#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/53/2005349.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_2005349
loop_
_publ_author_name
'Charfi, M.'
'Jouini, A.'
_publ_section_title
;
 1,6-Hexanediammonium cyclo-Hexaphosphate Hexahydrate
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2250
_journal_page_last               2253
_journal_paper_doi               10.1107/S0108270196003344
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '3C6 H18 N2 2+, P6 O18 6-, 6H2 O1'
_chemical_formula_moiety         '[N H3 (C H2)6 N H3]3 P6 O18, 6H2 O'
_chemical_formula_structural     '[N H3 (C H2)6 N H3]3 P6 O18, 6H2 O'
_chemical_formula_sum            'C18 H66 N6 O24 P6'
_chemical_formula_weight         936.59
_chemical_name_systematic
;
1,6-Diammoniumhexane cyclohexaphosphate hexahydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                112.98(3)
_cell_angle_beta                 87.85(3)
_cell_angle_gamma                104.90(2)
_cell_formula_units_Z            1
_cell_length_a                   11.085(3)
_cell_length_b                   11.678(4)
_cell_length_c                   8.995(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      10
_cell_volume                     1033.4(7)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0066
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3885
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.91
_diffrn_standards_decay_%        0.64
_diffrn_standards_interval_time  120
_diffrn_standards_number         '1 (031)'
_exptl_absorpt_coefficient_mu    0.349
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_meas      1.50
_exptl_crystal_density_method    'pycnometry (toluene as pycnometric liquid)'
_exptl_crystal_description       'transparent ?'
_exptl_crystal_F_000             498
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.351
_refine_ls_extinction_coef       0.020(2)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.955
_refine_ls_goodness_of_fit_obs   0.778
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         3633
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.955
_refine_ls_restrained_S_obs      0.778
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_obs          0.0282
_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^(F~o~^2^) + (0.0317P)^2^ + 1.2088P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.0954
_refine_ls_wR_factor_obs         0.0709
_reflns_number_observed          3088
_reflns_number_total             3633
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            du1153.cif
_cod_data_source_block           dahp
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'none' was changed to '?' - the value
