Supplementary Material (ESI) for Journal of Materials Chemistry
This journal is © The Royal Society of Chemistry 2001

data_global
_publ_contact_author               'Wiebcke, Michael'

_publ_contact_author_address 
;
Fachbereich Chemie
Universitat Konstanz
Fach M 730
Konstanz
D-78457
GERMANY
;
_publ_contact_author_email          michael.wiebcke@uni-konstanz.de

loop_
_publ_author_name

'Wiebcke, Michael'


_journal_coden_Cambridge      1145
_journal_name_full                 'Journal of Materials Chemistry'
_journal_volume                    ?
_journal_page_first                ?
_journal_page_last                 ?
_journal_year                      ?
_ccdc_journal_depnumber            ?
_ccdc_compound_id                  ?
_ccdc_biological_activity          ?
_ccdc_polymorph                    ?
_ccdc_chemdiag_type                ?
_ccdc_chemdiag_records
;
?
;
_ccdc_temp_data_collection          ?
_ccdc_ls_R_squared                  ?
_ccdc_disorder                      ?
_ccdc_comments
;
?
;
data_I

_database_code_CSD	166084

_audit_creation_date            2001-03-24T12:36:59-00:00
_audit_creation_method         'WinGX routine CIF_UPDATE'
_chemical_name_systematic
;
Hexane-1,6-diammonium zinc phosphate hydrogenphosphate boric-acid (1/3/2/1/1)
;
_chemical_formula_sum                   'C6 H22 B N2 O15 P3 Zn3'
_chemical_formula_weight                662.08
_symmetry_cell_setting                  monoclinic
_symmetry_space_group_name_H-M          'P 21 / c'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a                          12.955(1)
_cell_length_b                          8.295(1)
_cell_length_c                          18.805(2)
_cell_angle_alpha                       90
_cell_angle_beta                        91.34(1)
_cell_angle_gamma                       90
_cell_volume                            2020.3(4)
_cell_formula_units_Z                   4
_cell_measurement_temperature           293
_exptl_crystal_density_diffrn           2.177
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    1328
_exptl_special_details
;
?
;
_exptl_absorpt_coefficient_mu           3.846
_exptl_absorpt_correction_type          psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
;
_exptl_absorpt_correction_T_min         0.9161
_exptl_absorpt_correction_T_max         0.9987
_exptl_absorpt_correction_T_ave         0.9726
_diffrn_ambient_temperature             293
_diffrn_radiation_wavelength            0.71073
_diffrn_radiation_type                  MoK\a
_diffrn_radiation_monochromator         graphite
_diffrn_reflns_number                   5092
_diffrn_reflns_av_R_equivalents         0.0492
_diffrn_reflns_av_unetI/netI            0.1566
_diffrn_reflns_limit_h_min              0
_diffrn_reflns_limit_h_max              17
_diffrn_reflns_limit_k_min              0
_diffrn_reflns_limit_k_max              10
_diffrn_reflns_limit_l_min              -24
_diffrn_reflns_limit_l_max              24
_diffrn_reflns_theta_min                2.17
_diffrn_reflns_theta_max                28.03
_diffrn_reflns_theta_full               28.03
_diffrn_measured_fraction_theta_full
0.999
_diffrn_measured_fraction_theta_max
0.999
_reflns_number_total                    4885
_reflns_number_gt                       2712
_reflns_threshold_expression            >2sigma(I)
_computing_structure_refinement         'SHELXL-97 (Sheldrick, 1997)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness 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 threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0251P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary            direct
_atom_sites_solution_secondary          difmap
_atom_sites_solution_hydrogens          difmap
_refine_ls_hydrogen_treatment           mixed
_refine_ls_extinction_method            none
_refine_ls_number_reflns                4885
_refine_ls_number_parameters            298
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.1594
_refine_ls_R_factor_gt                  0.0523
_refine_ls_wR_factor_ref                0.097
_refine_ls_wR_factor_gt                 0.0776
_refine_ls_goodness_of_fit_ref          0.989
_refine_ls_restrained_S_all             0.989
_refine_ls_shift/su_max                 0.026
_refine_ls_shift/su_mean                0.001
_refine_diff_density_max                0.793
_refine_diff_density_min                -0.81
_refine_diff_density_rms                0.196
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 0 '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 0.006 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
Zn1 Zn 0.89594(6) 0.85952(10) 0.19334(4) 0.01495(18) Uani 1 1 d . . .
