# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2010


data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Cao, Rong'
_publ_contact_author_email       rcao@fjirsm.ac.cn

_publ_section_title              
;
Construction of a trigonal bipyramidal
cage-based metal-organic framework with hydrophilic
pore surface via flexible tetrapodal ligands
;
loop_
_publ_author_name
'Tian-Fu Liu'
'Jian Li'
'Xi Lin'
'Rong Cao'

# Attachment '- 780176.cif'

data_1
_database_code_depnum_ccdc_archive 'CCDC 780176'
#TrackingRef '- 780176.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C49.50 H36 N0 O19 Zn4'
_chemical_formula_weight         1196.26

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R-3c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   26.918(4)
_cell_length_b                   26.918(4)
_cell_length_c                   86.67(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     54386(17)
_cell_formula_units_Z            12
_cell_measurement_temperature    78(2)
_cell_measurement_reflns_used    8178
_cell_measurement_theta_min      2.3587
_cell_measurement_theta_max      27.4797

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7260
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  0.897
_exptl_absorpt_correction_T_min  0.897
_exptl_absorpt_process_details   crystalclear

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      78(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  
;
Saturn70 (4x4 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            130957
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_sigmaI/netI    0.0439
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -112
_diffrn_reflns_limit_l_max       107
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         27.45
_reflns_number_total             13777
_reflns_number_gt                8236
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  '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.

SQUEEZE routine of PLATON was applied to remove the contributions to the
scattering from the disordered solvent molecules.

Restraints both on geometry and thermal parameters of disordered atoms were used
during the LS refinement (DELU and SIMU functions of SHELXL-97).

;

