# Copyright The Royal Society of Chemistry, 1999
# CCDC Number: 440/093



data_data

_audit_creation_method            SHELXL
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_formula_moiety          ?
_chemical_formula_structural      ?
_chemical_formula_analytical      ?
_chemical_formula_sum             'C4 H14 N3 O16 P4 Zn5'
_chemical_formula_weight          811.01
_chemical_melting_point           ?
_chemical_compound_source         ?

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    Cc

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

_cell_length_a                    27.070(2)
_cell_length_b                    5.2154(4)
_cell_length_c                    17.9202(15)
_cell_angle_alpha                 90.00
_cell_angle_beta                  130.2560(10)
_cell_angle_gamma                 90.00
_cell_volume                      1930.8(3)
_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           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.789
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              1206
_exptl_absorpt_coefficient_mu     6.543
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?

_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        'Siemens P4'
_diffrn_measurement_method        '\w scans'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             3775
_diffrn_reflns_av_R_equivalents   0.0504
_diffrn_reflns_av_sigmaI/netI     0.0697
_diffrn_reflns_limit_h_min        -29
_diffrn_reflns_limit_h_max        29
_diffrn_reflns_limit_k_min        -5
_diffrn_reflns_limit_k_max        5
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        17
_diffrn_reflns_theta_min          1.97
_diffrn_reflns_theta_max          23.28
_reflns_number_total              2089
_reflns_number_observed           1994
_reflns_observed_criterion        >2sigma(I)

_computing_data_collection        'Siemens XSCANS'
_computing_cell_refinement        'Siemens XSCANS'
_computing_data_reduction         'Siemens SHELXTL'
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics     'Siemens SHELXTL'
_computing_publication_material   'Siemens SHELXTL'

