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

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'M Schroder'
_publ_contact_author_email       M.SCHRODER@NOTTINGHAM.AC.UK

_publ_section_title              
;
Exceptionally High H2 Storage by a Metal Organic
Polyhedral Framework
;
loop_
_publ_author_name
'M Schroder'
'Alexander Blake'
'Neil Champness'
'Anne Dailly'
'P Hubberstey'
'Xiang Lin'
;
Y.Yan
;
'Sihai Yang'

# Attachment 'cupyda.cif.txt'

data_cupyda1

_database_code_depnum_ccdc_archive 'CCDC 706575'

# SQUEEZE RESULTS (APPEND TO CIF)
# 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
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 -0.004 -0.009 -0.005 76250 11071 ' '

_platon_squeeze_details          
;
Approximately 75% of the unit cell volume comprises a large region of
disordered solvent which could not be modelled as discrete atomic sites.
We employed PLATON SQUEEZE to calculate the contribution to the diffraction
from the solvent region. SQUEEZE estimated a total count of 11071 electrons
per unit cell, and thereby produced a set of solvent-free diffraction
intensities. The final formula was calculated from the TGA results combined
with elemental analysis data.
;

_refine_special_details          
;
Two phenyl rings in the middle of the large organic linker were affected by
disorder problems. These were modelled as two sets of half-occupied carbon
sites with the atoms refined isotropically. Limitations in the disorder
modelling and the very high solvent content are responsible for the
high value for R(int).
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'(Cu3 C48 H30 O15) (C2 H6 S O)8 (C3 H7 N O)15 (H2 O)3'
_chemical_formula_sum            'C109 H189 Cu3 N15 O41 S8'
_chemical_formula_weight         2812.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000 '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'
Cu Cu 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   Fm-3m

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

_cell_length_a                   47.005(3)
_cell_length_b                   47.005(3)
_cell_length_c                   47.005(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     103856(11)
_cell_formula_units_Z            32
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9847
_cell_measurement_theta_min      5.00
_cell_measurement_theta_max      43.95

_exptl_crystal_description       slab
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             47712
_exptl_absorpt_coefficient_mu    0.702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.800
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.6939
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Daresbury SRS Station 9.8'
_diffrn_radiation_monochromator  Si(111)
_diffrn_measurement_device_type  'SMART APEXII CCD area detector'
_diffrn_measurement_method       omega
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            159321
_diffrn_reflns_av_R_equivalents  0.126
_diffrn_reflns_av_sigmaI/netI    0.032
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_k_min       -58
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_theta_min         1.20
_diffrn_reflns_theta_max         25.73
_reflns_number_total             5086
_reflns_number_gt                3877
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       'Bruker APEX2 Version 1.0-27 (Bruker, 2004)'
_computing_cell_refinement       'Bruker SAINT version 7.12A (Bruker, 2004)'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    ' ? '
_computing_publication_material  'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'

