# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013

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#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
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data_1
#TrackingRef '1.CIF'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H22 N2 O12 P4 Zn3'
_chemical_formula_weight         658.27

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'
P P 0.1023 0.0942 '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'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

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                   9.7412(5)
_cell_length_b                   13.0955(6)
_cell_length_c                   15.6922(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.092(5)
_cell_angle_gamma                90.00
_cell_volume                     1993.89(14)
_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       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.193
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1320
_exptl_absorpt_coefficient_mu    3.963
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.6477
_exptl_absorpt_correction_T_max  0.7422
_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       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15514
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         26.50
_reflns_number_total             4129
_reflns_number_gt                3317
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0451P)^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         4129
_refine_ls_number_parameters     262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0376
_refine_ls_wR_factor_ref         0.0858
_refine_ls_wR_factor_gt          0.0817
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_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
Zn1 Zn 0.28845(4) 0.13752(3) 0.25016(3) 0.01897(12) Uani 1 1 d . . .
Zn2 Zn -0.18929(4) 0.02908(3) 0.43410(3) 0.01789(12) Uani 1 1 d . . .
Zn3 Zn -0.40300(4) -0.13144(3) 0.09005(3) 0.02153(13) Uani 1 1 d . . .
P1 P 0.35934(9) 0.03917(8) 0.08559(6) 0.0201(2) Uani 1 1 d . . .
H1 H 0.4602 0.1130 0.1138 0.024 Uiso 1 1 d R . .
P2 P 0.10195(9) 0.11297(8) 0.40618(6) 0.0199(2) Uani 1 1 d . . .
H2 H 0.1707 0.1963 0.4555 0.024 Uiso 1 1 d R . .
P3 P -0.50266(9) 0.12727(7) 0.40727(7) 0.0202(2) Uani 1 1 d . . .
H3 H -0.5633 0.0605 0.4453 0.024 Uiso 1 1 d R . .
P4 P -0.30293(10) -0.12087(7) 0.28634(7) 0.0215(2) Uani 1 1 d . . .
H4 H -0.4377 -0.0928 0.3115 0.026 Uiso 1 1 d R . .
O1 O 0.2535(2) 0.0507(2) 0.15029(16) 0.0248(6) Uani 1 1 d . . .
O2 O 0.4607(3) 0.1067(3) 0.3140(2) 0.0469(9) Uani 1 1 d . . .
O3 O 0.3059(4) 0.2672(2) 0.1954(2) 0.0509(9) Uani 1 1 d . . .
O4 O 0.1304(3) 0.1183(2) 0.31320(18) 0.0354(8) Uani 1 1 d . . .
O5 O -0.0497(2) 0.13240(19) 0.41590(17) 0.0242(6) Uani 1 1 d . . .
O6 O -0.3513(2) 0.1131(2) 0.43073(19) 0.0334(7) Uani 1 1 d . . .
O7 O -0.1537(3) -0.0142(2) 0.55209(17) 0.0284(7) Uani 1 1 d . . .
O8 O -0.1910(3) -0.0658(2) 0.34168(18) 0.0319(7) Uani 1 1 d . . .
O9 O -0.2928(3) -0.0975(3) 0.19354(19) 0.0472(9) Uani 1 1 d . . .
O10 O -0.2998(3) -0.0704(2) 0.00292(17) 0.0310(7) Uani 1 1 d . . .
O11 O -0.4467(3) -0.2715(2) 0.0643(2) 0.0363(7) Uani 1 1 d . . .
O12 O -0.5822(3) -0.0671(2) 0.0864(2) 0.0376(8) Uani 1 1 d . . .
C1 C 0.2088(4) -0.3524(3) 0.2823(3) 0.0342(11) Uani 1 1 d . . .
H1A H 0.3000 -0.3828 0.2883 0.041 Uiso 1 1 calc R . .