_refine_special_details
;
 Refinement on F^2^ for ALL reflections except for 0 with very negative 
F^2^
 or flagged by the user for potential systematic errors.  Weighted R-
factors
 wR and all goodnesses 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 observed 
criterion
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0702P)^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     ?
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0060(4)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    0.48(3)
_refine_ls_number_reflns          2089
_refine_ls_number_parameters      291
_refine_ls_number_restraints      2
_refine_ls_R_factor_all           0.0433
_refine_ls_R_factor_obs           0.0389
_refine_ls_wR_factor_all          0.1168
_refine_ls_wR_factor_obs          0.0901
_refine_ls_goodness_of_fit_all    1.140
_refine_ls_goodness_of_fit_obs    0.903
_refine_ls_restrained_S_all       1.140
_refine_ls_restrained_S_obs       0.903
_refine_ls_shift/esd_max          0.001
_refine_ls_shift/esd_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_thermal_displace_type
 _atom_site_occupancy
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_group
Zn1 Zn -0.40994(7) -1.3149(3) -0.86990(10) 0.0124(4) Uani 1 d . .
Zn2 Zn -0.78267(6) -1.7957(3) -1.27425(10) 0.0137(4) Uani 1 d . .
Zn3 Zn -0.53550(6) -1.7189(2) -0.97442(10) 0.0123(4) Uani 1 d . .
Zn4 Zn -0.63240(7) -1.2283(2) -1.10692(11) 0.0141(4) Uani 1 d . .
Zn5 Zn -0.52330(7) -1.1260(3) -0.70228(11) 0.0143(4) Uani 1 d . .
P1 P -0.6397(2) -1.7481(6) -1.2055(3) 0.0110(7) Uani 1 d . .
P2 P -0.7726(2) -1.2772(6) -1.1649(3) 0.0122(8) Uani 1 d . .
P3 P -0.4239(2) -0.8102(6) -0.9751(3) 0.0108(7) Uani 1 d . .
P4 P -0.5251(2) -1.2159(6) -0.8740(3) 0.0113(7) Uani 1 d . .
O1 O -0.3178(4) -1.3757(16) -0.7645(6) 0.015(2) Uani 1 d . .
O2 O -0.4378(4) -1.0947(16) -0.9766(6) 0.019(2) Uani 1 d . .
O3 O -0.4482(4) -1.6596(16) -0.9275(7) 0.018(2) Uani 1 d . .
O4 O -0.4529(5) -1.2316(17) -0.8199(7) 0.020(2) Uani 1 d . .
O5 O -0.7780(5) -1.5624(17) -1.1857(7) 0.027(2) Uani 1 d . .
O6 O -0.7094(4) -1.8388(20) -1.2684(7) 0.025(2) Uani 1 d . .
O7 O -0.8519(4) -1.7477(17) -1.4131(8) 0.022(2) Uani 1 d . .
O8 O -0.5630(4) -1.3743(16) -0.9721(6) 0.015(2) Uani 1 d . .
O9 O -0.5997(4) -1.8841(16) -1.1041(6) 0.017(2) Uani 1 d . .
O10 O -0.5500(4) -0.9351(15) -0.9025(6) 0.017(2) Uani 1 d . .
O11 O -0.7054(4) -1.1758(19) -1.1142(8) 0.025(2) Uani 1 d . .
O12 O -0.6317(4) -1.4596(17) -1.1890(7) 0.024(2) Uani 1 d . .
O13 O -0.5416(4) -1.3171(16) -0.8131(7) 0.018(2) Uani 1 d . .
O14 O -0.6123(4) -1.1644(17) -0.7542(7) 0.016(2) Uani 1 d . .
O15 O -0.4601(5) -1.2920(15) -0.5784(7) 0.018(2) Uani 1 d . .
O16 O -0.7892(5) -1.2227(16) -1.0991(8) 0.022(2) Uani 1 d . .
N2 N -0.3078(6) -0.7651(21) -0.5521(9) 0.020(3) Uani 1 d . .
H9 H -0.3055(6) -0.6095(21) -0.5715(9) 0.024 Uiso 1 calc R .
H8 H -0.3078(6) -0.8842(21) -0.5885(9) 0.024 Uiso 1 calc R .
N1 N -0.1675(5) -0.5528(23) -0.4335(8) 0.026(3) Uani 1 d . .