Zn2 Zn 0.13392(6) 0.85849(10) 0.27816(4) 0.01567(18) Uani 1 1 d . . .
Zn3 Zn 0.88265(6) 0.95977(9) 0.41356(4) 0.01372(17) Uani 1 1 d . . .
P1 P 0.94640(12) 0.6451(2) 0.32172(8) 0.0124(3) Uani 1 1 d . . .
P2 P 0.11549(13) 0.0745(2) 0.41751(8) 0.0123(4) Uani 1 1 d . . .
P3 P 0.26216(13) 0.5740(2) 0.21492(8) 0.0150(4) Uani 1 1 d . . .
O1 O 0.9941(3) 0.7588(5) 0.2640(2) 0.0173(10) Uani 1 1 d . . .
O2 O 0.9017(3) 0.7426(5) 0.3822(2) 0.0187(10) Uani 1 1 d . . .
O3 O 0.9680(3) 1.0345(5) 0.1483(2) 0.0183(10) Uani 1 1 d . . .
O4 O 0.0005(3) 0.1073(5) 0.4271(2) 0.0175(11) Uani 1 1 d . . .
O5 O 0.8276(3) 0.9392(5) 0.50949(19) 0.0153(10) Uani 1 1 d . . .
O6 O 0.1335(3) 0.9151(5) 0.3782(2) 0.0181(10) Uani 1 1 d . . .
O7 O 0.8603(3) 0.5467(6) 0.2846(2) 0.0180(10) Uani 1 1 d . . .
O8 O 0.3830(3) 0.5376(6) 0.2098(2) 0.0265(12) Uani 1 1 d . . .
O9 O 0.1653(3) 0.2139(5) 0.3760(2) 0.0161(10) Uani 1 1 d . . .
O10 O 0.2199(4) 0.5829(6) 0.1395(2) 0.0279(12) Uani 1 1 d . . .
O11 O 0.2226(4) 0.4299(6) 0.2558(2) 0.0260(12) Uani 1 1 d . . .
O12 O 0.2511(4) 0.7307(6) 0.2548(2) 0.0258(12) Uani 1 1 d . . .
O13 O 0.3640(4) 0.1520(9) 0.3591(3) 0.0341(14) Uani 1 1 d . . .
O14 O 0.3776(4) 0.0676(8) 0.4821(3) 0.0344(14) Uani 1 1 d . . .
O15 O 0.5238(4) 0.0896(8) 0.4105(3) 0.0369(16) Uani 1 1 d . . .
B B 0.4189(6) 0.1039(10) 0.4176(4) 0.0229(19) Uani 1 1 d . . .
H1 H 0.316(6) 0.052(11) 0.484(4) 0.05 Uiso 1 1 d . . .
H2 H 0.315(6) 0.152(13) 0.364(5) 0.05 Uiso 1 1 d . . .
H3 H 0.549(7) 0.068(11) 0.443(4) 0.05 Uiso 1 1 d . . .
N1 N 0.1098(5) 0.6768(8) 0.4835(3) 0.0249(15) Uani 1 1 d . . .
H11 H 0.077(7) 0.626(11) 0.457(4) 0.05 Uiso 1 1 d . . .
H12 H 0.133(6) 0.757(10) 0.453(4) 0.05 Uiso 1 1 d . . .
H13 H 0.057(6) 0.723(10) 0.508(4) 0.05 Uiso 1 1 d . . .
N2 N 0.6564(5) 0.6547(10) 0.2901(4) 0.0364(18) Uani 1 1 d . . .
H21 H 0.750(6) 0.623(9) 0.284(4) 0.05 Uiso 1 1 d . . .
H22 H 0.633(6) 0.681(10) 0.246(4) 0.05 Uiso 1 1 d . . .