is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1033.4(6)
_cod_database_code               2005349
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_occupancy
_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_type_symbol
P1 1 0.77327(5) 0.51804(5) 0.32682(6) 0.0200(2) Uani d P
P2 1 0.94537(5) 0.72793(5) 0.58775(6) 0.0198(2) Uani d P
P3 1 1.11003(5) 0.69600(5) 0.80720(6) 0.0207(2) Uani d P
OE21 1 0.9848(2) 0.80500(15) 0.4864(2) 0.0286(4) Uani d O
OE31 1 1.1673(2) 0.8253(2) 0.9318(2) 0.0365(4) Uani d O
OE11 1 0.8081(2) 0.5705(2) 0.2019(2) 0.0343(4) Uani d O
OE12 1 0.65042(15) 0.5213(2) 0.3982(2) 0.0310(4) Uani d O
OL12 1 0.88159(15) 0.58147(14) 0.4713(2) 0.0259(4) Uani d O
OE22 1 0.8679(2) 0.7745(2) 0.7235(2) 0.0336(4) Uani d O
OE32 1 1.0066(2) 0.6084(2) 0.8524(2) 0.0318(4) Uani d O
OL23 1 1.06986(14) 0.7092(2) 0.6464(2) 0.0275(4) Uani d O
OL13 1 0.77927(14) 0.37080(14) 0.2615(2) 0.0262(4) Uani d O
OW1 1 1.1497(3) 1.0606(3) 0.9380(3) 0.0673(8) Uani d O
OW2 1 1.1266(3) 0.9602(3) 1.2572(3) 0.0528(6) Uani d O
OW3 1 0.7579(2) 0.6400(2) -0.0444(3) 0.0454(5) Uani d O
N1 1 1.1498(2) 1.0582(2) 0.6350(3) 0.0316(5) Uani d N
N2 1 1.0765(2) 0.6564(2) 0.1892(3) 0.0265(4) Uani d N
N3 1 0.5907(2) 0.6337(2) 0.7192(3) 0.0289(4) Uani d N
C1 1 1.2811(2) 1.0553(3) 0.6018(3) 0.0340(6) Uani d C
C2 1 0.6307(2) 0.8117(2) 0.3332(3) 0.0318(5) Uani d C
C3 1 0.4944(2) 0.8117(2) 0.3578(3) 0.0321(5) Uani d C
C4 1 0.5904(2) 0.3232(2) 0.6849(3) 0.0332(6) Uani d C
C5 1 1.2706(2) 0.6682(3) 0.3294(3) 0.0298(5) Uani d C
C6 1 1.2148(2) 0.6845(3) 0.1897(3) 0.0285(5) Uani d C
C7 1 0.5736(3) 0.7609(3) 0.7409(3) 0.0333(6) Uani d C
C8 1 0.5312(3) 0.8302(3) 0.9036(3) 0.0354(6) Uani d C
C9 1 1.4834(3) 1.0403(3) 1.0825(3) 0.0398(6) Uani d C
H1N1 1 1.1276(27) 1.1147(30) 0.6049(36) 0.039(8) Uiso d H
H2N1 1 1.1402(29) 1.0770(31) 0.7441(44) 0.050(9) Uiso d H
H3N1 1 1.0949(34) 0.9808(37) 0.5799(43) 0.061(10) Uiso d H
H1N2 1 1.0468(26) 0.5810(30) 0.1878(32) 0.029(7) Uiso d H
H2N2 1 1.0484(29) 0.6522(29) 0.0973(41) 0.044(8) Uiso d H
H3N2 1 1.0522(32) 0.7089(34) 0.2790(46) 0.056(10) Uiso d H
H1N3 1 0.6425(26) 0.6405(25) 0.7969(34) 0.028(7) Uiso d H
H2N3 1 0.5169(29) 0.5843(28) 0.7206(34) 0.034(7) Uiso d H
H3N3 1 0.6245(28) 0.5969(29) 0.6249(40) 0.042(8) Uiso d H
H1C1 1 1.2869(27) 1.0131(28) 0.4892(39) 0.041(8) Uiso d H
H2C1 1 1.3050(29) 0.9970(30) 0.6479(38) 0.049(9) Uiso d H
H1C2 1 0.6545(24) 0.7615(25) 0.3874(31) 0.027(6) Uiso d H
H2C2 1 0.6411(30) 0.7696(31) 0.2284(42) 0.052(9) Uiso d H
H1C3 1 0.4719(25) 0.8535(26) 0.2955(33) 0.033(7) Uiso d H
H2C3 1 0.4842(25) 0.8663(27) 0.4695(36) 0.034(7) Uiso d H
