# 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
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Banglin Chen'
_publ_contact_author_email       BANGLIN@UTPA.EDU

_publ_section_title              
;
A New MOF-505 Analogy Exhibiting High Acetylene Storage
;
loop_
_publ_author_name
'Banglin Chen.'
'Junfeng Bai.'
'Yunxia Hu.'
'Lei Wang.'
'Shengchang Xiang.'
;
Zhuxiu Zhang
;
'Wenwei Zhang.'

# Attachment 'MOF1.cif'

data_cu
_database_code_depnum_ccdc_archive 'CCDC 744108'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            Cu2(C18H6O8)(H2O)2
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H10 Cu2 O10'
_chemical_formula_weight         513.34

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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-3m

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'
'-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                   18.6844(11)
_cell_length_b                   18.6844(11)
_cell_length_c                   32.862(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     9935.3(14)
_cell_formula_units_Z            9
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.8
_cell_measurement_theta_max      28.3

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.772
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2304
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20186
_diffrn_reflns_av_R_equivalents  0.1434
_diffrn_reflns_av_sigmaI/netI    0.1890
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         1.77
_diffrn_reflns_theta_max         28.33
_reflns_number_total             2954
_reflns_number_gt                1209
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

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
_platon_squeeze_void_content
1 -0.033 -0.021 -0.001 6652 1833 ' '
_platon_squeeze_details          
;
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
;
_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 solvent molecules.

Checkcif output:

PLAT432_ALERT_2_A Short Inter X...Y Contact C1 .. C1 .. 2.42 Ang.
PLAT432_ALERT_2_A Short Inter X...Y Contact C1 .. C2 .. 2.76 Ang.
PLAT432_ALERT_2_A Short Inter X...Y Contact C2 .. C2 .. 2.38 Ang.
PLAT432_ALERT_2_A Short Inter X...Y Contact C3 .. C4 .. 2.61 Ang.
PLAT432_ALERT_2_A Short Inter X...Y Contact C4 .. C4 .. 1.17 Ang.
PLAT432_ALERT_2_A Short Inter X...Y Contact C5 .. C6 .. 2.51 Ang.

Due to the high degree of the structural symmetry, only a quarter of the
organic ligand, 5,5'-(ethyne-1,2-diyl)diisophthalate, is given during the
refinement. In fact, all of these carbon atoms referred in PLAT432 Alerts
belong to a single organic ligand. Platon mistakenly judges the contact
between the carbons from the symmetry-related quarters within a single
organic ligand as the inter-molecular contact.

PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for Cu1

Terminal oxygen atom coordinated to copper ion has slightly high thermal
motion.

PLAT430_ALERT_2_B Short Inter D...A Contact O1 .. O1 .. 2.72 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact O1 .. O2 .. 2.78 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact O2 .. O2 .. 2.73 Ang.

These atoms are carbonxylate O atoms bound to two copper ions to form
paddle-wheel nodes. The corresponding distances in other paddle-wheel
compounds also range from 2.72 to 2.78 Ang.

PLAT049_ALERT_1_B Calculated Density less than 1.0 gcm-3 ......... 0.77

The unit cell includes a large region of disordered solvent molecules,
which could not be modeled as discrete atomic sites. We employed
PLATON/SQUEEZE to calculate the diffraction contribution of the
solvent molecules and, thereby, to produce a set of solvent-free d
iffraction intensities. The final density were calculated from
the SQUEEZE results, which is the density for the framework.

Final res file:

TITL c in R-3m
CELL 0.71073 18.6844 18.6844 32.8617 90.000 90.000 120.000
ZERR 9 0.0011 0.0011 0.0039 0.000 0.000 0.000
LATT 3
SYMM -Y, X-Y, Z
SYMM -X+Y, -X, Z
SYMM Y, X, -Z
SYMM X-Y, -Y, -Z
SYMM -X, -X+Y, -Z
SFAC C H O Cu
UNIT 162 90 90 18
REM Fomula "Cu2(C18H6O8)(H2O)2"

