# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Prof. guangshan zhu'
_publ_contact_author_email       zhugs@mail.jlu.edu.cn

_publ_section_title              
;
A novel low density metal-organic
framework with pcu topology by dendritic ligand

;
loop_
_publ_author_name
'Guangshan Zhu'
'Jiangtao Jia'
'Bian Zheng'
'Lianxun Gao'
'Xiao Liang'
'Fuxing Sun'
'Kun Cai'
'Qianrong Fang'
'Huijun Zhao'

# Attachment '- s1.cif'

data_s1
_database_code_depnum_ccdc_archive 'CCDC 804509'
#TrackingRef '- s1.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C66 H36 O13 Zn4'
_chemical_formula_sum            'C66 H36 O13 Zn4'
_chemical_formula_weight         1298.51

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

_cell_length_a                   20.4586(8)
_cell_length_b                   20.4586(8)
_cell_length_c                   80.370(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     29132(2)
_cell_formula_units_Z            12
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9986
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      25.99

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.50
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.888
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7872
_exptl_absorpt_coefficient_mu    1.015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.549
_exptl_absorpt_correction_T_max  0.602
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 6.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            51924
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -99
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_theta_min         1.26
_diffrn_reflns_theta_max         26.08
_reflns_number_total             6430
_reflns_number_gt                4997
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker saint'
_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          
;
The structure was refined using the SQUEEZE method in the PLATON program.
One (O5) of the caboxylate O atoms has a large U~eq~ value, indicating
partly disorder of O5. This disorder was not modeled because the poor
quality of the data.

DELU instruction of SHELXTL was applied to O5 and O2 atoms.
ISOR instruction of SHELXTL was applied to O5, C15 and C16 atoms.

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^)+(0.1794P)^2^] 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    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6430
_refine_ls_number_parameters     250
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0743
_refine_ls_wR_factor_ref         0.2375
_refine_ls_wR_factor_gt          0.2258
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.092
_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
C1 C 0.3787(2) 0.5541(2) 0.05028(5) 0.0371(8) Uani 1 1 d . . .
C2 C 0.3964(2) 0.5053(2) 0.03923(5) 0.0409(9) Uani 1 1 d . . .
C3 C 0.3375(2) 0.4341(3) 0.03397(5) 0.0506(10) Uani 1 1 d . . .
H1 H 0.2887 0.4156 0.0379 0.061 Uiso 1 1 calc R . .
C4 C 0.3531(2) 0.3928(3) 0.02300(6) 0.0517(11) Uani 1 1 d . . .
H2 H 0.3138 0.3469 0.0192 0.062 Uiso 1 1 calc R . .
C5 C 0.4266(2) 0.4172(2) 0.01719(5) 0.0442(9) Uani 1 1 d . . .
C6 C 0.4833(2) 0.4856(2) 0.02321(6) 0.0489(10) Uani 1 1 d . . .
H4 H 0.5329 0.5028 0.0199 0.059 Uiso 1 1 calc R . .
C7 C 0.4681(3) 0.5288(2) 0.03391(6) 0.0504(10) Uani 1 1 d . . .
H3 H 0.5074 0.5749 0.0376 0.060 Uiso 1 1 calc R . .
C8 C 0.4410(2) 0.3707(2) 0.00525(5) 0.0413(9) Uani 1 1 d . . .
C9 C 0.5108(2) 0.3738(2) 0.00479(5) 0.0406(9) Uani 1 1 d . . .
H5 H 0.5484 0.4046 0.0123 0.049 Uiso 1 1 calc R . .
C10 C 0.5250(2) 0.3306(2) -0.00690(5) 0.0351(8) Uani 1 1 d . . .
C11 C 0.4690(2) 0.2867(2) -0.01832(5) 0.0412(9) Uani 1 1 d . . .
H7 H 0.4780 0.2585 -0.0261 0.049 Uiso 1 1 calc R . .
C12 C 0.3995(2) 0.2841(2) -0.01838(5) 0.0442(10) Uani 1 1 d . . .
C13 C 0.3869(2) 0.3269(3) -0.00643(5) 0.0478(10) Uani 1 1 d . . .
H6 H 0.3408 0.3257 -0.0064 0.057 Uiso 1 1 calc R . .
C14 C 0.3404(2) 0.2397(3) -0.03066(6) 0.0540(12) Uani 1 1 d . . .
C15 C 0.2656(3) 0.2031(4) -0.02667(7) 0.095(2) Uani 1 1 d U . .
H10 H 0.2520 0.2064 -0.0158 0.114 Uiso 1 1 calc R . .
C16 C 0.2090(4) 0.1613(4) -0.03801(8) 0.097(2) Uani 1 1 d U . .
H11 H 0.1587 0.1351 -0.0347 0.116 Uiso 1 1 calc R . .
C17 C 0.2297(3) 0.1596(4) -0.05469(7) 0.0747(16) Uani 1 1 d . . .
C18 C 0.3048(3) 0.1972(3) -0.05889(6) 0.0623(13) Uani 1 1 d . . .
H9 H 0.3188 0.1967 -0.0699 0.075 Uiso 1 1 calc R . .
C19 C 0.3595(3) 0.2352(3) -0.04720(6) 0.0573(12) Uani 1 1 d . . .
H8 H 0.4101 0.2583 -0.0503 0.069 Uiso 1 1 calc R . .
C20 C 0.5979(2) 0.3321(2) -0.00695(5) 0.0323(8) Uani 1 1 d . . .
C21 C 0.5995(2) 0.2646(2) -0.00682(5) 0.0333(8) Uani 1 1 d . . .
H12 H 0.5545 0.2186 -0.0067 0.040 Uiso 1 1 calc R . .
C22 C 0.2166(5) 0.4994(3) 0.09964(9) 0.096(2) Uani 1 1 d . . .
O1 O 0.31116(17) 0.53057(17) 0.05368(4) 0.0506(7) Uani 1 1 d . . .
O2 O 0.2096(2) 0.4822(2) 0.08433(5) 0.0696(10) Uani 1 1 d . . .
O3 O 0.3333 0.6667 0.07665(5) 0.0289(9) Uani 1 3 d S . .
O4 O 0.18151(17) 0.56685(17) 0.05526(4) 0.0512(8) Uani 1 1 d . . .
O5 O 0.2698(5) 0.5663(4) 0.10626(9) 0.167(3) Uani 1 1 d U . .
Zn1 Zn 0.26087(2) 0.56571(2) 0.069132(5) 0.0357(2) Uani 1 1 d . . .
Zn2 Zn 0.3333 0.6667 0.101809(14) 0.0813(4) Uani 1 3 d S . .

