) 0.0797(3) 0.0253(10) Uani 1 1 d . . .
O15 O 0.9132(3) -0.9347(4) -0.1006(3) 0.0214(10) Uani 1 1 d . . .
O16 O 0.9847(3) -0.6400(4) -0.0806(3) 0.0244(10) Uani 1 1 d . . .
C10 C 0.9853(4) -0.4766(7) 0.0398(4) 0.0189(14) Uani 1 1 d . . .
C20 C 1.0255(4) -0.9788(7) 0.0522(4) 0.0196(14) Uani 1 1 d . . .
N1 N 0.9147(4) -0.4502(5) 0.2224(3) 0.0344(14) Uani 1 1 d . . .
H1 H 0.8983 -0.5195 0.2531 0.052 Uiso 1 1 calc R . .
H2 H 0.9712 -0.4244 0.2549 0.052 Uiso 1 1 calc R . .
H3 H 0.9102 -0.4837 0.1666 0.052 Uiso 1 1 calc R . .
C1 C 0.8545(4) -0.3206(7) 0.2097(4) 0.0340(18) Uani 1 1 d . . .
H4 H 0.8587 -0.2851 0.2704 0.041 Uiso 1 1 calc R . .
H5 H 0.7928 -0.3491 0.1750 0.041 Uiso 1 1 calc R . .
C2 C 0.8804(4) -0.2010(7) 0.1578(4) 0.0291(16) Uani 1 1 d . . .
H6 H 0.9453 -0.1984 0.1795 0.035 Uiso 1 1 calc R . .
H7 H 0.8611 -0.1092 0.1749 0.035 Uiso 1 1 calc R . .
C3 C 0.8433(4) -0.2114(7) 0.0520(4) 0.0253(15) Uani 1 1 d . . .
H8 H 0.8820 -0.1569 0.0284 0.030 Uiso 1 1 calc R . .
H9 H 0.8446 -0.3123 0.0342 0.030 Uiso 1 1 calc R . .
N2 N 0.7491(3) -0.1548(5) 0.0066(3) 0.0190(12) Uani 1 1 d . . .
H10 H 0.7104 -0.2236 0.0096 0.023 Uiso 1 1 calc R . .
H11 H 0.7424 -0.0766 0.0385 0.023 Uiso 1 1 calc R . .
C4 C 0.7269(4) -0.1138(7) -0.0928(4) 0.0243(15) Uani 1 1 d . . .
H12 H 0.7276 -0.2000 -0.1287 0.029 Uiso 1 1 calc R . .
H13 H 0.7722 -0.0474 -0.0969 0.029 Uiso 1 1 calc R . .
C5 C 0.6364(4) -0.0427(7) -0.1339(4) 0.0303(16) Uani 1 1 d . . .
H14 H 0.6319 0.0323 -0.0917 0.036 Uiso 1 1 calc R . .
H15 H 0.5902 -0.1145 -0.1407 0.036 Uiso 1 1 calc R . .
C6 C 0.6214(4) 0.0237(7) -0.2278(4) 0.0280(16) Uani 1 1 d . . .
H16 H 0.6679 0.0949 -0.2211 0.034 Uiso 1 1 calc R . .
H17 H 0.6255 -0.0515 -0.2702 0.034 Uiso 1 1 calc R . .
N3 N 0.5314(3) 0.0955(5) -0.2684(3) 0.0254(13) Uani 1 1 d . . .
H18 H 0.5242 0.1337 -0.3238 0.038 Uiso 1 1 calc R . .
H19 H 0.5279 0.1655 -0.2301 0.038 Uiso 1 1 calc R . .
H20 H 0.4887 0.0299 -0.2755 0.038 Uiso 1 1 calc R . .

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
As1 0.0197(4) 0.0159(4) 0.0178(3) 0.0000(3) 0.0116(3) -0.0006(3)
As2 0.0200(4) 0.0138(3) 0.0195(3) -0.0008(3) 0.0124(3) 0.0008(3)
As3 0.0173(3) 0.0103(3) 0.0202(3) 0.0013(3) 0.0111(3) 0.0008(3)
Zn1 0.0207(4) 0.0151(4) 0.0195(4) -0.0004(3) 0.0118(3) 0.0003(3)
Zn2 0.0208(4) 0.0137(4) 0.0228(4) -0.0006(3) 0.0128(3) -0.0002(3)
Zn3 0.0206(4) 0.0148(4) 0.0198(4) 0.0009(3) 0.0116(3) 0.0007(3)
O1 0.031(3) 0.026(3) 0.021(2) -0.0084(19) 0.018(2) -0.011(2)
O2 0.022(2) 0.029(3) 0.027(2) 0.004(2) 0.011(2) 0.014(2)
O3 0.019(2) 0.025(3) 0.017(2) 0.0005(18) 0.0075(19) 0.0012(18)
O4 0.050(3) 0.026(3) 0.035(3) -0.002(2) 0.029(2) -0.016(2)
O5 0.033(3) 0.013(2) 0.026(2) 0.0015(18) 0.011(2) -0.0067(19)
O6 0.037(3) 0.029(3) 0.028(2) 0.003(2) 0.025(2) 0.005(2)
O7 0.025(2) 0.016(2) 0.036(2) -0.0019(19) 0.023(2) 0.0024(19)
O8 0.027(3) 0.038(3) 0.026(2) -0.001(2) 0.012(2) -0.004(2)
O9 0.032(3) 0.015(2) 0.037(2) 0.011(2) 0.022(2) 0.0029(19)
O10 0.016(2) 0.013(2) 0.030(2) 0.0041(18) 0.0106(19) 0.0004(17)
O11 0.029(2) 0.018(2) 0.023(2) -0.0041(18) 0.014(2) -0.0054(19)
O12 0.028(2) 0.019(2) 0.025(2) -0.0058(18) 0.016(2) 0.0066(19)
O13 0.031(3) 0.012(2) 0.030(2) -0.0042(18) 0.024(2) -0.007(2)
O14 0.030(3) 0.021(3) 0.025(2) -0.006(2) 0.010(2) 0.010(2)
O15 0.023(2) 0.019(2) 0.022(2) -0.0001(19) 0.008(2) 0.006(2)
O16 0.028(3) 0.020(3) 0.034(2) -0.008(2) 0.021(2) -0.006(2)
C10 0.016(3) 0.017(4) 0.023(3) -0.003(3) 0.007(3) 0.003(3)
C20 0.013(3) 0.029(4) 0.020(3) 0.002(3) 0.009(3) -0.005(3)
N1 0.056(4) 0.025(3) 0.031(3) 0.004(3) 0.027(3) 0.008(3)
C1 0.034(4) 0.039(5) 0.030(4) 0.004(3) 0.013(3) 0.014(3)
C2 0.026(4) 0.022(4) 0.034(4) -0.003(3) 0.007(3) 0.004(3)
C3 0.021(4) 0.028(4) 0.033(4) 0.004(3) 0.017(3) 0.006(3)
N2 0.022(3) 0.007(3) 0.031(3) 0.001(2) 0.014(2) 0.000(2)
C4 0.031(4) 0.018(4) 0.027(4) 0.004(3) 0.014(3) -0.001(3)
C5 0.031(4) 0.033(4) 0.032(4) 0.005(3) 0.018(3) 0.003(3)
C6 0.026(4) 0.031(4) 0.029(4) 0.008(3) 0.012(3) 0.005(3)
N3 0.031(3) 0.021(3) 0.023(3) 0.003(2) 0.009(3) -0.003(2)

