# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2009

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Myoung Soo Lah'
_publ_contact_author_email       MSLAH@HANYANG.AC.KR

_publ_section_title              
;
A metal-organic framework based on an unprecedented
nonanuclear cluster as a secondary building unit: structure and gas
sorption behavior
;
loop_
_publ_author_name
'Myoung Soo Lah'
'Jong-San Chang'
'Dohyun Moon'
'Mira Park'
'Jiwoong Yoon'

# Attachment 'mslah_rev21.CIF'

data_l8_08b
_database_code_depnum_ccdc_archive 'CCDC 705881'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C102 H109 N10 O38.50 Zn9'
_chemical_formula_sum            'C102 H109 N10 O38.50 Zn9'
_chemical_formula_weight         2679.32

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           Rhombohedral
_symmetry_space_group_name_H-M   R32

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

_cell_length_a                   21.4718(18)
_cell_length_b                   21.4718(18)
_cell_length_c                   22.420(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     8951.7(18)
_cell_formula_units_Z            3
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6949
_cell_measurement_theta_min      2.73
_cell_measurement_theta_max      27.84

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4107
_exptl_absorpt_coefficient_mu    1.858
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6243
_exptl_absorpt_correction_T_max  0.7310
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(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       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            41726
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         28.31
_reflns_number_total             4924
_reflns_number_gt                4275
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  WinGX

_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. Because of the severe
disorder of one of the lattice solvent sites, the structure refinement was
performed after modification of the data for the electrons of the lattice
solvent region using the PLATON SQUEEZE calculation.
;

_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^)+(0.0596P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.002(16)
_refine_ls_number_reflns         4924
_refine_ls_number_parameters     211
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0339
_refine_ls_wR_factor_ref         0.1016
_refine_ls_wR_factor_gt          0.0996
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.533
_refine_ls_shift/su_mean         0.082

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 0.81813(2) 0.481612(19) 0.768128(14) 0.02856(11) Uani 1 1 d . . .
Zn2 Zn 0.75631(2) 0.3333 0.8333 0.02558(13) Uani 1 2 d S . .
O1M O 0.75768(13) 0.42435(13) 0.8333 0.0220(6) Uani 1 2 d S A .
O1 O 0.81100(14) 0.43799(14) 0.69233(10) 0.0370(6) Uani 1 1 d . . .
O2 O 0.76359(14) 0.32995(15) 0.73629(10) 0.0379(6) Uani 1 1 d . A .
O3 O 0.83537(16) 0.08030(17) 0.56263(11) 0.0425(7) Uani 1 1 d . . .
O4 O 0.82779(16) 0.07908(16) 0.46225(11) 0.0438(7) Uani 1 1 d . . .
C1 C 0.7889(2) 0.2779(2) 0.62928(14) 0.0355(8) Uani 1 1 d . A .
H1 H 0.7890 0.2543 0.6651 0.043 Uiso 1 1 calc R . .
C2 C 0.78424(19) 0.3377(2) 0.63217(15) 0.0334(8) Uani 1 1 d . . .
C3 C 0.7810(2) 0.3720(2) 0.57960(15) 0.0358(8) Uani 1 1 d . A .
H3 H 0.7774 0.4142 0.5822 0.043 Uiso 1 1 calc R . .
C4 C 0.7832(2) 0.3448(2) 0.52471(17) 0.0444(9) Uani 1 1 d . . .
H4 H 0.7802 0.3679 0.4895 0.053 Uiso 1 1 calc R A .
C5 C 0.7952(3) 0.2544(3) 0.46480(16) 0.0524(12) Uani 1 1 d . . .
H5 H 0.7915 0.2756 0.4288 0.063 Uiso 1 1 calc R A .
C6 C 0.8058(3) 0.1964(3) 0.46290(16) 0.0482(10) Uani 1 1 d . A .
H6 H 0.8092 0.1777 0.4254 0.058 Uiso 1 1 calc R . .
C7 C 0.8118(2) 0.1644(2) 0.51563(17) 0.0396(9) Uani 1 1 d . . .
C8 C 0.8051(2) 0.1898(3) 0.56956(16) 0.0418(9) Uani 1 1 d . A .
H8 H 0.8080 0.1673 0.6051 0.050 Uiso 1 1 calc R . .
C9 C 0.7938(2) 0.2490(2) 0.57332(14) 0.0369(8) Uani 1 1 d . . .
C10 C 0.7898(2) 0.2826(2) 0.52031(15) 0.0409(9) Uani 1 1 d . A .
C11 C 0.78488(18) 0.3699(2) 0.69212(14) 0.0313(7) Uani 1 1 d . A .
C12 C 0.8266(2) 0.1039(2) 0.51342(17) 0.0391(9) Uani 1 1 d . A .
O1D O 0.8511(11) 0.335(2) 0.8333(13) 0.0500(15) Uani 1 2 d SDU A -1
C1D C 0.8904(5) 0.3368(6) 0.7967(5) 0.063(3) Uani 0.50 1 d PDU A -1
H1D H 0.8767 0.3348 0.7562 0.076 Uiso 0.50 1 calc PR A -1
N1D N 0.9570(7) 0.3413(9) 0.8089(7) 0.101(5) Uani 0.50 1 d PDU A -1
C2D C 0.9722(14) 0.3424(11) 0.8744(10) 0.167(9) Uani 0.50 1 d PDU A -1
H2D1 H 1.0171 0.3865 0.8841 0.251 Uiso 0.50 1 calc PR A -1
H2D2 H 0.9768 0.3005 0.8846 0.251 Uiso 0.50 1 calc PR A -1
H2D3 H 0.9326 0.3410 0.8973 0.251 Uiso 0.50 1 calc PR A -1
C3D C 0.9915(8) 0.3372(8) 0.7581(11) 0.160(8) Uani 0.50 1 d PDU A -1
H3D1 H 0.9983 0.2954 0.7609 0.239 Uiso 0.50 1 calc PR A -1
H3D2 H 1.0385 0.3811 0.7545 0.239 Uiso 0.50 1 calc PR A -1
H3D3 H 0.9623 0.3323 0.7230 0.239 Uiso 0.50 1 calc PR A -1

