#------------------------------------------------------------------------------
#$Date: 2008-01-26 19:25:03 +0200 (Sat, 26 Jan 2008) $
#$Revision: 20 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/1004031.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_sfh1

_audit_creation_method            SHELXL
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_formula_moiety          'H2 O8 P2 Zn, C5 H14 N2, H2 O'
_chemical_formula_structural      ?
_chemical_formula_analytical      ?
_chemical_formula_sum             'C5 H18 N2 O9 P2 Zn'
_chemical_formula_weight          377.52
_chemical_melting_point           ?
_chemical_compound_source         ?

_publ_section_title
;
Synthesis and characterization of the one-dimensional zincophosphate
Mu-22 : [Zn(HPO4)2]8[C5H13N2]8•8H2O
;
_publ_author_name
  'S. Fleith, L. Josien,  A. Simon-Masseron, V. Gramlich, J. Patarin'
_journal_name_full                 'Solid State Sci. 2002, 4, 135'

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    C2/c

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'
 '-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                    13.917(13)
_cell_length_b                    9.091(14)
_cell_length_c                    20.489(19)
_cell_angle_alpha                 90.00
_cell_angle_beta                  102.36(8)
_cell_angle_gamma                 90.00
_cell_volume                      2532.2(51)
_cell_formula_units_Z             8
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     12
_cell_measurement_theta_min       10
_cell_measurement_theta_max       11

_exptl_crystal_description        'prism'
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.1
_exptl_crystal_size_mid           0.1
_exptl_crystal_size_min           0.1
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.981
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              1552
_exptl_absorpt_coefficient_mu     2.237
_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        'SYNTEX P21 4-circle diffractometer'
_diffrn_measurement_method        ' \w scans'
_diffrn_standards_number          1
_diffrn_standards_interval_count  120
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         0
_diffrn_reflns_number             2428
_diffrn_reflns_av_R_equivalents   0.0269
_diffrn_reflns_av_sigmaI/netI     0.0264
_diffrn_reflns_limit_h_min        0
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        0
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -24
_diffrn_reflns_limit_l_max        23
_diffrn_reflns_theta_min          2.70
_diffrn_reflns_theta_max          25.18
_reflns_number_total              2251
_reflns_number_observed           1904
_reflns_observed_criterion        >2sigma(I)

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

_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^)+(0.0653P)^2^+0.5728P] 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        0.0057(4)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          2251
_refine_ls_number_parameters      189
_refine_ls_number_restraints      4
_refine_ls_R_factor_all           0.0304
_refine_ls_R_factor_obs           0.0268
_refine_ls_wR_factor_all          0.0751
_refine_ls_wR_factor_obs          0.0740
_refine_ls_goodness_of_fit_all    0.853
_refine_ls_goodness_of_fit_obs    0.921
_refine_ls_restrained_S_all       0.854
_refine_ls_restrained_S_obs       0.922
_refine_ls_shift/esd_max          0.035
_refine_ls_shift/esd_mean         0.002

