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

_publ_section_title              
;
Large H2 Storage Capacity of a New Polyhedron-based
Metal-Organic Framework with High Thermal and Hygric Stability
;
loop_
_publ_author_name
'Myoung Soo Lah'
'Jong-San Chang'
'Seunghee Hong'
'Minhak Oh'
'Mira Park'
'Ji Woong Yoon'

# Attachment 'mslah_rev2.CIF'

data_1
_database_code_depnum_ccdc_archive 'CCDC 707996'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C288 H144 O120 Zn24'
_chemical_formula_weight         7092.91

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'
Zn Zn 0.2839 1.4301 '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'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'z, x+1/2, y+1/2'
'z, -x+1/2, -y+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z+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'
'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, 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'
'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'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'z+1/2, x, y+1/2'
'z+1/2, -x, -y+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, z, -x+1/2'
'y+1/2, -z, -x+1/2'
'-y+1/2, -z, x+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, 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'
'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'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'z+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, -y'
'y+1/2, z+1/2, x'
'-y+1/2, z+1/2, -x'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z+1/2, x'
'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, 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'
'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'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'-x, y+1/2, z+1/2'
'-z, -x+1/2, -y+1/2'
'-z, x+1/2, y+1/2'
'z, x+1/2, -y+1/2'
'z, -x+1/2, y+1/2'
'-y, -z+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'
'-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, -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'
'-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'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y, z+1/2'
'-z+1/2, -x, -y+1/2'
'-z+1/2, x, y+1/2'
'z+1/2, x, -y+1/2'
'z+1/2, -x, y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/2, -z, x+1/2'
'-y+1/2, z, x+1/2'
'y+1/2, z, -x+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, -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'
'-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'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-z+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, y'
'-y+1/2, -z+1/2, -x'
'y+1/2, -z+1/2, x'
'-y+1/2, z+1/2, x'
'y+1/2, z+1/2, -x'
'-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, -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'
'-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'

_cell_length_a                   42.854(5)
_cell_length_b                   42.854(5)
_cell_length_c                   42.854(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     78699(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4347
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      30.25

_exptl_crystal_description       block
_exptl_crystal_colour            'pale brown'
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             14208
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6611
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_process_details   HKL2000-Scalepack

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.77489
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Fixed gap multiple wiggler beamline'
_diffrn_radiation_monochromator  'Pt coated Si double crystal'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            147398
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_sigmaI/netI    0.0145
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_k_min       -55
_diffrn_reflns_limit_k_max       55
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_theta_min         2.26
_diffrn_reflns_theta_max         30.25
_reflns_number_total             4347
_reflns_number_gt                3890
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'PAL ADSC Quantum-210'
_computing_cell_refinement       HKL2000
_computing_data_reduction        HKL2000
_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.
;

_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^)+(0.1653P)^2^+22.0024P] 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    riding
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00045(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         4347
_refine_ls_number_parameters     99
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0653
_refine_ls_wR_factor_ref         0.2434
_refine_ls_wR_factor_gt          0.2344
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_restrained_S_all      1.136
_refine_ls_shift/su_max          0.003
_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 0.871098(8) 0.371098(8) 0.0865(3) Uani 1 4 d S . .
Zn2 Zn 0.0000 0.821355(8) 0.321355(8) 0.0884(3) Uani 1 4 d S . .
O1 O 0.0000 0.90408(8) 0.40408(8) 0.175(3) Uani 1 4 d S . .
O2 O 0.0000 0.78863(7) 0.28863(7) 0.150(2) Uani 1 4 d S . .
O3 O 0.03258(6) 0.84197(6) 0.38774(7) 0.1323(9) Uani 1 1 d . . .
O4 O 0.03265(6) 0.80531(7) 0.35079(6) 0.1295(8) Uani 1 1 d . . .
C1 C 0.04216(8) 0.81728(9) 0.37565(9) 0.1154(10) Uani 1 1 d . . .
C2 C 0.06824(9) 0.80116(9) 0.39227(9) 0.1220(11) Uani 1 1 d . . .
C3 C 0.08249(8) 0.81536(12) 0.41751(8) 0.1102(12) Uani 1 2 d S . .
H3 H 0.0750 0.8348 0.4250 0.132 Uiso 1 2 calc SR . .
C4 C 0.07824(10) 0.77210(11) 0.38198(11) 0.1482(17) Uani 1 1 d . . .
H4 H 0.0677 0.7618 0.3655 0.178 Uiso 1 1 calc R . .
C5 C 0.10382(13) 0.75846(16) 0.39618(13) 0.164(3) Uani 1 2 d S . .
C6 C 0.1137(2) 0.7279(2) 0.3863(2) 0.229(5) Uani 1 2 d S . .
C7 C 0.1218(2) 0.7023(3) 0.3782(2) 0.269(8) Uani 1 2 d S . .
C8 C 0.1358(2) 0.6754(2) 0.3642(2) 0.236(6) Uani 1 2 d S . .
C9 C 0.1232(2) 0.6620(2) 0.3380(2) 0.246(7) Uani 1 2 d S . .
H9 H 0.1052 0.6711 0.3289 0.296 Uiso 1 2 calc SR . .

