# Supplementary Material (ESI) for Journal of Materials Chemistry
# This journal is (C) The Royal Society of Chemistry 2009


data_global
_journal_name_full               J.Mater.Chem.
_journal_coden_cambridge         1145
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
loop_
_publ_author_name
A.Cheetham
J.Eckert
E.Falcao
Z.Hulvey
_publ_contact_author_name        'A Cheetham'
_publ_contact_author_email       AKC30@CAM.AC.UK

_publ_section_title              
;
Enhanced H2 adsorption enthalpy in the low-surface area,
partially fluorinated coordination polymer
Zn5(triazole)6(tetrafluoroterephthalate)2(H2O)2 . 4H2O
;

data_zn_tpam
_database_code_depnum_ccdc_archive 'CCDC 716720'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H24 F8 N18 O14 Zn5'
_chemical_formula_weight         1315.60

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'
F F 0.0171 0.0103 '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           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.137(5)
_cell_length_b                   10.228(5)
_cell_length_c                   12.747(7)
_cell_angle_alpha                74.562(8)
_cell_angle_beta                 83.796(9)
_cell_angle_gamma                60.952(7)
_cell_volume                     1113.3(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.950
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             644
_exptl_absorpt_coefficient_mu    2.771
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.287
_exptl_absorpt_correction_T_max  0.435
_exptl_absorpt_process_details   sadabs