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 0.36834(2) 0.12700(3) 0.473350(13) 0.01569(14) Uani 1 d . .
P2 P 0.44521(4) -0.11796(6) 0.58699(3) 0.0149(2) Uani 1 d . .
P1 P 0.36036(4) 0.36324(6) 0.59184(3) 0.0149(2) Uani 1 d . .
O1 O 0.43283(12) 0.4854(2) 0.61688(9) 0.0247(4) Uani 1 d . .
O5 O 0.44239(14) -0.0069(2) 0.64022(9) 0.0270(4) Uani 1 d . .
O2 O 0.38603(14) 0.2909(2) 0.53184(9) 0.0277(4) Uani 1 d . .
N1 N 0.37951(15) 0.5448(2) 0.32925(11) 0.0212(5) Uani 1 d . .
H1A H 0.44465(15) 0.5478(2) 0.34643(11) 0.030 Uiso 1 d R .
N4 N 0.3200(2) 0.7448(2) 0.42117(10) 0.0208(5) Uani 1 d . .
H4A H 0.2541(2) 0.7472(2) 0.40744(10) 0.029 Uiso 1 d R .
H4B H 0.3368(2) 0.8049(2) 0.45667(10) 0.029 Uiso 1 d R .
O8 O 0.38191(13) -0.2533(2) 0.60007(11) 0.0311(5) Uani 1 d D .
H8 H 0.4070(28) -0.3390(30) 0.6037(20) 0.060(12) Uiso 1 d D .
O4 O 0.3708(2) 0.2480(2) 0.64892(10) 0.0383(5) Uani 1 d D .
H4 H 0.3962(34) 0.1642(34) 0.6449(25) 0.088(16) Uiso 1 d D .
O7 O 0.39505(14) -0.0618(2) 0.51815(9) 0.0260(4) Uani 1 d . .
C2 C 0.3302(2) 0.4923(3) 0.38201(14) 0.0271(6) Uani 1 d . .
H2A H 0.3526(2) 0.3948(3) 0.39542(14) 0.038 Uiso 1 d R .
H2B H 0.2606(2) 0.4880(3) 0.36445(14) 0.038 Uiso 1 d R .
C5 C 0.3656(2) 0.7987(3) 0.36710(13) 0.0236(6) Uani 1 d . .
H5A H 0.4353(2) 0.8079(3) 0.38353(13) 0.033 Uiso 1 d R .
H5B H 0.3399(2) 0.8943(3) 0.35313(13) 0.033 Uiso 1 d R .
C6 C 0.3465(2) 0.6960(3) 0.30853(13) 0.0245(6) Uani 1 d . .
H6A H 0.2773(2) 0.6948(3) 0.28898(13) 0.034 Uiso 1 d R .
H6B H 0.3806(2) 0.7301(3) 0.27533(13) 0.034 Uiso 1 d R .
O3 O 0.25820(13) 0.4251(2) 0.57905(10) 0.0303(5) Uani 1 d . .
C3 C 0.3516(2) 0.5934(3) 0.44143(14) 0.0262(6) Uani 1 d . .
H3A H 0.3168(2) 0.5595(3) 0.47425(14) 0.037 Uiso 1 d R .
H3B H 0.4207(2) 0.5920(3) 0.46114(14) 0.037 Uiso 1 d R .
C7 C 0.3621(2) 0.4437(3) 0.2714(2) 0.0394(8) Uani 1 d . .
H7A H 0.3841(2) 0.3465(3) 0.2858(2) 0.055 Uiso 1 d R .
H7B H 0.2931(2) 0.4415(3) 0.2517(2) 0.055 Uiso 1 d R .
H7C H 0.3977(2) 0.4779(3) 0.2390(2) 0.055 Uiso 1 d R .
O1W O 0.3743(2) 0.9402(3) 0.75675(12) 0.0435(6) Uani 1 d D .
H1W H 0.4019(29) 0.9463(49) 0.7230(16) 0.070(14) Uiso 1 d D .
H2W H 0.4188(36) 0.9199(74) 0.7857(26) 0.148(28) Uiso 1 d D .
O6 O 0.54736(13) -0.1714(2) 0.58780(9) 0.0243(4) 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 0.0134(2) 0.0143(2) 0.0187(2) -0.00063(11) 0.00176(12) 0.00030(10)
P2 0.0136(3) 0.0126(3) 0.0180(3) 0.0012(2) 0.0023(2) 0.0007(2)
P1 0.0139(3) 0.0113(3) 0.0180(3) -0.0011(2) -0.0002(2) -0.0002(2)
O1 0.0139(9) 0.0159(9) 0.0404(11) -0.0054(8) -0.0030(8) -0.0004(7)
O5 0.0419(12) 0.0195(9) 0.0205(9) 0.0002(8) 0.0089(8) 0.0054(8)
O2 0.0411(11) 0.0180(10) 0.0257(10) -0.0050(8) 0.0109(8) -0.0004(8)
N1 0.0155(10) 0.0211(11) 0.0247(11) -0.0043(9) -0.0007(9) 0.0028(9)
N4 0.0175(11) 0.0219(11) 0.0221(11) -0.0041(9) 0.0024(9) -0.0012(9)
O8 0.0162(10) 0.0142(9) 0.0628(14) 0.0097(9) 0.0085(9) 0.0012(8)
O4 0.070(2) 0.0197(10) 0.0297(11) 0.0061(9) 0.0196(10) 0.0134(10)
O7 0.0339(11) 0.0155(9) 0.0224(9) 0.0013(8) -0.0078(8) -0.0007(8)
C2 0.0252(14) 0.0177(13) 0.038(2) 0.0036(12) 0.0050(12) -0.0006(11)
C5 0.0258(14) 0.0180(13) 0.0278(14) 0.0036(11) 0.0078(11) -0.0031(11)
C6 0.0295(15) 0.0215(14) 0.0209(13) 0.0033(11) 0.0020(11) 0.0021(12)
O3 0.0147(9) 0.0294(10) 0.0425(12) -0.0086(9) -0.0036(8) 0.0017(8)
C3 0.0288(15) 0.0247(14) 0.0266(14) 0.0080(12) 0.0090(12) 0.0056(12)
C7 0.039(2) 0.037(2) 0.038(2) -0.0204(14) -0.0012(14) 0.0019(15)
O1W 0.0313(12) 0.069(2) 0.0291(12) 0.0005(12) 0.0037(10) 0.0012(12)
O6 0.0175(9) 0.0281(9) 0.0295(10) 0.0090(8) 0.0102(8) 0.0056(8)