H1C4 1 0.5743(29) 0.3787(30) 0.8004(40) 0.049(9) Uiso d H
H2C4 1 0.5679(26) 0.3593(27) 0.6152(35) 0.038(7) Uiso d H
H1C5 1 1.2265(27) 0.5844(29) 0.3307(35) 0.040(8) Uiso d H
H2C5 1 1.2541(28) 0.7310(30) 0.4330(39) 0.046(8) Uiso d H
H1C6 1 1.2429(24) 0.7675(27) 0.1981(31) 0.026(6) Uiso d H
H2C6 1 1.2354(29) 0.6239(30) 0.0865(39) 0.047(8) Uiso d H
H1C7 1 0.5163(26) 0.7441(26) 0.6530(34) 0.033(7) Uiso d H
H2C7 1 0.6482(28) 0.8062(27) 0.7170(34) 0.037(8) Uiso d H
H1C8 1 0.4543(30) 0.7784(30) 0.9257(37) 0.047(8) Uiso d H
H2C8 1 0.5904(29) 0.8421(28) 0.9860(38) 0.045(8) Uiso d H
H1C9 1 1.5514(31) 1.0574(30) 1.1711(39) 0.051(9) Uiso d H
H2C9 1 1.4139(32) 0.9899(32) 1.1132(40) 0.053(9) Uiso d H
H1W1 1 1.1496(38) 0.9958(43) 0.9404(48) 0.069(13) Uiso d H
H2W1 1 1.1317(46) 1.0975(49) 1.0127(61) 0.088(18) Uiso d H
H1W2 1 1.1281(32) 1.0285(37) 1.2596(42) 0.052(10) Uiso d H
H2W2 1 1.1320(36) 0.9241(39) 1.1606(54) 0.070(12) Uiso d H
H1W3 1 0.7608(33) 0.6186(35) 0.0215(45) 0.053(11) Uiso d H
H2W3 1 0.8261(40) 0.6503(37) -0.0791(49) 0.069(13) Uiso d H
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'
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
OE11 P1 OE12 . . 119.65(10) y
OE11 P1 OL13 . . 110.62(10) y
OE12 P1 OL13 . . 106.18(9) y
OE11 P1 OL12 . . 110.35(10) y
OE12 P1 OL12 . . 108.71(10) y
OL13 P1 OL12 . . 99.36(9) y
OE22 P2 OE21 . . 118.37(10) y
OE22 P2 OL23 . . 111.61(10) y
OE21 P2 OL23 . . 106.36(9) y
OE22 P2 OL12 . . 110.96(10) y
OE21 P2 OL12 . . 108.81(9) y
OL23 P2 OL12 . . 98.89(9) y
OE31 P3 OE32 . . 118.15(11) y
OE31 P3 OL13 . 2_766 107.21(10) y
OE32 P3 OL13 . 2_766 110.82(9) y
OE31 P3 OL23 . . 109.51(10) y
OE32 P3 OL23 . . 110.97(10) y
OL13 P3 OL23 2_766 . 98.31(9) y
P2 OL12 P1 . . 132.11(10) y
P2 OL23 P3 . . 132.71(11) y
P3 OL13 P1 2_766 . 132.11(10) y
P2 P1 P3 . 2_766 107.68(4) y
P1 P2 P3 . . 125.55(4) y
P2 P3 P1 . 2_766 117.65(4) y
H1W1 OW1 H2W1 . . 107.(5) n
H1W2 OW2 H2W2 . . 98.(4) n
H1W3 OW3 H2W3 . . 108.(4) n
C1 N1 H1N1 . . 111.7(19) n
C1 N1 H2N1 . . 109.(2) n
H1N1 N1 H2N1 . . 111.(3) n
C1 N1 H3N1 . . 112.(2) n
H1N1 N1 H3N1 . . 106.(3) n
H2N1 N1 H3N1 . . 107.(3) n
C6 N2 H1N2 . . 109.2(18) n
C6 N2 H2N2 . . 108.(2) n
H1N2 N2 H2N2 . . 105.(3) n
C6 N2 H3N2 . . 112.(2) n
H1N2 N2 H3N2 . . 105.(3) n
H2N2 N2 H3N2 . . 117.(3) n
C7 N3 H1N3 . . 111.5(17) n
C7 N3 H2N3 . . 107.3(18) n
H1N3 N3 H2N3 . . 110.(3) n
C7 N3 H3N3 . . 112.2(19) n
H1N3 N3 H3N3 . . 106.(3) n
H2N3 N3 H3N3 . . 110.(3) n
N1 C1 C2 . 2_776 111.9(2) y
N1 C1 H1C1 . . 109.6(18) n
C2 C1 H1C1 2_776 . 110.8(18) n
N1 C1 H2C1 . . 109.0(18) n
C2 C1 H2C1 2_776 . 111.7(18) n
H1C1 C1 H2C1 . . 103.(3) n
C1 C2 C3 2_776 . 113.3(2) y
C1 C2 H1C2 2_776 . 108.3(15) n
C3 C2 H1C2 . . 109.3(15) n