_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_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9014
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_sigmaI/netI    0.0938
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.30
_diffrn_reflns_theta_max         26.02
_reflns_number_total             4219
_reflns_number_gt                2710
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.1029P)^2^+0.1860P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4219
_refine_ls_number_parameters     351
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.1102
_refine_ls_R_factor_gt           0.0634
_refine_ls_wR_factor_ref         0.1822
_refine_ls_wR_factor_gt          0.1515
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.000
_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
Zn1 Zn 0.5000 0.5000 0.0000 0.0210(3) Uani 1 2 d S . .
Zn2 Zn 0.49213(9) 0.40457(9) 0.28511(6) 0.0218(3) Uani 1 1 d . . .
Zn3 Zn 0.15489(9) 0.11381(9) 0.15381(7) 0.0245(3) Uani 1 1 d D . .
C1 C 0.8383(8) 0.2257(8) 0.2528(6) 0.0253(17) Uani 1 1 d D . .
C2 C 0.8324(8) 0.2914(9) 0.0801(6) 0.0258(17) Uani 1 1 d D . .
C3 C 0.3023(8) 0.2699(9) 0.2336(6) 0.0260(17) Uani 1 1 d D . .
C4 C 0.3133(8) 0.3114(9) 0.0646(6) 0.0287(18) Uani 1 1 d . . .
H4 H 0.3007 0.3145 -0.0074 0.026(8) Uiso 1 1 calc R . .
C5 C 0.3235(8) 0.7623(8) 0.2434(6) 0.0249(17) Uani 1 1 d D . .
C6 C 0.3303(8) 0.8226(8) 0.0730(5) 0.0270(18) Uani 1 1 d . . .
H6 H 0.3155 0.8798 0.0010 0.026(8) Uiso 1 1 calc R . .
C7 C 0.4846(8) 0.2818(9) 0.5079(6) 0.0281(18) Uani 1 1 d . . .
C8 C 0.3940(8) 0.2609(9) 0.6072(6) 0.0253(17) Uani 1 1 d . . .
C9 C 0.3027(9) 0.3844(9) 0.6545(6) 0.0280(17) Uani 1 1 d . . .
C10 C 0.3925(8) 0.1242(9) 0.6555(6) 0.0302(18) Uani 1 1 d . . .
C11 C 0.2160(10) 0.3697(9) 0.7448(6) 0.034(2) Uani 1 1 d . . .
C12 C 0.3055(10) 0.1119(9) 0.7445(6) 0.036(2) Uani 1 1 d . . .
C13 C 0.2148(9) 0.2339(9) 0.7881(6) 0.0281(18) Uani 1 1 d . . .
C14 C 0.1152(9) 0.2205(8) 0.8806(5) 0.0259(17) Uani 1 1 d . . .
F1 F 0.3016(6) 0.5201(6) 0.6119(4) 0.0514(14) Uani 1 1 d . . .
F2 F 0.4706(6) 0.0035(6) 0.6104(4) 0.0561(15) Uani 1 1 d . . .
F3 F 0.1296(7) 0.4918(6) 0.7863(4) 0.0576(16) Uani 1 1 d . . .
F4 F 0.3061(7) -0.0259(6) 0.7863(4) 0.0616(17) Uani 1 1 d . . .
N1 N 0.6945(6) 0.3160(7) 0.2211(4) 0.0213(13) Uani 1 1 d . . .
N2 N 0.6902(6) 0.3571(7) 0.1094(5) 0.0233(14) Uani 1 1 d . . .
N3 N 0.9302(6) 0.2088(7) 0.1660(5) 0.0239(14) Uani 1 1 d . . .
N4 N 0.3782(7) 0.3449(7) 0.2043(5) 0.0281(15) Uani 1 1 d . . .
N5 N 0.3839(7) 0.3735(7) 0.0918(5) 0.0287(15) Uani 1 1 d . . .
N6 N 0.2589(7) 0.2412(7) 0.1490(5) 0.0233(14) Uani 1 1 d . . .
N7 N 0.4001(6) 0.6318(7) 0.2135(5) 0.0246(14) Uani 1 1 d . . .
N8 N 0.4049(7) 0.6712(7) 0.1013(5) 0.0280(15) Uani 1 1 d . . .
N9 N 0.2769(7) 0.8877(7) 0.1589(5) 0.0258(14) Uani 1 1 d . . .
O1 O 0.4055(6) 0.3880(6) 0.4275(4) 0.0364(14) Uani 1 1 d . . .
O2 O 0.6198(6) 0.1940(7) 0.5077(4) 0.0439(16) Uani 1 1 d . . .
O3 O -0.0238(7) 0.2698(9) 0.8522(5) 0.064(2) Uani 1 1 d . . .
O4 O 0.1643(6) 0.1669(6) 0.9769(4) 0.0284(12) Uani 1 1 d . . .
O11 O 0.1631(6) 0.0581(7) 0.3437(4) 0.0375(14) Uani 1 1 d D . .
O12 O 0.0877(8) 0.5914(9) 0.3702(6) 0.070(2) Uani 1 1 d . . .
O13 O 0.0672(10) 0.2995(10) 0.4471(7) 0.091(3) Uani 1 1 d . . .
H1 H 0.868(7) 0.182(8) 0.326(2) 0.026(8) Uiso 1 1 d D . .
H2 H 0.871(7) 0.292(8) 0.010(3) 0.026(8) Uiso 1 1 d D . .
H3 H 0.281(8) 0.246(8) 0.305(2) 0.026(8) Uiso 1 1 d D . .
H5 H 0.309(8) 0.772(8) 0.315(3) 0.026(8) Uiso 1 1 d D . .
H11A H 0.102(8) 0.127(5) 0.372(2) 0.05(2) Uiso 1 1 d D . .
H11B H 0.208(8) -0.016(5) 0.394(4) 0.05(2) 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
Zn1 0.0213(6) 0.0206(6) 0.0192(6) -0.0041(5) 0.0017(5) -0.0092(5)
Zn2 0.0220(5) 0.0212(5) 0.0195(4) -0.0052(3) 0.0043(3) -0.0088(4)
Zn3 0.0201(5) 0.0197(5) 0.0329(5) -0.0082(4) 0.0043(4) -0.0086(4)
C1 0.024(4) 0.023(4) 0.026(4) -0.009(3) 0.008(3) -0.009(3)
C2 0.014(4) 0.032(4) 0.023(4) -0.007(3) 0.002(3) -0.005(3)
C3 0.029(4) 0.037(5) 0.019(4) -0.007(3) 0.004(3) -0.022(4)
C4 0.036(5) 0.036(5) 0.024(4) -0.009(3) 0.005(3) -0.025(4)
C5 0.031(4) 0.024(4) 0.019(4) -0.009(3) 0.001(3) -0.012(3)
C6 0.035(4) 0.020(4) 0.015(4) -0.004(3) 0.001(3) -0.004(3)
C7 0.024(4) 0.032(4) 0.030(4) -0.012(4) 0.006(3) -0.013(4)
C8 0.027(4) 0.029(4) 0.021(4) -0.006(3) 0.003(3) -0.015(3)
C9 0.036(4) 0.031(4) 0.025(4) -0.005(3) 0.005(3) -0.024(4)
C10 0.030(4) 0.022(4) 0.032(4) -0.013(3) 0.010(3) -0.006(3)
C11 0.051(5) 0.028(4) 0.032(4) -0.018(4) 0.018(4) -0.024(4)
C12 0.053(5) 0.030(5) 0.020(4) 0.000(3) 0.008(4) -0.021(4)
C13 0.031(4) 0.036(5) 0.022(4) -0.007(3) 0.009(3) -0.021(4)
C14 0.047(5) 0.016(4) 0.014(4) 0.000(3) -0.008(3) -0.014(3)
F1 0.083(4) 0.045(3) 0.046(3) -0.021(2) 0.029(3) -0.046(3)
F2 0.073(4) 0.031(3) 0.053(3) -0.017(2) 0.029(3) -0.018(3)
F3 0.090(4) 0.041(3) 0.051(3) -0.029(3) 0.040(3) -0.037(3)
F4 0.095(4) 0.031(3) 0.056(3) -0.014(3) 0.037(3) -0.033(3)
N1 0.019(3) 0.022(3) 0.019(3) -0.007(2) 0.005(2) -0.007(3)
N2 0.018(3) 0.030(3) 0.023(3) -0.008(3) 0.004(2) -0.012(3)
N3 0.021(3) 0.027(3) 0.022(3) -0.006(3) 0.002(3) -0.011(3)
N4 0.034(4) 0.033(4) 0.022(3) -0.011(3) 0.008(3) -0.019(3)
N5 0.030(4) 0.036(4) 0.024(3) -0.007(3) 0.005(3) -0.019(3)
N6 0.029(3) 0.024(3) 0.025(3) -0.007(3) 0.007(3) -0.020(3)
N7 0.026(3) 0.021(3) 0.021(3) -0.008(3) 0.000(3) -0.006(3)
N8 0.039(4) 0.022(3) 0.022(3) -0.006(3) 0.005(3) -0.015(3)
N9 0.025(3) 0.022(3) 0.026(3) -0.008(3) 0.004(3) -0.008(3)
O1 0.025(3) 0.046(4) 0.022(3) -0.001(3) 0.009(2) -0.010(3)
O2 0.032(3) 0.046(4) 0.032(3) 0.002(3) 0.008(3) -0.009(3)
O3 0.046(4) 0.112(6) 0.031(3) -0.011(4) 0.010(3) -0.041(4)
O4 0.029(3) 0.032(3) 0.024(3) -0.010(2) 0.010(2) -0.014(2)
O11 0.036(4) 0.039(4) 0.029(3) -0.008(3) 0.001(3) -0.011(3)
O12 0.047(4) 0.097(6) 0.051(4) -0.008(4) 0.006(3) -0.028(4)
O13 0.110(7) 0.083(6) 0.077(6) -0.039(5) 0.033(5) -0.041(5)