H3 H -0.1310(5) -0.5651(23) -0.4241(8) 0.039 Uiso 1 calc R .
H2 H -0.1605(5) -0.4589(23) -0.3859(8) 0.039 Uiso 1 calc R .
H1 H -0.1979(5) -0.4784(23) -0.4909(8) 0.039 Uiso 1 calc R .
N3 N -0.4874(5) -0.7723(19) -0.6878(9) 0.015(3) Uani 1 d . .
H14 H -0.5074(5) -0.6388(19) -0.6912(9) 0.018 Uiso 1 calc R .
C2 C -0.2512(7) -0.8033(26) -0.4483(11) 0.022(3) Uani 1 d . .
H7 H -0.2560(7) -0.9631(26) -0.4258(11) 0.027 Uiso 1 calc R .
H6 H -0.2489(7) -0.6650(26) -0.4100(11) 0.027 Uiso 1 calc R .
C1 C -0.1892(6) -0.8107(26) -0.4327(11) 0.025(3) Uani 1 d . .
H5 H -0.1556(6) -0.8923(26) -0.3704(11) 0.030 Uiso 1 calc R .
H4 H -0.1960(6) -0.9133(26) -0.4837(11) 0.030 Uiso 1 calc R .
C3 C -0.3674(7) -0.7845(31) -0.5671(12) 0.031(4) Uani 1 d . .
H10 H -0.3669(7) -0.6578(31) -0.5270(12) 0.037 Uiso 1 calc R .
H11 H -0.3700(7) -0.9529(31) -0.5468(12) 0.037 Uiso 1 calc R .
C4 C -0.4250(8) -0.7430(29) -0.6711(12) 0.025(4) Uani 1 d . .
H12 H -0.4247(8) -0.8658(29) -0.7114(12) 0.030 Uiso 1 calc R .
H13 H -0.4232(8) -0.5724(29) -0.6907(12) 0.030 Uiso 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 0.0108(7) 0.0130(7) 0.0104(8) 0.0001(6) 0.0054(6) 0.0003(6)
Zn2 0.0107(8) 0.0157(8) 0.0115(8) 0.0002(6) 0.0057(7) -0.0011(6)
Zn3 0.0127(8) 0.0111(7) 0.0108(8) -0.0014(6) 0.0066(7) -0.0014(6)
Zn4 0.0140(8) 0.0133(7) 0.0113(8) -0.0010(6) 0.0065(7) -0.0011(6)
Zn5 0.0137(7) 0.0165(7) 0.0103(7) 0.0011(6) 0.0066(6) 0.0002(6)
P1 0.010(2) 0.011(2) 0.009(2) -0.0006(12) 0.005(2) -0.0005(11)
P2 0.010(2) 0.015(2) 0.008(2) 0.0010(12) 0.005(2) 0.0002(12)
P3 0.010(2) 0.011(2) 0.007(2) -0.0014(13) 0.0039(15) -0.0009(12)
P4 0.011(2) 0.011(2) 0.008(2) -0.0001(13) 0.004(2) 0.0016(12)
O1 0.009(4) 0.014(4) 0.010(4) -0.004(4) 0.001(4) 0.001(3)
O2 0.023(5) 0.015(5) 0.016(5) 0.000(4) 0.011(4) -0.002(4)
O3 0.019(5) 0.014(4) 0.024(5) -0.004(4) 0.015(5) 0.000(3)
O4 0.015(5) 0.030(5) 0.013(6) -0.004(4) 0.009(5) 0.000(3)
O5 0.045(6) 0.014(5) 0.017(5) -0.002(4) 0.018(5) -0.001(4)
O6 0.014(5) 0.045(6) 0.014(5) -0.008(4) 0.008(4) -0.009(4)
O7 0.013(5) 0.036(6) 0.014(5) 0.005(4) 0.007(5) 0.000(4)
O8 0.023(5) 0.009(4) 0.007(4) 0.001(4) 0.006(4) 0.002(3)
O9 0.021(5) 0.014(4) 0.008(4) 0.000(4) 0.006(4) -0.004(4)
O10 0.026(4) 0.009(4) 0.023(5) 0.003(4) 0.019(4) 0.004(4)
O11 0.011(5) 0.034(6) 0.021(5) -0.003(4) 0.006(4) -0.003(4)
O12 0.040(5) 0.014(5) 0.020(5) -0.003(4) 0.021(5) -0.002(4)
O13 0.018(5) 0.020(5) 0.019(5) -0.001(4) 0.013(5) 0.001(3)
O14 0.017(5) 0.024(5) 0.009(5) 0.000(4) 0.009(5) 0.001(4)
O15 0.025(6) 0.015(5) 0.008(5) -0.004(4) 0.008(5) 0.002(4)
O16 0.025(6) 0.022(5) 0.019(6) 0.002(4) 0.014(6) 0.004(4)
N2 0.013(6) 0.025(6) 0.022(8) -0.005(5) 0.011(6) -0.002(4)
N1 0.023(6) 0.037(7) 0.011(6) -0.007(5) 0.008(5) -0.009(5)
N3 0.012(7) 0.014(5) 0.017(7) -0.006(4) 0.008(6) 0.000(4)
C2 0.022(8) 0.032(8) 0.017(8) 0.003(6) 0.014(7) -0.004(6)
C1 0.014(8) 0.035(9) 0.013(8) -0.004(6) 0.003(7) -0.003(6)
C3 0.026(9) 0.052(11) 0.021(9) 0.006(7) 0.018(8) 0.010(7)
C4 0.022(9) 0.039(9) 0.013(9) -0.007(6) 0.010(8) -0.006(6)