H1B H 0.1673 -0.3669 0.2251 0.041 Uiso 1 1 calc R . .
C2 C 0.1217(4) -0.3977(3) 0.3476(3) 0.0310(10) Uani 1 1 d . . .
H2A H 0.0310 -0.4146 0.3206 0.037 Uiso 1 1 calc R . .
H2B H 0.1640 -0.4600 0.3707 0.037 Uiso 1 1 calc R . .
C3 C 0.0777(4) -0.1977(3) 0.3010(3) 0.0342(11) Uani 1 1 d . . .
H3A H 0.0170 -0.2217 0.2528 0.041 Uiso 1 1 calc R . .
H3B H 0.0797 -0.1237 0.2992 0.041 Uiso 1 1 calc R . .
C4 C 0.0247(4) -0.2329(3) 0.3838(3) 0.0288(10) Uani 1 1 d . . .
H4A H 0.0317 -0.1778 0.4252 0.035 Uiso 1 1 calc R . .
H4B H -0.0715 -0.2524 0.3738 0.035 Uiso 1 1 calc R . .
C5 C 0.3038(4) -0.2182(3) 0.3788(3) 0.0288(10) Uani 1 1 d . . .
H5A H 0.2958 -0.1469 0.3942 0.035 Uiso 1 1 calc R . .
H5B H 0.4001 -0.2332 0.3734 0.035 Uiso 1 1 calc R . .
C6 C 0.2500(4) -0.2855(3) 0.4473(3) 0.0287(10) Uani 1 1 d . . .
H6A H 0.3113 -0.3432 0.4588 0.034 Uiso 1 1 calc R . .
H6B H 0.2472 -0.2469 0.4999 0.034 Uiso 1 1 calc R . .
C7 C 0.2851(5) -0.1909(4) 0.2223(3) 0.0499(14) Uani 1 1 d . . .
H7A H 0.3763 -0.2179 0.2197 0.075 Uiso 1 1 calc R . .
H7B H 0.2904 -0.1183 0.2307 0.075 Uiso 1 1 calc R . .
H7C H 0.2307 -0.2054 0.1697 0.075 Uiso 1 1 calc R . .
C8 C 0.0443(5) -0.3693(3) 0.4911(3) 0.0379(11) Uani 1 1 d . . .
H8A H -0.0468 -0.3927 0.4722 0.057 Uiso 1 1 calc R . .
H8B H 0.0389 -0.3194 0.5355 0.057 Uiso 1 1 calc R . .
H8C H 0.0991 -0.4260 0.5129 0.057 Uiso 1 1 calc R . .
N1 N 0.2198(3) -0.2391(3) 0.2953(2) 0.0270(8) Uani 1 1 d . . .
N2 N 0.1087(3) -0.3227(2) 0.4180(2) 0.0216(7) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.0201(2) 0.0217(2) 0.0150(2) -0.00069(18) 0.00075(17) 0.00373(17)
Zn2 0.0159(2) 0.0213(2) 0.0159(2) -0.00172(18) -0.00178(17) 0.00147(17)
Zn3 0.0238(2) 0.0226(3) 0.0176(2) 0.00337(19) -0.00119(18) -0.00324(18)
P1 0.0194(5) 0.0231(5) 0.0177(5) -0.0029(4) 0.0014(4) -0.0037(4)
P2 0.0159(5) 0.0284(6) 0.0156(5) 0.0007(4) 0.0023(4) -0.0008(4)
P3 0.0146(5) 0.0189(5) 0.0263(6) 0.0021(4) -0.0026(4) 0.0028(4)
P4 0.0268(5) 0.0164(5) 0.0203(6) -0.0026(4) -0.0034(4) 0.0000(4)
O1 0.0245(14) 0.0302(16) 0.0203(15) -0.0089(12) 0.0048(11) -0.0067(11)
O2 0.0289(16) 0.073(2) 0.036(2) -0.0185(17) -0.0114(14) 0.0168(16)
O3 0.098(3) 0.0188(17) 0.036(2) 0.0004(14) 0.0082(19) -0.0002(17)
O4 0.0269(15) 0.062(2) 0.0176(15) 0.0075(14) 0.0058(12) 0.0042(14)
O5 0.0171(13) 0.0266(15) 0.0292(16) 0.0000(12) 0.0042(11) -0.0008(11)
O6 0.0167(14) 0.0356(17) 0.045(2) -0.0126(14) -0.0120(13) 0.0092(12)
O7 0.0320(15) 0.0365(17) 0.0169(14) 0.0028(13) 0.0028(12) 0.0075(12)
O8 0.0308(15) 0.0350(17) 0.0283(17) -0.0151(14) -0.0067(13) 0.0030(13)
O9 0.063(2) 0.052(2) 0.0233(17) 0.0082(15) -0.0117(15) -0.0313(17)
O10 0.0291(15) 0.0444(18) 0.0198(15) 0.0101(14) 0.0038(12) -0.0078(13)
O11 0.0375(16) 0.0243(16) 0.047(2) 0.0013(14) 0.0055(14) -0.0112(13)
O12 0.0327(16) 0.0334(17) 0.048(2) 0.0036(15) 0.0119(14) 0.0096(13)
C1 0.042(3) 0.032(3) 0.028(2) -0.014(2) -0.003(2) 0.0084(19)
C2 0.034(2) 0.019(2) 0.039(3) -0.0097(19) -0.004(2) 0.0009(17)
C3 0.039(2) 0.030(2) 0.032(3) 0.001(2) -0.005(2) 0.0136(19)
C4 0.028(2) 0.026(2) 0.032(2) 0.0010(19) -0.0022(18) 0.0110(17)
C5 0.027(2) 0.028(2) 0.031(2) -0.0027(19) -0.0045(18) -0.0058(17)
C6 0.025(2) 0.029(2) 0.030(2) 0.0000(19) -0.0105(17) -0.0027(17)
C7 0.070(4) 0.055(3) 0.028(3) 0.016(2) 0.019(3) 0.010(3)
C8 0.038(3) 0.037(3) 0.039(3) 0.010(2) 0.007(2) 0.001(2)
N1 0.0356(19) 0.0264(19) 0.0191(18) -0.0006(15) 0.0022(15) 0.0046(15)
N2 0.0225(16) 0.0189(17) 0.0223(18) -0.0001(14) -0.0041(13) 0.0022(13)