_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 N2 2.135(6) 2_665 ?
Zn1 N2 2.135(6) . ?
Zn1 N5 2.191(6) . ?
Zn1 N5 2.191(6) 2_665 ?
Zn1 N8 2.226(6) . ?
Zn1 N8 2.226(6) 2_665 ?
Zn2 O1 1.932(5) . ?
Zn2 N1 1.981(6) . ?
Zn2 N4 2.010(6) . ?
Zn2 N7 2.014(6) . ?
Zn3 N3 2.003(6) 1_455 ?
Zn3 N9 2.010(6) 1_545 ?
Zn3 N6 2.022(6) . ?
Zn3 O4 2.178(5) 1_554 ?
Zn3 O11 2.335(6) . ?
C1 N1 1.328(9) . ?
C1 N3 1.357(9) . ?
C2 N2 1.322(8) . ?
C2 N3 1.351(9) . ?
C3 N4 1.296(9) . ?
C3 N6 1.355(9) . ?
C4 N5 1.284(9) . ?
C4 N6 1.351(9) . ?
C5 N7 1.315(9) . ?
C5 N9 1.347(9) . ?
C6 N8 1.313(9) . ?
C6 N9 1.359(9) . ?
C7 O2 1.220(9) . ?
C7 O1 1.269(9) . ?
C7 C8 1.511(10) . ?
C8 C10 1.377(10) . ?
C8 C9 1.401(10) . ?
C9 F1 1.344(9) . ?
C9 C11 1.392(10) . ?
C10 F2 1.346(8) . ?
C10 C12 1.376(10) . ?
C11 F3 1.340(9) . ?
C11 C13 1.358(10) . ?
C12 C13 1.363(11) . ?
C12 F4 1.365(9) . ?
C13 C14 1.489(10) . ?
C14 O4 1.250(8) . ?
C14 O3 1.302(10) . ?
N1 N2 1.372(8) . ?
N3 Zn3 2.003(6) 1_655 ?
N4 N5 1.386(8) . ?
N7 N8 1.381(8) . ?
N9 Zn3 2.010(6) 1_565 ?
O4 Zn3 2.178(5) 1_556 ?