_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are 
taken
 into account individually in the estimation of esds in distances, 
angles
 and torsion angles; correlations between esds in cell parameters are 
only
 used when they are defined by crystal symmetry.  An approximate 
(isotropic)
 treatment of cell esds is used for estimating esds involving l.s. 
planes.
;

loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Zn1 O2 1.919(9) . ?
Zn1 O4 1.922(9) . ?
Zn1 O1 1.950(8) . ?
Zn1 O3 1.997(8) . ?
Zn2 O6 1.931(9) . ?
Zn2 O7 1.934(10) . ?
Zn2 O5 1.938(9) . ?
Zn2 O1 2.021(8) 4_414 ?
Zn3 O10 1.933(8) 1_545 ?
Zn3 O3 1.953(8) . ?
Zn3 O8 1.956(8) . ?
Zn3 O9 1.986(8) . ?
Zn4 O12 1.911(9) . ?
Zn4 O11 1.913(9) . ?
Zn4 O9 1.987(8) 1_565 ?
Zn4 O8 2.020(9) . ?
Zn5 O15 1.922(9) . ?
Zn5 O14 1.952(9) . ?
Zn5 O13 1.977(9) . ?
Zn5 N3 2.022(10) . ?
P1 O6 1.518(9) . ?
P1 O12 1.522(9) . ?
P1 O14 1.536(9) 2_524 ?
P1 O9 1.561(9) . ?
P2 O11 1.510(10) . ?
P2 O5 1.518(9) . ?
P2 O16 1.535(10) . ?
P2 O1 1.580(9) 4_424 ?
P3 O15 1.525(10) 2_534 ?
P3 O7 1.526(10) 4_525 ?
P3 O2 1.527(8) . ?
P3 O3 1.582(9) 1_565 ?
P4 O13 1.517(10) . ?
P4 O4 1.521(10) . ?
P4 O10 1.554(8) . ?
P4 O8 1.580(9) . ?
O1 P2 1.580(9) 4_525 ?
O1 Zn2 2.021(8) 4_515 ?
O3 P3 1.582(9) 1_545 ?
O7 P3 1.526(10) 4_424 ?
O9 Zn4 1.987(8) 1_545 ?
O10 Zn3 1.933(8) 1_565 ?
O14 P1 1.536(9) 2_525 ?
O15 P3 1.526(10) 2_535 ?
N2 C3 1.46(2) . ?
N2 C2 1.47(2) . ?
N2 H9 0.90 . ?
N2 H8 0.90 . ?
N1 C1 1.47(2) . ?
N1 H3 0.89 . ?
N1 H2 0.89 . ?
N1 H1 0.89 . ?
N3 C4 1.52(2) . ?
N3 H14 0.86 . ?
C2 C1 1.51(2) . ?
C2 H7 0.97 . ?
C2 H6 0.97 . ?
C1 H5 0.97 . ?
C1 H4 0.97 . ?
C3 C4 1.48(2) . ?
C3 H10 0.97 . ?
C3 H11 0.97 . ?
C4 H12 0.97 . ?
C4 H13 0.97 . ?