L.S. 10
ACTA
BOND
BOND $H
FMAP 2
PLAN 10
WGHT 0.005190
FVAR 1.05031
CU1 4 -0.190051 0.619898 0.199835 10.50000 0.03827 0.02692 =
0.02829 0.00213 0.00106 0.01346
C1 1 -0.096895 0.516274 0.115342 11.00000 0.05683 0.03386 =
0.04722 -0.00092 0.00414 0.02933
C2 1 -0.064151 0.531561 0.076971 11.00000 0.08542 0.04153 =
0.04652 0.01662 0.02196 0.04023
AFIX 43
H2A 2 -0.052848 0.580279 0.063920 11.00000 -1.20000
AFIX 0
C3 1 -0.047473 0.476264 0.057146 10.50000 0.08288 0.05331 =
0.04767 0.01540 0.03081 0.04144
C4 1 -0.012924 0.493538 0.016677 10.50000 0.11459 0.04888 =
0.05483 0.01228 0.02456 0.05730
C5 1 -0.113495 0.443253 0.135143 10.50000 0.04365 0.03972 =
0.03344 0.00247 0.00495 0.02182
AFIX 43
H5A 2 -0.135430 0.432288 0.161301 10.50000 -1.20000
AFIX 0
C6 1 -0.119307 0.574321 0.135672 11.00000 0.03327 0.03768 =
0.04390 -0.00954 -0.00111 0.01104
O1 3 -0.149827 0.554952 0.170930 11.00000 0.05849 0.03903 =
0.04532 -0.00019 0.00899 0.02806
O2 3 -0.108880 0.635936 0.114973 11.00000 0.06886 0.03496 =
0.04623 0.00642 0.02073 0.03007
O3 3 -0.226080 0.547839 0.254780 10.50000 0.11508 0.09055 =
0.06331 0.03984 0.01992 0.04528

HKLF 4

REM c in R-3m
REM R1 = 0.0472 for 1209 Fo > 4sig(Fo) and 0.1052 for all 2954 data
REM 76 parameters refined using 0 restraints

END

WGHT 0.0478 0.0000
REM Highest difference peak 0.543, deepest hole -0.300, 1-sigma level 0.076
Q1 1 -0.3049 0.4549 0.2553 11.00000 0.05 0.54
Q2 1 -0.2434 0.5763 0.2913 11.00000 0.05 0.51
Q3 1 -0.2192 0.5616 0.2936 10.50000 0.05 0.50
Q4 1 -0.2217 0.5567 0.2239 10.50000 0.05 0.47
Q5 1 -0.1582 0.5618 0.2859 11.00000 0.05 0.46
Q6 1 -0.1686 0.6628 0.1841 10.50000 0.05 0.40
Q7 1 -0.1596 0.5909 0.1827 11.00000 0.05 0.38
Q8 1 -0.1211 0.6851 0.1124 11.00000 0.05 0.38
Q9 1 -0.1874 0.6253 0.2291 10.50000 0.05 0.35
Q10 1 -0.1102 0.5387 0.1207 11.00000 0.05 0.28

;