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
N2 Zn1 N2 180.0 2_665 . ?
N2 Zn1 N5 90.1(2) 2_665 . ?
N2 Zn1 N5 89.9(2) . . ?
N2 Zn1 N5 89.9(2) 2_665 2_665 ?
N2 Zn1 N5 90.1(2) . 2_665 ?
N5 Zn1 N5 180.0 . 2_665 ?
N2 Zn1 N8 89.7(2) 2_665 . ?
N2 Zn1 N8 90.3(2) . . ?
N5 Zn1 N8 92.4(2) . . ?
N5 Zn1 N8 87.6(2) 2_665 . ?
N2 Zn1 N8 90.3(2) 2_665 2_665 ?
N2 Zn1 N8 89.7(2) . 2_665 ?
N5 Zn1 N8 87.6(2) . 2_665 ?
N5 Zn1 N8 92.4(2) 2_665 2_665 ?
N8 Zn1 N8 180.0 . 2_665 ?
O1 Zn2 N1 137.8(2) . . ?
O1 Zn2 N4 101.5(2) . . ?
N1 Zn2 N4 101.9(2) . . ?
O1 Zn2 N7 106.1(2) . . ?
N1 Zn2 N7 103.8(2) . . ?
N4 Zn2 N7 99.9(2) . . ?
N3 Zn3 N9 119.6(3) 1_455 1_545 ?
N3 Zn3 N6 119.9(2) 1_455 . ?
N9 Zn3 N6 120.4(3) 1_545 . ?
N3 Zn3 O4 97.9(2) 1_455 1_554 ?
N9 Zn3 O4 89.6(2) 1_545 1_554 ?
N6 Zn3 O4 86.9(2) . 1_554 ?
N3 Zn3 O11 86.2(2) 1_455 . ?
N9 Zn3 O11 90.4(2) 1_545 . ?
N6 Zn3 O11 89.0(2) . . ?
O4 Zn3 O11 175.3(2) 1_554 . ?
N1 C1 N3 111.2(6) . . ?
N2 C2 N3 112.8(6) . . ?
N4 C3 N6 113.5(6) . . ?
N5 C4 N6 114.5(7) . . ?
N7 C5 N9 113.2(6) . . ?
N8 C6 N9 113.6(6) . . ?
O2 C7 O1 125.8(7) . . ?
O2 C7 C8 120.1(7) . . ?
O1 C7 C8 113.9(6) . . ?
C10 C8 C9 115.8(7) . . ?
C10 C8 C7 123.5(7) . . ?
C9 C8 C7 120.7(7) . . ?
F1 C9 C11 119.4(7) . . ?
F1 C9 C8 118.5(6) . . ?
C11 C9 C8 122.1(7) . . ?
F2 C10 C12 119.7(7) . . ?
F2 C10 C8 118.9(7) . . ?
C12 C10 C8 121.3(7) . . ?
F3 C11 C13 120.2(7) . . ?
F3 C11 C9 119.7(7) . . ?
C13 C11 C9 120.1(7) . . ?
C13 C12 F4 119.6(7) . . ?
C13 C12 C10 122.2(7) . . ?
F4 C12 C10 118.2(7) . . ?
C11 C13 C12 118.4(7) . . ?
C11 C13 C14 120.2(7) . . ?
C12 C13 C14 121.4(7) . . ?
O4 C14 O3 124.2(7) . . ?
O4 C14 C13 121.3(7) . . ?
O3 C14 C13 114.5(6) . . ?
C1 N1 N2 107.3(5) . . ?
C1 N1 Zn2 139.6(5) . . ?
N2 N1 Zn2 113.2(4) . . ?
C2 N2 N1 105.6(5) . . ?
C2 N2 Zn1 125.1(5) . . ?
N1 N2 Zn1 129.3(4) . . ?
C2 N3 C1 103.2(6) . . ?
C2 N3 Zn3 123.9(5) . 1_655 ?
C1 N3 Zn3 132.5(5) . 1_655 ?
C3 N4 N5 105.9(6) . . ?
C3 N4 Zn2 134.3(5) . . ?
N5 N4 Zn2 119.6(5) . . ?
C4 N5 N4 105.5(6) . . ?
C4 N5 Zn1 133.7(5) . . ?
N4 N5 Zn1 120.8(5) . . ?
C4 N6 C3 100.7(6) . . ?
C4 N6 Zn3 130.9(5) . . ?
C3 N6 Zn3 128.3(5) . . ?
C5 N7 N8 106.3(6) . . ?
C5 N7 Zn2 137.3(5) . . ?
N8 N7 Zn2 116.1(4) . . ?
C6 N8 N7 105.3(6) . . ?
C6 N8 Zn1 130.6(5) . . ?
N7 N8 Zn1 123.7(4) . . ?
C5 N9 C6 101.6(6) . . ?
C5 N9 Zn3 131.2(5) . 1_565 ?
C6 N9 Zn3 127.2(5) . 1_565 ?
C7 O1 Zn2 120.0(5) . . ?
C14 O4 Zn3 157.4(5) . 1_556 ?

_diffrn_measured_fraction_theta_max 0.962
_diffrn_reflns_theta_full        26.02
_diffrn_measured_fraction_theta_full 0.962
_refine_diff_density_max         1.584
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.188