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 O4 111.3(4) . . ?
O2 Zn1 O1 119.7(3) . . ?
O4 Zn1 O1 111.5(4) . . ?
O2 Zn1 O3 106.6(4) . . ?
O4 Zn1 O3 100.1(4) . . ?
O1 Zn1 O3 105.4(3) . . ?
O6 Zn2 O7 101.0(4) . . ?
O6 Zn2 O5 120.5(4) . . ?
O7 Zn2 O5 118.0(4) . . ?
O6 Zn2 O1 114.9(4) . 4_414 ?
O7 Zn2 O1 95.9(3) . 4_414 ?
O5 Zn2 O1 104.3(4) . 4_414 ?
O10 Zn3 O3 121.0(4) 1_545 . ?
O10 Zn3 O8 106.1(3) 1_545 . ?
O3 Zn3 O8 102.5(4) . . ?
O10 Zn3 O9 97.2(3) 1_545 . ?
O3 Zn3 O9 118.2(4) . . ?
O8 Zn3 O9 111.5(4) . . ?
O12 Zn4 O11 124.1(4) . . ?
O12 Zn4 O9 111.4(4) . 1_565 ?
O11 Zn4 O9 107.2(4) . 1_565 ?
O12 Zn4 O8 102.6(4) . . ?
O11 Zn4 O8 104.9(4) . . ?
O9 Zn4 O8 104.8(3) 1_565 . ?
O15 Zn5 O14 114.0(4) . . ?
O15 Zn5 O13 113.0(4) . . ?
O14 Zn5 O13 92.2(4) . . ?
O15 Zn5 N3 105.5(4) . . ?
O14 Zn5 N3 119.8(4) . . ?
O13 Zn5 N3 112.1(4) . . ?
O6 P1 O12 113.9(5) . . ?
O6 P1 O14 108.1(5) . 2_524 ?
O12 P1 O14 110.2(5) . 2_524 ?
O6 P1 O9 108.5(5) . . ?
O12 P1 O9 108.6(5) . . ?
O14 P1 O9 107.5(5) 2_524 . ?
O11 P2 O5 112.2(5) . . ?
O11 P2 O16 108.1(6) . . ?
O5 P2 O16 109.9(5) . . ?
O11 P2 O1 104.8(5) . 4_424 ?
O5 P2 O1 109.6(5) . 4_424 ?
O16 P2 O1 112.2(5) . 4_424 ?
O15 P3 O7 109.3(6) 2_534 4_525 ?
O15 P3 O2 111.1(5) 2_534 . ?
O7 P3 O2 112.9(5) 4_525 . ?
O15 P3 O3 108.4(5) 2_534 1_565 ?
O7 P3 O3 106.9(5) 4_525 1_565 ?
O2 P3 O3 108.0(5) . 1_565 ?
O13 P4 O4 112.2(6) . . ?
O13 P4 O10 107.3(5) . . ?
O4 P4 O10 111.4(5) . . ?
O13 P4 O8 109.7(5) . . ?
O4 P4 O8 108.9(5) . . ?
O10 P4 O8 107.1(5) . . ?
P2 O1 Zn1 125.7(5) 4_525 . ?
P2 O1 Zn2 117.5(5) 4_525 4_515 ?
Zn1 O1 Zn2 115.6(4) . 4_515 ?
P3 O2 Zn1 129.1(5) . . ?
P3 O3 Zn3 119.9(5) 1_545 . ?
P3 O3 Zn1 117.9(5) 1_545 . ?
Zn3 O3 Zn1 116.4(4) . . ?
P4 O4 Zn1 129.1(6) . . ?
P2 O5 Zn2 139.6(6) . . ?
P1 O6 Zn2 138.1(6) . . ?
P3 O7 Zn2 133.0(6) 4_424 . ?
P4 O8 Zn3 121.4(5) . . ?
P4 O8 Zn4 124.6(5) . . ?
Zn3 O8 Zn4 113.2(4) . . ?
P1 O9 Zn3 126.1(5) . . ?
P1 O9 Zn4 114.8(5) . 1_545 ?
Zn3 O9 Zn4 117.4(4) . 1_545 ?
P4 O10 Zn3 122.5(5) . 1_565 ?
P2 O11 Zn4 141.3(7) . . ?
P1 O12 Zn4 134.7(6) . . ?
P4 O13 Zn5 123.2(5) . . ?
P1 O14 Zn5 131.3(6) 2_525 . ?
P3 O15 Zn5 129.7(5) 2_535 . ?
C3 N2 C2 110.3(12) . . ?
C3 N2 H9 109.6(8) . . ?
C2 N2 H9 109.6(7) . . ?
C3 N2 H8 109.6(8) . . ?
C2 N2 H8 109.6(7) . . ?
H9 N2 H8 108.1 . . ?
C1 N1 H3 109.5(7) . . ?
C1 N1 H2 109.5(7) . . ?
H3 N1 H2 109.5 . . ?
C1 N1 H1 109.5(7) . . ?
H3 N1 H1 109.5 . . ?
H2 N1 H1 109.5 . . ?
C4 N3 Zn5 119.8(8) . . ?
C4 N3 H14 120.1(7) . . ?
Zn5 N3 H14 120.1(3) . . ?
N2 C2 C1 111.2(12) . . ?
N2 C2 H7 109.4(7) . . ?
C1 C2 H7 109.4(7) . . ?
N2 C2 H6 109.4(7) . . ?
C1 C2 H6 109.4(8) . . ?
H7 C2 H6 108.0 . . ?
N1 C1 C2 112.2(11) . . ?
N1 C1 H5 109.2(7) . . ?
C2 C1 H5 109.2(8) . . ?
N1 C1 H4 109.2(7) . . ?
C2 C1 H4 109.2(8) . . ?
H5 C1 H4 107.9 . . ?
N2 C3 C4 111.2(13) . . ?
N2 C3 H10 109.4(8) . . ?
C4 C3 H10 109.4(8) . . ?
N2 C3 H11 109.4(8) . . ?
C4 C3 H11 109.4(9) . . ?
H10 C3 H11 108.0 . . ?
C3 C4 N3 111.5(12) . . ?
C3 C4 H12 109.3(8) . . ?
N3 C4 H12 109.3(7) . . ?
C3 C4 H13 109.3(9) . . ?
N3 C4 H13 109.3(7) . . ?
H12 C4 H13 108.0 . . ?