_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 1.895(3) . ?
Zn1 O3 1.915(3) 7_556 ?
Zn1 O6 1.933(2) 5_656 ?
Zn1 O7 1.944(3) . ?
P2 O5 1.493(2) . ?
P2 O6 1.499(2) . ?
P2 O7 1.522(2) . ?
P2 O8 1.570(2) . ?
P1 O3 1.499(2) . ?
P1 O2 1.503(2) . ?
P1 O1 1.514(2) . ?
P1 O4 1.553(2) . ?
N1 C7 1.478(4) . ?
N1 C2 1.478(4) . ?
N1 C6 1.483(4) . ?
N4 C5 1.473(3) . ?
N4 C3 1.477(4) . ?
C2 C3 1.504(4) . ?
C5 C6 1.498(4) . ?
O3 Zn1 1.915(3) 7_556 ?
O6 Zn1 1.933(2) 5_656 ?

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 121.88(9) . 7_556 ?
O2 Zn1 O6 103.35(10) . 5_656 ?
O3 Zn1 O6 107.51(11) 7_556 5_656 ?
O2 Zn1 O7 114.19(12) . . ?
O3 Zn1 O7 96.11(10) 7_556 . ?
O6 Zn1 O7 114.15(9) 5_656 . ?
O5 P2 O6 112.60(13) . . ?
O5 P2 O7 111.82(13) . . ?
O6 P2 O7 111.40(13) . . ?
O5 P2 O8 107.58(14) . . ?
O6 P2 O8 108.03(13) . . ?
O7 P2 O8 104.99(12) . . ?
O3 P1 O2 113.81(14) . . ?
O3 P1 O1 108.80(14) . . ?
O2 P1 O1 109.90(13) . . ?
O3 P1 O4 108.48(14) . . ?
O2 P1 O4 108.69(14) . . ?
O1 P1 O4 106.93(15) . . ?
P1 O2 Zn1 147.13(13) . . ?
C7 N1 C2 111.3(2) . . ?
C7 N1 C6 111.1(2) . . ?
C2 N1 C6 110.2(2) . . ?
C5 N4 C3 111.8(2) . . ?
P2 O7 Zn1 137.50(11) . . ?
N1 C2 C3 110.6(2) . . ?
N4 C5 C6 111.3(2) . . ?
N1 C6 C5 110.9(2) . . ?
P1 O3 Zn1 136.82(14) . 7_556 ?
N4 C3 C2 110.3(2) . . ?
P2 O6 Zn1 129.10(12) . 5_656 ?

_refine_diff_density_max    0.736
_refine_diff_density_min   -0.344
_refine_diff_density_rms    0.080