_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
Zn1 O3 1.918(3) . ?
Zn1 O4 1.919(3) . ?
Zn1 O2 1.919(3) . ?
Zn1 O1 1.942(3) . ?
Zn2 O8 1.909(3) . ?
Zn2 O6 1.921(2) . ?
Zn2 O7 1.938(3) . ?
Zn2 O5 1.957(2) . ?
Zn3 O11 1.918(3) . ?
Zn3 O9 1.918(3) . ?
Zn3 O12 1.935(3) . ?
Zn3 O10 1.940(3) . ?
P1 O12 1.503(3) 1_655 ?
P1 O10 1.513(3) 3 ?
P1 O1 1.517(3) . ?
P1 H1 1.4207 . ?
P2 O4 1.511(3) . ?
P2 O7 1.516(3) 3_556 ?
P2 O5 1.520(3) . ?
P2 H2 1.4650 . ?
P3 O11 1.497(3) 2_455 ?
P3 O6 1.500(2) . ?
P3 O2 1.500(3) 1_455 ?
P3 H3 1.2383 . ?
P4 O3 1.494(3) 2_545 ?
P4 O9 1.500(3) . ?
P4 O8 1.515(3) . ?
P4 H4 1.4513 . ?
O2 P3 1.500(3) 1_655 ?
O3 P4 1.494(3) 2 ?
O7 P2 1.516(3) 3_556 ?
O10 P1 1.513(3) 3 ?
O11 P3 1.497(3) 2_445 ?
O12 P1 1.503(3) 1_455 ?
C1 N1 1.501(5) . ?
C1 C2 1.509(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.492(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N1 1.497(5) . ?
C3 C4 1.513(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N2 1.504(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N1 1.507(5) . ?
C5 C6 1.518(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N2 1.494(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N1 1.498(5) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 N2 1.487(5) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Zn1 O4 117.02(14) . . ?
O3 Zn1 O2 108.16(15) . . ?
O4 Zn1 O2 114.06(13) . . ?
O3 Zn1 O1 99.99(12) . . ?
O4 Zn1 O1 104.37(12) . . ?
O2 Zn1 O1 112.36(12) . . ?
O8 Zn2 O6 113.60(11) . . ?
O8 Zn2 O7 121.63(12) . . ?
O6 Zn2 O7 105.69(12) . . ?
O8 Zn2 O5 107.38(12) . . ?
O6 Zn2 O5 100.34(12) . . ?
O7 Zn2 O5 105.90(11) . . ?
O11 Zn3 O9 119.82(14) . . ?
O11 Zn3 O12 103.16(13) . . ?
O9 Zn3 O12 111.06(15) . . ?
O11 Zn3 O10 111.41(13) . . ?
O9 Zn3 O10 102.42(12) . . ?
O12 Zn3 O10 108.81(12) . . ?
O12 P1 O10 111.85(18) 1_655 3 ?
O12 P1 O1 111.41(17) 1_655 . ?
O10 P1 O1 111.08(15) 3 . ?
O12 P1 H1 112.1 1_655 . ?
O10 P1 H1 107.5 3 . ?
O1 P1 H1 102.5 . . ?
O4 P2 O7 111.96(17) . 3_556 ?
O4 P2 O5 110.64(16) . . ?
O7 P2 O5 112.87(15) 3_556 . ?
O4 P2 H2 111.1 . . ?
O7 P2 H2 106.8 3_556 . ?
O5 P2 H2 103.0 . . ?
O11 P3 O6 112.31(16) 2_455 . ?
O11 P3 O2 113.18(18) 2_455 1_455 ?
O6 P3 O2 111.17(17) . 1_455 ?
O11 P3 H3 107.3 2_455 . ?
O6 P3 H3 107.2 . . ?
O2 P3 H3 105.2 1_455 . ?
O3 P4 O9 112.99(19) 2_545 . ?
O3 P4 O8 112.47(18) 2_545 . ?
O9 P4 O8 110.70(17) . . ?
O3 P4 H4 99.4 2_545 . ?
O9 P4 H4 110.6 . . ?
O8 P4 H4 110.2 . . ?
P1 O1 Zn1 121.15(15) . . ?
P3 O2 Zn1 126.36(19) 1_655 . ?
P4 O3 Zn1 141.2(2) 2 . ?
P2 O4 Zn1 136.76(17) . . ?
P2 O5 Zn2 126.37(15) . . ?
P3 O6 Zn2 149.91(18) . . ?
P2 O7 Zn2 133.35(18) 3_556 . ?
P4 O8 Zn2 134.66(17) . . ?
P4 O9 Zn3 134.01(19) . . ?
P1 O10 Zn3 125.31(16) 3 . ?
P3 O11 Zn3 149.0(2) 2_445 . ?
P1 O12 Zn3 138.03(19) 1_455 . ?
N1 C1 C2 109.6(3) . . ?
N1 C1 H1A 109.8 . . ?
C2 C1 H1A 109.8 . . ?
N1 C1 H1B 109.8 . . ?
C2 C1 H1B 109.8 . . ?
H1A C1 H1B 108.2 . . ?
N2 C2 C1 109.5(3) . . ?
N2 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
N2 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
N1 C3 C4 109.3(3) . . ?
N1 C3 H3A 109.8 . . ?
C4 C3 H3A 109.8 . . ?
N1 C3 H3B 109.8 . . ?
C4 C3 H3B 109.8 . . ?
H3A C3 H3B 108.3 . . ?
N2 C4 C3 109.1(3) . . ?
N2 C4 H4A 109.9 . . ?
C3 C4 H4A 109.9 . . ?
N2 C4 H4B 109.9 . . ?
C3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
N1 C5 C6 108.5(3) . . ?
N1 C5 H5A 110.0 . . ?
C6 C5 H5A 110.0 . . ?
N1 C5 H5B 110.0 . . ?
C6 C5 H5B 110.0 . . ?
H5A C5 H5B 108.4 . . ?
N2 C6 C5 109.7(3) . . ?
N2 C6 H6A 109.7 . . ?
C5 C6 H6A 109.7 . . ?
N2 C6 H6B 109.7 . . ?
C5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C3 N1 C7 110.6(3) . . ?
C3 N1 C1 108.1(3) . . ?
C7 N1 C1 110.1(3) . . ?
C3 N1 C5 108.4(3) . . ?
C7 N1 C5 110.7(3) . . ?
C1 N1 C5 108.9(3) . . ?
C8 N2 C2 111.7(3) . . ?
C8 N2 C6 109.6(3) . . ?
C2 N2 C6 107.9(3) . . ?
C8 N2 C4 110.0(3) . . ?
C2 N2 C4 109.3(3) . . ?
C6 N2 C4 108.2(3) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.113
_database_code_depnum_ccdc_archive 'CCDC 927967'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1
#TrackingRef 'CCDC-927968.CIF'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H25 N2 O12 P4 Zn3'
_chemical_formula_weight         673.30