_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^)+(0.1730P)^2^+0.0000P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13777
_refine_ls_number_parameters     219
_refine_ls_number_restraints     96
_refine_ls_R_factor_all          0.1323
_refine_ls_R_factor_gt           0.0855
_refine_ls_wR_factor_ref         0.2850
_refine_ls_wR_factor_gt          0.2446
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.001
_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 0.0000 0.0000 0.137282(7) 0.0782(2) Uani 1 3 d S . .
O1 O 0.06615(13) -0.00152(14) 0.12870(4) 0.1223(10) Uani 1 1 d . . .
C1 C 0.1005(2) -0.0134(2) 0.13553(6) 0.1201(14) Uani 1 1 d . . .
Zn2 Zn -0.072215(16) -0.064246(17) 0.167142(4) 0.08229(19) Uani 1 1 d . . .
O2 O 0.10458(17) -0.01898(17) 0.15042(4) 0.1428(12) Uani 1 1 d . . .
C2 C 0.14603(18) -0.01526(19) 0.12605(5) 0.1073(11) Uani 1 1 d U . .
O3 O 0.27711(11) -0.01606(11) 0.10124(3) 0.1009(7) Uani 1 1 d . . .
C3 C 0.15397(19) 0.0019(2) 0.11083(5) 0.1150(12) Uani 1 1 d U . .
H3 H 0.1300 0.0144 0.1063 0.138 Uiso 1 1 calc R . .
O4 O 0.43068(11) 0.06626(12) 0.06470(3) 0.1130(8) Uani 1 1 d . . .
C4 C 0.19702(18) 0.0011(2) 0.10206(5) 0.1146(12) Uani 1 1 d U . .
H4 H 0.2020 0.0125 0.0915 0.138 Uiso 1 1 calc R . .
O5 O 0.55197(12) 0.25585(13) 0.01310(3) 0.1138(8) Uani 1 1 d . . .
C5 C 0.23184(17) -0.01598(17) 0.10862(4) 0.0971(10) Uani 1 1 d U . .
O6 O 0.61331(14) 0.22186(17) 0.01439(5) 0.1466(13) Uani 1 1 d . . .
C6 C 0.2235(2) -0.0345(2) 0.12345(6) 0.1271(13) Uani 1 1 d U . .
H6 H 0.2469 -0.0481 0.1277 0.153 Uiso 1 1 calc R . .
O7 O 0.0000 0.0000 0.15975(4) 0.0712(8) Uani 1 3 d S . .
C7 C 0.1809(2) -0.0339(2) 0.13249(5) 0.1277(13) Uani 1 1 d U . .
H7 H 0.1759 -0.0460 0.1429 0.153 Uiso 1 1 calc R . .
C8 C 0.29692(14) 0.01583(14) 0.08739(4) 0.0840(8) Uani 1 1 d . . .
H8A H 0.3009 0.0542 0.0887 0.101 Uiso 1 1 calc R . .
H8B H 0.2692 -0.0042 0.0790 0.101 Uiso 1 1 calc R . .
C9 C 0.35540(15) 0.02206(15) 0.0833 0.0760(10) Uani 1 2 d S . .
C10 C 0.37884(15) 0.06352(15) 0.06961(4) 0.0916(9) Uani 1 1 d . . .
H10A H 0.3506 0.0496 0.0611 0.110 Uiso 1 1 calc R . .
H10B H 0.3864 0.1021 0.0727 0.110 Uiso 1 1 calc R . .
C11 C 0.46036(17) 0.10422(19) 0.05313(5) 0.1148(12) Uani 1 1 d U . .
C12 C 0.44540(19) 0.1399(2) 0.04620(6) 0.1223(13) Uani 1 1 d U . .
H12 H 0.4112 0.1394 0.0492 0.147 Uiso 1 1 calc R . .
C13 C 0.47982(19) 0.1775(2) 0.03461(6) 0.1219(13) Uani 1 1 d U . .
H13 H 0.4679 0.2013 0.0296 0.146 Uiso 1 1 calc R . .
C14 C 0.53047(18) 0.1808(2) 0.03032(6) 0.1167(13) Uani 1 1 d U . .
C15 C 0.5467(2) 0.1443(2) 0.03754(6) 0.1350(15) Uani 1 1 d U . .
H15 H 0.5815 0.1458 0.0347 0.162 Uiso 1 1 calc R . .
C16 C 0.5116(2) 0.1061(2) 0.04880(6) 0.1354(15) Uani 1 1 d U . .
H16 H 0.5223 0.0811 0.0536 0.162 Uiso 1 1 calc R . .
C17 C 0.56761(19) 0.2223(2) 0.01848(5) 0.1132(13) Uani 1 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 0.0854(3) 0.0854(3) 0.0640(4) 0.000 0.000 0.04270(15)
O1 0.122(2) 0.144(2) 0.119(3) 0.0109(18) 0.0243(17) 0.080(2)
C1 0.148(4) 0.135(3) 0.104(3) 0.018(3) 0.034(3) 0.091(3)
Zn2 0.0869(3) 0.0920(3) 0.0677(3) 0.00295(16) -0.00030(16) 0.0445(2)
O2 0.177(3) 0.186(3) 0.113(3) 0.024(2) 0.038(2) 0.127(3)
C2 0.116(3) 0.130(3) 0.095(3) 0.021(2) 0.028(2) 0.076(2)
O3 0.1118(17) 0.1178(17) 0.0816(16) 0.0156(13) 0.0276(13) 0.0639(14)
C3 0.112(3) 0.157(3) 0.093(3) 0.012(2) 0.016(2) 0.080(2)
O4 0.1032(17) 0.1250(19) 0.118(2) 0.0383(16) 0.0370(15) 0.0624(15)
C4 0.115(3) 0.156(3) 0.084(2) 0.009(2) 0.0168(19) 0.076(2)
O5 0.114(2) 0.1159(19) 0.105(2) 0.0250(16) 0.0087(15) 0.0527(17)
C5 0.110(2) 0.117(2) 0.081(2) 0.0086(18) 0.0246(18) 0.068(2)
O6 0.121(2) 0.172(3) 0.153(3) 0.062(3) 0.051(2) 0.077(2)
C6 0.147(3) 0.163(3) 0.109(3) 0.026(3) 0.034(3) 0.106(3)
O7 0.0753(12) 0.0753(12) 0.063(2) 0.000 0.000 0.0377(6)
C7 0.156(3) 0.158(3) 0.100(3) 0.032(2) 0.041(2) 0.102(3)
C8 0.089(2) 0.088(2) 0.0688(19) -0.0036(15) 0.0056(15) 0.0395(16)
C9 0.0817(18) 0.0817(18) 0.061(2) -0.0019(9) 0.0019(9) 0.038(2)
C10 0.089(2) 0.093(2) 0.092(2) 0.0060(18) 0.0132(17) 0.0449(17)
C11 0.100(2) 0.127(3) 0.124(3) 0.037(2) 0.026(2) 0.061(2)
C12 0.105(3) 0.132(3) 0.134(3) 0.037(3) 0.030(2) 0.063(2)
C13 0.106(3) 0.134(3) 0.128(3) 0.042(2) 0.020(2) 0.062(2)
C14 0.101(2) 0.122(3) 0.124(3) 0.035(2) 0.025(2) 0.054(2)
C15 0.121(3) 0.146(3) 0.151(4) 0.057(3) 0.038(3) 0.077(3)
C16 0.123(3) 0.146(3) 0.152(4) 0.058(3) 0.046(3) 0.078(3)
C17 0.102(3) 0.120(3) 0.108(3) 0.030(2) 0.015(2) 0.048(2)