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
C1 0.047(2) 0.038(2) 0.0317(19) -0.0018(15) 0.0015(16) 0.0247(18)
C2 0.043(2) 0.043(2) 0.041(2) -0.0082(17) -0.0010(17) 0.0247(18)
C3 0.041(2) 0.060(3) 0.055(3) -0.015(2) -0.0019(19) 0.029(2)
C4 0.040(2) 0.049(2) 0.064(3) -0.018(2) -0.007(2) 0.0215(19)
C5 0.043(2) 0.052(2) 0.046(2) -0.0132(18) -0.0054(17) 0.030(2)
C6 0.044(2) 0.049(2) 0.057(3) -0.0123(19) 0.0008(19) 0.025(2)
C7 0.047(2) 0.039(2) 0.062(3) -0.014(2) 0.001(2) 0.0193(19)
C8 0.036(2) 0.049(2) 0.043(2) -0.0145(17) -0.0066(16) 0.0238(18)
C9 0.038(2) 0.042(2) 0.043(2) -0.0183(17) -0.0104(16) 0.0208(17)
C10 0.0297(18) 0.0359(19) 0.042(2) -0.0081(16) -0.0034(15) 0.0182(15)
C11 0.036(2) 0.041(2) 0.046(2) -0.0178(17) -0.0042(16) 0.0190(17)
C12 0.0309(19) 0.055(2) 0.046(2) -0.0173(19) -0.0092(17) 0.0207(18)
C13 0.035(2) 0.064(3) 0.054(2) -0.024(2) -0.0108(18) 0.032(2)
C14 0.038(2) 0.070(3) 0.049(3) -0.025(2) -0.0130(19) 0.023(2)
C15 0.048(3) 0.149(6) 0.054(3) -0.041(3) -0.005(2) 0.024(3)
C16 0.067(3) 0.120(4) 0.076(3) -0.031(3) 0.000(3) 0.026(3)
C17 0.049(3) 0.096(4) 0.059(3) -0.031(3) -0.023(2) 0.021(3)
C18 0.059(3) 0.082(4) 0.039(2) -0.021(2) -0.010(2) 0.030(3)
C19 0.042(2) 0.078(3) 0.045(2) -0.013(2) -0.0046(19) 0.025(2)
C20 0.0329(18) 0.0287(17) 0.038(2) -0.0039(15) -0.0024(15) 0.0171(15)
C21 0.0298(18) 0.0284(17) 0.040(2) -0.0035(14) 0.0034(15) 0.0132(15)
C22 0.136(6) 0.049(3) 0.074(4) 0.031(3) 0.049(4) 0.024(4)
O1 0.0441(16) 0.0513(17) 0.0586(19) -0.0176(14) 0.0028(14) 0.0255(14)
O2 0.079(2) 0.067(2) 0.058(2) 0.0326(18) 0.0166(18) 0.033(2)
O3 0.0285(12) 0.0285(12) 0.030(2) 0.000 0.000 0.0143(6)
O4 0.0477(17) 0.0483(17) 0.0564(19) -0.0057(14) -0.0230(14) 0.0232(14)
O5 0.211(7) 0.103(4) 0.098(4) 0.036(3) 0.036(4) 0.011(4)
Zn1 0.0355(3) 0.0347(3) 0.0361(3) 0.00207(17) 0.00059(17) 0.0169(2)
Zn2 0.0995(6) 0.0995(6) 0.0449(7) 0.000 0.000 0.0498(3)