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'
P P 0.1023 0.0942 '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'

_symmetry_cell_setting           monoclini
_symmetry_space_group_name_H-M   P21/m

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

_cell_length_a                   7.9578(6)
_cell_length_b                   14.7728(2)
_cell_length_c                   9.2582(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.755(3)
_cell_angle_gamma                90.00
_cell_volume                     1087.87(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.055
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             678
_exptl_absorpt_coefficient_mu    3.634
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.5940
_exptl_absorpt_correction_T_max  0.7126
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6241
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.56
_diffrn_reflns_theta_max         26.50
_reflns_number_total             2325
_reflns_number_gt                2128
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+4.5946P] 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         2325
_refine_ls_number_parameters     148
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0428
_refine_ls_wR_factor_ref         0.0893
_refine_ls_wR_factor_gt          0.0883
_refine_ls_goodness_of_fit_ref   1.276
_refine_ls_restrained_S_all      1.276
_refine_ls_shift/su_max          0.001
_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
Zn1 Zn 0.12271(11) 0.2500 0.23452(8) 0.0295(2) Uani 1 2 d S . .
Zn2 Zn 0.12592(8) 0.11069(4) -0.36466(5) 0.03143(16) Uani 1 1 d . . .
P1 P 0.0699(2) 0.2500 -0.09579(17) 0.0268(4) Uani 1 2 d S . .
H1 H -0.1005 0.2500 -0.0283 0.032 Uiso 1 2 d SR . .
P2 P -0.13133(16) 0.10635(8) -0.63728(13) 0.0283(3) Uani 1 1 d . . .
H2 H -0.2449 0.1567 -0.6557 0.034 Uiso 1 1 d R . .
P3 P 0.3805(2) 0.2500 -0.50843(18) 0.0269(4) Uani 1 2 d S . .
H3 H 0.5449 0.2500 -0.5053 0.032 Uiso 1 2 d SR . .
O1 O 0.3410(7) 0.2500 0.3320(6) 0.0508(15) Uani 1 2 d S . .
O2 O -0.0031(6) 0.1406(3) 0.2607(4) 0.0583(12) Uani 1 1 d . . .
O3 O 0.1910(6) 0.2500 0.0338(5) 0.0332(11) Uani 1 2 d S . .
O4 O 0.0824(7) 0.1646(3) -0.1802(4) 0.0611(13) Uani 1 1 d . . .
O5 O 0.1915(5) -0.0131(2) -0.3178(4) 0.0430(9) Uani 1 1 d . . .
O6 O 0.3266(5) 0.1645(3) -0.4368(5) 0.0518(10) Uani 1 1 d . . .
O7 O -0.0772(5) 0.1141(3) -0.4812(4) 0.0475(10) Uani 1 1 d . . .
C1 C 0.5071(7) 0.0824(4) -0.0821(6) 0.0440(13) Uani 1 1 d . . .
H1A H 0.3990 0.0758 -0.1345 0.053 Uiso 1 1 calc R . .
C2 C 0.4713(7) 0.0807(4) 0.0764(6) 0.0426(13) Uani 1 1 d . . .
H2A H 0.4013 0.1323 0.0986 0.051 Uiso 1 1 calc R . .
H2B H 0.5765 0.0873 0.1311 0.051 Uiso 1 1 calc R . .
C3 C 0.5732(15) 0.1680(8) -0.1203(16) 0.061(4) Uani 0.50 1 d P . .
H3A H 0.5954 0.1686 -0.2217 0.091 Uiso 0.50 1 calc PR . .
H3B H 0.6758 0.1788 -0.0658 0.091 Uiso 0.50 1 calc PR . .
H3C H 0.4932 0.2144 -0.0994 0.091 Uiso 0.50 1 calc PR . .
C4 C 0.7934(7) 0.0091(4) -0.0630(7) 0.0511(15) Uani 1 1 d . . .
H4A H 0.7913 0.0114 0.0405 0.077 Uiso 1 1 calc R . .
H4B H 0.8472 0.0624 -0.0985 0.077 Uiso 1 1 calc R . .
H4C H 0.8546 -0.0436 -0.0921 0.077 Uiso 1 1 calc R . .
C5 C 0.6246(9) 0.0006(6) -0.2880(6) 0.067(2) Uani 1 1 d . . .
H5A H 0.5131 -0.0023 -0.3303 0.101 Uiso 1 1 calc R . .
H5B H 0.6869 -0.0520 -0.3154 0.101 Uiso 1 1 calc R . .
H5C H 0.6801 0.0540 -0.3217 0.101 Uiso 1 1 calc R . .
N1 N 0.6149(5) 0.0041(3) -0.1247(5) 0.0377(10) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.0433(5) 0.0285(4) 0.0170(3) 0.000 0.0030(3) 0.000
Zn2 0.0500(4) 0.0245(3) 0.0196(3) -0.0017(2) -0.0014(2) -0.0094(3)
P1 0.0348(9) 0.0294(9) 0.0163(7) 0.000 0.0019(6) 0.000
P2 0.0356(7) 0.0223(6) 0.0267(6) -0.0016(5) -0.0027(5) -0.0022(5)
P3 0.0243(8) 0.0301(9) 0.0264(8) 0.000 0.0012(6) 0.000
O1 0.046(3) 0.076(4) 0.031(3) 0.000 -0.003(2) 0.000
O2 0.084(3) 0.048(2) 0.044(2) -0.0061(19) 0.021(2) -0.028(2)
O3 0.032(3) 0.050(3) 0.018(2) 0.000 0.0015(19) 0.000
O4 0.119(4) 0.037(2) 0.0275(18) -0.0114(17) 0.009(2) -0.015(2)
O5 0.056(2) 0.0247(18) 0.047(2) -0.0004(15) -0.0127(18) -0.0088(17)
O6 0.047(2) 0.042(2) 0.066(3) 0.017(2) 0.005(2) -0.0100(19)
O7 0.057(2) 0.057(2) 0.0285(18) -0.0068(17) -0.0078(16) -0.004(2)
C1 0.046(3) 0.034(3) 0.052(3) 0.008(2) 0.007(3) 0.009(2)
C2 0.043(3) 0.033(3) 0.052(3) -0.010(2) 0.007(3) 0.006(2)
C3 0.038(7) 0.049(7) 0.095(10) 0.013(7) 0.016(7) 0.001(6)
C4 0.047(3) 0.054(4) 0.052(3) -0.002(3) 0.003(3) 0.005(3)
C5 0.070(5) 0.097(6) 0.035(3) 0.002(3) 0.008(3) 0.017(4)
N1 0.039(2) 0.039(2) 0.035(2) 0.0008(19) 0.0029(18) 0.007(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
Zn1 O2 1.920(4) . ?
Zn1 O2 1.920(4) 4_565 ?
Zn1 O1 1.933(6) . ?
Zn1 O3 1.952(4) . ?
Zn2 O7 1.917(4) . ?
Zn2 O6 1.922(4) . ?
Zn2 O4 1.925(4) . ?
Zn2 O5 1.946(4) . ?
P1 O4 1.489(4) . ?
P1 O4 1.489(4) 4_565 ?
P1 O3 1.516(5) . ?
P1 H1 1.5102 . ?
P2 O7 1.499(3) . ?
P2 O2 1.499(4) 1_554 ?
P2 O5 1.513(4) 3_554 ?
P2 H2 1.1791 . ?
P3 O6 1.495(4) 4_565 ?
P3 O6 1.495(4) . ?
P3 O1 1.501(5) 1_554 ?
P3 H3 1.3080 . ?
O1 P3 1.501(5) 1_556 ?
O2 P2 1.499(4) 1_556 ?
O5 P2 1.513(3) 3_554 ?
C1 C3 1.418(13) . ?
C1 N1 1.500(7) . ?
C1 C2 1.503(7) . ?
C1 H1A 0.9800 . ?
C2 N1 1.504(7) 3_655 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 N1 1.516(7) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 N1 1.518(7) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
N1 C2 1.504(7) 3_655 ?