C1 C2 H2C2 2_776 . 111.(2) n
C3 C2 H2C2 . . 111.(2) n
H1C2 C2 H2C2 . . 104.(3) n
C4 C3 C2 2_666 . 112.3(2) y
C4 C3 H1C3 2_666 . 112.4(17) n
C2 C3 H1C3 . . 107.3(17) n
C4 C3 H2C3 2_666 . 109.6(16) n
C2 C3 H2C3 . . 110.8(16) n
H1C3 C3 H2C3 . . 104.(2) n
C3 C4 C5 2_666 2_766 115.4(2) y
C3 C4 H1C4 2_666 . 107.4(18) n
C5 C4 H1C4 2_766 . 110.4(18) n
C3 C4 H2C4 2_666 . 109.6(17) n
C5 C4 H2C4 2_766 . 106.5(17) n
H1C4 C4 H2C4 . . 107.(2) n
C6 C5 C4 . 2_766 111.4(2) y
C6 C5 H1C5 . . 109.2(17) n
C4 C5 H1C5 2_766 . 109.6(17) n
C6 C5 H2C5 . . 110.3(18) n
C4 C5 H2C5 2_766 . 112.0(18) n
H1C5 C5 H2C5 . . 104.(2) n
N2 C6 C5 . . 111.5(2) y
N2 C6 H1C6 . . 106.3(16) n
C5 C6 H1C6 . . 110.7(16) n
N2 C6 H2C6 . . 107.6(18) n
C5 C6 H2C6 . . 109.6(18) n
H1C6 C6 H2C6 . . 111.(2) n
N3 C7 C8 . . 113.1(2) y
N3 C7 H1C7 . . 105.6(16) n
C8 C7 H1C7 . . 113.4(16) n
N3 C7 H2C7 . . 106.4(17) n
C8 C7 H2C7 . . 114.2(18) n
H1C7 C7 H2C7 . . 103.(2) n
C7 C8 C9 . 2_777 110.2(2) y
C7 C8 H1C8 . . 111.7(18) n
C9 C8 H1C8 2_777 . 111.3(18) n
C7 C8 H2C8 . . 109.6(18) n
C9 C8 H2C8 2_777 . 110.2(18) n
H1C8 C8 H2C8 . . 104.(3) n
C9 C9 C8 2_877 2_777 113.7(3) y
C9 C9 H1C9 2_877 . 110.6(17) n
C8 C9 H1C9 2_777 . 107.9(18) n
C9 C9 H2C9 2_877 . 109.(2) n
C8 C9 H2C9 2_777 . 115.(2) n
H1C9 C9 H2C9 . . 100.(3) n
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 OE11 . 1.473(2) y
P1 OE12 . 1.487(2) y
P1 OL13 . 1.604(2) y
P1 OL12 . 1.609(2) y
P2 OE22 . 1.472(2) y
P2 OE21 . 1.497(2) y
P2 OL23 . 1.591(2) y
P2 OL12 . 1.599(2) y
P3 OE31 . 1.476(2) y
P3 OE32 . 1.488(2) y
P3 OL13 2_766 1.599(2) y
P3 OL23 . 1.604(2) y
OL13 P3 2_766 1.599(2) n
OW1 H1W1 . 0.76(4) n
OW1 H2W1 . 0.70(5) n
OW2 H1W2 . 0.79(4) n
OW2 H2W2 . 0.81(4) n
OW3 H1W3 . 0.73(4) n
OW3 H2W3 . 0.81(4) n
N1 C1 . 1.481(3) y
N1 H1N1 . 0.89(3) n
N1 H2N1 . 0.93(4) n
N1 H3N1 . 0.91(4) n
N2 C6 . 1.483(3) y
N2 H1N2 . 0.85(3) n
N2 H2N2 . 0.87(3) n
N2 H3N2 . 0.88(4) n
N3 C7 . 1.482(3) y
N3 H1N3 . 0.89(3) n
N3 H2N3 . 0.88(3) n
N3 H3N3 . 0.90(3) n
C1 C2 2_776 1.505(4) y
C1 H1C1 . 0.95(3) n
C1 H2C1 . 1.01(3) n
C2 C1 2_776 1.505(4) n
C2 C3 . 1.519(3) y
C2 H1C2 . 0.98(3) n
C2 H2C2 . 0.90(3) n
C3 C4 2_666 1.518(4) y
C3 H1C3 . 0.95(3) n
C3 H2C3 . 0.98(3) n
C4 C3 2_666 1.518(4) n
C4 C5 2_766 1.522(3) y
C4 H1C4 . 1.02(3) n
C4 H2C4 . 0.95(3) n
C5 C6 . 1.517(3) y
C5 C4 2_766 1.522(3) n
C5 H1C5 . 0.98(3) n
C5 H2C5 . 0.98(3) n
C6 H1C6 . 0.91(3) n
C6 H2C6 . 0.98(3) n
C7 C8 . 1.496(4) y
C7 H1C7 . 0.96(3) n
C7 H2C7 . 0.93(3) n
C8 C9 2_777 1.518(4) y
C8 H1C8 . 0.97(3) n
C8 H2C8 . 0.95(3) n
C9 C9 2_877 1.506(5) y
C9 C8 2_777 1.518(4) n
C9 H1C9 . 1.04(3) n
C9 H2C9 . 0.95(3) n
P1 P2 . 2.932(2) y
P2 P3 . 2.9260(10) y
P1 P3 2_766 2.9270(10) y
