#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2007037.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2007037
loop_
_publ_author_name
'Stock, N.'
'Schnick, W.'
_publ_contact_author
;
    Prof. Wolfgang Schnick
    Laboratorium f\"ur Anorganische Chemie
    Universit\"atsstr. 30
    D-95440 Bayreuth
    Germany
;
_publ_section_title
;
 Tetraammonium Tetrametaphosphimate Tetrahydrate
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              171
_journal_page_last               174
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '(N H4)4  (P O2 N H)4 , 4H2 O'
_chemical_formula_moiety         '(N H4)4 +, (P O2 N H)4 4-, 4H2 O'
_chemical_formula_structural     '(N H4)4 (P O2 N H)4 4H2 O'
_chemical_formula_sum            'H28 N8 O12 P4'
_chemical_formula_weight         456.18
_chemical_name_common
'Tetraammonium tetrametaphosphimate tetrahydrate'
_chemical_name_systematic
;
 Tetraammonium-tetra-\m-imido-cyclotetraphosphate tetrahydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.920(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.5295(8)
_cell_length_b                   11.0584(7)
_cell_length_c                   12.2954(7)
_cell_measurement_reflns_used    44
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      15.14
_cell_measurement_theta_min      6.53
_cell_volume                     886.65(13)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        'SHELXTL (Sheldrick, 1994)'
_computing_molecular_graphics    'SHELXTL, KPLOT (Hundt, 1979)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0102
_diffrn_reflns_av_sigmaI/netI    0.0107
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4404
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.48
_diffrn_standards_decay_%        2.07
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_T_max  0.9228
_exptl_absorpt_correction_T_min  0.8315
_exptl_absorpt_correction_type
;
numerical, using HABITUS (Herrendorf & Baernighausen, 1993)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             480
_exptl_crystal_size_max          1.19
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.348
_refine_ls_extinction_coef       0.0059(16)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.124
_refine_ls_goodness_of_fit_obs   1.143
_refine_ls_hydrogen_treatment
;
H atoms were refined using the riding model, starting from fourier
coordinates
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_restrained_S_obs      1.143
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_obs          0.0262
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.0407P)^2^+0.6573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all         0.0778
_refine_ls_wR_factor_obs         0.0765
_reflns_number_observed          1916
_reflns_number_total             2042
_reflns_observed_criterion       I>2sigma(I)
_[local]_cod_data_source_file    sk1143.cif
_[local]_cod_data_source_block   n12c1
_[local]_cod_cif_authors_sg_H-M  'P 21/n'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2007037
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'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
P1 0.0129(2) 0.0095(2) 0.0114(2) 0.00208(12) 0.00018(13) -0.00016(12)
P2 0.0115(2) 0.0106(2) 0.0102(2) 0.00053(12) 0.00136(13) -0.00039(12)