_refine_diff_density_max    1.159
_refine_diff_density_min   -1.002
_refine_diff_density_rms    0.268

data_datam

_audit_creation_method            SHELXL
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_formula_moiety          ?
_chemical_formula_structural      ?
_chemical_formula_analytical      ?
_chemical_formula_sum             'C1 H7 N5 O8 P2 Zn2'
_chemical_formula_weight          409.8
_chemical_melting_point           ?
_chemical_compound_source         ?

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)/n

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

_cell_length_a                    8.0893(8)
_cell_length_b                    12.7708(14)
_cell_length_c                    10.0663(11)
_cell_angle_alpha                 90.00
_cell_angle_beta                  105.275(2)
_cell_angle_gamma                 90.00
_cell_volume                      1003.2(2)
_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           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.713
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              603
_exptl_absorpt_coefficient_mu     5.151
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?

_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        'Siemens P4'
_diffrn_measurement_method        '\w scans'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             4109
_diffrn_reflns_av_R_equivalents   0.0894
_diffrn_reflns_av_sigmaI/netI     0.0697
_diffrn_reflns_limit_h_min        -8
_diffrn_reflns_limit_h_max        5
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -11
_diffrn_reflns_limit_l_max        10
_diffrn_reflns_theta_min          2.63
_diffrn_reflns_theta_max          23.28
_reflns_number_total              1436
_reflns_number_observed           1193
_reflns_observed_criterion        >2sigma(I)

_computing_data_collection        'Siemens XSCANS'
_computing_cell_refinement        'Siemens XSCANS'
_computing_data_reduction         'Siemens SHELXTL'
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics     'Siemens SHELXTL'
_computing_publication_material   'Siemens SHELXTL'