_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^)+(0.1857P)^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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5075
_refine_ls_number_parameters     102
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0755
_refine_ls_wR_factor_ref         0.253
_refine_ls_wR_factor_gt          0.243
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_restrained_S_all      1.08
_refine_ls_shift/su_max          0.002
_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 0.340588(9) 0.159412(9) 0.0000 0.0501(3) Uani 1 4 d S . .
Cu2 Cu 0.380723(9) 0.119277(9) 0.0000 0.0521(3) Uani 1 4 d S . .
O1 O 0.32332(5) 0.13548(5) 0.02922(5) 0.0766(7) Uani 1 1 d . . .
O2 O 0.35706(5) 0.10199(5) 0.02935(5) 0.0742(6) Uani 1 1 d . . .
O5 O 0.30859(6) 0.19141(6) 0.0000 0.0844(14) Uani 1 4 d S . .
O6 O 0.41362(8) 0.08638(8) 0.0000 0.128(2) Uani 1 4 d S . .
C1 C 0.33436(7) 0.11298(7) 0.03836(7) 0.0666(8) Uani 1 1 d . . .
C2 C 0.33288(10) 0.07478(7) 0.07478(7) 0.0672(11) Uani 1 2 d S . .
H2A H 0.3506 0.0679 0.0679 0.081 Uiso 1 2 calc SR . .
C3 C 0.31961(8) 0.09804(7) 0.06189(7) 0.0758(10) Uani 1 1 d . . .
C4 C 0.29347(10) 0.10735(9) 0.07141(9) 0.1028(15) Uani 1 1 d . . .
H4A H 0.2845 0.1230 0.0622 0.123 Uiso 1 1 calc R . .
C5 C 0.28000(14) 0.09422(12) 0.09422(12) 0.111(2) Uani 1 2 d S . .
C6 C 0.25203(17) 0.10416(13) 0.10416(13) 0.120(2) Uiso 1 2 d S . .
C7 C 0.2455(2) 0.1023(2) 0.1324(2) 0.107(3) Uiso 0.50 1 d P A 1
H7A H 0.2583 0.0927 0.1447 0.128 Uiso 0.50 1 calc PR A 1
C8 C 0.2197(3) 0.1145(3) 0.1443(3) 0.144(4) Uiso 0.50 1 d P A 1
H8B H 0.2164 0.1151 0.1643 0.173 Uiso 0.50 1 calc PR A 1
C9 C 0.2320(2) 0.1153(2) 0.0868(3) 0.121(3) Uiso 0.50 1 d P A 2
H9A H 0.2358 0.1163 0.0670 0.145 Uiso 0.50 1 calc PR A 2
C10 C 0.2058(3) 0.1256(3) 0.0968(3) 0.144(4) Uiso 0.50 1 d P A 2
H10A H 0.1920 0.1327 0.0837 0.173 Uiso 0.50 1 calc PR A 2
C11 C 0.2001(3) 0.12528(19) 0.12528(19) 0.165(4) Uiso 1 2 d S . .
C12 C 0.1731(3) 0.1371(2) 0.1371(2) 0.193(5) Uiso 1 2 d S A .
C13 C 0.16155(17) 0.1234(3) 0.16155(17) 0.164(4) Uiso 1 2 d S . .
H13A H 0.1695 0.1066 0.1695 0.197 Uiso 1 2 calc SR A .