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 0.0770(4) 0.0913(3) 0.0913(3) -0.0308(3) 0.000 0.000
Zn2 0.0801(4) 0.0925(3) 0.0925(3) -0.0314(3) 0.000 0.000
O1 0.287(9) 0.120(2) 0.120(2) -0.044(3) 0.000 0.000
O2 0.192(6) 0.130(3) 0.130(3) -0.055(3) 0.000 0.000
O3 0.1194(16) 0.1267(18) 0.151(2) -0.0237(16) -0.0263(15) 0.0346(14)
O4 0.1110(15) 0.149(2) 0.1288(17) -0.0297(16) -0.0244(13) 0.0323(14)
C1 0.0958(19) 0.123(2) 0.127(2) -0.0125(19) -0.0086(16) 0.0171(16)
C2 0.111(2) 0.130(3) 0.125(2) -0.031(2) -0.0186(18) 0.0292(18)
C3 0.1114(17) 0.108(3) 0.1114(17) -0.0164(16) -0.005(2) 0.0164(16)
C4 0.140(3) 0.156(3) 0.148(3) -0.060(3) -0.049(3) 0.060(3)
C5 0.161(3) 0.168(5) 0.161(3) -0.082(4) -0.064(4) 0.082(4)
C6 0.235(6) 0.217(8) 0.235(6) -0.141(6) -0.138(7) 0.141(6)
C7 0.261(8) 0.285(11) 0.261(8) -0.184(9) -0.175(9) 0.184(9)
C8 0.244(7) 0.220(8) 0.244(7) -0.146(7) -0.158(8) 0.146(7)
C9 0.239(9) 0.250(8) 0.250(8) -0.165(9) -0.152(8) 0.152(8)