_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
As1 O1 1.660(4) . ?
As1 O2 1.665(4) . ?
As1 O3 1.677(4) . ?
As1 O4 1.741(4) . ?
As2 O6 1.649(4) . ?
As2 O5 1.664(4) . ?
As2 O7 1.702(4) . ?
As2 O8 1.725(4) . ?
As3 O9 1.671(4) . ?
As3 O12 1.678(4) . ?
As3 O11 1.684(4) . ?
As3 O10 1.689(4) . ?
Zn1 O6 2.009(4) 4_546 ?
Zn1 O2 2.041(4) . ?
Zn1 O13 2.116(4) . ?
Zn1 O15 2.153(4) . ?
Zn1 O14 2.159(4) . ?
Zn1 O16 2.194(4) . ?
Zn2 O12 1.927(4) 2_644 ?
Zn2 O5 1.944(4) 4_546 ?
Zn2 O1 1.950(4) . ?
Zn2 O10 1.980(4) 4_556 ?
Zn3 O11 1.927(4) 3_644 ?
Zn3 O9 1.934(4) . ?
Zn3 O7 1.968(4) . ?
Zn3 O3 1.980(4) . ?
O4 H30 0.8200 . ?
O5 Zn2 1.944(4) 4_545 ?
O6 Zn1 2.009(4) 4_545 ?
O8 H40 0.8200 . ?
O10 Zn2 1.980(4) 4 ?
O11 Zn3 1.927(4) 3_644 ?
O12 Zn2 1.927(4) 2_654 ?
O13 C10 1.267(7) . ?
O14 C20 1.250(7) . ?
O15 C20 1.269(6) 3_735 ?
O16 C10 1.245(6) 3_745 ?
C10 O16 1.245(6) 3_745 ?
C10 C10 1.534(11) 3_745 ?
C20 O15 1.269(6) 3_735 ?
C20 C20 1.557(11) 3_735 ?
N1 C1 1.501(7) . ?
N1 H1 0.8900 . ?
N1 H2 0.8900 . ?
N1 H3 0.8900 . ?
C1 C2 1.507(8) . ?
C1 H4 0.9700 . ?
C1 H5 0.9700 . ?
C2 C3 1.516(8) . ?
C2 H6 0.9700 . ?
C2 H7 0.9700 . ?
C3 N2 1.504(6) . ?
C3 H8 0.9700 . ?
C3 H9 0.9700 . ?
N2 C4 1.487(7) . ?
N2 H10 0.9000 . ?
N2 H11 0.9000 . ?
C4 C5 1.502(8) . ?
C4 H12 0.9700 . ?
C4 H13 0.9700 . ?
C5 C6 1.505(8) . ?
C5 H14 0.9700 . ?
C5 H15 0.9700 . ?
C6 N3 1.497(7) . ?
C6 H16 0.9700 . ?
C6 H17 0.9700 . ?
N3 H18 0.8900 . ?
N3 H19 0.8900 . ?
N3 H20 0.8900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 As1 O2 116.74(19) . . ?
O1 As1 O3 112.28(18) . . ?
O2 As1 O3 111.31(19) . . ?
O1 As1 O4 102.09(19) . . ?
O2 As1 O4 106.7(2) . . ?
O3 As1 O4 106.66(18) . . ?
O6 As2 O5 118.2(2) . . ?
O6 As2 O7 105.37(19) . . ?
O5 As2 O7 112.22(19) . . ?
O6 As2 O8 107.24(19) . . ?
O5 As2 O8 106.61(19) . . ?
O7 As2 O8 106.52(19) . . ?
O9 As3 O12 106.83(19) . . ?
O9 As3 O11 111.04(19) . . ?
O12 As3 O11 110.23(18) . . ?
O9 As3 O10 110.76(18) . . ?
O12 As3 O10 110.59(18) . . ?
O11 As3 O10 107.42(18) . . ?
O6 Zn1 O2 93.41(16) 4_546 . ?
O6 Zn1 O13 97.60(15) 4_546 . ?
O2 Zn1 O13 105.30(16) . . ?
O6 Zn1 O15 101.20(16) 4_546 . ?
O2 Zn1 O15 88.19(15) . . ?
O13 Zn1 O15 156.13(15) . . ?
O6 Zn1 O14 88.88(16) 4_546 . ?
O2 Zn1 O14 165.32(15) . . ?
O13 Zn1 O14 88.73(15) . . ?
O15 Zn1 O14 77.14(14) . . ?
O6 Zn1 O16 174.60(16) 4_546 . ?
O2 Zn1 O16 86.56(16) . . ?
O13 Zn1 O16 77.23(14) . . ?
O15 Zn1 O16 84.19(15) . . ?
O14 Zn1 O16 92.51(15) . . ?
O12 Zn2 O5 123.07(16) 2_644 4_546 ?
O12 Zn2 O1 107.80(15) 2_644 . ?
O5 Zn2 O1 106.58(17) 4_546 . ?
O12 Zn2 O10 111.61(16) 2_644 4_556 ?
O5 Zn2 O10 105.60(15) 4_546 4_556 ?
O1 Zn2 O10 99.59(16) . 4_556 ?
O11 Zn3 O9 116.74(16) 3_644 . ?
O11 Zn3 O7 117.37(16) 3_644 . ?
O9 Zn3 O7 111.63(16) . . ?
O11 Zn3 O3 101.62(16) 3_644 . ?
O9 Zn3 O3 102.46(16) . . ?
O7 Zn3 O3 104.31(15) . . ?
As1 O1 Zn2 130.5(2) . . ?
As1 O2 Zn1 128.2(2) . . ?
As1 O3 Zn3 117.5(2) . . ?
As1 O4 H30 109.5 . . ?
As2 O5 Zn2 127.4(2) . 4_545 ?
As2 O6 Zn1 138.6(2) . 4_545 ?
As2 O7 Zn3 127.2(2) . . ?
As2 O8 H40 109.5 . . ?
As3 O9 Zn3 139.6(2) . . ?
As3 O10 Zn2 120.05(19) . 4 ?
As3 O11 Zn3 126.1(2) . 3_644 ?
As3 O12 Zn2 125.3(2) . 2_654 ?
C10 O13 Zn1 115.2(3) . . ?
C20 O14 Zn1 114.8(3) . . ?
C20 O15 Zn1 114.7(4) 3_735 . ?
C10 O16 Zn1 112.8(4) 3_745 . ?
O16 C10 O13 125.2(5) 3_745 . ?
O16 C10 C10 117.9(7) 3_745 3_745 ?
O13 C10 C10 116.9(6) . 3_745 ?
O14 C20 O15 126.7(5) . 3_735 ?
O14 C20 C20 117.0(7) . 3_735 ?
O15 C20 C20 116.3(7) 3_735 3_735 ?
C1 N1 H1 109.5 . . ?
C1 N1 H2 109.5 . . ?
H1 N1 H2 109.5 . . ?
C1 N1 H3 109.5 . . ?
H1 N1 H3 109.5 . . ?
H2 N1 H3 109.5 . . ?
N1 C1 C2 110.9(5) . . ?
N1 C1 H4 109.5 . . ?
C2 C1 H4 109.5 . . ?
N1 C1 H5 109.5 . . ?
C2 C1 H5 109.5 . . ?
H4 C1 H5 108.1 . . ?
C1 C2 C3 116.7(5) . . ?
C1 C2 H6 108.1 . . ?
C3 C2 H6 108.1 . . ?
C1 C2 H7 108.1 . . ?
C3 C2 H7 108.1 . . ?
H6 C2 H7 107.3 . . ?
N2 C3 C2 113.6(5) . . ?
N2 C3 H8 108.9 . . ?
C2 C3 H8 108.9 . . ?
N2 C3 H9 108.9 . . ?
C2 C3 H9 108.9 . . ?
H8 C3 H9 107.7 . . ?
C4 N2 C3 112.2(4) . . ?
C4 N2 H10 109.2 . . ?
C3 N2 H10 109.2 . . ?
C4 N2 H11 109.2 . . ?
C3 N2 H11 109.2 . . ?
H10 N2 H11 107.9 . . ?
N2 C4 C5 111.4(5) . . ?
N2 C4 H12 109.3 . . ?
C5 C4 H12 109.3 . . ?
N2 C4 H13 109.3 . . ?
C5 C4 H13 109.3 . . ?
H12 C4 H13 108.0 . . ?
C4 C5 C6 111.3(5) . . ?
C4 C5 H14 109.4 . . ?
C6 C5 H14 109.4 . . ?
C4 C5 H15 109.4 . . ?
C6 C5 H15 109.4 . . ?
H14 C5 H15 108.0 . . ?
N3 C6 C5 111.3(5) . . ?
N3 C6 H16 109.4 . . ?
C5 C6 H16 109.4 . . ?
N3 C6 H17 109.4 . . ?
C5 C6 H17 109.4 . . ?
H16 C6 H17 108.0 . . ?
C6 N3 H18 109.5 . . ?
C6 N3 H19 109.5 . . ?
H18 N3 H19 109.5 . . ?
C6 N3 H20 109.5 . . ?
H18 N3 H20 109.5 . . ?
H19 N3 H20 109.5 . . ?