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 Zn1 O2 114.6(3) . 4_565 ?
O2 Zn1 O1 113.93(16) . . ?
O2 Zn1 O1 113.93(16) 4_565 . ?
O2 Zn1 O3 106.37(13) . . ?
O2 Zn1 O3 106.37(13) 4_565 . ?
O1 Zn1 O3 99.9(2) . . ?
O7 Zn2 O6 119.26(17) . . ?
O7 Zn2 O4 108.49(19) . . ?
O6 Zn2 O4 108.13(19) . . ?
O7 Zn2 O5 111.46(16) . . ?
O6 Zn2 O5 104.25(17) . . ?
O4 Zn2 O5 104.19(17) . . ?
O4 P1 O4 115.8(3) . 4_565 ?
O4 P1 O3 111.4(2) . . ?
O4 P1 O3 111.4(2) 4_565 . ?
O4 P1 H1 107.0 . . ?
O4 P1 H1 107.0 4_565 . ?
O3 P1 H1 103.3 . . ?
O7 P2 O2 113.6(2) . 1_554 ?
O7 P2 O5 114.4(2) . 3_554 ?
O2 P2 O5 110.5(2) 1_554 3_554 ?
O7 P2 H2 106.7 . . ?
O2 P2 H2 103.3 1_554 . ?
O5 P2 H2 107.5 3_554 . ?
O6 P3 O6 115.3(3) 4_565 . ?
O6 P3 O1 112.5(2) 4_565 1_554 ?
O6 P3 O1 112.5(2) . 1_554 ?
O6 P3 H3 106.9 4_565 . ?
O6 P3 H3 106.9 . . ?
O1 P3 H3 101.6 1_554 . ?
P3 O1 Zn1 128.1(4) 1_556 . ?
P2 O2 Zn1 137.0(3) 1_556 . ?
P1 O3 Zn1 124.4(3) . . ?
P1 O4 Zn2 146.4(3) . . ?
P2 O5 Zn2 135.5(2) 3_554 . ?
P3 O6 Zn2 139.1(3) . . ?
P2 O7 Zn2 138.9(3) . . ?
C3 C1 N1 113.7(6) . . ?
C3 C1 C2 110.0(8) . . ?
N1 C1 C2 111.8(4) . . ?
C3 C1 H1A 107.0 . . ?
N1 C1 H1A 107.0 . . ?
C2 C1 H1A 107.0 . . ?
C1 C2 N1 113.9(4) . 3_655 ?
C1 C2 H2A 108.8 . . ?
N1 C2 H2A 108.8 3_655 . ?
C1 C2 H2B 108.8 . . ?
N1 C2 H2B 108.8 3_655 . ?
H2A C2 H2B 107.7 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C1 N1 C2 107.2(4) . 3_655 ?
C1 N1 C4 113.6(4) . . ?
C2 N1 C4 111.0(4) 3_655 . ?
C1 N1 C5 109.6(4) . . ?
C2 N1 C5 107.8(5) 3_655 . ?
C4 N1 C5 107.5(4) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.186
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.098