_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 1.999(5) . ?
Zn1 O3 2.004(2) 100 ?
Zn1 O3 2.004(2) 42_554 ?
Zn1 O3 2.004(2) 139_554 ?
Zn1 O3 2.004(2) . ?
Zn1 Zn2 3.0147(7) . ?
Zn2 O2 1.984(4) . ?
Zn2 O4 2.006(2) . ?
Zn2 O4 2.006(2) 100 ?
Zn2 O4 2.006(2) 139_554 ?
Zn2 O4 2.006(2) 42_554 ?
O3 C1 1.248(4) . ?
O4 C1 1.251(4) . ?
C1 C2 1.494(5) . ?
C2 C3 1.383(4) . ?
C2 C4 1.389(5) . ?
C3 C2 1.383(4) 166 ?
C3 H3 0.9500 . ?
C4 C5 1.383(4) . ?
C4 H4 0.9500 . ?
C5 C4 1.383(4) 166 ?
C5 C6 1.441(8) . ?
C6 C7 1.201(9) . ?
C7 C8 1.434(8) . ?
C8 C9 1.371(4) . ?
C8 C9 1.371(4) 59_465 ?
C9 C8 1.371(4) 80_556 ?
C9 H9 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 Zn1 O3 100.88(8) . 100 ?
O1 Zn1 O3 100.88(8) . 42_554 ?
O3 Zn1 O3 87.58(19) 100 42_554 ?
O1 Zn1 O3 100.88(8) . 139_554 ?
O3 Zn1 O3 158.24(16) 100 139_554 ?
O3 Zn1 O3 88.33(18) 42_554 139_554 ?
O1 Zn1 O3 100.88(8) . . ?
O3 Zn1 O3 88.33(18) 100 . ?
O3 Zn1 O3 158.24(16) 42_554 . ?
O3 Zn1 O3 87.58(19) 139_554 . ?
O1 Zn1 Zn2 180.00(14) . . ?
O3 Zn1 Zn2 79.12(8) 100 . ?
O3 Zn1 Zn2 79.12(8) 42_554 . ?
O3 Zn1 Zn2 79.12(8) 139_554 . ?
O3 Zn1 Zn2 79.12(8) . . ?
O2 Zn2 O4 101.67(8) . . ?
O2 Zn2 O4 101.67(8) . 100 ?
O4 Zn2 O4 88.49(17) . 100 ?
O2 Zn2 O4 101.67(8) . 139_554 ?
O4 Zn2 O4 86.82(18) . 139_554 ?
O4 Zn2 O4 156.67(15) 100 139_554 ?
O2 Zn2 O4 101.67(8) . 42_554 ?
O4 Zn2 O4 156.67(15) . 42_554 ?
O4 Zn2 O4 86.82(18) 100 42_554 ?
O4 Zn2 O4 88.49(17) 139_554 42_554 ?
O2 Zn2 Zn1 180.00(13) . . ?
O4 Zn2 Zn1 78.33(7) . . ?
O4 Zn2 Zn1 78.33(8) 100 . ?
O4 Zn2 Zn1 78.33(7) 139_554 . ?
O4 Zn2 Zn1 78.33(7) 42_554 . ?
C1 O3 Zn1 127.6(3) . . ?
C1 O4 Zn2 128.5(2) . . ?
O3 C1 O4 126.5(4) . . ?
O3 C1 C2 116.1(3) . . ?
O4 C1 C2 117.4(3) . . ?
C3 C2 C4 120.4(4) . . ?
C3 C2 C1 120.0(3) . . ?
C4 C2 C1 119.6(3) . . ?
C2 C3 C2 119.8(4) 166 . ?
C2 C3 H3 120.1 166 . ?
C2 C3 H3 120.1 . . ?
C5 C4 C2 118.9(4) . . ?
C5 C4 H4 120.5 . . ?
C2 C4 H4 120.5 . . ?
C4 C5 C4 121.2(5) 166 . ?
C4 C5 C6 119.2(3) 166 . ?
C4 C5 C6 119.2(3) . . ?
C7 C6 C5 180(2) . . ?
C6 C7 C8 167.8(18) . . ?
C9 C8 C9 118.1(7) . 59_465 ?
C9 C8 C7 121.0(3) . . ?
C9 C8 C7 121.0(3) 59_465 . ?
C8 C9 C8 121.9(7) 80_556 . ?
C8 C9 H9 119.0 80_556 . ?
C8 C9 H9 119.0 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        30.25
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.059

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 -0.004 -0.015 -0.005 58763.6 2619.6
_platon_squeeze_details          
; ?
;

#===END

data_2
_database_code_depnum_ccdc_archive 'CCDC 722583'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H6 Cu1 O5'
_chemical_formula_sum            'C288 H144 Cu24 O120'
_chemical_formula_weight         7048.99

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           Cubic
_symmetry_space_group_name_H-M   Fm-3m

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

_cell_length_a                   42.833(3)
_cell_length_b                   42.833(3)
_cell_length_c                   42.833(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     78583(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    12703
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      28.17

_exptl_crystal_description       hexagonal
_exptl_crystal_colour            'pale blue'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             14112
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7993
_exptl_absorpt_correction_T_max  0.9180
_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            95044
_diffrn_reflns_av_R_equivalents  0.1675
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_theta_min         1.58
_diffrn_reflns_theta_max         24.99
_reflns_number_total             3375
_reflns_number_gt                2860
_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.
;