_diffrn_measured_fraction_theta_max    0.999
_diffrn_reflns_theta_full              23.25
_diffrn_measured_fraction_theta_full   0.999
_refine_diff_density_max    0.554
_refine_diff_density_min   -0.725
_refine_diff_density_rms    0.138

#EOF

#COMPOUND II
data_sad
_database_code_CSD                  184190

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
'C12 H45 As7 N6 O29 Zn6'
_chemical_formula_weight          1654.20

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'
'Zn'  'Zn'   0.2839   1.4301
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'As'  'As'   0.0499   2.0058
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting            Triclinic
_symmetry_space_group_name_H-M    P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                    9.1724(4)
_cell_length_b                    9.2118(4)
_cell_length_c                    25.7459(11)
_cell_angle_alpha                 87.2650(10)
_cell_angle_beta                  86.4770(10)
_cell_angle_gamma                 71.2700(10)
_cell_volume                      2055.38(15)
_cell_formula_units_Z             2
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?

_exptl_crystal_description        rod-like
_exptl_crystal_colour             colorless
_exptl_crystal_size_max           0.2
_exptl_crystal_size_mid           0.12
_exptl_crystal_size_min           0.12
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.673
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1604
_exptl_absorpt_coefficient_mu     9.140
_exptl_absorpt_correction_type    SADABS
_exptl_absorpt_correction_T_min   0.349564
_exptl_absorpt_correction_T_max   1.000000
_exptl_absorpt_process_details    ?

_exptl_special_details
;
?
;

_diffrn_ambient_temperature       293(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   
;
Siemen's SMART-CCD
;
_diffrn_measurement_method        '\w scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             14656
_diffrn_reflns_av_R_equivalents   0.0606
_diffrn_reflns_av_sigmaI/netI     0.0756
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -10
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -28
_diffrn_reflns_limit_l_max        28
_diffrn_reflns_theta_min          1.59
_diffrn_reflns_theta_max          23.24
_reflns_number_total              5838
_reflns_number_gt                 4579
_reflns_threshold_expression      >2sigma(I)

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

_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^)+(0.0388P)^2^+0.0000P] 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     mixed
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.00121(11)
_refine_ls_extinction_expression
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          5838
_refine_ls_number_parameters      542
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0458
_refine_ls_R_factor_gt            0.0341
_refine_ls_wR_factor_ref          0.0965
_refine_ls_wR_factor_gt           0.0929
_refine_ls_goodness_of_fit_ref    0.969
_refine_ls_restrained_S_all       0.969
_refine_ls_shift/su_max           0.010
_refine_ls_shift/su_mean          0.001