_database_code_depnum_ccdc_archive 'CCDC 927968'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H15 N2 O12 P3 Zn2'
_chemical_formula_weight         542.86

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'
P P 0.1023 0.0942 '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'

_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                   16.2387(2)
_cell_length_b                   9.3708(7)
_cell_length_c                   10.5007(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.898(3)
_cell_angle_gamma                90.00
_cell_volume                     1594.19(14)
_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       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1088
_exptl_absorpt_coefficient_mu    3.380
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.7287
_exptl_absorpt_correction_T_max  0.8767
_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       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12322
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.26
_diffrn_reflns_theta_max         26.50
_reflns_number_total             3273
_reflns_number_gt                2917
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+1.2984P] 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         3273
_refine_ls_number_parameters     235
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0275
_refine_ls_wR_factor_ref         0.0723
_refine_ls_wR_factor_gt          0.0705
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_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
Zn1 Zn 0.047483(18) 0.42901(3) 0.83836(3) 0.01479(10) Uani 1 1 d . . .
Zn2 Zn 0.414866(19) 0.62609(3) 0.86153(3) 0.01656(10) Uani 1 1 d . . .
P1 P -0.06158(4) 0.70717(7) 0.88843(6) 0.01559(15) Uani 1 1 d . . .
P2 P 0.24612(4) 0.47725(8) 0.88173(7) 0.01839(16) Uani 1 1 d . . .
P3 P 0.46048(4) 0.61325(7) 1.15908(7) 0.01644(16) Uani 1 1 d . . .
O1 O -0.15933(12) 0.7193(2) 0.86390(19) 0.0260(5) Uani 1 1 d . . .
H1A H -0.1817 0.6724 0.9178 0.039 Uiso 1 1 calc R . .
O2 O -0.03859(14) 0.5676(2) 0.8298(2) 0.0354(6) Uani 1 1 d . . .
O3 O 0.02891(13) 0.3368(2) 0.67577(19) 0.0286(5) Uani 1 1 d . . .
O4 O 0.03912(13) 0.2872(2) 0.96968(18) 0.0259(5) Uani 1 1 d . . .
O5 O 0.15615(12) 0.5140(2) 0.8667(2) 0.0285(5) Uani 1 1 d . . .
O6 O 0.27016(14) 0.3996(2) 1.0059(2) 0.0319(5) Uani 1 1 d . . .
O7 O 0.26852(14) 0.3744(2) 0.7694(2) 0.0335(5) Uani 1 1 d . . .
H7A H 0.2265 0.3351 0.7392 0.050 Uiso 1 1 calc R . .
O8 O 0.29864(12) 0.6097(2) 0.8707(2) 0.0267(5) Uani 1 1 d . . .
O9 O 0.42981(17) 0.7868(3) 0.7545(2) 0.0448(6) Uani 1 1 d . . .
O10 O 0.45747(13) 0.4505(2) 0.7926(2) 0.0308(5) Uani 1 1 d . . .
O11 O 0.46479(13) 0.6818(2) 1.02846(19) 0.0257(5) Uani 1 1 d . . .
O12 O 0.40062(14) 0.4804(3) 1.1466(2) 0.0367(6) Uani 1 1 d . . .
H12A H 0.4211 0.4185 1.1035 0.055 Uiso 1 1 calc R . .
C1 C 0.8680(2) 1.1143(4) 0.9873(3) 0.0354(8) Uani 1 1 d . . .
H1B H 0.9210 1.1463 0.9747 0.042 Uiso 1 1 calc R . .