H23 H 0.662(7) 0.753(11) 0.307(4) 0.05 Uiso 1 1 d . . .
C1 C 0.1892(6) 0.5918(10) 0.5267(4) 0.0312(19) Uani 1 1 d . . .
H1A H 0.1557 0.5071 0.5551 0.037 Uiso 1 1 calc R . .
H1B H 0.2225 0.6691 0.5601 0.037 Uiso 1 1 calc R . .
C3 C 0.3444(6) 0.6306(10) 0.4444(4) 0.0350(19) Uani 1 1 d . . .
H3A H 0.3784 0.7008 0.4805 0.042 Uiso 1 1 calc R . .
H3B H 0.304 0.7001 0.4113 0.042 Uiso 1 1 calc R . .
C5 C 0.5023(6) 0.6493(11) 0.3665(4) 0.0361(19) Uani 1 1 d . . .
H5A H 0.4649 0.7156 0.3305 0.043 Uiso 1 1 calc R . .
H5B H 0.5349 0.723 0.4018 0.043 Uiso 1 1 calc R . .
C2 C 0.2719(5) 0.5145(9) 0.4810(4) 0.0307(19) Uani 1 1 d . . .
H2A H 0.3139 0.4413 0.5116 0.037 Uiso 1 1 calc R . .
H2B H 0.237 0.4475 0.4441 0.037 Uiso 1 1 calc R . .
C4 C 0.4267(5) 0.5408(10) 0.4032(4) 0.0303(18) Uani 1 1 d . . .
H4A H 0.4655 0.4695 0.4366 0.036 Uiso 1 1 calc R . .
H4B H 0.392 0.4714 0.3671 0.036 Uiso 1 1 calc R . .
C6 C 0.5842(6) 0.5532(10) 0.3310(4) 0.036(2) Uani 1 1 d . . .
H6A H 0.624 0.4923 0.3677 0.043 Uiso 1 1 calc R . .
H6B H 0.5509 0.4742 0.2984 0.043 Uiso 1 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 0.0169(4) 0.0152(4) 0.0126(3) -0.0003(3) 0.0001(3) -0.0021(4)
Zn2 0.0182(4) 0.0151(4) 0.0138(4) 0.0005(3) 0.0017(3) 0.0008(4)
Zn3 0.0146(4) 0.0152(4) 0.0114(3) -0.0013(3) 0.0007(3) 0.0012(4)
P1 0.0160(8) 0.0114(8) 0.0098(7) -0.0011(7) 0.0018(6) 0.0007(8)
P2 0.0130(8) 0.0150(9) 0.0089(7) -0.0004(7) 0.0004(6) -0.0001(7)
P3 0.0139(9) 0.0171(9) 0.0141(8) -0.0001(7) 0.0006(7) 0.0002(8)
O1 0.015(2) 0.021(2) 0.016(2) 0.004(2) 0.0017(18) -0.002(2)
O2 0.026(3) 0.011(2) 0.020(2) -0.003(2) 0.009(2) 0.002(2)
O3 0.023(3) 0.012(2) 0.019(2) 0.002(2) -0.001(2) -0.006(2)
O4 0.010(2) 0.016(3) 0.026(2) 0.0008(19) 0.0017(19) 0.0013(19)
O5 0.012(2) 0.026(3) 0.0080(19) 0.003(2) 0.0027(17) -0.001(2)
O6 0.023(3) 0.017(2) 0.014(2) -0.0020(19) 0.0042(19) 0.002(2)
O7 0.019(2) 0.018(2) 0.017(2) -0.004(2) -0.0013(19) -0.003(2)
O8 0.016(3) 0.033(3) 0.031(3) 0.009(2) 0.004(2) 0.005(3)
O9 0.012(2) 0.020(3) 0.016(2) 0.007(2) -0.0002(18) 0.002(2)
O10 0.030(3) 0.030(3) 0.024(3) 0.004(2) -0.005(2) -0.009(2)
O11 0.026(3) 0.021(3) 0.031(3) 0.005(2) 0.010(2) 0.002(2)