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
As1 As 0.06566(8) 0.91391(8) 0.08054(3) 0.0145(2) Uani 1 1 d . . .
As2 As 0.43096(8) 0.28518(8) -0.00593(3) 0.0137(2) Uani 1 1 d . . .
As3 As 0.60861(8) 0.43946(8) 0.41397(3) 0.0166(2) Uani 1 1 d . . .
As4 As 0.75730(8) -0.05590(8) 0.50425(3) 0.0145(2) Uani 1 1 d . . .
As5 As 0.91838(8) 0.08918(8) 0.29708(3) 0.0172(2) Uani 1 1 d . . .
As6 As 0.42201(9) 0.54703(9) 0.19195(3) 0.0224(2) Uani 1 1 d . . .
As7 As -0.12641(9) 0.63421(9) 0.27100(3) 0.0222(2) Uani 1 1 d . . .
Zn1 Zn 0.65046(10) 0.42290(10) 0.28264(4) 0.0234(2) Uani 1 1 d . . .
Zn2 Zn 0.09518(10) 0.80892(9) 0.21099(3) 0.0186(2) Uani 1 1 d . . .
Zn3 Zn 0.32660(10) 0.57043(9) 0.07177(4) 0.0190(2) Uani 1 1 d . . .
Zn4 Zn 0.90517(9) 0.14627(9) 0.42564(4) 0.0178(2) Uani 1 1 d . . .
Zn5 Zn 0.53787(10) 0.73899(9) 0.48518(4) 0.0176(2) Uani 1 1 d . . .
Zn6 Zn -0.25983(10) 0.98140(9) 0.01317(3) 0.0168(2) Uani 1 1 d . . .
O1 O -0.1212(5) 0.9819(6) 0.0685(2) 0.0254(13) Uani 1 1 d . . .
O2 O 0.0760(7) 0.9195(6) 0.1446(2) 0.0342(15) Uani 1 1 d . . .
O3 O 0.1446(6) 0.7410(5) 0.0548(2) 0.0259(14) Uani 1 1 d . . .
O4 O 0.1549(6) 1.0380(5) 0.0553(2) 0.0270(14) Uani 1 1 d . . .
O5 O 0.5906(6) 0.1848(5) 0.0242(2) 0.0239(13) Uani 1 1 d . . .
O6 O 0.3477(6) 0.1775(5) -0.0369(2) 0.0242(13) Uani 1 1 d . . .
O7 O 0.4734(5) 0.4045(5) -0.0524(2) 0.0205(12) Uani 1 1 d . . .
O8 O 0.3019(5) 0.3936(5) 0.0384(2) 0.0194(12) Uani 1 1 d . . .
O9 O 0.7931(6) 0.3645(6) 0.4295(2) 0.0331(15) Uani 1 1 d . . .
O10 O 0.5569(6) 0.6288(5) 0.4214(2) 0.0234(13) Uani 1 1 d . . .
O11 O 0.4929(6) 0.3591(6) 0.4496(2) 0.0264(13) Uani 1 1 d . . .
O12 O 0.5846(7) 0.3997(6) 0.3529(2) 0.0312(14) Uani 1 1 d . . .
O13 O 0.9060(6) -0.0797(6) 0.5406(2) 0.0362(16) Uani 1 1 d . . .
O14 O 0.7739(6) 0.0218(6) 0.4448(2) 0.0254(13) Uani 1 1 d . . .
O15 O 0.7336(5) -0.2266(5) 0.4970(2) 0.0213(13) Uani 1 1 d . . .
O16 O 0.6032(6) 0.0623(5) 0.5389(2) 0.0218(13) Uani 1 1 d . . .
O17 O 1.0575(6) -0.0261(6) 0.2593(2) 0.0288(14) Uani 1 1 d . . .
O18 O 0.9923(6) 0.0952(6) 0.3536(2) 0.0286(14) Uani 1 1 d . . .
O19 O 0.8541(6) 0.2642(6) 0.2685(2) 0.0273(14) Uani 1 1 d . . .
O20 O 0.7608(6) 0.0274(6) 0.3054(2) 0.0287(14) Uani 1 1 d . . .
H50 H 0.7864 -0.0589 0.3189 0.043 Uiso 1 1 calc R . .
O21 O 0.3039(6) 0.6892(6) 0.2261(2) 0.0424(17) Uani 1 1 d . . .
O22 O 0.5133(7) 0.4004(6) 0.2308(2) 0.0402(17) Uani 1 1 d . . .
O23 O 0.3384(6) 0.4921(6) 0.1443(2) 0.0271(13) Uani 1 1 d . . .
O24 O 0.5632(7) 0.6131(8) 0.1612(3) 0.061(2) Uani 1 1 d . . .
H60 H 0.6102 0.6393 0.1831 0.091 Uiso 1 1 calc R . .
O25 O -0.1382(7) 0.7423(6) 0.3219(2) 0.0358(15) Uani 1 1 d . . .
O26 O -0.0662(6) 0.7096(6) 0.2163(2) 0.0264(13) Uani 1 1 d . . .
O27 O 0.0093(6) 0.4597(6) 0.2846(3) 0.0419(17) Uani 1 1 d . . .
H70 H -0.0183 0.4212 0.3112 0.063 Uiso 1 1 calc R . .
O28 O -0.2944(6) 0.6071(6) 0.2604(2) 0.0323(15) Uani 1 1 d . . .
O100 O 0.7701(8) 0.1738(8) 0.1662(3) 0.063(2) Uani 1 1 d . . .
N1 N 0.5042(7) -0.1157(7) 0.6181(3) 0.0267(17) Uani 1 1 d . . .
H1 H 0.5179 -0.1894 0.5954 0.040 Uiso 1 1 calc R . .
H2 H 0.4944 -0.0271 0.6010 0.040 Uiso 1 1 calc R . .