_refine_special_details
;
 Refinement on F^2^ for ALL reflections except for 0 with very negative 
F^2^
 or flagged by the user for potential systematic errors.  Weighted R-
factors
 wR and all goodnesses 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 observed 
criterion
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+3.2779P] 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     ?
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          1436
_refine_ls_number_parameters      163
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0554
_refine_ls_R_factor_obs           0.0422
_refine_ls_wR_factor_all          0.1095
_refine_ls_wR_factor_obs          0.0993
_refine_ls_goodness_of_fit_all    1.082
_refine_ls_goodness_of_fit_obs    1.090
_refine_ls_restrained_S_all       1.082
_refine_ls_restrained_S_obs       1.090
_refine_ls_shift/esd_max          -0.001
_refine_ls_shift/esd_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_thermal_displace_type
 _atom_site_occupancy
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_group
Zn1 Zn 0.12537(10) 0.59596(6) 0.02375(8) 0.0140(3) Uani 1 d . .
Zn2 Zn -0.22612(10) 0.99096(6) 0.04551(8) 0.0123(3) Uani 1 d . .
P1 P 0.0512(2) 0.82083(14) 0.0749(2) 0.0117(4) Uani 1 d . .
P2 P 0.0107(2) 0.50656(13) -0.2828(2) 0.0111(4) Uani 1 d . .
O1 O -0.0254(6) 0.7147(4) 0.0279(5) 0.0187(12) Uani 1 d . .
O2 O 0.0183(6) 0.4967(3) -0.1289(5) 0.0125(11) Uani 1 d . .
O3 O -0.3542(6) 0.9461(4) -0.1354(5) 0.0167(11) Uani 1 d . .
O4 O -0.0710(6) 0.8816(4) 0.1416(5) 0.0165(11) Uani 1 d . .
O5 O -0.0888(6) 1.1167(4) 0.0423(5) 0.0154(11) Uani 1 d . .
O6 O -0.3243(6) 1.0426(4) 0.1925(5) 0.0148(11) Uani 1 d . .
O7 O 0.2185(6) 0.8010(4) 0.1939(5) 0.0212(12) Uani 1 d . .
H10 H 0.2633(6) 0.8572(4) 0.2218(5) 0.032 Uiso 1 calc R .
O8 O -0.0006(6) 0.6217(4) -0.3247(5) 0.0174(11) Uani 1 d . .
N1 N 0.6108(8) 0.6837(5) -0.0315(7) 0.027(2) Uani 1 d . .
H2 H 0.5977(8) 0.7179(5) -0.1072(7) 0.033 Uiso 1 calc R .
H1 H 0.7122(8) 0.6700(5) 0.0187(7) 0.033 Uiso 1 calc R .
N2 N 0.5021(8) 0.5947(5) 0.1254(6) 0.025(2) Uani 1 d . .
H3 H 0.6045(8) 0.5803(5) 0.1727(6) 0.030 Uiso 1 calc R .
N3 N 0.3125(7) 0.6670(4) -0.0582(6) 0.0143(13) Uani 1 d . .
N4 N 0.2846(7) 0.7260(5) -0.1831(6) 0.0178(14) Uani 1 d . .
H4 H 0.3706(7) 0.7486(5) -0.2099(6) 0.021 Uiso 1 calc R .
H5 H 0.1819(7) 0.7387(5) -0.2313(6) 0.021 Uiso 1 calc R .
N5 N 0.3601(7) 0.5599(5) 0.1680(6) 0.0205(15) Uani 1 d . .
H6 H 0.3675(7) 0.5274(5) 0.2443(6) 0.025 Uiso 1 calc R .
C1 C 0.4745(9) 0.6519(6) 0.0078(7) 0.017(2) Uani 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 0.0122(5) 0.0172(5) 0.0130(5) -0.0008(4) 0.0040(3) -0.0001(3)
Zn2 0.0133(5) 0.0158(5) 0.0084(5) 0.0003(3) 0.0038(4) 0.0004(3)
P1 0.0106(10) 0.0132(9) 0.0120(10) 0.0012(8) 0.0041(7) -0.0004(7)
P2 0.0091(10) 0.0155(10) 0.0090(10) 0.0016(7) 0.0030(7) 0.0007(7)
O1 0.012(3) 0.016(3) 0.029(3) 0.001(2) 0.006(2) -0.003(2)
O2 0.013(3) 0.018(3) 0.008(3) -0.002(2) 0.006(2) -0.003(2)
O3 0.018(3) 0.025(3) 0.005(3) 0.002(2) -0.001(2) 0.006(2)
O4 0.018(3) 0.019(3) 0.013(3) 0.000(2) 0.005(2) 0.005(2)
O5 0.020(3) 0.021(3) 0.006(2) 0.003(2) 0.005(2) -0.005(2)
O6 0.018(3) 0.023(3) 0.007(3) 0.000(2) 0.008(2) -0.003(2)
O7 0.015(3) 0.028(3) 0.016(3) 0.009(2) -0.005(2) -0.002(2)
O8 0.013(3) 0.019(3) 0.019(3) 0.010(2) 0.003(2) 0.002(2)
N1 0.007(3) 0.055(5) 0.020(4) 0.004(3) 0.003(3) -0.008(3)
N2 0.014(3) 0.048(4) 0.011(3) 0.011(3) 0.000(3) 0.004(3)
N3 0.018(3) 0.018(3) 0.007(3) 0.005(3) 0.002(3) -0.002(3)
N4 0.011(3) 0.027(4) 0.014(3) 0.008(3) 0.001(3) 0.001(3)
N5 0.012(3) 0.038(4) 0.012(3) 0.005(3) 0.006(3) -0.002(3)
C1 0.013(4) 0.017(4) 0.020(4) -0.002(3) 0.003(3) -0.001(3)

_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 O1 1.954(5) . ?
Zn1 O2 2.004(4) . ?
Zn1 N3 2.110(6) . ?
Zn1 N5 2.115(6) . ?
Zn1 O2 2.126(4) 3_565 ?
Zn1 Zn1 3.137(2) 3_565 ?
Zn2 O3 1.929(5) . ?
Zn2 O4 1.955(5) . ?
Zn2 O5 1.957(5) . ?
Zn2 O6 1.968(5) . ?
P1 O1 1.514(5) . ?
P1 O5 1.521(5) 3_575 ?
P1 O4 1.543(5) . ?
P1 O7 1.573(5) . ?
P2 O3 1.526(5) 2_444 ?
P2 O8 1.526(5) . ?
P2 O2 1.539(5) . ?
P2 O6 1.553(5) 4_675 ?
O2 Zn1 2.126(4) 3_565 ?
O3 P2 1.526(5) 2_454 ?
O5 P1 1.521(5) 3_575 ?
O6 P2 1.553(5) 4_576 ?
O7 H10 0.82 . ?
N1 C1 1.330(9) . ?
N1 H2 0.86 . ?
N1 H1 0.86 . ?
N2 C1 1.359(9) . ?
N2 N5 1.401(8) . ?
N2 H3 0.86 . ?
N3 C1 1.318(9) . ?
N3 N4 1.432(8) . ?
N4 H4 0.86 . ?
N4 H5 0.86 . ?
N5 H6 0.86 . ?