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 0.0282(2) 0.02628(19) 0.01946(16) 0.00096(13) -0.00137(13) 0.00480(17)
Zn2 0.02187(19) 0.0265(3) 0.0299(2) 0.0027(2) 0.00135(10) 0.01326(13)
O1M 0.0179(10) 0.0179(10) 0.0241(15) 0.0002(6) -0.0002(6) 0.0044(12)
O1 0.0340(14) 0.0433(15) 0.0251(11) -0.0062(10) -0.0021(10) 0.0130(12)
O2 0.0498(15) 0.0458(15) 0.0264(12) -0.0025(11) 0.0035(10) 0.0301(12)
O3 0.0568(17) 0.070(2) 0.0292(13) -0.0090(12) -0.0083(11) 0.0527(17)
O4 0.0578(17) 0.068(2) 0.0297(13) -0.0098(12) -0.0060(11) 0.0492(16)
C1 0.041(2) 0.054(2) 0.0246(16) -0.0035(15) -0.0015(14) 0.033(2)
C2 0.0303(17) 0.046(2) 0.0261(16) -0.0070(14) -0.0020(13) 0.0210(16)
C3 0.040(2) 0.044(2) 0.0298(17) -0.0025(14) -0.0021(14) 0.0259(17)
C4 0.063(3) 0.055(3) 0.0291(18) 0.0005(16) -0.0032(16) 0.040(2)
C5 0.089(3) 0.068(3) 0.0267(17) -0.0047(18) -0.0053(19) 0.059(3)
C6 0.069(3) 0.074(3) 0.0248(17) -0.0086(19) -0.0020(18) 0.054(3)
C7 0.049(2) 0.060(3) 0.0290(17) -0.0047(16) -0.0016(16) 0.041(2)
C8 0.054(2) 0.068(3) 0.0256(16) -0.0035(17) -0.0034(16) 0.048(2)
C9 0.043(2) 0.059(2) 0.0247(15) -0.0045(16) -0.0036(13) 0.038(2)
C10 0.052(2) 0.065(3) 0.0243(16) -0.0056(17) -0.0034(16) 0.043(2)
C11 0.0249(16) 0.046(2) 0.0256(16) -0.0059(14) -0.0038(12) 0.0196(15)
C12 0.044(2) 0.063(3) 0.0306(17) -0.0072(17) -0.0032(16) 0.042(2)
O1D 0.037(12) 0.063(4) 0.064(3) 0.013(3) -0.001(8) 0.036(12)
C1D 0.040(5) 0.059(6) 0.097(7) -0.005(6) 0.004(5) 0.030(5)
N1D 0.057(6) 0.062(9) 0.187(14) -0.026(11) -0.002(8) 0.031(6)
C2D 0.17(2) 0.059(11) 0.254(15) -0.014(12) -0.150(14) 0.045(12)
C3D 0.059(8) 0.071(10) 0.33(2) -0.033(15) 0.078(11) 0.019(7)

_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 O1 1.909(2) . ?
Zn1 O1M 1.9333(19) . ?
Zn1 O3 1.950(3) 12_666 ?
Zn1 O4 2.034(3) 9_665 ?
Zn1 Zn1 2.9262(8) 16_546 ?
Zn1 Zn2 3.1320(4) . ?
Zn2 O1M 1.9399(15) . ?
Zn2 O1M 1.9396(15) 3_665 ?
Zn2 O1D 2.015(5) . ?
Zn2 O2 2.185(2) 17_556 ?
Zn2 O2 2.185(2) . ?
Zn2 Zn1 3.1320(4) 17_556 ?
O1M Zn1 1.9333(19) 16_546 ?
O1M Zn2 1.9396(15) 2_655 ?
O1 C11 1.277(5) . ?
O2 C11 1.239(4) . ?
O3 C12 1.267(5) . ?
O3 Zn1 1.950(3) 12_656 ?
O4 C12 1.270(4) . ?
O4 Zn1 2.034(3) 14_644 ?
C1 C2 1.339(5) . ?
C1 C9 1.426(5) . ?
C2 C3 1.409(5) . ?
C2 C11 1.508(4) . ?
C3 C4 1.372(5) . ?
C4 C10 1.415(6) . ?
C5 C6 1.376(6) . ?
C5 C10 1.414(5) . ?
C6 C7 1.404(5) . ?
C7 C8 1.363(5) . ?
C7 C12 1.486(6) . ?
C8 C9 1.412(6) . ?
C9 C10 1.415(5) . ?
O1D C1D 1.164(19) . ?
C1D N1D 1.411(12) . ?
N1D C3D 1.386(15) . ?
N1D C2D 1.501(15) . ?

