#------------------------------------------------------------------------------
#$Date: 2009-11-21 12:50:34 +0200 (Sat, 21 Nov 2009) $
#$Revision: 900 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/1100165.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100165
loop_
_publ_author_name
     'Mohammad Abul-Haj'
     'Miguel Quiros'
     'Juan M. Salas'
_journal_name_full                  'Polyhedron'
_journal_volume         23
_journal_page_first     743
_journal_page_last      747
_journal_year           2004
_chemical_name_systematic
;
 Diaqua bis(4,7-dihydro-1,2,4-triazolo[1,5-a]pyrimidine-7-one-N3)zinc(II) tetrah
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum    'C10 H18 N8 O8 Zn'
_chemical_formula_weight          443.69
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'
_symmetry_cell_setting            orthorhombic
_symmetry_space_group_name_H-M    'P b c a'
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 '-x, y+1/2, -z+1/2'
 'x+1/2, -y+1/2, -z'
 '-x, -y, -z'
 'x-1/2, y, -z-1/2'
 'x, -y-1/2, z-1/2'
 '-x-1/2, y-1/2, z'
_cell_length_a                    7.5430(8)
_cell_length_b                    13.1384(12)
_cell_length_c                    17.2599(10)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      1710.5(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     24
_cell_measurement_theta_min       12.5
_cell_measurement_theta_max       19.5
_exptl_crystal_description        'brick shaped'
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.2
_exptl_crystal_size_mid           0.24
_exptl_crystal_size_min           0.32
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.723
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              912
_exptl_absorpt_coefficient_mu     1.497
##_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_type    psi-scan
_exptl_absorpt_correction_T_min   0.6309
_exptl_absorpt_correction_T_max   0.7119
_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        'STOE STADI4 4-circle-diffractometer'
_diffrn_measurement_method
; Scan width (omega) = 0.26 - 2.16, scan ratio 2theta:omega = 1.00
  I(Net) and sigma(I) from profile fitting (Clegg, 1981)
;
_diffrn_standards_number          3
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   60
_diffrn_standards_decay_%         5.3
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             2487
_diffrn_reflns_av_R_equivalents   0.0000
_diffrn_reflns_av_sigmaI/netI     0.0449
_diffrn_reflns_limit_h_min        0
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        0
_diffrn_reflns_limit_k_max        18
_diffrn_reflns_limit_l_min        0
_diffrn_reflns_limit_l_max        24
_diffrn_reflns_theta_min          2.36
_diffrn_reflns_theta_max          29.97
_reflns_number_total              2487
_reflns_number_gt                 1389
_reflns_threshold_expression      >2sigma(I)
_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^)+(0.1400P)^2^+6.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      heavy
_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          2487
_refine_ls_number_parameters      142
_refine_ls_number_restraints      9
_refine_ls_R_factor_all           0.1402
_refine_ls_R_factor_gt            0.0872
_refine_ls_wR_factor_ref          0.2760
_refine_ls_wR_factor_gt           0.2186
_refine_ls_goodness_of_fit_ref    1.025
_refine_ls_restrained_S_all       1.023
_refine_ls_shift/su_max           0.005
_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
Zn Zn 0.5000 0.5000 0.5000 0.0289(3) Uani 1 2 d S . .
N1 N 0.5663(8) 0.6072(4) 0.7330(3) 0.0380(12) Uani 1 1 d . . .
C2 C 0.5665(10) 0.6056(4) 0.6561(3) 0.0381(13) Uani 1 1 d . . .
H2 H 0.6153 0.6585 0.6273 0.080 Uiso 1 1 d R . .
N3 N 0.4916(6) 0.5241(4) 0.6217(3) 0.0312(11) Uani 1 1 d . . .
C3A C 0.4325(8) 0.4677(4) 0.6814(3) 0.0287(11) Uani 1 1 d . . .
N4 N 0.3473(7) 0.3804(4) 0.6811(3) 0.0349(11) Uani 1 1 d . . .
C5 C 0.3027(9) 0.3442(4) 0.7521(3) 0.0399(13) Uani 1 1 d . . .
H5 H 0.2359 0.2847 0.7537 0.080 Uiso 1 1 d R . .
C6 C 0.3468(9) 0.3887(5) 0.8212(3) 0.0379(14) Uani 1 1 d . . .
H6 H 0.3143 0.3575 0.8675 0.080 Uiso 1 1 d R . .
C7 C 0.4414(9) 0.4793(5) 0.8234(3) 0.0354(13) Uani 1 1 d . . .
O7 O 0.4936(5) 0.5290(4) 0.8816(2) 0.0383(10) Uani 1 1 d . . .