_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 O7 1.947(4) . ?
Zn1 O1 1.949(3) . ?
Zn1 O1 1.949(3) 3 ?
Zn1 O1 1.949(3) 2 ?
O1 C1 1.266(6) . ?
C1 O2 1.311(6) . ?
C1 C2 1.497(6) . ?
Zn2 O2 1.920(3) 3 ?
Zn2 O6 1.923(3) 34_545 ?
Zn2 O7 1.9541(12) . ?
Zn2 O5 1.966(3) 35_445 ?
O2 Zn2 1.920(3) 2 ?
C2 C3 1.379(6) . ?
C2 C7 1.382(6) . ?
O3 C5 1.377(4) . ?
O3 C8 1.416(4) . ?
C3 C4 1.395(5) . ?
C3 H3 0.9500 . ?
O4 C11 1.368(4) . ?
O4 C10 1.425(4) . ?
C4 C5 1.358(6) . ?
C4 H4 0.9500 . ?
O5 C17 1.261(5) . ?
O5 Zn2 1.966(3) 29 ?
C5 C6 1.356(6) . ?
O6 C17 1.286(5) . ?
O6 Zn2 1.923(3) 28 ?
C6 C7 1.397(6) . ?
C6 H6 0.9500 . ?
O7 Zn2 1.9541(12) 2 ?
O7 Zn2 1.9541(12) 3 ?
C7 H7 0.9500 . ?
C8 C9 1.538(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.534(4) . ?
C9 C10 1.534(4) 18_544 ?
C9 C8 1.538(4) 18_544 ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.354(6) . ?
C11 C16 1.406(6) . ?
C12 C13 1.398(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.373(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.405(6) . ?
C14 C17 1.478(6) . ?
C15 C16 1.390(6) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?

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
O7 Zn1 O1 112.44(12) . . ?
O7 Zn1 O1 112.44(12) . 3 ?
O1 Zn1 O1 106.35(13) . 3 ?
O7 Zn1 O1 112.44(12) . 2 ?
O1 Zn1 O1 106.35(13) . 2 ?
O1 Zn1 O1 106.35(13) 3 2 ?
C1 O1 Zn1 128.1(3) . . ?
O1 C1 O2 127.1(4) . . ?
O1 C1 C2 117.7(4) . . ?
O2 C1 C2 114.8(5) . . ?
O2 Zn2 O6 115.06(19) 3 34_545 ?
O2 Zn2 O7 111.66(15) 3 . ?
O6 Zn2 O7 110.67(12) 34_545 . ?
O2 Zn2 O5 103.99(14) 3 35_445 ?
O6 Zn2 O5 103.84(15) 34_545 35_445 ?
O7 Zn2 O5 111.12(10) . 35_445 ?
C1 O2 Zn2 129.7(3) . 2 ?
C3 C2 C7 119.3(4) . . ?
C3 C2 C1 120.4(4) . . ?
C7 C2 C1 120.3(4) . . ?
C5 O3 C8 117.3(3) . . ?
C2 C3 C4 120.4(4) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C11 O4 C10 116.7(3) . . ?
C5 C4 C3 119.8(4) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C17 O5 Zn2 130.1(3) . 29 ?
C6 C5 C4 120.4(3) . . ?
C6 C5 O3 115.1(4) . . ?
C4 C5 O3 124.6(3) . . ?
C17 O6 Zn2 132.5(3) . 28 ?
C5 C6 C7 120.9(4) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
Zn1 O7 Zn2 109.15(10) . 2 ?
Zn1 O7 Zn2 109.15(10) . 3 ?
Zn2 O7 Zn2 109.79(10) 2 3 ?
Zn1 O7 Zn2 109.15(10) . . ?
Zn2 O7 Zn2 109.79(10) 2 . ?
Zn2 O7 Zn2 109.79(10) 3 . ?
C2 C7 C6 119.2(4) . . ?
C2 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
O3 C8 C9 108.3(3) . . ?
O3 C8 H8A 110.0 . . ?
C9 C8 H8A 110.0 . . ?
O3 C8 H8B 110.0 . . ?
C9 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
C10 C9 C10 110.6(4) . 18_544 ?
C10 C9 C8 111.22(19) . 18_544 ?
C10 C9 C8 106.43(18) 18_544 18_544 ?
C10 C9 C8 106.43(18) . . ?
C10 C9 C8 111.24(19) 18_544 . ?
C8 C9 C8 111.0(4) 18_544 . ?
O4 C10 C9 107.8(3) . . ?
O4 C10 H10A 110.2 . . ?
C9 C10 H10A 110.2 . . ?
O4 C10 H10B 110.2 . . ?
C9 C10 H10B 110.2 . . ?
H10A C10 H10B 108.5 . . ?
C12 C11 O4 125.8(4) . . ?
C12 C11 C16 119.4(4) . . ?
O4 C11 C16 114.7(4) . . ?
C11 C12 C13 120.5(4) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C14 C13 C12 121.2(4) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C13 C14 C15 118.7(4) . . ?
C13 C14 C17 120.7(4) . . ?
C15 C14 C17 120.6(4) . . ?
C16 C15 C14 119.7(4) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C15 C16 C11 120.4(4) . . ?
C15 C16 H16 119.8 . . ?
C11 C16 H16 119.8 . . ?
O5 C17 O6 124.7(4) . . ?
O5 C17 C14 117.2(4) . . ?
O6 C17 C14 118.2(4) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.039
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.060

# SQUEEZE RESULTS
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.054 -0.065 -0.001 44086.7 1080.9
_platon_squeeze_details          
;
;