_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^)+(0.0052P)^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         2954
_refine_ls_number_parameters     76
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0472
_refine_ls_wR_factor_ref         0.1101
_refine_ls_wR_factor_gt          0.1077
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_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
Cu1 Cu -0.19005(2) 0.61990(5) 0.19983(2) 0.0324(2) Uani 1 2 d S . .
C1 C -0.0969(3) 0.5163(3) 0.11534(14) 0.0430(12) Uani 1 1 d . . .
C2 C -0.0642(3) 0.5316(3) 0.07697(13) 0.0540(15) Uani 1 1 d . . .
H2A H -0.0528 0.5803 0.0639 0.065 Uiso 1 1 calc R . .
C3 C -0.0475(5) 0.4763(2) 0.0571(2) 0.058(2) Uani 1 2 d S . .
C4 C -0.0129(5) 0.4935(3) 0.01668(18) 0.065(2) Uani 1 2 d S . .
C5 C -0.1135(4) 0.44325(18) 0.13514(18) 0.0385(17) Uani 1 2 d S . .
H5A H -0.1354 0.4323 0.1613 0.046 Uiso 1 2 calc SR . .
C6 C -0.1193(3) 0.5743(3) 0.13567(14) 0.0413(13) Uani 1 1 d . . .
O1 O -0.14983(18) 0.55495(17) 0.17093(9) 0.0460(9) Uani 1 1 d . . .
O2 O -0.10888(18) 0.63594(18) 0.11497(9) 0.0482(10) Uani 1 1 d . . .
O3 O -0.22608(16) 0.5478(3) 0.25478(14) 0.0924(19) Uani 1 2 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
Cu1 0.0383(4) 0.0269(5) 0.0283(4) 0.0021(4) 0.0011(2) 0.0135(3)
C1 0.057(4) 0.034(3) 0.047(3) -0.001(3) 0.004(3) 0.029(3)
C2 0.085(4) 0.042(4) 0.047(3) 0.017(3) 0.022(3) 0.040(4)
C3 0.083(6) 0.053(4) 0.048(4) 0.015(2) 0.031(5) 0.041(3)
C4 0.115(7) 0.049(3) 0.055(6) 0.012(3) 0.025(5) 0.057(4)
C5 0.044(5) 0.040(3) 0.033(4) 0.0025(17) 0.005(3) 0.022(2)
C6 0.033(3) 0.038(3) 0.044(3) -0.010(3) -0.001(3) 0.011(3)
O1 0.058(2) 0.039(2) 0.045(2) -0.0002(18) 0.0090(18) 0.0281(19)
O2 0.069(3) 0.035(2) 0.046(2) 0.0064(17) 0.0207(17) 0.0301(19)
O3 0.115(4) 0.091(4) 0.063(4) 0.040(3) 0.0199(16) 0.045(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
Cu1 O2 1.952(3) 11_565 ?
Cu1 O2 1.952(3) 25_465 ?
Cu1 O1 1.963(3) . ?
Cu1 O1 1.962(3) 23_455 ?
Cu1 O3 2.149(4) . ?
Cu1 Cu1 2.6540(14) 25_465 ?
C1 C2 1.368(5) . ?
C1 C6 1.501(6) . ?
C1 C5 1.399(5) . ?
C2 C3 1.382(5) . ?
C2 H2A 0.9300 . ?
C3 C4 1.443(7) . ?
C3 C2 1.382(5) 24_565 ?
C4 C4 1.173(11) 19_565 ?
C5 C1 1.399(5) 24_565 ?
C5 H5A 0.9300 . ?
C6 O2 1.266(5) . ?
C6 O1 1.262(5) . ?
O2 Cu1 1.952(3) 25_465 ?

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
O2 Cu1 O2 88.87(18) 11_565 25_465 ?
O2 Cu1 O1 90.59(12) 11_565 . ?
O2 Cu1 O1 168.36(12) 25_465 . ?
O2 Cu1 O1 168.36(12) 11_565 23_455 ?
O2 Cu1 O1 90.59(12) 25_465 23_455 ?
O1 Cu1 O1 87.59(17) . 23_455 ?
O2 Cu1 O3 94.97(14) 11_565 . ?
O2 Cu1 O3 94.97(14) 25_465 . ?
O1 Cu1 O3 96.67(14) . . ?
O1 Cu1 O3 96.66(14) 23_455 . ?
O2 Cu1 Cu1 83.67(9) 11_565 25_465 ?
O2 Cu1 Cu1 83.67(9) 25_465 25_465 ?
O1 Cu1 Cu1 84.71(9) . 25_465 ?
O1 Cu1 Cu1 84.71(9) 23_455 25_465 ?
O3 Cu1 Cu1 178.08(16) . 25_465 ?
C2 C1 C6 121.1(4) . . ?
C2 C1 C5 119.4(5) . . ?
C6 C1 C5 119.5(4) . . ?
C1 C2 C3 121.5(5) . . ?
C1 C2 H2A 119.2 . . ?
C3 C2 H2A 119.2 . . ?
C4 C3 C2 120.7(3) . 24_565 ?
C4 C3 C2 120.7(3) . . ?
C2 C3 C2 118.7(6) 24_565 . ?
C4 C4 C3 178.1(12) 19_565 . ?
C1 C5 C1 119.6(6) 24_565 . ?
C1 C5 H5A 120.2 24_565 . ?
C1 C5 H5A 120.2 . . ?
O2 C6 O1 126.6(5) . . ?
O2 C6 C1 116.5(4) . . ?
O1 C6 C1 116.8(4) . . ?
C6 O1 Cu1 121.7(3) . . ?
C6 O2 Cu1 123.3(3) . 25_465 ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        28.33
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.076