C2 C 0.8567(2) 1.0060(4) 1.0711(3) 0.0378(8) Uani 1 1 d . . .
H2D H 0.9016 0.9658 1.1176 0.045 Uiso 1 1 calc R . .
C3 C 0.7783(2) 0.9568(3) 1.0862(3) 0.0336(8) Uani 1 1 d . . .
H3A H 0.7703 0.8827 1.1430 0.040 Uiso 1 1 calc R . .
C4 C 0.72582(18) 1.1277(3) 0.9359(3) 0.0226(6) Uani 1 1 d . . .
H4A H 0.6818 1.1705 0.8892 0.027 Uiso 1 1 calc R . .
C5 C 0.71111(19) 1.0167(3) 1.0176(3) 0.0227(6) Uani 1 1 d . . .
C6 C 0.6253(2) 0.9603(3) 1.0266(3) 0.0319(7) Uani 1 1 d . . .
H6A H 0.6163 0.9402 1.1152 0.038 Uiso 1 1 calc R . .
H6B H 0.5858 1.0323 0.9964 0.038 Uiso 1 1 calc R . .
C7 C 0.8167(3) 1.2934(4) 0.8349(4) 0.0476(10) Uani 1 1 d U . .
H7B H 0.7648 1.3257 0.7962 0.071 Uiso 1 1 calc R . .
H7C H 0.8511 1.2614 0.7697 0.071 Uiso 1 1 calc R . .
H7D H 0.8436 1.3705 0.8815 0.071 Uiso 1 1 calc R . .
N1 N 0.80261(16) 1.1748(3) 0.9228(2) 0.0265(6) Uani 1 1 d . . .
N2 N 0.61159(16) 0.8276(3) 0.9495(2) 0.0252(5) Uani 1 1 d . . .
H2A H 0.5603 0.7967 0.9564 0.038 Uiso 1 1 calc R . .
H2B H 0.6471 0.7608 0.9782 0.038 Uiso 1 1 calc R . .
H2C H 0.6192 0.8461 0.8680 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
Zn1 0.01316(16) 0.01762(16) 0.01360(16) 0.00005(11) 0.00108(11) 0.00006(12)
Zn2 0.01518(17) 0.01861(17) 0.01591(17) 0.00125(12) 0.00117(12) -0.00252(12)
P1 0.0153(3) 0.0169(3) 0.0145(3) 0.0017(3) 0.0006(3) 0.0002(3)
P2 0.0134(3) 0.0217(3) 0.0199(4) 0.0006(3) 0.0004(3) -0.0050(3)
P3 0.0156(4) 0.0191(3) 0.0145(3) -0.0037(3) 0.0003(3) 0.0015(3)
O1 0.0172(10) 0.0323(11) 0.0287(11) 0.0132(9) 0.0033(8) 0.0024(9)
O2 0.0330(13) 0.0319(12) 0.0397(14) -0.0138(10) -0.0088(10) 0.0149(10)
O3 0.0328(12) 0.0336(11) 0.0186(10) -0.0114(9) -0.0028(9) 0.0117(10)
O4 0.0341(12) 0.0278(11) 0.0155(10) 0.0062(8) -0.0008(8) -0.0075(9)
O5 0.0149(10) 0.0337(11) 0.0368(13) 0.0002(10) 0.0004(9) -0.0056(9)
O6 0.0264(12) 0.0418(13) 0.0273(12) 0.0120(10) -0.0006(9) -0.0031(10)
O7 0.0233(12) 0.0399(13) 0.0376(13) -0.0160(10) 0.0035(10) -0.0076(10)
O8 0.0167(10) 0.0227(10) 0.0408(13) -0.0016(9) 0.0030(9) -0.0056(8)
O9 0.0592(17) 0.0449(14) 0.0305(13) 0.0177(11) 0.0048(12) -0.0195(13)
O10 0.0270(12) 0.0319(12) 0.0318(12) -0.0096(9) -0.0094(9) 0.0111(9)
O11 0.0273(11) 0.0327(11) 0.0165(10) 0.0015(9) -0.0032(8) -0.0094(9)
O12 0.0351(13) 0.0375(13) 0.0364(13) 0.0070(10) -0.0058(10) -0.0133(11)
C1 0.0235(17) 0.0382(18) 0.044(2) -0.0101(15) -0.0031(14) -0.0057(14)
C2 0.0329(19) 0.0345(18) 0.043(2) -0.0041(15) -0.0191(15) 0.0040(15)
C3 0.048(2) 0.0239(16) 0.0278(17) 0.0028(13) -0.0060(15) -0.0015(15)
C4 0.0220(15) 0.0228(14) 0.0222(15) -0.0034(11) -0.0031(11) 0.0032(12)
C5 0.0273(15) 0.0188(13) 0.0220(15) -0.0055(11) 0.0024(12) -0.0032(12)
C6 0.0331(18) 0.0292(16) 0.0347(18) -0.0086(14) 0.0130(14) -0.0060(14)
C7 0.059(2) 0.0389(19) 0.045(2) 0.0061(16) 0.0053(18) -0.0144(18)
N1 0.0298(14) 0.0240(12) 0.0256(13) -0.0027(10) 0.0006(11) -0.0060(11)
N2 0.0242(13) 0.0244(12) 0.0270(13) -0.0002(10) 0.0025(10) -0.0050(10)