H3 H 0.4193 -0.1073 0.6381 0.040 Uiso 1 1 calc R . .
C1 C 0.6390(9) -0.1543(9) 0.6512(3) 0.029(2) Uani 1 1 d . . .
H4 H 0.7312 -0.1648 0.6292 0.035 Uiso 1 1 calc R . .
H5 H 0.6508 -0.2525 0.6689 0.035 Uiso 1 1 calc R . .
C2 C 0.6253(9) -0.0360(9) 0.6913(3) 0.030(2) Uani 1 1 d . . .
H6 H 0.7156 -0.0724 0.7119 0.036 Uiso 1 1 calc R . .
H7 H 0.5368 -0.0327 0.7144 0.036 Uiso 1 1 calc R . .
C3 C 0.6089(9) 0.1268(9) 0.6733(3) 0.028(2) Uani 1 1 d . . .
H8 H 0.5079 0.1737 0.6595 0.033 Uiso 1 1 calc R . .
H9 H 0.6159 0.1849 0.7030 0.033 Uiso 1 1 calc R . .
N2 N 0.7298(7) 0.1353(7) 0.6324(2) 0.0192(15) Uani 1 1 d . . .
H10 H 0.6961 0.1259 0.6010 0.023 Uiso 1 1 calc R . .
H11 H 0.8154 0.0551 0.6374 0.023 Uiso 1 1 calc R . .
C4 C 0.7722(9) 0.2821(9) 0.6316(3) 0.027(2) Uani 1 1 d . . .
H12 H 0.8454 0.2749 0.6580 0.033 Uiso 1 1 calc R . .
H13 H 0.6808 0.3686 0.6391 0.033 Uiso 1 1 calc R . .
C5 C 0.8431(10) 0.3059(10) 0.5778(4) 0.038(2) Uani 1 1 d . . .
H14 H 0.7672 0.3184 0.5519 0.045 Uiso 1 1 calc R . .
H15 H 0.9297 0.2155 0.5696 0.045 Uiso 1 1 calc R . .
C6 C 0.8983(9) 0.4472(9) 0.5754(4) 0.042(3) Uani 1 1 d . . .
H16 H 0.8759 0.4997 0.5418 0.051 Uiso 1 1 calc R . .
H17 H 0.8421 0.5175 0.6021 0.051 Uiso 1 1 calc R . .
N3 N 1.0659(7) 0.4045(7) 0.5830(3) 0.0275(17) Uani 1 1 d . . .
H18 H 1.0942 0.4885 0.5810 0.041 Uiso 1 1 calc R . .
H19 H 1.1178 0.3406 0.5584 0.041 Uiso 1 1 calc R . .
H20 H 1.0864 0.3587 0.6142 0.041 Uiso 1 1 calc R . .
N4 N 0.7038(7) -0.1320(7) 0.1476(3) 0.0310(18) Uani 1 1 d . . .
H21 H 0.7718 -0.1883 0.1698 0.047 Uiso 1 1 calc R . .
H22 H 0.7439 -0.0681 0.1294 0.047 Uiso 1 1 calc R . .
H23 H 0.6811 -0.1934 0.1260 0.047 Uiso 1 1 calc R . .
C7 C 0.5604(9) -0.0419(9) 0.1772(3) 0.028(2) Uani 1 1 d . . .
H24 H 0.5846 0.0245 0.2011 0.033 Uiso 1 1 calc R . .
H25 H 0.5166 -0.1109 0.1973 0.033 Uiso 1 1 calc R . .
C8 C 0.4453(10) 0.0538(10) 0.1390(4) 0.035(2) Uani 1 1 d . . .
H26 H 0.4917 0.1195 0.1181 0.042 Uiso 1 1 calc R . .
H27 H 0.4205 -0.0137 0.1157 0.042 Uiso 1 1 calc R . .
C9 C 0.2983(9) 0.1521(9) 0.1665(3) 0.027(2) Uani 1 1 d . . .
H28 H 0.2490 0.0875 0.1866 0.033 Uiso 1 1 calc R . .
H29 H 0.3218 0.2196 0.1901 0.033 Uiso 1 1 calc R . .
N5 N 0.1932(7) 0.2446(7) 0.1262(3) 0.0227(16) Uani 1 1 d . . .
H30 H 0.2425 0.3006 0.1071 0.027 Uiso 1 1 calc R . .
H31 H 0.1729 0.1801 0.1047 0.027 Uiso 1 1 calc R . .
C10 C 0.0443(9) 0.3498(10) 0.1479(4) 0.036(2) Uani 1 1 d . . .
H32 H 0.0650 0.4061 0.1759 0.043 Uiso 1 1 calc R . .
H33 H -0.0182 0.2892 0.1626 0.043 Uiso 1 1 calc R . .
C11 C -0.0458(9) 0.4627(9) 0.1077(4) 0.037(2) Uani 1 1 d . . .
H34 H -0.1428 0.5228 0.1244 0.044 Uiso 1 1 calc R . .
H35 H 0.0112 0.5326 0.0974 0.044 Uiso 1 1 calc R . .
C12 C -0.0808(10) 0.3989(10) 0.0596(4) 0.041(3) Uani 1 1 d . . .
H36 H -0.1061 0.4796 0.0329 0.049 Uiso 1 1 calc R . .
H37 H 0.0110 0.3192 0.0473 0.049 Uiso 1 1 calc R . .
N6 N -0.2082(9) 0.3348(8) 0.0669(4) 0.062(3) Uani 1 1 d . . .
H38 H -0.2233 0.2989 0.0369 0.093 Uiso 1 1 calc R . .
H39 H -0.2936 0.4078 0.0774 0.093 Uiso 1 1 calc R . .
H40 H -0.1849 0.2589 0.0908 0.093 Uiso 1 1 calc R . .