_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
C1 O1 1.245(5) . ?
C1 O4 1.248(5) 2_665 ?
C1 C2 1.510(5) . ?
C2 C7 1.363(6) . ?
C2 C3 1.413(6) . ?
C3 C4 1.366(6) . ?
C3 H1 0.9300 . ?
C4 C5 1.406(6) . ?
C4 H2 0.9300 . ?
C5 C6 1.384(6) . ?
C5 C8 1.480(5) . ?
C6 C7 1.376(6) . ?
C6 H4 0.9300 . ?
C7 H3 0.9300 . ?
C8 C13 1.384(5) . ?
C8 C9 1.399(5) . ?
C9 C10 1.415(5) . ?
C9 H5 0.9300 . ?
C10 C11 1.391(5) . ?
C10 C20 1.476(5) . ?
C11 C12 1.396(5) . ?
C11 H7 0.9300 . ?
C12 C13 1.407(6) . ?
C12 C14 1.470(5) . ?
C13 H6 0.9300 . ?
C14 C15 1.364(7) . ?
C14 C19 1.401(6) . ?
C15 C16 1.383(8) . ?
C15 H10 0.9300 . ?
C16 C17 1.411(8) . ?
C16 H11 0.9300 . ?
C17 C18 1.374(8) . ?
C17 C22 1.504(7) 28 ?
C18 C19 1.367(6) . ?
C18 H9 0.9300 . ?
C19 H8 0.9300 . ?
C20 C21 1.387(5) 3_665 ?
C20 C21 1.398(5) . ?
C21 C20 1.387(5) 2_655 ?
C21 H12 0.9300 . ?
C22 O2 1.268(8) . ?
C22 O5 1.361(10) . ?
C22 C17 1.504(7) 34 ?
O1 Zn1 1.964(3) . ?
O2 Zn1 1.928(3) . ?
O3 Zn1 1.9407(14) 3_565 ?
O3 Zn1 1.9408(14) 2_665 ?
O3 Zn1 1.9408(14) . ?
O3 Zn2 2.022(4) . ?
O4 C1 1.248(5) 3_565 ?
O4 Zn1 1.979(3) . ?
O5 Zn2 1.834(6) . ?
Zn2 O5 1.834(6) 2_665 ?
Zn2 O5 1.834(6) 3_565 ?