N8 N 0.4802(6) 0.5171(3) 0.7488(3) 0.0283(10) Uani 1 1 d . . .
O1W O 0.5919(7) 0.3492(3) 0.5142(3) 0.0423(11) Uani 1 1 d D . .
H11W H 0.656(10) 0.339(6) 0.474(3) 0.080 Uiso 1 1 d D . .
H12W H 0.578(12) 0.291(3) 0.536(4) 0.080 Uiso 1 1 d D . .
O2W O 0.2328(6) 0.4447(4) 0.5042(2) 0.0396(10) Uani 1 1 d D . .
H21W H 0.181(10) 0.474(6) 0.543(2) 0.080 Uiso 1 1 d D . .
H22W H 0.188(10) 0.468(6) 0.463(2) 0.080 Uiso 1 1 d D . .
O3W O 0.8544(7) 0.2856(3) 0.4198(2) 0.0461(12) Uani 1 1 d D . .
H31W H 0.846(11) 0.239(4) 0.386(3) 0.080 Uiso 1 1 d D . .
H32W H 0.872(12) 0.344(3) 0.399(4) 0.080 Uiso 1 1 d 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
Zn 0.0385(6) 0.0355(5) 0.0128(4) -0.0012(3) 0.0008(3) 0.0023(4)
N1 0.051(3) 0.044(3) 0.019(2) -0.0026(19) -0.002(2) -0.007(2)
C2 0.057(4) 0.036(3) 0.021(3) 0.000(2) 0.002(3) -0.005(3)
N3 0.038(3) 0.038(2) 0.018(2) -0.0016(17) -0.0012(17) -0.001(2)
C3A 0.036(3) 0.037(3) 0.013(2) -0.004(2) 0.003(2) 0.005(2)
N4 0.048(3) 0.038(2) 0.019(2) -0.0043(18) -0.001(2) 0.000(2)
C5 0.053(4) 0.035(3) 0.031(3) 0.001(3) 0.009(3) 0.001(3)
C6 0.047(4) 0.040(3) 0.027(3) -0.002(2) 0.009(2) 0.000(3)
C7 0.042(3) 0.050(3) 0.014(2) -0.003(2) 0.000(2) 0.010(3)
O7 0.050(3) 0.053(2) 0.0123(19) -0.0069(17) 0.0051(15) 0.0007(19)
N8 0.033(2) 0.037(2) 0.016(2) -0.0026(17) -0.0010(16) -0.0016(18)
O1W 0.056(3) 0.036(2) 0.035(2) 0.0035(18) 0.012(2) 0.007(2)
O2W 0.043(2) 0.059(3) 0.0168(18) 0.0018(17) 0.0030(16) 0.000(2)
O3W 0.070(3) 0.041(2) 0.027(2) -0.0061(18) 0.006(2) 0.008(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
Zn O1W 2.113(4) . ?
Zn N3 2.125(5) . ?
Zn O2W 2.143(5) . ?
N1 C2 1.327(7) . ?
N1 N8 1.377(7) . ?
C2 N3 1.348(8) . ?
N3 C3A 1.346(7) . ?
C3A N4 1.315(8) . ?
C3A N8 1.379(7) . ?
N4 C5 1.356(7) . ?
C5 C6 1.370(8) . ?
C6 C7 1.389(9) . ?
C7 O7 1.262(7) . ?
C7 N8 1.411(7) . ?
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
O1W Zn N3 92.00(19) . . ?
O1W Zn O2W 89.25(19) . . ?
N3 Zn O2W 89.37(16) . . ?
C2 N1 N8 100.6(5) . . ?
N1 C2 N3 116.9(5) . . ?
C3A N3 C2 103.8(5) . . ?
C3A N3 Zn 133.3(4) . . ?
C2 N3 Zn 122.8(4) . . ?
N4 C3A N3 129.7(5) . . ?
N4 C3A N8 122.9(5) . . ?
N3 C3A N8 107.4(5) . . ?
C3A N4 C5 115.0(5) . . ?
N4 C5 C6 125.2(6) . . ?
C5 C6 C7 120.9(6) . . ?
O7 C7 C6 128.7(6) . . ?
O7 C7 N8 118.7(6) . . ?
C6 C7 N8 112.6(5) . . ?
N1 N8 C3A 111.2(5) . . ?
N1 N8 C7 125.5(5) . . ?
C3A N8 C7 123.3(5) . . ?
_diffrn_measured_fraction_theta_max    0.997
_diffrn_reflns_theta_full              29.97
_diffrn_measured_fraction_theta_full   0.997
_refine_diff_density_max    1.497
_refine_diff_density_min   -1.329
_refine_diff_density_rms    0.175