O12 0.027(3) 0.020(3) 0.031(3) -0.012(2) 0.000(2) 0.004(2)
O13 0.017(3) 0.052(4) 0.034(3) 0.010(3) 0.003(2) 0.007(3)
O14 0.021(3) 0.056(4) 0.027(3) 0.007(3) 0.004(2) 0.004(3)
O15 0.017(3) 0.064(4) 0.030(3) 0.003(3) 0.003(2) 0.007(3)
B 0.017(4) 0.022(5) 0.030(5) -0.006(3) 0.002(4) 0.004(4)
N1 0.030(4) 0.024(4) 0.021(3) -0.002(3) 0.003(3) -0.002(3)
N2 0.029(4) 0.044(5) 0.037(4) -0.006(4) 0.011(3) -0.011(4)
C1 0.030(4) 0.039(5) 0.025(4) 0.005(3) 0.005(3) 0.006(4)
C3 0.031(4) 0.032(5) 0.041(5) 0.000(4) 0.008(4) 0.002(4)
C5 0.032(4) 0.039(5) 0.038(4) 0.004(4) 0.009(4) -0.003(4)
C2 0.025(4) 0.037(5) 0.030(4) -0.003(4) 0.002(3) -0.002(4)
C4 0.026(4) 0.033(5) 0.033(4) -0.001(4) 0.008(3) 0.004(4)
C6 0.031(4) 0.037(5) 0.041(5) 0.002(4) 0.008(4) -0.006(4)
_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 O11 1.919(5) 2_655 ?
Zn1 O3 1.932(4) . ?
Zn1 O9 1.933(4) 2_655 ?
Zn1 O1 2.000(4) . ?
Zn2 O12 1.911(5) . ?
Zn2 O6 1.939(4) . ?
Zn2 O7 1.960(4) 2_655 ?
Zn2 O1 2.003(4) 1_455 ?
Zn3 O2 1.913(4) . ?
Zn3 O10 1.934(5) 2_655 ?
Zn3 O5 1.963(4) . ?
Zn3 O4 1.969(4) 1_665 ?
P1 O2 1.522(4) . ?
P1 O3 1.536(5) 2_745 ?
P1 O7 1.537(4) . ?
P1 O1 1.575(4) . ?
P2 O4 1.529(4) . ?
P2 O6 1.536(4) 1_545 ?
P2 O9 1.545(4) . ?
P2 O5 1.547(4) 3_666 ?
P3 O12 1.509(5) . ?
P3 O10 1.509(5) . ?
P3 O11 1.516(5) . ?
P3 O8 1.600(5) . ?
O1 Zn2 2.003(4) 1_655 ?
O3 P1 1.536(5) 2_755 ?
O4 Zn3 1.969(4) 1_445 ?
O5 P2 1.547(4) 3_666 ?
O6 P2 1.536(4) 1_565 ?
O7 Zn2 1.960(4) 2_645 ?
O9 Zn1 1.933(4) 2_645 ?
O10 Zn3 1.934(5) 2_645 ?
O11 Zn1 1.919(5) 2_645 ?
O13 B 1.356(9) . ?
O14 B 1.370(9) . ?
O15 B 1.373(9) . ?
N1 C1 1.475(9) . ?
N2 C6 1.487(10) . ?
C1 C2 1.530(10) . ?
C3 C2 1.521(10) . ?
C3 C4 1.526(9) . ?
C5 C6 1.496(10) . ?
C5 C4 1.510(10) . ?
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
O11 Zn1 O3 113.0(2) 2_655 . ?
O11 Zn1 O9 101.86(19) 2_655 2_655 ?
O3 Zn1 O9 111.61(18) . 2_655 ?
O11 Zn1 O1 107.42(19) 2_655 . ?
O3 Zn1 O1 107.39(18) . . ?
O9 Zn1 O1 115.55(19) 2_655 . ?
O12 Zn2 O6 112.19(19) . . ?
O12 Zn2 O7 105.13(19) . 2_655 ?
O6 Zn2 O7 113.12(18) . 2_655 ?
O12 Zn2 O1 117.46(19) . 1_455 ?
O6 Zn2 O1 101.89(18) . 1_455 ?
O7 Zn2 O1 107.23(18) 2_655 1_455 ?