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
As1 0.0134(4) 0.0113(4) 0.0176(5) -0.0052(3) 0.0000(3) -0.0020(3)
As2 0.0136(4) 0.0089(4) 0.0180(5) -0.0061(3) 0.0014(3) -0.0025(3)
As3 0.0164(4) 0.0108(4) 0.0219(5) -0.0067(3) 0.0027(4) -0.0031(3)
As4 0.0129(4) 0.0116(4) 0.0189(5) -0.0059(3) 0.0000(3) -0.0030(3)
As5 0.0169(4) 0.0122(4) 0.0207(5) -0.0079(3) 0.0015(4) -0.0016(3)
As6 0.0195(4) 0.0187(4) 0.0272(5) -0.0099(4) -0.0041(4) -0.0020(4)
As7 0.0258(5) 0.0161(4) 0.0265(5) -0.0014(4) -0.0032(4) -0.0086(4)
Zn1 0.0219(5) 0.0216(5) 0.0252(6) -0.0069(4) -0.0018(4) -0.0039(4)
Zn2 0.0196(5) 0.0159(5) 0.0190(6) -0.0065(4) 0.0004(4) -0.0032(4)
Zn3 0.0193(5) 0.0127(5) 0.0228(6) -0.0062(4) 0.0028(4) -0.0019(4)
Zn4 0.0142(5) 0.0146(5) 0.0230(6) -0.0060(4) -0.0001(4) -0.0019(4)
Zn5 0.0180(5) 0.0125(5) 0.0219(6) -0.0057(4) 0.0008(4) -0.0036(4)
Zn6 0.0157(5) 0.0134(4) 0.0209(6) -0.0060(4) 0.0010(4) -0.0035(4)
O1 0.010(3) 0.027(3) 0.034(4) -0.010(3) -0.005(3) 0.003(2)
O2 0.048(4) 0.033(3) 0.026(4) 0.000(3) -0.007(3) -0.018(3)
O3 0.021(3) 0.011(3) 0.041(4) -0.016(2) -0.001(3) 0.004(2)
O4 0.032(3) 0.016(3) 0.035(4) -0.008(2) 0.007(3) -0.010(3)
O5 0.018(3) 0.015(3) 0.035(4) -0.003(2) -0.002(3) 0.000(2)
O6 0.030(3) 0.021(3) 0.027(3) -0.008(2) -0.001(3) -0.014(3)
O7 0.020(3) 0.017(3) 0.025(3) -0.002(2) -0.001(2) -0.007(2)
O8 0.018(3) 0.012(3) 0.025(3) -0.014(2) 0.008(2) -0.001(2)
O9 0.019(3) 0.015(3) 0.067(5) -0.008(3) -0.005(3) -0.006(2)
O10 0.030(3) 0.007(3) 0.032(4) -0.009(2) -0.004(3) -0.002(2)
O11 0.026(3) 0.025(3) 0.029(4) -0.004(3) 0.001(3) -0.009(3)
O12 0.050(4) 0.031(3) 0.020(3) -0.012(3) 0.006(3) -0.023(3)
O13 0.021(3) 0.048(4) 0.038(4) -0.007(3) -0.016(3) -0.007(3)
O14 0.026(3) 0.021(3) 0.031(4) -0.003(2) 0.002(3) -0.010(2)
O15 0.016(3) 0.013(3) 0.035(4) -0.008(2) 0.004(3) -0.005(2)
O16 0.022(3) 0.009(3) 0.028(3) -0.008(2) 0.003(3) 0.003(2)
O17 0.025(3) 0.029(3) 0.031(4) -0.021(3) 0.008(3) -0.005(3)
O18 0.024(3) 0.032(3) 0.024(4) -0.010(3) 0.000(3) 0.000(3)
O19 0.029(3) 0.019(3) 0.030(4) 0.000(2) -0.003(3) -0.001(3)
O20 0.023(3) 0.020(3) 0.043(4) -0.005(3) 0.003(3) -0.007(2)
O21 0.033(4) 0.031(3) 0.049(4) -0.024(3) -0.015(3) 0.015(3)
O22 0.038(4) 0.026(3) 0.053(5) -0.006(3) -0.027(3) -0.001(3)
O23 0.040(3) 0.031(3) 0.020(3) -0.002(3) -0.007(3) -0.024(3)
O24 0.055(5) 0.077(5) 0.074(6) -0.023(4) 0.014(4) -0.054(4)
O25 0.061(4) 0.029(3) 0.022(4) -0.005(3) -0.005(3) -0.020(3)
O26 0.033(3) 0.024(3) 0.027(4) -0.005(3) 0.001(3) -0.016(3)
O27 0.031(4) 0.027(3) 0.067(5) 0.010(3) -0.015(3) -0.008(3)
O28 0.021(3) 0.025(3) 0.052(4) 0.004(3) -0.005(3) -0.009(3)
O100 0.085(6) 0.058(5) 0.060(5) -0.022(4) 0.013(4) -0.042(4)
N1 0.033(4) 0.028(4) 0.027(4) -0.005(3) 0.002(3) -0.020(3)
C1 0.032(5) 0.021(4) 0.034(6) -0.001(4) -0.001(4) -0.007(4)
C2 0.027(5) 0.040(5) 0.028(5) -0.006(4) -0.001(4) -0.019(4)
C3 0.032(5) 0.033(5) 0.021(5) -0.013(4) 0.005(4) -0.014(4)
N2 0.017(3) 0.020(3) 0.021(4) -0.008(3) -0.001(3) -0.005(3)
C4 0.021(5) 0.025(5) 0.036(6) -0.005(4) -0.008(4) -0.007(4)
C5 0.026(5) 0.037(5) 0.051(7) 0.000(5) 0.003(5) -0.011(4)
C6 0.024(5) 0.027(5) 0.072(8) 0.004(5) -0.001(5) -0.005(4)
N3 0.029(4) 0.019(4) 0.037(5) -0.005(3) -0.001(3) -0.011(3)
N4 0.021(4) 0.033(4) 0.036(5) -0.005(3) 0.002(3) -0.005(3)
C7 0.029(5) 0.022(4) 0.029(5) -0.009(4) 0.005(4) -0.005(4)
C8 0.033(5) 0.034(5) 0.035(6) -0.004(4) 0.001(4) -0.008(4)
C9 0.028(5) 0.022(4) 0.033(6) -0.006(4) -0.004(4) -0.007(4)
N5 0.025(4) 0.018(3) 0.028(4) -0.008(3) 0.004(3) -0.011(3)
C10 0.020(5) 0.038(5) 0.044(6) -0.022(5) -0.002(4) 0.003(4)
C11 0.021(5) 0.022(5) 0.066(7) -0.022(5) 0.001(5) -0.002(4)
C12 0.037(6) 0.036(5) 0.030(6) 0.001(4) -0.006(5) 0.017(5)
N6 0.068(6) 0.022(4) 0.102(8) 0.000(4) -0.059(6) -0.012(4)