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 Zn1 O2 111.2(2) . . ?
O1 Zn1 N3 101.0(2) . . ?
O2 Zn1 N3 100.5(2) . . ?
O1 Zn1 N5 127.4(2) . . ?
O2 Zn1 N5 121.1(2) . . ?
N3 Zn1 N5 75.9(2) . . ?
O1 Zn1 O2 89.7(2) . 3_565 ?
O2 Zn1 O2 81.2(2) . 3_565 ?
N3 Zn1 O2 167.6(2) . 3_565 ?
N5 Zn1 O2 92.7(2) . 3_565 ?
O1 Zn1 Zn1 103.16(14) . 3_565 ?
O2 Zn1 Zn1 42.05(13) . 3_565 ?
N3 Zn1 Zn1 141.1(2) . 3_565 ?
N5 Zn1 Zn1 111.2(2) . 3_565 ?
O2 Zn1 Zn1 39.15(12) 3_565 3_565 ?
O3 Zn2 O4 111.7(2) . . ?
O3 Zn2 O5 113.2(2) . . ?
O4 Zn2 O5 107.5(2) . . ?
O3 Zn2 O6 125.9(2) . . ?
O4 Zn2 O6 101.6(2) . . ?
O5 Zn2 O6 94.6(2) . . ?
O1 P1 O5 112.1(3) . 3_575 ?
O1 P1 O4 109.3(3) . . ?
O5 P1 O4 110.9(3) 3_575 . ?
O1 P1 O7 107.1(3) . . ?
O5 P1 O7 111.6(3) 3_575 . ?
O4 P1 O7 105.7(3) . . ?
O3 P2 O8 110.9(3) 2_444 . ?
O3 P2 O2 108.0(3) 2_444 . ?
O8 P2 O2 109.9(3) . . ?
O3 P2 O6 109.5(3) 2_444 4_675 ?
O8 P2 O6 109.7(3) . 4_675 ?
O2 P2 O6 108.7(3) . 4_675 ?
P1 O1 Zn1 119.7(3) . . ?
P2 O2 Zn1 127.9(3) . . ?
P2 O2 Zn1 131.6(3) . 3_565 ?
Zn1 O2 Zn1 98.8(2) . 3_565 ?
P2 O3 Zn2 121.5(3) 2_454 . ?
P1 O4 Zn2 123.0(3) . . ?
P1 O5 Zn2 132.4(3) 3_575 . ?
P2 O6 Zn2 121.3(3) 4_576 . ?
P1 O7 H10 109.5(2) . . ?
C1 N1 H2 120.0(4) . . ?
C1 N1 H1 120.0(4) . . ?
H2 N1 H1 120.0 . . ?
C1 N2 N5 118.6(6) . . ?
C1 N2 H3 120.7(4) . . ?
N5 N2 H3 120.7(3) . . ?
C1 N3 N4 115.1(6) . . ?
C1 N3 Zn1 117.4(5) . . ?
N4 N3 Zn1 127.3(4) . . ?
N3 N4 H4 120.0(3) . . ?
N3 N4 H5 120.0(3) . . ?
H4 N4 H5 120.0 . . ?
N2 N5 Zn1 112.4(4) . . ?
N2 N5 H6 123.8(3) . . ?
Zn1 N5 H6 123.8(2) . . ?
N3 C1 N1 126.7(7) . . ?
N3 C1 N2 115.5(6) . . ?
N1 C1 N2 117.7(6) . . ?

_refine_diff_density_max    0.769
_refine_diff_density_min   -0.813
_refine_diff_density_rms    0.188