O2 Zn3 O10 115.5(2) . 2_655 ?
O2 Zn3 O5 104.69(18) . . ?
O10 Zn3 O5 105.09(19) 2_655 . ?
O2 Zn3 O4 121.32(19) . 1_665 ?
O10 Zn3 O4 105.1(2) 2_655 1_665 ?
O5 Zn3 O4 103.47(18) . 1_665 ?
O2 P1 O3 109.1(2) . 2_745 ?
O2 P1 O7 109.7(3) . . ?
O3 P1 O7 111.1(3) 2_745 . ?
O2 P1 O1 111.0(2) . . ?
O3 P1 O1 108.6(2) 2_745 . ?
O7 P1 O1 107.3(2) . . ?
O4 P2 O6 111.7(3) . 1_545 ?
O4 P2 O9 110.2(2) . . ?
O6 P2 O9 109.3(2) 1_545 . ?
O4 P2 O5 110.8(2) . 3_666 ?
O6 P2 O5 106.8(2) 1_545 3_666 ?
O9 P2 O5 107.9(2) . 3_666 ?
O12 P3 O10 112.8(3) . . ?
O12 P3 O11 113.0(3) . . ?
O10 P3 O11 113.3(3) . . ?
O12 P3 O8 107.3(3) . . ?
O10 P3 O8 106.7(3) . . ?
O11 P3 O8 103.0(3) . . ?
P1 O1 Zn1 117.0(2) . . ?
P1 O1 Zn2 121.6(2) . 1_655 ?
Zn1 O1 Zn2 118.3(2) . 1_655 ?
P1 O2 Zn3 141.7(3) . . ?
P1 O3 Zn1 129.7(3) 2_755 . ?
P2 O4 Zn3 129.0(3) . 1_445 ?
P2 O5 Zn3 130.2(3) 3_666 . ?
P2 O6 Zn2 132.8(3) 1_565 . ?
P1 O7 Zn2 131.2(3) . 2_645 ?
P2 O9 Zn1 129.7(3) . 2_645 ?
P3 O10 Zn3 133.5(3) . 2_645 ?
P3 O11 Zn1 140.9(3) . 2_645 ?
P3 O12 Zn2 132.6(3) . . ?
O13 B O14 125.1(7) . . ?
O13 B O15 116.6(7) . . ?
O14 B O15 118.3(7) . . ?
N1 C1 C2 112.4(6) . . ?
C2 C3 C4 111.5(6) . . ?
C6 C5 C4 111.2(7) . . ?
C3 C2 C1 115.9(7) . . ?
C5 C4 C3 114.2(7) . . ?
N2 C6 C5 113.0(7) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O8 H8 O9 . . . 0.89 1.65 2.538(5) 170 ?
O14 H1 O5 . . 3_665 0.81(8) 1.87(8) 2.666(6) 169(9) ?
O13 H2 O9 . . 1_655 0.64(8) 2.02(8) 2.651(7) 165(13) ?
O15 H3 O14 . . 3_665 0.71(8) 2.02(8) 2.700(8) 160(10) ?
N1 H11 O3 . . 1-655 0.77(9) 2.19(8) 2.904(7) 155(8) ?
N1 H12 O6 . . 1_655 0.93(8) 1.92(8) 2.820(7) 160(7) ?
N1 H13 O4 . . 3_665 0.92(8) 2.02(8) 2.861(7) 152(7) ?
N2 H21 O7 . . . 1.22(8) 1.59(8) 2.793(9) 167(6) ?
N2 H22 O13 . . 2_645 0.92(8) 1.97(8) 2.812(9) 151(7) ?
N2 H23 O8 . . . 0.88(9) 2.45(9) 3.216(10) 146(7) ?
N2 H23 O11 . . . 0.88(9) 2.42(9) 2.911(9) 116(6) ?
C1 H1A O2 . . 3_655 0.99 2.50 3.480(9) 169 ?
C1 H1B O10 . . 3_665 0.99 2.54 3.450(9) 152 ?
C2 H2B O9 . . 1_645 0.99 2.49 3.449(9) 163 ?