_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^)+(0.0633P)^2^+465.1444P] 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    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3375
_refine_ls_number_parameters     103
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1228
_refine_ls_R_factor_gt           0.0944
_refine_ls_wR_factor_ref         0.1846
_refine_ls_wR_factor_gt          0.1721
_refine_ls_goodness_of_fit_ref   1.273
_refine_ls_restrained_S_all      1.273
_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
Cu1 Cu 0.324805(17) 0.324805(17) 1.0000 0.0298(3) Uani 1 4 d S . .
Cu2 Cu 0.368755(17) 0.368755(17) 1.0000 0.0284(3) Uani 1 4 d S . .
O1 O 0.35089(8) 0.30570(8) 0.96791(7) 0.0435(9) Uani 1 1 d . . .
O2 O 0.38800(8) 0.34314(8) 0.96800(8) 0.0467(9) Uani 1 1 d . . .
O3 O 0.28930(14) 0.28930(14) 1.0000 0.081(3) Uani 1 4 d SD . .
H3O H 0.276(2) 0.296(3) 0.989(3) 0.122 Uiso 0.50 1 d PD . .
O4 O 0.40402(14) 0.40402(14) 1.0000 0.130(5) Uani 1 4 d SD . .
H4O H 0.401(3) 0.4224(6) 1.0000 0.196 Uiso 1 2 d SD . .
C1 C 0.37592(11) 0.31787(12) 0.95781(10) 0.0377(12) Uani 1 1 d . . .
C2 C 0.39243(12) 0.30176(12) 0.93227(11) 0.0459(13) Uani 1 1 d . . .
C3 C 0.38174(13) 0.27330(13) 0.92117(13) 0.0587(16) Uani 1 1 d . . .
H3 H 0.3642 0.2637 0.9307 0.070 Uiso 1 1 calc R . .
C4 C 0.39634(17) 0.2587(2) 0.89634(17) 0.075(3) Uani 1 2 d S . .
C5 C 0.41789(11) 0.31561(17) 0.91789(11) 0.0408(17) Uani 1 2 d S . .
H5 H 0.4256 0.3349 0.9256 0.049 Uiso 1 2 calc SR . .
C6 C 0.3855(2) 0.2279(3) 0.8855(2) 0.101(4) Uani 1 2 d S . .
C7 C 0.3751(2) 0.2054(3) 0.8751(2) 0.123(6) Uani 1 2 d S . .
C8 C 0.3621(2) 0.1776(3) 0.8621(2) 0.124(6) Uani 1 2 d S . .
C9 C 0.3363(2) 0.1637(2) 0.8757(3) 0.112(5) Uani 1 2 d S . .
H9 H 0.3280 0.1720 0.8946 0.134 Uiso 1 2 calc SR . .