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
O1 C1 O4 125.5(4) . 2_665 ?
O1 C1 C2 117.5(3) . . ?
O4 C1 C2 117.1(3) 2_665 . ?
C7 C2 C3 118.9(4) . . ?
C7 C2 C1 121.5(4) . . ?
C3 C2 C1 119.6(4) . . ?
C4 C3 C2 119.2(4) . . ?
C4 C3 H1 120.4 . . ?
C2 C3 H1 120.4 . . ?
C3 C4 C5 122.3(4) . . ?
C3 C4 H2 118.9 . . ?
C5 C4 H2 118.9 . . ?
C6 C5 C4 116.7(4) . . ?
C6 C5 C8 122.8(4) . . ?
C4 C5 C8 120.5(4) . . ?
C7 C6 C5 121.6(4) . . ?
C7 C6 H4 119.2 . . ?
C5 C6 H4 119.2 . . ?
C2 C7 C6 121.2(4) . . ?
C2 C7 H3 119.4 . . ?
C6 C7 H3 119.4 . . ?
C13 C8 C9 118.7(3) . . ?
C13 C8 C5 120.3(4) . . ?
C9 C8 C5 120.9(3) . . ?
C8 C9 C10 120.8(3) . . ?
C8 C9 H5 119.6 . . ?
C10 C9 H5 119.6 . . ?
C11 C10 C9 118.7(3) . . ?
C11 C10 C20 120.6(3) . . ?
C9 C10 C20 120.6(3) . . ?
C10 C11 C12 121.5(3) . . ?
C10 C11 H7 119.2 . . ?
C12 C11 H7 119.2 . . ?
C11 C12 C13 118.3(3) . . ?
C11 C12 C14 122.2(4) . . ?
C13 C12 C14 119.6(4) . . ?
C8 C13 C12 122.0(4) . . ?
C8 C13 H6 119.0 . . ?
C12 C13 H6 119.0 . . ?
C15 C14 C19 117.4(4) . . ?
C15 C14 C12 122.1(4) . . ?
C19 C14 C12 120.5(4) . . ?
C14 C15 C16 123.2(5) . . ?
C14 C15 H10 118.4 . . ?
C16 C15 H10 118.4 . . ?
C15 C16 C17 118.3(6) . . ?
C15 C16 H11 120.9 . . ?
C17 C16 H11 120.9 . . ?
C18 C17 C16 119.0(5) . . ?
C18 C17 C22 123.4(5) . 28 ?
C16 C17 C22 117.6(5) . 28 ?
C19 C18 C17 121.2(5) . . ?
C19 C18 H9 119.4 . . ?
C17 C18 H9 119.4 . . ?
C18 C19 C14 120.9(4) . . ?
C18 C19 H8 119.5 . . ?
C14 C19 H8 119.5 . . ?
C21 C20 C21 119.8(4) 3_665 . ?
C21 C20 C10 120.1(3) 3_665 . ?
C21 C20 C10 120.1(3) . . ?
C20 C21 C20 120.2(4) 2_655 . ?
C20 C21 H12 119.9 2_655 . ?
C20 C21 H12 119.9 . . ?
O2 C22 O5 125.5(5) . . ?
O2 C22 C17 117.9(6) . 34 ?
O5 C22 C17 115.5(6) . 34 ?
C1 O1 Zn1 132.9(3) . . ?
C22 O2 Zn1 115.7(4) . . ?
Zn1 O3 Zn1 110.78(11) 3_565 2_665 ?
Zn1 O3 Zn1 110.78(11) 3_565 . ?
Zn1 O3 Zn1 110.78(11) 2_665 . ?
Zn1 O3 Zn2 108.13(12) 3_565 . ?
Zn1 O3 Zn2 108.13(12) 2_665 . ?
Zn1 O3 Zn2 108.13(12) . . ?
C1 O4 Zn1 129.8(3) 3_565 . ?
C22 O5 Zn2 144.3(6) . . ?
O2 Zn1 O3 122.22(17) . . ?
O2 Zn1 O1 103.22(16) . . ?
O3 Zn1 O1 108.97(11) . . ?
O2 Zn1 O4 106.35(15) . . ?
O3 Zn1 O4 110.94(10) . . ?
O1 Zn1 O4 103.36(14) . . ?
O5 Zn2 O5 116.30(16) 2_665 . ?
O5 Zn2 O5 116.29(16) 2_665 3_565 ?
O5 Zn2 O5 116.29(16) . 3_565 ?
O5 Zn2 O3 101.2(2) 2_665 . ?
O5 Zn2 O3 101.2(2) . . ?
O5 Zn2 O3 101.2(2) 3_565 . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.08
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.731
_refine_diff_density_min         -2.137
_refine_diff_density_rms         0.132