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 0.0534(3) 0.0534(3) 0.0435(4) 0.000 0.000 0.0148(3)
Cu2 0.0553(3) 0.0553(3) 0.0457(4) 0.000 0.000 0.0184(3)
O1 0.0811(15) 0.0750(14) 0.0737(14) 0.0222(11) 0.0178(11) 0.0230(12)
O2 0.0842(15) 0.0718(13) 0.0667(13) 0.0208(10) 0.0176(11) 0.0228(11)
O5 0.085(2) 0.085(2) 0.083(3) 0.000 0.000 0.041(3)
O6 0.128(4) 0.128(4) 0.130(5) 0.000 0.000 0.079(4)
C1 0.076(2) 0.0693(18) 0.0541(16) 0.0071(14) 0.0024(14) 0.0097(15)
C2 0.079(3) 0.0615(15) 0.0615(15) 0.0078(19) 0.0033(15) 0.0033(15)
C3 0.086(2) 0.076(2) 0.0656(18) 0.0121(16) 0.0114(16) 0.0200(17)
C4 0.116(3) 0.100(3) 0.092(3) 0.038(2) 0.037(2) 0.044(3)
C5 0.105(4) 0.114(3) 0.114(3) 0.043(4) 0.050(3) 0.050(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
Cu1 O1 1.952(2) . ?
Cu1 O5 2.127(4) . ?
Cu1 Cu2 2.6680(8) . ?
Cu2 O2 1.950(2) . ?
Cu2 O6 2.187(5) . ?
O1 C1 1.254(3) . ?
O2 C1 1.259(4) . ?
C1 C3 1.482(5) . ?
C2 C3 1.397(4) . ?
C2 H2A 0.9500 . ?
C3 C4 1.379(5) . ?
C4 C5 1.390(4) . ?
C4 H4A 0.9500 . ?
C5 C6 1.472(9) . ?
C6 C9 1.352(12) . ?
C6 C7 1.365(11) . ?
C7 C8 1.456(15) . ?
C7 H7A 0.9500 . ?
C8 C11 1.379(15) . ?
C8 H8B 0.9500 . ?
C9 C10 1.404(15) . ?
C9 H9A 0.9500 . ?
C10 C11 1.367(15) . ?
C10 H10A 0.9500 . ?
C11 C12 1.494(15) . ?
C12 C13 1.426(8) . ?
C13 H13A 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
O1 Cu1 O1 89.43(15) 99 . ?
O1 Cu1 O1 89.09(16) 174 . ?
O1 Cu1 O1 166.98(13) . 80 ?
O1 Cu1 O5 96.51(6) . . ?
O1 Cu1 Cu2 83.49(6) . . ?
O5 Cu1 Cu2 180.00(11) . . ?
O2 Cu2 O2 90.09(16) 99 . ?
O2 Cu2 O2 167.53(13) 99 174 ?
O2 Cu2 O2 88.56(16) . 174 ?
O2 Cu2 O2 167.53(13) . 80 ?
O2 Cu2 O6 96.24(6) . . ?
O2 Cu2 Cu1 83.76(6) . . ?
C1 O1 Cu1 123.7(2) . . ?
C1 O2 Cu2 123.4(2) . . ?
O1 C1 O2 125.6(3) . . ?
O1 C1 C3 117.5(3) . . ?
O2 C1 C3 117.0(3) . . ?
C3 C2 C3 118.6(4) 112 . ?
C3 C2 H2A 120.7 . . ?
C4 C3 C2 120.4(3) . . ?
C4 C3 C1 120.6(3) . . ?
C2 C3 C1 119.0(3) . . ?
C3 C4 C5 121.0(4) . . ?
C3 C4 H4A 119.5 . . ?
C5 C4 H4A 119.5 . . ?
C4 C5 C4 118.5(5) 112 . ?
C4 C5 C6 120.7(5) . . ?
C9 C6 C9 89.1(11) . 112 ?
C9 C6 C7 117.1(9) . . ?
C9 C6 C7 55.2(6) . 112 ?
C7 C6 C7 94.2(11) . 112 ?
C9 C6 C5 123.6(7) . . ?
C7 C6 C5 119.3(6) . . ?
C6 C7 C8 122.5(11) . . ?
C6 C7 H7A 118.8 . . ?
C8 C7 H7A 118.8 . . ?
C11 C8 C7 116.8(13) . . ?
C11 C8 H8B 121.6 . . ?
C7 C8 H8B 121.6 . . ?
C6 C9 C10 122.9(12) . . ?
C6 C9 H9A 118.6 . . ?
C10 C9 H9A 118.6 . . ?
C11 C10 C9 119.7(14) . . ?
C11 C10 H10A 120.2 . . ?
C9 C10 H10A 120.2 . . ?
C10 C11 C10 88.9(15) 112 . ?
C10 C11 C8 60.3(8) 112 . ?
C10 C11 C8 120.7(14) . . ?
C8 C11 C8 91.8(14) 112 . ?
C10 C11 C12 121.8(10) . . ?
C8 C11 C12 117.5(10) . . ?
C13 C12 C13 125.8(15) . 9 ?
C13 C12 C11 117.1(8) . . ?
C12 C13 C12 114.1(15) . 17 ?
C12 C13 H13A 122.9 . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.73
_diffrn_measured_fraction_theta_full 0.992

_refine_diff_density_max         0.73
_refine_diff_density_min         -0.55
_refine_diff_density_rms         0.07

#=== END of CIF