O1 0.0135(5) 0.0183(5) 0.0154(5) 0.0032(4) -0.0003(4) 0.0004(4)
O2 0.0268(6) 0.0099(5) 0.0176(5) 0.0020(4) -0.0035(4) -0.0008(4)
O3 0.0173(5) 0.0210(6) 0.0111(5) 0.0013(4) 0.0032(4) -0.0010(4)
O4 0.0167(5) 0.0135(5) 0.0198(5) -0.0028(4) 0.0003(4) 0.0009(4)
N1 0.0123(5) 0.0128(6) 0.0124(6) -0.0003(4) 0.0000(4) 0.0015(4)
N2 0.0164(6) 0.0106(6) 0.0130(6) 0.0024(5) 0.0044(5) 0.0029(4)
N3 0.0249(7) 0.0222(7) 0.0168(6) -0.0033(6) 0.0046(5) -0.0037(5)
N4 0.0174(7) 0.0234(7) 0.0274(7) 0.0023(5) 0.0021(5) -0.0095(6)
OW1 0.0178(6) 0.0454(9) 0.0448(8) -0.0008(6) 0.0026(6) 0.0289(7)
OW2 0.0221(6) 0.0133(5) 0.0200(6) 0.0004(4) -0.0030(4) -0.0006(4)
loop_
_atom_site_label
_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_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
P1 0.25491(6) 0.14488(3) 0.45685(3) 0.01129(12) Uani d . 1 P
P2 0.48244(5) 0.03938(3) 0.65373(3) 0.01076(12) Uani d . 1 P
O1 0.0358(2) 0.13149(10) 0.41286(9) 0.0158(2) Uani d . 1 O
O2 0.3185(2) 0.27089(10) 0.48884(9) 0.0183(2) Uani d . 1 O
O3 0.3952(2) 0.03391(10) 0.76520(9) 0.0164(2) Uani d . 1 O
O4 0.6295(2) 0.13826(10) 0.63067(9) 0.0167(2) Uani d . 1 O
N1 0.2827(2) 0.05210(11) 0.56258(10) 0.0125(2) Uani d . 1 N
H1 0.1862(2) -0.00588(11) 0.56225(10) 0.018(5) Uiso d R 1 H
N2 0.4155(2) 0.09709(11) 0.36421(10) 0.0132(3) Uani d . 1 N
H2 0.4490(2) 0.15352(11) 0.32039(10) 0.033(6) Uiso d R 1 H
N3 0.4498(2) 0.39339(13) 0.68772(11) 0.0212(3) Uani d . 1 N
H31 0.5408(2) 0.43661(13) 0.65996(11) 0.029(6) Uiso d R 1 H
H32 0.3360(2) 0.43341(13) 0.69826(11) 0.034(6) Uiso d R 1 H
H33 0.4189(2) 0.33881(13) 0.63936(11) 0.043(7) Uiso d R 1 H
H34 0.4879(2) 0.37541(13) 0.75996(11) 0.039(7) Uiso d R 1 H
N4 -0.2518(2) 0.30918(14) 0.44758(12) 0.0227(3) Uani d . 1 N
H41 -0.1322(2) 0.25467(14) 0.43885(12) 0.042(7) Uiso d R 1 H
H42 -0.2166(2) 0.37717(14) 0.49835(12) 0.040(7) Uiso d R 1 H
H43 -0.3944(2) 0.28727(14) 0.46055(12) 0.108(14) Uiso d R 1 H
H44 -0.2641(2) 0.33857(14) 0.36215(12) 0.134(18) Uiso d R 1 H
OW1 0.4994(2) 0.30712(14) 0.22858(12) 0.0360(4) Uani d . 1 O
H11 0.3811(2) 0.32636(14) 0.19964(12) 0.059(9) Uiso d R 1 H
H12 0.5888(2) 0.34066(14) 0.20104(12) 0.061(9) Uiso d R 1 H
OW2 0.7186(2) 0.00975(10) -0.08651(9) 0.0186(2) Uani d . 1 O
H21 0.6149(2) 0.01720(10) -0.11920(9) 0.036(7) Uiso d R 1 H
H22 0.7413(2) 0.08070(10) -0.05810(9) 0.046(7) Uiso d R 1 H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 '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'
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'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
1 7 -4
1 2 8
3 4 -4
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 P1 O1 . . 115.41(6) yes
O2 P1 N1 . . 110.56(6) yes
O1 P1 N1 . . 106.48(6) yes
O2 P1 N2 . . 107.29(7) yes
O1 P1 N2 . . 109.90(6) yes
N1 P1 N2 . . 106.91(6) yes
O4 P2 O3 . . 118.52(7) yes
O4 P2 N2 . 3_656 111.87(6) yes
O3 P2 N2 . 3_656 104.77(6) yes
O4 P2 N1 . . 107.28(6) yes
O3 P2 N1 . . 106.98(6) yes
N2 P2 N1 3_656 . 106.79(6) yes
P1 N1 P2 . . 128.61(8) yes
P2 N2 P1 3_656 . 130.10(8) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
P1 O2 . 1.5006(11) yes
P1 O1 . 1.5105(11) yes
P1 N1 . 1.6588(13) yes
P1 N2 . 1.6729(13) yes
P2 O4 . 1.4920(11) yes
P2 O3 . 1.5121(11) yes
P2 N2 3_656 1.6689(13) yes
P2 N1 . 1.6818(13) yes
N2 P2 3_656 1.6689(13) ?