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 Zn1 O1M 119.83(10) . . ?
O1 Zn1 O3 118.81(11) . 12_666 ?
O1M Zn1 O3 110.38(9) . 12_666 ?
O1 Zn1 O4 102.08(11) . 9_665 ?
O1M Zn1 O4 102.68(8) . 9_665 ?
O3 Zn1 O4 98.54(13) 12_666 9_665 ?
O1 Zn1 Zn1 154.65(9) . 16_546 ?
O1M Zn1 Zn1 40.82(6) . 16_546 ?
O3 Zn1 Zn1 86.45(7) 12_666 16_546 ?
O4 Zn1 Zn1 74.08(7) 9_665 16_546 ?
O1 Zn1 Zn2 91.57(8) . . ?
O1M Zn1 Zn2 36.11(3) . . ?
O3 Zn1 Zn2 146.11(8) 12_666 . ?
O4 Zn1 Zn2 88.46(8) 9_665 . ?
Zn1 Zn1 Zn2 63.539(10) 16_546 . ?
O1M Zn2 O1M 121.51(14) . 3_665 ?
O1M Zn2 O1D 118.2(11) . . ?
O1M Zn2 O1D 120.3(11) 3_665 . ?
O1M Zn2 O2 91.03(7) . 17_556 ?
O1M Zn2 O2 93.91(7) 3_665 17_556 ?
O1D Zn2 O2 85.0(9) . 17_556 ?
O1M Zn2 O2 93.91(7) . . ?
O1M Zn2 O2 91.03(8) 3_665 . ?
O1D Zn2 O2 84.9(9) . . ?
O2 Zn2 O2 169.88(13) 17_556 . ?
O1M Zn2 Zn1 35.97(4) . . ?
O1M Zn2 Zn1 136.63(5) 3_665 . ?
O1D Zn2 Zn1 93.9(10) . . ?
O2 Zn2 Zn1 116.54(7) 17_556 . ?
O2 Zn2 Zn1 64.41(7) . . ?
O1M Zn2 Zn1 136.62(5) . 17_556 ?
O1M Zn2 Zn1 35.96(4) 3_665 17_556 ?
O1D Zn2 Zn1 95.8(10) . 17_556 ?
O2 Zn2 Zn1 64.41(7) 17_556 17_556 ?
O2 Zn2 Zn1 116.54(7) . 17_556 ?
Zn1 Zn2 Zn1 170.31(2) . 17_556 ?
Zn1 O1M Zn1 98.36(13) 16_546 . ?
Zn1 O1M Zn2 111.13(2) 16_546 . ?
Zn1 O1M Zn2 107.93(2) . . ?
Zn1 O1M Zn2 107.94(2) 16_546 2_655 ?
Zn1 O1M Zn2 111.14(2) . 2_655 ?
Zn2 O1M Zn2 118.49(14) . 2_655 ?
C11 O1 Zn1 116.5(2) . . ?
C11 O2 Zn2 141.3(2) . . ?
C12 O3 Zn1 120.8(2) . 12_656 ?
C12 O4 Zn1 132.5(2) . 14_644 ?
C2 C1 C9 121.1(3) . . ?
C1 C2 C3 120.4(3) . . ?
C1 C2 C11 119.7(3) . . ?
C3 C2 C11 119.8(3) . . ?
C4 C3 C2 120.5(4) . . ?
C3 C4 C10 120.2(3) . . ?
C6 C5 C10 120.1(3) . . ?
C5 C6 C7 120.9(3) . . ?
C8 C7 C6 119.9(4) . . ?
C8 C7 C12 119.4(4) . . ?
C6 C7 C12 120.7(4) . . ?
C7 C8 C9 120.8(3) . . ?
C8 C9 C10 119.4(3) . . ?
C8 C9 C1 121.8(3) . . ?
C10 C9 C1 118.7(3) . . ?
C5 C10 C4 122.3(3) . . ?
C5 C10 C9 118.8(4) . . ?
C4 C10 C9 118.9(3) . . ?
O2 C11 O1 126.1(3) . . ?
O2 C11 C2 118.6(3) . . ?
O1 C11 C2 115.2(3) . . ?
O3 C12 O4 125.5(4) . . ?
O3 C12 C7 117.4(3) . . ?
O4 C12 C7 117.0(3) . . ?
C1D O1D Zn2 135.3(19) . . ?
O1D C1D N1D 124.1(14) . . ?
C3D N1D C1D 113.1(13) . . ?
C3D N1D C2D 133.3(16) . . ?
C1D N1D C2D 113.3(13) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        28.31
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.094