_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
As1 O2 1.661(6) . ?
As1 O1 1.669(5) . ?
As1 O3 1.674(5) . ?
As1 O4 1.692(5) . ?
As2 O5 1.674(5) . ?
As2 O6 1.686(5) . ?
As2 O8 1.699(5) . ?
As2 O7 1.699(5) . ?
As3 O10 1.671(4) . ?
As3 O12 1.675(5) . ?
As3 O9 1.675(5) . ?
As3 O11 1.683(5) . ?
As4 O13 1.652(5) . ?
As4 O14 1.678(5) . ?
As4 O15 1.675(5) . ?
As4 O16 1.711(5) . ?
As5 O18 1.653(5) . ?
As5 O17 1.666(5) . ?
As5 O19 1.679(5) . ?
As5 O20 1.714(5) . ?
As6 O21 1.657(5) . ?
As6 O22 1.666(6) . ?
As6 O23 1.665(5) . ?
As6 O24 1.735(6) . ?
As7 O25 1.660(5) . ?
As7 O28 1.678(5) . ?
As7 O26 1.682(5) . ?
As7 O27 1.724(5) . ?
Zn1 O12 1.895(5) . ?
Zn1 O22 1.951(6) . ?
Zn1 O28 1.972(5) 1_655 ?
Zn1 O19 1.994(5) . ?
Zn2 O21 1.931(5) . ?
Zn2 O2 1.936(6) . ?
Zn2 O17 1.942(5) 1_465 ?
Zn2 O26 1.970(5) . ?
Zn3 O3 1.946(5) . ?
Zn3 O7 1.953(5) 2_665 ?
Zn3 O8 1.958(5) . ?
Zn3 O23 1.967(5) . ?
Zn4 O13 1.893(5) 2_756 ?
Zn4 O14 1.941(5) . ?
Zn4 O9 1.946(5) . ?
Zn4 O18 1.990(5) . ?
Zn5 O11 1.918(5) 2_666 ?
Zn5 O10 1.942(5) . ?
Zn5 O15 1.964(5) 1_565 ?
Zn5 O16 1.969(5) 2_666 ?
Zn6 O4 1.944(5) 2_575 ?
Zn6 O6 1.944(5) 2_565 ?
Zn6 O5 1.956(5) 1_465 ?
Zn6 O1 1.968(5) . ?
O4 Zn6 1.944(5) 2_575 ?
O5 Zn6 1.956(5) 1_645 ?
O6 Zn6 1.944(5) 2_565 ?
O7 Zn3 1.953(5) 2_665 ?
O11 Zn5 1.918(5) 2_666 ?
O13 Zn4 1.893(5) 2_756 ?
O15 Zn5 1.964(5) 1_545 ?
O16 Zn5 1.969(5) 2_666 ?
O17 Zn2 1.942(5) 1_645 ?
O20 H50 0.8200 . ?
O24 H60 0.8200 . ?
O27 H70 0.8200 . ?
O28 Zn1 1.972(5) 1_455 ?
N1 C1 1.484(10) . ?
N1 H1 0.8900 . ?
N1 H2 0.8900 . ?
N1 H3 0.8900 . ?
C1 C2 1.507(11) . ?
C1 H4 0.9700 . ?
C1 H5 0.9700 . ?
C2 C3 1.510(11) . ?
C2 H6 0.9700 . ?
C2 H7 0.9700 . ?
C3 N2 1.500(9) . ?
C3 H8 0.9700 . ?
C3 H9 0.9700 . ?
N2 C4 1.521(9) . ?
N2 H10 0.9000 . ?
N2 H11 0.9000 . ?
C4 C5 1.529(12) . ?
C4 H12 0.9700 . ?
C4 H13 0.9700 . ?
C5 C6 1.538(11) . ?
C5 H14 0.9700 . ?
C5 H15 0.9700 . ?
C6 N3 1.483(10) . ?
C6 H16 0.9700 . ?
C6 H17 0.9700 . ?
N3 H18 0.8900 . ?
N3 H19 0.8900 . ?
N3 H20 0.8900 . ?
N4 C7 1.496(9) . ?
N4 H21 0.8900 . ?
N4 H22 0.8900 . ?
N4 H23 0.8900 . ?
C7 C8 1.519(11) . ?
C7 H24 0.9700 . ?
C7 H25 0.9700 . ?
C8 C9 1.516(11) . ?
C8 H26 0.9700 . ?
C8 H27 0.9700 . ?
C9 N5 1.498(10) . ?
C9 H28 0.9700 . ?
C9 H29 0.9700 . ?
N5 C10 1.492(9) . ?
N5 H30 0.9000 . ?
N5 H31 0.9000 . ?
C10 C11 1.512(12) . ?
C10 H32 0.9700 . ?
C10 H33 0.9700 . ?
C11 C12 1.491(12) . ?
C11 H34 0.9700 . ?
C11 H35 0.9700 . ?
C12 N6 1.468(12) . ?
C12 H36 0.9700 . ?
C12 H37 0.9700 . ?
N6 H38 0.8900 . ?
N6 H39 0.8900 . ?
N6 H40 0.8900 . ?