_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
Zn1 O2 1.906(2) . ?
Zn1 O3 1.919(2) . ?
Zn1 O4 1.9263(19) . ?
Zn1 O5 1.940(2) . ?
Zn2 O8 1.903(2) . ?
Zn2 O9 1.905(2) . ?
Zn2 O10 1.944(2) . ?
Zn2 O11 1.952(2) . ?
P1 O2 1.503(2) . ?
P1 O3 1.504(2) 2_556 ?
P1 O4 1.511(2) 3_567 ?
P1 O1 1.595(2) . ?
P2 O5 1.499(2) . ?
P2 O8 1.514(2) . ?
P2 O6 1.521(2) . ?
P2 O7 1.585(2) . ?
P3 O9 1.482(2) 4_576 ?
P3 O10 1.516(2) 3_667 ?
P3 O11 1.521(2) . ?
P3 O12 1.579(2) . ?
O1 H1A 0.8200 . ?
O3 P1 1.504(2) 2_546 ?
O4 P1 1.511(2) 3_567 ?
O7 H7A 0.8200 . ?
O9 P3 1.482(2) 4_575 ?
O10 P3 1.516(2) 3_667 ?
O12 H12A 0.8200 . ?
C1 N1 1.345(4) . ?
C1 C2 1.364(5) . ?
C1 H1B 0.9300 . ?
C2 C3 1.373(5) . ?
C2 H2D 0.9300 . ?
C3 C5 1.385(4) . ?
C3 H3A 0.9300 . ?
C4 N1 1.338(4) . ?
C4 C5 1.380(4) . ?
C4 H4A 0.9300 . ?
C5 C6 1.499(4) . ?
C6 N2 1.492(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N1 1.473(4) . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C7 H7D 0.9600 . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 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 Zn1 O3 101.20(9) . . ?
O2 Zn1 O4 114.63(10) . . ?
O3 Zn1 O4 108.18(9) . . ?
O2 Zn1 O5 112.58(10) . . ?
O3 Zn1 O5 114.06(10) . . ?
O4 Zn1 O5 106.30(9) . . ?
O8 Zn2 O9 105.10(11) . . ?
O8 Zn2 O10 109.26(9) . . ?
O9 Zn2 O10 112.75(11) . . ?
O8 Zn2 O11 109.20(9) . . ?
O9 Zn2 O11 104.87(10) . . ?
O10 Zn2 O11 115.12(9) . . ?
O2 P1 O3 114.47(14) . 2_556 ?
O2 P1 O4 112.60(13) . 3_567 ?
O3 P1 O4 110.20(12) 2_556 3_567 ?
O2 P1 O1 105.53(12) . . ?
O3 P1 O1 104.35(12) 2_556 . ?
O4 P1 O1 109.13(12) 3_567 . ?
O5 P2 O8 110.71(12) . . ?
O5 P2 O6 113.04(13) . . ?
O8 P2 O6 110.15(13) . . ?
O5 P2 O7 109.45(13) . . ?
O8 P2 O7 106.42(12) . . ?
O6 P2 O7 106.77(14) . . ?
O9 P3 O10 110.52(14) 4_576 3_667 ?
O9 P3 O11 112.39(14) 4_576 . ?
O10 P3 O11 112.05(13) 3_667 . ?
O9 P3 O12 108.71(15) 4_576 . ?
O10 P3 O12 103.83(13) 3_667 . ?
O11 P3 O12 108.92(12) . . ?
P1 O1 H1A 109.5 . . ?
P1 O2 Zn1 140.82(15) . . ?
P1 O3 Zn1 136.37(13) 2_546 . ?
P1 O4 Zn1 131.15(13) 3_567 . ?
P2 O5 Zn1 142.34(14) . . ?
P2 O7 H7A 109.5 . . ?
P2 O8 Zn2 129.48(13) . . ?
P3 O9 Zn2 163.9(2) 4_575 . ?
P3 O10 Zn2 122.39(13) 3_667 . ?
P3 O11 Zn2 130.94(13) . . ?
P3 O12 H12A 109.5 . . ?
N1 C1 C2 120.1(3) . . ?
N1 C1 H1B 119.9 . . ?
C2 C1 H1B 119.9 . . ?
C1 C2 C3 119.4(3) . . ?
C1 C2 H2D 120.3 . . ?
C3 C2 H2D 120.3 . . ?
C2 C3 C5 120.5(3) . . ?
C2 C3 H3A 119.7 . . ?
C5 C3 H3A 119.7 . . ?
N1 C4 C5 120.9(3) . . ?
N1 C4 H4A 119.5 . . ?
C5 C4 H4A 119.5 . . ?
C4 C5 C3 117.7(3) . . ?
C4 C5 C6 120.4(3) . . ?
C3 C5 C6 121.8(3) . . ?
N2 C6 C5 111.4(2) . . ?
N2 C6 H6A 109.3 . . ?
C5 C6 H6A 109.3 . . ?
N2 C6 H6B 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
N1 C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C7 H7D 109.5 . . ?
H7B C7 H7D 109.5 . . ?
H7C C7 H7D 109.5 . . ?
C4 N1 C1 121.2(3) . . ?
C4 N1 C7 119.9(3) . . ?
C1 N1 C7 118.8(3) . . ?
C6 N2 H2A 109.5 . . ?
C6 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
C6 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?

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
O1 H1A O6 0.82 1.82 2.585(3) 154.3 3_567
O7 H7A O1 0.82 1.84 2.623(3) 159.6 2_546
O12 H12A N2 0.82 2.42 3.060(3) 135.2 3_667
O12 H12A O11 0.82 2.57 3.319(3) 153.1 3_667
N2 H2A O11 0.89 2.07 2.916(3) 157.9 .
N2 H2B O6 0.89 2.01 2.883(3) 165.0 3_667
N2 H2C O10 0.89 2.25 2.943(3) 134.4 2_656
N2 H2C O7 0.89 2.42 3.142(3) 139.1 2_656

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.089
_database_code_depnum_ccdc_archive 'CCDC 940009'