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 0.0321(4) 0.0321(4) 0.0254(6) 0.000 0.000 -0.0152(5)
Cu2 0.0317(4) 0.0317(4) 0.0219(6) 0.000 0.000 -0.0143(5)
O1 0.048(2) 0.044(2) 0.0386(19) -0.0158(16) 0.0176(16) -0.0133(17)
O2 0.046(2) 0.049(2) 0.045(2) -0.0176(17) 0.0132(16) -0.0182(17)
O3 0.062(5) 0.062(5) 0.120(10) 0.000 0.000 -0.045(6)
O4 0.053(4) 0.053(4) 0.286(16) 0.000 0.000 -0.032(5)
C1 0.041(3) 0.048(3) 0.024(2) 0.005(2) 0.004(2) -0.004(2)
C2 0.053(3) 0.044(3) 0.040(3) -0.010(2) 0.011(2) -0.012(3)
C3 0.063(4) 0.062(4) 0.051(3) -0.023(3) 0.027(3) -0.031(3)
C4 0.076(4) 0.073(6) 0.076(4) -0.045(4) 0.046(5) -0.045(4)
C5 0.038(2) 0.046(4) 0.038(2) -0.005(2) 0.005(3) -0.005(2)
C6 0.102(6) 0.100(8) 0.102(6) -0.057(6) 0.066(7) -0.057(6)
C7 0.130(7) 0.107(8) 0.130(7) -0.089(7) 0.088(8) -0.089(7)
C8 0.119(6) 0.133(10) 0.119(6) -0.097(7) 0.085(8) -0.097(7)
C9 0.115(6) 0.115(6) 0.105(8) -0.081(6) 0.081(6) -0.069(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
Cu1 O1 1.951(3) 110 ?
Cu1 O1 1.951(3) . ?
Cu1 O1 1.951(3) 13_557 ?
Cu1 O1 1.951(3) 98_557 ?
Cu1 O3 2.151(8) . ?
Cu1 Cu2 2.6622(14) . ?
Cu2 O2 1.940(3) 110 ?
Cu2 O2 1.940(3) . ?
Cu2 O2 1.940(3) 13_557 ?
Cu2 O2 1.940(3) 98_557 ?
Cu2 O4 2.136(9) . ?
O1 C1 1.268(5) . ?
O2 C1 1.277(5) . ?
O3 H3O 0.81(2) . ?
O4 H4O 0.79(2) . ?
C1 C2 1.474(6) . ?
C2 C5 1.386(6) . ?
C2 C3 1.386(7) . ?
C3 C4 1.383(6) . ?
C3 H3 0.9500 . ?
C4 C3 1.383(6) 168_455 ?
C4 C6 1.472(12) . ?
C5 C2 1.386(6) 168_455 ?
C5 H5 0.9500 . ?
C6 C7 1.154(12) . ?
C7 C8 1.427(12) . ?
C8 C9 1.384(6) . ?
C8 C9 1.384(6) 78_456 ?
C9 C8 1.384(6) 60_565 ?
C9 H9 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 89.1(2) 110 . ?
O1 Cu1 O1 89.6(2) 110 13_557 ?
O1 Cu1 O1 167.56(19) . 13_557 ?
O1 Cu1 O1 167.56(19) 110 98_557 ?
O1 Cu1 O1 89.6(2) . 98_557 ?
O1 Cu1 O1 89.1(2) 13_557 98_557 ?
O1 Cu1 O3 96.22(10) 110 . ?
O1 Cu1 O3 96.22(10) . . ?
O1 Cu1 O3 96.22(10) 13_557 . ?
O1 Cu1 O3 96.22(10) 98_557 . ?
O1 Cu1 Cu2 83.78(10) 110 . ?
O1 Cu1 Cu2 83.78(10) . . ?
O1 Cu1 Cu2 83.78(10) 13_557 . ?
O1 Cu1 Cu2 83.78(10) 98_557 . ?
O3 Cu1 Cu2 180.0(2) . . ?
O2 Cu2 O2 88.9(2) 110 . ?
O2 Cu2 O2 89.9(2) 110 13_557 ?
O2 Cu2 O2 168.59(19) . 13_557 ?
O2 Cu2 O2 168.59(19) 110 98_557 ?
O2 Cu2 O2 89.9(2) . 98_557 ?
O2 Cu2 O2 88.9(2) 13_557 98_557 ?
O2 Cu2 O4 95.71(10) 110 . ?
O2 Cu2 O4 95.71(10) . . ?
O2 Cu2 O4 95.71(10) 13_557 . ?
O2 Cu2 O4 95.71(10) 98_557 . ?
O2 Cu2 Cu1 84.29(10) 110 . ?
O2 Cu2 Cu1 84.29(10) . . ?
O2 Cu2 Cu1 84.29(10) 13_557 . ?
O2 Cu2 Cu1 84.29(10) 98_557 . ?
O4 Cu2 Cu1 180.0(2) . . ?
C1 O1 Cu1 123.5(3) . . ?
C1 O2 Cu2 123.3(3) . . ?
Cu1 O3 H3O 105(10) . . ?
Cu2 O4 H4O 127(10) . . ?
O1 C1 O2 125.1(4) . . ?
O1 C1 C2 117.8(4) . . ?
O2 C1 C2 117.1(4) . . ?
C5 C2 C3 119.0(5) . . ?
C5 C2 C1 120.5(5) . . ?
C3 C2 C1 120.5(4) . . ?
C4 C3 C2 120.8(5) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C3 119.4(7) 168_455 . ?
C3 C4 C6 120.3(4) 168_455 . ?
C3 C4 C6 120.3(4) . . ?
C2 C5 C2 121.1(6) 168_455 . ?
C2 C5 H5 119.5 168_455 . ?
C2 C5 H5 119.5 . . ?
C7 C6 C4 173.0(16) . . ?
C6 C7 C8 180(2) . . ?
C9 C8 C9 119.2(9) . 78_456 ?
C9 C8 C7 120.4(4) . . ?
C9 C8 C7 120.4(4) 78_456 . ?
C8 C9 C8 120.6(9) 60_565 . ?
C8 C9 H9 119.7 60_565 . ?
C8 C9 H9 119.7 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.488
_refine_diff_density_min         -1.679
_refine_diff_density_rms         0.061

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 -0.004 -0.017 -0.004 58663.7 15115.1
_platon_squeeze_details          
;
;