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
O2 As1 O1 106.3(3) . . ?
O2 As1 O3 115.6(3) . . ?
O1 As1 O3 109.9(2) . . ?
O2 As1 O4 104.8(3) . . ?
O1 As1 O4 109.3(3) . . ?
O3 As1 O4 110.7(3) . . ?
O5 As2 O6 114.5(2) . . ?
O5 As2 O8 108.8(3) . . ?
O6 As2 O8 109.5(2) . . ?
O5 As2 O7 109.9(2) . . ?
O6 As2 O7 105.7(2) . . ?
O8 As2 O7 108.3(2) . . ?
O10 As3 O12 110.8(3) . . ?
O10 As3 O9 107.5(2) . . ?
O12 As3 O9 111.3(3) . . ?
O10 As3 O11 112.2(3) . . ?
O12 As3 O11 102.9(3) . . ?
O9 As3 O11 112.1(3) . . ?
O13 As4 O14 114.5(3) . . ?
O13 As4 O15 108.9(3) . . ?
O14 As4 O15 108.1(2) . . ?
O13 As4 O16 104.8(3) . . ?
O14 As4 O16 110.0(2) . . ?
O15 As4 O16 110.6(2) . . ?
O18 As5 O17 107.3(3) . . ?
O18 As5 O19 111.5(3) . . ?
O17 As5 O19 109.8(3) . . ?
O18 As5 O20 110.8(3) . . ?
O17 As5 O20 112.0(2) . . ?
O19 As5 O20 105.5(2) . . ?
O21 As6 O22 111.0(3) . . ?
O21 As6 O23 113.8(3) . . ?
O22 As6 O23 112.1(3) . . ?
O21 As6 O24 107.7(3) . . ?
O22 As6 O24 106.3(3) . . ?
O23 As6 O24 105.4(3) . . ?
O25 As7 O28 112.7(3) . . ?
O25 As7 O26 111.7(3) . . ?
O28 As7 O26 108.5(3) . . ?
O25 As7 O27 106.4(3) . . ?
O28 As7 O27 109.3(3) . . ?
O26 As7 O27 108.2(3) . . ?
O12 Zn1 O22 115.2(3) . . ?
O12 Zn1 O28 119.5(2) . 1_655 ?
O22 Zn1 O28 105.7(2) . 1_655 ?
O12 Zn1 O19 108.9(2) . . ?
O22 Zn1 O19 106.8(2) . . ?
O28 Zn1 O19 99.0(2) 1_655 . ?
O21 Zn2 O2 114.3(3) . . ?
O21 Zn2 O17 100.7(2) . 1_465 ?
O2 Zn2 O17 101.7(2) . 1_465 ?
O21 Zn2 O26 119.2(2) . . ?
O2 Zn2 O26 106.8(2) . . ?
O17 Zn2 O26 113.0(2) 1_465 . ?
O3 Zn3 O7 116.9(2) . 2_665 ?
O3 Zn3 O8 105.0(2) . . ?
O7 Zn3 O8 111.5(2) 2_665 . ?
O3 Zn3 O23 116.9(2) . . ?
O7 Zn3 O23 106.2(2) 2_665 . ?
O8 Zn3 O23 99.0(2) . . ?
O13 Zn4 O14 112.9(2) 2_756 . ?
O13 Zn4 O9 115.3(2) 2_756 . ?
O14 Zn4 O9 112.0(2) . . ?
O13 Zn4 O18 97.3(2) 2_756 . ?
O14 Zn4 O18 108.1(2) . . ?
O9 Zn4 O18 110.2(2) . . ?
O11 Zn5 O10 119.2(2) 2_666 . ?
O11 Zn5 O15 99.8(2) 2_666 1_565 ?
O10 Zn5 O15 109.8(2) . 1_565 ?
O11 Zn5 O16 123.2(2) 2_666 2_666 ?
O10 Zn5 O16 98.0(2) . 2_666 ?
O15 Zn5 O16 106.3(2) 1_565 2_666 ?
O4 Zn6 O6 117.7(2) 2_575 2_565 ?
O4 Zn6 O5 113.1(2) 2_575 1_465 ?
O6 Zn6 O5 110.5(2) 2_565 1_465 ?
O4 Zn6 O1 111.9(2) 2_575 . ?
O6 Zn6 O1 103.3(2) 2_565 . ?
O5 Zn6 O1 98.0(2) 1_465 . ?
As1 O1 Zn6 139.5(3) . . ?
As1 O2 Zn2 147.3(3) . . ?
As1 O3 Zn3 131.8(3) . . ?
As1 O4 Zn6 123.5(3) . 2_575 ?
As2 O5 Zn6 132.6(3) . 1_645 ?
As2 O6 Zn6 132.9(3) . 2_565 ?
As2 O7 Zn3 128.3(3) . 2_665 ?
As2 O8 Zn3 124.3(3) . . ?
As3 O9 Zn4 122.5(3) . . ?
As3 O10 Zn5 128.3(3) . . ?
As3 O11 Zn5 145.5(3) . 2_666 ?
As3 O12 Zn1 142.8(3) . . ?
As4 O13 Zn4 167.7(4) . 2_756 ?
As4 O14 Zn4 125.1(3) . . ?
As4 O15 Zn5 125.8(3) . 1_545 ?
As4 O16 Zn5 126.7(3) . 2_666 ?
As5 O17 Zn2 141.7(3) . 1_645 ?
As5 O18 Zn4 134.7(3) . . ?
As5 O19 Zn1 126.5(3) . . ?
As5 O20 H50 109.5 . . ?
As6 O21 Zn2 127.1(3) . . ?
As6 O22 Zn1 121.3(3) . . ?
As6 O23 Zn3 126.5(3) . . ?
As6 O24 H60 109.5 . . ?
As7 O26 Zn2 125.8(3) . . ?
As7 O27 H70 109.5 . . ?
As7 O28 Zn1 125.0(3) . 1_455 ?
C1 N1 H1 109.5 . . ?
C1 N1 H2 109.5 . . ?
H1 N1 H2 109.5 . . ?
C1 N1 H3 109.5 . . ?
H1 N1 H3 109.5 . . ?
H2 N1 H3 109.5 . . ?
N1 C1 C2 113.2(6) . . ?
N1 C1 H4 108.9 . . ?
C2 C1 H4 108.9 . . ?
N1 C1 H5 108.9 . . ?
C2 C1 H5 108.9 . . ?
H4 C1 H5 107.8 . . ?
C1 C2 C3 119.1(7) . . ?
C1 C2 H6 107.5 . . ?
C3 C2 H6 107.5 . . ?
C1 C2 H7 107.5 . . ?
C3 C2 H7 107.5 . . ?
H6 C2 H7 107.0 . . ?
N2 C3 C2 112.6(6) . . ?
N2 C3 H8 109.1 . . ?
C2 C3 H8 109.1 . . ?
N2 C3 H9 109.1 . . ?
C2 C3 H9 109.1 . . ?
H8 C3 H9 107.8 . . ?
C3 N2 C4 114.8(6) . . ?
C3 N2 H10 108.6 . . ?
C4 N2 H10 108.6 . . ?
C3 N2 H11 108.6 . . ?
C4 N2 H11 108.6 . . ?
H10 N2 H11 107.6 . . ?
N2 C4 C5 109.2(6) . . ?
N2 C4 H12 109.8 . . ?
C5 C4 H12 109.8 . . ?
N2 C4 H13 109.8 . . ?
C5 C4 H13 109.8 . . ?
H12 C4 H13 108.3 . . ?
C4 C5 C6 111.9(8) . . ?
C4 C5 H14 109.2 . . ?
C6 C5 H14 109.2 . . ?
C4 C5 H15 109.2 . . ?
C6 C5 H15 109.2 . . ?
H14 C5 H15 107.9 . . ?
N3 C6 C5 111.8(6) . . ?
N3 C6 H16 109.3 . . ?
C5 C6 H16 109.3 . . ?
N3 C6 H17 109.3 . . ?
C5 C6 H17 109.3 . . ?
H16 C6 H17 107.9 . . ?
C6 N3 H18 109.5 . . ?
C6 N3 H19 109.5 . . ?
H18 N3 H19 109.5 . . ?
C6 N3 H20 109.5 . . ?
H18 N3 H20 109.5 . . ?
H19 N3 H20 109.5 . . ?
C7 N4 H21 109.5 . . ?
C7 N4 H22 109.5 . . ?
H21 N4 H22 109.5 . . ?
C7 N4 H23 109.5 . . ?
H21 N4 H23 109.5 . . ?
H22 N4 H23 109.5 . . ?
N4 C7 C8 109.0(7) . . ?
N4 C7 H24 109.9 . . ?
C8 C7 H24 109.9 . . ?
N4 C7 H25 109.9 . . ?
C8 C7 H25 109.9 . . ?
H24 C7 H25 108.3 . . ?
C9 C8 C7 111.9(7) . . ?
C9 C8 H26 109.2 . . ?
C7 C8 H26 109.2 . . ?
C9 C8 H27 109.2 . . ?
C7 C8 H27 109.2 . . ?
H26 C8 H27 107.9 . . ?
N5 C9 C8 108.3(7) . . ?
N5 C9 H28 110.0 . . ?
C8 C9 H28 110.0 . . ?
N5 C9 H29 110.0 . . ?
C8 C9 H29 110.0 . . ?
H28 C9 H29 108.4 . . ?
C10 N5 C9 114.3(6) . . ?
C10 N5 H30 108.7 . . ?
C9 N5 H30 108.7 . . ?
C10 N5 H31 108.7 . . ?
C9 N5 H31 108.7 . . ?
H30 N5 H31 107.6 . . ?
N5 C10 C11 113.1(7) . . ?
N5 C10 H32 109.0 . . ?
C11 C10 H32 109.0 . . ?
N5 C10 H33 109.0 . . ?
C11 C10 H33 109.0 . . ?
H32 C10 H33 107.8 . . ?
C12 C11 C10 117.4(7) . . ?
C12 C11 H34 108.0 . . ?
C10 C11 H34 108.0 . . ?
C12 C11 H35 108.0 . . ?
C10 C11 H35 108.0 . . ?
H34 C11 H35 107.2 . . ?
N6 C12 C11 113.9(8) . . ?
N6 C12 H36 108.8 . . ?
C11 C12 H36 108.8 . . ?
N6 C12 H37 108.8 . . ?
C11 C12 H37 108.8 . . ?
H36 C12 H37 107.7 . . ?
C12 N6 H38 109.5 . . ?
C12 N6 H39 109.5 . . ?
H38 N6 H39 109.5 . . ?
C12 N6 H40 109.5 . . ?
H38 N6 H40 109.5 . . ?
H39 N6 H40 109.5 . . ?

_diffrn_measured_fraction_theta_max    0.993
_diffrn_reflns_theta_full              23.24
_diffrn_measured_fraction_theta_full   0.993
_refine_diff_density_max    0.978
_refine_diff_density_min   -0.816
_refine_diff_density_rms    0.175